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

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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

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    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
                                                                    1/85

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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

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                                                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
   ^- fu
   oo in
   en 
     cr>

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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.
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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.
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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
                                                                 1/85

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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
                                                                   1/85

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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.
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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
                                                                   1/85

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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
                                                                   1/85

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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.

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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

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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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22

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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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