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METHOD 3060A

ALKALINE DIGESTION FOR HEXAVALENT CHROMIUM1.0SCOPE AND APPLICATION

1.1Any reference in this method to “Method 3060\" refers to this version of that method,

and does not refer to previously published versions (e.g., in the Second Edition of this manual).When published as a new method to SW-846, a method’s number does not include a letter suffix.Each time a method is revised and made a part of SW-846 update, it receives a suffix. However,a method reference found within the text of SW-846 methods always refers to the latest version ofthat method published in SW-846, even if the method number at that location does not include theappropriate letter suffix.

1.2Method 3060 is an alkaline digestion procedure for extracting hexavalent chromium

[Cr(VI)] from soluble, adsorbed, and precipitated forms of chromium compounds in soils, sludges,sediments, and similar waste materials. To quantify total Cr(VI) in a solid matrix, three criteria mustbe satisfied: (1) the extracting solution must solubilize all forms of Cr(VI), (2) the conditions of theextraction must not induce reduction of native Cr(VI) to Cr(III), and (3) the method must not causeoxidation of native Cr(III) contained in the sample to Cr(VI). Method 3060 meets these criteria fora wide spectrum of solid matrices. Under the alkaline conditions of the extraction, minimal reductionof Cr(VI) or oxidation of native Cr(III) occurs. The addition of Mg2+ in a phosphate buffer to thealkaline solution has been shown to suppress oxidation, if observed. The accuracy of the extractionprocedure is assessed using spike recovery data for soluble and insoluble forms of Cr(VI) (e.g.,K2Cr2O7 and PbCrO 4), coupled with measurement of ancillary soil properties, indicative of thepotential for the soil to maintain a Cr(VI) spike during digestion, such as oxidation reduction potential(ORP), pH, organic matter content, ferrous iron, and sulfides. Recovery of an insoluble Cr(VI) spikecan be used to assess the first two criteria, and method-induced oxidation is usually not observedexcept in soils high in Mn and amended with soluble Cr(III) salts or freshly precipitated Cr(OH)3.1.3The quantification of Cr(VI) in Method 3060 digests should be performed using a

suitable technique with appropriate accuracy and precision, for example Method 7196(colorimetrically by UV-VIS spectrophotometry) or Method 7199 (colorimetrically by ionchromatography (IC)). Analytical techniques such as IC with inductively coupled plasma - massspectrometric (ICP-MS) detection, high performance liquid chromatography (HPLC) with ICP-MSdetection, capillary electrophoresis (CE) with ICP-MS detection, etc. may be utilized onceperformance effectiveness has been validated. 2.0

SUMMARY OF METHOD

2.1This method uses an alkaline digestion to solubilize both water-insoluble (with the

exception of partial solubility of barium chromate in some soil matrices, see Reference 10.9) andwater soluble Cr(VI) compounds in solid waste samples. The pH of the digestate must be carefullyadjusted during the digestion procedure. Failure to meet the pH specifications will necessitateredigestion of the samples.

2.2The sample is digested using 0.28M Na2CO3/0.5M NaOH solution and heating at 90-95EC for 60 minutes to dissolve the Cr(VI) and stabilize it against reduction to Cr(III).

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2.3The Cr(VI) reaction with diphenylcarbazide is the most common and reliable method

for analysis of Cr(VI) solubilized in the alkaline digestate. The use of diphenylcarbazide has beenwell established in the colorimetric procedure (Method 7196), in rapid-test field kits, and in the ionchromatographic method for Cr(VI) (Method 7199). It is highly selective for Cr(VI) and fewinterferences are encountered when it is used on alkaline digestates.

2.4For additional information on health and safety issues relating to chromium, refer to

References 10.7 and 10.10.3.0

INTERFERENCES

3.1When analyzing a sample digest for total Cr(VI), it is appropriate to determine the

reducing/oxidizing tendency of each sample matrix. This can be accomplished by characterizationof each sample for additional analytical parameters, such as pH (Method 9045), ferrous iron (ASTMMethod D3872-86), sulfides (Method 9030), and Oxidation Reduction Potential (ORP) (ASTM MethodD 1498-93 - aqueous samples). Method 9045 (Section 7.2 of Method 9045) is referenced as thepreparatory method for soil samples. The ORP and temperature probes are inserted directly into thesoil slurry. The displayed ORP value is allowed to equilibrate and the resulting measurement isrecorded. Other indirect indicators of reducing/oxidizing tendency include Total Organic Carbon(TOC), Chemical Oxygen Demand (COD), and Biological Oxygen Demand (BOD). Analysis of theseadditional parameters establishes the tendency of Cr(VI) to exist or not exist in the unspikedsample(s) and assists in the interpretation of QC data for matrix spike recoveries outsideconventionally accepted criteria for total metals.

3.2Certain substances, not typically found in the alkaline digests of soils, may interfere

in the analytical methods for Cr(VI) following alkaline extraction if the concentrations of theseinterfering substances are high and the Cr(VI) concentration is low. Refer to Methods 7196 and7199 for a discussion of the specific agents that may interfere with Cr(VI) quantification. Analyticaltechniques that reduce bias caused by co-extracted matrix components may be applicable incorrecting these biases after validation of their performance effectiveness.

3.3For waste materials or soils containing soluble Cr(III) concentrations greater than four

times the laboratory Cr(VI) reporting limit, Cr(VI) results obtained using this method may be biasedhigh due to method-induced oxidation. The addition of Mg2+ in a phosphate buffer to the alkalineextraction solution has been shown to suppress this oxidation. If an analytical method for Cr(VI) isused that can correct for possible method induced oxidation/reduction, then the Mg2+ addition isoptional. The presence of soluble Cr(III) can be approximated by extracting the sample withdeionized water (ASTM methods D4646-87, D5233-92, or D3987-85) and analyzing the resultantleachate for both Cr(VI) and total Cr. The difference between the two values approximates solubleCr(III).4.0

APPARATUS AND MATERIALS4.14.24.3

Digestion vessel: borosilicate glass or quartz with a volume of 250 mL.Graduated Cylinder: 100-mL or equivalent.

Volumetric Flasks: Class A glassware, 1000-mL and 100-mL, with stoppers orequivalent.

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4.44.5

Vacuum Filtration Apparatus.

Filter membranes (0.45 µm). Preferably cellulosic or polycarbonate membranes.When vacuum filtration is performed, operation should be performed with recognitionof the filter membrane breakthrough pressure.

Heating Device - capable of maintaining the digestion solution at 90-95EC withcontinuous auto stirring capability or equivalent.

Volumetric pipettes: Class A glassware, assorted sizes, as necessary.Calibrated pH meter.Calibrated balance.

Temperature measurement device (with NIST traceable calibration) capable ofmeasuring up to 100EC (e.g. thermometer, thermistor, IR sensor, etc.).

An automated continuous stirring device (e.g. magnetic stirrer, motorized stirring rod,etc.), one for each digestion being performed.

4.64.74.84.94.104.11

5.0

REAGENTS

5.1Nitric acid: 5.0 M HNO3, analytical reagent grade or spectrograde quality. Store at

20-25EC in the dark. Do not use concentrated HNO3 to make up 5.0 M solution if it has a yellowtinge; this is indicative of photoreduction of NO3- to NO 2, a reducing agent for Cr(VI).5.2Sodium carbonate: Na2CO3, anhydrous, analytical reagent grade. Store at 20-25ECin a tightly sealed container.

5.3Sodium hydroxide: NaOH, analytical reagent grade. Store at 20-25EC in a tightly

sealed container.

5.4Magnesium Chloride: MgCl2 (anhydrous), analytical reagent grade. A mass of 400

mg MgCl2 is approximately equivalent to 100 mg Mg2+. Store at 20-25EC in a tightly sealedcontainer.

5.5

Phosphate Buffer:5.5.15.5.2

K2HPO4: analytical reagent grade.KH2PO4: analytical reagent grade.

5.5.30.5M K2HPO4/0.5M KH 2PO4 buffer at pH 7: Dissolve 87.09 K 2HPO4 and 68.04

g KH2PO4 into 700 mL of reagent water. Transfer to a 1L volumetric flask and dilute tovolume.

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5.6Lead Chromate: PbCrO4, analytical reagent grade. The insoluble matrix spike is

prepared by adding 10-20 mg of PbCrO4 to a separate sample aliquot. Store under dry conditionsat 20-25EC in a tightly sealed container.

5.7Digestion solution: Dissolve 20.0 ± 0.05 g NaOH and 30.0 ± 0.05 g Na2CO3 in

reagent water in a one-liter volumetric flask and dilute to the mark. Store the solution in a tightlycapped polyethylene bottle at 20-25EC and prepare fresh monthly. The pH of the digestion solutionmust be checked before using. The pH must be 11.5 or greater, if not, discard.

5.8Potassium dichromate, K2Cr2O7, spiking solution (1000 mg/L Cr(VI)): Dissolve 2.829

g of dried (105EC) K2Cr2O7 in reagent water in a one-liter volumetric flask and dilute to the mark.Alternatively, a 1000 mg/L Cr(VI) certified primary standard solution can be used (Fisher AASstandard or equivalent). Store at 20-25EC in a tightly sealed container for use up to six months.

5.8.1Matrix spiking solution (100 mg/L Cr(VI)): Add 10.0 mL of the 1000 mg

Cr(VI)/L made from K2Cr2O7 spiking solution (Section 5.8) to a 100 mL volumetric flask anddilute to volume with reagent water. Mix well.

5.9Reagent Water - Reagent water will be free of interferences. Refer to Chapter One

for a definition of reagent water.6.0.

SAMPLE COLLECTION, PRESERVATION, AND HANDLING

6.1Samples must have been collected using a sampling plan that addresses the

considerations discussed in Chapter Nine of this manual.

6.2Samples should be collected using devices and placed in containers that do not

contain stainless steel (e.g., plastic or glass).

6.3

Samples should be stored field-moist at 4 ± 2EC until analysis.

6.4Hexavalent chromium has been shown to be quantitatively stable in field-moist soil

samples for 30 days from sample collection. In addition, Cr(VI) has also been shown to be stablein the alkaline digestate for up to 168 hours after extraction from soil.

6.5Hexavalent chromium solutions or waste material that are generated should be

disposed of properly. One approach is to treat all Cr(VI) waste materials with ascorbic acid or otherreducing agent to reduce the Cr(VI) to Cr(III). For additional information on health and safety issuesrelating to chromium, the user is referred to References 10.7 and 10.10.7.0

PROCEDURE

7.1Adjust the temperature setting of each heating device used in the alkaline digestion

by preparing and monitoring a temperature blank [a 250 mL vessel filled with 50 mLs digestionsolution (Section 5.7)]. Maintain a digestion solution temperature of 90-95EC as measured with aNIST-traceable thermometer or equivalent.

7.2Place 2.5 ± 0.10 g of the field-moist sample into a clean and labeled 250 mL

digestion vessel. The sample should have been mixed thoroughly before the aliquot is removed.CD-ROM

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For the specific sample aliquot that is being spiked (Section 8.5), the spike material should be addeddirectly to the sample aliquot at this point. (Percent solids determination, U.S. EPA CLP SOW forOrganic Analysis, OLM03.1, 8/94 Rev.) should be performed on a separate aliquot in order tocalculate the final result on a dry-weight basis).

7.3Add 50 mL ± 1 mL of digestion solution (Section 5.7) to each sample using a

graduated cylinder, and also add approximately 400 mg of MgCl2 (Section 5.4) and 0.5 mL of 1.0Mphosphate buffer (Section 5.5.3). For analytical techniques that can correct for oxidation/reductionof Cr, the addition of Mg2+ is optional. Cover all samples with watch glasses.

7.4Stir the samples continuously (unheated) for at least five minutes using an

appropriate stirring device.

7.5 Heat the samples to 90-95EC, then maintain the samples at 90-95EC for at least 60

minutes with continuous stirring.

7.6Gradually cool, with continued agitation, each solution to room temperature. Transfer

the contents quantitatively to the filtration apparatus; rinsing the digestion vessel with 3 successiveportions of reagent water. Transfer the rinsates to the filtration apparatus. Filter through a 0.45µmmembrane filter. Rinse the inside of the filter flask and filter pad with reagent water and transfer thefiltrate and the rinses to a clean 250-mL vessel.

NOTE: The remaining solids and filter paper resulting from filtration of the matrix spike inSection 7.6 should be saved for possible use in assessing low Cr(VI) matrix spike recoveries.See Section 8.5.2. for additional details. Store the filtered solid at 4 ± 2EC.

7.7Place an appropriate stirring device into the sample digest beaker, place the vessel

on a stirrer, and, with constant stirring, slowly add 5.0 M nitric acid solution to the beaker dropwise.Adjust the pH of the solution to 7.5 ± 0.5 if the sample is to be analyzed using Method 7196 (adjustthe pH accordingly if an alternate analytical method is to be used; i.e. 9.0 ± 0.5 if Method 7199 is tobe used) and monitor the pH with a pH meter. If the pH of the digest should deviate from the desiredrange, discard the solution and redigest. If overshooting the desired pH range occurs repeatedly,prepare diluted nitric acid solution and repeat digestion procedure. If a flocculent precipitate shouldform, the sample should be filtered through a 0.45 µm membrane filter. If the filter becomes cloggedusing the 0.45 µm filter paper, a larger size filter paper (Whatman GFB or GFF) may be used toprefilter the samples.

CAUTION: CO2 will be evolved. This step should be performed in a fume hood.

7.8Remove the stirring device and rinse, collecting the rinsate in the beaker. Transfer

quantitatively the contents of the vessel to a 100 mL volumetric flask and adjust the sample volumeto 100 mL (to the mark for the volumetric flask) with reagent water. Mix well.

7.9The sample digestates are now ready to be analyzed. Determine the Cr(VI)

concentration in mg/kg by a suitable technique with appropriate accuracy and precision, for exampleMethod 7196 (colorimetrically by UV-VIS spectrophotometry) or Method 7199 (colorimetrically by ionchromatography (IC)). Another analytical technique such as IC with inductively coupled plasma -mass spectrometric (ICP-MS) detection, high performance liquid chromatography (HPLC) with ICP-

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MS detection, capillary electrophoresis (CE) with ICP-MS detection, etc. may be utilized onceperformance effectiveness has been validated.

7.10 CALCULATIONS

7.10.1Sample Concentration

Concentration =

where:A

BCDE

=====

A x D x E------------ B x C

Concentration observed in the digest (µg/mL)Initial moist sample weight (g)% Solids/100Dilution Factor

Final digest volume (mL)

7.10.2Relative Percent Difference

RPD =where:S

D

(S - D)-------------[(S + D)/2]==

Initial sample resultDuplicate sample result

7.10.3Spike Recovery

Percent Recovery

=

(SSR - SR)SA

where:SSR

SRSA

8.0

QUALITY CONTROL

===

Spike sample result

Sample (unspiked) resultSpike added

x 100

8.1The following Quality Control (QC) analyses must be performed per digestion batch

as discussed in Chapter One.

8.2A preparation blank must be prepared and analyzed with each digestion batch, as

discussed in Chapter One and detected Cr(VI) concentrations must be less than the methoddetection limit or one-tenth the regulatory limit or action level, whichever is greater or the entire batchmust be redigested.

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8.3Laboratory Control Sample (LCS): As an additional determination of method

performance, utilize the matrix spike solution prepared in Section 5.8.1 or the solid matrix spikingagent PbCrO4 (Section 5.6) to spike into 50 mL of digestion solution (Section 5.7). Alternatively, theuse of a certified solid reference material (if available) is recommended. Recovery must be withinthe certified acceptance range or a recovery range of 80% to 120% or the sample batch must bereanalyzed.

8.4 A separately prepared duplicate soil sample must be analyzed at a frequency of one

per batch as discussed in Chapter One. Duplicate samples must have a Relative Percent Difference(RPD) of < 20%, if both the original and the duplicate are > four times the laboratory reporting limit.A control limit of ± the laboratory reporting limit is used when either the original or the duplicatesample is < four times the laboratory reporting limit.

8.5Both soluble and insoluble pre-digestion matrix spikes must be analyzed at a

frequency of one each per batch of < 20 field samples. The soluble matrix spike sample is spikedwith 1.0 mL of the spiking solution prepared in Section 5.8.1 (equivalent to 40 mg Cr(VI)/Kg)) or attwice the sample concentration, whichever is greater. The insoluble matrix spike is prepared byadding 10-20 mg of PbCrO4 (Section 5.6) to a separate sample aliquot. It is used to evaluate thedissolution during the digestion process. Both matrix spikes are then carried through the digestionprocess described in Section 7.0. More frequent matrix spikes must be analyzed if the soilcharacteristics within the analytical batch appear to have significant variability based on visualobservation. An acceptance range for matrix spike recoveries is 75-125%. If the matrix spikerecoveries are not within these recovery limits, the entire batch must berehomogenized/redigested/reanalyzed. If upon reanalysis, the matrix spike is not within the recoverylimits, but the LCS is within criteria specified in Section 8.3, information such as that specified onFigures 1 and 2 and in Section 3.1 should be carefully evaluated . The Cr(VI) data may be valid foruse despite the perceived \"QC failure.\" The information shown on Figure 1 and discussed belowis provided to interpret ancillary parameter data in conjunction with data on spike recoveries.

8.5.1 First measure the pH (Method 9045) and Oxidation Reduction Potential (ORP)

(ASTM Method D 1498-93 - aqueous samples, Method 9045 preparatory for soil samples),in the field if possible. If not possible, the measurements are to be made in the laboratoryprior to the determination of the spike recovery data. When and where the measurementsare taken must be noted by the analyst. Adjust the ORP measurement based on referenceelectrode correction factor to yield Eh values. The pH and Eh values should be plotted onFigure 2 in order to give an initial indication of the sample’s reducing/oxidizing nature. Uponcompletion of the analysis of the analytical batch, the LCS should be evaluated. If the LCSis not within 80 - 120% recovery or the certified acceptance range, then the entire analyticalbatch (plus the QC samples) should be redigested and reanalyzed. If the LCS was withinacceptance criteria and the pre-digestion matrix spike recoveries for Cr(VI) were less thanthe acceptance range minimum (75%), this indicates that the soil samples reduced Cr(VI)(e.g., anoxic sediments), and no measurable native Cr(VI) existed in the unspiked sample(assuming the criteria in Section 8.3 are met). Such a result indicates that the combined andinteracting influences of ORP, pH and reducing agents (e.g., organic acids, Fe2+ and sulfides)caused reduction of Cr(VI) spikes. Characterize each matrix spike sample for additionalanalytical parameters, such as ferrous iron (ASTM Method D3872-86), and sulfides (Method9030). Laboratory measurements of pH and ORP should also be performed to confirm thefield measurements. Other indirect indicators of reducing/oxidizing tendency include TotalOrganic Carbon (TOC), Chemical Oxygen Demand (COD), and Biological Oxygen Demand(BOD). Analysis of these additional parameters assists in evaluating the tendency of Cr(VI)

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to exist or not exist in the unspiked sample(s) and assists in the interpretation of QC data formatrix spike recoveries outside conventionally accepted criteria for total metals.

A value of Eh-pH below the bold diagonal line on Fig. 2 indicates a reducing soil for

Cr(VI). The downward slope to the right indicates that the Eh value, at which Cr(VI) isexpected to be reduced, decreases with increasing pH. The solubility and quantity of organicconstituents influence reduction of Cr(VI). The presence of H2S or other strong odorsindicates a reducing environment for Cr(VI). In general, acidic conditions acceleratereduction of Cr(VI) in soils, and alkaline conditions tend to stabilize Cr(VI) against reduction.If pre-digestion matrix spike recovery is not within the recovery limits, the reductive natureof the sample must be documented. This is done by plotting the Eh and pH data on the Eh-pH diagram (Fig. 2) to see if spike recovery is or is not expected in the soil. If the data pointfalls below the Cr(VI)-Cr(III) line on the diagram, then the data is not qualified or rejected.The sample is reducing for Cr(VI). If the data point falls above the line, then the sample iscapable of supporting Cr(VI). In this case, technical error may be responsible for the poorspike recovery, and the extraction should be repeated, along with the Eh and pHmeasurements. If re-extraction results in a poor spike recovery again, then the data isqualified. At this point, review of other soil characteristics, such as levels of pH, Eh, TOC,sulfides, Fe(II), is appropriate to understand why poor spike recovery occurred. This extrareview of these soil properties is only necessary if the unspiked sample contains detectableCr(VI).

8.5.2 If a low or zero percent pre-digestion matrix spike recovery is obtained, an

alternate approach can be used to determine the potential contribution of the sample matrixto Cr(VI) reduction. This approach consists of performing a mass balance, whereby totalchromium is analyzed (Method 3052) for two samples: (1) a separate unspiked aliquot of thesample previously used for spiking, and (2) the digested solids remaining after the alkalinedigestion and filtration of the matrix spike (i.e., the filtered solids from the matrix spike inSection 7.6).

The difference between the total chromium measurements should be approximately equalto the amount of the spike added to the matrix spike. If the LCS (Section 8.3) met theacceptance criteria and the Cr(VI) spike is accounted for in the filtered solids as totalchromium, it is likely that the reduction of the Cr(VI) to insoluble Cr(III) resulted from thereducing matrix of the original sample subjected to Cr(VI) spiking.

8.6A post-digestion Cr(VI) matrix spike must be analyzed per batch as discussed in

Chapter One. The post-digestion matrix spike concentration should be equivalent to 40 mg/kg ortwice the sample concentration observed in the unspiked aliquot of the test sample, whichever isgreater.

8.6.1 Dilute the sample aliquot to a minimum extent, if necessary, so that the

absorbance reading for both the unspiked sample aliquot and spiked aliquot are within theinitial calibration curve.

8.6.2 A guideline for the post-digestion matrix spike recovery is 85-115%. If not

achieved, consider the corrective actions/guidance on data use specified in Section 8.5 orthe Method of Standard Additions (MSA) as specified in Section 8.0 of Method 7000. If theMSA technique is applied post digestion and no spike is observed from the MSA, theseresults indicate that the matrix is incompatible with Cr(VI) and no further effort on the part of

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the laboratory is required. These digestates may contain soluble reducing agents for Cr(VI),such as fulvic acids. METHOD PERFORMANCE9.1

A commercial laboratory analyzed soil/sediment samples containing Cr(VI) with theresults found in Table 1.

9.0

10.0REFERENCES

10.1United States Environmental Protection Agency, 1982. Test Methods for EvaluatingSolid Wastes, Physical/Chemical Methods. SW-846, Second Edition. Office of Solid Waste andEmergency Response, Washington, D.C.

10.2New Jersey Department of Environmental Protection and Energy (NJDEPE).

NJDEPE Modified Methods 3060/7196. 1992.10.3Vitale, R., G. Mussoline, J. Petura, B. James, 1993. A Method Evaluation Study ofan Alkaline Digestion (Modified Method 3060) Followed by Colorimetric Determination (Method 7196)for the Analysis for Hexavalent Chromium in Solid Matrices. Environmental Standards, Inc. ValleyForge, PA 19482.

10.4Zatka, V.J., 1985. Speciation of Hexavalent Chromium in Welding FumesInterference by Air Oxidation of Chromium. J. Ray Gordon Research Laboratory, INCO Limited,Sheridan Park, Mississauga, Ontario L5K 1Z9, Am. Ind. Hyg. Assoc. J., 46(6) : 327-331.

10.5ASTM (American Society for Testing and Materials), 1981. Standard Practice forOxidation Reduction Potential of Water. ASTM Designation:D1498-93.10.6Vitale, R.J., Mussoline, G.R., Petura, J.C. and James, B.R. 1994. HexavalentChromium Extraction from Soils: Evaluation of an Alkaline Digestion Method. J. Environ. Qual.23:1249-1256.

10.7U.S. Department of Health and Human Services - Agency for Toxic Substances and

Disease Registry. Toxicological Profile for Chromium. April, 1993.10.8Vitale, R.J., Mussoline, G.R., Petura, J.C. and James, B.R. 1995. HexavalentChromium Quantification in Soils: An Effective and Reliable Procedure. Am. Env. Lab., April Ed.10.9James, B.R., Petura, J.C., Vitale, R.J., and Mussoline, G.R. 1995. HexavalentChromium Extraction form Soils: A Comparison of Five Methods. Environ. Sci. Technol. 29:2377-2381.

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10.10U.S. Environmental Protection Agency. 1993. IRIS: A continuously updated electronicdatabase maintained by the U.S. Environmental Protection Agency. National Library of Medicine,Bethesda, MD.

10.11ASTM (American Society for Testing and Materials), 1981. Standard Test Method forFerrous Iron in Iron Oxides. ASTM Designation:D3872-86.10.12ASTM (American Society for Testing and Materials), 1981. Standard Test Method for24-h Batch-Type Measurement of Contaminant Sorption by Soil and Sediments. ASTMDesignation:D4646-87.

10.13ASTM (American Society for Testing and Materials), 1981. Standard Test Method forSingle Batch Extraction Method for Waters. ASTM Designation:D5233-92.10.14ASTM (American Society for Testing and Materials), 1981. Standard Test Method forShake Extraction of Solid Waste with Water. ASTM Designation:D3987-85.10.15U.S. EPA Contract Laboratory Program, Statement of Work for Organic Analysis,

Multimedia Multiconcentration Document, OLM03.1, 8/94 Rev.

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TABLE 1

SINGLE LABORATORY METHOD EVALUATION DATA

Sample TypeEh(mV)bpHdS(ppm)c<10.0<10.0<10.0<10.025.0<10.0

2-

Mean NativeCr(VI) Conc.(mg/kg)4.1NDND759NDND

Mean Cr(VI)Spike Conc.(mg/kg)42.062.563.18133819.8

Matrix SpikeRecoveryRange,%89.8-11665.0-70.337.8-71.185.5-94.8

075.5-86.3

COPRa/SoilBlendsLoamClayCOPRaAnoxicSedimentQuartz Sand

550620840460-189710

7.46.43.07.47.25.3

Source: Reference 10.3Notes:

NDabcd

-----Not detected

COPR - chromite ore processing residue

Corrected for the reference electrode, laboratory field moist measurementField measurement

Laboratory field moist measurement

CD-ROM3060A-11

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FIGURE 1

QUALITY CONTROL FLOW CHART

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FIGURE 1

QUALITY CONTROL FLOW CHART (Continued)

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FIGURE 2

Eh/pH PHASE DIAGRAM

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METHOD 3060A

ALKALINE DIGESTION FOR HEXAVALENT CHROMIUMCD-ROM3060A-15

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