EPA REGION V SAMPLE CONFIRMATION FORM · PDF fileEPA REGION V SAMPLE CONFIRMATION FORM ... (COCs, tags, SAS PLs, etc.) ... dates of each preparation step, with associated weights

EPA Region 5 Records Ctr.

217001

EPA REGION VSAMPLE CONFIRMATION FORM

FAX THIS COMPLETED FORM TO BRIAN P. FREEMAN AT US EPAby TUESDAY of the PRECEEDIN6 WEEK BY 12 NOON! (312) 353-4342

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* ALL SAS WORK Scheduled through the Region REQUIRES 3-4 veeks lead time, and anapproved SAS form.

NOTIFY THE FOLLOWING PERSONS PRIOR to SHIPMENT, FOR CONFIRMATION

RAS - Roger NowakOWSki (SMO) (703) 519-1353SAS - (If Scheduled through Region) - Cecilia Luckett

(312) 886-1488

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PE92H322

U.S. ENVIRONMENTAL PROTECTION AGENCYCLP Sample Management Office SAS NO.P.O. Box 818 - Alexandria, Va. 22313Phone: (703) 557-2490

SYNTHETIC PRECIPITATION LEACHING PROCEDUREFOR SEMIVOLATILE ORGANIC COMPOUNDS AND PESTICIDE/PCBS

FOR THE MIDCO TREATABILITY STUDY SOIL SAMPLESSPECIAL ANALYTICAL SERVICES

Client Request

Regional Transmittal Telephone Request

INTRODUCTION

A. EPA Region and Client: Region V, U.S. EPA

B. Regional Representative: Richard Boice, Remedial ProjectManager

C. Telephone Number: (312) 886-4740

D. Date of Request: April 11, 1995

E. Site Name: Midco I and Midco II, Gary, Indiana

DESCRIPTION OF WORK

1. General description of analytical service requested under thisSAS:

The work under this Special Analytical Services Request (SAS) willbe part of a treatability study being conducted by U.S. EPA toevaluate the effectiveness of soil treatment by solidification/stabilization (S/S) at the Midco I and Midco II hazardous wastesites. This SAS provides for analysis of semivolatile organiccompounds (SVOCs) and Pesticide/PCBs in the extract from theSynthetic Precipitation Leaching Procedure (SPLP) for bothuntreated soils and for for the S/S matrix after treatment.

Leachate from the soil and S/S matrix samples shall be generatedusing the Synthetic Precipitation Leaching Procedure (SPLP), Method1312, November 1990 from proposed update to SW-846 (a copy of thisis attached). The laboratory shall analyze the SPLP extracts forthe Target Compound (TCL) List of SOCs and pesticide/PCBs. The SASfor the SOCs and pesticide/PCBs in the SPLP are being combinedbecause these fractions can utilize the same extraction fluid. Itis also possible to use the same SPLP extraction as used for themetals.

The TCL is from Exhibit C of OLMO1.0. The analysis of the extractsfor SOCs and pesticide/PCBs shall be conducted in accordance with

the most recent version of OLM01.0, subject to the modificationslisted in item 7 below.

2. Definition and number of work units: 26 samples plus 3duplicates

3. Purpose of analysis: The overall objective of the study is toevaluate the potential effectiveness of soil treatment by S/S foruse in remedial actions at the Midco I and Midco II Superfundsites, to define final performance standards, and to evaluate theperformance of a number of binders.

4. Estimated date of sample collection: The untreated soilsamples were collected in August 1993, and were treated with thebinders in August 1993. The treated samples were cured at roomtemperature under humid conditions for 30 days and then placed intoglass bottles with Teflon lined caps for shipment to CRL foranalysis. CRL collected the needed amount of sample for theiranalyses and then returned the remainder of the sample to the glassjars.

5. Estimated dates and method of shipment: Since the time ofanalysis, the samples have been in storage at CRL at roomtemperature in the glass jars. CRL is requested to obtain thesamples from storage for these additional analyses.

6. Schedule and reporting:

In accordance with Method 1312 (Section 6.6) , the laboratory shouldanalyze the SPLP extract as soon as possible following extraction,but in any event the laboratory shall meet the following deadlines:

solvent extraction for the SOCs and pesticide/PCBs in the SPLPextracts shall be completed within 7 days of generation of theSPLP extracts;

analyses of all solvent extracts must be completed within 40days of generation of the SPLP extract (or earlier asnecessary to meet the deadline in the following item);

all analyses must be complete and the data package containingthe analytical results submitted to U.S. EPA, Region V byJune 30, 1995. The data package must include original copiesof all sampling handling documentation (COCs, tags, SAS PLs,etc.) and data.

7. Analytical protocol and special technical instructions:

Leachate from the soil samples and S/S matrix samples shall begenerated using the Synthetic Precipitation Leaching Procedure(SPLP), Method 1312, November 1990 from the proposed addition toSW-846 (see attachment) with the following modifications and

conditions:

a. The instructions in Sections 1.2, 1.3, and 1.4 of Method 1312should be disregarded;

b. The laboratory shall not correct the measured values of theorganic compounds for the MS/MSD results as provided for inSection 8.2.5 of the SPLP.

c. Extraction fluid #1 shall be used for SPLP extractions forSOCs and pesticide/PCBs (Section 5.4 of Method 1312). Thisextraction may be combined with the SPLP extraction formetals. The laboratory shall make sure that a large enoughportion of the soil sample is extracted to generate enoughextract for all the analyses including the MS/MSD analyses.

d. For the untreated soils samples, the filtration procedure(Sections 7.1.1.3-7.1.1.7 of Method 1312) may producefiltrate. For the filtration procedure, the laboratory shallnot discard water collecting on top of a soil sample, but thiswater shall be mixed with the sample prior to filtration. TheSPLP extracts may be a combination of liquid filtrate andsolid SPLP extract (Sections 7.2.13.2 and 7.3.14 of Method1312) .

e. For the samples treated by S/S, the size reduction step in7.1.3 of the SPLP must be implemented. The equipment to beused should be determined following inspection of the samples.A mortar and pestle or hammer and chisel may be appropriate.

The leachate generated by the SPLP shall be analyzed in accordancewith the most recent version of OLM01.0 for SOCs and pesticide/PCBs(this includes the sample handling, storage and chain-of-custodyrequirements) with the following modifications and conditions:

a. The same SPLP extraction can be used to analyze both SOCs,pesticide/PCBs, and metals.

b. The operations in OLM01.0 to identify or quantify tentativelyidentified compounds need not be conducted;

c. The laboratory shall prepare matrix spike/matrix spikeduplicate sample (MS/MSD) using a portion of one of the SPLPextracts in each Group. The MS/MSD level in the SPLP extractshall be set at ten times the contract required quantitationlevel (CRQL) for each target organic compound (Section 8.2).

d. Data requirements and QC requirements are further summarizedon Attachment 1.

8. Reporting and documentation of results:

Reporting and documentation of results shall be in accordance withthe requirements of Method 1312, and the most recent version ofOLM01.0 as appropriate, with the following additions:

The laboratory shall report any problems in sample preparationin the case narrative;

The laboratory shall utilize and prepare sample preparationlogs to record all variables in sample preparation providedfor in Method 1312, including (but not necessarily limitedto) :

weights of extracted samples (25 gram minimum for 100%solids);volume of any filtrate obtained;parameters for determination of percent solids;dates of each preparation step, with associated weightsand measured volumes.

Any QA/QC problem should be discussed with the RemedialProject Manager to help determine whether corrective action isneeded.

The schedule for submission of the samples data summarypackage is revised as described in Item 7 above.

9. Other:

10. Name of sampling/shipping contact:

Richard Boice, Remedial Project Manager, HSRL-6JU.S. EPA, Region V77 West Jackson St.Chicago, II. 60604(312) 886-4740

ATTACHMENT 1

I. DATA REQUIREMENTS

PARAMETERS: Target Compound List of SOCs and pesticide/PCBs inExhibit C of the most recent version of OLM01.0.

QUANTISATION LIMITS: As required in OLM01.0 for SOCs andpesticide/PCBs.

DUPLICATE PRECISION DESIRED: As provided for in OLM01.0 for SOCs,and pesticide/PCBs.

SURROGATES: Surrogates of OLM01.0 are required.

II. QC REQUIREMENTS

The laboratory shall perform all QC requirements of OLM01.0 exceptas noted below.

AUDITS

Blanks forextraction fluid.This will replacethe required methodblanks.

Surrogates

MS/MSD

FREQUENCY

Per OLM01.0

Each blank and eachSPLP extract fororganic

Per OLM01.0

LIMITS*

Less than theCRQLs .

Per OLM01.0 fororganics

As defined inOLM01.0


SYNTHETIC PRECIPITATION LEACHING PROCEDURE FOR METALSFOR MIDCO TREATABILITY STUDY SAMPLES

AFTER TREATMENT BY SOLIDIFICATION/STABILIZATION (S/S)SPECIAL ANALYTICAL SERVICES

Client Request


INTRODUCTION

A. EPA Region and Client: Region V, U.S. EPA





DESCRIPTION OF WORK


The work under this Special Analytical Services Request (SAS) willbe part of a treatability study being conducted by EPA to evaluatethe effectiveness of soil treatment by solidification/stabilization(S/S) at the Midco I and Midco II hazardous waste sites. This SASprovides for analysis of metals in the extract from the syntheticprecipitation leaching Procedure (SPLP) for both untreated soilsand for the S/S matrix after treatment. The results will be usedto evaluate the performance of S/S.

The laboratory shall generate extracts from the untreated soils,and from the S/S matrix using the Synthetic Precipitation LeachingProcedure (SPLP), Method 1312 (leaching fluid #1), November 1990from proposed update to SW-846 (a copy of this is attached). Thelaboratory shall analyze the SPLP extract for metals in accordancewith ILM02.0.

2. Definition and number of work units: 26 samples plus 3duplicates

3. Purpose of analysis:

The overall objective of the study is to evaluate the potentialeffectiveness of soil treatment by S/S for use in remedial actionsat the Midco I and Midco II Superfund sites, to define finalperformance standards for the S/S, and to evaluate the performanceof a number of binders. The metals of primary concern inevaluating the effectiveness of the S/S are: arsenic; barium;cadmium; chromium; copper; lead; nickel; vanadium; and zinc.



6. Schedule:

In accordance with Method 1312 (Section 6.6), the laboratory mustanalyze the SPLP extract as soon as possible following extraction.It is requested that CRL extract and analyze the samples, submitthe Sample Data Package, submit the data in computer readable form,and complete the SDG file by June 30, 1995.


The laboratory shall generate leachate from the S/S samples usingprocedures in the Synthetic Precipitation Leaching Procedure(SPLP), Method 1312, November 1990 from the proposed addition toSW-846 (see attachment) with the following modifications andconditions:

a. The laboratory shall disregard the instructions in Sections1.2, 1.3, and 1.4 of Method 1312.

b. Extraction fluid #1 shall be used for the SPLP extracts thatwill be analyzed for metals (Method 1312, Section 5.4.1). Thesame SPLP extraction can be used for the metals and for theSVOCs and pesticide/PCBs. The laboratory shall make sure thata large enough portion of the soil sample is extracted to

generate enough extract for all the analyses including thematrix spike analyses.

c. For the samples treated by S/S, the size reduction step in7.1.3 of the SPLP must be implemented. The equipment to beused should be determined following inspection of the samples.A mortar and pestle or hammer and chisel may be appropriate.

The laboratory shall analyze the SPLP extracts using procedures inthe most recent version of ILM02.0 (including sample handling,storage and chain-of-custody requirements) for inorganics(excluding cyanide and mercury) with the following modificationsand conditions:

a. Precise results for the SPLP before and after treatment areneeded to determine the percentage reductions for arsenic,barium, cadmium, chromium, copper, lead, nickel, vanadium, andzinc. The results for the other metals are only being usedas background information and screening purposes. Therefore,analysis of the metals other than those listed above shallonly be by ICP only, even if the detection limit goals ofILM02.0 are not met. Since precise results are needed, it isunacceptable to analyze undigested extract as suggested inSection 7.2.14 of Method 1312 to determine whether it is aboveor below a regulatory limit.

b. The laboratory need only prepare matrix spikes for thefollowing parameters: arsenic; barium; cadmium; copper; lead;nickel; vanadium; and zinc. The laboratory shall prepare onematrix spike. The matrix spike level in the SPLP extractshall be set at ten times the contract required detectionlimits (CRDL) for arsenic, barium, chromium, and lead. Thematrix spike level shall be set at five times the CRDL forcadmium, copper, nickel, and vanadium. The spike level shallbe set at 100 times the CRDL for zinc. The purpose of thesedilutions is so that the spiked sample will be in the generalrange of the concentration limits listed on the attached Table1. If the leachate after treatment with a given binder meetsthe concentration limits or the percentage reductions listedin Table 1, the binder satisfies the Minimum PerformanceStandards for the S/S treatment.

f. The laboratory shall not correct the measured values of themetals for the spiked sample results as provided for in Method1312, Section 8.2.5. Since the untreated samples have beenweathered for many years, and the treated samples aresolidified, the SPLP extract is not expected to have high TDS.However, the results should be screened for the potential needto correct for matrix effects using the MS/MSD results, andinterelement corrections made as needed. The need for anyunusual procedures should be discussed with the RemedialProject Manager. If it is determined that reanalysis of some

samples is necessary because of the potential need to correctfor matrix affects, EPA will notify the laboratory of thesamples that need to be reanalyzed and the spike levels thatshall be used.

g. The laboratory shall dilute all samples to within thecalibration range even if reanalysis is required.

h. The laboratory shall use the furnace technique if necessarypursuant to the most recent version of ILM02.0 for thefollowing metals: arsenic; cadmium; chromium; and lead.

i. The SPLP extracts for metals shall be preserved byacidification to a pH less than 2 unless precipitation occurs(Method 1312, Sections 6.6 and 7.2.14). If precipitation isobserved upon addition of nitric acid to a small aliquot ofthe extract, then the remaining portion of the extract formetals analyses shall not be acidified and the extract shallbe analyzed as soon as possible (Method 1312, Section 7.2.14).

j. Data requirements and QC requirements are further summarizedon Attachment 1.


Reporting and documentation of results shall be in accordance withthe requirements of Method 1312 and the most recent version ofILM02.0 subject to the revisions noted in item 7 above and thefollowing additions:



weights of extracted samples (25 gram minimum for 100%solids);volume of any filtrate obtained;preliminary evaluation of percent solids;parameters for determination of percent solids;dates of each preparation step, with associated weightsand measured volumes.

Any QA/QC problems should be discussed with the RemedialProject Manager to help determine whether corrective action isneeded.

9. Other:

5



ATTACHMENT 1


PARAMETERS: Target Analyte List of metals in Exhibit C of the mostrecent version of ILM02.0 excluding cyanide and mercury.

DETECTION LIMITS: As required in ILM02.0 for the following metals:arsenic; barium; cadmium; chromium; copper; lead; nickel; vanadium;and zinc. For the other metals whatever detection limit isattained using the ICP will be acceptable. If necessary, detectionlimits can be compromised to make necessary background corrections.

DUPLICATE PRECISION DESIRED: As provided for in ILM02.0.

II. QC REQUIREMENTS

The laboratory shall perform all QC requirements of ILM02.0 asmodified by item 8 except as noted below.

AUDITS

Analyze extractionfluid blank, andanalyze preparationblank usingextraction fluid.

Spiked samples(SPLP extractsspiked)

FREQUENCY

One for eachdelivery group orbatch.

One for eachdelivery group orbatch.

LIMITS

Less than CRDL, orless than 10% ofthe concentrationlimits listed inTable 1 (attached) .

As defined inILM02.0.

30

Alternatively, the SPLP trMted can be reduced to the following

Concentration Limits. If SPLPra- MMte is below a Concentration

Limit listed below, no further reduction of leachate

concentration is required, although the treated sample should

not increase* such leachate concentration above the

concentration limit.

CONCENTRATION

LIMIT fua/1)

50

2000

5

100

43

15

100

233

1150

CONSTITUENT

arsenic

barium

cadmium

chromium

copper

lead

nickel

vanadium

zinc

STABILIZATION

T4&L E 1,PERCENTAGE

REDUCTION

90

90

95

95

95

99

95

90

90

OF ORGANICS

Using total waste analyses (using methylene chloride

extraction for semivolatile organics, and methanol extraction

for volatile organics), a 50% reduction in concentrations

shall be attained based on total waste analyses of the sample

of untreated waste (TWApaMMtste ) and the sample treated by S/S

(TWA trottd ) calculated in accordance with the formula:


SYNTHETIC PRECIPITATION LEACHING PROCEDUREFOR CYANIDE

FOR THE MIDCO TREATABILITY STUDY SOIL SAMPLES (GROUP 3)SPECIAL ANALYTICAL SERVICES

Client Request


INTRODUCTIONA. EPA Region and Client: Region V, U.S. EPA





DESCRIPTION OF WORK


The work under this Special Analytical Services Request (SAS) willbe part of a treatability study being conducted by U.S. EPA toevaluate the effectiveness of soil treatment by solidification/stabilization (S/S) at the Midco I and Midco II hazardous wastesites. This SAS provides for analysis of cyanide in the extractfrom the synthetic precipitation leaching Procedure (SPLP) for bothuntreated soils and for the S/S matrix after treatment. Theresults will be used to evaluate the performance of S/S.

Leachate from the untreated soil samples and from the S/S matrixsamples shall be generated using the Synthetic PrecipitationLeaching Procedure (SPLP), Method 1312, November 1990 from proposedupdate to SW-846 (a copy of this is attached) . The laboratoryshall analyze the SPLP extract for cyanide. Cyanide in the SPLP isbeing analyzed separately because it requires a differenceextraction fluid than the other inorganic compounds. The analysesof the extracts for cyanide shall be in accordance with the mostrecent version of ILM02.0.

2. Definition and number of work units: 13 samples plus twoduplicates.

3. Purpose of analysis: The overall objective of the study is toevaluate the potential effectiveness of soil treatment by S/S foruse in remedial actions at the Midco I and Midco II Superfundsites.



6. Schedule and reporting:

In accordance with Method 1312 (Section 6.6), the laboratory shouldanalyze the SPLP extract as soon as possible following extraction,but in any event the laboratory shall meet the following deadlines:

all analyses must be complete and the data package containingthe analytical results submitted to U.S. EPA, Region V within35 days of generation of the last SPLP extract within a sampledelivery group, or by June 30, 1995, whichever is earlier.The data package must include original copies of all samplinghandling documentation (COCs, tags, SAS PLs, etc.) and data.


Leachate from the soil samples and the S/S matrix shall begenerated using the Synthetic Precipitation Leaching Procedure(SPLP), Method 1312, November 1990 from the proposed addition toSW-846 (see attachment) with the following modifications andconditions:

a. The instructions in Sections 1.2, 1.3, and 1.4 of Method 1312should be disregarded;

b. The particle size reduction step (Section 7.3.6 of Method1312) shall implemented for the S/S matrix samples, but is notexpected to be needed for the untreated soil samples.

c. To test samples for CN, the laboratory must conduct theextraction in a zero head space extraction (ZHE) vessel andutilize ZHE extract collection and transfer devices (Sections4.2.1, 4.3.1, 4.6 of Method 1312).

d. Extraction fluid #3 shall be used for the SPLP extracts thatwill be analyzed for cyanide (Section 5.4 of Method 1312) .The reagent water used for the extraction must meet theconditions identified in both Sections 5.2.1 and 5.2.2.

e. For the untreated soil samples, the filtration procedure(Sections 7.1.1.3-7.1.1.7 of Method 1312) may producefiltrate. For the filtration procedure, the laboratory shallnot discard water collecting on top of a soil sample, but thiswater shall be mixed with the sample prior to filtration. TheSPLP extracts may be a combination of liquid filtrate andsolid SPLP extract (Sections 7.2.13.2 and 7.3.14 of Method1312) .

The leachate generated by the SPLP shall be analyzed in accordancewith the most recent version of ILM02.0 for cyanide (this includesthe sample handling, storage and chain-of-custody requirements)with the following modifications and conditions:

a. Data requirements and QC requirements are further summarizedon Attachment 1.


Reporting and documentation of results shall be in accordance withthe requirements of Method 1312, the most recent version of ILM02.0as appropriate, and with the following:



weights of extracted samples (25 gram minimum for 100%solids);volume of any filtrate obtained;parameters for determination of percent solids;dates of each preparation step, with associated weightsand measured volumes.

Any QA/QC problem should be discussed with the RemedialProject Manager to help determine whether corrective action isneeded.

The schedule for submission of the samples data summarypackage is revised as described in Item 7 above.

9. Other:

4



ATTACHMENT 1


PARAMETERS: cyani de.

QUANTITATION LIMITS: As required in the most recent version ofILM02.0.

DUPLICATE PRECISION DESIRED: As provided for in ILM02.0.

II. QC REQUIREMENTS

The laboratory shall perform all QC requirements of ILM02.0 exceptas noted below.

AUDITS

Blanks forextraction fluid.This will replacethe required methodblanks.

MS/MSD

FREQUENCY

Per ILM02.0.

Per ILM02.0

LIMITS

Per ILM02.0

Per ILM02.0.

Documents

EPA REGION V SAMPLE CONFIRMATION FORM · PDF fileEPA REGION V SAMPLE CONFIRMATION FORM ... (COCs, tags, SAS PLs, etc.) ... dates of each preparation step, with associated weights