MIDWEST RESEARCH INSTITUTE
ASSESSMENT OF AIRBORNE EXPOSURE AND DERMAL CONTACT
TO ACRYLAMIDE DURING CHEMICAL GROUTING OPERATIONS
QUALITY ASSURANCE PROJECT PLAN
foe the
Office of TOXIC Substances
EPA Priire Contract No. 68-02-3933
Work Assignment No. 47
MRI Project No. 3501-A(47)
her
U.S Environmenta"! Protection Agency
Office of Toxic Substances
Field Studies Branch, TS-7S8
401 M Street, S.W.
Washington, O.C. 2C460
Attn: Mr. Tom Murr^v
MIDWEST RESEARCH INSTITUTE 425 VOLKER BOULEVARD. KANSAS CITY. MISSOURI 64110 • 816 753-7600
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ASSESSMENT OF AIRBORNE EXPOSURE AND DERMAL CONTACT
TO ACRYLAMIDE DURING CHEMICAL GROUTING OPERATIONS
QUALITY ASSURANCE PROJECT PLAN
for the
Office of Toxic Substances
EPA Prime Contract No. 68-02-3938
Work Assignment No. 47
MRI Project No. 8501-A(47)
For
U.S Environmental Protection Agency
Office of Toxic Substances
Field Studies Branch, TS-798
401 M Street, S.W.
Washington, D.C. 20460
Attn: Mr. Tom Murray
MIDWEST RESEARCH INSTITUTE 425 VOLKER BOULEVARD, KANSAS CITY, MISSOURI 64110-816 753-7600
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Section No.: 1.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 1
SECTION 1.0
ASSESSMENT OF AIRBORNE EXPOSURE AND DERMAL CONTACT
TO ACRYLAMIDE DURING CHEMICAL GROUTING OPERATIONS
Quality Assurance Project Plan
EPA Contract No. 68-02-3938
Work Assignment No. 47
Approval for: Approval for:
MIDWEST RESEARCH INSTITUTE ENVIRONMENTAL PROTECTION AGENCY
_ _
C. Constant v Date Joseph J. Breen Date
Program Manager Project Officer
Carol L. Green Date Joseph S. Carra
Quality Assurance Officer EPA Quality Assurance
Officer
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Section No.: 2.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 1
SECTION 2.0
TABLE OF CONTENTS
Section
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
11.0
Heading
Title Page
Table of Contents
Project Description
Project Organization and Management
Personnel Qualifications
Facilities, Equipment, Consumables,
and Services
Data Generation
Data Processing
Data Quality Assessment
Corrective Action
Documentation and Reporting
Pages
1
1
1
4
1
3
13
2
3
2
2
Revision
2
2
1
1
2
2
2
1
2
1
1
Date
4/15/86
4/15/86
4/3/86
4/3/86
4/15/86
4/15/86
4/15/86
4/3/86
4/15/86
4/3/86
4/3/86
Appendix A - Field Sampling Protocol
Appendix B - Field Observation Sheets
Appendix C - Analytical Protocol
List of Plan Holders:
Midwest Research Institute:
J. Spigarelli, J. Going, P. Constant, J. Hosenfeld, J. Balsinger,
C. Green, J. McHugh, D. Hooton
Environmental Protection Agency:
J. Breen, J. Carra, E. Reilly-Weidow, T. Murray
National Institute of Occupational Safety and Health:
B. Hills
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Section No.: 3.0
Revision No.: 1
Date: April 3, 1986
Page 1 of 1
SECTION 3.0
PROJECT DESCRIPTION
The Environmental Protection Agency/Office of Toxic Substances (EPA/OTS) under
the Existing Chemicals Program has initiated a plan to conduct field studies to
assess airborne exposure and dermal contact to acrylamide during sewer grouting
operations. The results obtained from these studies will be used to prepare a
quantitative risk assessment.
The overall objectives of the proposed field studies are:
1. Quantitative measurement of occupational exposure to airborne acryl-
amide particulate and vapor in the breathing zone of chemical grout-
ing operators during sewer line and manhole sealing operations.
2. Quantitative measurement of dermal contact to acrylamide during these
same operations using direct and indirect methods.
3.1 Scope of Work
The scope of work will consist of the following subtasks:
A. Review applicable methodologies for assessing dermal contact to
acrylamide.
B. Review applicable air sampling methods for measuring occupational
airborne exposures to acrylamide.
C. Evaluate and finalize an analytical method for determination of
acrylamide in air and dermal samples.
0. Develop a QA/QC project plan.
E. Perform the necessary laboratory analysis of the samples collected
in the field.
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Section No.: 4.0
Revision No.: 1
Date: April 3, 1986
Page 1 of 4
SECTION 4.0
PROJECT ORGANIZATION AND MANAGEMENT
The project organizational chart is shown in Figure 4-1. All MRI personnel
may be reached by telephone at (816) 753-7600.
4.1 Program Management
Mr. Paul Constant, will represent management and serve as program manager.
He will be assisted in this effort by Mr. John Hosenfeld. Together they
wi 11:
Assure that all necessary resources are available.
Assure that the Quality Assurance Manager (QAM)/Quality Assurance
Coordinator (QAC) is fully informed and involved in the project.
Assure that all personnel are informed of project QA policy.
Review all communication from the QAM/QAC regarding the project.
Assure that any problems, deviations, etc., reported by the QAM/QAC
receive immediate corrective action.
Review all technical work and reports for overall technical accuracy.
4.2 Quality Assurance Manager (QAM)/Qua1ity Assurance Coordinator (QAC)
Ms. Carol Green, Quality Assurance Manager, will represent QA management.
She will be assisted by Mr. Jack Balsinger who will serve as QAC. To-
gether they wil1:
Assure that all QA policies and procedures are available and under-
stood by project staff by conducting training courses.
Assure MRI management that the facilities, equipment, personnel,
methods, records, and controls are consistent with project objectives/
requirements by conducting or directing inspections and/or audits.
These inspection/audit results are reported to project and MRI man-
agement. Corrective action is requested in these reports.
Help prepare the project QA plan.
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Section No.: 4.0
Revision No.: 1
Date: April 3, 1986
Page 2 of 4
QUALITY ASSURANCE
MANAGER
C. Green
QUALITY ASSURANCE
COORDINATOR
J. Balsinger
QUALITY CONTROL
COORDINATOR
J. Long
PROGRAM MANAGER
P. Constant
DEPUTY PROGRAM
MANAGER
J. Hosenfeld
WORK ASSIGNMENT
LEADER
J. McHugh
Figure 4-1. Project organizational chart.
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Section No.: 4.0
Revision No.: 1
Date: April 3, 1986
Page 3 of 4
Reinspect or audit to assure that appropriate corrective actions
were implemented. Report unresolved corrective actions to MRI's
Associate Director of K.C. Operations and the Senior Vice President
for resolution.
Review and audit data reports and supporting evidence prior to sub-
mission to EPA.
Prepare and direct the preparation of QA reports to be submitted
to EPA.
4.3 QC Coordinator (QCC)
Ms. Julie Long will serve as QCC. She will:
Conduct systems audit(s) and report findings to the QAM/QAC.
Prepare performance audit samples.
Review notebooks, chromatograms, printouts, and other hard copy
information during systems audits.
Report audit findings to project leader and program management after
QAM/QAC approval.
4.4 Work Assignment Leader
Mr. James McHugh will be the work assignment leader. He will:
Help prepare the project QA plan.
Be responsible for training staff where required.
Be responsible for sample receipt and traceability.
Enforce instrument calibration and maintenance procedures.
Maintain document control of lab and sampling data, notebooks,
records, and other hard copy information.
Review and approve all data prior to submittal to EPA.
Review/validate raw data (e.g., notebooks, forms, strip charts,
etc.).
Ensure that any deviations from protocol are approved and documented.
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Section No.: 4.0
Revision No.: 1
Date: April 3, 1986
Page 4 of 4
Be responsible for analytical data traceability.
Take corrective action on any problems and communicate them in
writing to the QAC/QAM, the QCC, and the program and department
managements.
Prepare and submit monthly and triannual reports.
Prepare and submit other reports as requested by the work assignment
manager in conjunction with project staff.
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Section No.: 5.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 1
SECTION 5
PERSONNEL QUALIFICATION
Mr. Paul C. Constant, and Mr. John Hosenfeld will serve as program manager
and deputy manager, respectively. Mr. Hosenfeld will assist Mr. Constant.
Mr. Constant has recently been assigned to this position but has served as
program liaison officer and as deputy program manager on the previous contract.
Their credentials were previously submitted in the proposal for this contract.
Mr. James McHugh will serve as the Work Assignment Leader. He is a certified
industrial hygenist-and has served as Project Leader on field studies conducted
for the Department of Defense and the National Institute of Occupational Safety
and Health. His credentials w/ere submitted in the proposal for this contract.
Ms. Carol Green will be the Quality Assurance Manager. She has served in this
capacity since May 1983. Her credentials were previously submitted in the
proposal for this contract.
Mr. Jack Balsinger will be the Quality Assurance Coordinator. He has been with
the QA Unit since June 1985. His credentials were previously submitted in the
proposal for this contract.
Ms. Julie Long will serve as Quality Control Coordinator. She is skilled in
spectrophotometric analysis, and generating and analyzing vapors and aerosols.
Ms. Long has received QCC training from Mr. Jack Balsinger, the Quality Assur-
ance Coordinator, and has functioned as a Quality Control Coordinator on
EPA/OTS tasks 6 and 37.
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Section No.: 6.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 3
SECTION 6.0
FACILITIES. EQUIPMENT. CONSUMABLES. AND SERVICES
6.1 Facilities
Sample preparation will be performed in MRI Lab 315W designated, in part,
for the project. The laboratory will be equipped with fume hoods, glove
boxes, and an analytical balance.
Sample analyses will be performed on a Varian 5000 Liquid Chromatograph
located in MRI Lab 120N.
Data file processing will be performed on a Hewlett-Packard 9826 micro-
computer located in MRI Lab 119N.
6.2 Equipment
The equipment used on this task includes:
Varian 5000 Liquid chromotographic system with autosampler and chart
recorder.
Nelson Analytical A/D interface box and related chromatography soft-
ware package (Model 4400).
Hewlett-Packard Model 9826 microcomputer and peripherals used to run
the software.
Mettler AE-163 analytical balance, capable of weighing to the nearest
0.1 mg.
Battery operated air sampling pumps.
6.2.1 The LC system will be calibrated prior to sample analysis over
a concentration range of •>• 0.1 to 100 |jg/mL by injecting a ser-
ies of four acrylamide (electrophoresis grade) standard solu-
tions prepared from one stock standard plus a check standard
solution prepared from an independently weighed standard. The
linear regression equation parameters will be calculated from
the standard data and plotted for visual evaluation of linear-
ity. The correlation coefficient for the standard data should
be greater than 0.995 to define a linear operating range for
the analytical system. One of the midpoint standards will be
injected after every fifth sample to monitor the precision of
the system over the entire analysis; the responses for this
standard will be plotted on a control chart and should exhibit
less than a 10% relative standard deviation.
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Section No.: 6.0
Revision No.: 2
Date: April 15, 1986
Page 2 of 3
6.2.1.1 The Nelson Analytical chromatography software and
Hewlett-Packard hardware have built-in system checks
to monitor their performance. Error messages will
be displayed if problems occur. A copy of the speci-
fic version of the software program used for proces-
sing the data points will be archived.
6.2.1.2 The Mettler AE-163 analytical balance is checked
twice monthly to confirm performance according to
manufacturer's specifications. The weight will.be
traceable to or checked against National Bureau of
Standards weights.
6.2.2 Maintenance
Maintenance of the analytical equipment used in this task will
be done according to manufacturer's specifications and at their
recommended frequency. This is summarized in Table 6-1.
6.3 Consumables
All water used for the analysis will be deionized water filtered through
a Milli-Q® system; pH adjustments will be made using a reagent grade
sulfuric acid:water solution (1:10, v/v).
Blank collection media (dermal pads, surface wipes, air monitors, and
hand rinses) will be spiked both in the field during sample collection
and also in the laboratory to check for chemical recovery and for any
loss of chemical during transit back to the laboratory. All sample
collecting media spiking experiments, both in the laboratory and those
spiked in the field during sample collection, will use collecting media
identical to those used in actual field sample collection.
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Section No.: 6.0
Revision No.: 1
Date: April 3, 1986
Page 3 of 3
Table 6-1. Maintenance
Equipment
Service
Frequency
Van'an 5000 Liquid
Chromatograph
Hewlett-Packard 9826
Balance
General As needed
Limited requirements As needed
Cleaning and adjustment for
calibration 1 year
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 13
SECTION 7.0
DATA GENERATION
7.1 Sample Data Collection
7.1.1 Field Sampling Plan
See Appendix A for the field sampling protocol
7.1.2 Air Sampling Data
Personal and area samples will be collected on a 0.8 u mixed
cellulose ester filter and silica gel sampling train using
calibrated, battery operated sampling pumps at a nominal flow
rate of 1.0 L/min. One area sample will be collected inside
the Mobil Reveal and Seal Unit where the mixing tanks are lo-
cated. Personal samples will be collected in the breathing
zone of workers during the chemical grout mixing operation and
during the grout injection operation whenever the manhole
is entered.
Air sampling data will be recorded on the Air Sampling Data
Sheets (Figure 7-1). The information collected for each per-
sonal or area air sample collected will include: employee and
work site data, sampling equipment data, sampling parameters,
exposure data, calibration data and general observations.
7.1.3 Dermal Contact Assessment Data
Dermal contact assessment sampling will be performed using the
dermal pad and hand rinse methods as described by Durham and
Wolfe (1962). Observations made during a preliminary site
visit to a chemical grouting operation indicated that signifi-
cant dermal contact occurs on the face, neck, and forearms of
workers protected with impervious clothing. The worker's torso,
upper arms, and legs are protected by the impervious suit.
Assuming that full protective clothing is used by the worker,
dermal pads will be placed at six body locations to assess
dermal contact to the face, neck and forearms. If protective
clothing is not utilized dermal pads will be placed at ten body
locations to assess dermal contact to the entire body. Hand
rinses will be conducted using the bag techniques as first
described by Durham and Wolfe (1962). Dermal contact assess-
ments will be conducted during equipment assembly operations,
grout mixing operations, grout injection operations, and equip-
ment disassembly operations.
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 2 of 13
Company Mane
Site ID
Contract Number: Date (Mo/Da/Yr:' .
63-92-mS
WorK rissigment No. 47 Substance Mom ror«d: ;
ACRYLAMIDE ]
EMPLOYEE AND UCRK AREA DATA
Employee Name
Job Tit la/Work Duties
Work Location Description
!
Weather Conditions
SAMPLING EQUIPMENT
Instrument
Model No. Serial No.
[] Personal U Area U Bulk Samole Collection Media: Lot No.
3.8u MIXED CELLULOSE ESTER FILTER AND SILICA GEL THEE
FIELD SAMPLING INFORMATION
Field Sample ID Number
3'art Tisie
S'oo Fine
Sditoie Duration
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 3 of 13
CALIBRATION DATA
Calibration Method
Volume Resistance
Pre Date
1.
2.
3.
Signature
Post Date {Calculations
i
1. |
2.
1
i :
Signature j.-.Tt aye Ti.te Ficwrate 1
I Additional Ccranents, Observations, Diagrams, Data References, etc.
Figure 7-1 (continued)
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 4 of 13
Dermal sampling data will be recorded on Dermal Assessment Data
Sheets (Figure 7-2). The information collected for each worker
sampled will include: employee and work site data, weather
conditions, protective equipment utilized, sampling parameters,
exposure data and general observations.
7.1.4 Wipe Sampling Data
Wipe samples will be conducted using glass fiber filters mois-
tened with distilled water. Wipe samples will be collected at
a number of equipment surfaces and protective equipment sur-
faces which come in frequent contact with the skin.
Wipe sampling data will be recorded on Wipe Sampling Data
Sheets (Figure 7-3). The information collected for each wipe
sample will include: work site data, sampling parameters, and
detailed description of the wipe sample location.
7.1.5 General Observation
The field observation sheets (Appendix B) will be completed
for each site visited. The information collected will include:
Grouting contractor information, a description of the site,
workforce description, employee health information, safety
procedures, protective equipment used, and general work
practices.
7.2 Sample Traceability
Sample traceability protocol (SOP SC-1) will be followed for sample track-
ing for this project. Traceability records will start with sample col-
lection. These records will accompany the samples when shipped to MRI.
Examples of the field and laboratory traceability forms are shown in
Figures 7-4 and 7-5.
7.3 Laboratory Analysis Procedures
See Appendix C for analytical protocol. A flow chart of the steps in-
volved in the analytical method is shown in Figure 7-6.
7.4 Internal Quality Control Checks
With each batch of samples, appropriate QC samples will be included so
the quality of the sample data can be assessed. These QC samples include
method blanks, spikes, field blanks, and field spiked blanks.
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 5 of 13
Cowan y Name
. Site ID
Contract Number Date Ulo/Di/Yr>
o8-82-3P39
Work Assigment No. Substance Monitored
47 ACRYLMICE
EMPLOYEE AND WORK AREA DATA
Employee Name
Job Title/ Work Duties:
: PERSONAL PROTECTIVE EQUIPMENT
E/9 Protection
, coots/ Shoes
, Sesoiracor
1
NOTE: Specify type, material, brand, ere. 1
Head Protection
Gloves
! Protective Suit/Coueral Is '
!
DERMAL SflMPLlNB DATA
! Dermal Pad Media: WHATMAN CHRCMATOGRAPHY PAPER Mo. 17 ( 4 X 4 inch Pads)
I Side
1
1
! Chest
i
i
j For earns
i
i :r:ouicirs
i
i
i '.11 ens
i
Shins
[
Hand Rinses
Sol •«(»»:
DISTILLED
tttTE?
Start
Time
StoD Duration
Time i
i
!
=^==^^!^=^=^^=^=^==^===s
Lot No.
Samole Numbers :
i
L«ft fight
LetJ
Left
Left
Lett
Left
Left
Right
Right
Right
Right
Right *
Right !
;i9natur* [Date !a«tf«d!»: i
Figure 1-2. Dermal assessment data sheet.
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 6 of 13
Conpanr Nine Contract Number Date (Mo/Da/Yr)
68-82-3?38
Site ID Uork Assigaent No. Substance Monitored:
47 ACRYLAMIDE
Uipe Sanpling Media and Method Lot No.
UHATMAN 37mn GLASS FIBER FILTER MOISTENED WITH DISTILLED UATER
Wipe Saiole No.
Tine
Location Description
TOP OF THE CONTROL PANEL IN THE MOBILE REVEAL AND SEAL UNIT
OUTSIDE OF TIE ACRYLAMIOE MIXINB TANK
OUTSIDE OF THE CATALYST MIXING TANK
HANDLE OF THE INJECTION HM (Manhole sealing operation only)
OR SIDE OF PACKER (main line or lateral line sealing operation only)
HYDRAULIC HOSING ATTACHED TO INJECTION GIN OR PACKER
SIDE OF SAFETY ONE OF THE ROAD
INSIDE OF THE RESPIRATOR
OUTSIDE OF THE RESPIRATOR
BACK OF IMPERVIOUS UORK GLOUE
Signature Date
Figure 7-3. Wipe sampling data sheet.
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 7 of 13
(See Bock of Pag* for Explanation of Numb*n)
CHAIN OF CUSTODY OR TRACEA8IUTY RECORD
Q Chain of Ctotody Record
Project Numbar
Location ___^_______
Container No.
QTraceabiliry Lay
Data of Field Sampling .
Type of Sample.
Storage Requirements.
Sample No.
Detcriptlon
Orher
loent.
Sampier
Level Check
Comments
Dare
Seal Inracr
Dare
Checked by
(Initiali)
Rilirquiihvd by
Oar*"
Tim*
Rtc»iv*d by
Figure 7-4. Sample traceability form.
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 8 of 13
FILLING OUT CHAI.V OF CUSTODY/TKACEABILITY LOG
1 Check chain of custody, or
2. Traceability log.
3. Eater project and cask number.
<• Eater daces the first ann Use samples were C3ll.ected that are recorded on
each, log sheet.
5 Sneer sampling location- plant name and/or cicv
Enter type of sample. •. e , ~enax trip, conaensace. BU!« feea etc Record
,/niv one type of sample on i fom.
" Eater shipping cuntaiser aunoer la i-nic.i samples are packed Each snipping
container must contain only one cvpe of sample.
a Enter storage requirements, i e , wee ice, dry ice. in plastic aags, ecc
9 Enter entire sample lumoer
'.C inter anv ocner sample description required
il Enter other sample identification, i e , Tenax cuoe numoers
'.; Enter name or .aitials of person collecting sample
13 Four columns are provided for inventory checkoff eac.i time sample custody is
transferred As the samples are inventoried, place a cneckmark in --tie appropriate
aox If sannles are Liquid, the liquid level snould be confirmed at tne same time
Changes in »e level snould oe noted and dated under the rommments Column li 'her.
tae inventor/ is canreiecea. enter t.ie date in 15 directly 'inner c.h.e column cneckel
3::
Sixteen througn ".3 are provided for samples collected under Chain of Cuscodv
£jca shipping containers with samples must ae sealed uith evidence laoe .nen not
.n tne custodian s pre'eace. The seal is not to be broicen by jny other oerson
Evidence tape must be placed over the joint between the container and container
..a. the cape is signed and Jaceo by the custodian. Eacn container vith samples
•ausc 3e -.isoected at tae oegioning of eaca
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 9 of 13
(See Baci of Page for Explanation of Numbers)
LABORATORY C2AIN OF CUSTODY OR T3AGA3ILITY RZCCRD
Amount of
Sample Removed
(zive date)
Cccseats !
|
i
t
i
Laboratory/Area
Custody Office
Sample Preparation
Petals
GC/MS
Otaer
(Identify)
Relinquished by: Received bv:
(signature) Data/Time ( sisnatur=:' ^at-'T.ae
i ' —
.
J
Notebook Reference Pages f
Analyst Cements
19) Motaoook No.
Figure 7-5. Laboratory traceability record.
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Section No.: 7.0
Revision No.: 1
Date: April 3, 1986
Page 10 of 13
FILLING OUT CHAII1 Of CUSTODY/T3AC2ABILIT? LOG
I. Check chain of custody or
2. Traceability log.
3. Eater project and task number.
it. Enter data samples --ere received by custody office.
5. Enter sampling Location: plant aame and/or city.
6. Enter type of sample, i.e., Teaax trap, condensate, bulk feed, etc.
Record only one type of sample on a fora.
7. Enter container type, i.e., Tenax trap, XAD trap, petri dish, narrow
mouth quart bottle, 2-dram vial, 2 oz Rx bottle, etc.
8. Enter storage location samples will be taken from ana returned L.O roc-
custody office possession.
9. Enter laboratory sample numoer.
10. Enter field sample number.
11. Entar any additional sample description, i.e., hazards in handling the
sample, appearance, Tenax trap number, etc.
12. Enter any amount of sample expended and date.
13. Enter any comments pertinent to tie tracking of the entire samole, i e ,
sample composited to form a new sanple, sample transfer to a new custoav
form, sample split to give two or more items to '
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 11 of 13
Dermal Pads
Air Monitor Samples
Wipe Samples
Field QC Samples & Blanks
Extract aery1 amide with volume
of water adjusted to pH 3.7
Hand rinse samples
(using known volume of rinse)
Standard Solution
Lab QC Sample
Blanks
Analyze by HPLC
Calculate total weight of
acrylamide per sample (ug/L)
corrected for dilutions
Figure 7-6. Flow chart for the determination of acrylamide
in field samples.
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 12 of 13
7.4.1 General
New lots of reagents are checked prior to use, or current lots
of reagents are checked when method blank problems are experi-
enced.
7.4.2 The control checks that will be utilized are the following:
Method blanks: At least one per sample group tested.
Field filter blanks: At least two per sample group tested for
each type of collection medium.
Spiked blank filters: Replicate samples will be prepared to
check on extraction recovery.
7.4.3 Calibration
The LC system will be calibrated prior to sample analysis over
a concentration range of ^ 0.1 to 100 ug/mL by injecting a ser-
ies of four acrylamide (electrophoresis grade) standard solu-
tions prepared from one stock standard plus a check standard
solution prepared from an independently weighed standard. The
linear regression equation parameters will be calculated from
the standard data and plotted for visual evaluation for linear-
ity. The correlation coefficient for the standard data should
be greater than 0.995 to define a linear operating range for
the analytical system. One of the midpoint standards will be
injected after every fifth sample to monitor the precision of
the system over the entire analysis; the responses for this
standard will be plotted on a control chart and should exhibit
less than a 10% relative standard deviation.
If response values for the midpoint standard vary from its mean
response by more than 10% relative standard deviation, the
source of loss in precision will be corrected and the calibra-
tion curve repeated before subsequent samples are analyzed.
7.4.4 Definitions
7.4.4.1 Method blanks: Procedural blanks are carried through
the entire procedure to check for contamination.
7.4.4.2 Field blanks: The field filter blank is taken to the
field and handled in the normal fashion except it
is not exposed to the contaminant.
7.4.4.3 Spiked blanks: Collecting media will be spiked
with known amounts of acrylamide.
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Section No.: 7.0
Revision No.: 2
Date: April 15, 1986
Page 13 of 13
7.5 Systems and Performance Audits
7.5.1 Systems audits: Systems audits by the QCC/QAC shall include:
Inspecting facilities and equipment for adequacy, appro-
priateness, and safety during use.
Reviewing actual practices versus written procedures and
protocols.
Inspecting the records of maintenance and calibration.
Inspecting QC practices.
Assisting/conducting data audit prior to report submittal.
Preparing and submitting a report with recommended correc-
tive actions to the QAC/QAM, and after approval, to the
work assignment leader and program manager.
Conduct additional audits as directed by the QAC/QAM.
Assisting/preparing QA report for the EPA's work assignment
manager.
7.5.2 Performance Audits
The performance audit sample is designed to check the operation
of the equipment. Several blind performance samples will be
independently prepared by the QCC and submitted for analysis
before and during the analysis of the regular samples. Perfor-
mance audit samples will also be analyzed if (1) the QCC be-
lieves the analysis procedures has changed, (2) analytical
problems are suspected, or (3) the MRI work assignment leader
of the EPA work assignment manager requests samples.
7.5.3 QAC/QAM Audits
Additional audits will be conducted or directed by the QAC/QAM
as follows:
Schedule and conduct additional audits as needed, e.g.,
staff credentials, quality control data and practices,
documentation practices, data audit, and QA compliance.
Review and approve the report and supporting evidence for
accuracy and QA compliance prior to report submittal to
OTS.
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Section No.: 8.0
Revision No.: 1
Date: April 3, 1986
Page 1 of 2
SECTION 8.0
DATA PROCESSING
8.1 Collection
Data collection will utilize both manual and computerized acquisition
systems. All activities shall be legibly recorded using permanent ink
in the project notebook or on worksheets. Each person who records data
shall sign and date each sheet. Strip charts, magnetic tapes, etc.,
shall be labeled with a format identifier, project number, date, the
ID(s) of the instrument, and the name of the person responsible for the
data. Custody of the original data media will be the responsibility of
assigned project staff until archived.
8.2 Data Reduction
Standard data reduction procedures with built-in checks will be used.
For example, if an integrator or computer is used to calculate concentra-
tions, the standards used to generate the curve must be back-calculated
using the curve to ensure satisfactory curve fitting over the anticipated
range. In addition, all sample manipulations (e.g., weighing, dilution,
concentration, etc.) must be clearly documented.
8.3 Data Validation
The work assignment leader will be responsible for assuring data validity
which will include:
Validating all equations and computer programs and documenting the
validating and evidence.
Validating and checking electronic data transfer.
Proofreading all data transfers by the analyst or a second project
staff member.
Screening data for consistency by a second project staff member.
Checking calculations.
Performing outlier checks.
Reporting of all associated blank, standard, and QC data along with
results for analyses of each batch of samples.
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Section No.: 8.0
Revision No.: 1
Date: April 3, 1986
Page 2 of 2
Examining QC data and QC checks.
Maintaining records of reviewing, proofing, and validation.
Examining data/information for completeness, representativeness,
and comparability.
Reviewing and approving all data by the work assignment leader.
Reporting protocol deviations and assumptions with the results.
8.4 Transfers
Data transfer will be kept to a minimum to prevent errors. The analyt-
ical data will be transferred manually from a computerized output to
data tables. These data will be checked for transfer errors.
8.5 Storage
Raw data will be documented in laboratory notebooks, on printed paper,
as strip chart recordings, or on magnetic tape or disk. Permanent stor-
age of work assignment data in the formal project file and hard copy from
magnetic media will be archived (SOP-QA7). The storage of magnetic media
will be reported.
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Section No.: 9.0
Revision No.: 2
Date: April 15, 1986
Page 1 of 3
SECTION 9.0
DATA QUALITY ASSESSMENT
The objective of precision for this method will be to obtain total weight of
acrylamide for replicate spiked filter samples which have relative differences
± 20% of each other. The objective for accuracy will be to obtain total
weights of acrylamide on replicate spiked filter samples which have relative
errors ± 30% of the actual acrylamide present on the air filter. Average re-
covery efficiencies for acrylamide using spiked filters should fall within
the range of 70 to 130% to yield meaningful data.
9.1 Analytical Precision
Precision is determined by performing replicate analysis. For data sets
with a small number of points (2 ^ n £ 8), the estimate of precision will
be expressed as range percent (R%):
R% =
x 100
where Xx = highest value determined
X2 = lowest value determined
X = mean value of the set
and
II I* •
x= z -1
-•_-i n
where Xi = ith determination
n = number of determinations
The estimated detection limit (EDL) for the analytical system will be
defined as the corresponding concentration equal to three times the
noise level from the detector.
For large data sets (n > 8), the estimate of precision will be expressed
as percent relative standard deviation (% RSD):
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Section No.: 9.0
Revision No.: 2
Date: April 15, 1986
Page 2 of 3
n
I (Xi - X)2
R.S.D. =
where n = number of replicate determinations.
= mean =
The precision of the analytical system will be monitored through repli-
cate injections of a midpoint standard throughout the analysis and
plotted on a control chart.
9.2 Accuracy
The accuracy of the analytical method can only be established for known
spiked samples. Accuracy may be indicated by comparing the total weight
of aery1 amide on spiked sample collection media determined using the
analytical method to the theoretical or actual amount of chemical that
was spiked onto the blanks.
Accuracy will be measured by calculating the relative error (RE):
RE (%) = -- x 100
where F = found weight of chemical
A = actual weight of chemical
9.3 Recovery
Recovery will be indicated from the results of the spiked blank analyses.
Spiked acrylamide recovery will be determined by a direct comparison of
the spiking solution to the solution obtained from extracting the spiked
blank.
R (%) = -HI x 100
CSTD
where c-.-i = concentration of extract
CSTD = concentratlon °f spiking solution
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Section No.: 9.0
Revision No.: 2
Date: April 15, 1986
Page 3 of 3
9.4 Traceability of Instrumentation
All collection and measuring instrumentation will have a unique identifi-
cation number. Maintenance, calibration, and use logs will be maintained.
9.5 Traceability of Samples
All samples will have a unique identification number along with informa-
tion on field site, monitoring location, exposure time and conditions,
collection device, etc. The samples will be labeled with adhesive bar-
code labels to identify the samples and trace them through the sampling
and analytical procedures.
9.6 Traceability of Data
Data will be documented and filed to allow complete reconstruction, from
initial field records to data archiving.
9.7 Completeness
Due to the variety of data points available per field test site, complete-
ness of the data will be crucial in order to obtain meaningful data.
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Section No.: 10.0
Revision No.: 1
Date: April 3, 1986
Page 1 of 2
SECTION 10
CORRECTIVE ACTION
The work assignment leader has primary responsibility for taking corrective
action; if he is unavailable, the program manager, and/or the QAC/QAM shall
be contacted for instructions. Some of the types of problems and corrective
actions to be taken are listed below. Unresolved problems are reported by
the QAM to the Associate Director of K.C. Operations and to the Senior Vice
President for resolution.
10.1 Performance/Systems Audits
If problems are detected during an audit:
The auditor shall notify the person responsible, the work assignment
leader, and the QAC/QAM of the problem(s) and any action(s) he has
taken.
The work assignment leader and the person responsible shall correct
the problem, then notify the QAC/QAM.
The auditor shall then prepare, and after QAC/QAM approval, send a
problem/action taken memo to the program manager and the work as-
signment leader.
10.2 Loss of Data
The work assignment leader shall investigate the problem, then perform
one or more of the following actions:
If the problem is limited in scope, the problem/action taken is
documented in the notebook; the work assignment leader then pre-
pares and sends a problem/action taken memo to the QAC/QAM, and
the program manager.
If a large quantity of data is affected, the problem/action taken
is documented in the notebook; the work assignment leader then pre-
pares and sends a problem/action-taken memo to the QAC/QAM, project
manager, and the EPA work assignment manager.
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Section No.: 10.0
Revision No.: 1
Date: April 3, 1986
Page 2 of 2
10.3 Significant QA Problems
In general, the work assignment leader shall identify technical problems.
The work assignment leader prepares and sends a problem memo to the
QAC/QAM and program manager; if the problems are significant, the
action is determined collectively.
The action taken is documented in the notebook.
The problem and action taken is reported to the EPA work assignment
manager.
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Section No.: 11.0
Revision No.: 1
Date: April 3, 1986
Page 1 of 2
SECTION 11
DOCUMENTATION AND REPORTING
11.1 Documentation
All documentation shall be in permanent ink.
Corrections will be performed as follows: Draw a single line
through an incorrect entry so that the original entry remains legi-
ble. Add the correct entry; then explain, initial, and date the
correction.
New information may be added to an original page. It will be ini-
tialed, dated, and explained.
All deviations from standard operating procedures (SOPs), procedures,
and protocols will be documented.
Strip charts, magnetic tapes, etc., will be labeled with a format
identifier, the date, the ID(s) of the sampling equipment, and the
name of the person responsible for the data recording equipment.
11.2 Document Control
Raw sampling data will be documented and stored in laboratory note-
books, on sequentially numbered sampling forms, on printer paper,
on magnetic tape, and as strip chart recordings.
A logbook of the data media created during each test period will be
established to document the existence and flow of data through the
data processing cycle.
All project-related documents will be assigned a unique numerical
designation in a document control system maintained by assigned
project staff.
11.3 QA Reports to Management
The QAC/QAM, in cooperation with the work assignment leader, shall iden-
tify critical phases of the project which will be subject to inspection.
The inspection will include a review of:
• Staff credentials.
• Equipment maintenance and calibration records.
• Equipment performance.
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Section No.: 11.0
Revision No.: 1
Date: April 3, 1986
Page 2 of 2
• Documentation practices.
• Recordkeeping practices.
• Adherence to protocols, SOPs, and QA plan.
• Assessment of data accuracy, precision, and completeness.
The results of inspections and audits will be reported quarterly by the
QAM to MRI management; summaries will be reported to the EPA work assign-
ment manager.
11.4 Report Design
Progress, draft final, final reports, and QA summary reports will be
submitted in accordance with the provisions for reporting in the contract.
Verbal status reports will be made biweekly to the work assignment leader.
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APPENDIX A
FIELD SAMPLING PROTOCOL
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1.0 AIRBORNE EXPOSURE ASSESSMENT
1.1 Air Sampling Protocol
Airborne acrylamide aerosols and vapor are collected on a sampling
train consisting of a mixed cellulose ester filter and silica gel tube at a
flow rate of 1 L/min. The collected material is desorbed from the sampling
media with deionized water followed by HPLC analysis.
The sampling media will consist of a Millipore 37 mm MAWP filter cas-
sette assembly available from Millipore Corporation of Bedford, Massachusetts.
On the outlet side of the filter cassette assembly a SKC No. 226-10 silica
gel tube available from SKC, Inc. of Eighty Four, Pennsylvania shall be at-
tached with a short section of tygon tubing of minimum length. The sampling
train shall be attached to a calibrated, Ni-Cad battery operated personal
sample pump. The sampling pump is calibrated before and after the sampling
period using a volumetric buret and stop watch with the sampling train in line.
The MAWP filter cassettes and silica gel tubes are to be labeled
prior to the site visit with a unique number using adhesive barcode labels.
A set of six identical barcode labels will be printed for each sample. One
of the adhesive labels in the set will be affixed to each filter cassette and
silica gel tube. The samples are then placed in individual zip-lock plastic
bags. Another label from the same set will be affixed directly to the outside
of the plastic bag. The remainder of the labels in the set will be placed
inside the plastic bag. The sample numbers will be logged with a laptop com-
puter and light pen using barcode software.
At the survey site, a corresponding barcode label from the filter
cassettes and silica gel tubes will be affixed to the Air Sampling Data Sheet
which contains pertinent information concerning site location, employee and
work area information, sampling equipment and methods, calibration data, and
sampling and analytical data.
Breathing zone air sampling shall be conducted during the grouting
chemical mixing operation and during sealing operations when the worker enters
the manhole. Area sampling shall be conducted inside the Reveal and Seal
Mobile Unit near the mixing tanks. If possible, an area sample will also be
collected inside the maintenance and storage facility at the grouting contrac-
tor's place of business. The recommendation flow rate is 1.0 L/min. The recom-
mended sample volume is 480 L. The pump rotometer should be checked frequently
during the sampling period to maintain the calibrated flow rate. Pertinent
information concerning the air sample such as ambient temperature, atmospheric
pressure, sample duration, flow rate, site location, subject information shall
be referenced to the sample number and recorded on an Air Sampling Data Sheet.
At the end of the sampling period, the sample train is disassembled
and the filter cassette and silica gel tube recapped. Place the sampling
media in a water tight container and store in a chest containing ice or blue
ice packs for transport to the laboratory. Do not use dry ice. The samples
will be sent to the laboratory in sealed ice chests using a next-day delivery
service. A Chain-of-Custody or Traceability record will be filled out in the
field and accompany all shipments to the laboratory.
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1.2 Quality Control Field Samples
On each day of sampling two sets of field blanks and two sets of
spiked samples shall be prepared. Field blanks are required in order to ac-
count for any possible contamination which may occur while collecting, trans-
porting, or handling field samples prior to extraction in the laboratory.
Spiked or fortified samples are required to account for stability and vola-
tility of the grouting chemical.
Field blanks of the collection media should be handled in the same
manner as the exposed sample except that no air is drawn through them. The
end caps of the filter cassette blanks are to be removed in the field and im-
mediately resealed and labelled. The ends of the glass tube on the silica
gel blank shall be broken in the field and immediately recapped and labelled.
One set of field blanks shall be prepared at the beginning of the sampling
period and one set at the end of the sampling period. The blanks shall be
stored and shipped with the exposed air samples.
Two filter cassettes and two silica gel tubes are to be spiked with
a known quantity of acrylamide diluted to the approximate concentration used
in the grouting material (100 g of acrylamide per liter of water). The amount
of acrylamide added to the collecting media should be approximately the levels
that are expected to impinge on the sampling media during the field studies.
One spiked sample set shall be prepared at the beginning of the sampling
period and the other at the end of the sampling period. Both samples should
be handled, stored and shipped with the exposed samples.
2.0 DERMAL CONTACT ASSESSMENT
2.1 Background
The methodologies for assessment of dermal contact to toxicants have
been developed principally for pesticides exposure monitoring. The methods
described by Durham and Wolfe (1962) and Davis (1980) remain the established
protocols utilized by pesticide manufacturers and formulators to conduct ex-
posure monitoring of pesticide applicators.
Durham et al. (1962) reviewed the primary methods for measurement
of dermal exposure. One method involves placing absorbent pads at various
points on the worker's body. The worker then performs his usual job functions.
The pads are removed and transported to a laboratory, where the toxicant is
extracted and analyzed. The amount of pesticide that comes into contact with
the skin is calculated using an anatomical model, which is extrapolated to
the entire surface area of the body part represented by the pad. The neces-
sary assumption that the pad area is representative of the entire body part
being measured is a shortcoming of this technique.
A variation of the absorbent pads method involves the use of knit
cotton garments that cover the study area during exposure. One such method
was described by Davis (1980) to assess exposure to the hands using cotton
gloves as the collecting media. Durham et al. felt that the use of absorbent
A-3
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gloves might result in overestimations of exposure to the hands. The gloves
tend to absorb much more liquids than could be expected to adhere to flesh.
This method however, is quick and easy to implement in the field.
The other primary method described by Durham et al. involves swab-
bing or rinsing the skin with a solvent that will remove the toxicant. The
rinse solutions are collected and analyzed. The swabbing technique uses sur-
gical gauze moistened with solvent. The gauze pads are handled with forceps
to rub the body surface with light pressure. The procedure is very tedious
and time-consuming and will not remove residues that are absorbed into the
skin during the exposure period.
Use of the swab method for estimating contamination of the hands
was found to be unsatisfactory. It is not easy to swab correctly between
fingers and around the fingernails. Durham and Wolfe described a bag rinse
technique suitable for the hands. The procedure involves the use of poly-
ethylene bags containing a suitable solvent for washing the pesticide from
the hands. The hand is inserted into the bag containing a given quantity of
solvent. While the bag is held tightly around the wrist to prevent leakage,
the hand is shaken vigorously. The rinse is collected and transported to a
laboratory for analysis. The procedure is faster than the swabbing technique;
however, it also will not remove residues that are absorbed into the skin
during the exposure period. Durham and Wolfe (1962) reported percentage of
extractable parathion pesticide using the hand rinse method ranging from 77
to 94% for the first rinse and 89 to 98% for the second rinse. The hand rinse
recoveries for acrylamide are expected to be higher because acrylamide is more
soluble in water.
Taking into account the advantages and disadvantages of the various
monitoring devices listed above, the simple absorbent pad method as described
by Durham and Wolfe (1962) is recommended for all body parts except the hands.
Durham et al. validated the effectiveness of alpha-cellulose pads by comparing
the residues found on the pads to those found on adjacent areas of skin
swabbed with ethanol and found acceptable agreement.
Most dermal studies of pesticide have essentially adopted the number
and location of dermal pads used by Durham and Wolfe (1962). They recommended
that each worker be monitored with a set of ten pads. The location of the
pads are: the front of the legs just below the knees, the front of the
thighs, the back of the forearms, on top of the shoulders, the back of the
neck at the edge of the collar, and on the upper chest near the jugular notch.
If protective clothing is worn, the worker is monitored by pads attached to
the upper back and chest to assess exposures to the face and neck. In addi-
tion, pads attached to the forearm can be utilized to assess dermal contact
to the arms if not protected by the impervious clothing.
Dermal exposure studies of pesticide workers demonstrate the impor-
tant contribution of hand exposure to overall dermal contact. Hand exposure
as a percentage to total dermal exposure range from 37 to 98%. The bag rinse
method appears to be the method of choice. Durham and Wolfe (1962) found that
they could recover approximately twice as much residue from the worker's hands
by using the bag rinse method rather than the swab method.
A-4
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2.2 Dermal Contact Assessment (except of hands) Using the Dermal Pad
Method
2.2.1 Sampling Protocol
Pads to be used for estimating dermal contact are to be constructed
from preparative chromatography paper (17 Chr) available in sheets from
Whatman, Inc. of Clifton, New Jersey. The chromatography paper is cut into
4-in. (10.2-cm) squares which are then stapled to the center of a 5 in. square
protective backing of glassine paper available from Schleicher and Schuell,
Inc. Both materials are also readily available through laboratory supply
companies. When handling the absorbent pads, skin contact should be avoided
by wearing disposable surgical gloves.
The pads are to be labeled prior to the site visit using barcode
labels which will identify the samples and track them through the sampling
and analytical procedures. A set of six identical barcode labels will be
printed for each sample. Each set of labels will have a unique number. One
of the adhesive labels in the set shall be affixed to the back of the glassine
protective backing. Each pad shall then be placed into individual zip-lock
plastic bags. The other five adhesive labels from the same set shall be af-
fixed to the outside of the plastic bag. The sample numbers will be logged
with a laptop computer and light pen using barcode software.
At the survey site, a corresponding barcode label from the dermal
pad will be affixed to a Dermal Assessment Data Sheet which contain pertinent
information concerning the site location, sampling data, subject information,
etc. Following the sampling period, each dermal pad shall be returned to its
original container.
Assuming that full impervious protective clothing is used by the
subject, six pads will be attached to the worker. The locations of the pads
are:
1. On the right forearm midway between the wrist and elbow, on the
side of the arm opposite the palm - the pad shall be positioned face up with
the glassine backing taped flush against the skin. Attach the pad with sur-
gical tape applied only to the glassine backing.
2. On the left forearm midway between the wrist and elbow, on the
side of the arm opposite the palm - the pad shall be positioned face up with
the glassine backing flush against the skin using surgical tape as described
above.
3. On the subject's upper back immediately below the collar. The
pad shall be positioned face up on the outside of the protective clothing
using safety pins.
4. On the upper chest near the Jugular notch. The pad shall be
positioned face up on the outside of the protective clothing using safety pins.
A-5
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5. On the top of the right shoulder - the pad shall be positioned
face up with the glassine backing against the outside of the workers' protec-
tive clothing using safety pins.
6. On top of the left shoulder - the pad shall be positioned face
up with the glassine backing against the outside of the worker's protective
clothing using safety pins.
If impervious protective clothing is not worn by the worker, 10
dermal pads will be attached to the worker. The locations of the pads are:
1. On the right forearm, midway between the wrist and elbow, on
the side of the arm opposite the palm - the pad shall be positioned face up
with the glassine backing flush against the outside of worker's street clothes
using safety pins. If the worker is wearing a short sleeve shirt, attach the
pad directly against the skin using surgical tape.
2. On the left forearm midway between the wrist and elbow, on the
side of the arm opposite the palm - the pad shall be positioned face up with
the glassine backing flush against the outside of the worker's street clothes
using safety pins. If the worker is wearing a short sleeve shirt, attach the
pad directly against the skin using surgical tape.
3. On the subject's upper back immediately below the collar. The
pad shall be positioned face up on the outside of the worker's street clothes
using safety pins.
4. On the upper chest near the jugular notch. The pad shall be
positioned face up on the outside of the worker's street clothes using safety
pins.
5. On the top of the right shoulder - the pad shall be positioned
face up with the glassine backing against the outside of the worker's street
clothes using safety pins.
6. On top of the left shoulder - the pad shall be positioned face
up with the glassine backing against the outside of the worker's street
clothes using safety pins.
7. On the right front thigh - the pad shall be positioned face up
with the glassine backing against the outside of the worker's street clothes
using safety pins.
8. On the left front thigh - the pad shall be positioned face up
with the glassine backing against the outside of the worker's street clothes
using safety pins.
9. On the right front shin just below the knee - the pad shall be
positioned face up with the glassine backing against the outside of the
worker's clothes using safety pins. If the worker is wearing shorts, the pad
will be attached directly against the skin using surgical tape.
A-6
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10. On the left front shin just below the knee - the pad shall be
positioned face up with the glassine backing against the outside of the
worker's clothes using safety pins. If the worker is wearing shorts, the pad
will be attached directly against the skin using surgical tape.
Dermal pad sampling is to be performed during the grout equipment
assembly, grout mixing operations, grout injection operations, and equipment
disassembly operations. Sampling duration shall not exceed 4 h. If the
grouting operations exceed 4 h duration, the pads shall be changed to fresh
pads.
At the end of the sampling period the pads shall be carefully re-
moved from the worker using surgical gloves. Care should be taken not to
touch the absorbent pad. Slide the pad and glassine backing into its original
prelabeled plastic bag and seal. Place the plastic bags from a single test
subject in a sealed wide mouth jar. Seal the jar inside a plastic bag and
store the samples in a chest containing ice or blue ice packs for transport
to the laboratory. Do not use dry ice. Send the samples to the lab at the
end of each day of sampling using a next-day delivery service. A Chain-of-
Custody or Traceability Record will be filled out and accompany all samples
sent to the laboratory. A barcode label from each sample in the shipment will
be affixed to this form and sent with the sample to MRI.
2.2.2 Quality Control Field Samples
On each day of sampling two field blanks and two spiked samples
shall be prepared. Field blanks of the dermal pads should be handled in the
same manner as the exposed pads except they are not attached to the worker.
An absorbent pad is to be removed from the plastic bag container and immedi-
ately returned to the bag and resealed. One field blank shall be prepared at
the beginning of the sampling period and one at the end of the sampling period.
The field blanks shall be stored and shipped with the exposed samples.
Two pads are to be spiked with a known quantity of acrylamide di-
luted to the approximate concentration used in the grouting material (100 g
of acrylamide per liter of water). The amount of acrylamide added to the pad
should be approximately the levels that are expected to impinge on the pads
during the field studies. One spiked sample shall be prepared at the begin-
ning of the sampling period and exposed to the same weather conditions as the
exposed samples for the duration of the sampling period. The other spiked
sample shall be prepared at the end of the sampling period. Both samples
should be handled, stored and shipped in the same manner as the exposed
samples.
2.2.3 Dermal Contact Calculations
Dermal contact will be calculated using the method described by
Durham and Wolfe (1962). An anatomical model is used to calculate dermal
contact from the amount of acrylamide found on the dermal pads. The anatom-
ical model shown in Table A-l represents surface areas of an adult male and
is derived from the data of Berkow (1931), Diem and Lentner (1970), and Durham
and Wolfe (1962). The suggested pairing of exposure pad locations and body
A-7
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Table A-l. Dermal Exposure Pad Locations Used for Calculation of
Dermal Contact and Surface Areas of those Regions
Exposure pads used to Surface area of
Body region represent body regions regions (cm2)
Face Shoulder pads 650
Back of neck Back pad 110
Front of neck Chest pad 150.
Hands Total residue in hand rinse 820
Back Back pad 3,550
Chest and stomach Chest pad 3,550
Upper arms Shoulder and forearm pads 1,320
Forearms Forearm pads 1,210
Thighs Thigh pads 2,250
Lower legs Shin pads 2,380
Calculated from data of Berkow (1931), Diem and Lentner (1970), and
.Durham and Wolfe (1962).
Surface area of hands is only necessary if partial swabbing or pads attached
to the hands are used for collection of residues.
A-8
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regions is also shown in Table A-l. The amount of acrylamide per unit area
of the pad is divided by the exposure time and then multiplied by the surface
area of the unprotected body region represented by the pad. If more than one
pad represents a body region, the amount of acrylamide per unit area per expo-
sure time for each pad is averaged and then multiplied by the surface area of
the body region represented by the pads. The dermal contact to the hand is
simply the total residue as determined by the bag rinse, divided by the expo-
sure time. The total dermal contact to the body is the sum of the calculated
dermal contact to the individual body region.
2.3 Dermal Contact Assessment Using the Hand Rinse Method
2.3.1 Sampling Protocol
Hand rinses shall be performed using the bag technique as first de-
scribed by Durham and Wolfe (1962). The bag shall be a 5-1/2 in. by 15 in.
polyethylene Whirlpak (No. 81027) supplied by NASCO of Fort Atkinson, Wisconsin.
The hand rinses shall be transferred into 402 mason jars which shall be cleaned
and labeled prior to the site visit using a barcode system.
A set of six identical barcode labels will be printed for each sample.
Each set of labels will have a unique number. Prior to the site visit, all
six labels shall be affixed to the outside of the mason jar. The sample num-
bers will be logged with a laptop computer and light pen using barcode software.
At the survey site, one of the corresponding barcode labels from the mason
jar will be transferred to a Dermal Assessment Data Sheet which contains per-
tinent information concerning the site location, sampling data, subject infor-
mation, etc.
Prior to sampling the polyethylene bag shall be rinsed twice with
100 ml of distilled water. Discard the rinse water. Add 50 ml of distilled
water to the bag. Insert the subject's hand into the bag. While the bag
tightly held below the wrist bone, the hand is shaken vigorously in the dis-
tilled water for 50 shakes. Allow the water to drain from the hand for 10 s
before removing the hand. Transfer the wash water to a clean, 4 oz wide-mouth
mason jar. The mason jars are to be cleaned prior to the site visit with
Alconox followed by two rinses with deionized water. Rinse the bag with 25
ml of distilled water and add the rinse to the wash water in the mason jar.
Seal the mason jar with a Teflon-lined cap. Seal each sample in a plastic
bag and place them in a chest containing ice or blue ice packs for transport
to the laboratory. Do not use dry ice. Ship the samples to the laboratory
at the end of each sampling day using a next-day delivery service.
Hand rinses should be conducted at the start of the workshift, imme-
diately after the equipment assembly operation and immediately after the equip-
ment disassembly operation. For manhole sealing operations a hand rinse should
be performed immediately after the injection gun operator exits the manhole.
A hand rinse should be performed after the workers remove their protective
clothing at break periods and at the end of the day.
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2.3.2 Quality Control Field Samples
On each day of sampling two field blanks and two spiked samples
shall be prepared. The field blanks are prepared using the same method and
materials as the samples. Pre-rinse the fresh polyethylene bag as described
above but instead of discarding the water transfer the rinse water into a
clean prelabeled wide-mouth mason jar. Next add 50 ml of distilled water to
the bag, shake vigorously 50 times and transfer the distilled water to a sec-
ond prelabeled mason jar. Post-rinse the bag as described in the sampling
procedure. Seal the mason jar with a Teflon-lined cap and place the field
blank in the ice chest with the other samples. One field blank should be
prepared at the beginning of the sampling period and the other at the end.
Two spiked field samples shall be prepared using the same method as
the blank, except that a known amount of acrylamide is added to the distilled
water just prior to shaking the bag. The concentration of acrylamide in the
fortified samples should be approximately the concentration expected in hand
washes. One spiked field sample should be prepared at the beginning of the
sampling period and the other at the end.
3.0 EQUIPMENT WIPE SAMPLING PROTOCOL
Wipe samples shall be collected on representative surfaces of equip-
ment regularly handled by the chemical grouting operators to evaluate surface
contamination. The collecting media will be 37-mm glass fiber filters mois-
tened with distilled water. Clean disposable surgical gloves (individual
packaged powderless type) will be worn whenever the filters are handled. Care
should be taken not to contaminate the exterior of the glove when they are
donned.
The wipe samples are to be shipped back to the lab in glass vials.
Prior to the site visit, the vials shall be cleaned with Alconox and rinsed
twice with deionized water. The sample vials are to be labeled using barcode
adhesive labels. A set of six identical barcode labels will be printed for
each sample. Each set of labels will have a unique number. One of the adhe-
sive labels in the set shall be affixed to the sample vial and then placed
into individual zip-lock plastic bags. Another adhesive label from the same
set shall be affixed to the outside of the plastic bag. The other labels in
the set shall be placed inside the plastic bag. The sample numbers will be
logged with a laptop computer and light pen using barcode software.
At the sampling site, remove the filter from the packaging while
wearing clean disposable gloves. Moisten the filter with distilled water.
Gently wipe approximately 100 cm2 of the surface to be sampled. Use a mea-
sured 100 cm2 template as a guide to judge the size of the area to be wiped.
Without allowing the filter to contact any other surfaces, fold the filter
with the exposed side in, then fold it again. Return the filter to the la-
beled glass vial and seal with a teflon lined cap. Affix one of the barcode
labels on a Wipe Sampling Data Sheet and record the pertinent information
concerning the site location, complete description of the sampling location,
etc., that can be traced to the unique sample number. Seal the vials in its
A-10
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original plastic bag and store them in a chest containing ice or blue ice
packs for transport to the laboratory. Do not use dry ice. Ship the samples
to the laboratory at the end of each sampling day using a next-day delivery
service.
Wipe sampling shall be conducted on the following equipment; top of
the control panel desk in the Mobile Reveal and Seal Unit, outside of each
mixing tank after mixing operations, the back of work gloves, inside and out-
side of respirators, the handle of the injection gun (manhole sealing opera-
tions only), side of the packer (main and lateral line operations only), the
hydraulic hose connected to the injection gun or packer, and the side of a
safety cone in the road. Wipe sampling need not be limited to this list.
Wipe samples should be collected on any other frequently handled equipment
that appear to be contaminated, with grouting material.
3.1 Quality Control Field Samples
On each day of sampling two field blanks and two spiked wipe samples
shall be prepared. Field blanks of the collection media should be handled in
the same manner as the exposed filter media. Moisten a wipe filter with dis-
tilled water and immediately place the filter into a labeled vial container.
One field blank shall be prepared at the beginning of the sampling period and
one at the end of the sampling period. The blanks are to be stored and
shipped with the exposed samples.
Two glass fiber filters are to be spiked with a known quantity of
aery1 amide diluted to the approximate concentration used in the grouting mate-
rial (100 g of acrylamide per liter of water). The amount of aery1 amide added
to the filters should be approximately the levels that are expected to be
collected on the wipe samples during the field studies. One spiked sample
shall be prepared at the beginning of the sampling period and the other at
the end of the sampling period. The spiked samples should be handled, stored
and shipped in the same manner as the exposed samples.
4.0 REFERENCES
American Cyanamid Company. 1981. Stamford Laboratory: Validation of
an Analytical and Air Sampling Method for Acrylamide in Air.
Berkow SG. 1931. Value of surface area proportions in the prognosis of
cutaneous burns and scalds. Amer. J. Surg., 11, 315.
Diem K and Lentner C. 1970. Documenta Geigy Scientific Tables, 7th ed.,
Basel: J. R. Geigy, SA.
Durham WF and Wolfe HR. 1962. Measurement of Exposure of Workers to
Pesticides. Bull. WHO(26), 75.
Durham WF. 1965. Pesticides Exposure Levels in Man and Animal. Arch.
Environ. Health, 10, 842.
A-11
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Davis JE. 1980. Minimizing Occupational Exposure to Pesticides:
Personal Monitoring. Residues Review. 75, 33.
Midwest Research Institute. 1979. Sampling and Analysis of Selected
Toxic Substances; Task 1: Acrylamide for EPA/USEPA. Washington, D.C.
A-12
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APPENDIX B
FIELD OBSERVATION SHEETS
B-l
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GENERAL OBSERVATIONS - Sewer Chemical Grouting Operation
Site ID:__- Date: Time:
Signature: Title:
I. GROUTING CONTRACTOR INFORMATION
Name:
Address:
II. DESCRIPTION OF SITE
Street:
County: City:
State:
III. WORKFORCE
A. Number of employees on site:
B. Workforce Description
Job Title: Duties:
1.
2.
3.
4.
5.
B-2
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Site ID:
Signature:
Date:
Time:
Title:
IV. EMPLOYEE INFORMATION
NOTE: Fill out one information sheet for each employee on site
Employee Name: Job Title:
Comments:
A. Has this employee
received training?
If yes, specify.
B. Is this employee
licensed?
If yes, specify.
C. Did the grouting
material come in
contact with this
employee's skin?
If yes, specify.
Yes No
Yes No
Yes No
[] []
D. Has this employee experienced any of the following symptoms
since he/she has worked with grouting chemicals?
Yes No
[] []
1. Shortness of
Breath?
Yes
2. Muscular weakness []
of the hands, arms
legs or feet?
No
3. Numbness or
tingling of the
hands or feet?
4. Excessive sweat-
ing of the hands
or feet?
Yes No
Yes No
[] []
Yes No
5. Red or peeling [] []
skin of the hands
or feet?
Yes No
6. Excessive fatigue [] []
or lethargy?
B-3
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Site ID: Date: Time:
Signature: Title:
V. PRE-OPERATION SAFETY PROCEDURES:
A. Does this company have a written safety and Yes No
health program? [ ] [ j
B. Do the employees know the company's safety and Yes No
health policy? [] []
C. Are employees aware of the hazards of confined Yes No
space entry? [ ] [ ]
Yes No
D. Was an entry permit issued from the sewer district? [] []
E. Was confined space atmospheric testing performed Yes No
prior to entry into the sewer? [] []
F. Was confined space atmospheric testing performed Yes No
during the operation? [ ] []
G. Was the airspace in the sewer ventilated prior Yes No
to entry? ri ri
H. Was the airspace in the sewer ventilated during Yes No
the grouting operation? [j [j
I. Were procedures for stand-by, communication and Yes No
rescue followed? [] [j
Yes No
J. Is a first aid kit available? [] [j
K. Are any employees on site trained in first aid Yes No
and/or CPR? [ j [ j
Yes No
L. Are spillage cleanup kits available? [] []
Yes No
M. Is safety equipment kept in good operating condition? [] []
N. Are adequate skin and eye washing facilities Yes No
available on site? [] []
0. Are respirators fit tested? Do beard, sideburn, or Yes No
temple of glasses, etc. interfere with respirator fit?[] []
B-4
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Site ID: Date: Time:
Signature: Title:
VI. PERSONAL PROTECTIVE EQUIPMENT (PPE)
NOTE: Fill out one information sheet for each employee on site
Job Title:
Yes No Comments:
A. Impervious [] []
gloves?
Specify type.
Yes No '
B. Glove liners? [] []
Specify type. ^^
Yes No
C. Impervious [] []
Coveralls?
Specify type.
Yes No ~
D. Safety [] []
harness?
Yes No
E. Respiratory [] []
Protection? ZZ^ZZZZHZZZZZZI^ZI^IIIZZZI^^II
Specify type. ZZZ^ZZZ^HH^^HZIZIII^^Z^^I^~I
Yes No '
F. Head protection? [] []
Specify type. ^ZI^^IZ^IZZZZZZ^ZIII^IIZZl^Z
Yes No ~~
G. Eye protection? [] []
Specify type.
Yes No
H. Impervious boots? [] []
Specify type.
Yes No "
I. Change of [] []
Clothes? ~
Comments on general condition of PPE:
B-5
-------
Site ID: Date: Time:
Signature; Title:
VII. CHEMICAL GROUTING PROCESS:
Type of grouting operation performed? [] Main line sealing
[] Lateral line sealing
[] Manhole sealing
Step 1. Equipment preparation and assembly •»
A. Is there visible grouting residue on the Yes No
equipment? r i r i
B. Are gloves and protective clothing worn by Yes No
the operators during the assembly process? [] []
C. Was direct skin contact to grouting materials Yes No
observed during this operation? r] r i
General Observations:
D. Approximate duration of assembly operation. minutes
Step 2. Installing the equipment assembly in the manhole
A. Are gloves and protective clothing worn by Yes No
the operators during the installation process? [] []
B. Was direct skin contact to grouting materials Yes No
observed during this operation? [ ] [ ]
General Observations:
C. Approximate duration of installation operation. minutes
B-6
-------
Site ID: Date: Time:
Signature: Title:
Step 3. Chemical grout mixing operation
A. Product name of grouting material(s):
B. Name and address of manufacturer(s):
C. The monomer used was [] acrylamide [] acrylate
Yes No
D. Was spillage observed during the mixing process? [] []
Yes No
E. Was spillage observed during the gel test? [] []
F. Was spillage immediately cleaned up? Yes No
(specify method in general comments section) [] []
G. Was visible airborne dust observed during the Yes No
mixing operation? (acrylamide only) [] []
H. Was direct skin contact with chemical grouting Yes No
materials observed during the mixing operation? [] []
I. Was the mixing area ventilated? Yes No
(specify in general comments section) [] []
J. Was respiratory protection used during the Yes No
mixing process? [] []
K. Were bags, cups, grout test samples disposed Yes No
of in enclosed containers? [] []
L. Approximate duration of each batch mixing operation:
M. Quantities of chemical grout materials used:
General Comments:
B-7
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Site ID: Date: Time:
Signature: Title:
General Observations:
Step 4. Chemical grout injection operation " W
A. Was the injection process performed remotely Yes No
using a packer and video camera? [] []
B. Was the chemical grout injected manually using Yes No
an injection gun? [] []
C. Was respiratory protection used during manual Yes No
injection operations? [] []
D. Were there any apparent leaks in the injection Yes No
equipment? [ j [ j
E. Was direct skin contact to grouting chemicals Yes No
observed during the pumping operation? [] []
F. Was the injection gun equipped with an Yes No
anti-splash back guard? (manual operation only) [] []
G. Approximate duration of pumping operation. minutes
B-8
-------
Site ID:
Signature:
Date:
Time:
Title:
Step 5. Equipment disassembly and cleanup
A. Was spillage observed during the equipment Yes No
disassembly operation? [ ] [ ]
B. Was direct skin contact with grouting materials Yes No
observed during the disassembly operation? [] []
C. Was direct skin contact with contaminated Yes No
protective equipment observed when it was removed? [] []
D. Is grouting equipment routinely washed at Yes No
the end of the day? [] [j
E. Are respirators and protective clothing routinely Yes No
cleaned after each use? [] ri
F. Are respirator and protective clothing properly Yes No
disposed of or otherwise stored after use? [] []
G. Are disposal containers equipped with a tight Yes No
fitting lid? [j j-j
H. Are disposal and storage containers properly Yes No
labelled as to their contents? [] []
General observations and comments:
I. Approximate duration of disassembly operation.
J. Approximate duration of cleanup operation.
minutes
minutes
B-9
-------
Site ID: Date: Time:
Signature: Title:
VIII. SCHEMATICS
A. Worksite:
B. Service van:
B-10
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APPENDIX C
ANALYTICAL PROTOCOL
C-l
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1.0 Analytical Method for Acrylamide
1.1 This method has been developed for the determination of trace quan-
tities of acrylamide in field test samples (dermal pads, surface
wipes, air monitors, and hand rinses) for assessment of worker expo-
sure to acrylamide during chemical grouting operations.
1.2 This method yields the total weight of acrylamide present per field
sample. Information about the exposure levels of acrylamide must
be related to the type of sample and collection parameters.
2.0 SUMMARY OF METHOD
This method describes the procedures to determine the total quantity of
acrylamide present in field test samples. A general diagram of the
method is shown in Figure C-l.
The analysis procedure will consist of extracting acrylamide from field
test samples with a minimum known volume of acidic (pH 3.7) water. An
aliquot of the sample extract will be filtered and analyzed by HPLC.
The chromatograms of the sample extracts will then be obtained and digit-
ized by means of an A/D converter box interfaced with the HPLC system.
One or more field blank samples will be extracted and analyzed concomi-
tantly for comparative purposes. All of the sample and blank chromato-
graphs will be stored on floppy disks for future data manipulation.
3.0 INTERFERENCES
3.1 Due to the nature of the analytical technique used, this method is
susceptible to low UV interferences. Glassware should therefore be
thoroughly rinsed with the solvent before use.
3.2 All glassware used in the sampling and analytical procedures will
be thoroughly cleaned with Alconox and rinsed twice with deionized
water.
4.0 SAFETY
All manipulations made with acrylamide samples should be performed in a
fume hood or glove box. Gloves and other appropriate safety apparel
should be worn at all times. Solid and liquid waste should be disposed
of in the proper manner.
5.0 APPARATUS AND MATERIALS
5.1 Solution Preparation
5.1.1 1,000 mL graduated cylinder
C-2
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Dermal Pads
Air Monitor Samples
Wipe Samples
Field QC Samples and Blanks
Extract Aery1 amide with Known
Water Adjusted to pH 3.7
Hand Rinse Samples
(using known volume of rinse)
Standard Solutions
Lab QC Samples
Blanks
Analyze by HPLC
Calculate Total Weight of
Acrylamide (ug/L) for Sample,
Corrected for Dilutions.
Figure C-l. Flow chart for the determination of acrylamide
in field samples.
C-3
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5.1.2 1 gal. glass bottle
5.1.3 Glass volumetric pipets (TD) - 2, 4, 5, 6, 8, and 10 ml
5.1.4 Volumetric flasks - 50, 100, and 250 ml (low actinic or
foil-wrapped)
5.1.5 Disposable pipettes
5.1.6 Beakers - 100 ml
5.1.7 Filters - (0.2) urn Millex FG membranes (Millipore)
5.1.8 Glass jars (opaque) - 4 oz with Teflon®-!ined lid liners
5.1.9 10-mL disposable syringe (Luer tip)
5.2 Balance - Analytical capable of accurately weighing to 0.00001 g.
5.3 Shaker - Capable of shaking 4-oz jars at 1 oscillation/s. If a
wrist-action type shaker is employed, Teflon®-!ined lid liners must
be used on the glass jars.
5.4 Ultrasonic bath
5.5 HPLC data storage system
5.5.1 HPLC system
Instrument: Varian Model 5000 liquid chromatograph with autosampler
Van an UV-50 variable wavelength detector, Heath Model
255B chart recorder
Column: Altex Ultrasphere (TM) ODS dp = 5u, 4.6 mm x 25 cm
5.5.2 Nelson Analytical Model 4400 Chromatography Data System,
or equivalent.
5.5.3 Nelson Analytical A/D interface box, or equivalent.
5.5.4 Magnetic media for data storage - 5-1/4 in. floppy disks,
or equivalent.
6.0 REAGENTS
6.1 Acrylamide, electrophoresis grade
6.2 Deionized water, Milli-Q water system
6.3 Sulfuric acid, reagent grade
C-4
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7.0 METHOD VALIDATION
The analytical method will be validated by evaluating the method for
accuracy, linearity, and precision. Recovery will be determined by
spiking duplicate blank sample collecting media with a known quantity of
aery 1 amide. Validation will be confirmed if the average recovery effi-
ciency for acryl amide falls in the range 70 to 130%.
8.0 SAMPLE STORAGE
8.1 Unless instructed otherwise, field samples will be stored in the
dark at subambient temperature in their original packing containers
until the analysis is completed.
8.2 Individual samples will be retained at the discretion of EPA. Sub-
ambient temperature storage is advised if samples are to be retained
for long periods of time.
9.0 SAMPLE EXTRACTION
9.1 Carefully transfer the filter or train adsorbent sample to a 4-oz
opaque glass jar. Pipette 20 mL of water (pH 3.7) into the cassette
holder, cap tightly, and shake the cassette vigorously for 30 s.
9.2 Transfer the cassette rinse solution to the 4-oz jar using a dis-
posable glass pipette.
9.3 Place the jar in a shaker for 10 min. The shaker must oscillate at
least once per second.
9.4 The extract solution must be analyzed the same day of preparation.
10.0 STANDARD SOLUTION PREPARATION
10.1 Prepare a stock standard solution by accurately weighing (to the
nearest 0.1 mg) approximately 500 mg of electrophoresis grade
acryl amide and transferring the chemical to a 100-mL volumetric
flask. Dissolve the chemical to a 100-mL volume by adding the
acidic water-solution (concentration = 5,000
10.2 Dilute the stock standard solution prepared in 10.1, 5 mL to 250 mL
to make a 100 ug/mL standard solution.
10.3 Dilute the 100 ug/mL standard solution, prepared in 10.2, 5 mL to
50 mL to make a 10 ug/mL standard solution.
10.4 Dilute the 10 ug/mL standard solution, prepared in 10.3, 5 mL to
50 mL to make a 1 ug/mL standard solution.
C-5
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10.5 Dilute the 1 ug/mL standard solution, prepared in 10.4, 5 mL to 50 ml
to make a 0.1 pg/mL standard solution.
10.6 Standard solutions should be analyzed the same day of preparation.
10.7 Prepare check standard solutions by repeating steps 10.1 through
10.3.
11.0 PREPARATION OF SPIKED FILTER BLANKS
11.1 Place a blank filter into a 4-oz glass jar.
11.2 Using a 50-uL syringe, carefully load 30 uL of the acrylamide stock
standard solution from Step 10.1 onto the filter.
11.3 Analyze this spiked filter blank with the samples the same day of
preparation according to the procedures outlined in Steps 9.1-9.4.
11.4 Repeat Steps 11.1-11.5 for the duplicate spiked filter blank.
12.0 ANALYSIS OF ACRYLAMIDE SOLUTIONS
12.1 HPLC Operating System
Instrument: Varian Model 5000 Liquid Chromatograph with
Autosampler
Varian UV-50 variable wavelength detector, Heath Model
255B chart recorder
Column: Altex Ultrasphere (TM) ODS du = 5 p, 4.6 mm x 25 cm
Eluting Solvent: Water adjusted to pH 3.7 with sulfuric acid:
H20 (1:10 v/v)
Flow: 1.0 mL/min
Detection: UV at 200 nm
Chart: 0.1 in/min
Injection volume: 100 pL
Retention time of acrylamide: ~ 4 min
12.2 Analog/Digital Computer Interface Box Operating Parameters
Maximum input voltage: 10 V
Run time: 8 min
Sampling time: 1 point/s
12.3 Analysis of Acrylamide Solutions
12.3.1 Withdraw a portion of each standard, blank, or sample
into a 10-mL disposable syringe, attach a 0.2-um Mi Ilex
GF filter onto the end, and filter into a autosampler vial,
C-6
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12.3.2 Establish the calibration curve by injecting the series
of standards prepared in Steps 10.2-10.6 in duplicate using
the HPLC/data system described in 10.1-10.2. Adjust the
absorbance range attenuation and injection volume to make
the aery1 amide peak of the highest concentrated standard
~ 90% full scale on the chart recorder. Analyze the sam-
ples using duplicate injection with a mid-point standard
injected after every five samples to monitor the perfor-
mance of the HPLC system. Start the A/D box at the begin-
ning of the run.
12.3.3 If the concentration of the sample exceeds the linear
range of the calibration curve, prepare an appropriate
dilution of that sample and reanalyze it.
12.3.4 Plot the data file in the "re-detect" mode of the
integration software.
12.3.5 Obtain a hardcopy of the file integration for archiving
purposes.
13.0 CALCULATIONS
13.1 Using the integration software from Nelson analytical, prepare a
peak summary table of the integrated areas of the analysis.
13.2 Evaluate the calibration curve by calculating the correlation coef-
ficient and linear regression equation for the standard data. The
correlation coefficient should be greater than 0.995. Calculate
the relative standard deviation (RSD) for the responses of the mid-
point standard solution that was injected throughout the analysis.
The RSD should not exceed ±20%.
13.3 Calculate the total weight of acrylamide in each sample using peak
areas and the linear regression equation computed from the standard
data, corrected for sample dilution.
13.4 Calculate the recovery values for the spiked standards using the
following formula:
Recovery (%) = Found weight of acrylamide x 1QO
Actual weight of acrylamide spiked
13.5 Evaluate the precision of the analytical system by preparing a con-
trol chart of the responses from the mid-point standard solution
that was injected throughout the analysis of the samples.
C-7
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14.0 REFERENCES
American Cyanamid Company. 1981. Stamford Laboratory: Validation of
an Analytical and Air Sampling Method for Acrylamide in Air.
Berkow SG. 1931. Value of surface area proportions in the prognosis
of cutaneous burns and scalds. Amer. J. Surg., 11, 315.
Diem K and Lentner C. 1970. Documenta Geigy Scientific Tables, 7th
ed., Basel: J. R. Geigy, SA.
Durham WF and Wolfe HR. 1962. Measurement of Exposure of Workers to
Pesticides. Bull. WHO(26), 75.
Durham WF. 1965. Pesticides Exposure Levels in Man and Animal. Arch.
Environ. Health, 10, 842.
Davis JE. 1980. Minimizing Occupational Exposure to Pesticides:
Personal Monitoring. Residues Review. 75, 33.
Midwest Research Institute. 1979. Sampling and Analysis of Selected
Toxic Substances; Task 1: Acrylamide for EPA/USEPA. Washington, D.C.
C-8
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