United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 80-BRK-1
April 1980
Air
Building  Brick and
Structural Clay Industry
Emission Test Report
Lee Brick and Tile
Company
Sanford, North  Carolina

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  BUILDING BRICK AND STRUCTURAL CLAY INDUSTRY
          Lee Brick and Tile Company
            Sanford,  North Carolina
               Prepared for the
     U.S. Environmental Protection Agency
         Emission Measurement Branch
Research Triangle Park, North Carolina  27711
                   Prepared by
    Clayton Environmental Consultants,  Inc.
             25711 Southfield Road
         Southfield, Michigan   48075
             EMB REPORT NO. 80-BRK-l

               Work  Assignment  22

            Contract No.  68-02-2817

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                  TABLE OF  CONTENTS

                                                    Page

1.0   Introduction                                    1

2.0   Summary and Discussion of  Results               4

3.0   Process Description and  Operation              21

4.0   Location of Sampling  Points                    30

5.0   Sampling and Analytical  Procedures             36


APPENDICES

A.    Project Participants

B.    Field Data Sheets

      B-l.    Particulate

              Sulfur Oxides

              Nitrogen Oxides

              Particle Size

              Visible Emissions

      B-2.    Sampling Summary Data

      B-3.    Summary of Visible Emissions

C.    Particle Size Distribution Tables

      C-l.    Particle Size Distribution
              - North Kiln  (Condition  1)

      C-2.    Particle Size Distribution
              - North Kiln  (Condition  2)

      C-3.    Particle Size Distribution
              - South Kiln  (Condition  1)

      C-4.    Particle Size Distribution
              - South Kiln  (Condition  2)

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           TABLE OF CONTENTS  (CONTINUED)


D.     Example Calculations

E.     Calibration Data

F.     Process Conditions

G.     Particulate Weight by  Fraction

H.     Surface Analysis and Research,  Inc,
       Analytical Report

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                  LIST OF FIGURES
Figure                                              Page

 1.1.     Plant Roof and Source Layout                3
          (plan view)

.2.1.     Particle Size Distribution  -  North         15
          Kiln, Condition 1

 2.2.     Particle Size Distribution  -  North         16
          Kiln, Condition 2

 2.3.     Particle Size Distribution  -  South         18
          Kiln, Conditions 1 and  2

 3.1.     Lee Brick and Tile Co.,  Process Flow       22
          Diagram

 4.1.     North Kiln Stack Cross-Section             32
          and Sampling Point Locations

 4.2.     South Kiln Stack Cross-Section             33
          and Sampling Point Locations

 4.3.     Bottom Kiln Stack Cross-Section            34
          and Sampling Point Locations

 4.4.     Dryer Stack Cross-Section and              35
          Sampling Point Locations

 5.1.     Particulate Sampling Train                 38

 5.2.     Sulfur Oxides Sampling  Train               43

 5.3.     Nitrogen Oxides Sampling Train             45

 5.4.     Particle Sizing Sampling Train             48

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                    LIST OF TABLES



Table                                             Page

 1.1.    Testing Program Protocol                   2

 2.1.    Particulate Concentrations and             5
         Emission Rates

 2.2.    Exhaust Gas Composition                   10

 2.3.    Sulfur Oxides Concentrations and          11
         Emission Rates

 2.4.    Nitrogen Oxides Concentrations and        14
         Emission Rates

 2.5.    Coal and Clay Samples, Ash and Sulfur     20
         Analyses

 4.1.    Physical Parameters of Sources            31

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                  1.0   INTRODUCTION




     The U.S. Environmental Protection  Agency  (EPA)




retained Clayton Environmental Consultants,  Inc.  to




conduct an emission study at Lee  Brick  and  Tile




Company, in Sanford, North Carolina.  The purpose




of the study was to determine various emission data




from the kiln/dryer exhausts  (four locations)  under




two operating conditions.  The results  of this study




will be used in research and development efforts  for




supporting New Source Performance Standards  for




the Building Brick and  Structural Clay  Industry.




This study was commissioned as EMB Project No. 80-BRK-




1, Contract No. 68-02-2817, Work  Assignment  No.  22.




     Testing was conducted under  two kiln firing




conditions: low ash coal  (Condition  1), and  high  ash




coal (Condition 2).  Table 1.1 presents the  distribu-




tion of the various tests conducted.




     Auxiliary data gathered for  each source included




exhaust gas compositions, moistures, temperatures, and




flowrates.   Figure 1.1 presents a plan  view  of the




four sampling locations. A list of the  project partic-




ipants is presented in Appendix A.

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                                  TABLE  1.1.   TESTING  PROGRAM PROTOCOL
Test Type1
Particulate
Nitrogen Oxides
Sulfur Oxides
Particle Size
Coal Sample
(Sulfur and ash content)
Opacities
North Kiln
Cond. 1 Cond. 2
3 1
1 0
1 0
1 1
3 1
South Kiln
Cond. 1 Cond. 2
3 1
1 0
1 0
1 1
3 1
Recorded for the duration of each
particulate run.
Bottom Kiln
Cond. 1 Cond. 2
3 1
1 0
1 0
1 0
3 1
Dryer
Cond. 1 Cond. 2
3 1
1 0
1 0
1 0
3 1
I
NJ
I
   Clay  samples  were  acquired  from each brick car which was in the kiln during  sulfur  oxide sampling,

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I
us
                                           r
                     Penthouse
                                               Brick
                                               dryer
                                                                            Dryer
                                                                           exhaus t
                                                        Bottom
                                                         kiln

               Coal
             handling
             Elevator
                  N
Railroad
  tracks
                                                                       Kiln
       South
North   kiln
Jciln	
           I
           I
           I
                                                               Pulverized
                                                                  coal
                                                                transport
                                                   Coal storage
                                                  and processing
         Figure 1.1.  Plant roof and source  layout  (plan view).

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        2.0  SUMMARY AND DISCUSSION OF  RESULTS




     For all particulate,  sulfur oxide,  nitrogen  oxide,




and gas composition results discussed in this  section,




Sample Nos. 1, 2, and 3 were collected  during  Condition




1  (low ash coal) and Sample No. 4 during Condition  2




(high ash coal). Field  data sheets  are  presented  in




Appendix B.





PARTICULATE EMISSIONS




     Table 2.1 presents a  summary of the particulate




concentrations and emission rates for each  of  the  four




sampling locations.  All results from Sample Nos.  1,  2,




and 3 representing Condition 1 are averaged for each




location, and results from Sample No. 4,  representing




Condition 2, are shown  separately.  Concentrations  are




presented in grains per dry standard c.ubic  foot (gr/dscf)




and milligrams per dry  standard cubic meter  (mg/dscm).




Emission rates are presented in pounds  per hour (Ib/hr)




and kilograms per hour  (kg/hr).




North Kiln




     Filterable particulate concentrations  for Sample




Nos. 1, 2,  and 3 ranged from 0.133 to 0.151 gr/dscf




(305 to 346 mg/dscm) and averaged 0.143  gr/dscf (328




mg/dscm).  Total particulate concentrations ranged




from 0.144 to 0.161 gr/dscf (329 to 368  mg/dscm) and




averaged 0.155 gr/dscf  (355 mg/dscm).   The  filterable
                       - 4 -

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                               TABLE  2.1.  PARTICIPATE CONCENTRATIONS AND EMISSION  RATES
Sampling
Location
Sample
Number3
1980
Data
Stack Gas
Parameters
Flowrate
dscfm
Temp
F
Concentration
Filterable
gr/dscf
mg/dscm
Total
gr/dscf
mg/dscm
Emission Rate
Filterable
Ib/hr
kg/hr
Total .
Ib/hr
kg/hr
1
2
North 3
Kiln

4
1
2
South 3
Kiln

4
1
2
3
Bottom
Kiln
4
1
2
3
Dryer

4
1-9
1-10
1-11
Average
1-12
1-9
1-10
1-11
Average
1-12
1-9
1-10
1-11
Average
1-12
1-9
1-10
1-11
Average
1-12
6,840
6,8&0
6,860
6,830
7,280
10,600
10,500
10,100
10,400
10,500
4,200
4,230
3,970
4,130
4,230
45,800
47,000
45,800
46,200
45,700
520
520
489
510
496
184
192
197
191
192
136
130
144
137
144
84.1
82.1
81.9
82.7
83.9
0.133
0.146
0.151
0.143
0.190
0.035
0.036
0.035
0.035
0.053
0.004
0.004
0.003
0.004
0.006
0.001
0.002
0.001
0.001
0.001
305
334
346
328
434
80.1
82.4
80.8
81.1
120
8.96
9.80
7U08
8.61
13.6
2.13
3.58
2.71
2.81
2.52
0.144
0.161
0.161
0.155
0.190
0.037
0.037
0.037
0.037
0.057
0.007
0.006
0.005
0.006
0.007
0.004
0.003
0.003
0.003
0.004
329
368
367
355
436
85.4
84.7
84.9
85.0
131
15.8
13.1
11.3
13.4
16.5
8.14
7.92
7.20
7.75
8.07
7.81
8.51
8.89
8.40
11.8
3.19
3.24
3.05
3.16
4.74
0.141
0.155
0.105
0.134
0.215
0.366
0.630
0.466
0.487
0.430
3.54
3.86
4.03
3.81
5.36
1.45
1.47
1.38
1.43
2.15
0.064
0.070
0.048
0.061
0.098
0.166
0.286
0.211
0.221
0.195
8.43
9.36
9.44
9.08
11.9
3.40
3.33
3.20
3.31
5.16
0.248
0.208
0.168
0.208
0. 2«1
1.40
1.39
1.23
1.34
1.38
3.82
4.25
4.28
4.12
5.39
1.54
1.51
1.45
1,50
2.34
0.113
0.094
0.076
0.094
0.118
0.633
0.632
0.560
0.608
0.626
'Sample  Nos.  1,  2,  and  3  were
 sampling locations.
collected during Condition 1 with  Sample  No.  4 collected during Condition 2f for  all
                                                         -  5  -

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emission rate ranged from 7.81 to 8.89  Ib/hr  (3.54




to 4.03 kg/hr) and averaged 8.40 Ib/hr  (3.81  kg/hr).




The total emission rate ranged from 8.43 to 9.44  Ib/hr




(3.82 to 4.28 kg/hr) and averaged 9.08  Ib/hr  (4.12




kg/hr).  The filterable concentration for  Sample  No.




4 was 0.190 gr/dscf (434 mg/dscm).   Total partic-




ulate concentration was 0.190 gr/dscf (436 mg/dscm).




The filterable and total emission rates were  11.8 Ib/hr




(5.36 kg/hr) and 11.9 Ib/hr (5.39 kg/hr),  respectively.




South Kiln




     During Condition 1, filterable particulate concentra-




tions ranged from 0.035 to 0.036 gr/dscf (80.1 to 82.4




mg/dscm) and averaged 0.035 gr/dscf (81.1  mg/dscm).




Total particulate concentrations were 0.037 gr/dscf  for




each sample (ranging from 84.7 to 85.4  mg/dscm, averaging




85.0 mg/dscm).  The filterable and total emission rates




ranged from 3.05 to 3.24 Ib/hr   (1.38 to 1.47 'kg/hr)3




and 3.20 to 3.40 Ib/hr  (1.45 to 1.54 kg/hr),  respectively,




averaging 3.16 Ib/hr (1.43 kg/hr) and 3.31 Ib/hr  (1.50




kg/hr), respectively.   The concentrations  of  filterable




and total particulate for Sample No. 4 were 0.053  gr/dscf




(120 mg/dscm) and 0.057 gr/dscf (131 mg/dscm), respectively.




The filterable and total emission rates were  4.74  Ib/hr




(2.15 kg/hr) and 5.16 Ib/hr (2.34 kg/hr), respectively.
                        - 6 -

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Bottom Kiln




     Filterable particulate concentrations  for  Sample




Nos. 1, 2, and 3 ranged  from 0.003  to  0.004  gr/dscf




(7.08 to 9.80 mg/dscm) and averaged 0.004 gr/dscf




(8.61 mg/dscm).  Total particulate  concentrations




ranged from 0.005 to 0.007 gr/dscf  (11.3 to  15.8




mg/dscm) averaging 0.006 gr/dscf  (13.4 mg/dscm).




The emission rates of filterable  and total  particulate




ranged from 0.105 to 0.155 Ib/hr  (0.048 to  0.070




kg/hr) and 0.168 to 0.248 Ib/hr  (0.076 to 0.113 kg/hr)




respectively, averaging  0.134 Ib/hr  (0.061  kg/hr)  and




0.208 Ib/hr (0.094 kg/hr), respectively,  For Sample




No. 4 the filterable and total particulate  concentrations




were 0.006 gr/dscf (13.6 mg/dscra) and  0.007  gr/dscf




(16.5 mg/dscm), respectively.  The  emission  rates  of




filterable and total particulate  were  0.215  Ib/hr




(0.098 kg/hr) and 0.261  Ib/hr (0.118 kg/hr), respectively.




Dryer Stack




     Filterable particulate concentrations  for  Sample




Nos. 1, 2, and 3 ranged  from 0.001  to  0.002  gr/dscf




(2.13 to 3.58 mg/dscm) and averaged 0.001 gr/dscf  (2.81




mg/dscm).   Total particulate concentrations  ranged from




0.003 to 0.004 gr/dscf (7.20 to 8.14 mg/dscm) and




averaged 0.003 gr/dscf (7.75 mg/dscm).  The  emission




rates for filterable and total particulate  ranged  from




0.366 to 0.630 Ib/hr (0.166 to 0.286 kg/hr)  and 1.23

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to  1.40  Ib/hr  (0.560  to  0.633  kg/hr)  respectively,




averaging  0.487  Ib/hr  (0.221 kg/hr) and  1.34  Ib/hr




 (0.608 kg/hr), respectively.  The  filterable and




total particulate concentrations  for  Sample No.  4




were 0.001 gr/dscf  (2.52 mg/dscm) and 0.004 gr/dscf




 (8.07 mg/dscm), respectively.   Filterable and  total




particulate emission  rates were 0.430 Ib/hr (0.195




kg/hr) and 1.38  Ib/hr  (0.626 kg/hr)f respectively.





     Examination of the data reveals a high degree of




reproducibility for concentrations and emission rates




at each sampling location.   Additionally, flowrates




are quite consistent at each location, even between




the two conditions.




     The  single run under Condition 2 shows higher total




concentrations and emission rates than the average of




the three runs under Condition 1 for each location.




The increase in total particulate concentrations from




Condition 1 to Condition 2  ranges from 16.7-percent




at the bottom kiln location to 54.1-percent at




the south kiln location.  Total particulate emission




rates increased in Condition 2 from Condition  1




from 2.8-percent at the dryer stack to 56-percent at




the south kiln stack.
                       - 8 -

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EXHAUST GAS  COMPOSITION




     Table 2.2 displays the exhaust  gas  composition




and moisture content results  for each  sampling




location.  Initially,  four determinations  of  carbon




dioxide, oxygen, and carbon monoxide were  made,




one for each sampling  location^  The Orsat  analyses




at the bottom kiln and dryer  locations  failed  to




detect either carbon dioxide  or carbon  monoxide  in  the




integrated bag sample  acquired simultaneously with




the first particulate  run.  Following  this  analysis,




no subsequent samples were collected at  these locations,




The values obtained from the  first sample were used




for all remaining tests.  Samples were taken  for  gas




composition and analyzed simultaneously  with  each




particulate run at the north  and south kilns.




SULFUR OXIDES




     Table 2.3 presents the sulfur oxides results.




Concentrations of sulfur dioxide are presented in parts




per million  (ppm) and emission rates in  pounds per




hour (Ib/hr) and kilograms per hour  (kg/hr).  Concentra-




tions ranged from less than 3.65 ppm at  the bottom




kiln to 36.5 ppm at the north kiln.  Emission rates




ranged from less than 0.151 Ib/hr (0,068 kg/hr) at




the bottom kiln to 6.10 Ib/hr (2.77 kg/hr) at the dryer




stack.









                          9 -

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                       TABLE 2.2. EXHAUST GAS COMPOSITION
Sampling
Location
Sample
Number
Moisture
Content,
Percent
Exhaust Gas Composition, Dry Basis, Percent
Carbon
Dioxide
Oxygen
Carbon
Monoxide
Nitrogen and
Other Inerts


North
Kiln


South
Kiln


Bottom
Kiln


Dryer
1
2
3
Average
4
1
2
3
Average
4
1
2a
3a
Average
4a
1
2a
3a
Average
4a
5.95
5.69
6.59
6.08
5.31
2.45
2.57
3.27
2.76
1.99
0.747
0.654
1.476
0.959
0.402
2.94
2.79
3.49
3.07
2.19
3.3 16.1 <0.1
3.4 16.4 <0.1
3.2 16.3 <0.1
3.3 16.3 <0.1
3.5 16.2 <0.1
0.7 19.5 <0.1
1.0 19.0 <0.1
1.1 18.7 <0.1
0.93 19.1 <0.1
1.0 18.8 <0.1
<0. 1 20. 2 <0. 1
<0.1 20.2 <0.1
<0. 1 20. 2 <0. 1
<0. 1 20. 2 <0. 1
<0.1 20.2 <0.1
<0.1 20.4 <0,1
<0. 1 20.4 <0. 1
<0.1 20.4 <0.1
<0.1 20.4 <0.1
<0.1 20.4 <0.1
80.6
80.2
80.5
80.4
80.3
79.8
80.0
80.2
80.0
80.2
79.8
79.8
79.8
79.8
79.8
79.6
79.6
79.6
79.6
79.6
aSince the initial Orsat analyses indicated no combustion gases at this
 location, samples were not collected during Runs 2, 3, and 4.   Therefore,
 values from the first test were'used for the remaining tests.
                                  -  10  -

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         TABLE 2.3.  SULFUR OXIDES CONCENTRATIONS. AND EMISSION  RATES
Sampl ing
Location
Sample
Number
1980
Date
Stack Gas Flowrate
d scf m
Sulfur Dioxide
Concentration
ppm
Emission Rate
Ib/hr kg/hr
North
Kiln
South
Kiln
Bottom
Kiln
Dryer
1
1
1
1
1-10
1-10
1-10
1-10
6,830a
10,400a
4,130a
46,200a
36.5
7.52
<3. 65
13.2
2.49
0.781
< 0 . 1 5 1
6. 10
1.13
0. 354
<0.068
2.77
An average of the three particulate  runs  conducted during Condition 1.

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     Although the reproducibility of these values is




uncertain due to taking only single samples at each




location, the relative magnitude of sulfur dioxide




concentrations for each location is logical.  Sulfur




dioxide in the dryer stack originates primarily from




the waste heat exhaust of the kiln.  The waste heat




is withdrawn from the cooling zone, just downline




from the kiln firing zone.  Although particulate




could possibly settle out in the kiln and ductwork




leading to the dryer, sulfur dioxide,being a gas,




would be carried over.  Therefore, everything else being




equal,  the sulfur dioxide concentrations could probably




be expected to be about the same at the waste heat




intake in the dryer as in the firing zone.  However,




when the addition of dilution air is considered, it is




logical that the dryer emitted lower sulfur dioxide




concentrations than measured in the north kiln stack.




Given that the flowrate in the dryer stack was much




higher than any of the other stacks, the mass emission




of sulfur dioxide was highest at the dryer.  The sulfur




dioxide found at the north and south kiln is from a




combination of the sulfur in the clay and combustion




gases from the coal.  As expected, more sulfur dioxide




was detected at the north kiln than the south kiln




because the north kiln stack exhausts the actual burning




zone of the kiln,whereas the south kiln stack exhausts








                       - 12 -

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 the entrance to the burning zone in the tunnel.




 NITROGEN OXIDES




      A summary of nitrogen oxides results is




 presented in Table 2.4.   Concentrations are given




 in parts per million (ppm) and emission rates are in




 pounds per hour (Ib/hr)  and kilograms per hour (kg/hr).




      Single nitrogen oxides samples were taken at each




 location.  Concentrations ranged from 14.5 ppm at




 the dryer stack to 134  ppm at the north kiln.  Emission




 rates ranged from 2.12  Ib/hr (0.963 kg/hr) at the bottom




 kiln to 6.58 Ib/hr (2.99 kg/hr) at the north kiln.




 Since nitrogen oxides formation is proportional to




 temperature, it was  expected that the highest levels




 of nitrogen oxides would be found at the north kiln,




 which had the  highest stack gas temperatures of the




 four locations.  Similarly, the lowest concentration




 of nitrogen oxides was  found at the dryer stack,




 which was also the coolest of the four locations.




 PARTICLE SIZE




     Tables C-l and C-2 in Appendix C display the particle




size distribution at the north kiln under Conditions 1




and 2, respectively.  Both distributions are graphically




displayed in Figures 2.1 and 2.2, respectively. The




particle size distribution is nearly the same for both




conditions.  During Condition 1, approximately 50-




percent of the particles were 7.7 microns or less,
                         - 13  -

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            TABLE  2.4.  NITROGEN OXIDES  CONCENTRATIONS AND EMISSION RATES
Sampling
Loca t ion
Sample
Number
1980
Date
Stack Gas Flowrate
d sc f m
Nitrogen Oxides (as N02)
Concentration
ppm
Emission Rate
Ib/hr kg/hr
North 1 1-10
Kiln
South 1 1-10
Kiln
Bottom 1 1-10
Kiln
Dryer 1 1-10
6,830*

10,400a

4,130a

46 ,200a
134. 6.58 ' 2.99

40.2 3.00 1.36'

71.7 2.12 0.963.

14.5 4.81 2.18
An average of the three particulate tests conducted  during  Condition 1.

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 Effective
 par ti cle
 d iamet er
 (microns'
Ui

i
          0.3
          0.2.
          O.L
                           Condition
                           :     1
                Figure 2.1.   Particle
                 size distribution  -
                     north  kiln
              0.01  0.05 0.1 0.2   0.5   1
10
      20
30   40  !30   60  70   80
90
                                        95
                                                                                             93

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Effective
 particle  2 • °-
 d iameter
(microns)
           0.3
           0.2
           0.1
                             Condition
                                 2
Figure  2.2.    Particle  ijrr:
 size distribution  -
     north kiln
               0.01  0.05 0.1  0.2   0.5   1   2     5    10     20   30  40  50  60   70   80     90    95    98

                     Cumulative Percentage  Less Than  Indicated Diameter, by Weight

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whereas in Condition 2, 50-percent  of  the  particles




were 9.0 microns or less.




     Tables C-3 and C-4 in Appendix C  display the




particle size distributions  at  the  south kiln under




Conditions 1 and 2, respectively.    These  distributions




are graphically displayed in Figure 2.3.   In  comparing




these two conditions at this location,  it  is  found




that Condition 1  resulted in particle sizes  which




were somewhat evenly balanced over  the distribution




spectrum.  Particle sizes for Condition 2  were relatively




large in diameter.  During Condition  1, approximately




50-percent of the particles were  7.0  microns  or less,




while during Condition 2, approximately 76-percent




were 7.7 microns or larger.




     Particle sizing runs were  conducted at  the bottom




kiln and dryer locations, but due to  extremely low




particulate levels for these two  locations,  an accurate




determination of the size distribution was not possible.




VISIBLE EMISSIONS




     A summary of visible emissions is  found  in Appendix




B-3.  At the north kiln during  Condition 1,  opacities




ranged from 5 to 23-percent, based  on  6-minute averages.




For Condition 2, opacities range  from  16 to  43-percent,




also based on 6-minute averages.  For  the  south kiln




during Condition 1, opacities ranged  from  0  to 13-percent,









                         - 17 -

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Ef f ec t i ve
 Particle
Diameters
fe

oo
         0.2-
         0.1
                             Condition
                                  2
                                                                         Figure  2.3.  Particle
                                                                          size distribution -
                                                                              south  kiln
              0.01  0.05 0.1 0.2  0.5  1    2     5    10     20   30   40  50  60  70   80     90    95

                   Cumulative Percentage Less  Than Indicated  Diameter, by  Weight.

98   99
S9.8

-------
while Condition 2 opacities  ranged  from 7  to 20-percent,




both based on 6-minute  averages.




CLAY AND COAL SAMPLES




     Table 2.5 displays  the  results of  the analyses




for percent sulfur and  ash  in  the  coal  samples and




percent sulfur in the clay  sample.   During Condition




1,  the percent ash in the coal  samples  ranged from




4.1 to 4.4-percent, and  averaged 4.3-percent.  During




Condition 2, the ash content was 6.9-percent.   The




sulfur content of the coal  samples  acquired during




Condition 1 ranged from  0.70 to  0.82-percent,  and




averaged 0.76-percent.   The  sulfur  content was 0.64-




percent during Condition 2.  The sulfur content of




the clay sample was 0.04-percent.




     The ash content of  the  coal was 38-percent higher




for Condition 2 than the average of the three samples




acquired during Condition 1.   The  sulfur analysis revealed




a 19-percent decrease from  Condition 1  to  Condition 2.




     Since the clay sample  was  acquired from brick




cars which had passed through  the  dryer,  the sulfur




content of the "raw" clay is unknown.   However,  the




sulfur content of dried  bricks  is  insignificant with




respect to the sulfur content  of the coal.




     An example of calculations  and calibration data




used for all data reduction  are  presented  in Appendix




D and E, respectively.







                          -  19  -

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TABLE 2.5.  COAL AND CLAY SAMPLES, ASH AND SULFUR ANALYSES
Sample Type
Analysis
Percent Ash
Percent Sulfur
 Coal
Run 1




Run 2




Run 3
4.4




4.3




4.1
0.75




9.70




0.82
 Average
                  4.3
                       0.76
 Coal  Run  4
 Clay
                  6.9
                       0.64
                                         0.04
                           -  20 -

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       3.0  PROCESS DESCRIPTION AND OPERATION
 (Provided by Energy and Environmental Analysis, Inc.)

     Lee Brick and Tile started operation in 1946.

The new fully automated plant was built in 1976; this

facility utilizes one tunnel kiln and one dryer.

The plant operates 24 hours per day, seven days

per week, with a two to six week shutdown for plant

maintenance.  This shutdown period each year will

vary in length depending upon market conditions.

     The building brick process is a very steady opera-

tion without any typical variations in production.

The normal production rate for Lee Brick is 96,768

brick per day; the design maximum capacity is 116,928

brick per day, but this production rate is seldomly

used .

     The processes of interest in the building brick

industry are the drying and firing operations used to

"cure" the brick.  These two sources are being studied

as a single unit process.   There are no controls utilized

at Lee Brick, but this facility will provide data for

baseline emissions resulting from firing coals with

different ash content.


PROCESS DESCRIPTION

     Figure 3.1. demonstrates the basic steps utilized

in the production of building brick  at Lee Brick and

also shows locations of the various emission tests



                          -  21  -

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                             Common Clay
                              Stockpile
                                                 (Odd-size  Brick)
Particulate  Emissions
SO  Emissions
NOX Emissions
Visible Emissions
Particle Size
Dry Brick Samples
for Sulfur Content
Pulverized Coal  Samples
for Sulfur, Ash,  etc.
                              Dehacker

                                  4-
                              Packaging

                                  4-
                           Outside Storage
    Figure 3.1.  Lee  Brick  and Tile Co.,  Process Flow Diagram.
                                 -  22  -

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administered during the source test program.




     The clay is brought from the stockpile to the




pug mill on a belt conveyor.  Water is added to the




raw material and then mixed in the pug mill until




the proper consistency is reached.  The material is




then moved through the deaerating section of the pug




mill to remove any bubbles or air holes.  This




mixture is extruded in a continuous column onto a




conveyor which passes the clay column through the




cutting machine.  Odd-sized brick are returned to




the pug mill by another conveyor, where they are




reworked into the raw material.




     The unfired (green) brick continues on the conveyor




and may or may not be glazed  (during the testing program




no glazing was done).  The bricks are then stacked




on the kiln cars in two stacks by an automatic hacker.




Each kiln car (ware) holds 8,064 bricks (3 1/2" x 8"




x 2 1/4").




     From the loading area, kiln cars are moved to a




holding station, where they sit until they are moved




into the dryer.   There are always cars in the holding




station so that the drying and firing processes can




continue to operate during the night when the production




line is down or in case of a malfunction in the production




line during the day.








                        - 23  -

-------
     The tunnel dryer can hold up to  24 cars.  The




brick  remain in the dryer for 48-hours before




entering the kiln.  Waste heat is drawn from the




rapid cooling zone of the kiln and used to dry the




brick.




     The tunnel kiln can accommodate  21 cars. The




movement of the cars throughout the kiln is not




continuous; they are moved intermittently, or




indexed.  Each car is indexed one-half its length




every hour.  This allows the heat from the burners




to be directed between the cars and between the




stacks of brick on each car.




     The kiln is fired by a total of  47 burners.




Lee Brick uses a side-firing configuration.  The




kiln can use natural gas, No. 2 fuel  oil or coal




as its primary fuel.  Several crown burners ensure




even heating throughout the top of the kiln and




always fire gas, independent of the primary fuel.




The burners used for oil and gas are  the same;




however, the burner nozzles are different for the




two types of fuel.  Different burners, however, are




needed for coal-firing.  When firing with coal,




only half the number of side burners  are needed because




they fire across the entire width of  the kiln as




opposed to gas/oil firing.   The burners in the latter




case fire just half-way across the kiln, thus,











                        - 24 -

-------
necessitating opposing burners on each side of the




kiln.  During coal-firing, the first pair of side




burners are fired with gas to produce an effective




environment for coal combustion.  Currently, normal




coal-firing procedures call for the first five




burner pairs to use gas.  This procedure was estab-




lished due to earlier particulate source tests




accomplished during the burning of 8 1/2-percent ash




coal.  These early tests showed that five burner




pairs had to fire gas to enable the kiln's partic-




ulate emission rate to conform with state regulations.




     As the cars move through the firing zone, the




temperature is gradually increased, reaching a max-




imum of approximately 2000F.  After the firing zone,




the brick move into the cooling zone of the kiln.




Ambient air is drawn into the kiln, passed over the




hot bricks, and then this heated air is passed to the




dryer.




     When the fired brick come from the kiln, they are




moved to an automatic dehacker, which takes the brick




from the kiln cars and restacks them to marketable




bundles.  They are then packaged and taken to an




outside storage area.






PROCESS OPERATIONS




      The  purpose  of  this  test  program was to measure




emission  levels  from a  coal-fired kiln. There are









                         - 25  -

-------
three exhaust stacks from the kiln; the north and




south kiln stacks exhaust waste gases from inside




the kiln, while the bottom kiln stack pulls exhaust




gases from underneath the kiln.  In addition to the




sampling of the three kiln stacks, measurements




were also taken from the dryer exhaust stack.  A




stack extension with portholes had to be added to




the exhaust stack from the dryer. .




     Process conditions were carefully observed and




testing was performed during normal operating condi-




tions (7.26 tons/hr of brick + 0.42 tons/hr of coal);




the process was very steady with no interruptions in




production.  During the test, operating conditions




were monitored and recorded on process data sheets.




These data sheets are included in Appendix F.




     The following process parameters were monitored:




     (1)  Relative humidity in the dryer exhaust gas;




     (2)  Temperature of the dryer exhaust gas;




     (3)  Temperature of kiln waste heat entering the




           dryer;




     (4)  Maximum kiln temperature which controls the




           coal feeding rate;




     (5)  Internal kiln pressure; and,




     (6)  Natural gas flowrate.




     The natural gas flowrate was determined by taking




gas meter readings at the beginning and end of the








                         -  26  -

-------
day and averaging the total amount of gas over  the




length of the day.  Relative changes in .the  flowrate




could be observed on the gas flow recorder  (also  shown




on process data sheets); however, this instrument does




not give a good indication of the absolute  flowrates.




     Process monitoring began approximately  six hours




before the start of emission testing on January 9,  1980.




Simultaneous particulate emissions testing  on  the three




kiln stacks and dryer stack began around 3:00  pm  and




were concluded by 7:30 pm.  Low ash coal (4.3-percent ash)




was burned during this test period and no irregularities,




process changes, or malfunctions occurred during  this




tim.e.  The coal feeding rate was estimated  to  be  0.42




tons/hr.




     On January 10, 1980, process monitoring began  at




8:00 am; testing began at 11:00 am and ended at 6:30  pm.




The tests occurring this day included simultaneous




particulate emission testing on all four stacks,  nitrogen




oxides emission testing on all four stacks,  sulfur




oxides emission testing on all four stacks,  and a




particle size test on the north kiln stack.  The




absolute coal feeding rate was constant throughout




testing and had not been changed from the previous  day.




There was a slight change in the distribution  of  the




coal (2-percent increase in Zone 1 of the kiln) through-




out the day due to a malfunction of one of  the burners.









                         - 27 -

-------
The coal used this day was the same as the day before




(4.3-percent ash).




     Process monitoring began at 8:00 am on January




11, 1980.  Once again, the coal being fired was  low




ash coal.  Simultaneous particulate emissions testing




on all four stacks began around 11:00 am.  The only




other tests performed on this day were particle  sizing




tests on the dryer, bottom kiln,and south kiln stacks.




After the testing was completed, high ash coal




(6.9-percent ash) was fired to stabilize the system




for the following day's tests during high ash coal-




firing.  The coal feeding rate was increased by  S^percent




in Zone 1 of the kiln once the 6.9-percent coal  reached




the burne rs.                                     .




     During testing on January 12, 1980, high ash coal




was fired.   Process monitoring began at 9:00 am,while




testing began at 9:30 am.  At 10:30 am the coal  feeding




rate had to be increased by 2-percent in Zone 1  because




the maximum temperature in the kiln had dropped.   The



temperature dropped again at 2:30 pm, thus, the  flow -




rate was increased by another 2-percent.  As the




temperature continued to drop, the flowrate was




further increased.  Additional problems in maintaining




temperature were encountered at the end of the tests




so the operation was shut down after source testing




was completed at 5:00 pm.  Simultaneous particulate
                        - 28 -

-------
emission  tests on all four kilns began around 10:00




am.  The only other tests accomplished this day were




particle size tests on the south kiln stack and the




north kiln stack.




     Lee's head fireman stated that the minor increases




in the coal feed rate and the partial malfunction




of one burner are relatively insignificant process




upsets.   These problems should not cause any noticeable




changes  in the stack emissions.  The continuing temper-




ature drops during January 12 were not a problem by the




time the testing was finished, but if the trend had




continued, production variations would have occurred.




Since Lee was operating its kiln on only high ash coal




solely for EPA testing purposes, Lee shut down the opera-




tion once the testing was completed instead of trying to




correct  the problem.
                         -  29  -

-------
          4.0  LOCATION OF SAMPLING POINTS




     All four sampling locations were at roof level.




Each stack was accessed through two ports which were




90-degrees apart.  Additional physical parameters




for each stack are provided in Table 4.1. Sampling




locations and each of the traverse points with their




respective distances from the duct wall for the north




kiln, south kiln, bottom kiln, and dryer stack are




presented in Figures 4.1, 4.2, 4.3 and 4.4, respectively.




      All sampling locations  were  considered adequate




 in their original configuration,  with the exception




 of the  dryer stack.   An extension to the stack was




 needed  since the original stack height did not allow for




 sampling port placement which would meet the minimum




 upstream and downstream.distances from disturbances




 as required by EPA Method 1.   Originally, the traverse




 at the  dryer stack was to consist of 24 sampling




 points  per port.  Since Point 24  was too close to the




 stack wall, Point 23 was sampled  for twice the




 normal  duration.  Also, Points 1  and 2 could not be




 sampled because the  port nipples  were not flush with




 the stack wall and extended  into  the stack by 1.75-




 inches.  Therefore,  Point 3  was sampled for three times




 the normal duration.
                        - 30  -

-------
                           TABLE  4.1.   PHYSICAL PARAMETERS OF SOURCES
  Parameters
  North Kiln
   South Kiln
  Bottom Kiln
                                                                                Dryer
    Stack
Diameter (I.D.)
   Diameters
  Downs tream
(disturbances)
   Diameters
   Ups tream
(disturbances)
No. of sampling
  points per
   traverse
35.8 in(90.9cm)
     3.4
(fan coupling)
     1.3
(top of stack)
      20
35.9 in(91.2cm)
      3.4
(fan coupling)
      1.2
(top of stack)
       20
22.8 in(57.9cm)
      5.0
(bend in duct)
      1.0
(top of stack)
       20
 ,72.1 in(183cm)
       2.4
(reducing coupler)
      .0.5
  (top of stack)
        24

-------
                                                                         Elevation view
I

tjO
Point
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Distance
(Inche s )
0.5
1.4
2.4
3.5
4.6
5.9
7.3
8.9
10.9
13.9
21.9
24.9
26.9
28.5
29. 9
31.2
32.3
33.4
34.4
35.3
                                       Cross-sectional
                                            view
                                                               N
                                                              t
35 3/4" ..
               44 1/2"
                                                                                              Sampling
                                                                                                port
                                                                                            35  1/2"
                                                                                               Roof
                                                                                           84"  to  fan
                                                                                             Jcoupling
        Figure 4.1.  North kiln stack cross-section and sampling point locations (not to scale).

-------
                                                                           Elevation view
CO
Point
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Distance
(Inches)
0.5
1.4
2.4
3.5
4.6'
5.9
7.3
9.0
11.0
13.9
22.0
24.9
26.9
28.6
30.0
31.3
32.4
33.5
34.5
35.4
                                         Cross-sectional
                                              view
                                                                N
                                                                t
                                                                              -35  7/8'i.
                                                                                             43"
                                                                                               Sampling
                                                                                              • r  port
                                                                                             37"
                                                                                            \
                                                                                             84" to fan
                                                                                               coupling
         Figure 4.2. South kiln stack cross-section and sampling  point  locations  (not  to  scale).

-------
-p-
I
Point
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Distance
(Inches )
0.3
0.9
1.5
2.3
2.9
3.8
4.6
5.7
7.0
8.9
13.9
15.8
17.1
18.2
19.0
19.9
20.5
21.3
21.9
22.5
                                                                             Elevation  view
                                                                                 3.8 3/4"
                                       Cross-sectional
                                             view
                                                                            •B-
                                              22 3/4"-
24"
                                                                                                 Sampling
                                                                                                   port
                                                                                               55"
                                                              Roof
                                                       TT
     Figure 4.3.  Bottom kiln  stack
         locations   (not to scale).
cross-section and  sampling  point
                                                           60" to
                                                            Imanifold

-------
       Cross-sectional view
                                                Elevation view
Point
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
Distance
(Inches )
0.8
2.3
4.0
5.7
7.6
9.5
11.6
14.0
16.6
19.6
23.3
28.7
43.4
48.8
52.5
55.5
58.1
60.5
62.6
64.5
66.4
68.1
69.8
71.3
                                      18"
                                      39"
                                  133  1/2
                                                                      u
                                                     72 1/8"-
                                              1  3/4"
                                                         62"
                                                                        Sampli]
                                                                         port
   Figure 4.4.   Dryer stack cross-
section and sampling point locations
(not to scale).
                                     36
                                  -  35  -
                                               Reducer coupling
                                                                          Roof

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


     Exhaust gas sampling was conducted in accordance


with the procedures outlined in the U.S. Environmental


Protection Agency's (EPA) Standards of Performance  for


New S'tationary Sources Methods 1-7  (Federal Register,


40CFR60, December 23, 1971, as amended through August,18


1977).  An EPA Method 5 particulate sampling train  was


used at each location with the following modification:

               /R)
flexible Teflon^ tubing was used in the dryer and


bottom kiln sampling train to connect the filter


holder to the impinger series.


     During a preliminary velocity  traverse  conducted


prior  to  testing, each stack was divided  into  equal


annular areas at whose midpoints exhaust  gas  veloc-


ities  and  temperatures were measured,  in  accordance


with  EPA  Methods 1  and 2.   Velocity pressures  were


measured  at each sampling  point  using  an  S-type  Pitot


tube  and  inclined  0 to  10-inch water gauge  manometer.


Temperatures  were  measured  with  an  iron constantan


(Type-J)thermocouple attached  to  the Pitot tube and


to  a  calibrated  Omega  Engineering,  Model  199,  digital


pyrometer.   Exhaust gas  flowrates  and  a nozzle size


required  to  maintain isokinetic  sampling  rates were


calculated from the preliminary  velocity  traverse


data.   Stack gas moisture  content  was  determined


using the volumetric condensate  procedure outlined


  in EPA Method 4.



                        - 36 -

-------
PARTICULATE EMISSIONS




      Four particulate samples were extracted




simultaneously and isokinetically from each of




the four stack locations.  The tunnel dryer stack




was sampled for 192 minutes at three minutes per




point while the three kiln locations were each




sampled for 200 minutes at four minutes per point.





      Each  sampling  train (Figure  5.1)  consisted of a




 sharp,  tapered,  stainless  steel  sampling  nozzle;  a




 heated  glass  probe;  a  heated,  preweighed  110-mm Type




 A  glass-fiber filter;  flexible Teflon® tubing  at  the




 tunnel  dryer  and  bottom  kiln  only;  two  Greenburg-Smith




 impingers,  the first modified, the  second standard, each




 containing  100-ml of distilled water;  an  empty modified




 Greenburg-Smith, impinger serving  as a  dry trap; a modifi-




 ed  Greenburg-Smith  impinger  containing  approximately 300




 grams  of  silica  gel; a leakless  pump with vacuum gauge;




 a  calibrated  dry  gas meter equipped with  bimetallic




 inlet  and  outlet  thermometers; and, a  calibrated  orifice-




 type  flowmeter connected to  an inclined  0 to  10-inch




 water  gauge manometer.




      The  impinger trains were  immersed  in ice  baths to




 maintain  the  temperature in  the  last  impinger  at  70F or




 less.   All  sampling  train glassware was  connected by




 ground  joints, sealed  with stopcock grease,  and clamped




 to  prevent  leakage.
                        - 37 -

-------
00

i
         >1
         Iron/constantan thermocoup.
   fr
   p—-,
Heated
 glass
 probe
                      S-type Pitot
                          tube
              Inclined
             manometer
             Inclined
             manometer
                                               -Heated  110-mm glass-fiber filter

                                                                            •Thermometer
y                                             Refer  to  figure caption   I
                                         i	^.         below            I
                                              100-ml
                                             distilled
                                               water
                                 Thermometers
                                                                    Dry  200-300 grams
                                                                    trap    silica gel
                                                                  valve
                                                                          Vacuum
                                                                          gauge
                                                      Vacuum
                                                       pump
    Figure 5,1.   Particulate sampling train.  A  Teflon*5' extension  was  used, for
                         the bottom and dryer stack  sampling  locations.

-------
     The sampling train was checked for leaks before




each sample run in accordance with the requirement




that the initial leak rate shall not exceed 0.02 cubic




feet per minute at 15-inches of mercury vacuum.




     During the course of testing, the probe, thermo-




couple, and pitot tube assembly was moved to each sampling




point, the velocity pressures and stack gas temperature




were measured, and isokinetic sampling rates were




adjusted accordingly, using an orifice meter to indicate




instantaneous flowrates.  Throughout the test, the filter




temperature was maintained at 250+25F.




     Upon the conclusion of each particulate run, the




sampling train was again leak tested in accordance with




the requirement that the leak rate cannot exceed 0.02




cubic feet per minute at the greatest vacuum incurred




during the run.




     Following the leak check, each sampling train was




transferred to a clean-up area.  The volumes of the




itnpinger contents were measured and volume increases




recorded.  The solutions were placed in glass  (or




polyethylene) sample bottles with Teflon^-lined caps.




The silica gel was weighed to determine the weight gain




(as condensate).  The glass fiber filter was returned




to its original plastic petri dish and sealed.  The probe,




nozzle, and front-half of the glass-filter holder were




rinsed and brushed with acetone.  These rinsings were










                        - 39  -

-------
collected in separate glass sample bottles with  Teflon®-




lined caps.  The Teflon® tubing, the back-half of  the




glass—filter holder, and the impinger assembly were




initially rinsed with water, and placed in the same




sample bottle as the impinger contents.  These same




components were then rinsed with acetone and placed  in




separate glass sample bottles with Teflon®-lined caps.




Thus, four fractions were collected for each particulate




sample:




     (1)  acetone rinsings of probe, nozzle, and




          front-half of the glass-filter holder;




     (2)  110-mm type A glass-fiber filter;




     (3)  impinger contents and distilled water




          rinsings; and,




     (4)  acetone rinsings of the Teflon®



          extension, back-half of the glass-




          filter holder, impingers, and inter-




          connecting glassware.




Filterable particulate was the sum of Fractions  1  and  2,




and  total particulate the sum of Fractions 1,  2, 3,  and  4,




The  particulate weights, by fraction, are presented  in




Appendix G.




     In the laboratory, the liquid fractions were




measured volumetrically and transferred to tared




beakers.  Fraction 3 was then evaporated to  residue  at




105C and the particulate weight determined.  Fractions




1 and 4 were evaporated at room temperature  and  weighed




until constant.  Fraction 2 was desiccated at  room







                        - 40  -

-------
temperature and weighed until constant.  All weight




determinations were performed on an analytical  balance




having a sensitivity of 0.1 milligrams.




ORSAT ANALYSIS




     Simultaneously with each particulate  sample  run




at the north and south kiln locations,integrated  exhaust




gas samples were withdrawn in accordance with EPA Method




3.  The gas sample was extracted by a  pump  through a




probe, tubing, and condenser to a three-cubic-foot




Tedlar®bag.  Exhaust gas gradually filled  the bag at  a




controlled flowrate during the run.  At the end of each




run,  an aliquot of the gas in the bag  was  passed  through




an Orsat apparatus which measured the  concentrations  of




carbon dioxide, oxygen, and carbon monoxide.  Volume




decreases were noted after each gaseous component was




selectively absorbed from the aliquot  sample.   These




results were used to calculate the specific gravity of




the exhaust gas relative to dry air.






VISIBLE EMISSIONS



     Visible emissions were recorded  for  the duration of




each sample run on  the north and south kiln stacks.




Each of  these  observations was performed  in accordance




with EPA Method 9 by a certified observer  of visible




emissions.  Visible emissions were  not recorded for  the










                         - 41 -

-------
bottom kiln and dryer stacks since neither source




involved combustion.  In addition, the dryer exhaust




plume was mostly steam.




SULFUR OXIDES




     Sulfur oxides emissions were measured at  each



location in accordance with EPA Method 6.  The sampling




train  (Figure 5.2) consisted of a heated  stainless  steel




probe; Teflon® tubing; four midget impingers connected in




series and immersed in an ice bath,  the  first  impinger




containing 15-ml of 80-percent isopropanol,  the second




and third each containing 15-ml of 3-percent hydrogen




peroxide, and the fourth, dry; a  limiting orifice;  a




vacuum pump; and a dry gas meter.  A glass wool plug




inserted in the glass impinger connector  separated  the




first and second impingers.




      Sampling was conducted at approximately one-liter




per minute for 20-minutes.  A leak check  was performed




before and after each  test as per procedures outlined




in "An Alternative Method for Stack  Gas  Moisture




Determination", US EPA, August, 1978.  Following the   -




leak  test, the sampling train was purged  with  ambient




air for  15-minutes.  After the purge,  the hydrogen




peroxide was transferred along with  distilled  water




rinses to polyethylene sample bottles.
                          -  42  -

-------
                       Stack wall
                                     Glass wool
                  Heated stainless      plug
              _J    steel probe
                                                      Thermometer
      Glass
       woo 1
                                 80%     37° hydrogen
                             isopropanol   peroxide
Dry
trap
        Inclined
       manometer
                                                Fine
                                                valve
                                               Vacuum
                                                pump
                                                                  Vacuum
                                                                   gauge
                                                           Coarse
                                                           valve
Figure 5.2. Sulfur oxides  sampling  train..

-------
     In the laboratory, the hydrogen peroxide  solution




was diluted to 100-ml with distilled water.  A  20-ml




aliquot was then combined with 80-ml of  100-percent




isopropanol and two to four drops of thorin  indicator




This solution was then titrated with barium  perchlorate




to a pink endpoint and the results reported  as  sulfur




dioxide.




NITROGEN OXIDES




     Nitrogen oxides were measured at  each  location  in




accordance with EPA Method 7.  The sampling  train




 (Figure 5.3.) consisted of a stainless  steel  probe,




polyvinyl chloride tubing, a  three-way stopcock,  and  a




gas collection flask.  A 25-ml quantity  of  0.02-percent




hydrogen peroxide and 0.03-percent sulfuric  acid  reagent




was added to each flask.




     The glass collection flask was  then evacuated with




a  vacuum pump capable of drawing  a vacuum to within




3-inches of absolute barometric pressure.   The three-way



stopcock was opened until a vacuum gauge,  placed  in-line




between the stopcocks, indicated  a vacuum of approximately




27-inches of mercury within the flask.  The  stopcock  was




closed, the pump was turned off,  the vacuum  was observed




for one minute to assure there was no  leakage  into  the




flask, and the flask vacuum was recorded.   The stopcock




was then closed and the evacuated flask  was  connected




via tubing to the probe located in  the gas  stream.









                        - 44  -

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Stack
wa 11
              Stainless
                steel
                probe
           PVC
         tubing
 Pump
va Ive
                                           Flask
                    Glass wool plug
 Sample flask

Flask shield
                                      ab so rbing
                                      solution
                                                                           Vacuum
                                                                            pump
         Figure 5.3.  Nitrogen oxides sampling  train.

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     After the sampling line was purged with  stack  gas,




the stopcock was opened to allow the exhaust  gas  to




fill the evacuated flask.  Upon reaching equilibrium,




the stopcock was closed.  After the exhaust gas  sample




was collected, the flask was shaken for five  minutes  and




the reagent was allowed to remain in contact  with  the  gas




sample for approximately 24-hours to absorb the  desired




gas fractions.




     At the end of the absorbing period, the  flask  was




again shaken and the pressure of the gas sample  was




measured by connecting a U-tube mercury manometer  to  the




stoppered flask.  After recording the  final flask  pressure




and temperature, the sample solution was rinsed  from  the




flask with two 5-ml portions of distilled water  and




transferred to a polyethylene bottle.  This solution  was




then made basic with 1.0 N sodium hydroxide and  sealed




for transport to the laboratory.




     In the laboratory, the sample solution was  trans-




ferred to a tared beaker and evaporated to dryness  in




an oven at 105 C.  The dried residue was treated




successively with phenoldisulfonic acid solution,




distilled water, and sulfuric acid.  The resulting




solution was made basic by the dropwise addition of




ammonium hydroxide, transferred to a volumetric  flask,




and diluted to volume with distilled water.   The




absorbance of the solution at 420 nanometers  was measured,




and the concentration of nitrogen oxides, expressed as









                        - 46  -

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nitrogen dioxide, was determined by reference to a




calibration curve prepared from potassium nitrate




s tandards.




PARTICLE SIZE




     Particle sizing tests were conducted at all four




sampling locations.  A single 60-minute isokinetic




cascade impactor sample was obtained from the dryer and




bottom kiln stacks during Condition 1.  One 30-minute




sample, during each of Conditions 1 and 2, was obtained




from the north and south kiln stacks;  Figure 5.4 depicts




the particle sizing sampling train.  The sample was with-




drawn from a single point which represented the average gas




velocity profile of the stack.  The impactor was calibrated




by the manufacturer for unit particle densities of 1 g/cc




with constant shape and size.




     During the test, particles with equivalent aero-




dynamic diameters were collected on each stage of the




impactor at an optimal flowrate of approximately 0.75




acfm.  The impactor system was leak checked before the




sample run at 5-inches of mercury vacuum to insure a




leak rate less then 0.02 cfm.




     Each stage of the impactor was transferred




with acetone or distilled water rinses into




glass sample bottles.  Additionally, glass-fiber filters




associated with stages 1-7, plus the back-up stage were




transferred to their original petri dishes.
                      - 47 -

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co
                Stack
                wall
           Heated probe
                     3DO
                   Heated
                  particle
                   sizing
                  impactor
                        S-type Pitot tube
                                 Inclined
                               ^manometer
                                   Thermometers
              Inclined
             manometer
                                                        Silica
                                                         gel
                                                        Fine
                                                        valve
vacuum
 'pump
                                                                    Coarse
                                                                    valve
        Figure 5.4.  Particle  sizing  sampling  train,

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     In the laboratory, gravimetric analysis was




determined for each fraction in an identical manner




as corresponding fractions from the particulate runs.




The percentage of the total weight gain was determined




for each stage.




CLAY SAMPLES




     In conjunction with the Energy and Environmental




Analysis Inc. Project Manager, samples of  the  extruded




clay brick were obtained at the exit of the dryer, before




entering the kiln, for sulfur content determination.  One




brick was removed from each car as it left  the dryer




to represent those contained within the kiln during




the sulfur oxides tests.  Chips of approximately




equal size were acquired from each brick to form  a com-




posite sample.




     The brick composite was analyzed by Surface  Analysis




and Research, Inc. for percent sulfur by weight.




Sulfur was determined by the quantitative  energy




dispersion X-ray spectrographic method.  In this




procedure, the brick material was bombarded with




electrons to induce X-ray emissions.  These X-rays




were measured with an X-ray spectrometer and compared




to the spectra generated by sulfur standards to




quantitate the sulfur in the sample.




COAL SAMPLES




     At the beginning, middle, and end of  each particulate




run, pulverized coal grab samples were obtained to form  a
                      - 49 -

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composite sample from a Swindell air slide coal distributor




above the kiln.  The coal samples were collected in plastic




containers.  These coal samples were analyzed for




percent ash and sulfur by weight.  Ash content



was determined in accordance with ASTM Method D3174.




Sulfur content was determined by Surface Analysis and




Research, Inc. in accordance with the quantitative energy




dispersion X-ray spectrographic method.  Appendix  H




contains the analytical results reported by  Surface




Analysis and Research, Inc.
                        - 50 -

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