UNC

02/14/18

SOP No. KNOX-MS-0015
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1.

SCOPE AND APPLICATION
1.1.

This method is applicable to the determination of volatile organic compounds inwaters, wastewater, organic waste, soils, sludges, and other solid matrices. Standard
analytes are listed in Tables 1 and 2.

1.2.

This SOP is based on SW-846 Method 8260B, 5030B,5035 and 5035A.

1.3.

This method can be used to quantify most volatile organic compounds that haveboiling points below 200C and are insoluble or slightly soluble in water. Volatilewater soluble compounds can be included in this analytical technique; however, formore soluble compounds, quantitation limits are approximately ten times higher
because of poor purging efficiency.

1.4.

The method is based upon a purge and trap, gas chromatograph/mass spectrometric(GC/MS) procedure. The approximate working range is 5 to 400 g/L for 5 mL
waters, 1 to 80 µg/L for 25 mL purge waters, 5 to 400 g/kg for low-level soils, and
250 to 20,000 g/kg for high-level soils, and 1250 to 100,000 µg/Kg for waste.
Reporting limits are listed in Tables 1, and 2.
1.4.1. Analysis in Selected Ion Monitoring Mode (SIM) for select analytes will
have a lower working range. Analytes and reporting limits are listed in Table
1A

1.5.

2.

Method performance is monitored through the use of surrogate compounds, matrix
spike/matrix spike duplicates, and laboratory control spike samples.

SUMMARY OF METHOD
2.1.

Volatile compounds are introduced into the gas chromatograph by the purge andtrap method. The components are separated via the chromatograph and detectedusing a mass spectrometer, which is used to provide both qualitative andquantitative information.

2.2.

Aqueous samples are purged directly. Generally, soils are preserved by extracting
the volatile analytes into methanol. If low detection limits are required, soil samples
may be preserved with sodium bisulfate and purged directly.

2.3.

In the purge and trap process, an inert gas is bubbled through the solution atambient temperature or at 40oC (40oC required for low level soils) and the volatilecomponents are efficiently transferred from the aqueous phase to the vapor phase.
The vapor is swept through a sorbent column where the volatile components aretrapped. After purging is completed, the sorbent column (trap) is heated andbackflushed with inert gas to desorb the components onto a gas chromatographic

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column. The gas chromatographic column is then heated to elute the componentsthat are detected with a mass spectrometer.
2.4.

Qualitative identifications are confirmed by analyzing standards under the same
conditions used for samples and comparing the resultant mass spectra and GC
retention times. Each identified component is quantified by relating the MS
response for an appropriate selected ion produced by that compound to the MS
response for another ion produced by an internal standard.
2.4.1. Qualitative identification in SIM mode may provide a lesser degree ofconfidence in the compound identification.

3.

DEFINITIONS
3.1.

Batch: The batch is a set of up to 20 samples of the same matrix processed using thesame procedures and reagents within the same 24 hour time period. Using thismethod, each BFB analysis will normally start a new batch. Batches for high levelsoils, waste or other extracts, are defined at the sample preparation stage and may
be analyzed on multiple instruments over multiple days, although reasonable effort
should be made to keep the samples together. See section 11.3.2.
3.1.1.

The Quality Control batch must contain a matrix spike/spike duplicate(MS/MSD), a Laboratory Control Sample (LCS), and a method blank.
When there is insufficient sample to analyze an MS/MSD, an LCS/LCSD
is analyzed. In some cases, at client request, the MS/MSD may bereplaced with a matrix spike and sample duplicate. Refer to the QC
Program document (QA-003) for further details of the batch definition.

3.2.

Method Blank: A method blank consisting of all reagents added to the samples
must be analyzed with each batch of samples. The method blank is used to identify
any background interference or contamination of the analytical system that may
lead to the reporting of elevated concentration levels or false positive data.

3.3.

Laboratory Control Sample (LCS): Laboratory Control Samples are wellcharacterized, laboratory generated samples used to monitor the laboratory's day-today performance of routine analytical methods. The LCS, spiked with a group of
target compounds representative of the method analytes, is used to monitor theaccuracy of the analytical process, independent of matrix effects. Ongoing
monitoring of the LCS results provides evidence that the laboratory is performing
the method within accepted QC guidelines for accuracy and precision. An LCS
from a source other than that of the calibration standards may also be used as thecalibration verification (CCV) as long as the acceptance criteria for both the LCS
and CCV are met.

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4.

3.4.

Surrogates: Surrogates are organic compounds which are similar to the target
analyte(s) in chemical composition and behavior in the analytical process, butwhich are not normally found in environmental samples. Each sample, blank, LCS,
and MS/MSD is spiked with surrogate standards. Surrogate spike recoveries mustbe evaluated by determining whether the concentration (measured as percent
recovery) falls within the required recovery limits.

3.5.

Matrix Spike/Matrix Spike Duplicate (MS/MSD): A matrix spike is anenvironmental sample to which known concentrations of target analytes have been
added. A matrix spike duplicate is a second aliquot of the same sample that is
prepared and analyzed along with the sample and matrix spike. Matrix spikes andduplicates are used to evaluate accuracy and precision in the actual sample matrix.

3.6.

Calibration Check Compound (CCC): CCCs are a representative group ofcompounds that are used to evaluate initial calibrations and calibration
verifications. Relative percent difference for the initial calibration and % drift (or %difference) for the calibration verification response factors are calculated andcompared to the specified method criteria.

3.7.

System Performance Check Compounds (SPCC): SPCCs are compounds that are
sensitive to system performance problems and are used to evaluate system
performance and sensitivity. A response factor from the calibration verification is
calculated for the SPCC compounds and compared to the specified method criteria.

3.8.

Internal Standards (IS): Internal Standards are compounds added to every standard,
QC sample, client sample or extract at a known concentration prior to analysis forthe purpose of quantitation. For example, internal standards are used as the basis forquantitation of target compounds by GC/MS.

3.9.

Additional definitions can be found in the TestAmerica Knoxville Quality
Assurance Manual (QAM), current revision.

INTERFERENCES
4.1.

Method interferences may be caused by contaminants in solvents, reagents,
glassware, and other processing apparatus that lead to discrete artifacts. All of thesematerials must be routinely demonstrated to be free from interferences underconditions of the analysis by running laboratory method blanks as described in the
Quality Control section. The use of ultra high purity gases, pre-purged purified
reagent water, and approved lots of purge and trap grade methanol will greatly
reduce introduction of contaminants. In extreme cases the purging vessels may be
pre-purged to isolate the instrument from laboratory air contaminated by solventsused in other parts of the laboratory.

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5.

4.2.

Samples can be contaminated by diffusion of volatile organics (particularly
methylene chloride and fluorocarbons) into the sample through the septum seal
during shipment and storage. A field blank prepared from reagent water and carriedthrough the sampling and handling protocol can serve as a check on suchcontamination.

4.3.

Matrix interferences may be caused by non-target contaminants that are coextracted
from the sample. The extent of matrix interferences will vary considerably fromsource to source depending upon the nature and diversity of the site being sampled.

4.4.

Cross-contamination can occur whenever high-level and low-level samples areanalyzed sequentially or in the same purge position on an autosampler. Wheneveran unusually concentrated sample is analyzed, it should be followed by one or more
blanks to check for cross-contamination. The purge and trap system may require
extensive bake-out and cleaning after a high-level sample.

4.5.

Some samples may foam when purged due to surfactants present in the sample. The
samples may be diluted to preserve instrument integrity.

SAFETY
5.1.

Employees must abide by the policies and procedures in the TestAmerica
Environmental Health and Safety Manual, and this document.

5.2.

Specific Safety Concerns or Requirements

5.3.

5.2.1.

The gas chromatograph and mass spectrometer contain zones that haveelevated temperatures. The analyst needs to be aware of the locations of
those zones, and must cool them to room temperature prior to working onthem.

5.2.2.

The mass spectrometer is under deep vacuum. The mass spectrometermust be brought to atmospheric pressure prior to working on the source.
Depending on the type of work involved, either turn the power to the
instrument off, or disconnect it from its source of power.

Primary Materials Used: The following is a list of the materials used in this method,which have a serious or significant hazard rating. NOTE: This list does not include
all materials used in the method. The table contains a summary of the primaryhazards listed in the SDS for each of the materials listed in the table. A
complete list of materials used in the method can be found in the reagents andmaterials section. Employees must review the information in the SDS for eachmaterial before using it for the first time or when there are major changes to the
SDS.

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Material

Hazards

Exposure
Limit (2)Signs and symptoms of exposure

MethanolFlammable
PoisonIrritant

200 ppmTWA

A slight irritant to the mucous membranes. Toxic effects exerted
upon nervous system, particularly the optic nerve. Symptoms ofoverexposure may include headache, drowsiness and dizziness.
Methyl alcohol is a defatting agent and may cause skin to become
dry and cracked. Skin absorption can occur; symptoms may parallel
inhalation exposure. Irritant to the eyes.

1– Exposure limit refers to the OSHA regulatory exposure limit.

5.3.1.

6.

Chemicals that have been classified as carcinogens, or potential
carcinogens, under OSHA include acrylonitrile, benzene, carbon
tetrachloride, chloroform, 1,2-dibromo-3-chloropropane, 1,4dichlorobenzene, and vinyl chloride.

5.4.

Exposure to chemicals must be maintained as low as reasonably achievable,
therefore, unless they are known to be non-hazardous, all samples should be
opened, transferred, and prepared in a fume hood, or under other means ofmechanical ventilation. Solvent and waste containers will be kept closed unlesstransfers are being made.

5.5.

The preparation of standards and reagents will be conducted in a fume hood withthe sash closed as far as the operations will permit.

5.6.

All work must be stopped in the event of a known or potential compromise to thehealth and safety of an associate. The situation must be reported immediately to alaboratory supervisor.

EQUIPMENT AND SUPPLIES
6.1.

Microsyringes: 10 L and larger, 0.006 inch ID needle.

6.2.

Syringe: 5 or 25 mL glass with luerlok tip, if applicable to the purging device.

6.3.

Balance capable of weighing 0.01 g.

6.4.

Glassware:

6.5.

6.4.1.

Vials, with screw caps and Teflon liners: 5 ml, 20 ml and 40 ml.

6.4.2.

Volumetric flasks: 10 mL and 100 mL, class A with ground-glass
stoppers.

Spatula: Stainless steel.

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6.6.

Disposable pipets: Pasteur.

6.7.

pH paper: Wide range.

6.8.

Stir bars.

6.9.

Gases:

6.10.

6.11.

6.9.1.

Helium: Ultra high purity, gr. 5, 99.999%.

6.9.2.

Compressed air: Used for instrument pneumatics.

6.9.3.

Liquid nitrogen: Used for cryogenic cooling if necessary.

Purge and Trap Device: The purge and trap device consists of the sample purger,
the trap, the desorber and the transfer line to the GC.
6.10.1.

Sample Purger: The recommended purging chamber is designed to accept
25 mL samples with a water column at least 3 cm deep. The purge gas
must pass through the water column as finely divided bubbles, each with adiameter of less than 3 mm at the origin. The purge gas must be
introduced no more than 5 mm from the base of the water column.
Alternative sample purge devices may be used provided equivalent
performance is demonstrated. Low level soils are purged directly from a
VOA vial.

6.10.2.

Trap: A variety of traps may be used, depending on the target analytes
required. For most purposes the Vocarb 3000 trap is suitable. Other traps,
such as Vocarb 4000, or Tenax/Silica gel/Charcoal may be used if thequality control criteria are met.

6.10.3.

Desorber: The desorber should be capable of rapidly heating the trap to
250C. Many such devices are commercially available.

6.10.4.

Sample Heater: A heater capable of maintaining the purge device at 40C
is necessary for low level soil analysis.

Gas Chromatograph/Mass Spectrometer System:
6.11.1.

Gas Chromatograph/Mass Spectrometer (GC/MS) System: An HP5973
analytical system complete with a temperature-programmable gas
chromatograph. The GC capillary column is directly coupled to the MS
source.

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7.

6.11.2.

Column: 20 m x 0.18 mm I.D. 1-µm film thickness silicon-coated fusedsilica capillary column (J&W DB-624 or equivalent).

6.11.3.

Mass Spectrometer: The mass spectrometer must be capable of scanning35-300 AMU every two seconds or less, using 70 volts electron energy inthe electron impact mode and capable of producing a mass spectrum thatmeets the required criteria when 50 ng of 4-bromofluorobenzene (BFB)
are injected onto the gas chromatograph column inlet.

6.11.4.

Data System: A computer system must be interfaced to the mass
spectrometer. The system must allow the continuous acquisition andstorage on machine-readable media of all mass spectra obtained
throughout the duration of the chromatographic program. The computer
must have software that allows searching any GC/MS data file for ions ofa specific mass and can plot such ion abundances versus time or scannumber. This type of plot is defined as the Extracted Ion Current Profile(EICP). Software must also be available that allows integrating theabundances in any EICP between specified time or scan-number limits.
Also, for the non-target compounds, software must be available thatallows for the comparison of sample spectra against reference library
spectra. The most recent release of the NIST/EPA mass spectral libraryshould be used as the reference library. The computer system must also becapable of backing up data for long-term off-line storage.

6.11.5.

Autosampler: Varian Archon, Tekmar Solatek, Tekmar Aquatek, OI
Analytical Sample Processor or equivalent.

REAGENTS AND STANDARDS
7.1.

7.2.

Reagents
7.1.1.

Methanol: Purge and Trap Grade, High Purity

7.1.2.

Reagent Water: High purity water that meets the requirements for amethod blank when analyzed. (See section 9.4) Reagent water may bepurchased as commercial distilled water and prepared by purging with aninert gas overnight. Other methods of preparing reagent water are
acceptable.

7.1.3.

Sodium bisulfate

7.1.4.

Reagent sand (e.g., Ottawa sand), Fisher Scientific , Cat# S801561 orequivalent. No expiration date applied to sand.

Standards

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7.2.1.

Calibration Standards
7.2.1.1.

Stock Solutions: Stock solutions may be purchased as certified
solutions from commercial sources or prepared from purestandard materials as appropriate. These standards are preparedin methanol and stored in Teflon-sealed screw-cap bottles withminimal headspace at -10°to -20°C.
NOTE: Unopened stock solutions expire according to the
manufacturer’s expiration date. Once opened, the stock
solution expires on the manufacturer’s expiration date or in 6
months, whichever is shorter. Stock standards prepared frompure standard materials expire 6 months from date of
preparation. Stock standards for gases expire one week after
opening.

7.2.1.2.

Working standards: A working solution containing thecompounds of interest prepared from the stock solution(s) inmethanol. These standards are stored in the freezer or asrecommended by the manufacturer. Working standards aremonitored by comparison to the initial calibration curve. If anyof the calibration check compounds drift in response from theinitial calibration by more than 20% then corrective action isnecessary. This may include steps such as instrument
maintenance, preparing a new calibration verification standard
or tuning the instrument. If the corrective actions do not correct
the problem, then a new initial calibration must be performed.

7.2.1.3.

Aqueous Calibration Standards are prepared in reagent waterusing the secondary dilution standards. These aqueous
standards must be prepared daily.
NOTE: The following expiration criteria apply to working
standards from above and the standards described in 7.2.2 –7.2.6. Working standards made from stock solutions shall be
replaced after one week. Stock standards for gases shall be
replaced after one week. When using premixed certified
standards, the unopened standard expiration is according to
manufacturer’s expiration.

7.2.2.

Internal Standards: Internal standards are added to all samples, standards,
and blank analyses. Refer to Table 3 (or Table 3A for SIM) for internal
standard components.

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7.2.3.

Surrogate Standards: Refer to Table 4 (or Table 4A for SIM) for surrogate
standard components and spiking levels.

7.2.4.

Laboratory Control Sample Spiking Solutions: Refer to Tables 1 and 2 for
LCS components. Full analyte spikes are typically used (Tables 1 and 2).

7.2.5.

Matrix Spiking Solutions: The matrix spike contains the same components
as the LCS. Refer to Tables 1,and 2.

7.2.6.

Tuning Standard: A standard is made up that will deliver 50 ng on column
upon injection. A recommended concentration of 50 ng/L of 4-Bromofluorobenzene in methanol is prepared as described in Sections 7.2.1.1 and7.2.1.2.
7.2.6.1. Note: A tuning standard is not required for SIM analysis

8.

SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1.

Sampling is not performed for this method by TestAmerica Knoxville. For
information regarding sample shipping, refer to SOP KNOX-SC-0003, Sample
Receipt and Log In, current revision.

8.2.

Holding times for all volatile analysis are 14 days from sample collection. The
holding time for surface or ground water samples that are known to be notpreserved prior to receipt is 7 days from collection.

8.3.

The maximum holding time is 14 days from sampling until the sample is analyzed.
Samples must be either preserved in the field or delivered in EnCore samplers forlaboratory preservation. Lack of preservation must be addressed in the casenarrative. Maximum holding time for the EnCore sampler (before the sample isadded to methanol or sodium bisulfate or water) is 48 hours.

8.4.

Aqueous samples are stored in 40ml glass vials with Teflon lined septa not frozen
at ≤6°C, with minimum headspace.

8.5.

Methanol solid extracts are allocated into 2 - 20 mL glass vials with Teflon lined
caps and stored at ≤6°C.

8.6.

Water samples are normally preserved at pH ≤ 2 with hydrochloric acid. If residual
chlorine is present, 2 drops of 10% sodium thiosulfate are added.

8.7.

Soil samples are typically taken using the EnCore™ sampler and preserved in thelab within 48 hours of sampling. Solid samples may be field preserved with sodium
bisulfate solution for low level analysis, or with methanol for high level analysis.

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For low level soil samples with carbonaceous material present, reagent water may
be used.
8.8.

There are several methods of sampling soil. The recommended method, which
provides the minimum of field difficulties, is to take a 5 g EnCore sample.
Following shipment back to the lab, the soil is preserved in methanol. This is thehigh level procedure. If very low detection limits are needed (< 200 g/kg), then it
will be necessary to use two additional 5 g EnCore samplers or to use fieldpreservation.

8.9.

Sample collection for high level analysis using EnCore samplers.

8.10.

8.9.1.

Ship one 5 g EnCore sampler per field sample position.

8.9.2.

An additional bottle must be shipped for percent moisture determination.

8.9.3.

When the samples are returned to the lab, extrude the (nominal) 5g sample
into a tared VOA vial containing 5 mL methanol. Obtain the weight of thesoil added to the vial and note on the label.

8.9.4.

Prepare a method blank and an LCS for each batch by adding 5 mL
methanol to 5 g sand.

8.9.5.

Shake the samples for two minutes to distribute the methanol throughout
the soil.

8.9.6.

Allow to settle, then remove a portion of methanol and store in a clean
Teflon capped vial at ≤6°C until analysis.

Sample collection for high level analysis using field methanol preservation
8.10.1.

Prepare a 20 ml sample container by adding 5.0 mL purge and trap grade
methanol.

8.10.2.

Seal the bottle and attach a label.

8.10.3.

Weigh the bottle to the nearest 0.1g and note the weight on the label.

8.10.4.

Ship with appropriate sampling instructions.

8.10.5.

Each sample will require an additional bottle with no preservative forpercent moisture determination.

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8.10.6.

At client request, the methanol addition and weighing may also be
performed in the field.

8.10.7.

When the samples are returned to the lab, obtain the weight of the soil
added to the vial and note on the label.

8.10.8.

Prepare a method blank and an LCS for each batch by adding 5 mL
methanol to 5 g sand.

8.10.9.

Shake the samples for two minutes to distribute the methanol throughout
the soil.

8.10.10. Allow to settle, then remove a portion of methanol and store in a clean
Teflon capped vial at ≤6°C until analysis.
8.11.

Low level procedure
8.11.1.

If low detection limits are required (typically < 200 g/kg), sodium
bisulfate preservation must be used. However, it is also necessary to take asample for the high level procedure (field methanol preserved or using the
EnCore sampler), in case the concentration of analytes in the soil isabove the calibration range of the low level procedure.

8.11.2.

A purge and trap autosampler capable of sampling from a sealed vial isrequired for analysis of samples collected using this method (Varian
Archon).

8.11.3.

The soil sample is taken using a 5g EnCore sampling device andreturned to the lab. It is recommended that two EnCore samplers be used
for each field sample position to allow for any reruns that may benecessary. A separate sample for % moisture determination is also
necessary.

8.11.4.

Prepare VOA vials by adding a magnetic stir bar, approximately 1 g of
sodium bisulfate and 5 mL of reagent water.

8.11.5.

Seal and label the vial. It is strongly recommended that the vial is labeledwith an indelible marker rather than a paper label, since paper labels may
cause the autosampler to bind and malfunction. The label absolutely must
not cover the neck of the vial or the autosampler will malfunction.

8.11.6.

Weigh the vial to the nearest 0.1g and note the weight in the TALS prepbatch.

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8.11.7.

Extrude the soil sample from the EnCore sampler into the prepared
VOA vial. Reweigh the vial to obtain the weight of soil and note in the
TALS prep batch.
NOTE: Soils containing carbonates may effervesce when added to thesodium bisulfate solution. If this is the case, add 5 mL of water instead,and freeze at <-10°C until analysis. The holding time for the frozen
sample is 14 days from sampling. If one sample from a lot (site)
effervesces, all soil samples from the site will be preserved in water toprotect the integrity of the samples, unless otherwise specified by theclient.

8.12.

8.11.8.

Alternatively the sodium bisulfate preservation may be performed in thefield. This is not recommended because of the many problems that canoccur in the field setting. Ship at least two vials per sample. The fieldsamplers must determine the weight of soil sampled. Each sample will
require an additional bottle with no preservative for percent moisturedetermination, and an additional bottle preserved with methanol for thehigh level procedure. Depending on the type of soil, it may also benecessary to ship vials with no or extra preservative.

8.11.9.

A preservation blank is prepared using the same reagents (i.e., sodium
bisulfate/water solution) as the samples. A stir bar and 5 grams sand is
added to the vial. The preservation blank is analyzed and evaluated using
the same criteria as the method blank.

Unpreserved soils
8.12.1.

8.13.

At specific client request, unpreserved soils packed into glass jars or brass
tubes may be accepted and subsampled in the lab. This is the oldprocedure based on method 5030. It is no longer included and is likely togenerate results that are biased low, possibly by more than an order ofmagnitude.

Holding Blank
8.13.1.

Sample receiving prepares holding blanks using reagent water obtained
from the Metals laboratory and places the vials in the refrigerators used tostore samples for volatiles analysis. These are logged into TALS once
each week and are removed for analysis after two weeks.

8.13.2.

The holding blanks are analyzed according to this SOP. The holding blankmust be less than ½ the standard 25-ml purge reporting limit (RL) (<RL
for common laboratory contaminants). If the holding blank is greater than
½ RL but less than the RL (for analytes that are not common lab

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contaminants) document this on the quantitation report for the holding
blank. If the holding blank is greater than the RL for any analyte,
document this on the quantitation report and in a nonconformance memo.
As corrective action, review associated method blanks and samples for thepresence of any analyte greater than the RL that may be due to laboratory
contamination that was observed in the associated holding blank. Iflaboratory contamination is observed in client samples, ensure that thedata is appropriately flagged (B qualifier). Also discuss thenonconformance in the project narrative.
8.14.

The methanol extracts are stored prior to analysis at ≤6°C. When long term storage
after the analysis is requested by the client, the methanol extracts are also stored at≤6°C.

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EnCore procedure when low level is not required (field steps in gray)
Extrude soil sample

Ship one EnCore
sampler and one bottle
for %moisture persample location

Reweigh vial to obtainsoil weight.

from EnCore into tared

Take core sample and% moisture sample

septum capped vial
containing 5 mL
methanol

Shake for 2
minutes. Allow

Sample is ready for
analysisto settle.

EnCore procedure when low level is required
Ship three 5 g EnCore
samplers and one
bottle for%moisture per sample
location

Reweigh vial to obtainsoil weight.

Extrude the two 5g
samplers into separate
tared VOA vials
containing 5 mL
sodium bisulfate
solution*

Extrude 5g soil
sample from EnCore
into tared septum
capped vial containing
5 mL methanol

Take core samples and% moisture sample

Shake for 2 minutes.
Allow to settle.

Store for low level
analysis if needed

Sample is ready for
analysis

Sample is ready for
analysis* Or 5 ml reagent water if samples from the lot or site effervesce.

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Field methanol extraction procedure (field steps in gray)Prepare a septum
capped vial containing
5 mL methanol foreach sample location

Weigh the vial andrecord the weight to thenearest 0.01g on thelabel.

Ship following DOT
regulations for
flammable liquids andinclude a separate
bottle for each sample
location for % moisture

Weigh the vial andensure that the weightis the same as that
listed on the label. (Ifnot, use a different vial)

Take a (nominal) 5g
core sample using an
EnCore sampler or acut off plastic syringe

Extrude the sample
into the vial, taking
care not to splash any
methanol out of the vial

Cap the vial and record
the weight on the label

Take a separate
sample for % moistue

Return to the lab
following DOT shipping
regulations for
flammable liquids.

Weigh the sample vial
on receipt. If different
from the weight notedby the sampling crew,note as an anomaly
and contact the client

Shake for two minutes.
Allow to settle.

Sample is ready for
analysis

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Field bisulfate preservation procedure (field steps in gray)Prepare a septum
capped vial containing
1g sodium bisulfate in
5 mL water for eachsample location

Weigh the vial andrecord the weight to thenearest 0.01g on thelabel.

Ship following DOT
regulations forcorrosive liquids andinclude a separate
bottle for each sample
location for % moisture

Weigh the vial andensure that the weightis the same as that
listed on the label. (Ifnot, use a different vial)

Take a (nominal) 5g
core sample using an
EnCore sampler or acut off plastic syringe

Extrude the sample
into the vial, taking
care not to splash any
sodium bisulfate out ofthe vial

Evaluate for
effervescence. Any
significant
effervescence willcause loss of volatiles
and may result in thevial exploding

The field methanol or
EnCore procedures arerecommended for soils
that effervesce withbisulfate

Cap the vial and record
the weight on the label

Take a separate
sample for % moistue

Return to the lab
following DOT shipping
regulations forcorrosive liquids.

Weigh the sample vial
on receipt. If different
from the weight notedby the sampling crew,note as an anomoly
and contact the client

Sample is ready for
analysis.

Notes:
1.
When following this procedure, a methanol
preserved sample must also be collected, for screening
and in case the sample contains high levels of analytes.
2.
Due to the high probability of sampling problems,
this method is not recommended

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9.

QUALITY CONTROL
9.1.

Initial Demonstration of Capability
9.1.1.

9.2.

Control Limits: In-house historical control limits must be determined forsurrogates, matrix spikes, and laboratory control samples (LCS). These limits are
determined annually. The historical control limits are set to the mean recovery +/- 3
standard deviations for surrogates, matrix spikes and LCS as described in SOP
KNOX-QA-0004, current revision.
9.2.1.

9.3.

The initial demonstration described in section 13 and method detection
limit (MDL) studies must be acceptable before analysis of samples may
begin. MDLs must be analyzed for soils and aqueous samples. See section
13 for acceptance criteria.

All surrogate, LCS, and MS recoveries (except when surrogates are
diluted greater than 5X) must be entered into TALS (when available) orother database so that accurate historical control limits can be generated.
For tests without a separate extraction, surrogates and matrix spikes will
be reported for all dilutions.

Surrogates: Every sample, blank, and QC sample is spiked with surrogates.
Surrogate recoveries in samples, blanks, and QC samples must be assessed toensure that recoveries are within established limits. The compounds included in thesurrogate spiking solutions are listed in Table 4 (or Table 4A for SIM). Reanalyze
samples with failing surrogates if sufficient sample material is available and matrix
effects have not already been confirmed. The client may be contacted for input if
the reanalysis is expected to take place after the sample holding time has been
exceeded. If any surrogates are outside limits, the following corrective actions musttake place (except when surrogates are diluted greater than 5X):

 Check all calculations for error.
 Ensure that instrument performance is acceptable.
 Recalculate the data and/or reanalyze if either of the above checks reveal aproblem.
 Reprepare and reanalyze the sample or flag the data as “EstimatedConcentration” if neither of the above resolves the problem.
The surrogate dibromofluoromethane has been determined to degrade inaqueous samples with pH ≥10, as well as soils where the preserved sample
solution has a resulting pH ≥10. In these cases, the samples do not need to bereanalyzed. This should be noted in the narrative.

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9.4.

9.3.1.

The decision to reanalyze or flag the data should be made in consultation
with the client. It is only necessary to reprepare/reanalyze a sample once
to demonstrate that poor surrogate recovery is due to matrix effect, unlessthe analyst believes that the repeated out of control results are not due tomatrix effect.

9.3.2.

If the surrogates are out of control for the sample, matrix spike and matrix
spike duplicate, then matrix effect has been demonstrated for that sample
and repreparation is not necessary as long as the LCS and method blankare acceptable. If the sample is out of control and the MS and/or MSD isin control, then reanalysis or flagging of the data is required.

9.3.3.

Refer to the QC Program document (QA-003) for further details of thecorrective actions.

Method Blanks: For each batch of samples, analyze a method blank. The method
blank is analyzed after the calibration standards, normally before any samples. The
method blank contains the same reagents as the samples (e.g. 1 gram of sodium
bisulfate per 5 ml reagent water for low level soils). For low-level waters, themethod blank consists of reagent water. For high-level volatiles, the method blankconsists of 5.0 mL of methanol and 5 g reagent sand. Surrogates are added and themethod blank is carried through the entire analytical procedure. The method blankmust not contain any analyte of interest at or above the reporting limit (except
common laboratory contaminants, see below) or at or above 10% of the measured
concentration of that analyte in the associated samples, whichever is higher.

 If the analyte is a common laboratory contaminant (methylene chloride,
acetone, 2-butanone and toluene) the data may be reported with qualifiers when
the concentration of the analyte is less than five times the reporting limit.
 Reanalysis of samples associated with an unacceptable method blank is required
when reportable concentrations are determined in the samples.
 If there is no target analyte greater than the RL in the samples associated withan unacceptable method blank, the data may be reported with qualifiers. Suchaction should be done in consultation with the client.
9.4.1.

The method blank must have acceptable surrogate recoveries. If surrogate
recoveries are not acceptable, the data must be evaluated to determine if
the method blank has served the purpose of demonstrating that theanalysis is free of contamination. If surrogate recoveries are low and there
are reportable analytes in the associated samples, re-extraction of theblank and affected samples will normally be required. Consultation withthe client should take place.

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9.5.

9.4.2.

If reanalysis of the batch is not possible due to limited sample volume orother constraints, the method blank is reported, all associated samples are
flagged with a "B", and appropriate comments may be made in a narrative
to provide further documentation.

9.4.3.

Refer to the QC Program document (QA-003) for further details of thecorrective actions.

A laboratory control sample (LCS) is prepared and analyzed with every batch ofsamples. The LCS contains the standard set of target analytes (See Tables 1, and2). The analytes are spiked at the same concentration as the calibration verification
standard.
9.5.1.

All target analytes requested that are listed in Tables 1 and 2 areconsidered control analytes in the LCS. Historical LCS limits are basedon the mean recovery +/- 3 standard deviations as described in SOP
KNOX-QA-0004, current revision. Marginal exceedances are allowed
depending on the number of target analytes requested. The control limits
for marginal exceedences are set to mean +/- 4 standard deviations. See
the following table for the number of allowed marginal exceedances.

Number of target analytes in LCS

Allowable # of marginal exceedances of LCS
control limits>90

5

71 – 904

51 – 703

31 – 50

2

11 – 30

1

< 11

0

9.5.2.

An LCS is considered to be “out of control” if any target analyte is outside
marginal exceedance limits, or if the total number of marginalexceedances is more than the allowed number. A nonconformance memomust be issued and corrective action must occur.

9.5.3.

If marginal exceedances are observed, the analyst must review theprevious LCS (e.g., review the control chart) for each analyte marginally
exceeding the control limits to determine if the marginal exceedance is aconsecutive occurrence. If there are two consecutive marginal

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exceedances for the same analyte, the LCS is considered “out of control”
and an NCM must be generated and corrective action taken.
9.5.3.1.

9.5.4.

9.6.

When evaluating the control chart, the analyst should also
check whether there was more than one out of the last threeconsecutive LCSs outside control limits. If more than one outof the last three LCSs was outside the LCS control limits but
within the marginal exceedance limits, then the analyst should
evaluate the system for non-random systematic trends.

Samples in the same batch as an LCS determined to be “out of control”
shall be considered suspect and the samples re-analyzed or the datareported with appropriate data qualifying codes.
9.5.4.1.

If the LCS recovery for a target analyte is biased high outside
acceptance limits and that target analyte is not detected in anyof the associated samples above the reporting limit, the sample
data may be reported with qualification in the project narrative.
Analytes that are biased high in the LCS and not detected in
the associated samples are counted in the total number ofallowable marginal exceedances.

9.5.4.2.

If the batch is not reanalyzed, the reasons for reporting thebatch must be clearly presented in the project narrative (e.g.
due to limited sample volume)

9.5.5.

Ongoing monitoring of the LCS provides evidence that the laboratory is
performing the method within accepted QC guidelines for accuracy andprecision .

9.5.6.

Refer to the QC Program document (QA-003) for further details of thecorrective action.

Matrix Spike/Matrix Spike Duplicate (MS/MSD): A matrix spike/matrix spike
duplicate (MS/MSD) is prepared and analyzed with every batch of samples. The
MS/MSD is spiked with the same analytes as the LCS. Compare the percent
recovery and relative percent difference (RPD) to that in the laboratory specific,
historically generated limits; limits are based on the mean recovery +/- 3 standard
deviations
9.6.1.

If any individual spiked target analyte recovery or RPD falls outside theacceptable range, corrective action must occur. The initial corrective
action will be to check the recovery of that analyte in the LCS. If the LCS
meets the acceptance limits stated in Section 9.5, then the laboratory

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operation is in control and analysis may proceed; spike recovery or spike
RPD failure is attributed to matrix effects.

10.

9.6.2.

If a MS/MSD is not possible due to limited sample, then a LCS duplicate
should be analyzed. RPD of the LCS and LCSD are compared to historicallimits.

9.6.3.

The matrix spike/duplicate must be analyzed at the same dilution as theunspiked sample, even if the matrix spike compounds will be diluted out.

9.7.

For internal standard recovery acceptance criteria, refer to section 11.9.1.

9.8.

Nonconformance and Corrective Action: Any deviations from QC procedures must
be documented as a nonconformance, with applicable cause and corrective action
approved by the facility QA Manager or designee.

9.9.

Quality Assurance Summaries: Certain clients may require specific project orprogram QC that may supersede these method requirements. Quality Assurance
Summaries should be developed to address these requirements.

CALIBRATION AND STANDARDIZATION
10.1.

Refer to CA-Q-S-002, Manual Integration Practices, current revision for
information on manual integration practices and documentation requirements.

10.2.

Summary
10.2.1.

Prior to the analysis of samples and blanks, each GC/MS system must be
tuned and calibrated. Hardware tuning is checked through the analysis of
the 4-bromofluorobenzene (BFB) to establish that a given GC/MS systemmeets the standard mass spectral abundance criteria. The GC/MS system
must be calibrated initially at a minimum of five concentrations (analyzed
under the same BFB electronic settings), to determine the linearity of the
response utilizing target calibration standards. Once the system has beencalibrated, the calibration must be verified each twelve hour time period
for each GC/MS system. The use of separate calibrations is required forwater and low soil matrices.
10.2.1.1. Note: A BFB tune is not required for SIM analysis. The mass
spectrometer is tuned as needed using perfluorotributylamine(PFTBA) and the instrument data system autotune program.
Select the BFB tune optimization profile for the autotune
program.

10.3.

Recommended Instrument Conditions

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10.3.1.

General (full scan mode)
Electron Energy:
Mass Range:
Scan Time:70 volts (nominal)
35–300 AMU
to give at least 5 scans/peak, but not to exceed 2
second/scan
Injector Temperature: 200–250C
Source Temperature: According to manufacturer's specifications
Transfer Line
Temperature: 250–300C
Purge Flow:
40 mL/minute
Carrier Gas
Flow: 30 mL/minuteInjector Condition:
1/35 split
10.3.2.

SIM mode
Recommended GC & GC/MS Conditions are the same as 10.3.1 except
the mass range is determined by the quantitation and secondary/tertiaryions monitored for each analyte, internal standard, and surrogate. See
table 8 for the primary ion for quantitation, and use at least one of thesecondary and/or tertiary ions as a monitor ion. Use the retention times
from the full-scan analysis to set the MID switchpoints so that eachanalyte’s elution time falls within their respective MID groups. See
Figure 1 for example of GC & GC/MS conditions and settings.

10.3.3.

Gas chromatograph suggested temperature program
10.3.3.1.

BFB Analysis: 150C for 1 minute, then 20C/minute until
200C.

10.3.3.2.

Sample Analysis
Initial Temperature:
Initial Hold Time:
Temperature Program:
Final Temperature:
Second Temperature
Final Temperature:
Final Hold Time:10.4. Instrument Tuning

40C
3 minutes
11C/minute
195C
Program: 25C/minute
220C
2.0 minutes

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10.4.1.

Each GC/MS system must be hardware-tuned to meet the abundance
criteria listed in Table 5 for a maximum of a 50 ng injection or purging of
BFB. Analysis must not begin until these criteria are met. These criteria
must be met for each twelve-hour time period. The twelve-hour time
period begins at the moment of injection of BFB.
10.4.1.1. Note: A BFB tune is not required for SIM analysis. The 12hour period begins at the moment of injection of the first
acceptable ICAL point.

10.4.2.

10.5.

Inject 50 ng of the GC/MS tuning standard (1 uL of the 50 ug/ml solution)
into the GC/MS system. Obtain a mass spectra of BFB and confirm that
all the key m/z criteria in Table 5 are achieved. The typical approach is to
use the average of the peak apex, the scan immediately before the apex,
and the scan immediately after the apex, with background subtraction of asingle scan. This single scan must be prior to and within 20 scans of thestart of the BFB elution but must not be part of the BFB peak.
Alternatively the peak apex may be used. Background subtraction isrequired. If all the criteria in Table 5 are not achieved, the analyst must
retune the mass spectrometer and repeat the test until all criteria areachieved. The performance criteria must be achieved before any samples,blanks, or standards are analyzed.

Initial Calibration
10.5.1.

A series of five or more initial calibration standards is prepared andanalyzed for the target compounds and each surrogate compound. Typicalcalibration levels are given in Tables 9 and 10 (or Table 9A for SIM).
Other calibration levels and purge volumes may be used depending on thecapabilities of the specific instrument. However, the same purge volume
must be used for calibration and sample analysis, and the low levelstandard must be at or below the reporting limit.

10.5.2.

It may be necessary to analyze more than one set of calibration standards
to encompass all of the analytes required for some tests.

10.5.3.

Internal standard calibration is used. The internal standards are listed inTable 3 (or Table 3A for SIM). Target compounds are typically referenced
to the nearest internal standard (see Table 8). Each calibration standard isanalyzed and the response factor (RF) for each compound is calculatedusing the area response of the characteristic ions against the concentrationfor each compound and internal standard. See section 12.4.1 forcalculation of response factor.

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10.5.4.

The high point calibration standard is checked for saturation. If aquantitation ion saturates the mass spectrometer, the analyte will be
removed from the calibration series, and the next highest concentration ischecked for saturation as well. Saturation is present when an ion peak in
Chrom reaches a Y axis maximum of 8.4 X 106.

10.5.5.

The % RSD of the calibration check compounds (CCC) must be less thanor equal to 30%. Refer to Table 7 for the CCCs.

10.5.6.

The average RF must be calculated for each compound. A system
performance check is made prior to using the calibration curve. The fivesystem performance check compounds (SPCC) are checked for aminimum average response factor. Refer to Table 6 for the SPCC
compounds and required minimum response factors.
10.5.6.1.

If none of the SPCCs are required analytes, project specificcalibration specifications must be agreed to with the client.

10.5.7.

The analyst will evaluate analytes with %RSD > 15% for calibration on a
curve.

10.5.8.

A read-back of the low calibration point used in the calibration curveshould have a read-back (%D) of no more than 50% for any calibration
model. However, common laboratory contaminants (i.e. methylene
chloride and acetone) and poor performing compounds (defined by QA
and control charts) may have a read-back limit of no more than 80%.

10.5.9.

Linear or quadratic curve fits may be used. Use of 1/Concentration2
weighting may be used to improve the accuracy of quantitation at the low
end of the curve. The correlation coefficient (coefficient of determination
for non-linear curves) must be > 0.990.
10.5.9.1.

Analyst may elect to drop points from the calibration to
improve subsequent quantitation. The rules for dropping pointsare: May drop points below the RL as long as there is a point
remaining at or below the RL.
 May drop high points, decreasing linear range.
 May NOT drop a point between points.
For more guidance see “CA-Q-P-003, Calibration Curves
and the Selection of Calibration Points, current revision.”

10.5.9.2.

Rules for curve use:
 The r^2 value obtained from Chrom™ must be >0.990.

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 At least 5 points must be used for average or linear curve.
 At least 6 points must be used for a quadratic curve.
 For quadratic curves, the tangent line to the slope of thecurve must be continuous and have either only positive or
negative slopes (i.e., no parabolas or breaks in the curve).
Quadratic curves cannot be used to extend the calibration
range.
 Forcing through zero is allowed. To activate “force
through zero” in Chrom, pick a “Curve Select” model thatuses a “Force” for “Origin”. “Include” zero for “curve
origin” must NOT be used.
 If “forced through zero” is not used, the X and Y-intercept
must be below the RL.
 To evaluate the X- and Y-intercept, evaluate eachanalyte’s Curve Details in Chrom to ensure that the Zero
Intercept flag is not activated due to improper intercept.
10.5.9.3. See corporate policy, CA-Q-P-003, “Calibration Curves &Selection of Calibration Points” current revision, fordefinitions and calculations using the different curve models.
10.5.10. If time remains in the 12-hour period initiated by the BFB injection before
the initial calibration, samples may be analyzed. Otherwise, proceed tocalibration verification.
10.5.11. A separate five point calibration must be prepared for analysis of lowlevel soils. Low level soils analysis requires the use of a closed vial
autosampler (Varian Archon). Each standard is prepared by spiking themethanolic standard solution through the septum of a VOA vial containing
5 mL of water and 1 g sodium bisulfate. The standards are heated to 40C
for purging. All low-level soil samples, standards, and blanks must also beheated to 40C for purging. Alternatively, add 5 ml of water to a 40 ml
VOA vial for soil samples that effervesce or are received in jars.
10.5.12. Initial Calibration Verification Standard (2nd Source Standard): A midlevel standard from a second source is analyzed as an initial calibration
verification (ICV). The ICV shall be analyzed with each initial calibration.
The ICV must be within +/- 30% of its expected value. Poorer performing
analytes may have an alternate acceptance criterion with QA approval(e.g., ketones < 35% and alcohols <40%). If the criteria are not met, theanalyst must first verify the concentrations of the primary and secondary
source standards and calculations. If no errors are found, repeat the ICV
analysis.

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10.6.

Calibration verification: The initial calibration must be verified every twelve hours.
10.6.1.

Calibration verification begins with analysis of BFB as described in
Section 10.4. If the system tune is acceptable, the calibration verification
standard(s) are analyzed. The level 3 calibration standard is suggested as
the calibration verification.
10.6.1.1. Note: A BFB tune is not required for SIM analysis. The 12hour period begins at the moment of injection of an acceptable
CCV.

10.6.2.

The RF data or concentrations from the standards are compared with theaverage RF or concentrations from the initial five-point calibration todetermine the percent difference or drift of the CCC compounds. The
calculation is given in Section 12.4.4.

10.6.3.

The % drift or difference of the CCCs must be ≤ 20% for the calibration
verification to be valid. The SPCCs are also monitored. The SPCCs mustmeet the criteria described in Table 6. In addition, the % drift of all
analytes must be ≤ 50%.
10.6.3.1.

If none of the CCCs are required analytes, then project specificcalibration specifications should be negotiated with the client.

10.6.4.

If the CCCs and or the SPCCs do not meet the criteria in Sections 10.6.3,
the system must be evaluated and corrective action must be taken. The
BFB tune and calibration verification must be acceptable before analysis
begins. Extensive corrective action such as the installation of a newcolumn will require a new initial calibration.

10.6.5.

Once the above criteria have been met, sample analysis may begin. Initial
calibration average RFs (or the calibration curve) will be used for sample
quantitation, not the calibration verification RFs. Analysis may proceed
until 12 hours from the injection of the BFB have passed. (A sample
desorbed less than or equal to 12 hours after the BFB is acceptable.)
10.6.5.1. Note: For SIM, the 12-hour clock is from the injection of an
acceptable CCV or first point in the initial calibration series.

10.6.6.

If the retention time for any internal standard in the calibration verification
changes by more than 0.5 minutes from the mid-level initial calibration
standard, the chromatographic system must be inspected for malfunctions
and corrected. Reanalysis of samples analyzed while the system was
malfunctioning is required.

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11.

10.6.7.

If the internal standard response in the calibration verification is more than
200% or less than 50% of the response in the mid-level of the initial
calibration standard, the chromatographic system must be inspected formalfunctions and corrected. Reanalysis of samples analyzed while thesystem was malfunctioning is required.

10.6.8.

If the calibration verification does not meet acceptance criteria, corrective
action is required before sample analysis.

10.6.9.

If routine corrective action procedures fail to produce a second
consecutive (immediate) calibration verification within acceptancecriteria, then the laboratory has to demonstrate performance after
corrective action with two consecutive successful calibration verifications.
If the laboratory has not demonstrated acceptable performance, sample
analyses must not occur until a new initial calibration curve is establishedand verified.

PROCEDURE
11.1.

11.2.

Procedural Variations
11.1.1.

One time procedural variations are allowed only if deemed necessary in
the professional judgment of supervision to accommodate variation insample matrix, radioactivity, chemistry, sample size, or other parameters.
Any variation in procedure except those specified by project specificinstructions shall be completely documented using a Nonconformance
Memo and approved by a Supervisor or group leader and QA Manager. If
contractually required, the client shall be notified.

11.1.2.

Any unauthorized deviations from this procedure must also be
documented as a nonconformance, with a cause and corrective action
described.

Preliminary Evaluation
11.2.1.

Where possible, samples are screened by headspace or GC/MS off-tune
analysis to determine the correct aliquot for analysis. Alternatively, anappropriate aliquot can be determined from sample histories.

11.2.2.

Dilutions should be done just prior to the GC/MS analysis of the sample.
Dilutions are made in volumetric flasks or in a Luerlok syringe. Calculate
the volume of reagent water required for the dilution. Fill the syringe withreagent water, compress the water to vent any residual air and adjust thewater volume to the desired amount. Adjust the plunger to the mark andinject the proper aliquot of sample into the syringe. If the dilution required

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would use less than 1 µL of sample, then serial dilutions must be made involumetric flasks.
11.2.2.1.
11.3.

Sample Analysis Procedure
11.3.1.

All analysis conditions for samples must be the same as for the calibration
verification standards (including purge time and flow, desorb time andtemperature, column temperatures, multiplier setting etc.).

11.3.2.

All samples must be analyzed as part of a batch. The batch is a set of up to
20 samples of the same matrix processed using the same procedures andreagents within the same 24 hour time period. The batch also must containa MS/MSD, a LCS, and a method blank. If insufficient sample is available
to perform an MS/MSD pair, an LCS/LCSD pair will be prepared andanalyzed.

11.3.3.

11.4.

The diluted concentration is to be estimated to be in the upper
half of the calibration range. See section 11.10 for guidance.

11.3.2.1.

If there is insufficient time in the 12-hour tune period toanalyze 20 samples, the batch may be continued into the nexttune period. For high level soils, waste, or other extracts, thebatch is defined at the sample preparation stage.

11.3.2.2.

Laboratory generated QC samples (blank, LCS, MS/MSD) do
not count towards the maximum 20 samples in a batch. Field
QC samples are included in the batch count.

11.3.2.3.

It is not always necessary to reanalyze batch QC withreanalyses of samples. For example, if the samples need to beanalyzed at a different dilution, batch QC does not need to bereanalyzed. If samples need to be reanalyzed because the batch
QC failed, then batch QC must be reanalyzed. Also, any reruns
must be part of a valid batch

Weight/volume entries in the TALS Preparation Batch are not to be
included in the Chrom Worklist, which would lead to “double-calculation”
of the preparation step (e.g. initial/final weight/volumes & dilution
factors).

Water Samples
11.4.1.

All samples and standard solutions must be at ambient temperature before
analysis.

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11.5.

11.4.2.

Fill a syringe with the sample. If a dilution is necessary it may be made in
the syringe if the sample aliquot is ≥ 1 µL. Check and document the pH of
the remaining sample.

11.4.3.

Add each internal and surrogate standard at the concentrations stated inTables 3 and 4 or Tables 3A and 4A for SIM. The internal standards andthe surrogate standards may be mixed and added as one spiking solution
via the autosampler. Inject the sample into the purging chamber.

11.4.4.

The sample is purged for eleven minutes (the trap must be at or below
40C).

11.4.5.

After purging is complete, desorb the sample, start the GC temperature
program, and begin data acquisition. After desorption, bake the trap for 510 minutes to condition it for the next analysis. When the trap is cool, it isready for the next sample.

11.4.6.

Desorb and bake time and temperature are optimized for the type of trap
in use. The same conditions must be used for samples and standards.

Methanol Extract Soils
11.5.1.

11.6.

Add no more than 100 µL methanolic extract (from Section 8.9 or 8.10) to
the 40 ml VOA vial containing 5 ml of organic free water. Add internal
standards and surrogates through the 40 ml vial septum or allow theautosampler to add the appropriate amount. Add the appropriate matrix
spike solution to the vial for the LCS/LCSD/MS/MSD as needed. Loadthe sample onto the autosampler/purge and trap device and analyze as forsoil samples. If less than 1µL of methanolic extract is to be added to thewater, dilute the methanolic extract such that a volume no less than 1µL
will be added to the water in the 40 ml VOA vial.

Liquid wastes that are soluble in methanol and insoluble in water.
11.6.1.

Pipet 2 mL of the sample into a tared vial. Use a top-loading balance.
Record the weight to the nearest 0.1 gram.

11.6.2.

Quickly add methanol, and bring the final volume to 10 mL. Cap the vial
and invert several times to mix thoroughly.

11.6.3.

Add no more than 100 µL methanolic extract to the 40 ml VOA vial
containing 5 ml of organic free water. Add internal standards andsurrogate through the 40 ml vial septa or allow the autosampler to add theappropriate amount. Add the appropriate matrix spike solution to the vial
for the LCS/LCSD/MS/MSD as needed. Load the sample onto the

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autosampler/purge and trap device and analyze as for soil samples. If lessthan 1µL of methanolic extract is to be added to the water, dilute themethanolic extract such that a volume no less than 1µL will be added to
the water in the 40 ml VOA vial.
11.7.

11.8.

Aqueous and Low level Soil Sample Analysis (Purge and Trap units that sample
directly from the VOA vial)
11.7.1.

Units that sample from the VOA vial should be equipped with a modulethat automatically adds surrogate and internal standard solution to thesample prior to purging the sample.

11.7.2.

If the autosampler uses automatic IS/SS injection, no further preparationof the VOA vial is needed. Otherwise the internal and surrogate standards
must be added to the vial. Note: Aqueous samples with high amounts of
sediment present in the vial may not be suitable for analysis on this
instrumentation, or they may need to be analyzed as soils. If multiple vials
are provided and all have sediment present, decant the liquid layer intoanother clean 40-mL VOA vial for analysis, leaving the sediment in theoriginal vial (the sediment is not analyzed).

11.7.3.

Soil samples must be quantitated against a curve prepared with standards
containing about the same amount of sodium bisulfate or water as the
samples (1 g in 5 mL).

11.7.4.

Soil sample remaining in the vial after sampling with one of thesemechanisms is no longer valid for further analysis. A fresh VOA vial must
be used for further sample analysis.

11.7.5.

For aqueous samples, check and document in the TALS batch worksheet
the pH of the sample remaining in the VOA vial after analysis iscompleted.

Low-Level Solids Analysis (from bulk container/jar)Note: This technique may seriously underestimate analyte concentration andmust not be used except at specific client request for the purpose ofcomparability with previous data. It is no longer part of SW-846.
This method is based on purging a heated sediment/soil sample mixed with reagent
water containing the surrogate and internal standards, and matrix spiking standards
when applicable. Analyze all reagent blanks and standards under the same
conditions as the samples (e.g., heated). The calibration curve is also heated during
analysis. Purge temperature is 40oC.

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11.9.

11.8.1.

Do not discard any supernatant liquids. Mix the contents of the container
with a narrow metal spatula.

11.8.2.

Weigh out 5 g (or other appropriate aliquot) of sample into a 40 ml VOA
vial. Record the weight to the nearest 0.1 g. If method sensitivity isdemonstrated, a smaller aliquot may be used. Do not use aliquots less than
0.5 g. If the sample is contaminated with analytes such that a purgeamount less than 0.5 g is appropriate, use the high level method describedin section 11.5.

11.8.3.

Add 5 mL of organic free water, and add matrix spike solutions (ifrequired), directly to the sample from section 11.8.2.

11.8.4.

The above steps should be performed rapidly and without interruption to
avoid loss of volatile organics.

11.8.5.

Analyze as described in Section 11.7.

Initial review and corrective actions
11.9.1.

Any samples that do not meet the internal standard criteria for thecalibration verification must be evaluated for validity. Note: The sample
internal standard recovery is referenced against the calibration
verification, not the initial calibration; see sections 10.6.6 and 10.6.7. If
the change in sensitivity is a matrix effect confined to an individual
sample reanalysis is not necessary. The sample in question must be
bracketed by acceptable runs. If the change in sensitivity is due to
instrument problems, all affected samples must be reanalyzed after the
problem is corrected.

11.9.2.

The surrogate standard recoveries are evaluated to ensure that they arewithin limits. Corrective action for surrogates out of control will normallybe to reanalyze the affected samples. However, if the surrogate standard
response is out high and there are no target analytes or tentatively
identified compounds, reanalysis is not necessary. Out of control surrogate
standard response may be a matrix effect; obvious matrix effects (i.e., highlevel interfering peaks) that affect the surrogate quantitation do not need
to be reanalyzed. It is only necessary to reanalyze a sample once todemonstrate matrix effect, but reanalysis at a dilution should beconsidered.

11.10. Dilutions: If the response for any compound exceeds the working range of the
GC/MS system, a dilution of the extract or sample is prepared and analyzed. An
appropriate dilution should be in the upper half of the calibration range. Samples
may be screened to determine the appropriate dilution for the initial run. If the

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initial diluted run has no hits or hits below 20% of the calibration range and thematrix allows for analysis at a lesser dilution, then the sample must be reanalyzed ata dilution targeted to bring the largest hit above 50% of the calibration range.
11.10.1. Guidance for Dilutions Due to Matrix
11.10.1.1. If the sample is initially run at a dilution and the baseline rise isless than half the height of the internal standards, or if
individual non-target peaks are less than twice the height of theinternal standards, then the sample should be reanalyzed at amore concentrated dilution. This requirement is approximate
and subject to analyst judgment.
11.10.1.2. If samples have reportable results greater than 2x the reporting
limit or ¼ the internal standard height for non-target analytes
for a methanol prep, a low level prep is not required, unlessotherwise specified by the client.
11.10.2. Reporting Dilutions: The most concentrated dilution with no target
compounds above the calibration range will be reported. Other dilutions
will only be reported at client request.
11.11. Troubleshooting Guide (Refer to the manufacturer’s manual for specific guidance)
11.11.1. Daily Instrument Maintenance: In addition to the checks listed in the
instrument maintenance schedule in TestAmerica Knoxville QAM, thefollowing daily maintenance should be performed as necessary.
11.11.1.1. Install new or cleaned injection port liner.
11.11.1.2. Install new septum.
11.11.1.3. Install new inlet seal.
11.11.1.4. Perform/adjust mass calibration (autotune/BFB tune).
11.11.1.5. Increase/decrease EM voltage to desired sensitivity based oninternal standard response.
11.11.2. Major Maintenance: A new initial calibration is necessary following major
maintenance. Major maintenance includes changing the column, repairing
the source, changing electronics, replacing the multiplier or replacing trapin the purge and trap.
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11.11.3.1. Minor maintenance includes daily instrument maintenancedescribed in 11.11.1, cleaning injector port, replacing filters,changing pump oil, autotuning, cleaning the source, replacing
source insulators, replacing or switching filaments, replacing
transfer line, change/refill IS/surrogate standard vial, changing
seals and o-rings, ballasting pump, replacing fuses, or
replacing roughing pumps.
11.11.3.2. Replace filters and change pump oil about every 6-12 months.
11.11.3.3. A multiplier gain check is performed if sensitivity is still poor
and/or analyst suspects that the multiplier is going bad.
11.11.3.4. Autotuning is performed if the analyst notices mass
misassignments or a drift in the response of analytes or internal
standards.
11.11.3.5. If minor maintenance does not result in acceptable
chromatography, it may be necessary to change the column or
clean the source.
11.12. Refer to current revision of TestAmerica Knoxville SOP-KNOX-IT-0001, “Good
Automated Laboratory Practices”, for requirements for computer hardware andsoftware.
12.

DATA ANALYSIS AND CALCULATIONS
12.1.

Refer to Appendix A for an example data review checklists used to perform anddocument the review of the data. Using the data review checklist, the analyst also
creates a narrative which includes any qualifications of the sample data.

12.2.

Qualitative identification: An analyte is identified by retention time and bycomparison of the sample mass spectrum with the mass spectrum of a standard of
the suspected compound (standard reference spectrum). Mass spectra for standard
reference may be obtained on the user's GC/MS by analysis of the calibration
standards or from the NIST Library. Two criteria must be satisfied to verify
identification: (1) elution of sample component at the same GC retention time as thestandard component; and (2) correspondence of the sample component and thestandard component characteristic ions. (Note: Care must be taken to ensure thatspectral distortion due to co-elution is evaluated.) The characteristic ions from thereference mass spectrum are defined as the three ions with greatest relative
intensity, or any ions over 30% relative intensity, if less than three such ions arepresent in the reference spectrum (i.e. characteristic ions have relative intensity>30%).

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 The sample component retention time must compare to within ± 0.2 min. of theretention time of the standard component. For reference, the standard must be
run within the same twelve hours as the sample.
 All characteristic ions must maximize in the same scan or within one scan ofeach other.
 The relative intensities of ions should agree to within ±30% between thestandard and sample spectra. (Example: For an ion with an abundance of 50%
in the standard spectra, the corresponding sample abundance must be between
20 and 80 percent.)
 Note: For SIM analysis, since not all of the ions in a compound may bemonitored, comparison of the sample mass spectrum with the mass spectrum ofa standard of the suspected compound (standard reference spectrum) cannot be
performed.
12.2.1.

12.3.

12.4.

If a compound cannot be verified by all the above criteria, but in thetechnical judgment of the analyst, the identification is correct, then theanalyst shall report that identification and proceed with quantitation.

Tentatively Identified Compounds (TICs): Library searches of peaks present in thechromatogram that are not target compounds (Tentatively Identified Compounds,
TIC) may be performed if required by the client. They are evaluated using the
TestAmerica Knoxville SOP KNOX-MS-0014, current revision, “Determination of
Tentatively Identified Compounds (TICs)”.
12.3.1.

The laboratory defaults to a TIC quality match of 85%. It is project
manager’s responsibility to relay any special TIC client requirements via
special instructions.

12.3.2.

Note: A TIC search cannot be performed when data has been acquired in
SIM mode.

Calculations.
12.4.1.

Response factor (RF):

RF 

AxCis
AisCx

Where:
Ax = Area of the characteristic ion for the compound to be measured
Ais = Area of the characteristic ion for the specific internal standard

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Cis = Concentration of the specific internal standard, ng
Cx = Concentration of the compound being measured, ng
12.4.2.

Standard deviation (SD):SD ( Xi  X ) 2

N 1
i 1
N

Xi = Value of X at i through N
N = Number of points
X = Average value of Xi
12.4.3.

Percent relative standard deviation (%RSD):% RSD 12.4.4.

S ta n d a r d D e v ia tio n
RF

 100

Calibration verification percent drift and difference from the initial
calibration (note: Chrom/TALS uses “%D” in the report header for both% difference and % drift):% Drift =Cfound - Cexpecte
 100
Cexpecte

Where
entratio indCexpecte  Known
Cfound = Measured oncentrat on using selected% Difference 

antitatio method

RF  RRF 100
RFRRF  Average Analyte Response Factor from Initial Calibration
RF = Measured Analyte Response Factor from Calibration Verification

12.4.5.

Target compound and surrogate concentrations: Concentrations in thesample may be determined from linear or second order (quadratic) curve

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fitted to the initial calibration points, or from the average response factorof the initial calibration points. Average response factor may only be used
when the RSD criteria listed in section 10.5.7 are met.
12.4.5.1.

Cpv = Concentration in purge vessel, ug/L
On-column concentration of sample as determined by the
initial calibration curve model (see 10.5.9.3).

12.4.5.2.

Calculation of Concentration for Water Samples:

Concentration, g/L =Cpv  DF  Uf  Vt
Vo  1000

Where:
Vt = Total Volume Purged (ul)Vo = Sample Volume used (ml)DF = Dilution Factor (e.g. for a one to ten dilution D=10)
Uf = Unit correction factor (default =1 [ml/ul])
12.4.5.3. Calculation of Concentration for Methanol Extracted Soils:
Concentration , g/kg =Cpv  DF  Wd  Vt
Va  Ws  X

Where:Vt= Final Methanol Extract Volume, uL

Va= Nominal Volume of extract analyzed, 100 µL

Ws = Weight of sample extracted, g
Wd = Default volume of water purged, ml (Default=5ml)
X= (100 - % moisture in sample)/100, for a dry weightbasis or 1 for a wet weight basis (moisture factor
applied by LIMS)

DF = Dilution Factor (e.g., if 10 uL of methanol extract are
analyzed, the dilution factor is 10)

12.4.5.4. Calculation of Concentration for Low Level Soils:
Concentration , g/kg =Cpv  DF  Vt
Ws  X  1000

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Where:
Vt = Low Soil Sample Purge Volume, uL
Ws = Weight of sample extracted, g
X = (100 - % moisture in sample)/100, for a dry weight basis
or 1 for a wet weight basis (moisture factor applied by
LIMS)

12.4.6. MS/MSD Recovery
Matrix Spike Recovery, % =SSR  SR 100
SA

SSR = Spike sample result
SR = Sample result
SA = Spike added

12.4.7. Relative % Difference calculation for the MS/MSD
RPD =MSR - MSDR
1 (MSR + MSDR)
2

 100

Where:RPD = Relative percent difference
MSR = Matrix spike result
MSDR = Matrix spike duplicate result
13.

METHOD PERFORMANCE

13.1. Method Detection Limit: Method Detection Limit (MDL) - An MDL must be
determined for each analyte in each routine matrix prior to the analysis of any
samples. Method Detection limits are determined and verified as specified in thecurrent revision of SOP CA-Q-S-006 based on 40 CFR Part 136 Appendix B.
13.2. Initial Demonstration: Each analyst must perform an initial demonstration ofcapability (IDOC) for each target analyte prior to performing the analysis
independently. The IDOC is determined by analyzing four replicate spikes (e.g.,
LCSs) as detailed in TestAmerica Knoxville SOP KNOX-QA-0009. This requires
analysis of QC check samples containing all of the routine analytes for the method(Table 1 and 2). The QC check sample is made at 10 ug/L (0.1 ug/L for SIM) or at
the current LCS spike level. For some tests it may be necessary to use more than
one QC check mix to cover all analytes of interest.

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13.2.1. Four aliquots of the QC check sample are analyzed using the sameprocedures used to analyze samples, including sample preparation.
13.2.2. Calculate the average recovery and standard deviation of the recovery foreach analyte of interest. The %RSD should be ≤ 15% for each analyte, andthe % recovery should be within 70-130%.
13.2.3. If any analyte does not meet the acceptance criteria, determine if historical
data indicates that the analyte purges poorly. In this case, QA approval isrequired for the IDOC to be acceptable. If the recovery or precision is
outside the 70-130% limits and the above criteria is not met, the test must
be repeated. Only those analytes that did not meet criteria in the first testneed to be evaluated. Repeated failure for any analyte indicates the needfor the laboratory to evaluate the analytical procedure and take corrective
action.
13.3. Training Qualification: The group/team leader has the responsibility to ensure that
this procedure is performed by an associate who has been properly trained in its use
and has the required experience. Refer to SOP KNOX-QA-0009 current revision
for further requirements for performing and documenting initial and on-going
demonstrations of capability.
14.

POLLUTION PREVENTION

14.1. This method does not contain any specific modifications that serve to minimize or
prevent pollution.
15.

WASTE MANAGEMENT

15.1. All waste will be disposed of in accordance with Federal, State and Local
regulations. Where reasonably feasible, technological changes have been
implemented to minimize the potential for pollution of the environment.
Employees will abide by this method and the policies in section 13 of the
TestAmerica Environmental Health and Safety Manual for “Waste Management
and Pollution Prevention.”
15.2. The following waste streams are produced when this procedure is carried out.
 Aqueous waste generated from analysis. This material may have a pH of lessthan 2. This waste will be placed in an acid satellite accumulation container.
 Solvent waste generated from analysis is placed in the flammable waste stream,
contained in a steel satellite accumulation container type or flammable solvent
container.
 VOA vials containing extracted soil samples, which will contain small amountsof methanol will be placed in the vial waste stream 55 gallon open top drum.
 Expired Standards are stored in metal closed-top containers.

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16.

REFERENCES

16.1. SW846, Test Methods for Evaluating Solid Waste, Third Edition, Gas Chromatography/Mass Spectrometry for Volatile Organics, Method 8260B, Update III,
December 1996.
16.2. SW846, Method 5030B, “Purge and Trap for Aqueous Samples”, Revision 2,
December 1996.
16.3. SW846, Method 5035, “Closed-System Purge and Trap and Extraction for Volatile
Organics in Soil and Waste Samples”, Revision 0, December 1996.
16.4. TestAmerica Knoxville Quality Assurance Manual (QAM), current revision.
16.5. CA-Q-S-002, Manual Integration, current revision.
16.6. Method 8000C “Determinative Chromatographic Separations”, March 2003.
16.7. Method 5035A “Closed-System Purge-and-Trap and Extraction for Volatile
Organics in Soil and Waste Samples”, draft revision 1, July, 2002.
17.

MISCELLANEOUS

17.1. Modifications from the reference method
17.1.1. Ion 119 is used as the quantitation ion for chlorobenzene-d5 for 25 mL
purge tests.
17.1.2. A retention time window of 0.2 minutes is used for all components, sincesome data systems do not have the capability of using the relative
retention time units specified in the reference method.
17.1.3. The quantitation and qualifier ions for some compounds have beenchanged from those recommended in SW-846 in order to improve thereliability of qualitative identification.
17.1.4. This SOP allows for the use of the NIST library in the qualitative
identification of an analyte. Method 8260B allows for the use of the mass
spectra for standard reference from the user’s instrument.
17.1.5. Section 7.3.6 of method 5035 states that methanolic extracts are stored at
4°C. Section 11.3.6 of method 5035A states that extracts must be stored at
4°C. Section 6.1 of method 5030B states that samples are stored at 4°C or
less. This SOP allows the storage of extracts to be ≤6°C.

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17.1.6.

8260B indicates that the surrogates are calibrated using a minimum of
five different concentrations. The concentration of the surrogates in thisSOP is constant throughout the initial calibration event, as noted in tables
9 & 10. The EPA has recognized an option for allowing the autosampler
to spike the initial calibration standards with surrogates in the samemanner as the samples are spiked.

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Table 1 - Standard Analytes and Reporting Limits

Water1
Low soil2
Med. Soil2
Compound
µg/L
µg/kg
µg/kg
Acetone1020
1000
Benzene1
5250
Bromochloromethane
1
5
250
Bromodichloromethane
1
5
250
Bromoform
1
5
250
Bromomethane210500
2-Butanone (syn: methyl ethyl ketone, MEK)
5
20
1000
Carbon disulfide
1
5
250
Carbon tetrachloride
1
5250
Chlorobenzene
15250
Chlorodibromomethane
15250
Chloroethane
2
10500
Chloroform
15250
Chloromethane
210500
1,2-Dibromoethane (EDB)
1
5250
Dibromomethane (syn: methylene bromide)
15250
1,1-Dichloroethane
15250
1,2-Dichloroethane
15250
1,1-Dichloroethene1
5250
cis-1,2-Dichloroethene
1
5
250
trans-1,2-Dichloroethene
15250
1,2-Dichloroethene (Total)
15250
1,2-Dichloropropane
15250
2,2-Dichloropropane
15
250
563-58-6
1,1-Dichloropropene
1
525010061-01-5
cis-1,3-Dichloropropene
1
525010061-02-6trans-1,3-Dichloropropene
15250
Ethylbenzene
100-41-4
1
5
250
2-Hexanone
591-78-6
5
20
1000
Methylene chloride
75-09-2
2
5
250
4-Methyl-2-pentanone (syn: methyl isobutyl ketone, MIBK)
108-10-1
520
1000
Styrene100-42-51
5250
1,1,1,2-Tetrachloroethane630-20-61
5250
1,1,2,2-Tetrachloroethane
79-34-51
5250
Tetrachloroethene127-18-4
1
5
250
Toluene108-88-3
1
5250
1,1,1-Trichloroethane
71-55-61
5250
1,1,2-Trichloroethane79-00-51
5250
Trichloroethene79-01-61
5250
Vinyl chloride
75-01-4210500o-xylene
95-47-615250m-Xylene and p-Xylene
136777-61-2
2
10500
Xylenes (total)
1330-20-7
3
15
750
1
Levels for 5 mL purge water samples are 5 times higher. This is achieved by analyzing 5 mL sample in a 25 mL final
volume.
2
Reporting limits listed for soil/sediment are based on wet weight. The reporting limits calculated by the laboratory forsoil/sediment, calculated on dry weight basis, will be higher.
CAS
Number67-64-1
71-43-2
74-97-5
75-27-4
75-25-2
74-83-9
78-93-3
75-15-0
56-23-5
108-90-7
124-48-1
75-00-3
67-66-3
74-87-3
106-93-4
74-95-3
75-34-3
107-06-2
75-35-4
156-59-2
156-60-5
540-59-0
78-87-5594-20-7

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Table 1A – Reporting limit for SIM analytes
Compound
Chlorobenzene
Tetrachloroethene

CAS
Number
75-05-8
107-13-1

Table 2 - Additional Analytes and Reporting Limits
CompoundAcetonitrile
Acrylonitrile
Bromobenzene
1,3-Butadienen-Butylbenzene
Sec-Butylbenzene
tert-Butylbenzene
2-Chloropropane
2-Chlorotoluene
4-Chlorotoluene
1,2-Dibromo-3-chloropropane
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
cis-1,4-dichloro-2-butene
trans-1,4-dichloro-2-butene
1,4-dichloro-2-butene (Total)
Dichlorodifluoromethane
1,3-Dichloropropane
Hexachlorobutadiene
HexaneIodomethane (syn: methyl iodide)Isopropylbenzene (syn: Cumene)
Isopropyltoluene (syn: p-Cymene)
Methyl tert-butyl ether (MTBE)
Methyl methacrylate
Napthalenen-Propylbenzene
Tetrahydrofuran
1,2,3-Trichlorobenzene
1,2,4-Trichlorobenzene
Trichlorofluoromethane
1,2,3-Trichloropropane
1,1,2-Trichloro-1,2,2-trifluoroethane (Freon 113)
1,2,4-Trimethylbenzene
1,3,5-Trimethylbenzene
Vinyl acetate
Vinyl bromide
Methyl Acetate
Cyclohexane
Methyl Cyclohexane

CAS
Number
75-05-8
107-13-1
108-86-1
106-99-0
104-51-8
135-98-8
98-06-6
75-29-6
95-49-8
106-43-4
96-12-8
95-50-1
541-73-1
106-46-7
1476-11-5
110-57-6
164-41-0
75-71-8
142-28-9
87-68-3
110-54-3
74-88-4
98-82-8
99-87-6
1634-04-4
80-62-6
91-20-3
103-65-1
109-99-9
87-61-6
120-82-1
75-69-4
96-18-4
76-13-1
95-63-6
108-67-8
108-05-4
593-60-2
79-20-9
110-82-7
108-87-2

Water1 µg/L
0.01
0.01

Water1
µg/L
20
20
1
1
1
1
1
1
1
1
2
1
1
1
2
2
4
2
1
2
2
2
1
1
1
1
1
1
4
1
1
2
1
2
1
1
2
2
1
1
1

Low soil2
µg/kg
100
100
5
5
5
5
5
5
5
5
10
5
5
5
10
10
20
10
5
10
10
10
5
5
5
5
5
5
20
5
5
10
5
10
5
5
10
10
5
5
5

Med. Soil2
µg/kg
5000
5000
250
250
250
250
250
250
250
250
500
250
250
250
500
500
1000
500
250
500
500
500
250
250
250
250
250
250
1000
250
250
500
250
500
250
250
500
500
250
250
250

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2-Propanol3
67-63-050
Levels for 5 mL purge water samples are 5 times higher. This is achieved by analyzing 5 mL sample in a 25 mL final
volume.
2
Reporting limits listed for soil/sediment are based on wet weight. The reporting limits calculated by the laboratory forsoil/sediment, calculated on dry weight basis, will be higher.
3
Analyte exhibits poor precision and accuracy, not used as a control analyte in the LCS
1Table 3 - Internal Standards
Amount added to sample being purged, ng
Quantitation ion
Fluorobenzene
250
96
Chlorobenzene-d5
250
117 (119)
1,4-Dichlorobenzene-d4
250152
Notes:
1) This results in a concentration of each internal standard in the sample of 50µg/L for a 5 mL purge or
10 µg/L for a 25 mL purge or 50 ug/kg for a 5 gram soil purge.
2) This is achieved by spiking 5 uL of a 50 ug/mL standard manually, or if an autosampler loop isused, the concentration of the solution is adjusted to the volume of the spiking loop.
3) Mass 119 is used for Chlorobenzene-d5 for 25ml analyses4) Except for high level soils, the surrogate and internal standards may be combined in one solution.

Table 3A - Internal Standards (SIM)Amount added to sample being purged, ng
Quantitation ion
Secondary ion
Chlorobenzene-d5
2.5
117
82
1,4-Dichlorobenzene-d4
2.5
152
150
Note: This results in a concentration of each internal standard in the sample of 0.1 µg/L for a 25 mL purge

Table 4 - Surrogate Standards
Surrogate Compounds
Amount added to sample being purged, ng
1,2-Dichloroethane-d4
150
Dibromofluoromethane
150
Toluene-d8
150
4-Bromofluorobenzene
150
Notes:
1) This results in a concentration of each surrogate in the sample of 6 µg/L for a 25 mL purge or 30
ug/kg for a 5 gram soil purge.
2) This is achieved by spiking 5 uL of a 30 ug/mL standard manually, or if an autosampler loop is used, theconcentration of the solution is adjusted to the volume of the spiking loop.
3) Except for high level soils and waste, the surrogate and internal standards may be combined in one solution.
4) Recovery limits for surrogates are generated from historical data and are maintained by the QA department.

Table 4A - Surrogate Standards (SIM)Surrogate Compounds
Amount added to sample being purged, ng
Toluene-d8
2.5
4-Bromofluorobenzene
2.5
Note: This results in a concentration of each surrogate in the sample of 0.1 µg/L for a 25 mL purge

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 45 of 59

Table 5 - BFB Key Ion Abundance Criteria (not required for SIM)
Mass
50
75
95
96
173
174
175
176
177

Ion Abundance Criteria
15% to 40% of Mass 95
30% to 60% of Mass 95
Base Peak, 100% Relative Abundance
5% to 9% of Mass 95
Less Than 2% of Mass 174
Greater Than 50% - 120% of Mass 95
5% to 9% of Mass 174
Greater Than 95%, But Less Than 101% of Mass 174
5% to 9% of Mass 176

Table 6 - SPCC Compounds and Minimum Response Factors
Compound
Chloromethane
1,1-Dichloroethane
Bromoform
1,1,2,2-Tetrachloroethane
Chlorobenzene

8260B Min. RF
0.100
0.100
0.100
0.300
0.300

Table 7 - CCC compounds
CompoundVinyl Chloride
1,1-Dichloroethene
Chloroform
1,2-Dichloropropane
TolueneEthylbenzene

Max. %RSD from Initial
Calibration
≤30
≤30
≤30
≤30
≤30
≤30

Max. %D for Calibration
Verification
≤20
≤20
≤20
≤20
≤20
≤20

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 46 of 59

Table 8 - Quantitation Reference and Quantitation Ions***
CompoundDichlorodifluoromethane
Chloromethane
Vinyl chloride
1,3-Butadiene
Bromomethane
Chloroethane
Vinyl bromide
Trichlorofluoromethane
2-Chloropropane
1,1-Dichloroethene
1,1,2-Trichloro-1,2,2-trifluoroethane (Freon 113)
Iodomethane
Carbon disulfide
AcetoneAcetonitrile
Methylene chloride
Acrylonitriletrans-1,2-Dichloroethene
Methyl tert butyl ether
Hexane1,1-Dichloroethane
Vinyl acetate
cis-1,2-Dichloroethene
2,2-Dichloropropane
2-Butanone
Tetrahydrofuran
Bromochloromethane
Chloroform
1,1,1-Trichloroethane
Carbon tetrachloride
1,1-Dichloropropene
1,2-Dichloroethane
BenzeneTrichloroethene
1,2-Dichloropropane
Dibromomethane
Methyl methacrylate
Bromodichloromethanecis-1,3-Dichloropropene
4-Methyl-2-pentanone
Toluenetrans-1,3-Dichloropropene
1,1,2-Trichloroethane
Tetrachloroethene
1,3-Dichloropropane
2-Hexanone
Chlorodibromomethane

IS Group
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1 (2 for soil)
2
2
2
2
2
2
2

Primary*
85
50
62
39
94
64
106
101
43
96
151
142
76
43
41
84
53
96
73
57
63
86
96
77
43
42
128
83
97
117
75
62
78
130
63
93
41
83
75
43
91
75
97
164 (166SIM)
76
43
129

Secondary
87
52
64

Tertiary
50
49
61

96
66

49

103

66

61
101
127
78
58
40
49
52
61

98
153
141

43
65
43
61
97
72**

39
51
51
98

83
98

130
85
99
119
77
64
52
95
65
174
69
85
77
58
92
77
83

49
47
117
121
110
98
77
97
41
95
100
129
39
57
65
39
85

166
78
58
127

131
57

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 47 of 59

Table 8 - Quantitation Reference and Quantitation Ions (continued)
CompoundIS Group
Primary*
Secondary
Tertiary
1,2-Dibromoethane
2
107
109
188
Chlorobenzene
2
112
114
77
1,1,1,2-Tetrachloroethane
2
131
133
119
Ethylbenzene
210691m-Xylene and p-Xylen
210691
o-Xylene
2
106
91
Styrene
2
104
103
78
Bromoform
2
173
171
175
Isopropylbenzene
2
105
120
Cis-1,4-Dichloro-2-butene
2
53
88/89
1,1,2,2-Tetrachloroethane
2
83
85
131
Bromobenzene
2
156
158
77
1,2,3-Trichloropropane
3
110
75
Trans-1,4-Dichloro-2-butene
3
53
88/89
n-Propylbenzene
391120
2-Chlorotoluene
391
126
1,3,5-Trimethylbenzene
3
105
120
4-Chlorotoluene
3
91
126
tert-Butylbenzene
3
119
91
134
1,2,4-Trimethylbenzene
3
105
120
sec-Butylbenzene
3
105
134
1,3-Dichlorobenzene
3
146
148
111
p-isopropyltoluene
3
119
134
91
1,4-Dichlorobenzene
3
146
148
111
n- Butylbenzene
3
91
92
134
1,2-Dichlorobenzene
3
146
148
111
1,2-Dibromo-3-chloropropane
3
157
155
75
1,2,4-Trichlorobenzene
3
180
182
145
Hexachlorobutadiene
3
225
223
227
Naphthalene
3
128
129
127
1,2,3-Trichlorobenzene
3
180
182
145
Methyl Acetate
1
43
74
59
Cyclohexane
1
56
84
41
Methyl Cyclohexane
1
83
55
98
1,2-Dichloroethane-d4 (Surrogate)
1
65
102
Dibromofluoromethane (Surrogate)
1
113
111
Toluene-d8 (Surrogate)
2
98
70
100
4-Bromofluorobenzene (Surrogate)
3
95
174
176
* The primary ion should be used for quantitation unless interferences are present, in which case a secondary ion
may be used.
** m/z 43 may be used for quantitation of 2-Butanone, but m/z 72 must be present for positive identification.
***The Chrom software designates the nature of the ions as “Quant”, “Qual” or “Monitor”.
 Quant- i.e., quantitate; designates that ion for quantitation of the target analyte Qual – i.e., qualify; designates that ion that must be present in order to identify (or integrate) that analyte.
 Monitor- designates that ion as a monitor for additional qualitative analysis. The Chrom software does not
use this mode to determine if a peak will be integrated.
Primary ions listed in this SOP shall be used in the “Quant” mode unless there are interferences present. In that case, asecondary ion is used. Secondary and tertiary ions can be designated as either “Qual” or “Monitor” mode.

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 48 of 59

Table 9 - Typical Water Calibration Levels (ug/L) - 25ml Purge
CompoundDichlorodifluoromethane
Chloromethane
Vinyl chloride
1,3-Butadiene
Bromomethane
Chloroethane
Vinyl bromide
Trichlorofluoromethane
2-Chloropropane
1,1-Dichloroethene
1,1,2-Trichloro-1,2,2-trifluoroethane (Freon 113)
Iodomethane
Carbon disulfide
AcetoneAcetonitrile
Methylene chloride
Acrylonitriletrans-1,2-Dichloroethene
Methyl tert butyl ether
Hexane1,1-Dichloroethane
Vinyl acetate
cis-1,2-Dichloroethene
2,2-Dichloropropane
2-Butanone
Bromochloromethane
Tetrahydrofuran
Chloroform
1,1,1-Trichloroethane
Carbon tetrachloride
1,1-Dichloropropene
1,2-Dichloroethane
BenzeneTrichloroethene
1,2-Dichloropropane
Dibromomethane
Methyl methacrylate
Bromodichloromethanecis-1,3-Dichloropropene
4-Methyl-2-pentanone
Toluenetrans-1,3-Dichloropropene
1,1,2-Trichloroethane
Tetrachloroethene
1,3-Dichloropropane
2-Hexanone
Chlorodibromomethane
1,2-Dibromoethane

Level 1
1
1
1
1
1
1
1
1
1
1
1
1
1
4
10
1
10
1
1
1
1
2
1
1
4
1
2
1
1
1
1
1
1
1
1
1
1
1
1
4
1
1
1
1
1
4
1
1

Level 2
2
2
2
2
2
2
2
2
2
2
2
2
2
8
20
2
20
2
2
2
2
4
2
2
8
2
4
2
2
2
2
2
2
2
2
2
2
2
2
8
2
2
2
2
2
8
2
2

Level 3
10
10
10
10
10
10
10
10
10
10
10
10
10
40
100
10
100
10
10
10
10
20
10
10
40
10
20
10
10
10
10
10
10
10
10
10
10
10
10
40
10
10
10
10
10
40
10
10

Level 4
20
20
20
20
20
20
20
20
20
20
20
20
20
80
200
20
200
20
20
20
20
40
20
20
80
20
40
20
20
20
20
20
20
20
20
20
20
20
20
80
20
20
20
20
20
80
20
20

Level 5
40
40
40
40
40
40
40
40
40
40
40
40
40
160
400
40
400
40
40
40
40
80
40
40
160
40
80
40
40
40
40
40
40
40
40
40
40
40
40
160
40
40
40
40
40
160
40
40

Level 6
80
80
80
80
80
80
80
80
80
80
80
80
80
320
800
80
800
80
80
80
80
160
80
80
320
80
160
80
80
80
80
80
80
80
80
80
80
80
80
320
80
80
80
80
80
320
80
80

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 49 of 59

Table 9 - Typical Water Calibration Levels (ug/L) - 25ml Purge (continued)
CompoundMethyl Acetate
Cyclohexane
Methyl Cyclohexane
Chlorobenzene
1,1,1,2-Tetrachloroethane
Ethylbenzene
m-Xylene and p-Xylene
o-Xylene
StyreneBromoform
Isopropylbenzene
cis-1,4-Dichloro-2-butene
1,1,2,2-Tetrachloroethane
Bromobenzene
1,2,3-Trichloropropane
trans-1,4-Dichloro-2-butene
n-Propylbenzene
2-Chlorotoluene
1,3,5-Trimethylbenzene
4-Chlorotoluene
tert-Butylbenzene
1,2,4-Trimethylbenzene
sec-Butylbenzene
1,3-Dichlorobenzene
p-isopropyltoluene
1,4-Dichlorobenzene
n- Butylbenzene
1,2-Dichlorobenzene
1,2-Dibromo-3-chloropropane
1,2,4-Trichlorobenzene
Hexachlorobutadiene
Naphthalene
1,2,3-Trichlorobenzene
1,2-Dichloroethane-d4 (Surrogate)
Dibromofluoromethane (Surrogate)
Toluene-d8 (Surrogate)
4-Bromofluorobenzene (Surrogate)

Level 1
5
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
6
6
6
6

Level 2
10
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
6
6
6
6

Level 3
50
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
6
6
6
6

Level 4
100
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
6
6
6
6

Level 5
200
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
6
6
6
6

Level 6
400
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
80
6
6
6
6

Table 9A - Typical Water Calibration Levels (ug/L) - 25ml Purge (SIM)CompoundTetrachloroethene
Chlorobenzene
Toluene-d8 (Surrogate)
4-Bromofluorobenzene (Surrogate)

Level 1
0.004
0.004
0.1
0.1

Level 2
0.01
0.01
0.1
0.1

Level 3
0.025
0.025
0.1
0.1

Level 4
0.1
0.1
0.1
0.1

Level 5
0.5
0.5
0.1
0.1

Level 6
1.0
1.0
0.1
0.1

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 50 of 59

Table 10 - Typical Soil Calibration Levels (ug/kg) – Low Level
CompoundDichlorodifluoromethane
Chloromethane
Vinyl chloride
1,3-Butadiene
Bromomethane
Chloroethane
Vinyl bromide
Trichlorofluoromethane
2-Chloropropane
1,1-Dichloroethene
1,1,2-Trichloro-1,2,2-trifluoroethane (Freon 113)
Iodomethane
Carbon disulfide
AcetoneAcetonitrile
Methylene chloride
Acrylonitriletrans-1,2-Dichloroethene
Methyl tert butyl ether
Hexane1,1-Dichloroethane
Vinyl acetate
cis-1,2-Dichloroethene
2,2-Dichloropropane
2-Butanone
Bromochloromethane
Tetrahydrofuran
Chloroform
1,1,1-Trichloroethane
Carbon tetrachloride
1,1-Dichloropropene
1,2-Dichloroethane
BenzeneTrichloroethene
1,2-Dichloropropane
Dibromomethane
Methyl methacrylate
Bromodichloromethanecis-1,3-Dichloropropene
4-Methyl-2-pentanone
Toluenetrans-1,3-Dichloropropene
1,1,2-Trichloroethane
Tetrachloroethene
1,3-Dichloropropane
2-Hexanone
Chlorodibromomethane
1,2-Dibromoethane
Chlorobenzene

Level 1
5
5
5
5
5
5
5
5
5
5
5
5
5
20
50
5
50
5
5
5
5
10
5
5
20
5
10
5
5
5
5
5
5
5
5
5
5
5
5
20
5
5
5
5
5
20
5
5
5

Level 2
10
10
10
10
10
10
10
10
10
10
10
10
10
40
100
10
100
10
10
10
10
20
10
10
40
10
20
10
10
10
10
10
10
10
10
10
10
10
10
40
10
10
10
10
10
40
10
10
10

Level 3
50
50
50
50
50
50
50
50
50
50
50
50
50
200
500
50
500
50
50
50
50
100
50
50
200
50
100
50
50
50
50
50
50
50
50
50
50
50
50
200
50
50
50
50
50
200
50
50
50

Level 4
100
100
100
100
100
100
100
100
100
100
100
100
100
400
1000
100
1000
100
100
100
100
200
100
100
400
100
200
100
100
100
100
100
100
100
100
100
100
100
100
400
100
100
100
100
100
400
100
100
100

Level 5
250
250
250
250
250
250
250
250
250
250
250
250
250
1000
2500
250
2500
250
250
250
250
500
250
250
1000
250
500
250
250
250
250
250
250
250
250
250
250
250
250
1000
250
250
250
250
250
1000
250
250
250

Level 6
400
400
400
400
400
400
400
400
400
400
400
400
400
1600
4000
400
4000
400
400
400
400
800
400
400
1600
400
800
400
400
400
400
400
400
400
400
400
400
400
400
1600
400
400
400
400
400
1600
400
400
400

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/2018
Page: 51 of 59

Table 10 - Typical Soil Calibration Levels (ug/kg) – Low Level (continued)
Compound
1,1,1,2-Tetrachloroethane
Ethylbenzene
m-Xylene and p-Xylene
o-Xylene
StyreneBromoform
Isopropylbenzene
cis-1,4-Dichloro-2-butene
1,1,2,2-Tetrachloroethane
Bromobenzene
1,2,3-Trichloropropane
trans-1,4-Dichloro-2-butene
n-Propylbenzene
2-Chlorotoluene
1,3,5-Trimethylbenzene
4-Chlorotoluene
tert-Butylbenzene
1,2,4-Trimethylbenzene
sec-Butylbenzene
1,3-Dichlorobenzene
p-isopropyltoluene
1,4-Dichlorobenzene
n- Butylbenzene
1,2-Dichlorobenzene
1,2-Dibromo-3-chloropropane
1,2,4-Trichlorobenzene
Hexachlorobutadiene
Naphthalene
1,2,3-Trichlorobenzene
1,2-Dichloroethane-d4 (Surrogate)
Dibromofluoromethane (Surrogate)
Toluene-d8 (Surrogate)
4-Bromofluorobenzene (Surrogate)

Level 1
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
30
30
30
30

Level 2
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
30
30
30
30

Level 3
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
30
30
30
30

Level 4
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
30
30
30
30

Level 5
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
30
30
30
30

Level 6
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
30
30
30
30

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:52 of 59

Appendix A: Example Data Review Checklist

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:53 of 59

Appendix A: Example Data Review Checklist, continued

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:54 of 59

Appendix A: Example Data Review Checklist, continued

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:55 of 59

Appendix A: Example Data Review Checklist, continued

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:56 of 59

Appendix A: Example Data Review Checklist, continued

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:57 of 59

FIGURE 1 – Example GC and GC/MS Conditions for SIM.

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:58 of 59

FIGURE 1 – Example GC and GC/MS Conditions for SIM. (Continued)

SOP No. KNOX-MS-0015
Revision No. 18
Revision Date: 01/29/18
Page:59 of 59

FIGURE 1 – Example GC and GC/MS Conditions for SIM. (Continued)