United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park NC 27711
EMB Report 78-CUS-8
February 1979
Air
Arsenic
Non-Ferrous Smelters
Emission Test Report
Phelps-Dodge Copper
Smelter
Douglas, Arizona
-------
EMISSION TESTING OF PHELPS-DODGE COPPER SMELTER
DOUGLAS, ARIZONA
TO
ENVIRONMENTAL PROTECTION AGENCY
Contract #68-02-2812
Work Assignment #15
April 10, 1979
By
Thomas Rooney
TRW
ENVIRONMENTAL ENGINEERING DIVISION
One Space Park, Redondo Beach, CA 90278
-------
CONTENTS
Figures iii
Tables iii
1. Introduction •. 1
2. Summary and Discussion of Results 2
3. Process Description 14
4. Location of Sampling Points 15
I
5. Sampling and Analytical Procedure 19
Appendices
A. Field and Laboratory Data 25
1. Traverse Point Location 25
2. Field Data Sheets 27
3. Analytical Data Sheets 42
4. Particle Sizing Analysis 54
5. Meter Box Calibration Data Sheets 61
B. Sample Calculations 71
C. Daily Activity Log. . . . ' 78
n
-------
FIGURES
Number Page
1 Inlet to calcine/roaster baghouse 16
2 Outlet from calcine/roaster baghouse 17
3 Calcine/roaster fugitive emission system 18
4 EPA method 5 particulate sampling train 21
5 Brinks impactor particle sizing system schematic 24
TABLES
Number Page
1 Inlet to Calcine/Roaster Baghouse Particulate Results 3
2 Outlet from Calcine/Roaster Baghouse Particulate Results .... 4
3 Inlet to Calcine/Roaster Baghouse Arsenic/SOp Results 5
4 Outlet from Calcine/Roaster Baghouse Arsenic/S02 Results .... 6
5 Particle Sizing Data Summary 7
6 Process Sample Analytical Results 7
7 Mass Spectrometry Analysis Results 8
-------
SECTION 1
INTRODUCTION
Under the Environmental Protection Agency's program for developing new
source performance standards, TRW performed emission tests at the Phelps-
Dodge copper smelter located in Douglas, Arizona. Testing was conducted May
1 through May 5, 1978.
The process tested was the calcine/roaster baghouse which collected the
fugitive emissions during the loading process of the train car. The train
car was used to transport the concentrate to the Reverb furnace operation.
The fugitive emission system operated on an intermittent basis.
Testing consisted of simultaneously sampling the inlet and outlet from
the calcine/roaster baghouse. Three arsenic/sulfur dioxide tests, three
participate tests and two particle sizing tests were performed at the bag-
house inlet. Three arsenic/sulfur dioxide tests, two particulate tests and
one particle sizing test were performed at the baghouse outlet. Each testing
location consisted of a 42 inch diameter horizontal duct with ports located
for vertical and horizontal sampling. These tests were coordinated by an
Environmental Protection Agency observer to assure simultaneous sampling
during the train car loading.
This report presents the results of the testing program. The following
sections of the report contain: a summary of the results, description of
sampling points, description of process, and sampling procedure with the la-
boratory analytical procedure. The appendices contain: field data, sample
calculations and daily activity log.
-------
SECTION 2
SUMMARY AND DISCUSSION OF RESULTS
The summary of results for calcine/roaster baghouse inlet and outlet are
presented in Tables 1-5. The particulate data are summarized in Tables 1 and
2. The arsenic data is presented in Table 3 and Table 4. Table 5 is a pre-
sentation of the particle sizing done at the above locations.
Two main problems were encountered in the testing program at the Phelps-
Dodge copper smelter. When the TRW personnel arrived at the site, the plant
was not operating due to mechanical malfunction. This problem caused a one
and a half day delay in the testing program.
The second problem was the intermittent process operation. The emissions
being measured were during the loading of train cars that transported the
calcine. The loading operation took two to five minutes and the process
occurred once every twenty-five to thirty minutes. The testing necessitated
one traverse point per loading operation due to the variability in loading
times. Stop watches were utilized to obtain accurate times. All data was
time weighted to achieve the averages. This was accomplished to account for
variability in loading times.
During the data reduction, the meter volume was back calculated to account
for sulfur dioxide that was removed th the impingers containing 10% hydrogen
peroxide. The back calculation for sulfur dioxide was accomplished in the
following order. First parts per million sulfur dioxide at standard condi-
tions was calculated, then parts per million was converted to a fraction by
dividing by 106. This number was added to one and the result multiplied by
volume of gas collected through the dry meter at standard conditions. The
result of multiplication yielded the actual gas volume collected at standard
conditions. Since SOg removal by the peroxide impingers does not reach the
dry gas meter, corrected values for dry gas meter volumes (at meter condi-
tions) found on the summary sheets will be slightly higher than those ob-
tained from the field data sheets.
-------
TABLE 1. INLET TO CALCINE/ROASTER BAGHOUSE PARTICIPATE RESULTS
RUN NUMBER
I DATE
II STACK PARAMETERS
Pst - Static Pressure, "Hg (mmHg)
Ps - Stack Gas Pressure, "Hg Absolute (mmHg)
J C02 - Volume I Dry
J 02 - Volume I Dry
I S02- Volume I Dry
I N2 - Volume I Dry
Ts - Average Stack Temperature °F (°C)
I H20 - I Moisture 1n Stack Gas, By Volume
As - Stack Area, ft2 (cm2)
Hd - Molecular Weight of Stack Gas, Dry Basis
Ms - Molecular Height of Stack Gas, Wet Basis
Vs - Stack Gas Velocity, ft/sec, (m/sec)
Qa - Stack Gas Volumetric Flow at Stack Conditions, ACFM (Nm3/m'n)
Qs - Stack Gas Volumetric Flow at Standard Conditions, DSCFM (Nm /m1n)
% EA - Percent Excess A1r
III TEST CONDITIONS
Pb - Barometric Pressure, "Hg (mmHg)
Dn - Sampling Nozzle Diameter. In. (mm)
T - Sampling Time, m1n
Vm - Sample Volume, ACF (m )
Np - Net Sampling Points
Cp - Pltot Tube Coefficient
Tm - Average Meter Temperature °F (°C)
Pm - Average Orifice Pressure Drop, "HgO (mmH^O)
Vic - Condensate Collected (Implngers and Gel), mis
AP - Stack Velocity Head " H.O (mmH,0)
IV TEST CALCULATIONS
Vw - Condensed Water Vapor, SDCF (Mm3)
Vm - Volume of Gas' Sampled at Standard Conditions, DSCF (Mm )
IHgO - Percent Moisture, By Volume
Vs - Stack Velocity, ft/sec (m/sec)
2 I - Percent Isoklnetlc
V ANALYTICAL DATA
A) Parttculates Front Half
Probe (mg)
Cyclone (mg)
Filter (mg)
Partlculates Front Half Total (mg)
grs/SOCF . (mg/m3)
Jhr. (kg/hr)
B) Partlculates - Condensables
Organic {mg)
grs/SDCF, (mg/m3)
J/hr, (kg/hr)
Inorganic (mg)
grs/SOCF, (mg/m3)
*/hr, (kg/hr)
C) Partlculates - Total Condensables (mg)
grs/SOCF. (mg/m3)
l/hr, (kg/hr)
D) Total Partlculates (mg)
grs/SOCF .(mg/m3)
J/hr, (kg/hr)
1
ENGLISH UNITS
-.37
25.57
0.0
20.0
.13
79.87
69.33
1.2
10.08
28.80
28.67
59.471
isqfifl.06
3U<:y3.57
4.735
2S.94
.250
55.58
63.933
12
.84
78.15
3.68
-
OS
.65
55.12
1.2
28.67
59.471
96.8
1.766
asn.lln
.0028
.726
.
.0533
13.843
.0561
14.568
1.8224
475.879
METRIC UNITS
-9.40
649.48
0.0
20.0
.13
79.87
20.7
1.2
.937
28.80
28.67
18.127
lolfl.m .
858.17
4.735
658.88
6.35
55.58
1.810
12
..184
25.6
93.47
13.8
in n
.02
1.5607
1.2
28.67
18.127
96.8
1467.3
4842.6
6309.9
4045.08
208.039
10.0
6.407
.329
190.58
122.112
6.284
200.58
128.518
6.613
6510.48
4171.511
214.652
2
ENGLISH UNITS
-.37
25.57
0.0
20.0
.21
79.79
73.9
0.0
10.08
28.80
28.80
57.034
M444.16
29153.37
4.735
25.94
.250
46.66
51.191
12
.84
83.88
3.82
R7
0
43.68
0.0
28.80
57.034
95.0
.
3.067
765.802
.002
.547
.097
'4.133
.099
24.680
3.166
790.482
METRIC UNITS
-9.40
649.48
0.0
20.0
.21
79.79
23.3
0.0
.937
28.80
28.80
17.384
977.17
U25.87
4.735
658.88
6.35
46.66
1.450
12
.84
28.8
97.03
.10
22.098
0
1.2870
0.0
28.80
17.384
95.0
472.4
8209.5
8681 .9
7018.512
347.618
6.2
5.012
.248
273.6
221.180
10.955
279.8
226.192
11.203
8961 .70
7244.704
358.207
3
ENGLISH UNITS
-.37
25.57
0.0
20.0
.18
79.82
65
0.6
10.08
28.80
28.74
"56.194
T>QRfi.l3
29035.67
4.735
25.73
.179
36.44
22.623
12
.84
78
.93
-
.85
.11
19.20
0.6
28.74
56.194
105.4
_
.
2.692
669.551
.038
9.533
.195
48.410
.233
57.943
2.925
727.494
METRIC UNITS
-9.40
649.48
0.0
20.0
.18
79.82
18.3
0.6
.938
28.80
28.74
17.128
uo2.78
822.54
4.735
644.14
4.55
36.44
0.641
12
.84
25.6
23.62
2.4
21.59
.00
0.5437
0.6
28.74
17.128
105.4
461.5
2888.6
3350.10
6161.670
303.927
47.7
87.732
4.327
242.22
445.503
21.974
289 92
533.235
26.302
3640 02
6694.90
•nn.229
AVERAGE
ENGLISH UNITS
-.37
25.57
0.0
20.0
.17
79.83
69.41
0.6
10.08
28.80
28.74
57.57
WH18.34
2938U.16
4.735
25.87
0.226
46.23
45.92
12
.84
80.01
2.81
-
0.89
0.253
39.33
0.6
28.74
57.57
99.07
.
.
2.508:
631.22
.014i
3.602
.1151
28.795
0.129<
32.397
2.638
663.616
METRIC UNITS
-9.40
649.48
0.0
20.0
.17
79.83
20.77
0.6
.937
28.80
28.74
17.70
986.36
832.30
4.735
653.97
5.75
46.23
•1.30
12
.84
26.67
71.37
5.43
22.61
.0067
1.113!
0.6
28.74
17.546
99.07
800.4
_
5313.57
6113.97
5741.923
.286.527
21.30
33.050
1.635
235.47
262.932
13.071
256 77
295.98
14.706
6037.04
301.233
-------
TABLE 2. OUTLET FROM CALCINE/ROASTER BAGHOUSE PARTICULATE RESULTS
RUN NUMBER
I DATE
II STACK PARAMETERS
PST - STATIC PRESSURE, "He (mHo)
Ps - STACK GAS PRESSURE, "Ho ABSOLUTE (MMHG)
I C02 - VOLUME I DRY
Z Oo - VOLUME X DRY
%SQ2- VOLUME Z DRY
% N2 - VOLUME J DRY
Ts - AVERAGE STACK TEMPERATURE °F (°C)
I H20 - 2 MOISTURE IN STACK GAS, BY VOLUME
As - STACK AREA, fr- (tr)
MD - MOLECULAR WEIGHT OF STACK GAS, DRY BASIS
Ms - MOLECULAR WEIGHT OF STACK GAS, WET BASIS
Vs - STACK GAS VELOCITY, FT/SEC, (M/SEC)
QA - STACK GAS VOLUMETRIC FLOW AT STACK CONDITIONS, ACFM (NM'/MIN)
Gs - STACK GAS VOLUMETRIC FLOW AT STANDARD CONDITIONS, DSCFM (NMVMIN)
J EA - PERCENT EXCESS AIR
III TEST CONDITIONS
PB - BAROMETRIC PRESSURE, "Ho (MMHG)
DN - SAMPLING NOZZLE DIAMETER, IN. (MM)
T - SAMPLING TIME, MIN
VH - SAMPLE VOLUME, ACF (n'i
Np - NET SAMPLING POINTS
CP - PITOT TUBE COEFFICIENT
TM - AVERAGE METER TEMPERATURE °F (°C)
PM - AVERAGE ORIFICE PRESSURE DROP, "I^O (MMM)
VLC - CONDENSATE COLLECTED (IMPINGERS AND GEL), MLS
AP - STACK VELOCITY HEAD "H20 (nMH20)
IV TEST CALCULATIONS
Vw - CONDENSED HATER VAPOR, SDCF (NM3)
VM - VOLUME OF GAS SAMPLED AT STANDARD CONDITIONS, DSCF
1 HjO - PERCENT MOISTURE, BY VOLUME
Ms - MOLECULAR WEIGHT OF STACK GAS, WET BASIS
Vs - STACK VELOCITY, FT/SEC (M/SEC)
% I - PERCENT ISOKINETIC
V ANALYTICAL DATA
A) PARTICULATES FRONT HALF
PROBE (MG)
CYCLONE (MG)
FILTER (MG)
PARTICULATES FRONT HALF TOTAL (MG)
GRS/SDCF, (MG/M3)
0/HR, KG/HR)
B) PARTICULATES - CONDENSABLES
QBSANJI (MO)
GRS/SDCF, (MG/M3)
f/HR, (KG/HR)
InosfiAiuc (MG)
GRS/SDCF, (MG/M3) •
/J/HR, (KG/HR)
f.) PABTICUIATFS - TOTAL CONDENSABLES (MG)
GRS/SDCF, (MG/M3)
#/HR, (KG/HR)
D) TOTAL PARTICULATES (MG)
GRS/SDCF, (MG/M3)
C/HR, (KG/HR)
1
ENGLISH
UNITS
.15
26.09
0.0
20.0
.09
79.91
73.3
1.3
9.62
28.80
28.66
59.729
34475.579
29017.84
4.735
25.94
.250
65
73.975
12
.84
76.15
4.07
.97
0.83
63.30
1 .3
28.66
59.729
93.6
.
.0031
.75
-
.0020
.503
.
.0396
9.847
.
.0416
10.349
.
.0447
11.107
1
METRIC
UNITS
3.81
662.69
0.0
20.0
.09
79.91
22.9
1.3
.894
28.80
28.66
18.205
976.45
882.014
4.735
658.88
6.35
65
2.069
12
.84
24.5
103.38
17.6
24.638
.02
1.7925
1 .3
28.66
18.205
93.6
11.3
.
1.2
12.5
6.973
.344
8.3
4.630
.228
162.54
90.677
4.469
170.84
95.307
4.698
183.34
102.280
5.042
2
ENGLISH
UNITS
.15
26.09
0.0
20.0
.19
79.81
65.0
0.6
9.62
28.80
28.73
61.581
35544.553
30984.647
4.735
25.94
.250
41.99
46.086
12
.84
80.25
3.78
.
1.05
0.25
39.59
0.6
28.73
61.581
87.7
-
_
.0150
3.982
-
.007
.186
-
.1770
46.989
-
.1777
47.175
.1927
51.158
METRIC
UNITS
3.81
662.69
0.0
20.0
.19
79.81
18.3
0.6
.894
28.80
28.73
18.770
1006.928
877.752
4.735
658.88
6.35
41.99
1.305
12
.84
26.8
96.01
5.3
26.670
.01
1.1210
0.6
28.73
18.770
87.7
27.2
_
11.3
38.5
34.344
1.808
1.8
1.605
.085
454.3
405.263
21.329
456.10
406.868
21.414
496.60
441.212
23.222
3
ENGLISH
UNITS
METRIC
UNITS
AVERAGE
ENGLISH
UNITS
.15
26.09
0.0
20.0
0.14
79.86
69.15
0.95
9.62
28.80
28.70
60.66
35012.052
3175.246
4.735
25.94
.250
53.50
59.581
12
.84
78.2
3.93
1.01
0.54
51.445
0.95
28.70
60.66
90.65
_
_
0.009
2.369
-
.0013
.3445
-
0.1083
28.418
-
0.1096
28.763
-
0.1187
31.133
METRIC
UNITS
3.81
662.69
0.0
20.0
0.14
79.86
20.6
0.95
.894
28.80
28.70
18.49
991 .868
906.05
4.735
658.88
6.35
53.50
1.687
12
.84
25.65
99.70
11.45
25.654
0.015
1.457
0.95
28.70
18.49
90.65
19.25
6.25
25 5
20.6405
1.076
5.05
3.1175
.1564
308.42
247.97
12.899
313.47
251.088
13.056
388.97
271.746
14.132
-------
TABLE 3. INLET TO CALCINE/ROASTER BAGHOUSE ARSENIC/SO- RESULTS
RUN NUMBER
1 1 STACK PARAMETERS
PST - STATIC PRESSURE, "Ho (rwHo)
Ps - STACK GAS PRESSURE, "HG ABSOLUTE (MMHG)
I COj - VOLUME Z DRY
% 0, - VOLUME I DRY
X SOj' VOLUME I DRY
I N2 - VOLUME I DRY
Ts - AVERAGE STACK TEMPERATURE °F (°C)
I H20 - I MOISTURE IN STACK GAS, BY VOLUME
As - STACK AREA, FT (M )
MD - MOLECULAR WEIGHT OF STACK GAS, DRY BASIS
Ms - MOLECULAR WEIGHT OF STACK GAS, WET BASIS
Vs - STACK GAS VELOCITY, FT/SEC, (M/SEC)
OA - STACK GAS VOLUMETRIC FLOW AT STACK CONDITIONS, ACFM (NM'/MIN)
Os - STACK GAS VOLUMETRIC FLOW AT STANDARD CONDITIONS, DSCFM (NMVMIN)
I EAi- PERCENT EXCESS AIR
III TEST CONDITIONS
PB - BAROMETRIC PRESSURE, "Ho (MMHG)
DN - SAMPLING NOZZLE DIAMETER, IN. (NM)
T - SAMPLING 1 1Mb, MIN
VM - SAMPLE VOLUME, ACF (M')
NP - NET SAMPLING POINTS
CP - PITOT TUBE COEFFICIENT
TM - AVERAGE METER TEMPERATURE °F (°C)
PM - AVERAGE ORIFICE PRESSURE DROP, "t^O (MMHnO)
VLC - CONDENSATE COLLECTED (IMPINGERS AND GEL), MLS
&p - STACK VELOCITY HEAD "I^O (MM^O)
IV TEST CALCULATIONS
Vw - CONDENSED WATER VAPOR, SDCF (NM3) 7
VM - VOLUME OF GAS SAMPLED «T STANDARD CONDITIONS, DSCF (NnJ)
% ^ • PERCENT MOISTURE, BY VOLUME
Ms - MOLECULAR WEIGHT OF STACK GAS, WET BASIS
Vs - STACK VELOCITY, FT/SEC (M/SEC)
% I - PERCENT ISOKINETIC
V ANALYTICAL DATA
A) ARSENIC FRONT HALF
PROBE (MG)
CYCLONE (MG)
FILTER (MG)
ARSENIC FRONT HALF TOTAL (MG)
PPM, (MG/M')
PHR, (KG/HR)
B) ARSENIC - IMPINGER COLLECTION
IMPINGER #1. 2,3 (MG)
PPM, (MG/M3)
fl/HR, (KG/HR)
IflPIHGER-K 1,5. 6 (MS)
PPM, (MG/M^)
#/HR, (KG/HR)
r.) ARSENIC - IMPINGER TOTAL (MG)
PPM, (MG/M )
film, (KG/HR)
D) TOTAL ARSENIC (MG)
PPM, (MG/M3)
S/HR, (KG/HR)
D EfflLa^ (MG)
PPM
GRS/SDCF, (MG/KT)
If/at, (KG/HR)
1
ENGLISH
UNITS
5/3/78
(-).IS
26.09
0.0
20.0
.13
79.87
76.3
.5
10. oa
28.80
28.75
57.483
34765.72
29697.02
4.735
25.94
.245
54.92
61.117
12
.84
76.3
3.82
.91
.26
52.83
.5
28.75
57.483
97.4
"
.0003
.0001
.0186
.0066
-
.0186
.0066
.0189
.0067
1.5644
408.919
METRIC
UNITS
5/3/78
3.81
662.68
0.0
20.0
.13
79.87
24.6
.5
.937
28.80
28.75
17.521
984.86
841.28
4.735
658.88
6.22
54.92
1.73
12
.84
24.6
97.03
5.6
23.114
.01
1.50
.5
28.75
17.521
97.4
.0007
"
.0005
.0012
.0008
.0000
.0870
.0581
.0030
.
-
.0870
.0581
.0030
.0882
.0589
.0031
5356.23
1343.37
3582.55
185.619
2
ENGLISH
UNITS
V1/78
-.37
25.57
0.0
20.0
.21
79.79
72.4
.8
10.08
28.80
28.72
59.433
11045.08
322019.27
4.735
25.94
.245
49.08
52.049
12
.84
81.5
3.74
,945
.35
44.53
.8
28.72
59.433
91.7
-
.0269
.0096
.0442
.0158
-
.0442
.0158
.0711
.0254
2.5080
657.299
METRIC
UNITS
5/V78
-9.39
649.47
0.0
20.0
.21
79.79
22.5
.8
.937
28.80
28.72
18.115
inin.?7
856.13
4.735
658.88
6.22
49.08
1.47
14
.84
27.5
95.00
7.4
24 .003
.01
1.26
.8
28.72
18.115
91.7
.105
•
.0002
.1057
.0838
.0044
.174
.1379
.0072
.174
.1379
.0072
.2797
.2217
.0115
7238.10
2153.71
5743.62
298.365
3
ENGLISH
UNITS
5/5/78
-.37
25.36
0.0
20.0
.18
79.82
65.2
2.0
10.08
28.80
28.58
52.943
32019.93
26738.89
4.735
25.73
.185
38.27
74.783
12
.84
78.3
1.01
.75
.44
20.99
2.0
28.58
52.943
110.0
-
-
.1343
.0424
.0701
.0221
•
.0701
.0221
.2044
.0645
2.1342
494.324
METRIC
UNITS
5/5/78
-9.39
644.14
0.0
20.0
.18
79.82
18.5
2.0
.938
28.80
28.58
16.137
907.08
757.47
4.735
653.54
4.69
38.27
.702
12
.84
25.7
25.65
9.3
19.05
.01
.59
2.0
28.58
16.137
110.0
.245
.004
.249
.4188
.0192
.130
.2186
.0100
.130
.2186
.0100
.3790
.6374
.0293
2903.28
1832.70
4887.54
224.387
AVERAGE
ENGLISH
UNITS
-.20
25.67
0.0
20.0
.17
79.83
71.3
1.1
10.08
28.80
28.68
56.620
34243.58
2885.81
4.735
25.87
.225
47.62
45.913
12
.84
78.7
2.85
.868
.350
39.45
1.1
28.68
56.620
99.7
-
-
.
.0538
.017
,
.0443
.0149
.0443
.0149
.0981
.0322
2.0689
520.181
METRIC
UNITS
-4.99
652.10
0.0
20.0
.17
79.83
21.9
1.1
.938
28.80
28.68
17.258
970.07
818.29
4.735
657.10
5.71
47.62
1.30
12
.84
25.93
72.56
7 43
22.056
.01
1.12
1.1
28.68
17.258
99.7
.117
-
.002
.119
.1678
.0079
.130
.1382
.0067
.130
.1382
.0067
.2490
.3060
.0146
5165.87
1776.59
4737.90
236.124
-------
TABLE 4. OUTLET FROM CALCINE/ROASTER BAGHOUSE ARSENIC/S02 RESULTS
RUN NUMBER
1 1 STACK PARAMETERS
PST - STATIC PRESSURE, "Ho (MMHG)
Ps - STACK GAS PRESSURE, "Ho ABSOLUTE (MMHG)
I C02 - VOLUME 1 DRY
I Oj - VOLUME 1 DRY
I SOV VOLUME I DRY
X N2 - VOLUME % DRV
Ts - AVERAGE STACK TEMPERATURE °F (°C)
% H20 - X MOISTURE IN STACK GAS, BY VOLUME
As - STACK AREA, FT (M )
MD - MOLECULAR HEIGHT OF STACK GAS, DRV BASIS
Ms - MOLECULAR HEIGHT OF STACK GAS, HET BASIS
Vs - STACK GAS VELOCITY, FT/SEC, (M/SEC)
DA - STACK GAS VOLUMETRIC FLOW AT STACK CONDITIONS, ACFM (NMVPIN)
Os - STACK GAS VOLUMETRIC FLOW AT STANDARD CONDITIONS, DSCFM (NMVMIN)
X EA>- PERCENT EXCESS AIR
III TEST CONDITIONS
PB - BAROMETRIC PRESSURE, "Ho (MMHG)
DN - SAMPLING NOZZLE DIAMETER, IN. (MM)
T - SAMPLING 1 1Mb, MIN
VM - SAMPLE VOLUME, ACF (M3)
NP - NET SAMPLING POINTS
CP - PITOT TUBE COEFFICIENT
TM - AVERAGE METER TEMPERATURE °F (°C)
Pn - AVERAGE ORIFICE PRESSURE DROP, "H20 (MnH20)
VLC - CONDENSATE COLLECTED (I«P1NGERS AND GEL), MLS
£P - STACK VELOCITY HEAD "H20 /HR, (KG/HR)
IMPINGER •# 1.5. 6 (MG)
PPM, (MG/M )
#/HR, (KG/HR)
C) ARSENIC - IMPINGER TOTAL (MG)
PPM, (MG/M3)
#/HR, (KG/HR)
D) TOTAL ARSENIC (MG)
PPM, (MG/M3)
*/HR, (KG/HR)
E) TOTAL SCV. (MG)
PPM
GRS/SDCF, (MG/n )
#/HR, (KG/HR)
1
ENGLISH
UNITS
5/3/78
+ .15
26.09
0.0
20.0
.08
79.9
73.3
1.0
10.20
28.86
28.69
59.706
36540.07
31539.3
4.735
25.94
.250
65.0
75.929
12
.84
73.33
4.14
.98
.68
66.13
1.0
28.69
59.706
96.5
-
.0082
.0030
-
.0565
.0208
"
"
.0565
.0208
.0647
.0283
1.0462
282.629
METRIC
UNITS
5/3/78
3.61
662.69
0.0
20.0
.08
79.9
23.0
1.0
.946
28.86
28.69
16.198
1039.55
893.1
4.735
658.88
6.35
65.0
2.15
12
.84
23.0
105.16
14.4
24.892
.02
1.67
1.0
28.69
18.198
96.5
.037
-
.011
.048
;0256
.0014
.330
.1762
.0094
.330
.1762
.0094
.3780
.2018
.0108
4480.73
898.45
2396.03
128.-293
2
ENGLISH
UNITS
W78
t.15
26.09
0.0
20.0
.19
79.8
65.4
.9
10.20
28.86
28.71
60.745
37175.94
32296.4
4.735
25.94
.250
41.7
49.504
12
.84
77.5
4.24
1.02
.37
42.80
.9
28.71
60.745
95.0
-
-
-
.
.0217
.0082
.0793
.0299
-
"
.0793
.0299
.1010
.0361
-
2.2535
623.360
METRIC
UNITS
5/1/78
3.81
662.69
0.0
20.0
.19
79.6
18.6
.9
.948
28.86
28.71
18.515
1057.63
914.5
4.735
658.68
6.35
41.7
1.40
12
.64
25.3
107.70
7.9
25.908
.01
1.21
.9
28.71
18.515
95.0
.047
- .035
.082
.0676
.0037
.300
.2474
.0136
-
.2474
.0136
.3820
.3151
.0173
6237.77
1935.15
5160.76
282.960
3
ENGLISH
UNITS
5/5/78
*.15
25.88
0.0
20.0
.15
79.8
78.7
1.4
10.20
26.86
28.65
62.122
38016.66
31780.9
4.735
25.73
.250
39.6
44.312
12
.84
76.3
3.79
1.03
.54
38.00
1.4
28.65
62.122
90.0
-
-
-
.0506
.0186
.
.0191
.0071
-
"
.0191
.0071
.0697
.0259
1.7890
486.97
METRIC
UNITS
5/5/78
3.81
657.35
0.0
20.0
.15
79.8
25.9
1.4
.948
28.86
28.65
18.935
1081.61
899.9
4.735
653.54
6.35
39.8
1.25
12
.84
24.6
96.27
11.5
26.162
.02
1.07
1.4
28.65
18.935
90.0
.020
.150
.170
.1579
.0085
.064
.0595
.0032
.064
.0595
.0032
.2340
.2174
.0117
4405.9
1536.27
4096.99
221.049
AVERAGE
ENGLISH
UNITS
t.15
26.02
0.0
20.0
.14
79.8
72.5
1.1
10.20
28.86
28.68
60.857
37244.69
31872.2
4.735
25.87
.250
48.8
56.581
12
.84
75.71
4.06
1.01
.53
48.976
1.10
28.68
60.86
93.8
-
. -
.0268
.0100
.0516
.0193
"
.0516
.0193
.0785
.0293
-
1.6962
464.32
KETRIC
UNITS
3.61
660.91
0.0
20.0
.14
79.8
22.5
1.1
.948
28.86
28.68
18.549
1059.59
902.5
4.735
657.10
6.35
46.8
1.60
12
.84
24.3
103.04
11.3
25.654
.017
1.383
1.10
28.68
18.55
93.8
.0347
-
.065
.100
.0837
.0045
.231
.1610
.0087
-
.231
.1610
.0087
.3313
.2447
.0133
5041.47
1456.62
3884.59
210.77
-------
TABLE 5. PARTICLE SIZING SUMMARY
(LOCATION, PHELPS-DODGE, DOUGLAS, ARIZONA)
LOCATION
Inlet
Inlet
Outlet
TEST
#1
#2
#1
PARTICLE SIZE
>5y 3-5y
70.0 10.0
64.0 12.0
33.0 11.0
DISTRIBUTION %
l-3y
14.0
17.0
25.0
-------
TABLE 7
MASS SPECTROMETRY ANALYSIS RESULTS
PREPARED BY
COMMERCIAL TESTING & ENGINEERING CO.
14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 928 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 313 726-8434
Reply tO INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Mr. Tony Eggelston ^Nl^^
TRW Mmi^m.
One Space Park 1"~'™
Bldg. R4, Room 2158
Redondo Beach, CA 90278
P. O. No.: 38866JC8E
Sample No.: DO-P-2 5/4/78
e
Date: July 19, 1978
Analyst: S. Sweeney
IAD No.: 97-B371-130-15
CONCENTRATION IN pg/ml
ELEMENT CONC.
Uranium
Thorium
Bismuth ±0.02
Lead 0.2
Thallium 10.01
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium 0.06
Cesium
Iodine 0.02
Tellurium
Antimony
Tin <0.01
Indium STD
Cadmium <0.009
Silver
Palladium
Rhodium
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
0.06.
0.02
0.008
0.04
0.02
0.02
0.03
1
<0.004
0.2
*6
0.2
0.02
3
0.07
0.05
ELEMENT
Vanadium
Titanium
Scandi urn
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.002
0.3
<0.006
4
1
0.2
1
0.2
2
0.7
0.5
MC
=2
NR
NR
NR
0.03
<0.001
NR
*Heterogeneous
NR - Not Reported
All elements not .detected <0.004 yg/ml
Approved:
MC - Major component Note: Partlculate matter was contained Kit ttfe^sample. Sample was shaken
and an anquot taken for analysis. r
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 928 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 726-8434
Reply tO INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Mr. Tony Eggelston ^M^^
TRW JUiSm.
One Space Park • """"•
Bldg. R43 Room 2158
Redondo Beach, CA 90278
P.O. No.:' 38866 JC8E
Sample No.: DO-P-2 5/11/78
Date: July 18, 1978
Analyst: S. Sweeney
IAD No.: 97-B371-130-15
CONCENTRATION IN y.g/ml
ELEMENT CONC.
Uranium 0.02
Thorium
Bi smuth
Lead 0.02
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
-v
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium 0.003
Lanthanum 0.003
Barium 0.04
Cesium
Iodine
Tellurium
Antimony
Tin
Indium STD
Cadmi urn
Silver <0.001
Palladium
Rhodium
i r\
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttri urn
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
0.01
<0.002
0.002
0.02
<0.001
<0.004
0.02
<0.001
0.07
0.1
0.04
<0.003
0.3
0.003
0.004
ELEMENT
Vanadium
Titanium
Scandi urn
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
CONC.
<0.001
0.01
<0.002
2
0.2
0.009
2
0.1
0.4
0.05
0.2
0.4
-0.4
NR
NR
NR
<0.001
0.002
NR
NR - Not Reported
All elements not detected
MC — Major Component
=0.002 ug/rnl
Approved:
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 238 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 6060) • AREA CODE 319 798-8434
Reply tO INSTRUMENTAL ANALYSIS DIVISION. 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 60401, PHONE: 303-278-9521
To: Mr. Tony Eggelston J\
TRW Mm\
One Space Park
Bldg. R4, Room 2158
Redondo Beach, CA 90278
P. 0. No.: 38866JC8E
Sample No.: DI-P-2
ELEMENT CONC.
Uranium 0.07
Thorium
Bismuth 0.005
Lead Q.02
Thallium
Mercury MR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
£> Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
5/4/78
CONCENTRATION
ELEMENT CONC.
Terbi urn
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium Q.02
Cesium
Iodine 0.005
Tellurium
Antimony 0.007
Tin <0.005
Indium STD
Cadmi urn
Silver 0.009
Palladium
Rhodium
11
k
i»Ot
Date: July
Analyst: $
18, 1978
. Sweeney
IAD No.: 97-B371-130-15
IN yq/ml
ELEMENT .
Ruthenium
Molybdenum
Niobium
Zirconium
Yttri urn
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
-
CONC.
0.02
*0.01
<0.008
0.004
0.01
<0.001
0.01
0.03
0.01
<0.002
0.002
0.1
0.1
*3
*0.5
0.2
0.003
*1
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.002
0.03
<0.002
0.4
0.06
0.1
0.4
0.2
2
0.03
0.3
0.07
=0.2
NR
NR
NR
0.002
<0.001
NR
NR - Not Reported
All elements not detected
MC — Major Component
<0.002 yg/ml Approved:
*Heterogeneous
-------
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 9SB NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 736-8434
Reply tO INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Mr. Tony Eggleston ^1
TRW JUk
One Space Park
Bldg. R4, Room 2158
Redondo Beach, CA 90278
P. 0. No.: 38866JC8E
Sample No.: AC-P-2
ELEMENT CONC.
Uranium 0.04
Thorium
Bismuth Q.003
Lead Q.02
Thallium
Mercury NR
Gold
Platinum
Iridium o.l
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
NR - Not Reported
All elements not detected
CONCENTRATION
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymi urn
Cerium 0.003
Lanthanum 0.003
Barium o.l
Cesium
Iodine
Tellurium
Antimony
Tin *0.01
Indium STD
Cadmium <0.002
Silver 0.002
Palladium
Rhodi urn
12
<0.002 pg/ml
*Hotov
k
I»O»
IN yg/ml
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttri urn
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
Approved: X*'
•nnanonnc A
Date: July 18, 1978
Analyst: s. Sweeney
IAD No.: 97-B371-130-15
CONC.
0.03
0.003
0.004
<0.001
0.04
<0.001
0.009
0.5
0.2
<0.001
0.02
0.1
0.09
<0.002
0.7
0.01
0.03
7/J/t,
ELEMENT
Vanadium
Titanium
Scandi um
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
<0.001
<0.03
<0.001
2
0.1
0.02
0.8
0.3
0.5
0.07
0.3
1
-0.05
NR
NR
NR
<0.001
0.002
NR
^y
^A
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 238 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 736-8494
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Mr. Tony Eggleston • .^I^L
TRW AilEk
~ — r\ 1 SiNCt I*O«
One Space. Park
Bldg. R4, Room 2158
Redondo Beach, CA 90278
P. 0. No.: 38866JC 8E
Sample No.: DI-P-2
Date: July 18, 1978
Analyst: S. Sweeney
IAD No.: 97-B371-130-15
CONCENTRATION IN yg/ml
ELEMENT CONC.
Uranium 0.04
Thorium
Bismuth
Lead O.006
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmi urn
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymi urn
Cerium
Lanthanum
Barium1 0.02
Cesium
Iodine
Tellurium
Antimony
Tin
Indium STD
Cadmium O.001
Silver <0.001
Palladium
Rhodium
It
ELEMENT .
Ruthenium
Molybdenum
Niobium
Zirconium
Yttri urn
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
!
CONC.
0.004
0.005
0.002
0.004
0.004
-------
SECTION 3
PROCESS DESCRIPTION
14
-------
SECTION 4
LOCATION OF SAMPLING POINTS
Inlet to Calcine/Roaster Baghouse
Samples from the inlet to the calcine/roaster baghouse were taken from a
43" diameter horizontal duct located approximately 25 feet above the ground.
Sampling ports on the bottom and side allowed for vertical and horizontal tra-
verses. The nearest upstream disturbance was 24 feet (8 diameters) away from
the sampling point. The nearest downstream disturbance was the intake to the
baghouse located 7 feet (2 diameters) away from the sampling point. Twelve
traverse points .were selected for particulate and arsenic/sulfur dioxide tests0
Outlet from Calcine/Roaster Baghouse
Samples from the outlet of the calcine/roaster baghouse were taken from a
42" diameter horizontal duct located approximately 35 feet above the ground.
Sampling ports on the bottom and side allowed for vertical and horizontal tra-
verses. The nearest upstream disturbance was 42 (12 duct diameters) away from
the sampling point. The nearest downstream disturbance was a 90° bend located
28 feet (8 duct diameters) from the sampling point. Twelve traverse points
were utilized for particulate and arsenic/sulfur dioxide tests. Figure 2 is a
schematic of the sampling location.
15
-------
Tra-
verse
point
loca- Fraction of
tions stack I.D.
1
2
3
4
5
6
.044
.146
.296
.704
.854
.956
Distance
from inside
wall (in)
l.«7
6.30
12.72
30.28
36.70
41.13
TO
«—
BAGHOU3K
CALCINE/ROASTER
FUGITIVE EMISSION
SYSTEM
Figure 1 . Inlet to calcine/roaster baghouse.
16
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TRAVERSE POINT LOCATIONS
42
Tra-
verse
point
loca-
tions
.1
2
3
4
5
6
Fraction of
stack I.D.
.044
.146
.296
.704
.854
.956
Distance
from inside
wall (in)
1.83
6.15
12.43
29.57
35.85
40.17
CALCINE//
ROASTER
BAGHOUSE
Figure 2. Outlet from calcine/roaster baghouse.
17
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DOUGLAS
ROASTERS
oo
I I I I • I
•SAMPLE
POINT
INLET
I
CALCINE DISCHARGE HOODS & DUCTS
BAGHOUSE
TO STACK
SAMPLE
POINT
OUTLET
CYCLONE
Figure 3 . Calcine/roaster fugitive emission system.
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SECTION 5
SAMPLING AND ANALYTICAL PROCEDURE
A) Particulate Sampling
Particulate sampling was performed according to EPA Method 5, as revised
in the Federal Register, Volume 42, Number 160, Thursday, August 18, 1977.
Figure 4 is a diagram of the sampling train used for the particulate tests.
Before each test a velocity traverse of the stack was done to determine
the average stack temperature and velocity pressure. The velocity traverse
was done according to EPA Methods 1 and 2. A grab sample of the stack gas was
taken and analyzed with a Fryrite apparatus for C02. Before the first test at
each location the moisture content of the gas stream was estimated by either
condensation in impingers as in EPA Method 4, or by wet and dry bulb thermo-
meter if the stack gas temperature was below 120°F.
The particulate samples were taken at traverse points at the center of
equal areas within the stack. The number of travers points was determined by
the number of duct diameters upstream and downstream from the nearest flow dis-
turbances. The sampling rate was adjusted to isokinetic conditions using a
nomograph which had been set based on the preliminary velocity traverse data,
and moisture estimate.
The sampling time per traverse point varied since the baghouse operated
only when calcine was being pulled from the roaster building. Loading time
for the train varied and one point was sampled per loading.
Leak checks of the sampling train were done at the beginning of each test,
just before the sampling port change, and at the end of the test. At the end
of each test the sampling train was inspected for cracked or broken glassware,
and to assure that the filter remained intact.
Sample Recovery
After completing the particulate test the sampling probe was removed from
the sampling train, the nozzle wiped off, and the probe rinsed into a clean
sample container with acetone, using a nylon brush with a teflon handle to
scrub particulates out of the probe. The filter holder of the sampling train
was then capped and the filter holder and impingers were removed to the mobile
laboratory for sample recovery.
The collected particulate sample was recovered and placed in four contain-
ers. The particulate filter was folded and placed in a polyethylene jar, and
the jar was labelled and sealed. The acetone rinse of the nozzle, probe liner,
and front half of the filter was placed in a 250 ml glass jar with teflon lined
19
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lid, labelled and sealed. The impinger solutions were measured, and placed in
a glass jar along with a water rinse of the impingers. The front half of the
filter holder, first three impingers, and connecting glassware were rinsed with
acetone. This rinse was placed in a glass jar with a teflon lid liner, sealed
and labelled.
Analysis
The front half aceton rinse and back half acetone rinse were placed in
tared glass beakers and evaporated. The impinger solutions and water rinse
were extracted with ether and chloroform, and the fractions .placed in separate
tared beakers and evaporated. Aqueous fractions were dried on a steam bath.
The filter and tared beakers were then placed in a dessicator until they reach-
ed a constant weight and weighed to a tenth of a milligram.
B) Arsenic/Sulfur Dioxide Sampling
The sampling train used for arsenic/sulfur dioxide collection consisted
of an EPA method 5 train modified by adding three additional impingers in ser-
ies to the four used in method 5 train. The first two impingers contained 150
milliliters of distilled water. The third, was empty, the fourth, fifth and
sixth impingers contained 150 milliliters of 10% hydrogen peroxide and seventh
impinger containing 250 grams of silica gel.
The sampling procedure was identical with that used in method 5 particu-
late sampling. The sampling was done isokinetically at the centers of equal
areas within the duct.
Sample Recovery
The sampling nozzle and probe liner were rinsed with 0.1N NaOH and brushed
out with a nylon bristle brush with a teflon tubing handle. The remainder of
the sampling train was removed to the mobile laboratory. The front half of the
filter and connecting glassware were rinsed with 0.1N NaOH, and this rinse was
added to the nozzle and probe rinse. The filter was removed from the filter
holder and placed in a polyethylene container, which was labelled and sealed.
The first two impinger solutions were measured and placed in a glass sample
container along with a 0.1N NaOH rinse of the impingers. The contents of the
fourth, fifth and sixth impingers were measured and placed in a separate glass
sample container along with a distilled water rinse of the impingers. The
third impinger was rinsed with 0.1N NaOH and placed in a separate glass sample
container. The silica gel in the seventh impinger was weighed to the nearest
gram, and regenerated.
Sulfur Dioxide Analysis
The samples were analyzed for sulfur dioxide by taking an aliquot of the
hydrogen peroxide impinger solutions and titrating with barium perchlorate
solution and thorin indicator as described in EPA Method 6 "Determination of
Sulfur Dioxide Emissions from Stationary Sources".
20
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12
13
17
Figure 4. EPA method 5 particulate sampling train
1. Calibrated Nozzle
2. Heated Probe
3. Reverse Type Pi tot
4. Cyclone Assembly
5. Filter Holder
6. Heated Box
7. Ice Bath
8. Impinger - (Water)
9. Impinger - (Water)
10. Impinger - (Water)
11. Impinger - (Silica Gel)
KEY .
12. Thermometer
13. Check Valve
14. Vacuum Line
15. Vacuum Gauge
16. Main Valve
17. Air Tight Pump
18. ByPass Valve
19. Dry Test Meter
20. Orifice
21. Pi tot Manometer
22. Thermometer
21
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Arsenic Analysis
1. Filter - Warm filter and loose particulate matter with 50 ml 0.1N
NaOH for about 15 minutes. Add 10 ml concentrated HN03 and bring to boil for
15 minutes. Filter solution through No. 41 Whatman paper and wash with hot
water. Evaporate filtrate, cool, redissolve in 5 ml of 1:1 HMOs, transfer to
a 50 ml volumetric flask and dilute.
2. Probe Wash and Impinger Solns - These should be combined and a 200 ml
sample withdrawn. Add 10 ml concentrated HNOs and evaporate to b few mill IT-
liters. Redissolve with 5 ml 1:1 HNOs and dilute to 50 mis. A reagent blank
should be carried through the same procedure. The resulting blank solution
should be used in the dilution of standards to matrix match samples and stan-
dards.
3. All the samples prepared above should be screened by air/acetylene
flame. The filter samples may require dilution with 0.8N HN03. Impinger solu-
tions containing more than 25 mg/1 of arsenic should be diluted since linearity
decreases dramatically above that level.
Since an entrained hydrogen flame provides about five times as much sen-
sitivity as the air/acetylene flame, a matrix check of a sample in a hydrogen
flame should be carried out by the method of standard additions, and compared
with a value obtained from matrix matched standards in a hydrogen flame. If
values are comparable (+5%) the air entrained hydrogen flame may be used.
Due to high concentrations of copper on the filter an air/acetylene flame
should always be used to dissociate any AsCu compounds stable in the cooler
hydrogen flame.
4. For samples below the lmg/1 level, hydride generation is necessary.
An appropriate aliquot of digested sample in 0.8N HNOs containing less than
about 10 yg of arsenic is chosen (some screening may be necessary). Five mis
of concentrated H2$04 is added to the sample which is then placed on a hot
plate until SOs fumes fill the flask. A reduction in volume to about 5 ml or
less may be necessary. This step removes HNOs which causes a violent reaction
when the reducing agent is added resulting in poor reproducibility and lowered
sensitivity by producing 12, N02 and possibly other species.
One ml of 30% KI and 1 ml of 30% SnCl2 are added to the sample, the former
to act as a catalyst in hydride formation and the latter to reduce all the ar-
;senic to As +3. The sample is then diluted to about 15 ml and 15 ml of concen-
trated HC1 is added. Powdered Zn (or NaBH4) is then added, the reaction ves-
sel is immediately closed and the nitrogen or argon carrier flow initiated. A
peak should be produced within a few seconds.
C. Particle Sizing
The size distribution of the particulates was estimated with a Brinks six
stage impactor. Figure 5 is a diagram of the Brinks impactor sampling system
used.
22
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Sampling Procedure
The Brinks impactor was introduced into the gas stream through the sampl-
ing port with the nozzle facing the flow of gas. The sampling pump was turned
on and the pressure drop across the impactor adjusted with the bypass valve.
The pressure drop across the impactor was read from the mercury manometer. The
pressure drop is proportional to the flowrate through the impactor and to the
particle sizing cutoffs of each stage.
Sampling time at each location varied according to grain loading in the
particular duct being sampled. The impactor plates were inspected after each
test and the sampling time altered on the succeeding test to optimize the a-
mount of particulate sampled. Sampling for too long results in carryover from
one stage to the next, while sampling for too short a time can result in insuf-
ficient particulate on one or more of the stages for accurate analysis.
Analysis
The impactor plates and filters had been dessicated to a constant weight
before the tests, and tare weights taken. After the test the same procedure
was used to get the final weights of the impactor plates and filters. The dif-
ference between the tare weight and final weight is the weight of particulate
collected.
The cumulative percentage of the total particulate catch which" was col-
lected in each stage was plotted on log normal graph paper against the size
cutoffs for each stage. The resulting best fit straight line is the estimated
particle size distribution of the collected particulates.l
Brink, J.A. "Cascade Impactor for Adiabatic Measurements", Industrial
and Engineering Chemistry, Vol. 5, No. 4, April 1958, page 647.
23
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BRINKS IMPACTOR
47 MM GLASS FIBER FILTER
BY PASS VALVE
ORIFICE
MERCURY
MANOMETER
PUMP
DRY GAS
METER
MANOMETER
Figure 5. Brinks impactor particle sizing system schematic
24
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