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75-27-4 75-25-2 74-83-9 56-23-5 108-90-7 75-00-3 110-75-8 67-66-3 74-87-3 124-48-1 95-50-1 541-73-1 106-46-7 75-34-3 107-06-2 75-35-4 156-60-5 75-43-4 75-09-2 78-87-5 10061-01-5 10061-02-6 79-34-5 127-18-4 71-55-6 79-00-5 79-01-6 75-69-4 75-01-4

File Name: 75-27-4_75-25-2_74-83-9_56-23-5_108-90-7_75-00-3_110-75-8_67-66.asp

                      EA LABORATORIES                                       EAL-M-8010A           GROUP: Volatiles
ANALYTICAL METHOD
Halogenated Volatile Organics by Gas Chromatography Page: 1 of: 12



WHEN STAMPED IN RED, THIS IS A CONTROLLED COPY. IF STAMP IS
NOT RED, VERIFY THAT YOU ARE USING THE CURRENT REVISION
BEFORE PROCEEDING WITH WORK UNDER THIS PROCEDURE
1.0 SCOPE AND APPLICATION

This method is used to determine the concentration of various volatile halogenated organic compounds. Table 1 lists
the compounds that are routinely determined by this method, and the laboratory Reporting Limit for each analyte.
Modifications to the analyte list or procedural changes to reach lower Reporting Limits are allowed if required by client,
project or program. Any changes in the analytical procedures must be approved by the Organic Division Manager and
the Quality Services Manager before samples can be analyzed.

TABLE 1. 8010A ANALYTE LIST
ANALYTE: CAS No.(a) Reporting Limit Reporting Limit
(礸/L) (礸/kg)
Bromodichloromethane 75-27-4 1 1
Bromoform 75-25-2 1 1
Bromomethane 74-83-9 1 1
Carbon tetrachloride 56-23-5 1 1
Chlorobenzene 108-90-7 1 1
Chloroethane 75-00-3 1 1
2-Chloroethyl vinyl ether 110-75-8 1 1
Chloroform 67-66-3 1 1
Chloromethane 74-87-3 1 1
Dibromochloromethane 124-48-1 1 1
1,2-Dichlorobenzene 95-50-1 1 1
1,3-Dichlorobenzene 541-73-1 1 1
1,4-Dichlorobenzene 106-46-7 1 1
1,1-Dichloroethane 75-34-3 1 1
1,2-Dichloroethane 107-06-2 1 1
1,1-Dichloroethene 75-35-4 1 1
trans-1,2-Dichloroethene 156-60-5 1 1
Dichlorofluoromethane 75-43-4 1 1
Dichloromethane (Methylene Chloride) 75-09-2 1 1
1,2-Dichloropropane 78-87-5 1 1
cis-1,3-Dichloropropene 10061-01-5 1 1
trans-1,3 Dichloropropene 10061-02-6 1 1
1,1,2,2-Tetrachloroethane 79-34-5 1 1
Tetrachloroethene 127-18-4 1 1
1,1,1-Trichloroethane 71-55-6 1 1
1,1,2-Trichloroethane 79-00-5 1 1
Trichloroethene 79-01-6 1 1
Trichlorofluoromethane 75-69-4 1 1
Vinyl Chloride 75-01-4 1 1

(a) Chemical Abstract Services Registry Number.




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Sample reporting limits are highly matrix-dependent. The reporting limits for various matrices are determined by
multiplying the reporting limits in Table 1 by the factor in Table 2, with the appropriate concentration units (礸/L-water,
礸/kg-soil). These are provided for guidance and may not always be achievable.

TABLE 2. DETERMINATION OF REPORTING LIMITS FOR VARIOUS MATRICES(a)
Matrix Factor
Water 1
Low-concentration soil 1
High-concentration soil and sludge 125

2.0 SUMMARY OF METHOD

This method provides gas chromatographic conditions for the detection of halogenated volatile organic compounds.
Samples will be introduced into the GC via purge-and-trap. A temperature program is used in the gas chromatograph to
separate the organic compounds. Detection is achieved by a electrolytic conductivity detector (ELCD).

3.0 DEFINITIONS

3.1 Method Blanks (MB) are samples of laboratory or DI water or sample solvents which are treated like samples.
Method blanks identify interferents or contaminants which are introduced by the analytical procedure.
3.2 Calibration Samples are certified standards containing measurable amounts of the analytes to be identified and
quantified.
3.3 Calibration Verification (CCV) is a same source calibration standard used to verify the initial calibration at the
beginning of each working day, after every 10 injections, and at the end of each analytical sequence.
3.4 Laboratory Control Samples (LCS) consist of laboratory pure water or solvent and a measured concentration of
the analyte(s) being tested. Laboratory control samples are treated like samples and subjected to all steps of the
analytical procedure. The LCS is made from an independent source standard.
3.5 Initial Continuing Verification (ICV) consist of laboratory pure water or solvent and a measured concentration of
the analyte(s) of interest. The ICV is analyzed after the initial calibration with the acceptance range of ?5% and is made
from an independent source standard.
3.5 Surrogate Spiking Compounds are compounds similar in performance to the compounds of interest which are
introduced into each sample, standard, and blank during organic analyses. They are utilized to determine the
performance of the analytes.
3.6 Matrix Spikes (MS) are field samples to which a measured amount of analyte(s) of interest are added. Recovery
of the matrix spike is utilized to determine the effects of sample matrix on the recovery of the analyte(s) of interest and
may be indicative of bias.
3.7 Matrix Spike Duplicates (MSD) are second aliquots of field samples treated identically as samples or sample matrix
spikes. These are utilized to determine sample matrix effects on analytical precision.
3.8 Analytical Batch refers to a group of samples and associated QC samples (blanks, spikes, duplicates) assembled
for the purpose of preparation and/or analysis.
3.9 Analytical Sequence refers to the gas chromatographic analysis run, usually beginning with calibration (initial or
continuing calibration verification), including all calibrations, blanks, QC samples, samples, and ends when all samples
have been analyzed, with an in-control continuing calibration verification standard.
3.10 Organic-free reagent water refers to water in which no target analyte is observed at the Reporting Limit of the
compounds of interest. EA Laboratories uses a McNew-Culligan reverse osmosis (R/O) water purification system to
generate organic-free deionized (DI) water which is further treated at the endpoint using a Barnsted filtration and UV
system to remove any remaining organic contaminants

4.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING

4.1 Under routine protocols, at least two aliquots are sent to the laboratory for each sample. Sample container,
preservation and holding time requirements are given in Table 3. While samples are in the custody of the laboratory,

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samples are stored in the volatiles walk-in at 4EC ?2EC prior to analysis. After analysis is completed, samples are stored
by the Sample Management Office in laboratory walk-ins until disposal.
4.2 Prior to analysis the analyst must check the sample vials for the presence of air bubbles, and should notify the
assigned Laboratory Project Manager (LPM) immediately, if present. The LPM will contact the client to determine if the
analysis should proceed. The analyst must initiate a Nonconformance Record (NCR) as described in EAL-SOP-072 and
forward it to the LPM.
4.3 The sample vial should indicate that the sample has been preserved, and the pH of the sample is determined after
the sample aliquot is removed from the sample vial. Do not dip the pH strip into the sample vial before the sample aliquot
is removed. Document the pH in the instrument log. Though the method requirement is that the sample be preserved
to a pH<2, the lack of preservation will not impact the determination of halogenated volatile compounds. Preserved
samples with pH >2 constitute a nonconformance and must be documented via a Non-Conformance Report (NCR).

[Note: 2-chloroethyl vinyl ether breaks down under acidic conditions. Determination of the presence of this compound
may be adversely affected under the required preservation conditions.]

Table 3. Sample Containers, Preservation Techniques, and Holding Times
Parameter Container Preservative Holding Time
Concentrated Waste Samples:
Halogenated Volatiles 8-oz. wide mouth glass None 14 days
with Teflon liner
Liquid Samples:
Halogenated Volatiles 2 40-mL vials with 4 drops conc. HCl, Cool, 4EC 14 days
(No Residual Chlorine Teflon lined septum
Present) caps
Halogenated Volatiles 2 40-mL vials with Collect sample in a 4oz. soil VOA 14 days
(Residual Chlorine Teflon lined septum container which has been pre-
Present) caps preserved with 4 drops of 10%
sodium thiosulfate. Gently mix
sample and transfer to a 40-mL
VOA vial that has been pre-
preserved with 4 drops conc.
HCl, Cool to 4EC
Soil/Sediments and Sludges:
Halogenated Volatiles 4oz (120-mL) wide Cool to 4EC 14 days
mouth glass with Teflon
liner

5.0 INTERFERENCES

5.1 Contamination by carryover can occur whenever high-concentration and low-concentration samples are sequentially
analyzed. To reduce carryover, the purging device must be rinsed out between samples with water or solvent. Whenever
an unusually concentrated sample is encountered, it should be followed by an analysis of a instrument blank to check
for cross contamination.
5.2 Samples can be contaminated by diffusion of volatile organics (particularly chlorofluorocarbons and methylene
chloride) through the sample container septum during shipment and storage. A trip blank prepared from organic-free
reagent water and carried through sampling and subsequent storage and handling can serve as a check on such
contamination. The most common laboratory contaminant is methylene chloride which is a common lab solvent. Another
is chloroform which originates from cartridge breakthrough in the laboratory DI water system.

6.0 APPARATUS AND MATERIALS


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6.1 Gas chromatograph: analytical system complete with gas chromatograph suitable for purge-and-trap sample
introduction and all required accessories, including detector, analytical columns, data system, and gases.

6.1.1 Columns: Wide bore capillary column RTX 502.2 (75m x 0.53 mm ID) or RTX 1 (75m x 0.53 mm).
6.1.2 Detector: Electrolytic conductivity (ELCD).

6.2 Glass scintillation vials: 20-mL, with screw-caps and Teflon liners or glass culture tubes with a screw-cap and Teflon
liner.
6.3 Spatula: Stainless steel.
6.4 Disposable pipettes: Pasteur.
6.5 Purge-and-trap device: The purge-and-trap device consists of three separate pieces of equipment: the sample purger,
the trap, and the desorber. All three pieces are commercially available in an automated unit. The Tekmar LSC2000
concentrator with the ALS2016 Autosampler with heater pockets for heated purge analysis is used at EA Laboratories.

6.5.1 Trap: VOCARB 3000 (Carbopack B/Carboxen 1000 and 1001). Before initial use, the trap should be conditioned
overnight at 270EC by backflushing with an inert gas flow of at least 20 mL/min.
6.5.2 The desorber should be capable of rapidly heating the trap to 260EC for desorption. The trap should not be heated
higher than 300EC.

6.6 Heater: Should be capable of maintaining the purging chamber to within 1EC over a temperature range from ambient
to 100EC.
6.7 Syringes: 5 mL gas-tight with shutoff valve.
6.8 Volumetric flasks, Class A: 10, 50, 100, 500, and 1,000 mL with a ground glass stopper.
6.9 Microsyringes: 10, 25 and 100 礚 needle (Hamilton 702N or equivalent).
6.10Balances: Analytical ( ?.0001 g accuracy) and Top Loading ( +0.01 g accuracy).

7.0 SAFETY AND CHEMICAL HYGIENE

The toxicity or carcinogenicity of each reagent used in this method has not been precisely defined; however, each
chemical compound should be treated as a potential health hazard, and exposure to these chemicals must be reduced
to the lowest possible level by whatever means available. The laboratory maintains a reference file of Material Safety
Data Sheets (MSDS) for the chemicals specified in this method. Additional information on laboratory safety is available
in the Chemical Hygiene Plan and from the Health and Safety Officer.

8.0 REAGENTS & STANDARDS

8.1 Methanol, CH3OH. Purge-and-trap grade or equivalent. Store away from other solvents.
8.2 Stock Standards: Stock solutions are purchased as certified solutions, stored at -10EC to -20EC. and protected from
light. Once stock standard ampules are opened, they are stored no longer than 1 week, for gases or for reactive
compounds such as 2-chloroethylvinyl ether. All other standards must be replaced after 1 month, or sooner if comparison
with check standards indicates a problem.
8.3 Secondary Dilution Standards: Using stock standard solutions, prepare secondary dilution standards in methanol,
as needed, containing the compounds of interest, either singly or mixed together. Secondary dilution standards should
be stored with minimal headspace for the same time period specified in 8.2.
8.4 Calibration Standards: Prepare calibration standards in organic-free reagent water from the secondary dilution or
stock standards, at the concentrations listed in Table 4. Each standard should contain each analyte for detection by this
method (including the surrogate compound). In order to prepare accurate aqueous standard solutions, the following
precautions must be observed. Refer to Table 4A. Standard Preparation.

8.4.1 Rapidly inject the alcoholic standard into the filled volumetric flask or 5 mL gas tight syringe. Remove the needle
as fast as possible after injection.
8.4.2 Mix aqueous standards by inverting the volumetric flask or syringe three times only.

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8.4.3 If the standard is prepared in a volumetric flask, fill the sample syringe from the standard solution contained in the
expanded area of the flask (do not use any solution contained in the neck of the flask).
8.4.4 Never use pipettes to dilute or transfer samples or aqueous standards.
8.4.5 Aqueous standards are not stable and should be discarded after one hour, unless properly sealed and stored. The
aqueous standards can be stored up to 24 hours, if held in sealed vials with zero headspace.

TABLE 4. INITIAL CALIBRATION STANDARD CONCENTRATIONS
Standard Analytes Concentration (礸/L)
1 All analytes in Table 1 plus 4-Bromofluorobenzene (surrogate) 3
2 " 10
3 " 50
4 " 80
5 " 100


TABLE 4 A. STANDARD PREPARATION

200 ppm Standard (uL) Deionized Water (ml) Concentration (ppb)

3 200 3

10 200 10

1.25 5 50

2.0 5 80

2.5 5 100



8.5 Surrogate standards: The analyst will monitor both the performance of the analytical system and the effectiveness
of the method in dealing with each sample matrix by spiking each sample, LCS, and organic-free reagent blank with the
surrogate compound 4-bromofluorobenzene (BFB) at 50 礸/L (water), 50 礸/kg (low soil) and 6250 礸/kg (medium soil).
8.6 LCS: The analyst will monitor both the performance of the analytical system and the effectiveness of the method by
spiking an organic-free reagent blank with the matrix spike compounds 1,1-dichloroethene, trichloroethene and
chlorobenzene at 50 礸/L (water), 50 礸/kg (low soil) and 6250 礸/kg (medium soil).

9.0 PROCEDURE

Volatile compounds are introduced into the gas chromatograph using purge-and-trap. Purge-and-trap may be used
directly on ground water samples or low-concentration contaminated soils and sediments. For medium-concentration
soils or sediments, methanol extraction is performed prior to purge-and-trap analysis. Gas chromatographic conditions
are set to ensure acceptable method performance.

9.1 Calibration: A calibration curve is required for all target compounds, including surrogate compounds. The calibration
summary form will show the calibration factors (CF), relative percent standard deviation (%RSD). Establish gas
chromatographic operating parameters. Prepare calibration standards using the procedures indicated in Section 8.0.
Calibrate the chromatographic system.

9.1.1 Initial Calibration. For water and medium level soil matrices, the initial calibration is performed at ambient
temperature. For low level soils, the initial calibration is performed at 40EC.




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Each calibration standard is introduced into the gas chromatograph using the same technique that will be used to
introduce the actual samples (e.g. purge-and-trap). Tabulate area responses against the mass injected. Average CF is
used for quantitation unless the %RSD is greater than 20%.

CF = A ?M

where: CF = Calibration Factor
A = Total peak area
M = Mass injected (in nanograms)

If the %RSD criteria for initial calibration exceeds 20%, a regression analysis (r $ 0.990) is used to establish the curve
and used for quantitation.

Following successful initial calibration, establish the retention time window for each target analyte calculated as the
average retention time from the initial calibration standards ?0.2 min. Confirm that all calibration standards are within
the windows. If not, calibration fails and the initial calibration is performed again.

9.1.2 Calibration Verification: The working calibration curve or calibration factor must be verified on each working day
and after every ten injections with a mid-level (continuing) calibration standard. If the continuing calibration standard
or QC Check standard fails the criterion the standard should be reanalyzed immediately. If the standard fails again, the
analysis is stopped, initial calibration performed and all samples after the last successful calibration are reanalyzed. If
the response for any analyte in the continuing calibration standard varies from the predicted response by more than +/-
15%, a new calibration curve must be prepared for that analyte. See Table 6 for calibration and quality control acceptance
criteria for the QC Check standard. However, in the case where criteria fails with a positive %D or high recovery, the
analyst should determine the impact on data usability before proceeding with reanalysis, and may proceed with the
approval of the Laboratory Supervisor. If the calibration verification is not acceptable, inspect the GC system to
determine the cause and perform whatever maintenance, if necessary, before recalibrating and proceeding with sample
analysis.

Percent Difference = (R1 - R2) 鱎1 x 100

where:
R1 = Calibration Factor from first analysis.
R2 = Calibration Factor from succeeding analyses.

9.2 Sample Preparation:

9.2.1 Water Samples: Set the GC conditions: Adjust the purge gas flow rate (helium), on the purge-and-trap device.
Optimize the flow rate to provide the best response for chloromethane and bromoform, if these compounds are analytes.
Excessive flow rate reduces chloromethane response, whereas insufficient flow reduces bromoform response. Calibrate
the instrument. All calibration criteria must be met before analyzing samples.

Prepare the Standards and Samples: Remove the plunger from a 5-mL syringe and attach a closed syringe valve. Open
the sample bottle, which has been allowed to come to ambient temperature, and carefully pour the sample into the syringe
barrel to just short of overflowing. Replace the syringe plunger and compress the sample. Open the syringe valve and
vent any residual air while adjusting the sample volume to 5.0 mL. This process of taking an aliquot destroys the validity
of the liquid sample for future analysis; therefore, if there is only one VOA vial, the analyst should fill a 20-mL VOA vial
(with no headspace) after taking sample aliquot to protect against possible loss of sample integrity. This second sample
is maintained only until such time when the analyst has determined that the first sample has been analyzed properly. If
a second analysis is needed from the 20-mL VOA vial, it must be analyzed as soon as possible.




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If the initial analysis of a sample or a dilution of the sample has a concentration of analytes that exceeds the initial
calibration range, the sample must be reanalyzed at a higher dilution. An acceptable dilution factor has the analyte(s)
that initially exceeded calibration range in the upper half of the calibration range.

Diluting Purgeable Samples: All steps must be performed without delay until the diluted sample is in a gas-tight syringe.
Dilutions may be made in volumetric flasks or in the 5-mL gas tight syringe. Intermediate dilutions may be necessary for
extremely large dilutions.

Add the surrogate spiking solution to the sample or diluted sample in the 5-mL syringe through the valve bore of the
syringe; then close the valve. Matrix spiking solutions, if indicated, should be added to the sample at this time.

Purging: Attach the syringe-syringe valve assembly to the syringe valve on the purging device. Open the syringe valves
and inject the sample into the purging chamber. Close both valves and purge the sample for 11 minutes at ambient
temperature.

Desorption: At the conclusion of the purge time, the purge and trap device advances to the desorb mode, and begins
the gas chromatographic temperature program and GC data acquisition. Concurrently, the trapped materials are
introduced to the gas chromatographic column by rapidly heating the trap to 260EC while backflushing the trap with
helium between 20 and 60 mL/min for 4 minutes.

Recondition the Trap: After desorbing the sample, the purge and trap advances to the bakeout mode. The trap
temperature should be maintained at 270EC. Trap temperatures up to 290EC may be employed; however, the higher
temperature will shorten the useful life of the trap. After approximately 7 min, the purge and trap device will advance and
start to cool the trap. When cool, the trap is ready for the next sample.

9.2.2 Water-miscible liquids are analyzed as water samples after first diluting them at least 50-fold with reagent water.
Initial and serial dilutions can be prepared by pipetting 2 mL of the sample to a 100-mL volumetric flask and diluting to
volume with reagent water. Transfer immediately to a 5-mL gas-tight syringe. Alternatively, prepare dilutions directly
in a 5-mL syringe filled with reagent water by adding at least 20 礚, but not more than 100-礚 of liquid sample. The sample
is ready for addition of surrogate and matrix spiking standards (if applicable).
9.2.3 Sediment/soil and waste samples: It is highly recommended that all samples of this type be screened prior to the
purge-and-trap GC analysis to determine whether to use the low-level method (0.005-1 mg/kg) or the high-level method
(>1 mg/kg). The GC system should be set up as in Section 9.0 prior to the preparation of the sample to avoid loss of
volatiles from standards and samples. A heated purge calibration curve must be prepared and used for the quantitation
of all samples analyzed with the low-level method. Follow the initial and daily calibration instructions, except for the
addition of a 40 EC purge temperature.

9.2.3.1 Low-level Method: This is designed for samples containing individual purgeable compounds of <1 mg/kg. The
low-level method is based on purging a heated sediment/soil sample mixed with reagent water containing the surrogate
and, if applicable, matrix spiking standards. Analyze all reagent blanks and standards under the same conditions as the
samples.

Sample Preparation: Refer to the Table 5. Sample Preparation to determine the appropriate sample amount for the
expected concentrations of <0.1 to 0.5 mg/kg. The sample consists of the entire contents of the sample container. Do
not discard any supernatant liquids. Mix the contents of the sample container with a narrow metal spatula. Weigh the
amount into a tared purge device. Note and record the actual weight to the nearest 0.1 g.


TABLE 5. SAMPLE PREPARATION

Expected Concentration Sample Amount Required
(mg/kg) (g)



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<0.1 5.0

0.1 - 0.2 2.5

0.2 - 0.5 1.0

Remove the plunger from a 5-mL Luerlock type syringe equipped with a syringe valve and fill until overflowing with
reagent water. Replace the plunger and compress the water to vent trapped air. Adjust the volume to 5.0 mL. Add the
surrogate spiking solution to the syringe through the valve. Matrix spiking solutions, if indicated, should be added to
the sample at this time.

Add the spiked reagent water to the purge device, which contains the weighed amount of sample, and connect the device
to the purge-and-trap system. NOTE: These steps must be performed rapidly and without interruption to avoid loss of
volatile organics. These steps must be performed in a laboratory free of solvent fumes.

Heated Purge: Heat the sample to 40EC and purge the sample for 11 minutes. Proceed with the analysis as described for
low-level water samples. If any target analytes exceed the calibration range, either a smaller sample aliquot must be
analyzed (smallest volume allowed is 1.0 g.) or the high-level method must be followed.

9.2.3.2 High-level Method: The method is based on extracting the sediment/soil with methanol. A waste sample is either
extracted or diluted, depending on its solubility in methanol. An aliquot of the extract is added to reagent water
containing surrogate and matrix spiking standards. This is purged at ambient temperature. All samples with an expected
concentration of >0.5 mg/kg should be analyzed by this method.

Sample Preparation: The sample consists of the entire contents of the sample container. Do not discard any supernatant
liquids. Mix the contents of the sample container with a narrow metal spatula. For sediment/soil and waste that are
insoluble in methanol, weigh 4 g (wet weight) of sample into a tared 20-mL vial. Use a top-loading balance. Note and
record the actual weight to 0.1 gram. For waste that is soluble in methanol, weigh 1 g (wet weight) into a tared vial or a
10-mL volumetric flask. (If a vial is used, it must be calibrated prior to use. Pipette 10.0 mL of methanol into the vial and
mark the bottom of the meniscus. Discard this solvent.)

Quickly add 9.75 mL of methanol; then add 0.25 mL of the surrogate spiking solution to the vial. Cap and shake for 2 min.
NOTE: These steps must be performed rapidly and without interruption to avoid loss of volatile organics. These steps
must be performed in a laboratory free from solvent fumes.

Pipette approximately 1 mL of the extract to a GC vial for storage, using a disposable pipette. The remainder may be
disposed of. Transfer approximately 1 mL of reagent methanol to a separate GC vial for use as the method blank for each
set of samples. These extracts may be stored at 4 ?2EC in the dark, prior to analysis.

The GC system should be set up as in Section 9.0 prior to the addition of the methanol extract to reagent water. Estimate
the concentration range of the sample from the low-level analysis to determine the appropriate volume of the methanol
extract (Table 5A). If the sample was submitted as a high-level sample, start with 100 礚. All dilutions must keep the
response of the major constituents (previously saturated peaks) in the upper half of the calibration range.

TABLE 5A. QUANTITY OF METHANOL EXTRACT REQUIRED FOR ANALYSIS OF HIGH-LEVEL
SOILS/SEDIMENTS
Concentration Range Approximate Volume of Methanol Extract(a)
500-10,000 礸/kg 100 礚
1,000-20,000 礸/kg 50 礚
5,000-100,000 礸/kg 10 礚
25,000-500,000 礸/kg 100 礚 of 1/50 dilution(b)


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(a) The volume of methanol added to 5 mL of water being purged should be kept constant. Therefore, add to the 5-mL
syringe whatever volume of methanol is necessary to maintain a volume of 100 礚 added to the syringe.
(b) Dilute an aliquot of the methanol extract and then take 100 礚 for analysis.

Calculate appropriate dilution factor for concentrations exceeding this table.

Remove the plunger from a 5.0-mL Luerlock type syringe equipped with a syringe valve and fill until overflowing with
reagent water. Replace the plunger and compress the water to vent trapped air. Adjust the volume to 4.9 mL. Pull the
plunger back to 5.0 mL to allow volume for the addition of the sample extract and of standards. Add the volume of
methanol extract determined and a volume of methanol solvent to total 100 礚 (excluding surrogate and matrix spike
standards).

Attach the syringe-syringe valve assembly to the syringe valve on the purging device. Open the syringe valve and inject
the water/methanol sample into the purging chamber. Proceed with the analysis, and analyze all reagent blanks on the
same instrument as that used for the samples. For a matrix spike in the high-level sediment/soil samples, add 9.5 mL of
methanol, 0.25 mL of surrogate spike solution and 0.25 mL of matrix spike solution. Add a 100-礚 aliquot of this extract
to 5 mL of water for purging.

9.3 Gas Chromatographic Analysis:

9.3.2 Samples are analyzed in a set referred to as an analysis sequence. The sequence begins with instrument calibration
or calibration verification followed by samples or extracts.
9.3.3 If the sample responses exceed the calibration range of the system, dilute the extract and reanalyze. The dilution
factor is acceptable if the target analyte response is within the upper half of the calibration range.
9.3.4 Tentative identification of an analyte occurs when a peak from a sample extract falls within the retention time
window. Unless otherwise required by client, project or program, qualitative confirmation is required: on a second GC
column; by GC/MS if concentration permits; or by other recognized confirmation techniques. Confirmation may not be
necessary if the composition of the sample matrix is well established by prior analyses.
9.3.5 Reanalysis sequence sample volume injected, dilutions and standards are identified in the instrument injection log
(EAL-SOP-100).
9.3.6 Using the calibration procedure (Section 9.1), determine the identity and quantity of each component peak (using
equations in Section 10.0) in the sample chromatogram which corresponds to the compounds used for calibration
purposes.

10.0 CALCULATIONS

No calculated results below the reporting limit are reported.

Aqueous Samples.

Concentration (礸/L) = (A)(D)
(CF)(V(s))

where:
CF = Average calibration factor from the initial calibration
A = Response for the analyte in the sample, units may be in area counts or peak height.
D = Dilution factor, if dilution was made on the sample prior to analysis. If no dilution was made,
D = 1, dimensionless.
V(s) = Volume of sample purged in mL.

Nonaqueous Samples.

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Halogenated Volatile Organics by Gas Chromatography Page: 10 12
of:



Concentration (礸/kg) = (A(x))(D)
(CF)(V)(W)
where:
W = Weight of sample extracted or purged, in grams. The wet weight or dry weight may be used,
depending upon the specific applications of the data.
V = Volume of methanol extract added to reagent water for purge and trap analysis, in 礚.

A(x), CF, and D have the same definition as for aqueous samples when a solid sample is analyzed.

11.0 QUALITY CONTROL

11.1 Before processing any samples, the analyst must demonstrate the ability to generate acceptable accuracy and
precision, the analyst must perform the following operations.

11.1.1 Analyze four Quality Control Check Standards (20 ug/L) according to the method beginning with preparation of
the samples.
11.1.2 Calculate the average recovery (x) in ug/L, and the standard deviation of the recovery (s) in ug/L, for each analyte
of interest using the four results.
11.1.3 For each analyte compare (s) and (x) with the LCS laboratory control limits for precision and accuracy, established
from historical data. If (s) and (x) for all analytes meet the acceptance criteria, the system performance is acceptable and
analysis of actual samples can begin. If any individual s exceeds the precision limit or any individual falls outside the
range for accuracy, then the system performance is unacceptable for that analyte.
11.1.4 When one or more of the analytes tested fail at least one of the acceptance criteria, the analyst must locate and
correct the source of the problem and repeat the test for those analytes that failed to meet criteria. Repeated failure,
however, will confirm a general problem with the measurement system. If this occurs, locate and correct the source of
the problem and repeat the test for all method compounds.

12.0 CONFIRMATION

Any reported compound of interest must be qualitatively confirmed by second column or by GC/MS.

13.0 REFERENCES

United States Environmental Protection Agency. 1986. Revised July 1992. Test Methods for Evaluating Solid Waste.
Physical/Chemical Methods. EPA SW-846, 3rd edition, including Update II. U.S. EPA, Washington, D.C.

TABLE 6. CALIBRATION AND QC ACCEPTANCE CRITERIA
Analyte Range for Q Limit Range for x Range P, P(s) (%)
(礸/L) for S (礸/L)
(礸/L)
Bromodichloromethane 15.2-24.8 4.3 10.7-32.0 42-172
Bromoform 14.7-25.3 4.7 5.0-29.3 13-159
Bromomethane 11.7-28.3 7.6 3.4-24.5 D-144
Carbon tetrachloride 13.7-26.3 5.6 11.8-25.3 43-143
Chlorobenzene 14.4-25.6 5.0 10.2-27.4 38-150
Chloroethane 15.4-24.6 4.4 11.3-25.2 46-137
2-Chloroethylvinyl ether 12.0-28.0 8.3 4.5-35.5 14-186
Chloroform 15.0-25.0 4.5 12.4-24.0 49-133
Chloromethane 11.9-28.1 7.4 D-34.9 D-193
Dibromochloromethane 13.1-26.9 6.3 7.9-35.1 24-191
1,2-Dichlorobenzene 14.0-26.0 5.5 1.7-38.9 D-208

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Halogenated Volatile Organics by Gas Chromatography Page: 11 12
of:



1,3-Dichlorobenzene 9.9-30.1 9.1 6.2-32.6 7-187
1,4-Dichlorobenzene 13.9-26.1 5.5 11.5-25.5 42-143
1,1-Dichloroethane 16.8-23.2 3.2 11.2-24.6 47-132
1,2-Dichloroethane 14.3-25.7 5.2 13.0-26.5 51-147
1,1-Dichloroethene 12.6-27.4 6.6 10.2-27.3 28-167
trans-1,2-Dichloroethane 12.8-27.2 6.4 11.4-27.1 38-155
Dichloromethane 15.5-24.5 4.0 7.0-27.6 25-162
1,2-Dichloropropane 14.8-25.2 5.2 10.1-29.9 44-156
cis-1,3-Dichloropropene 12.8-27.2 7.3 6.2-33.8 22-178
trans-1,3-Dichloropropene 12.8-27.2 7.3 6.2-33.8 22-178
1,1,2,2-Tetrachloroethane 9.8-30.2 9.2 6.6-31.8 8-184
Tetrachloroethene 14.0-26.0 5.4 8.1-29.6 26-162
1,1,1-Trichloroethane 14.2-25.8 4.9 10.8-24.8 41-138
1,1,2-Trichloroethane 15.7-24.3 3.9 9.6-25.4 39-136
Trichloroethene 15.4-24.6 4.2 9.2-26.6 35-146
Trichlorofluoromethane 13.3-26.7 6.0 7.4-28.1 21-156
Vinyl chloride 13.7-26.3 5.7 8.2-29.9 28-163
Q = Concentration measured in Quality Control Check Standard, in 礸/L.
s = Standard deviation of four recovery measurements, in 礸/L.
X = Average recovery for four recovery measurements, in 礸/L.
P, Ps = Percent recovery measured.
D = Detected; result must be greater than zero.




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SUMMARY OF LABORATORY QUALITY CONTROL REQUIREMENTS AND CORRECTIVE ACTION PROCEDURES FOR SW-846 METHODS (A)


SW-8010 - Halogenated Volatile Organics in Waters by GC/ELCD

Holding time 14 days from sampling Analysis is completed within holding time. Notify client, determine if laboratory to proceed or if client will resample.

Initial Calibration Established initially at 5 Initial calibration %RSD for all target analytes is less than 1. Reanalyze standards.
concentration levels 20 percent, or use calibration curve (r >0.990) if %RSD 2. If similar results are obtained, verify standard concentrationss and recalibrate instrument.
>20%. 3. Document actions taken in a Nonconformance Record, and in the analytical report

Continuing Calibration Verify initial clibration daily at Continuing calibration percent D from initial +/-15% 1. Reanalyze continuing calibration standard.
mid level 2. If similar results are obtained, recalibrate instrument.
3. Document actions taken in a Nonconformance Record, and in the analytical report.
4. Should the analyzed results fail with >15% difference and the compound(s) of interest is not detected,
the analysis is considered valid and the failing CCV result is noted in the report narrative.

Method Blank 1 per analytical batch Concentration is common laboratory contaminants methylene chloride and 2. Take appropriate corrective action and document.
chloroform are <5X MDL. 3. Reanalyze or reprepare analytical batch.
4. If samples cannot be reanalyzed or reprepared, qualify data.

LCS 1 per analytical batch Values are within EA Laboratories' historically established 1. Check instrument parameters, sensitivity and linearity. Correct any problems.
control limits. 2. Validate LCS preparation. If error is found, reprepare the LCS, and reanalyze the method blank, LCS
and all field samples in the batch.
3. If LCS is valid, evaluate against project specific DQOs and report data if there is not impact on data
usability.
4. If data is not usable, reprepare and reanalyze the method blank, LCS and all field samples in the batch.
5. If repreparation of samples is not possible, qualify data, and note in the report narrative.
6. Document all actions taken in a Nonconformance Record and in the report narrative.

Surrogate spike All laboratory QC and field Surrogate spiking compounds spike concentrations and 1. If surrogate in LCS and/or MB is out-of-control, check quantitation. If quantitation is correct reanalyze.
samples. control limits are within EA Laboratories' historically If similar results are obtained from reanalysis, obtain fresh, verified surrogate solution and reanalyze the
established control limits. analytical batch. If samples cannot be reprepared, qualify data.
2. If surrogate spike in LCS and MB are acceptable but out-of-control for samples, validate preparation of
samples. If no errors or problems are discovered for sample preparation, qualify data.
3. If errors are discovered in preparation of samples, reprepare QC samples and all affected samples.
4. Document actions taken. in

MS/MSD 1 set per analytical batch Matrix spiking compounds, spike concentrations, and 1. Validate spiking solution.
control limits are within EA Laboratories' historically 2. If spiking solution is valid, qualify data.
established control limits. 3. If spiking solution is not valid, obtain fresh, certified spiking solution and reanalyze the sample and the
associated matrix spikes.
4. If reanalysis of samples is not possible, qualify data.
5. Document actions taken.




M:\GROUP\QA\METHOD\FINAL\8010A.R00 September 15, 1999
EA Engineering, Science, and Technology, Inc.

EA Laboratories

Method

Number: 8010A Rev. No.: 0

Title: Halogenated Volatile Organics by Gas Chromatography




Prepared By: W.E.Miller, Q.C. Chemist 10 January 1996


Revised By:
D.C. Miser, Volatile Group Leader Date

Approved By:
M.M. Uhlfelder, Quality Services Manager Date

Approved By:
P.A. Christopher, Operations Manager Date
EA Engineering, Science, and Technology, Inc.

EA Laboratories

Method


Procedure No.: 8010A Revision No.: 0



Revisions
Rev. Date of Description
No. Release
0 Initial distribution.
EA Engineering, Science, and Technology, Inc.

EA Laboratories

Method


Procedure No.: 8010A Revision No.: 0




Controlled Distribution




Name Manual No.

Walt Miller 2
Magge Wilcox 4
Natasha Sullivan 8
Steven Warren 9
Jeffrey Black 10
Carl Simmons 12
Phyllis Christopher 13
Craig Schenning 17
Reza Karimi 18
Cathy Atkinson 19

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