739 - Digital Library/67531/metadc... · MDC for methods and systems used to discriminate between TRU and LLW or methods and systems used to define a waste stream as TRU. Satisfaction

@

651 '739 ........... . . . .. . . . . . . . . . . . . . . . ___. . . . Pagal O f &

ENGINEERING CHANGE NOTICE

2. ECN Category (mark one) 3. Originatoh Name, Organization. MSIN, and Telephone No. 4. USQ Required? 5. Date

0 @Yes ONO 09-14-99

0 0

0

Supplemental CE wills, WRAP Engineering, DiredRevision @ T4-52, 373-9844 Change ECN

Temporary

Standby Supersedure sheet no. and rev.)

7. Bldg./Sys./Fac. No.

2336-W Q

6. Approval Designator 6. Project TtlelNo.fWork Order No.

WRAP Facility/AJ60

Q. Document Numbers Changed by this ECN (includes 10. Related ECN No(s). 11. Related PO No.

CancelNoid 0 HNF-4051, Rev. L A , All I N/A I N/A 0 Yes (fill out Elk. 12b) 0 No NA Blks. 12b,

1% Modification Work 12b. Work Package No. 12c. Modification WorkCompleted 12d. Restored to Ori inal Condition (Temp. or Standby ECds only)

N/A N/A N/A Design AuthoritylCo Engineer Signature 8 Design AuthoritylCo Engineer Signature 8

!2c, 12d) d i t e d i t e

13a. Description of Change 13b. Design Baseline Document? 0 Yes @ No

Newly generated QAO data has been added to more completely describe instrument performance over the range of analysis. In addition, Minimum Detectable Concentration calculations are provided for the IPAN and GEA Systems.

1 4 . Justification (markone) I&. Justification Details

Criteria Change 0 Design verification not required Design Improvement 0

0 Environmental Additions made in response to WIPP audit comments

USQ WRP-99- (99 Facilty Deadivation

As-Found

Faciltate Const.

See attached distribution sheet

A-79M)-0152 (10B7) A-780&0151

I I 1. ECN (use no. from oa. 1

6. Design Verification Required

ENGINEERING CHANGE NOTICE

17. Cost impact 18. Schedule Impact (days) ENGINEERING CONSTRUCTiON

. - Page 2 of 2 ECN-651739

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- SDDmD 0 Fundional Design Criteria 0 Operating Specification 0 Criticality Specification 0 Conceptual Design Report 0 Equipment Spec. 0 Const. Spec. 0 Procurement Spec. 0 Vendor Information 0 OM Manual 0 FSAWSAR 0 Safety Equipment List 0 Radiation Work Permit 0

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Tank Calibration Manual 0 Health Physics Procedure 0 Spares Multiple Unit Listing 0

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Process Flow Chart

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ADDITIONAL

A-7WJ-0133 (10197)

-___-_I..- .-

HNF-4051, Rev. 2

Quality Assurance 0 bjectives for Nondestructive Assay at The Waste Receiving and Processing Faci I ity

CE Wills Waste Management Federal Services of Hanford, Inc., Richland, Wa. 99352 Richland, WA 99352 U.S. Department of Energy Contract DE-AC06-96RL13200

EDTIECN: ECN- 65173 9 u c : 506

Org Code: 32600 Charge Code: AJ60 B&R Code: EW02J16 Total Pages: 31

Keywords: QAP, NDA, WRAP, WIPP, TRU, CAO, Source Certificates

Abstract: This report summarizes the validation of the WRAP NDA systems against the various QAOs. A brief description of each test and any significant conclusions is included. Variables which may have affected test outcomes are examined. This report will be reviewed semi-annually and updated as necessary.

TRADEMARK DISCLAIMER. Reference herein to any specific commercial product, process. or service by trade name trademark, manufacturer, or otherwise, does not necessarily constitute or imply Rs endorsement, recommendation. or favoring by the United States Government or any agency thereof or its contractors or subcontractors

Prinlea n tne LnRed Stales of Amerca To onain copies of this OocLmenl. contact DocLment Contro Serv ces P 0 Box 950 Mailstop ri6CB. Richland WA 99352. Pnone (5091 372-2420, Fax (509) 37649

4 I 15 I94 Release Approval bate I

DATE: HANFORD

GLUJ Release StamD

Approved For Public Release

A-6400073.1 (1w97)

( 1 ) Document Nunber RECORD OF REVISION

QUALITY ASSURANCE OBJECTIVES FOR NONDESTRUCTIVE ASSAY AT THE WRAP F A C I L I T Y

I I

I

I I I

A-7320.005 (08/91) UEF168

_.

HNF-405 1, Revision 2

Quality Assurance Objectives for Nondestructive Assay at the Waste Receiving and Processing Facility

Craig Wills and Michael G. Cantaloub, Waste Management Hanford

HNF 4051 Rev. 2 I

Executive Summary

The Waste Receiving and Processing (WRAP) facility, located on the Hanford Site in southeast Washington, is a key link in the certification of transuranic (TRU) waste for shipment to the Waste Isolation Pilot Plant (WIPP). Waste characterization is one of the vital functions performed at WRAP, and nondestructive assay (NDA) measurements of TRU waste containers is one of two required methods used for waste characterization. The WIPP Quality Assurance Program Plan (WIPP-QAPP) specifies a series of quality assurance objectives (QAOs) which each NDA system must meet before a site can be certified to ship TRU waste to WIPP. These QAOs ensure that systems meet minimum standards for measurement parameters such as precision and accuracy.

This report summarizes the validation of the WRAP NDA systems against the various QAOs. A brief description of each test and any significant conclusions is included. Variables which may have affected test outcomes are examined. This report will be reviewed semi-annually and updated as necessary.

HN F 40s I

Table of Contents

Rev. 2 -

.. Executive Summary ......................................................................................................................... 11

Table of Contents ..................... Introduction ..... . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . .. . . . . . .. . .. . . . . . . . .. . .. . .. . . . 1 Descnption of Tests ...................................................................................................................... 4 Summary of IPAN A Tests - Accuracy, Precision and Bias ......................................................... 6 Summary of GEA A Tests - Accurancy, Precision and Bias ..................................................... 10 Summary of IPAN Tests - Minimum Detectable Concentration ............................................... 14 Summary of GEA A Tests - Minimum Detectable Concentration ........................................... 15 Discussion of Results .................................................................................................................. 16 Future Considerations .................................. .................................................... ........................... 18 Attachments . . . . . . . . . .. . . . . . . . .. . . . . . . . . .. . . . . . .. . .. . . . . . .. .. . .. . . . . . . . .. . . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . ._ . . . .

... . . . . . , . . . . . .................................................................. 111

. .

... 111

HNF4051 Rev.2

Introduction

The WRAP facility has four primary NDA systems: two imaging passive/active neutron (IPAN) systems and two gamma energy assay (GEA) systems. The two IPAN units are identical, as are the GEA units, thus the systems are designated as follows: IPAN A, IPAN B, GEA A, and GEA B. This report documents the conformance of IPAN A and GEA A to the precision, accuracy and minimum detectable concentration (MDC) NDA QAOs for WIPP. The total measurement uncertainty (TMU) QAO required for each system is addressed in a separate document (HNF 4050).

WIPP sets forth four nominal testing points for NDA. Although these are normally defined in alpha curies, they are also defined in grams of Pu-239. Due to the nature of available sources, WRAP uses the nominal Pu gram quantities for testing. This report documents testing of the IPAN A and GEA A systems at the 0.1 g, 1 .O g, 10 g, and 160 g levels for the precision and accuracy QAOs. MDCs for the IPANs and GEA-A are also reported. The MDC QAO is predominately determined from instrument background evaluations. As such, no TRUiradioactive sources were required for the MDC QAO.

Precision and Accuracy

To comply with QAO requirements, facilities must determine precision and accuracy values obtained for 15 replicate measurements of waste containers containing known quantities of TRU isotopes at the nominal test points. This must be done for each system which is to be certified. The equations used to determine these values, tabulated later in this report, are listed below.

Equation 1 calculates precision as the %RSD of the distribution of 15 replicate measurements:

S % RSD= = * 100

Y

where

%RSD = percent relative standard deviation; s = standard deviation; y = mean of the replicate measurements.

Equation 2 determines the standard deviation:

where s = standard deviation; Yi = the measured value of the i" replicate measurement; Y = the mean of the replicate measurements; n = the number of replicate measurements.

Equation 3 determines the accuracy for a standard reference material as percent recovery:

I

HNF 405 1 Rev. 2

C % R = A * 1 0 0 C s m

where

%R = percent recovery; Cm = Cvm=

average result of the 15 replicate determinations; known value for the waste container used in the measurements.

The minimum detectable concentration (MDC) provides the smallest concentration of material which can be detected with 95% confidence, while also having 95% confidence that “activity” is not detected falsely from a null sample. For an MDC determined from a blank - a drum with as similar a matrix as an expected sample but with no known activity added - the calculated value is an a priori estimate of the best sensitivity that can be expected from the sample measurements and conditions. When MDC is determined from an actual sample specbum, the background at the energy or region of interest will most likely be higher. This increase is due to the continuum generated by Compton scattering and by bremsstrahlung. Thus the MDC from an actual sample, calculated a posleriori, is expected to be slightly higher than the a priori estimate. WRAP is required to demonstrate compliance with the MDC for methods and systems used to discriminate between TRU and LLW or methods and systems used to define a waste stream as TRU.

Satisfaction of the MDC QAO requires the MDC be determined from the appropriate relationship using nominal facility values and the data collected from 15 replicate measurements performed on an appropriate waste container. Equation 4 gives the expression for determining MDC:

MDC =KlK,(2.71+4.65*s,)

where

KI = the proportionality constant relating the detector response (counts) to the activity, such as,K =l/e where e is an overall detection efficiency, or K = 1/I& where I, is the gamma ray emission probability per decay and q is the detection efficiency for the gamma ray;

the factor which relates the total activity determined by the measurement system to an activity concentration in waste under a given set of measurement conditions, for example, the weight of waste assayed and a self-adsorption correction;

K2 =

Sb = the standard deviation or uncertainty of the background.

For calculating the MDC, the variance or standard deviation of the background is determined by the expression:

2

HNF 4051 Rev. 2 I

where

counts =

CR =

Tc =

the total counts acquired in the region of interest for a photon of energy E;

count rate in the region of interest for a photon of energy E(cps);

count time for the assay (second)

Substituting appropriate terms for the GEA system into Equation 4 yields the final expression for determining the MDC on the GEA system:

where

CR(W =

Tc

e(&) =

I(&) =

M =

37 =

count rate in the region of interest for a photon of energy E (cps);

count time for the assay (second);

the detection efficiency for the photon of energy E (countsiphoton);

yield or intensity for the photon of energy E(photon/second);

mass of the drum matrix (8);

conversion factor relating decays per second to nCi (dpsinci);

- ~

A similar expression is used to determine the MDC for the IPAN system for 'active mode' operation:

(2.71 + 4 . 6 5 G )

(IR)( WGE)(12.3)(1 0-9)M MDC =

where

[CBKGD]'' = overall background uncertainty in light matrix background counts for the 28 detector bundles (counts);

instrument fissile material conversion factor for a light matrix (counts/g Pu-239);

weapons grade Pu enrichment conversion factor (g Pu-239/ g WGPu);

IR =

WGE =

3

HNF 405 1 Rev. 2

Source Pu Quantity QAo19 ID (grams)

NTP-0068 0.03

12.3 = weapons grade Pu to Ci Pu conversion factor (g WGPdCi - typical value for Hanford waste);

mass of the drum matrix (g); M =

10-9 = Ci to nCi conversion.

QAOZO qa021 QA024 QAO-W21

T1, P3 T2,PlO

DescriDtion of Tests

NTP-0070 NTP-0075 NTP-0077 NTP-0084 NTP-0089


For testing of the NDA systems against the WIPP QAO requirements, the PDP “combustibles” matrix drum was loaded with sources to approximate the nominal test points. The combustibles drum was selected because it is the nearest approximation to the prevalent waste matrix for WRAP. The table below shows the arrangement of sources within the test drum. The test arrangement number (e.g., QA021) is shown in the next section where specific test results are tabulated.

0.03 T2, P1S T3,P19 t1,p0 0.03 T3, P18 0.03 Tl,PO T1P9 0.03 Tl,Pl8 0.30 T2, P6

NTP-0091 NTP-0098 NTP-0 103

0.30 T3, P6 0.30 T3,PO 0.30 T233

NTP-0119 NTP-0126

WRAP-2KiPU

NTP-0105 1 0.30 1 T1,PlS I T1,PlS 1 NTP-0112 I 3.00 I T1. P6 I I 1 1

3.00 T2, P1S 3.00 T3, P1S 5.00 T3, P19

A

HNF 405 1 Rev. 2

The “T” and “ P references are to tube number and pin height, respectively. Tube 1 is centered in the drum, while tube 2 is located about halfway between the center and the outer wall of the drum. Tube 3 is located near the outer wall of the drum, opposite tube 2. The pin numbers refer to height (in inches) above the bottom of the drum at which the source is placed. The sources are composed of Pu dispersed in diatomaceous earth, doubly enclosed in concentric stainless steel cylinders. They are nine inches long and about two inches in diameter.

The GEA system MDC was determined by using the daily operations checks background drum (drum ID: GEABKGD). The drum has a matrix density that most closely approximates the present WRAP waste stream. No activity was added (Le. a confounding matrix) as current waste streams contain few fission products or radioactive components other than Pu and Am. Data was acquired for 15 replicate counts on the GEABKGD drum using the WRAP operating procedures for the GEA system (WRPl- OP-0906).

No background measurements were conducted on the IPAN for use in determining the MDC. The data required to calculate the MDC for active IPAN analysis can he found in the active matrix library file, KEHam. This file contains the value of the fissile signal background for each of the 28 grouped detector packages, the error associated with each background value, as well as the fissile signal value per 0.500 g Pu-239 for each detector package and the 20 defined spatial locations. The K E H a m file is stored on the instrument with the IPAN system files and is accessed during sample analysis. The MDC calculation is based on the ‘‘light’’ matrix library file, the most non-interfering matrix for which the system is calibrated. Being identically built, both IPANs use the same KEHamx file, and therefore the MDC calculation applies to both IPAN A and IPAN B.

Test Results

Results for the IPAN and GEA systems are presented in tabular form on the following pages. Tables for the precision and accuracy QAOs (IPAN then GEA) are given first, followed by the MDC results for the IPAN and GEA-A system.

5

HNF4051 Rev.2 I

QAO-W21 IPAN A

Summary of IPAN A Tests - Accuracv. Precision and Bias

IPAN A 160.00 g Pu (160 g nominal test value) 93.8% Pu-239

Pu-239 Mass %Actual Pu- (9) 239 Value

Run 1 1

Pu-239 7.54EM1 50.25

Pu-239 I 7.54E+01 I 50.27

Pu-239 7.47EM1 49.76 Pu-239 7.54EM1 50.26 Pu-239 7.42EMl 49.46 Pu-239 7.44EM1 49.56

Run 10 Pu-239 49.96

Run 13 Run 14 Run 15

Pu-239 7.62E+01 50.76 Pu-239 7.62E+01 50.79 Pu-239 7.45E+01 49.67

I I I 1 Averaee I Pu-239 I 7.52E+01 I 50.08

%R = 50.08

6

HNF 405 I Rev. 2

QA019

Run 1 Run 2 Run 3 Run 4

_____ IPAN A Pu-239 Mass %Actual Pu-

(8) 239 Value

Pu-239 1.03E+01 111.71 Pu-239 1.03E+01 111.38 Pu-239 I .04E+OI 112.14 Pu-239 1.04E+01 112.57

Run 5 Pu-239 I 1.05E+01 I 113.33 Run 6 I Pu-239

Average 1 Pu-239 I I.O4E+Ol I 111.96

std dev = 6.30E02 Precision I % RSD = n.61

~~~~ ....

Accuracy 1 %R = 11 1.96 TotalBias 1 110.84% (Low) to 113.33% (High)

7

HNF 405 1 Rev. 2

IPAN A 0.99 g Pu (1 .O g nominal test value) 94% Pu-239

QA020 IPAN A Pu-239 Mass % Actual Pu- (9) 239 Value

Average I Pu-239 1 9.62601 1 103.91

Accuracy

std dev = 6.0SE-02 Precision I % RSD = 6.29

% R = 103.91 Total Bias

8

94.53% (Low) to 114.51% (High)

HNF 405 1 Rev. 2

QA02 1 IPAN A Pu-239 Mass YO Actual Pu- (8) 239 Value

Run 1 Run 2 Run 3 Run 4 Run 5

Run 13 I Pu-239 I 7.69E-02 I 91.38 Run 14 1 Pu-239 I 7.80E-02 I 92.69

Pu-239 8.1 OE-02 96.26 Pu-239 1 .04E-O 1 123.95 Pu-239 8.96E-02 106.48 Pu-239 8.99E02 106.83 Pu-239 9.02E-02 107.19

~

Run 15 I Pu-239 I 8.54E-02 I 101.49 1 I I

Precision

, I I

Average 1 Pu-239 I 8.59E-02 I 102.12

% RSD = 12.23 I standard deviation = 1.05E-02

Total Bias 77.84% (Low) to 123.95% (High)

9

HNF 4051 Rev. 2 I

QAO-W2 1 Sum Seg Pu-239 Mass Activity (8)

(PCi)

Run 1 7.38EM6 1.19EM2

Summary of GEA A Tests - Accuracv and Precision

GEA A 160.00 g Pu (160 g nominal test value) 93.8% Pu-239

% Actual Pu- Comb All Pu-239 Mass %Actual h- 239 Value Activity (g) 239 Value

(KO __

79.26 7.68E+06 1.24EM2 82.48 Run 2 Run 3 Run 4 Run 5 Run 6

7.33EM6 1 . I 8E+02 78.72 7.69E+06 1.24E+02 82.59 7.39EM6 1.19EM2 79.37 7.64E+06 1.23E+02 82.05 7.41 E+06 1 .19E+02 79.58 7.80E+06 1.26E+02 83.77 7.30E+06 I . 1 8E+02 78.40 7.60E+06 1.23E+02 81.62 7.36E+06 1 .19E+02 79.05 7.73E+06 I .25E+02 83.02

Run 7 1 7.32E+06 I 1.18E+02 1 78.62 I 7.58E+06 I 1.22E+02 1 81.41 Run 8 I 7.34E+06 1 1.18E+02 1 78.83 1.23E+02 1 81.95

Precision Accuracy * Total Bias

Run 10 I 7.34E+06 I 1.1

std dev = 7.39E-01 % RSD = 0.62

78.08% (Low) to 79.69% (High)

std dev = 1.28E+00 % RSD = 1.03

80.66% (Low) to 83.77% (High) %R =78.83 %R = 82.35

- . . . ._ - - . . Run 15 I 7.27E+06 I 1.17E+02 I 78.08 I 7.51E+06 I 1.21E+02 I 80.

I I I I I 1 Average I 7.34E+06 I 1.18EM2 I 78.83 1 7.67EM6 1 1.24EM2 I 82.35

. ... ..

HNF 405 1 Rev. 2

GEA A 9.90 g Pu (10 g nominal test value) 94% Pu-239

Precision Accuracy * Total Bias

stddev = 1.26E-01 % RSD = 1.74

74.48% (Low) to 80.02% (High)

stddev = 1.44E-01 % RSD = 1.65

90.24% (Low) to 96.13% (High) %R = 71.17 %R =93.69

HNF 4051 Rev. 2

GEA A 0.99 g Pu (1.0 g nominal test value) 94% Pu-239

Precision

Total Bias Accuracy *

Run 15 1 4.64E+04 1 7.48E-01 1 80.37 I 4.90EM4 I 7.90E01 I 84.87 I I I I I I

std dev = 8.78E-02 % RSD = 12.25

46.25% (Low) to 85.56% (High)

std dev = 6.25E-02 % RSD = 7.80

71.53% (Low) to 97.34% (High) %OR = 77.03 %OR = 86.06

Average 1 4.45E+04 1 7.17E-01 I 77.03 1 4.97EM4 I 8.01E-01 I 86.06

QA024 Sum Seg Pu-239 Mass %Actual Pu- Comb All Pu-239 Mass % Actual h- Activity (8) 239 Value Activity (g) 239 Value

(PCO (KO

Run 6 1 3.59E+03 5.79E-02 I 68.71 I 4.28E+02 I 6.90E-03 I 8.20 Run 7 1 2.68E+03 1 4.32E-02 1 5 I .33 I 4.96E102 I 7.99E-03 I 9.50

Run 1 Run 2 Run 3 Run 4 Run 5

4.32EM3 6.9 6 E 0 2 82.75 I .14E+03 1.84E-02 21.84 4.33E+03 6.98E-02 82.94 4.33E+03 6.98E-02 82.94 4.53E+03 7.30E-02 86.77 1.02E+03 1.64E-02 19.54 4.46E+03 7.19E-02 85.43 1 .12E+03 1.8 1 E-02 2 I .45 3.68E+03 5.93E-02 70.49 5.1 5Ei-02 8.30E-03 9.86

13

Run 8 Run 9 Run 10 Run I 1 Run 12

3.71 E+03 5.98E-02 71.06 1 . 5 5 ~ ~ 3 2.50E-02 29.69 4.50E+03 7.25E-02 86.20 1.42EM3 2.29E-02 27.20 3.72E+03 6.00E-02 71.26 3.72E+03 6.OOE-02 71.26 4.75E+03 7.66E-02 90.98 4.75E+03 7.66E-02 90.98 5.22E+03 8.4 1 E-02 99.99 9.87E+02 1.59E-02 18.91

HNF 4051 Rev. 2 I

Summary of IPAN Tests - MDC

As mentioned previously, no background measurements were required for determining the IPAN MDC. The background information and instrument response factors are contained in the system operating files and were supplied by the manufacturer The uncertainty in the average neutron background for the 28 neutron detector bundles obtained from the active matrix library file is

==63 counts

The total instrument response is 237,529 counts per gram Pu-239 for the light matrix. The Pu-239 weapons grade enrichment (WGE) is 0.94, while the nominal matrix mass for a low-density or light matrix material is 15.6 kg.

Using these values and the expression derived for the IPAN yields and MDC of

[2.71+ 4.65(63)Eounts 237_529counts)[ - 0.94gPu239)( 12.3g W G P L I ] ~ ~ O ~ ~ O - ~ O C / / nCi 115,600g))

MDc=(( gPu239 g WGPu Ci Pu

MDC = 6.9nCiig

14

~ . . . .

HNF4051 Rev.2 I

Average Std dev + 20

Summary of GEA A Tests - MDC

GEA A Minimum Detectable Concentration

5.68 0.027 Average 8.34 39 0.601 0.001 5 Std dev 0.88 2.2 6.88 0.030 i 20 10.1 1 44

Measurements performed on “GEABKGD drum Nominal count time for drum assay is 300 seconds Nominal mass for 55-gallon (208 L) drum containing a low density matrix is 15,600 grams

15

.

HNF 405 I Rev. 2

Discussion of Results

The following table, taken from Table 9-1 of HNF-2599, Final Hunford Site Transuranic Waste Churacterization Quality Assurance Project Plan, shows the requirements for QAO validation.

Nominal compliance Parameter

Range of waste point activity in a-Curies” PrecisionC Accuracyd Total biase Completeness‘ MDC a-Curies” (g WG P u ) ~ (%RSD) (%R) (”/.I (%) (nCi/g)

>0.02 to 0.2

>0.2 to 2.0 High 300

High 150

a Applicable range of TRU activity in a 208-L (55-gal.) waste container to which the QAOs apply, units are Curies of alpha-emiding TRU isotopes with half-lives greater than 20 years.

The nominal activity (or weight of Fu) in the 208-L (55-gal.) waste container used to demonsbate that QAOs can be achieved for the corresponding range in column I , values in parentheses are the approximate equivalent weights of WG Pq 15 years a%r purification; for purposes of demonstrating QAOs, “nominalll means within 10 percent.

One standard deviation based on I5 replicate measurements o f a noninterfering matrix.

Ratio of measured to known values based on the average of 15 replicate measurements of a noninterfering matrix.

95 percent confidence bounds for system bias established by studies to determine contributions to total unce6nly from all significant sources. Units are confidence bound divided by true value, expressed as a percent. Requirement for the QAO for total uncertainly is to determine and document

Valid radioassay data are required for all waste containers.

b

e

It should be noted that a noninterfering matrix is a virtual impossibility. In the case of W”, a light (debris or combustibles) matrix was used; while the interference of this matrix is relatively small, it exists nonetheless. Of greater concern are the test sources themselves. Even if an empty drum matrix was used, the two walls of stainless steel surrounding the Pu source material do attenuate both neutron and gamma flux. The physics behind the neutron attenuation are obvious. The primary energy line used for gamma detection of Pu-239 is 414 keV, but at extremely low mass levels (such as 0.lg) the yield fraction of the 414 keV gamma is too low to be consistently detectable. At these mass values, the primary energy line becomes 129 keV, since it has a significantly higher yield fraction than the 414 keV line. This relatively low (129 keV) energy line can be easily attenuated by the encapsulating steel walls of the source. A preliminary review of test results shows this effect to be about 10-15%.


Comparison of the results tabulated earlier against the requirements listed above shows that both systems under test pass easily at the two middle points tested (1 g and 10 g). The GEA “Combine All

16

HNF 4051 Rev. 2

Results” fails at the 0.1 g level, and the IPAN fails at the 160 g level. For the IPAN units, only the active assay results are reported. As improvements are made to the passive algorithms, the passive results will be tested and documented as necessary. For the GEA units, the “Combine All Results” algorithm is preferred at all save the lowest gram levels; at approximately 0.5 g Pu the “Sum Segments” algorithm takes over. In the GEA, “Sum Segments” is also preferred for a lumped source up to about 2 g Pu. The table below summarizes the results, and shows the operating range for each system and for each method or algorithm. Results outside these ranges require validation through further testing. Refer to HNF-5140, Validation Data for NDA Systems ut WRAP, for details and supporting analysis.

Nominal Pu Value

0.10 g 1.00 g

10.0 g I60 g

Pu Mass WAN GEA Range Active Passive Combine All Sum Segments

0- 0.25 g I’;1ss U!\ Fail I%lSS

0.25 - 2.5 g I?lSS \1/ \ I?lSS I’ass 2.5-25g 1,. .lhS Ni.\ I’nss I’ms

> 2 5 g Fail \,‘?I I’ess I’ass

All testing was performed using the WRAP operating procedures for the IPAN and GEA systems (WRP1-OP-0905 and WRP1-OP-0906, respectively). The standard operating software for the systems was used to acquire data and report results. Testing was performed for 55-gallon (208 liter) waste drum configurations only.

For these results to be valid, full independence of source materials must be maintained. The QAO tests are performed using plutonium sources, each with its own pedigree and documentation. The IPAN units were calibrated using depleted uranium and californium sources, while the GEA calibrations utilize mixed sources containing cobalt, barium, cesium, and americium. No sources used in calibration are used in any testing.

MDC

The GEA-A MDC satisfies the 60 nCi/g QAO requirement. The average MDC from the replicate background runs is 39 nCUg for Pu-239 as determined from the region of the 129 keV line and 0.026 nCi/g for Am-241 using the 59.6 keV line. The low MDC for Am-241 is not surprising given the high yield and relatively high detection efficiency for the 59.6 keV photon. Similar to the GEA precision and accuracy requirements, at low plutonium masses the 129 keV photon becomes the dominant photon for the purpose of analysis. The calculated MDCs correspond to absolute TRU masses of 10 mg Pu-239 and 0.1 pg Am-241 respectively. MDC’s based on other regions of the spectrum (Le U- 235 at 185.7 keV) were not evaluated as Pu-239, and to a lesser extent Am-241, is the dominant waste stream isotope.

The IPAN MDC was determined to be 7 nCUg based on the background uncertainty and fissile signal data file for a light density matrix obtained from the IPAN active matrix library. The MDC is valid essentially for Pu-239 as that is the predominant waste stream isotope and the primary fissile nuclide detected during active operation of the IPAN-A system.

17

HNF 405 1 Rev. 2 I

Future Considerations

As further testing is completed this report will be revised to include validation of the IPAN B and GEA B systems at all four levels. QAO tests will be performed periodically as called out in WMH- 350 Section 2.4. Testing will be repeated annually, as a minimum, in order to meet the QAPjP (Section 9.5) requirement that “calibrations are verified for at least one counting geomebylsample matrix combination on an annual basis.”

HNF 405 1 Rev. 2 1

Los Alamos National Laboratory Ctrtificate of content anb Erateatiritp

Pu02-Diatomaceous Earth Standard WRAP-2 5.0GPU

Thls M)A standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this W R i i a re listed below. Complete information regarding the P u and Am content, Pu isotopic ratios, chemical composition, eiemental impurities, containment, and fabrication procedures are retained-in files by the Los Alamos National Laboratory CMR Analytical Chemistry Group.

NUCLEAR MATERIAL CONTENT

The nuclear material content and total alpha activity for this standard a re listed below. Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component.

Component PuOz in standard

P u Assay Pu in standard

I4'Am Assay "'Am in standard

Quantity o r Value 5.71060 grams

5.01 168 grams 1128.9 pg/g PuOz*

5.66 mg*

87.761 %'of PuOz*

95 % CI * 0.00021 grams

I O . 0 8 1 % (b) & 0.00472 grams ('I

i 0.3 pg/g (dl

t. 0.04 mg (')

Isotopic Weight Fraction*

'38Pu

"9Pu

"""

'"PU

0.00014

0.93809

0.05939

0.00185

0.00054

I0.000005 ('

i 0.000015('

I 0.000007 ('

i 0.000009 (o

i 0.000003 ('

Total Alpha Activity in standard 342.5 mCi** 1.267E+10 Bq I 3E+07 Bq I 5 0.9 m c i (E)

I *Decay corrected value on 1/21/99 ** Effective 1/21/99

Mi!&+ Robert S. Marshall, Project Manager EDA WRM Production

19

-. -I_.

HNF 405 1 Rev. 2 I

MEASUlUCMIShT METHOD AM) TRACEABILITY

The nuclear COOtCdb of this standard were characterized and quantaed wing the following methods with traceabaty to the National Institute of Standards and Technology (NIST) or New Bruoswick Laboratory (NBL) standards.

Measurement Measurement Method Reference Material

Wcighlng 5 place analytical balance NIST traceable weights h Assay Controlled Potential Coulometry NBL CRM # 126 Am &Y Isotope Dilution Mass Spectrometry NJ3L CkM # 128

Pu Isotopic Total Evaporation Mass Specirometry NBL CRM # 128 Alpha Activity Calculated from Pu and Am ms, and

isotope alpha specific activities listed below. Pu tln as stated for NET S W 4 6

Am tyl as stated for NET SILM4322B

338 3a9 The stated Alpha Activity was calculated using tbe.following isotope half lives (in years): 24,119; Pu: 6,560; ’“Pu: 14.34; Pu: 387,000; and ’“Am: 432.2.

PU: 87.74; Pu: 140 142

NOTES

Random and systematic error teims were combined and reported as 95% confidence intervals. Error t e r m include estimates of the following:

(a) Balance precision, buoyancy, standard wcight bias, and transfer lass. (b) Long and short term precision, control check bias, weighing precbion and bias (c) Above weighing and assay terms, and transfer lass (d) Long a n d short term precision, and bias. (e) Above wcighing t e rm, Am assay terms, and transfer loss. (0 Long and short term precision, and bias. (g) Based on propagated uncertainties on the PU mass, “‘Am mass and PU isotopic uncertainties M e d

above. No half-life uncertainty components a r e included and it is recommended that all facilities participating i n tbc hD.4 PDP program use the half-lives b t e d above to preclude Eacility-to-facility

’crror t c r m introduced by using different half life values.

20

HNF 405 I Rev. 2

Los Alamos National Laboratory Certificate of Content anb. QLrateabiIitp

Pu02-Diatomaceous Earth Standard WRAP-3 5.0GPU

This NDA standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this WRM are listed below. Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition, clemental impurities, . containment, and fabrication procedures are retainedjn files by the Los Alamos Nalional Laboratory CMR Analytical Chemistry Group.


The nuclear maferial content and total alpha activity for this standard a re listed below. Also listed are overall uncertainty estimates a t 95% confidence intervals (CI) for each component.

ComDoncnt PuO, i n standard

Pu Assay Pu in standard

'"Am Assay "'Am in standard

Quantity o r Value 5.69429 grams

4.99736 grams 1128.9 pg/g Pu02*

5.64 mg*

87.761 Yo ofPuO,*

95 Yo CI * 0.00031 grams ('I

* 0.081 % (b) * 0.00476 gra'ms ('I

6 0.3 pglg * 0.04 mg (')


"'Pu

l'9PU

lraP u

'I'PU

'41Pu

0.00014

0.93809

0.05939 '

0.00185

0.00054

,* 0.000005 (0

* 0.000015 (0

* 0.000009 (0 * 0.000007 "

i 0.000003

Total Alpha Activity i n standard 311.5 mCi'* 1.263Ec10 Bq

i 0.9 mCi (e) 3E+07 Bq ('I

'Decay corrected value on 1121199 ** Eflcctive 1/21/99

B i d J h & erlev, G r o u D h e a b r C h R Analyticai C h e m l i t w

obert S. Marshall, LU&,L3 Project Manager

NDA WRM Production

21

HNF4051 Rev.2

MEASUREMJZNT METHOD AND TRACEABILITY

The nuclear contents of this standard were characterized and quantified wing the following methods with traceability to the National Institute of Standards and Technology (NIST) or New Brunswick Laboratory (NBL) standards.


Wcighlng 5 place analytical balance NlST traceable weights Pu Assay Controlled Potential Coulometry NBL CRM # 126 Am k Y Isotope Dilution Mass Spectrometry NBL CiRM # 128 Pu Isotopic Total Evaporation Mass Spectrqinetry NBLCRM#128

Alpha Activity Calculated from Pu and Am ma%, and isotope alpba specific activities listed below.

hr tln as stated for NIST SRM946 Am tin as stated for NIST

SRM4322B

ud The stated Alpha Activity WPS calcula!ed using the following isotope half lives (in years): 24,119; "'PP,: 6,560; Pu: 14.34; Pu: 387,000; and"'Am: 432.2.

Pu: 87.74; "$u: 141 242

=S

Random and systematic c r ror t e r m were combined and reported as 95% confidence intervals. Er ror terms include estimates of the following:

(a) Balance precision, buoyancy, standard weight bias, and transfer loss. (b) Long and short term precision, control check bias, weighing precision and bias. (c) Above weighing and assay terms, and transfer loss. (d) Long and short term precision, and bias. (e) Above wcighig terms, Am assay terms, and transfer loss. (0 Long aod short term precision, and bias. (s) Based on propagated unccrtaintics on the Pu mass, "'Am mass and h isotopic uncertainties listed

above. No half-life uncertainly components a re inclnded and i t is recommended that all iacilitiea participating in the ND.4 PDP program use the half-lives listed above to preclude facilitY-td.WiliQ'

. crror t e r m introduced by using different half Life values.

22

HNF 405 I Rev. 2 J

Los Alamos National Laboratory Certifitate of amtent anb. QhateabiIifp

Pu02-Diatomaceous Earth Standard WRAPlOGPU

This NDA standard contains high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content of this WRM are listed below. Complete information regardinz the Pu and Am content, Pu isotopic ratios, chemical composition, elemental impurities, containment, and fabrication procedures a re retained i n files by the Los Alamos National Laboratory CMR Analytical Chemlrtry Group.

' ' NUCLEAR MATERIAL CONTENT

The nuclear material content and total alpha activity for this standard are listed below. Also listed a re overall uncertainty estimates a t 95% confidence intervals (CI) for each component.

Component Quantity o r Value 95 % CI PuO, in standard 11.40156 grams * O.OOOd9 grams ('I

P u in standard 10.00612.grams & 0.00945 grams(') Pu Assay 87.761 % of PuOi* * 0.081 % @)

"'Am Assay 1128.9 pg/gPuOl* * 0.3 pp/p (dl

,'"Am in standard 11.30 mg* * 0.09 mg+)

Isotoptc Weigh1 Fraction*

a'aPu 0.00014 * 0.000005

"'PU 0.93809 i 0.000015 ('

"OPU 0.05939 * 0.000007 "

l"Pu 0.00185 * 0.000009

XPu 0.00054 f 0.000003 ('

* 1.8 mCi (8'

* 7Et07 Bq (') Total Alpha Activity in standard 683.7 mCi**

2.530E+10 Bq

*Decay corrected value on 1/21/99 * & Effective 1/21/99

NDA WRM Production

23

_I . . . ..... .. . . . . . -. -

HNF 405 1 Rev. 2

MFASZTREMENT METHOD AND TRACEABILITY

The nuclear contenB of thic standard were characterized and quantified using the following methods with traceability to the National Institute of Standards and Technology (NIST) or New Brunswick Laboratory (NBL) standards.


W e i gh i n g

Pu &say Controlled Potential Coulometry NBL CRM # 126

5 place analytical balance NISI Paceable weigbh

A m - Y Isotope Dilution Mass Spectrometry Pu Isotopic Tolal Evaporation Mass SpecG9inett-j

NBL CRh? # 128

N B L c R M # 1 2 8 Alpha Activity Calculated &om Pu and Am ma, and

isotope alpha specific activities listed below. Pu tlp. as stated for NIST SRM946

Am tm as stated for NIST SRM4322B

118 The stated Alpha Activity was calculated using the following isotope half lives (in years): 24,119; "'Pu: 6,560; F'u: 14.34; "hu: 387,000; and "'Am: 432.2.

PU: 87.74; "'PU: I41

NOTES

Random and systematic error terms were combined and reported as 95% confidence intervals. E r ro r t e r m include estimates of the following:

(a) Balance precision, buoyancy, standard weight bias, and transfer loss. (b) Long and short term precision, control check bias, weighing precision and bias. (c) Above weighing and assay terms, and transfer loss. (d) Long and sbort term precision, and bias. (e) Above wc igh ig terms, Am assay terms, and transfer loss. (r) Long and short term precision, and bias. (s) Based on propagated uncertainties on the Pu mass, Am mass and Pu &topic uncertainties listed

above. No half-life uncertainty components are inclnded and i t is recommended that all facilities participating in the NDA PDP program use the half-lives listed above to preclude facilitY-t*&cmQ' crror terms introduced by using different half Life values.

1 4 1

24

HNF4051 Rev.2 I

Los Alamos National Laboratory UCertifitate of (Eontent anb ZErateabiIitp

Pu02-Diatomaceous Earth Standard WRAPZOGPU

This NDA standard contalns high purity plutonium dioxide dispersed in diatomaceous earth. Quantitative information and uncertainties on the nuclear content or this WRM are listed below. Complete information regarding the Pu and Am content, Pu isotopic ratios, chemical composition, elimental Impurities, contalnment, and fabrication procedures are retained .in files by the LQS Alamos National Laboratory CMR Analytical Chemistry Group.


The nuclear material content and total alpha activity for thls standard a re listed below. Also listed a re overall uncertainty estimates a t 95% confidence intervals (CI) for each component.

Component Quantity or Value 95 % (71

Pu Assay 87.761 % of PuO,* * 0.081 % (b)

PuOl in standard 22.19925 grams f 0.00062 grams (I)

Pu In standard 20.00884 grams rt 0.01875 grams '"Am Assay 1128.9 pg/gPu02* * 0.3 pg/g (d)

"'Am in standard 22.59 mg* i 0.17 mg ('I


'"PU

u9Pu

lroPu

IJiPU

'JzPu

0.00014

0.93809

0.05939

0.00185

0.00054

* 0.000005 (r)

f 0.000015 (O

rt 0.000007 (O

* 0.000009 (0

i 0.000003

Total Alpha Activity in standard 1367 mCi** 5.059E+10 Bq

i 4 m ~ i (9)

i 1E+08 Bq (e)

*Decay corrected value on 3/21/99 ** Effective 1121199

' * Kerley,Gro p eader CMR Analytical C h e m w y

--,. J Robert S. Marshall, Project Manage M)A WRM Production

HNF 405 1 Rev. 2

MEASUREMENT METHOD AND TRACEABILITY

The nuclear content8 of this standard were characterized and qnantified midg the following methods with traceability to the National Institute of Standards and Technology (NET) o r New B w m k k Laboratory (NEIL) standards.


Wcighing 5 place analytical balance NISI' traceable weights Pu Assay Controlled Potential Coulometry NBL CRM # 126 Am Isotope Dilution Mass Spectrometry NBL CR&5 # 128

Pu Isotopic Total Evaporation Mess Spectrometry NBL CRM # 128 Alpha Activity Calculated from Pu and Am mass, and

isotope alpha specific activities listed below. Pu tln as stated for NIST SRM946

Am tm as stated for NIST rnX4322B

lJ8 a9 ,The stated Alpha Activity was calculated using the following lrotope half lives (in years): Po: 87.74; PU:

140 mi 142 24,119; Pu: 6,560; Pu: 14.34; Pu: 387,000; and '"Am: 432.2.

NorES

Random and systematic error tcrms wcre combined and reported as 95% confidence intervals. Error terms include estimates of the following:

(a) Balance precision, buoyancy, standard wcight bias, and transfer loss. (b) Loug and short term precision, control check bias, weighing precision aud b i a s (c) Above weighing and assay terms, and transfer loss. (d) Long and short term precision, and bias. (e) Above weighing terms, Am assay terms, and transfer loss. (0 Long and short term precision, and bias. (9) Based on propagated uncertainties on the Pu mass, "'Am m a s s and Pu isotopic uncertainties listed

above. No balf-life uncertainty component$ a re included and it is recommended tha t all facilities participating in thc NDA PDP p r q r a m use the half-lives W e d above to preclude facility-t*faCxV

' crror tcrms introduced by using different half Life values.

26

DISTRIBUTION SHEET ~

To

D i s t r i b u t i o n

From Page 1 of 1 WRAP Engineer ing Date 09/14/99

MG Cantaloub

JK Kersten

JA Maupin

MA Purce l l

WR Thackaberry

CE Tay lo r

JR Weidert

CE W i l l s

DOE/RL Reading Room

Engineer ing F i l e s

Project Title/Work Order

WRAP Q A O ' s FOR NDA, HNF-4051, Rev. 2

T4-52

T4-52

T4-06

T6-50

T4-52

T4-52

T4-52

T4-52

H2-53

81-07

EDTNo. N/A

ECN NO. ECN-651739

X

X

X

X

Name

x X

X

X

Text Text Only Attach./ EDT/ECN MSlN With All Appendix Only

Attach. Only

A-6000-135 (01/93) UEF067

_.. ... . . . ~ . . __