Ambient Air Sampling
for
Volatile Organic Compound Analysis
Tribal Air Quality Program
August 2010
Ambient Air Sampling
for
Volatile Organic Compound Analysis
Tribal Air Quality Program
Prepared by:
Bertha Prince
Jennifer Dobson
Troy Ritter
Edward Lohr
Alaska Native Tribal Health Consortium
Division of Environmental Health and Engineering
1901 Bragaw Street, Suite 200
Anchorage, Alaska 99508
August 2010
Table of Contents
1 QA Plan Identification and Approval ...........................................................................................5
2 Distribution ...................................................................................................................................6
3 Organization and Responsibilities ................................................................................................6
3.1 Roles and Responsibilities .............................................................................................................. 6
3.2 EPA Office of Air Quality Planning and Standards ........................................................................ 8
3.3 EPA Region 10 ................................................................................................................................ 8
4 Problem Definition and Background ............................................................................................9
4.1 Problem Statement and Background ............................................................................................... 9
5 Scope and Application ..................................................................................................................9
5.1 Nuiqsut Ambient Air VOC Site Sampling Plan .............................................................................. 9
5.2 Sampling Schedule ........................................................................................................................ 10
5.3 Data Collection and Quality Objectives ........................................................................................ 11
5.4. Training/Certification ................................................................................................................... 11
5.5 Documentation and Records ......................................................................................................... 11
5.6 Sampling Procedures ..................................................................................................................... 11
5.7 VOCs ............................................................................................................................................. 12
5.8 Laboratory ..................................................................................................................................... 13
5.9 Standard Operating Procedures (SOPs) ........................................................................................ 13
6 Summary of the Method .............................................................................................................13
6.1. Grab Sampling.............................................................................................................................. 13
6.2. Sampling Techniques ................................................................................................................... 13
6.3. Compendium Methods ................................................................................................................. 14
7 Definitions...................................................................................................................................14
8 Interferences ................................................................................................................................15
8.1. Particulates ................................................................................................................................... 15
8.2. Contaminants................................................................................................................................ 15
8.3. Moisture and Carbon Dioxide ...................................................................................................... 15
8.4. Potential for Overlap .................................................................................................................... 15
9 Equipment Description ...............................................................................................................15
9.1. Sample and Shipping Containers: ................................................................................................ 15
9.2. Flow Restrictors and Samplers ..................................................................................................... 16
9.3. Gas Chromatograph/Mass Spectrometer System ......................................................................... 16
10 Reagents and Standards ............................................................................................................16
10.1 Organic Solvents (Purge & Trap Grade) ..................................................................................... 16
10.2 Laboratory Reagent Water .......................................................................................................... 16
10.2.1 Type 1 Laboratory Reagent Water ........................................................................................... 17
10.3 Helium, Nitrogen and Air............................................................................................................ 17
10.4 Internal Standard and Tuning Standard ....................................................................................... 17
10.5 Calibration Standards .................................................................................................................. 17
11 Equipment Cleaning and Certification Procedures ...................................................................18
11.1 Canister Cleaning Procedure ....................................................................................................... 18
11.2 Canister Certification Procedure ................................................................................................. 19
12 Sample Collection, Handling and Storage ................................................................................20
12.1 Sample Collection: ...................................................................................................................... 20
12.2 Sample Handling, Storage and Hold Times: ............................................................................... 21
13 Sample Analysis Procedure and Instrument Operating Conditions ..........................................22
13.1. Entech Concentrator and Auto-sampler Settings (typical): ........................................................ 22
13.2 Gas Chromotograph/Mass Spectrometer Conditions (typical): .................................................. 22
13.3 GC/MS Instrument File Names ................................................................................................... 22
13.4 GC/MS Tuning ............................................................................................................................ 23
13.5 Initial and Routine Calibration: ................................................................................................... 23
13.5.1 Average Response Factor ......................................................................................................... 24
13.6 PQL Check Standard (PQLCS) ................................................................................................... 24
13.7 Internal Standard Retention Time and Internal Standard Response ............................................ 24
13.8 Analysis Sequence....................................................................................................................... 25
13.9 Pre-Analysis Checklist for the GC/MS Run Sequence: .............................................................. 26
13.10 Post-Analysis Checklist: ........................................................................................................... 26
13.11 Qualitative Analysis: ................................................................................................................. 27
13.12 Quantitative Analysis ................................................................................................................ 28
14 Quality Control .........................................................................................................................28
15 Data Processing, Review and Reporting ...................................................................................29
15.1 Data Processing ........................................................................................................................... 29
1 QA Plan Identification and Approval
Title: Ambient Air Sampling into Stainless Steel Canisters for Volatile Organic
Compound Analysis for the Alaska Native Tribal Health Consortium, Division of
Environmental Health and Engineering department.
The Ambient Air Sampling into Stainless Steel Canisters for Volatile Organic Compound
Analysis Plan for the Alaska Native Tribal Health Consortium, Division of
Environmental Health and Engineering is recommended for approval and commits the
Program to follow the elements described within.
ANTHC
Troy Ritter, ANTHC ANV Air Project Manager
Date
Ed Lohr, ANTHC ANV Air Monitoring Project Coordinator
Date
EPA Region 10
Mary Manous, EPA Project Officer
Date
Christopher Hall, Quality Assurance Officer
Date
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2 Distribution
A copy of the Ambient Air Sampling into Stainless Steel Canisters for Volatile Organic
Compound Analysis is distributed to the following listed below:
Name
Troy Ritter
Position
Project
Manager
Organization
ANTHC
Ed Lohr
Project
Coordinator
ANTHC
Christopher
Hall
Quality
Assurance
Officer
EPA Region 10
Mary Manous EPA Project
Officer
EPA Region 10
Contact Information
1901 Bragaw St.
Anchorage, AK 99508
907-729-5683
tlritter@anthc.org
1901 Bragaw St.
Anchorage, AK 99508
907-729-3527
elohr@anthc.org
1200 Sixth Avenue
OEA-095
Seattle, WA 98101
206-553-0521
hall.christopher@epa.gov
1200 Sixth Avenue, Suite 900,
AWT-107
Seattle, WA 98101
206-553-1059
manous.mary@epamail.epa.gov
3 Organization and Responsibilities
3.1 Roles and Responsibilities
Federal, State, Tribal and local agencies all have important roles in developing and
implementing satisfactory ANV air monitoring programs. As part of the planning effort,
EPA is responsible for developing National Ambient Air Quality Standards (NAAQS),
and identifying a minimum set of QC samples from which to judge data quality. The
state and local organizations are responsible for taking this information and developing
and implementing a quality system that will meet the data quality measurements. Then, it
is the responsibility of both EPA and ANTHC and local organization to assess the quality
of the data and take corrective action when appropriate. The responsibilities of each
organization follow.
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Title and responsibilities of key personnel are:
ANV Air Quality Program Manager-Troy Ritter
● Management of the overall ANV Air Quality Program
ANV Air Quality Program Assistants- Jennifer Dobson, Chris Fish
●Community Planning and Support
●Air Monitoring Procedures and Training Support
ANV Air Quality Monitoring Program Assistant-Bertha Prince
●Air Monitoring Procedures and Training
●Quality Assurance Policies, Plans, and Procedures
●Performance and System Audits
●Reporting
Technical Services Section Manager, TBD
●Calibration and Quality Control Standards
●Air Monitoring Equipment Procurement, Testing, and Calibration
●Parts and Supplies Inventory
ANV Air Toxics Project Coordinator, TBD
●Network Evaluation and Design Coordination
●Station Installment and Operation Coordination
●Air Toxics Data Management
●Final Reports
ANV Air Monitoring Station Operators, TBD
Note: An operator in Nuiqsut will be hired by June 30, 2010.
●Station Installation, Operation, Sample Collection
●Sample Shipments to ANTHC
●Quality Control and Precision Checks
●First Level Data Validation
●Routine Maintenance and Repair
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Figure 1 represents the organizational structure of the areas of the ANV Air Quality
Monitoring Program that are responsible for the activities defined above.
Figure 1 ANV Air Quality Monitoring Program Organizational Chart
Troy Ritter,
ANV Air Quality
Program Manager
EPA Staff
Mary Manous
Christopher Hall
Jennifer Dobson,
Chris Fish,
Bertha Prince,
ANV Air Quality
Program Assistant
ANV Air Quality
Program Assistant
ANV Air Quality
Program Assistant
3.2 EPA Office of Air Quality Planning and Standards
3.3 EPA Region 10
The EPA Regional Offices will address environmental issues related to the States within
their jurisdiction and to administer and oversee regulatory and congressionally mandated
programs. The major quality assurance responsibilities of EPA’s Regional Offices are
the coordination of quality assurance matters at the Regional levels with the State and
local agencies. This is accomplished by the designation of EPA Regional Project
Officers who are responsible for the technical aspects of the program including:
Reviewing QAPP’s be Regional QA Officers who are delegated authority by the
Regional Administrator to review and approve QAPP’s for the agency.
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4 Problem Definition and Background
4.1 Problem Statement and Background
The North Slope of Alaska is home to the largest oil field in North America, Prudhoe
Bay, as well as several other smaller oil fields. ConocoPhillips began oil production at
the Alpine oil field in November 2000. The Alaska Native village of Nuiqsut is located
56 miles away from Prudhoe Bay and 8 miles from the Alpine oil field where oil is
extracted and undergoes initial refinement. Natural gas is generated as a waste product of
oil drilled and ‘flared off’ as a means of disposal. Nuiqsut is an Inupiat Eskimo
community of 425 people, many of whom follow a traditional subsistence lifestyle.
Some community residents have expressed concerns about the proximity to nearby oil
development, resulting in air pollution and potential health implications.
There is one air monitor currently operating in Nuiqsut that measures only PM10. This air
monitor is reportedly funded by ConocoPhillips. Data from the monitor is collected by
ConocoPhillips and then provided to the community. Nuiqsut community members have
expressed concerns about the legitimacy of this data. There has been no independent
assessment of the impact of oil industry activities on the health of Nuiqsut residents.
There is currently no available data on background levels of volatile organic compounds
(VOC’s) in Nuiqsut’s ambient air. It is unknown if the nearby oilfield contributes to VOC
levels in the community. This activity aims to determine ambient VOC levels in Nuiqsut
and serve as a first-order assessment to determining if VOC’s produced at the oil field are
influencing the community. It is unknown if other conditions will contribute to elevated
VOC levels. Future projects may evaluate the effect of severe weather conditions such as
southerly winds and inversion on extreme cold weather days, and process conditions such
as flare purging.
5 Scope and Application
5.1 Nuiqsut Ambient Air VOC Site Sampling Plan
This document details the locations of sampling sites for organic compounds (VOC’s) in
ambient air using stainless steel canisters. Samples will be taken at four locations around
the perimeter of Nuiqsut using the combined EPA methods TO14A/TO-15 as described
in this plan, with the possibility of adding two more locations. The rationale behind the
locations of these samples is to identify the presence of contaminants as they may be
transported into and through Nuiqsut as well as the possibility of dispersion and
identifying other contaminant sources within the village. In the future, meteorological
data from the airport station may be cross referenced with sample results.
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Figure 5.1 Sampling Site Map
NW sample
location
NE sample
location
SW sample
location
SE sample
location
5.2 Sampling Schedule
The ANV Air Quality Program is proposing conducting 4 rounds of sampling following
this QAPP; one conducted June 30-31, 2010, one for September 7-8, 2010, and the
remaining two sampling activities will be completed during the winter months. Due to the
nature of travel in Rural Alaska, additional sampling schedules will be proposed and
added as the project progresses and timelines can be confirmed.
Table 5.2 Sample Schedule, September 2010
Sample Location
Northwest
Northeast
Southwest
Southeast
Method
EPA Method
TO-14A/15
EPA Method
TO-14A/15
EPA Method
TO-14A/15
EPA Method
TO-14A/15
Ambient Air Sampling VOC’s
Start
9/7/2010
10:30am
9/7/2010
10:50am
9/7/2010
11:20am
9/7/2010
11:45am
End
9/8/2010
10:30am
9/8/2010
10:50am
9/8/2010
11:20am
9/8/2010
11:45am
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Rate
0.928
ml/min
0.928
ml/min
0.928
ml/min
0.928
ml/min
Volume
1 liter
1 liter
1 liter
1 liter
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9/6/2010
Jennifer Dobson will travel to Nuiqsut and arrive in the afternoon of 9/6/2010.
Accommodations will be setup. In the afternoon, all sampling equipment will be
inspected for damage. Missing items or other needs will be gathered.
9/7/2010
Jennifer will prepare for sampling, and proceed to the Northwest sample location, the
samples will be set up and sample runs will follow Table 5.2 Sample Schedule.
9/8/2010
Jennifer will collect the canister samplers following Table 5.2 Sample Schedule. The
canisters will be packed and shipped following the laboratory instructions.
5.3 Data Collection and Quality Objectives
This purpose of this project is to collect data on VOC’s in ambient air during mild
weather conditions and typical process conditions at the oilfield and refinery. This data
must be collected following the quality procedures set forth in this document. The quality
of this data is important because it will be used to determine if further monitoring will be
useful in defining the oilfield and refineries impacts on ambient VOC levels under other
than typical weather and process conditions.
The data to is to be collected and analyzed using the following methods:
 EPA Method TO-14A
 EPA Method TO-15
5.4. Training/Certification
Personnel responsible for collecting the samples in this project will be familiar with the
applicable EPA methods, laboratory established sample collection procedure and this
document prior to mobilizing on the project.
5.5 Documentation and Records
The most current QAPP will be provided by the ANV Air Quality Program Assistant to
all sampling personnel prior to mobilization on the project. A field data sheet and a field
log will be used to collect all relevant information during the project and maintained with
all project records. All calibration and equipment maintenance records will be maintained
by the equipment owner and referenced in the field data sheet. Copies of the laboratory
chain of custody and results will be maintained in the project records.
All relevant records collected will be appended to the final project report and maintained
with the project records and retained according to EPA requirements.
5.6 Sampling Procedures
This document details the procedures for sampling volatile organic compounds (VOC’s)
in ambient air using stainless steel canisters. The whole air samplers are collected in
stainless steel canisters using air sampling equipment. The samples are subsequently
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analyzed by gas chromatography/mass spectrometry (GC/MS). The procedures describe
the operational details required to collect sub-atmospheric pressure samples.
5.7 VOCs
This standard operational procedure is applicable to VOC’s known to be stable when
stored in stainless steel canisters. The compounds given in table 1 are listed in the EPA
Methods TO-14A and TO-15, which describe the analysis of VOC’s in ambient air at sub
parts-per billion (ppb) level.
TABLE 1. List of Compounds and Associated Analysis Method:
Acetone
Acrolein
TO-15
TO-15
Allyl chloride
Benzene
Benzyl chloride
Bromodichloromethane
Bromoform
Bromomethane
1,3-Butadiene
2-Butanone (MEK)
TO-15
TO-14A
TO-15
TO-15
TO-15
TO-14A
TO-15
TO-15
Carbon disulfide
TO-15
Carbon tetrachloride
Chloroethane
Chlorobenzene
Chloroethane
Chloroform
Chloromethane
Cyclohexane
Dibromochloromethane
1,2-Dibromoethane
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-15
TO-15
TO-14A
TO-14A
TO-14A
TO-14A
Dichlorodifluoromethane
(Freon 12)
TO-14A
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethene
Cis-1,2-Dichloroethene
Trans-1,2-Dichloroethene
1,2-Dichloropropane
Cis-1,3-Dichloropropene
Trans-1,3Dichloropropene
TO-14A
TO-14A
TO-14A
TO-14A
TO-15
TO-14A
TO-14A
TO-14A
Ambient Air Sampling VOC’s
1,4-Dioxane
1,2-Dichloro-2,2,3,3tetrafluoroethane (Freon
114)
Ethyl acetate
Ethyl benzene
4-Ethyl toluene
Heptane
Hexachloro-1,3 butadiene
2-Hexanone
Methylene chloride
4-Methyl-2-pentanone
(MIBK)
Methyl-t-butyl ether
(MTBE)
2-Propanol
Propylene
Styrene
1,1,2,2-Tetrachloroethane
Tetrachloroethene
Tetrahydrofuran
Toluene
1,2,4-Trichlorobenzene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethene
Trichlorofluoromethane
(Freon 11)
1,1,2-Trichloro-1,2,2trifluoroethane (Freon
113)
1,2,4-Trimethylbenzene
1,3,5-Trimethylbenzene
Vinyl acetate
Vinyl bromide
Vinyl chloride
ortho-Xylene
meta-Xylene
para-Xylene
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TO-15
TO-14A
TO-15
TO-14A
TO-15
TO-15
TO-14A
TO-15
TO-14A
TO-15
TO-15
TO-15
TO-15
TO-14A
TO-14A
TO-14A
TO-15
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-14A
TO-15
TO-15
TO-14A
TO-14A
TO-14A
TO-14A
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5.8 Laboratory
ANTHC will be collaborating with Galson Laboratories in East Syracuse, New York for
calibration, cleaning and analysis of the mini-canisters. Test ID’s and equivalent EPA
methods covered by this SOP:
● A-TO14/15-EPA Method TO-14A and TO-15 analysis, Canister Air Analysis
5.9 Standard Operating Procedures (SOPs)
Refer to the following Standard Operating Procedures (SOPs) for additional information:
These supporting SOPs contain critical details not fully described within this
method SOP. The analyst should be completely familiar with all of these SOPs.
5.9.1. Safety and Waste Management Practices in the Organic Analysis Groups
5.9.2. Glassware and Equipment Cleaning Procedures
5. 9.3. Data Review/Authorization Procedures for the Volatile Organic and
Methyl Mercury Laboratory
5.9.4. Quality Assurance/Quality Control Measurements in the Volatile Organics
(VOC) Laboratory
5.9.5. Non-Conformance Reporting System
5.9.6. Laboratory Policy Regarding Manual Chromatographic Peak Integration
5.9.7. Standard Operating Procedure for Reporting Qualified Data
5.9.8. Standard Operating Procedure for Records Storage and Retention
6 Summary of the Method
6.1. Whole Air Sampling
The passivated canister is designed to offer flexibility in collecting air samples. The
primary mode for collecting samples will be: (1) Whole air sampling of ambient air.
Specialized field equipment is described for both short-term and long-term monitoring
scenarios. For this activity, 1 liter canisters equipped with 24 hour regulators will be
used.
6.2. Sampling Techniques
Whole air is collected into evacuated canisters using passive or pump-assisted air
sampling techniques. Both of these techniques draw a sample of ambient air through a
sampling train that removes particulates, regulates sampling flow rate, controls sample
start and end times, and monitors start and end pressures. The instrumentation included
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in the procedures may be used to collect and analyze both sub-atmospheric pressure and
pressurized samples.
The volatile compounds collected in the canisters are transported to the laboratory and
are analyzed by gas chromatography / mass spectrometry, which provides both
qualitative and quantitative information. During analysis in the laboratory, the sample
canister is attached to an auto sampler where typically 10 to 1000 mL of the air sample is
pumped out of the canister and collected on a cryogen-cooled glass bead trap. Internal
standard and tuning compounds are also collected on the trap with the sample. The
sample and internal standard compounds are then transferred to a second stage Tenax
trap, effectively removing most of the water and CO2. The VOC compounds are then
transferred to a third stage where they are cryogenically focused prior to injection onto
the GC column. The detector used in the analysis is a mass spectrometer.
6.3. Compendium Methods
The analysis method is based on TO-14A and TO-15 in the Compendium of Methods for
the Determination of Toxic Organic Compounds in Ambient Air, Second Edition
(EPA/625/R-96/010b). All of the procedures described here are designed to meet or
exceed the criteria from both of these EPA quantitative methods. Please refer to these
EPA guidance documents for additional details.
7 Definitions
Cryogen: a refrigerant (typically liquid nitrogen) used to obtain sub-ambient temperatures
in the VOC concentrator instrument prior to sample introduction on the analytical
column. The cryogen used by our instruments is liquid nitrogen.
Dynamic Calibration: calibration of the analytical system with gas standard
concentrations at similar concentrations, in a form identical and through the same
analytical path as in the real samples.
Dynamic Dilution: means of preparing calibration mixtures or diluting a sample in which
a concentrated gas stream is continually blended with zero air in a manifold and
introduced at the inlet of the analytical system or a receiving canister.
Pressure, Absolute: pressure measured with reference to absolute zero pressure expressed
in psia. An absolute pressure value of zero is indicative of an evacuated system
(vacuum).
Pressure, Gauge: pressure measured with reference to the surrounding atmospheric
pressure expressed in units of psi. A gauge pressure value of zero is equal to atmospheric
pressure.
Sub-atmospheric Sampling: collection of ambient air into an evacuated canister with a
final canister pressure below atmospheric pressure. This is the normal practice when
collecting air with passive sampling devices since the sample collection must be stopped
prior to completely filling the canister.
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8 Interferences
8.1. Particulates
Particulates that cause blockage in the sample collection pathway are a potential problem
during sample collection. The field equipment must be tested periodically to insure the
integrity of the sampling equipment. The presence of these problems can often be
observed by monitoring and recording the initial and final pressure when sampling.
8.2. Contaminants
Contamination may occur in the sampling and concentrator systems if the equipment is
improperly cleaned before each use. All sampling and analysis equipment coming into
contact with the sample must be thoroughly cleaned and tested on a regular basis.
8.3. Moisture and Carbon Dioxide
Moisture and carbon dioxide are two of the primary interferences encountered in whole
air measurements due to the normally high concentration of these compounds in ambient
air. Elevated levels of water or carbon dioxide may severely restrict the sample size that
can be measured. Compendium Method TO-15 provides guidance for water management
systems as it pertains to the analysis of polar organic compounds.
8.4. Potential for Overlap
The potential for overlap of eluting compounds in the chromatography is significant
when dealing with such an extensive compound list from two air analysis methods. The
potential for encountering interferences is significantly reduced by using cryogenic
focusing, a smaller ID capillary column and a mass spectrometer detector. Cryogen
focusing and the small ID capillary column used in this method provides for an enhanced
compound separation such that overlapping compounds are minimized. Also, the mass
spectrometer can effectively resolve many of the remaining overlapped compounds based
on the mass spectra of the compounds.
9 Equipment Description
The operation, cleaning and scheduled maintenance procedures prescribed by the
equipment manufactures are followed as provided in the manufacturer’s instructions.
Documentation of cleaning, maintenance or system modification is recorded in a
maintenance logbook that accompanies each instrument system.
9.1. Sample and Shipping Containers:
Galson Lab canisters with fused silica lining in the can and valve. The laboratory
maintains more than 20 canisters in its inventory.
●400-mL Entech canister with fused silica lining in the can and valve. The
laboratory maintains 4 extra canisters, in addition to the 26 canisters in the field for
the Bureau of Emergency Response.
●Aluminum shipping container that holds two 1-L canisters. The laboratory
maintains 4 shipping canister in its inventory.
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●Entech CS1200P Flow Controller with sampling belt and holster.
●Entech Vacuum Check Gauge equipped with a quick connect adapter for the 400mL canisters
●Docosil Weather proof case used to transport 400-mL canisters and samplers
●Entech 3100A Canister Cleaner equipped with Entech SmartLab software
9.2. Flow Restrictors and Samplers
The fill times indicated below are for the 400-mL mini-canisters. The larger canisters
will require a longer fill time proportional to the volume. Most of the samplers are
equipped with quick connections, but some have Swagelock connections.
●Quick Fill Grab Sampler
●1 Minute Fill Sampler
●15 Minute Fill Sampler
●8 Hour Fill Sampler
●24 hour Fill Sampler (only for 1 liter container)
9.3. Gas Chromatograph/Mass Spectrometer System
●Agilent 6890 or Finnigan Trace Gas Chromatograph.
●Agilent 5973 Inert or Finnigan Polaris Q Mass Spectrometer
●Entech 7100A Pre-concentrator
●Entech 7016CA 16-Position Auto-sampler
●Entech 4600A Dynatmic Diluter
●IBM-compatible Personal Computer.
●Agilent Enviroquant or Finnigan Xcalibur Computer Software.
●Entech SmartLab Network Software
●J&W Scientific DB-5MS, 60 m x 0.25 mm ID capillary column, 0.25 μm film
thickness.
●Supelco High Capacity Gas Purifier
10 Reagents and Standards
Working with volatile compounds presents a number of challenges not normally
confronted in the handling of most other chemicals. Volatile compounds may escape
from sample containers or, when present in the laboratory environment, can contaminate
analytical equipment.
Sources of the reagents and chemicals are given, but may change based on availability,
quality and cost. The use of a different source is acceptable without modification of the
procedures provided the products are equivalent.
10.1 Organic Solvents (Purge & Trap Grade)
Methanol: CH3OH-Purge & Trap grade methanol is purchased in 500 mL amber bottles.
10.2 Laboratory Reagent Water
Type 1 laboratory reagent water is prepared in the laboratory. The criterion for
laboratory reagent water is that it must not contain any analytes of interest at a
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concentration greater that 20% of the reporting limit. Other non-target compounds may
be detected in the laboratory reagent water, but must not interfere with the analysis of the
target compounds. Examples of non-target compounds commonly observed are methanol
(used in glassware cleaning and standard preparation) and siloxanes (from surfactants,
pump oils and column bleed).
10.2.1 Type 1 Laboratory Reagent Water
Municipal water is purified with Solution 2000 Water Purification System that uses
activated carbon cartridges and ion-exchange cartridges to remove impurities.
10.3 Helium, Nitrogen and Air
Ultra high purity grade in gas cylinders from Air Products. Helium is used as the carrier
gas in the GC/MS instrument system.
10.4 Internal Standard and Tuning Standard
100 ppbv Internal Standard and Tune Standard Mixture: the internal standard and tune
standard mixture is purchased in a 3395 L (2A) cylinder from Spectra Gases at a
concentration of 100ppbv. The internal standard compounds are bromochlorobenzene,
chlorobenzene-d5, and 1,4-difluorobenzene. The mass spectrometer tune standard
compound is 4-bromofluorobenzene. The 4 compounds in this mixture are prepared in
nitrogen at a final cylinder pressure of 2000 psig. The standard mixture is certified by
Spectra Gases for one year from preparation.
10.5 Calibration Standards
●100 ppbv TO-14A Calibration Standard Mixture: The TO-14A calibration standard
is purchased in a 3395 L (2A) cylinder from Spectra Gases at a concentration of 100
ppbv. The TO-14A standard mixture contains 39 of the compounds listed in Table 1
and includes all of the Compendium Method TO-14A target compounds, except for
benzyl chloride. The compound benzyl chloride is included in the TO-15 calibration
mixture. The 39 compounds in this mixture are prepared in nitrogen at a final
cylinder pressure of 2000 psig. The standard mixture is certified by Spectra Gases for
one year from preparation.
●100 ppbv TO-15 Calibration Standard Mixture: The TO-15 calibration standard is
purchased in a 3395 L (2A) cylinder from Spectra Gases at a concentration of 100
ppbv. The TO-15 standard mixture contains 25 of the compounds listed in Table 1
and includes only a subset of the Compendium Method TO-15 target compounds,
except for benzyl chloride. The 39 compounds in this mixture are prepared in
nitrogen at a final cylinder pressure of 2000 psig. The standard mixture is certified by
Spectra Gases for 6 months from preparation.
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11 Equipment Cleaning and Certification Procedures
The equipment used for sample collection and analysis must be clean and certified before
use.
11.1 Canister Cleaning Procedure
The laboratory prepares the sample canisters by cleaning and testing the canisters in
batches of 4 at a time using the Entech 3100A Canister Cleaner. The passivated canisters
are expensive, so handle them with care. Please refer to the canister cleaner operating
manual for more detailed operation and maintenance instructions. Use the following
cleaning and testing procedure to prepare the canisters:
11.1.1 Inspect each canister for damage, corrosion and visible contamination. Make
repairs as needed to insure the integrity of each canister. Inspect for loose or
missing parts as well. Remove any external contamination with DI water or
methanol solvents and soft cloth wipe. Do not use other solvents or abrasives
unless specifically approved by your supervisor.
11.1.2 Turn on the power for the Entech 3100A cleaner and diaphragm pump. Enter the
Entech SmartLab software to make sure the instrument is communicating and that
the valves to the manifold are all closed. Turn on the molecular drag pump and
allow it to come up to speed (check indicator on front instrument panel). At this
point the instrument is ready to use. The manifold valves must be kept closed
during the aforementioned startup procedures.
11.1.3 Program the Entech SmartLab software for the type of cleaning cycle (light,
medium or heavy-duty). The type of cycle used depends on the previous use of
the canisters. If the canisters are already relatively clean then use a light-duty
cleaning cycle. Use the heavy-duty cleaning cycle for more contaminated
canisters.
11.1.4 Remove the protective fitting plugs on the canisters and the manifold connections
on the Entech 3100A canister cleaner.
11.1.5 Attach the canisters to the cleaner manifold. The current cleaning unit is designed
to accept 4 canisters, but can be extended for up to 8 canisters. Each canister is
attached to the manifold with a Swagelock fitting. Do not over-tighten or crossthread the fittings.
11.1.6 Open the valves on all of the canisters after all of the manifold ports have been
connected to canisters or sealed with plugs.
11.1.7 Perform a leak check of the canisters and manifold through the SmartLab
software. L ocate and correct any leaks. Pressurizing the manifold and canisters
with Helium and using the leak detector is an excellent way to locate leaks. Do
not over-tighten fittings. Leaking canisters must be repaired before being placed
into service. Consult a supervisor on repairing canisters.
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11.1.8 Initiate the cleaning cycle through the Entech SmartLab software.
11.1.9 Slip the canister heater bands onto each canister and connect the heater band
electrical cord. Take care to remove all combustible materials from the area
around the heater bands and avoid direct contact with the heater elements. Turn
on the electrical heater bands.
11.1.10 Monitor the first cleaning cycle to make sure the Entech 3100A cleaner is
working properly. The heater bands should heat up quickly and the molecular
drag pump indicator must be on. Monitor to see if the instrument’s overheating
light comes on at any time during operation. Shut the system down and consult
the supervisor if any irregularities are noted.
11.1.11 The cleaner will perform vacuum/pressure cycles using moist (UPC) nitrogen for
pressurization.
11.1.12 After the cleaning cycle is complete, turn off and remove the heater bands, close
the manifold and close the valve to one of the canisters. The canister with the
closed valve will be used to QC test the entire batch and must be marked with
batch date.
11.1.13 Allow the manifold and open canisters to fill with zero-grade nitrogen or zero air
using the controls in the SmartLab software. Close the manifold after the
canisters have filled with nitrogen.
11.1.14 Open the valve on the QC canister (closed previously) so that nitrogen will flow
from each of the open canisters attached to the manifold into the evacuated QC
canister. Close the valve to the QC canister only after equilibrium is reached.
11.1.15 Evacuate the remaining open canisters to a vacuum of less than 5 mTorr through
the SmartLab software.
11.1.16 Close the manifold and canister valves. Remove the QC canister for testing.
11.2 Canister Certification Procedure
●A single QC canister from each cleaning batch must be analyzed for volatile
organics before the canisters may be used to collect air samples
●Attach the QC canister from a cleaning batch onto one of the connections on the
Entech 7016CA 16-position auto-sampler
●Perform a leak check on the auto-sampler connections
●Perform an analysis of the QC canister as though it is a real sample
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●The canisters in the cleaning batch may be used for sample collection if the QC
canister results are < 0.10 ppbv and are free of other interferences
●Reattach the QC canister to the cleaning manifold
●Repeat the cleaning process if the QC check indicates that the canisters are
contaminated
●Once tested clean, the canisters are evacuated to < 5 mtorr. Close the manifold
and canister valve, remove the canisters from the cleaner manifold and replace the
dust caps on the open fittings
●Attach an identification tag that gives the date of cleaning and your initials
●The canisters are now ready for collection of air samples.
12 Sample Collection, Handling and Storage
The sampling process begins with the preparation of the canisters used to collect the
sample. The canisters are provided by the laboratory and are prepared based on the
sample requests received. This section describes the steps involved in collecting and
handling the air samples.
12.1 Sample Collection:
Select the type of sampling to be performed. Samples are collected with either a passive
critical orifice sampler or an active pump sampler with a mass flow controller.
The canisters and sampling unit must be certified clean prior to collecting samples as
described in Section 11.
The flow rate setting of the sampler must be established prior to collecting samples. The
internal flow control device in the sampling unit must be calibrated with a NIST certified
flow meter prior to use. The sample collection time, canister volume and flow rate
setting are interrelated by the equation:
F=
PxV
T x 60
Where:
F = flow rate, mL/min.
P = final canister pressure, atmospheres
V = canister volume, mL.
T = sample period, hours.
Remove the protective caps from the canister valve and selected sampler unit. Place the
sampling apparatus in the area in which you wish to sample (i.e. breathing zone or
contaminated area). Connect the canister to the sampling unit. The mini-canisters are
equipped with quick-connections instead of the Swagelock fittings on the 6-liter
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canisters. Do not over tighten the Swagelock connection since this can result in leaks and
damage the fitting.
Place the sampling orifice into the sampling zone. Be careful not to protect the orifice
from precipitation or contact with standing liquids.
The canister vacuum should be at least 26 inches Hg as measured by the canister test
gauge. Do not use the canister if the internal vacuum is less.
The mini-canisters begin collecting the sample immediately after they are connected
since there is no manual valve. The mini-canister connection is maintained for a period
of time equal to or less than the time stamped on the flow restrictor orifice and is then
disconnected to end the sampling period.
The 6-liter canisters are equipped with a manual on-off valve. Once the 6-liter canister is
connected to the sampler, whole air is collected using the passive canister sampler by
simply opening the canister valve. The canister valve is left open for a period of time
equal to or less than the time determined by the flow rate of the restrictor orifice.
More complex sampling devices can have timers and electronic valves to collect the air
sample such as the AVOCs sampler manufactured by Graseby-Anderson. Please refer to
the manufacture instruction manual for details of operation.
After the air sample is collected, close the canister valve and cap the valve connections.
The outside of the sample container must be tagged with a field identification. The minicanisters may be placed into a Ziplock bag and a chain-of-custody labels may be placed
across the bag opening to give added protection to the integrity of the sample. Fill out all
applicable chain-of custody forms that accompany the samples.
A final canister pressure reading may be taken with the manual pressure gauge and
recorded.
Avoid attaching sticky labels directly onto the canisters since these labels are difficult to
remove. Use labeled bags or tags instead. Place the canisters into the designated
aluminum or plastic shipping boxes for added safety and convenience.
12.2 Sample Handling, Storage and Hold Times:
The canisters are kept in the aluminum shipping boxes for added protection when they
are not being sampled or analyzed.
The chain-of-custody form for the cleaned canisters will have an expiration date listed for
each of the canisters. The “use by” expiration date for the routine sampling containers is
1 month, although the containers are known to be stable for more than 6 months.
Sample preservation includes storage of the canisters in a cool, dry location. The canister
samples must be maintained in a secure and air-conditioned (25 °C) environment until
submitted to the DEP laboratory for analysis.
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The passivated sampling train and canisters are designed to hold an ambient air sample
for up to 30 days with minimal degradation. The hold time for the compounds listed in
this analysis is 30 days.
The sample pressure must not exceed 40 psi. Increased pressure may cause the
compounds in the canister to degrade more quickly
13 Sample Analysis Procedure and Instrument Operating
Conditions
Suggested Instrument Conditions: The instrument conditions are given below. Specific
instrument conditions may vary.
13.1. Entech Concentrator and Auto-sampler Settings (typical):
Line Temp = 100°C
Bulk Head 1 = 30°C
Bulk Head 2 = 30°C
Module 1 Trap = -150°C
Module 1 Preheat = 20°C
Module 1 Desorb = 20°C
Module 1 Bake = 130° C
Module 1 Bake Time = 5 min
Module 2 Trap = -10°C
Module 2 Preheat = off
Module 2 Desorb = 180°C
Module 2 Bake = 190°C
Module 2 Desorb Time = 3.5 min
Module 3 Trap = -180°C
Module 3 Inject = 2 min
Module 3 Bake Time = 2 min
Module 3 Event = 3
Module 3 Wait Time = 25 min
Pressure Comp Factor = 25
Loop Flush = 30 seconds
13.2 Gas Chromotograph/Mass Spectrometer Conditions (typical):
Initial Temperature = -20°C
Initial Time = 0 min
Ramp Rate = 7 C/min
MS Source Temp =210°C
Final Temperature = 200°C
Final Time = 1 min
Rate (A) = 5°C/min
Note: The GC/MS software used by the ? Instrument is designed to collect MS data,
setup calibration files, automatically perform calculations, report pass/fail for tuning, and
report detect/non-detect for compound identification based on the method criteria.
13.3 GC/MS Instrument File Names
The GC/MS Instrument file names are generated using the 9-character naming
convention YYMDDI##
YY
M
DD
I
Year (2010 = 10, 2011 = 11)
Month (1 = January, 2 = February, 3 = March, 4 = April, 5 = May, 6 = June, 7 =
July, 8 = August, 9 = September, O = October, N = November, D = December)
Day (1-31)
Instrument number (1-4)
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##
Sequential sample numbers from 01-99.
13.4 GC/MS Tuning
The GC/MS system must be checked to ensure that acceptable performance criteria are
achieved for the tuning compound bromofluorobenzene (BFB) at the beginning of each
day and every 12 hours thereafter for as long as analysis are to be performed. This
performance test must be passed and maintained before any samples or standards are
analyzed.
The internal standard and surrogate mixture added automatically by the sample
concentrator contains BFB as one of the surrogates. Analysis of a humid zero air sample
will serve as a GC/MS performance test.
The tune analysis must meet the criteria listed in EPA Methods TO-14A and TO-15 for a
25-ng injection of BFB (bromofluorobenzene). Obtain the BFB mass spectrum average
for the apex plus 1 scan before and after the apex. Confirm that all of the m/z criteria in
Table 2 are achieved. If the criteria are not achieved, the operator must retune the mass
spectrometer and repeat the test until all criteria are achieved.
Table 2. BFB m/z Abundance Criteria
Mass, m/z
50
75
95
96
173
174
175
176
177
Abundance Criteria
8-40% of mass 95
30-66% of mass 95
Base peak, 100%
5-9% of mass 95
<2% of mass 174
50-120% of mass 95
4-9% of mass 174
>93% but < 101% of mass 174
5-9% of mass 176
13.5 Initial and Routine Calibration:
Each instrument is calibrated according to the procedures specified within EPA Method
TO-14A and EPA Method TO-15. Clarification of the calibration requirements and
practices of this laboratory are discussed below. Refer to the EPA method protocols for
additional detail.
Analytical standards for the initial calibration must be certified and NIST traceable. The
standard solutions for the calibration and standard spiking solutions must be from
independent sources. The term “independent source” means that the origin of the
standard preparations is known to be different from one another. In practical terms this
requires that the solutions be prepared by two different suppliers or at a minimum, have
different lot numbers from the same supplier.
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Initial calibration of the GC/MS is performed before sample analysis, with the assistance
of the Entech 7100 calibration system. The Entech 7100 draws standard gas from
cylinders purchased at a concentration of 100 ppbv. The standard gas flow into the
Entech 7100 concentrator is regulated by a mass flow controller that is set through the
system software. The calibration must include three concentration levels and a humid
zero air sample as a minimum. The Relative Standard Deviation (RSD) for any one of
the compounds must be <30% for sample analysis to proceed.
For routine analysis, a single point calibration check (CCV) sample is evaluated daily to
insure proper calibration. If the Relative Percent Difference (RPD) for the compounds in
the single point check sample are <30%, then analysis of samples may continue.
However, if the RPD for the single point check is >30%, then recalibration is required.
13.5.1 Average Response Factor
An average response factor can be calculated for each target compound once the
calibration curves satisfy the linearity requirement. The average response factor is
calculated as follows:
Average Response Factor = As x Cis / Ais x Cs
Where:
As
=
Cis
=
Ais
=
Cs
=
Peak area of analyte or surrogate
Peak area of internal standard
Concentration of analyte or surrogate
Concentration of internal standard
The retention time of the target analytes in each calibration standard must agree within
within ± 6 seconds. Late-eluting compounds usually have much better agreement.
A reference mass spectrum library must be generated for all the target compounds. The
reference spectra can be extracted the calibration data, provided that the target
compounds do not coelute. In the case of coelution, an individual compound standard
analyzed using the same method conditions will be required to produce the reference
mass spectrum. The reference spectra will be used for qualitative and quantitative
analysis as described later in this section
13.6 PQL Check Standard (PQLCS)
A sensitivity check sample is analyzed on a daily basis at the start of each analytical run.
The PQL check standard contains analytes of interest at a concentration level of 1-2X the
method PQL. The accuracy of the PQL check standard must be in the range of 70-130 %
for analysis to continue.
13.7 Internal Standard Retention Time and Internal Standard Response
The internal standard responses and retention times of each standard and sample analyzed
are evaluated after data acquisition. If the retention time for any internal standard
changes by more than 30 seconds from the QCCS in the most recent initial calibration,
then the chromatographic system must be inspected for malfunctions and corrections
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must be made, as required. If the extracted ion response for any internal standard varies
by more than 50% from the last QCCS, the GC/MS system must be inspected for
malfunctions and corrections must be made, as appropriate. Any standard or sample
failing these internal standard checks must be re-analyzed. The system is re-calibrated, if
necessary.
13.8 Analysis Sequence
The Analysis Sequence should be similar to the following:
●Zero Air Check/BFB tune check (the zero air check and tune check can be
analyzed together)
●Calibration Check Standard every 24 hours
●PQL calibration check standard every 24 hours
●Replicate laboratory fortified blanks (LFB1 and LFB2)
●Replicate matrix spikes
●Zero air check
●Samples (including duplicate sample)
●Zero air check
●Calibration Check Standard (Include CCV at the end of every analysis batch)
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13.9 Pre-Analysis Checklist for the GC/MS Run Sequence:
●Check the GC temperature program
●Check the autosampler program
●Check the quantity of internal standard and liquid nitrogen
●Check the zero air cylinder pressure
●Check the Entech 7100 concentrator settings
●Check the job folders and field sheets for any special instructions
●Setup the acquisition sequence in the instrument log and in the computer
acquisition program
●Check the acquisition parameters in the computer program
●Arrange the canisters on the auto-sampler
●Double check the order of the sample cylinders to insure that it is consistent with
the computer acquisition and the instrument log
●Flush and pressure test the cylinder connections on the auto-sampler
●Open the valves on the sample cylinders.
13.10 Post-Analysis Checklist:
The results of each analytical run must be examined promptly upon completion. The
instruments are designed to create both an electronic file and hardcopy for each sample
analyzed. The following items must be checked following each batch analysis:
●Check all tune blanks for compliance with tuning requirements
●Check to make sure the internal standards and spikes are in the retention time
window and their mass spectra are correct.
●Check the surrogate and spike recoveries against acceptance limits. The
acceptance criteria are tabulated in the Laboratory Information Management
System (LIMS) statistics section and are updated quarterly. As a guide, the
recovery limits for the surrogates are approximately 80 to 120%. The recovery
limits for the spike compounds are approximately 70 to 130%.
●The zero air sample must be free of target compounds (less than 20% of the
compound MDLs).
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●Duplicate sample results must be comparable. Reanalyze the sample if the
duplicate varies by more than 20%.
●All detected target compounds must be within the calibration range. Reanalyze
samples at a more appropriate dilution level if compounds are out of range.
●For complete reporting procedures, refer to SOP VO-010 for specific
procedures.
●Hardcopies of all sample data must be put into the associated job folders.
●Hardcopies of the blanks, QC samples, calibration samples, LFBs, matrix spike
must be put into the Daily QC folder.
13.11 Qualitative Analysis:
Qualitative identification of each compound is based on retention time and comparison of
the sample mass spectrum with characteristic ions in the reference mass spectrum. The
characteristic ions from the reference mass spectrum are defined to be the three ions of
greatest intensity or any ions over 30% relative intensity. Compounds are identified as
present when the following criteria are met:
●The characteristic ions of a compound maximize in the same scan or within one
scan of each other.
●The retention time of the compound is within ± 6 seconds of the retention time of
the standard component.
●The relative intensities of the characteristic ions agree within 30% of the relative
intensities of these ions in the reference spectrum. The presence of coeluting
compounds may alter the relative intensities and complicate the compound
identification. Examination of extracted ion current profiles can aid in the selection
of spectra and in qualitative identification of compounds.
●Structural isomers that produce similar mass spectra and are sufficiently resolved
are identified as individual isomers. If the height of the valley between two close
eluting isomers is more than 25% of the sum of the two peak heights, then the
structural isomers must be identified as isomeric pairs.
●A library search must be performed for unknown chromatographic peaks when the
total ion chromatogram of the sample contains unknown peaks larger than the
internal standard peaks. A tentative identification can be assigned provided that
relative intensities of major ions in the library reference spectrum are present in the
sample spectrum and the relative intensities agree within ±20%.
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13.12 Quantitative Analysis
The quantitation of identified compounds is based on the integrated abundance of the
extracted ion current profile of the primary characteristic ion(s). The internal standard
used for quantitation is the one nearest to the retention time of the analyte.
The average response factors from the initial calibration are used to calculate the
concentration of each compound in the sample. See References 14.1 and 14.2 for the
equations describing internal standard calibration.
14 Quality Control
Quality control procedures for the air sampling operations include the following item.
Please refer to the Chemistry Section Quality Manual for the laboratory to gain a broader
prospective.
●A site sampling plan must be prepared and available.
●All data must be documented on site log books, field data sheets and chain-ofcustody forms.
●Equipment evaluation and calibration must occur and be documented according to
procedures.
●The GC/MS system must be tuned to meet the BFB specifications.
●Blank or “zero air” samples must be analyzed at a frequency of no less than 5% of
the samples.
●LFBs and matrix spikes must be analyzed at a frequency of no less than 5% of the
samples.
●The laboratory must analyze a duplicate matrix spike sample for every 20 samples
analyzed.
●The accuracy (% Recovery) and precision (%RPD) are calculated for every pair of
spikes and a statistical analysis is performed quarterly on the last 20 points to
calculate and update the quality control tables in the LIMS. The control limits are
then set at R +/- 3s, where R is the average of %Recovery (for precision it is the
average of %RPD) and s is the standard deviation. Appropriate corrective measures
must be taken if the analyte recoveries or RPDs are outside of these limits and the
affected samples must be reanalyzed. The spike recoveries and statistical analysis
are uploaded into the LIMS and printed in the final report for the job.
●Evaluation of retention time windows to ensure that all compounds are detected
within their respective time windows and meet the ± 6 second requirement
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●For more specific information regarding QA/QC measures see the TO-14A and
TO-15 EPA Methods and SOP VO-001.
15 Data Processing, Review and Reporting
15.1 Data Processing
The Quality Control Manager module in the LIMS is used for data processing. The data
processing steps include such operations as converting raw instrument data, loading raw
files into the QC-Manager, performing data calculation, and uploading into the LIMS.
The software program is designed to take a significant amount of information from the
data file including the raw data, sample name, sample type and dilution factor.
Start QC Manager and Load File: Load the QC Manager program within the LIMS and
choose the laboratory instrument on which the data was collected. Load the .RAW file to
be reviewed by choosing the Open option from the Files menu, select the desired .RAW
filename, and click OK.
Review the TYPE and DILUTION FACTOR columns of the sample table to verify that
the QC Manager program set them correctly, when necessary make appropriate
selections:
The TYPE column is used to define sample type. Use the following guidelines to set the
TYPE if necessary:
SAMP - Type used for ordinary samples. Assign this type to all samples that do not fit in
another category.
SRM - Assign this type to all Standard Reference Materials solutions.
CCV - Assign this type to all Continuing Calibration samples.
REPL - Assign this type to duplicate and replicate samples.
SPK - Assign this type to spiked samples.
MDL - Assign this type to all reagent blank samples.
NONE - Assign this type to samples where calculations are not desired.
The DILUTION FACTOR column should contain the dilution factors used by the
instrument. Correct the DILUTION FACTOR when necessary.
Select SPIKE CODES, SPIKE FACTORS, LIMS TESTS, MATRIX, BATCH ID;
WEIGHT FACTORS and PREPARATION VOLUME:
LIMS TEST ID and MATRIX: Edit the LIMS Test ID for the samples to match the test
requested (W-VOC-MS or W-VOC-MS-A, for example), then enter the Matrix when
prompted.
Batch Assignments: A batch is a group of samples including precision and spike recovery
samples and all of the associated samples analyzed together by the same method.
Highlight the samples and click the header box on the BATCH column to assign a batch
ID to that batch.
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Spike Code: Assign the appropriate spike code for the spikes by highlighting all spikes
that used a common spike stock solution and clicking on the Spike Code header box and
choosing the correct code.
Spike Factor: Assign spike factors to spiked samples to reflect the amount of spike added
to the sample. For instance, a normal spike level as given in the spike tables would have
a spike factor of ‘1’.
Weight Factors: This is not used for water or air samples, but is entered using the % dry
weights for soils and is entered on a wet weight basis for waste samples.
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