&EPA
             United States
             Environmental Protection
             Agency
                 Office of
                 Toxic Substances
                 Washington. D.C. 20460
EPA 560/5-90-010
April 1990
             Toxic Substances
TEXTILE DYE WEIGHING
MONITORING STUDY
Supplement

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                                    EPA 560/5-90-010
                                    April 1990
TEXTILE DYE WEIGHING MONITORING  STUDY

              SUPPLEMENT
     Exposure Evaluation Division
  Economics and Technology Division
     Office of Toxic Substances
 U.S. Environmental Protection Agency
          401 M Street,  S.W.
       Washington, D.C.  20460
                                          Printed on Recycled Paper

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     This document has been reviewed and approved for publication b
the Office of Toxic Substances, Office of Pesticides and Toxic
Substances, U.S. Environmental Protection Agency.  The use of trade
names or commercial products does not constitute Agency endorsement
or recommendation for use.
                                 ii

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                              CONTENTS

A. QUALITY ASSURANCE PROJECT PLANS  	  A-l
   THE WASHINGTON CONSULTING GROUP  	  A-3
   PEI ASSOCIATES   	A-25
   MIDWEST RESEARCH INSTITUTE   	 A-47

B. DATA QUALITY OBJECTIVES	  B-l

C. LETTERS, TO ENCOURAGE PLANT PARTICIPATION  	  C-l

D. FIRST PHASE QUESTIONNAIRE	  D-l

E. IN-PLANT QUESTIONNAIRE	  E-l
                                 iii

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50272-101
 REPORT DOCUMENTATION
        PAGE
                        1. REPORT NO.
4. Title and Subtitle
 Textile Dye Weighing Monitoring Study
7. Author(s)
        EPA/Office  of Toxic  Substances
 9. Performing Organization Name and Address
  EPA/EED
  Economic and  Technology Division
  401  M St., S.W.
  Washington, D.C.   20460
3. Recipient's AcjBs»ioj»s|l*o.
  EPA  560/5-90-009
5. Report Date
April 1990
                                                                        6.
                                                                        8. Performing Organization Rept. No.
                                                                        10. Project/Task/Work Unit No.
11. Contract(C) or Grant(G) No.

(0

(G)
 12. Sponsoring Organization Name and Address
   EPA/OPTS
   Exposure Evaluation Division
   401 M St.,  S.W.
   Washingotn.  D.C.   20460	
                                                                        13. Type of Report & Period Covered
14.
 IS. Supplementary Notes
 16. Abstract (Limit: 200 words)
 Dye weighers  in textile dyeing and printing  plants are involved in the  weighing and  trans-
 fer of relatively small quantities of numerous powder dyes  and other chemicals.  This  re-
 sults in a  potential exposure to a diverse range of chemicals which exhibit a broad
 spectrum of toxicological  properties.   In order to gain more detailed information about
 workplace exposure to poweder dyes, a study  has been conducted to measure  concentrations
 of dyes in  the  workplace air, atid to characterize worker  activities and industrial hygiene
 practices.  This study was unique in that both government (U.S. Environmental Protection
 Agency) and industry (American Textile  Manufacturers Institute and Ecological and Toxico-
 logical Association of Dyestuffs Manufacturing Industry)  collaborated on an impartial
 basis and the dyehouses studies participated on a strictly  voluntary basis.

 The study included a survey of 24 randomly selected textile dyeing or printing sites which
 used power dyes.   At each  site, one worker was observed for an 8-hour shift; personal
 monitoring and  area sampling data were  taken.   Certified  industrial hygienists recorded
 worker activities,  duration of potential expsoure, personal and engineering controls in
 use,  and quantities and frequency of use of  each dye that was handled during the monitoring
 period.  Bulk samples of each dyes were also taken.  The  particulates collected on  the air
 monitoring filters  were analyzed for commercial dye content using a spectrophotometric
 method developed  for the study.	
 17. Document Analysis  a. Descriptors
    b. Identifiers/Open-Ended Terms
    c. COSATI Reid/Group
 18. Availability Statement
                                                         19. Security Class (This Report)
                                                         20. Security Class (This Page)
                                                                                   21. No. of Pages
                                                                                   22. Price
(See ANSI-Z39.18)
                                         See Instructions on Reverse
           OPTIONAL FORM 272 (4-7
           (Formerly NTIS-35)
           Department of Commerce

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        SUPPLEMENTAL A



QUALITY ASSURANCE PROJECT PLANS
             A-l

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 QUALITY ASSURANCE PROJECT PLANS



THE WASHINGTON CONSULTING GROUP
              A-3

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                                      August 10, 1986
QUALITY ASSURANCE PROJECT PLAN, Part I


                for  the


      TEXTILE DYE DRUG ROOM  STUDY


                  by


            Bradley  Schultz
      Washington  Consulting Group
         1625  Eye Street,  N.W.
        Washington,  D.C.   20006
      EPA  Contract  No.  68-02-4229


           Work Assignment  5
EPA Task Manager: Margaret G. Conomos
 EPA Project Officer:  Philip Robinson

    Design and Development Branch
      Office of Toxic Substances
Exposure Evaluation Division  (TS-798).
 U.S.  Environmental  Protection Agency
          401 M Street,  S.W.
       Washington, D.C.   20460
                 A-5

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                    QUALITY ASSURANCE PROJECT PLAN, Part I
                                    for  the
                          TEXTILE DYE DRUG ROOM  STUDY
                          EPA Contract No.  68-02-4229
                               Work Assignment  5
Approval  for:
WASHINGTON  CONSULTING GROUP
                                        Approval for:
                                        ENVIRONMENTAL  PROTECTION AGENCY
U
   AMdAl
                              5ate
Bryan K.  Porter
Quality Assurance Officer
                                                     cr.
                                        Margaret G.  Conomos
                                        Task Manager
to I
                                                                     Date
                                          Philip Robinson
                                          Project Officer
                                                                       Date
                                        ^
                                        E
                                           ileen Reilly-Wiedow
                                          Quality Assurance Officer
                                                                       Date
                                     A-6

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                   QUALITY ASSURANCE PROJECT  PLAN


     There are two parts  to this quality assurance plan.  The first
part is the statistical design and analysis section.  Following
this is Part II on the chemical analysis and field collection
procedures.  An overview  of the study may be found in the data
quality objectives for this study.


                          Part I Contents


1.   FRAME CONSTRUCTION

2.   FIRST PHASE QUESTIONNAIRE

3.   RESPONSE RATE FOR SECOND PHASE

4.   SELECTION OF PLANTS

5.   SELECTION OF WORKER WITHIN PLANT

6.   PILOT PLANT MONITORING

7.   QA VISITS

8.   VERIFYING IN-PLANT RECORDING FORMS

9.   DATA ENTRY

10.  DATA ANALYSIS

     APPENDIX: PROJECT PERSONNEL
                               A-7

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                   QUALITY ASSURANCE PROJECT PLAN

     Quality assurance  (QA)  is an integral part of the textile dye"
study.  The following describes the components of the QA program.

1.   FRAME CONSTRUCTION

     The list of  textile  plants using powder dyes (the frame) was
first constructed by using  the names provided by Davison's Blue
Book of textile manufacturers.  This was first cross-checked with
the Standard Industrial Classification listings to identify plants
within classifications  which include textile dyeing and printing
plants.  Then this list was  cross-checked with a list of plants
known to discharge dye-containing effluent.  This list was then
supplemented by EPA personnel  familiar with  the textile dyeing
industry.  Finally, as  a  last  check, textile dye industry
representatives affiliated  with the American Textile Manufacturers
Institute  (ATMI)  and the  Ecological and Toxicological Association -
of the Dyestuffs  Manufacturing Industry (ETAD) revised the list •
based on their  intimate knowledge of the industry.  Although as
with virtually  any frame,  it is known that  this list is not
perfect, numerous cross-checkings and reviews were made to ensure,
the highest quality possible at a reasonable cost.

     The final  examination  involved drawing  a (simple) random
sample of  240 plants from the list  of 1390  plants on the list.
This allowed EPA  and industry representatives to carefully examine
a list of  manageable size to insure  that no  systematic omissions'
were being made.   Furthermore, this allowed  for a detailed
examination of  the eligibility of each plant in this rapidly
changing industry (i.e.,  an eligible plant  is one that uses powder
dyes to color textiles).

2.   FIRST PHASE  QUESTIONNAIRE

     Although in-plant  monitoring of dye exposure levels is the
most  important  aspect  of  the study,  the first phase questionnaire
accomplishes a  number  of  QA tasks,  for the  monitoring study:

      1.    allows  a final  check on the frame.  If the 240 plants
           (randomly) selected were  to have  deviated in some
           systematic manner from  the known  make-up of the dye
           industry then the frame's  accuracy would have come into
           question. The  random  sample of  240 provides a manageable
           list  to carefully examine.

      2.    enhances knowledge of  the dye industry for preparation of
           in-plant monitoring

      3.    allows  the possibility  of  stratification of the sample
           for  in-plant monitoring  (the entire frame of 1390  is  too
           large to accurately classify with reasonable cost).
                                A-8

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     For  the  first  phase  questionnaire  itself,  responses are  being
hand checked  for  consistency  between answers  by  EPA Chemical
Engineering Branch  personnel  familiar with  the dye industry.
Results of the questionnaire  are  being  double-entered  to keep data
entry errors  to a very  low  level.

3.   RESPONSE RATE  FOR  SECOND PHASE

     One  of the most  critical components of a sound study is a high
response  rate, since  each refusal adds  an uncontrolled bias to the
results.  Given the potential for such  problems  in a voluntary
survey, we should take  steps  to increase the acceptance rate of in-
plant monitoring  before the first contact is made.

     In conformance with  government standards and good scientific
practice, we  should aim for a target of 75-80% participation.  Due
to the inherent difficulties  in this particular study and the poor
quality of the available  data, a  response rate of 60% of the 171
eligible  plants is a  reasonable lower limit on the participation
rate,-}since the necessary caveats attached to such results should
still not negate  the  worthwhile contribution of the study.   But
given potential refusals, we  need a strategy in place to encourage
participation in  every way possible.

     In preparation for actual methods  to bolster the response
rate, possible benefits and disadvantages of the in-plant
monitoring from the plant management's perspective were considered.

     Since there  are  only 30  plants for the on-site monitoring,  the
plan is to contact plants in  an individualized manner.   However,
the sequence of contacts  (extensive follow-up will be made  with
plants that initially refuse  to participate) for most plants will
be:

     1.    a telephone contact  to a high level company official
          asking  for  permission to monitor dye concentrations at
          the plant.  If  permission is granted,  a carefully crafted
          letter  on ATMI  letterhead will be sent explaining the
          study,  confirming the telephone agreement,  and describing
          the potential benefits  (in an industry-wide sense, and
          with respect to free plant monitoring  and a written
          report  on the site  visit).


     Based on the type of refusal met,  the following  contacts will
     be made in an order  appropriate for the particular plant
     contacted:

     2.    a letter from another appropriate trade group (e.g.,
          Carpet  and Rug  Institute,  or hosiery group,  if
          appropriate)
                              A-9

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     3.   a letter from Bill Dyson (Health & Hygiene) describing
          procedure

     4.   a personal contact to the Chief Executive Officer .of the
          company, from a Chief Executive Officer of another firm
          favorable to the study

     5.   a letter from a plant that Bill Dyson has already
          monitored stating that the monitoring team "was
          practically  invisible"

     6.   a letter from EPA assuring the reluctant plant in writing
          that enforcement action will not be taken based, on the
          site visit

     These letters will be carefully crafted to maximize the
likelihood of acceptance of monitoring.

     If a response rate of at  least 60% is not achieved, the study
will be reevaluated at that time. (But this worst case scenario is
not anticipated.)

     The refusing plants will  be characterized to determine if
there  is any detectable pattern in those refusing plants versus the
cooperative ones.

     For cooperating plants, the on-site arrangements will be made
by Bill Dyson.

4.   SELECTION OF PLANTS

     Of the 1390 plants  in the U.S. with the potential for dyeing
textiles 240 were chosen by simple random sampling and mailed
questionnaires;  the  result was:

     o   69 were determined to be ineligible (i.e., the plants
          were out of  business, or for some other reason did not
          really use powder dyes to dye or print textiles, with
          mechanical equipment);

     o   81 had responded by  the cutoff date, February 18, 1986;

     o   90 did not respond to the mailed-out questionnaire, but
          were determined  to eligible by EPA (CEB), ATMI, or ETAD
          (determination coordinated by CEB's George Heath).

     Several criteria  were considered for stratification, but the
one arrived at was  to  group the 171 eligible plants by whether or
not the plant  responded  to the mailed-out questionnaire.  Although
whether a plant  responded  to the mailed-out questionnaire was not
considered  to  be of  direct inherent value as a dividing
                               A-10

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characteristic  between  types of drug  rooms, examina6ion of  the
responses  to  the mailed-out questionnaire suggested  that  it  serves
as a proxy  for  carpet plants, since it was conjectured that  a
higher percentage of non-respondents  were carpet plants than the
percentage  among respondents.  Also the act of responding to the
questionnaire is seen to separate into two groups based on  the
likelihood  of allowing  in-plant monitoring (and thus reducing
somewhat the  refusal bias by replacing in-plant refusals with
another plant in the same strata).

     A completely random sample of 14 respondent eligibles will be
drawn from  the  list of  81 respondent  eligibles and 16 from  the list
of 90 (for  a  total of 30 plants for in-plant monitoring) in order
to represent  plants from each strata  with the number of plants
proportional  to the total number of plants in each strata.   If any
refuse to allow dye level monitoring, they will be replaced by a
plant from  the  same list that the refusing plant was on.

5.   SELECTION OF WORKER WITHIN PLANT

     One weigher from each plant will be selected.  First, the
shift of the  worker will be selected, based upon the facility's (or
plant manager's) seven  digit telephone number (obtained from the
first phase questionnaire) as follows:

No of shifts             Middle 3 digits of            Shift to be
operated                 telephone number              observed

   1                          000-999                     1st

   2                          000-499                     1st
                              500-999                     2nd

   3                          000-323                     1st
                              334-666                     2nd
                              667-999                     3rd

This will ensure a random selection of shifts for observation and
will provide  a mechanism for knowing the shift prior to the visit.
Although not  exact,  it will allow for a nearly random selection of
worker within plant.

     The employee to be monitored will be selected within the
chosen shift  as follows:

     1.    collect last  three digits of social security number (SSN)
          for all weighers from all dye areas
     2.    select worker with last three SSN digits closest to 500
                               A-ll

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6.   PILOT PLANT MONITORING

     Methods for in-plant monitoring, recording observations, and
making the chemical analysis, will be pre-tested at a pilot plant
(i.e., an actual plant with textile dyeing operations).

     Of particular note are the  testing of:
          the ability of  the  two member team to collect all of the
          information, particularly the number of weighings and the
          mass of dye measured
          the chemical analysis  method

7.   QA VISITS

     Three QA visits will be  made during the on-site visits, one at
the beginning, one near the middle, and one near the end of the
site visits.  A  report will be made on the quality.of the data
collected based  on information collected as shown in Appendix B.
(At the beginning of the  study,  corrections may be made to
procedures.)  This will also  allow the task team to become
intimately acquainted with the usefulness and  limitations of the
collected data.  Two site visits will be conducted by the Design
and Development  Branch of OTS (one of these by their contractor,
The Washington Consulting Group  (WCG)) and one by the Field Studies
Branch of OTS.   Besides enhancing understanding, the site visits
will check the procedure  for  selecting the shift and weigher chosen
(and thus also the drug  room  chosen), the determination of  the
number of weighers, and all other data collected at the site — but
with particular  attention paid to those items  which are recorded in
prespecified  categories.  Part II, sections 7  and 10 discuss
chemical audits  in detail.

8.   VERIFYING IN-PLANT RECORDING FORMS

                                                                on-
 si
     In-plant data collection forms will be compared by the two
  te industrial hygienists for accuracy of the information.

9.   DATA PROCESSING AND ENTRY

     ATMI mailed out the first phase questionnaire.  After return
to ATMI the coded, unidentified questionnaires were forwarded to
EPA and then to WCG.  All questionnaire responses were computerized
by WCG and double-entered to reduce keypunch errors to a minimum.
George Heath, of EPA's Chemical Engineering Branch, who is familiar
with the dyeing industry and its operations, may provide a list of
obviously incorrect questionnaire answers where there was a
misunderstanding or other error on the part of the respondent (if
corrections appropriate).  The list of changes would be provided to
the study partners (EPA and industry) along with a brief
explanation, and this list and explanation would be provided with
the summary table results.  At the end of the study, all response
forms will be returned to ATMI and destroyed.
                               A-12

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     Most of the second-phase data handling will be done in the
field and at the laboratory (discussed in part II of QA plan).
After the site visit and the verification of collected information,
the data collection protocol will be split into two parts:  the dye
monitoring cartridges and accompanying information, and the
observational results.  The observational results will be forwarded
to Margaret Conomos of the Design and Development Branch, and
George Heath.

     Margaret Conomos will then forward the entire data collection
record to Bradley Schultz of WCG, to conduct the statistical
analysis.  WCG will then enter the following information, for each
of the 30 plants, into a computer data base for statistical
analysis, and presentation of summary tables:

 1.  2-digit plant identification number
 2.  date (month, day, year)
 3.  shift (categorized as closest to 1st shift (7am-3pm),  2nd(3pm-
     llpm), or 3rd{llpm-7am))
 4.  total number of weighers working at  plant (all work areas, all
     shifts)
 5.  number of printing machines running  during observed shift
     (average of beginning and end of shift)
 6.  number of continuous/semi-continuous dyeing machines running
     during observed shift (average)
 7.  number of batch dyeing machines running during observed shift
     (average)
 8.  number of weighers working in observed drug room shift (note
     difference with item 5)
 9.  number of other workers working in observed drug room  shift
10.  age of worker at time of site visit  (number of years)
11.  life time work experience of monitored worker handling powder
     dyes (number of years)
12.  experience at observed facility as powder dye handler  (number
     of years)
13.  whether or not weigher wore dust mask during shift (yes/no)
14.  whether or not weigher ate in drug room during shift (yes/no)
15.  whether or not weigher smoked in drug room during shift
     (yes/no)
16.  total amount of all dyes weighed by  worker observed during
     shift (nearest pound)
17.  number of dyes weighed by worker observed during shift
18.  number of hours weigher monitored was in  drug room (nearest
     tenth of hour)
19.  dye level measurement (mg/m3),  time-weighted 8-hour average
     from personal monitor
20.  dye level measurement (mg/m3),  time  weighted 8-hour average
     from area sampler
21.  number of hours personal  monitor running  (nearest tenth of
     hour)
22.  gravimetric weight of all dust  on personal monitor cartridge
23.  gravimetric weight of all dust  on area sampler cartridge
                              A-13

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All data will be double-entered to keep keypunch errors to a
minimum.   Bradley Schultz will examine summaries of the data to
look for gross errors from what might be expected.  Suspicious
results will be reported to EPA's Margaret Conomos.

     Any computer programs written by WCG (i.e., Douglas Harder) to
fulfill the needs of the project will be checked for accuracy by
Bradley Schultz.  Reputable commercial computer packages will be
assumed accurate; however, Doug Harder of WCG will briefly examine
output as a final check.  The choice of software used, appropriate-
ness of the statistical analysis, and use of tables will be with
the approval of both Bradley Schultz and David Cox.


10.  DATA ANALYSIS

     There will be two major components to the data analysis:

     1.   characterizing the distribution of dye levels in plants
          and among weighers
     2.   examining the correlation of dye level with other factors

     Other items of interest are discussed in section 10.4 - 10.5.

     10.1 DISTRIBUTION OF DYE LEVELS IN PLANTS

     At each of the 30 plants, the 8-hour time-weighted exposure
(mg/mj) will be taken from the weigher's personal monitor.  From
these 30 data values, the distribution of plant dye levels will be
characterized.

     In particular, the average plant exposure level will be
calculated, along with its 95% confidence interval.  Also, the
85th, 90th, and 95th percentiles will be calculated and 95%
nonparametric tolerance limits will be obtained for the 85th and
90th percentiles.  Although a nonparametric (distribution-free)
approach for 95% tolerance limits is not possible due to the number
of plants in the study, the use of probability distribution-based
approaches (such as using the normal distribution) will be explored
for obtaining a 95% confidence interval for the 95th percentile.

     10.2 ESTIMATE OF AVERAGE WORKER EXPOSURE

     Estimates of average worker exposure in the population of
textile dye weighers and the 85th percentile of worker exposure
(the dye weighers are the only workers directly covered in this
study).

     In contrast with the analysis of section 10.1, this estimate
takes into account the  number of weighers working at each plant
and is weighted according to the number working at the monitored
                               A-14

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plant during a typical 24 hour period.  For example  statements
could be made about the 85th percentile of worker exposure by
weighting plant estimates by the number of weighers in each plant.
This would result in a statement such as "It is estimated that 85%
of weighers are exposed to levels lower than xxx mg/mj during an 8-
hour shift."  Note that this differs from the estimate of 85th
percentile of plant levels (objective 1) which results in a
statement such as:  "It is estimated that the average exposure in
85% of textile dyeing and printing plants is less than zzz mg/m ,
time-weighted 8-hour average" (xxx and zzz determined from study).

     This estimate will use the total dye exposure (mg/m3) obtained
from each worker's personal monitor.

10.3 CORRELATION OF DYE "LEVEL WITH OTHER FACTORS

     10.3A     Primary focus

          The exposure level (mg/m3) will be examined for
     correlation with:
                          r
     1.   mass of weighing during shift by worker of interest
     2.   number of weighings during shift by worker of interest
     3.   combination of the two above factors.

     If such a correlation exists, a functional relationship will
     be explored between the dye level and other factors.

     10.3B     Secondary measurements to examine association with
               dye level

     The rate of exposure (mg/m3/hr) will also be examined for
correlation with several other variables of secondary importance.
These are:             *••

     1.   Production volume of textiles (pounds per year), from
          mailed-out questionnaire
     2.   Management of dye house (vertical, commission or both),
          from mailed-out questionnaire
     3.   Management of dye house (public or private), from mailed-
          out questionnaire
     4.   Color index class of dyes used, for any dye used during
          observed shift by monitored weigher (acid,
          basic/cationic, reactive, direct, disperse, other), from
          site visit log as classified by Chemical Engineering
          Branch
     5.   Total number of dyeing and printing machines serviced by
          monitored weigher (average of beginning and end of shift
          numbers),  from site visit questionnaire
     6.   Fiber type dyed or printed (acrylic/modacrylic,
          rayon/cotton, nylon, polyester, other), from mailed-out
          questionnaire  '
                               A-15

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It should be noted that a data set of only 30 observations is
likely to result in some spurious large correlation when many
correlations are calculated.  Thus the correlations of this section
(10.2.B) will be interpreted in that light.
10.4 AMOUNT OF DYE WEIGHED OUT

     The average, and distribution of/ amount of individual dye
compund weighed out during a shift will be calculated and displayed
(averages and histograms will be presented by dye class and
aggregated).
10.5 SUMMARY TABLES

     10.5.1.  On-site questionnaire

     Summary tables will be presented for several other variables
collected from the on-site questionnaire with categorized
responses.  These will include averages or proportions as
appropriate.  The variables to be tabulated are:

1.   Number of textile dyeing plants in each EPA geographical
     region
2.   Number of
     typical 24
3.   Number of
4.   Number of
5.   Number of
6.   Number of
7.   Number of
8.   Number of
9.   Number of
     visit
10.  Number of
plants by number of weighers,  at all shifts  during a
 hour period
plants by pounds of dye weighed during shift
plants by number of dyes weighed during shift
plants by number of dye weighings during shift
workers by amount of time in drug room
workers that used dust mask during site visit
workers that used respirator during site visit
workers that smoked in drug room area during site

workers that ate in drug room area during site  visit
                               A-16

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     10.5.2    Mailed-out questionnaire

     As an appendix in the final report, the following variables
will be tabulated from the first-phase, mailed-out questionnaire:

*11. Number of textile dyeing plants in each EPA geographical
     region
 12. Number of plants by number of dyeing or printing operations
     within the company that owns the selected plant
@13. Number of plants by management of house (vertical, commission,
     or both)
@14. Number of plants by management of house (public, or private)
@15. Distribution of plants by product volume
 16. Number of plants by product line (carpet,  yarn, fabric, other)
#17. Number of plants by type of dyeing or printing equipment
     available (batch, semi-continuous/continuous, printing)
@18. Number of plants by fiber dyed or printed (acrylic/modacrylic,
     rayon/cotton, nylon, polyester, other)
@19. Number of plants by color index class of powder dye (acid,
     basic/cationic, reactive, direct, disperse,  other)
 20. Number of plants by number of dyes weighed per 24 hours (less
     than 10, 10 to 20, over 20)
&21. Number of plants by pounds of dye used per 24 hours (less than
     50, 50 to 200,  over 200)
&22. Number of plants by number of powder dye weighings per 24
     hours (less than 50, 50 to 500, over 500)
 23. Number of plants by number of dye weighing rooms ( 1 room, 2
     or more rooms)
 24. Number of plants by number of worker shifts  per 24 hours (1,
     2, 3)
 25. Number of plants by number of operating days per week
     (1 to 4, 5, 6 or 7)
 26. Number of plants by number of employees exposed to powder dyes
     (1, 2, 3, 4 or  more)
Notes
     This is also tabulated from site visit data
     Similar information is also collected in the on-site
     questionnaire and is used in the secondary correlation
     analysis (see Appendix A)
     A portion of the data on this variable will be used in the
     secondary correlation analysis (see Appendix A)
     Similar information also collected in the on-site
     questionnaire and is used in the primary correlation analysis
                               A-17

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     10.6 AREA SAMPLER RESULTS

     Although the area sampler measurements will be chemically
analyzed for each plant, the results will be used solely for post-
study exploratory work and possibly for quality assurance purposes
(if a s.trong correlation is found between personal samplers and
area sampler results).  The area samplers may provide a useful
quality assurance role at the data analysis phase.  If the personal
monitor result is suspect at one plant for some reason, the area
sampler measurement provides a rough cross-check for such a suspect
value.  As in any study, it is hoped that no such incidents will
take place.
                               A-18

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APPENDIX; PROJECT PERSONNEL

     Bradley Schultz is the WCG work assignment leader.  He will be
the statistician involved in the design and analysis of the study.
David Cox is the overall Project Director for the WCG contract with
EPA.  Doug Marder and Keith Johnston will set up and oversee the
creation and use of the data bases.  Terri Stiteler will manage the
data bases and coordinate the data entry.  Credentials are on file
with the Design and Development Branch of EPA.
                              A-19

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                            APPLN'DIX B



               TEXTILE DYE/DRUG ROOM EXPOSURE STUDY
                          =  _ . ..    .» -S-f  < ;  ,.    .,-      -*


            QUALITY ASSURANCE AUDIT FOR A PLANT*VISIT
Section I.  Basic Audit  Information
A.  Auditor Information
  1.  Nane(s)/Affiliation;
  2.  Date of Audit:                ,  19
B.  Textile  Plant  Information
      Plant  I.D.
C.  Industrial  Hygienists:


  1.  Health  and  Hygiene,  Inc
  2.  PEI
                             A-20

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Section II.  Sampling  Design

              ->   ~   ••••
  1.  Was the selection of  the  shift and/or the weigher clone  on  a

      random basis?    Yes       No
                             A-21

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Section III  Air Monitoring Methods








  1.  Were all air sampling instruments calibrated




      accurately prior to field use?   (Note means of



      verification). Yes      No








  2.  Were the personal samplers operating at a  flow rate between




      2 and 2.5 liters/minute?  Yes	  No	








  3.  Did anything occur that might interfere with  the airflow on




      the personal sampler  (i.e tubing became twisted)?



      Yes	   No	








  4.  Were the area  samplers operating at a flow rate between 5



      and 8 liters/minute?  Yes	   No	








  5.  Was the location of the area samplers appropriate?




      Yes	   No	








  6.  Were filter blanks taken  into the field?   Yes	  No	








  7.  Did splashing  of liquids  occur  onto the filter?




      Yes     No
                             A-22

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Section IV  Drug Room Observations








  1.   Was each container of bulk dye taken labelled and




      appropriately identified on the corresponding form?



      Yes	  No	








  2.   Were appropriate methods used to collect bulk dye samples,




      i.e. non-obtrusive and non-dust-generating?  Yes	  No	
  3.   Were all entries and exits into and out of the drug room by




      the weighes recorded?  Yes	  No	








  4.   Were all weighings recorded with name of the dye noted and




      corresponding to the name of the bulk dye sampled?



      Yes	  No	








  5.   Was a validation of all dyes recorded conducted between the




      two industrial hygienists?  Yes	  No	
                             A-23

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Section V  Qualitative Performance of  the Field Visit








  1.  Was a positive rapport evident between management and  the



      visiting industrial hygienists?  Yes	  No	








  2.  Was management well-informed about the objectives of the



      study and fully co-operative?  Yes	^_ No	








  3.  Was the weigher who was wearing  the sampling device



      informed about the objectives of the  study and fully



      cooperative?  Yes	  No	








  4.  Were the weigher's work activities altered or  interrupted



      by the visiting industrial  hygienists?  Yes	 No	
                             A-24

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QUALITY ASSURANCE PROJECT PLANS




         PEI ASSOCIATES
             A-25

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DRAFT                                   Sec t iCJi:  I . 0
                                        Revision:   1.
                                        Date:  July 14, 1986
                                        Page:  1 of 1
                           SECTION 1.0


                          EPA/ETAD/ATMI


                       DYE EXPOSURE STUDY
                    QUALITY ASSURANCE PROGRAM
                               FOR
                FIELD SAMPLE AND DATA COLLECTION
                                 A-27

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                                        Section:  2.0
                                        Revision:  1
                                        Date:  July 14, 1986
                                        Page:  1 of 1
                           SECTION 2.0

                         TABLE  OF  CONTENT
Section         Heading

 1.0    Title Page

 2.0    Table of Content

 3.0    Project Description

 4.0    Facilities, Equipment
        Consumables, and Services

 5.0    Sample and Data Generation

 6.0    Data Processing

 7.0    Data Quality Assessment

 8.0    Corrective Action

 9.0    Documentation and Reporting

10.0    Personnel and Management
Pages  Revision    Date

  1       1      07/14/86

  1       1      07/14/86

  3       1      07/14/86
3
6
1
1
1
1
1
1
1
1
1
1
1
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07/14/86
07/14/86
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07/14/86
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                                  A-28

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                                       Sec L i en:
                                       Revision:  1
                                       Date:   July 14, 1986
                                       Page:   1 of 3


                          SECTION 3.0

                      PROJECT DESCRIPTION


The American  Textile Manufacturers  Institute  (ATMI),   the U.S.
Operating Committee  of the  Ecological and Toxicological
Association of the Dyestuffs Manufacturing Industry  (ETAD),  and
the  U.S.  Environmental Protection Agency  (EPA)  are  jointly
sponsoring a  study  to  assess the  potential  exposure of  dye
weighers in textile drug rooms  to airborne dye dust.   Data from
this study will be used to estimate  worker exposure  as new dyes
are proposed  for introduction  into commerce  and  in addressing
concerns on existing products.

The  study is divided  into three parts.   The  first is  the
selection of textile facilities  to be visited.  This will be done
on a random basis from the total  universe  of  textile dyeing and
printing facilities  in  the U.S. by the Washington Research Group
under contract to the  EPA  with  assistance from ETAD and  ATMI.
The second is the  collection of data and samples at the  30
facilities selected.  This will  be done by  Health & Hygiene, Inc.
as a contractor to ETAD  and ATMI,  and is the  subject  of this
quality  assurance plan.  The  third  is  the analyses  of samples
collected at  the facilities  to  determine the  dye content of the
airborne dust  in the drug rooms.   This  will be done  by Midwest
Research Institute as a  contractor to the EPA and is the subject
of a separate  quality assurance  document.

The field sample and  data  collection part  of this study  is
comprised of the following activities:

     3.1  Preliminary Arrangements

          Agreement by a  selected  facility to participate in the
          study will be  obtained by ATMI with assistance from
          ETAD and  others.  Once consent  has  been given,
          telephone contact will be  made by Health  & Hygiene to
          schedule a visit.  Preliminary  information necessary to
          prepare  for the  visit such as the number  of shifts of
          drug room operation and  the approximate number of dyes
          weighed per shift,  will  be  obtained during this contact
          (Attachment 3-1).  Other activities including obtaining
          necessary supplies, calibrating air sampling pumps, and
          preweighing sample filters and  blanks  will  be done
          prior to the visit.

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                                  Sec::.;.:::   3.0
                                  Revision:   1
                                  Date:   July 14, 1986
                                  Page:   2  of 3
3.2  Field Visits
     Visits to the  selected facilities will  be  made by a two
     person  team of industrial  hygienists,  one each from
     Health  &  Hygiene,  Inc.  and PEI Associates,  Inc.   The
     team  will  arrive  at the facility at least four hours
     prior  to   the start  of   the  shift selected  for
     sampling/observation to obtain  information about the
     facility,  determine how to obtain dye  weighing data
     most  efficiently,  and  take a brief  familiarization
     tour.  During  the selected shift, personal and area air
     samples  will  be taken;  bulk samples of  dyes weighed
     during  the shift collected;  temperature, barometric
     pressure,  and relative  humidity  measurements made; the
     time  the  monitored  employee spends in  the drug room
     recorded;  data on  the number  and quantity  pf  dyes
     weighed obtained; and observations about conditions and
     controls in the drug  room made.  Upon completion of the
     sampling and observations a closing conference will be
     held with management.

3.3  Gravimetric Determinations

     Total  potential dust exposure of  the employee during
     the monitoring period will  be determined  by  reweighing
     the  air sampling filters  collected at each  facility.
     After weighing, the  filters and bulk dye samples will
     be  sent to Midwest Research  Institute  (MRI)  for
     analytical determination  of the dye content on the
     filters.   The gravimetric  determination  of total dust
     will provide an  upper  bound  against which  the
     nonspecific analysis  by MRI  can be compared.
                            A-30

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                                         :."•-•-• i. 2 c.:-.:  -'• - 0
                                         Revision:  1
                                         Date:   July 14, 1986
                                         Page:   3 of 3
                          ATTACHMENT 3-1

                    PRE-VISIT  TELEPHONE CONTACT
Facility:

Address:
Contact:
Telephone No.
Scheduled Visit Date:
Number Of Shifts Drug Room Operated;
   *

Shift to be observed/sampled:  	

Comments:  	                	
Approximate number dyes weighed/shift:

Approximate number dyes weighings/shift:

Local accommodations:  	
                                  A-31

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                                       Section:  4.0
                                       Revision:  1
                                       Date:  July 14, 1986
                                       Page:  1 of 3

                           SECTION 4.0

        FACILITIES, EQUIPMENT, CONSUMABLES.  AND SERVICES

4.1  Facilities

     Filter  weighing and  reweighing will be  done  at Burlington
     Industries'  Industrial  Hygiene Laboratory,  Doyle  Street.
     Greensboro,  North Carolina.  This laboratory has a constant
     temperature-humidity room in which  the  filters and blanks
     can be equilibrated prior to each weighing.

     Sample pump  calibrations  will be performed  in the industrial
     hygiene laboratory at Health & Hygiene, Inc.


4.2  Equipment

     Equipment which will be used on this project includes:

     • Mettler ME 30 microbalance, capable of weighing to the
       nearest microgram

     * Gilian HFS 113  air sampling pumps with timers

     • Cast Model 1531 vacuum  pumps with critical orifices

     • GCA/Precision Scientific wet test meter

     • Buck Model M-5  mini-calibrator

     • Bacharach  Sling Psychrometer


     4.2.1     Calibration

               The Mettler ME  30 microbalance is checked prior to
               each set of weighings  with an  internal  100  mg
               weight.  Zero checks are made periodically during
               the  weighings to assure  that  drift  is not
               occurring.  If  the balance cannot be calibrated or
               zeroed  a Mettler service  representative  will  be
               called.

               Flow rates  for  the Gilian  sampling  pumps  will  be
               calibrated in the laboratory prior to  field visits
               with an  SKC 311-100 soap film  calibrator.   Prior
               to site visits  while in the  field the Buck mini-
               calibrator will be used.  Further, the

                                A-32

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                                        sec ._•.::::   4.0
                                        Revision:   1
                                        Date:   July 14.  1986
                                        Page:   2 of 3
               rotameter setting  will be noted during calibration
               and checked periodically during sampling.  Should
               low  flows  be noted during  sampling,  a  post-
               sampling  flow rate  will  be determined with the
               mini-calibrator and an average value used.

               Flow rates for the Cast vacuum pumps with critical
               orifices will be  determined prior to field visits
               with the wet test  meter.
     4.2.2     Maintenance

               Maintenance  of  equipment used in this project will
               be  done  according  to  the  manufacturer's
               specifications.  The Mettler microbalance has just
               been serviced  and is on a yearly  schedule.   All
               other equipment  is serviced as needed.
                         ;
4.3  Consumables

     Consumables supplies which will be used during this project
     include:

     • Gelman  Vinyl  Metricel VM-1 filters with support pads

     • Gelman  4339   3-piece cassettes

     . UV Light Absorbing Plastic Bottles (for bulk samples)

     • Plastic spoons

     • Plastic bags

4.4  Services

     Filter weighing  will  be done  at Burlington Industries'
     Industrial Hygiene  Laboratory.   Services to be  provided by
     this laboratory include:

     • Equilibrate,  preweigh, and place filters in numbered
       cassettes prior to field visits, including
     • field blanks
     • Equilibrate and reweigh filters and blanks after
       sampling                  'J
                               A-33

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                                 Section:  4.0
                                 Revision:  1
                                 Date:  July 14, 1986
                                 Page:  3 of 3
Place samples in unused cassettes
Record results in a permanent laboratory notebook
Send samples, cassettes, field blanks, filter blanks
and recorded results of weighings to MRI
                         A-34

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                                       ^ec: - !•.,:•:  5.C
                                       Revision:  1
                                       Date:  July 14, 1986
                                       Page:  1 of 6
                          SECTION 5.0

                   SAMPLE AND DATA GENERATION
5.1  Employee Selection

     For each of  the  thirty  (30) facilities visited, only one dye
     weigher will be  selected for exposure monitoring.  This will
     be done in a random fashion.  the  shift  to  be observed and
     sampled will be  selected based on the middle three digits of
     the facility's  (or  facility contact's) seven digit telephone
     number as follows:

       No.  Shifts      Middle 3 digits        Shift to be.
        Operated      of  telephone number    observed/sampled

           1              001-999                1st
           2               001-500                1st
                          501-999                2nd

           3               001-333                1st
                          334-666                2nd
                          667-999                3rd

     This  will ensure  a  random selection  of the  shift  for
     sampling  and  will  provide  a mechanism f6r knowing the shift
     prior  to  the  visit.   If contact with the  facility indicates
     that the  shift selected in the above fashion is unreasonable
     due  to the dye weighing activities  being  conducted,  then an
     alternative  selection will  be made based  on professional
     j udgment.

     Where  the  facility has more than  one dye weigher  on  the
     selected  shift,  the  one selected for monitoring will  be  the
     dye  weigher whose  last three Social  Security  Number  digits
     are  closest  to 500.   Assistants  and helpers will  not be
     considered  for inclusion.  Selection of the employee will be
     done in the opening  conference  with management.  The  method
     of selection  will  be documented for  both  shift and weigher
     if different  from normal procedure (page 2 of survey form.
                                A-35

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                                      Section:  5.0
                                      Revision:  1
                                      Date:  July 14,  1986
                                      Page:  2 of 6
5.2  Air Sample Collection
     At each facility visited,  a total  of four air  samples will
     be collected,  two worn by the dye weigher  selected for
     monitoring and two at stationary locations in the drug  room.
     Air will be drawn through pre-weighed 37 mm polyvinyl
     chloride filters  (Gelman  VM-1)  in three-piece cassettes.
     Personal samples  will be  taken using  portable, battery
     operated pumps worn by the employee  as he performs his  work.
     Flow  rates  of  approximately  2.0 L/min  and a sampling
     duration  of  seven  or more hours, including  breaks, will be
     used.   Stationary  area samples  will be  obtained using
     electrical vacuum pumps operated at approximately 7.4  L/min
     for roughly  the same  duration as  the  personal samples'.
     Sampling will—be done  in an  "open-face"  configuration.
     After  collection, the samples will be recapped, returned to
     the laboratory, equilibrated,  reweighed  to  the nearest
     microgram, and  submitted  to MRI  for  determination of dye
     content.

     5.2.1.    Sample Identification

              As  the filters  are preweighed  and  placed into
              cassettes, a unique  identifying number will be
              written on the bottom  section of the cassette with
              an  indelible marker.   This will serve  as the
              sample identifier  on all documentation  of the
              visit  and  subsequent  analysis.   When the  filters
              are reweighed after collection and placed into new
              cassettes,  the bottom  section of the new cassettes
             , will  be identified by  the  same number  as the
              sample plus a prime   (') mark  to distinguish it
              from  the  original  cassette.   Both will  be
              submitted to MRI.

     5.2.2     Duplicate Personal Samples

              Both  personal  samples  at  a  facility will be
              collected from the same dye weigher.

     5.2.3.    Air Flow Checks

              The personal  sampling pumps  used  have electronic
              feedback  systems which  maintain set flow  rates
              even  as  dust  on the filter increases resistance.
              These  pumps also  have  rotameters.   The setting of
              the rotameter will be  noted during calibration and

                                A-36

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                                      Sec L _cn :   :>. J
                                      Revision:  1
                                      Date:  July 14, 1986
                                      Page:  3  of 6
              observed  two to three  times during  sampling  to
              ensure that no change has occurred.  If it appears
              that  the  air flow rate  has changed,  a post-
              sampling flow calibration check will be made using
              the mini-Buck calibrator.   Should significant
              variation  be found the  average of the  pre-  and
              post-sampling calibrations  will be used  as  the
              flow rate for dust  level calculations.

              Air flow rates for  the two area  samplers will  be
              maintained with critical  orifices.   These  are
              generally quite  steady.   A rotameter will be used
              to check air flow periodically during the sampling
              period.  Should  significant variation  be found,  a
              post-sampling calibration will  be made  and  the
              average value used  as the flow rate.

5.3   Data Collection

     Information on  the  time the dye  weigher being observed
     actually  spends  in  the  drug  room,  the  number of  dye
     weighings made,   and  the total quantity  of  each  dye weighed
     during  the  sampling  period will be  obtained.   Observations
     will  be made of ventilation in  the drug  room,  the  use  of
     personal protective equipment, work practices being used,
     and cleanliness  of  the  area.    In addition,  limited
     demographic data will be obtained from the dye weigher being
     monitored/observed and temperature,  barometric pressure,  and
     relative humidity  in the  drug room will be  recorded.   The
     use of any particularly dusty dyes will be recorded.

     5.3.1     Exposure Duration

              Dye weighers are typically quite mobile.  They
              move freely in and  out of the drug room.   Since it
              is assumed that the majority of exposure occurs
              while  he is in the drug room,  this parameter will
              be measured.

              The boundary of  the drug  room will be  established
              by agreement between the  two site visitors.    A
              rough  sketch of the dye weighing area will be made
              indicating the boundary chosen.  The  actual time
              the dye weigher  being  observed spends  in the drug
              room will be measured by recording the  time, to
                               A-37

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                                  Sectjon:   5.C
                                  Revision:   1
                                  Date:  July 14,  1986
                                  Page:  4  of 6
          the nearest minute,  that he enters and exits the
          area.   The total potential exposure time will be
          the sum of  the periods he spends in the drug room.

5.3.2     Weighings of Solid Materials

          All weighings of solid  materials made  during the
          sampling period will  be observed  to determine
          three  important parameters - the total number of
          individual weighings made,  the total number of
          individual  solids weighed, and the total mass or
          quantity  of  each  solid .weighed.   Whenever
          possible,  batch tickets used by the  dye weigher
          will be obtained and  the  weighing data  recorded
          from these.  If batch  tickets  are  not available.*.
          the data will  be obtained by  direct  observation
          and,  if necessary, questioning the dye  weigher.

          The method  for obtaining  these data  will be
          discussed with management  in  the  preliminary
          conference.   Their  suggestions as to the most
          efficient way to obtain  the data in their  facility
          will be considered and used where possible.

5.3.3     General Observations

          During  the sampling  period,  general observations
          will  be recorded about  the type of personal
          protective  equipment used by the dye weigher,  work
          practices  used,  the cleanliness of  the drug room,
          and engineering  controls such  as  ventilation  used
          to reduce dust  exposure.  Whether or  not the dye
          weigher smokes will also be recorded.

5.3.4     Dye Weigher Interview

          During  a break period,  the  dye weigher will be
          asked  several questions to determine  his age and
          how many years  he has been handling dyes, both at
          the facility visited and elsewhere.

5.3.5     Temperature/Relative Humidity

          Temperature, barometric pressure,  and  relative
          humidity will  be measured intermittently  during
          the sampling period.

                           A-38

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                                       Section:   5.0
                                       Revision:   1
                                       Date:   July 14,  1986
                                       Page:   5  of 6
5.4  Bulk Dye Samples
     For each individual  dye weighed  during  the  sampling period,
     a bulk sample of approximately one ounce will be obtained.
     These samples will be taken from the original  dye drums used
     by the weigher.  Disposable plastic spoons will be used to
     avoid contamination.

     The bulk  dye  sample bottles will be  labeled  sequentially
     using the labels provided  by  MRI.   Corresponding labels  (of
     the same number)  will be placed  on  the  data sheet where  the
     full  name of the dye,   its lot number,  if possible,  and  its
     supplier will be recorded along with  the  name used on  the
     batch ticket or weighing record.   Samples will also be taken
     of those solids wheighed by the  weigher which may interfere
     with  the dye analysis   (e.g.  colored materials or chemicals
     which may react with dyes).

5.5  Filter Weighings

     Air  sampling  cassettes  will b-e  returned  to  Burlington
     Industries' Industrial Hygiene Laboratory.   They  will be
     equilibrated  overnight in  the constant  temperature  and
     humidity area  prior   to  being  reweighed  to  the  nearest
     microgram.   Ten field blanks - preweighed  filters in
     cassettes  through  which  no  air has  been  drawn which have
     been  handled and  transported  with the sample  filters - will
     be equilibrated  and  weighed  at the same time.  The average
     weight change  of  these  ten blanks will  be used as the blank
     correction values  in  calculating dust  exposure  levels.
     Significant problems  in filter weighing should be detected
     through the use of these blanks.

     Note:  The ten  field blanks  may apply  to  air samples from
     more  than  one facility if two  or  more are visited in  the
     same  week.

5.6  Shipping  and Handling

     After  collection and  reweighing, all materials  will be
     shipped  to MRI.   This includes bulk  samples, air sample
     filters,  and data collection forms.

     Bulk  sample bottles will be placed  in  plastic  bags in groups
     of four.   These will be shipped to MRI separately from  the
     air samples to  avoid  the  potential for contamination.   To
     minimize  handling, bulk samples  will  be sent directly from
     Health &  Hygiene.

                               A-39

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                                  Sec Li on:  5.0
                                  Revision:  1
                                  Date:  July 14, 1986
                                  Page:  6 of 6
Air samples will be  hand  carried  to Burlington Industries'
Industrial Hygiene Laboratory.   After reweighing,  they will
be  shipped  directly  to  MRI.    For each  facility,  these
shipments will include the four air sample  filters  in new
cassettes, four empty field cassettes, two field blanks, and
ten unused filters from the same lot.

Data  collection  forms, minus  the  identifying  cover sheet,
will  be  hand  delivered along with  the air samples  to
Burlington's laboratory.  After post-sampling weights are
recorded, the  forms  will  be  sent  along  with  the samples to
MRI.   The facility  identification  sheet will  be  mailed to
ATMI from Health & Hygiene.
                           A-40

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                                        Sec.: t \ o;>:   6 .1
                                        Revision:   1
                                        Date:   July  14,  1986
                                        Page:   1 of  1


                           SECTION  6.0

                         DATA PROCESSING


6.1  Collection

     All data will be collected manually.  Recording will be done
     legibly  in  permanent  ink  on  worksheets.   Each  person
     involved in recording  data will sign and date the worksheet
     Corrections will be  initialed.

6.2  Data Reduction

     ATI  sample  manipulations will  be  clearly documented.
     Standard data reduction  techniques  will be used.

6.3  Data Validation

     The data validation  process  will include:

     • Air flow rate  checks

     • Timing checks  with second  watch

     * Checking calculations

     * Comparisons with original batch tickets

     • Reviews for internal consistency by site visitors

     • Use of field blanks

     The site visitor from Health  & Hygiene will  be responsible
     for assuring  data validity.

ۥ4  Transfer

     Original recording sheets will be included with field visit
     documentation to allow checking of data transfers at a later
     date.
                                A-41

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                                       Seclion:   7.0
                                       Revision:   1
                                       Date:   July 14,  1986
                                       Page:   1  of 1

                          SECTION 7.0

                     DATA QUALITY ASSESSMENT


7.1  Filter Weighings

     The microbalance used  for filter weighings  is capable of +1
     microgram  precision  and, since net weight change is being
     measured,  accuracy.  However, zero drift is  slightly greater
     than this,  approximately +3 micrograms.   Zero will be reset
     after every third weighing.

     Greater variability is caused by moisture collection on the
     filters.  A constant temperature and relative humidity room
     is  used to equilibrate the  filters before weighings to
     reduce this variability.  Ten blank filters  through which no
     air has been drawn are weighed and reweighed with the sample
     filters.  The average weight change of  these blanks is used
     as  a  blank correction  in calculating dust levels.   This
     correction is generally  less  than +30 micrograms.

7.2  Traceability of Samples  and Data

     All air and bulk samples will  have unique identification
     numbers.  All data collected on the samples will be related
     to  these  numbers.   Simplified  traceability logs will be
     completed  and  signed  when samples  are  transferred to
     Burlington's laboratory  and to MRI.

7.3  Completeness

     The Health &  Hygiene site  visitor will  review all data
     collected prior  to  leaving  the  facility   to  assure
     completeness.   This  will include  a verification that the
     record of dyes weighed/sampled is consistent.
                                A-42

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                                       b.-ctior,:  f.O
                                       Revision:  1
                                       Date:  July 14,  1986
                                       Page:  1 of 1
                          SECTION 8.0

                       CORRECTIVE ACTION
The Health & Hygiene site visitor has primary responsibility  for
taking  corrective actions  as necessary.  Examples of  problems
which might be  encountered and possible corrective actions  are as
follows:

   Personal  sampling pump  stops -  Record time  from built-in
   timer,  submit  sample, make second sample primary

   Flow rate variation during  sample - average pre- and post-
   sampling rates

   Large blank  filter weight variation - check balance, examine
   filters for  loss of material or contamination from backup pad.

   Failure  to  obtain bulk  dye  sample  - Contact  facility  for
   assistance in  obtaining

   Incomplete dye weighing  data  - Obtain original batch tickets
   from facility  if possible

   yfater spray  or other inadvertent contamination  of  air  sampling
   filter - use  second sample  if  not  contaminated,  conduct
   sampling again
                               A-43

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                                       S-=c l io:.:   9.0
                                       Revision:   0
                                       Date:   June 9,  1986
                                       Page:   1  of 1


                          SECTION 9.0

                   DOCUMENTATION AND REPORTING

9.1  Documentation

     Field  sample and  data collection  will be  documented  in
     permanent ink on the  forms  provided by  the EPA.  The data
     related to sample collection will  be compiled by the  Health
     & Hygiene site visitor and Burlington lab personnel.  Other
     data will be completed by the PEI,  Inc.  site visitor.  Any
     corrections  will be marked through and  initialed.  Raw data
     on air flow  calibrations and  filter weighings for which  no
     space  is  provided  on  the EPA  forms will be  recorded  on
     standard  forms from  Health  &  Hygiene  and  accompany the
     documentation for a facility visit.

9.2  Transmittal  to MRI

     MRI is acting as the central repository for all data  related
     to this study.  Data collected prior to  and during  facility
     visits will  be  submitted to MRI along with  the  samples for
     that  facility by both Health &  Hygiene and  PEI.  The
     identification sheet for  each  facility will  be sent
     separately to ATMI  by Health & Hygiene.

9.3  Reports

     Trip reports will be prepared by the PEI, Inc.  site  visitor
     for each facility visited.   Upon completion of  the  study,  a
     composite report of dye dust exposure in textile drug rooms
     from  an  industrial hygiene point of view  will  be prepared
     jointly"by PEI,  Inc. and Health & Hygiene, Inc.
                                A-44

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                                       SO-CL:C:::   10.0
                                       Revision:  1
                                       Date:  July 14, 1986
                                       Page:  1 of 1
                          SECTION 10.0

                    PERSONNEL AND MANAGEMENT
10.1  Health & Hygiene personnel

      Dr.  William L.  Dyson, CIH, Vice President will have primary
      management  responsibility  for this  project  at Health &
      Hygiene.  Other personnel who may participate in the study
      are Ronald Hill.  CIH and David S.  Davis,  both  industrial
      hygienists.  The  Burlington Industries Industrial Hygiene
      Laboratory person  for the project  is Sharon Lonon.  She has
      more than seven years experience  with filter weighing for
      cotton dust and other sampling at  Burlington.

10.2  PEI, Inc.  Personnel

      Personnel  from  PEI who may participate on this project are
      Leslie J.  Ungers,  CIH and Robert W. Willson.  CIH."

10.3  Project Coordination

      Scheduling visits  to the  textile facilities will  be done by
      Health  &  Hygiene.   Conducting  the preliminary  management
      conference and coordinating  sample  and data collection at
      the facility are the responsibility of the Health & Hygiene
      site visitor.
                                A-45

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QUALITY ASSURANCE PROJECT PLANS



  MIDWEST RESEARCH INSTITUTE
              A-47

-------
DYES - ANALYTICAL METHODOLOGY DEVELOPMENT AND
          ANALYSIS OF FIELD SAMPLES
    DRAFT QUALITY ASSURANCE PROJECT PLAN
                   for the
         Office of Toxic Substances
      EPA Prime Contract No.  68-02-4252
           Work Assignment No.  56
         MRI Project No.  8856-A(01)
                     For

    U.S.  Environmental  Protection Agency
         Office of Toxic Substances
        Field Studies Branch,  TS-798
           Washington,  D.C.  20460

           Attn:   Mr.  Richard  Kent
                   A-49

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                                                        Section No.:   1.0
                                                        Revision  No.:   3
                                                        Date:  April 30, 1987
                                                        Page  1 of 1
                                  SECTION  1.0

                DYES - ANALYTICAL METHODOLOGY DEVELOPMENT AND
                          ANALYSIS  OF  FIELD SAMPLES
                     Draft  Quality Assurance  Project  Plan

                         EPA  Contract  No.  68-02-4252
                            Work Assignment No.  56
 Approval  for:

 MIDWEST  RESEARCH  INSTITUTE
Approval for:

ENVIRONMENTAL PROTECTION AGENCY
^      onstant^
'Program  Manager
Date
_
Joseph J. Breen
Project Officer
Date
 JackBsfsingerv—^\          Date
 Quality  Assurance  Coordinator
Eileen Reilly-WiedowDate
Quality Assurance Officer
                                   A-50

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                                                        Section No.:   2.0
                                                        Revision No.:   3
                                                        Date:   April  30, 1987
                                                        Page 1 of 1
                                 SECTION 2.0
                              TABLE OF CONTENTS

Section                 Heading
  1.0     Title Page
  2.0     Table of Contents
  3.0     Project Description
  4.0     Project Organization and Management
  5.0     Personnel Qualifications
  6.0     Facilities, Equipment, Consumables,
            and Services
  7.0     Data Generation
  8.0     Data Processing
  9.0     Data Quality Assessment
 10.0     Corrective Action
 11.0     Documentation and Reporting
Pages
  1
  1
  2
  4
  1

  3
  8
  2
  3
  2
  2
Revision
3
3
3
2
2
3
3
3
2
2
2
Date
4/30/87
4/30/87
4/30/87
4/30/87
4/30/87
4/30/87
4/30/87
4/30/87
4/30/87
4/30/86
4/30/87
Appendix A - Standard Operating Procedure for Checking the Calibration of
               the Cary 219 Spectrophotometer
Appendix B - Analytical Protocol
List of Plan Holders:
     Midwest Research  Institute:
       J.  Spigarelli,  J.  Going,  P.  Constant,  J.  Hosenfeld, J. Balsinger,
          C.  Green,  D.  Harbin,  J.  Long,  R.  Ayling, R.  Rembecki
     Environmental  Protection Agency:
       J.  Breen,  E.  Reilly-Wiedow,  R.  Kent
                                   A-51

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                                                       Section No.:  3.0
                                                       Revision No.:   3
                                                       Date:  April 30, 1987
                                                       Page 1 of 2
                                 SECTION 3.0

                             PROJECT DESCRIPTION


The Environmental Protection Agency (EPA) has initiated a joint study with the
Ecological and Toxicological Association of Dyestuffs Manufacturing Industry
(ETAD) and the American Textile Manufacturers Institute (ATMI) to assess the
exposure of textile plant dye weighers to airborne dye particles which are
present in so-called "drug rooms" in the textile facilities.  As prime con-
tractor for the Office of Toxic Substances, Midwest Research Institute (MRI)
has been directed to develop the analytical methodology necessary to determine
the total amount of dyes present on air sampling filters.

After extensive discussions between industrial dye chemists and analytical
chemists at MRI, it was concluded that conventional quantisation of individ-
ual dyes on each air filter was not feasible, given the low quantities ex-
pected to be present.  Various alternative methods based on measuring phys-
ical properties of dyes as a class of compounds were considered.  A method
based on spectrophotometry was deemed to be the most applicable to the analy-
sis of dyes in general, especially at low levels.

The use of quantisation methods that are general (i.e., nonspecific) for a
class of compounds will frequently result in final values which are more un-
certain than those values obtained from a more specific method.  The spectro-
photometric approach to the determination of total dyes on an air filter will
result in an estimation of the amount of dyes that are present.  This is be-
cause the method assumes that all dyes that are weighed in the drug room are
present on the air filter and appear in amounts proportional to the amount of
each dye handled during the air monitoring period.  Adding to the uncertainty
of the value is the inability to determine (in most instances) the suitability
of using these analytical assumptions in analyzing the actual samples.  One
distinct advantage of the spectrophotometric method, however, is that its
accuracy improves with the number of dyes present on the filter, i.e., in-
creasing sample complexity will give better dye estimates.

A means of assessing the approximate uncertainty of the dye estimate can be
found by undertaking a statistical treatment of the absorbance characteristics
of the individual dyes comprising the sample set.  In this fashion, probable
errors in the dye estimate can be generated for different dye mixture scenarios
of the sample set.  Absorbance spectrum profiles and/or drug room dye utiliza-
tion data can then be employed to either favor or rule out certain dye mixture
scenarios.

The scope of work is comprised of two tasks as described below.


3.1  Subtask A:  Analytical Methodology Development

     MRI will develop analytical methodology for estimating the amount of
     dyes collected on a filter during air sampling in dye drug rooms.  The


                                   A-52

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                                                       Section No.:  3.0
                                                       Revision No.:   3
                                                       Date:   April 30, 1987
                                                       Page 2 of 2
     experimental  lab study will  focus on estimation of unknown quantities
     of dyes by a visible absorbance method.   Various aspects of this dye
     estimation method will be investigated.   These include determining the
     detection limits of various  groups of dyes,  establishing the uncertainty
     of the estimate, devising an efficient filter extraction scheme, and de-
     termining dye recoveries from air filters for different groups of dyes.


3.2  Subtask B:  Analysis of Dye  Drug Room Field  Samples

     MRI will  analyze air filter  samples collected during surveys of a number
     of dye drug rooms.   These analyses will  be carried out by the methodology
     developed in Subtask A.   Both area and personal  air sampling will take
     place.  The monitoring period will consist of one complete work shift at
     each drug room site.   Two personal air samplers  will  be worn by one drug
     room worker per plant.  Field air filter blanks  and filter lot blanks
     will be collected for background correction  and  determination of dye
     recoveries for certain groups of dyes.   Samples  of the bulk dyes han-
     dled in the drug room will be taken at the end of the shift after pump
     shut-off, or during the shift if it is the judgment of the industrial
     hygienist that this will not affect the  air  samples.

     Sample analysis will  consist of extracting all  dyes from the air filters,
     measuring and storing the visible absorbance data points from the extract
     solutions, and calculating the estimated quantity of dyes present on each
     filter based on a physical constant derived  from the individual  bulk dyes
     which were handled during the monitoring period.   The uncertainty in the
     value of this constant will  be proportional  to the precision of the indi-
     vidual dye absorptivity values.   The precision of the absorptivity values
     will be documented by performing them in duplicate for the trial  plant
     analysis.  An average airborne dye concentration will  be calculated by
     dividing the total  dye estimate by the volume of air sampled during the
     monitoring period.
                                   A-53

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                                                       Section No.:  4.0
                                                       Revision No.:   2
                                                       Date:  April 30, 1987
                                                       Page 1 of 4
                                 SECTION 4.0

                     PROJECT ORGANIZATION AND MANAGEMENT


The work assignment 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, Program Manager, will represent management.  He will
      be assisted in this effort by Mr. John Hosenfeld, Deputy  Program Manager.
      Together they will:

      •  Assure that all necessary resources are available.

      •  Assure that the 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 QAC or QAM regarding the project.

      •  Assure that any problems, deviations, etc., reported by the QAC or
         QAM  receive immediate  corrective action.

      •  Assure that the financial standing of 'the project is fully reported
         to the EPA project officer and work assignment manager.

      •  Review all technical work and  reports for overall technical accuracy.

4.2   Quality Assurance Manager (QAM)

      Ms. Carol Green, Quality  Assurance Manager  (QAM), will represent MRI.

      •  Review the project QA  plan to  assure that it is consistent with
         corporate and client policies  and procedures.

      •  Assure MRI management  that the facilities,  equipment,  personnel,
         procedures, and records  are  consistent with corporate  and  client  QA
         objectives and  requirements  by conducting or directing independent
         inspections and/or audits.

      •  Monitor  the work  assignment  QA activities.

      •  Report unresolved corrective actions to  corporate management for
         resolution.
                                     A-54

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Work Assignment Organization Chart
                                                     Section No.:  4.0
                                                     Revision No.:   2
                                                     Date:  April 30, 1987
                                                     Page 2 of 4
                                 DIRECTOR
                               KANSAS CITY
                                OPERATIONS

                                D. Sunder man
                                J. Spigarelli

QA MANAGER
Carol Green
!
QAC OTS
PROGRAM
Jack Bal singer
1
QCC
Randy Ay ling
	 ^w
i
*-^ 	

' -


PROGRAM
MANAGER
Paul Constant
t
WA LEADER
Don Harbin
ASSISTANT
WA LEADER
Julie Long
t
ANALYTICAL
Project Staff
                                Figure 4.1
                                 A-55

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                                                       Section No.:  4.0
                                                       Revision No.:  2
                                                       Date:  April 30, 1987
                                                       Page 3 of 4
4.3   The Quality Assurance Coordinator  (QAC)

      Mr. Jack Balsinger will serve as the Quality Assurance Coordinator and
      will represent program management with respect to quality assurance.
      He will:

      •  Assure that all corporate and client QA policies and procedures are
         available and  understood by  the project staff by conducting  inspec-
         tions and audits.

      •  Help prepare the project QA  plan.

      •  Approve the project QA plan.

      •  Assure that the facilities,  equipment, personnel,  methods, records,
         and controls are consistent  with project objectives and  requirements
         by conducting  or directing inspections and/or audits.  Inspection/
         audit results  and  corrective action requests will  be reported  to the
         program management, MRI management, and the QAM.

       •  Reinspect or audit to assure that appropriate corrective actions were
         implemented.   Report unsolved actions to the program management and
         the QAM  for  resolution.

       •  Conduct  additional audits  as directed by the program manager and/or
         QAM.

       •  Review and audit data reports and supporting evidence prior  to sub-
         mission  to EPA.

       •  Prepare  QA reports to be  submitted  to EPA.


 4.4  Quality  Control Coordinator  (QCC)

      Mr.  Randy Ayling  will  serve  as  the QCC.  He will:

       •  Conduct  systems  audit(s),  which include  reviewing  notebooks,
         chromatograms, printouts,  and other hardcopy  information and report
         the  findings to  the  QAC.

       .   Prepare  performance  audit samples.

       •   Report  audit findings to  program manager after  QAC review and
         approval.

       •  Conduct  additional audits as directed by the QAC.
                                    A-56

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                                                      Section No.:  4.0
                                                      Revision No.:  2
                                                      Date:  April 30, 1987
                                                      Page 4 of 4
4.5  Work Assignment Leader/Assistant Work Assignment Leader
     Mr.  Don Harbin will be the work assignment leader.   He will be assisted
     by Ms.  Julie Long, assistant work assignment leader.  Together they will:
     •   Help prepare and update 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 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,  documented,
        and  reported.
     •   Be responsible for analytical  data traceability.
     •   Take corrective action  on any  problems and  communicate  them in writ-
        ing  to the QAC and the  program and department managements.
        Prepare and submit monthly reports.
     •   Prepare and submit other reports as  requested by  the  EPA work
        assignment manager in conjunction with project staff.
                                 A-57

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                                                       Section No.:   5.0
                                                       Revision No.:   2
                                                       Date:  April  30, 1987
                                                       Page 1 of 1
                                 SECTION 5.0

                           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 also 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;.;.'
                               "ii : > ...• I    ';
Mr.  Don Harbin will serve as the Work Assignment Leader.  He has significant
experience in the high pressure liquid chromatographic analysis of dyes as
well as trace .quantisation methods for the
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                                                       Section No.:  6.0
                                                       Revision No.:   3
                                                       Date:  April 30, 1987
                                                       Page 1 of 3
                                 SECTION 6.0

              FACILITIES,  EQUIPMENT. CONSUMABLES. AND SERVICES
6.1  Facilities

     Sample preparation will  be performed in a laboratory designated, in part,
     for this project (MRI  Lab 324-W).   This laboratory is equipped with fume
     hoods and an analytical  balance contained in a vented glove box.  The
     windows are covered with low actinic film.   The fluorescent lights have
     been replaced with red lighting.

     Sample analyses will be  performed  on a Cary 219 spectrophotometer (located
     in MRI Lab 324-W) or other equivalent spectrophotometers.

     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:

     •   Cary 219 spectrophotometer or equivalent;  modified to allow an analog
        detector signal  to  be output to an integration  device.

     •   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 H20 analytical  balance  or equivalent; capable of weighing to
        the nearest 0.01 mg.

     •   DuPont P4000 personal  monitoring pumps or  equivalents.

     •   Volumetric glassware,  Low Actinic.

     6.2.1  Calibration

            6.2.1.1  The spectrophotometer is  checked on a weekly basis  by
                     qualified MRI  personnel.  A holmium oxide  film traceable
                     to  the National  Bureau of Standards is used to ensure
                     that wavelength readings meet the  manufacturer's speci-
                     fications.   Oxford Spectrochek® QA buffer  solutions are
                     used to  ensure that absorbance readings  meet specifica-
                     tions.   If the instrument performance falls outside of
                     the acceptable range,  it will  be reported  to the Instru-
                     ment Services  Group of MRI  and corrective  action will
                     be  taken.
                                   A-59

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                                                       Section No.:   6.0
                                                       Revision No.:   3
                                                       Date:  April  30, 1987
                                                       Page 2 of 3
            6.2.1.2  The Nelson Analytical chromatography software and Hewlett-
                     Packard hardware have built-in system checks to monitor
                     their performance.   Error messages wil be displayed if
                     problems occur.  A copy of the specific version of the
                     software program used for processing the data points
                     will be archived.

            6.2.1.3  The analytical balance is checked before use with weights
                     that are traceable to or checked against National Bureau
                     of Standards weights to confirm performance according to
                     manufacturer's speci fications.

            6.2.1.4  Personal air sampling pumps will be of the feedback flow-
                     adjusting type.  Each sampling pump will be calibrated
                     for an airflow of 2 to 2.5 L/min prior to use and checked
                     afterwards.
     6.2.2  Maintenance
            Maintenance of the analytical equipment used in this task will be
            done according to manufacturer's specifications and at their rec-
            ommended frequency.  This is summarized in Table 6.1
                           Table 6.1.  Maintenance
Equipment                       Service                          Frequency


Spectrophotometer               General                          As needed

Hewlett-Packard 9826            Limited requirements             As needed

Balance                         .Cleaning and adjustment for
                                  calibration                    1 year

DuPont P4000 personal           Replace belts and inlet          As needed
  monitor pumps                   filters
6.3  Consumables

     All dimethyl sulfoxide (DMSO) used will be A.C.S. reagent grade or better.
     All pH 7.0 and pH 3.0 buffer will be reagent grade.  All filter spiking
     experiments will use filters identical to those used during the field
     sampling.  Bulk sample containers will be amber pill vials.
                                    A-60

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                                                       Section No.:   6.0
                                                       Revision No.:   3
                                                       Date:   April  30, 1987
                                                       Page 3 of 3
6.4  Services
     Health and Hygiene, Inc., will  conduct the air sampling at the selected
     drug room sites and will  perform the following services:

     •   Preweigh and postweigh air sampling filters,  including field air
        filter blanks.

     •   Provide calibrated air sampling pumps for use at the site.

     •   Take bulk samples of all  powder dyes handled  in the drug room during
        the monitoring period.

     •   Take bulk samples of all  non-dye compounds handled in  the drug room
        during the monitoring  period which might interfere with the analyt-
        ical analysis method.

     •   Provide all  survey information regarding site conditions and monitor-
        ing period activity by the drug room worker.

     •   Transfer field air filter samples to new cassettes (not required for
        field air filter blanks)  after postweighing and ship to MRI along
        with original cassettes and  support pads.

        Provide suitable documentation for calibration and maintenance of all
        air sampling and weighing equipment for inclusion in the work assign-
        ment archives.
                                  A-61

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                                                        Section No.:   7.0
                                                        Revision No.:   3
                                                        Date:  April  30, 1987
                                                        Page 1 of 8
                                SECTION 7.0

                              DATA GENERATION


7.1  Experimental Design

     The sampling design will be prepared by EPA.  A flow chart of the steps
     involved in the analytical method is shown in Figure 7-1.

7.2  Sample Collection (Health and Hygiene, Inc.)

     7.2.1  Area Sampling

            Area sampling will be performed using samplers operating under
            critical flow conditions of 5 to 8 L/min.  One area sampler will
            be placed near the drug room weighing station and another will be
            located at a bulk dye storage area.  The sampling period will be
            for the entire 8-h shift.

     7.2.2  Personal Sampling

            One drug room worker will be monitored at each plant.  The worker
            will wear two personal air samplers.  The 37-mm open-face sampling
            cassettes will be operated at air flow rates of 2 to 2.5 L/min.
            When sampling, the inlet of the cassettes will be pointed downward
            so that only airborne material will be collected during the 8-h
            shift.

     7.2.3  Blanks

            Filter lot blanks and field air filter blanks will be provided by
            Health and Hygiene.  Filter lot blanks will be filters from the
            same lot as those used to collect field samples, but which will
            not be sent out  to the drug room site.  Field air filter blanks
            will be filters  which are handled in the same manner as the sampl-
            ing filters except that no air will be drawn through them.

     7.2.4  Bulk Dye Samples

            Small samples of each powder dye handled in the drug room during
            the monitoring period will be taken and labeled with unique bar-
            code stickers provided by MRI.  An identical bar-code sticker will
            be placed on the bulk dye inventory sheet along with the full dye
            name, manufacturer, and lot number.  Bulk samples will be taken
            with disposable  spoons (one for each dye).
                                    A-62

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                                            Section No.:  7.0
                                            Revision No.:  3
                                            Date:  April 30, 1987
                                            Page 2 of 8
Prepare solutions of
each individual  dye
at known concentrations
in dye solvent.
                      Field Air  Filter Samples
                     and Air Sampling Cassettes
                                                                Spike blank air
                                                                filters with a known
                                                                dye mixture (e.g.,
                                                                spiking standard
                                                                solution) at levels
                                                               Bracketing the amount
                                                                estimated on the
                                                                personal air filters.
                                                                Pull  air through the
                                                                filters for 6 to 8 hr.
                     Extract dyes from each filter
                     or cassette using a known
                     volume of dye solvent.
                                                        Prepare reference
                                                        standards using
                                                        known amounts of the
                                                        same spiking standard
                                                        solution used to
                                                        spike the blank air
                                                        filters.
                     Scan solution over 800-330 nm
                     range on spectrophotometer and
                     store spectrum.
_ - I/	absorbance (A.
     dye recovery

   I  cafculatimi

Compare total
absorbance of  each
spiked filter
extract to that of
the corresponding
reference standard.
Calculate the  average
percent recovery, R.
                     Integrate area beneath the
                     spectrum to obtain total
                                                        individual
                                  TOP
                     air filter or
                     cassette extract

                     Calculate the total
                     dye estimate on the air
                     filters and sampling
                     cassettes.
                                                           dyes
                                1
I
                  Calculate the spectral
                  absorptivity constant
                       for each dye.
                             Correct air filter dye
                             estimates by using dye
                             recovery and dye purity
                             information.   Correct
                             cassette dye estimates
                             by using only dye purity
                             information.
i
                                                   Calculate the weighted
                                                   average spectral ab-
                                                   sorptivity constant
                                                   (a ) for the dye analysis
                                                   set.
 Figure 7-1.
                     Obtain estimate of mg
                     total dye/m3 of air.

       Flow chart for the estimation of total dyes on an air filter.
                              A-63

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                                                        Section No.:   7.0
                                                        Revision No.:   3
                                                        Date:   April  30, 1987
                                                        Page 3 of 8
     7.2.5  Collection Conditions

            Temperature,  relative humidity,  and barometer measurements will
            be monitored  and recorded during the test.   A general  description
            of the airflow characteristics in the drug room will  be recorded.
            The sampling  time,interval  will  also be documented.

     7.2.6  Shipping and  Handling

            After gravimetric analyses  of the field air filters  have been
            performed at  Health and Hygiene, Inc., the air filters, original
            cassettes and support pads, bulk dye samples, field  air filter
            blanks, filter lot blanks,  and the field data forms  will be
            shipped to MRI by overnight courier.  Bulk dye samples will be
            shipped separately to minimize the chances of contamination.

7.3  Sample Traceability

     Tracking of field air filter samples, field air filter blanks, and bulk
     dye samples will be  achieved using the field data forms (Figure 7-2).
     During each phase of field testing (e.g., air sampling, gravimetric analy-
     sis) all samples will be assigned/identified using a unique sample identi-
     fication number.

7.4  Laboratory Analysis  Procedures

     See Appendix B for the analytical  protocol.

7.5  Internal Quality Control Checks for Sample Analyses

     7.5.1  General

            New and current lots of reagents are checked prior to use.

     7.5.2  Calibration

            Proper instrument performance will be confirmed and documented
            (see Section 6.2.1).
                                    A-64

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                               Section No.:   7.0
                               Revision No.:   3
                               Date:   April 30,  1987
                               Page  4 of 8
PERSONAL AREA AIR SAMPLING DATA SHEET
Plant ID No: Sampling Performed by: (Date (Mo/Da/Yr)
Worker Monitored: 1 Job Title/Work Duties:
SAMPLING EQUIPMENT AND CALIBRATION
Flowmeter Model Number: Flowmeter Serial Number:
Flowmeter Calibration Date: Calibration Traceable to:
Sampling Pump Model No:
Sampling Pump Serial No:
Pre-sampling Flowrate:
Date:
Time:
Post-sampling Flowrate:
Date:
Time:







i
Signature! s ) :
FIELD SAMPLING DATA
Sample ID Number:
Sampler Location:
Sample Start Time:
Sample Stop Time:
Sample Duration: (min)
Pump Flow Rate: (L/min)
! 	 . 	 ,. 	
left [] right [] left [] right []



1
Sample Air Volume: (m3) i| '..
Signature: Date:
Calculations Checked by: Date:
TRACEABILITY RECORD
jSent by: Date:
! Sent by: Date:




Figure 7-2
A-65

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                             Section No.:   7.0
                             Revision No.:   3
                             Date:   April  30, 1987
                             Page 5 of 8
STATIOKARY AREA AIR SAMPLING DATA SHEET
Plant ID No: [sampling Performed by: Date (Mo/Da/Yr)
SAMPLING EQUIPMENT AND CALIBRATION
Floumeter Model Number: Flowmeter Serial Number:
Flowmeter Calibration Date: Calibration Traceable to:
Sampling Pump Model No:
Sampling Pump Serial No:
Pre-sampling Flowrate:
Date:
Time:
Post-sampling Flowrate:
Date:
Time:
Signature! s) :


















FIELD SAMPLING DATA
Sample ID Number:
Sampler Location:
Sample Start Time:
Sample Stop Time:
Sample Duration: (mini
Pump Flow Rate: (L/min)
Sample Air Volume: (m3)





1
	
Signature :







Date:
Calculations Checked by: Date:
TRACEABILITY RECORD
j=============_=====?===========r==========================================================
Sent by: . Date: Time: 	 > Rec'd by: Date: Time:
Sent by: Date:
T\ rtiA • _______ S PCM-% ' H V

>y: Date: Time:
Figure 7-2 (continued)

        A-66

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                                                         Section No.:   7.0
                                                         Revision  No.:   3
                                                         Date:  April  30, 1987
                                                         Page 6 of 8
ANALYTICAL DATA
GRAVIMETRIC ANALYSIS (Health and Hygiene)

Sample ID Number:
Filter Preweight:
Filter Postweight:
Sample Weight:
Blank Correction:
Personal Filters





Adjusted Weight: i





-——-——--- — - — 	 	 -— — -1
Area Filters






1
1
Signatured): Date:







Blank Filters





I :






Calculations Checked by:
                     VISIBLE SPECTROPHOrOMETRIC ANALYSIS (MRI)
c===========================
Filter Extract. Date:
i
Data File Number: i
Sample Prepared by: '
!
Total Absorbance: j
Corr. Total Absorbance: |
I
Absorptivity : ( As )
Dye Estimate: (ug)
Avg. Recovery: (*)
i
Corr. Dye Est: (ug) !
Est. Airborne Dyes: (ug/m3)l
Data Reference Number: ;
Signature ( s ) :



1





i



1
i
i
*
i
i
!
i
i
i 	 |
,
i !
!
Date: Ca


1








Iculations Checked by:
==========3











                         Figure 1-2  (concluded)

                                 A-67

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                                                        Section No.:   7.0
                                                        Revision No.:   3
                                                        Date:   April  30, 1987
                                                        Page 7 of 8
     7.5.3   Internal  QC  Samples

            With  each batch of samples,  appropriate QC samples will  be in-
            cluded so the quality of the sample data can be assessed.   These
            QC  samples include reagent blanks,  field air filter blanks, and
            spiked filter controls for determining extraction efficiency.

            7.5.3.1  Reagent blanks:   At least  one reagent blank will  be
                     analyzed each analysis day to check for solvent inter-
                     ferences.   No filters will be used .for this determina-
                     tion.

            7.5.3.2  Field air filter blanks:   The field air filter blanks
                     are filters from the same  lot as the air sampling fil-
                     ters.   Field air filter blanks will be subjected to the
                     same handling procedures as the field air filter samples
                     except that no exposure to the drug room environment will
                     be allowed.  At least one  field air filter blank will be
                     collected and analyzed for each drug room site monitored.

            7.5.3.3  Spiked filter controls:  Filter lot blanks will be spiked
                     with known amounts of a dye mixture comprising a subset
                     of the total number of dyes handled in the drug room.
                     This dye mixture (i.e., the spiking standard solution)
                     will be composed of the individual dyes which account
                     for at least 80% of the total quantity of dye handled by
                     the drug room worker during the monitoring period.  The
                     relative amounts of the component dyes in the spiking
                     standard solution will reflect their actual usage during
                     the monitoring period.  Spiked filter controls will be
                     prepared in replicate to check the precision of the re-
                     covery experiments.

7.6  Systems and Performance Audits

     7.6.1  Systems audits:  Systems audits by the QAC or QCC shall include:

            •  Inspecting facilities and equipment for adequacy, appropriate-
               ness, and safety during use.

            •  Reviewing actual practices versus written procedures and pro-
               tocols.

            •  Inspecting the records of maintenance and calibration.

            •  Inspecting QC practices.

            •  Preparing and submitting a report with recommended corrective,
               actions to the QAC, and after approval, to the work assignment
               leader, program management, and the QAM.
                                  A-68

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                                                   Section No.:  7.0
                                                   Revision No.:  3
                                                   Date:  April 30, 1987
                                                   Page 8 of 8
7.6.2  Performance Audits

       A performance audit sample (PAS) is designed to check the opera-
       tion of the equipment as well as the analytical method and data
       reduction procedures.   Performance audit samples will be prepared
       independently by the QAC or QCC using the bulk dyes and will be
       analyzed along with regular samples.  The audit samples will be
       included periodically (beginning, middle, and end) during analysis
       of each drug room set (e.g.,  during field air filter analysis,
       during bulk dye analysis, and during the dye recovery experiments).
       The analyst will report to the QCC or QAC the total absorbance of
       each PAS.  The QAC or QCC will calculate a "found" concentration
       for each PAS using the spectral absorptivity constant of the
       specific dye(s).  If the found concentration does not agree within
       ± 30% of the actual bulk dye  concentration, one or more of the
       actions listed below will be  taken:

       1.   The QAC or QCC will supply another audit sample for analysis,
           using the same bulk dye(s) as before.

       2.   Calibration check of the  Gary 219 spectrophotometer to verify
           that absorptivity and wavelength requirements fall  within
           specifications.

       3.   Confirm the spectral  absorptivity constant of the dye(s) used
           for the PAS by repeat analysis.

       All performance audit sample  results and any corrective actions
       taken will  be reported to the work assignment leader,  program
       management, and the QAM.

       Performance audit samples will also be analyzed if (1)  the QCC or
       QAC believes the analysis procedure has changed,  (2)  analytical
       problems are suspected, (3) the MRI work assignment leader or the
       EPA work assignment manage/1 requests samples.

7.6.3  QAC Data Audits

       Data audits will be conducted or directed by the  QAC  by reviewing,
       auditing, and approving all reports and supporting evidence for
       accuracy and QA compliance prior to report submittal  to EPA.
                             A-69

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                                                       Section No.:  8.0
                                                       Revision No.:  3
                                                       Date:  April 30, 1987
                                                       Page 1 of 2
                                 SECTION 8.0

                               DATA PROCESSING


8.1  Collection

     Data collection will utilize both manual and computerized acquisition
     systems.  All raw data obtained manually shall be legibly recorded using
     permanent ink.  Each person who records data shall sign/initial and date
     the data.  Strip charts shall be labeled to allow traceability of all
     data.  All data collected and manipulated using computerized aquisition
     systems shall be retained in hardcopy form for archiving.  Custody of
     the original data media will be the responsibility of assigned project
     staff until archived.  All data will be handled in a confidential manner.

8.2  Data Reduction

     Standard data reduction procedures, as given in Appendix B, will be used.
     All data reduction will be performed manually or by using a database com-
     puter software program.  In addition, all sample manipulations (e.g.,
     weighing, dilution,  etc.) will be clearly documented.

8.3  Data Validation

     The data validation  process will include:

     •  Checking field data forms to ensure accuracy and completeness of bulk
        dye  sampling, amounts of dyes weighed, and the associated number of
        weighings.

     •  Validating all equations and computer programs and documenting the
        validation and evidence.

     •  Validating and checking electronic data transfer.

        Proofreading all  data entries for transfer errors.  Data transfer will
        be kept to a minimum to prevent errors.  The analytical data will be
        transferred manually from a computerized output to data tables, then
        from the data tables to a computerized data reduction program to
        obtain final results.  Data will be checked for transfer errors.

        Screening  data for  consistency by a second project staff member.

     •  Checking calculations, randomly.

        Performing outlier  checks.

     •  Documentating of  all associated blank, standard, and QC data along
        with results of analyses for each batch of samples.
                                    A-70

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                                                       Section No.:   8.0
                                                       Revision No.:   3
                                                       Date:   April  30, 1987
                                                       Page 2 of 2
        Examining QC data and QC checks.

     •   Maintaining records of reviews and validation.

        Examining data/information for completeness,  representativeness, and
        comparability.

        Reviewing and approving of all records by the work assignment leader.

        Reporting protocol  deviations and assumptions with the results.

     The work assignment leader will  be responsible for assuring data validity.

8.4  Storage

     Raw data will  be documented in laboratory notebooks,  on data forms  or
     printer paper, as strip chart recordings, or as  hardcopy originals  from
     magnetic tapes or disks.   Permanent storage of work assignment records
     will be archived in a  formal  project file (SOP-QA7).
                                                  Material belongs tor
                                                  "
                                                  401
                                                          n^V'
                                                 (202)382-3944
                                  A-71

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                                                       Section No.:  9.0
                                                       Revision No.:   2
                                                       Date:  April 30, 1987
                                                       Page 1 of 3
                                 SECTION 9.0

                           DATA QUALITY ASSESSMENT


This analytical method gives an estimate of total dye content on an air filter
and should not be considered as a quantitative determination of the amount of
dyes present.  The precision of the analytical method should meet expected
standards for a spectrophotometric method which involves the extraction of
microgram quantities of analytes from an air filter.  The objectives of pre-
cision for this method will be to obtain dye recoveries for replicate spiked
filter samples which have relative differences ± 25% of each other.  The ob-
jective for accuracy will be to obtain total dye estimates on replicate spiked
filter samples which have relative errors ± 50% of the actual dye present on
the air filter.  Average extraction efficiencies for the dyes using spiked
filters should fall within the range of 60 to 140% recovery to yield meaning-
ful data.

9.1  Precision

     The precision of the analytical method will be determined by analyzing
     replicate spiked filter samples and calculating their respective percent
     recoveries.  Percent relative difference, R.D., will be calculated as
     follows:

                                R.D. (%) = Rl " R2 x 100
     where   RI = the % recovery for one replicate
             R2 = the % recovery for the other  replicate
             R  =  the average % recovery calculated from R! and
9.2  Accuracy
     The  accuracy  of 'the  analytical method  can  only  be  established  for  known
     dye  spike  samples.   Accuracy may  be  indicated by comparing  the total dye
     estimate for  spiked  filter  controls  to the  actual  amount spiked on the
     filters.   Accuracy will be  measured  by calculating the  relative error,
     R.E. ,  of the  total dye estimate:

                                    DFST  "  DACT
                          R.E.  (%) = -^ - — x 100
                                        UACT
                                      A-72

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                                                       Section No.:   9.0
                                                       Revision No.:  2
                                                       Date:  April  30, 1987
                                                       Page 2 of 3
     where  DEST = the total dye estimate in ug
                 = the actual total dye quantity spiked in |jg
9.3  Uncertainty

     The uncertainty of the total dye estimation will be primarily dependent
     on the specific group of dyes being analyzed.  The dye estimation is
     based on the weighted average absorptivity of all of the dyes handled
     during the monitoring period.  In general, the uncertainty of the dye
     estimate will be proportional to the standard deviation of the individ-
     ual dye absorptivities.   For this reason it is not possible to establish
     a specific uncertainty value for the total dye estimate.

     Probable errors in the total dye estimate can be obtained by using a
     statistical computer program that selects dye mixtures from the given
     group of dyes.  Specific dye handling information is input into the
     program to weight the dye selection process.   As a result, the more
     heavily used dyes have a higher probability of being selected than the
     minor use dyes.  In this manner the errors associated with various sub-
     sets of the entire group of dyes can be approximated.   Additional data,
     such as the number of dye weighings or dustiness observations, can then
     be used to focus in on dye subsets which are more likely to occur on the
     air filter.

9.4  Recovery

     The efficiency of the filter extraction procedure will be indicated from
     the recovery results of the spiked filter analyses.   Dye recovery will
     be determined by a direct comparison of the spiking solution (e.g.,
     reference standard) to the solution obtained from extracting the spiked
     filter.


                              R (%) = T^- x 100
                                      MSTD

     where  Af.^ = total absorbance of spiked filter extract

                 = total absorbance of reference standard
9.5  Traceability of Instrumentation

     All collection and measuring instrumentation will  have a unique identi
     fication number.   Maintenance, calibration,  and use logs will  be main-
     tained.
                                   A-73

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                                                       Section No.:   9.0
                                                       Revision No.:   2
                                                       Date:   April  30, 1987
                                                       Page 3 of 3
9.6  Traceability of Samples

     All samples will have a unique identification number along with infor-
     mation about the worker being monitored, the plant site, monitoring lo-
     cation, exposure time and conditions, collection device, etc.

9.7  Traceability of Data

     Data will be documented and  filed to allow complete reconstruction, from
     initial field records to data archiving.

9.8  Completeness

     Due to the  very small number of  data points available per drug room site,
     completeness of the data will be crucial in order to obtain  meaningful
     data.
                                    A-74

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                                                       Section No.:  10.0
                                                       Revision No.:   2
                                                       Date:   April 30, 1986
                                                       Page 1 of 2
                                 SECTION 10.0

                              CORRECTIVE ACTION


The work assignment leader has primary responsibility for taking corrective
action; if he is unavailable,  the program manager shall  be contacted for in-
structions.   Unresolved problems are reported to the program manager and the
QAM.  The Associate Director of K.C.  Operations and the  Senior Vice President
are notified of unresolved problems by the QAM.

Some of the types of problems  and corrective actions to  be taken are listed
below.

8.1  Performance/Systems Audits

     If problems are detected  during an audit:

     •   The auditor shall notify the person responsible,  the work assignment
        leader, and the QAC of the problem(s) and any action(s) that have been
        taken.

     •   The work assignment leader and the person responsible shall correct
        the problem, then notify the QAC.

     •   The auditor, with the  approval of the QAC,  shall  prepare a corrective
        action request and send it to the program manager, work assignment
        leader, and the QAM.

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 docu-
        mented in the project  records; the work assignment leader then pre-
        pares and sends a problem/action taken memo to the QAC and the program
        manager.

        If a large quantity of data is affected, the problem/action taken is
        documented in the project records;  the work assignment leader then
        prepares and sends a problem/action-taken memo to the QAC, the program
        manager, and to the EPA work assignment manager.

10.3 Significant QA Problems

     In general, the work assignment leader shall identify technical problems.
                                   A-75

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                                               Section No.:   10.0
                                               Revision No.:   2
                                               Date:   April  30, 1986
                                               Page 2 of 2
The work assignment leader prepares and sends a problem memo to the
QAC and program manager; if the problems are significant, the action
is determined collectively.

The action taken is documented in the project records.

The problem and action taken is reported to the EPA work assignment
manager.
                           A-76

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                                                       Section No.:   11.0
                                                       Revision No.:  2
                                                       Date:  April 30, 1987
                                                       Page 1 of 2
                                 SECTION 11.0

                         DOCUMENTATION AND REPORTING
11.1 Documentation
     •  All documentation shall be in permanent ink or on computer printouts.

     •  Corrections will be performed as follows:   Draw a single line through
        an incorrect entry so that the original entry remains legible.  Add
        the correct entry; then explain, initial,  and date the correction.

        New information may be added to original raw data.  It will be
        initialed, dated, and explained.

     •  All deviations from standard operating procedures (SOPs), procedures,
        and protocols will be documented.

     •  All assumptions and interpretations 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.
        Hardcopies of all magnetic data will be generated for archiving
        purposes.

11.2 Document Control

        Raw data will be documented in laboratory  notebooks, on  sampling
        forms, on analytical  forms, on printer paper,  as hardcopies from
        magnetic tape, and as strip chart recordings.

     •  A raw data packet for each drug room site  monitored will  be generated,
        along with data tracking forms to document the existence and flow of
        data through the data processing cycle.

     •  All project-related documents will  be maintained by assigned project
        staff until archived.

11.3 QA Reports to Program Management

     The QAC, in cooperation  with the work assignment  leader, shall identify
     critical areas 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.
                                    A-77

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                                                       Section No.:   11.0
                                                       Revision No.:   2
                                                       Date:   April  30, 1987
                                                       Page 2 of 2
     •   Documentation practices.
     •   Recordkeeping practices.
     •   Adherence to protocols, SOPs, and the QA project plan.
     •   Assessment of data accuracy, precision, and completeness.

     The results of inspections and audits will be reported to the work
     assignment leader, the program manager, and QAM.

11.4 Report Design

     Progress, draft final, final reports, and QA summary reports will be sub-
     mitted in accordance with the provisions for reporting in the contract.
     Verbal status reports will be made biweekly to the work assignment leader.
                                   A-78

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                                        Section No.:   Appendix A
                                        Revision No.:   2
                                        Date:   April  30, 1987
                                        Page A-l of 4
                       APPENDIX A

STANDARD OPERATING PROCEDURE FOR CHECKING  THE  CALIBRATION
            OF THE GARY 219 SPECTROPHOTOMETER
                        A-79

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                                                  Section No.:   Appendix A
                                                  Revision No.:   2
                                                  Date:   April  30, 1987
                                                  Page A-2 of 4
          STANDARD OPERATING PROCEDURE FOR CHECKING THE CALIBRATION
                      OF THE CARY 219 SPECTROPHOTOMETER


          Absorbance and wavelength verification of the Gary 219 spectropho-
tometer (or equivalent) is performed and documented weekly by MRI.  The ab-
sorbance is monitored using Oxford Spectrochek® QA solutions (or equivalent).
The wavelength is monitored using a NBS traceable holmium oxide film.  If the
instrument does not pass verification, the Instrument Services Group of MRI
will be notified and corrective action will be taken.  Verification documents
will remain on file at MRI.

          The following steps outline the operating procedure for conducting
the spectrophotometric calibration check:

I.   Wavelength Verification via Holmium Oxide Film

     A.   Turn main power switch to "on" position.  Allow Vis-UV light source
          to warm up for at least 20 min.

     B.   Initially, an air versus air scan will be performed to zero the
          instrument.  The conditions for setup are identical to those listed
          in Appendix B, Section 13.1.2 except for the following changes:

          - Slit:   1.0 nm
          - Scanning rate:  0.5 nm/s
          - Chart display:  5

     C.   Close the covers to the cuvette compartments on the spectrophotom-
          eter.

     D.   Set the upper wavelength  limit at 750 nm using the wavelength  1 dial
          and set the  lower wavelength limit  at 250  nm using the wavelength  2
          dial.

     E.   Using the "scan" dial, turn dial (+) or (-) to set the wavelength
          at 750  nm.

     F.   Turn the  timer mode  knob  fully clockwise,  then back to  "wavelength."

     G.   Turn the  autobaseline  knob  fully clockwise to the "record" position
          and hold  for a couple of  seconds, making sure the red recording
          light comes  on.

     H.   Adjust  the balance knob to  give  an  absorbance reading of  0.1000 (or
          as close  as  possible)  on  the digital display.

     I.   Insure  measurement dial is  set on serial.
                                    A-80

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                                                  Section No.:   Appendix A
                                                  Revision No.:   2
                                                  Date:   April  30, 1987
                                                  Page A-3 of 4
     J.    Press "step"  button and scan the wavelength range.
     K.    When the scan is finished,  the instrument will  return the wave-
          length to 750 nm.
     L.    Turn the pen  off.
     M.    Turn the timer mode knob fully counter-clockwise to "off" position.
          Line up pen on a dark graduation.
     N.    Adjust the balance knob so  the digital  readout  shows 0.000 (or as
          close as possible).
     0.    Turn timer mode knob fully  clockwise,  then back to  "wavelength."
     P.    Turn measurement knob to overlay.
     Q.    Turn pen on and press "step" button to begin scan.
     R.    When scan is  finished, turn the pen off.   Watch to  be sure the
          paper retracts properly.
     S.    Turn the timer mode knob to "off."
     T.    Remove the sample cover,  place the  holmium oxide film into the sam-
          ple turret, and close the lid.
     U.    Check to be sure the pen has realigned itself to the same starting
          point as in step M.
     V.    Turn timer mode knob fully  clockwise,  then back to  "wavelength."
     W.    Turn pen on and press "step" button to begin.scan.
     X.    When the scan has finished, turn the pen  and the timer mode knob to
          off positions.
     Y.    Remove the holmium oxide film.

II.   Absorbance Verification via Oxford Spectrochek® QA Buffer Solutions
     A.    Initally, a water versus water scan will  be performed to zero the
          instrument, using two 1-cm  path width cuvettes  filled with deionized
          water.  Clean the outer surface of  each cuvette with an appropriate
          tisue to remove any smudges.
                                    A-81

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                                             Section No.:  Appendix A
                                             Revision No.:  2
                                             Date:  April 30, 1987
                                             Page A-4 of 4
B.    Place one cuvette in the reference compartment and place the other
     cuvette in the sample compartment.

C.    Dial in 690 nm for the upper wavelength limit and 300 nm for the
     lower wavelenght limit using the wavelength 1 and 2 dials, respec-
     tively.  Using the "scan" dial, turn the dial to (-) to set the
     wavelength at 690 nm.

D.    At this point, follow the steps outlined~in F through S for the wave-
     length verification via the hoi mi urn oxide film.  (Switch scan rate
     to 2.0 nm/s at this point.)

E.    Remove the cuvette from the sample compartment.  Fill with solution
     no. 2, rinsing the cuvette prior to filling with ~ 2 ml of the same
     solution.  Wipe the cuvette surface and replace in sample compartment.

F.    Reset the wavelength range to  scan from 690 to 400 nm.

G.    Fully turn the timer mode knob clockwise, then back to "wavelength."

H.    Turn the pen on and press "step" button to start the scan.

I.    When the scan  is finished and  the wavelength  has returned to 690  nm,
     turn the pen and the timer mode  knob off.

J.   Open the sample compartment and  remove the sample cuvette.  Rinse
     the cuvette with solution no.  1  and fill.  Replace into sample com-
     partment and close  lid.

K.   Repeat  steps G through  I.

L.   Remove  the  sample cuvette,  rinse with  solution  no. 4 and  fill.
     Place  back  into the  sample  compartment and close lid.

M.   Reset  the wavelength  range  to  scan  from 400  nm  to 300  nm.  Using
     the "scan"  dial, turn  the dial to  (-)  to  set  the wavelength at
     400 nm.

N.   Repeat steps G through  I.

0.   Remove the  sample cuvette and  repeat  steps G  through  I  using
     solution  no. 3.
                                A-82

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                        Section No.:  Appendix B
                        Revision No.:   3
                        Date:  April 30, 1987
                        Page B-l of 20
     APPENDIX B


ANALYTICAL PROTOCOL
         A-83

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                                                    Section No.:   Appendix B
                                                    Revision No.:   3
                                                    Date:   April  30, 1987
                                                    Page B-2 of 20
            ANALYTICAL METHOD FOR THE ESTIMATION OF TOTAL DYES IN
                  TRACE QUANTITIES ON AIR SAMPLING FILTERS


1.0   SCOPE AND APPLICATION

      1.1   This method has been developed for the estimation of trace quan-
            tities of groups of dyes from the following dye classes:   acid,
            basic, direct, disperse, and reactive.  Dyes from other major
            classes have not been investigated.

      1.2   This method yields an estimate of the total quantity of a group
            of dyes present on an air sampling filter.   Information about the
            quantity of each individual dye on the air filter is not possible
            with this method.

      1.3   This method is suitable for use by technicians possessing nominal
            experience with spectrophotometric equipment and procedures.


2.0   SUMMARY OF METHOD

      This method describes the procedures for estimating the total quantity
      of a group of dyes present on an air sampling filter.  A general dia-
      gram of the method is shown in Figure B-l.

      The analysis procedure consists of extracting the dyes from each air
      filter using a minimum volume of buffered dye solvent.  An aliquot of
      each filter extract is passed through a 0.45 urn Gelman Acrodisc (or
      equivalent) and transferred to the measuring cell in the spectrophotometer.
      The visible absorption spectrum of each extract is obtained and digitized
      by means of an A/D converter box interfaced with the spectrophotometer.
      Air sampling cassettes and one or more field air filter blanks are also
      extracted and scanned.  All spectra are stored on floppy disks for fu-
      ture data manipulation.

      Spectra of each individual dye handled in the drug room during the air
      monitoring period are obtained by analyzing known solutions of bulk dye
      samples collected at the plant site.  These dye spectra are then used
      to form a data base for estimating the total quantity of dye on the air
      filters (and sampling cassettes) taken during that monitoring period.
      Spectra obtained on identical bulk dyes at different plants will not be
      employed so as to avoid possible lot-to-lot variations in absorption
      characteristics.
                                   A-84

-------
                                                    Section No.:  Appendix B
                                                    Revision No.:  3
                                                    Date:   April 30, 1987
                                                    Page B-3 of 20
                              Field Air Filter Samples
                             and Air Sampli
               ig Cassettes
 Spike blank air
 filters with a known
 dye mixture (e.g.,
 spiking standard
 solution) at levels
^bracketing the amount
 estimated on the
 personal air filters.
 Pull air through the
 filters for 6 to 8 hr.
                             Extract dyes from each filter
                             or cassette using a known
                             volume of dye solvent.
Prepare solutions of
each individual  dye
at known concentrations
in dye solvent.
                                    Prepare reference
                                    standards  using
                                  /known  amounts  of the
                                    same spiking standard
                                    solution used  to
                                    spike  the  blank air
                                    filters.
                             Scan solution over 800-330  nm
                             range on spectrophotometer  and
                             store spectrum.
     dye recovery

   I  calculation
  T
Compare total
absorbance of each
spiked filter
extract to that of
the corresponding
reference standard.
Calculate the average
percent recovery, R.
 Integrate  area beneath  the
 spectrum to  obtain  total
.absorbance
 individual
air filter or
cassette extract

Calculate the total
dye estimate on the air
filters and sampling
cassettes.
                                       dyes
          1
            I
                               Calculate  the  spectral
                               absorptivity constant
                               (ac)  for each  dye.
                             Correct air filter dye
                             estimates by using dye
                             recovery and dye purity
                             information.   Correct
                             cassette dye estimates
                             by using only dye purity
                             information.
        I
                               Calculate  the weighted
                               average  spectral  ab-
                               sorptivity constant
                               (a )  for the dye  analysis
                               set.
                             Obtain estimate of mg
                             total  dye/m3 of air.

 Figure B-l.   Flow chart for the estimation of total  dyes on an air filter.
                                   A-85

-------
                                                    Section No.:   Appendix B
                                                    Revision No.:   3
                                                    Date:   April  30, 1987
                                                    Page B-4 of 20
      The  total  sample absorbance in the visible wavelength region is used to
      estimate  the total  quantity of dye present on each air filter and its
      corresponding cassette.   This entails electronically integrating the
      area beneath the absorption spectra of each filter or cassette extract
      and  each  individual  dye.   The area values are readily converted to total
      absorbance (AjQj) by using an appropriate factor (i.e.,  area count value
      -r 106 area counts/ absorbance unit).

      Spectral  absorptivity (a ) constants for each individual  dye used dur-
      ing  the monitoring period are calculated based on Beer's  law.   From the
      individual a  values, and dye handling information, a weighted average
      spectral  absorptivity constant (a ) for the group of dyes is calculated.

      The  total amount of dyes contained on each air filter, and its corre-
      sponding cassette, is then calculated using this weighted average.  The
      dye  estimates are corrected wherever appropriate for the  amount of ac-
      tive ingredient in each dye (i.e., purity) and for the average recovery
      (R)  of dyes off the air filters.


3.0   INTERFERENCES

      3.1   Because of possible reactivity with the dye solvent at the estab-
            lished pH (pH 7), some basic dyes may not be quantifiable using
            the standard analytical procedure.  Use of pH 3 dye solvent is
            recommended if the bulk dyes handled at the plant site are pre-
            dominantly of the basic class.

      3.2   Due to the nature of the analytical technique used, this method
            is not particularly susceptible to other interferences except
            those from other dyes, i.e., cross-contamination.   Therefore,
            after each use, glassware is immediately rinsed with methanol to
            remove all traces of dye and dye solvent.  The glassware is then
            washed with soap/h^O, rinsed with deionized water followed by
            acetone, and allowed to air dry prior to re-use.

      3.3   Since fluorescent brighteners are not to be included in the total
            dye estimate, the lower wavelength limit of the absorbance scan
            may have to be shifted upward if brighteners were handled during
            the air sampling period.  If this change in the wavelength scan
            range should be necessary, all the individual dye and filter/
            cassette extract solutions in the dye analysis set must be scanned
            over this same wavelength range.


4.0   SAFETY

      All  manipulations made with dyestuff samples are performed in a fume
      hood or glove box.  Gloves and other appropriate safety apparel are
                                     A-86

-------
                                                    Section No.:   Appendix B
                                                    Revision No.:   3
                                                    Date:   April  30, 1987
                                                    Page B-5 of 20
      worn at all  times.   Solid and liquid waste is  disposed of in the proper
      manner.
5.0   APPARATUS AND MATERIALS

      5.1   Solution Preparation

            5.1.1  500 and 1,000 mL graduated cylinders
            5.1.2  1 gal  glass bottle with 10 mL Repipettor®
            5.1.3  Volumetric pipets (TD)  - 2,  3,  5,  6,  8,  10,  and 20  mL
            5.1.4  Volumetric flasks - 10,  25,  50,  100,  250,  500,  and  1,000 mL
                   (low actinic)
            5.1.5  Disposable pipets
            5.1.6  Beakers -  100 mL
            5.1.7  Filters -  0.45 urn Gelman Acrodisc  (or equivalent)
            5.1.8  Glass  jars (amber) - 4  oz with  DMSO-resistant  lid liners
                   (optional)
            5.1.9  10-mL  disposable syringe (Luer  tip)
            5.1.10 Stainless  steel  forceps

      5.2   Balance - Analytical; capable  of accurately  weighing  to 0.01 mg

      5.3   Shaker - Capable  of shaking 4-oz jars  at  1 oscillation/s.   If  a
            wrist-type shaker is employed,  DMSO-resistant lid liners must  be
            used on the glass jars.

      5.4   Ultrasonic bath

      5.5   Spectrophotometer/data storage system

            5.5.1  Spectrophotometer - Dual  beam instrument capable of scan-
                   ning in the visible wavelength  region (800-330  nm).   The
                   Spectrophotometer must  have  a 1 or 10 V  analog  signal out-
                   put, or allow such a signal  to  be  obtained (such as by
                   using  the  strip chart pen signal).

            5.5.2  Cuvettes - Standard 1 cm pathlength.

            5.5.3  Nelson Analytical  Model  4400 Chromatography  Data System,
                   or equivalent.

            5.5.4  Nelson Analytical  A/D interface  box,  or  equivalent.

            5.5.5  Magnetic media for data storage  -  5-1/4  in.  floppy  disks,
                   or equivalent.
                                   A-87

-------
                                                    Section No.:  Appendix B
                                                    Revision No.:   3
                                                    Date:  April 30, 1987
                                                    Page B-6 of 20
6.0   REAGENTS

      6.1   Dimethyl sulfoxide (DMSO), ACS certified grade

      6.2   Buffer, pH 7 and pH 3 - reagent grade (uncolored)

      6.3   Dye solvent (pH 7) - prepared by adding 9 parts DMSO to 1 part
            pH 7.0 buffer

      6.4   pH 3 dye solvent - prepared by adding 9 parts DMSO to 1 part pH
            3.0 buffer


7.0   METHOD VALIDATION (Average Recovery Determination, R)

      The analytical method is validated using a subset of the dyes handled
      in the drug room during the monitoring period.  This subset is composed
      of the individual dyes used most during the monitoring period (based on
      weight).  The component dyes in the subset should represent at least
      80% of the total quantity of dye handled and be in proportion to their
      usage.

      Duplicate blank filters are spiked at two levels with a solution of the
      dye subset (i.e., spiking standard solution) so as to bracket the absorb-
      ance of the personal air filters.  After drying, clean, humid air is
      pulled through the filters using similar conditions (time, flow rate)
      used in the field.  Validation is confirmed if the average recovery for
      the spiked filters falls in the 60 to 140% range.


8.0   SAMPLE RECEIPT AND STORAGE

      8.1   Sample Receipt

            8.1.1  Samples received from the field consist of:

                     1.  Personal and area air sampling filters, which were
                         removed from their original cassettes and stored in
                         fresh cassettes after gravimetric weight determina-
                         tion.

                     2.  The original air sampling cassettes used during the
                         monitoring period.

                     3.  Field air filter blanks in cassettes, which were
                         carried in the field along with the actual air fil-
                         ter samples.
                                    A-88

-------
                                                    Section No.:  Appendix B
                                                    Revision No.:   3
                                                    Date:   April 30, 1987
                                                    Page B-7 of 20
                     4.   Filter lot blanks (unexposed air filters for use in
                         the recovery experiments).

                     5.   Individual bulk dyes.

            8.1.2  Upon receipt,  each filter/cassette sample is examined and
                   logged-in using Form A-0.   Individual  bulk dyes,  identified
                   by bar-code labels,  are logged-in via  use of an appropriate
                   bar-code reader.

      8.2   Sample Storage

            8.2.1  Unless instructed otherwise,  samples are stored in the dark
                   in room 324W at room temperature  in their original packing
                   containers until the analysis is  completed.   After analysis,
                   bulk dye samples are retained at  the discretion of EPA.

            8.2.2  Although field air filter  samples should be  analyzed as
                   soon as possible after receipt at MRI,  analysis will  not
                   be performed without (a) a performance  audit sample (PAS)
                   being analyzed concurrently,  and  (b) without knowledge of
                   what type of dye solvent should be used to perform the
                   analyses (i.e.,  pH 7 or pH 3).  When air filters  arrive  at
                   MRI,  the EPA work assignment  manager will  be contacted.
                   Air filter analysis  will be delayed until  (a) the indi-
                   vidual bulk dyes (which are used  to prepare  the PAS)
                   arrive at MRI  and (b)  basic dye information  regarding the
                   dyes handled during  the monitoring period is received.
                   The above measures will be observed unless instructions  to
                   the contrary are given by  EPA.


9.0   EXTRACTION OF PERSONAL AND  AREA FILTERS, CORRESPONDING AIR SAMPLING
        CASSETTES, AND FIELD AIR  FILTER BLANKS

      9.1   Using stainless steel  forceps, carefully transfer the air filter
            and filter support from the cassette holder to a 4-oz amber glass
            jar.   (Note:   Each original  air sampling cassette will contain
            only a filter support.)

      9.2   Using the Repipettor® calibrated  to  8.0  mL, pipet approximately
            2 mL of the dye solvent into  the  cassette holder, dispensing the
            remaining ^ 6.0 mL of dye solvent into the jar.

      9.3   Cap the cassette holder tightly and  shake vigorously for 30 s.
            Transfer the cassette rinse solution to  the 4-oz jar using a dis-
            posable glass pipette.   Cap the jar  securely.
                                  A-89

-------
                       FORM A-0.  SAMPLE RECEIPT FORM

                                 8856-A(01)
                                                              Section  No.:  Appendix B
                                                              Revision No.:   3
                                                              Date:  April  30,  1987
                                                              Page  B-8 of  20
Plant ID:

Test Date:
Date Received:

Received by:
Were all samples received in good condition?  Yes     No

Sample Storage:  	
            (circle  one)
Sample ID No.
















Sample Description (Check One)
Original Air
Filter Cassette
















Personal
Air Filter
















Area
Air Filter
















Field Blank
Air Filter
















Were  any blank filters  received?   Yes     No

Brand and Lot No.:
(circle one)
                                    A-90

-------
                                                    Section No.:  Appendix B
                                                    Revision No.:   3
                                                    Date:  April 30, 1987
                                                    Page B-9 of 20
      9.4   Place the jar in a shaker for 30 min.   The shaker must oscillate
            at least once per second.  After 30 min, visually examine the air
            filter and/or filter support.   If the dye extraction appears in-
            complete, place the jar in an ultrasonic bath for a maximum of
            10 min.

      9.5   The extract solution must be analyzed within 45 min of initial
            contact with the dye solvent (i.e., Step 9.2).Dye analysis
            schedules (Form A-l) are prepared and followed for each set of
            filters/cassettes analyzed.
                                i
      9.6   Only when deemed appropriate after consultation between MRI and
            EPA, should the pH 3 dye solvent (Step 6.4) be used to perform
            the extractions.
10.0  INDIVIDUAL DYE SOLUTION PREPARATION

      Note:   Dye solutions must be analyzed within 45 min of initial
      contactwith the dye solvent (Step 10.2).   Dye analysis schedules
      (Form A-l) are prepared and followed for each set of bulk dyes
      analyzed.

      10.1  Accurately weigh (to the nearest 0.01 mg) approximately 40 mg of
            the bulk dye sample into a pre-tared 100-mL volumetric  flask (low
            actinic).   Record the weights on the Individual  Dye Solution
            Preparation Form (Form A-2).

      10.2  Add 50-70 ml of dye solvent to the flask and place in an  ultra-
            sonic bath for 10 min.   After the flask has cooled to room
            temperature, dilute to volume with dye solvent and mix  well.

      10.3  Pipet 10.0 ml from the flask in Step 10.2 to a 250-mL low actinic
            volumetric flask.   Dilute to volume with dye solvent and  mix well.

      10.4  Repeat Steps 10.1 through 10.3 for every dye in the dye analysis
            set.

      10.5  If pH 3 dye solvent was used in Steps 9.2-9.5,  use the  pH 3 dye
            solvent (Step 6.4) to prepare the dye solutions.


11.0  PREPARATION OF SPIKED FILTER CONTROLS AND BLANKS (Forms A-3 and A-4)

      11.1  Based on the average total  dye estimate for the personal  air fil-
            ters (obtained from Step 16.5 and using Section I of Form A-3),
            calculate the total dye level which is 130% of that value.   This
            calculated dye level is the target total dye concentration for
            the spiking standard solution.
                                   A-91

-------
                                                  FORM A-l.   DYE ANALYSIS SCHEDULE

                                                               8856-A(01)
        Date:	
        Name(s):
        LNB:  page no.
Plant(s):
Samples Analyzed:
Air FiIters:	
Bulk Dyes:
                                               Spiked  Filter  Controls:
Extraction/dilution schedule
Time
8:00
:15
:30
:45
9:00
:15
:30
:45
10:00
:15
:30
:45
11:00
:15
:30
:45
1:00
:15
:30
:45
2:00
:15
:30
:45
3:00
:15
:30
:45
4:00
:15
:30
:45
5:00
Plant
1.0.
. /.
































Sample 1.0.



i





























1° Oiln.a

































Analysis schedule
Time
8:00
:15
:30
:45
9:00
:15
:30
:45
10:00
:15
:30
:45
11:00
:15
:30
:45
1:00
:15
:30
:45
2:00
:15
:30
:45
3:00
:15
:30
:45
4:00
:15
:30
:45
5:00
Sample 1.0.

































Cycle
no.

































2° Diln

































ATOT

































Corrected
ATOT

































t
N9
         Sonicated all PASs and bulk dyes  for  10 min after primary dilution (1° diln.).   Agitated all filters on shaker for 30 min
         after primary dilution.

         Corrected A,OT = ATOT field air filter sample extract - A,.-, field air filter blank extract.

-------
                                  Form A-2

                                 8856-A(01)

                  INDIVIDUAL DYE SOLUTION PREPARATION FORM'
                                       Section No.:  Appendix  B
                                       Revision No.:  3
                                       Date:  April 30, 1987
                                       Page B-ll of 20
Plant ID:
        Prepared by:
Analytical  Balance ID:
                Model No.:
Calibration Weights Used:
Instrument Calibration:   Post-Tare
                         Pre-Tare
                 	 mg weight =
                     Date:
                     MRI No.:

                     MRI No.:
                                     (accuracy =
Sample ID No.
Pre-Tare (g)
Post-Tare (g)
Dye Weight (g)
 See Dye Analysis Schedule for dilutions of the above weighed dyes.
                                  A-93

-------
                                              Section No.:   Appendix B
                                              Revision No.:   3
                                              Date:  April  30, 1987
                                              Page B-12 of 20
11.2  Based on the dye usage data from the drug room site, determine
      the major use dye subset (i.e., those dyes which comprise at
      least 80% of the total dye quantity handled during the monitoring
      period).  Using Section II of Form A-3, calculate the relative
      weight fraction for each of these dyes.  Using this value and the
      target dye concentration value (calculated in Step 11.1), calculate
      target concentrations of each dye in the dye subset.

11.3  Using Form A-4 and the dye solvent, prepare the spiking standard
      solution containing all of these dyes in proportion to their weight
      fractions.  The total dye concentration of the spiking standard
      solution should be as close to the target value (calculated in
      Step 11.1) as possible.

11.4  Place a blank air filter (i.e., filter blank from the same lot as
      was used at the drug  room site) and pad into a three-piece 37-mm
      cassette and secure with the extension piece.

11.5  Using a 100-uL syringe, carefully dispense 100 uL of spiking
      standard solution from Step 11.3 onto the air filter.  The volume
      delivered represents  the 130% high level of total dyes calculated
      in Step 11.1.  Deliver the spike in a scattered pattern over the
      entire  filter.  Set aside to dry.

11.6  Repeat  Steps 11.4 and 11.5 for the duplicate high-level spiked
      filter  control.

11.7  Deliver the same volume of spiking standard solution used in
      Step 11.5 into an empty 4 oz amber glass jar.  Set aside to dry,
      leaving the jar uncapped.  This is the reference standard at the
      high level.

11.8  Repeat  Step 11.7 for  the duplicate high-level reference standard.

11.9  Repeat  Steps 11.4 through 11.6 for the spiked filter controls at
      the low dye  level, using 50 uL of the spiking standard solution
      prepared  in Step 11.3.

11.10 Repeat  Steps 11.7 and 11.8 for the low-level reference standards
      using 50 uL of the spiking standard solution for each.

11.11 Repeat  Steps 11.4 through 11.6 for the spiked filter blanks, using
      dye solvent in place  of the spiking standard solution.  Use the
      same volume used to spike the high-level spiked filter controls,
      e.g., 100 pL for each blank.

11.12 If the  pH 3 dye solvent was used in Step 9.2, use the pH 3 dye
      solvent (Step 6.4) to perform Steps 11.3-11.11.
                              A-94

-------
                                   Form A-3
                 Section No.:  Appendix B
                 Revision No.:  3
                 Date:  April 30, 1987
                 Page B-13 of 20
                                  8856-A(01)

                   SPIKING STANDARD SOLUTION ESTIMATION FORM
 Plant:
 Date:
Name:
 I.  Total Dye Estimate on Personal Air Filters
Filter ID No.


Corrected ATQT


Total Dye Estimate (pg)a


Average Total
Dye Estimate
(M9>

 a .          ATOT x Dilution Volume  -  _
  where |jg =	;  a  -

                       as
 II.  Target Values for Dye Subset Comprising ^ 80-90% of Total Quantity Dye
      Handled:
      Spiking Standard Solution's Target Total  Dye Concentration =

      130% x	ug (avg.  total dye estimate)  _
          100 uL (high level spike volume)       	
Bulk Dye
ID No.













% of Total Quantity
of Dye Handled













Relative Weight Fraction =
% Total for Dye
% Total in Dye Subset













Target Cone. (ug/uL)
(Rel. Wt. Fraction x
Target Tot. Dye Cone.)













 % Total
  in Dye
\  Subset
                                   A-95

-------
                                                    Section No.:  Appendix B
                                                    Revision No.:   3

                                  Form A 4          £ate:  April 30> 1987
                                  form A-4          Page B_14 of 2Q

                                 8856-A(01)

    SPIKING STANDARD SOLUTION PREPARATION FORM AND DATA  ON SPIKED FILTERS

Plant:  	          Date:  	

Analyst:  	
                                       LNB:  page no.:
I.  Spiking Standard Solution Preparation:
     Analytical balance ID:
     Calibration weight ID:
     Calibration:
       Post-Tare:  	
       Pre-Tare:
           mg weight =
                                             (accuracy =
II.  Dye Weights (Use additional sheets  if  necessary)

     Dilution Volume:
     Post-Tare:
      Pre-Tare:
Dye No.	 wt.:
  Actual Cone.:"

     Post-Tare:
      Pre-Tare:
Dye No.	 wt.:
  Actual Cone.:
                             Post-Tare:
                              Pre-Tare:
                        Dye No.	 wt.:
                 ug/uL    Actual Conc.T

                             Post-Tare:
                              Pre-Tare:
                        Dye No.	 wt.:"
                 ug/uL    Actual Conc.:^
     Post-Tare:
      Pre-Tare:
Dye No.	 wt.:
  Actual  Cone.:

     Post-Tare:
      Pre-Tare:
Dye No.	 wt.:
  Actual  Cone.:
III.  Spiked Filter Data

A.  Filter ID:
B.
    No. of High-Level Spiked  Filter  Controls  Prepared
    No. of Low-Level Spiked Filter Controls Prepared _
    No. of Spiked  Filter Blanks  (DMSO  only) Prepared 	.
    No. of "Dry" High-Level Spiking  Std.  Controls  Prepared_
    No. of "Dry" Low-Leye.1 Spiking Std.  Controls Prepared_
Date filters placed on sampling pumps:
Date filters and "dry" controls are to
                                                     ;  Vol. Spiked 	 uL
                                                      Vol. Spiked 	 uL
                                                      Vol. DMSO used
      be extracted/analyzed:
                                     short-term
                                     long-term
                                     longest-term
    No. of filters to be prepared/analyzed:
                                   Filters
       (short-term)
       (long-term)
       (longest-term)
high;
high;
high;
low;
low;
low;
blank
blank
blank
     ;  Vol.  Spiked
      Vol.  Spiked _

         (name)
 ML
_ML
  ML
                                                           "Dry" Controls
                                                           	 high; 	
                                                           	 high; 	
                                                              high; 	
                      low
                      low
                      low
                                   A-96

-------
                                                    Section No.:   Appendix B
                                                    Revision No.:   3
                                                    Date:   April  30, 1987
                                                    Page B-15 of 20
      11.13 Very low dye spiking levels (e.g.,  < 50 ug) result in weak ab-
            sorbances which are difficult to quantitate with a high degree of
            confidence.   As a result,  recovery  data based on low spike levels
            are more uncertain than those obtained for higher dye spiking
            levels.   To address this potential  problem, low personal air
            filter dye estimates will  be bracketed by the high and low spiking
            levels,  but spiking will also be done at an elevated level (e.g.,
            100 ug)  as well.


12.0  EXPOSURE OF SPIKED FILTER CONTROLS, BLANKS. AND REFERENCE STANDARDS

      12.1  Calibrate personal air pumps to draw air at a rate of 2 to
            2.5 L/min.

      12.2  Attach the dry spiked filter cassettes prepared in Section 11.0
            to individual  personal  air pumps and draw air through the cassettes
            for 6 to 8 h.   (Relative humidity in the immediate vicinity should
            be in the range of 30 to 70%.   Fluorescent lights should be on
            during the exposure period.)

      12.3  During Step 12.2, place the reference standards in the immediate
            vicinity of the aerating filters so they are exposed to the same
            lighting and humidity conditions.


13.0  ANALYSIS OF DYE SOLUTIONS

      13.1  Spectrophotometer Operating Parameters

            13.1.1 Turn main  power switch to "on" position.   Allow Visible-UV
                   light source to warm up for  at least 20 min.

            13.1.2 Adjust  the following parameters to their proper settings:

                  Source  select:   auto
                  Beam interchange:   normal
                  Mode:   autogain
                  Timer mode:   off
                  Slit:   2.0 nm
                  Abs.  zero  suppression:   0
                  Range:   1.0 absorbance units full  scale
                  Chart:   off
                  % zero  suppression:   off
                  Period:  0.5 s
                  Pen:  on
                  Autobaseline:   on
                                  A-97

-------
                                                   Section No.:  Appendix B
                                                   Revision No.:  3
                                                   Date:  April 30, 1987
                                                   Page B-16 of 20
                  Scanning rate:  1 nm/s
                  Chart display:  50
                  Scan:  off
                  Function:  off
                  Measurement:  serial
                  Log A offset:  0.1
                  Concentration:  turn  knob completely  to  left
                  Analog signal output:  0-10 V

           13.1.3 Set the  upper wavelength limit  (e.g., 800  nm  )  using  the
                  wavelength 1 dial.  Set the lower wavelength  limit  (e.g.,
                  330 nm ) using the wavelength 2 dial.

           13.1.4 Using the "scan" dial, turn dial (+)  or  (-) to  set
                  the wavelength at the upper limit (e.g., 800  nm).

      13.2  Analog/Digital  Computer Interface Box  Operating Parameters

           Maximum  Input Voltage:  10 V
           Run  Time:   interface box run time must exceed actual analysis
                       run  time  required to scan the wavelength  range, e.g.,
                       at 1 nm/s from 800 nm to 330 nm,  the analysis run
                       time is  7.83 min.  Therefore, an  interface  run  time
                       of > 8 min  is required.
           Sampling Time:  1 point/s

      13.3  Absorbance  Measurement of Filter Extract Solutions

           13.3.1   Zero the  spectrophotometer by  placing the dye  solvent
                    (filtered  using a 0.45 urn Gelman Acrodisc)  in
                    both the  sample and  reference  cuvettes.   Turn  the  auto-
                    baseline  knob  to "record" and  check  to  see  that red  light
                    comes on.   (Autobaseline knob  will automatically return  to
                    "on" position.)  Adjust the balance  knob  to  give an  absor-
                    bance reading  of *  0.1000 on  the digital  display.  Turn
                    timer mode  knob to  "sample and wavelength,"  then back  to
                    "wavelength."  Depress  "step"  button and  scan  the  wave-
                    length  range (note:   upon completion of the  scan,  the  upper
                    wavelength  will automatically be reset).   After the  wave-
                    length  is  reset, turn the timer mode knob to the "off"
                    position.   Adjust the balance  knob to give an  absorbance
                    reading of *• 0.0500  on  the digital  display.   Turn  timer


aThe maximum voltage  must correspond  to the maximum  signal  input of  the
   A/D box.
b  This setting can  be  anywhere in the  range 750-800  nm.
c  This setting can  be  anywhere in the  range 300-350  nm.  It is usually  deter-
   mined by the point where the grating in the  spectrophotometer changes
   from the visible  to  the  ultraviolet  region.
                                   A-98

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                                                 Section No.:  Appendix B
                                                 Revision No.:  3
                                                 Date:  April 30, 1987
                                                 Page B-17 of 20
                 mode knob to "sample and wavelength," then back to "wave-
                 length."  Depress "step" button, simultaneously starting
                 the Nelson interface box, and scan the wavelength range
                 to obtain a flat baseline from 800-330 nm.  Empty the
                 sample cuvette.

         13.3.2  Analyze each filter extract solution, according to the
                 Dye Analysis Schedule, by withdrawing the filter extract
                 solution into a 10-mL disposable syringe.   Attach a
                 0.45 urn Gelman Acrodisc filter onto the end of the
                 syringe and filter the extract solution into the sample
                 cuvette.  Retain the remainder of the extract solution.

         13.3.3  Scan the filter extract solution over the wavelength
                 range, starting the A/D box at the beginning of the scan.
                 Examine the scan during the analysis run.   If the dye
                 absorbance exceeds 1.0, abort the analysis run immedi-
                 ately  and make an appropriate dilution of an aliquot of
                 the extract solution.   Scan immediately.   Document dilu-
                 tion and time deviations on the Dye Analysis Schedule.

   13.4  Absorbance Measurement of Individual Dye Solutions

         13.4.1  Zero the spectrophotometer according to the procedure out-
                 lined in Step 13.3.1.


         13.4.2  Analyze each dye solution, according to the Dye Analysis
                 Schedule, by withdrawing the dye solution from Step 10.3
                 into a 10-mL disposable syringe, attaching a 0.45 urn
                 Gelman Acrodisc filter onto the end, and filtering into
                 the sample cuvette.

         13.4.3  Scan the dye solution over the same wavelength range used
                 for the filter extract solutions, starting the A/D box at
                 the beginning of the scan.

         13.4.4  The maximum absorbance in the dye spectrum should be in
                 the range of 0.1 to 1.0 absorbance units.   If the dye
                 absorbance does not fall within this range, abort the
                 analysis run immediately and repeat Step 13.4.3 using an
                 appropriate dilution of an aliquot from the flask in Step
                 10.2.   Scan immediately.  Document dilution and time devi-
                 ations on the Dye Analysis Schedule.
Turn the timer mode knob to "off" and stop the Nelson Box.   Turn the scan
knob to (+) side and increase scan rate until  the wavelength is ~ 790 nm.
Return scan rate to 1.0 nm/s.   Turn scan knob  to "off" position at 800 nm.
                               A-99

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                                                    Section No.:  Appendix B
                                                    Revision No.:   3
                                                    Date:  April 30, 1987
                                                    Page B-18 of 20
14.0  ANALYSIS OF SPIKED FILTER CONTROLS AND BLANKS

      14.1  Extract all spiked filter controls and blanks as outlined in
            Steps 9.1-9.6.

      14.2  Scan each spiked filter extract solution as outlined in Steps 13.3.1
            through 13.3.3.

      14.3  Dilute each reference standard with 8.0 ml of dye solvent, cap, and
            mix well.

      14.4  Scan each reference standard solution in the same manner as the
            spiked filter  extracts in Step 14.2.


15.0  Determination of Total Area Counts in a Dye Scan

      15.1  For spectrum  integration purposes, calculate, to the the nearest
            0.01 min, the  time required to scan the sample over the desired
            wavelength range.  (Scanning from 800-380 nm at 1 nm/s takes
            420 s = 7.00  min.)

      15.2  Plot the  data  file in the "re-detect" mode of the Nelson integra-
            tion software.   Using the cursor, manually integrate the area
            above the baseline from 50 s (0.8333 min = 750 nm) to the calcu-
            lated time (e.g., 7.00 min = 380 nm).

            Note:  The height of the baseline is determined by integration of
            the dye  solvent over the calculated time period.  In some cases,
            due to baseline drift, the baseline used for integrating data
            files may deviate slightly.

      15.3  Obtain a  hardcopy of the file  integration for archiving purposes.


 16.0  CALCULATIONS

      16.1  Total Absorbance (ATOT).  -^  integration software from Nelson
            Analytical divides the maximum signal  into 106 parts (counts).
            Since the full scale  signal  at any  particular wavelength  is
            equal to  1.0  absorbance  units,  there  are 106 area counts per
            absorbance unit.  Therefore, by  dividing the total area counts
             (obtained in  Section  15.0) by  a  factor of 106, a total absorbance
            value  is  obtained.

            Note:  ATnT  values  for  field air filter samples and  air sampling
            cassettes are corrected  for  background absorbance by subtract-
             ing the  ATnT  value  for  the  corresponding  field air filter blank(s).
            ATnT values  for individual  bulk dye solutions are not  subject  to
             these  background absorbances and therefore  need  no correction.
                                    A-100

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                                              Section No.:  Appendix  B
                                              Revision No.:   3
                                              Date:  April 30, 1987
                                              Page B-19 of 20
16.2  Spectral Absorptivity Constant (a ) for Individual Dyes:  Based
      on Beer's law, each individual dyl's spectral absorptivity con-
      stant (a ) is calculated using the formula:


                                ATOT
                          d  —
                          *s    b x c
      where b is the cuvette pathlength in cm (e.g., 1 cm), c is the
      dye concentration in vg/ml, and ATOT is the total absorbance of
      the dye solution.  The dye concentration will be expressed in
      terms of a commercial dye basis (i.'e., assume 100% purity) and an
      active ingredient basic (i.e,  using dye purity values supplied by
      ETAD).

16.3  Weighted Average Spectral Absorptivity Constant (a ) for the Dye
      Analysis Set:   This value is obtained from the individual  dye a
      constants in the dye analysis  set,  using the dye handling informa-
      tion to obtain the appropriate weight fraction for each component
      dye.

16.4  Dye Recovery Determination for Spiked Filter Controls:
      The recovery value for the group of major use dyes is calculated
      from the ATQT values obtained  from  the spiked filter controls and
      the corresponding reference standard solutions.   Percent recovery,
      R, is calculated using the formula:

   _ AjQ-p of Spiked Filter Control - ATOT of Spiked Filter Blank   -.Q0

                         of Reference Standard


16.5  Total Dye Estimate on the Air  Filter:   This is calculated using
      the formula:

                                         TOT X
             Total  Dye Estimate (ug) =   IUI
                                         a  x b


      where V is the volume of the filter extract solution in ml (AjOT,
      a ,  and b are defined above).

16.6  Correction of Dye Estimate for Percent Active Ingredient of Dyes:
      The  total dye estimate is also reported in terms of the active
      ingredient content from the individual dyes.   This correction, made
      by using dye lot purity information provided by ETAD,  is per-
      formed on all field air filters as well as their corresponding
      cassettes.
                           A-101

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                                              Section No.:   Appendix B
                                              Revision No.:   3
                                              Date:   April  30, 1987
                                              Page B-20 of 20
16.7  Correction of Dye Estimate for Extraction Efficiency:   The total
      dye estimate is also corrected for the extraction efficiency of
      the analytical method.   The overall average dye recovery value is
      used to make the correction.   This correction is performed only
      on the field air filter samples.

16.8  Average Airborne Dye Concentration:  This is calculated by divid-
      ing the total dye estimate (in mg) by the total volume of air
      sampled during the monitoring period (in m3).
                            A-102

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    SUPPLEMENTAL B



DATA QUALITY OBJECTIVES
         B-l

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8-28-86
                     DATA QUALITY OBJECTIVES
               FOR THE TEXTILE DYE DRUG ROOM STUDY
I.   STUDY OBJECTIVES

1.   Estimate the distribution of the 30 breathing zone dye
     concentrations observed in the monitored plants (8 hour time-
     weighted concentration), specifically:

     a.   the average breathing zone dye concentration at the
          plants
     b.   the upper percentiles (85th percentile)
     c.   confidence intervals for both estimates
2.   Determine if dye concentration in breathing zone, adjusted
     for time in drug room is correlated with mass of dye weighed,
     number of weighings/shift, or other factors (see Appendix A),
     and if so, determine a functional relationship  between
     concentration and factors.

3.   Estimate the average, and distribution of, mass and number of
     weighings of individual solid dye compounds weighed out
     during a shift (averages and histograms need to be presented
     by dye class and aggregated)

4.   Summarize selected drug room observations and general plant
     information in table form (see Appendix B for items to be
     summarized)

5.   Obtain an extensive first-hand, qualitative view of drug room
     operations (the final result will be an individual industrial
     hygiene report for each of the 30 plants visited)

Objective 1 is the most important; items 2-5, all of roughly equal
importance, are supplemental to objective 1 but will also enhance
the knowledge of dye exposure.  Besides the objectives of the
study, other aspects of the data will be explored (see Appendix
C).


II.  BACKGROUND

     About 1000 domestic textile dyeing or printing sites have
been identified where there is potential for workers to be exposed
to numerous powder dyes via inhalation or dermal routes.  There
are reasonable indications that some dyes or their metabolites
                               B-3

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might be carcinogens or mutagens.  Data which document potential
exposure levels of workers associated with the weighing or mixing
of powder dyes are limited, some of which were obtained from non-
textile dyeing operations.  The objective here is to conduct a
well designed study of textile dye weighing rooms in order to
improve the assessment of exposure (and associated risk) with the
use of powder dyes in the American textile industry.  This study
is being sponsored jointly by the American Textile Manufacturers
Institute  (ATMI), the Ecological and Toxicological Association of
the Dyestuffs Manufacturing Industry (ETAD) and the Office of
Toxic Substances  (OTS) of EPA.


III. DATA COLLECTION APPROACH

     A two phase  approach was chosen for the study.  The first
phase was a mailed out questionnaire to 240 plants selected as a
simple random sample from 1390 textile facilities thought to
potentially use powder dyes.  The first phase goals were: to make
sure that  the list of 1390 plants was not missing any major groups
of dyeing plants  (and thus provide a pool from which to draw that
is not grossly unrepresentative); to provide valuable general
information on drug  room operations including data useful to
industrial hygienists in preparing for in-plant monitoring; and
possibly  to provide  assistance for stratified random sampling.

     The  second phase will be a  stratified random sample with the
two  strata being: 1. Respondents to first phase questionnaire; 2.
Non-respondents  to  first phase questionnaire.  Plants will be
selected  with  representation proportional to strata sizes.  Actual
in-plant  airborne dye-level monitoring and drug room observation
will  take place  in  30 plants at  this phase.  The two strata were
chosen  to separate  first phase respondents from nonrespondents
since  there might be differences in the nature of exposure levels,
and  since it  is  desired  that the final representation from the two
groups  reflect  the  actual population of dyeing plants.

     Within each  of  the  30 plants selected, a two member team will
record  measurements  and  observations in the plant to satisfy the
study  objectives  (see Appendices A and B  for the approximately 40
items  recorded  and the Quality Assurance  Project Plan for the
methods).   For  one randomly  selected dye  weigher at each plant, a
more extensive  examination of practices and potential exposure
will be  conducted (only  one  weigher will  be chosen  to balance the
needs  of  the  six  objectives  between themselves  in the presence of
limited  resources).   This  weigher will be observed  and monitored
during  one randomly selected  shift.  The  monitoring will take
place  during  nearly an  entire  8-hour period by personal monitoring
equipment designed to  collect  solids from the air in the breathing
zone of  the  selected worker.  These will  be laboratory analyzed to
determine total  dust mass  and  total dye mass.  For  the monitored
weigher,  observers will  also  record the mass of each powder dye
                                B-4

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and chemical weighed, the total number of powder dyes weighed,
the amount of time the weigher spends in the weighing area, and
other qualitative and quantitative measurements.  Also, the
observers will record information on size of dyeing operation,
cleanliness, ventilation, possible routes of exposure, and other
qualitative information.
IV-  DATA QUALITY OBJECTIVES

1.   Sources of Variability

     a.   Error Associated with Chemical Analytical Procedures

          The 95% confidence bounds for the measured dye level
          will differ from plant to plant (since essentially a
          unique material will be collected at each plant).
          These error bounds will also differ within any given
          plant depending on whether dyes measurement is on a
          commercial dye or an active ingredient basis.  The
          potential range of variability is so great, in fact,
          that it is not feasible to predict the magnitude of the
          95% confidence bounds for any dyes measurement until
          all of the component dyes have been analyzed.

          After examination of the 95% confidence bounds for the
          results from each of the 24 plant sites in the study,
          it can be stated that these confidence bounds will
          generally be ^ 70% of the reported value on a
          commercial dye basis and + 80% on an active ingredient
          basis.  The largest part of the uncertainty for any of
          the dye measurements is the use of a weighted average
          as constant to approximate the absorption
          characteristics of the dye mixture on the air filter.
          Other sources of error in the dye measurement, such as
          those due to systematic errors in the laboratory,
          method precision, or uncertainties in the dye recovery
          values, are relatively minor components of the total
          error estimates described above.
                               B-5

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b.   Sampling Error Associated with the Survey

     The sampling error discussed here is the error
     introduced from selecting a sample of textile dyeing
     plants versus monitoring one shift for the entire
     population of textile dyeing plants.

     The total sampling error introduced will depend upon  the
     variability between plants.  However, using the data
     collected by the National Institute for Occupational
     Safety and Health  (NIOSH) and the CIBA-GEIGY dye firm,
     for three textile  dyeing and one paper dyeing plant,  the
     standard error expected for estimating the average
     exposure is approximately 15% of the estimated average
     (2 standard errors = + 30% on this basis), due to the
     sampling error as  described.  For estimating the 85th
     percentile, a nonparametric 95% tolerance interval would
     utilize  the second highest measured plant value as its
     upper bound  (again, this includes error associated with
     the plant sampling procedure and not such things as
     chemical measurement error); however more precise
     intervals are likely to be obtained through the use of
     probability distributions to estimate the 85th
     percentile and  its confidence interval.

 c.   Nonrandom Error Associated with the Survey

     There are several  potential sources of error  (i.e.,
     nonsampling errors) besides the four random-type errors,
     such as  refusal to allow monitoring  (this is a voluntary
     study),  and possibly encountering artificially clean
     conditions at the  time of the site visit.  Only
     qualitative,  subjective  judgments can be made about
     these  factors.  However,  to help preserve the usefulness
     of the  study, an  energetically pursued target of
     obtaining  entry to at  least 75% of selected plants has
     been  set.  But  given the  existing data, a lower bound of
     60% monitoring  acceptance has been set.  Should the
     acceptance  rate drop below  60% the current objectives
     will  not be  met and a  reevaluation of  the approach will
     be made.
                           B-6

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2.   Completeness

     The survey collection is considered complete when 30 plants
have been monitored, with a second phase response rate of at least
60%, and all 30 chemical analyses are determined to be possible.
3.   Comparability

     All chemical analyses will be done at a single laboratory,
Midwest Research Institute.  All field collection will be
conducted by Health and Hygiene, Inc. under contract with
participating industry trade associations, and by the firm PEI
Associates, Inc. under contract with EPA.  All observational data
will be collected via answers to direct questions or open ended
questions with suggested answers provided, wherever possible, to
maintain comparability between responses at the 30 plants.  Also,
directing the scope of the answers on the data collection form
insures that the reported observations actually answer the
questions that EPA and the dye industry want answered.

     No other such data collection has been done in the past, nor
has the method for estimating total amount of dye been used
before.  The earlier studies by NIOSH and CIBA-GEIGY measured the
amount of a limited number of specific dyes, and only three of the
plants were textile mills.


4.   Representativeness (assumptions and universe of interest)

     a.   The stratified simple random sampling plan will provide
          estimates on a national scale and with an
          (approximately) known amount of uncertainty due to plant
          sampling.

     b.   Plants were considered to be within the scope of the
          study if they dyed or printed textiles using powder dyes
          with mechanical equipment.  Any amount of dyeing was
          considered within the scope of the study.

          Drug rooms are considered within the scope of the study
          if any amount of weighing takes place there on a regular
          basis.

          Weighers are the only type of worker represented in the
          study.  Interest focuses on the weigher since he or she
          is the one handling the largest amount of powder dyes.
          No direct statement can be made about other workers
          except that they are assumed to be exposed to
                               B-7

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     substantially lower levels of dye.

c.   Although the primary goal is to obtain estimates of
     average plant levels and the distribution of plant
     levels, it is possible to obtain estimates of average
     weigher exposure by randomly selecting a worker within
     the plant.  For example/ statements could be made about
     the 85th percentile of worker exposure by weighing plant
     estimates by the number of weighers in each plant.  This
     would  result in a statement such as "It is estimated
     that 85% of weighers are exposed to levels lower than
     xxx mg/m3 during an 8-hour shift."  Note that this
     differs from the estimate of 85th percentile of plant
     levels which results in a statement such as:  "It is
     estimated that the average exposure in 85% of textile
     dyeing and printing plants is less than zzz mg/m3, time-
     weighted 8-hour average" (xxx and zzz determined from
     study).
                           B-8

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APPENDIX A     SECONDARY MEASUREMENTS TO EXAMINE FOR ASSOCIATION
               WITH DYE LEVEL

     The dye concentration adjusted for time in drug room, (total
dye collected)(time personal monitor on/time in drug room), will
also be examined for correlation with several other variables of
secondary importance.  These are:
                                *    f
     1.   Production volume of textiles (pounds per year), from
          mailed-out questionnaire
     2.   Management of dye house (vertical, commission or both),
          from mailed-out questionnaire
     •3.   Management of dye house;(public or private),  from
          mailed-out questionnaire
     4.   Color index class of dyes used, for any dye used during
          observed shift by monitored weigher (acid,
          basic/cationic, reactive, direct,  disperse, other), from
          site visit log as classified  by Chemical Engineering
          Branch
     5.   Total number of dyeing and printing machines  serviced by
          monitored weigher (average of beginning and end of shift
          numbers), from site visit questionnaire
     6.   Number of fiber types dyed or printed
          (acrylic/modacrylic, rayon/cotton, nylon, polyester,
          other) at site, taken from mailed-out questionnaire

     It should be noted that a data set of only 30 observations is
likely to result in some spurious large correlation when many
correlations are calculated.  Thus the  correlations of  this
section will be interpreted in that light.
                               B-9

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APPENDIX B
SUMMARY TABLES
     1.  ON-SITE QUESTIONNAIRE

     Summary tables will be presented for several other variables
collected from the on-site questionnaire with categorized
responses.  The variables to be tabled are:
1.   Number of
     a typical
2.   Number of
3.   Number of
4.   Number of
5.   Number of
6.   Number of
7.   Number of
8.   Number of
     visit
9.   Number of
     visit
plants by number of weighers,  at all shifts during
24 hour period
plants by pounds of dye weighed during shift
plants by number of dyes weighed during shift
plants by number of dye weighings during shift
workers by amount of time in drug room
workers that used dust mask  during site visit
workers that used respirator during site visit
workers that smoked in drug  room area during site

workers that ate in drug room area during site
                              B-10

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     2. MAILED-OUT QUESTIONNAIRE

     As an appendix in the final report, the following variables
will be tabulated from the first-phase, mailed-out questionnaire:

*11. Number of textile dyeing plants in each EPA geographical
     region
 12. Number of plants by number of dyeing or printing operations
     within the company that owns the selected plant
@13. Number of plants by management of house (vertical,
     commission, or both)
@14. Number of plants by management of house (public, or private)
@15. Distribution of plants by product volume
 16. Number of plants by product line (carpet, yarn, fabric,
     other)
#17. Number of plants by type of dyeing or printing equipment
     available (batch, semi-continuous/continuous, printing)
@18. Number of plants by fiber dyed or printed
     (acrylic/modacrylic, rayon/cotton, nylon, polyester, other)
@19. Number of plants by color index class of powder dye (acid,
     basic/cationic, reactive, direct, disperse, other)
 20. Number of plants by number of dyes weighed per 24 hours (less
     than 10, 10 to 20, over 20)
&21. Number of plants by pounds of dye used per 24 hours (less
     than 50, 50 to 200, over 200)
&22. Number of plants by number of powder dye weighings per 24
     hours (less than 50, 50 to 500, over 500)
 23. Number of plants by number of dye weighing rooms ( 1 room, 2
     or more rooms)
 24. Number of plants by number of worker shifts per 24 hours (1,
     2, 3)
 25. Number of plants by number of operating days per week
     (1 to 4, 5, 6 or 7)
 26. Number of plants by number of employees exposed to powder
     dyes (1, 2, 3, 4 or more)


Notes

*    This is also tabulated from site visit data
#    Similar information is also collected in the on-site
     questionnaire and is used in the secondary correlation
     analysis (see Appendix A)
@    A portion of the data on this variable will be used in the
     secondary correlation analysis (see Appendix A)
&    Similar information also collected in the on-site
     questionnaire and is used in the primary correlation analysis
                              B-ll

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             APPENDIX C   NOTES ON STUDY OBJECTIVE 1
     Although the primary objective of the study is as stated in
objective 1, the approach chosen warrants discussion.

1.   The main objective and procedure

     One worker  (dye weigher) will be monitored at each of the 30
plants visited.  This measured value will be used to represent a
typical measurement from that plant.  These 30 breathing zone dye
concentrations will be used for an estimate of the distribution of
dye concentrations typically found in plants across the U.S.


2.   Another way of looking at exposure distribution which will be
     presented in a report appendix

     Note that the above procedure focuses on levels typically
found  in textile dyeing plants.  Another approach is to look at
the distribution of weigher  (worker) exposures.  This implies that
a plant with three  (3) workers should receive three  (3) times as
much weight as a plant with one  (1) worker, since the workers
there  represent  three  (3)  times as much of the population.  This
approach has considerable  appeal; however, practical problems are
discussed in Section 4 of  this Appendix.


3.   Distinction with  the  main objective

     Although  Section  2 of this Appendix discusses the main
difference  between  the chosen procedure focusing on  typical levels
found  in plants  and the alternative approach, this section
elaborates  upon  the distinction.

     In contrast with  objective  1, the alternate approach takes
into account the number of weighers working at each  plant and is
weighted according  to  the  number working at the monitored plant
during a typical  24-hour period.  For example, statements could be
made about  the 85th percentile of worker breathing zone dye
concentration  by weighing  plant  estimates by the number of
weighers in each plant.  This would result in a statement such as
"It  is estimated that  85%  of weighers are potentially exposed to
concentrations lower  than  xxx mg/m3 during an 8-hour shift."  Note
that this differs  from the estimate of the 85th percentile of
 •)lant  levels  (objective 1) which results in a statement such as:
  It  is estimated that  the  average concentration in 85 percent of
  »xtile dyeing and  printing  plants  is less than zzz  mg/m3, time-
   ighted 8-hour  average"  (xxx and zzz determined from study).
                               B-12

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4.   Reason for chosen emphasis

     Although it would be ideal to sample every weigher at every
shift of the sampled plants, it is not feasible for several
reasons:

     o    cost:  monitoring more than one weigher per visit would
          raise laboratory and site visit costs dramatically.  At
          least one extra person would need to travel to the plant
          site to record the dyes weighed by an extra weigher, the
          relative amounts of each dye weighed, set up the
          personal air samplers, and collect specimens of each dye
          weighed by the additional weigher.  The laboratory would
          then need to develop a new procedure to chemically
          analyze the mixture of dyes weighed by the second
          worker.

     o    personnel maximum;  monitoring workers by having more
          than two (2) observers per site is often not feasible
          due to limited workspace at the sites.  Furthermore,
          cooperation in this voluntary study could be impaired by
          requesting to send a larger delegation.

     o    balance with other objectives;  sending a larger team to
          each site would allow for some information on the
          importance between worker variability and allow for a
          s.omewhat better estimate of the distribution of
          breathing zone dye concentrations associated with the
          population of dye weighers.  However, much of the study
          concentrates on observations made on conditions and
          possible routes of exposure at the plant/drug room
          visited (i.e., more dye measurements would not
          necessarily improve these aspects of the study
          appreciably); the potential routes of exposure on a
          plant by plant (or drug room by drug room) basis are
          also of direct interest.

     o    correlation between reported dye concentrations at the
          same plant:  simply monitoring two workers at the same
          plant does not provide for two independent estimates of
          dye concentration due to the nature of the chemical
          analysis method.  That is, the error in the chemical
          measurement is such that repeated measurements at the
          same site will tend to be repeatedly too high or too low
          if the same dyes tend to be used (and, less importantly,
          that the mechanism for exposure remains the same).  This
          is due to the fact that the proportional amount of dyes
          in the mixture on the filter is not known, so that the
          error in using the average absorbance value tends to be
          in the same direction for repeated chemical analyses of
          similar mixtures  (also, the percent recovery estimate
          will have a similar tendency to be repeatedly too high
          or too low for the same unknown mixture).  However, this
          should cancel out when estimating the 30-plant average.
                              B-13

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             SUPPLEMENTAL C



LETTERS, TO ENCOURAGE PLANT PARTICIPATION
                 C-l

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                      AMERICAN TEXTILE MANUFACTURERS INSTITUTE, INC.

                      1101 CONNECTICUT AVENUE, N W . SUITE 300. WASHINGTON. D.C. 20036
                                                            TWX: 710-822-9489
                                                             TEL: 202 862-0500
                                                 November 18, 1985
 Dear

       The American Textile Manufacturers Institute (ATMI) and the
 Ecological and Toxicological Association of the Dyestuffs Manufacturing
 Industry (ETAD) are performing a study to determine the .extent to which
 textile workers may be exposed to dye dust when weighing and mixing
 powder dyes.  This study is being done in cooperation with the U.S.
 Environmental Protection Agency (EPA).

       Your plant is one of 200 textile dyeing or printing sites which
 has been randomly selected for surveying.  The purpose of this
 preliminary survey is to gather information about production
 capabilities, fibers processed, product lines, dyeing/printing
 operations and prevailing practices of worker protection in order to
 obtain a broad picture on the use of dyestuffs for textiles and the
 potential for worker exposure.  From these 200 companies, 30 will be
 selected as representing typical plants in the textile dyeing/printing
 industry.  They will be requested to permit voluntary monitoring using
 personal monitors of the workers in drugrooms by a private consulting
 firm, Health and Hygiene Company of Greensboro, North Carolina, who will
 be accompanied by an EPA representative.  The professional staff of
 Health and Hygiene have considerable textile experience and are highly
 suited and well qualified for this assignment.

       Monitoring data will be used by industry and EPA as a basis for
 estimating potential levels of exposure of workers to powder dyes.  No
 regulatory action will be generated against individual participants as a
w/'\

    £                            C-3

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result of this data gathering program.  Data will be coded by ATMI and
submitted only in coded form to EPA.  After the survey forms have been
reviewed for completeness, the code will be destroyed.

      You are requested to voluntarily complete the enclosed survey
forms which will provide  information which is necessary to initiate the
program.  To aid you, we  have included with the survey forms,
instructions and an example of a completed survey.  If any proprietary
business information  is provided which should be treated as
confidential, so indicate by encircling the Y on the confidential
business information  (CBI) line at the top of the appropriate page(s).
Your request will be  respected.  We would appreciate hearing from you by
December 5, 1985.  If you have any questions, please contact Maggie
Dean, (202) 862-0580.  We extend our thanks for your cooperation and
assistance in this industry -government cooperative program.

                                                Sincerely,
                                                Carlos Moore
                                                Executive Vice President
Enclosure
OIS/7T/1-2/CS
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                      o
                         AMERICAN TEXTILE MANUFACTURERS INSTITUTE, INC.
                         1101 CONNECTICUT AVENUE, N.W.. SUITE 300. WASHINGTON. D.C. 20036
                                                               TWX: 710-822-9489
                                                               TEL: 202,862-0500
                                                  December 20, 1985
  Dear Mr.  Carton:

        This  confirms  our recent telephone  conversation relative to the
  Textile  Drug Room Monitoring Study.  Your par-ticipation in this survey
  is of the utmost  importance.   The  answers you provide will help us move
  to the second phase  of a. survey whose ultimate goal is to gather
  information that  will  be shared with the  U.S.  Environmental Protection
  Agency (EPA)  to characterize the workplace exposure levels of the dyes
  in dye weighing and  mixing rooms of textile dyehouse and printing
  operations.

        The value for  an exposure level which EPA currently uses in
  existing  chemical assessments  is based  on the level detected in the
  leather  industry,  which is probably a higher number than might be
  observed  in the textile industry.  Ultimately,  in this survey, the
  measured  levels of dye in the  air  of 30 drug rooms of the sampled
  textile dyeing and printing plants will provide a more representative,
  and most  likely a lower,  value than the one the EPA is currently using.
  This survey has the  support of ATMI and also the Dyescuff Manufacturers.
  The corferuflsTons drawn  from the current  survey will affect all members of
  the textile and dye  industry.

        We  look forward  to your  completed questionnaire.   Please feel free
  to call Maggie Dean  of ATMI at (202) 862-0&30  if you have any questions.

                                                  Sincerely,
                                                  Carlos  Moore
                                                  Executive Vice President
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                          AMERICAN TEXTILE MANUFACTURERS INSTITUTE, INC.

                          1101 CONNECTICUT AVENUE. N.W., SUITE 300. WASHINGTON. D.C 20036
                                                                TWX: 710-822-9489
                                                                 TEL: 202/862-0500
This letter is  in regard  to  a  contact you had recently with WESTAT relative to
a joint industry/EPA sponsored study of textile drug rooms.  We want you to
know ATMI is actively  supporting this effort and your participation in the
survey is very  important.  The answers you provide will help us move to the
second phase of  the study, which is to assess exposure levels to dyes in
weighing and mixing rooms of textile dyehouse and printing operations.  The
information is  intended to help EPA in evaluating applications for manufacture
of new dyes.  You perhaps are  aware that the Toxic Substances Control Act
requires the agency to assess  potential health risks before approving the
manufacture of  any new chemicals or chemical compounds.

EPA's current strategy for assessing dyes is based on exposure levels found in
the leather industry thereby resulting in fewer approvals of new dyes.
Ultimately, this study will  establish levels representative of dye in the air
of 30 textile drug rooms. We expect it to support our position that exposure
levels in the textile  industry are much lower than those assumed by EPA.

We urge you to  join in this  study and we look forward to receiving your
completed questionaire .  .If  you, have any questions, please feel free to call
Maggie Dean of  ATMI at (202) 862-.0580.
                                             Since
                                             Director /"Government
                                             Reglations/Regulatory
  o _
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                             AMERICAN TEXTILE MANUFACTURERS INSTITUTE, INC.

                             1101 CONNECTICUT AVEM'E. N.W.. SUITE 300. WASHINGTON. DC 20036
                                                                   TWX: 710-822-9489
                                                                   TEL: 202 862-0500
                                              May 23, 1986
 Thank you for participating in the first phase of the joint study with ATML,
 the Ecological and Toxicological Association of the Dyestuffs Manufacturing
 Industry (ETAD) and the U.S.  Environmental Protection Agency (EPA) to
 determine worker exposure to dye dust.   The second phase of this project
 involves the  measurement  of actual exposure levels in a representative group
 of U.S.  textile plants.   Your plant is one of thirty textile plants selected
 at random for the second  part of this important study.  The validity of the
 study depends upon achieving a high level of participation from the 30
 plants.  Vie encourage your participation for this reason.

 The next phase will be conducted on-site by a field team of two certified
 industrial hyglenists.  Total time on-site over a 2-day period will be about
 14-16 hours.   Every effort will be made  to minimize any inconvenience to your
 plant from the visit.  In fact,  the validity of the study can only be
 maintained by avoiding disruption  of workplace activities.  An individual site
 report will be prepared and you will receive a copy following completion of
 the study.  The overall survey results will be presented in a 30-site
 composite  report,  individual  plants will not be identified in this final
 report.

More details of the study are provided in the attached statement on objectives
and protocol.
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There will be  some direct benefits  to participants  in this study, they include:

         1.  A confidential report  which characterizes  industrial hygiene
             practices at the plant and  measures dye  concentration levels in
             the drug room.

         2.  An opportunity for participating companies to compare their
             results with those of  other participating plants.

         3.  The current EPA approach, which is based on worst case
             assumptions, is excluding from the U S.  market many new dyes
             which are available to U S. competitors  abroad.  A direct
             objective of this study  is  to secure a more realistic assessment
             of potential risks.

         4.  A final report which characterizes the industry based on
             consolidation of results from the questionaire and monitoring
             study of all participants.  This report will not identify
             specific sites.

Within the next few days Ms. Maggie Dean, ATMI's Director of Safety, Health
and Environment, will phone you to  discuss arrangements and possible dates for
the two-day on-site visit by the field study team.  Currently, we plan to
begin site visits the week of June  16.   Shortly after, Dr. William Dyson will
phone you to schedule the on-site visit  and answer any specific questions
about the monitoring procedure.  Your participation in this second and final
phase of the study is important and I personally encourage you to take part.
If you have any questions, please contact Maggie at (202) 862-0580.
                                             Sincerely ,
                                             Carlos Moore
                                             Executive Vice President
CM:jt
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                            AMERICAN TEXTILE  MANUFACTURERS INSTITUTE,  INC.

                            1101 CONNECTICUT AVENUE. N Vt.. SUITE 300. WASHINGTON. D.C 20036
                                                                  TWX: 710-822-948^
                                                                  TEL  202/862-0500
                                              January 15, 1987
Dear

A study  is  currently being sponsored jointly with ATMI, the Ecological and
Toxicological Association of the Dyestuffs Manufacturing Industry (ETAD) and
the U.S. Environmental  Protection Agency (EPA)  to determine worker exposure to
dye dust.   Phase  I  surveyed 200 textile dyeing  or printing sites to obtain a
broad picture on  the use  of dyestuffs for textiles and the potential for
worker exposure.  The study will not be used to develop regulations.  The
objective is to provide a more realistic assessment of textile workers
exposure to powdered dyes which we hope will help dye manufacturers pass
premanufacturing  notification requirements for  new dyes.   Strict
confidentiality of  plant  identification will be kept by ATMI and not be
available to EPA.

The next phase will be  conducted on-site by  a field team of two certified
industrial  hygienists and an EPA representative.   Total time on-site over a
2-day period will be about 14-16 hours.   Every  effort will be made to minimize
any inconvenience to your plant from the visit.  In fact, the validity of the
study can only be maintained by avoiding disruption of workplace activities.
An individual site  report will be prepared and  you will receive a copy
following completion of the study.   The overall survey results will be
presented in a 30-site  composite report; individual plants will not be
identified  in this  final  report.

More details of the study are provided in the attached statement on objectives
and protocol.
   O i&m  rs                           C-9

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There will be some direct benefits to participants in this study; they include:

         1.  A confidential report which characterizes industrial hygiene
             practices at the plant and neasures dye concentration levels in
             the drug room.

         2.  An opportunity for participating companies to compare their
             results with those of other participating plants.

         3.  The current EPA approach, which is based on worst case
             assumptions, is excluding from the U S. market many new dyes
             which are available to U S. competitors abroad.  A direct
             objective of this study is to secure a more realistic assessment
             of potential risks.

         4.  A final report which characterizes the industry based on
             consolidation of results from the questionaire and monitoring
             study of all participants.  This report will not identify
             specific sites.

Your participation in this second and final phase of the study is very
important to the project's success and we personally encourage you to take
part.  We plan to conduct site visits during the next few months and will
phone you next week to secure your agreement and answer any questions about
the study and monitoring procedures.
                                             Sincerely,
                                             Maggie Dean
                                             Director
                                             Safety Health and Environment
                                             ATMI
                                             Eric Clarke
                                             Executive Secretary
                                             Ecological and Toxicological
                                               Association of the Dyestuffs
                                               Manufacturing Industry
                                      C-10

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                   TEXTILE DRUG ROOM MONITORING STUDY (TDRMS)
                            OBJECTIVES AND MECHANISM
About 1000 domestic textile dyeing or printing sites have been Identified
where there Is potential for workers to be exposed to numerous powder dyes via
Inhalation or dermal routes.  There are reasonable Indications that some dyes
(both new submissions and existing) or their metabolites might be carcinogens
or mutagens.  Data which document potential  exposure levels of workers
associated with the weighing or mixing of powder dyes are limited, some being
derived from other than the textile Industry.  Our objective 1s to conduct a
well-designed study of textile dye weighing rooms In order to Improve the
assessment of exposure (and associated risk) with the use of powder dyes In
the American textile industry.  This study is being sponsored jointly by the
American Textile Manufacturers Institute (ATMI), the Ecological and
Toxicological Association of the Dyestuffs Manufacturing Industry (ETAO) and
the Office of Toxic Substances (OTS) of EPA.

The mechanism of accomplishment will consist of monitoring one randomly
selected dye weigher in each of 30 randomly selected sites which use solid
dyestuffs in the dyeing or printing of textile fibers.  The on-site field team
will consist of two certified industrial hygienists.  One will be an employee
of Health and Hygiene, Inc. (H+H) of Greensboro, NC.  The other will be an
employee of PEI Associates, Inc. (PEI) of Cincinnati, OH.
                                   c-n

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On site observers will record the identity of each solid substance weighed by
the person being monitored, the number of weighings of each, the total mass of
each substance weighed and the duration of time that the worker is within the
weighing area.  They will characterize each work area in respect to number-of
dyeing/printing units in operation, materials flow, cleanliness and
ventilation including engineering controls.  They will also characterize each
person being monitored relative to work habits, work history and protection
equipment utilized including clothing and personal protective controls.

Over an 8 hour period, solids will be collected from the air in the breathing
zone of each selected worker.  At a later time, collection filters will be
analyzed for total dust and for total dye.  Observers will also collect
analytical standardization controls consisting of samples of each dye and
other materials which may interfere with the analysis.

The field team is expected to be at each site for a period no greater than 2
consecutive days.  Projected activities and duration will be as follows:

     Sequence                Activities                Duration

Pre-Monitoring          Gain site familiarity          2-4 hrs
                        Characterize site

Monitoring              Monitor worker                 8 hrs
                        Record Dyes/chemicals
                        weighed
                        Characterized worker
                                    C-12

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Post-monitoring         Collect samples                2-4 hrs
                        Review and completion
                        of data/sample collection
                        Review with plant offical

Observers will preserve the confidentiality of operations and formulations of
the sites visited.  As a courtesy and to ensure validity, they will
conscientiously refrain from any interference in workers' performance of
duties.  Within one month of the monitoring date, observers will issue a joint
report which characterizes each site and the monitored individual.
                                   C-13

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                                            June 12, 1987
Dear          :

The American Textile Manufacturers Institute, Inc., the Ecological and
Toxicological Association of the Dyestuffs Manufacturing Industry and the
Office of Toxic Substances of the U.S. Environmental Protection Agency, thank
you for participating in the joint industry-government textile drug room
monitoring study.

The monitoring phase of the survey of dustiness in textile drug rooms of 24
randomly selected volunteer plant sites was completed in May 1987.  Reports
are now being prepared characterizing, but not identifying, each site which
participated.  A copy of the report on your facility will be
within the next two months.  In addition, at a later date, you will recieve a
copy of the final report which summarizes data gathered from all participating
sites without identifying any individual participants.

We believe this study will provide new insights on worker exposure to dyes in
textile drug rooms.  Again, we greatly appreciate the time and assistance you
provided.  The study could not have been done without your cooperation and
that of the other volunteer participants.

                                            Very truly yours,
                                            Maggie Dean
                                            Director
                                            Safety, Health and Environment
                                            ATMI
MMD/sgt                                     Eric Clarke
                                            Executive Secretary
                                            Ecological and Toxicological
                        .725.029/              Association of the Dyestuffs
                                            Manufacturing Industry

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     SUPPLEMENTAL D



FIRST PHASE QUESTIONNAIRE
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                 PLEASE GIVE  THE ACTUAL PHYSICAL LOCATION OF THE FACILITY
                 RATHER THAN  THE HAILING ADDRESS (IF DIFFERENT FROM LABEL).
Street Address:
City:
State:


STREET OR P.O. BOX
Zip Code: I I I I I I

                PLEASE RECORD THE NAME AND ADDRESS OF THE PARENT COMPANY
                (CORPORATE HEADQUARTERS) OF THIS FACILITY.  IF THIS FACILITY
                HAS NO PARENT COMPANY, PLEASE WRITE 'NOT APPLICABLE' IN THE
                SPACE PROVIDED FOR PARENT COMPANY NAME.
Parent Company Name:
Address:
STREET
1
1 1 1 1 1
CITY STATE
                   PLEASE RECORD THE NAME, TITLE AND PHONE NUMBER OF THE
                   PERSON MHO MAY BE CONTACTED FOR FURTHER INFORMATION.
Name of Contact:

Title: 	
Phone Number: (   )
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                                  GENERAL INSTRUCTIONS


All information requested concerns solid (powder or granular) dyes only.  Exclude information
for operations using only pigments or liquid dyes.

Located in the upper right corner of each page of the questionnaire is a box in which you may
indicate the presence of confidential business information (CBI) on that page.  Pieace circle
Y (yes) or N (no) to indicate the presence or absence of proprietsry information on each page.

Most questions will have specific instructions to assist you in their completion.  If you have
a situation not covered by the instructions, please don't hesitate to call the number in the
box below for aaaistance.

An identification number will be assigned by ATMI as a reference in order to protect the
identity of each participant.  This number .will appear in the top right corner of each page.
            PLEASE COMPLETE THIS QUESTIONNAIRE AS SOON AS POSSIBLE.  AS SOON
            AS IT HAS BEEN COMPLETED, RETURN IT TO	IN THE ENCLOSED,
            POSTAGE-PAID ENVELOPE.  IF YOU HAVE ANY QUESTIONS ABOUT HOW TO
            COMPLETE THE QUESTIONNAIRE, PLEASE CALL	AT
        PLEASE RECORD  THE FOLLOWING  INFORMATION ONLY  IF DIFFERENT FROM LABEL ABOVE.
Name of Dyeing or Printing Facility:
Mailing Address:
STREET OR P.O. BOX

CITY STATE



J 1 1 1 1 1
ZIP
                                       NOVEMBER  1985
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                                                                           CBI:   Y   N
1.   What are the total number of sites within the  entire corporation where dyeing or printing
     operations are performed?  (PLEASE COUNT  EACH  SEPARATE  DYE  HOUSE OR PRINT SHOP.)

                                                t OF  SITES:
2.   Is thia particular  facility publicly or  privately owned?   (MARK AN 'X1  IN THE APPROPRIATE
     BOX.)


                        PUBLIC  |	|             PRIVATE |	|



3.   Does.this facility  operate  on  a vertical  (integrated) or coanuasion  basis?  (MARK AN 'X1  IN
     THE  APPROPRIATE  BOX.)


                        VERTICAL  |	|           COMMISSION |	|
                                             D-5

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CBI:
Y N
                                 PRODUCT LINES DYED OR PRINTED

4.   In the table below, please specify the following information:
COLUMN 1:
COLUMN 2:
COLUMN 3:
                IN THIS COLUMN PLEASE HARK AN 'X1  IN THE BOX CORRESPONDING TO EACH PRODUCT EITHER
                DYED OR PRINTED AT THIS FACILITY.   PRODUCT LINES WHICH DO NOT FIT ANY OF THE
                INDICATED CATEGORIES SHOULD BE ENTERED ON THE OTHER (SPECIFY) LINES.

                IN THIS COLUMN, INDICATE ON THE APPROPRIATE LINE THE AMOUNT X EACH PRODUCT WHICH
                IS SUBJECTED TO A DYING OPERATION USING POWDER DYES.  THIS SHOULD BE POUNDS OF
                GOODS PROCESSED.  IF IT IS INCONVENIENT FOR YOU TO SPECIFY THE NUMBERTTTBUNDS
                PLEASE MARK AN 'X' IN THIS BOX I   I AND RECORD YOUR ANSWER IN PERCENT OF TOTAL
                PRODUCTION.  THE TOTAL FIGURE AT~THE BOTTOM OF THE COLUMN SHOULD BE GIVEN  IN
                POUNDS OF FIBER DYED (WITH POWDER DYES) PER YEAR.

                IN THIS COLUMN, INDICATE ON THE APPROPRIATE LINE THE AMOUNT OF EACH PRODUCT WHICH
                IS PRINTED WITH POWDER DYES.  THIS SHOULD BE AS POUNDS OF GOODS PROCESSED.  IF IT
                IS INCONVENIENT FOR YOU TO SPECIFY THE NUMBER OF POUNDS PLEASE MARK AN  'X1 IN
                THIS BO* | ~TA"ND RECORD YOUR ANSWER IN PERCENT OF TOTAL PRODUCTION.  THE  TOTAL
                FIGURE AT THE BOTTOM OF THE COLUMN SHOULD BE GIVEN IN POUNDS OF FIBER PRINTED
                (WITH POWDER DYES) PER YEAR.  IF ANY GOODS ARE BOTH DYED AND PRINTED AT THIS
                SITE, LIST THE QUANTITIES IN BOTH COLUMN 2 (DYt) AND COLUMN 3 (PRINT) BRACKETED
                BY PARENTHESES.
                     PRODUCT LINE
                                                 COLUMN 1

                                                 PRODUCT
                                                 DYED OR
                                                 PRINTED
  COLUMN 2


AMOUNT DYED
  PER YEAR
 IN POUNDS
COLUMN 3

 MOUNT
 PRINTED
PER YEAR
IN POUNDS
     a.  Staple
     b.  Yarn/thread
     c.  General apparel - woven
     d.  General apparel • knitted
     e.  Carpet/rug (include automotive)
     f.  Other home furnishings
     g.  Other transportation fabrics
     h.  Other pile fabrics
     i.  Outerwar/cloaking fabrics
     j.  Towels/terry cloth
     k.  Sheets/linens
     1.  Linings/woven continuous filament
     •.  Narrow fabrics
     n.  Light wight fabrics
     o.  Hoaiery/intiMte war
     p.  Fabricated goods (as sweaters, socks, etc.)
     q.  Other woven fabrics (SPECIFY)
     r.  Other knitted fabrics (SPECIFY)
     a.  Other substrataa (SPECIFY)
                                                  I—I
                                                  LJ
                                                       LJ
                                                       LJ
                   Total pounds per year
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                                                                           CBI:
5.   Which of the following fibers are dyed or printed at this facility?  (MARK AN 'X' IN THE BOX
     FOR EACH FIBER USED.  IF FIBERS OTHER THAN THOSE LISTED ARE USED, PLEASE SPECIFY IN THE
     SPACE PROVIDED.)
               Acrylic/Modacrylic. . . |   |

               Rayon	|	|

               Cotton	|	|

               Nylon	|_J

               Polyester	|   |
Acetate	|__|

*>ol	|__|

Other (SPECIFY)

  	- - LJ

  	- - U
6.   Which of the color index classes of powder (solid) dyes are used at this facility?  (MARK
     AN 'X' IN THE BOX FOR EACH DYE CLASS USED.  IF DYE CLASSES OTHER THAN THOSE LISTED ARE USED,
     PLEASE SPECIFY IN THE SPACE PROVIDED.)
         Acid (include metallized). . . |	|

         Basic/Cat ionic	|	|

         Reactive	|	|

         Direct	|_J

         Disperse	|	|

         Naphthol/Azoic	|	|
 Chrome/Mordant

 Sulfur
 Vat

 Other (SPECIFY)
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                                                                           CB1:
7.   How many units of the following types of dyeing or printing equipment are used it this
     facility on • regular basis?  (RECORD THE NUMBER OF PRODUCTION SIZE UNITS OF EQUIPMENT USED
     AT THIS FACILITY IN THE BOX PROVIDED.  IF EQUIPMENT OTHER THAN THAT LISTED IS USED, PLEASE
     SPECIFY IN THE SPACE PROVIDED.)
               Beck. .

               Beam. .

               Jet  . .

               Jigg. .

               Package

               Paddle.
                                           A.  Batch
Rotary	

Stock/Top . . .

Skein .....

Other (SPECIFY)
                                 B.   Continuous/Semi-Continuous
               Pad  .

               Flood

               J-Box

               Spray
Narp Dye. . . .

Other (SPECIFY)
                  • I.
                                            C.   Print
               Flat  Bed  Screen:
                  Hand	
                  Machine  .  .  .

                  Rotary Screen

                  Roller.  .  .  .
Space Dye

Polychromatic  .  .  .  |_

Other (SPECIFY)
                                      D-8

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                                                                           CBI:   Y   N

                                                                           "»:  LJ_U_U
                           FREQUENCY AND VOLUME OF POWDER DYE HANDLING
8.    In the table below, please specify the following information:

     COLUMN 1:  IN THIS COLUMN, PLEASE RECORD YOUR BEST ESTIMATE OF QUANTITIES SPECIFIED FOR.A
                TYPICAL DAY/WEEK BASED ON PRODUCTION FIGURES OVER THE PAST YEAR.

     COLUMN 2:  IN THIS COLUMN, PLEASE RECORD YOUR BEST ESTIMATE OF BOTH THE LOW AND HIGH LEVELS
                OF QUANTITIES SPECIFIED BASED ON PRODUCTION OVER THE PAST 12 MONTHS.  DO NOT
                INCLUDE EXTREMES WHICH ARE THE- RESULT OF ABNORMAL CONDITIONS SUCH AS ZERO PRODUC-
                TION DURING A CHRISTMAS WEEK CLOSING, OR EXCESSIVELY HIGH PRODUCTION RESULTING
                FROM A "CATCH-UP WEEK" FOLLOWING AN EXTENDED POWER OUTAGE.
                                                         Column 1
                                                         Typical
    Column 2
Low/High for Yaar
a.  Number of individual powder dyes weighed per
    24 hour day; (INCLUDE EACH DYE ONLY ONCE
    REGARDLESS OF THE NUMBER OF TIMES IT IS USED)

b.  Number of pounds of powder dyes weighed per
    24 hour day;

c.  Number of weighings of powder dyes per 24 hour
    day; (COUNT EACH DYE WITHIN A FORMULA SEPAR-
    ATELY.  INCLUDE BOTH STARTING FORMULAS AND
    COLOR ADDS OR FEEDS);

d.  Number of dye weighing rooms or areas at this
    facility;

a.  Number of shifts operating per typical
    day/24 hours;

f.  Number of days of operation per typical week;

g.  Number of enployees who weigh, aix, handle
    or are otHerwise exposed to powder dyes on a
    typical day.
                                               D-9

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                                                                          CBI:
                      DRUG  ROOM EXPOSURE CONTROLS WHEN WEIGHING POWDER DYE
9.   In the table below,  please  apecify the  following information:

     COLUMN 1:   IN THIS COLUMN,  PLEASE MARK  AN  'X1 IN THE BOX FOR EACH CONTROL IF IT IS AVAILABLE
                BUT ITS USE  IS NOT  REQUIRED.

     COLUMN 2:   IN THIS COLUMN,  PLEASE MARK  AN  'X1 FOR EACH CONTROL IF ITS USE IS MANDATORY
                EITHER  BY COMPANY DECREE  OR  REGULATION.

     GENERAL:  "*NY CONTROL  NOT  MARKED IN EITHER COLUMN WILL BE ASSUMED TO NOT BE IN USE AT THIS
                FACILITY. IF CONTROLS OTHER THAN  THOSE LISTED ARE USED, PLEASE SPECIFY IN THE
                SPACE PROVIDED.
                                                        Column  1
                                                        Available
                                                       Not Required
  Column 2

Mandatory Use
       a.  General ventilation

       b.  Local exhaust or hood

       c.  Dust mask

       d.  Respirator

       e.  Long sleeve clothing

       f.  Impervious gloves

       g.  Goggles

           Other (SPECIFY)

       h.           	
       i.
    L-\
    LJ
                                    D-10

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   SUPPLEMENTAL E



IN-PLANT QUESTIONNAIRE
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                                                  Plant I.D. (2 digits)	/_
                                                  Recorder:      	
                     JOINT DYE/DRUG ROOMS MONITORING SURVEY
                   OF TEXTILE DYEING &  PRINTING INDUSTRIES BY

     ATMI     -     American Textile Manufacturers Institute
     ETAD     -     Ecological & Toxicological Association of the Dyestuffs
                   Manufacturing Industry
     US EPA   -     United States Environmental Protection Agency
Name of Dyeing  or  Printing  Facility:

Street Address:  	

City:  	
       State:
                  Zip Code:  //////
Name of Contact:

Title:
                    Phone Number:  (    )
SELECTION OF WORK  SHIFT

Identify the number of shifts  where powder dyes are weighed.   Circle number in
Column A.  Based on the above  phone number, circle the appropriate digits in
Column B.  Circle  the observed shift  in Column C.
A
No. of shifts where
powder dye weighed
1
2
3
B
Middle 3 digits of 7-digit
telephone number
000-999
000-499
500-999
000-333
334-666
667-999
C
Shift to be observed
1st
1st
2nd
1st
2nd
  Record Times of Shift:
From
:	 a.m./p.m.
To
a.m./p.m.
SELECTION OF WEIGHER IN OBSERVED  SHIFT TO BE ASSIGNED MONITOR
To select the weigher to be monitored from the chosen shift,  collect the last 3
digits of social security numbers  (SSN) for all weighers from all drug room(s)
operating during observed shift.   List:
Select the weigher with the  last  three SSN digits closest to 500.
Recorder the Weigher's Name:
                        SSN:

                       I.D.  f
                                                          Date:
                                      E-3
                                                                  mo. date year

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                                                  Plant I.D. (2 digits)
                                                  Recorder:
SAMPLING AREA  INFORMATION

SKETCH LAYOUT  OF  DRUG ROOM/AREA FOR WEIGHING POWER DYES.

Include:  walls,  windows, entrances,  exits, tables, storage containers, air
intake points,  vents, fans.   Mark  stations  (table/scales) where weighing occurs
(*W).  Note approximate dimensions of room/area.  Indicate at margins location
within facility and  give locational name  (e.g., "east wing").  Give North/South
orientation.   Define with arrow and dotted  lines the flow of dyes from storage
through mixing.
TEMPERATURE AND HUMIDITY

Record the temperature and humidity at the beginning, middle, and end of the
shift/ and at times when the room conditions change noticeably.
Temperature
Humidity
Time Recorded


*
*


•
•


•
•


•
•


•
•


•
•


•
•
                                       E-4

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                                                  Plant I.D.  (2 digits)
                                                  Recorder:       	
WEIGHER WORKER  INTERVIEW

To be asked  of  weigher  (Name) _ selected on first page.

I'd like  to  ask some  questions  about  you and your work history handling powder
dyes.
1.  When were  you  born?
                                                       month    day     year

2.  How many years  have you worked at  this site?                _ years

3.  How many years  have you handled  (weighed and/or mixed)
    powder dyes at  this site?                                   _ years

4.  In your lifetime work experience,  indicate how long you have
    worked in any industry handling  (weighing and/or mixing)
    powder dyes?                                                _ years

5.  What information have you  received in the safe handling of dyes, such as
    training, courses, and literature?
OBSERVATION OF WEIGHER PRACTICES  (Part I)

                                                If yes, describe
1.  Did monitored weigher
    wear dust mask or        No {_	{_ Yes {_	f_ 	
    respirator?                               	
2.  Did monitored weigher
    smoke in weigh area?     No {_	£_ Yes [_	{_ 	
3.  Did monitored weigher
    eat in weigh area?       No /_	{_ Yes f_	{_ 	


QUESTIONS FOR WEIGHER'S SUPERVISOR

1.  What is the total number of dyeing or printing machines being serviced today
    by the monitored weigher:
Equipment
A. Printing
B. Semi-continuous/Continuous
C. Batch dyeing
Number at
Start of Shift



Number at
End of Shift



2.  What is the total number of weighers at your plant on a typical day?

     a. first shift  	

     b. second shift 	

     c. third shift  	          E~5

     d. Total

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                                                  Plant  I.D.  (2 digits)	/
                                                  Recorder:
DETAILED WORKER/SAMPLING AREA OBSERVATIONS

Actual Time Periods Monitored:  From  	:	 a.m./p.m.   To 	:	 a.m./p.m.

Job Category:
Specific Duties:
A.  Clothing & Personal Protective Equipment Utilized:
B.  Worker Practices:  Note equipment used and dermal  contact;
    Drum Relocation:

    Weigh:  	
    Mix:


    Strain:
    Transport:
C.  General  Cleanliness:
     Walls:
     Equipment:
     Inventory:
     Floors: 	
     Spills:  _
D.  Engineering  Controls:
     Ventilation:
     Drainage: 	
E.  Building:
     Ventilation:
                                      E-6

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                                                  Plant  I.D.  (2 digits)	/_
                                                  Recorder:      	
TIME IN/OUT OF THE DRUG ROOM
Weigher I.D. #_
ENTER
HR. MIN.






















EXIT
HR. MIN.






















TOTAL
TIME
HR. MIN.























ENTER
HR. MIN.






















EXIT
HR. MIN.






















TOTAL
TIME
HR. MIN.






















                                                        GRAND TOTAL
                                                        FOR PAGE
                                                            Page
                 of
                                      E-7

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                                                   Plant I.D.  (2  digits)
                                                   Recorder:
MASS OF EACH  WEIGHING OF POWDERED DYE OR CHEMICAL
DYE OR CHEMICAL WEIGHED
BATCH TICKET NAME
























MASS OF WEIGHINGS (SPECIFIC UNITS)
123
( ) ( )














































( ) ( )
1












































( ) I )
1
1
1
1


1
























1








Complete this  information if this  is  a  continuation sheet page 	 of 	 pages,
                                      E-8

-------
                                                  Plant I.D.  (2 digits)
                                                  Recorder:        	

Bulk
Sample I.D.

























INVENTORY OP POWDERED DYES (D) AND CHEMICALS (C) WEIGHED
Batch Ticket
Name

























FULL TRADE NAME

























D/C

























Lot No.

























Supplier

























Complete this information if this is a continuation sheet page 	 of 	 pages,
                                       E-9

-------
 PERSONAL MR SAMPLING DATA SHEET
• Company:
i  Plant  in  No.
         i Dnte {Mo/Da/Yr)
I
Worker  Monitored:
1  Worker  ID No.
         : ss NO.
'Job  Title/Work Duties:
Sampling  Performed  by:
                             SAMPLING EQUIPMENT AND  CALIBRATION
 ?lowm«ter  Model  Number:

 j_	
 Flowmeter  Serial Number:


 iFlowmeter  Calibration  Dal'?:
 Calibration  Traceable To:
j« =«..«:=»«==>*:===. ==«==«,== = = -=
PERSONAL
Model No. :
1
Serial No:
jFlowrate:
Time:
Date:
PUMP *1





Signature(s ) :








PUMP *2






FIELD SAMPLING DATA
Sample ID Number:
Sampler Location:
Sample Start Time:
•Sample Stop Time:
[Sample Dura t- on: (MIN)
jPump Flow Rate: (L/MIN)
•Sample Air Volume: (n3)
PUMP
*l






PUMP
*2






{Signature:
 Date:
Calc. Checked By:
                                          E-10

-------
  STATIONARY AREA AIR SAi'TMSG DATA SHEET




• Company:
                                                  Plant  ID No:
          Date  fMo/Oa.'vr)
 Sampling  Performed  v>y:
j Flowmeter Model Number:
                               SAMPLING  EQUIPMENT AND CALIBRATION
! Flowmeter Serial  Number:
 Flowmeter Calibration Dat»:
 Calibration Traceable  to:

L	
j Sampling Pump Serial Numbrr
j Sampling Pump Model Numb"1




j Pre-sampling Flowrate:
i   Date:
   Time:

; Post-sampling Flowrnte:
   Date:
   Time:
i Signature(s):

                                    FIELD SAMPLING DATA
 Sample ID Number:
              Field Blnnk
 Sampler Location:
; Sample Start Time:
i Sample Stop Time:
j Sample Duration: (win)
I Pump Flow Rate: (L/min)
• Sample Air Volume: (m3)
' Signature:
Date:
 Calculations Checked by:
Date:
                                           E-ll

-------
ANALYTICAL DATA
                                   GRAVIMETRIC ANALYSIS
                                                                               f-  Blank
Sample ID Number:
Filter Preweight:
Filter Postweight:
Sample Weight:
Blank Correction:
Adjusted Weight:
Signature!s):
Date:
Calculations Checked  by:
                             VIS I OLE SrrCTROPHOTOMETRIC ANALYSIS
                                                     T
Filter Extraction Dnte:
Data File Number:
Sample Prepared by: (
Total Absorbance:
Corrected Total Absorbanc":
Absorptivity: (As)
Dye Estimate: (ug)
Average Filter Spike Recovery: (^)
Corrected Dye Estimate: (nr.) '•
i
Estimate. Airborne Dyes: (ug/m3) :
Data Reference Number: i
LSignature(s) :



r
i
i
i
i
Calculations Checked by:
===,'„,=,,„,««,.„=„„,=„„===„„====,=
                                         E-12

-------
                      (S#» Bock of fog* for Explanation of

                    CHAIN OF CUSTODY OR TTUCEAHUTY R£CO*D
Q Chain of Cutfody beard
Project Nmnh*f
Location
Container No.
                                     1 Loo
                          Oat* of Field Sampling .
                          Tyo* of SamaJa      -
                          Storaga
 Sampl* No.
Dwcripflon
Ch*ck
                                               Oaf*
S*al Inraer
Oar*
G*ck»dby
(InlHali)
Oar*
Tim*
R«c«iv*d by

























































                                E-13

-------
                 FILLING OUT CHAIN OF CUSTODY/TRACEABILITY LOG


 1.      Check chain of custody  form.

 2.      Traceability log.

 3.      Enter project and  task  number.

 4.      Enter dates the first and last samples were collected that are recorded
        on each log sheet.

 5.      Enter sampling location:  plant name and/or city.

 6.      Enter type of sample, i.e., Tenax trap, condensate, bulk feed, etc.
        Record only one type of sample on a form.

 7.      Enter shipping container number in which samples are packed.  Each
        shipping container must contain only one type of sample.

 8.      Enter storage requirements, i.e., wet ice, dry ice, in plastic bags,
        etc.

 9.      Enter entire sample number.

10.      Enter any other sample  description required.

11.      Enter other sample identification, i.e., Tenax tube numbers.

12.      Enter name or initials  of person collecting sample.

13.      Four columns are provided for inventory checkoff each time sample
        custody is transferred. As the samples are inventoried, place a
        checkmark in the appropriate box.  If samples are liquid, the liquid
        level should be confirmed at the same time.  Changes in the level should
        be noted and dated under the comments Column 14.  When the inventory is
        completed, enter the data in 15 directly under the column checked off.

        Sixteen through 18 are  provided for samples collected under Chain of
        Custody.  Each shipping containers with samples must be sealed with
        evidence tape when not  in the custodian's presence.  The seal.is not to
        be broken by any other  person.  Evidence tape must be placed over the
        joint between the  container and container lid; the tape is signed and
        dated by the custodian. Each container with samples must be inspected
        at the beginning of each day.  Check off that the seal is intact in 16,
        record the inspection date in 17, and initial in 18.  After seal
        inspection, the seal may be broken to add additional samples or ice.
        The container may  remain unsealed while in the presence of the
        custodian.

        Columns 19 through 22 must be used to record a change in sample
        custodian following either Chain of Custody or Traceability.  Each time
        the custodian is changed, the samples must be inventoried using Column
        13 and the transfer recorded using 19 through 22.  Samples never change
        custody without being inventoried and signed off.  The Chain of Custody
        Record or Traceability  Log must travel with the samples until
        transferred to the laboratory custodian.  After transfer, provide the
        laboratory custodian with copies of the forms and give the originals to
        the crew chief.

                                    E-14

-------