united States
           Environmental Protection
           Agency
 Office of Air Quality
 Planning and Standards
 Research Triangle Park NC 27711
March 1991
           Air
dEPA     Determination of Perchloroethylene

           Content of Waste Materials from

           Filters and Still Bottoms
          Conditional Test Method
           control
technology center

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                              EPA REVIEW NOTICE

     This report has been reviewed by the U.S. Environmental Protection
Agency and approved for publication.  Approval does not signify that the
contents necessarily reflect the views and policy of the Agency, nor does
mention of trade names or commercial products constitute endorsement or
recommendations for use.

     This document is available to the public through the National Technical
Information Service,  Springfield,  Virginia  22161.

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                                                 March  1991
              DETERMINATION  OF
CONTENT  OF  WASTE  MATE RIALS   FROM

      FILTERS  AND  STILL  BOTTOMS



        CONDITIONAL  TEST  METHOD
                              by

                     \; John D. Jeffrey
              Alliance Technologies Corporation
                      213 Burlington Road
                 Bedford,  Massachusetts 01730

                       Contract Number
                          68-02-4465
                       Project Officers

                       ^Robert Judge
              Air Management Division, Region I
             U.S. Environmental Protection Agency
               John F. Kennedy Federal Building
                 Boston, Massachusetts 02203

                             and
                                       j
                      Anthony  P. Wayne
                  Technical Support Division
         Office of Air Quality Planning and Standards
             U.S. Environmental Protection Agency
         Research Triangle Park, North Carolina 27711
                         Prepared for

                  Control Technology Center
             U.S.  Environmental Protection Agency
         Research Triangle Park, North Carolina 27711

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                          PREFACE
    The  "Determination of Perchloroethylene Content of Waste
Materials from Filters and Still Bottoms - Conditional Test
Method" was funded as a cooperative project by the Control
Technology Center (CTC) and the Air Management Division, EPA
Region I.  The project was implemented by Region I and the EPA's
Emission Measurement Branch, Technical Support Division, Office
of Air Quality Planning and Standards (OAQPS).

    The  CTC was established by EPA's Office of Research and
Development (ORD) and OAQPS to provide technical assistance to
State and local air pollution control agencies and EPA regional
offices.  Three levels of assistance can be accessed through the
CTC.  First, a CTC HOTLINE has been established to provide
telephone assistance on matters relating to air pollution control
technology.  Second, more in-depth engineering assistance can be
provided when appropriate.  Third, the CTC can provide technical
guidance through publication of technical guidance documents,
development of personal computer software, and presentation of
workshops on control technology matters.

    The  technical guidance projects, such as  this one,  focus on
topics of national or regional interest that are identified
through contact with State and local agencies or regional
offices.  In this case, the CTC joined EPA Region I to develop
this conditional test method as part of Region I's 1990 Rule
Effectiveness Study.  The Test Support Section, Emission
Measurement Branch, OAQPS, was responsible for project oversight.
The Emission Measurement Branch supports and  is an integral part
of the Emission Measurement Technical Information Center  (EMTIC).
The purpose of this project was to evaluate a test method for
determining the perchloroethylene content of wastes from dry
cleaning facilities.  The result is a conditional test method
that is now available for use by State an local agencies  in their
development of ozone non-attainment State Implementation Plans.

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               EMISSION MEASUREMENT TECHNICAL  INFORMATION CENTER
                            CONDITIONAL TEST METHOD
                 DETERMINATION OF  PERCHLOROETHYLENE CONTENT OF
              WET WASTE MATERIALS FROM FILTERS AND STILL BOTTOMS
1.0  APPLICABILITY AND PRINCIPLE

1.1  Applicability.  This method is applicable to the sampling and
determination of perch!oroethylene in wet waste material  from diatomaceous
earth filters and solvent stills at perchloroethylene dry-cleaners on a weight
percent basis.

1.2  Principle.  Samples are obtained from waste material at a
perchloroethylene dry-cleaner.  A known sample mass is mixed with water and
placed in a glass still equipped with a Liebig straight-tube type reflux
condenser and a Bidwell-Sterling type graduated trap.  Water and
perchloroethylene in the sample are seperated through repeated distillation
until all of the perchloroethylene has been recovered in the trap and the
volume recorded.  The mass of perchloroethylene collected is determined from
the product of its volume and specific gravity.  The total weight of
perchloroethylene obtained is divided by the total weight of sample analyzed
to obtain the perchloroethylene content of the wet waste residue.


2.0  APPARATUS

2.1  Flask.  Round bottom, short-necked flask having a nominal capacity of
500 ml.  Figure 1 shows recommended designs of glass connections.

2.2  Condenser.  Liebig straight-tube type, with a jacket not less than 400 mm
long and with an inner tube having an outside diameter of 10 to  13 mm.  Figure
1 shows recommended designs of glass connections.

2.3  Trap.  Bidwell-Sterling type, graduated from 0 to 5 ml in 0.1-ml
divisions.  Calibrate at four or more points by first filling the trap with
water and then adding a hydrophobic solvent with a specific gravity greater
than water from a standard buret having a calibrated capacity at least equal
to that of the trap.  The error of the indicated volume  shall not exceed
0.05 ml.  Figure 2 shows characteristic details of a suitable trap.
Prepared by Tony Wayne, Emission Measurement Branch               EMTIC  CTM-010
Technical Support Division, OAQPS, EPA                            March  8,  1991

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EMTIC CTM-010           EMTIC CONDITIONAL TEST METHOD                    Page  2


2.4  Heater.  Any suitable gas burner or electric  heater for  the  glass  flask.

2.5  Sample container.  Metal can with a leak proof closure,  150  ml.


3.0  PROCEDURE

3.1  Sampling.

3.1.1  From distiller (cooker).  After a cycle of  the  perchloroethylene
distilling and the still bottoms have come to approximately room  temperature
(i.e., 21 to 38*C), obtain three 150 ml samples of the wet waste  residue from
the distiller (cooker) drain.  Completely fill each sample container  (three
total) to avoid evaporation loss.  Immediately close the sample container lid
securely.

3.1.2  From wet waste containers.

3.1.2.1  Large unmixed containers.  Using a clean  sampling spoon, spatula,  or
other appropriate device, obtain three 150 ml samples.  Each  sample shall  be
comprised of an approximately 50 ml sub-sample from the top,  bottom,  and mid-
point locations of the container.  Transfer the three  sub-samples to  each
sample container.  Completely fill the sample container to avoid  evaporation
loss.  Immediately close the sample container lid  securely .

3.1.2.2  Small containers.  If the waste container can be thoroughly  mixed
prior to sampling, mix the container contents thoroughly and obtain the sample
by pipetting.  The pipette should have at least a  150 ml capacity and should
be long enough to reach within 2 cm of the bottom  of the container.  Obtain
three 150 ml samples.  Transfer the sample to each sample container.
Completely fill the sample container to avoid evaporation loss.  Immediately
close the sample container lid securely.

3.1.3  Label the containers.  Use waterproof and oil-proof ink for labeling.

3.1.4  Storage.  Store the sample in a cool dry atmosphere.

3.1.5  Shipment.  Transfer the sample to the appropriate laboratory for
analysis within 48 hours of obtaining the sample.   The sample shall remain
sealed until the time of analysis.

3.2  Analysis.  Conduct duplicate analyses of each sample container and record
the recovered perchloroethylene from each analysis.

3.2.1  For each analysis, weigh and record the weight of an empty  flask and
stopper, W-, to the nearest 0.1 mg.  Mix each unopened sample container
by shaking.  Open the sample container and immediately transfer

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EMTIC CTH-010 _  EMTIC CONDITIONAL TEST METHOD _ Page  3


approximately 20 ml of wet waste material to the flask.   Stopper the flask  and
reseal the sample container.  Weigh and record the  weight of the flask plus
added portion, d., to the nearest 0.1 g.   The mass  added to the flask shall
not exceed 35 g.  Add water to the flask to make a  total  mixture volume of
approximately 250 ml.  Fill the trap with cold water.   Connect the flask to
the distillation trap.

3.2.2  Assemble the apparatus as shown in Figure 1  or  2 so that the tip of  the
condenser is directly over the indentation in the trap.

3.2.3  Heat the flask so that refluxing starts within  7 to 10 minutes.  Adjust
the rate of boiling so that the condensed distillate is discharged from the
condenser at a rate of 1 to 3 drops per second.

3.2.4  From the time refluxing starts, obtain readings of the amount of
perchloroethylene collected after 5, 15,  and 30 minutes, and each following
15 minutes.  End the test when the volume of perchloroethylene is increased  by
not more than 0.1 ml in a 15 minute period or the amount of perchloroethylene
exceeds the trap capacity.

3.2.6  At the end of the test run turn off the heater.  Allow the equipment to
stand at least 30 minutes to allow the distillate to settle clear and to cool
to room temperature.  Read the volume of perchloroethylene collected in the
trap.  If the amount of perchloroethylene exceeded  the calibrated capacity of
the trap, report the volume of perchloroethylene as 5.0 ml plus.


4.0  CALCULATIONS

4.1  Nomenclature.

            0  - Density of perchloroethylene at 20*C, 1.6227 g/ml .
            f^ * Weight of perchloroethylene in the portion, g.
            s- = Weight of the wet waste portion, g.
            V- « Volume of perchloroethylene collected in the trap, ml.
            w. » Weight of the empty flask and stopper, g.
            d.. * Weight of the flask plus portion,  g.

4.1  Calculate the total mass of the portion in the flask:
                                 si =

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EMTIC CTM-010
            EMTIC CONDITIOMAL TEST METHOD
Page 4
4.2  Calculate the total mass of perch!oroethylene,  f•,  collected in the trap
from each analysis:
                                  f,- = Vj x D
                                                             Eq.  2
4.3  The perch!oroethylene content of the wet waste (R), expressed in
kg per 100 kg wet waste material, is equal to the total  weight of the
perch!oroethylene obtained from the portions divided by the total weight of
the analyzed portions, multiplied by 100.
                                   100 x
                                          n

                                         E
                                         7=1
                                          n

                                         E
                                         7=1
                                                             Eq.  3
where:
n = the total number of analyses.
5.0  PRECISION AND ACCURACY

5.1  Accuracy.  Concentrations of audit samples obtained by the analyst shall
agree within 10 percent of the actual concentrations.  If the 10-percent
specification is not met, reanalyze the compliance samples and audit  samples,
and include initial and reanalysis values in the test report.

5.2  Precision.  Duplicate results produced by the same analyst should be
considered suspect if they differ by more than 5 percent.

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1TIC CTM-010
,EMTIC  CONDITIONAL TEST METHOD
Page  5
                 i*ot>rrvric»»  s-r mm
                 Zt-ti mm 0.8.
                                                                       100 WL.  FLASK
                                                                         xtoirr
                                                                       MOON* 10TTOM
                                                        .. ^	
                                                                                        	f  '

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      EMTIC CTM-010
 EMTIC CONDITIONAL TEST METHOD
Pace 6
£310 CONDENSER
                           LIE51G CONDENSES
                             UEEIG CONDENSER
                               BALL 1 SOCKET-
                               35/25
                               2-4/40
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                                         »re in mfllijnwm
             Fig. 1  Alternate Closures for Trap

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