vvEPA
United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
DIRECTIVE NUMBER: 9235.2-03
TITLE: FIELD STANDARD OPERATING PROCEDURES MANUALS: FSOP
. AIR SURVEILLANCE
APPROVAL DATE: oi/oi/85
EFFECTIVE DATE: 01/01/85
ORIGINATING OFFICE: Office of Solid Waste
0 FINAL
D DRAFT
STATUS:
REFERENCE (other documents):
OSWER OSWER OSWER
/£ DIRECTIVE DIRECTIVE Di
-------
03/19/87 United States Environmental Protection Agency
Washington, D.C. 20460
EPA OSWER Directive Initiation Request
2. Originator Information
Name of Contact Person Mail Code Offlca
DORRLER . OERR/HRSD/
1. Directive Number
9285.2-03
Telephone Number
340-6470
3. Title
FIELD STANDARD OPERATING PROCEDURES MANUALS: FSOP #8 -
AIR SURVEILLANCE
4. Summary of Directive (Include brief statement of purpose)
Provides air monitoring procedures that field
personnel can use to obtain the data needed to
minimize the risk of exposure to hazardous
substances. (1/85, 33 pp) w.
5. Keywords
SUPERFUND, CERCLA, SITE SAFETY, EMPLOYEE HEALTH
PROCEDURES
6a. Does this Directive Supercede Previous Directives)?) | yes | ^ No
b. Does it Supplement Previous Dlrectlves(s)? | | yes 1 X NO What
7. Draft Level ' . • .
A-SlgnedbyAA/DAA B - Signed by Office Director C- For Review «
This Request Meets OSWER Directives System Format
8. Signature of Lead Office Directives Coordinator
9. Name and Title of Approving Official
HEDEMAN
AND SAFETY
What directive (number, title)
directive (number, title)
i
i Comment In Development
Date
Date
01/01/85
OSWER OSWER OSWER
DIRECTIVE DIRECTIVE
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OSWER Directive 9285-2-03
FIELD STANDARD OPERATING PROCEDURES
FOR
AIR SURVEILLANCE*
F.S.O.P. 8
U.S. ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF EMERGENCY'AND REMEDIAL RESPONSE
HAZARDOUS RESPONSE SUPPORT DIVISION
WASHINGTON, D.C. 20460
-------
The mention of trade names or commercial products in this manual is
for illustration purposes and does not constitute endorsement or
*•'
recommendation for use by the Environmental Protection Agency.
Contents of this manual do not necessarily reflect the views and
policies of the Environmental Protection Agency.
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TABLE OF CONTENTS
I. INTRODUCTION
Objectives 1
Background 1
Brier Description of Air Surveillance 1
Types of Incidents 1
General Surveillance Methods 2
II. EQUIPMENT '4
Equipment for Air Surveillance and Sampling 4
III. FLOW CHART for AIR SURVEILLANCE „. 5
IV. PROCEDURE for ON-SITE AIR SURVEILLANCE 6
V. U.S. ENVIRONMENTAL PROTECTION AGENCY, ENVIRONMENTAL 9
RESPONSE TEAM'S GENERIC ASBESTOS AIR MONITORING
GUIDES FOR HAZARDOUS WASTE SITES :
VI. PROCEDURES FOR WELL HEADSPACE SURVEILLANCE .10
Direct Pull Technique 11
Water Sample Headspace Technique 12
VII. PSCAM 127 • 13
VIII BLANK SITE WORK MAP : 23
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SECTION I
INTRODUCTION
1/85
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F.S.O.P. #8
PROCESS: AIR SURVEILLANCE
I. Objectives
This document provides air monitoring procedures that field
personnel can use to obtain the data needed to minimize the risk of
exposure to hazardous substances.
II. Background
These procedures have been derived by reorganizing the U.S.
Environmental Protection Agency, Office of Emergency and Remedial
Responses, (U.S. EPA, OERR), Washington, DC. "Standard Operating
Safety Guides", November 1S84, to a format more appropriate for use
in the field at hazardous material, air, spill, and well monitoring
responses. *
III. Brief Description of Air Surveillance
1. Personnel entering sites of hazardous substance incidents must use
adequate safety precautions to minimize exposure to contaminants
which may have health effects. These safety precautions encompass
both monitoring methodologies used to characterize site hazards as
well as personal protective equipment and procedures (refer to FSOP
#4 and #7 'for Site Entry/Decon). Air monitoring is one of the first
methods of gaining important information on site hazards. From
initial monitoring surveys, decisions for appropriate levels of
protection may be based.
Air surveillance is accomplished using direct reading instruments
and air sampling (collecting air on suitable media followed by
analysis) in order to determine the type and quantity of airborne
contaminants present during the incident. Information gained by
these means can also be used to help characterize water pollution.
(This procedure is described in Section VI, Page 16, Procedures for
Air Monitoring in Well Headspace.) •
2. Types of Incidents
Two general types of incidents are encountered:
Environmental emergencies, including chemical fires, spills, or
other releases of hazardous substances which occur over a
relatively short period of time. Air sampling generally is
limited unless the release continues long enough for appropriate
equipment to be brought in and you can afford to wait for the
analyses of the samples.
Longer-term cleanup, including planned removals and remedial
actions at abandoned waste sites, as well as restoration after
emergency problems have been controlled. During this period,
especially at waste sites, workers and the public may be exposed
to a wide variety of airborne materials over a much longer
Page 1
1/85
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F.S.O.P. No. 8
period of time. Air sampling can usually be used in those
situations.
3. General Surveillance Methods .
During site operations, data are needed about air contaminants and
any changes that may occur in air quality. Air sampling and
subsequent analysis is the most informative method of evaluating air
contaminants but is costly and time consuming. Direct reading
instruments (DRI) can be used to provide approximate total
concentrations and detect many organics and a few inorganics.
Caution must be taken, however, when using these instruments. .Under
certain conditions the data obtained can be grossly misinterpreted.
To obtain air quality data rapidly at tflfe site, instruments
utilizing flame ionization detectors (FIDs) and photoibnization
detectors (PIDs) can be used. These may be used as survey
instruments (total concentration mode) or operated as gas
chromatographs (gas chromatograph mode). As gas chromatographs,
these instruments can provide real-tine, qualitative/quantative data
when calibrated with standards of the air contaminants, if known.
Combined with selective laboratory analysis of samples, these field
gas chromatographs provide a tool for evaluating airborne organic
hazards on a real-time basis at a lower cost than taking and
analyzing all the samples needed to get the same amount of data.
For more complete information about air contaminants, measurements
obtained with direct reading instruments must be supplemented by
collecting and analyzing air samples. To assess air contaminants
more thoroughly, air sampling devices equipped with appropriate
collection media are placed at various locations (sampling stations)
throughout the area. These samples provide air quality information
for the period of time they operate, and can indicate contaminant
types and concentrations over the lifetime of site operations if
continuously operated. In addition to air samplers, direct reading
instruments equipped with recorders can be operated continuously.
Area sampling stations are located in various places as described in
Table 8-1.
Accurate calibration of air surveillance equipment is required in
order to have confidence in the resultant data. As a minimum, the
system should be calibrated before and after use. The system should
also be calibrated periodically during use. The overall frequency
of calibration will depend upon the general handling and use of a
given sampling system.
Page 2
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F.S.O.P. No. 8
Table 8-1
Sampling Station Location
Location
1. Upwi nd
2. Support Zone
3. Contamination Reduction Zone
4. Exclusion Zone
5. Downwi nd
Rationale
Establish background air contaminant
levels
Ensure that command post and other
support facilities are located in a
"clean" area
*
Ensure that decontamination workers are
properly protected and that on-site
workers are not removing protective gear
in a contaminated area
Verify and continually confirm and
document selection of proper levels of
worker protection as well as provide
continual record of a.fr contaminants
Indicate if any air contaminants are
leaving the site.
Page 3
1/85
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SECTION II
EQUIPMENT^
FOR
AIR SURVEILLANCE
1/85
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F.S.O.P. No. 8
PROCESS: Equipment Surveillance
III. Equipment
At present, the following equipment is used for organic gas/vapor
monitoring. However, other equivalent equipment can be substituted;
- Photo lonization Detectors (PID)
- Organic Vapor Analyzers (FID)
- 5 - 200 cc/min personal sampling pumps
- 0.5-3 L/min personal .sampling pumps
- Tenax adsorption (metal) tubes
- Carbon sphere adsorption (metal) tubes
- Carbon-packed (glass) adsorption tubes
(150 milligram and 600 milligram sizes)
- Florisi 1-packed (glass) adsorption tilbes
(150 milligram size)
- Real-time Aerosol Monitors
- Colorimetric Detection tubes
- Silica-packed (glass) adsorption tubes
Table II
Compounds and Collection Media
Compound
Possible Collection Media
Organic Vapors w/bp above 0°C
High M.W. hydrocarbons,
organophosphorous compounds,
and certain pesticides vapors
Aromatic Amines
PCBs
Inorganic Gases
Aerosols
Known specific compound
Activated Carbon Tube (P+CAM 127)*
Tenax or Chromasorb
Silica gel tube (P+CAM 168)*
Florisi 1 Tube (P+CAM 253)*
Silica gel tube (P+CAM 339)**
Particulate filter (glass fiber or
membrane type)
Colorimetric detector tube
- P+CW 127 *
P+CAM 168
P+CAM 253
- P+CAM 339 **
NIOSH Manual of
Analytical Methods
Volume 1, April, 1977
NIOSH Manual of Analytical
Methods Volume 7, August, 1981
Page 4
1/85
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SECTION III
•
FLOW CHART
FOR
AIR SURVEILLANCE
1/85
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F.S.O.P. No. 8
PROCESS AIR SURVEILLANCE
Generic Procedural Steps
Wind Direction
DETERMINE CONTAMINANTS
LEAVING SITE
COLLECT DUPLICATES OF STEP 3
POSITIVES FOR OFF SITE ANALYSIS
EXCLUSION
ZONE
3 COLLECT AREA SAMPLES
(THERMAL TUBES FOR SCREENING)
DETERMINE CONCENTRATION ON-SITE
CONTAMINATION
REDUCTION
ZONE
SUPPORT ZONE
1 DETERMINE BACKGROUND
CONCENTRATIONS
Page 5
1/85
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SECTION IV
PROCEDURES
FOR
ON-SITE AIR MONITORING
Note: This procedure is generally applicable to most
responses, but may need to be modified for specific
responses.
1/85
-------
FIELD STANDARD OPERATING PROCEDURES
:SOP NO: 8
'ROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
DERATING PROCEDURES
STEP SEQUENCE
INFORMATION/OPERATING GOALS/SPECIFICATIORS
janic Vapor Surveillance
GUIDE/NOTES
<
isures Taken
Step 1:
Determine Background
Concentratibns
Step 2:
Determine On-site
Concentrations
Step 3: Collect Area Samples
Take background readings of total organic gases
and vapors using direct reading instruments
(Fin/PID) upwind of site (in areas not expected to
contain air contaminants). Be sure that sources
such as highways and industries do not affect
results. Additional monitoring may be necessary in
areas adjacent to the site to determine
concentrations leaving the site.
Monitor on-site area at both ground and breathing
zone levels on initial walk through. This is to
determine general ambient concentrations and to
locate "hot spots". Record concentrations on a site
map. Perform additional morrftoring to thoroughly
define hot spots.
Locate sampling stations throughout the site.
Consider factors such as hot spots, active work
areas, and weather conditions. Routinely,
two/four-hour samples are collected in morning and
afternoon using personal sampling pumps equipped
with Tenax and/or carbon sphere thermal desorption
tubes to be analyzed by G.C. Determine total
gas/vapor concentration.
»-• "O
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FIELD STANDARD OPERATING PROCEDURES
FSOP NO:
PROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
I OPERATING PROCEDURES
STEP SEOUENCE
INFORMATION/OPERATING GOALS/SPECIFICATIONS
TRAINING
GUI DEMOTES
Organic vapor Surveillance
Measures Taken
Step 4:
On-site
Analysis
Desorb samples with a thermal desorber and analyze
on a Gas Chromatograph for total organic
concentration and number of peaks. Compare
chromatograms from various stations and times for
information concerning air contaminant patterns. If
high concentrations are acquired during initial DRI
surveys, samplers equipped with carbon collection
tubes to be sent out for analysis are run next to
field-analyzed Tenax/carbon sphere samplers. These
tubes are then to be analyzed by an AIHA accredited
laboratory for identification and quantification of
contaminants.
CO IO
en CD
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FIELD STANDARD OPERATING PROCEDURES
FSOP NO:
PROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
OPERATING PROCEDURES
STEP SEQUENCE
INFOBMATIOM/OPEftATING GOALS/SPECIFICATIONS
TRAIHIHG
GUIOFVNOTES
Organic Vapor Surveillance
Measures Taken
Step 5: Identify Specific
Contaminants
Run personal monitoring pumps w/glass media
collection tubes concurrent with Tenax/carbon tube
equipped samplers after hot spots have been
confirmed. When only a few peaks are seen in the
previous onsite G.C. analysis, 100-150 mg glass
carbon tubes are used to collect 30-50 liters of air
(flow rate = 100-500cc/minute). When many peaks are
detected, 600 mg glass carbon columns are operated
at 0.5-1 liter/min. to collect 90-150 liters of
air. At some stations you may wish to run several
tubes at different flow rates to determine the
optimum flow rate. Samples collected every 3rd and
5th day are analyzed by an AIHA accredited
laboratory using the appropriate NIOSH P+CAM
method.' For outdoor sampling, flow rates are
generally increased slightly. The remaining samples
are placed in refrigerated storage. One should
check with the laboratory performing the analysis to
determine the appropriate maximum length for
refrigerated storage. These can be analyzed at a
later time if 3rd and 5th day samples indicate
chanqes in air contaminant patterns.
OOtQ
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FIELD STANDARD OPERATING PROCEDURES
FSOP NO:
8
PROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
OPERATING PROCEDURES
STEP SEQUENCE
INFORMATION/OPERATING GOALS/SPECIFICATIONS
TRAINING
GUIHE/NOTES
)rganic Vapor Surveillance
leasures Taken
Step 6: Determine Contaminants
Leaving The Site
Step 7: Determine The Need
To Monitor For
Participates
Take additional DRI readings downwind of site to
determine whether any contaminants are actually
leaving the site.
Based on conditions and contaminants found,
determine If there Is a need to monitor for
partlculates. Incidents where partlculates might be
present are: pesticide or chemical fires.
situations Involving heavy metals, arsenic or
cyanide compounds and mitigation operations that
create dust (I.e., excavation of contaminated
soil). Sampling media and analytical methods for
these air contaminants should follow guidance given
In the NIOSH Manual of Analytical Methods (Vol.
'1-7). In addition, field real-time aerosol
instruments are available which may assist in
determining the level of particulates present.
OOU3
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vo
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SECTION V
ASBESTOS AIR MONITORING
NOTE: Contact the U.S. Environmental Protection Agency,
Environmental Response Team (201) 321-6740 or FTS 340-6740
to obtain a copy of the latest procedure for asbestos air
monitoring for hazardous waste sites.
Page 10
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SECTION VI
it
PROCEDURES
FOR
AIR SURVEILLANCE
IN
WELL HEADSPACE
1/85
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F.S.O.P. No. 8
PROCESS: Air Surveillance
The objective of these headspace monitoring procedures is:
1) To establish safety procedures to be enforced for personnel working
at the well.
2) To obtain some gross measure of what contaminants are in the well.
3) To allow for the development of a site-specific relative
concentration measure (i.e., if well "A has 100 ppm of benzene in
the headspace and 250 ppm in the water, and well "B" has a similar
headspace concentration, then it may have similar concentrations in
the water).
The following is an outline of procedures use,d to monitor headspace in
wells. While the procedures may seem straightforward, there are^a.number
of factors which need be considered when evaluating results. These
include: 1) Cap design - whether vented or non-vented, threaded or slip
on, or if a cap exists at all. 2) Location - is the well located in a
windy area, shade, or direct sunlight? What is the proximity to roadways
or railways, rivers, ponds, recharge basins? 3) Well construction -
what is the well diameter? Where is the top of the screen relative to
the water level? What is the distance from top of casing to water
level? 4) Well condition and use - is it a domestic or supply well?
What*is the pumping schedule? Are there pumps, wiring, piping etc. in
the well? If a monitoring well, wh&n was it last evacuated and sampled?
These factors should be considered and accounted for when evaluating
results.
Page 11
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FIELD STANDARD OPEPATING PROCEDURES
FSOP NO:
PROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
OPERATING PROCEDURES
STEP SEQUENCE
INFORMATION/OPERATING GOALS/SPECIFICATIONS
TRAINING
GUIDE/NOTES
irect Pull Technique
easures Taken
Step 1: Approach Wei 1
Step 2: Remove Caps
Step 3: Evacuate Well
Step 4: Determine Water
Level
Step 5: Lower Sampling
Hose or Probe .
Step 6: Determine Presence
of H2S
Step 7: Evaluate Results
Approach well from upwind side, (w/appropriate
safety equipment)
Remove outer and inner caps from well orifice.
Evacuate well three times.
Using a flashlight or mirror, determine
approximate water level.
Lower tube 1 foot above water surface and draw
sample.
If looking for Hj>S, lower, appropriate detector
tube into well, draw sample* and analyze tube.
Consider aforementioned factors and how they may
have affected results obtained.
00 UD
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FIFLD STANDARD OPERATING PROCEDURES
FSOP MO:
PROCESS: AIR SURVEILLANCE
Prepared by:
Approved by:
Date:
OPERATING PROCEDURES
STEP SEQUENCE
INFORMATION/OPERATING GOALS/SPECIFICATIONS
TRAINING
GUIPF/NOTES
s. 01
OO UD
in <\>
Step 1: Approach Wei 1
Step 2: Remove Caps
Step 3: Determine Water Level
Step 4: Evacuate Well
Step 5: Lower Bailer
Step 6: Prepare to Withdraw
Sample
Step 7: Remove Bailer
Step 8: Remove Contents
of Bailer
Step 9: Cap and Shake
Step 10: Sample Headspace
Step 11: Evaluate Results
Approach well from upwind side.(w/appropr1ate safety
equipment)
Remove outer and Inner caps from well oraflce.
Measure water level.
Evacuate well 3 times.
Slowly lower narrow diameter bailer to center of
screened area.
Raise and lower (approximately 3-4 feet, but not
exceeding 1/2 screen length) 3 times.
Raise bailer slowly and steadily out of well.
•
Pump from mid length of bailer into a 1 liter
or VOA bottle. Fill halfway.
Cap bottle and shake vigorously for 10 seconds.
(Ambient temperature range 60°F+.)
Insert probe or tube into headspace of sample (3
inches) using gloved hand to seal. If It is to be
analyzed by G.C., insert sampling needle through cap
and draw sample. Inject sample into sample port on
G.C. (must be VOA bottle).
Consider aforementioned factors and how they may
have affected results obtained.
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SECTION VII
P4CAM 127
1/85
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3.3 It must be emphasized that any compound which has the same retention
time as the specific compound under study at the operating conditions
described in this method is an interference. Hence, retention time
data on a single column, or even on a number of columns, cannot be
considered as proof of chemical identity. For this reason it is
important that a sample of the.bulk solvents(s) be submitted at the
same time so that identity(ies) can be established by other means.
3.4 If the possibility of interference exists, separation conditions
(column packing, temperatures, etc.) must be changed to circumvent
the problem.
4. Precision and Accuracy
4.1 The mean relative standard deviation of the analytical method is 8%
(11.4).
*•
4.2 The mean relative standard deviation of the analytical method plus
field sampling using an approved personal sampling pump is 10%
(11.4). Part of the error associated with the method is related to
uncertainties in the sample volume collected. If a more powerful
vacuum pump with associated gas-volume integrating equipment is used,
sampling precision can be improved.
4.3 The accuracy of the overall sampling and analytical method is 10%
(NIOSH-unpublished data) when the personal sampling pump is
calibrated with a charcoal tube in the line.
5. Advantages and Disadvantages of the Method
5.1 The sampling device is small, portable, and involves no liquids.
Interferences are minimal, and most of those which do occur can be
eliminated by altering chromatographic conditions. The tubes are
analyzed by means of a quick, instrumental method. The method can
also be used for the simultaneous analysis of two or more solvents
suspected to be present in the same sample by simply changing gas
chromatographic conditions from isothermal to a temperature-
programmed mode of operation.
5.2 One disadvantage of the method is that the amount of sample which can
be taken is limited by the number of milligrams that the tube will
hold before overloading. When the sample value obtained for the
backup section of the charcoal tube exceeds 25% of that found on the
front section, the possibility of sample loss exists. During sample
storage, the more volatile compounds will migrate throughout the tube
until equilibrium is reached (33% of the sample on the backup
section).
5.3 Furthermore, the precision of the method is limited by the
reproducibility of the pressure drop across the tubes. This drop
will affect the flow rate and cause the volume to be imprecise,
because the pump is usually calibrated for one tube only.
Page 15
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6. Apparatus
6.1 .An approved and calibrated personal sampling pump for personal
samples. For an area sample, any vacuum pump whose flow can be
determined accurately at 1 liter per minute or less.
6.2 Charcoal tubes: glass tube with both ends flame sealed, 7 cm long
w.ith a 6-mm O.D-. and 4-mrn I.D., containing 2 sections of 20/40 mesh
activated charcoal separated by a 2-mrn portion of urethane foam. The
activated charcoal is prepared from coconut shells and is fired at
600°C prior to packing. The absorbing section contains 100 mg of
charcoal, the backup section 50 mg. A 3-mm portion of urethane foam
is placed between the outlet end of the tube and the backup section.
A plug of silyated glass wool is placed in front of the absorbing
section. The pressure drop across the tube must be less than one
inch of mercury at a flow rate of 1 liter pm.
6.3 Gas chrdmatograph equipped with a flame ibnization. detector.
6.4 Column (20 ft X 1/8 in.) with 10% FFAP stationary phase on 80/100
mesh, acid-washed DMCS Chromosorb W solid support. Other columns
capable of performing the required separations may be used.
6.5 A mechanical or electronic integrator or a recorder and some method
for determining peak area. . :
6.6 Microcentrifuge tubes, 2.5 ml, graduated.
6.7 Hamilton syringes^ 10 uL, and convenient sizes for making standards.
6.8 Pi pets: 0.5-mL delivery pi pets or 1.0-mL type graduated in 0.1 -mi
increments.
6.9 Volumetric flasks: 10 ml or convenient sizes for making standard
solutions.
7. Reagents
7.1 Spectro quality carbon disulfide (Matheson, Coleman, and Bell).
7.2 Sample of the specific compound under study, preferrably
chromatoquality grade.
7.3 Bureau of Mines Grade A helium.
7.4 Prepurified hydrogen.
7.5 Filtered compressed air.
Page 16
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8. Procedure
8.1 Cleaning of Equipment: All glassware used for the laboratory
analysis should be detergent washed and thoroughly rinsed with tap
water and distilled water.
8.2 Calibration of Personal Pumps. Each personal pump must be calibrated
with a representative charcoal tube in the line. This will minimize
errors associated with uncertainties in the sample volume collected.
8.3 Collection and Shipping of Samples
8.3.1 Immediately before sampling, the ends of the tube should be
broken to provide an opening at least one-half the internal
diameter of the tube (2 mm).
8.3.2 The small section of charcoaj is used as a back-up and should
be positioned nearest the sampling pump.
8.3.3 The charcoal tube should be vertical during sampling to
reduce channeling through the charcoal.
8.3.4 Air being sampled should not be passed through any hose.or
tubing before entering the charcoal tube.
8.3.5 The flow, time, and/or volume must be measured as accurately
as possible. The sample should be taken at a flow rate of 1
liter per minute or less to attain the total sample volume
required. The minimum and maximum sample volumes quoted must
be collected if the desired sensitivity is to be achieved.
8.3.6 The temperature and pressure of the atmosphere being sampled
should be measured and recorded.
8.3.7 The charcoal tube should be capped with the supplied plastic
caps immediately after sampling. Under no circumstances
should rubber caps be used.
8.3.8 One tub should be handled in the same manner as the sample
tube (break, seal, and transport), except that no air is
sampled through this tube. This tube should be labeled as a
blank.
8.3.9 Capped tube should be packed tightly before they are shipped
to minimize tube breakage during shipping.
8.3.10 Samples of the suspected solvent(s) should be submitted to
the laboratory for qualitative characterization. These
liquid bulk samples should not be transported in the same
container as the samples or blank tube. If possible, a bulk
air sample (at least 50 liters of air drawn through tube)
should be shipped for qualitative identification purposes.
Page 17
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8.4 Analysis of Samples
8.4.1 Preparation of Samples. In preparation for analysis, each
charcoal tube is scored with a file in front of the first
section of charcoal and broken open. The glass wool is
removed and discarded. The charcoal in the first (larger)
section is transferred to a small stoppered test tube. The
separating section of foam is removed and discarded; the
second section is transferred to another test tube. These
two sections are analyzed separately.
8.4.2 Desorption of Samples. Prior to analysis, one-half ml of
carbon disulfide is pipetted into each test tube. (All work
with carbon disulfide would be performed in a hood because of
its high toxicity.) Tests indicate that desorption is
complete in 30 minutes if the sample is stirred occasionally
during this period. «
8.4.3 GC Conditions. The typical operating conditions for the gas
chromatograph are:
1. 85 cc/min. (70 psig) helium carrier gas flow.
2. 65 cc/min. (24 psig) hydrogen gas flow to detector.
3. 500 cc/tain. (50 psig) air flow to detector.
4. 200°C injector temperature.
5. 200°C manifold temperature (detector).
6. Isothermal oven or column temperature - refer to Table 1
for specific compounds.
8.4.4 Injection. The first step in the analysis is the injection
of the sample into the gas chromatograph. To eliminate
difficulties arising from blowback or distillation within the
syringe needle, one should employ the solvent flush injection
technique. The 10 uL syringe is first flushed With solvent
several times to wet the barrel and plunger. Three
microliters of solvent are drawn into the syringe to increase
the accuracy and reproducibility of the injected sample
volume. The needle is removed from the solvent, and the
plunger is pulled back about 0.2 uL to separate the solvent
flush from the sample with a pocket of air to be used as a
marker. The needle is then immersed in the sample, and a
5-uL aliquot is withdrawn, taking into consideration the
volume of the needle, since the sample in the needle will be
completely injected. After the needle is removed from the
sample and prior to injection, the plunger is pulled back a
short distance to minimize evaporation of the sample from the
tip of the needle. Duplicate injections of each sample and
standard should be made. No more than a 3% difference in
area is to be expected.
8.4.5 Measurement of area. The area of the sample peak is measured
by an electronic integrator or some other suitable form of
Page 18
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area measurement, and preliminary results are read from a
standard curve prepared as discussed below.
8.5 Determination of Desorption Efficiency
8.5.1 Importance of determination. The desorption efficiency of a
particular compound can vary from one laboratory to another
and also from one,batch of charcoal to another. Thus, it is
necessary to determine at least once the percentage of the
specific compound that is removed in the desorption process
for a'given compound, provided the same batch of charcoal is
used. NIOSH has found that the desorption efficiencies for
the compounds in Table 1 are between 81% and 100% and vary
with each batch of charcoal.
8.5.2 Procedure for determining desorption efficiency. Activated
charcoal equivalent to the aipount in the first section of the
sampling tube (100 mg) is measured into a 5-cm, 4-mm I.D.
glass tube, flame sealed at one end (similar to commerically
available culture tubes). This charcoal must be from the
same batch as that used in obtaining the samples and can be
obtained from unused charcoal tubes. The open end is capped
with Parafilm. A known amount of the compound is injected
directly into the activated charcoal with a microliter
syringe, and the tube is capped with more Parafilm. The
amount injected is usually equivalent to that present in a
10-liter sample at a concentration equal to the Federal
standard.
At least five tubes are prepared in this manner and allowed
to stand for at least overnight to assure complete absorption
of the specific compound onto the charcoal. These five tubes
are referred to as the samples. A parallel blank tube should
be treated in the same manner except that no sample is added
to it. The sample and blank tubes are desorbed and analyzed
in exactly the same manner as the sampling tube described in
Section 8.4.
Two or three standards are prepared by injecting the same
volume of compound into 0.5 ml of C$2 with the same syringe
used in the preparation of the samples. These are analyzed
with the samples.
The desorption efficiency equals the difference between the
average peak area of the samples and the peak area of the
blank divided by the average peak of the standards, or
Desorption Efficiency s Area sample - Area blank
Area Standard
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9. Calibration and Standards
It is convenient to express concentration of standards in terms of mg/0.5
ml C$2 because samples are desorbed in this amount of CS2- T°
minimize error due to the volatility of carbon disulfide, one can inject
20 times the weight into 10 mL of C$2. For example, to prepare a 0.3
mg/0.5 ml standard, one would inject 6.0 mg into exactly 10 ml of CSg in
a glass-stoppered flask. The density of the specific compound is used to
convert 6.0 mg into microliters for easy measurement with a microliter
syringe.- A series of standards, varying in concentration over the range •
of interest, is prepared and analyzed under the same GC conditions and
during the same time period as the unknown samples. Curves are
established by plotting concentration in mg/0.5 ml versus peak area.
NOTE: Since no internal standard is used in the method, standard
solutions must be analyzed at the same time that the sample analysis is
done This will minimize the effect of known day-to-day variations and
variations during the same day of the FID response.
10. Calculations
10.1 The weight, in mg, corresponding to each peak area is read from the
standard curve for the particular compound. No volume corrections
are needed, because the standard curve is based on mg/0.5 ml C$2
and the volume of sample is identical to the volume of the standards
injected.
10.2 Corrections for the blank must be made for each sample.
Correct mg = mgs - mg0
where:
mgs = mg found in front section of sample tube
mgjj = mg found in front section of blank tube
A similar procedure is followed for the backup sections.
10.3 The corrected amounts present in the front and backup sections of the
same sample tube are added to determine the total measured amount in
the sample.
10.4 This total weight is divided by the determined desorption efficiency
to obtain the corrected mg per sample.
10.5 The concentration of the analyte in the air sampled can be expressed
in mg per m3.
mg/m3 » Corrected mg (Section 10.4) X 1000 (1iters/m3)
Air volume sampled (liters)
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10.6 Another method of expressing concentration is ppm (corrected to
standard conditions of 25°C and 760 mm Hg).
ppm = mg/m3 X 24.45 X 76£ X (T + 273)
MW P "793
where :
P s pressure (mm Hg) of air sampled
T = temperature (°C) of air sampled
24.45 = molar volume (liter/mole) at 25°C and 760 mm Hg
MW = molecular weight
760 = standard pressure (mm Hg)
298 = standard temperature (K)
11. References
tf
11.1 White, L. D., D. G. Taylor, P. A. Mauer, and R. E. Kupel , "A
Convenient Optimized Method for the Analysis of Selected Solvent
Vapors in the Industrial Atmosphere", Am. Ind. Hyg. Assoc. J. ,
31:225, 1970.
11.2 Young, D. M. and A. D. Crowell , Physical Adsorption of Gases, pp.
137-146, Butterworths, London, 1 962. "
11.3 Federal Register. 37:202:22139-22142. October 18, 1972.
11.4 NIOSH Contract HSM -99-72-98, Scott Research Laboratories, Inc.,
"Collaborative Testing of Activated Charcoal Sampling Tubes for
Seven Organic Solvents", pp. 4-22, 4-27, 1973.
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Table 1 :
Parameters Associated With P&CAM Analytical Method No. 127
Organic Solvent
Acetone
Benzene
Carbon Tetrachloride
Chloroform
Dlchloromethane
p-Oloxane
Ethyl ene Dlchlorlde
Methyl Ethyl Ketone
Styrene
Tetrachl oroethyl ene
1 ,1 ,2-Trlchloroethane
1 , 1 , 1 -Trf chl oroethane
(Methyl Chloroform)
Trl chl oroethyl ene
Toluene
Xylene
Method
Classification
0
A
A
A
D
A
D
B
0
B
B
B
A
B
A
Detection Limit
(mg/sample)
— ^
0.01
0.20
0.10
0.05
0.05
0.05
0.01
0.10
0.06
0.05
0.05
0.05
0.01
0.02
Sample Volume (liters)
Mlnimum(a) Maximum(b)
' 0.5
0.5
10
0.5
": 0.5
1
1
0.5
- 1.5
1
10
0.5
1
0.5
' 0.5
7.7
55
60
13
3.8
18
12
13
34
•25
97
13
17
22
31
GC Column
Temp. (OC)
60
90
60
80
85
100
90
80
150
130
150
150
90
120
100
Moleci
Weigf-
58.
78.
154.
119
84.
88.
99.
72.
104
166
133
133
131
92.
106
(a) Minimum volume, in liters, required to measure 0.1 times the OSHA standard.
(b) These are breakthrough volumes calculated with data d'erived from the potential plot (11.2:
for activated coconut charcoal. Concentrations of vapor In air at 5 times the OSHA stand;
(11.3) or SCO ppm, whichever Is lower, 25°C, and 760 torr were assumed. These values will
be as much as 50S lower for atmospheres of high humidity. Th effects of multiple
contaminatns have not been Investigated, but ft is suspected that less volatile compounds
displace more volatile compounds (See 3.1 and 3.2).
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SECTION VIII
BLANK SITE WORK MAP
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SITE WORK MAP
The preparation of a site map Is an essential task when sampling an area where
existing maps are not available. The map, when finished, will yield sample
point Information such as compass direction, street addresses, grid system
orientations as well as environmental features. A site map will also enable
the sampler to relate discreet analytical data points to the overall site
contamination at the time sampling had been performed. Maps are useful in
report writing, plume construction, and future sampling investigations at the
site.
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EXCLUSION AREA
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