EPA
         United States
         Environmental Protection
         Agency
          Office of Air Quality
          Planning and Standards
          Research Triangle Park NC 27711
EMB Report 86-CAD-2
November 1986
         Air
Cadmium
Screening
Study Test Report

Cadmium Sulfide
Pigments
Harshaw/Filtrol
Partnership
Louisville,
Kentucky

-------
                                                             MESHAP DEVELOPMENT
                                                CADMIUM MISSION TESTING AT THE
                                                    HARSHAW/FILTROL PARTNERSHIP
                                                           LOUISVILLE, KENTUCKY

                                                                      JULY 1986
EPA Contract No. 86-02-4337
ESED Project No. 80/42
Work Assignment No. 1
CAD-2 Louisville, KY
TRC Project No. 3497-E81-90

Prepared for:

Michael Toney, EPA/EMB
Task Manager
           Prepared By:


         John H. Powell
Work Assignment Manager

     Richard A. Pirolli
       Project Engineer

          November 1986

-------
                               TABLE OF CONTENTS

SECTION                                                                    PAGE

                  PREFACE	     vii

  1.0             INTRODUCTION  	       1
      1.1           Background	       1
      1.2           Summary of Process	       2
      1.3           Applicability of EPA Reference Test Methods ....       2
          1.3.1       EPA Method 5 Configuration Modified for Cadmium .       2
      1.4           Measurement Program Summary 	       3
          1.4.1       Spray Tower and Venturi 	       3
      1.5           Report Sections 	       4

  2.0             SUMMARY AND DISCUSSION OF RESULTS 	       5
      2.1           Spray Tower 	       5
          2.1.1       Cadmium Emissions 	       5
          2.1.2       Visible Emissions 	       5
          2.1.3       Stack Conditions  	       9
      2.2           Venturi Scrubber  	       9
          2.2.1       Cadmium Emissions 	       9
          2.2.2       Visible Emissions .	      15
          2.2.3       Stack Conditions  	      15
      2.3           Trace Metals	      15

  3.0             PROCESS AND OPERATIONS	      21
      3.1           Process Equipment 	      21
      3.2           Control Equipment 	      21

  4.0             SCOPE OF SAMPLING PROGRAM  	      22
      4.1           Belt Dryer	      22
      4.2           Rotary Calciner and Vacuum Pan Dryer  	      22
      4.3           Visible Emission Observations (Method 9)   	      26

  5.0             SAMPLING AND ANALYTICAL PROCEDURES   	      29
      5.1           EPA Method 5 Configuration Modified for Cadmium . .      29
      5.2           Sample Recovery	      31
      5.3           Sample Analyses	      33
      5.4           Visible Emissions Observation 	      34

  6.0             QUALITY ASSURANCE 	      36
                                      -111-

-------
                                   APPENDICES
A   EXAMPLE EQUATIONS AND CALCULATIONS
    A.I  Cadmium

B   FIELD DATA SP ETS
    B.I  EPA Method 5
      B.I.I  Spray Tower
      B.I.2  Venturi Scrubber

C   SAMPLING LOGS
    C.I  Daily Summary Log
    C.2  Sampling Task Logs
    C.3  Sample ID Log
    C.4  Chain of Custody Forms
    C.5  Crew Chief Field Operation Log
    C.6  Recovery Sample Sheet
    C.7  Train Operators Field Log

D   VISIBLE EMISSIONS
    D.I  Observer Certification
    D.2  Visible Emissions Field Data Sheets
      D.2.1  Spray Tower Visible Emissions
      D.2.2  Venturi Scrubber Visible Emissions

E   CALIBRATION DATA
    E.I  Summary of Equipment Used During Testing
    E.2  Orifices, Dry Gas Meter
    E.3  Pitot Tubes
    E.4  Nozzles

F   SAMPLING AND ANALYSIS PROCEDURES
    F.I  EPA Method 5 Modified for Cadmium
    F.2  EPA Method 9 (Visible Emissions)

G   LABORATORY ANALYSIS DATA
    G.I  Cadmium
    G.2  Trace Metals

H   PARTICULATE
                                      -iv-

-------
                                LIST OF FIGURES

FIGURE                                                                     PAGE

  2-1     Summary of Visible Emissions,  Spray Tower 103,  Harshaw/
            Filtrol Partnership 	      10

  2-2     Summary of Visible Emissions,  Spray Tower 103,  Harshaw/
            Filtrol Partnership 	      11

  2-3     Summary of Visible Emissions,  Spray Tower 103,  Harshaw/
            Filtrol Partnership 	      12

  2-4     Summary of Visible Emissions,  Venturi Scrubber  201,  Harshaw/
            Filtrol Partnership 	      17

  2-5     Summary of Visible Emissions,  Venturi Scrubber  201,  Harshaw/
            Filtrol Partnership 	      18

  2-6     Summary of Visible Emissions,  Venturi Scrubber  301,  Harshaw/
            Filtrol Partnership 	      19

  4-1     Belt Dryer Venturi Scrubber Outlet  	 	      23

  4-2     EPA Method 1, Sample and Velocity Traverse for  Stationary
            Sources	      24

  4-3     Calciner and Pan Dryer Spray Tower Outlet .	      25

  4-4     EPA Method 1, Sample and Velocity Traverse for  Stationary
            Sources	      27

  4-5     Observers Location Visible Emission, Spray Tower and Venturi
            Scrubber, Harshaw/Filtrol 	      28

  5-1     Modified EPA Cadmium Sampling Train (August 18, 1977 Federal
            Register)	      30

  5-2     Schematic of Sample Analyses  	      35
                                       -v-

-------
                                 LIST OF TABLES

TABLE                                                                      PAGE

  2-la    Summary of Controlled Cadmium Emissions,  Spray Tower 103,
            Harshaw/Filtrol Partnership, July 1986   	       6
  2-lb    Summary of Controlled Cadmium Emissions,  Spray Tower 103,
            Harshaw/Filtrol Partnership, July 1986   	
  2-2     Summary of Visible Emissions,  Spray Tower 103,  Hawshaw/
            Filtrol Partnership, July 1986  	
  2-3a    Summary of Controlled Cadmium Emissions,  Venturi Scrubber
            201, Harshaw/Filtrol Partnership, July  1986 	      13

  2-3b    Summary of Controlled Cadmium Emissions,  Venturi Scrubber
            201, Harshaw/Filtrol Partnership, July  1986 	      14

  2-4     Summary of Visible Emissions, Venturi Scrubber 201, Harshaw/
            Filtrol Partnership, July 1986  	      ] 6

  2-5     Trace Metal Analysis	      20
                                      -vi-

-------
                                    PREFACE




    The  work   described   herein  was   conducted  by   personnel  from   TRC




Environmental Consultants, Inc.,  Midwest  Research Institute (MRI), the  United




States Environmental  Protection Agency Emission  Measurement Branch (EPA/EMB),




and Harshaw/Filtrol Partnership in Louisville,  Kentucky.




    The  scope  of  work   was  issued  under  EPA  Contract  68-02-4337,  Work




Assignment 1.  The work was performed under the supervision of John H.  Powell,




TRC Work Assignment Manager, and Richard A. Pirolli, TRC Field Team Leader.




    Mark Turner of  MRI  monitored process operations.  MRI  was  responsible for




preparing Section 3 of  this report, which deals  with  process  descriptions and




operations.   Sam  Narvarte,   Technical  Superintendent  of   Harshaw/Filtrol,




provided  invaluable  assistance  and  guidance  to  TRC,   EPA,  and  MRI   in  the




performance  of the   test  program.   Michael  Toney,  Office  of  Air  Quality




Planning  and Standards  (OAQPS),  Emission Measurement  Branch,  EPA,  served as




Task Manager and was responsible for coordinating the test program.
                                      -vi i-

-------
1.0 INTRODUCTION




1.1 Background




    Section 112 of the Clean Air Act  of  1977 charges the administrator of  the




United  States  Environmental  Protection  Agency with  the  responsibility  of




establishing National Emission Standards  for Hazardous Air  Pollutants  (NESHAP)




from  sources  that  may  significantly  contribute   to  air  pollution.    When




promulgated,  these  standards  of  performance  are  to reflect  the  degree  of




emission  limitation  achievable  through  application  of  the best  demonstrated




emission control technology.   Emission data collected from controlled  sources




in the cadmium  industry may provide a portion of the data base used by EPA to




develop a NESHAP.




    EPA  Industrial  Studies  Branch  (ISB) selected  Hawshaw/Filtrol  Partnership




in Louisville, Kentucky, as  a  site  for an emission test program  because  there




is no  data currently  available  to quantify cadmium  emissions  accurately from




belt  dryers,   rotary   calciners    or  vacuum  pan   dryers  used   in  pigment




manufacturing  plants.   The  test  program  was designed  to develop controlled




emission factors for cadmium sulfide pigment industries.




    TRC  Environmental  Consultants,   Inc.  was  retained by the  EPA  Emission




Measurement   Branch   (EMB)    to   perform   emission   measurements   at   the




Harshaw/Filtrol  Partnership  in Louisville,  Kentucky.   Testing was performed on




the red  and yellow belt dryer venturi scrubber  stacks  (SD-301  & 201)  and the




rotary calciners/vacuum  pan  dryer  spray  tower stack  (S-103).   This report has




been  prepared   in  accordance  with  EPA  Contract   No.  68-02-4337  under  the




provisions of Work Assignment No.  1.




    Midwest Research  Institute (MRI), the  NESHAP contractor,  was  responsible




for coordinating the  overall  test  program  with Harshaw/Filtrol  personnel and




for assuring that  process  and  control   equipment  operating  conditions  were




suitable for testing.  Related process data were monitored and recorded by MRI.
                                       -1-

-------
1.2 Summary of Process
1.3 Applicability of EPA Reference Test Methods



    EPA  is  required to  publish a  national  reference  test  method for  each




regulated  source  category and  pollutant  for  which  a NESHAP is  established.




Reference  test methods  are usually  specified  by a  State  regulatory  agency




during  the State implementation  planning process and may  be different  from




national reference test methods.



    The purpose of  establishing a national reference test method  is to ensure




that emission  data  collected from a specific  source  is  representative  of that




source  and  comparable  to  data collected  at  other  designated sources.   The




primary  purpose  of  this  test  program  was  to collect  emission  data  using




standardized test methods that  will  allow the  data to be  evaluated to  develop




a  NESHAP.    One  test method was  selected by EPA to measure emissions  from




cadmium  pigment  manufacturers.  This  method is  briefly  described  in  the




following  subsection and is described in detail in Section 5.








    1.3.1  EPA Method 5 Configuration Modified for Cadmium




    Cadmium  sampling was performed by using a  modification of the  standard EPA




Method  5  train.'   This modification  consisted  of  placing flexible  Teflon




tubing  between the  filter  and the  impingers  and the use of  5%  Nitric  acid
                                       -2-

-------
solution  in  the  first  two  impingers,  teflon tubing  was  used due  to  the




particularly difficult sampling locations.




    Five percent  Nitric acid  is  used as the impinger solution because  metals




are  readily soluble in  Nitric acid  and also  Nitric acid increases  capture




efficiency.








1.4 Measurement Program Summary




    The measurement  program was  conducted  at the Harshaw/Filtrol  Partnership




in  Louisville,  Kentucky  during  the  week  of July 14,  1986.    Tests  were



performed  at  the red  and yellow belt  dryer venturi scrubber  stacks and  the




rotary calciners/vacuum pan dryer spray tower stack.




    All  emission  testing  was performed  by  TRC.   MRI  personnel  monitored




process operating conditions.  Michael Toney of EMB observed the test program.








    1.4.1  Spray Tower and Venturi




    Preliminary Measurements




    Preliminary testing  was performed on July 14,  1986 to determine volumetric




flowrate and  stack  gas  moisture  content.   An  integrated  gas sample was  also




taken  to  determine  concentrations of  COz,  Oz,  and CO,  which were found to




be ambient.  Stack diameter and the sampling  port  configuration were confirmed




at this time.








    Method 5 Modified For Cadmium




    Six Method 5 tests modified for  cadmium  were  performed,  two  tests  on the




yellow  belt dryer  venturi  scrubber  (SD-201),  one test  on the red  belt dryer




venturi  scrubber  stack (SD-301) and  three  tests on  the  rotary calciner/vacuum








1Code of Federal Regulations 40, Part 60 Appendix A, July, 1981.
                                       -3-

-------
pan dryer spray  tower (S-103).  Testing  at these  locations  was performed  on




July 15, 16 and 17, 1986.








    Method 9 - Visible Emissions




    Visible  emissions from  the spray  tower  stack and  the  venturi  scrubber




stacks were observed concurrently with each Method 5 modified  for cadmium test.








1.5 Report Sections




    The  remaining  sections  of this report  present  the Slummary  and  Discussion



of  Results  (Section  2),  Process  Description  and Operations  (Section  3),




Description  of  Sampling  Locations  (Section  4),   Sampling   and  Analytical




Procedures   (Section  5),  and  Quality  Assurance  (Section  6).   Methods  and




procedures,  field  and   laboratory  data,  and  calculations  are  presented  in




various  appendices as noted in the Table of Contents.
                                       -4-

-------
2.0 SUMMARY AND DISCUSSION OF RESULTS




    A summary of all  emission  measurements and collected data is presented  in




this  section.    Section  2.1  presents  cadmium  and visible  emission  results




collected  at  spray  tower 103  and  a  complete breakdown  and  discussion  of




parameters.   Cadmium,  and  visible  emission  results  collected  at  venturi




scrubber  201  and  301 are  presented  in  Section  2.2.   Section  2.3  presents




results of the trace metals.









2.1 Spray Tower




    A total of three tests were conducted  at  spray tower 103 using a  Method 5




sampling  train  modified for  cadmium.   All tests  were acceptable with a leak




rate of <0.02cfm and isokinetics of 100  10%.








    2.1.1  Cadmium Emissions




    Tables  2-la  (English Units)  and 2-lb (Metric Units) present a  summary of




measured cadmium emissions from spray tower 103.




    The  average  total  cadmium emission  rate  was 4.04 x  10"3  Ib/hr  (5.09 x




10" 4  g/sec)  and  ranged from  2.75  x  10"3   Ib/hr (3.46  x  10"4   g/sec)  to




4.97   x  10"3   Ib/hr   (6.26  x  10~4  g/sec).    The   average   total  cadmium




concentration was  1.98  x  10~4 gr/DSCF and  ranged  from 1.07  x 10~4  gr/DSCF




to  2.44 x  10~4  gr/DSCF. All  significant  cadmium  concentrations and emission




rates were collected in  the front half of the sampling train.









    2.1.2  Visible Emissions




    A   summary  of  visible  emission  observations  from  the spray  tower  is




presented  in Table 2-2.   Average opacities  are presented for  6 minute  time




periods during  each two hour test.  The average opacity was 1% for tests 1 and
                                       -5-

-------
                                TABLE  2-la

                              (ENGLISH UNITS)

                  SUMMARY OF CONTROLLED CADMIUM EMISSIONS
                              SPRAY TOWER 103
                        HARSHAW/FILTROL PARTNERSHIP
                                 JULY 1986
TEST NO
DATE
TIME
1
7/15/86
1056-1500
2
7/16/86
0832-1245
3
7/17/86
0846-1251
AVG
Sample Conditions
Volume (DSCF)1
Front Half Catch (pg)
Back Half Catch (>ig)
Total Catch (pg)
Isokinesis (%)
Stack Conditions
Flowrate (DSCFM)
Temperature (F)
Moisture (%)
Oxygen (%)
Opacity (%)
Process Conditions
Production Rate (ton/hr)
Cadmium Emissions
Front
Half
Concentration
Mass

Back
Emission

Half
Concentration
Mass

Total
Emission


Concentration
Mass

Emission


(gr/DSCF)
Rate (Ib/hr)
(Ib/ton)

(gr/DSCF)
Rate (Ib/hr)
(Ib/ton)

(gr/DSCF)
Rate (Ib/hr)
(Ib/ton)
107.65
1680
13.6
1694
101.7
2120
101
11.4
20.9
1
0

2
4
2

1
3
2

2
4
2
.15

.41x10""
.38xlO"3
.92xlO"2

.95xlO"6
.54xlO"s
.36x10""

.43x10""
.41xlO~3
.94xlO"2
118.29
1860
7.2
1867
96.2
2380
99
3.2
20.9
1
0

2
4
3

9
1
1

2
4
3
.15

.43x10""
.95xlO~3
.30xlO~2

.39xlO"7
,92xlO"5
.28x10""

.44x10""
. 97x10" 3
.31xlO"2
150.66
1030
10.2
1040
97.0
3010
103
5.5
20.9
0
0

1
2
1

1
2
1

1
2
1
.15

.06x10""
.72xlO"3
.SlxlO"2

.OSxlO"6
.70xlO"s
.80x10""

.07x10""
.75xlO"3
.83xlO"2
2500
101
6.7
20.9
1
0.

1.
4.
2.

1.
2.
1.

1.
4.
2.
15

97x10"
02x10"
68x10"

31x10"
72x10"
81x10"

98x10"
04x10"
69x10"


4
3
2

b
S
2

4
3
2
Standard Conditions:   29.92 in.  Hg @ 68F
                                    -6-

-------
                                 TABLE 2-lb

                               (METRIC UNITS)

                  SUMMARY OF CONTROLLED CADMIUM EMISSIONS
                              SPRAY TOWER 103
                        HARSHAW/FILTROL PARTNERSHIP
                                 JULY  1986
TEST NO 1
DATE 7/15/86
TIME 1056-1500
Sample Conditions
Volume (NM3)1
Front Half Catch (ug)
Back Half Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
Flowrate (NM3/MIN)
Temperature (C)
Moisture (%)
Oxygen (%)
Opacity (%)
Process Conditions
Production Rate (ton/hr)
Cadmium Emissions
Front Half
Concentration (Mg/NM3)
Mass Emission Rate (g/sec)
(g/ton)
Back Half
Concentration (Mg/NM3)
Mass Emission Rate (g/sec)
(g/ton)
Total
Concentration (Mg/NM3)
Mass Emission Rate (g/sec)
(g/ton)

3.05
1680
13.6
1694
101.7

60.04
38
11.4
20.9
1

0.15


551
S.SlxlO'4
13.22

4.46
4.46xlO~6
0.107

555
5.55xlO"4
13.32
2
7/16/86
0832-1245

3.35
1860
7.2
1867
96.2

67.40
37
3.2
20.9
1

0.15


555
6.24xlO'4
14.98

2.15
2.41xlO"6
0.058

557
6.26x10""
15.02
3
7/17/86
OEI46-1251

4U27
1030
10.2
1040
97.0

85.24
39
5.5
20.9
0

0.15


241
3.43xlO~4
8.23

2.39
3. 39x10" 6
0.081

244
3.46xlO"4
8.30
AVG







70.89
38
6.7
20.9
1

0.15


449
5.06xlO"4
12.14

3.00
3.42xlO~6
0.082

452
5.09x10""
12.21
Standard Conditions:  760 mm in. Hg @ 20C
                                     -7-

-------
          TABLE  2-2

SUMMARY OF VISIBLE EMISSIONS
       SPRAY TOWER 103
 HARSHAW/FILTROL PARTNERSHIP
          JULY 1986
TEST NO 1
7/15/86
1040-1413
SIX MINUTE
TIME PERIOD
1040-1046
1046-1052
1052-1058
1058-1104
1104-1110
1110-1116
1116-1122
1122-1128
1128-1134
1134-1140
STOP TEST
1313-1319
1319-1325
1325-1331
1331-1337
1337-1343
1343-1349
1349-1355
1355-1401
1401-1407
1407-1413
AVG
AVERAGE
OPACITY (%)
1
2
3
2
3
2
1
0
0
0

0
0
0
0
0
1
0
0
0
1
1
TEST NO 2
7/16/86
0824-1135
SIX MINUTE
TIME PERIOD
0824-0830
0830-0836
0836-0842
0842-0848
0848-0854
0854-0900
0900-0906
0906-0912
0912-0918
0918-0924
STOP TEST
1035-1041
1041-1047
1047-1053
1053-1059
1059-1105
1105-1111
1111-1117
1117-1123
1123-1129
1129-1135
AVG

AVERAGE
OPACITY (%)
1
1
0
0
0
0
0
0
1
1

1
0
2
0
0
1
0
1
1
0
1
TEST NO 3
7/17/86
0745-1114
SIX MINUTE
TIME PERIOD
0745-0751
0751-0757
0757-0803
0803-0809
0809-0815
0815-0821
0821-0827
0827-0833
0833-0839
0839-0845
STOP TEST
1014-1020
1020-1026
1026-1032
1032-1038
1038-1044
1044-1050
1050-1056
1056-1102
1102-1108
1180-1114
AVG

AVERAGE
OPACITY
0
0
0
0
0
0
1
0
0
0

0
0
0
0
0
0
0
0
0
0
0
             -8-

-------
2  and  0%  for  test  3.    These  6-minute  average  opa.ci.ties  are  presented




graphically in Figures 2-1 through 2-3.








    2.1.3  Stack Conditions




    An  average volumetric  flowrate of  2500 DSCFM was  measured exiting  the




spray  tower stack at  101F,  6.7%  moisture  and 20.9%  oxygen.   For  the  first




test,  the  volumetric flowrate  was  2120 DSCFM  at  101F.  11.4  % moisture  and




20.9%  oxygen.   This  volumetric  flowrate was  30% lower than test 3.   This  may




be accounted for  by  the high moisture seen  in  the first  test.   Test 3  had a



volumetric flowrate of 3010 DSCFM at 103F, 5.5% moisture and 20.9% oxygen.








2.2 Venturi Scrubber




    Two  tests  were performed  at venturi  scrubber  stack  201  and one test  on




venturi  scrubber  301  using a  Method  5 sampling  train modified for cadmium.



All tests  were acceptable  with a  leak  rate  of <0.02cfrn  and 100  10 percent




isokinetics.








    2.2.1  Cadmium Emissions




    Tables  2-3a  (English  Units) and 2-3b  (Metric Units)  present a  summary of




measured  cadmium  emissions from  the  venturi  scrubber.    The   average  total



cadmium  emission  rate was  4.85 x  10"3  Ib/hr (6.10  x  10"4 g/sec)  and  ranged




from  4.45  x  10'3 Ib/hr  (5.61  x  10'4  g/sec)   to  5.16 x 10"3   Ib/hr  (6.50 x




10~4 g/sec).




    The  average  total cadmium  concentration  was  5.17  x 10"4  gr/DSCF  and




ranged from 4.49  x   10~4  gr/DSCF  to  6.18  x 10"4  gr/DSCF.  All  significant




cadmium  concentrations  and emission rates were  collected  in the front half of




the sampling train.
                                       -9-

-------
   25-
   20-
                                   TEST 1 7/15/86
   15-
a:
Q.
O
C3
f.
Of
   10-
    5 -
                                      STOP
                                      TEST
                                                                      P.
                                                            STOP
                                                            TEST
                                  T
      1040
1058
1116
I
 1313
                                     T
1134     1313      1331

6 MINUTE TIME RECORD
                                                            1349
1407
                          Figure 2-1.  Summary of Visible Emissions
                                      Spray Tower 103
                                      Harshaw/Filtrol  Partnership
                                         -10-

-------
   25 -
   20 -
                                     TEST 2 7/16/86
O-
o
ts

2  10
UJ
s
t
    5 _
                                    STOP
                                    TEST
n
      STOP
      TEST
                                                      ru
     0824    0842     0900     0918     1035     1053

                                 6 MINUTE TIME RECORD
          1111
1129
                       Figure 2-2. Summary of Visible Emissions
                                  Spray Tower 103
                                  Harshaw/Filtrol  Partnership
                                      -11-

-------
    25-
   20-
                                TEST 3  7/17/86
    15-
Q.
O
   10-
C
UJ


-------
                                   TABLE 2-3a

                                 (ENGLISH UNITS)

                    SUMMARY OF CONTROLLED CADMIUM EMISSIONS
                              VENTURI  SCRUBBER 201
                          HARSHAW/FILTROL PARTNERSHIP

                                   JULY 1986
TEST NO
DATE
TIME
Sample Conditions
Volume (DSCF)Z
Front Half Catch (ug)
Back Half Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
Flowrate (DSCFM)
Temperature (F)
Moisture (%)
Oxygen (%)
Opacity (%)
Process Conditions
1
7/15/86
1058-1515

96.05
3010
11.0
3021
97.0

1070
130
6.6
20.9
0

2
7/16/86
0820-1227

85.72
3420
11.8
3432
99.8

930
138
9.4
20.9
0

31
7/17/86
0754-1200

120.03
3460
33.5
3494
96.8

1340
140
7.3
20.9
4

AVG







1110
136
7.8
20.9
1

Production Rate (ton/hr)   0.063
Cadmium Emissions
0.063
0.063
  Test No. 3 on Venturi Scrubber 301
  Standard Conditions:  29.92 in Hg @ 68F
0.063
Front Half
Concentration (gr/DSCF)
Mass Emission Rate (Ib/hr)
(Ib/ton)
Back Half
Concentration (gr/DSCF)
Mass Emission Rate (Ib/hr)
(Ib/ton)
Total
Concentration (gr/DSCF)
Mass Emission Rate (Ib/hr)
(Ib/ton)

4
4
7

1
1
2

4
4
7

.84x10"
.44x10"
.05x10"

.77x10"
.62x10"
.57x10"

.85x10"
.45x10"
.06x10"

4
3
2

E
5
4

4
3
2

6
4
7

2
1
2

6
4
7

.16x10"
.91x10"
.79x10"

.13x10"
.69x10"
.68x10"

.18x10"
.93x10"
.83x10"

4
3
2

6
S
4

4
3
2

4
5
8

4
4
7

4
5
8

.45x10"
.11x10"
.11x10"

.31x10"
.95x10"
.86x10"

.49x10"
.16x10"
.19x10"

4
3
2

6
S
4

4
3
2

5.
4.
7.

2.
2.
4.

5.
4.
7.

15xlO"4
82xlO"3
65xlO"2

74xlO"6
75xlO"s
37xlO"4

17xlO"4
85xlO"3
69xlO"2
                                      -13-

-------
                                TABLE 2-3b

                               (METRIC UNITS)

                  SUMMARY OF CONTROLLED CADMIUM EMISSIONS
                            VENTURI  SCRUBBER 201
                        HARSHAW/FILTROL PARTNERSHIP

                                 JULY 1986
TEST NO 1
DATE 7/15/86
TIME . 1058-1515
Sample Conditions
Volume (MM3)2
Front Half Catch (ug)
Back Half Catch (ug)
Total Catch (ug)
Isokinesis (%)
Stack Conditions
Flowrate (NM3/MIN))
Temperature (C)
Moisture (%)
Oxygen (%)
Opacity (%)
Process Conditions
Production Rate (ton/hr)
Cadmium Emissions
Front Half
Concentration (ug/NM3)
Mass Emission Rate (g/sec)
(g/ton)
Back Half
Concentration (ug/NM3)
Mass Emission Rate (g/sec)
(g/ton)
Total
Concentration (ug/NM3)
Mass Emission Rate (g/sec)
(g/ton)

2.72
3010
11.0
3021
97.0

30.30
54
6.6
20.9
0

0.063


1107
5.59x10""
31.94

4.04
2. 04x10" 6
0.117

1111
5.61x10""
32.06
2
7/16/86
0820-1227

2.43
3420
11.8
3432
99.8

26.34
59
9.4
20.9
0

0.063


1407
6.18x10""
35.31

4.86
2.13xlO'6
0.122

1412
6.20x10""
35.43
31
7/17/86
0754-1200

3.40
3460
33.5
3494
9S.8

37.95
60
7.3
20.9
4

0.063


1018
6.44x10""
36.80

9.85
6.23xlO"s
0.356

1028
6.50x10'"
37.14
AVG







31.53
58
7.8
20.9
1

0.063


1177
6.07x10""
34.68

6.25
3.47xlO"6
0.198

1184
6.10x10'"
34.88
Test No. 3 on Venturi Scrubber 301
Standard Conditions:  760 mm Hg @ 20C
                                    -14-

-------
    2.2.2  Visible Emissions




    A  summary of  visible  emission  observations  from  the  venturi  scrubber




stacks  is  presented  in  Table  2-4.    Average  opacities   are   presented   for




6-minute time  periods during each  two  hour  test.   The average opacity was  0%




for tests  1  and  2 and 4% for test  3.   Opacity observations were conducted  on




venturi  scrubber  301  for test  3.   The  opacity was high  (12%  to 0%) for  the




first hour of observation.  During  the second hour of observation, the average




opacity was  0%.   These  6-minute average opacities  are  presented graphically in




Figures 2-4 through 2-6.








    2.2.3  Stack Conditions




    The volumetric flowrate  exiting venturi  scrubber stack 201  was  10700  DSCFM




at 130F,  6.6% moisture and 20.9% oxygen for  Test  1 and  930  DSC '4 at  138F,




9.4%  moisture  and 20.9%  oxygen for Test  2.   Test 3 was  conducted  at venturi




scrubber stack 301 and  the  volumetric flowrate was  1340 DSCFM  at 140F,  7.3%




moisture and 20.9% oxygen.









2.3 Trace Metals




    One sample and blank per set of tests were analyzed for  trace metals.   The




trace   metals   analyzed  for  were  barium,   chromium,  copper,  iron,   lead,




magnesium, manganese, nickel  and zinc.   Mercury was not  analyzed  due to  the




different  digestion procedure.   Table 2-5 presents a summary of  trace metals.




Sample  train results were corrected for  field  and/or laboratory blanks.   Trace




metals  in  the  field  blanks were high.  This may be caused from the  nitric acid




rinse of the nozzles.   The  sample  train results are representative  due to  the




significant difference between blanks and runs.
                                      -15-

-------
                                   TABLE 2-4

                          SUMMARY  OF VISIBLE EMISSIONS
                             VENTURI  SCRUBBER  201
                          HARSHAW/FILTROL PARTNERSHIP
                                   JULY 1986
TEST NO
7/15/86
1

1157-1513
SIX MINUTE
TIME PERIOD
1157-1203
1203-1209
1209-1215
1215-1221
1221-1227
1227-1233
1233-1239
1239-1245
1245-1251
1251-1257
STOP TEST
1413-1419
1419-1425
1425-1431
1431-1437
1437-1443
1443-1449
1449-1455
1455-1501
1501-1507
1507-1513
AVG
AVERAGE
OPACITY (%)
0
1
0
0
0
1
1
0
0
0

0
0
0
0
0
0
0
0
1
0
0
TEST NO 2
7/16/86
0930-1244
SIX MINUTE
TIME PERIOD
0930-0936
0936-0942
0942-0948
0948-0954
0954-1000
1000-1006
1006-1012
1012-1018
1018-1024
1024-1030
STOP TEST
1144-1150
1150-1156
1156-1202
1202-1208
1208-1214
1214-1220
1220-1226
1226-1232
1232-1238
1238-1244
AVG


TEST NO
7/17/86
3*

0851-1217
AVERAGE
OPACITY (%)
0
0
0
0
0
1
1
0
0
0

0
0
0
0
0
0
0
0
0
0
0
SIX MINUTE
TIME PERIOD
0851-0857
0857-0903
0903-0909
0909-0915
0915-0921
0921-0927
0927-0933
0933-0939
0939-0945
0945-0951
STOP TEST
1117-1123
1123-1129
1129-1135
1135-1141
1141-1147
1147-1153
1153-1159
1159-1205
1205-1211
1211-1217
AVG
AVERAGE
OPACITY
11
12
7
11
10
9
9
7
6
3

0
0
0
0
0
0
0
0
0
0
4
* Opacity Observations at scrubber 301
                                      -16-

-------
    25-
    20-
                                 TEST 1  7/15/86
    15-
Q.
O
CJ

-------
    25-
    20-
                                  TEST 2  7/16/86
    15-
f.
o.
o
o

-------
    25-
    20-
    15-

-------
                                              TABLE 2-5
                                       SUMMARY OF TRACE METALS
                                     HARSHAW/FILTROL PARTNERSHIP
                                              JULY 1986
Sample1
Location
Barium (ug)
Chromium (ug)
Copper (ug)
Iron (ug)
Lead (ug)
M Magnesium (ug)
o
Manganese (ug)
Nickel (ug)
Zinc (ug)
Blank 1
Venturi
201
nd2<50
253
9
1010
nd<46
115
22
94
90
Run 1
Venturi
201
nd<50
1280
39
6800
nd<46
153
183
676
6320
Blank 1 Run 1
Spray Tower Spray Tower
103 103
nd<50
53
15
282
' nd<46
104
7
44
110
nd<50
100
37
892
nd<46
174
13
126
4050
HN03
Blank
nd<25
nd<5
nd<3
8
nd<23
1.4
nd<4
nd<7
nd
-------
3.0 PROCESS AND OPERATIONS (Provided by MRI)
3.1 Process Equipment
3.2 Control Equipment
                                      -21-

-------
4.0 SCOPE OF SAMPLING PROGRAM




    Sampling train operators maintained a detailed log of their test times  for




each run.   Data sheets  present  all necessary  information  in concise  legible




form.




    Method  5  test  data  such  as:   percent isokinetics,  moisture,  flowrate




(DSCFM) and stack temperatures was calculated daily.  Results were  recorded on




a daily summary sheet.









4.1 Belt Dryer




    Prior  to  emission  testing,   the  flowrate  of the  stack was  measured  in




accordance  with EPA  Methods  1-2.   Duct  measurements  were  verified  at  this




time.   Stack  gas  moisture  content  was  determined  using  wet  bulb/dry  bulb




thermometers.




    Cadmium  samples were  collected from a 10 inch  circular duct.   Two  3-inch




sample  ports  were  placed  90  apart  in the  duct.   Figure  4-1 presents  the




sample  port configuration.  Sample  point A  indicates  the  Method   5  sampling




location.   According  to EPA Method 1, 24 traverse points  are  required.   Each




traverse point was  sampled for ten minutes  for a total test time of  4  hours.




An  "EPA Method 1,  Sampling and Velocity Traverse" sheet is presented in Figure




4-2.









4.2 Rotary Calciner and Vacuum Pan Dryer




    Prior  to emission testing, routine preliminary measurements were conducted




as described  in Section 4.1.




    Cadmium  samples  were  collected  in  two ports positioned  90 apart  and




located 26  inches  (2 diameters)  downstream from  the  fan and  14 inches  (1




diameter)  upstream  from the top of  the  stack.  The location of the  sampling




ports are presented in Figure 4-3.
                                      -22-

-------
 SAMPLE  POINT B
 SAMPLE  POINT  A-
                          10"
T
 19"



I
                                    20"
                                    i
NOT TO SCALE
                         FAN
         Figure 4-1.  Belt Dryer Venturi Scrubber Outle"
                                      -23-

-------
            Environmental
            Consultants, Inc.
           EPA Method  1   Sample  and Velocity Traverse
              Figure 4-2               for  Stationary Sources
"
-------
   SAMPLE POINT B
   SAMPLE POINT A
   NOT  TO  SCALE
                           FAN
                                      T
                                       14"
                                      26
Figure 4-3.   Calciner and Pan Dryer Spray Tower Outlet



                                       -25-

-------
    According  to  EPA Method  1,  24  traverse  points  were  sampled  at   this




location for  ten minutes per point for a  total  test time of 4 hours.  Sample




port and traverse point locations are presented in Figure 4-4.









4.3 Visible Emission Observations (Method 9)




    Visible  emission  observations  were  conducted  in  accordance  with  EPA




Method 9.  Observations  were performed at  the venturi  scrubber  stack and  the




spray tower  stack separately.   Each location was observed for two hours during




each cadmium  emission test.  A diagram showing the  observers  location can  be




found in Figure 4-5.
                                      -26-

-------
            Environmental
            Consultants, Inc.
EPA Method 1    Sample and Velocity Traverse
    Figure 4-4              for Stationary Sources
-rHnn  Ventrui  Scrubber Outlet Number of Ports
Diameters  UpstreamJ	 Points Per Port
Total  Traverse  Points Required.
24
                                   12
Diameters  Downstream,
Traverse (  Horizontal or Vertical).
 rMINIMUM NUMBER OF TRAVERSE POINTS FOR PARTICULATE
           AND NONPART1CULATE TRAVERSES

   Duct Diameters  Upstream from Flow Dlsturoance
                    (Distance A)

0.5          1.0    -    1.5         2.0
50


40
30

"
1


i i i i i i i
H'OHift Nuutift it ton
HIC7AMOUUAH VTACU OH OUCTI
* 0
.*- PARTICIPATE
24 or 28 f
L"

T
A


 
\

rf| AXUff |wl VT
OinUMANCI
^ 	 1


*
-

1Q I 16 TACK OIAMITIR> 0.11 C4UJ
' 4 II 12
^NONPARTICULATE
8 or 9
tTACK DIAMITtA -CJO TO O.n m (1J-J4 UJ
1 1 1 1 I 1 1
 23     4     5     6     7     8     9     10
   Duct Diameters Downstream from Flow Disturbance
                    (Distance 6)

 vLOCATION OF TRAVERSE POINTS  IN CIRCULAR STACKS
Point
Number
On A
Diameter '
. 1
2
3
4
5
6
7
8
9.
10
11
12 ;
(Percent of stack diameter from
Inside wall to traverse point)
Number Of Traverse Points On A Diameter
46 8 10 12
6
25
75
93








.7
.0
.0
.3








4.
14.
29.
70.
85.
95.






4
6
6
4
4
6






3.
10.
19.
32.
to.
80.
89.
96.




2
5
4'
3
7
6
5
8




2
8
14
22
34
65
77
85
91
97


6
.2
.6
.6
.2
.8
.4
.4
.8
.4


2
6
11
17
25
35
64
75
82
88
93
97
.1
.7
.8
.7
.0
.6
.4
.0
.3
.2
.3
.9
                                                                       Sample
                                                                        Port  "
                                               9"

                                                                              20"
                                                                     i
                                                              2LW
                                                         eq
                                                                                    1
                        CROSS-SECTIONAL LAYOUT
                        FOR RECTANGULAR STACKS
                           Total
                      Traverse Points   Matrix
                            9           3x3-
                            12           4x3
                            16          .4x4
                            20           5x4  '
                     	25           5x5
                                                           'TRAVERSE POINT LOCATIONS
No.
1
2
3
4
5
6
7
8
9
10
11
12
Distance
From Wall
0.2"
0.7"
1.2"
1.8" i
2.5" ...
3.6"
6.4"
7.5" 
8.2"
8."
9.3"
9 . 8"
Nipple
Size







.




 Total
Distance













-------
                  301    201             103

                        PIGMENT  BUILDING
NJ
00
I
                        TEST 2
SUN

 TEST 1  and 3
                                  Figure 4-5.  Observers  Location
                                               Visible  Emissions
                                               Spray  Tower  and  Venturi  Scrubber
                                               Harshaw/Filtrol  Partnership
                                               July 1986

-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES




    This  section presents  descriptions of  sampling and  analyses  procedures




which were employed during  the emission testing  conducted at  Harshaw/Filtrol




Partnership facility in Louisville,  Kentucky.




    A combination of EPA  Methods  1, 2, 3,  4,  5 (modified for  cadmium) and  9




were  used to  measure  cadmium,  visible and  trace  metals  emissions from  the




venturi scrubber stack  and the spray tower  stack.









5.1 EPA Method 5 Configuration Modified for Cadmium




    Sampling was  performed using a modification  to the standard EPA Method  5




sampling train1.  It is  shown schematically in Figure  5-1 and consists of  a




nozzle, probe,  filter  with  glass  frit, a flexible Teflon umbilical  line,  four




impingers,  vacuum  pump,  dry  gas  meter,   and an  orifice  flow  meter.    The




modification of  the standard  EPA  Method 5  train consisted of  placing flexible




Teflon  tubing  between  the  filter  and the  impingers.   This modification  made




the sampling  equipment much  easier to handle.  A second modification  was  the




use  of  5% nitric  acid  in  first   two  impingers.   The  sampling  train  was




calibrated before and  after this  test program at  TRC.   This  method is based on




the proposed methodology presented in the Appendix.




    A  nozzle  was  attached to a  stainless steel  glass-lined  probe which  was




heated  to prevent  condensation.    Whatman EPM-1000  fiberglass  filter  paper




supported  in a  4-1/2  inch glass filter holder  with  a  glass  frit was used as  a




particulate collection medium.   Filters were  desiccated and pre  weighed.   A




visible  inspection  for  irregularities in  the  filter  material was  conducted.




The  filter  assembly  was  enclosed  in a  heated  box  to  keep  the   filter




temperature at  approximately  150   F  (10).    A  thermocouple,   located inside
  Code of Federal Regulations 40, Part 60 Appendix A, July 81
                                      -29-

-------
i
to
O
I
                    \c
16
I



14
16
A^__, ! J
              STACK. WALL-
                                 13
           LEGEND

 1 - NOZZLE
 2 - PROBE
 3 - FILTER HOLDER
 4 - HEATED FILTER BOX
 5 - IMPINGER ICE BATH
 6 - UMBILICAL CORD
 7 - VACUUM GAUGE
 8 - MAIN VALVE TO PUMP
 9 - PUMP
10 - BYPASS VALVE
11 - DRY GAS METER
12 - ORIFICE AND MANOMETER
13 - PITOT TUBE AND MANOMETER
14 - THERMOCOUPLE READOUT
15 - FLEXIBLE TEFLON SAMPLE LINE
16 - THERMOCOUPLES
17 -  IMPINGER  OUTLET  TEMPERATURE
                                        Figure 5-1.   Modified EPA Method 5 cadmium sampling  train
                                                     (August 18, 1977 Federal  Register)

-------
the back  half  of the  filter holder,  monitored the gas stream  temperature  to




ensure proper filter temperature.




    Four  impingers  immersed in an  ice bath  were  attached to the back  end  of




the filter holder with  a flexible Teflon tube.  The  first two  impingers  each




contained  100  ml  of  5%  nitric  acid,  the  third was  empty and  the  fourth




contained 200 grams of  silica  gel to remove any remaining moisture.   Impinger




outlet temperatures were kept between 50F and 80F.




    Flexible tubing, vacuum  gauge,  needle  valve,  leakless vacuum pump,  bypass




valve, dry gas meter,  calibrated  orifice and inclined manometer completed the



sampling train.   A check valve was not used in the  TRC sampling train.




    A  nomograph  was  used  to  quickly  determine   the  orifice  pressure  drop



required  for  any pitot  velocity  pressure and  stack  temperature  in order  to




maintain  isokinetic  sampling conditions.   Sampling flow was  adjusted  by means




of the bypass valve.   Before and after  each  particulatei  test  run as well  as



port  changes,  the  sampling  train was leak  checked.   Sample time was  4 hours




per run.




    Test  data  recorded  at  ten  minute  intervals  for   each   sampling  point




included; test time, sampling duration at each  traverse point,  pitot pressure,




stack  temperature,  dry  gas  meter volume and  inlet-outlet temperatures, probe




temperature, and orifice pressure drop.








5.2 Sample Recovery




    Sample  recovery  was performed  in a clean, wind-free  area to avoid sample




contamination.   The  TRC mobile  environmental  laboratory  was  adjacent  to the




test  site and  utilized for sample  recovery.   Working surfaces were  covered




with  fresh  Kimwipes  prior  to each  sample  recovery to  mitigate  contamination.




Personnel  wore  disposable  gloves  when  recovering  samples.    Brushes  and




tweezers were kept in plastic bags when not in  use.  Each  sample probe  had its
                                      -31-

-------
own  brush  to  lessen  cross  contamination.    All  sampling  equipment  had  no

exposed openings  before  and  after  sampling*   The following  sample  fractions

were recovered:



    Container No. 1           Glass fiber filter.

    Container No. 2           Probe,  nozzle,   and front  half  of  the  filter
                              housing HMOs rinses.

    Container No. 3           Impinger  solution.  Teflon  line,  impingers  and
                              back-half of the filter housing  HMOs  rinses.

    Container No. 4           Silica gel.


    The probe,  nozzle and  front half of  the filter were  rinsed and  brushed

three  times  with  5%  HN03.   A  200  ml  flask  with  28/12  socket   joint  was

attached  to the ball  end  of  the  probe.   Approximately 50  ml  of   HNOs  were

rinsed  through  the probe  and  collected in the flask.   A  blunt   end  brush

constructed of nylon  bristles and  a  stainless steel shaft was then  passed 3

times  each with  a fresh  immersion  of  5%  HN03  solution  held in  the flask.

The brush was then  removed  and rinsed into the sample  jar.  Recovery personnel

sealed  the opposite end  of the  probe with a gloved finger and inverted twice

allowing  the  HNOs  to  pass  along the  inside  of  the probe.   A final  flush of

fresh  5%  HNOs through  the  probe was made into the  sample container rotating

the  probe so  that HN03 made  contact  with all parts  of the glass  liner.   This

sample was  labeled  and weighed for  shipping.

    The  contents of  the first  three  impingers  were  weighed, recorded,  and

deposited  in  Container  No.   3.   The back   half of the  filter  housing,  the

flexible  Teflon  line,  and the  first  three  impingers and  their  connecting

glassware were  rinsed  3 times  with 5% HNOs solution and combined  with the

impinger  contents.  A 200 ml  flask  with  28/12 socket joint was  attached to one

end  of the flexible  Teflon  line.   Approximately  50 ml of 5%  HNOs  was passed
                                      -32-

-------
through the  line and  collected  three times  with  fresh  5%  HNOs.   The  final

volume was  weighed and  recorded.   Silica gel  moisture gain was weighed  on a

triple beam balance and recorded.

    The glass fiber  filter was removed,  placed into a contamination free petri

dish, sealed with parafilm and labeled.

    The sample container was labeled with the following information:
        1.  Sample I.D.  (determined by location, run number and content)
        2.  Project Name
        3.  Date of Sampling
        4.  Shipping weight
        5.  Comments

    Sample recovery data  sheets were used to record: volumes recovered, filter

ID  numbers,   silica  gel  weights  and  visual  descriptions  of  the  samples.

Completed forms can be found in the Appendix.

    A sample  log  sheet was  completed recording:  date,  run  number,  sample ID,

sample description and remarks.  Completed copies of this; form is presented in

the Appendix.



5.3 Sample Analyses

    Sample analyses  was  performed in  TRC Environmental Laboratories  in East

Hartford, CT.  The sample fractions were analyzed as follows:


    Container No. 1 The filter  was desiccated  and  weighed for particulate
                    measurement.   The  filter and probe wash was digested,
                    extracted  and analyzed  for cadmium by  flame  atomic
                    absorption.    One   set  of  samples  was   analyzed  for
                    trace metals by flame atomic absorption.

    Container No. 2 Nozzle  and probe rinse  were dried  and  weighed;  then
                    brought  back  to  solution  with HNOs.    The  solution
                    was extracted  and analyzed with Container No. 1.

    Container No. 3 The  solution  was  analyzed separately   as  Container
                    No. 2.
                                      -33-

-------
    A flow diagram of the sample analysis procedure is presented in Figure  5-2.

    Trace metals standards purchased  from J.T.  Baker Standards, which are  MBS

traceable, was used  for  all  trace metals analyses.   Samples were  concentrated

or  diluted in  order to  bring  the  analysis  range  into  the  center  of   the

linearity  curve.   All  samples were  analyzed and three  readings  taken as  a

measure of precision.  A complete description of  the analytical procedure  can

be found in the Appendix.

    The trace metals to be analyzed for were:


                  Barium
                  Chromium
                  Copper
                  Iron
                  Lead
                  Magnesium
                  Manganese
                  Nickel
                  Zinc



5.4 Visible Emissions Observation

    A certified visible emissions observer read exhaust opacity  at  the  outlets

of  the  venturi scrubber  arid spray tower.   Sample Point B in  Figures  4-1 and

4-2 depicts the exhaust points.

    The  observer's  location  was determined on-site in  accordance with  EPA

Method 9 and considering obstructions and traffic problems in the area.

    The  Method 9  data  reduction was  calculated  by averaging  24  consecutive

observations  recorded at  15-second  intervals  to  calculate  an  average  for

observation for a 6 minute time period.
                                      -34-

-------
                                     METHOD 5
                                   CADMIUM TRAIN
             FRONT HALF
        (PROBE RINSE & FILTER)
PROBE AND FILTER
  HOLDER RINSE
  FILTER
 EVAPORATE HN03
     WEIGH
 DESICCATE
   WEIGH
   RESULTS (mg)  |      | RESULTS (mg)
DISSOLVE RESIDUE
   WITH HN03
PLACE FILTER
 WITH PROBE
   RESIDUE
    ADD HN03 AND HEAT FOR 10 MINUTES  |
          ADD CONCENTRATED HNOs
        AND REFLUX FOR 30 MINUTES
             COOL SOLUTION
|     ADD HC1 AND HEAT FOR  10 MINUTES  |
             COOL SOLUTION
        DILUTE TO KNOWN VOLUME
    ADJUST SAMPLE FOR LINEARITY CURVE
       ANALYZE  FOR Cd  BY  FLAME AA
                   I
                Cd
                                              BACK HALF
                                         (IMPINGER SOLUTION)
                  ADD CONCENTRATED
                      HN03 AND
                  REFLUX FOR 30 MIN.
                   COOL SOLUTION
                           ALIQUOT
                       (1 SAMPLE ONLY)
                  ADD HC1 AND HEAT
                   FOR 10 MINUTES
 DILUTE TO
KNOWN VOLUME
COOL SOLUTION
                                             ADJUST SAMPLE FOR
                                              LINEARITY CURVE
                                             DILUTE TO
                                            KNOWN VOLUME
                      ANALYZE FOR TRACE
                       METALS BY FLAME
                       OR GRAPHITE AA
                                                                ADJUST SAMPLE FOR
                                                                 LINEARITY CURVE
                                          ANALYZE FOR Cd
                                             FLAME AA
                                                RESULTS 
-------
6.0 QUALITY ASSURANCE




    TRC's  quality  assurance  program   for  source  emission  measurement   is




designed so that the  work  is done by competent,  experienced  individuals  using




properly calibrated  equipment and approved procedures for  sample  collection,




recovery and analysis with proper documentation.




    Specific  details  of  TRC's quality  assurance  program  for stationary  air




pollution  sources  may  be  found  in  the Quality  Assurance  Handbook  for  Air




Pollution Measurement Systems, Volume III (EPA-600/4-7-027b).




    At the beginning of each day, an organizational meeting was held  to orient




personnel  to  the day's  activities,  to  discuss results from  the  previous day,




and to  determine  if  any special considerations are  appropriate for  the  day's




work.








Method 5




    TRC's  measurement devices,  pitot tubes,  dry  gas meters,  thermocouples,




probes  and  nozzles   are uniquely  identified  and  calibrated  with  documented




procedures  and  acceptance  criteria  before  and  after  each  field  effort.




Records of  all  calibration data are maintained in TRC files.  Samples of these




Calibration forms for  equipment  used during the  test  program are presented in




the Appendix.




    All  Method  5 sampling  was  100    10  percent  isokinetic.   Filter outlet




temperatures were maintained at 15010F.




    Clean-up evaluations were performed  on  each initial set  of glassware prior




to   collecting   field  samples.   The   evaluation   tests  were  performed  at




Harshaw/Filtrol Partnership facility.




    Each Method 5 sampling train had a clean-up sequence as follows:
                                      -36-

-------
                  Blank 1
                  Method 5 Run 1
                  Method 5 Run 2
                  Method 5 Run 3
                  Blank 2
    All  blank  sample  recovery was  conducted  identically  to sample  recovery

procedures outlined in Section 5.

    Blanks  of  all   solution  used  during  the  test  program   (HNOs)   were

collected and analyzed.

    In summary, the  evaluation tests were designed to precondition  the  sample

collectors, to establish  blank background values, and to educate  the  clean-up

personnel in specific sample recovery procedures.

    All  sample  recovery  were  performed  by  a  one  person  clean-up  crew.

Appropriate  sample  recovery  data  were recorded on  the sample  identification

log, sample  recovery, chain  of custody  form,  and  analytical  data forms  as

presented in the Appendix.

    Recovered samples were secured in padlocked,  shock-proof,  steel  containers

for storage and shipment for analysis.

    All  preparation  and  analysis  of  Method 5  samples  were performed by  TRC.

TRC  adhered to  the  standards of  quality assurance as  set forth  in  Quality

Assurance  Handbook   for  Air  Pollution  Measurement   Systems,  Volume   III

(EPA-600/4-7-027b)  and the  Handbook for  Analytical  Quality Control  in Water

and Wastewater Laboratories.   (EPA-600/4-79-019, March 1979).



Analytical Quality Control

    The  analytical  quality control  procedures consisted of analyzing duplicate

spikes,  and blanks  on  10%  of the  samples  as  described  in  TRC  Technical

Standard T/S-902  section  E  & F.    Balances were calibrated  with  four  class S

rates  daily.   Since stack samples (filters,  probe wash and  impingers)  cannot
                                      -37-

-------
be split before  the  metals digestion, duplicates were not  done.   Each type  of

sample  was  analyzed for  cadmium  by  the  method  of  standard  addition  to

determine  if  there are  any  matrix interferences.   If this result differed  by

more  than  5%  from the  routine analysis,  all  the  samples were  analyzed  by

standard  addition.   The  atomic  absorption  spectrophotometer  was  calibrated

with  four  standards.  Three  measurements were taken on  sach  sample for  flame

analysis  and  two  for   furnace  analyses.   Refer  to Appendix  A  for  sample

calculations.

    The  laboratory  participates  in  the following  inter-laboratory  quality

control programs:


      State  of  Connecticut,  Department of  Health  Services,  Laboratory
       Division, Laboratory Improvement Program (annually).

      EPA,  Environmental  Monitoring  and  Support  Laboratory,  Quality
       Assurance   Branch,    Water   Pollution   Laboratory   Performance
       Evaluation and Water Supply Performance Evaluation (voluntary).

      NIOSH, Proficiency Analytical Testing Program (quarterly).

      EPA  Environmental Monitoring  Systems  Laboratory  Quality Assurance
       Division.   Stationary  Source  and Ambient  Air,   Inter-Laboratory
       Studies (semi-annually).


Method 9

    The  TRC  emissions  observer was certified  within the  past  6  months  to

perform  visible emission  evaluations.   Documentation verifying  the observers

certification is provided  in  Appendix D.
                                      -38-

-------