STANDARD OPERATING PROCEDURES

SOP: 1701
PAGE: 1 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

CONTENTS

1.0 SCOPE AND APPLICATION*

2.0 METHOD SUMMARY

3.0 SAMPLE PRESERVATION, CONTAINERS, HANDLING AND STORAGE

3.1 Sample Storage

3.2 Holding Times

4.0 INTERFERENCES AND POTENTIAL PROBLEMS

5.0 EQUIPMENT/APPARATUS

6.0 REAGENTS

7.0 PROCEDURES

7.1 GC/MS Operating Conditions

7.2 Standard/Sample Injection
7.3 GC/MS Tuning
7.4 Initial Calibration
7.5 Continuing Calibration
7.6 Method (Instrument) and System Blanks
7.7 Tedlar Bag Analysis

8.0 CALCULATIONS

9.0 QUALITY ASSURANCE/QUALITY CONTROL

9.1 GC/MS Tuning and Performance Criteria

9.2 Initial Calibration
9.3 Continuing Calibration
9.4 Blanks
9.5 Dilution Analysis
9.6 Replicate Analysis
9.7 Internal Standard Evaluation
9.8 Target Compound Identification
9.9 Tentatively Identified Compounds
9.10 Quantitation Limit
9.11 Manual Integrations
9.12 Initial Demonstration of Capability
9.13 Work Assignment Field Change Form*
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 2 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

CONTENTS (cont)

10.0 DATA VALIDATION*

11.0 HEALTH AND SAFETY

12.0 REFERENCES

13.0 APPENDICES

A - Tables
B - Figures

* These sections affected by Revision 1.1

SUPERCEDES: SOP #1701; Revision 1.0; 11/7/05; US EPA Contract EP-W-09-031.

 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 3 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

1.0 SCOPE AND APPLICATION

The purpose of this standard operating procedure (SOP) is to describe the field Gas Chromatography/Mass
Spectrometry (GC/MS) analysis of air samples collected in Tedlar bags. This procedure generates field screening
data in parts per billion by volume (ppbv) and is based on Environmental Protection Agency (EPA) Compendium
Method TO-15. The data generated using this SOP meets the Screening Data objective for a quick, preliminary
assessment of site contamination, and provides analyte identification and quantification. Screening data without
associated confirmation data are generally not considered to be data of known quality. The field screening data may
be definitively confirmed by the analysis of additional samples collected in SUMMA canisters and sent to a
laboratory to be analyzed using methods and quality control (QC) criteria associated with definitive data. A list of
the volatile organic compounds (VOCs) that may be analyzed by this method is presented in Table 1, Appendix A.

2.0 METHOD SUMMARY

Ambient air is drawn by vacuum into a Tedlar bag. An aliquot of sample is withdrawn from the bag using a glass
syringe and subsequently injected into a modified purge & trap (P/T) concentrator. The VOCs are thermally
desorbed from the trap, separated by GC and analyzed by positive ion electron impact MS.

3.0 SAMPLE PRESERVATION, CONTAINERS, HANDLING, AND STORAGE

3.1 Sample Storage

Samples collected in Tedlar bags should be placed in a clean and cool environment (at room temperature)
out of direct sunlight to prevent photo degradation. The bag samples should arrive at the mobile
laboratory with the valve closed and an identification tag attached.

3.2 Holding Times

For best results, samples should be analyzed within the first 12 hours of collection. Samples must be
analyzed within 24 to 48 hours after collection.

Samples may be recorded on a chain of custody (COC) record (optional for screening locations) indicating
sampling locations, sample numbers, date collected, sample matrix, and sample volumes. The COC record should
agree with the information on the Tedlar bag labels and discrepancies should be noted on the COC record or
injection logbook at the time of receipt by the mobile laboratory. In addition, any obvious physical damage or
contamination (e.g., broken valves, condensate in the bag, or bags being flat) should also be recorded on the COC
record or in the injection logbook.

4.0 INTERFERENCES AND POTENTIAL PROBLEMS

Structural isomers having co-eluting retention times and identical mass spectra will interfere with this method.
The most common interference seen in these methods is between meta-xylene and para-xylene.
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 4 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

Artifacts in Tedlar bags may result from improper cleaning procedures by the vendor, long term storage of
clean Tedlar bags, sampling or sample storage.

Organic compounds in the carrier gas, the GC/MS system, the sample preparation system or solvent vapors in
the laboratory may contribute to contamination problems.

5.0 EQUIPMENT/APPARATUS

Hewlett-Packard (HP) 6890 GC/5973 mass selective detector (MSD), equipped with Chem Station software,
or equivalent

Sample Concentrator, capable of ambient to approximately 350 degrees Centigrade ( C) temperature range,
equipped with a GC interface (OI Analytical P/T concentrator or equivalent)

Restek Rtx-Volatile capillary column, 20 meter (m) long x 0.18 millimeter (mm)inner diameter (ID), 2.0
micron (um) film thickness, or equivalent

Tedlar Bags , 1-liter (L), equipped with both sampling and injection valves (SKC, Inc. or equivalent).

Glass Syringe, Micro-Mate hypodermic with Luer lock, 5, 10, 30, 50, 250, and 1000 milliliter (mL) (Popper
& Son, Inc., or equivalent)

Syringe Needles, various gauges with Luer lock tip (Benton -Dickson Inc., or equivalent)

Syringe Sampling Valves, On-off Teflon two-way valves (Supelco, Inc., or equivalent).

6.0 REAGENTS

Calibration standard, approximately 1.0 part per million by volume (ppmv) in nitrogen (Scott Specialty Gases,
Inc., or equivalent)

p-Bromofluorobenzene (BFB), approximately 1.0 ppmv in nitrogen (Scott Specialty Gases, Inc., or
equivalent), used as the mass spectrometer performance standard

Internal Standards, consisting of bromochloromethane (BCM), 1,4-difluorobenzene, and chlorobenzene-

d5,each at approximately 1.0 ppmv in nitrogen ( Scott Specialty Gases, Inc., or equivalent)

Perfluorotributylamine (PFTBA), for tuning the MS (Hewlett Packard, Inc., or equivalent)

Helium, ultra high purity 99.999 - 99.9999 percent (%), used as the carrier and purge gas in the P/T GC/MS
unit

Nitrogen, ultra high purity 99.999% - 99.9999%, used for the preparation of blanks, dilution, and purging of
Tedlar bags
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 5 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

7.0 PROCEDURES

7.1 GC/MS Operating Conditions

Example GC/MS operating conditions are as follows:

Initial Temperature : 33 C
Initial Time : 3.0 minutes
Ramp Rate : 10.0 C/minute
Final Temperature : 240 C
Final Time : 0.5 minutes
Scan Rate : 3.26 sec-1
Mass Scan Range : 35 to 260 atomic mass unit (amu)

Operating conditions for the concentrator and trap should be set according to the manufacturer’s
instructions. Example operating conditions for the concentrator are as follows:

Pre-Heat Temperature: 45 C
Pre-Heat time: 1 minute
Trap Purge Temperature 25 C
Purge Time: 10 minutes or as needed
Dry Purge Time: 1 minute
Desorb Temperature: 190 C
Desorb Time: 4 minutes
Bake Temperature: 200 C
Bake Time: 8 minutes
Transfer Line Temperature: 160 C

These parameters are subject to change based on chromatographic and analytical objectives.

7.2 Standard/Sample Injection

Introduce all standards and samples into the GC/MS system via a modified OI Analytical P/T
concentrator. The standard or sample is first pre-concentrated in an adsorbent trap in the P/T unit. After
the dry purge removes oxygen, the trap is thermally desorbed using helium so that all VOCs are swept
onto the head of the GC column where VOCs are separated by temperature programming of the GC oven.
In operation, a glass syringe is inserted into the hold-tip connected to a two-way valve assembly attached
to the concentrator. When the vacuum pump is turned on and the two-way valve assembly is opened
(Figure 1, Appendix B), the air in the syringe is drawn to the trap. After the injection, the pump is turned
off and the two-way valve is closed. When the concentrator steps to desorb, the unit automatically starts
GC/MS data acquisition.

7.3 GC/MS Tuning

 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 6 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

At the beginning of each day, the GC/MS system should be tuned, either automatically or manually,
using PFTBA to set the proper mass calibration, mass resolution and ion abundance ratios. After
PFTBA tuning is successfully completed, analyze 50 nanograms (ng) (7 mL) of BFB to check the
analytical system performance and confirm that the ion abundance ratios for BFB meet the
requirements listed in Table 2, Appendix A.

Acquire the mass spectrum of BFB meeting the criteria in the following manner. Three scans (the
peak apex and the scans immediately preceding and following the apex) are acquired and averaged.
Background subtraction is conducted using a single scan prior to the elution of BFB.

7.4 Initial Calibration

Before any sample or blank analyses, calibrate the GC/MS system using target analytes and internal
standards contained in pressurized cylinders or canisters at a nominal 1.0 ppmv concentration in nitrogen.

A multipoint calibration, typically a 5-point calibration, should be established before sample

injection. The initial calibration may include standards at 1, 5, 25, 50, and 100 nanoliter (nL). These
concentrations result from injections of 1, 5, 25, 50, and 100 mL of the 1.0 ppmv calibration
standard. One of the calibration standards should be near the quantitation limit (QL) for the
compound(s) of interest. A minimum of three calibration standards must be used to generate a
calibration curve.

Internal standards are added by typically spiking with 10 mL (equivalent to 10 nL) of the nominal
1.0 ppmv internal standard mixture.

Quantitation ions for target analytes are shown in Table 1, Appendix A. The primary ion should be
used for quantitation unless interferences are present, in which case a secondary ion is used.

Data generated by use of an average response factor (RFaverage) or a linear regression forced through
zero are acceptable. The preferred approach is to first create a calibration using the response factor
(RF). Refer to Table 3, Appendix A. The initial calibration is acceptable when the calculated
percent relative standard deviation (%RSD) for each analyte is less than or equal to ( ) 30.0% with
at most two exceptions with a limit up to 40.0%. RFaverage is then used for calculating sample
concentrations.

Linear regression forced through zero (Table 4, Appendix A) may be used if the criteria for the
RFaverage are not met. An acceptable correlation coefficient of 0.95 must be met for all target
analytes.

 For each compound in the calibration, the retention time and relative abundance of selected ions are
stored on the hard disk of the GC/MS computer to be used for compound identification.

 If the initial calibration acceptance criteria are not met, inspect the system for problems. It may be
necessary to clean the ion source, change the column, or take other corrective actions.
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 7 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

7.5 Continuing Calibration

For each day of analysis and after BFB criteria have been met, analyze a continuing calibration
standard at the mid-point concentration to check that the initial calibration remains under control.
For each target analyte, calculate the RF using the equation from Table 3, Appendix A. Compare
this daily RF with the RFaverage from the initial calibration.

Calculate the percent difference (%D) using the equation listed in Table 3, Appendix A. The
continuing calibration is acceptable if the %D for all response factors (RFs) are within ± 30%.
When using linear regression, compare the calculated concentration of the mid-level standard to the
known concentration. Calculate a %D for each target analyte. The continuing calibration is
acceptable if the %D for all response factors (RFs) are within ± 30%.

If acceptance criteria are not met, re-analyze the continuing calibration check sample. If acceptance
criteria are not met for the second check sample, the initial calibration must be re-analyzed.

7.6 Method (Instrument) and System Blanks

Method (Instrument) blanks are analyzed after the initial calibration standards and the continuing
calibration standard and prior to any sample analyses to assess possible laboratory contamination.

Measure 10 mL of the internal standards in a glass syringe and trap onto the concentrator. Proceed
with analysis.

System blanks may also be necessary after analyzing samples with high levels of VOC target analytes
and/or non-target VOCs to ensure no carryover.

7.7 Tedlar Bag Analysis

Lot (Tedlar bag) are analyzed after the Method (Instrument) blank and prior to any sample analyses to
assess possible contaminants from the Tedlar bag.

 Prior to use each Tedlar bag is purged three times with ultra-pure nitrogen. Using a nitrogen purged
Tedlar bag, fill with nitrogen and hold for at least one-hour before analyzing.

 Using a Luer-Lock fitted adaptor, directly vent the nitrogen blank from the Tedlar bag to a glass
syringe. The volume used for the Lot blank can range from 250 mL to 1000 mL. Allow the syringe
to fill with a volume slightly greater than the amount to be used for analysis. Adjust to the exact
sample volume required, allow the pressure to equilibrate, and close the valve at the syringe end.

 Place syringe in the Luer-Lock tip valve in the front of the concentrator and start pump to place onto
the sorbent trap. Fill a glass syringe with 10 mL of the internal standard and place onto the sorbent
trap. Proceed with analysis.
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 8 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

8.0 CALCULATIONS

Calculate the concentrations of target compounds in the air samples using the GC/MS computer software. The
target compound calculation is presented in Table 5, Appendix A. All target analyte concentrations are reported to
two significant figures.

9.0 QUALITY ASSURANCE/QUALITY CONTROL

The following quality assurance/quality control (QA/QC) protocols apply to this procedure. The QA/QC
requirements in this section may be waived by the Work Assignment Manager (WAM) or their designee depending
on the data quality objectives of the project. All waivers must be documented in field logbooks or on a Work
Assignment Field Change Form.

9.1 GC/MS Tuning and Performance Criteria

BFB must be analyzed each day of operation and must meet the BFB ion abundance criteria listed in
Table 2, Appendix A.

9.2 Initial Calibration

An acceptable initial calibration must be performed using a minimum of three standards before sample
analysis begins. The initial calibration range is acceptable if the %RSD is less than or equal to 30.0% for
the RFaverage for each VOC; two compounds may have a %RSD up to 40.0%. When using linear
regression, the correlation coefficient must be 0.95. Samples are quantitated using the RFaverage of each
compound from the initial calibration or the linear regression formula.

9.3 Continuing Calibration

Once an initial calibration has been established, a continuing calibration standard must be analyzed on
each day of sample analysis. The RF of the mid-level calibration standard is compared against the
RFaverage from the current initial calibration when response factors are used for quantitation. The
calculated concentrations of the mid-level calibration standard are compared to the known concentration
when using linear regression. If the calculated %D for any VOC in the continuing calibration standard
differs by more than ±30%, the continuing calibration must be reanalyzed. If the continuing calibration
fails a second time, the initial calibration must be re-analyzed.

9.4 Blanks

The blanks should not contain any target analyte at concentrations above the limit of quantitation (lowest
standard in initial calibration) or additional compounds which may co-elute or interfere with identification
of the target analytes. If contamination is a problem, the source of the contamination must be investigated.
Appropriate corrective actions should be taken and documented.

If an analyte found in the blank is also found in the associated samples, those sample results are to be
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 9 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

flagged as possibly contaminated.

9.5 Dilution Analysis

All target analyte concentrations should be within the calibration range. Use the results of the initial
analysis to determine an appropriate dilution factor (DF). The DF should bring the target analyte
concentration within the initial calibration range.

9.6 Replicate Analysis

One sample replicate should be analyzed each day of analysis. The sample should be randomly chosen
and re-analyzed. Calculate the relative percent difference (RPD) for any concentration detected. The
RPD is given as the absolute difference of the replicate values divided by their mean, expressed as a
percentage.

9.7 Internal Standard Evaluation

Internal standards are added to all standards, blanks and samples. The area response for each internal
standard must be within ±40% of the area response of the most recent calibration standard. In addition,
the sample retention times must be within 20 seconds of the latest daily (24-hour) calibration check
standard.

Internal standard responses and retention times should be evaluated immediately after data acquisition. If
criteria are not met, inspect system for malfunctions and take corrective actions if necessary. Re-analyze
the sample.

9.8 Target Compound Identification

Two criteria must be satisfied to verify the identification of a target compound:

Retention Time - A sample target analyte retention time (RT) must be within ±0.50 minutes of the
RT of the target analyte in the calibration standard. The calibration standard must be analyzed on the
same 24 hour clock as the sample.

Spectra - (1) All ions present in the standard mass spectra at a relative intensity greater than 10%
(where the most abundant ion in the spectrum equals 100%) must be present in the sample
spectrum, and (2) The relative intensities of the ions specified above must agree within ±20%
between the sample and the reference spectra.

9.9 Tentatively Identified Compounds

A library search should be performed for tentatively identified compounds (TICs) present in method
blanks, lot blanks, and samples for the purpose of tentative identification. In this case, the National
Institute for Standards and Technology (NIST) Mass Spectral Library (or equivalent reference mass
spectra system) should be used for identification search.
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 10 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

1. Guidelines for making tentative identification of a non-target compound:

Relative intensities of major ions greater than 10% of the most abundant ion in the reference
spectrum should be present in the sample spectrum.
The relative intensities of the major ions should agree within ±20% between the standard and
sample spectra. For example, if an ion has an abundance of 50% in the standard spectra, the
corresponding sample ion abundance must be between 30-70%.

Molecular ions present in reference spectrum should be present in sample spectrum.

Ions present in the sample spectrum but not in the reference spectrum should be reviewed for
possible background contamination or the presence of co-eluting compounds.

Ions present in the reference spectrum but not in the sample spectrum should be reviewed for
possible subtraction from the sample spectrum because of background contamination or the
presence of co-eluting compounds.

The peak area for the non-target compound is greater than 10% of the peak area of the nearest
internal standard.

NOTE: Data system library reduction programs can sometimes create these discrepancies.

2. If all of the above conditions for a compound are met, that compound will be reported as a TIC. If
the mass spectral interpretation specialist indicates that no valid tentative identification can be made,
the compound should be reported as unknown. The mass spectral interpretation specialist should
give additional classification of the unknown compound, if possible. Up to 20 TICs and/or
unknowns may be reported.

3. An estimated concentration for TICs should be calculated using the internal standard method. The
nearest internal standard free of interferences should be used for quantitation; a response factor of 1.0
will be used. All non-target analyte concentrations are reported to two significant figures.

9.10 Quantitation Limit

The lowest standard used in the initial calibration will be used for the quantitation limit or an elevated
reporting limit may be used.

9.11 Manual Integrations

Manual integration of all target analytes, surrogates, and internal standards will be submitted for review.
The manual integration results will be flagged with a “M” using the instrument software and verified
during the data review process. Evidence of review will be documented on the Field Analytics Manual
Integration Review Sheet (Figure 2, Appendix B). Documentation of the manual integration of
quantitation ion peaks must be included in the data package. Refer to Scientific, Engineering, Response
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 11 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

and Analytical Services (SERAS) SERAS SOP #1001, Chromatographic Peak Integration Procedures.

9.12 Initial Demonstration of Capability

Initial proficiency in VOC analysis must be demonstrated by each analyst initially and each time
significant changes are made in the procedure or for instrumentation. Each analyst will generate
precision and accuracy data using a reference standard other than the source used for calibration. Four
replicates of a well-mixed reference standard is analyzed using the procedures outlined in this SOP.
Calculate the average mean in ppbv and the standard deviation (s) in ppbv. The Quality Assurance
Officer (QAO) will tabulate the results from all of the analysts per matrix per parameter, and calculate
control limits.

9.13 Work Assignment Field Change Form

A Work Assignment Field Change Form must be generated to initiate any on-site change in the scope of a
project. This form must document the original scope of work that is being changed, the new scope and
the signatures of the SERAS Task Leader or their designee and the Work Assignment Manager.

10.0 DATA VALIDATION

The data is reviewed using the Quality Assurance/Quality Control considerations listed in Section 9.0 by the analyst
prior to submittal to the client to ensure that the instrument has been operated in accordance with this SOP and
manufacturer’s recommendations and that all QA/QC checks have been performed. The Screening data objective
requires that the calibration and detection limits be evaluated. All field analytical reports must be reviewed in
accordance with Administrative Procedure (AP) #22, Peer Review of SERAS Deliverables.

11.0 HEALTH AND SAFETY

When working with potentially hazardous materials, follow Environmental Protection Agency (EPA), Occupational
Safety and Health Administration (OSHA) and corporate health and safety practices.

12.0 REFERENCES

United States Environmental Protection Agency, 1999. Compendium of Methods for the Determination of Toxic
Organic Compounds in Ambient Air. EPA /625/R-96/010b, Office of Environmental Research and Development,
Compendium Methods TO-15.

National Environmental Laboratory Accreditation Committee (NELAC), Quality Systems, current approved
version.

US EPA. 1999. Statement of Work for Organic Analysis, Document Number OLM04.2, Contract Laboratory
Program.

13.0 APPENDICES
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 12 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

A - Tables
B - Figures
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 13 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

APPENDIX A
Tables
SOP #1701
January 2006
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 14 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

TABLE 1. Typical Method Target Analytes (Quant Ions) and Corresponding Internal Standards

Bromochloromethane (49) 1,4-Difluorobenzene (114) Chlorobenzene-d5 (117)

Propylene (41) Carbon tetrachloride (117) Toluene (91)

Chlorodifluoromethane (51) 1,2-Dichloroethane (62) trans-1,3-Dichloropropene (75)
Dichlorodifluoromethane (85) Benzene (78) 1,1,2-Trichloroethane (97)
Dichlorotetrafluoroethane (85) Heptane (43) 2-Hexanone (43)
Chloromethane (50) Trichloroethene (130) Tetrachloroethene (166)
Vinyl chloride (62) 1,2-Dichloropropane (63) Dibromochloromethane (127)
1,3-Butadiene (39) 1,4-Dioxane (88) 1,2-Dibromoethane (107)
Bromomethane (94) Methyl isobutyl ketone (43) Chlorobenzene (112)
Chloroethane (64) cis-1,3-Dichloropropene (75) Ethylbenzene (91)
Trichlorofluoromethane (101) m&p-Xylenes (91)
Isopropyl alcohol (45) o-Xylene (91)
Acetone (43) Styrene (104)
Trichlorotrifluoroethane (151) Bromoform (173)
1,1-Dichloroethene (61) 1,1,2,2,-Tetrachloroethane (83)
Methylene chloride (49) 4-Ethyltoluene (105)
MTBE (73) 1,3,5-Trimethylbenzene (105)
trans-1,2-Dichloroethene (61) 1,2,4-Trimethylbenzene (105)
Hexane (57) 1,3-Dichlorobenzene (146)
1,1-Dichloroethane (63) 1,4-Dichlorobenzene (146)
2-Butanone (43) 1,2-Dichlorobenzene (146)
cis-1,2-Dichloroethene (61) 1,2,4-Trichlorobenzene (180)
Ethyl acetate (43)
Chloroform (83)
Tetrahydrofuran (42)
1,1,1-Trichloroethane (97)
Cyclohexane (56)
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 15 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

TABLE 2. GC/MS Performance Criteria for p-Bromofluorobenzene*

m/z Ion Abundance Criteria 1

50 8.0 - 40% of mass 95

75 30 - 66% of mass 95
95 Base Peak, 100% relative abundance
96 5.0 - 9.0% of mass 95
173 Less than 2% of mass 174
174 50 - 120% of mass 95
175 4.0 - 9.0% of mass 174
176 93 - 101% of mass 174
177 5.0 - 9.0% of mass 176

1
All ion abundances must be normalized to m/z 95, the nominal base peak.
Three scans (the peak apex and the scans immediately preceding and following the apex) are acquired
and averaged. Background subtraction is conducted using a single scan prior to the elution of BFB.

* US EPA. 1999. Statement of Work for Organic Analysis, Document Number OLM04.2, Contract
Laboratory Program.
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 16 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

TABLE 3. Average Response Calibration Equations

Ax Cis
RRF
Ais Cx
where:

RF = Response factor
Ai = Area of analyte I
Ais = Area of internal standard
Ci = Concentration of analyte I
Cis = Concentration of internal standard

RF1 ... RFn

RFavg
n
where:

RFaverage= Average response factor from initial calibration

n = Number of analysis

n
2
RFi RFaverage
i 1
SD
n 1

RFcc RFaverage
(%D = x 100
RFaverage

where:

%D = Percent difference
RFcc = Response factor of compound in continuing calibration
SD = Standard deviation
 STANDARD OPERATING PROCEDURES
SOP: 1701
PAGE: 17 of 22
REV: 1.1
DATE: 01/19/06
FIELD ANALYSIS OF VOLATILE ORGANIC COMPOUNDS
IN TEDLAR BAG AIR SAMPLES BY GC/MS
(TRIAD GC/MS - Based on EPA TO-15A)

TABLE 4. Linear Regression Calibration Equations

The regression will produce the slope and intercept terms for a linear equation in the form: