s WHC-SP-1182

UC-2070

Analysis of Sludge from Hanford K East Basin Floor and Weasel Pit

Contributors:

T. L. W e l s h , Statistics and Chemistry R. B. Baker, In-Basin Experience D. R. H a n s e n , Organic Chemistry Westinghouse Hanford Company

G. R. Golcar , Physical Properties Pacific Northwest National Laboratory

Compiled and Edited by:

B. J. Makenas

Date Published April 1996

Prepared for the U.S. Department of Energy Office of Environmental Restoration and Waste Management

Westinghouse p.o BOX 1970 H a n f o r d C o m p a n y Richland, Washington

Management and Operations Contractor for the U.S. Department of Energy under Contract DE-AC06-87RL10930

Approved for Public Release

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ANALYSIS OF SLUDGE FROM K EAST BASIN FLOOR AND WEASEL PIT E WHO Project or Program

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Document Number: WHC-SP-1182

Document Title- ANALYSIS OF SLUDGE FROM HANFORD K EAST BASIN FLOOR AND WEASEL PIT

Release Date: 5/4/96

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WHC-SP-1182

Document Title: ANALYSIS OF SLUDGE FROM THE HANFORD K EAST BASIN FLOOR AND WEASEL PIT

Compiled by:

Reviewed by:

Reviewed by:

Reviewed by:

Approved by:

ST^^^^y *-/'/?* B. J. Makenas Date Spent Nuclear Fuel Evaluations

f6 6a£*~ *7*/?C R. B. Baker Date Spent Nuclear Fuel Evaluations

T. L. Welsh Date Process Chemistry and Statistics

Gjfc>tM^ Ux- 5\^\i(o G. R. Golttr Da Pacific Northwest National Laboratory

Lui^o zlMsk-R. P< Dmberg, Manages Date Spent Nuclear Fuel Evaluations

n

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ACKNOWLEDGEMENT

The analyses and inferences in this report draw heavily on the data reports from George Miller and Kurt Silvers and the work of their respective laboratory staffs at Hanford 222-S and 325 Buildings. Dave Bechtold and Bev Crawford of 222-S Laboratory, provided many of the initial observations and insights, and Kathleen Pearce provided the primary interface with the Tank Waste Arena. Many helpful discussions with Joel Tingey and Evan Jensen of the 325 Building laboratory are gratefully acknowledged. Finally the equipment development which made sampling possible is due to the particular efforts of Al Bridges and Paul MacFarlan.

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ANALYSIS OF SLUDGE FROM THE HANFORD K EAST BASIN FLOOR AND WEASEL PIT

Contributors: T. L. Welsh, Statistics and Chemistry G. R. Golcar,* Physical Properties R. B. Baker, In-Basin Sampling Experience D. R. Hansen, Organic Chemistry

Compiled and Edited By: B. J. Makenas

ABSTRACT

Sludge samples from the floor of the Hanford K East Basin fuel storage

pool have been retrieved and analyzed. Both chemical and physical properties

have been determined. The results are to be used to determine the disposition

of the bulk of the sludge and possibly assess the impact of residual sludge on

dry storage of the associated intact metallic uranium fuel elements.

♦Pacific Northwest National Laboratory.

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CONTENTS

1.0 SUMMARY AND CONCLUSIONS 1 1.1 SAMPLE GATHERING AND ANALYSIS 2 1.2 CONCLUSION 5

2.0 INTRODUCTION 9 3.0 RESULTS, ANALYSIS, AND EXPLANATION OF APPENDICES 12

3.1 IN-BASIN SAMPLING EXPERIENCE 12 3.2 CHEMISTRY AND PHYSICAL PROPERTIES 15

4.0 DISCUSSION AND CAUTIONS 31 5.0 REFERENCES 46

APPENDIX A DEPTHS OF SLUDGE OBSERVED DURING SAMPLING AND THE REVISED CALCULATED VOLUME OF SLUDGE IN THE K EAST WEASEL PIT A-l

APPENDIX B THE CHEMISTRY OF CENTRIFUGED SLUDGE B-l APPENDIX C THE CHEMISTRY OF AS-SETTLED SLUDGE C-l APPENDIX D THE CHEMISTRY OF DRIED SLUDGE D-l APPENDIX E MAPS OF ANALYTE CONCENTRATION VERSUS

BASIN LOCATION E-l APPENDIX F STATISTICAL ANALYSIS OF CHEMISTRY DATA F-l APPENDIX G ORGANIC CHEMISTRY G-l APPENDIX H SUMMARY OF POLYCHLORINATED BIPHENYL RESULTS H-l APPENDIX I VISCOSITY, PARTICLE SIZE, AND ZETA POTENTIAL .... 1-1 APPENDIX J EXAMPLES OF SLUDGE PARTICLE SHAPES J-l APPENDIX K COMPOUNDS DETECTED USING X-RAY DIFFRACTION

AND ELECTRON DIFFRACTION K-l APPENDIX L SETTLING TIMES L-l APPENDIX M THERMO-GRAVIMETRIC ANALYSIS M-l APPENDIX N REGRESSION ANALYSIS FOR EUROPIUM ISOTOPES VERSUS

PLUTONIUM CONTENT IN SLUDGE N-l

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LIST OF FIGURES

1.1. K East Basin Fuel Sludge was Sampled from the Floor Between Canisters 6

1.2. Locations for Sampling of Sludge in the Hanford K East Basin . . . 6 1.3. Example Particle Size Distribution for K Basin Sludge 7 1.4. Settling of K East Basin Sludge 8 1.5. Example of Thermo-Gravimetric Analysis Drying Curve

for K East Basin Floor Sludge 8 2.1. Flow Chart of Sludge Sample Processing and Analyses 11 3.1. Overview of the Equipment Developed for Sampling the Sludges

on the Floor of the K East Basin and Remote Pits 23 3.2. Examples of the 10.2 cm (4 inch) and 5.1 cm (2 inch) Diameter

Isolation Tubes Inserted in K East Sludge 24 3.3. Preparations of Sample Bottles, their Associated Shielding

and Cart (holding bottles and pump) on Basin Grating 25 3.4. Overview of Sampling Activity on Grating 26 3.5. Sample Bottle KES-E-11 in Analytical Laboratory Hot Cell

not Long After Sampling in K Basin 27 3.6. Nozzle Used on Extraction Tube with Openings to Exclude

Particles Greater than 6.4 mm (0.25 inch) in Diameter 27 3.7. Final Sample Locations in K East Weasel Pit 28 3.8. Final Sample Locations in the K East Main Basin 29 3.9. The Appearance of As-Settled K East Basin Floor Sludge 30

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LIST OF TABLES

3.1. Final Sludge Sample Detail 18 3.2. Sampling Dates and General Observations 21 4.1. Sludge Characterization Data—Per Gram Centrifuged Sludge .... 33 4.2. Sludge Characterization Data—Per Gram As-Settled Sludge 36 4.3. Sludge Characterization Data—Per mL As-Settled Sludge 39 4.4. Sludge Characterization Data—Per Gram Dried Sludge 42 4.5. Comparison of Latest Data for Dried K East Basin Floor Sludge

Versus Earlier Data for the K East Basin Floor 44 4.6. Comparison of Latest K East Floor Sludge Data with Previous

Sandfilter Backwash Pit Data 45

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ANALYSIS OF SLUDGE FROM THE HANFORD K EAST BASIN FLOOR AND WEASEL PIT

1.0 SUMMARY AND CONCLUSIONS

The two Hanford K Basins are water-filled concrete pools which contain over 2,000 tons of N Reactor metal fuel elements stored in aluminum or stainless steel canisters. Associated with this Spent Nuclear Fuel (SNF) is an accumulation of particulate layered material which is generally called sludge. Sludge is found on the basin floors, in canisters, and in the basin pits which are used for miscellaneous tasks such as cask handling. In fact, 14 different types of sludge have been tentatively identified depending on which basin, canister type, or pit location that the particular sludge is found. Each type of sludge is a unique nonhomogeneous mixture possibly containing corroded fuel, debris such as windblown sand or insects, rack and canister corrosion products, and/or fission products. All of the various sludges will need to be transported away from the K Basins and disposed. This report addresses the characterization of sludge found on the K East Basin floor and that currently found in the K East Basin Weasel Pit.

Measurements of sludge depths in the K East Basin were reported previously (Makenas 1994; Baker 1995a) and have shown that the floor is covered with sludge to a depth of 5 to 19 cm (2 to 7.5 in.), with a calculated volume of 21.7 m3 (765 ft3). Some of the canisters in K East Basin have screened bottoms and slotted sides. All of the K East canisters are open top (Figure 1.1). This means that fuel corrosion products (uranium oxide and fission products mostly) found in canisters have, to some extent, mixed with the expected wind blown debris and corrosion products (from aluminum canisters and steel racks) in basin areas which are in close proximity to canisters. Also sludge retrieved from the Basin for processing and disposal will, at least initially, contain a significant amount of water. This is because any foreseeable sludge retrieval method will entrain basin water and, perhaps, add additional water to aid the suspension and transport of sludge through pipes and equipment.

The central problem addressed in the current sludge characterization effort is "What is an acceptable way to retrieve sludge from the K East Basin (and Weasel Pit) and to process, transport, and store the material until a permanent repository becomes available?" The first part of this effort (i.e., retrieval, transportation, and processing of the sludge) will possibly require the specification, design, and fabrication of sludge handling/ processing/dewatering equipment or the procurement of similar commercial services. Sludge will, for example, need to be pumped and dewatered with devices such as filters and hydrocyclones. Such an effort will require the knowledge of various physical parameters (i.e., fluid viscosity, particle size, etc.) which could be used directly to design equipment and/or could be utilized to specify sludge simulants which can be used for evaluation of candidate equipment. Furthermore, knowledge of the Special Nuclear Materials content of the sludge will also be necessary to maintain accountability of material which leaves the Basin.

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The second part of the problem is to designate a storage method whereby sludge can be stored away from K Basins in a more environmentally acceptable area. Two prime alternatives for storage have been identified. These are (1) transferring sludge to Hanford double shell waste tanks and ultimate disposition along with other tank wastes, or (2) processing the sludge into a form (dry or grout) appropriate for solid waste disposal. In these two cases the chemistry of the sludge must be determined, either to ensure compatibility of sludge with any waste encountered in the tanks or to ensure that sludge does not contain chemicals which are incompatible with the grout-forming process or interim dry storage.

1.1 SAMPLE GATHERING AND ANALYSIS A campaign to retrieve 20 representative samples of sludge from K East

Basin and Weasel Pit has been completed. Locations for sampling (Figure 1.2) were chosen to span a diversity of expected sludge constituents. Equipment was designed and utilized which assured that full core samples of material were collected from only specific localized areas.

Samples were taken from (1) areas with deep and shallow accumulations of sludge, (2) areas near aluminum and stainless steel canisters, and (3) areas near to and far from corroded fuel.

The following is a summary of the chemical and physical property data obtained from the K East Basin samples. The 20 samples ranged in total as-settled volume from 100 to 500 ml. Unless otherwise noted concentrations given below are for centrifuged sludge (i.e., with some bulk water removed). The task of renormalizing to as-settled or dry sludge bases is discussed in the accompanying text and appendices.

1.1.1 X-Ray Diffraction X-Ray Diffraction (XRD) provided an identification of crystallographic

phases present. A major goal of this sludge sampling campaign was to ascertain if any metallic uranium, hydride, or metallic zirconium could be identified in the sludge. These species are cause for more concern over pyrophoricity than oxides. None of these constituents were found in any of the samples. Sixteen virgin sludge samples were analyzed as well as six samples of undigestible residue from chemical analysis. Several samples contained SiO, and most nonresidue samples contained some Fe0(0H). Uranium was found in two forms, U02 and U04 • 4H20. No U03 hydrates were detected. Ti02 (possibly from paint chips) was identified. Also found were complicated structures containing Li, Pb, Na, and Mg which are probably ion exchange resin beads (used to condition basin water and inadvertently spilled into the basin). Aluminum was found only combined in Mg, Si, Ca, and/or Na oxides (hydrated) and not as pure A1203.

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1.1.2 Particle Size Particle size analyses were performed on the upper and lower layers from

two samples designated "research samples" in the SAP (Welsh 1995). Most particles (number frequency) were less than 1 micron in diameter while most of the sample volume consisted of 1 to 100 micron particles. Ultrasonic treatment tended to break apart many of the large particles (indicating they were originally clusters of smaller particles) while other large particles (probably ion exchange resin beads) remained intact. Example distributions are shown in Figure 1.3.

1.1.3 Appearance, Settling Rate, Dissolution, and Density Sludge color ranged from reddish brown to black with black indicative of

higher uranium content. The reddish material was flocculent while brown sand-like material settled to the very bottom of containers. One sample contained a large volume fraction of ion exchange resin beads. Settled densities of sludge normally were in the range of 1.0 to 1.8 g/ml and centrifuged densities usually were in this same range. The sample with the highest uranium content however, had the highest settled and centrifuged density values of 2.3 and 3.8 g/ml respectively. Dry particle densities were 2.6 to 3.9 g/ml, measured for three samples which did not include the high uranium sample because of small initial sample size.

Figure 1.4 is an example plot which illustrates settling time (i.e., time for sludge to decrease in volume). Most of the sludge settled quickly (in hours) although, for a minority of samples, murky water persisted for longer periods (days) after primary settling had occurred.

From 1 to 34 wt% of each centrifuged sludge sample could not be acid digested for chemical analysis. This fraction consisted primarily of the sand, Ti02 and (Al, Na, Ca, Mg, and Si) oxides discussed above in Section 1.1.1.

1.1.4 pH, Ammonia, Cyanide, and Ion Chromatography These analyses were performed on water which was in intimate contact with

the solid sludge particles and which was recovered by centrifuging. pH ranged from 7.52 to 7.95. For ammonia all but one of the sample concentrations were below detection limits. All samples were below detection limit for cyanide, phosphate and nitrite. Fluoride, chloride, and nitrate ranged up to 2.2, 4.2, and 4.6 jug/ml (of separated liquid) respectively while sulphate was as high as 88 /tg/ml.

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1.1.5 Inductively Coupled Plasma Metals These results were all from acid digests of solid sludge samples. Note

that iron contents of some samples were significant (occasionally exceeding 25 wt% of centrifuged sludge) and were principally due to the corrosion of low carbon steel painted racks which hold the fuel canisters in the pool. Aluminum concentrations ranged up to 4 wt%. Traces of 13 other metals were found in the sludge.

1.1.6 Uranium Total uranium values with one exception ranged from 1 x 104 to

2 x 105 /jg/g of centrifuged sludge (approximately 20 wt% maximum). Note that one low uranium value (0.1 wt%) is from a sample with 50 vol% ion exchange resin beads. The U levels were below detection and 235U values were approximately 0.7 at.% of total uranium.

1.1.7 Plutonium, Americium, Strontium, and Gamma Energy Analysis Americium values were less than 28 /.Ci/g and 239Pu/240Pu contents were

less than or equal to 22 /»Ci/g. The Cs values ranged up to 724 /»Ci/g and 90Sr up to 678 /.Ci/g with highest values corresponding to samples with high uranium content. The 106Ru/Rh, 134Cs, 1MCe/Pr, wNb, and 226Ra were below detection limits in most cases. Cobalt-60 was found up to 1.9 /.Ci/g. The 154Eu and Eu ranged up to 4.4 and 2 /.Ci/g respectively with highest values corresponding to samples with high uranium and plutonium contents. These isotopes are being evaluated as accountability tools which might serve (through gamma counting) as markers for fissile material. The ^ N p values were below detection limits or extremely small (10"3 to 10"4 /iCi/g).

1.1.8 Radioactivity Alpha activity was less than 55 /iCi/g for all samples and beta values

ranged from 30 to 1,520 M CV9- Highest alpha and beta radioactivity values corresponded to samples with highest uranium content.

1.1.9 Thermo-Gravimetric Analysis and Differential Scanning Calorimetry From both laboratories in total, 27 subsamples were run for Thermo-

Gravimetric Analysis (TGA)/Differential Scanning Calorimetry (DSC). The centrifuged sludge contained between 16 and 84% water (mass loss). Exothermic reactions (in DSC under nitrogen atmosphere) were not seen unless a large volume fraction of a particular sample consisted of ion exchange resin beads. Twenty four of the samples showed at least some secondary weight loss (in addition to bulk water loss) between 160 and 300 °C. An example is shown in Figure 1.5.

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1.1.10 Carbon Total carbon ranged from 1,050 to 5,450 /ig/g of centrifuged sludge.

Total inorganic carbon ranged from 640 to 2,620 /ig/g while organic carbon ranged from 562 to 3,350 jug/g.

1.2 CONCLUSION A campaign of sludge sampling for the Hanford K East Basin has been

completed. Sampling and analyses have been performed in a far more rigorous manner than previous sampling attempts (Baker 1995a). K East Basin floor sludge was found to contain significant amounts of iron and uranium as well as numerous minor constituents. The sludge settles quickly in most cases and contains no detectable pyrophoric materials.

Future campaigns will address characterization of the more highly radioactive sludge inside the fuel canisters as well as sludge in the other Hanford fuel storage basin, K West.

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Figjre 1.1 K East Basin Fuel Sludge was Sampled from the Floor Between Canisters

Note: The errpty canister is an example of a slotted container which will allow fuel corrosion products to mix with floor sludge.

Figure 1.2. Locations for Sampling of Sludge in the Hanford K East Basin.

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Figure 1.3. Example Particle Size Distribution for K Basin Sludge. The size distribution is shown based both on volume and number of particles.

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Figure 1.4. Settling of K East Basin Sludge. This figure shows the decreasing volume of a sludge

sample versus time after agitation.

Figure 1.5. Example of Thermo-Gravimetric Analysis Drying Curve for K East Basin Floor Sludge.

Step Analysis Height -14.95 mg

-43.34%

Step Analysis Height -2.04 mg

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2.0 INTRODUCTION

The Hanford K East Basin is being used to store N Reactor fuel in open top canisters made of aluminum or stainless steel. The sludge in the Hanford K East Basin consists of a mixture of sand, fuel, and fission products (from damaged fuel elements), organic material such as insects, paint chips, canister corrosion products, and concrete spallation. A recent campaign was completed to sample sludge from the K East Basin and Weasel Pit. It was performed to supply a characterization of sludge from carefully chosen basin areas with attention to those details which would make the resulting data applicable to the needs of the SNF Project Paths Forward for sludge and to some extent fuel.

This report supplies a reviewed set of chemical and physical property values for these two particular kinds of sludge and, in addition, calls attention to particular insights about sludge which have been gained during sampling and data reduction. Data Quality Objectives (DQOs) for the sampling effort (Makenas 1995) indicate that the sampling and subsequent analyses serve the needs of several Spent Nuclear Fuel (SNF) project objectives: storage of the bulk of the sludge away from K Basins (in tanks or as processed solid waste), nuclear materials accountability, sludge recovery and transportation, sludge handling equipment design, sludge simulants, and storage of fuel with some residual sludge.

The analyses performed on sludge recovered from the K East Basin and Weasel Pit fall into several classes:

1. Physical properties: Viscosity, particle shape, particle size, settling rate, zeta potential, and wet/dry densities.

2. Radionuclide content: Includes transuranic elements as well as fission products. Techniques employed include gamma and alpha energy analyses, Gamma Energy Analysis and Alpha Energy Analysis (GEA and AEA).

3. Radiological Properties: Total alpha, beta and gamma emission rates per volume of sludge.

4. Chemistry: Includes Inductively Coupled Plasma (ICP) spectroscopy, which gives the content of certain metals in sludge and Ion Chromatography (IC) which determines the concentration of certain ions in water which is in intimate contact with sludge.

5. Chemical Reactivity Determinations: The TGA gives the percent water in a sample but also highlights specific temperatures where water and other volatiles exit the sludge. The DSC indicates exothermic and endothermic reactions of the sludge in a particular medium. X-Ray diffraction (XRD) is utilized to give indications of particular crystalline phases. In the case of sludge, potentially pyrophoric compounds such as uranium hydride and uranium metal were specifically targeted for analysis by XRD.

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The methodology for choosing particular basin locations for sampling is covered in reference (Welsh 1995). Twenty targeted locations were chosen near to or far from known damaged fuel, near aluminum or stainless steel canisters, and from areas of deep or shallow sludge. The capabilities of the sampling equipment used to recover sludge samples are reviewed in (Baker 1995b). It should be noted that since the sludge was pumped to the pool surface, considerable additional water was entrained in the sludge samples as a result of the pumping process. An isolation tube was inserted into the sludge prior to each sampling attempt to ensure that a representative core sample was obtained.

Samples were collected from the K East Basin and Weasel Pit in August/September 1995. The material was first sent to 222-S laboratories where settling studies were performed along with the decanting of excess water. Subsamples were then sent to 325 Building laboratories for certain analyses (primarily physical properties) or retained at 222-S for other analyses (primarily chemistry). Figure 2.1 is a flowchart of how the samples were processed and analyzed. Note that many of the analyses (primarily chemistry determinations) required special processing steps such as centrifuging (to remove excess water) or drying at higher temperature. These steps were not performed where they would compromise the data (e.g., physical properties such as viscosity).

Fifteen samples were taken from the Main Basin and five from the Weasel Pit. Two of the samples were split into layers (after settling) with equivalent analyses done separately on each layer in order to illuminate differences between strata. In this case two layers were identified based on color, texture, etc., in each of these two samples. Two other samples were subjected to long term settling and were not part of the chemical and physical property determinations.

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Sludge Sample Equipment Blank & Hot Cell Blank

Settling Rale (30 Days) Appearance

| Decant Wa te r | Sludge | Water

Appearance (Photography) Settling Rata (<S days) Settled density

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3.0 RESULTS, ANALYSIS, AND EXPLANATION OF APPENDICES

The results obtained from this sludge sampling campaign can be divided into those inferences derived from the actual sample retrieval and the results obtained from laboratory analyses.

3.1 IN-BASIN SAMPLING EXPERIENCE This section provides a summary of the sampling method, sample locations,

and operational observations.

3.1.1 Overview of Sampling Method For each sample the specially developed sampling equipment described in

System Design Description (Baker 1995b) was used to draw a representative core sample on order of 250 ml or more into two or more four liter sample bottles, Figure 3.1. These bottles were then transported to a Hanford analytical laboratory using PAS-1 casks with specially designed inserts. At the laboratories the bottles were unloaded from the casks. Analyses and partitioning of the samples then followed. The sampling equipment was developed with a set of functions and requirements consistent with the Sampling and Analysis Plan (SAP) for this characterization effort, (Welsh 1995).

The general sequence for drawing a sample using the sampling equipment, illustrated in Figure 3.1, was:

1. The sampling area on the K East Basin grating was prepared with the installation of sampling and monitoring equipment.

2. Through a slot or equipment opening in the grating an isolation tube was placed into the sludge isolating a representative core of sludge from the sludge surface to the floor (the isolation tube has a sharp beveled edge that seats to the basin floor and is long enough to extend up through the grating once seated). Three different diameter isolation tubes were used to control the volume of the sample taken (i.e., about 250 ml or more): a larger 10.2 cm (4 in.) ID tube was used for shallow sludge, a 5.1 cm (2 in.) tube for moderate depth sludge, and a 2.5 cm (1 in.) diameter tube for deep sludge or where space was restricted, Figure 3.2.

3. Three sample bottles (each 4 liter) were then prepared in their shielded cart at the sample site, see Figure 3.3. The bottles are connected to sequentially fill. Only the first two bottles were intended for the sample. The third bottle was a safety backup to catch overflow if the final checkvalve, in the second bottle, failed to close thus allowing time to stop the sampling.

12

WHC-SP-1182

4. The extraction tube, Figure 3.1, was then positioned within the isolation tube just above the core of sludge and the sealed sludge sample bottles were evacuated using a peristaltic pump.

5. The main control valve was then opened. The sludge core sample and water were then pulled through the extraction nozzle and into the evacuated bottles by the suction of the negative differential pressure. During sample recovery the extraction tube nozzle was moved up and down (to assure enough water to mix with the sludge so sludge would not plug the nozzle) working to the bottom of the sludge core within the isolation tube, Figure 3.4.

6. With the sample in the bottles, the pump was stopped and the remaining vacuum released from the bottles. If the sludge was extremely deep Step 5 was repeated with additional bottles until retrieved water was generally free of solids.

7. The bottles containing the sample were then prepared and transported to the Hanford analytical laboratory using the PAS-1 Cask system, Figure 3.5. The multiple bottles for each sample were combined at the laboratory to provide the single sample of sludge for each case.

The material in the sludge sample was to be limited to particles of 6.4 mm (0.25 in.) or less (Welsh 1995). The nozzle of the extraction tube was designed to keep particles greater than this diameter from being pulled into the sample bottles, (Figure 3.6).

The K Basin Master Work Plan used for this sampling was MWP-95-003. In addition to the sampling equipment system described in the System

Design Description (Baker 1995b), a set of special brackets were designed and fabricated to support the sample equipment isolation tubes in the Weasel Pit Equipment Opening, Figure 3.7. These brackets allowed (1) the operators to remain behind the permanent handrails that surrounded the main equipment opening, (2) located the tubes so the "T" handles on the extraction tube of the sampling equipment did not strike the handrails during sampling, while maintaining a fixed position in the pit, and (3) allowed placement of the isolation tubes at any location across the equipment opening as long as the "T" handles cleared the surrounding handrails.

3.1.2 Final Sample Locations The general character of the sludge on the K East basin floor as

understood prior to this sampling effort is discussed in (Baker 1995a). The Sampling and Analysis Plan (SAP) for the K East Floor and Weasel Pit sludge, (Welsh 1995) provides a set of proposed sampling locations based on this prior-knowledge. These locations were selected based on the objectives set forth in the SAP responding to the Data Quality Objectives (Makenas 1995). The current sampling addressed three identified primary variables that the Main Basin floor sludge character could be dependent on: (1) local depth of the sludge on the floor, (2) the condition of the fuel (e.g., failed, etc.) in a locale, and (3) the type of spent fuel storage canister (e.g., aluminum,

13

WHC-SP-1182

stainless steel, slotted barrels, etc.) in a locale. These were addressed using a factorial design to select sample locations. Several factorial design points were not possible. Secondary variables included variations between the three separate bays in the K East Main Basin (i.e., East, Center and West) and the potential impact of locations near the mouths of the transfer channels entering the Main Basin from the four remote pits. The secondary variables were used to determine substitute locations for the factorial points that were not possible. A total of 15 sample locations were identified (including archive and contingent samples).

In addition, five samples were selected to characterize the floor sludge in the Weasel Pit. These were to be located under the open grating areas of the pit and distributed as much as possible throughout this area to give as wide a coverage as possible. No other variables were identified for the Weasel Pit because the sludge in this pit had been pumped in, thus mixing the material.

The K East Basin provides a very challenging area to sample for sludge because of the degraded condition of the fuel, canisters, and debris; the various forms of sludge; the nuclear environment and dose rate of the samples potentially being brought to the grating; and depth of water involved. Because of this, some adjustments in locations for samples called for in the SAP were expected. A few of the original proposed sample locations were moved slightly to allow improved sampling (e.g., to avoid debris such as identification disks buried in the sludge), to improve ALARA considerations for the operators of the sampling equipment, or to improve logistics of the sampling (e.g., location of the Weasel Pit samples to allow operation of the sampling equipment within the constraints of architectural obstructions). In all cases the alternate sampling locations provided equivalent or more representative samples.

Table 3.1 and Figure 3.8 provide a summary of the final physical locations of the samples in the Main Basin. Table 3.1 corresponds to Table B2 in the SAP (Welsh 1995). Figure 3.7 provides the final locations for the Weasel Pit samples.

Appendix A provides additional detail on the sampling of the Weasel Pit including improved estimates of depths and volumes of sludge contained in this pit at the time of sampling.

3.1.3 Summary Observations Made During Sludge Sampling The samples were taken at the basin and tracked with chain of custody

forms. Table 3.2 indicates the dates samples were taken, the number of four liter sample bottles used and a review of the depth of sludge present. It also includes any general comments the Spent Nuclear Fuel Evaluation group Test Engineers had from observations made during the sampling process. Note that the samples were designated with a KES prefix, followed by a letter ranging from A to T, and followed by a number ranging from 1 to 20. The

14

WHC-SP-1182

letter designation, in general, corresponds to the order the samples were taken, starting with "A." The number corresponds to the sample designations called out in the SAP (Welsh 1995). In general the samples were taken from the easiest and lowest expected dose rate locale to the most aggressive.

It should be noted that the final volume of each sludge sample was not proportional to the depth of sludge in the basin because the diameter of the isolation tube was varied to control the sample volumes to roughly 250 ml or more where feasible. For example, sample KES-0-09, had a relatively small volume because the isolation tube used was small in diameter in order to fit between canister barrels, but this sample actually came from one of the deepest sludge areas in the K East Main Basin. Thus caution should be used in application of the results when interpreting the total volume of a constituent in the overall basin. In these cases the locations of the samples versus the indicated volumes in various locations need to be considered {i.e., using the depth and volume data derived in 1994 (Baker 1995a)].

3.2 CHEMISTRY AND PHYSICAL PROPERTIES The raw data from analyses of K East Basin and Weasel Pit sludge are

reported in (Miller 1995; Miller 1996) (the former being a summary of the latter) and in (Silvers 1995). Note that most of the chemical composition values given in the three references are for as-centrifuged sludge (i.e., compositional values when stated on a per gram basis, have been normalized to an initial sample mass which includes the water which is removed later by the drying which itself is routinely done prior to chemical analysis). Conversely this total mass of as-centrifuged sample does not include bulk water removed from as-settled sludge by centrifuging. The chemical and radionuclide composition values for centrifuged sludge samples are given in Appendix B.

Depending on the application of the data, compositional values based on either a wet as-settled mass or a dried mass of sludge may be appropriate. Appendices C and D present the compositional data (initially presented in Appendix B as centrifuged sludge) renormalized to wet and dry conditions respectively. The renormalization has been performed using the mass loss data supplied in Reference (Miller 1995) for the centrifuging and drying steps.

As-centrifuged and as-settled densities for sludge samples are also presented along with the chemistry summaries in Appendices B and C. Three samples, however also were subject to dry particle density measurements (i.e., helium pycnometry). The top layer of sample M13* had a dry density of 3.1 to 3.4 g/cc, the values for the top layer of sample T20 were 2.6 to 3.9 g/cc and for the bottom layer of sample T20 were 2.6 to 3.1 g/cc. The samples with highest uranium content (such as 09 and L01) were not subjected to this measurement and may well have had higher dry densities. The presence of ion exchange resin beads, known to be present in the sludge, may bias the dry densities toward a low value.

*In order to simplify the text of this report, samples may be referred to by compressed designation.

15

WHC-SP-1182

Plots of the chemical and radionuclide content of the sludge versus basin sample location are presented in Appendix E. The plots were constructed utilizing the values from Appendix B or C and the locations supplied in Appendix A.

Appendix F is the statistical analysis of the chemistry results listed in Appendices B through D. Included is an analysis of variance determining the effects of the three primary variables, and an estimate of the analytical variability. Box plots showing the distribution of data are also included.

A general summary of specific organic chemicals detected in sludge is given in Appendix G. Analyses for volatile and semi-volatile compounds are the source of this information. Note that analyses for total carbon, total inorganic carbon, and total organic carbon are presented with the noncarbonacious analyses listed in Appendices B through D. Three samples were found to contain polychlorinated biphenyls (PCBs). A specific focus on PCB compounds is provided by Appendix H.

Appendix I is a comprehensive treatment of physical properties including viscosity, zeta potential, and particle size for each layer of the research samples. It should be noted that original plans for viscosity measurements called for measurements on as-received sludge as well as on sludge diluted with water to give a family of data curves. Since the as-received sludge was exceptionally non-viscous, the sludge was thickened by centrifuging, rather than diluted, for the later viscosity runs. This appendix also discusses the implications of the physical property measurements on the methodology of choosing sludge simulants and the choice of sludge handling equipment. Another finding of significance discussed in Appendix I is the effect of ultrasonic application to sludge particles i.e., the size of sludge particles decreases with increasing severity of ultrasonic treatment which implies that large particles may be agglomerates of smaller entities.

Appendix J presents examples of sludge particle shapes as seen in Transmission Electron Microscopy (TEM) for each layer of the research samples. Both irregular amorphous structures and needle-like particles are evident. Correlations between particle shape and elemental content (uranium, iron, aluminum etc.) can also be drawn based on accompanying Energy Dispersive X-Ray Analysis. These observations are for a limited number of particles in a limited number of samples and should not be used to draw inferences on frequency of shape or element occurrence. They do confirm that large particles appear to be agglomerates of smaller particles as discussed above.

Appendix K consists of both X-Ray Diffraction (XRD) and electron diffraction results. These techniques identify crystalline phases. Electron diffraction data was obtained on the same samples used for shape measurement described in Appendix J. Those phases observed by these two methods are listed in the tables found in this appendix. It is of significance to note that no pyrophoric materials such as metallic uranium, metallic zirconium, or uranium hydrides were detected in any sample. Most of the diffraction work was performed on as-settled sludge for TEM or centrifuged sludge for XRD. However, many of chemical determinations, discussed in the preceding appendices, are done by wet chemistry methods. Therefore, sludge was acid digested for these chemistry analyses such as GEA and ICP. Some residues were

16

WHC-SP-1182

invariably left after digestion and these residues also were analyzed by XRD to detect such insoluble compounds as sand. Diffraction methods do not give good results for cases where compounds are amorphous (noncrystalline) or where very small particles are involved (<0.1 /»m) approximately). This is apparently true to some extent where larger particles are often agglomerates of smaller particles (see Appendix I for size measurements). There is virtually no chance, however, that such small undetectable particles, if they originated as uranium metal or as hydrides, would remain unoxidized on a water environment such as the K Basin pools.

Included in Appendix L are data on sludge settling times. Settled sludge varied in appearance from reddish brown to black in color (Figure 3.9). Sand­like material was often seen at the bottom of settled samples and one sample (H8) contained a large volume fraction of ion exchange resin beads (in excess of 50%). Settling times were usually short (hours) but some exceptions are discussed in Appendix L.

Appendix M shows the TGA drying curves for the sludge samples. Side-by-side plots are shown where data for the same sample are available from both 222-S and 325 Building laboratories and duplicate runs are shown where available. Percent-water determinations derived from these curves are listed in the chemistry tables in Appendix B. Centrifuged samples varied in weight loss from 36 to 84% when heated during TGA under a nitrogen atmosphere. The reader is referred to References (Miller 1995; Silvers 1995) for data on DSC and Differential Thermal Analysis (DTA). The DSC data is also summarized in Appendices B and C. It should be noted that no exothermic reactions were detected (in DSC) for sludge while heating in 1 atmosphere nitrogen. The lone exception to this statement was sample H8 which was anomalous during several property determinations due to the significant ion exchange resin bead content. Resin beads are probably present to some degree in other samples also.

17

Sample Number (KES-)

L-01 A-02 B-03 C-04 N-05 J-06

G-07 H-08 0-09

F-10 E-ll K-12 M-13 D-14 1-15 P-16

Q-17

R-18

S-19

T-20

Type Sample"

N N N N N N

N N N

N N N R R N N

N

N

N

R

Factorial Design Pointh

(x,y,z) 1,2,1 1,2,2 1,2,1 1,2,2 2,1,1 2,2,2

1,2,1 2,2,2 3,1,1

3,2,2 1,2,1 3,2,2 2,1,1 1,2,2 3,2,2 Weasel Pit Weasel Pit Weasel Pit Weasel Pit Weasel Pit

1n (x) 1 3 1 5 1 0 0 5 2 6 2 5

0 7 3 7 7 5

4 6 0 9 5 6 2 7 0 5 5 6 12

30

28

34

35

Fuel Condition

(y)

G NA

NA

NA

NA

NA

Canister Type w Al/S

SS Al/S SS Al/S SS

Al/S SS Al

SS Al SS Al/S SS SS NA

NA

NA

NA

NA

Sample Location

Lattice Location0

1257 4S16 2935 2771° 1268 0133

5253 6755 6070

6718 1424 0168 1266 2771° West of 6722 Slot West

Slot Hid

Opening Hid North Opening Hid South Opening East End

North/South South North South North South South

North South North

South South North North South In Slot to Pit" See Figure 3 7

See Figure 3 7

See Figure 3 7

See Figure 3 7

See Figure 3 7

Between

No No No No No No

No No Yes

No No No No No No NA

NA

NA

NA

NA

Isolation

Diameter,*

4 4 4 4 4 4

4 2 1

2 4

Calculated Sludge Volume,'

ml

268 309 206 102 535 494

144 190 97

237 185 288 556 102 322 154

386

360

437

450

Original Estimated

Rate'

H L H L N H

L L H

L L H H L H H

H

H

H

H

Comments"

Substitute for Index (1,1,1) Substitute for Index (1,1,2)

Similar Location to KES-D-14

Substitute Index (2,1,2)/ Weasel Houth Substitute for Index (2,2,1)

Peak Depth In Haln Basin Fit between Barrels Substitute for Index (3,1,2) Substitute for Index (3,2,1) Houth Dummy Elevator Pit Near Location KES-N-OS Similar Location to KES-C-04 15.2 cm (6 Inch) Outside Pit Depth from Isolation Tube (Appendix A) Depth from Isolation Tube (Appendix A) Depth from Isolation Tube (Appendix A) Depth from Isolation Tube (Appendix A) Depth from Isolation Tube (Appendix A)

Sample Number (KES-) L-01 A-02 B-03 C-04 N OS J-06 G-07 H-08 0-09

F-10 E-ll K-12

H 13 D 14 1-15

P-16 Q-I7 R-ie S-19 T-20

Type Sample

N N N N N N N N N

N N N

P. R N

N N N N R

Sample Location

Lattice Location' 1257 4516 2935 2771 1268 0133 5253 6755 6070

6718 1424 0168

1266 2771 West of 6722 Slot West Slot Hid Open Mid N Open Hid S Open E End

North/South South North South North South South North South North

North South North

North South In Slot to Pit" NA NA NA NA NA

Under Slot?

Yes Yes Yes Yes Yes Yes Yes Yes Yes

Yes Yes Yes

Yes Yes Yes

Yes Yes Yes Yes Yes

Bay Coverage*

E/NW C/SW C/SE C/NE E/NW E/SE W/NE W/NW W/NW

W/SW E/SW E/NE

E/NW C/NE W/SW

-----

Depth Measure''

No Yes Yes Yes No Yes No No Yes

No No Yes

No Yes Yes (6722)

No No No No No

Wall"

No No No No No No No No No

No No No

No No No

No No Yes No No

Depth Survey Tape Location1

Tape Log Number

NA 6 4 6 3 6 3 NA 6 1 NA NA 6 4

NA NA 6 1

NA 6 3 6 5

NA NA NA NA NA

Time, M m

0 27 04 1 04 17 0 41 SO

0 27 58 NA NA 1 00 59

NA NA 0 42 48

0 41 50 56 46

-----

Canister On Side of Interest"

1256 4517 2934 2770° 1267 0132 5254 6754 6070

6719 1423 0169 or 0167 1267 2770

------

Comments

Video Okay Video Okay Video Okay Video Okay Video Okay Video Okay Video Okay Video Okay Video Okay

Video Okay Video Okay Video Caution Debris Surrounds Video Okay Video Okay Video Okay

WHC-SP-1182

Table 3.1. Final Sludge Detail. (Continued) Footnotes aN—Normal, R—Research, see SAP Reference 3 for definition. bx = "1" for less than 6 cm (2.4 in.); "2" for less than 6 cm but greater

than 12 cm (4.7 in.); "3" for greater that 12 cm. y = "1" for poor/very bad fuel (P/VB); "2" good/fair fuel (G/F). z = "1" for canisters with aluminum slotted barrels (Al/S) or aluminum

unslotted (Al); "2" for stainless steel (SS) solid barrels. cLattice location and sub-location for sample in main basin. "North" or "South" are indicated as to which side of the empty cubical sampling should be made to be adjacent to canister of interest. For Weasel Pit see Figure 3.2.

d"Yes" = Sample is to be taken between canister barrels. "No" = Sample is to be taken in empty cubical location as far north or south

as possible (as indicated). isolation tube diameter used on sampler to obtain sample volume. Calculated volume of sludge to be recovered given estimated sludge depth and isolation tube size.

9Pre-sampling estimate of dose rate expected in sample bottles: "L" = low [<1R at 1.5 cm (2 in.)], "M" = medium (between 1 and 5 R), "H" = high (greater than 5 R). These generally agreed with sample drawn.

h"Substitute for Index (1,1,2)" - sample indicated is a substitute for a sample with factorial see SAP, (Welsh 1995) index (1,1,2) because no available location could meet all the criteria for (1,1,2).

'A secondary variable is general coverage of the three bays in the main basin ("E" = East, "C" - Central and "W" = West bays)/the quadrants of the bay the sample is located is also indicated (e.g., "NW" = Northwest, etc).

jWas there a direct measurement of sludge depth made (and video recorded) in 1994 campaign (Baker 1995a)

Sampling cannot be made next to wall (not directly under slot) though depths were measured in some locations in 1994.

lTape log number and time on video tapes, made during sludge depth measuring campaign in 1994, showing the location the sample will be taken.

"This is the location of the fuel canister of interest (i.e., has the variables shown on prior page of this table under "Factorial Design Point"). In an empty cubical the canister of interest should be directly adjacent to sampling location (i.e., reason for the indicated "north" or "south" portion of sample location).

"Sample taken 12 in. west of 6722 in transfer channel slot but still 15.2 cm (6 in.) into Main Basin.

"Original position was 2769, sample was taken in 2771 north next to empty canister, nearest fueled canister is 2770 which is shown on table, within 10.2 cm (4 in.) to sample KES-D-14.

20

WHC-SP-1182

Table 3.2. Sampling Dates and General Observations.

Sample Number (KES-) L-01 A-02 B-03 C-04

N-05 J-06 G-07

H-08

0-09

F-10

E-ll

K-12 M-13 D-14

Sludge Depth

Verified* Yes Yes Yes Yes

Yes Yes Yes

Yes

Yes

Yes

Yes

Yes Yes Yes

Number of

Sample Bottles

2 2 2 2

2 2 2

2

2

2

2

2 2 2

Date Sampled 09/07/95 08/18/95 08/18/95 08/23/95

09/11/95 09/07/95 08/29/95

08/29/95

09/13/95

08/25/95

08/25/95

09/13/95 09/11/95 08/23/95

Comments

Position moved from original of 2769 to 2771. — — Problems encountered seating isolation tube before final placement. Bubbles apparent from sludge as isolation tube was inserted. During sampling sample being collected was first brown then turned black. (Note ion exchange beads observed on fuel canister near by) Taken at deepest floor sludge in Main Basin. Only sample taken between canister barrels. Debris in cubical in the way of isolation tube being placed in requested "North" position. Went to "South" side. May have seated on metal plate (identification disk?) raising tube somewhat. Sludge very dark. Isolation tube moved somewhat during sampling. A piece of something white (what appears to be paper?) was stuck in nozzle ports at one point stoppinq flow. — — Position moved from original of 2769 to 2771.

21

WHC-SP-1182

Sample Number (KES-) 1-15

P-16 Q-17 R-18

S-19

T-20

Equipment Blank

Sludge Depth

Verified* Yes

New New New

New

New

NA

Number of

Sample Bottles

2

2 2 4

6

4

2

Date Sampled 09/05/95

09/15/95 09/19/95 09/19/95

09/25/95

09/19/95

09/25/95

Comments Sampled about 12 in. in from the last main basin north/south grating slot along grating slot for transfer channel to South Loadout Pit, still within main basin about 15.2 cm (6 in.). Metal identification disks in sludge caused obstructions, extraction tube plugged after sufficient sample taken. Plug could not be backflushed at time, later was cleared. — — Sludge was hard packed at first but eventually loosened enouqh to sample. Hard packed sludge. About 15.2 cm (6 in.) of core sample in bottles A, B, D, and E. Clog on third set (bottles G and H) cleared by stopping and restarting sampling. Top about 40.6 cm (16 in.) of core sample in isolation tube went to bottles A and B — sludge was hard packed with lots of solids. Rest of core went into bottles D and E — sludge was a darker material. Water from K East main basin pulled above cubical Location 0430.

*Yes - Isolation tube scale of sludge depth confirms general depth from 1994 study (Table 3.1).

New - Isolation tube scale of sludge depth provides new data—there is no prior data to compare to, see Appendix A.

22

FLEXIBLE TUBING

EXTRACTION TUBE HANDLE

SAMPLING BOTTLES AND SHIELDING

PUMP TO EVACUATE BOTTLES

CART FOR BOTTLES, SHIELDING AND PUMP

Water level

20'-9

» - h

Basin Floor

WHC-SP-1182

Figure 3.2. Examples of the 10.2 cm (4 inch) and 5.1 cm (2 inch) Diameter Isolation Tubes Inserted in K East Sludge (see Appendix A

for example of 2.5 cm (1 inch) isolation tube)

24

WHC-SP-1182

BEST AVAILABLE COPY Figure 3.3. Preparations of Sample Bottles, their Associated Shielding

and Cart (holding bottles and pump) on Basin Grating.

25

WHC-SP-1182 BEST AVAILABLE CO. Figure 3 4 Overview of Sampling Activity on Grating (Note 'T' handled extraction nozzle handle with striped handles between operators and lower photograph of sludge

moving to second sequential sample bottle as first is filled )

$*z

( 1 ^

26

WHC-SP-1182

Figure 3 b Sample Bottle KES-E 11 in Analytical Laboratory Hot Cell not Long After Sampling in K Basin

Figure 3 6 Nozzle Used on Extraction Tube with Openings to Exclude Particles Greater than 6 4 mm (0 25 inch) in Diameter

BEST AVAILABLE CO:

27

WHC-SP-1182

Figure 3.7. Final Sample Locations in K East Weasel Pit (special brackets developed allow sampling in the open

equipment area for samples KES-R-18, KES-S-19, and KES-T-20). p [168cm(5-6')]

-N —

m(2--10")]

[691em(22'-6")]

|315cn,(l0-4")]

- [36cm(V-r>]

[340cm(ir-2"VJ

-[l3Scm(4'-5-)]

1. SCREEN BETWEEN WEASEL PIT AND TRANSFER CHANNEL TO MAIN BASIN

2 SPECIAL BRACKETS TO SUPPORT ISOLATION TUBES.

28

WHC-SP-1182

Figure 3.8. Final Sample Locations in the K East Main Basin.

29

A\ - \f,

I j i i „ > 1 [ | p " jpf N t ' l f " f , ■ I tIC1:

o O E "3

X

o c o o

5

2s

T

>T AVAILABLE COPY

THIS PAGE INTENTIONALLY LEFT BLANK

WHC-SP-1182

4.0 DISCUSSION AND CAUTIONS

The reader will find that some of the chemistry data listed in the appendices are not available in the raw data reports (Miller 1995; Miller 1996). These analytes were found to be relevant to sludge transportation issues after the issuance of the data reports. They are included here because they could be recovered from existing laboratory records with no further analyses and cost. These include K, Se, 1 Sb, 152Eu, 'i43/S44Cm, and Bi. Furthermore, a number of the values given in the appendices for chemical constituents differ somewhat from those numbers reported in past interim progress reports. This is because the inorganic chemistry values listed in the appendices take into account analyses for duplicate samples while previous analyses reported only the original singular set of data.

The reader will also find that in some cases the same type analyses were performed on portions of the same samples at both 222-S and 325 Building laboratories. The TGA and semi-volatile organic analysis (SVOA) are examples. In the case of total uranium three different values are available. The SVOA determinations are in fair agreement between laboratories while percent water (TGA) determinations are not. The latter disagreements are probably due to different storage times (i.e., drying times) resulting from shipping between laboratories. These disagreements are not taken as significant given that sludge transported from the basin will contain an unknown amount of entrained water due to processing/pumping. The relative agreement of the three uranium values is discussed in the statistical section, Appendix F.

Tables 4.1 to 4.4 are summaries of the representative constituents of K East floor and Weasel Pit sludge. These values were calculated from the data listed on Appendices B, C, and D. The reader is cautioned that straight numerical averaging of the data in the appendices may not be representative of homogenous mixing of all K East Basin sludge since data were taken from basin areas having different depths of sludge and the data presented here-in is not volume weighted. Tables 4.5 and 4.6 compare the most recent data with previous data from the floor and Sandfilter Backwash Pit (Baker 1995). In all cases the maximum analyte concentrations from the current floor sludge campaign exceed those of the prior analyses from the Sandfilter Backwash Pit. An evaluation of sludge analyses against the prime sampling variables (sludge depth, proximity to aluminum versus stainless steel canisters, and proximity to corroded fuel) is given in Appendix F.

Chemistry determinations made during campaign for K East floor and pit sludge are not all-inclusive, with respect to the periodic table, as noted in the DQO document covering this effort (Makenas 1995). Some process knowledge was used to justify particular analyses. For example, mercury was not determined because there was no reason to suspect mercury presence, and the cost and time for this separate analysis was significant. Other analyses, such as silicon, are not compatible with the current acid digestion and wet chemistry procedure.

31

WHC-SP-1182

Achieving a mass balance for the sludge analyses would be very difficult if not impossible. Sludge consists of the chemical constituents that have been analyzed (listed in the appendices). It also contains water (which is determined by TGA) from sludge which has had some chance to dry and to therefore lose water. Finally sludge includes residuals which could not be acid digested for chemistry. For a mass balance one would also have to make an assumption on the valence state of specifically targeted elements in order to compute the weight of oxygen, hydrogen etc., which might be combined with the target species. Organic compounds such as insect protein are too numerous to ever be totally identified. Total organic carbon does provide some information in this vein whereas VOA and SVOA analyses quantify only those organic compounds which are volatile or soluble in specific organic solvents.

Some of the analytes chosen for this sludge analysis campaign had the specific goal of confirming that certain marker isotopes could serve as an accountability tool to track special nuclear materials (SNM) such as plutonium. Chief among these were the europium isotopes. The acceptability of these isotopes for accountability purposes remains to be determined. Regression analysis for these analytes versus plutonium concentrations is given in Appendix N.

Finally a caution is in order for future work with K Basin sludge. The current experience showed that sludge was rather high in beta activity. Therefore, although the low gamma activity may allow work in a glovebox, rather than a hot cell, the high beta dose may at times make hands-on work inappropriate. Also the alpha activity appears, under certain circumstances to create enough static electric charge that migration of dry unconfined sludge particles around a work area (such as hoods) is a distinct possibility.

32

WHC-SP-1182 Table 4 . 1 . Sludge Charac t e r i za t i on Data--Per Gram Centrifuged Sludge.

Analyte

"to '"Cs

l»Cs

■*Eu

'"Eu

»Ce/Pr

"Nb

">1WKh ^■Ra OTTl 2>2Bi

1HEu

l2sSb

2"Am - GEA

Alpha Total

Total Beta 239/M0pu

2J«pu

'"Up

»™>C 24'Am - AEA

»Sr

U-222S phosphorescence

fluorescence

U-222S ICP 2!J„

» U 2«U

»«U

"«U

U n i t *

nCi/s

«Ci/S

uCi/g

uCi/g

UCi/g

UCi/g

«Cl/g

(iCl/g

(iCi/g

fCi/g

«Cl/g

/"Ci/g

/iCi/g

(■Cl/g

(iCi/g

(iCi/g

dCi/g

«Ci/g

cCi/g

fiCi/g

(iCi/g

liCi/g

*/.

U g / g

«/. Atom X

Atom X

Atom X

Atom X

Atom I

Minimum Concentration

Observed

7 03E-02

1 10E+01

< 8 33E-03

< 1 56E-02

< 4 50E-02

< 9 51E-02

< 6 75E-03

< 1 62E-01

< 1 81E-01

< 1 19E-01

< 8 70E-02

< 1 13E-02

< 3 84E-02

1 51E-01

3 76E-01

3 06E+01

1 53E-01

2 35E-02

< 5 78E-04

< 9 50E-02

1 31E-01

2 54E+00

1 09E+03

1 20E+03

9 46E+02

< 1 00E-03

6 OOE-03

6 94E-01

5 OOE-02

9 92E+01

Maximum Concentration

Observed

1 91E+00

7 24E+02

< 3 54E-01

4 37E+00

2 01E+00

< 4 69E+00

< 1 54E-01

< 7 01E+00

< 9 06E+00

< 5 83E+00

< 1 74E+00

< 2 37E-01

< 1 B4E+00

2 63E+01

5 46E+01

1 52E+03

2 20E+01

< 7 61E+00

< 4 14E-03

< 6 31E+00

2 75E+01

6 78E+02

2 97E+04

2 10E+05

1 31E+05

< 1 OOE-03

8 30E-03

7 34E-01

8 OOE-02

9 92E+01

N S

19

19

7

17

16

NA

NA

NA

NA

NA

NA

2

NA

19

19

19

19

9

10

NA

19

19

10

15

16

NA

15

15

15

15

Mean*

8 26E-01

1 35E+02

7 72E-02

1 40E+00

6 50E-01

NA

NA

NA

NA

NA

NA

7 5IE-02

NA

7 89E+D0

1 80E+01

3 59E+02

7 82E+00

9 95E-01

1 30E-03

NA

7 77E+00

1 24E+02

3 99E+04

3 26E+04

NA

7 14E-03

7 04E-01

7 48E-02

9 92E+01

Standard $ Deviation

4 04E-01

1 79E+02

5 21E-02

1 15E+00

5 46E-01

NA

HA

NA

NA

NA

NA

3 54E-04

NA

7 09E+00

1 56E+01

4 18E+02

5 76E+00

6 37E-01

3 17E-04

NA

7 17E+00

1 70E+02

1 02E+04

5 27E+04

3 06E+04

NA

6 05E-04

9 97E-03

7 12E-03

5 67E-03

RSD #

49 0

132 9

67 5

82 2

83 9

NA

NA

1IA

»A

NA

NA

0 5

NA

89 9

86 7

116 4

73 7

64 0

24 3

NA

92 4

136 8

67 2

132 1

93 9

NA

8 5

1 4

9 5

0 0

A per g centrifuged sludge $ Summary statistics calculated from the real analytical values # RSD is the relative standard deviation standard deviation divided by the mean

NA Not applicable for these data * g centrifuged sludge/mL centrifuged sludge & Calculated using the PNL total uranium (fluorescence) data

33

WHC-SP-1182 Table 4 . 1 . Sludge Charac te r i za t ion Data--Per Gram

Centrifuged Sludge. (Continued)

Analyte

Al

Co

Co-

Cr

Cu

Fe

K

Mg

Mn

Na

Pb

Zn

Zr

Ag

B

Ba

Be

S.

Sm

TI

TIC

TOC

TC

CN

TGA

TGA

TGA-PNNL

DSC-wet wt

DSC-dry wt

DSC-PNNL

Unit *

mil

mil

mil

mil

mil

Mil

mil

mil

mil

nil

mil

mil

mil

mil

mil

mil

mil

mil

m/i

mil

mil

mil

m/i

mil

WtLo»s%

mil

WtLossX

Joules/g

Joules/g

Joules/g

Minimum Concentration

Observed

7 10E+03

3 68E+02

2 14E+01

3 56E+01

2 05E+01

5 75E+03

< 9 40E+01

1 95E+02

7 89E+01

1 28E+02

6 07E+01

4 52E+01

2 35E+01

< 8 45E-01

< 4 90E+01

3 68E+01

1 47E+00

< 8 45E+00

< 8 45E+00

< 1 69E+01

6 40E+02

5 62E+02

1 05E+03

< 3 36E-01

3 58E+01

3 58E+05

4 40E+00

0 00

0 00

0 00

Maximum Concentration

Observed

3 38E+04

1 57E+04

6 32E+01

8 35E+Q2

4 57E+02

2 42E+05

1 23E+03

1 65E+03

4 48E+02

1 24E+04

4 21E+02

9 21E+02

5 29E+02

< 1 92E+01

1 31E+02

4 09E+02

3 23E+01

< 1 92E+02

< 1 92E+02

< 3 85E+02

2 62E+0!

3 35E+0 1

5 45E+03

< 1 87E+00

8 41E+01

8 41E+05

7 86E+01

6 18E+01

1 91E+02

8 05E+00

N S

16

16

16

16

16

16

4

16

16

16

16

16

16

1

13

12

14

»A

NA

NA

16

16

16

NA

11

11

15

11

11

16

Mean S

2 18E+04

3 80E+03

4 21E+01

3 56E+02

2 31E+02

1 21E+05

9 50E+02

8 02E+02

2 33E+02

1 05E+03

2 21E+02

4 51E+02

2 14E+02

2 62E+00

8 57E+01

1 42E+02

1 49E+01

NA

NA

NA

1 12E+03

1 26E+03

2 37E+03

NA

5 69E+01

5 69E+05

3 22E+01

5 62E+00

1 74E+01

5 03E-01

Standard $ Deviation

7 36E+03

4 18E+03

1 43E+01

2 50E+02

1 07E+02

7 83E+04

3 85E+02

4 13E+02

1 01E+02

3 04E+03

1 10E+02

2 31E+02

1 36E+02

NA

2 42E+01

1 23E+02

7 99E+00

NA

NA

NA

5 75E+02

7 21E+02

1 13E+03

NA

1 84E+01

1 84E+05

2 72E+01

1 86E+01

5 76E«1

2 01E+00

RSD # (%) 33 8

109 9

34 1

70 2

46 4

64 5

40 6

51 5

43 1

288 0

50 0

51 2

63 4

NA

28 3

86 5

53 6

NA

NA

NA

51 5

57 2

47 7

NA

32 3

32 3

84 7

331 7

331 7

400 0

* per g centrifuged sludge $ Summary statistics calculated from the real analytical values * RSD is the relative standard deviation standard deviation divided by the mean

NA Not applicable for these data * g centrifuged sludge/mL centrifuged sludge & Calculated using the PNL total uranium (fluorescence) data

34

WHC-SP-1182 Table 4 . 1 . Sludge Cha rac t e r i za t i on Data- -Per Gram

Centrifuged Sludge. (Continued)

Analyte

OH demand

S042

P04>

NO,

NO,

CI

F

PH NH, Density

Residue (acid insoluble) 2MU & 2 ! 4U ii

2MU s

™V 4 !S"U S,

Unit.

moles OH/g

Hg/mL

(ig/mL

ml-i. ml*L ws/mL HS/mL

pH units

«/.*. g / 1 .

,g/g

M / B

*g/g

«g/g

«/S

m/i

Minimum Concentration

Observed

1 23E-04

3 95E-01

< 1 19E-01

3 63E-01

< 1 07E-01

< 1 90E-01

< 1 30E-02

7 52E+00

< 5 OOE+00

9 90E-01

9 36E+03

< 1 17E-02

9 16E-02

8 34E+00

9 18E-01

1 19E+03

Maximum Concentration

Observed

4 90E-04

1 03E+02

< 6 22E+00

4 61E+00

< 2 25E+00

4 16E+00

2 22E+00

7 95E+00

< 5 00E+01

3 81E+00

3 70E+05

< 2 06E+00

1 71E+01

1 52E+03

1 04E+02

2 08E+05

N $

14

19

NA

7

NA

17

5

11

NA

18

19

NA

15

15

15

15

Mean S

2 54E-04

1 88E+01

NA

1 82E+00

NA

1 10E+00

9 88E-01

7 69E+00

NA

1 52E+00

9 29E+04

NA

2 92E+00

2 82E+02

2 65E+01

3 96E+04

Standard $ Deviation

9 35E-05

2 84E+01

NA

1 93E+00

NA

1 05E+00

8 09E-01

1 58E-01

NA

6 27E-01

1 02E+05

NA

4 26E+00

3 82E+02

2 79E+01

5 23E+04

RSD # (X)

36 8

151 3

NA

106 2

NA

95 1

81 9

2 1

NA

41 2

10,5

NA

145 9

135 5

105 3

132 1

* per g centrifuged sludge 5 Summary statistics calculated from the real analytical values * RSD is the relative standard deviation, standard deviation divided by ths mean NA Not applicable for these data * g centrifuged sludgB/mL centrifuged sludge 6 Calculated using the PNL total uranium (fluorescence) data

35

WHC-SP-1182 Table 4 . 2 . Sludge Charac t e r i za t ion Data--Per Gram As-Se t t l ed Sludge.

Analyte

«°Co

'"Cs

■«Cs

'"Eu

■«Eu 144Ce/Pr

"Nb ""WRh *fca 20« n

2<2Bi

■>2Eu

125Sb

M 1A m - GEA

Alpha Total

Total Beta 239/2<0pu

23«p„

2"Np

^■"Cm

24,Am - AEA

»Sr

U-222S phosphorescence

fluorescence

U-222S ICP 2»U £ 2*B &

" % S, 2MU &

M«U «,

Unit.

tfCi/g

»<Ci/g

fCi/g

fail |iCi/g

|iCi/g

(iCi/g

«Ci/g

("Ci/g

(iCi/g

«Ci/g

(•Ci/g

MCl/g

JiCi/g

liCi/g

/iCi/g

<"Ci/g

liCl/g

(•Ci/g

liCi/g

JiCi/g

liCi/g

„/. «/.

«/.

Mg/g

mil

mil

mil

mil

Minimum Concentration

Observed

6 99E-02

2 47E+01

< 3 16E-02

< 1 55E-02

< 4 47E-02

< 2 42E-01

< 1 02E-02

< 3 53E-01

< 4 85E-01

< 6 79E-02

< 5 42E-02

< 1 OOE-02

< 2 16E-02

1 50E-01

3 73E-01

1 48E+01

1 52E-01

2 34E-02

< 5 15E-04

< 9 44E-02

1 30E-01

1 26E+00

1 08E+03

1 19E+03

9 40E+02

< 1 16E-02

9 11E-02

8 29E+00

9 13E-01

1 18E+03

Maximum Concentration

Observed

1 49E+00

6 50E+02

< 3 87E-01

3 90E+00

1 80E+00

< 5 06E+00

< 2 93E-01

< 7 37E+00

< 9 65E+00

< 5 21E+00

< 1 56E+00

< 4 39E-01

< 1 64E+00

2 35E+01

4 87E+01

1 36E+03

1 96E+01

< 4 78E+00

< 4 86E-03

< 5 63E+00

2 45E+01

6 05E+02

2 39E+04

1 87E+05

7 98E+04

< 1 83E+00

1 53E+01

1 36E+03

9 29E+01

1 86E+05

R $

20

20

NA

18

16

NA

NA

NA

NA

NA

NA

NA

NA

20

20

20

20

9

10

NA

20

20

10

20

17

NA

20

20

20

20

Mean

6 54E-01

1 26E+02

NA

1 03E+00

4 68E-01

NA

NA

NA

NA

NA

NA

NA

NA

5 82E+00

1 33E+01

3 09E+02

5 80E+00

6 85E-01

1 04E-03

NA

5 70E+00

1 05E+02

1 15E+04

3 10E+04

2 49E+04

NA

2 29E+00

2 18E+02

2 11E+01

3 07E+04

Standard Deviation

3 84E-01

1 55E+02

NA

9 02E-01

4 42E-01

NA

NA

NA

NA

NA

NA

NA

NA

5 46E+00

1 18E+01

3 68E+02

4 55E+00

4 18E-01

2 04E-04

NA

5 59E+00

1 44E+02

8 25E+03

4 11E+04

2 05E+04

NA

3 32E+00

2 97E+02

2 20E+01

4 08E+04

RSD #

58 7

123 8

DA

87 9

94 4

NA

NA

NA

NA

NA

NA

NA

NA

93 8

88 9

119 1

78 5

61 0

19 6

NA

98 1

137 5

71 6

132 8

82 0

1IA

145 0

136 6

104 0

132 8

* per g as-settled sludge 5 Summary statistics calculated from the real analytical values * RSD is the relative standard deviation standard deviation divided by the mean

NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data * g as-settled sludge/mL as-settled sludge

36

WHC-SP-1182 Table 4 . 2 . Sludge Charac t e r i za t ion Data- -Per Gram

As-Se t t l ed Sludge. (Continued)

Analyte

Al

Ca

Cd

Cr

Cu

Fe

K

Mg

Mn

». Pb

Zn

Zr

Ag

B

Ba

Be

S.

Sm

TI

TIC

TOC

TC

CN

TGA-222S

TGA-PNNL

DSC-wet wt (222S)

DSC-dry wt C222S)

DSC-wet wt (PNNI)

Unit.

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

Joules/g

Joules/g

Joules/g

Minimum Concentration

Observed

7 06E+03

1 91E+02

1 36E+01

3 54E+01

2 04E+01

5 72E+03

< 6 01E+01

1 20E+02

5 52E+01

6 45E+01

4 03E+01

4 50E+01

2 33E+01

< 8 41E-01

< 2 86E+01

2 23E+01

1 46E+00

< 8 41E+00

< 8 41E+00

< 1 68E+01

5 36E+00

3 58E+02

6 42E+02

< 2 49E-01

4 54E+05

9 51E+04

0 00

0 00

0 00

Maximum Concentration

Observed

3 67E+04

2 07E+04

4 77E+01

1 19E+03

5 92E+02

3 26E+05

1 59E+03

3 01E+03

6 15E+02

1 23E+04

6 72E+02

1 31E+03

6 60E+02

< 2 36E+01

4 79E+02

3 52E+02

2 20E+01

< 2 36E+02

< 2 36E+02

< 4 72E+02

1 99E+03

3 33E+03

5 42E+03

< 1 16E+00

9 05E+05

8 53E+05

6 14E+01

1 90E+02

8 00E+00

N S

17

17

17

17

17

17

5

17

17

17

17

17

17

1

14

13

15

Na

NA

NA

17

16

16

NA

11

16

" 11

16

Mean

1 76E+04

4 14E+03

3 16E+01

3 32E+02

1 97E+02

1 08E+05

1 01E+03

7 65E+02

2 06E+02

1 04E+03

1 99E+02

4 00E+02

1 93E+02

1 57E+00

9 35E+01

1 32E+02

1 09E+01

NA

NA

NA

8 01E+02

1 03E+03

1 90E+03

NA

6 62E+05

4 74E+05

5 59E+00

1 73E+01

5 OOE-01

Standard Deviation

8 76E+03

5 60E+03

1 01E+01

3 06E+02

1 34E+02

8 76E+04

4 54E+02

6 88E+02

1 44E+02

2 94E+03

1 52E+02

3 05E+02

1 67E+02

NA

1 12E+02

1 28E+02

4 93E+00

NA

NA

NA

4 97E+02

7 56E+02

1 24E+03

NA

1 70E+05

2 54E+05

1 B5E+01

5 72E+01

2 OOE+00

RSD # (I)

49 9

135 4

32 0

92 1

67 9

81 0

45 2

89 9

70 0

283 6

76 6

76 3

86 5

NA

120 1

97 3

45 3

NA

NA

NA

62 1

73 7

65 0

NA

25 7

53 6

3317

33! 7

400 0

* per g as-settled sludge 5 Summary statistics calculated from the real analytical values * RSD is the relative standard deviation, standard deviation divided by the mean NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data * g as-settled sludge/tnL as-settled sludge

37

WHC-SP-1182 Table 4 . 2 . Sludge Charac te r i za t ion Data--Per Gram

As-Se t t l ed Sludge. (Continued)

Analyte

OH demand

so42

PC.'

NO,

NO,

CI

F

NH,

Density

Residue (acid insoluble)

Unit.

moles OH/g

mil

mil

mil

mil

m/i

m/i

mil

s / m l . mil

Minimum Concentration

Observed

9 93E-05

2 02E-02

< 2 03E-02

2 86E-02

< 1 16E-02

1 40E-02

< 8 89E-04

< 6 22E-02

1 04E+00

5 58E+03

Maximum Concentration

Observed

3 34E-04

1 28E+01

< 1 70E+00

1 93E+00

< 8 14E-01

3 96E-01

1 16E+00

< 5 41E+00

2 28E+00

3 68E+05

N $

14

19

NA

7

NA

17

5

NA

20

20

Mean

1 89E-04

3 09E+00

NA

4 44E-01

HA

1 73E-01

2 96E-01

NA

1 39E+00

8 25E+04

Standard Deviation

6 60E-05

3 38E+00

NA

6 84E-01

NA

1 01E-01

4 88E-01

NA

2 97E-01

9 63E+04

RSD # (%) 35 0

109 6

NA

154 1

NA

58 7

165 1

HA

21 3

116 7

* per g as-settled sludge 5 Summary statistics calculated from the real analytical values * RSD is the relative standard deviation, standard deviation divided by the mean NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data * g as-settled sludge/mL as-settled sludge

38

WHC-SP-1182 Table 4 .3 . Sludge Characterization Data--Per mL As-Settled Sludge.

Analyte

fflCo

137Cs

l34Cs

154Eu

1JSEu

144Ce/Pr

wNb l0ftRu/Rh

™R* 2 » T 1

2l2Bl

,nEu

'"Sb 24'Am - GEA

Alpha Total

Total Beta 239/240pu

238pu

237Np

243/244cm

24lAm - AEA

^Sr

U-222S phosphorescence

U-PNNL fluorescence

U-222S

" 3U &

2*U &

»*U &

"6u &

»8ij &

Unit *

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

uCi/mL

.g/ml.

.g/ml

«/-. .g/ml

.g/ml

.g/ml

.g/ml

.g/ml

Minimum Concentration

Observed

8 46E-02

2 73E+01

< 3 83E-02

< 1 87E-02

< 5 41E-02

< 2 93E-01

< 1 23E-02

< 4 27E-01

< 5 86E-01

< 9 51E-02

< 7 59E-02

< 1 40E-02

< 3 02E-02

1 82E-01

4 52E-01

2 07E+01

1 84E-01

2 83E-02

< 7 21E-04

< 1 14E-01

1 57E-01

1 77E+00

1 31E+03

1 44E+03

1 14E+03

< 1 41E-02

1 10E-01

1 00E+01

1 10E+00

1 43E+03

Maximum Concentration

Observed

2 34E+00

1 48E+03

< 8 83E-01

8 90E+00

4 10E+00

< 1 15E+01

< 4 50E-01

< 1 68E+01

< 2 20E+01

< 1 19E+01

< 3 55E+00

< 7 02E-01

< 3 75E+00

5 35E+01

1 11E+02

3 09E+03

4 48E+01

< 1 09E+01

< 8 54E-03

< 1 28E+01

5 60E+01

1 38E+03

3 67E+04

4 27E+05

9 18E+04

< 4 18E+00

3 49E+01

3 10E+03

2 12E+02

4 24E+05

N S

20

20

NA

18

16

NA

NA

NA

NA

NA

NA

NA

NA

20

20

20

20

9

10

NA

20

20

10

20

17

HA

20

20

20

20

Mean

9 43E-01

2 11E+02

NA

1 59E+00

7 19E-01

NA

NA

NA

HA

NA

NA

NA

NA

8 98E+00

2 04E+01

5 15E+02

8 88E+00

8 62E-01

1 41E-03

NA

8 87E+00

1 79E+02

1 61E+04

5 18E+04

3 43E+04

NA

3 90E+00

3 66E+02

3 39E+01

5 14E+04

Standard Deviation

6 24E-01

3 38E+02

HA

1 98E+00

9 70E-01

NA

NA

NA

NA

NA

NA

HA

HA

1 17E+01

2 46E+01

7 54E+02

9 86E+00

4 99E-01

4 50E-04

NA

1 21E+01

3 11E+02

1 27E+04

9 32E+04

2 85E+04

NA

7 58E+00

6 75E+02

4 77E+01

9 24E+04

(!) 66 2

160 2

HA

124 6

134 9

NA

NA

HA

NA

NA

HA

NA

HA

129 8

121 0

146 5

111 1

57 9

31 9

HA

136 6

174 1

78 8

179 7

83 1

NA

194 5

184 2

140 7

179 7

* per mL as-settled sludge $ Summary statistics calculated from the real analytical values # RSD is the relative standard deviation, standard deviation divided by the mean NA Not applicable for these data

& Calculated using the PNL total uranium (fluorescence) data

39

WHC-SP-1182 Table 4 . 3 . Sludge Charac te r i za t ion Data--Per mL

As-Se t t l ed Sludge. (Continued)

Analyte

Al

Ca

Cd

Cr

Cu

Fe

K

Mg

Ha

N.

Pb

Zn

Zr

Ag

B

Ba

Be

S.

Sm

TI

TIC

TOC

TC

CN

TGA-222S

TGA-PNNL

DSC-wet wt

DSC-dry wt

DSC-PNNL

Unit.

.g/ml

.g/mL

.8/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.8/mL

.g/mL

.g/mL

.g/mL

.8/mL

.g/mL

.g/mL

.6/»L

.g/mL

.g/ml

.8/mL

.8/mL

Joules/mL

Joules/mL

Joules/mL

Minimum Concentration

Observed

8 54E+03

2 68E+02

1 90E+01

4 15E+01

2 46E+01

6 92E+03

< 6 25E+01

1 28E+02

6 14E+01

9 03E+01

4 20E+01

5 44E+01

2 82E+01

< 1 02E+00

< 4 01E+01

2 32E+01

1 76E+00

< 1 02E+01

< 1 02E+01

< 2 04E+01

7 50E+00

3 87E+02

6 68E+02

< 3 11E-01

6 99E+05

1 24E+05

0 00

0 00

0 00

Maximum Concentration

Observed

5 87E+04

3 31E+04

7 64E+01

1 91E+03

9 47E+02

5 22E+05

2 54E+03

4 82E+03

9 84E+02

1 49E+04

1 08E+03

2 09E+03

1 06E+03

< 3 77E+01

7 66E+02

5 64E+02

2 64E+01

< 3 77E+02

< 3 77E+02

< 7 55E+02

3 26E+03

4 03E+03

6 55E+03

< 1 34E+00

9 78E+05

9 80E+05

7 43E+01

2 30E+02

9 68E+00

N S

17

17

17

17

17

17

5

17

17

17

17

17

17

1

14

13

15

NA

HA

NA

17

16

16

NA

11

16

11

11

16

Mean

2 44E+04

6 21E+03

4 19E+01

4 88E+02

2 74E+02

1 56E+05

1 53E+03

1 11E+03

2 94E+02

1 34E+03

2 85E+02

5 72E+02

2 78E+02

1 74E+00

1 31E+02

1 95E+02

1 42E+01

HA

NA

NA

1 08E+03

1 39E+03

2 58E+03

NA

8 36E+05

5 97E+05

6 76E+00

2 09E+01

6 05E-01

Standard Deviation

1 48E+04

9 13E+03

1 43E+01

4 97E+02

2 14E+02

1 38E+05

7 60E+02

1 14E+03

2 41E+02

3 57E+03

2 50E+02

5 OOE+02

2 75E+02

HA

1 85E+02

2 11E+02

6 44E+00

NA

HA

NA

7 88E+02

1 02E+03

1 75E+03

NA

9 68E+04

2.57E+05

2 24E+01

6 93E+01

2 42E+00

RSD # (2)

60 6

147 1

34 1

101 8

78 2

88 3

49 6

103 3

81 8

265 5

87 6

87 4

98 9

NA

141 3

108 4

45 2

NA

NA

" NA

72 8

73 8

67 9

HA

11 6

43 0

331 7

331 7

400 0

* per mL as-settled sludge 5 Summary statistics calculated from the 'real' analytical values # RSD is the relative standard deviation, standard deviation divided by the mean. NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data

40

WHC-SP-1182 Table 4 . 3 . Sludge Charac t e r i za t ion Data- -Per mL

As-Se t t l ed Sludge. (Continued)

Analyte

OH demand

SO,2

P04>

NO,

«°2 CI

F

NH,

Residue (acid insoluble)

Unit.

moles OH/mL

.g/mL

.g/mL

.g/mL

.g/mL

.g/mL

.8/mL

.8/mL

.g/mL

Minimum Concentration

Observed

1 24E-04

2 45E-02

< 2 45E-02

3 46E-02

< 1 41E-02

1 70E-02

< 1 08E-03

< 7 52E-02

5 80E+03

Maximum Concentration

Observed

4 OOE-04

2 03E+01

< 2 38E+00

2 15E+00

< 9 04E-01

5 28E-01

1 62E+00

< 1 23E+01

4 45E+05

N S

14

19

NA

7

HA

17

5

NA

20

Mean

2 44E-04

4 59E+00

HA

5 05E-01

NA

2 39E-01

4 20E-01

HA

1 20E+05

Standard Deviation

9 40E-05

5 39E+00

NA

7 56E-01

NA

1 39E-01

6 81E-01

NA

1 34E+05

RSD # (I)

38 5

117 4

NA

149 8

NA

58 2

162 1

NA

1117

* per mL as-settled sludge 5 Summary statistics calculated from the real analytical values # RSD is the relative standard deviation standard deviation divided by the mean NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data

41

WHC-SP-1182 Table 4 . 4 . Sludge Charac te r i za t ion Data--Per Gram Dried Sludge.

Analyte

"Co

™Cs 134Cs

>"Eu IJJEu

""Ce/Pr

"Nb 106Ru/Rh

^ a

Mll 212Bi

" 2Eu

'"Sb 24lAm - GEA

Alpha Total

Total Beta 239/240pu

23«p„

2J7Np 2«<™Cm 241Am - AEA

»°Sr

U-222S phosphores c enc e

U-PNNL fluorescence

U-222S ICP 2BU & 2«U &

"'U & 2'«U A 2MU &

Unit *

.Ci/g

.Ci/g

.Cl/g

.Cl/g

.Ci/g

.Ci/6

.Ci/8

.Ci/g

.Cl/g

.Ci/g

.Ci/8

.Cl/g

.Cl/g

.Ci/8

.Cl/g

.Ci/g

.Cl/g

.Cl/g

.Ci/g

.Ci/g

.Ci/g

.Cl/g

.8/g

.g/g

.8/6

.8/8

.g/g

.8/8

.8/8

.8/8

Minimum Concentration

Observed

1 85E-01

2 76E+01

< 2 09E-02

< 4 10E-02

< 1 18E-01

< 2 38E-01

< 1 78E-02

< 4 04E-01

< 4 53E-01

< 2 98E-01

< 1 92E-01

< 2 83E-02

< 9 61E-02

3 97E-01

9 88E-01

6 98E+01

4 03E-01

6 18E-02

< 1 18E-03

< 2 50E-01

3 43E-01

6 36E+00

2 87E+03

3 14E+03

2 49E+03

< 3 08E-02

2 41E-01

2 20E+01

2 42E+00

3 12E+03

Maximum Concentration

Observed

5 40E+00

1 27E+03

5 78E-01

1 18E+01

5 76E+00

< 7 17E+00

< 2 68E-01

< 1 07E+01

< 1 39E+01

< 8 91E+00

< 2 S9E+0D

< 3 62E-01

< 2 81E+00

7 44E+01

1 68E+02

2 66E+03

6 73E+01

< 3 48E+01

< 1 22E-02

< 1 58E+01

7 13E+01

1 22E+03

1 31E+05

3 27E+05

4 37E+05

< 3 20E+00

2 62E+01

2 33E+03

2 47E+02

3 25E+05

N $

19

19

7

17

16

NA

NA

NA

NA

HA

HA

2

HA

19

19

19

19

9

10

HA

19

19

10

15

16

NA

15

15

15

15

Mean

2 20E+00

3 06E+02

1 99E-01

4 15E+00

1 95E+00

NA

NA

NA

NA

NA

NA

1 65E-01

NA

2 31E+01

5 29E+01

8 21E+02

2 31E+01

3 78E+00

4 49E-03

NA

2 26E+01

2 82E+02

4 13E+04

9 87E+04

9 13E+04

NA

7 01E+00

6 93E+02

6 93E+01

9 80E+04

Standard Deviation

1 24E+00

3 57E+02

1 82E-01

3 52E+00

1 63E+00

NA

NA

NA

NA

NA

NA

3 77E-02

NA

2 16E+01

4 98E+01

8 40E+02

2 03E+01

3 68E+00

3 34E-03

NA

2 13E+01

3 42E+02

1 00E+05

1 01E+05

NA

7 59E+00

7 18E+02

6 52E+01

9 96E+04

RSD # U )

56 4

116 9

91 4

84 7

83 5

NA

NA

NA

NA

HA

HA

22 8

NA

93 7

94 1

102 3

87 7

97 4

74 3

NA

93 9

121 5

85 0

1017

110 9

NA

108 2

103 6

94 1

1017

* per g dried sludge $ Summary statistics calculated from the real analytical values # RSD is the relative standard deviation, standard deviation divided by the mean

NA Not applicable for these data & Calculated using the PNL total uranium (fluorescence) data

42

WHC-SP-1182 Table 4 . 4 . Sludge Charac t e r i za t ion Data- -Per Gram

Dried Sludge. (Continued)

Analyte

Al

Ca

Cd

Cr

Cu

Fe

K

Ms Mn

N.

Pb

Zn

Zr A8

B

Ba

Be

Se and Sm

TI

CH

TIC

TOC

TC

OH demand

SO.2

PO.'

NO,

NO;

Cl

F

Residue (acid insoluble)

unit.

.8/8

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

mil

moles OH/g

.g/g

.6/6

.8/8

.6/6

mil

mil

mil

Minimum Concentration

Observed

1 87E+04

9 21E+02

3 92E+01

9 38E+01

5 39E+01

1 51E+04

5 93E+02

6 51E+02

2 08E+-02

2 92E+02

1 60E+02

1 19E+02

6 18E+01

< 2 22E+00

< 8 07E+01

< 1 13E+02

3 86E+00

< 2 22E4-01

< 4 45E+01

< 6 67E-01

1 26E+03

1 88E+03

3 23E+03

1 87E-04

6 17E-01

< 6 27E-02

2 27E-01

< 5 64E-02

2 12E-01

< 2 03E-02

5 73E+04

Maximum Concentretion

Observed

1 33E+05

2 89E+04

3 50E+02

1 53E+03

1 33E+03

4 46E+05

2 66E+03

5 04E+03

8 47E+02

3 26E+04

1 08E+03

1 94E+03

8 87E+02

< 3 53E+01

6 19E+02

6 57E+02

1 62E+02

< 3 53E+02

< 7 07E+02

< 6 24E+00

2 06E+04

8 81E+03

1 43E+04

2 OOE-03

6 70E+01

< 1 22E+01

1 67E+01

< 7 02E+00

3 70E+00

3 35E+00

9 73E+05

N S

16

16

16

16

16

16

5

16

16

16

16

16

16

1

13

12

14

NA

NA

HA

16

16

16

14

19

NA

7

NA

17

5

19

Mean

5 93E+04

8 87E+03

1 30E+02

7 76E+02

6 24E+02

2 66E+05

1 77E+03

1 98E+03

5 72E+02

2 72E+03

5 25E+02

1 10E+03

5 37E+02

1 24E+01

2 61E+02

3 38E+02

5 02E+01

NA

NA

NA

3 65E+03

3 24E+03

6 20E+03

7 66E-04

1 76E+01

NA

4 69E+00

NA

1 42E+00

1 08E+00

2 03E+05

Standard Deviation

3 07E+04

8 50E+03

9 73E+01

3 94E+02

3 57E+02

1 24E+05

7 49E+02

1 04E+03

1 B5E+02

7 99E+03

2 10E+02

4 49E+02

2 80E+02

NA

1 59E+02

1 72E+02

4 56E+01

NA

NA

NA

4 61E+03

1 71E+03

2 80E+03

4 94E-04

1 85E+01

NA

5 92E+00

NA

1 08E+00

1 32E+00

(») 51 8

95 8

74 8

50 8

57 2

46 7

42 3

52 3

32 4

294 0

40 1

41 0

52 2

HA

60 8

51 0

90 8

NA

NA

NA

126 4

52 6

45 1

64 5

105 2

NA

126 2

NA

76 1

122 1

105 4

* per g dried sludge 5 Summary statistics calculated from the real analytical values # RSD is the relative standard deviation, standard deviation divided by the mean NA Not applicable for these data 6 Calculated using the PNL total uranium (fluorescence) data

43

WHC-SP-1182 Table 4 . 5 . Comparison of La tes t Data for KE Floor Sludge

vs. E a r l i e r Data for the KE Floor .

Analyte Unit

KE Basin Sludge Samples (Miller 1996)

Minimum Concentration

Observed

Maximum Cone entr at i on

Observed

KE Basin Sludge Samples (Bechtold 1993)

Minimum Concentration

Obs erved

Maximum Concentration

Observed

per gram dried sludge

*Co ,37Cs

, MEu

'"Eu

341 Am - GEA

Alpha Total

Total Beta

239/240pu

I41Am - AEA

"Sr

U-222S

Al

Ca

Cd

Cr

Cu

Fe

K

Mg

Mn

Na

Pb

Zn

Zr Ba

Be

Sm

TI

MCi/g

(*Ci/g

/*Ci/g

^Ci/g

MCi/g

/.Ci/g

WCi/g

*Ci/g

MCi/g

/iCi/g

M/g

Mg/g

*.g/g

Mg/g

*g/g

w/s *g/ s

M / 8

*g/g

^8/8

Mg/g

M8/g

«/e Mg/g

Mg/g

^8/8

*g/g

Mg/g

1 85E-01

2 76E+01

< 4 10E-02

< 1 18E-01

3 97E-01

9 88E-01

6 98E+01

4 03E-01

3 43E-01

6 36E+00

2 87E+03

1 87E+04

9 21E+02

3 92E+01

9 38E+01

5 39E+01

1 51E+04

5 93E+02

6 51E+02

2 08E+02

2 92E+02

1 60E+02

1 19E+02

6 18E+01

< 1 13E+02

3 86E+00

< 2 22E+01

< 4 45E+01

5 40E+00

1 2^E+03

1 18E+01

5 76E+00

7 44E+01

1 68E+02

2 66E+03

6 73E+01

7 13E+01

1 22E+03

1 31E+05

1 33E+05

2 89E+04

3 50E+02

1 53E+03

1 33E+03

4 46E+05

2 66E+03

5 04E+03

8 47E+02

3 26E+04

1 08E+03

1 94E+03

8 87E+02

6 57E+02

1 62E+02

< 3 53E+02

< 7 07E+02

4 30E-01

1 05E+01

3 70E-01

1 70E-01

1 66E+00

3 92E+00

4 60E+01

1 92E+00

5 07E+00

7 01E+00

7 81E+03

3 60E+03

6 35E+02

5 06E+01

3 60E+01

9 40E+01

1 17E+04

4 42E+01

1 72E+02

1 56E+02

3 72E+01

4 38E+01

1 60E+02

1 69E+01

2 71E+01

3 09E+00

1 32E+01

3 10E+01

1 63E+00

4 75E+01

1 66E+00

9 72E-01

8 13E+00

1 70E+01

2 39E+02

6 83E+00

6 88E+01

8 81E+01

4 04E+05

2 43E+04

4 38E+03

9 59E+01

1 18E+03

3 69E+02

2 85E+05

2 OOE+02

1 07E+03

4 30E+02

1 50E+02

6 19E+02

1 25E+03

2 22E+02

1 16E+02

2 48E+01

6 65E+02

2 17E+02

per gram centrifuged sludge

Density g/mL S [J 0 99 3 81 | 1 22 1 67

per gram as-settled sludge

Density g/mL & || 1 0 * 2 28 || 1 11 1 54 "5 g centrituged sludge/mL centriluged sludge & g as-settled sludge/mL as-settled sludge

44

WHC-SP-1182

Table 4.6. Comparison of Latest K East Floor Sludge Data Versus Previous Sandfilter Backwash Pit Data.

Analyte Un„

KE Basin Sludge Samples (Miller 1996)

Minimum Concentration

Observed

Maximum Concentration

Observed

KE Basin Sandfifter Backwash Pit (SFBWP) Samples

(Welsh 1994)

Minimum Concentration

Observed

Maximum Concentration

Observed

per mL as-settled sludge

6°Co

' " c .

<5*Eu

'6 5

Eu

2 4 1Am ■ GEA

Alpha Total

Total Beta

239/240pu

2 4 1Am - AEA

U-222S

Al

C .

Cd

C,

Cu

Fe

M g

M n

Na

Pb

2n

Ba

Be

Sm

Density

UOImL

*0/mL

.C,/mL

AO/mL

K V m l

jKWmL

.Ci/mL

.Ci /ml

.CI/mL

« /mL

«g/mL

« t a L

«,/mL

«,/mL

« /mL

« /mL

OT/mL

« /mL

M'mL

.8/mL

.g/mL

.g/mL

« /mL

«/mL

g/mL-

8 46E 02

2 73E + 01

< 1 87E-02

< 5 41E-02

1 82E 01

4 52E-01

2 07E + 01

1 84E-01

1 57E-01

1 31E + 03

8 54E + 03

2 68E + 02

1 90E + 01

4 15E + 01

2 46E + 01

6 92E + 03

1 28E + 02

6 14E + 01

9 03E + 01

4 20E + 01

5 44E + 01

2 32E + 01

1 76E + 00

< 1 02E + 01

1 0 4

2 34E + 00

1 48E + 03

8 90E + 00

4 10E + 00

5 35E + 01

1 11E + 02

3 09E + 03

4 48E+01

5 60E + 01

3 67E + 04

5 87E + 04

3 31E+04

7 64E + 01

1 91E + 03

9 47E + 02

5 22E + 05

4 82E + 03

9 84E + 02

1 49E + 04

1 08E + 03

2 09E + 03

5 64E + 02

2 64E + 01

< 3 77E+02

2 28

1 46E-01

5 02E + 00

161E-01

8 54E-02

6 60E 01

1 36E + 00

7 77E + 00

7 68E 01

7 73E-01

3 48E + 03

3 00E + 03

1 85E + 02

6 70E + 00

3 06E + 01

5 43E + 01

6 59E + 03

6 53E + 01

411E + 01

4 63E + 01

3 49E + 01

6 10E + 01

1 03E + 01

1 70E + 0O

NA

1 0 4

2 98E 01

2 21E + 01

3 54E-01

1 90E-01

1 82E + 00

3 05E + 00

7 07E + 01

2 24E+00

1 66E + 00

9 20E+03

7 49E + 03

8 44E + 03

5 15E + 01

2 76E + 02

3 15E + 02

5 82E + 04

7 32E + 02

2 78E + 02

7 47E + 02

7 41E + 01

2 64E + 02

1 20E + O2

4 37E + 00

5 80E + 01

, 5 3

NA Not available * g as settled sludge/ mL as-settled sludge

45

WHC-SP-1182

5.0 REFERENCES

Baker, R. B., 1995a, Summary Status of K Basins Sludge Characterization, WHC-SD-SNF-TI-006.

Baker, R. B., 1995b, "System Design Description: for Sampling Sludge Equipment for K Basin Floor Sludge," WHC-SD-SNF-SDD-003, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

Bechtold, D. B., 1995, "Report of Laboratory Test Plan for Analysis of K East Basin Backwash Pit Samples," WHC-SD-NR-TRP-021, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

Bechtold, D. B., and M. A. Mier, 1995, "Analyses of 105-K East Basin Sludge Samples," WHC-12110-PCL-069, Westinghouse Hanford Company, Richland, Washington.

Golcar, G. R., and M. R. Powell, 1994, "Strategy for Development of Accurate Simulants for Waste Retrieval and Transport Testing, DSTRTP-CY94-004, Letter Report prepared for the U.S. Department of Energy by Pacific Northwest Laboratory, Richland, Washington.

Makenas, B. J., et al., 1994, "DOE Spent Nuclear Fuel Challenges and Initiatives," Salt Lake, page 326, Westinghouse Hanford Company, Richland, Washington.

Makenas, B. J., 1995, "Data Quality Objectives for K East Basin Floor and Weasel Pit Sludge Sampling," WHC-SD-SNF-DQO-005, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

Meling, T. A., "Sludge Measurement Results for 105 K East Basin," WHC-SD-WM-ANAL-037, October 26, 1994.

Miller, G. L., 1995, "Interim Chemical and Radiochemical Analytical Report of 105-K East Basin Sludge," WHC-SD-SNF-DP-004, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

Miller, G. L., 1996, "Chemical and Radiochemical Analytical Report of 105-K East Basin Sludge," WHC-SD-SNF-DP-004, Rev. 1C, Westinghouse Hanford Company, Richland, Washington.

Silvers, K. L., 1995, "K Basin Sludge Sample Analysis," Rev. 0, Pacific Northwest National Laboratory, Richland, Washington.

Welsh, T. L., et al., 1995, "Sampling and Analysis Plan for Floor Sludge in the 105-K East Main Basin and Weasel Pit," WHC-SD-SNF-PLN-006, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

Welsh, T. L., 1994, "Statistical Evaluation of the Data Obtained from the K East Basin Sandfilter Backwash Pit Samples," WHC-SD-SNF-TI-004, Rev. 0, Westinghouse Hanford Company, Richland, Washington.

46

WHC-SP-1182

A P P E N D I X A

DEPTHS OF SLUDGE OBSERVED DURING SAMPLING AND THE REVISED CALCULATED VOLUME OF SLUDGE IN THE K EAST WEASEL PIT

R. B. Baker, P. J. MacFarlan, and S. L. Hecht

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WHC-SP-1182

APPENDIX A DEPTHS OF SLUDGE OBSERVED DURING SAMPLING AND THE REVISED

CALCULATED VOLUME OF SLUDGE IN THE K EAST WEASEL PIT

The design of the K Basin Floor Sludge Sampling equipment uses isolation tubes (i.e., the tubes used to isolate the cores of sludge) which have scales showing distance in inches from the bottom of the tube. These scales were viewed with underwater video cameras during the sludge sampling. Observed depths of floor sludge being sampled were compared to these scales. The resulting depth measurements were similar (Section 3.1, Table 3.2) to the local sludge depths measurements made at K East in 1994 using more accurate methods (Meling 1994). While the sludge depths were generally found to correspond, there were prior depth measurements only available for the sludge on the K East Main Basin floor. (The only remote pit at K East that has had sludge depth measurements was the Sandfilter Backwash Pit, Baker 1995a).

There were no prior direct measures of sludge depths for the Weasel Pit Floor. Prior estimates of depths (Baker 1995a) and corresponding sludge volumes were made based on staff observations from the grating, then conservatively assuming depths biased toward the deeper values. Experience has shown that such estimates can be inexact and misleading because of parallax in the deep water and lack of known reference points of depth. The insertion of the isolation tubes for the sampling of sludge in the Weasel Pit provided the first opportunity to obtain accurate measurements of the sludge depths and the corresponding calculation of sludge volume.

Figure Al shows one of the five isolation tubes, used in the Weasel Pit, inserted into the sludge with the scale in evidence (i.e., sludge depth is about 30 in.). Figure A2 indicates the sludge depths measured and recorded on video tape. The Weasel Pit has the deepest accumulations of sludge in the K East Basin with depths ranging from 0.33 to 0.96 m (12 to 35 in.). The depths were:

KES-S-16 30.4 cm (12 in.) KES-Q-17 76.2 cm (30 in.) KES-R-18 71.1 cm (28 in.) KES-S-19 86.4 cm (34 in.) KES-S-20 88.9 cm (35 in.)

Three dimensional curve fitting software was used to fit the spacial data on sludge depth versus location in the Weasel Pit, similar to that done previously for the Sandfilter Backwash Pit. The resulting sludge surface is shown in Figures A3 and A4 (the linear dimensions in these figures are in centimeters).

The Weasel Pit has a micron level screen across West end which allows a flow of water and small particles back into the Main Basin. The sludge depths are significantly lower on this end of the pit. On the deeper East end it was noted that there may be a foundation or step in the concrete floor of the pit, because the isolation tube extended higher by about 15.2 cm (6 in.) out of the pool even when seated firmly on the floor at this location. The later is not

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WHC-SP-1182

represented in any of the figures as this "step" was not characterized, being beyond the scope of this sampling. The placement of the Eastern most isolation tube reflects (note distance from south wall) the attempt to move the tube off this step, however this could not be accomplished.

Given the mathematical fit of the surface of the sludge, as indicated in Figures A3 and A4, an integration was made to calculate the volume of sludge present in the Weasel Pit. The result was 7.4 m (260 ft ) providing an approximate average sludge depth of about 0.7 m (27 in.). This is 30% less than estimates previously made (Baker 1995a) of 10.3 m (365 ft3). Any quantification of volumes of components of the sludge (i.e., from the chemical analyses) should use this more accurate value for volume. While the data on depths in the Weasel Pit do not come from locations intended to optimize accuracy of the volume integration they represent a significant improvement in accuracy over any prior estimates. It should be further noted that the Weasel Pit has continued to have sludge from both the Main Basin and the South Loadout Pit pumped into it since the depth measurements described here were made. The impact of this pumping is beyond the scope of the present evaluation.

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WHC-SP-1182

Figure Al Isolation Tube Seated in Weasel Pit Sludge

BEST AVAILABLE COPY

WHC-SP-1182

Figure A2. Weasel Pit Sampling Sludge Sampling Locations and Corresponding Sludge Depths.

-N —

KES-R-18 |71cm(28 )|

KES-0-17 |76cm(30")|

KES-P-16 |30cm(12")|

-[l6Bcm(5 -6")]

KES-S-19 J86cm(34 )J

[315cm(10-4-)l

•[36cm(1 -2 - ) ]

[340cm(,1 -2 )]

-[I35cm(4 -5")]

M 1 SCREEN BETWEEN WEASEL

PIT AND TRANSFER CHANNEL TO MAIN BASIN

2 SPECIAL BRACKETS TO SUPPORT ISOLATION TUBES

i | SLUDGE DEPTH MEASURED

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Figure A3. Three Dimensional Representation of Sludge Surface in K East Weasel Pit.

A-7 BEST AVAILABLE COPY

WHC-SP-1182

Figure A4. Two Dimensional Representation of Sludge Surface in K East Weasel Pit.

w in _ u3 i/> u> c o m s s N t o m i f l i o i n ' e v v n n

Q CVJ <o O i CO CO

X Oi Q

» 0=

o o o o o LO O LO O

i - i - CM

A-8 BEST AVAILABLE COrY

WHC-SP-1182

A P P E N D I X B

THE CHEMISTRY OF CENTRIFUGED SLUDGE

T. L. Welsh, D. B. Bechtold, and B. A. Crawford

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WHC-SP-1182 The 222-S analytical data presented in the following tables were generated using an electronic transfer from LABCORE, the 222-S Laboratory database. The PNNL analytical data presented in the following tables were obtained from Silvers, 1995. The sample locations, used in the following tables, are defined as follows;

Location

1 2 3 4 5 6

8 9 10 11 12

15

16 17 18 19 20 21 22 23

Archived

Archived

SAP Sample Number

L-01

A 02

B-03

C-04

N-05

J-06

H-08

0-09

F-10

E-11

K 12

1-15

P-16

Q-17

R-18

S-19

M-13 (top)

M 13 (bottom)

T-20 (top)

T-20 (bottom)

G-07

D-14

Lattice Location

1257

4516

2935

2771

1268

0133

6755

6070

6718

1424

0168

Uest of 6722

Slot Uest

Slot Mid

Opening Mid North

Opening Mid South

1266

1266

Opening East End

Opening East End

5253

2771

North/south

South

North

South

North

South

south

South

North

south

south North

NA NA NA NA

North

North

NA NA

North

South

Mam Basin

Main Basin

Main Basin

Main Basin

Main Basin

Mam Basin - Ueasel Pit mouth

Main Basin

Main Basin

Main Basin

Main Basin

Main Basin mouth of Dummy Elevator Pit

Mam Basin - mouth of South Loadout Pit

Weasel Pit

Weasel Pit

Weasel Pit

Weasel Pit

Mam Basin (near #5)

Main Basin (near #5)

Ueasel Pit

Ueasel Pit

Mam Basin

Main Basin (near #4)

The tables in this appendix do not include the duplicate analyses data which were performed according to the SAP. If both the analytical result and the duplicate result were "real" numbers, then the two values were averaged. If the analytical result was a "real" number and the duplicate result was a "less than" number, then the "real" number was reported. If the analytical result was a "less than" number and the duplicate result was a "real" number, then the "real" number was reported. If both the analytical result and the duplicate result were both "less than" numbers, then the maximum value of the "less thans" was reported. Research samples (M-13 and T-20) were shipped to PNNL on an as-settled sludge basis. Sample S-19 was also shipped to PNNL on an as-settled sludge basis. All other samples were shipped to PNNL on a centrifuged sludge basis. Research sample T-20

B-3

WHC-SP-1182 (top) was analyzed at 222-S Laboratory on an as-settled sludge basis. All other samples were analyzed at 222-S Laboratory on a centrifuged basis. The analyses of the water soluble analytes were performed on the supernatant water from the centrifugation of the sludge samples. These analytes include sulfate, phosphate, nitrate, nitrite, chloride, fluoride, ammonia, and pH. The units associated with these analyses are /Vg/mL separated liquid.

Four water samples were also analyzed by both laboratories. The four water samples were:

• water collected from sample M-13 prior to centrifugation • water collected from sample T-20 prior to centrifugation • an equipment blank (water from KE-Basin) • a hot cell blank.

The reported units for these samples are either /vg/mL liquid or ,1/Ci/mL liquid. The water results for all but the hot cell blank are also included here. The PNNL uranium isotopic results were reported in atom %. The units for the uranium isotopics were changed to /jg/g centrifuged sludge using the following formula. For each sample location, Au was calculated using equation 1.

_ 2 3 3 . 0 4 / 2 n a + 2 3 4 . 0 4 / »»„ + 2 3 5 . 0 4 / 2 3 S a

* " + 2 3 6 . 0 5 / 2 J S „ + 2 3 8 . 0 5 / J S e D ( 1 )

where = atom%u1

100 K '

Equation 3 was then used to convert the units, each isotope separately, to g/g centrifuged sludge.

Dl D T^ 100 (3)

where U, = 233U, U2 = 2 M U , U3 = 235U, U4 = 236U, U5 > 23aU,

A, = 233.04, A2 - 234.04, A3 = 235.04, A4 = 236.05, A5 = 238.05,

%, is the atom% for the uranium isotope of interest, Cu is the total uranium concentration (C), as measured by PNNL (units of yg/g

centrifuged sludge), for the sample of interest.

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Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

"Co uCi/g

5.60E-01 8.84E-01 6.88E-01 8.88E-01 6.41E-01 6.30E-01 7.03E-02 6.98E-01 1.91E+00 6.46E-01 1.30E+00 9.67E-01 1.22E+00 9.94E-01 3.00E-01 1.04E+00 7.10E-01 4.50E-01 NA 1.09E*00

'"Ce/Pr uCi/q

< 1.47E+00 < 1.97E-01 < 1.53E-01 < 2.55E-01 < 2.44E-01 < 1.72E-01 < 1.93E-01 < 4.69E+00 < 1.35E-01 < 1.64E-01 < 9.51E-02 < 1.68E-01 < 7.87E-01 < 8.60E-01 < 2.50E-01 < 1.56E*00 < 1.12E+00 < 1.46E*00

NA < 1.16E+00

"'Cs uCi/g

1.59E+02 2.24E+01 1.77E+01 4.77E+01 4.59E+01 2.30E+01 5.46E+01 7.24E*02 2.07E+01 2.36E+01 1.10E+01 3.29E+01 9.13E+01 7.95E*01 5.33E+01 3.39E+02 2.76E+02 2.03E+02 NA 3.35E*02

"Nb uCi/g

< 8.03E-02 < 1.59E-02 < 1.50E-02 < 2.29E-02 < 1.62E-02 < 1.31E-02 < 6.75E-03 < 1.54E-01 < 1.22E-02 < 1.49E-02 < 8.45E-03 < 1.06E-02 < 3.25E-02 < 4.57E-02 < 1.04E-02 < 5.21E-02 < 4.88E-02 < 6.92E-02

NA < 4.83E-02

'"Cs uCi/g

< 1.10E-01 < 1.28E-02 < 1.28E-02 < 2.10E-02

1.91E-02 < 9.19E-03

2.77E-02 < 3.54E-01 < 1.20E-02 < 1.36E-02 < 8.33E-03 < 1.36E-02 < 4.99E-02 < 6.75E-02

2.08E-02 1.18E-01 1.26E-01 9.92E-02 NA 1.30E-01

""Ru/Rh uCi/g

< 2.14E+00 < 3.10E-01 < 2.49E-01 < 4.07E-01 < 3.80E-01 < 2.69E-01 < 2.91E-01 < 7.01E+00 < 2.31E-01 < 2.60E-01 < 1.62E-01 < 2.59E-01 < 9.62E-01 < 1.31E+00 < 3.83E-01 < 2.37E+00 < 1.53E+00 < 2.15E+00

NA < 1.76E-KI0

"'Eu «Ci/g

3.54E+00 9.34E-01 1.09E4-00 2.34E+00 1.02E+00 7.06E-01

< 1.56E-02 4.37E+00 3.21E-01 1.14E+00 2.56E-01

< 3.39E-01 1.29E+00 1.11E+00 2.41E-01 6.36E-01 1.85E+00 2.31E+00 NA 7.05E-01

'"Ra oCi/g

< 2.78E+00 < 3.79E-01 < 2.92E-01 < 4.93E-01 < 4.74E-01 < 3.31E-01 < 3.97E-01 < 9.06E+00 < 2.74E-01 < 3.16E-01 < 1.81E-01 < 3.41E-01 < 1.32Et00 < 1.69E+00 < 4.88E-01 < 3.03E+00 < 2.45E-1-00 < 2.99E+00

NA < 2.37E+00

'"Eu uCi/g

1.73E+00 4.22E-01 5.34E-01 1.04E+00 4.47E-01 3.40E-01

< 4.50E-02 2.01E+00 1.63E-01 5.63E-01 1.70E-01 1.59E-01 7.30E-01 4.32E-01 1.38E-01

< 3.83E-01 6.30E-01 9.01E-01 NA

< 3.56E-01

"'TI uCi/g

< 1.79E-MM < 2.48E-01 < 1.91E-01 < 3.20E-01 < 3.08E-01 < 2.15E-01 < 2.60E-01 < 5.83E+00 < 1.82E-01 < 2.04E-01 < 1.19E-01 < 2.23E-01 < 8.33E-01 < 1.08E+00 < 3.15E-01 < 1.95E+00 < 1.49E+00 < 1.95E+00

NA < 1.55E1-00

//Ci/g: //Ci/g centrifuged sludge NA: Not analyzed.

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WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

" ! B i

uCi/Q

< 6.59E-01

< 1.37E-01

< 1.12E-01

< 1.86E-01

< 1.48E-01

< 1.10E-01

< 1.11E-01

< 1.74E+00

< 1.27E-01

< 1.12E-01

< 8.70E-02

< 1.11E-01

< 3.15E-01

< 4.20E-01

< 1.37E-01

< 7.84E-01

< 6.31E-01

< 6.38E-01

NA

< 7.21E-01

Tota l Beta

uCi/Q

7.97E+02

4.69E+01

6.15E+01

1.42E*02

1.23E*02

8.45E+01

1.40E+02

1.52E+03

3.81E+01

5.92E+01

3.06E+01

7.95E+01

3.03E+02

2.56E-MJ2

1.26E-M32

9.17E+02

4.72E+02

7.67E+02

NA

8.69E+02

' "Eu

uCi /g

< 1.07E-01

< 2.75E-02

< 1.91E-02

< 3.27E-02

< 2.26E-02

7.48E-02

< 8.31E-02

< 2.37E-01

< 2.21E-02

< 5.39E-02

< 1.13E-02

< 1.79E-02

< 6.09E-02

< 7.93E-02

7.53E-02

< 8.57E-02

< 5.39E-02

< 1.12E-01

NA

< 7.06E-02

" " " " P u

uCi /q

8.98E+00

5.90E+00

7.73E*00

1.48E+01

6.61E+00

5.75E+00

1.53E-01

2.20E+01

2.24E+00

7.90E+00

1.83E+00

2.46E+00

1.14E*01

8.19E+00

1.78E+00

5.17E*00

1.47E+01

1.62E+01

NA

4.85E+00

' "Sb

i iC i /q

< 5.68E-01

< 7.81E-02

< 6.04E-02

< 1.02E-01

< 9.77E-02

< 6.86E-02

< 8.45E-02

< 1.84E+00

< 5.98E-02

< 6.53E-02

< 3.84E-02

< 7.33E-02

< 2.48E-01

< 3.44E-01

< 1.01E-01

< 6.25E-01

< 4.51E-01

< 6.35E-01

NA

< 5.07E-01

'"PU

uCl /g

1.30E+00

< 1.92E+00

1.40E-1-00

2.25E*00

1.07E+00

9.19E-01

2.35E-02

< 5.36E*00

3.71E-01

< 1.92E+00

< 6.47E-01

< 9.55E-01

< 3.10E+00

< 1.38E+00

< 6.50E-01

8.50E-01

< 7.61E+00

< 4.31E*00

NA

7.73E-01

"'Am - GEA

l/Ci/q

2.23E+01

5.53E+00

6.72E+00

1.39E+01

6.32E+00

4.70E*00

1.51E-01

2.63E+01

2.00E*00

7.03E*00

1.49E*00

2.15E+00

8.74E+00

7.16E*00

1.37E+00

3.88E+00

1.10E*01

1.50E+01

NA

4.16E+00

" 'Np

j /C i /g

1.50E-03

< 1.49E-03

1.55E-03

1.10E-03

< 1.04E-03

< 9.75E-04

< 8.70E-04

< 4.14E-03

< 1.036-03

1.23E-03

< 5.78E-04

< 1.46E-03

9.07E-04

1.23E-03

1.49E-03

7.32E-04

1.62E-03

1.67E-03

NA

< 9.08E-04

Alpha Tota l

/<Cl/g

5.04E*01

7.48E+00

1.66E+01

3.40E+01

1.58E+01

1.34E+01

3.76E-01

5.46E+01

5.48E+00

1.37E+01

4.17E+00

5.10E+00

1.92E+01

1.68E*01

3.09E+00

1.06E+01

2.37E*01

3.73E+01

NA

1.02E+01

" " " ' C m

uCi /g

< 3.52E+00

< 7.42E-01

< 2.01E+00

< 3.21E+00

< 2.62E+00

< 6.15E-01

< 9.50E-02

< 6.31E+00

< 4.91E-01

< 2.21E+00

< 2.70E-01

< 2.51E-01

< 2.74E+00

< 1.29E+00

< 9.78E-01

< 9.96E-01

< 2.55E+00

< 5.55E+00

NA

< 1.01E»00

/ / C i / g : / /C i /g cen t r i f uged studge NA: Not analyzed.

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Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

"'Am - AEA

uCi /g

2.146+01

5.116+00

6.60E+00

1.416+01

6.246+00

4.366+00

1.316-01

2.756+01

1.926+00

6.736+00

1.386+00

2.046+00

8.536+00

6.706+00

1.616+00

4.056+00

1.076+01

1.466+01

NA

3.98E+00

™U

Atom) !

< 1.OOE-03

< 1.OOE-03

< 1.00E-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

< 1.OOE-03

NA

NA

NA

NA

NA

- S r

» c i / g

3.66E+02

1.51E+01

1.77E+01

7.01E+01

3.416+01

2.68E+01

3.67E+01

6.78E+02

4.37E+00

1.84E+01

2.54E+00

2.22E+01

1.24E+02

7.97E+01

3.77E+01

2.59E+02

1.15E+02

2.69E+02

NA

1.84E+02

™U

Atom X

7.05E-03

6.OOE-03

6.30E-03

6.90E-03

6.75E-03

7.55E-03

7.80E-03

8.30E-03

7.30E-03

7.30E-03

7.20E-03

6.80E-03

7.10E-03

6.80E-03

7.95E-03

NA

NA

NA

NA

NA

phosphorescence

uq/q

NA

NA

6.84E+03

NA

8.70E+03

9.75E+03

1.09E+03

NA

1.09E+04

2.84E+04

NA

NA

2.80E+04

2.97E+04

1.10E+04

1.67E+04

NA

NA

NA

NA

™u Atom %

7.13E-01

6.95E-01

7.00E-01

7.04E-01

7.01E-01

7.04E-01

7.07E-01

7.34E-01

6.95E-01

7.01E-01

6.94E-01

6.98E-01

7.09E-01

7.05E-01

6.97E-01

NA

NA

NA

NA

NA

. , U-PNNL f luorescence

ug/q

9.80E+04

1.99E+04

2.14E+04

2.03E+04

2.13E+04

2.26E+04

1.20E+03

2.10E+05

1.37E+04

2.20E+04

1.27E+04

1.76E+04

5.75E+04

4.77E+04

1.28E+04

NA

NA

NA

NA

NA

~u Atom %

7.60E-02

7.60E-02

8.00E-02

7.90E-02

7.70E-02

7.45E-02

7.75E-02

5.OOE-02

7.80E-02

7.30E-02

7.60E-02

7.90E-02

7.55E-02

7.50E-02

7.60E-02

NA

NA

NA

NA

NA

W S

uq/q

1.31E+05

2.37E+04

1.83E+04

3.66E+04

2.50E+04

2.49E+04

9.46E+02

NA

1.25E+04

2.22E+04

1.31E+04

1.89E+04

6.65E+04

4.81E+04

1.08E+04

3.33E+04

NA

NA

NA

3.55E+04

"•u Atom %

9.92045E+01

9.92230E+01

9.92140E+01

9.92100E+01

9.92160E+01

9.92145E+01

9.92080E+01

9.92070E+01

9.92200E+01

9.92180E+01

9.92220E+01

9.92160E+01

9.92085E+01

9.92140E+01

9.92190E+01

NA

NA

NA

NA

NA

/ / C i / g : / /C i /g cen t r i f uged sludge / / g / g : //g/g cen t r i f uged sludge

NA: Not analyzed.

B-7

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Al

1.94E+04 2.98E+04 1.69E+04 2.36E+04 2.22E+04 1.32E+04 7.10E+03 HA 2.40E+04 1.78E+04 2.39E+04 3.38E+04 1.91E+04 1.99E+04 1.44E+04 3.09E+04 NA NA NA 3.22E+04 Fe

2.44E+04 1.21E+05 2.06E+04 6.48E+04 3.56E+04 1.59E+05 5.75E+03 NA 2.18E+05 6.02E+04 1.51E+05 2.16E+05 2.06E+05 1.09E+05 2.42E+05 1.61E+05 NA NA NA 1.46E+05

Ca »g/g

7.69E+02 9.B3E+02 5.64E+02 2.04E+03 6.11E+03 2.81E+03 4.64E+03 NA 6.62E+02 1.63E+03 3.68E+02 9.45E+02 3.01E+03 3.36E+03 8.21E+03 9.00E+03 NA NA NA 1.57E+04 Mg

1.95E+02 6.59E+02 2.06E+02 7.46E+02 1.07E+03 1.01E+03 8.57E+02 NA 7.76E+02 4.1BE+02 5.23E+02 4.22E+02 7.45E+02 9.34E+02 1.14E+03 1.50E+03 NA NA NA 1.65E+03

Cd uq/q

4.10E+01 5.50E+01 4.46E+01 6.32E+01 5.26E+01 6.30E+01 2.24E+01 NA 4.38E+01 6.16E+01 2.79E+01 4.56E+01 3.47E+01 4.17E+01 2.14E+01 2.73E+01 NA NA NA 2.72E+01

Mn //g/g 9.04E+01 2.15E+02 9.90E+01 1.90E+02 1.56E+02 2.98E+02 7.89E+01 NA 2.58E+02 1.84E+02 2.45E+02 3.58E+02 2.94E+02 2.26E+02 3.14E+02 2.76E+02 NA NA NA 4.48E+02

Cr

8.33E+01 3.43E+02 6.67E+01 1.76E+02 1.04E+02 5.64E+02 3.56E+01 NA 4.33E+02 1.69E+02 3.07E+02 2.92E+02 7.30E+02 3.79E+02 8.35E+02 5.13E+02 NA NA NA 6.60E+02 Na

2.08E+02 3.15E+02 1.53E+02 1.79E+02 2.41E+02 2.25E+02 1.24E+04 NA 1.84E+02 1.56E+02 1.28E+02 1.69E+02 2.37E+02 2.03E+02 3.21E+02 8.96E+02 NA NA NA 8.43E+02

Cu i/g/q

1.53E+02 4.57E+02 1.70E+02 2.51E+02 1.85E+02 3.12E+02 2.05E+01 NA 2.51E+02 2.22E+02 1.26E+02 3.37E+02 2.19E+02 3.89E+02 2.44E+02 1.35E+02 NA NA NA 2.20E+02 Pb ug/g 7.07E+01 2.09E+02 6.63E+01 1.48E+02 1.08E+02 4.21E+02 6.07E+01 NA 2.69E+02 1.63E+02 2.59E+02 2.44E+02 3.39E+02 2.39E+02 3.74E+02 2.B5E+02 NA NA NA 2.78E+02

//g/g: //g/g centrifuged sludge NA: Not analyzed.

B-8

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Zn ug/g

1.946+02 4.90E+02 1.58E+02 3.93E+02 2.65E+02 7.55E+02 4.52E+01 NA 4.94E+02 3.38E+02 4.30E+02 4.43E+02 7.45E+02 4.30E+02 9.21E+02 6.08E+02 NA NA NA 5.01E+02

Be ug/g 1.83E+01 3.23E+01 2.06E+01 2.40E+01 1.63E+01 1.04E+01 1.47E+00 NA 1.05E+01 2.166+01

< 5.756+00 7.78E+00 1.08E+01 8.276+00

< 9.62E+00 1.03E+01 NA NA NA 1.63E+01

Zr ug/g

1.86E+02 3.25E+02 1.05E+02 2.29E+02 1.09E+02 2.76E+02 2.35E+01 NA 1.30E+02 1.74E+02 7.10E+01 8.24E+01 5.29E+02 2.47E+02 3.57E+02 1.86E+02 NA NA NA 3.94E+02 Se and Sm ug/g

< 5.25E+01 < 1.33E+02 < 1.87E+01 < 5.10E+01 < 2.52E+01 < 9.946+01 < 8.45E+00

NA < 1.30E+02 < 4.11E+0I < 1.15E+02 < 1.31E+02 < 1.06E+02 < 7.62E+01 < 1.92E+02 < 1.17E+02

NA NA NA

< 9.81E+01

Ag ug/g

< 5.25E+00 < 1.33E+01 < 1.87E+00 < 5.10E+00

2.62E+00 < 9.94E+00 < 8.45E-01

NA < 1.30E+01 < 4.11E+00 < 1.15E+01 < 1.31E+01 < 1.06E+01 < 7.62E+00 < 1.92E+01 < 1.17E+01

NA NA NA

< 9.81E+00 TI uq/g

< 1.05E+02 < 2.65E+02 < 3.75E+01 < 1.02E+02 < 5.03E+01 < 1.99E+02 < 1.69E+01

NA < 2.60E+02 < 8.22E+01 < 2.30E+02 < 2.62E+02 < 2.11E+02 < 1.52E+02 < 3.85E+02 < 2.35E+02

NA NA NA

< 1.96E+02

B ug/g

5.63E+01 1.06E+02 7.20E+01 8.04E+01 1.31E+02 9.48E+01 5.28E+01 NA 1.09E+02 6.35E+01

< 5.75E+01 9.38E+01 9.46E+01 5.64E+01 1.04E+02

< 5.86E+01 NA NA NA

< 4.90E+01

TIC ug/q 8.92E+02 7.50E+02 2.62E+03 6.82E+02 9.22E+02 6.406+02 8.45E+02 NA 6.91E+02 6.78E+02 NA 1.17E+03 1.02E+03 9.07E+02 1.64E+03 1.386+03 8.57E+02 NA NA 2.19E+03

Ba ug/g

6.95E+01 < 6.63E+01

3.68E+01 7.49E+01 6.12E+01 6.85E+01 1.91E+02 NA

< 6.50E+01 6.27E+01 1.81E+02

< 6.55E+01 1.11E+02 8.15E+01

< 9.62E+01 4.09E+02 NA NA NA 3.616+02 TOC ug/g 5.62E+02 8.30E+02 5.97E+02 8.47E+02 7.88E+02 1.44E+03 3.35E+03 NA 1.03E+03 6.49E+02 NA 1.23E+03 1.98E+03 1.73E+03 1.95E+03 1.30E+03 7.61E+02 NA NA 1.15E+03

//g/g: //g/g centrifuged sludge NA: Not analyzed.

TIC: Total inorganic carbon. TOC: Total organic carbon.

B-9

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

TC

ug/g

1.63E+03

1.69E+03

1.05E+03

1.64E+03

2.07E+03

2.00E+03

5.45E+03

NA

2.44E+03

1.08E+03

NA

2.69E+03

2.29E+03

2.12E+03

4.06E+03

2.86E+03

1.69E+03

NA

NA

3.26E+03

DSC-222S

Joules/g ♦

NA

NA

0.0

0.0

0.0

0.0

61.8

NA

0.0

0.0

NA

NA

0.0

0.0

0.0

0.0

NA

NA

NA

NA

cr //g/g

< 1.87E+00

NA

< 7.41E-01

< 7.07E-01

< 8.07E-01

< 3.36E-01

< 5.78E-01

NA

< 5.91E-01

< 7.79E-01

NA

< 3.866-01

< 5.35E-01

< 7.00E-01

< 6.42E-01

< 6.69E-01

NA

NA

NA

NA

DSC-222S

Jgules/g

NA

NA

0.0

0.0

0.0

0.0

191.0

NA

0.0

0.0

NA

NA

0.0

0.0

0.0

0.0

NA

NA

NA

NA

TGA-222S

Ut Loss (X)

NA

NA

84.1

67.9

75.3

54.8

67.6

NA

43.3

78.7

NA

NA

35.8

37.3

43.3

37.3

NA

NA

NA

NA

DSC-PNNL

Joules/g

0

0

0

0

0

0

8.05

0

0

0

0

0

0

0

0

NA

NA

NA

NA

NA

TGA-222S

Ut Loss (ug/g)

NA

NA

8.41E+05

6.79E+05

7.53E+05

5.48E+05

6.76E+05

NA

4.33E+05

7.87E+05

NA

NA

3.58E+05

3.73E+05

4.33E+05

3.73E+05

NA

NA

NA

NA

OH demand

moles OH/g *

3.22E-04

4.90E-04

2.55E-04

3.08E-04

1.96E-04

2.05E-04

1.66E-04

NA

3.26E-04

2.31E-04

NA

2.39E-04

2.98E-04

1.23E-04

1.46E-04

2.51E-04

NA

NA

NA

NA

TGA-PNNL

Ut Loss (X)

52.2

55.3

75.3

78.6

14.9

37.1

28.4

4.4

7.7

69.5

7.0

6.7

4.7

16.7

24.0

NA

NA

NA

NA

NA

so.'-

ug/tnL $

1.25E+00

3.95E-01

7.716-01

6.42E-01

9.87E+00

5.15E+00

3.25E+00

1.67E+01

1.56E+01

2.03E+00

8.82E+00

2.31E+01

1.02E+01

1.13E+01

2.67E+01

8.85E+01

1.02E+01

1.86E+01

NA

1.03E+02

/ / 9 /g : / /g/9 cen t r i f uged sludge NA: Not analyzed

♦ : Joules/g cen t r i f uged sludge * : moles OH/g cen t r i f uged sludge $: yg ana ly te / ml separated l i q u i d

B-10

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

PO.'-ug/mL $

< 2.966-01 < 2.96E-01 < 2.96E-01 < 2.96E-01 < 3.26E+00 < 3.26E+00 < 3.26E+00 < 3.26E+00 < 3.26E+00 < 1.19E-01 < 3.26E+00 < 6.22E+00 < 3.26E+00 < 1.19E-01 < 3.26E+00 < 3.26E+00 < 3.26E+00 < 3.266+00

NA < 3.266+00

PH pH units 7.95 7.72 7.62 7.54 7.80 7.92 NA NA 7.53 7.52 NA NA 7.63 7.83 7.58 NA NA NA NA NA

NO.-ug/mL $

3.74E-01 3.63E-01

< 4.24E-01 1.97E+00 4.44E+00

< 1.54E+00 4.61E+00

< 1.54E+00 < 1.54E+00

5.52E-01 < 1.54E+00 < 2.94E+00 < 1.54E+00

4.32E-01 < 1.54E+00 < 1.54E+00 < 1.54E+00 < 1.546+00

NA < 1.54E+00

NH. ug/mL $ 8.60E+00

< 1.00E+01 < 5.00E+00 < 5.00E+00 < 5.00E+00 < 5.006+00 < 1.00E+01 < 5.006+01 < 5.00E+00 < 5.00E+00 < 5.00E+00

NA < 5.00E+00 < 5.00E+00 < 5.00E+00 < 5.006+00

NA NA NA NA

NO," ug/mL $

< 1.07E-01 < 1.07E-01 < 1.07E-01 < 1.07E-01 < 1.87E+00 < 1.18E+00 < 1.87E+00 < 1.18E+00 < 1.18E+00 < 1.07E-01 < 1.18E+00 < 2.25E+00 < 1.18E+00 < 1.07E-01 < 1.18E+00 < 1.18E+00 < 1.18E+00 < 1.87E+00

NA < 1.18E+00

Density # g/mL 1.25 1.26 1.13 1.17 1.16 1.40 1.21 3.81 1.57 1.22 0.99 NA 1.69 1.72 1.68 1.82 1.16 1.38 NA 1.81

Ct" ug/mL S

5.41E-01 2.51E-01 2.92E-01

< 5.946-01 9.11E-01

< 1.90E-01 2.26E+00 1.03E+00 9.89E-01 5.15E-01 5.94E-01 4.16E+00 4.89E-01 4.02E-01 5.81E-01 2.30E+00 3.96E-01 7.68E-01 NA 2.24E+00 K

< 2.62E+02 < 6.63E+02 < 9.40E+01 < 2.55E+02 < 1.26E+02 < 4.97E+02

1.01E+03 NA

< 6.50E+02 < 2.06E+02 < 5.75E+02 < 6.55E+02 < 5.28E+02

3.89E+02 < 9.62E+02

1.23E+03 NA NA NA 1.17E+03

f-

< 1.30E-02 < 1.30E-02 < 3.60E-02 < 1.30E-02 < 1.43E-01 < 1.40E-01 < 1.43E-01 < 1.43E-01 < 1.40E-01 < 1.30E-02

2.22E+00 9.30E-01

< 1.43E-01 1.52E-01 1.23E+00

< 1.43E-01 < 1.43E-01 < 1.43E-01

NA 4.07E-01

Residue *

1.72E+04 5.81E+04 9.36E+03 4.29E+04 3.02E+04 5.11E+04 3.70E+05 6.16E+04 8.60E+04 3.296+04 5.61E+04 4.846+04 1.146+05 3.40E+05 7.69E+04 1.11E+05 2.76E+04 3.50E+04 NA 1.98E+05

$: ug analyte / mL separated liquid #: g centrifuged sludge/mL centrifuged sludge

//g/g: //g/g centrifuged sludge *: acid insoluble

B-ll

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

™\l 1

uq/g

< < < < < < < < < < < < < < <

9.596-01

1.956-01

2.106-01

1.99E-01

2.09E-01

2.21E-01

1.17E-02

2.06E+00

1.346-01

2.15E-01

1.24E-01

1.72E-01

5.62E-01

4.67E-01

1.25E-01

NA

NA

NA

NA

NA

" 'U ■

ug/g

6.79E+00

1.176+00

1.336+00

1.386+00

1.41E+00

1.67E+00

9.16E-02

1.71E+01

9.836-01

1.58E+00

8.99E-01

1.186+00

4.01E+00

3.19E+00

1.00E+00

NA

NA

NA

NA

NA

" U ■

ug/g

6.89E+02

1.37E+02

1.48E+02

1.41E+02

1.47E+02

1.57E+02

8.34E+00

1.52E+03

9.40E+01

1.52E+02

8.70E+01

1.21E+02

4.02E+02

3.32E+02

8.81E+01

NA

NA

NA

NA

NA

' "U B

ug/g

7.39E+01

1.50E+01

1.70E+01

1.59E+01

1.63E+01

1.67E+01

9.18E-01

1.04E+02

1.06E+01

1.59E+01

9.57E+00

1.38E+01

4.30E+01

3.55E+01

9.65E+00

NA

NA

NA

NA

NA

"•u ■ ug/g

9.72E+04

1.97E+04

2.12E+04

2.01E+04

2.11E+04

2.246+04

1.196+03

2.086+05

1.366+04

2.186+04

1.266+04

1.756+04

5.70E+04

4.73E+04

1.27E+04

HA

NA

NA

NA

NA

H: based on the total uranium (//g/g centrifuged sludge) by PNNL //9/g: //g/9 centrifuged sludge

B-12

WHC-SP-1182

KE Basin Uater Concentration

M-H20 T-H20

13 20

Ed Bile Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ea Blk Max/Mean

"Co

uCi/mL < 0.452 < 0.540 < 0.536 < 0.540

"'Cs

uCi/mL 38.6

< 2.3 < 1.5

38.6

'"Cs

uCi/mL < 0.656 < 0.584 < 0.584 < 0.656

"*Eu

uCi/mL < 1.334 < 1.880 < 1.794 < 1.880

,!*6u

uCi/mL < 2.040 < 1.660 < 1.362 < 2.040

'"Ce/Pr uCi/mL

< 8.08 < 6.48 < 5.98 < 8.08

'"Eu

uCi/mL < 0.00840 < 0.00877 < 0.00511 < 0.00877

'"Sb

uCi/mL < 0.00585 < 0.00430 < 0.00343 < 0.00585

"GKA" uCi/ml.

< 0.00960 < 0.00914 < 0.00792 < 0.00960

tofSt uCi/mL 0.000029 0.000004 0.000004 0.000013

Total Beta uCi/mL 0.12800 0.11550 0.00239 0.08196 ,M/140pu

uCi/mL < 0.000170 < 0.000193 < 0.000136 < 0.000195

. U-222S phosphorescence ug/mL

11.50 37.10 1.76 16.79

„, U-PNNL fluorescence ug/g

14.97 39.22 0.15 18.11

u7c¥ s

ug/mL 8.71

31.15 < 8.00

19.93

Al

ug/ml < 1.00

1.50 < 1.00

1.50

Ca

ug/mL 18.7 34.6

< 2.0 26.7

Cd ug/mL

< 0.2 < 0.2 < 0.2 < 0.2

Na

ug/mL 3.89 7.03 5.25 5.39

Ag

ug/mL < 0.2 < 0.2 < 0.2 < 0.2

B

ug/mL 1.094 1.239 2.807 1.713

Ba

ug/mL < 1 < 1 < 1 < 1

Be

uq/mL < 0.1 < 0.1 < 0.1 < 0.1

Sm uq/mL

< 2 < 2 < 2 < 2

TIC

ug/mL 10.39 14.60 5.90 10.30

TOC

ug/mL < 40 < 40 < 40 < 40

TC

ug/mL < 40 < 40 < 40 < 40

CN

ug/mL < 0.055 < 0.055 < 0.055 < 0.055

OH demand

moles OH/L < 0.0025 < 0.0025 < 0.0025 < 0.0025

SO/

5.22 27.14

< 1.50 16.18

Eq Blk: Equipment blank Max/Mean: The maximum value is reported if all the data are "less than" values.

The mean value (calculated from the "real" values) is reported if any of the three concentrations is a "real" value.

B-13

WHC-SP-1182

KE Basin Uater Concentration

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Eq Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

M-H20 T-H20

13 20

Ed Blk Max/Mean

"Nb uCi/mL

< 0.554 < 0.456 < 0.462 < 0.554

"*Ru/Rh uCi/mL

< 10.24 < 10.02 < 10.24 < 10.24

"*Ra uCi/mL

< 14.48 < 11.60 < 10.46 < 14.48

'"TI

uCi/mL < 0.0203 < 0.0178 < 0.0174 < 0.0203

'"Bi uCi/mL

< 0.0196 < 0.0226 < 0.0235 < 0.0235

PH pH units

7.68 7.67 7.64 7.66

'"Pu uCi/mL

< 0.000170 < 0.000195 < 0.000136 < 0.000195

"'Np uCi/mL 0.000404 0.000505

< 0.000535 < 0.000454

'"""Cm uCi/mL

< 0.000782 < 0.000567 < 0.000704 < 0.000782

A'ET uCi/mL

< 0.000782 < 0.000567 < 0.000704 < 0.000782

"Sr uCiymL 0.1440 0.0772 0.0011 0.0741

NH, ug/mL

< 5 < 5 < 5 < 5

Cr ug/mL

< 0.200 < 0.297 < 0.200 < 0.297

Cu ug/mL

< 0.2 < 0.2 < 0.2 < 0.2

Fe ug/mL

< 1 < 1 < 1 < 1

Mg

ug/mL < 2 < 2 < 2 < 2

Mn ug/mL

< 0.2 < 0.2 < 0.2 < 0.2

K «g/mL

< 10 < 10 < 10 < 10

Se ug/mL

< 2 < 2 < 2 < 2

TI ug/mL

< 4 < 4 < 4 < 4

Pb ug/mL

< 2 < 2 < 2 < 2

Zr

ug/mL < 0.2 < 0.2 < 0.2 < 0.2

Zn ug/mL 0.487 0.272 0.247 0.336

PO.*-ug/mL

< 3.260 < 0.296 < 3.256 < 3.260

NO, ug/mL 3.990 0.419

< 1.540 2.205

NO," ug/mL

< 1.870 < 0.107 < 1.177 < 1.870

cr ug/mL 0.504 0.727

< 0.187 0.615

F" ug/mL

< 0.143 0.287

< 0.143 0.287

Eq Blk: equipment blank Max/Mean: The maximum value is reported if all the data are "less than" values.

The mean value (calculated from the "real" values) is reported if any of the three concentrations is a "real" value.

B-14

WHC-SP-1182

A P P E N D I X C

THE CHEMISTRY OF AS-SETTLED SLUDGE

T. L. Welsh, D. B. Bechtold, and B. A. Crawford

C-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182 The conversion of centrifuged sludge results to as-settled sludge results utilized the following formulas. The 222-S analytical results (Miller 1996) for sample location 22 are reported as as-settled sludge and do not need to be converted. The PNNL results (Silvers 1995) for locations 19, 20, 21, 22 and 23 have also been reported as as-settled sludge and do not need to be converted. The assumption for converting from a centrifuged basis to an as-settled basis is as follows.

Centrifugation of settled sludge removes <Jg grams of excess water containing uw concentrations of analytes by analysis. The remaining water and solids with their respective analytes stay with the centrifuged sludge.

The following table defines the symbols used in deriving the formula to convert centrifuged-state analyses and water analyses to a settled-state.

Symbol c 9 u 6

P subscript f subscript s subscript u

Meaning gravimetric concentration

mass volumetric concentration

excess density

centrifuged state as-settled state

water state

Units Ug/g or //Ci/g

9 Ug/mL or /vCi/tnL

g/mL

By mass balance:

Sg„ = 3 f (1)

and

cs9a y8g w = c£gf (2)

3f (3)

C-3

WHC-SP-1182 But, by (1) we have

Therefore, by substitution:

(4)

3S P» 9; ( 1 - -^ ) (5)

The average density (pj, as measured by PNNL on the four water samples, is equal to 0.995 g/mL. The values for gf and g are listed in Table 5, columns 3 and 2 respectively, from letter report 75764-PCS95-109. This letter report is also Appendix A in Miller 1996. The values for cf, uu, and the sample location information are listed in Appendix B. The water concentrations (uH) for 60Co, 154Eu, and Eu listed in Appendix B were not used in equation 5. These water concentrations were "less than" values in the same range as the sample results. Instead, data for these isotopes were taken from KE Operations water monitoring sample GEA results. The water monitoring samples are taken weekly and GEA analyses performed. The substitute isotope concentrations were taken from the water monitoring samples which spanned the timeframe of this sludge sampling campaign. The conversion from a centrifuged basis to an as-settled basis for the water soluble analytes uses equation 5, but c, = 0. This assumes that the analytes (sulfate, phosphate, nitrate, nitrite, chloride, fluoride, ammonia, and pH) are soluble and that the analyte does not stay with the sludge. The conversion for the TGA results to as-settled basis uses the ug/g centrifuged result and the fact that uw = pu with the appropriate units. The PNNL uranium isotopic results were reported in atom % (Appendix B). The units for the uranium isotopics were changed to //g/g as-settled sludge using equation 3 of Appendix B, where Cu is the total uranium concentration (C), as measured by PNNL (units of //g/g as-settled sludge), for the sample of interest.

C-4

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

"Co uCi/g

3.42E-01 6.00E-01 4.10E-01 6.14E-01 3.64E-01 4.34E-01 6.99E-02 6.23E-01 1.49E+00 4.30E-01 6.28E-01 9.38E-01 1.04E+00 7.99E-01 2.45E-01 8.90E-01 3.70E-01 3.41E-01 1.46E+00 9.93E-01

"*Ce/Pr uCi/g

< 4.06E+00 < 2.74E+00 < 3.37E+00 < 2.68E+00 < 3.66E+00 < 2.65E+00 < 2.42E-01 < 5.06E+00 < 1.91E+00 < 2.836+00 < 4.256+00 < 4.076-01 < 1.88E+00 < 2.29E+00 < 1.70E+00 < 2.50E+00 < 4.486+00 < 3.076+00 < 3.326+00 < 1.806+00

"'Cs uCi/g

1.126+02 2.776+01 2.626+01 4.49E+01 4.29E+01 2.79E+01 5.45E+01 6.50E+02 2.47E+01 2.87E+01 2.546+01 3.316+01 8.356+01 7.15E+01 5.06E+01 2.966+02 1.626+02 1.64E+02 2.77E+02 3.08E+02

"Nb uCi/g

< 2.66E-01 < 1.90E-01 < 2.34E-01 < 1.88E-01 < 2.50E-01 < 1.83E-01 < 1.02E-02 < 1.97E-01 < 1.33E-01 < 1.96E-01 < 2.92E-01 < 2.71E-02 < 1.11E-01 < 1.466-01 < 1.11E-01 < 1.24E-01 < 2.93E-01 < 1.87E-01 < 1.20E-01 < 9.46E-02

'"Cs uCi/g

< 3.25E-01 < 2.20E-01 < 2.74E-01 < 2.18E-01 < 2.96E-01 < 2.12E-01 < 3.16E-02 < 3.87E-01 < 1.56E-01 < 2.30E-01 < 3.46E-01 < 3.31E-02 < 1.41E-01 < 1.846-01 < 1.38E-01 < 1.96E-01 < 3.82E-01 < 2.34E-01 < 2.586-01 < 1.78E-01

""Ru/Rh uCi/g

< 5.326+00 < 3.52E+00 < 4.316+00 < 3.466+00 < 4.67E+00 < 3.396+00 < 3.53E-01 < 7.376+00 < 2.466+00 < 3.626+00 < 5.416+00 < 5.626-01 < 2.356+00 < 3.086+00 < 2.216+00 < 3.50E+00 < 5.746+00 < 4.126+00 < 4.996+00 < 2.536+00

>"6u uCi/g

2.166+00 6.346-01 6.506-01 1.62E+00 5.77E-01 4.86E-01

< 1.55E-02 3.906+00 2.50E-01 7.56E-01 1.23E-01

< 3.29E-01 1.10E+00 8.92E-01 1.97E-01 5.45E-01 9.64E-01 1.76E+00 1.23E+00 6.41E-01

'"Ra uCl/g

< 7.38E+00 < 4.93E+00 < 6.056+00 < 4.846+00 < 6.576+00 < 4.766+00 < 4.856-01 < 9.656+00 < 3.446+00 < 5.08E+00 < 7.63E+00 < 7.696-01 < 3.296+00 < 4.22E+00 < 3.08E+00 < 4.68E+00 < 8.26E+00 < 5.78E+00 < 6.83E+00 < 3.486+00

'"Eu uCi/o

1.05E+00 2.87E-01 3.18E-01 7.16E-01 2.536-01 2.34E-01

< 4.47E-02 1.80E+00 1.27E-01 3.75E-01 8.20E-02 1.54E-01 6.22E-01 3.47E-01 1.12E-01

< 3.28E-01 3.27E-01 6.B4E-01

< 8.07E-01 < 3.23E-01

"•TI uCi/g

< 1.10E+00 < 1.75E-01 < 1.22E-01 < 2.28E-01 < 1.83E-01 < 1.546-01 < 2.59E-01 < 5.21E+00 < 1.46E-01 < 1.43E-01 < 6.79E-02 < 2.17E-01 < 7.12E-01 < 8.72E-01 < 2.61E-01 < 1.67E+00 < 7.85E-01 < 1.48E+00 < 4.43E+00 < 1.41E+00

//Ci/g: //Ci/g as-settled sludge

C-5

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

"*Bi uCi/g

< 4.11E-01 < 1.016-01 < 7.63E-02 < 1.36E-01 < 9.41E-02 < 8.31E-02 < 1.10E-01 < 1.56E+00 < 1.04E-01 < 8.24E-02 < 5.42E-02 < 1.08E-01 < 2.72E-01 < 3.42E-01 < 1.16E-01 < 6.75E-01 < 3.40E-01 < 4.90E-01 < 1.44E+00 < 6.57E-01

Total Beta uCi/g 4.86E+02 3.19E+01 3.67E+01 9.82E+01 6.956+01 5.82E+01 1.39E+02 1.366+03 2.976+01 3.94E+01 1.48E+01 7.71E+01 2.58E+02 2.06E+02 1.02E+02 7.85E+02 2.45E+02 5.82E+02 7.71E+02 7.906+02

'"Eu uCi/g

< 6.876-02 < 2.15E-02 < 1.49E-02 < 2.536-02 < 1.66E-02 < 5.42E-02 < 8.26E-02 < 2.12E-01 < 1.926-02 < 3.88E-02 < 1.OOE-02 < 1.76E-02 < 5.316-02 < 6.546-02 < 6.31E-02 < 7.476-02 < 3.236-02 < 8.716-02 < 4.396-01 < 6.506-02

i3B/a«pu

uCi/g 5.476+00 4.016+00 4.616+00 1.026+01 3.746+00 3.96E+00 1.52E-01 1.96E+01 1.746+00 5.266+00 8.836-01 2.396+00 9.666+00 6.586+00 1.456+00 4.42E+00 7.656+00 1.236+01 7.546+00 4.416+00

"=Sb uCi/g

< 3.496-01 < 5.49E-02 < 3.84E-02 < 7.23E-02 < 5.79E-02 < 4.91E-02 < 8.40E-02 < 1.64E+00 < 4.78E-02 < 4.546-02 < 2.166-02 < 7.136-02 < 2.12E-01 < 2.786-01 < 8.356-02 < 5.36E-01 < 2.37E-01 < 4.83E-01 < 1.42E+00 < 4.61E-01

'"Pu uCi/g 7.93E-01

< 1.306+00 8.356-01 1.56E+00 6.07E-01 6.336-01 2.346-02

< 4.78E+00 2.89E-01

< 1.28E+00 < 3.12E-01 < 9.26E-01 < 2.64E+00 < 1.11E+00 < 5.306-01

7.28E-01 < 3.96E+00 < 3.27E+00 < 1.86E+00

7.03E-01

"'Am- GEA uCi/g

1.36E+01 3.76E+00 4.01E+00 9.616+00 3.596+00 3.24E+00 1.50E-01 2.356+01 1.566+00 4.686+00 7.236-01 2.096+00 7.446+00 5.756+00 1.12E+00 3.33E+00 5.706+00 1.14E+01 7.33E+00 3.78E+00 '"Np uCi/g 1.09E-03

< 1.16E-03 1.116-03 9.01E-04

< 7.87E-04 < 8.14E-04 < 8.67E-04 < 3.74E-03 < 9.03E-04

9.71E-04 < 5.15E-04 < 1.43E-03

8.40E-04 1.08E-03 1.30E-03 6.93E-04 1.06E-03 1.38E-03

< 4.86E-03 < 8.67E-04

Aloha Total uCi/g

3.07E+01 5.08E+00 9.90E+00 2.356+01 8.936+00 9.236+00 3.73E-01 4.87E+01 4.26E+00 9.086+00 2.016+00 4.95E+00 1.63E+01 1.35E+01 2.52E+00 9.046+00 1.236+01 2.83E+01 1.766+01 9.23E+00

"""'Cm uCi/g

< 2.15E+00 < 5.046-01 < 1.206+00 < 2.226+00 < 1.49E+00 < 4.24E-01 < 9.44E-02 < 5.63E+00 < 3.B2E-01 < 1.47E+00 < 1.31E-01 < 2.43E-01 < 2.33E+00 < 1.046+00 < 7.98E-01 < 8.536-01 < 1.336+00 < 4.216+00 < 2.97E+00 < 9.186-01

//Ci/g: //Ci/g as-settled sludge

C-6

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18.

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

"'Am - AEA

uCi /g

1.30E+01

3.47E+00

3.93E+00

9.75E+00

3.53E+00

3.00E+00

1.306-01

2.456+01

1.496+00

4.486+00

6.666-01

1.98E+00

7.26E+00

5.38E+00

1.31E+00

3.476+00

5.576+00

1.10E+01

6.45E+00

3.61E+00

' " U B

ug/g

< 5.85E-01

< 1.32E-01

< 1.25E-01

< 1.376-01

< 1.186-01

< 1.526-01

< 1.166-02

< 1.83E+00

< 1.04E-01

< 1.43E-01

< 6.OOE-02

< 1.67E-01

< 4.796-01

< 3.756-01

< 1.02E-01

< 3.726-01

< 2.256-01

< 6.716-01

< 1.856-01

< 8.52E-02

" S r

uCi /g

2.236+02

1.036+01

1.066+01

4.856+01

1.936+01

1.856+01

3.656+01

6.056+02

3.426+00

1.226+01

1.266+00

2.156+01

1.066+02

6.406+01

3.076+01

2.226+02

5.966+01

2.04E+02

2.32E+02

1.676+02

' "U a

ug/g

4.146+00

7.976-01

7.916-01

9.526-01

8.026-01

1.156+00

9.116-02

1.536+01

7.666-01

1.05E+00

4.346-01

1.146+00

3.416+00

2.566+00

8.176-01

2.85E+00

1.90E+00

4.75E+00

1.44E+00

6.206-01

. U-222S Phosphorescence

ug/g

NA

NA

4.08E+03

NA

4.94E+03

6.72E+03

1.08E+03

NA

8.49E+03

1.89E+04

NA

NA

2.38E+04

2.396+04

8.986+03

1.436+04

NA

NA

NA

NA

™U ■

ug/g

4.20E+02

9.28E+01

8.82E+01

9.76E+01

8.36E+01

1.08E+02

8.296+00

1.366+03

7.326+01

1.016+02

4.206+01

1.186+02

3.426+02

2.676+02

7.19E+01

2.64E+02

1.56E+02

4.70E+02

1.31E+02

6.076+01

. , U-PNNL f luorescence

ug/g

5.98E+04

1.35E+04

1.286+04

1.406+04

1.21E+04

1.55E+04

1.19E+03

1.87E+05

1.076+04

1.466+04

6.136+03

1.716+04

4.896+04

3.836+04

1.046+04

3.806+04

2.306+04

6.866+04

1.896+04

8.706+03

"*U ■

ug/g

4.506+01

1.026+01

1.016+01

1.106+01

9.23E+00

1.156+01

9.136-01

9.296+01

8.256+00

1.066+01

4.626+00

1.346+01

3.666+01

2.856+01

7.886+00

2.976+01

1.81E+01

5.37E+01

1.426+01

6.47E+00

uw

ug/g

7.98E+04

1.61E+04

1.09E+04

2.536+04

1.426+04

1.72E+04

9.40E+02

NA

9.76E+03

1.48E+04

6.32E+03

1.83E+04

5.66E+04

3.87E+04

8.84E+03

2.86E+04

NA

NA

4.56E+04

3.22E+04

™U ■

ug/g

5.93E+04

1.34E+04

1.276+04

1.396+04

1.206+04

1.546+04

1.186+03

1.86E+05

1.06E+04

1.45E+04

6.09E+03

1.69E+04

4.85E+04

3.80E+04

1.04E+04

3.77E+04

2.28E+04

6.80E+04

1.88E+04

8.63E+03

/ / C i / g : / /C i /g a s - s e t t l e d sludge / / g / g : / /g/g a s - s e t t l e d sludge

NA: Not analyzed. ■: based on the t o t a l uranium (//g/g a s - s e t t l e d sludge) by PNNL

C-7

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Al ug/g

1.18E+04 2.02E+04 1.01E+04 1.63E+04 1.26E+04 9.11E+03 7.06E+03 NA 1.87E+04 1.18E+04 1.15E+04 3.286+04 1.636+04 1.606+04 1.176+04 2.656+04 NA NA 3.676+04 2.935+04

Fe ug/g 1.496+04 8.22E+04 1.23E+04 4.48E+04 2.02E+04 1.096+05 5.726+03 NA 1.696+05 4.006+04 7.286+04 2.106+05 1.756+05 8.796+04 1.986+05 1.386+05 NA NA 3.26E+05 1.33E+05

Ca ug/g

4.79E+02 6.76E+02 3.47E+02 1.42E+03 3.48E+03 1.94E+03 4.61E+03 NA 5.21E+02 1.10E+03 1.91E+02 9.176+02 2.56E+03 2.716+03 6.71E+03 7.71E+03 NA NA 2.07E+04 1.43E+04

Mg ug/g 1.20E+02 4.48E+02 1.23E+02 5.16E+02 6.05E+02 6.96E+02 8.51E+02 NA 6.04E+02 2.79E+02 2.536+02 4.10E+02 6.35E+02 7.50E+02 9.306+02 1.286+03 NA NA 3.01E+03 1.50E+03

Cd ug/g

2.51E+01 3.74E+01 2.67E+01 4.38E+01 2.99E+01 4.35E+01 2.23E+01 NA 3.41E+01 4.11E+01 1.36E+01 4.42E+01 2.96E+01 3.35E+01 1.75E+01 2.34E+01 NA NA 4.77E+01 2.47E+01

Mn ug/g 5.52E+01 1.46E+02 5.91E+01 1.31E+02 8.87E+01 2.06E+02 7.84E+01 NA 2.01E+02 1.22E+02 1.18E+02 3.47E+02 2.51E+02 1.81E+02 2.57E+02 2.36E+02 NA NA 6.15E+02 4.08E+02

Cr ug/g

5.09E+01 2.33E+02 3.996+01 1.22E+02 5.916+01 3.896+02 3.546+01 NA 3.376+02 1.13E+02 1.48E+02 2.83E+02 6.216+02 3.056+02 6.81E+02 4.39E+02 NA NA 1.19E+03 6.006+02

Na ug/g 1.296+02 2.16E+02 9.33E+01 1.26E+02 1.39E+02 1.56E+02 1.23E+04 NA 1.44E+02 1.06E+02 6.45E+01 1.64E+02 2.03E+02 1.64E+02 2.63E+02 7.686+02 NA NA 1.80E+03 7.666+02

Cu ug/g

9.346+01 3.106+02 1.016+02 1.736+02 1.056+02 2.156+02 2.046+01 NA 1.956+02 1.486+02 6.09E+01 3.27E+02 1.866+02 3.136+02 1.996+02 1.166+02 HA HA 5.92E+02 2.006+02

Pb ug/g 4.396+01 1.436+02 4.036+01 1.03E+02 6.21E+01 2.90E+02 6.04E+01 NA 2.10E+02 1.09E+02 1.26E+02 2.366+02 2.896+02 1.926+02 3.056+02 2.446+02 NA NA 6.726+02 2.536+02

ug/g: ug/g as-settled sludge NA: Not analyzed.

C-8

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Zn ug/g

1.186+02 3.336+02 9.416+01 2.726+02 1.516+02 5.206+02 4.506+01 NA 3.846+02 2.256+02 2.086+02 4.296+02 6.346+02 3.466+02 7.516+02 5.216+02 NA NA 1.316+03 4.55E+02

Be ug/g 1.12E+01 2.20E+01 1.236+01 1.666+01 9.286+00 7.226+00 1.466+00 NA 8.176+00 1.44E+01

< 2.82E+00 7.55E+00 9.22E+00 6.66E+00

< 7.876+00 8.84E+00 NA NA 1.35E+01 1.48E+01

Zr ug/g

1.13E+02 2.216+02 6.276+01 1.586+02 6.216+01 1.906+02 2.336+01 NA 1.016+02 1.166+02 3.436+01 7.996+01 4.506+02 1.996+02 2.91E+02 1.59E+02 NA NA 6.60E+0Z 3.58E+02

Sm ug/g

< 3.28E+01 < 9.10E+01 < 1.206+01 < 3.59E+01 < 1.51E+01 < 6.91E+01 < 8.41E+00

NA < 1.02E+02 < 2.80E+01 < 5.65E+01 < 1.27E+02 < 9.01E+01 < 6.16E+01 < 1.57E+02 < 1.01E+02

NA NA

< 2.36E+02 < 8.93E+01

Ag ug/g

< 3.28E+00 < 9.10E+00 < 1.206+00 < 3.596+00

1.576+00 < 6.916+00 < 8.416-01

NA < 1.026+01 < 2.806+00 < 5.65E+00 < 1.27E+01 < 9.01E+00 < 6.16E+00 < 1.57E+01 < 1.016+01

HA HA

< 2.366+01 < 8.936+00

TI ug/g

< 6.56E+01 < 1.81E+02 < 2.40E+01 < 7.186+01 < 3.03E+01 < 1.38E+02 < 1.68E+01

HA < 2.03E+02 < 5.61E+01 < 1.13E+02 < 2.54E+02 < 1.80E+02 < 1.23E+02 < 3.15E+02 < 2.02E+02

NA NA

< 4.72E+02 < 1.79E+02

B ug/g

3.50E+01 7.25E+01 4.36E+01 5.61E+01 7.486+01 6.586+01 5.25E+01 NA 8.52E+01 4.28E+01

< 2.86E+01 9.10E+01 8.07E+01 4.56E+01 8.48E+01

< 5.05E+01 NA HA 4.79E+02

< 4.47E+01

TIC ug/g 5.48E+02 5.12E+02 1.57E+03 4.75E+02 5.27E+02 4.44E+02 8.40E+02 NA 5.40E+02 4.55E+02 5.36E+00 1.14E+03 8.72E+02 7.31E+02 1.34E+03 1.18E+03 4.S1E+02 NA NA 1.996+03

Ba ug/g

4.286+01 < 4.536+01

2.236+01 5.216+01 3.516+01 4.746+01 1.906+02 NA

< 5.086+01 4.206+01 8.786+01

< 6.366+01 9.506+01 6.576+01

< 7.876+01 3.506+02 NA NA 3.526+02 3.286+02

TOC ug/g 3.586+02 5.766+02 3.726+02 5.986+02 4.646+02 1.006+03 3.336+03 NA 8.096+02 4.456+02

1.196+03 1.696+03 1.406+03 1.60E+03 1.12E+03 4.15E+02 NA NA 1.05E+03

/ / g / g : / /g/g a s - s e t t l e d sludge NA: Not analyzed.

TIC: Tota l inorgan ic carbon. TOC: Tota l organic carbon.

C-9

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location

1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

«g/s NA 1

TC ug/g

1.016+03 1.166+03 6.426+02 1.146+03 1.196+03 1.396+03 5.42E+03 NA 1.90E+03 7.29E+02 NA 2.61E+03 1.95E+03 1.71E+03 3.326+03 2.456+03 8.966+02 NA NA 2.96E+03

DSC-222S Jqules/g dry ut HA NA 0.0 0.0 0.0 0.0

189.9 NA 0.0 0.0

NA HA 0.0 0.0 0.0 0.0

HA NA NA NA

: Total carbon. : ug/9 as-settled s : Joules/g as-sett : Not analyzed. : moles OH/g as-se : soluble

CN ug/g

< 1.166+00 NA

< 4.646-01 < 5.066-01 < 4.816-01 < 2.496-01 < 5.756-01

HA < 4.726-01 < 5.376-01

NA < 3.766-01 < 4.64E-01 < 5.73E-01 < 5.34E-01 < 5.81E-01

HA HA NA NA DSC-PNNL Joules/g net ut 0.0 0.0 0.0 0.0 0.0 0.0 8.00 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 NA NA NA NA

ludge led sludge tied sludge

TGA-222S Wt Loss (ug/g)

NA NA 9.05E+05 7.78E+05 8.60E+05 6.89E+05 6.78E+05 NA 5.59E+05 8.58E+05 NA NA 4.546+05 4.966+05 5.376+05 4.63E+05 NA NA NA NA OH demand

moles OH/g *

1.97E-04 3.34E-04 1.53E-04 2.14E-04 1.12E-04 1.42E-04 1.65E-04 HA 2.54E-04 1.54E-04 NA 2.32E-04 2.54E-04 9.93E-05 1.20E-04 2.156-04 NA NA NA NA

TGA-PNNL Ut Loss (ug/g)

7.096+05 6.966+05 8.536+05 8.52E+05 5.17E+05 5.676+05 2.88E+05 1.47E+05 2.82E+05 7.97E+05 5.52E+05 9.51E+04 1.89E+05 3.31E+05 3.80E+05 3.28E+05 NA NA NA NA so.'- $ «9/9

4.91E-01 1.27E-01 3.13E-01 1.99E-01 4.30E+00 1.61E+00 2.02E-02 1.81E+00 3.48E+00 6.83E-01 4.59E+00 7.006-01 1.536+00 2.236+00 4.936+00 1.286+01 4.916+00 4.51E+00 NA 9.45E+00

DSC-222S Joules/g ♦ uet ut

NA NA 0.0 0.0 0.0 0.0

61.4 NA 0.0 0.0

HA NA 0.0 0.0 0.0 0.0

NA NA NA NA po.'- $ ug/g

< < < < < < < < < < < < < < < < < <

1.166-01 9.556-02 1.206-01 9.196-02 1.426+00 1.02E+00 2.036-02 3.526-01 7.276-01 4.006-02 1.706+00 1.88E-01 4.88E-01 2.35E-02 6.03E-01 4.70E-01 1.57E+00 7.91E-01 NA

< 2.98E-01

C-10

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

NO," $ ug/g

1.47E-01 1.17E-01

< 1.72E-01 6.10E-01 1.93E+00

< 4.82E-01 2.86E-02

< 1.66E-01 < 3.43E-01

1.86E-01 < 8.02E-01 < 8.91E-02 < 2.31E-01

8.53E-02 < 2.85E-01 < 2.22E-01 < 7.436-01 < 3.746-01

NA < 1.416-01

Density g/mL # 1.15 1.20 1.04 1.15 1.11 1.25 1.21 2.28 1.35 1.14 1.40 1.3 & 1.54 1.51 1.50 1.59 1.11 1.75 1.6 8, 1.64

NO," $ ug/g

< 4.206-02 < 3.456-02 < 4.356-02 < 3.326-02 < 8.146-01 < 3.706-01 < 1.166-02 < 1.286-01 < 2.63E-01 < 3.60E-02 < 6.14E-01 < 6.82E-02 < 1.77E-01 < 2.12E-02 < 2.18E-01 < 1.70E-01 < 5.696-01 < 4.546-01

NA < 1.086-01

Se uq/q

< 3.286+01 < 9.106+01 < 1.206+01 < 3.596+01 < 1.516+01 < 6.916+01 < 8.416+00

NA < 1.02E+02 < 2.80E+01 < 5.65E+01 < 1.27E+02 < 9.01E+01 < 6.16E+01 < 1.576+02 < 1.016+02

NA HA

< 2.36E+02 < 8.93E+01

CI' $ ug/g

2.12E-01 8.10E-02 1.19E-01

< 1.84E-01 3.96E-01

< 5.95E-02 1.406-02 1.11E-01 2.20E-01 1.73E-01 3.09E-01 1.26E-01 7.32E-02 7.956-02 1.07E-01 3.32E-01 1.91E-01 1.86E-01 NA Z.05E-01

K ug/g

< 1.64E+02 < 4.53E+02 < 6.01E+01 < 1.79E+02 < 7.58E+01 < 3.45E+02

1.00E+03 NA

< 5.08E+02 < 1.40E+02 < 2.82E+02 < 6.36E+02 < 4.516+02

3.14E+02 < 7.87E+02

1.066+03 NA HA 1.59E+03 1.066+03

F- $ ug/g

< 5.106-03 < 4.206-03 < 1.466-02 < 4.03E-03 < 6.23E-02 < 4.38E-02 < 8.896-04 < 1.556-02 < 3.12E-02 < 4.37E-03

1.16E+00 2.82E-02

< 2.14E-02 2.99E-02 2.27E-01

< 2.06E-02 < 6.90E-02 < 3.476-02

HA 3.73E-02

Residue * ug/g 1.05E+04 3.94E+04 5.58E+03 2.96E+04 1.71E+04 3.52E+04 3.68E+05 5.50E+04 6.69E+04 2.196+04 2.71E+04 4.69E+04 9.67E+04 2.73E+05 6.28E+04 9.516+04 1.43E+04 2.66E+04 1.79E+05 1.80E+05

NH, S ug/g

3.38E+00 < 3.23E+00 < 2.03E+00 < 1.556+00 < 2.186+00 < 1.576+00 < 6.226-02 < 5.416+00 < 1.11E+00 < 1.68E+00 < 2.60E+00

HA < 7.49E-01 < 9.88E-01 < 9.256-01 < 7.206-01

NA NA NA NA

/ / g / g : / /g/9 a s - s e t t l e d sludge $ : so lub le

NA: Not analyzed. # : g a s - s e t t l e d sludge/mL a s - s e t t l e d sludge &: est imated * : ac id i nso lub le

c-n

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182 The conversion of //Ci/g as-settled sludge or //g/g as-settled sludge utilized the as-settled density (g as-settled sludge/mL as-settled sludge) measured for each of the samples. The as-settled density measurements (obtained using the 60-mL centrifuge cones) are listed in letter report 75764-PCS95-109 (Table 5, column 7), which is also Appendix A in Miller 1996. The as-settled density for location 22 (T-20 top) was not measured using the graduated settler or the 60-mL centrifuge cone. The as-settled density for location 15 (1-15) obtained using the graduated settlers is suspected to be erroneous and the information from the 60-mL centrifuge cone was not recorded.

In order to estimate the missing density values for locations 15 and 22, sample correlation coefficients were computed for all pairs of analytes. The correlation coefficient is a number whose purpose is to measure the strength of association between two variables. As-settled density had the "best" correlation coefficients with Total Beta, 137Cs, 90Sr, uranium (fluorescence), and chromium. A regression equation, of the form density = a + bX, was computed for each of the "best" variables (X). The predicted values for both locations 15 and 22 are listed in the following table. The estimated as-settled density values used for locations 15 (1-15) and 22 (T-20 top) are 1.3 and 1.6 respectively.

Analyte

Beta Total 137Cs 90Sr U (fluorescence) Cr

Mean

Location 15 (1-15) Predicted Density

1.23 1.24 1.25 1.30 1.32

1.3

Location 22 (T-20 top) Predicted Density

1.71 1.63 1.60 1.31

outside range of regression

1.6

The PNNL uranium isotopic results were reported in atom % (Appendix B). The units for the uranium isotopics were changed to //g/mL as-settled sludge using equation 3 of Appendix B, where Cu is the total uranium concentration (C), as measured by PNNL (units of //g/mL as-settled sludge), for the sample of interest.

C-13

WHC-SP-1182

This page intentionally l e f t blank.

C-14

WHC-SP-1182

Locat i on 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

"Co uCi/mL

3.936-01 7.206-01 4.27E-01 7.06E-01 4.046-01 5.426-01 8.466-02 1.426+00 2.016+00 4.906-01 8.796-01 1.226+00 1.606+00 1.216+00 3.676-01 1.416+00 4.106-01 5.976-01 2.346+00 1.636+00

'"Ce/Pr uCi/mL

< 4.676+00 < 3.296+00 < 3.516+00 < 3.096+00 < 4.066+00 < 3.31E+00 < 2.93E-01 < 1.15E+01 < 2.57E+00 < 3.22E+00 < 5.95E+00 < 5.29E-01 < 2.90E+00 < 3.45E+00 < 2.55E+00 < 3.98E+00 < 4.97E+00 < 5.37E+00 < 5.31E+00 < 2.95E+00

"'Cs uCi/mL

1.29E+02 3.32E+01 2.73E+01 5.17E+01 4.76E+01 3.49E+01 6.59E+01 1.48E+03 3.34E+01 3.27E+01 3.56E+01 4.30E+01 1.29E+02 1.08E+02 7.59E+01 4.71E+02 1.80E+02 2.87E+02 4.44E+02 5.04E+02

"Nb uCi/mL

< 3.06E-01 < 2.28E-01 < 2.43E-01 < 2.166-01 < 2.786-01 < 2.286-01 < 1.236-02 < 4.506-01 < 1.806-01 < 2.246-01 < 4.096-01 < 3.526-02 < 1.706-01 < 2.21E-01 < 1.666-01 < 1.986-01 < 3.256-01 < 3.276-01 < 1.92E-01 < 1.55E-01

'"Cs uCi/mL

< 3.73E-01 < 2.64E-01 < 2.85E-01 < 2.51E-01 < 3.29E-01 < 2.65E-01 < 3.83E-02 < 8.83E-01 < 2.10E-01 < 2.62E-01 < 4.84E-01 < 4.30E-02 < 2.17E-01 < 2.78E-01 < 2.07E-01 < 3.116-01 < 4.246-01 < 4.106-01 < 4.13E-01 < 2.92E-01

'°*Ru/Rh uCi/mL

< 6.12E+00 < 4.22E+00 < 4.48E+00 < 3.98E+00 < 5.19E+00 < 4.24E+00 < 4.276-01 < 1.686+01 < 3.326+00 < 4.126+00 < 7.576+00 < 7.306-01 < 3.626+00 < 4.65E+00 < 3.31E+00 < 5.57E+00 < 6.37E+00 < 7.20E+00 < 7.98E+00 < 4.16E+00

"*Eu uCi/mL

2.486+00 7.61E-01 6.76E-01 1.86E+00 6.41E-01 6.07E-01

< 1.87E-02 8.90E+00 3.37E-01 8.62E-01 1.73E-01

< 4.27E-01 1.69E+00 1.35E+00 2.95E-01 8.67E-01 1.07E+00 3.07E+00 1.98E+00 1.05E+00

"sRa uCi/mL

< 8.48E+00 < 5.92E+00 < 6.30E+00 < 5.56E+00 < 7.30E+00 < 5.95E+00 < 5.86E-01 < 2.20E+01 < 4.65E+00 < 5.796+00 < 1.076+01 < 1.00E+00 < 5.076+00 < 6.386+00 < 4.616+00 < 7.456+00 < 9.176+00 < 1.016+01 < 1.096+01 < 5.716+00

'"6u uCi/mL

1.216+00 3.446-01 3.316-01 8.246-01 2.816-01 2.936-01

< 5.415-02 4.10E+00 1.71E-01 4.27E-01 1.15E-01 2.00E-01 9.57E-01 5.246-01 1.685-01

< 5.226-01 3.645-01 1.205+00

< 1.296+00 < 5.306-01

""TI uCi/mL

< 1.265+00 < 2.106-01 < 1.276-01 < 2.626-01 < 2.045-01 < 1.936-01 < 3.136-01 < 1.196+01 < 1.975-01 < 1.636-01 < 9.516-02 < 2.826-01 < 1.106+00 < 1.326+00 < 3.916-01 < 2.666+00 < 8.716-01 < 2.606+00 < 7.096+00 < 2.316+00

//Ci/mL: //Ci/mL as-settled sludge

C-15

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

"°Bi

uCi/mL

< 4.735-01

< 1.216-01

< 7.946-02

< 1.566-01

< 1.046-01

< 1.046-01

< 1.346-01

< 3.555+00

< 1.415-01

< 9.406-02

< 7.596-02

< 1.416-01

< 4.186-01

< 5.176-01

< 1.746-01

< 1.076+00

< 3.776-01

< 8.576-01

< 2.306+00

< 1.086+00

Tota l Beta

uCi/mL

5.595+02

3.82E+01

3.826+01

1.136+02

7.716+01

7.286+01

1.685+02

3.096+03

4.016+01

4.496+01

2.076+01

1.005+02

3.976+02

3.116+02

1.546+02

1.256+03

2.726+02

1.025+03

1.236+03

1.306+03

' " 6 u

uCi/mL

< 7.906-02

< 2.586-02

< 1.556-02

< 2.916-02

< 1.856-02

< 6.786-02

< 1.005-01

< 4.846-01

< 2.596-02

< 4.436-02

< 1.406-02

< 2.295-02

< 8.18E-02

< 9.88E-02

< 9.46E-02

< 1.19E-01

< 3.58E-02

< 1.52E-01

< 7.02E-01

< 1.07E-01 aM/a«opu

uCi/mL

6.29E+00

4.816+00

4.796+00

1.18E+01

4.16E+00

4.95E+00

1.846-01

4.486+01

2.356+00

5.99E+00

1.246+00

3.106+00

1.496+01

9.946+00

2.175+00

7.046+00

8.496+00

2.146+01

1.216+01

7.236+00

"»Sb

uCi/mL

< 4.016-01

< 6.596-02

< 3.996-02

< 8.326-02

< 6.435-02

< 6.136-02

< 1.026-01

< 3.756+00

< 6.465-02

< 5.18E-02

< 3.026-02

< 9.266-02

< 3.265-01

< 4.196-01

< 1.256-01

< 8.536-01

< 2.646-01

< 8.466-01

< 2.275+00

< 7.575-01

' "Pu

uCi/mL

9.116-01

< 1.566+00

8.685-01

1.796+00

6.736-01

7.916-01

2.836-02

< 1.096+01

3.906-01

< 1.466+00

< 4.376-01

< 1.206+00

< 4.066+00

< 1.676+00

< 7.965-01

1.166+00

< 4.39E+00

< 5.72E+00

< 2.98E+00

1.15E+00

"'Am - GEA

uCi/mL

1.56E+01

4.51E+00

4.17E+00

1.11E+01

3.98E+00

4.05E+00

1.82E-01

5.355+01

2.105+00

5.346+00

1.016+00

2.716+00

1.145+01

8.696+00

1.686+00

5.296+00

6.336+00

1.996+01

1.17E+01

6.20E+00

" 'Hp

uCi/mL

1.25E-03

< 1.39E-03

1.15E-03

1.04E-03

< 8.745-04

< 1.025-03

< 1.056-03

< 8.546-03

< 1.225-03

1.115-03

< 7.216-04

< 1.866-03

1.29E-03

1.63E-03

1.956-03

1.106-03

1.186-03

2.416-03

< 7.786-03

< 1.426-03

Alpha Tota l

uCi/mL

3.535+01

6.096+00

1.036+01

2.706+01

9.916+00

1.155+01

4.526-01

1.116+02

5.766+00

1.046+01

2.826+00

6.436+00

2.516+01

2.046+01

3.785+00

1.445+01

1.376+01

4.956+01

2.816+01

1.516+01

" " " ' C m

uCi/mL

< 2.47E+00

< 6.055-01

< 1.256+00

< 2.556+00

< 1.656+00

< 5.306-01

< 1.146-01

< 1.286+01

< 5.166-01

< 1.686+00

< 1.835-01

< 3.166-01

< 3.596+00

< 1.575+00

< 1.206+00

< 1.366+00

< 1.475+00

< 7.375+00

< 4.755+00

< 1.516+00

//Ci/mL: //Ci/mL a s - s e t t l e d sludge

C-16

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

"'Am - A6A

uCi/mL

1.506+01

4.165+00

4.096+00

1.125+01

3.926+00

3.756+00

1.575-01

5.605+01

2.026+00

5.105+00

9.326-01

2.575+00

1.126+01

8.136+00

1.976+00

5.516+00

6.186+00

1.935+01

1.035+01

5.935+00

™U ■

ug/mL

< 6.736-01

< 1.596-01

< 1.306-01

< 1.586-01

< 1.316-01

< 1.905-01

< 1.416-02

< 4.186+00

< 1.416-01

< 1.635-01

< 8.416-02

< 2.176-01

< 7.375-01

< 5.675-01

< 1.536-01

< 5.916-01

< 2.496-01

< 1.176+00

< 2.966-01

< 1.406-01

~Sr

uCi/mL

2.565+02

1.235+01

1.105+01

5.585+01

2.156+01

2.316+01

4.416+01

1.386+03

4.615+00

1.395+01

1.77E+00

2.806+01

1.636+02

9.676+01

4.616+01

3.536+02

6.616+01

3.576+02

3.706+02

2.745+02

' "U B

ug/mL

4.766+00

9.575-01

8.226-01

1.106+00

8.906-01

1.446+00

1.106-01

3.496+01

1.036+00

1.206+00

6.086-01

1.486+00

5.266+00

3.876+00

1.236+00

4.546+00

2.106+00

8.325+00

2.305+00

1.025+00

^. I "2 2

" phosphorescence

ug/mL

NA

NA

4.256+03

NA

5.486+03

8.406+03

1.316+03

NA

1.155+04

2.166+04

HA

HA

3.676+04

3.605+04

1.356+04

2.276+04

NA

NA

NA

NA

' "U ■

ug/mL

4.836+02

1.116+02

9.186+01

1.126+02

9.285+01

1.356+02

1.006+01

3.106+03

9.886+01

1.166+02

5.886+01

1.536+02

5.276+02

4.035+02

1.086+02

4.196+02

1.746+02

8.235+02

2.096+02

9.956+01

. , U-PNNL f luorescence

ug/mL

6.876+04

1.626+04

1.336+04

1.616+04

1.346+04

1.946+04

1.446+03

4.276+05

1.446+04

1.676+04

8.596+03

2.22E+04

7.536+04

5.796+04

1.576+04

6.036+04

2.556+04

1.206+05

3.026+04

1.436+04

"*U B

ug/mL

5.185+01

1.226+01

1.056+01

1.266+01

1.026+01

1.436+01

1.106+00

2.126+02

1.116+01

1.216+01

6.476+00

1.746+01

5.645+01

4.306+01

1.186+01

4.736+01

2.016+01

9.40E+01

2.286+01

1.06E+01

uw

s

ug/mL

9.186+04

1.936+04

1.146+04

2.915+04

1.586+04

2.15E+04

1.146+03

NA

1.326+04

1.696+04

8.856+03

2.386+04

8.716+04

5.846+04

1.336+04

4.54E+04

NA

NA

7.306+04

5.296+04

™U B

ug/mL

6.826+04

1.616+04

1.325+04

1.606+04

1.336+04

1.935+04

1.436+03

4.246+05

1.435+04

1.666+04

8.526+03

2.205+04

7.476+04

5.746+04

1.566+04

5.996+04

2.536+04

1.19E+05

3.005+04

1.426+04

//Ci/mL: //Ci/mL a s - s e t t l e d sludge //g/mL: //g/mL a s - s e t t l e d sludge

NA: Not analyzed B: based on the t o t a l uranium (//g/mL a s - s e t t l e d sludge) by PNNL

C-17

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Al ug/mL

1.366+04 2.436+04 1.056+04 1.876+04 1.406+04 1.146+04 8.546+03 NA 2.525+04 1.35E+04 1.61E+04 4.26E+04 2.516+04 2.426+04 1.766+04 4.216+04 NA NA 5.876+04 4.806+04

Fe ug/mL 1.716+04 9.866+04 1.285+04 5.156+04 2.246+04 1.376+05 6.926+03 NA 2.296+05 4.57E+04 1.02E+05 2.735+05 2.70E+05 1.33E+05 2.97E+05 2.19E+05 NA NA 5.22E+05 2.18E+05

Ca ug/mL

5.51E+02 8.11E+02 3.61E+02 1.63E+03 3.865+03 2.43E+03 5.586+03 NA 7.036+02 1.256+03 2.686+02 1.196+03 3.956+03 4.095+03 1.015+04 1.236+04 NA NA 3.316+04 2.356+04

Mg ug/mL 1.386+02 5.386+02 1.286+02 5.946+02 6.726+02 8.706+02 1.035+03 NA 8.166+02 3.186+02 3.556+02 5.336+02 9.776+02 1.135+03 1.406+03 2.046+03 NA HA 4.826+03 2.465+03

Cd ug/mL

2.886+01 4.496+01 2.776+01 5.046+01 3.326+01 5.436+01 2.705+01 NA 4.616+01 4.685+01 1.906+01 5.756+01 4.556+01 5.066+01 2.626+01 3.736+01 NA NA 7.646+01 4.06E+01

Mn ug/mL 6.35E+01 1.75E+02 6.14E+01 1.51E+02 9.85E+01 2.57E+02 9.49E+01 NA 2.72E+02 1.406+02 1.66E+02 4.51E+02 3.86E+02 2.74E+02 3.85E+02 3.76E+02 NA NA 9.84E+02 6.68E+02

Cr ug/mL

5.856+01 2.805+02 4.156+01 1.405+02 6.566+01 4.865+02 4.296+01 HA 4.556+02 1.285+02 2.076+02 3.685+02 9.57E+02 4.606+02 1.026+03 6.996+02 HA HA 1.916+03 9.846+02 Ha ug/mL 1.486+02 2.596+02 9.706+01 1.456+02 1.545+02 1.966+02 1.496+04 HA 1.946+02 1.206+02 9.036+01 2.136+02 3.126+02 2.486+02 3.946+02 1.225+03 NA NA 2.885+03 1.266+03

Cu ug/mL

1.075+02 3.726+02 1.055+02 1.996+02 1.166+02 2.696+02 2.465+01 NA 2.636+02 1.696+02 8.525+01 4.256+02 2.875+02 4.726+02 2.996+02 1.846+02 NA NA 9.476+02 3.286+02

Pb ug/mL 5.055+01 1.715+02 4.206+01 1.186+02 6.89E+01 3.63E+02 7.31E+01 NA 2.83E+02 1.24E+02 1.76E+02 3.07E+02 4.45E+02 2.90E+02 4.58E+02 3.88E+02 NA NA 1.08E+03 4.15E+02

//g/mL: //g/mL a s - s e t t l e d sludge NA: Not analyzed

C-18

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Zn ug/mL

1.36E+02 3.99E+02 9.78E+01 3.12E+02 1.67E+02 6.50E+02 S.44E+01 NA 5.19E+02 2.565+02 2.915+02 5.586+02 9.766+02 5.226+02 1.136+03 8.285+02 NA NA 2.096+03 7.476+02

Be ug/mL 1.296+01 2.646+01 1.286+01 1.916+01 1.036+01 9.026+00 1.766+00 NA 1.106+01 1.646+01

< 3.956+00 9.81E+00 1.426+01 1.016+01

< 1.186+01 1.416*01 NA NA 2.166+01 2.436+01

Zr ug/mL

1.306+02 2.656+02 6.526+01 1.826+02 6.905+01 2.386+02 2.826+01 NA 1.376+02 1.32E+02 4.81E+01 1.04E+02 6.936+02

' 3.005+02 4.375+02 2.536+02 NA NA 1.066+03 5.875+02

Sm ug/mL

< 3.77E+01 < 1.096+02 < 1.256+01 < 4.13E+01 < 1.686+01 < 8.646+01 < 1.026+01

NA < 1.376+02 < 3.206+01 < 7.916+01 < 1.65E+02 < 1.396+02 < 9.306+01 < 2.366+02 < 1.606+02

NA NA

< 3.776+02 < 1.476+02

Ag ug/mL

< 3.776+00 < 1.096+01 < 1.256+00 < 4.136+00

1.746+00 < 8.646+00 < 1.02E+00

NA < 1.375+01 < 3.206+00 < 7.916+00 < 1.65E+01 < 1.396+01 < 9.305+00 < 2.366+01 < 1.606+01

NA HA

< 3.776+01 < 1.476+01

TI ug/mL

< 7.546+01 < 2.176+02 < 2.496+01 < 8.256+01 < 3.366+01 < 1.736+02 < 2.04E+01

HA < 2.746+02 < 6.396+01 < 1.58E+02 < 3.316+02 < 2.786+02 < 1.865+02 < 4.726+02 < 3.206+02

NA NA

< 7.556+02 < 2.936+02

B ug/mL

4.026+01 8.706+01 4.536+01 6.455+01 8.316+01 8.226+01 6.356+01 NA 1.156+02 4.886+01

< 4.016+01 1.186+02 1.24E+02 6.896+01 1.276+02

< 8.036+01 NA NA 7.666+02

< 7.346+01

TIC ug/mL 6.306+02 6.156+02 1.636+03 5.466+02 5.855+02 5.556+02 1.026+03 NA 7.296+02 5.185+02 7.506+00 1.485+03 1.345+03 1.10E+03 2.01E+03 1.88E+03 5.00E+02 HA HA 3.26E+03

Ba ug/mL

4.926+01 < 5.446+01

2.326+01 5.996+01 3.906+01 5.93E+01 2.306+02 HA

< 6.866+01 4.796+01 1.236+02

< 8.276+01 1.46E+02 9.926+01

< 1.186+02 5.57E+02 HA NA 5.646+02 5.386+02

TOC ug/mL 4.126+02 6.916+02 3.876+02 6.87E+02 5.155+02 1.256+03 4.03E+03 NA 1.096+03 5.086+02 NA 1.556+03 2.606+03 2.116+03 2.40E+03 1.785+03 4.616+02 NA NA 1.726+03

//g/mL: //g/mL a s - s e t t l e d sludge NA: Not analyzed

TIC: Tota l inorganic carbon TOC: Tota l organic carbon

C-19

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

TC

ug/mL

1.166+03

1.39E+03

6.686+02

1.316+03

1.326+03

1.735+03

6.55E+03

NA

2.57E+03

8.31E+02

NA

3.396+03

3.006+03

2.586+03

4.986+03

3.906+03

9.946+02

HA

HA

4.865+03

DSC-222S

Joules/mL

HA

HA

0.0

0.0

0.0

0.0

230

HA

0.0

0.0

HA

HA

0.0

0.0

0.0

0.0

NA

NA

NA

NA

CN'

ug/mL

< 1.345+00

NA

< 4.835-01

< 5.825-01

< 5.345-01

< 3.116-01

< 6.956-01

NA

< 6.376-01

< 6.126-01

NA

< 4.896-01

< 7.146-01

< 8.665-01

< 8.016-01

< 9.246-01

NA

NA

NA

NA

DSC-PNNL

Joules/mL

0.0

0.0

0.0

0.0

0.0

0.0

9.68

0.0

0.0

0.0

0.0

0.0

0.0

0.0

0.0

0.0

NA

NA

NA

NA

TGA-222S

ug/mL

NA

NA

9.426+05

8.946+05

9.556+05

8.615+05

8.216+05

NA

7.556+05

9.786+05

NA

HA

6.996+05

7.496+05

8.056+05

7.35E+05

NA

NA

NA

NA

OH demand

moles OH/mL *

2.27E-04

4.00E-04

1.59E-04

2.46E-04

1.246-04

1.776-04

2.00E-04

NA

3.43E-04

1.766-04

NA

3.015-04

3.916-04

1.506-04

1.796-04

3.426-04

NA

NA

NA

NA

TGA-PNNL

ug/mL

8.156+05

8.365+05

8.876+05

9.80E+05

5.746+05

7.086+05

3.486+05

3.356+05

3.806+05

9.096+05

7.726+05

1.246+05

2.91E+05

4.996+05

5.706+05

5.226+05

HA

HA

HA

HA

so.'- $

ug/mL

5.655-01

1.536-01

3.266-01

2.296-01

4.776+00

2.026+00

2.456-02

4.125+00

4.696+00

7.796-01

6.435+00

9.106-01

2.356+00

3.376+00

7.406+00

2.036+01

5.455+00

7.896+00

HA

1.555+01

DSC-222S

Joules/mL ♦ uet ut

NA

NA

0.0

0.0

0.0

0.0

74.3

NA

0.0

0.0

NA

NA

0.0

0.0

0.0

0.0

NA

NA

NA

NA

po.'- $

u g / m

< 1.346-01

< 1.156-01

< 1.256-01

< 1.065-01

< 1.586+00

< 1.286+00

< 2.456-02

< 8.046-01

< 9.816-01

< 4.56E-02

< 2.385+00

< 2.455-01

< 7.526-01

< 3.556-02

< 9.046-01

< 7.476-01

< 1.756+00

< 1.386+00

NA

< 4.905-01 7c": Tota l carbon

//g/mL: //g/mL a s - s e t t l e d sludge ♦ : Joules/mL a s - s e t t t e d sludge

NA: Not analyzed * : moles OH/mL a s - s e t t l e d sludge $: so lub le

C-20

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

NO," $ uo/mL

1.696-01 1.416-01

< 1.795-01 7.026-01 2.156+00

< 6.036-01 3.466-02

< 3.805-01 < 4.636-01

2.126-01 < 1.126+00 < 1.166-01 < 3.556-01

1.295-01 < 4.276-01 < 3.536-01 < 8.256-01 < 6.546-01

NA < 2.316-01

Se ug/mL

< 3.775+01 < 1.096+02 < 1.256+01 < 4.135+01 < 1.686+01 < 8.645+01 < 1.026+01

NA < 1.376+02 < 3.206+01 < 7.916+01 < 1.656+02 < 1.396+02 < 9.306+01 < 2.366+02 < 1.606+02

NA HA

< 3.776+02 < 1.475+02

NO,' » ug/mL

< 4.836-02 < 4.146-02 < 4.526-02 < 3.826-02 < 9.046-01 < 4.625-01 < 1.416-02 < 2.916-01 < 3.556-01 < 4.106-02 < 8.606-01 < 8.865-02 < 2.726-01 < 3.196-02 < 3.276-01 < 2.706-01 < 6.326-01 < 7.94E-01

NA < 1.775-01

K ug/mL

< 1.885+02 < 5.446+02 < 6.256+01 < 2.066+02 < 8.416+01 < 4.326+02

1.216+03 HA

< 6.866+02 < 1.605+02 < 3.956+02 < 8.266+02 < 6.945+02

4.756+02 < 1.186+03

1.686+03 NA NA 2.546+03 1.756+03

CI' $ ug/mL

2.446-01 9.726-02 1.236-01

< 2.126-01 4.406-01

< 7.446-02 1.706-02 2.546-01 2.985-01 1.976-01 4.336-01 1.646-01 1.136-01 1.206-01 1.616-01 5.286-01 2.126-01 3.265-01 HA 3.375-01

Residue * ug/mL 1.206+04 4.736+04 5.806+03 3.416+04 1.906+04 4.406+04 4.456+05 1.256+05 9.046+04 2.506+04 3.796+04 6.106+04 1.495+05 4.125+05 9.426+04 1.516+05 1.596+04 4.65E+04 2.876+05 2.956+05

F' » ug/mL

< 5.876-03 < 5.036-03 < 1.526-02 < 4.645-03 < 6.916-02 < 5.485-02 < 1.086-03 < 3.52E-02 < 4.216-02 < 4.986-03

1.626+00 3.666-02

< 3.306-02 4.526-02 3.415-01

< 3.286-02 < 7.666-02 < 6.076-02

HA 6.116-02

6.116-02

NH, $ ug/mL

3.886+00 < 3.876+00 < 2.116+00 < 1.786+00 < 2.426+00 < 1.966+00 < 7.526-02 < 1.236+01 < 1.506+00 < 1.926+00 < 3.646+00

NA < 1.155+00 < 1.496+00 < 1.396+00 < 1.155+00

HA HA NA NA

NA $: soluble

//g/mL: //g/mL as-settled sludge NA: Not analyzed * : acid insoluble

C-21

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This page intentionally l e f t blank.

C-22

WHC-SP-1182

APPENDIX D

THE CHEMISTRY OF DRIED SLUDGE

T. L. Welsh D. B. Bechtold B. A. Crawford

D-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

The conversion of centrifuged sludge results to as-dried sludge results u t i l i zed the following formulas. I t is assumed that the analytes are non-volati le. The following table defines the symbols used in deriving the formula to convert centrifuged-state analyses to a dried-state.

Symbol c 9 d

subscript f subscript d

Meaning gravimetric concentration

mass dried concentration centrifuged state

dried state

Units //g/g or //Ci/g

9 Ug/g or //Ci/g

By mass balance:

cf3f = cdgd (1)

Solving for cd gives the following conversion equation.

3d (2)

The values for c, and the sample location information are listed in Appendix B. The values for gf ana gd are listed in Table 7, columns 4 and 6 respectively, from letter report 75764-PCS95-109, Rev.l. This letter report is also Appendix A in Miller 1996. For volatile analytes, the concentration on a dried sludge basis is zero. The PNNL uranium isotopic results were reported in atom % (Appendix B). The units for the uranium isotopics were changed to //g/g dried sludge using equation 3 of Appendix B, where C is the total uranium concentration (C), as measured by PNNL (units of //g/g dried sludge), for the sample of interest.

D-3

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

"Co uCi/g

1.876+00 2.266+00 5.406+00 3.116+00 3.045+00 1.616+00 1.856-01 1.075+00 3.506+00 2.985+00 3.266+00 1.676+00 2.056+00 1.526+00 5.526-01 1.675+00 3.256+00 9.426-01 NA 1.806+00

'"Ce/Pr uCi/g

< 4.896+00 < 5.036-01 < 1.20E+00 < 8.916-01 < 1.156+00 < 4.426-01 < 5.086-01 < 7.176+00 < 2.486-01 < 7.556-01 < 2.386-01 < 2.896-01 < 1.326+00 < 1.31E+00 < 4.596-01 < 2.515+00 < 5.135+00 < 3.065+00

NA < 1.926+00

"'Cs uCi/g

5.316+02 5.736+01 1.396+02 1.676+02 2.175+02 5.906+01 1.446+02 1.116+03 3.796+01 1.096+02 2.766+01 5.686+01 1.536+02 1.215+02 9.796+01 5.456+02 1.276+03 4.265+02 NA 5.506+02

"Nb uCi/g

< 2.686-01 < 4.066-02 < 1.186-01 < 8.026-02 < 7.676-02 < 3.356-02 < 1.786-02 < 2.356-01 < 2.235-02 < 6.886-02 < 2.116-02 < 1.846-02 < 5.466-02 < 6.975-02 < 1.916-02 < 8.366-02 < 2.236-01 < 1.456-01

NA < 7.956-02

'"Cs uCi/g

< 3.686-01 < 3.285-02 < 1.016-01 < 7.346-02

9.046-02 < 2.356-02

7.306-02 < 5.426-01 < 2.206-02 < 6.266-02 < 2.095-02 < 2.365-02 < 8.386-02 < 1.036-01

3.826-02 1.906-01 5.786-01 2.086-01 NA 2.136-01

'"Ru/Rh uCi/g

< 7.146+00 < 7.926-01 < 1.966+00 < 1.426+00 < 1.806+00 < 6.916-01 < 7.656-01 < 1.076+01 < 4.236-01 < 1.206+00 < 4.046-01 < 4.485-01 < 1.616+00 < 2.006+00 < 7.045-01 < 3.806+00 < 7.006+00 < 4.506+00

NA < 2.89E+00

"*EU uCi/g

1.18E+01 2.39E+00 8.57E+00 8.18E+00 4.82E+00 1.816+00

< 4.106-02 6.685+00 5.886-01 5.235+00 6.406-01

< 5.866-01 2.166+00 1.695+00 4.435-01 1.026+00 8.496+00 4.856+00 NA 1.165+00

'"Ra uCi/g

< 9.275+00 < 9.696-01 < 2.295+00 < 1.736+00 < 2.256+00 < 8.476-01 < 1.046+00 < 1.396+01 < 5.036-01 < 1.456+00 < 4.536-01 < 5.896-01 < 2.226+00 < 2.586+00 < 8.976-01 < 4.876+00 < 1.126+01 < 6.266+00

NA < 3.906+00

'"5u uCi/g

5.766+00 1.086+00 4.195+00 3.636+00 2.126+00 8.726-01

< 1.186-01 3.086+00 2.996-01 2.596+00 4.256-01 2.756-01 1.236+00 6.586-01 2.536-01

< 6.166-01 2.886+00 1.895+00 NA

< 5.856-01

"•TI uCi/g

< 5.97E+00 < 6.346-01 < 1.505+00 < 1.126+00 < 1.465+00 < 5.516-01 < 6.845-01 < 8.916+00 < 3.336-01 < 9.406-01 < 2.986-01 < 3.855-01 < 1.405+00 < 1.655+00 < 5.796-01 < 3.136+00 < 6.826+00 < 4.086+00

NA < 2.556+00

//Ci/g: //Ci/g dried sludge NA: Not analyzed

D-5

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

" *B i

uC i /g

< 2.205+00

< 3.505-01

< 8.806-01

< 6.515-01

< 7.016-01

< 2.826-01

< 2.926-01

< 2.666+00

< 2.335-01

< 5.165-01

< 2.185-01

< 1.925-01

< 5.296-01

< 6.406-01

< 2.526-01

< 1.266+00

< 2.896+00

< 1.346+00

NA

< 1.196+00

Tota l Beta

uCi /g

2.665+03

1.206+02

4.836+02

4.976+02

5.806+02

2.176+02

3.675+02

2.326+03

6.986+01

2.736+02

7.666+01

1.375+02

5.096+02

3.906+02

2.315+02

1.475+03

2.166+03

1.616+03

NA

1.435+03

" ' 5 u

uCi /g

< 3.576-01

< 7.036-02

< 1.505-01

< 1.145-01

< 1.076-01

1.92E-01

< 2.196-01

< 3.626-01

< 4.056-02

< 2.486-01

< 2.836-02

< 3.096-02

< 1.025-01

< 1.216-01

1.386-01

< 1.386-01

< 2.476-01

< 2.356-01

NA

< 1.166-01 2w/a*>pu

uCi /g

3.006+01

1.515+01

6.076+01

5.186+01

3.135+01

1.475+01

4.036-01

3.365+01

4.106+00

3.646+01

4.585+00

4.256+00

1.916+01

1.256+01

3.266+00

8.305+00

6.73E+01

3.3BE+01

NA

7.98E+00

" ! Sb

uCi /g

< 1.90E+00

< 2.006-01

< 4.746-01

< 3.575-01

< 4.625-01

< 1.765-01

< 2.226-01

< 2.816+00

< 1.105-01

< 3.016-01

< 9.616-02

< 1.276-01

< 4.166-01

< 5.245-01

< 1.866-01

< 1.006+00

< 2.076+00

< 1.336+00

HA

< 8.346-01

"*Pu

uCi /g

4.34E+00

< 4.91E+00

1.10E+01

7.88E+00

5.06E+00

2.36E+00

6.18E-02

< 8.20E+00

6.79E-01

< 8.84E+00

< 1.62E+00

< 1.656+00

< 5.206+00

< 2.106+00

< 1.196+00

1.375+00

< 3.486+01

< 9.035+00

NA

1.276+00

"'Am - G5A

uCi /g

7.446+01

1.416+01

5.286+01

4.876+01

2.996+01

1.206+01

3.976-01

4.026+01

3.665+00

3.246+01

3.736+00

3.726+00

1.476+01

1.096+01

2.526+00

6.236+00

5.016+01

3.14E+01

NA

6.84E+00

" 'No

uCi /g

4.996-03

< 3.816-03

1.226-02

3.856-03

< 4.926-03

< 2.506-03

< 2.296-03

< 6.336-03

< 1.896-03

5.66E-03

< 1.45E-03

< 2.526-03

1.526-03

1.876-03

2.746-03

1.186-03

7.426-03

3.506-03

HA

< 1.496-03

Alpha Tota l

uCi /g

1.685+02

1.916+01

1.306+02

1.196+02

7.465+01

3.436+01

9.88E-01

8.356+01

1.006+01

6.296+01

1.046+01

8.81E+00

3.216+01

2.566+01

5.686+00

1.696+01

1.096+02

7.806+01

HA

1.676+01

" " " •Cm

uCi /g

< 1.176+01

< 1.906+00

< 1.586+01

< 1.125+01

< 1.246+01

< 1.586+00

< 2.506-01

< 9.656+00

< 8.995-01

< 1.026+01

< 6.766-01

< 4.345-01

< 4.606+00

< 1.975+00

< 1.806+00

< 1.606+00

< 1.176+01

< 1.165+01

NA

< 1.666+00

/ / C i / g : / /C i /g d r i e d sludge NA: Not analyzed

D-6

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

"'Am - A6A

uCi /g

7.136+01

1.316+01

5.186+01

4.946+01

2.95E+01

1.126+01

3.436-01

4.206+01

3.52E+00

3.106+01

3.456+00

3.536+00

1.436+01

1.026+01

2.966+00

6.506+00

4.906+01

3.056+01

NA

6.545+00

" U »

ug/g

< 3.206+00

< 4.986-01

< 1.65E+00

< 6.966-01

< 9.876-01

< 5.666-01

< 3.086-02

< 3.146+00

< 2.466-01

< 9.926-01

< 3.116-01

< 2.986-01

< 9.446-01

< 7.126-01

< 2.305-01

NA

NA

NA

NA

NA

" S r

uCi /g

1.226+03

3.866+01

1.396+02

2.456+02

1.616+02

6.B76+01

9.666+01

1.045+03

8.006+00

8.455+01

6.366+00

3.845+01

2.085+02

1.216+02

6.926+01

4.166+02

5.246+02

5.636+02

NA

3.036+02

' "U B

ug/g

2.275+01

3.006+00

1.046+01

4.825+00

6.696+00

4.296+00

2.416-01

2.626+01

1.805+00

7.276+00

2.256+00

2.035+00

6.736+00

4.866+00

1.845+00

NA

HA

HA

NA

NA

. U-222S phosphorescence

ug/g

NA

NA

5.375+04

NA

4.126+04

2.506+04

2.876+03

NA

2.006+04

1.316+05

NA

NA

4.706+04

4.536+04

2.026+04

2.68E+04

NA

NA

NA

NA

™U «

ug/q

2.306+03

3.496+02

1.165+03

4.945+02

6.975+02

4.026+02

2.206+01

2.336+03

1.726+02

7.016+02

2.186+02

2.105+02

6.75E+02

5.066+02

1.626+02

NA

NA

NA

NA

NA

„ U-PNNL f luorescence

ug/g

3.275+05

5.086+04

1.685+05

7.116+04

1.015+05

5.786+04

3.146+03

3.216+05

2.515+04

1.016+05

3.185+04

3.046+04

9.645+04

7.276+04

2.35E+04

HA

NA

NA

NA

NA

™U B

uq/q

2.476+02

3.836+01

1.336+02

5.576+01

7.706+01

4.276+01

2.426+00

1.596+02

1.946+01

7.346+01

2.406+01

2.386+01

7.226+01

5.416+01

1.776+01

NA

NA

NA

NA

NA

U" &

2 S

ug/g

4.376+05

6.066+04

1.445+05

1.286+05

1.186+05

6.395+04

2.49E+03

NA

2.306+04

1.02E+05

3.28E+04

3.276+04

1.126+05

7.336+04

1.996+04

5.366+04

NA

NA

NA

5.846+04

™U ■

ug/g

3.256+05

5.056+04

1.676+05

7.056+04

1.006+05

5.736+04

3.126+03

3.196+05

2.496+04

1.016+05

3.155+04

3.026+04

9.576+04

7.216+04

2.336+04

NA

NA

NA

NA

NA

/ / C i / g : / /C i /g d r i e d sludge / / g / g : / /g/g d r i e d sludge

B: based on the t o t a l uranium (//g/g d r i e d sludge) by PNNL

D-7

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Al ug/g

6.465+04 7.615+04 1.336+05 8.255+04 1.056+05 3.396+04 1.876+04 NA 4.396+04 8.186+04 5.985+04 5.846+04 3.216+04 3.046+04 2.646+04 4.976+04 NA NA NA 5.306+04

Fe ug/g 8.156+04 3.095+05 1.626+05 2.276+05 1.696+05 4.075+05 1.516+04 NA 3.986+05 2.776+05 3.786+05 3.746+05 3.465+05 1.675+05 4.466+05 2.596+05 NA NA NA 2.405+05

Ca ug/g

2.576+03 2.516+03 4.43E+03 7.146+03 2.896+04 7.206+03 1.226+04 NA 1.216+03 7.535+03 9.216+02 1.635+03 5.056+03 5.136+03 1.516+04 1.456+04 HA HA NA 2.596+04

Mg ug/g 6.516+02 1.686+03 1.626+03 2.616+03 5.046+03 2.595+03 2.256+03 NA 1.426+03 1.936+03 1.316+03 7.305+02 1.256+03 1.426+03 2.095+03 2.405+03 NA NA NA 2.716+03

Cd ug/g

1.376+02 1.416+02 3.506+02 2.216+02 2.496+02 1.626+02 5.905+01 NA 8.026+01 2.84E+02 6.986+01 7.886+01 5.825+01 6.356+01 3.926+01 4.39E+01 NA NA NA 4.476+01

Mn ug/g 3.026+02 5.496+02 7.776+02 6.656+02 7.406+02 7.656+02 2.086+02 NA 4.736+02 8.476+02 6.135+02 6.186+02 4.946+02 3.446+02 5.786+02 4.436+02 NA NA NA 7.386+02

Cr ug/g

2.786+02 8.766+02 5.246+02 6.156+02 4.92E+02 1.456+03 9.385+01 NA 7.936+02 7.796+02 7.686+02 5.046+02 1.235+03 5.786+02 1.536+03 8.24E+02 NA NA NA 1.096+03

Na ug/g 6.945+02 8.056+02 1.205+03 6.286+02 1.146+03 5.766+02 3.266+04 HA 3.366+02 7.185+02 3.206+02 2.926+02 3.996+02 3.096+02 5.896+02 1.446+03 NA NA HA 1.396+03

Cu ug/g

5.116+02 1.176+03 1.335+03 8.775+02 8.735+02 8.006+02 5.395+01 HA 4.596+02 1.026+03 3.156+02 5.825+02 3.685+02 5.936+02 4.496+02 2.175+02 NA NA NA 3.636+02

Pb ug/g 2.366+02 5.346+02 5.21E+02 5.166+02 5.116+02 1.086+03 1.606+02 NA 4.935+02 7.505+02 6.486+02 4.216+02 5.705+02 3.646+02 6.875+02 4.576+02 NA NA NA 4.586+02

//g/g: //g/g dried sludge NA: Not analyzed

D-8

WHC-SP-1182

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Location 1 2 3 4 5 6 8 9 10 11 12 15 16 17 18 19 20 21 22 23

Zn ug/g

6.476+02 1.256+03 1.246+03 1.376+03 1.265+03 1.946+03 1.196+02 NA 9.046+02 1.566+03 1.08E+03 7.656+02 1.256+03 6.565+02 1.696+03 9.766+02 NA NA NA 8.246+02

Be ug/g 6.116+01 8.256+01 1.625+02 8.386+01 7.716+01 2.675+01 3.866+00 NA 1.926+01 9.955+01

< 1.445+01 1.346+01 1.826+01 1.266+01

< 1.776+01 1.656+01 NA HA HA 2.686+01

Zr ug/g

6.216+02 8.306+02 8.25E+02 8.026+02 5.186+02 7.085+02 6.186+01 NA 2.386+02 8.036+02 1.786+02 1.426+02 8.876+02 3.776+02 6.566+02 2.986+02 HA NA NA 6.486+02

Sm and Se ug/g

< 1.755+02 < 3.406+02 < 1.475+02 < 1.796+02 < 1.195+02 < 2.556+02 < 2.225+01

NA < 2.386+02 < 1.895+02 < 2.886+02 < 2.266+02 < 1.776+02 < 1.166+02 < 3.536+02 < 1.886+02

NA NA NA

< 1.616+02

Ag ug/g

< 1.75E+01 < 3.406+01 < 1.475+01 < 1.796+01

1.246+01 < 2.556+01 < 2.226+00

NA < 2.385+01 < 1.896+01 < 2.886+01 < 2.266+01 < 1.776+01 < 1.166+01 < 3.535+01 < 1.886+01

NA NA NA

< 1.616+01

TI ug/g

< 3.506+02 < 6.776+02 < 2.946+02 < 3.576+02 < 2.385+02 < 5.106+02 < 4.455+01

NA < 4.766+02 < 3.795+02 < 5.766+02 < 4.536+02 < 3.546+02 < 2.326+02 < 7.075+02 < 3.775+02

NA NA NA

< 3.236+02

B ug/g

1.885+02 2.716+02 5.655+02 2.816+02 6.195+02 2.436+02 1.396+02 NA 2.006+02 2.936+02

< 1.446+02 1.625+02 1.595+02 8.596+01 1.906+02

< 9.425+01 NA NA HA

< 8.076+01

CN" ug/g

< 6.246+00 NA

< 5.82E+00 < 2.476+00 < 3.826+00 < 8.616-01 < 1.526+00

NA < 1.086+00 < 3.596+00

NA < 6.676-01 < 8.986-01 < 1.075+00 < 1.185+00 < 1.076+00

NA NA NA NA

Ba ug/g

2.326+02 < 1.696+02

2.896+02 2.626+02 2.906+02 1.755+02 5.036+02 NA

< 1.196+02 2.895+02 4.536+02

< 1.135+02 1.876+02 1.246+02

< 1.775+02 6.576+02 NA NA NA 5.946+02

K

< 8.746+02 < 1.695+03 < 7.385+02 < 8.936+02 < 5.966+02 < 1.276+03

2.666+03 NA

< 1.196+03 < 9.496+02 < 1.446+03 < 1.136+03 < 8.866+02

5.936+02 < 1.776+03

1.985+03 NA NA 1.706+03 1.936+03

/ / g / g : / /g/g d r i e d sludge NA: Not analyzed

D-9

WHC-SP-1182

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

Locat ion

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21

22

23

TIC

ug/g

2.985+03

1.915+03

2.065+04

2.396+03

4.365+03

1.645+03

2.226+03

NA

1.266+03

3.126+03

NA

2.025+03

1.726+03

1.385+03

3.015+03

2.226+03

3.926+03

NA

NA

3.605+03

PO.'- $ ug/g

< 6.966-01

< 4.636-01

< 2.045+00

< 7.446-01

< 1.226+01

< 5.126+00

< 5.356+00

< 1.736+00

< 2.736+00

< 4.316-01

< 4.935+00

< 4.556+00

< 2.226+00

< 6.276-02

< 2.756+00

< 1.996+00

< 1.175+01

•= 3.595+00

NA

< 2.126+00 C/TOC/TC: Tota l ino

TOC 8

ug/g

1.886+03

2.126+03

4.696+03

2.966+03

3.736+03

3.686+03

8.816+03

NA

1.886+03

2.995+03

NA

2.136+03

3.316+03

2.646+03

3.586+03

2.095+03

3.486+03

NA

NA

1.896+03

NO, $

ug/g

8.796-01

5.676-01

< 2.926+00

4.946+00

1.676+01

< 2.426+00

7.556+00

< 8.196-01

< 1.296+00

2.006+00

< 2.336+00

< 2.155+00

< 1.055+00

2.276-01

< 1.306+00

< 9.396-01

< 5.546+00

< 1.696+00

NA

< 1.006+00 game carbon/Total 0

TC 8

ug/g

5.425+03

4.306+03

8.256+03

5.725+03

9.775+03

5.116+03

1.436+04

NA

4.466+03

4.956+03

NA

4.656+03

3.846+03

3.235+03

7.466+03

4.596+03

7.725+03

NA

NA

5.365+03

NO, t

ug/g

< 2.51E-01

< 1.67E-01

< 7.37E-01

< 2.69E-01

< 7.02E+00

< 1.85E+00

< 3.07E+00

< 6.28E-01

< 9.86E-01

< 3.88E-01

< 1.78E+00

< 1.65E+00

< 8.05E-01

< 5.64E-02

< 9.94E-01

< 7.20E-01

< 4.25E+00

< 2.06E+00

NA

< 7.665-01 rgamc caroon, t o t a l

OH demand I

moles OH/g *

1.076-03

1.256-03

2.006-03

1.086-03

9.256-04

5.255-04

4.376-04

NA

5.975-04

1.066-03

NA

4.136-04

5.006-04

1.875-04

2.686-04

4.036-04

NA

NA

NA

HA

CI $

ug/q

1.276+00

3.926-01

2.016+00

< 1.496+00

3.426+00

< 2.996-01

3.70E+00

5.486-01

8.276-01

1.87E+00

8.976-01

3.056+00

3.346-01

2.126-01

4.896-01

1.416+00

1.426+00

8.456-01

NA

1.466+00 carbon.

so.'- $ ug/g

2.946+00

6.175-01

5.316+00

1.615+00

3.706+01

8.096+00

5.336+00

8.886+00

1.306+01

7.375+00

1.335+01

1.696+01

6.966+00

5.956+00

2.256+01

5.406+01

3.666+01

2.056+01

NA

6.706+01

F" %

ug/g

< 3.066-02

< 2.036-02

< 2.4B5-01

< 3.276-02

< 5.376-01

< 2.206-01

< 2.346-01

< 7.616-02

< 1.176-01

< 4.716-02

3.356+00

6.815-01

< 9.756-02

7.996-02

1.046+00

< 8.725-02

< 5.156-01

< 1.576-01

NA

2.646-01

//g/g: ug/g dried sludge 8: A portion of the TOC/TC may have evaporated during the drying process. I: The drying process may affect the caustic demand result. +: moles OH/g dried sludge $: based on the soluble concentration

D-10

WHC-SP-1182

Location

1

2 3

4

5

6

8 9

10

11

12

15

16

17

18

19 20

21

22

23

Residue (acid insoluble)

w/g 5.73E+04

1.48E+05

7.35E+04

1.50E+05

1.43E+05

1.31E+05

9.73E+05 9.42E+04

1.58E+05

1.52E+05

1.40E+05

8.36E+04

1.91E+05

5.18E+05

1.41E+05

1.78E+05 1.26E+05

7.33E+04

NA

3.26E+05 //g/g: //g/g dried sludge

D - l l

WHC-SP-1182

This page intentionally l e f t blank.

D-12

WHC-SP-1182

A P P E N D I X

MAPS OF ANALYTE CONCENTRATION VERSUS BASIN LOCATION

T. L. Welsh

The following figures illustrate the analyte concentrations as presented in Appendices B or C by basin location. Specific details on basin locations are provided in Table 3.1 and Appendix A.

E-l

WHC-SP-1182

This page intentionally left blank.

WHC-SP-1182

KE Main Basin Sample Results C06O - uCi/g centrifuged sludge

NS K12

KE Weasel Pit Sample Results C06O - uCi/g centrifuged sludge

1222

0 300^

P16

1039

Q17

E-3

WHC-SP-1182

KE Main Basin Sample Results Cs137 - uCi/g centrifuged sludge

NS K12

KE Weasel Pit Sample Results Cs137 - uCi/g centrifuged sludge

91

017 , NA.335

E-4

WHC-SP-1182

KE Main Basin Sample Results Cs134 - uCi/g centrifuged sludge

NS K12

0.126.0.0992

<0.110

.91 <0.0)833

M13

~L1

Ell

KE Weasel Pit Sample Results Cs134 - uCi/g centrifuged sludge

<0.0499 <0.0675

r 0.0208,

0.118

T20

E-5

WHC-SP-1182

KE Main Basin Sample Results Eu154 - uCi/g centrifuged sludge

>5 K12

KE Weasel Pit Sample Results Eu154 - uCi/g centrifuged sludge

I 290

0 241

017

0 636

WA,0 705

E-6

WHC-SP-1182

KE Main Basin Sample Results Eu155 - uCi/g centrifuged sludge

N5 K12

KE Weasel Pit Sample Results Eu155 - uCi/g centrifuged sludge

0 730

017 NA,<0 356

E-7

WHC-SP-1182

KE Main Basin Sample Results Ce/Pr144 - uCi/g centrifuged sludge

0 9

<ll. 168

135

A2

N5 K12

M13

LI

E l l

KE Weasel Pit Sample Results Ce/Pr144 - uCi/g centrifuged sludge

<0 860

0 250 ,

JSIA,<1 164

E-8

WHC-SP-1182

KE Main Basin Sample Results Nb94 - uCi/g centrifuged sludge

09

<o.o

F10

C4 N5 K12

M13

LI

KE Weasel Pit Sample Results Nb94 - uCi/g centrifuged sludge

O.0325 r <0 0457

<0.0104

<0 0521

Q17

E-9

WHC-SP-1182

KE Main Basin Sample Results RuRh106 - uCi/g centrifuged sludge

N5 K12

115

).!59 «l 1.231

B3

<0_.380 <0. <1.529,<2/150

M13

"LI

Ell

KE Weasel Pit Sample Results RuRh106 - uCi/g centrifuged sludge

<2.368

E-10

WHC-SP-1182

KE Main Basin Sample Results Ra226 - uCi/g centrifuged sludge

N5 K12

\ \ <0.|l

M13

-LI

A2 Ell

KE Weasel Pit Sample Results Ra226 - uCi/g centrifuged sludge

<1 320 <1 694

<0 488 ,

WA,<2 372

E - l l

WHC-SP-1182

KE Main Basin Sample Results TI208 - uCi/g centrifuged sludge

H8

115

F10

J.!23 <l 1.182

C4

B3

N5 K12

KE Weasel Pit Sample Results TI208 - uCi/g centrifuged sludge

M13

- L I

■:0.833 <1.080

017

<1.950

J)IA,<1.550

E-12

WHC-SP-1182

KE Main Basin Sample Results Bi212 - uCi/g centrifuged sludge

115

>. 111 =11.127

B3

N5 K12

M13

^ L l

KE Weasel Pit Sample Results Bi212 - uCi/g centrifuged sludge

■:0 315 <0 420

<0 137,

<0 784

-NA,<0 721

E-13

WHC-SP-1182

KE Main Basin Sample Results Eu152 - uCi/g centrifuged sludge

09

F10

B3

N5 K12

KE Weasel Pit Sample Results Eu152 - uCi/g centrifuged sludge

M13

-Ll

V <0 0793

<0 0857

-NA,<0 0706

E-14

WHC-SP-1182

KE Main Basin Sample Results Sb125 - uCi/g centrifuged sludge

N5 K12

0X733 <0 0598

F10

A2 E l l

M13

- L I

KE Weasel Pit Sample Results Sb125 - uCi/g centrifuged sludge

/ P16

<0.101,

J)IA,<0.507

T20

E-15

WHC-SP-1182

KE Main Basin Sample Results Am241 GEA - uCi/g settled sludge

N5 K12

KE Weasel Pit Sample Results Am241 GEA - uCi/g settled sludge

7.44

3.33

r.33,3.78 017

T20

E-16

WHC-SP-1182

KE Main Basin Sample Results Alpha Total - uCi/g settled sludge

N5 K12

KE Weasel Pit Sample Results Alpha Total - uCi/g settled sludge

16.30 R18

9.04

E-17

WHC-SP-1182

KE Main Basin Sample Results Total Beta - uCi/g settled sludge

N5 K12

KE Weasel Pit Sample Results Total Beta - uCi/g settled sludge

; 57.87 r 205.68

«p.50,789.87

E-18

WHC-SP-1182

KE Main Basin Sample Results Pu239/240 - uCi/g settled sludge

N5 K12

KE Weasel Pit Sample Results Pu239/240 - uCi/g settled sludge

9 66

P16

6 58

' 54,4 41

E-19

WHC-SP-1182

KE Main Basin Sample Results Pu238 - uCi/g settled sludge

C4 N5 K12

115

FIO

A2

KE Weasel Pit Sample Results Pu238 - uCi/g settled sludge

<2.64

r P16

0.73

T20

M13

-LI

E-20

WHC-SP-1182

KE Main Basin Sample Results Np237 - uCi/g settled sludge

09 C4

N5 K12

KE Weasel Pit Sample Results Np237 - uCi/g settled sludge

0 100840

P16 0 00130,

0 000693

-^OjmS6,<0 000867

T20

E-21

WHC-SP-1182

KE Main Basin Sample Results Cm243/244 - uCi/g settled sludge

0 9

1.243 cl 1.382

A2

N5 K12

<1486 <0. <1.327|<4.211

<2.146

KE Weasel Pit Sample Results Cm243/244 - uCi/g settled sludge

M13

-LI

<2 33 <104

<0 80_

-42 97,0 92

<0 85

R18

E-22

WHC-SP-1182

KE Main Basin Sample Results Am241 AEA - uCi/g settled sludge

KE Weasel Pit Sample Results Am241 AEA - uCi/g settled sludge

7 26 5 38

131

-6 45,3 61

E-23

WHC-SP-1182

KE Main Basin Sample Results Sr90 - uCi/g settled sludge

N5 K12

KE Weasel Pit Sample Results Sr90 - uCi/g settled sludge

' 05.54

30.74,

221.89

-23.1.50,167.25 Q17

E-24

WHC-SP-1182

KE Main Basin Sample Results U (222S) - ug/g settled sludge

N5 K12

phosphorescence

KE Weasel Pit Sample Results U (222S) - ug/g settled sludge

:!3831 23864

Q17

phosphorescence

8980,

NA.NA

E-25

WHC-SP-1182

KE Main Basin Sample Results U (PNNL) - ug/g settled sludge

fluorescence

KE Weasel Pit Sample Results U (PNNL) - ug/g settled sludge

'18893 r

fluorescence

38325

4B900.8700

T20

E-26

WHC-SP-1182

KE Main Basin Sample Results U (222S) - ug/g settled sludge

N5 K12

ICP

KE Weasel Pit Sample Results U (222S) - ug/g settled sludge

38654

8841

45640,32246 Q17

ICP

E-27

WHC-SP-1182

KE Main Basin Sample Results Al - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Al - ug/g settled sludge

6292

r 11723^

36673 29258

T20

E-28

WHC-SP-1182

KE Main Basin Sample Results Ca - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Ca - ug/g settled sludge

2563

r P16

2706

-20696,14306

E-29

WHC-SP-1182

H8

115

KE Main Basin Sample Results Cd - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Cd - ug/g settled sludge

30

48,25

E-30

WHC-SP-1182

KE Main Basin Sample Results Cr - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Cr - ug/g settled sludge

621

439

-,1191,600

-no

E-31

WHC-SP-1182

KE Main Basin Sample Results Cu - ug/g settled sludge

H8

115

F10

N5 K12

M13

-LI

186

KE Weasel Pit Sample Results Cu - ug/g settled sludge

-.592,200

E-32

WHC-SP-1182

KE Main Basin Sample Results Fe - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Fe - ug/g settled sludge

175451 87856

197821,

138027

-326298,132824

E-33

WHC-SP-1182

KE Main Basin Sample Results K - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results K - ug/g settled sludge

451

P16

017

1060

590,1060

E-34

WHC-SP-1182

KE Main Basin Sample Results Mg - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Mg - ug/g settled sludge

635 750

930

1282

3010,1497

E-35

WHC-SP-1182

KE Main Basin Sample Results Mn - ug/g settled sludge

N5 K12

M13

-LI

KE Weasel Pit Sample Results Mn - ug/g settled sludge

251 r 257

236

-.615,408 Q17

E-36

WHC-SP-1182

KE Main Basin Sample Results Na - ug/g settled sludge

N5 K12

M13

-LI

KE Weasel Pit Sample Results Na - ug/g settled sludge

203

1800,766

E-37

WHC-SP-1182

KE Main Basin Sample Results Pb - ug/g settled sludge

N5 K12

M13

-LI

KE Weasel Pit Sample Results Pb - ug/g settled sludge

289

305

672,253

E-38

WHC-SP-1182

KE Main Basin Sample Results Zn - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Zn - ug/g settled sludge

634

521

-,1306,455

T20

R18

E-39

WHC-SP-1182

KE Main Basin Sample Results Zr - ug/g settled sludge

N5 K12

r

KE Weasel Pit Sample Results Zr - ug/g settled sludge

159

017

E-40

WHC-SP-1182

KE Main Basin Sample Results Ag - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results Ag - ug/g settled sludge

<9 01

<15.73_

*23.59,<8.93

T20

E-41

WHC-SP-1182

KE Main Basin Sample Results B - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results B - ug/g settled sludge

81

<50

017

E-42

WHC-SP-1182

KE Main Basin Sample Results Ba - ug/g settled sludge

H8

N5 K12

KE Weasel Pit Sample Results Ba - ug/g settled sludge

/ <79

350

-352,328

T20

E-43

WHC-SP-1182

H8

115

KE Main Basin Sample Results Be - ug/g settled sludge

N5 K12

M13

-LI

KE Weasel Pit Sample Results Be - ug/g settled sludge

9

V

14,15

E-44

WHC-SP-1182

KE Main Basin Sample Results Se - ug/g settled sludge

09

H8

115

F10

r.16 01.62

C4

A2 B3

N5 K12

<32.79

r <5( .49

M13

-LI

Ell

KE Weasel Pit Sample Results Se - ug/g settled sludge

<90 r <62

-*236,<89

E-45

WHC-SP-1182

KE Main Basin Sample Results Sm - ug/g settled sludge

KE Weasel Pit Sample Results Sm - ug/g settled sludge

E-46

WHC-SP-1182

KE Main Basin Sample Results TI - ug/g settled sludge

09

.32 13.24

N5 K12

«

M13

-LI

KE Weasel Pit Sample Results TI - ug/g settled sludge

/ <123

<315,

R18

<202

E-47

WHC-SP-1182

KE Main Basin Sample Results TIC - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results TIC - ug/g settled sludge

872 r 1340,

-.NA.1987

E-48

WHC-SP-1182

KE Main Basin Sample Results TOC - ug/g settled sludge

KE Weasel Pit Sample Results TOC - ug/g settled sludge

1687

R18

1119

E-49

WHC-SP-1182

KE Main Basin Sample Results TC - ug/g settled sludge

N5 K12

KE Weasel Pit Sample Results TC - ug/g settled sludge

1951 r 1711

3321

-.NA.2962

T20

E-50

WHC-SP-1182

KE Main Basin Sample Results CN - ug/g settled sludge

0 9

H8

1.176 <l 1.472

F10

C4 N5 K12

M13

-LI

KE Weasel Pit Sample Results CN - ug/g settled sludge

■:0.464 <0.573

<0.534,

<0.581

NA.NA

E-51

WHC-SP-1182

09

KE Main Basin Sample Results TGA (222S) - weight loss (%)

N5 K12

A \ C4

KE Weasel Pit Sample Results TGA (222S) - weight loss (%)

35.8 37.3

37.3

E-52

WHC-SP-1182

KE Main Basin Sample Results TGA (PNNL) - weight loss (%)

N5 K12

KE Weasel Pit Sample Results TGA (PNNL) - weight loss (%)

4.7 16.7

32.8

NA.NA 017

E-53

WHC-SP-1182

KE Main Basin Sample Results DSC (wet wt) - joules/g settled sludge

N5 K12

M13

-LI

PNNL

E-54

WHC-SP-1182

KE Main Basin Sample Results DSC (wet wt) - joules/g settled sludge

N5 K12

M13

-LI

222S

KE Weasel Pit Sample Results DSC - joules/g settled sludge

o

V

222S and PNL

NA.NA

E-55

WHC-SP-1182

KE Main Basin Sample Results OH demand - moles OH/g settled sludge

A2

N5 K12

0,000112 NA °NW

M13

-LI

KE Weasel Pit Sample Results OH demand - moles OH/g settled sludge

0 300254 0 0000993

NANA

E-56

WHC-SP-1182

KE Main Basin Sample Results U233 - % atom

N5 KI2

M13

-LI

B3 Ell

KE Weasel Pit Sample Results U233 - atom %

•:0 001 <0 001

O001

- O . ,001, <0 001

T20

E-57

WHC-SP-1182

KE Main Basin Sample Results U234 - atom %

N5 K12

M13

-LI

B3

KE Weasel Pit Sample Results U234 - atom %

00710 0.00680

-000775,0.00725

E-58

WHC-SP-1182

KE Main Basin Sample Results U235 - atom %

N5 K12

KE Weasel Pit Sample Results U235 - atom %

c

/ P16

.7090 r 0.7050 r

/ 017

0.6970 W^

0 7000

\

0.7040

E-59

WHC-SP-1182

KE Main Basin Sample Results U236 - atom %

MS K12

KE Weasel Pit Sample Results U236 - atom %

0 0755

017

0 0790

-OJJ760.0.0750

E-60

WHC-SP-1182

KE Main Basin Sample Results U238 - atom %

N5 K12

KE Weasel Pit Sample Results U238 - atom %

S'9.209

017

99.209

-89, 217,99.212

E-61

WHC-SP-1182

KE Main Basin Sample Results S04 - ug/mL separated liquid

N5 K12

10

KE Weasel Pit Sample Results S04 - ug/mL separated liquid

-NA.103

E-62

WHC-SP-1182

KE Main Basin Sample Results P04 - ug/mL separated liquid

F10

<6 22 <3.26

C4

A2

N5 K12

M13

LI

E l l

KE Weasel Pit Sample Results PQ4 - ug/mL separated liquid

<3.26

<3.26,

<3.26

-MA,<3.26

E-63

WHC-SP-1182

KE Main Basin Sample Results N03 - ug/mL separated liquid

N5 K12

KE Weasel Pit Sample Results N03 - ug/mL separated liquid

<1 54 0.43

Q17

T20

E-64

WHC-SP-1182

KE Main Basin Sample Results N02 - ug/mL separated liquid

09 C4

N5 K12

115

F10

!. !50 < .180

<1.870 <1 <1.180,<1.870

A2

KE Weasel Pit Sample Results N02 - ug/mL separated liquid

<1.18

_MA,<1.18

Q17

M13

-LI

E-65

WHC-SP-1182

KE Main Basin Sample Results CI - ug/mL separated liquid

N5 K12

KE Weasel Pit Sample Results CI - ug/mL separated liquid

i)489 r 0 5 8 1 ,

R18

Q17

2 304

-MA.2 242

E-66

WHC-SP-1182

KE Main Basin Sample Results F - ug/mL separated liquid

C4 N5 K12

<0.143,<0.143

<0.013

M13

-LI

KE Weasel Pit Sample Results F - ug/mL separated liquid

<0 143 r 1230 ,

JJA.0 407

E-67

WHC-SP-1182

KE Main Basin Sample Results PH

N5 K12

KE Weasel Pit Sample Results pH

7.63 r 7.83

NA.NA

E-68

WHC-SP-1182

KE Main Basin Sample Results NH3 - ug/mL separated liquid

N5 K12

M13

-LI

KE Weasel Pit Sample Results NH3 - ug/mL separated liquid

<5

V

NANA

T7.0

E-69

WHC-SP-1182

KE Main Basin Sample Results Density - g set. sludge/mL set. sludge

N5 K12

M13

-LI

& = estimated

KE Weasel Pit Sample Results Density - g set. sludge/mL set. sludge

P16

1 54

V 151

& = estimated

1 50

,.60 8,, 164

TClT

E-70

WHC-SP-1182

A P P E N D I X F

STATISTICAL ANALYSIS OF CHEMISTRY DATA

T. L. Welsh

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182 Boxplots are an effective way to view a batch of data. A boxplot shows (1) where the middle of the data (also known as the median) lies, (2) how spread out the middle is, and (3) how the tails relate to it. The box encloses the middle 50 percent of the data. The median is the vertical line inside the box; the position of this line is an indication of the symmetry of the data. Horizontal lines (called whiskers) extend from each end of the box; the left whisker goes from the box (also known as the lower hinge) to the smallest data point within 1.5 interquartile ranges, while the right whisker goes from the box (also known as the upper hinge) to the largest data point within 1.5 interquartile ranges. The box and the whiskers provide a graphical view of the distribution of the data. Any data that are further than 3 times the interquartile ranges from the box are called "outliers" and are plotted as individual points.

The data illustrated in the following boxplots are listed in either Appendix B or Appendix C depending on the units provide with each figure. A boxplot was not made for analytes which had more than half the data reported as "less than" values. Interpretations of two boxplots are as follows. The boxplot for 137Cs on page F-5 indicates that there is one "outlier" on the upper end of this data set. This "outlier" represents the data from location 0-09. The plot depicts a strong skewness toward the lower end (the right whisker is longer than the left whisker, plus the median is to the left of center).

The boxplot for 23BU on page F-8 indicates that there are no "outliers" in this data set. The distribution of the data appears to be symmetrical, i.e., there is no evidence of skewness.

F-3

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

KE Bas in Sludge Ch; ICE Bas in Sludge Charac te r i ;

CB137 CuCi/cj S e t t Am241 CuCi /g 6

KE Bas in Sludge Ch; KE Bas in Sludge C n a r a c t e r l ;

r 1 " ■

F-5

WHC-SP-1182

KE Bas in Sludge Charai i Sludge C h a r a c t e r i z a t

. H

Pu233 O C i / g s PuZ38 CuCI/g se t t .

KE Bas in Sludge Charact< KE Basin SIudge Cnar

Am241 CuCi /g s e t t ■ I udge j - AEA

F-6

WHC-SP-1182

KE Basin SIuage Char; KE Basin Sludge Characteri:

r H

Sr90 CuCl /g ; phosphoresce i

i Sludge C h a r a c t e r i z a t i

h —1 ■\— 1

F-7

WHC-SP-1182

KE Bas in Sludge Char^

t H H

U335 Cotom %)

i S ludge Charac te r I; i Sludge C h a r a c t e r i .

r H

U238 Cotom SQ

F-8

WHC-SP-1182

KE Basin Sludge Characterizai KE Basin Sludge Characterizat.

r — |

KE Basin Sludge Characteri; KE Basin Sludge Characti

h — 1

F-9

WHC-SP-1182

KE B a s m Sludge Ch; i Sludge Char;

h 1 1

Copper Cug/g sei

KE Bas in Sludge Charact*

h —1

tenganese Cug/g

F-10

WHC-SP-1182

KE Basin Sludge Char act* KE Basin Sludge Characteri;

' h H ■ ■

Lead Cug/g sett

KE Basin Sludge Chi KE Basin Sludge Char;

F - l l

WHC-SP-1182

KE Basin Sludge Characterizatu KE Basin Sludge Characteri

Boron Cug^Q '

KE Basin Sludge Characterizatic

F-12

WHC-SP-1182

KE Basin Sludge Charac KE Basin Sludge Characterizatit

h H

TOC Cug/g sett Total Carbon £ug/g :

KE Basin Sludge Character I KE Basin Sludge Characterization

CoBO CuCI/g c fuged sIudge)

F-13

WHC-SP-1182

KE Bas in Sludge C h a r a c t e r i KE Basin Sludge Charact .

■ h H h 1-

Eu155 C^Ci /g t i f u g e d s Iudge }

KE Bas in SIudge C h a r a c t e r i ; KE Bas in Sludge Charai

F-14

WHC-SP-1182

KE Basin Sludge Charai KE Basin Sludge Characterizati<

h .

Chloride Qug/mL decantj

KE Basin Sludge Charai

■ h- 1 "

F-15

WHC-SP-1182

This page intentionally l e f t blank.

F-16

WHC-SP-1182 ANALYTICAL VARIABILITY

Random Analytical Variability The sampling and analysis plan called for duplicate analyses in order to estimate the random analytical variability. The duplicate data are presented in Miller 1996 and Silvers 1995 A one-way analysis of variance was computed for each analyte that had two or more duplicate analyses The one-way analysis of variance used the following model;

where X u is the analyte of interest (e.g., 137Cs or Al), // represents the population mean concentration, S, represents the different samples, and e~, represents the duplicate analyses performed by the laboratory The analysis of variance computation provides the variance estimate (6\) for each analytical method. The relative standard deviation (RSD) was then calculated using the following formula

v ^ RSD(%) = -L^i x 100 , where X = overall mean X

The random analytical variability estimate for each analyte is provided in Table Fl. In addition to the RSDs, the number of samples with duplicate measurements used in computing the variability estimate (i.e., the degrees of freedom associated with the variability estimate) is listed in Table Fl. Systematic Analytical Variability The systematic analytical variability is estimated from the analysis of laboratory standards or from the analysis of spiked samples The laboratory standard results and the spiked samples results are reported as percent recovery values using the following formulas

Percent Recovery (Laboratory standard) = x 100 known value

„ „ „ ,„ , , , N (Spiked sample result - sample result) 1 n n Percent Recovery (Spiked sample) = ±-£ - x 100

known spike amount

The systematic analytical var iab i l i t y (RSD) is estimated by the larger of either (1) the deviation of the mean percent recovery from 100 or (2) the standard deviation of the percent recovery values for the analyte of interest divided by the square root of n (the number of percent recovery values for the analyte of interest)

F-17

WHC-SP-1182 The estimates of the systematic analytical variability based on both the laboratory standards percent recovery and the spiked samples percent recovery are provided in Table Fl. The number of spike analyses performed and the number of laboratory standards analyzed is also listed in Table Fl. These systematic analytical variability estimates do NOT include any of the uncertainties associated with any of the steps prior to the actual laboratory (222-S or PNNL) analysis of the samples.

Table Fl. Random and Systematic Analytical Variability Estimates.

Analyte

PH OH demand NH, CN" TC TIC TOC so,2" CI" NO," NO," F' PO,3"

Random Variability Estimated from the duplicate sample

results

N * 6 6 NA NA 16 14 14 10 10 NA 4 3 NA

RSD (%) 0.1 9.2 NA NA 4.8 12.5 10.1 1.6 13.8 NA 6.7 1.5 NA

Systematic Variability Estimated from Spike Analyses

N $ NA NA 4 4 NA 6 6 2 2 2 2 2 2

RSD (%) NA NA

4.47 11.9 NA 2.3 9.8 3.45 2.25 5.55 4.2 2.9 7.7

Estimated from Analysis of Laboratory Standards

N # 3 6 5 5 3 7 7 8 8 8 8 8 8

RSD (%) 0.24 2.39 2.13 5.14 11

2.49 6.54 2.55 1.71 4.6 1.26 1.11 4.3

*: The number of samples which had duplicate analytical results from which the random analytical variability (RSD) was estimated.

$: The number of spike analyses performed from which the systematic analytical variability (RSD) was estimated.

#: The number of standard analyses performed from which the systematic analytical variability (RSD) was estimated.

NA: Not available. The analytical results were "less than" values; random variability cannot be computed. No spike analyses were performed; systematic variability cannot be computed. No laboratory standards exist for that analyte; systematic variability cannot be computed.

F-18

WHC-SP-1182 Table Fl. Random and Systematic Analytical

Variability Estimates. (Continued)

Analyte

DSC-222S TGA-222S Alpha Total Total Beta 137Cs 60Co 154Eu 155Eu 241Am - GEA 239/240pu

241 Am - AEA 237Np 90Sr U-222S phosphorescence U-PNL fluorescence U-222S ICP

Random Variability Estimated from the duplicate sample

results

N * NA NA 11 11 11 11 10 7 10 11 11 3 11 6

11

8

RSD (56) NA NA 4.3 1.6 1.6 2 5.3 10.2 5.0 7.8 1.4 19.3 5 4.2

9.5

0.8

Systematic Variability Estimated from Spike Analyses

N $ NA NA 2 2 NA NA NA NA NA 2 2 2 2 NA

NA

NA

RSD (%) NA NA

5.05 2.95 NA NA NA NA NA

12.9 18.4 21.8 1.8 NA

NA

NA

Estimated from Analysis of Laboratory Standards

N # 1 1 6 7 6 6 NA NA NA 7 7 7 7 3

5

7

RSD (%) 0.3 0.7 3.2 1.99 1.65 3.28 NA NA NA

4.59 13.07 25.19 1.6 0.31

3.2

2.62

*: The number of samples which had duplicate analytical results from which the random analytical variability (RSD) was estimated.

$: The number of spike analyses performed from which the systematic analytical variability (RSD) was estimated.

#: The number of standard analyses performed from which the systematic analytical variability (RSD) was estimated.

NA: Not available. The analytical results were "less than" values; random variability cannot be computed. No spike analyses were performed; systematic variability cannot be computed. No laboratory standards exist for that analyte; systematic variability cannot be computed.

F-19

WHC-SP-1182 Table Fl. Random and Systematic Analytical

Variability Estimates. (Continued)

Analyte

234U 235U 236U 238U Al Fe Ag B Ba Be Ca Cd Cr Cu K Mg Mn Na

Random Variability Estimated from the duplicate sample

results

N * 11 11 11 11 9 9 NA 5 7 7 8 8 8 8 4 8 8 8

RSD (56) 8 0.5 1.9

0.003 0.6 0.6 NA 1.2 0.5 1

0.8 3.6 1

0.6 16.0 1

0.7 1.5

Systematic Variability Estimated from Spike Analyses

N $ NA NA NA NA 2 2 2 2 2 2 2 2 2 2 2 2 2 2

RSD (%) NA NA NA NA

2.25 25.85 12.45 1.65 1.25 1

4.45 1.75 0.5 0.8 6.6 3.5 4.3 4.75

Estimated from Analysis of Laboratory Standards

N # 5 5 5 5 5 4 4 4 4 4 4 4 4 4 6 4 4 4

RSD (%) 4.9 0.22 0.078 0.0027 1.66 2.1 0.43 0.79 0.59 3.03 1.6 0.78 1.88 1.98 0.90 1.58 0.61 0.44

*: The number of samples which had duplicate analytical results from which the random analytical variability (RSD) was estimated.

$: The number of spike analyses performed from which the systematic analytical variability (RSD) was estimated.

#: The number of standard analyses performed from which the systematic analytical variability (RSD) was estimated.

NA: Not available. The analytical results were "less than" values; random variability cannot be computed. No spike analyses were performed; systematic variability cannot be computed. No laboratory standards exist for that analyte; systematic variability cannot be computed.

F-20

WHC-SP-1182 Table Fl. Random and Systematic Analytical

Variability Estimates. (Continued)

Analyte

Pb Sm Se TI Zn Zr

Random Variability Estimated from the duplicate sample

results

N * 8 NA NA NA 8 8

RSD (56) 3.9 NA NA NA 0.9 0.8

Systematic Variability Estimated from Spike Analyses

N $ 2 2 2 2 2 2

RSD (56) 1.3 3.5 1.40 4.25 1.95 3.7

Estimated from Analysis of Laboratory Standards

N # 4 4 7 4 4 4

RSD (56) 1.33 1.18 2.86 2.65 0.48 1.03

NA:

The number of samples which had duplicate analytical results from which the random analytical variability (RSD) was estimated. The number of spike analyses performed from which the systematic analytical variability (RSD) was estimated. The number of standard analyses performed from which the systematic analytical variability (RSD) was estimated. Not available. The analytical results were "less than" values; random variability cannot be computed. No spike analyses were performed; systematic variability cannot be computed. No laboratory standards exist for that analyte; systematic variability cannot be computed.

F-21

WHC-SP-1182

This page intentionally l e f t blank.

F-22

WHC-SP-1182 SAMPLE LOCATION PARAMETERS

The selection of the main basin sample locations was based on three parameters thought to influence the sludge characterization (see SAP for details). The three parameters are: (1) sludge depth; which had three levels, (2) fuel condition; which had two levels, and (3) canister type; which had two levels. A factorial design was employed to determine the twelve sampling locations within the main basin. A main basin location satisfying all the constraints (the appropriate level for each of the three parameters) was not available for six of the design points. Other basin locations, ensuring coverage of all three bays and the mouths of the pits (utilizing historical process knowledge), were substituted for these six sampling locations. The sampling locations along with the factorial design information are provided in Table F2.

Table F2. Sampling Locations - Factorial Design Information Location

1 2 3 4 5 6 8 9 10 11 12 15

20,21

Archived

Archived

SAP Sample Number

L-01

A-02

B-03

C-04

N-05

J-06

H-08

0-09

F-10

E-11

K-12

1-15

M-13

G-07

D-H

Factorial Design Point

(X,Y,Z)

1.2,1

1,2,2

1,2,1

1.2.2

2,1,1

2,2,2

2,2,2

3.1.1

3,2,2

1.2.1

3,2,2

3.2.2

2,1,1

1,2,1

1,2,2

Sludge Depth, in. <X)

1.3 1.5 1.0 0.5 2.6 2.5 3.7 7.5 4.6 0.9 5.6 5.6 2.7 0.7 0.5

Fuel Condition <Y>

F G F F P 0 G p F G G G P F F

Canister Type (Z)

Al/S

SS Al/S

SS Al/S

SS SS Al SS Al SS SS

Al/S

Al/S

SS

An analysis of variance (ANOVA) was performed for each variable of interest to determine if the changes in levels of the three parameters (sludge depth, fuel condition, and canister type) affect the sludge characterization results.

F-23

WHC-SP-1182 Since only six of the twelve design points were attainable, it is not possible to determine the significance of interactions between the three parameters; i.e.. are the three parameters independent?. Therefore, the statistical model used for the ANOVA is

rijk = U + «/ + Py + Yt + eljt

where Y1Jk = analyte of interest U = mean effect a, = effect of the ith level of sludge depth; i = 1 to 3 B3 = effect of the jth level of fuel condition; j = 1 to 2 Kk = effect of the kth level of canister type; k = 1 to 2 f1Jk = experimental variability.

Since replicates of some of the design points occurred, it was possible to estimate the experimental variability. Due to the heterogeneity of the sludge, it is possible that the experimental variability is quite large. If the experimental variability is large, then the statistical tests (determining whether the effects of the levels of the parameters are significant) most likely will indicate that the parameters do not affect the sludge characterization data. All statistical tests were evaluated at the 0.05 level of significance. The results of the ANOVA are listed in Table F3. Only 8 of the 44 analytes indicated at least one significant parameter effect.

Table F3. ANOVA results for the Sample Location Parameters. Analyte *

"Co

137Cs

1 M Eu

16SEu

" ' A m - GEA

Alpha Total

Total Beta a w M * ^

"8Pu

Sludge Depth

Not significant

Not significant

Not significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not significant

Fuel Condition

Not siqmficant

Not siqmficant

Not significant

Not siqmficant

Not significant

Not significant

Not significant

Siqmficant

Not significant

Canister Type

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not significant

Not significant

Not siqmficant

Not siqmficant

Not significant

Units are either //g/g as-settled sludge or //Ci/g as-settled sludge except for the uranium isotopics whose units are atom %.

F-24

WHC-SP-1182

Table F3. ANOVA results for the Sample Location Parameters. (Continued) Analyte *

J4lAm - AEA MSr

U-PNNL fluorescence

U-222S ICP 234y

2KU

23*11

:MU

Al

Ca

Cd

Cr

Cu

Fe

Mq

Mn

Na

Pb

Zn

Zr

B

8a

Be

TIC

TOC

TC

TGA-222S

TGA-PNNL

DSC-222S wet wt

DSC-PNNL wet wt

OH demand

S0„;

CI

Sludge Depth

Not s iqmf i can t

Not s ign i f i can t

Not s ign i f i can t

Not s ign i f i can t

Not s iqmf i can t

Not s iqmf i can t

Not s iqmf i can t

Not s ign i f i can t

Siqmficant

Siqmficant

Not significant

Not significant

Not significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not siqmficant

Not siqmficant

Siqmficant

Not significant

Siqmficant

Not significant

Not siqmficant

Not siqmficant

Siqmficant

Siqmficant

Not siqmficant

Not siqmficant

Not siqmficnat

Not siqmficant

Not siqmficant

Fuel Condition

Not siqmficant

Not siqmficant

Not Significant

Not significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not significant

Significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Siqmficant

Not siqmficant

Significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Canister Type

Not significant

Not siqmficant

Not significant

Not significant

Not significant

Not significant

Not siqmficant

Not siqmficant

Siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Significant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Siqmficant

Not siqmficant

Siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not siqmficant

Not significant

Not siqmficant

Not siqmficant

Significant

Not siqmficant

Not siqmficant

Units are either //g/g as-settled sludge or //Ci/g as-settled sludge except for the uranium isotopics whose units are atom %.

F-25

WHC-SP-1182 Table F3. ANOVA results for the Sample Location Parameters. (Continued)

Analyte *

CI pH Density

Sludge Depth

Not significant

Not significant

Not significant

Fuel Condition

Not significant

Not significant

Not significant

Canister Type

Not significant

Not significant

Not significant

Units are either //g/g as-settled sludge or //Ci/g as-settled sludge except for the uranium isotopics whose units are atom %.

F-26

WHC-SP-1182 Comparison of the Uranium analyses

The uranium analyses were performed using three different analytical measurement methods: phosphorescence by 222-S Laboratory, fluorescence by PNNL, and inductively coupled plasma (ICP) by 222-S Laboratory. The data, by sample location, are listed'in Table F4 and illustrated in Figure F.l. The uranium result for location 9, only analyzed using fluorescence, is quite a bit larger than all the other uranium results. To better illustrate the differences between the three analytical methods, the data have been plotted in Figure F.2 without location 9.

Table F4. Uranium Sludge Characterization Data.

Location

1

2

3

4

5

6

8

9

10

11

12 15

16

17

18 19

20 21

22 23

U (222-S) phosphorescence

j[7g/g as-settled sludge

NA

NA

4080

NA

4940

6720

1080

NA

8490

18900

NA

NA

23800

23900

8980

14300

NA

NA NA

NA

U-PNNL fluorescence

/^g/g as-settled sludge

59800

13500

12800

14000

12100

15500

1190

187000

10700

14600

6130

17100

48900

38300

10400

38000

23000

68600

18900

8700

U (222-S) ICP

Ug/g as-settled sludge

79800

16100

10900

25300

14200

17200

940

NA

9760

14800

6320

18300

56600

38700

8840

28600

NA

NA 45600

32200 NA: Not analyzed

F-27

WHC-SP-1182 To evaluate the three analytical measurement methods the differences and the relative differences (difference/mean x 100) per sample location were calculated. The differences and relative differences between the PNNL data and the 222-S Laboratory data are listed in Table F5.

Table F5. Differences between the uranium results.

Location

1

2

3

4

5

6

8

9

10

11

12

15

16

17

18

19

20

21 22 23

Difference

(PNNL-ICP)

/ / g / g as-settled sludge

-20000

-2600

1900

-11300

-2100

-1700

250

NA

940

-200

-190

-1200

-7700

-400

1560

9400

NA

NA -26700

-23500

Difference

(PNNL-222S*)

Ug/g as-settled sludge

NA

NA

8720

NA 7160

8780

110

NA

2210

-4300

NA

NA

25100

14400

1420

23700

NA

NA NA

NA

Relative $ Difference

(PNNL-ICP)

%

-28.65

-17.57

16.03 -57.51

-15.97

-10.40

23.47

NA

9.19

-1.36

-3.05

-6.78

-14.60

-1.04

16.22 28.23

NA

NA -82.79

-114.91

Relative $ Difference

(PNNL-222S* ) %

NA NA

103.32

NA

84.04

79.03

9.69

NA

23.03

-25.67

NA

NA

69.05

46.30 14.65

90.63

NA NA

NA NA

$: Difference/mean x 100 *: Phosphorescence

The average difference for (PNNL-ICP) is -4914 //g/g as-settled sludge with a standard deviation of 9851. Using a paired t-test the hypothesis that the average difference equals zero cannot be rejected at the 0.05 level of significance. Note that several of the differences are quite large. The

F-28

WHC-SP-1182 average difference for (PNNL-222S phosphorescence) is 8730 //g/g as-settled sludge with a standard deviation of 9813. Notice that (1) nine of the ten differences are positive (PNNL greater than phosphorescence) and (2) several of the differences are quite large. Using a paired t-test the hypothesis that the average difference equals zero is rejected at 0.05 level of significance. The relative differences between PNNL (fluorescence) and 222-S ICP indicate that at least three of the seventeen uranium results (locations 4, 22, and 23) are significantly different from each other based on the analytical measurement variability. The relative differences between PNNL (fluorescence) and 222-S (phosphorescence) indicate that six of the ten uranium results (locations 3, 5, 6, 16, 17, and 19) are significantly different from each other based on the analytical measurement variability.

The heterogeneity of the sludge itself along with the sampling variability may account for some of the differences.

Figure F.l. Uranium Data.

KE Basin Sludge Characterization Data Uranium (ug/g as-settled sludge)

200000

180000

160000-

140000

\120000

p 100000

o 80000-

60000

40000

20000

0

X phosphorescence n fluorescence X ICP

F-29

WHC-SP-1182

Figure F.2. Uranium Data - Edited.

KE Basin Sludge Characterization Data Uranium ( u g / g settled sludge)

80000-

70000-

60000-

50000-

40000-

30000-

20000-

10000-

0-

X

°

s s

x

° s s

a

s r-

I S

x

° s □

x

£ 1-

□

X

n

10 15 Location

X phosphorescence □ fluorescence X ICP

F-30

WHC-SP-1182

APPENDIX G

ORGANIC CHEMISTRY

D. R. Hansen T. L. Welsh

G-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182 Organic Analysis Results

Only the volatile and semi-volatile results will be discussed here. Total Organic Carbon (TOC) results are not directly comparable to the results presented here, as they are different, non-complementary techniques. Samples were analyzed for organic analytes at the Pacific Northwest National Laboratory (PNNL). Samples were also analyzed at the 222-S Laboratory for confirmation and did not include much of the supporting Quality Control (QC) data. Any results reported here are from PNNL unless otherwise stated. Any data qualifiers included with the sample results are based on the Environmental Protection Agency's Contract Lab Program (CLP). The samples consisted of sludge and decanted water samples from the K Basin along with an equipment blank and hot cell blank.

Volatile Organic Analyses (VOA): Several samples were found to contain part-per-million (ppm) amounts of

several requested analytes and are described below. The quantities found were at or below the bottom of the calibration curve, but above the method detection limits. The area between the detection limit and the lowest calibration standard has not been evaluated for linearity, limiting the usefulness of the data. Any sample results reported from this region of the curve must be treated as an estimated value and flagged with a J to indicate the value is only semi-quantitative.

Some of the compounds identified - acetone, 2-butanone, and methylene chloride were found in the hot cell blank at roughly the same concentrations as the samples, indicating that those compounds are probably contaminants introduced in the hot cell during sample preparation. These compounds were undetected in the samples analyzed at the 222-S Laboratory.

Vinyl acetate was found at trace levels (slightly above the detection limit) in the duplicate sample containing ion exchange resin beads (KES-H-08) but was not found in the original sample. Vinyl acetate is not a common contaminate, and may reasonably be attributed to breakdown of the resin. Sample inhomogeneity and trace levels may explain why it was detected in only one of the two samples. Sample inhomogeneity may also be responsible for the xylenes found at trace levels in one of two sludge samples from the Weasel Pit (KES-R-18).

Unknown compounds, referred to as Tentatively Identified Compounds (TICs), were found only in the Weasel Pit samples (KES-P-16 and KES-R-18). The TICs are compounds found in the sample that do not correspond to the requested analytes. A mass spectral library search is performed and a tentative identity may be assigned. Some partial identification may be possible, based on the mass spectra. The compound which is identified by this mass spectral library search is flagged with an "N". Any identification must be treated as tentative, however, unless a positive comparison has been made to a standard containing the compound of interest. The concentrations calculated for the TICs (see Table Gl) are based on the assumption that the response factor is equal to 1, where the response factor is defined as the ratio of the compound to the nearest internal standard. In reality, response factors can vary widely, and any concentration reported for TICs must be treated as an estimate and flagged with a J to indicate that the result is only semi-quantitative.

G-3

WHC-SP-1182 Semi-Volatile Organics Analyses:

Problems occurred during the extraction of semi-volatile compounds from the sludge samples in the hotcell and subsequent volume reduction of the extracts at PNNL. Data affected by these problems can only be used as estimates. Samples affected are KES-N-05D, KES-P-16 and -16D, KES-R-18D and -18MS, and KES-A-02D. Sludge Surrogate recoveries were uniformally poor, exceeding the upper QC limits set in the analysis method. The exceptions to this were samples KES-H-08 and -H08D, and KES-R-18, -18MS, and -18MSD. Sludge spike recoveries were also uniformally poor, with most of the spike compounds exceeding the upper QC limits set in the analysis method. The sludge QC results indicate that the sludge sample results are approximate at best.

Bis(2-ethylhexyl)phthalate was found in several of the water and sludge samples at trace amounts slightly above the detection limit. Phthalates are common environmental contaminants and may have been caused by the sampling process or the hotcell breakdown. If the samples came in contact with plastics, such as tygon tubing or polyethylene collection bottles, this may be the source of the phthalate. Due to the small sample size and the result being near the detection limit for this method, the concentrations reported for the phthalate can be treated only as estimates. The samples analyzed at 222-S Laboratory confirm the presence of bis(2-ethylhexyl)phthalate, but the concentrations can not be compared as the 222-S laboratory sample data was calculated using the TIC formula (see above volatile organics section for discussion of the calculation methodology), and not from a calibration curve for the compound.

Phenol was also found in one sample (KES-T-20) at a concentration between the detection limit and the bottom calibration point. It was not found in the duplicate analysis. This compound, however, is not a common contaminant, and since it is absent from the duplicate sample and only a trace amount found, it's presence is only surmised and not confirmed.

Tentatively Identified Compounds (TICs) (see Table G2) in the semi-volatile fraction were found only in the Weasel Pit sludge samples (KES-P-16 and KES-R-18). As described earlier in the Volatile Organics Analysis section, TIC concentrations are not accurate, but can be used only as an approximation of the actual value.

Of particular note is the identification of polychlorinated biphenols (PCBs) (Aroclor 1254) as a TIC in the Weasel Pit sludge samples. PCBs are not a common laboratory contaminant, and their presence was confirmed by independent analysis of the samples at the 222-S laboratory. The extracts were analyzed specifically for the PCB using a one point calibration, improving the quality of the reported concentration. Problems with the extraction and sample inhomogeneity, however, indicate the results can only be used as an estimate. The samples that contained PCBs at 222-S were re-extracted and analyzed using methods specific for samples containing PCBs. While this has improved the accuracy of the individual results, sample inhomogeneity still makes the accuracy of the PCB concentration in the Weasel Pit difficult to determine.

G-4

WHC-SP-1182 Summary

Samples L-01 (Basin), A-02 (Basin), N-05 (Basin), H-08 (Basin), P-16 (Weasel Pit), and R-18 (Weasel Pit) were analyzed by PNNL for volatile organic compounds and semi-volatile organic compounds. Tables Gl and G2 list the compounds detected by the PNNL organic analyses.

Samples N-05 (Basin), 1-15 (Basin), P-16 (Weasel Pit), and R-18 (Weasel Pit) were analyzed by 222-S Laboratory for volatile organic compounds and semi-volatile organic compounds. Sample L-01 (Basin) was analyzed by 222-S Laboratory for semi-volatile organic compounds only; there was insufficient sample for the volatile organic analyses. Tables G3 and G4 list the compounds detected by the 222-S Laboratory organic analyses.

G-5

WHC-SP-1182 Table Gl. Pacific Northwest National Laboratory Volatile Organic Sludge Characterization Data.

Analyte

Acetone

Toluene

Methylene Chloride

Benzene

2-Butanone

4 methyl-2-pentanone

Vinyl Acetate

Xylenes (total)

Alkanes

Sample Description

Prep Blank

Prep Blank

Basin

Basin

Ueasel Pit

Ueasel Pit

Prep Blank

Prep Blank

Prep Blank

Prep Blank

decant - Basin

decant-Ueasel Pit

decant-Ueasel Pit

Prep Blank

Prep Blank

Basin

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Basin

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Sample ID

B" Hot Cell Blank

325 Hot Cell Blank

N-05 Dup

H-08 Dup

P-16

R-18 Dup

B" Hot Cell Blank

B" Hot Cell Blank

Hot Cell Blank

Equipment Blank

M-13

T-20

T-20 Dup

B" Hot Cell Blank

325 Hot Cell Blank

H-08 Dup

P-16

R-18

R-18 Dup

R-18

H-08 Dup

R-18

P-16

P-16 Dup

R-18

R-18 Dup

Type Sludge

Hone

None

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Hone

Hone

Hone

Hone

None

None

None

None

None

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

< CRQL

< CROL

> CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

> CRQL

> CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

TICs

TICs

TICs

TICs

Flag

J

Cone

0.65

1.40

0.52

0.38

0.25

0.37

0.17

0.52

0.13

0.18

0.19

0.17

0.17

0.98

1.20

0.39

0.24

0.37

0.65

0.13

0.15

0.22

1.2 to 15

1.7 to 18

1.4 to 15

2.0 to 22

Units

ug/mL

ug/mL

ug/g

ug/g

ug/g

ug/g

ug/mL

ug/mL

ug/mL

ug/mL

ug/mL

ug/mL

ug/mL

ug/mL

ug/mL

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

CROL: Contract required quantitation limit. Cone: Concentratlon. TICs: Tentatively identified compounds.

G-6

WHC-SP-1182 Table G2.

Analyte

Phenol

Di n-butylphthalate

Bis(2-Ethylhexyl)phthalate

Unknown Alkanes

Unknown (biological origin)

1,1'Biphenyl,tetrachloro-

1,1'Biphenyl.hexachloro-

1,1'Biphenyl.pentachloro-

Aroclor 1254

Pacific Northw Organic Sludc

Sample Description

decant Ueasel Pit

Ueasel Pit

Basin

Basin

Basin

Basin

Basin

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

Ueasel Pit

est National Laboratory Semi-Volatile e Characterization Data.

Sample ID

T-20

P-16

L-01 Dup

A-02

A-02 Dup

N-05

N-05 Dup

P-16

P-16 Dup

R-18

R-18 Dup

P-16

P-16 Dup

R-18

R-18 Dup

R-18 Dup

R-18 Dup

R-18 Dup

R-18 Dup

P-16

P-16 Dup

R-18

R-18 Dup

R-18 MS

R-18 MSD

Type Sludge

Hone

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

Centrifuged

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

< CRQL

TICS

TICs

TICs

TICs

TICs

TICs

TICs

TICs

Flag

NJ NJ NJ

cone

0.76

0.70

4.20

4.60

5.30

5.30

23.0

5.00

5.60

2.00

3.50

4.0 to 8.4

1.8 to 8.9

5.9 to 6.1

3.4 to 12

6.90

5.00

4.1 to 6.4

2.8 to 5.2

19.0

18.0

23.0

86.0

76.0

53.0

Units

ug/mL

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

CRQL: Contract required quantitation limit. Cone: Concent ration. TICs: Tentatively identified compounds.

G-7

WHC-SP-1182 Table G3. 22

Analyte

Toluene

Non-ch lor inated Hydrocarbons

2-S Laboratory

Desc r ip t i on

Prep Blank

Ueasel P i t

Ueasel P i t

volat i le Ore Sample ID

Hot Cel l Blank

P-16

R-18

jamc Sludg Type Sludge

None

Centr i fuged

Centr i fuged

3 Charat < CRQL

TICs

TICs

teriz Flag

J

J

J

ation Dal Cone

24

2.2 to 16

2.1 to 19

a. Uni ts

ug/mL

ug/g

ug/g

Table G4. 222-S La Analyte

Unknown P o l y c h l o n n a t e d biphenyl (PCS)

B i s (2 -E thy lhexy l ) ph tha la te

Unknown Alkanes

3-Methyt-5-propylnonane

Aroc lo r 1254 (gas chromatograpn / e l e c t r o n capture)

boratory Semi-Volatile Sample

Desc r i p t i on

Ueasel P i t

Ueasel P i t

Basin

Ueasel P i t

Ueasel P i t

Ueasel P i t

Ueasel P i t

Basin

Basin

Ueasel P i t

Ueasel P i t

Sample ID

P-16

R-16

1-15

P-16

R-18

P-16

R-18

1-15

1-15

P-16

R-18

Organic Sludge Characterization Type Sludge

Centr i fuged

Centr i fuged

Centr i fuged

Centr i fuged

Cent r i fuged

Centr i fuged

Centr i fuged

Centr i fuged

Centr i fuged

Cent r i fuged

Centr i fuged

< CRQL

TICs

TICs

TICs

Flag

J

J

NJ

NJ

NJ

J

J

NJ

cone

2

12

91

16

6

10 t o 21

8 to 17

9

104

47.4

220

Data. u n i t s

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

ug/g

CRQL: Contract required quantitation limit. Cone- Concentration TICs: Tentatively identified compounds.

G-8

WHC-SP-1182

A P P E N D I X H

SUMMARY OF POLYCHLORINATED BIPHENYL RESULTS

B. J. Makenas

H-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

APPENDIX H SUMMARY OF POLYCHLORINATED BIPHENYL RESULTS

Polychlorinated biphenyls (PCBs) have been identified in sludge samples taken from K East Basin during the August/September 1995 sampling campaign. Twenty sludge samples were obtained and a minority of these received semi-volatile organic analysis (SVOA) for target and tentatively identified compounds at either 222-S or 325 Building laboratories. Figure HI indicates locations in the basin where all 20 samples were taken and which samples tested positive for PCBs. Table HI indicates which of the 20 samples were actually analyzed for semi-volatile organics, which laboratory performed the analyses, and the PCB levels reported.

In addition to analyses performed on actual sludge some analyses were performed on related water samples. These included a sample of basin water (run through the sampling equipment), a sample of water run only through laboratory equipment, and two samples of water which had been in intimate contact with sludge samples. None of these showed evidence of PCBs, thus, suggesting that neither the sampling equipment, basin water, or laboratories introduced the PCBs.

Analyses done at 325 laboratory were performed by Gas Chromatography/Mass Spectrometry (GC/MS). At 222-S laboratory samples were first analyzed by a Gas Chromatography/Flame Ionization Detector (GC/FID) as a screening tool. Those which tested positive for semi-volatile organics were quantitatively analyzed by GC/MS and ultimately by Electron Capture (EC). Both laboratories have expressed the opinion that the latter technique is the most accurate and accepted, given the procedures used in this case. It should be noted that all of the techniques used here assess only those compounds which can be extracted from the sludge by organic solvents. Also the sample preparation and analysis procedures were initially targeted toward other non-PCB compounds so that specific values of PCB concentration may be biased and should be used with caution. The particular PCB identified by both laboratories is Aroclor 1254.

H-3

Polychlorinated Biphenyls in K East Floor Sludge Samples

Sludge Samples

KES-L-1

KES-A-2 KES-B-3

KES-C-4 KES-N-5

KES-J-6 KES-G-7

KES-H-8 KES-O-9 KES-F-10

KES-E-11 KES-K-12 KES-D-14

KES-I-1S KES-P-16 KES-Q-17

KES-R-18 KES-S-19

KES-M-13 KES-T-20

Basin Water

Hot Cell Blank

Analyzed for Semi-Volallle

Organics? (Where?)

222-S/325

325 N/A N/A

222-S/325 N/A N/A

325 N/A N/A

N/A

N/A N/A

222-S

222-S/325 N/A

222-S/325 N/A

222-S/325 222-S/325

222-S/325

222-S/325

SVOAs Indicated

by GC/FID Screening

(222S) No

No

Yes

Yes

Yes

No No

No

No

PCBs Found by GC Mass

(222S)

None

2 ppm

12 ppm

PCBs Confirmed by Electron

Capture (222S)

104 ppm 47 ppm

220 ppm

PCBs Found by GC Mass

(325)'

None

None

None

None

18 to 19 ppm

23 to 86 ppm

None

None

None

None

N/A = Sample not analyzed lor Semi-Volatile Organic Compounds. *ppm = Micro grams per gram

KES-H-13 No PCBa Found a.^

KES-I-15X PCBs FoundN

KES-A-2' Ho PCBS Found

|I

" - I

"-"SKSE""*

WHC-SP-1182

A P P E N D I X I

VISCOSITY, PARTICLE SIZE, AND ZETA POTENTIAL

G. R. Golcar

1-1

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

APPENDIX I VISCOSITY, PARTICLE SIZE, AND ZETA POTENTIAL

1.1 INTRODUCTION The two K Basins at the Hanford site are water-filled concrete pools that

contain over 2,000 tons of N Reactor metal fuel elements stored in aluminum or stainless steel canisters. In addition to the Spent Nuclear Fuel (SNF) stored in the K Basins, a sedimented particle layer (sludge) has accumulated on the Main Basin and Weasel Pit floors. The sludge is a nonhomogeneous mixture of fuel elements and canister corrosion products, storage rack corrosion products, and windblown debris such as sand and insects. It is planned that the sludge be removed from the K Basins and then disposed of safely.

During the first quarter of FY 1996, physical, radiochemical, and organic analyses of sludge samples obtained from the K East Main Basin floor and Weasel Pit were performed by the staff from the Pacific Northwest National Laboratory (PNNL) 325 Building Analytical Chemistry Laboratory (ACL), 325 Building Chemical Process Technology (CPT), and Material and Chemical Research Section. In this appendix, the measured properties of viscosity, particle size distribution, and the zeta potential (Silvers 1995) are evaluated based on their influence on the specification, design, and performance of the candidate sludge removal and dewatering systems.*

The conclusions drawn from the characterization data and the recommendations for the on-going K East Main Basin and Weasel Pit sludge characterization activities are presented in Section 1.2 of this appendix. Section 1.3 includes background information about the prospective engineering systems for the cleaning of the K East Basin floor to remove the sludge and the approach used to develop waste simulants in cases where the scaled testing with actual radioactive basin material is not possible. The analytical results and their relation to the engineering system processes are explained in Section 1.4. Also, the terminologies used to assess these analytical results are explained in Section 1.4.

1.2 CONCLUSIONS AND RECOMMENDATIONS • The rheological measurements (in this case viscosity and shear

stress) of the "as received" samples from the K East Main Basin and the Weasel Pit show that the resuspended slurry has a low viscosity.

♦The removal and processing of the sludge from the basin floor may require resuspension/mobilization and pumping to the Weasel Pit followed by decreasing the sludge water content using a filtration and/or hydrocyclones systems.

1-3

WHC-SP-1182

• An effort to obtain the rheological measurements (shear strength, viscoelastic moduli) on the centrifuged solids was not successful, because only a small amount of solids was deposited at the bottom of the centrifuge tube cell after the "as-received" samples were centrifuged.

• The particle size distribution of the "as-received" sludge was measured and was compared to the particle size distribution of the same samples after being subjected to ultrasonication. The results are compared in Figures 14 to 17. The data show that under shearing conditions the particle cluster will break into a large number of fine particles smaller than 1 micron. The use of mechanical dewatering systems such as hydroclones should be reviewed with the propensity toward smaller particles in mind.

• The zeta potential measurements indicate that the isoelectric point for all the samples is reached at pH less than about 5. Therefore, for engineering purposes the optimal flocculation can not be achieved unless the basin's pH is adjusted to less than 5, which is impractical.

• The zeta potential measurements show that within the pH range of the interest (pH 7 to pH 10) the particles are negatively charged. In all cases, the value of the zeta potential does not decrease below -30 mV. If it is assumed that the surfaces of the particles are coated with ions of three or higher electron valency, these zeta potential values indicate that the solid particles are not electrically stable and floe formation is favorable.

1.3 BACKGROUND This section describes the prospective engineering systems for cleaning

the sludge from the Basin floor and Weasel Pit, as well as the approach used to design waste (i.e., sludge) simulants for scaled testing in cases where actual radioactive basin material cannot be used.

1.3.1 K East Floor Sludge Removal and De-Watering System Description To remove the sludge from the basin floor, the various cleaning steps of

retrieval and dewatering, and the water treatment systems need to be determined. Currently, it is assumed that the accumulated bulk sludge layer is a loosely packed suspension that can be easily drawn into a pipe by a centrifugal or diaphragm pump. The generated slurry will be transported through a pipe up to 61 m (200 ft) long, followed by a slurry settling step in the Weasel Pit. Depending on the settling rate, the settling process may need to be modified by mechanical means such as hydrocyclone systems or by the addition of a flocculating agent. In addition, the water may require further filtration treatment to remove the remaining fine particulates in the water stream. With these processes in mind, a list of the relevant physical and rheological properties of the sludge was prepared during FY 1995 to support

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the planned characterization activities. These properties were (1) particle size distribution, (2) particle mean density, (3) supernate viscosity, (4) compacted sludge shear strength and viscoelasticity, and (5) the suspension zeta potential and electrical conductivity. It should be noted again that the process of mobilizing the sludge is not being considered in the current plans, since it is assumed that the sludge is loosely packed.

1.3.2 Simulant Development Methodology A comprehensive simulant development strategy for retrieval and transport

technologies testing has been already developed (Golcar, Powell 1994). This reference describes the methodology used to design and develop waste simulants that take into account the relevant properties for the technology under development. The strategy also addresses how these simulants are validated through their interdependencies with waste characterization activities. Currently, non-hazardous waste simulants are being used to develop and demonstrate waste mobilization, pumping, transport, and settling system designs. These simulants are used because of the hazards and expense of testing these technologies using actual waste. For such tests, the applicability of the data that are generated to actual tank waste or other wastes (K Basin sludge) depends largely on the ability of the simulants to model the specific types of chemical or physical behavior of actual waste. Therefore, it is essential that accurate and scientifically-defensible waste simulants be used during testing. Since, it is not practical to develop simulants that duplicate all of the physical and rheological properties that influence each of the steps in the retrieval process, simulated wastes need to be developed to cover the expected range of critical physical, rheological, and/or chemical properties. Further, the simulants should bound the specific governing waste (i.e., K Basin sludge) properties that influence the performance of critical steps for a particular technology.

This simulant development methodology and its interdependencies with waste characterization activities are presented in a logic diagram shown in Figure II. In this figure, a critical path is outlined that is based on the most probable outcome of the prior steps. The decision points and rationale for making the decisions are included as part of this methodology, which consists of three main areas. These are described in the following paragraphs:

Establish Hypothetical Process Correlations. Many of the physical properties of wastes that are important for the development and demonstration of the retrieval technologies have not been well characterized. In addition, it is not necessary to use a simulant that mimics the full range of properties of a radioactive waste. The development of waste simulants appropriate for the testing of a discrete process only have to reflect the specific influence of the relevant waste properties on the process performance. The most logical path for designing simulants with the appropriate range of resistances to a retrieval and transport system, is to determine (1) the effect of waste properties on process performance and (2) to correlate the important process performance measures with key physical and rheological properties of the waste.

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Provide Characterization Data Needs. Once a specific process performance measure is correlated with the key waste properties, thereby establishing the process sensitivity to the key waste properties, the characterization data needs and the required measurement accuracies will be communicated to the waste characterization groups and laboratories through the Data Quality Objectives (DQO) process.

Simulant Performance Validation. Actual waste data for each of the key waste properties are needed to establish confidence in simulant performance. Once the actual waste data for the specific key properties have been provided, simulant performance can be validated.

1.4 PHYSICAL AND RHEOLOGICAL CHARACTERIZATION The physical and rheological measurements were performed on sludge

samples from the K East Main Basin floor and the Weasel Pit floor. These samples were designated as:

• KES-M-13 (Top); a subsample from the top strata of the K East Main Basin sludge

• KES-M-13 (Bottom); a subsample from the bottom strata of the K East Main Basin sludge

• KES-T-20 (Top); a subsample from the top strata of the K East Weasel Pit sludge

• KES-T-20 (Bottom); a subsample from the bottom strata of the K East Weasel Pit sludge.

In this section the measured constant shear rate-controlled viscosity, stress sweep oscillation, particle size analyses, and zeta potential of the samples are discussed.

1.4.1 Rheological Measurement The rheology of a suspension is primarily controlled by the effective

volume fraction of solid particles in the fluid. At one extreme, a dilute suspension behaves as a "liquid like" system, whereas a highly concentrated suspension acts as a "solid like" system. Therefore, the degree of importance of various rheological properties—viscosity, shear strength, yield point and viscoelastic moduli—predicting the flow behavior of a suspension system need to be determined. The practical concentration above which a suspension is considered concentrated is typically defined by the balance between the translational motion and the interparticle interactions. For instance, in a dilute suspension, the thermal motion of particles predominate and the particles do not "see" each other until collision occurs. The flow behavior of such system is typically time-independent and a time-averaged viscosity can be used. As the particle concentration is increased, the volume fraction of space occupied by the particles increases. When the volume fraction solids grows larger than 0.01, the particles increasingly enter the neighborhood of

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other particles, and the force of interaction between the particles plays a predominant role in determining the rheological properties of the system. In this regime, the increase in the particle volume fraction does not simply change the magnitude of the viscosity, it also can introduce deviations from Newtonian behavior (e.g., shear thinning, pseudoplasticity, shear thickening) that typically cause the viscosity to grow at an increasing rate with concentration. With further increase in particle concentration, the interactive contact between the particles increases until a situation is reached where a highly ordered structure is achieved. At this point, it is referred to as a "solid" suspension. In this case, the viscosity of the system has increased drastically and has reached infinity. At higher solid concentrations, the rheological properties are characterized by the shear strength, and the viscoelastic moduli rather than suspension viscosity.

In a highly concentrated sludge suspension, the particle movement is restricted to vibration within a small distance relative to the particle size and the suspension may behave anywhere from a highly viscous fluid to an ideal elastic solid. If the concentrated suspension is a viscous material, its rheological behavior is characterized by the viscous flow properties like viscosity, yield point, shear strength, thixotropy or pseudoplasticity. In general, a sludge sample will deform permanently if the magnitude of an applied stress exceeds the sludge yield strength. When the stress is removed, an ideal viscous material will remain fully deformed, while an ideal elastic material will return to its initial shape. However, viscoelastic suspensions are materials that behave neither as perfect elastic solids, nor as perfect viscous liquids. For viscoelastic materials, the stress may depend on both the strain and the rate of strain, as well as higher derivatives of the strain. Such time related anomalies reflect both solid-like and liquid-like behaviors.

Viscoelastic properties of materials can be determined by several experimental approaches. The "strain sweep" and the "frequency sweep" techniques are the most common experimental procedures. Viscoelastic properties determined by periodic loading patterns are characterized by the storage modulus (G'), the loss modulus (G"), the complex modulus (G*), and the loss tangent. The storage modulus (with units of Pa) is a measure of the energy stored and recovered per cycle of applied stress, and is defined as the stress in phase with the strain (in a sinusoidal deformation) divided by the strain. The loss modulus (with units of Pa) is a measure of the energy dissipated or lost as heat per cycle of sinusoidal deformation, and is defined as the stress ninety degrees out of phase with the strain (in a sinusoidal deformation) divided by the strain. In other words the storage modulus is a measure of the elastic or solid-like property of the sample that is often related to its cohesion. The loss modulus is a representation of the viscous or liquid like property of the sample. The loss tangent, which is dimensionless, is a measure of the ratio of the energy lost to the energy stored in a periodic deformation; it quantifies the relative importance of the

*This limit can be even lower for thin, platelike or long, rodlike particles.

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elastic and viscous characteristics of a sample. For example, when the loss tangent is much greater than 1.0, the sample is more viscous than elastic. When the loss tangent is much less than 1.0, the sample is more elastic than viscous. Experimental Results

In these analyses a Bolin CS rheometer was used. Since the effective volume fraction of solid particles in the "as-received" samples was low, the samples behave as a "liquid like" suspension. The flow behavior of samples KES-M-13 (Top) and KES-T-20 (Top) were determined by controlled rate viscosity measurements.

Figure 12 shows the viscosity and the shear stress plots as a function of shear rate for the Main Basin "Top" strata (KES-M-13) sample. The plot of viscosity as a function of shear rate indicates that the viscosity decreases over time as the shear rate increases, which represents a pseudoplastic flow behavior that is typically observed for dilute suspensions. Where, the decreasing viscosity with increasing shear rate can be caused by the breaking of a flocculated suspension or a change in the average solid particle orientation relative to the flow direction. Further, the yield strength of this sample is about 2.2 Pa, which demonstrates that the sample begins to flow when a shearing force greater that 2.2 Pa is applied.

Figure 13 shows the viscosity and the shear stress plots as a function of shear rate for the Weasel Pit "Top" strata (KES-T-20) sample. The plot shows the same type of flow characteristics (pseudoplastic flow) with a yield strength of about 0.9 Pa. In addition, the viscosity of the sample from the Weasel Pit decreases faster than the sample from the Main Basin floor, which can be caused by the lower effective volume of the solids in this Weasel Pit sample. These results on the "Top" portions show that the "as-received" sludge samples were of relatively low viscosity and that any additional viscosity measurements as function of dilution would not have provided further information on rheological properties of the samples.

The rheological measurements were not performed on the "Bottom" strata samples from either the Main Basin or the Weasel Pit. There was not enough sample available to perform rheological measurements on the "Bottom" strata sample taken from the Main Basin floor. In addition, a significant fraction of the bottom layer sample from the Weasel Pit was comprised of ion exchange resin beads. These are larger than 700 microns which was approximately the same size as the gap spacing used for cone and plate measuring sensor in the viscosity measurement equipment, making it impossible to make measurements. Also, the viscosity of these samples could not be measured by using a concentric cylinder measuring sensor, since the beads were fractured as the shear rate was increased. Future rheological characterization of bottom sludge strata may be required.

As indicated before, various sludge dewatering processes are being evaluated. Therefore, the rheological behavior of the available samples at high solid particle concentrations needed to be measured. To bound the rheological characteristics of these samples, it was planned that the "as-received" samples be centrifuged and the rheological measurements be

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performed on the centrifuged solids. Then the centrifuged samples were planned to be diluted and its flow properties measured. But, the effort to obtain the rheological measurements (shear strength, viscoelastic moduli) on the centrifuged solids was not successful, because only a small amount of solids was deposited at the bottom of the centrifuge tube cell after the samples were centrifuged. Therefore, future rheological characterization on concentrated sludge samples may need to be performed.

1.4.2 Particle Size Distribution Measurement One of the most important characteristics for both dilute and highly

concentrated suspensions is the particle size distribution (PSD). The PSD provides an indication of the relative importance of colloidal interactions and body-force interactions between particles. The behavior of small (submicron) particles is controlled primarily by surface chemistry and van der Waals attractions between particles. Much larger particles are effectively immune to these colloidal forces and are instead controlled by inertia! and frictional forces. The behavior of wet sand, for example, is much different from that of wet clay. This difference is due primarily to the dominating colloidal effects manifested in the clay that are absent in the sand.

In general, the PSD alone is not usually sufficient to determine the relative importance of colloidal and body-force effects, since the PSD does not take particle shape into account. For instance, the fact that clays tend to be composed of platelike particles, rather than spherical particles of the same volume, increases the relative importance of the colloidal effects in clays.

Experimental Results The histograms of PSD number density and PSD volume density analyses

for the K East Main Basin floor and Weasel Pit samples are presented in (Silvers 1995). Usually in a suspension that contains many different sizes of particles, such as the K East Main Basin floor and Weasel Pit sludge, there is a large difference between the by-volume and by-number size distributions. The PSD by number distribution statistics are computed by weighing all the particles equally. The PSD by volume distribution, however, is weighted by the volume of each particle measured, which is proportional to the cube of the particle diameter. In this case, the bigger particles are treated as more important than the smaller particles. Therefore, the PSD by volume distribution gives information about how the volume and the mass (assuming uniform density) is distributed among sizes. The PSD by number distribution provides information about the population of particles found in each size range.

In these experiments, the Leeds and Nortrup Microtrac X100 particle size analyzer was used. This device can measure particle mixtures between 0.12 to 704 microns. The analyzer works by analyzing the light scattered by the particles. The amount and direction of the light scattered by the particles is measured by an optical detector array.

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K East Main Basin Sludge—Samples M13 (TOD) and M13 (Bottom!. The particle number distribution and the particle volume distribution histograms for the K East Main Basin samples M13 (Top) and M13 (Bottom), documented in (Silvers 1995), were reviewed and are summarized in Figures I4a and I4b for sample M13 (Top), and Figures I5a and I5b for sample M13 (Bottom). The particle number distribution shown in Figures I4a and I5a indicates that about 80% of the particles are smaller than 1.0 micron. Also, the PSDs of these samples were obtained after sequential ultrasonication for: (1) 120 s at 25 W, and (2) 300 s at 40 W. These results are presented along with the "as-received" PSDs in Figures I4a, I4b, I5a, and I5b. The data indicate that agglomerates were originally present in the samples as evidenced by an increase in the number of smaller particles after ultrasonication. The presence of the agglomerates was further verified by the TEM results presented in Appendix J.

K East Weasel Pit Sludge—Samples T20 (TODI and T20 (Bottoml. The particle number distribution and the particle volume distribution histograms for the Weasel Pit samples [T20 (Top) and T20 (Bottom)] documented in (Silvers 1995), were reviewed and are summarized in Figures I6a and I6b for sample T20 (Top), and Figures I7a and I7b for sample T20 (Bottom). These samples were also ultrasonicated for 120 s at 25 W, and 300 s at 40 W. The resulting particle number distribution and particle volume distribution histograms were compared with the original PSDs in Figures I6a, I6b, I7a, and I7b. The drastic increase of the small particle population as the result of ultrasonication is seen in the particle number distribution histogram. These data indicate that agglomerates are also present in the Weasel Pit.

The particle volume distribution histograms for the cases after ultrasonication cases—presented in Figures I4a , I4b, I5a, I5b, I6a, I6b, I7a, and I7b—reveal a bimodal distribution that may indicate that the agglomerates are typically larger than 10 microns.

1.4.3 Zeta Potential Measurement A property known as zeta potential can have a major effect on the

behavior of suspension systems composed of fine solid particles where the solid particles are (1) roughly less than 10 /on and (2) the magnitude of the surface forces acting on the particles dominate the body/bulk forces. The zeta potential is the effective electrostatic charge at the shearing or slipping plane between the bulk liquid and the envelope of liquid (i.e., water) that moves with the particle. The actual charge on the surface is different from the zeta potential, but, to some extent, the zeta potential is comparable to the surface potential. One of the ways for particles to obtain a charge in a suspension is from the transfer of ions between the particle and the aqueous phase. The ions with the opposite charge to that of the particle will be pulled toward the particle surface and create a layer of charge near surface. The zeta potential is one of the few measurable properties that play a role in assessing the electrostatic double layer characteristics.

The zeta potential provides a measure of the strength of the repulsive forces between the particles. A strongly positive or negative zeta potential indicates that the repulsive forces between particles are strong. If the

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repulsive forces are strong enough to overcome the interparticle attractive forces (van der Waals and London dispersion forces) then the particles will remain segregated from each other. Alternatively, if the attractive forces between the particles dominate then the particles will tend to aggregate and form larger particles. Depending on the conditions of the suspension (i.e., the salt concentration in the liquid phase, the type of salt, the particle size distribution and particle shapes, etc.), there can be a particle-to-particle distance at which the attractive forces and electrostatic repulsive forces balance such that the particles have a tendency to form loosely aggregated clumps known as floe. This process is called flocculation.

In dealing with the complex suspension that will be formed during the K East Main Basin and the Weasel Pit sludge resuspension/mobilization, the separation mechanism of fine solid particles from the slurry can potentially be improved by the "floe" formation process, and it is desired to maximize the flocculation process. In this context the concept of zeta potential arises as a valuable measurement. The larger the zeta potential (with + or - ) , the more stable will be the suspension. As zeta potential approaches zero, the suspension is less stable and will tend to flocculate. At the isoelectric point the zeta potential is zero, and the potential energy of repulsion between the particles is minimum. By measuring the zeta potential as a function of pH the relative stability of the suspension with respect to flocculation can be evaluated.

Experimental Results K East Main Basin Sludge—Samples M13 (TQDI and M13 (Bottom!. The zeta potential values for samples M13 (Top) and M13 (Bottom) and their duplicated values, under measured pH, are presented in Figure I8a. The results shows that over the pH range of 3.8 to 10.6, the zeta potential for the sample M13 (Top) changes from about +5 to -30 mV, and the zeta potential for the sample M13 (Bottom) varies from roughly +30 to -27 mV. As the pH increases, both zeta potentials move through their isoelectric points and become negatively charged. The isoelectric points for sample M13 (Top) and M13 (Bottom) are reached at about a pH of 4.2 and 5.2 respectively. From pH 7 to pH 10.6 the surface of particles of samples M13 (Top) and M13 (Bottom) are negatively charged and the zeta potential varies from -15 to -30 mV.

K East Weasel Pit Sludge—Samples T20 (Top) and T20 (Bottom!. The zeta potential measurement for the samples T20 (Top) and T20 (Bottom) and their repeated values as a function of pH are shown in Figure I8b. All the samples exhibit the same trend with respect to pH change, where, at a selected pH, the difference in the zeta potential results between the samples [T20 (Top), T20 (Top) Duplicate, T20 (Bottom), and T20 (Bottom) Duplicate] are very small. These graphs indicate that over the entire pH range, from 3.5 to 11, the surface of the particles is negatively charged, and the zeta potential varies from approximately -7 mV at pH 3.5 to -27 mV at pH 11. It is expected that the isoelectric point will be around pH 2.

The results presented in Figures I8a and I8b reveal that over the pH range of interest, from pH 7 to pH 11, the surface of the particles are negatively charged, and pH manipulation over this range is unlikely to significantly affect the sedimentation rate.

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Figure II. Simulant Development Strategy.

Literature

Existing Pilot Scale and Application Status

Existing Actual Waste Data

Design Analytical Techniques and Test Apparatus

I 1 Establish Hypothetical Process Correlations

^— Provide Recommended Waste ■■■■■■■ Characterization Data Needs

I 1 Validate Simulant Performance

NO

Process

Refine Simulants

1 Performance Testing

with Simulants

yPredictionsX ^Accurate/

j YES

Establish Confidence in Simulants

New Waste Characterization Data

^ Standard Sets of Simulants for Testing

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Figure 12. K East Main Basin Sludge—Sample M13 (Top).

Viscosity

~ T , , 200 300 Shear Rate (1/s)

400 500

Yield / t Point/ '

100 200 300 400 500 Shear Rate (1/s)

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Figure 13. K East Weasel Pit Sludge—Sample T20 (Top).

0.2

0.15 -

0.1

0.05

0 100 200 300 400 500 Shear Rate (1/s)

2.5 -

1.5

Yield Point 0.5

shear stress

100 200 300 Shear Rate (1/s)

400 500

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Figure I4a. Particle Size for Sample M13 (Top).

50 00

45 00

40 00

35 00

Si 30 00

oc 25 00

SS 20 00

15 00

10 00

5 00

0 00

Particle Number Distribution of M13T

D As Received

025 Watts

■ 40 Watts

±L § 2

Particle Diameter (urn)

Particle Volume Distribution of M13T 10 00

9 00

8 00

7 00

gsoo

CCS 00

* 4 00

3 00

2 00

1 00

0 00

D As Received

B 25 Watts

■ 40 Watts

Particle Diameter (um)

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Figure I4b. Duplicate Particle Size Data for Sample M13 (Top).

Particle Number Distribution of M13T Duplicate

50 00

45 00

40 00

35 00

a 30 00

C 25 00

J 20 00 15 00

10 00

5 00

0 00

O As Received

B25 Watts

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c w m t n o o i Q c o o o Q O r - h - ^ w e o o K - o i o O T -a i w o > N e o w r » o w o * -o * - T - c \ i e * > w r * i - t o c \ i ' -

Partlcle Diameter (um)

Particle Volume Distribution of M13T Duplicate

10 00 9 00 8 00 7 00

Si 6 00 S 5 00 5 4 00

3 00 2 00 1 00 0 00

□ As Received

H25 Watts

■ 40 Watts

Particle Diameter (um)

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Figure I5a. Particle Size Distribution for Sample M13 (Bottom).

Particle Number Distribution of M13B

50 00

45 00

40 00

35 00

Si 30 00

a 25 00

5 20 00 15 00

10 00

5 00

0 00

□ As Received "B25 Watts - ■ 40 Watts

JLJUU

8 2 o . - . - c \ i P ) w r ~ Y - w c v i * -

Particle Diameter (urn)

Particle Volume Distribution of M13B

10 00

9 00

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Si 6 00

£ 5 00

J 4 00 3 00

2 00

1 00

0 00

□ As Received B25 Watts ■ 40 Watts

J L i l M i

Particle Diameter (urn)

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Figure I5b. Duplicate Particle Size Distribution for Sample M13 (Bottom).

Particle Number Distribution of M13B Duplicate

50 00

45 00

40 00

35 00

Si 30 00

IE 25 00

s! 20 00

15 00

10 00

5 00

0 00

D As Received B25 Watts ■ 40 Watts

AJ\J\ J „

Particle Diameter (urn)

Particle Volume Distribution of M13B Duplicate

10 00

9 00

8 00

7 00

6 00

5 00

4 00

3 00

2 00

1 00

0 00

□ As Received H25 Watts ■ 40 Watts

f: |-

g z

8 s

g Si

-n

g ?

Particle Diameter (pm)

1-18

50 00

45 00

40 00

35 00

Si 30 00

a? 2500

SS 20 00

15 00

10 00

5 00

0 00

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Figure I6a. Particle Size Distribution for Sample T20 (Top)

Particle Number Distribution of T20T

O As Received B 25 Watts ■ 40 Watts

Lift*.

8 8

Particle Diameter (urn)

Particle Volume Distribution of T20T

10 00

9 00

8 00

7 00

i 6 00

5 00

4 00

3 00

2 00

1 00

0 00

□ As Received H25 Watts ■ 40 Watts

Particle Diameter (urn)

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Figure I6b. Duplicate Particle Size Distribution for Sample T20 (Top)

Particle Number Distribution of T20T Duplicate

50 00

45 00

40 00

35 00

Si 30 00

a? 25 00

j8 20 00

15 00

10 00

5 00

0 00

□ As Received B25 Watts ■ 40 Watts

Particle Diameter (urn)

Particle Volume Distribution of T20T Duplicate

10 00

9 00

8 00

7 00

i 6 00

5 00

4 00

3 00

2 00

1 00

0 00

D As Received B25 Watts ■ 40 Watts

S s

Particle Diameter (jim)

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Figure I7a. Particle Size Distribution for Sample T20 (Bottom).

Particle Number Distribution of T20B

50 00

45 00

40 00

35 00

Si 30 00

S 25 00

S? 20 00

15 00

10 00

5 00

0 00

□ As Received

B25 Watts

to at n ci

10 00

9 00

8 00

7 00

Si 6 00

a 500

5 4 00

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Particle Diameter (urn)

Particle Volume Distribution of T20B

D As Received

D25 Watts

Bid i iB

to w in in (D ot m at

o . - . - CM n m

Particle Diameter (urn)

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Figure I7b. Duplicate Particle Size Distribution for Sample T20 (Bottom).

Particle Number Distribution of T20B Duplicate

50 00

45 00

40 00

35 00

Si 30 00

C 25 00

j ! 20 00

15 00

10 00

5 00

0 00

D As Received B25 Watts ■ 40 Watts

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Particle Diameter (urn)

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oc *

10 00 9 00 8 00 7 00 6 00 5 00 4 00 3 00 2 00 1 00 0 00

QAs Received D25 Watts ■ 40 Watts

iO O) CO o>

Particle Diameter rjim)

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Figure I8a. Main Basin Sludge Zeta Potent ia l Samples M13 (Top) and M13 (Bottom).

40

30 - r

ST 20

10-E-

0 c a o o- -10 A -20 +

-30 +

-40

• M13T □ M13T Duplicate

■ M13B o M13B Duplicate

»e ■ □ - □

tf A~

6 pH 8 10 12

Figure I8b. K East Weasel Pit Sludge Zeta Potential Data Samples T20 (Top) and T20 (Bottom).

40

30 • T20T Duplicate

D T20B Duplicate

■ T20B

o T20T

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A P P E N D I X J

EXAMPLES OF SLUDGE PARTICLE SHAPES

(Excerpted from the Work of J. Liu in Reference Silvers 1995)

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Figure Jl. Overall Structure of K East Basin Floor Sludge as Seen in Transmission Electron Microscopy (4500X).

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Figure J2. An Irregular Particle Consisting of FeO(OH) (35000X).

V

B E S T AVAILABLE COPY

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Figure J3. Elongated Particles Consisting Primarily of Uranium Compounds (35000X).

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Figure J4. A Particle with a High Concentration of Aluminum, Silicon, and Iron (4000X).

t

'S

I «»

r 4< i

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Figure J5 Needle-Like Particles Consisting of Magnesium, Aluminum, Iron, and Silicon (35000X)

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A P P E N D I X K

COMPOUNDS DETECTED USING X-RAY DIFFRACTION AND ELECTRON DIFFRACTION

(A Summary of the Work of E. D. Jenson and J. Liu in Reference Silvers 1995)

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Table Kl. Crystalline Phases Identified by X-Ray Diffraction in Centrifuged Sludge (Sixteen Samples Analyzed).

Note the absence of uranium and zirconium metal and uranium hydride.

Phase

U02

U04 ■ 4H20

FeOOH

Si02

Mg3 Si4010 (0H)2

Si

CaAl2Si20B • 4H20

CaCOj

CaU60„ • 12H20

K2 U04

L i 2 NiFe204

Na2 0 • A1203 • Si02 • H20

Si

L i x S i 1 t x 0 2 *

Na20 • A1203 • Si02 • H20

LiCuFe204

Number of Samples Containing th is

Phase

3

3

11

5

4

1

1

1

1

1

2

1

1

1

1

1

*Found only in the sample (H8) with large volume percent resin beads.

K-3

WHC-SP-1182

Table K2. Crystalline Phases in Centrifuged Sludge Identified by Electron Diffraction (Four Samples Analyzed

with Duplicates Run in All Four Cases).

Phase

FeOOH

Ca3 A l 2 Si3012

u3o„ Ti02

UF4 - 1.5H20

Fe203

(Fe, A l , Mg)6 (S iA l ) 4 010 (OH)8

Ca3Fe2 (S i04 )3 . x (0H)4.X

Fe 3 0 4

Number o f Samples Containing t h i s

Phase

3

1

2

1

2

2

2

1

1

Table K3. Crystalline Phases Identified by X-Ray Diffraction in the Residue Remaining after Acid Digestion (six samples analyzed).

Phase

Si02

Ti0 2 (pa in t pigment?)

Na Al S i 3 0a

(Na, Ca) Al ( S i , A l ) x 08

Mg3 S i 4 010 (0H)2

Mg4 A l 2 (0H)14 . 3H20

Pb7 (N03)4 (OH)10

Number o f Samples Containing t h i s

Phase

5*

2

2

2

1

1

1**

*Absent only in the sample with large volume percent of resin beads.

**Found only in the sample (H8) with large volume percent of resin beads.

K-4

WHC-SP-1182

A P P E N D I X L

SETTLING TIMES

(Excerpted from the work of D. B. Bechtold reported in Reference Miller 1995)

L-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

APPENDIX L SETTLING TIMES

Examples of the time-series sludge volume data for the samples are plotted in Figures LI through L4. All of the sludges except KES-E-11 had completed initial particulate settling and zone settling to form stable sludge volumes within 0.1 day after mixing. The KES-E-11 sample, in contrast, required about 1 day to do this. For samples KES-F-10, KES-G-07, KES-H-08, KES-I-15, KES-K-12, KES-0-09, KES-S-19, and KES-T-20, the particulates fell to stable sludge heights that did not settle further; settling had been completed by the time the sludge surface became defined, hence no data during the zone settling was obtainable. This absolute completion of settling and lack of compression settling was also evident for all other samples except four; KES-B-03, KES-D-14, KES-L-01, and KES-M-13 were the only ones which showed any further, long-term compression settling.

All samples formed well-defined sludges; however, KES-G-07, KES-I-15, and KES-K-12 otherwise did not settle completely. Rather, they retained murky water which was stable. The murkiness in the water above these solids would not agglomerate under gently, stirring shear. The data for sample KES-G-07 reflect a very slow settling of this murkiness to the extent that the long-term volume actually rose with time.

Where short-term zone settling data was available, it was fitted by an exponential decay of the form:

v (mL) = v£ + (v0 - v £ ) e - < b d a y ) (l)

where V is volume, V0 is a starting volume at time 0, Vf is the completed final volume at infinite time, and b is a rate constant. This choice of fitting function was made only because it had the right general shape for the short-term data. In fact, it does not adequately describe the final approach to completed settling for most samples. The parameters derived from it are useful only as a convenient way to compare the short-term settling behavior among samples or to simulate this behavior for an individual sample. The parameters derived by fitting this function to each amenable sample are listed in Table LI, along with statistics describing their accuracy. A graphical comparison of the relative rates of short-term settling among samples is provided by Figure L2, where the function is plotted in reduced form. The samples exhibit a wide range of short term settling rates.

L-3

WHC-SP-1182

As mentioned above, only four samples exhibited detectable long-term compression settling within the sensitivity of the experiments. The long-term data for these samples was fitted to a function:

(2) (day)1"

The resulting parameters are also included in Table LI. The exponents m are within the range derived for samples of backwash pit sludge studies in a previous campaign (Bechtold 1995), where long-term compression settling was the rule rather than the exception.

In summary, all samples formed sludges within 1 day after which very little, if any, further practical settling would occur.

L-4

WHC-SP-1182

Table Ll

KE Basin Sludge Sett l ing Parameters for F i t t i ng . V - Vf + (Vf - VJ*expf-b*day}

Or V - k*(dayp SAMPLE

KES-A-02

KES-B-03 SHORT TERM

KES-B-03 LONG TERM

KES-C-04

KES-D-14 SHORT TERM

KES-D-14 L0N8 TERM

KES-E-11

KES-J-06

KES-L-01 SHORT TERM

LONO TERM

PARAMETER

V, (mLl

V. (mLl

b (day1)

V, (mil

V. tmLI

b (day1!

k (mL-day""l

m

VMmL)

V. |mL>

btday*)

V . M J

V. (mLl

b (day'l

k (mL-day°°'*l

m

V, (mL)

V. (mil

b (day')

V, (mLl

V. Imt)

b Iday'l

V, ImL)

V. (mLl

b Iday']

k (mL-lay1""--)

m

VALUE

4.45x10*'

7x10*'

4 . 6 . 1 0 "

1.14.10*"

7 .5 .10* '

8 . 0 .10 -

1.034x10*'

3.70x10"

7 .9x10-

8.1.10* '

1.5x10*"

1.27x10*'

9.3x10*"

6 4x10"

1.16x10*'

1.9x10-

3.83x10*'

7.99x10*'

5.2x10°

1.56x10*'

6.5x10*'

7x10"

1.26x10*'

6.17x10*'

4 8,10*'

1.170»tO*'

1.63x10'

STANDARD ERROR

9.0x1ff'

4.5x10*"

6.4x10"

3.2X10*

1.5x10"

3.0x10°

8.5x10-'

5.8x10-"

3.1x10°

7.axto-

1.3x10"

3.7x10°

1.7x10-

2.2x10°

1.3x10°

5.0x10-

5.0x10°

5.4x10°

2.0x10'

3.7x10*

3.8x10*'

1.1x10"

2.6x10°

9.3x10°

1.6.10°

3.7x10'

3.2X10"

T VALUE

47.03

1.636

7.134

35.13

50.26

26.72

122.1

6.408

25.t2

10.39

11.34

34.47

54.8

29.62

83.37

4.022

77.24

147.9

22.75

4t.75

16.31

6.34

48.37

66.41

29.51

310 8

5.109

SIS. LEVEL

0.0001

0.116

0.0001

0.0001

0.0001

0.0001

0.001

0.001

0.0001

0.0001

0.0001

o.ooot

0 0001

0.0001

0.0001

0.001

0.000,

0.0001

0.0001

0.0001

0.0001

0.001

0.0001

0.0001

0.000,

0.001

0.0022

DEP.

COEFF.

0.124

0.994

0.995

0.251

0.546

0.626

0.187

0.187

0.204

0.866

0.877

0.254

0.587

0.658

0.755

0 7S5

0.339

0.499

0.622

0.222

0.856

0.868

0.283

0.554

0 643

O.00967

0.00967

L-5

WHC-SP-1182

Table LI (Continued)

KE Basin Sludge Sett l ing Parameters for F i t t i ng . V - Vf + (Vf - V0)*exp{-b*day}

Or V - k*(day)'*

KES-M-13 SHORT TERM

KES-M-13 LONO TERM

KES-N-05

KES-P-16

KES-Q-17

KES-R-18

VI (mLl

V. ImU

b May')

k Imt-daV*-0-)

m

VI (ml)

V. (ml)

b (day '1

V, (mil

V. tmtl

b (day'l

V, ImU

V. (mLl

b (day '1

V, l u l l

V. (ml)

b(day')

1.63x10*'

8.5x10"

3.7x10"

1.47xtO*'

3.2X10-'

1.61x10"

8.4,10*'

3.7x10*'

1.185x10"

2 . 2 . 1 0 "

1.2x10"

1.193.10*"

2.2.10*'

1.2.10*'

2.488.10*'

4.91X10"

7.0X10"

4.5x10°

1.2x10"

1.3x10°

1.4,10°

t . 1 . 1 0 '

4.9.10°

1.4.10-

1.5.10°

5.0.1 ff'

3 6 x 1 0 "

2.3x10"

7.0x10-'

6.4x10"

7.9x10-

9.0.1O'

9.5x10°

5.5x10°

36.13

72.39

27.91

104.5

2.851

32.91

60.23

24.62

235.5

6.101

5.231

165.2

3.489

1.527

274.0

51.68

12.75

0.0001

0.0001

0.0001

o.oot

0.0463

0.0001

0.0001

0.0001

0 0001

0 000,

0001

0.001

0.013

0 178

0.000,

0.0001

0.00,

0.307

0.501

0.615

0.492

0.492

0.313

0.546

0.648

0.244

0.955

0 957

0.181

0.994

0 994

0.25,

0 877

0.888

L-6

WHC-SP-1182

Figure LI. Example of Sludge that Settles Quickly Without Additional Compaction; Most Sludge Settles in this Manner.

aimai* cia.A.ga ai««aa sattiiaa oa«a

03 + 1 1 l i l l l l l l 1 1 I I H I M I 1 I I M i l l 1 1 I I I 1111

. , , 0 , -I 1 1 I I I I I I ! I 1 I I I l l l l 1 1 1 I I I I Mil 1.-03 1.-02 , a - 0 1 l a . 0 0 1 a - 0 ,

Days S a t t l . d

Figure L2. Example of Sludge that Settles with Some Long Term Compaction

■ Ci»_M_1» t ,a««a S a t t l i a a Dal

i«*03 1 1—i i i inn 1—Mil I I I I i—i i i mi l 1—i m m

■■°^-<h—<

-11-.02 I I I M IMU—■- I I I H I I I I I—I .t-H-IIH I I I M i l l i-J-03 1*-02 1.»- 0 1 1«*O0 i t . O I

Days Si I t I«0

L-7

WHC-SP-1182

Figure L3. Example of Sludge where Long Term Settling of Murky Water Results in Volume Increase with Time.

SIM*i* ci>_a_or )•••>•)• a

. t n i n | o>t*

1«*03 + 1—I I I Mi l l 1 I -M-HIH 1—■ t - f4t t l l 1—I I HUH 1—h-f

I I I I I Ml I I t I H i l l I t I I HIM I I I I r t l l l - f i r la-OS 1*-02 t«-01 1*4.00 1«*Q1

Days Set 11ed

Figure L4. Settling Rate Curves Derived for All Samples.

L-8

WHC-SP-1182

A P P E N D I X M

THERMO-GRAVIMETRIC ANALYSIS

Each page of this appendix displays Thermo-Gravimetric Analysis (TGA) data for a particular sample of centrifuged sludge. Shown side-by-side are data from 222-S and 325 Building laboratories (when complementary data are available) as well as any duplicate runs for the given sample. They are presented here as an indication of the release of bound water which may take place at temperatures above 100 °C. The magnitude of water release detected by the two laboratories varies in part because of the different environments and pretest drying times experienced at each laboratory. Percent water derived from these curves is listed with the chemistry results in Appendix B.

M-l

WHC-SP-1182

This page intentionally l e f t blank.

WHC-SP-1182

Figure Ml. Percent Weight Loss for Thermo-Gravimetric Analysis Sample L I . (Both runs are from 325 Building)

96-00526

( JO'saB ag) <n*ftrtrrCt> »■■■■

0.000 ag <Swl i r ,g>

<1«v pT(Mjr»»lC] (C/alnl [aln)> IN 20.0- 900 0 5.00 0 00

• 2 500.0- 30 0 100.00 0.00

TEMP C (Heating)

<SoBple> 3nov95d

E.B49 ng ( 6.849 ag)

<Reference>

O.ODO ng

<CoMnent> 96-00526D

<SMpling>

<Tenip.prograr-[C] [c/min) [mlnj> 1* 30.0- 300.0 S.OO 0.00

' 2 500.0- 30.0 100.00 0.00

nitrogen 300.0 ml/min 0.0 nl/nln

M-3

WHC-SP-1182

Figure M2. Percent Weight Loss for Sample A2 (Data is from 325 Building)

<Sample> 20nov35d

( 9.391 ng) <Refer«nce>

0.000 ng

<Tenp.progr3ii.ICl [C/min) fain]> IN 20.0- 500.0 5.00 0.00 2 500.0- 20.0 100.00 0.00

M-4

WHC-SP-1182

Figure M3. Percent Weight Loss for Sample B3. (The upper curve is from 325 Building and the

lower is from 222-S Laboratory)

<Saaple> 2nov95h

IB 9E4 eg ( IB 9G4 mg)

<Heference>

0 000 ng

<Tenp prograH[Cl 1« 20 0- 500 0 2 500 0- 30 0

(C/mln] [mln]> 5 00 0 00

100 00 0 00

S95K000094 SAM N2 32 094 pig Rata 10 0 C/aln

S*"pp Ana lys is H f i g h t - 2 7 00 mg

f-icciC 5 09 mg

\ Dpeak 117 0 C

100 200

File 00058 001 IdBftt 0 0

1 ' ' '

TG METTLEH 2-»-Nov-s5 222-s Laboratory

■ 1 ' ' ' ' 1

M-5

WHC-SP-1182

Figure M4. Percent Weight Loss for Sample C4. (The upper curve is from 325 Building and the

lower from 222-S Laboratory)

<Sf)mple>

[ 6.997 ng) <neference>

0.000 ng

<Connent> 96-0000529

<Tenp.program(C] [C/ain] [min]> IX 20.0- 500.0 5.00 0.00 2 500.0- 50.0 100.00 0.00

nitrogen

<Soapllng> 0.5 sec

1.0 nl /nln 0.0 nl/nin

S95K000095 SAM N2 40.622 no

-l \

100.

Bate:10.0 *C/»ln

Step Analys is He igh t -?7 .57 mo

Rc-jiC. 13.05 mq

Dpoak 113.O'C

200.

File: 00059.001 Ident: 0.0

300.

TG METTLER 2.1-222-5 Laboratory

, , . . i .

av-85

T

M-6

WHC-SP-1182

Figure M5. Percent Weight Loss for Sample N5. (The upper two curves are duplicate runs at 325 Building

and the lower curve was generated at 222-S Laboratory)

<Sanple> Gnov95f

( 7.3B7 ng) <fleference>

0.000 ng

<Co.w»ent> 96-00530

-cTenp. program tC] [C/mln] 1* 20.0- 500.0 6.00 2 500.0- 30.0 100.00

nitrorjen

[nin] >

<Sanpllno>

300.0 nl/nin 0.0 nl/nln

<5snple> 6nov95h

4.867 ng ( -1.867 ng]

<fleference>

0.000 ng

<Conaent> 96-005300

<Tenp. program [C] IK 20.0- 500.0 2 500.0- 30.0

nitrogen

<Sanpllng>

[C/ain) [nln]> 5.00 0.00

100.00 0.00

300.0 nl/nln 0.0 a l /n ln

/js-

595K000096 SAM UP. File: 00071.001 TG METTLER 26-Mov-93 31.305 ag Rate: 10.0 "C/ain Ident: 0.0 222-S Laboratory

Step Ana lys i s Heigh t -23 .57 mg

- 75 .30 % ResiC. 7.6B mg

2 4 . 5 4 X □peak 1 1 3 . 0 ' C

M-7

WHC-SP-1182

Figure M6. Percent Weight Loss for Sample J6. (The upper two curves are from 325 Building

and the lower is from 222-S Laboratory)

<Sanple> 2onov95h

13.666 atg t 13.666 ng)

<flefertnce>

0.000 ng

<Tenp. program. fCj {C/taln] 1* 20.0- 500.0 5.00 2 500.0- 20.0 100.00

<Sanple> 20nov95f

( 9.021 ng) <Reference>

0.000 ng

•CTenp. progran [C] [C/ainl 1« 20.0- 5O0.0 5.00 2 500.0- 20.0

nitrogen

bln)>

100.00 o.oo

300.0 nl/nln 0.0 l l / a l n

__4fci_ S95K000097 SAM N2 •16.091 ag date: 10.0 *C/ain

File: 00069.001 Idant: 0.0

TG METTLER 26-Nnv-95 ??2-S Laboratory

Step Analysis Height -1.97 mg

ResiC. 18.77 mg

M-8

WHC-SP-1182

Figure M7 Percent Weight Loss for Sample H8. (The lower run is from 222-S Laboratory and the upper two

are from 325 Building. This sample had the largest volume fraction of ion exchanae resin beads}

<Sanple> Gnov95d

12 530 mg ( 12 530 ng)

<Reference> Cu pan

0 000 mg

<CoB»ent> 96-005320

<Ssnpling>

<Tenp progran[C] [C/nln] [nin]> IN 20 0- 500 0 5 00 0 00 - — - * "1 0 00

300 0 nl/nln 0 0 ml/mln

_ 500 0- 30 0

nitrogen

<sample> 6nov95b

6 6B6 mg ( 6 6B6 ag]

<Reference>

0 000 ng

<Connent> 96-00532

<Teop progran[Cj [C/nln] [nln)> IN 20 0- 500 0 5 00 0 00 2 500 0- 30 0 100 00 0 00

nitrogen

<Sanpllng>

300 0 a l /n ln 0 0 nl/nln

VH S95K00009B SAM 1-.2 19 261 ag Rate 10 C

Step Anjlysi" Hcight-13 04 mg

flee C 6 20 no 32 15 X

Dpe ik 81 0 C

File 00067 001 TG METTLER 25 Nov-95 Idant 0 0 222-S Laboratory

Step Analysis Height -3 14 mg

-16 28 % ResiC 2 07 mg

Dpeak 3B7 O'C

M-9

WHC-SP-1182

Figure MS. Percent Weight Loss for Sample 09. (Data is from 325 Building. This sample had the

highest uranium content of any sample)

<Ssnple> 7nov95b

9.200 ng ( 9.200 ng)

<Beference> Cu pan

0.000 ng

<Tetap.progran[C] 1(4 20.0- 500.0 2 500.0- 30.0

nitrogen

[C/min] [minj> 5.00 0.00

100.00 0.00

300.0 Hi/win 0.0 ml/mln

M-10

WHC-SP-1182

Figure M9. Percent Weight Loss for Sample FIO. (The top curve is from 325 Building and the

bottom is from 222-S Laboratory)

<Saaple> 7nov95d

6.783 ng ( 6.783 ng)

<Reference>

0.000 mg

<Tenp. program [C] IK 20.0- 500.0 2 500.0- 30.0

nitrogen

[C/nin3 [nin)> 5.00 0.00

100.00 0.00

300.0 nl/min 0.0 nl/min

Fl«

S95K000099 SAM N2 34.492 ag Rata: 10.0 'C/nln

\

Step Ana lys is Hs lgh t -14 .95 mg

-43 .34 X ResiC. 19.51 ng

56.57 X Dpeak 91.0*C

\ \

\ M. ■

, 1 * ■ ■ * 1 ' * 100. 200.

File; 00063.001 TG METTLER I dent: o.o 222-s Laboratory

Step Ana lys i s Height -2 .04 mg

ResiC. 17.47 mg

~—==

^ f-1 ' 1 ■ ■ ' ' 1 ' ' '

300. 400.

4 ^ -

" -c

M-ll

WHC-SP-1182

Figure M10. Percent Weight Loss for Sample E l l . (Upper curve is from 325 Building and the

lower is from 222-S Laboratory)

<Sanple> 22nov93b

15.880 mg ( 15.880 ag]

<Reference> Cu pan

0.000 mg

<Tenp.program [Cl [C/min] [nin] > IN 20.0- 500.0 5.00 0.00 2 500.0- 20.0 100.00 0.00

nitrogen 300.0 nl/min

S95K000100 SAM N2 17.749 ag Rate: 10.0 'C/»in

Step Analysis Height-l3.96 mg

File: 00061.001 TG METTLER 25-Nov-93 222-S Laboratory

Step Analysis Height -0.56 mg

ReslC. 3.23 mg IB.IB X

!—

M-12

WHC-SP-1182

Figure Mi l . Percent Weight Loss for Sample K12. (Data is from 325 Building)

<Sanple> 9nov95d

6.322 mg ( 6.322 ng)

<fleference>

0.000 mg

<Conaent> 96-00536

<Te«p. program [C] [C/«in] IN 20.0- 500.0 5.00

- 2 500.0- 30.0 100.00

nitrogen 300.0 i <Sanpllng>

il/min

M-13

WHC-SP-1182

Figure M12. Percent Weight Loss for Sample 115. (Data is from 325 Building)

<Conaent> 96-00537

<Sanple>

11.130 ng t 11.130 ng)

«*fleference> Cu pan

O.OOO ng <Saapllng>

<Temp. program [C] [C/min] IK 20.0- 500.0 5.00 2 500.0- 50.0

nitrogen

tnln]>

100.66 0.00

300.0 nl/min 0.0 ml/min

M-14

WHC-SP-1182

Figure M13. Percent Weight Loss for Sample P16. (The top two curves are duplicate runs from 325 Building

and the bottom is from 222-S Laboratory)

( 7 060 ng) <Reference> nt Cu pen

0 000 ng <SampllnB>

<Temp program [C] 1* 20 0- 500 0 2 500 0- 20 0 nitrogen

[C/nln) 5 00

100 00 ■"Samplo 2Bnov95a

7 060 mg t 7 060 ng)

<Reforcnce> nt Cu pan

0 000 ag

<Tenp program [c] IK 20 0- 500 0 2 500 0- 20 0 nitrogen

[C/minJ [min]> 5 00 0 00

100 00 0 00

300 0 al/ain 0 0 al /a in

S95K00010? SAM N2 File OOO-'S 001 T

G METTLER 26-Nov-95 Rate 10 0 "C/nln

Step Analysis Height-IB 20 mg

-35 84 X flesiC 32 54 mg

54 07 X □peak 91 0*C

Ident 0 0

Step Ana lys is Height - 2 73 mg

-5 38 X R P S I C 2^ 31 mg

Dpeak ?b9 O'C

222-S Laboratory

M-15

WHC-SP-1182

Figure M14. Percent Weight Loss for Sample Q17. (Upper curve is from 325 Building and the

lower is from 222-S Laboratory)

<Sample> lnov95h

(11-197 mg) <t.eference>

0 000 ag

<Tenp program [C] IK 20 0- 500 0 2 500 0- 50 0 nitrogen

[C/nln] fmin]> 5 00 0 00

100 00 0 00

300 0 a l / a i n 0 0 ml/mln

S95K000103 SAM N2 39 --OS ng Rate 10 0 "C/pln

'v—1 \ \ \

! \ 1

Ctep A fu 1 ys i s H Q i g h t - M 60 mg

fleciC *> lO mg

Opr-ak A3 0*C

File 000""7 OOl Ident 0 0

Stpp A m l y s i j

TG METTLER B6-I ov-95 222-S Laboratory

Height - * 38 mg -3 --7 "fc

FlesiL 23 52 ng

M-16

WHC-SP-1182

Figure M15. Percent Weight Loss for Sample R18. (The top two are duplicate runs from 325 Building

and the lower is from 222-S Laboratory)

30nov95b ( 14! 791 ng)

<Heference> at Cu pan

0.000 ag

<ConMnt> 96-00540D

<Saapllng>

<Tenp .program [C] [C/ain] lain] > IN 20.0-500.0 5.00 0.00

■ 2 5O0.0- 20 0 100.00 0.00

nitrogen 300 0 al/ain . o 0 nl/aln

3l0ct95b 13 B20 ng

( 13 620 ng) <Reference>

0 000 ag

<Conaent> 96-00540

<Tenp. program [Cj 1* 20.0- 500 0 2 500.0- 50.0

nitrogen

<SampHng>

[C/aln] [mln]> 5.00 0.00

100.00 0.00

300.0 al /a ln 0.0 al /a ln

S95K000104 SAM i Rate* 10 0 "C/min

F i l e OOOBl.OOl TG METTLER 2B-No Ident* 0 0 222-S Laboratory

Step An . l y s i s Hcinh t -24 08 mg

-A3 26 X f l rs iC d l Cl mg

Dpf3k 107 O'C

Step Analysis Height -2.94 mg

ReslC. 2B 65 mg

M-17

WHC-SP-1182

Figure M16. Percent Weight Loss for Sample S19. (The upper curves are duplicate runs at 325 Building and the

lower curve was generated at 222-S Laboratory)

<Saaple> 9nov95b

8.681 ag ( 8.681 ng)

<Reference>

o.ooo ng

<Teap.program [C] [C/nln] [nln]> IK 20.0- 500.0 5.00 0.00 2 500.0- 30.0 100.00 0.00

nitrogen 300.0 nl/min 0.0 nl/min

<Sample> 7nov93f

11.B03 ng ( 11.B03 ng)

<Reference>

0.000 ng

<Tenp.progran[C) [C/aln] [min]> IN 20.0- 500.0 5.00 0.00 2 500.0- 30.0 100.00 0.00

nitrogen 300.0 ml/nln 0.0 n l /n in

S95K000105 SAM 1-.2 Rate: 10.0 * C/ain

Stop Analysis Heigl.t-iG.-17 mg

ResiC. 2C.05 mg

Dpeak 91.0'C

File: 00079.001 TG METTLER 26-Nov-SS Ident: 0.0 222-S Laboratory

Step Analysis Height -2.C3 mg

ResiC. 23.51 ing

—T— 200.

M-18

WHC-SP-1182

A P P E N D I X N

REGRESSION ANALYSIS FOR EUROPIUM ISOTOPES VERSUS PLUTONIUM CONTENT IN SLUDGE

T. L. Welsh

N-l

WHC-SP-1182

This page intentionally left blank.

WHC-SP-1182 Several correlations between the sludge characterization sample results are of interest: in particular, the correlations between (1) 239/240pu and 1 5 4£ u anrj (2) 239/240Pu and 155Eu. If a relationship between fission product radioisotopes (measured by gamma energy analyses translatable to field applications) and plutonium concentration (measured by an analytical laboratory method) can be identified, then the field gamma measurements may be used to predict the plutonium concentration of the sludge leaving the basin. Linear regression techniques were used to determine the correlations. Linear regression techniques provide equations of the form

Y = a + bx (N-l)

where Y is the dependent variable, X is the independent variable, b is the slope, and a is the y-intercept. 239/240Pu and 154Eu The regression analysis used the 154Eu data for the independent variable (X) and the 239/240pu data as the dependent variable (Y). Regression analyses were performed for the three sets of sludge characterization data; /vCi/g centrifuged sludge, /jCi/g as-settled sludge, and ilvCi/mL as-settled sludge. Equation N-2 was calculated from the regression analysis of the /vCi/g centrifuged sludge data.

Pu239 = 2.78006 + 4.13475 x Eul54 (N-2)

The R value for equation N-2 is 73.0%. The R value indicates the proportion of the variability in the dependent variable (Pu239) that is explained by the independent variable (Eul54). The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are illustrated in Figure N-l. The regression equation is represented by the solid line. The 95% confidence interval is represented by the inside dashed lines. The 95% prediction interval is represented by the outside dashed lines. The prediction interval illustrates the variability associated with predicting (using the regression equation) a new individual value for Y given an X value. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval, and the standard deviation used in calculating the 95% prediction interval are provided in Table Nl.

N-3

WHC-SP-1182

Figure N-l. KE Basin Sludge Characterization

per g centrifuged sludge

Eu154 CuCi/gj

Table Nl. 239/240pu vs. 154Eu - /yCi/g centrifuged sludge.

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21 23

"•Eu /'Ci/g

3.5380

0.9343

1.0910

2.3370

1.0180

0.7055

4.3720

0.3211

1.1365

0.2556

1.2895

1.1100

0.2412

0.6363

1.8535

2.3140

0.7050

*w-.°pu eCi/g

8.9750

5.9000

7.7300

14.8000

6.6050

5.7500

22.0000

2.2400

7.9000

1.8300

11.3500

8.1900

1.7750

5.1650

14.7000

16.1500

4.8500

Predicted ""'"°Pu pCi/g

17.409

6.643

7.291

12.443

6.989

5.697

20.857

4.108

7.479

3.837

8.112

7.370

3.777

5.411

10.444

12.348

5.695

Variability associated with a mean response s(Y„> - »Ci/g

1.567

0.789

0.756

0.948

0.770

0.858

2.062

1.012

0.748

1.042

0.732

0.752

1.049

0.882

0.784

0.938

0.858

Variability associated with the prediction of a

new y response s(YK,„„) - „ci/g

3.385

3.103

3.095

3.147

3.098

3.121

3.641

3.167

3.093

3.177

3.089

3.094

3.179

3.128

3.102

3.144

3.121

N-4

WHC-SP-1182

Equation N-3 was calculated from the regression analysis of the jL/Ci/g as-settled sludge data.

Pu239 = 1 .65218 + 4 . 5 3 2 7 3 x Eul54 (N-3)

The R2 value for equation N-3 is 82.2%. The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are illustrated in Figure N-2. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval, and the standard deviation used in calculating the 95% prediction interval are provided in Table N2.

Figure N-2. KE Basin SIudge Character Izat ion

per g as-se t t led sludge

Eu154 CuCi/g}

N-5

WHC-SP-1182

Table N2. 239/24

°Pu vs. 154

Eu - A/Ci/g as -se t t l ed sludge.

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21 22 23

'"Eu //Ci/g

2.1569

0.6344

0.6503

1.6155

0.5771

0.4857

3.9019

0.2499

0.7563

0.1233

1.0974

0.8917

0.1968

0.5451

0.9641

1.7557

1.2345

0.6408

•""""Pu ■/Ci/g

5.4716

4.0062

4.6078

10.2310

3.7443

3.9588

19.6342

1.7434

5.2572

0.8825

9.6590

6.5797

1.4485

4.4248

7.6463

12.2538

7.5350

4.4083

Predicted """"Pu /■Ci/g

11.429

4.528

4.600

8.975

4.268

3.854

19.338

2.785

5.080

2.211

6.626

5.694

2.544

4.123

6.022

9.610

7.248

4.557

Variability associated with a mean response s(Y„> - /,Ci/g

0.754

0.507

0.503

0.557

0.520

0.543

1.585

0.618

0.484

0.664

0.464

0.468

0.637

0.528

0.464

0.601

0.475

0.505

Variability associated with the prediction of

a new Y response s(Y„.„,) - //Ci/g

2.102

2.026

2.026

2.040

2.030

2.036

2.522

2.057

2.021

2.071

2.016

2.017

2.063

2.032

2.016

2.052

2.019

2.026

Equation N-4 was calculated from the regression analysis of the /vCi/mL as-settled sludge data.

PU239 = 1 . 8 6 9 7 6 + 4 . 9 0 9 0 7 x Eul54 ( N - 4 )

The R2 value for equation N-4 is 93.3%. The data, the regression equation,

the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are i l lust rated in Figure N-3. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence in terval , and the standard deviation used in calculating the 95% prediction interval are provided in Table N3.

N-6

WHC-SP-1182

Figure N-3. KE Basin SIudge Characterization

per mL as-settled sludge

Eu154 CuCi/mL^

Table N3. 239/240Pu vs. 154Eu - uCi/mi as-settled sludge.

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21 22 23

"*Eu //Ci/mL

2.4804

0.7613

0.6763

1.8579

0.6406

0.6072

8.8962

0.3374

0.8622

0.1726

1.6900

1.3465

0.2952

0.8667

1.0702

3.0725

1.9752

1.0509

"'""Pu //C i /ml

6.2923

4.8074

4.7921

11.7657

4.1562

4.9485

44.7661

2.3536

5.9932

1.2355

14.8749

9.9353

2.1728

7.0355

8.4874

21.4441

12.0560

7.2296

Predicted "'""Pu //Ci/mL

14.046

5.607

5.190

10.990

5.014

4.850

45.542

3.526

6.102

2.717

10.166

8.480

3.319

6.124

7.123

16.953

11.566

7.029

Variability associated with a mean response s(Y.) - //Ci/mL

0.696

0.689

0.700

0.638

0.705

0.710

2.478

0.755

0.676

0.785

0.633

0.638

0.762

0.676

0.655

0.797

0.645

0.657

Variability associated with the prediction of a

new Y response s<Y._,) - //Ci/mL

2.772

2.770

2.773

2.758

2.774

2.776

3.652

2.787

2.767

2.796

2.757

2.758

2.789

2.767

2.762

2.799

2.760

2.763

N-7

WHC-SP-1182

The SFBWP data were combined with the sludge characterization data (/vCi/mL as-settled sludge). Equation N-5 was calculated from the regression analysis of the combined /jCi/mL as-settled sludge data.

PU239 = 1.21059 + 5.06154 x Eul54 (N-5)

The R2 value for equation N-5 is 94.0%. The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are illustrated in Figure N-4. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval, and the standard deviation used in calculating the 95% prediction interval are provided in Table N4.

Figure N-4. KE Basin Sludge Characterization

per mL as-set t led sludge

Eu154 CuCi/mL3 SFBWP Data i nc I uded

N-8

WHC-SP-1182 Table N4 Combined 239/240pu vs

154Eu - /jCi/mL as-settled sludge

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21 22 23

SFBWP

SFBWP

SFBWP

SFBWP

SFBWP

SFBWP

SFBWP

SFBWP

"Eu //Cl/mL

2 4804

0 7613

0 6763

1 8579

0 6406

0 6072

8 8962

0 3374

0 8622

0 1726

1 6900

1 3465

0 2952

0 8667

1 0702

3 0725

1 9752

1 0509

0 163

0 164

0 179

0 281

0 161

0 322

0 354

0 241

"» ""Pu //Ci/mL

6 2923

4 8074

4 7921

11 7657

4 1562

4 9485

44 7661

2 3536

5 9932

1 2355

14 8749

9 9353

2 1728

7 0355

8 4874

21 4441

12 0560

7 2296

1 0185

0 9281

1 0458

1 6838

1 3068

2 2377

1 8854

1 5231

Predicted "" "°Pu //Cl/mL

13 765

5 064

4 634

10 614

4 453

4 284

46 239

2 918

5 575

2 084

9 764

8 026

2 705

5 597

6 627

16 762

11 208

6 530

2 036

2 041

2 117

2 633

2 026

2 840

3 002

2 430

Vanabi lity associated with a mean response s(Yh) //Ci/mL

0 566

0 464

0 470

0 486

0 473

0 475

2 073

0 502

0 459

0 522

0 471

0 454

0 507

0 459

0 452

0 672

0 498

0 453

0 523

0 523

0 521

0 508

0 524

0 504

0 500

0 513

Variability associated with the prediction of a

new Y response s(Y„n_,) //Ci/mL

2 370

2 348

2 349

2 352

2 350

2 350

3 097

2 356

2 347

2 360

2 349

2 346

2 357

2 347

2 346

2 398

2 355

2 346

2 360

2 360

2 360

2 357

2 360

2 356

2 355

2 358

The R2 values, calculated for each of the four 154Eu and 239/2'10Pu regression analyses (£/Ci/g centrifuged sludge, ̂ Ci/g as-settled sludge, yCi/mL as-settled sludge, and the combined ^/C/mL as-settled sludge), increased in value from 73 0% to 82 2% to 93 3% to 94 0% Based on the R2 values, the "best" prediction equation would be equation N-5 However, this increase in R2 values is caused by the increasing distance between the two subsets of data within each regression, the first subset of data is clustered at the low concentration values of 154Eu while the second subset (a single data point) is at the high concentration value of 154Eu Figures N-l, N-2, N-3, and N-4 illustrate the clustering of the data

N-9

WHC-SP-1182 239/240Pu and 155Eu

The regression analysis used the 155Eu data for the independent variable (X) and the 239/24°Pu data as the dependent variable (Y). Regression analyses were performed for the three sets of sludge characterization data; /vCi/g centrifuged sludge, /vCi/g as-settled sludge, and UCi/mL as-settled sludge.

Equation N-6 was calculated from the regression analysis of the /L/Ci/g centrifuged sludge data.

PU239 = 3.10355 + 8.52428 x Eul55 (N-6)

The R2 value for equation N-6 is 63.5%. The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are illustrated in Figure N-5. The prediction interval illustrates the variability associated with predicting (using the regression equation) a new individual value for Y given an X value. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval, and the standard deviation used in calculating the 95% prediction interval are provided in Table N5.

Figure N-5. Sludge Characterization Data uCi/g centrifuged sludge

N-10

WHC-SP-1182

Table N5 239/240pu v s . 155Eu - f/Ci/g centrifuged sludge.

Locat ion

1

2

3

4

5

6

9

10

11

12

16

17

18

19

20

21

' "Eu / /Ci /g

1 7265

0.4223

0.5337

1.0360

0 4469

0.3404

2.0140

0.1632

0.5632

0 1700

0.1589

0 7304

0 4318

0.1375

0.6296

0.9010

" ' - p u / /Ci /g

8.9750

5.9000

7.7300

14.8000

6.6050

5.7500

22.0000

2.2400

7.9000

1 8300

2 4600

11 3500

8.1900

1.7750

14.7000

16.1500

Predic ted •""••Pu / /Ci /g

17.821

6.703

7.653

11.935

6.913

6.005

20.271

4.495

7 904

4.553

4.458

9 330

6 784

4.276

8 470

10.784

Van abi 11 t y associated w i th a

mean response s(Y") - / /Ci /g

2.071

0.994

0.935

1.130

0.978

1.058

2.527

1.242

0.925

1.234

1.247

0.923

0.988

1.272

0.914

1.010

V a r i a b i l i t y assoc iated w i th the p r e d i c t i o n of a

new Y response s (Y„ „_ , ) - , /C l /g

4 198

3.784

3.769

3.822

3.780

3.802

4.440

3.857

3.767

3.854

3.858

3.766

3.783

3.867

3 764

3 789

Equation N-7 was calculated from the regression analysis of the /;Ci/g as-settled sludge data.

PU239 = 1 .70613 + 9 .64325 x EulSS (N-7)

The R2 value for equation N-7 is 77.3%. The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are i l lus t ra ted in Figure N-6. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval , and the standard deviation used in calculating the 95% prediction interval are provided in Table N6.

N - l l

WHC-SP-1182

Figure N-6. KE Basin Sludge Character izat ion

per g as-se t t led sludge

Eu154 CuCi/g}

Table N6. 239/240pu v s . 155Eu - /vCi/g as-settled sludge.

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21

'"Eu //Ci/g

1.053

0.287

0.318

0.716

0.253

0.234

1.797

0.127

0.375

0.082

0.154

0.622

0.347

0.112

0.327

0.684

""""Pu //Ci/g

5.472

4.006

4.608

10.231

3.744

3.959

19.634

1.743

5.257

0.883

2.386

9.659

6.580

1.449

7.646

12.254

Predicted "•""Pu //Ci/g

11.8560

4.4713

4.7739

8.6123

4.1489

3.9661

19.0391

2.9310

5.3203

2.4966

3.1923

7.7002

5.0513

2.7882

4.8642

8.2985

Variability associated with a mean response s(Y.) - //Ci/g

1.013

0.650

0.634

0.692

0.669

0.682

1.952

0.765

0.612

0.806

0.742

0.636

0.622

0.778

0.630

0.670

Variability associated with the prediction of

a new Y response s(Yh„„) - //Ci/g

2.598

2.480

2.475

2.491

2.485

2.488

3.088

2.512

2.470

2.525

2.505

2.476

2.472

2.516

2.474

2.485

N-12

WHC-SP-1182

Equation N-8 was calculated from the regression analysis of the /vCi/mL as-settled sludge data.

PU239 = 1.78796 + 10.64989 x Eul55 (N-8)

The R value for equation N-8 is 91.3%. The data, the regression equation, the confidence interval for a mean Y value associated with a given X value, and the prediction interval for an individual Y value associated with a given X value are illustrated in Figure N-7. The data, the predicted value for the observed X values, the standard deviation used in calculating the 95% confidence interval, and the standard deviation used in calculating the 95% prediction interval are provided in Table N7.

Figure N-7. Sludge Character izat ion Date

uCi/mL as-se t t led sludge

N-13

WHC-SP-1182 Table N7. 239/240pu vs. 155Eu - uCi/mL as-settled sludge.

Location

1 2 3 4 5 6 9 10 11 12 16 17 18 19 20 21

'"Eu

1.2104

0.3441 __,

0.3309

0.8236

0.2812

0.2929

4.0981

0.1715

0.4273

0.1148

0.2003

0.9572

0.5238

0.1683

0.3635

1.1963

"•"•'Pu

6.2923

4.8074

4.7921

11.7657

4.1562

4.9485

44.7661

2.3536

5.9932

1.2355

3.1017

14.8749

9.9353

2.1728

8.4874

21.4441

Predicted "'""Pu

14.679

5.453

5.312

10.559

4.782

4.908

45.433

3.614

6.338

3.010

3.922

11.982

7.367

3.580

5.659

14.529

Variability associated with a mean response s(Y„) - //Ci/mL

0.929

0.886

0.890

0.828

0.908

0.903

3.073

0.952

0.862

0.978

0.940

0.849

0.840

0.954

0.880

0.923

Variability associated with the prediction of a

neu Y response s(Y»,„,) - //Ci/mL

3.419

3.408

3.409

3.393

3.414

3.413

4.503

3.426

3.402

3.433

3.422

3.399

3.396

3.426

3.406

3.418

The R values, calculated for each of the three Eu and ' Pu regression analyses (,1/Ci/g centrifuged sludge, /vCi/g as-settled sludge, jL/Ci/mL as-settled sludge, and the combined ^C/mL as-settled sludge), increased in value from 63.5% to 77.3% to 91.3%. Based on these R2 values, the "best" prediction equation would be equation N-8. However, this increase in R2 values is caused by the increasing distance between the two subsets of data within each regression; the first subset of data is clustered at the low concentration values of Eu while the second subset (a single data point) is at the high concentration value of 155Eu. Figures N-5, N-6, and N-7 illustrate the clustering of the data.

N-14

WHC-SP-1182

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