United States Industrial Environmental Research EPA-600/2-79-045
Environmental Protection Laboratory February 1979
Agency Research Triangle Park NC 27711
Research and Development
Ferroalloy Process
Emissions Measurement
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL PROTECTION TECH-
NOLOGY series. This series describes research performed to develop and dem-
onstrate instrumentation, equipment, and methodology to repair or prevent en-
vironmental degradation from point and non-point sources of pollution. This work
provides the new or improved technology required for the control and treatment
of pollution sources to meet environmental quality standards.
EPA REVIEW NOTICE
This report has been reviewed by the U.S. Environmental Protection Agency, and
approved for publication. Approval does not signify that the contents necessarily
reflect the views and policy of the Agency, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/2-79-045
February 1979
Ferroalloy Process Emissions
Measurement
by
J.L. Rudolph. J.C. Harris, Z.A. Grosser, and P.L Levins
Arthur D. Little, Inc.
Acorn Park
Cambridge, Massachusetts 02140
Contract No. 68-02-2150
T. D. 21502
Program Element No. INE624
EPA Project Officer: Larry D. Johnson
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, NC 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
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ACKNOWLEDGEMENT
This report has been submitted by Arthur D. Little, Inc., in partial
fulfillment of the requirements of EPA Contract No. 68-02-2150,
Technical Directive 21502. The work on which this report is based
was performed for the Process Measurement and Metallurgical Processes
Branches of the Industrial Environmental Research Laboratory, Office
of Energy, Minerals, and Industry, Research Triangle Park, NC.
The sampling program was designed and carried out by personnel of
Monsanto Research Corporation (MRC), under EPA Contract No. 68-02-
1411. Mr. Darrell L. Harris of MRC was the program director. Con-
tributions were made by W. H. Hedley, M. J. Thalman, and W. R.
Feairheller of MRC.
Arthur D. Little, Inc., wishes to express its appreciation to Mr.
Craig Miller of Union Carbide Corporation, Niagara Falls, N.Y., and
to Mr. Richard Ratzlaff of Union Carbide Canada Limited for their
cooperation in providing process data for this report. The coopera-
tion of Mr. Pierre DuPont of Union Carbide Canada Limited was also
very important to the sampling crew.
Special thanks are extended to Mr. James L. Stauffer and Dr. Carl E.
Rechsteiner of Arthur D. Little, Inc., for the mass spectrometric
analyses.
Appreciation is expressed to the Project Officer, Dr. Larry Johnson
of the Process Measurement Branch. Others from the Process Measure-
ment Branch, to whom appreciation is expressed are Dr. Raymond
Merrill (Assistant Project Officer on the Arthur D. Little, Inc.,
effort and Project Officer on the Monsanto Research Effort) and Mr.
Robert V. Hendriks, Mr. Robert C. McCrillis, and Dr. Larry Twidwell
of the Metallurgical Processes Branch.
ii
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TABLE OF CONTENTS
Page
ACKNOWLEDGEMENT ii
LIST OF FIGURES v
LIST OF TABLES vi
SUMMARY ix
I. INTRODUCTION 1
II. TEST DESCRIPTION 2
A. Description of Facility and Sampling Sites . 2
B. Description of Process 4
C. Sampling Procedures 4
1. Sampling for Comprehensive Analysis . . 4
2. Sampling for On-Site Gas Analysis . . 8
3. Monitoring of Carbon Monoxide Exposure . 9
D. Analysis Procedures 10
1. Level 1 Organic Analysis 10
2. Polycyclic Organic Matter (POM) .... 18
3. Level 1 Inorganic Analysis 19
4. Level 1 Microscopic Analysis 19
E. Problems Encountered 19
1. Process 20
2. Sampling System Problems 20
III. TEST RESULTS 22
A. On-Site Analyses 22
B. Results of Comprehensive Analysis 25
1. Total Particulate Loading 25
2. Level 1 Organic Analysis 25
3. POM Analysis 40
4. Inorganic Analysis 45
5. Microscopic Analysis 61
continued....
iii
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TABLE OF CONTENTS (continued)
Page
IV. CONCLUSION 62
V. REFERENCES 70
APPENDIX A - Level 1 Organic Analysis Data . Ai
APPENDIX B - Inorganic Analysis Data ... Bi
iv
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LIST OF FIGURES
FIGURE No.
1 Gas Cleaning System
2 Source Assessment Sampling System
(SASS) Schematic 6
3 Analytical Procedures for Silicomanganese
Samples 14
4 Analytical Procedures for Ferromanganese
Samples 15
5 Analytical Procedures for Other Samples . 16
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LIST OF TABLES
TABLE No. page
1 Description of Process 5
2 Sample Series I. ..... .... n
3 Sample Series II 22
4 Other Samples 13
5 Summary of Sampling Data 23
6 Results of On-site Analyses 24
7 Total Mass of Emitted Particulates 26
8 Total Extractable Organics 28
9 Organic Extract Summary, IX 30
10 Organic Extract Summary, ISC 31
11 Organic Extract Summary, IIX 32
12 Organic Extract Summary, IICIF 33
13 Organic Extract Summary, IIPW 34
14 Total Organics for SASS Samples, Series I. ... 35
15 Total Organics for SASS Samples, Series II ... 35
16 Organic Extract Summary, Coal 37
17 Organic Extract Summary, Coke , 33
18 Total POM, Silicomanganese Series 41
19 Total POM} Ferromanganese Series 42
20 Total POM, Data Comparison, Level 1 vs GC/MS
Analyses • • 44
21 Arsenic, Mercury, and Antimony Determinations. . 46
22 Total Inorganics, Silicomanganese Series .... 47
23 Total Inorganics, Ferromanganese Series 48
24 Spark Source Mass Spectrometry Data, IC310 ... 49
25 Spark Source Mass Spectrometry Data, ICIF. ... 50
26 Spark Source Mass Spectrometry Data, IPW .... 51
27 Spark Source Mass Spectrometry Data, Ix 52
continued...
VI
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LIST OF TABLES (Continued)
TABLE No. page
28 Spark Source Mass Spectrometry Data, I imp 23 . 53
29 Spark Source Mass Spectrometry Data, IIC310 . . 54
30 Spark Source Mass Spectrometry Data, IIC1F. . . 55
31 Spark Source Mass Spectrometry Data, IIPW ... 56
32 Spark Source Mass Spectrometry Data, IIx. ... 57
33 Spark Source Mass Spectrometry Data, II imp 23. 58
34 Spark Source Mass Spectrometry Data, Coal ... 59
35 Spark Source Mass Spectrometry Data, Coke ... 60
36 Summary of Particulate Emission Data ..... 63
37 Summary of Organic Analysis Results 64
38 Comparison of AAS and SSMS Data 65
39 Comparison of AAS and SSMA Data for Arsenic
and Antimony in Selected Samples 69
vii
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SUMMARY
Sampling and analysis were undertaken to characterize and
quantify particulate, organic and inorganic chemical emissions in
effluents from a totally sealed metallurgical furnace at a ferro-
alloy production facility. Effluents were sampled downstream of
a Venturi scrubber during silicomanganese production (Test I) and
upstream of the scrubber during ferromanganese production (Test 11).
Sampling and analysis methodology used was essentially that of EPA's
Level 1 Environmental Assessment procedure, supplemented by a spe-
cific analysis of polynuclear aromatic hydrocarbons.
Measurements made in Test II indicated a particulate loading
of 68,000 mg/m3, equivalent to 17 Kg/MW-hr. Very high levels of
organics, including high molecular weight aromatic hydrocarbons,
were found. C ompound categories found include some polynuclear
aromatic species recognized as carcinogens. High levels of arsenic
were also measured in Test II. Measurement of gaseous effluent from
the Venturi scrubber in Test I indicated much lower levels of all
species of concern. Particulate loading was estimated to be 64 mg/m3
equivalent to 0.016 Kg/MW-hr. The major organic compound categories
were simple aromatic hydrocarbons and low molecular weight poly-
cyclics. The arsenic level was estimated to be less than 0.5 mg/m3.
In these tests, good agreement was observed between the results
of Level 1 organic analysis and the specific analysis of polynuclear
aromatic hydrocarbons. Good agreement was also found between the
atomic absorption and spark source mass spectroscopic analyses of
arsenic and antimony.
Because the two tests corresponded to different ferroalloy pro-
duction processes, the results cannot provide a quantitative measure
of the Venturi scrubber efficiency. However, the data imply good
particulate removal efficiency. The Venturi scrubber also appears
to be effective for removal of polynuclear aromatics, especially
species in the higher molecular weight range that includes the recog-
nized carcinogenic POM.
ix
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I, Introduc tion
Ferroalloy plants are of Interest to the Environmental Protection
Agency (EPA) because of their high emissions of particulates. Pre-
liminary data from a plant in Norway showed that the closed type of
metallurgical furnaces seemed to be efficient in lowering the
quantities of particulate emissions. However, it was also found
that these emissions contain a high percentage of polycyclic aro-
matic hydrocarbon materials. Further information is needed to
determine the accuracy and applicability of these early findings.
To supply this data, Monsanto Research Corporation was assigned by
EPA to sample the emissions from the Union Carbide Ferroalloy Plant
at Beauharnois, Quebec, Canada. Emissions from both the silico-
manganese process and the ferromanganese process carried out in
this plant were sampled. Arthur D. Little, Inc., was responsible
for the analysis of these samples.
This report, which was prepared by Arthur D. Little, Inc., integrates
the following information:
• sampling and on-site gas analysis data provided in rough
draft form by Monsanto Research Corporation.
• Process operation data provided by Union Carbide Canada
Limited.
o results of comprehensive chemical analyses by Arthur D.
Little, Inc.
Chapter II presents a description of the test, including the facility,
process and sampling and analysis plan. Chapter ill presents the test
results. Conclusions are presented in Chapter IV. Details of the
analytical results are presented in the Appendices.
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II. Test Description
A. Description of Facility and Sampling Sites
The Union Carbide Canada Limited plant in Beauharnois, Quebec, is a
modern (1974) integrated ferroalloy production facility incorpora-
ting a totally sealed electric furnace. In addition to the furnace,
the plant includes facilities for: raw material preparation and
storage; sintering of coke and ore fines; mix batching and delivery;
and air and water pollution abatement. The closed metallurgical
furnace and the associated air pollution control equipment were the
focus of the tests described in this report.
The 72,000 KVA totally sealed furnace is contained in a 15 m diameter
by 8.8 m deep shell, which has an air-cooled flat bottom. The inner
hearth diameter is 12.1 m, and the crucible depth is 6.3 m. Three
self-baking electrodes, 1.9 m diameter, are triangularly arranged
at 4.75 m center-to-center distances. Additional details of furnace
design are provided in Reference 1.
The air pollution abatement equipment for the closed furnace is shown
schematically in Figure 1. The system includes two parallel quen-
chers, a coarse dust separator, a Venturi scrubber, a mist elimi-
nator, and two fans in series. The sampling locations were upstream
and downstream of the Venturi scrubber. Figure 1 also shows the by-
pass stacks through which furnace off-gases can be vented and then
flared.
Sampling upstream of the Venturi scrubber utilized an existing 10 cm
(4 in) diameter port in the 1.03 m (40.5 in) diameter bypass stack,
before the flare. At this location, on the sixth floor of the furnace
building, the stack temperature is normally in the range of 480 to
870°C (900 to 1600°F). The stack is under slight negative pressure
at this point. The bypass stack gas typically contains about 41% carbon
monoxide, 8% hydrogen, 1% oxygen and 50% carbon dioxide (dry basis), and
has a moisture content of about 2%.
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1. Bypass Stacks
2. Quenchers
3. Dust Separator
4. Venturi Scrubber
5. Mist Eliminator
6. Fans
7. Recirculation Loop
8. Clean Gas Stack
9. Incinerator Ductwork
FIGURE 1 GAS CLEANING SYSTEM
Source: Reference 1, Reproduced with permission of R. G. Ratzlaff
-------
Sampling downstream of the Venturi scrubber was done at a point 6.1m
(20 ft) from the exit of the scrubber, using an existing port in the
0.74 m (29 in) pipe. This port is located approximately 3 m (10 ft)
above the floor in a room on the third story of the furnace building*
The temperature of the gas stream at this point is normally between
32 and 49°C (90 and 120°F). The stream is saturated with water and
is under a positive pressure of approximately 51 cm (20 inches) of
water. The major chemical components of the gas are the same as in
the bypass stack: 41% carbon monoxide, 8% hydrogen, 1% oxygen and
50% carbon dioxide.
B. Description of Process
Table 1 presents the process information provided to Arthur D. Little,
Inc., by Union Carbide Canada Limited, for the silicomanganese pro-
duction run on August 11, 1977, and the ferromanganese production run
on August 27, 1977, which were the two runs sampled.
C. Samplin% Procedures
The sampling plan for these tests was prepared by Monsanto Research
Corporation (MRC). A team from MRC under the direction of Mr.
Darrell L. Harris performed all the sample collection and on-site
gas analysis work. The methodology used was essentially that of
EPA's Level 1 Environmental Assessment procedures (2), except as
noted.
1. Sampling for Comprehensive Analysis
The objectives of this test program include quantitative estimation
of total particulate emissions and comprehensive characterization of
organic and inorganic materials emitted. To accomplish this, samples
were collected using the EPA Source Assessment Sampling System
(SASS) (2), shown schematically in Figure 2. This sampling
train incorporates three cyclones and a filter to provide
collection and size fractionation of particulates, a solid
sorbent module containing XAD-2 resin for collection of organic
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Table 1
Description of Process
Aug. 11/77
MIX ORDER (Ib) SiMn
Std. FeMn Slag 3000
Dried Manganese Ore (3% H20) 3000
Sinter
Dried Coke (4% H20) 1000
Limestone -
Steel Scrap 125
Quartz 1000
Coal 250
Aug. 27777*
Std. FeMn
5000
1000
900
500
200
OPERATING RESULTS
Average Load (while operating)(KW) 22500
Operating Time (%) 98
KWH/lb. of Alloy 1.
Production per Day (NT) 150
Electrode Consumption 60
(Ibs./N.T. Alloy)
75
17300
98.5
1.0
205
30
SLAG COMPOSITION (%)
MnO
A1203
CaO
12.1
32.4
27.0
15.9
41.3
21.1
15.6
13.4
ALLOY COMPOSITION (%)
Mn
Si
67.0
16.0
80
1.0
Venturi Scrubber Water Flow Rate
Venturl Scrubber Pressure Drop
90 gpm
90" water
90 gpm
90" water
Furnace in final stages of transition to Std. FeMn from SiMn.
-------
STACK T. C.
HEATER
CON-
TROLLER
CONVECTION
<^—I SS PROBE
F LJER , GAS COOLER
1
I
ON
ft
i <
1
1
!
GAS
TEMPERATURE
T.C.
XAD-2
CARTRIDGE
IMP/COOLER
TRACE ELEMENT
COLLECTOR
x~X CONDENSATE
__/ \-, COLLECTOR
DRY GAS METER ORIFICE METER
CENTRALIZED TEMPERATURE
AND PRESSURE READOUT
CONTROL MODULE
10 CFM VACUUM PUMPS
Figure 2. Source Assessment Sampling Schematic (from Reference 2)
1MPINGER
T.C.
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vapors, and oxidizing impingers for collection of volatile inorganics.
Several modifications to the standard SASS train were made to accom-
modate the special requirements of this sampling situation, especially
the risk of a possible hydrogen explosion in the event of leaks from
the train or the stack being sampled. Possible electrical ignition
sources in the SASS train were eliminated as follows:
• The probe and oven were modified so that they could be
heated by steam, rather than electricity.
• The oven and sorbent module were modified so that a
nitroben blanket could surround all spark sources on
these two components.
• The console and pumps from the SASS train were located
outside of the explosion hazard area, 15-25 m (50-75 ft)
away.
• A 15 m (45 ft), 2.5 cm (1 in) O.D., Tygon tubing line
attached to the outlet of the SASS dry test meter, to
vent the gases away from the console and operators during
runs.
An additional SASS train modification was to extend the Teflon-lined
stainless steel braided line connecting the oven to the sorbent
module, so that the probe and oven were the only train components
placed on the scaffolding platforms. The sorbent module and impingers
were placed on the floor below the sampling port.
The interface between the probe and the stack was accomplished by
adding a packing gland to the existing port and gate valve. The
probe was inserted into the packing gland which was purged with
nitrogen before the gate valve was opened. During sampling, the
probe nozzle was positioned in the stack at a fixed point of average
velocity, determined by a preliminary traverse with a Pitot tube
according to EPA Method 2. (3) The sampling system was operated as
close to isokinetic conditions as was possible within the constraints
of available nozzle sizes and operating parameters. The sampling
-------
plan called for collection of 30 m3 (1060 ft3, standard) of stack gas
at a rate of 1.4 to 2.4 x 10~3 m3/s (3 to 5 ft3/min.)
At the completion of each sampling run the train was disassembled and
samples recovered according to the EPA Level 1 procedures (2).
2. Sampling for On-Site Gas Analysis
a. Carbon Monoxide, Carbon Dioxide, Oxygen and Water
It was planned to collect integrated gas samples in Tedlar
bags for Orsat analysis of carbon monoxide, carbon dioxide
and oxygen according to EPA Method 3 (4). It was later
agreed that the readouts from the plant's instrumental
analyzers, located within a few feet of the sampling port
at the scrubbers outlet, could replace the Orsat analysis
for that stack.
Moisture determinations in both stacks were done according
to EPA Method 4 (5).
b. Organic Gases
Organic species in the -160 to +90°C boiling point range
were sampled and analyzed at the plant site. Stack gases
were collected in Tedlar bags. Analyses were performed
using an AID portable gas chromatograph with a flame ioni-
zation detector. A 1.8 m by 6.4 mm (6* x 1/4") stainless
steel Porapak Q column was operated isothermally at 50°C.
The procedure was calibrated using standard gas mixtures
taken to the field laboratory.
The GC system simply separates and analyzes mixtures of
materials with a given boiling point range (and polarity
in some cases) rather than individual pure compounds.
Since the chromatogram peaks represent mixtures of materials
present in a certain boiling range rather than pure,
-------
individual compounds, the chromatographic data were reported
as follows:
Corresponding
Designation B.P. Range Hydrocarbon
GCI -160 to -100 Methane, (^
GC2 -100 to -50 Ethane, C
2
(
GC4 0 to 30 Butane, C,
GC3 -50 to 0 Propane, „„
4
GC5 30 to 60 Pentane, C,
GC6 60 to 90 Hexane, C.
D
c. Sulfur Gases
Samples were collected in gas sampling bags and the concen-
trations of hydrogen sulfide, carbon oxysulfide, carbon
disulfide and sulfer dioxide were determined in the field.
An AID Model 511 gas chromatograph with a flame photometric
detector (393 run filter) was used for the analyses. An
8 m by 3 mm (8' by 1/8') Teflon column packed with 15% UCON
50 HB 280X on 40/60 Chromosorb T was operated isothermally
at 134°C. The procedure was calibrated using an AID Model
320A permeation tube system.
3- Monitoring of Carbon Monoxide Exposure
Several precautions were taken to minimize potential toxicity hazards
to the sampling crew due to the high levels of carbon monoxide in the
sampled streams. The plant safety procedures were explained in a
lecture by Union Carbide Canada Limited personnel. The plant was
equipped with continuous carbon monoxide monitors set to sound an
audible alarm at the 100 ppm level. Also, plant personnel took
DrMger tube readings of carbon monoxide levels in the working area
every 15 minutes and cleared the area if concentrations over 100 ppm
were measured. Further indication of possible carbon monoxide
hazard was provided by a Monsanto Research Corporation—designed
continuous monitor, set to give visible and audible alarms at the
-------
50 ppta level. The sampling crew cleared the area when this alarm
was triggered.
When sampling equipment was being inserted or removed from the
stacks, sampling crew members wore trailing air masks. It was at
these times that the probability of exposure to hazardous levels
of carbon monoxide was greatest.
D. Analysis Procedures
The SASS train samples collected by Monsanto Research Corporation
were sent to Arthur D. Little, Inc., for analysis. The samples
received for analysis included eighteen components from the two
SASS trains used for the two processes, two feed samples (coal and
coke), and two solvent blanks corresponding to the solvents used
for extraction of the sorbent condensate and for probe and cyclone
rinses. For simplification, each sample has been assigned a code
which is used throughout this report. Tables 2-4 identify the
samples and list their codes. The analytical plan was prepared by
Arthur D. Little, Inc., in consultation with the EPA project officer.
Each sample was subjected to the Level 1 analytical program, including
microscopy, inorganic and organic analysis. Figures 3-5 show the
actual step-by-step analysis scheme used for each sample. All samples
were carried through the entire level 1 program except in those cases
where the sample size was below that required for further analysis.
The samples were also analyzed for polycyclic aromatic hydrocarbons
and other key related species (POM) using a GC/MS procedure.
1. Level 1 Organic Analysis
Level 1 organic analysis procedures as described in the EPA procedures
manuals(2, 6) were followed. A brief summary of the various steps is
given below:
10
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Table 2
Sample Series I
Series
Process
Sampling Point
Volume of Gas Sampled
Silicomanganese
Outlet of Venturi Scrubber
32.12 in
SASS Components
cyclone catch >10y
cyclone catch >3vi
cyclone catch >ly
filter catch
probe and cyclone rinses
XAD-2 resin
sorbent module condensate
organic extract
Impinger soln #1
(including condensate
from sorbent module)
Impinger soln #2 and #3
Codes
IC10
IC3
IC1
IF
IPW
IX
ISC
I imp. 1
I imp. 23
( IC310
j after combining
i IC1F
.' after combining
11
-------
Table 3
Sample Series II
Series
Process
Sampling Point
Volume of Gas Sampled
II
Ferroroanganese
Bypass-
1.36 m
SASS Components
cyclone catch >10y
cyclone catch >3u
cyclone catch >lp
filter catch
probe and cyclone rinses
XAD-2 resin
sorbent module condensate
organic extract
Impinger soln #1
(including condensate
from sorbent module
Inpinger soln #2 and #3
Codes
IIC10
IIC3
IIC1
IIF
IIPW
IIX
IISC
II imp. 1
II imp. 23
IIC310
after combining
IIC1F
after combining
12
-------
Table 4
Other Samples
Coal CL
Coke CK
Blank (methylene chloride) BM
Blank BMM
(methylene chlorlde/methanol)
Solvent blank B
(ADL methylene chloride)
13
-------
IC10
IC3
IC1
IF
0)
O
O>
c
'c
o
o
a
o
IC310
^f IPI P
1
a
"»
c
o
re
o
O
o
o
-------
.
'S
a
IIC10
IIC3
c
'E
!5
§
O
•misio
to
I
I
.0
•4-f
O
£
X
LLJ
X
O
CO
O
O
O
a.
cj
a
o
1
1
LL
O
OC
O
a.
O
cc
O
a.
IIC1
IIP
>
•^ICIF
• •
IIPW
MX
-•—•-
use
I limp.
1
Ilimp.
23
FIGURE 4 ANALYTICAL PROCEDURES FOR FERROMANGANESE SAMPLES
15
-------
Coal
Coke
Blank CH9CU
2 2
(Field)
Blank CH2CI2
(Lab)
Blank CH2CI2/
MeOH
(Field)
*-»
•6
09
Q
CO
CO
X
0
'S
£
X
LU
flj
JC
X
o
CO
O
O
S
cc.
*
o
tn
O
-------
a. Participate Weights
The weights of the particulate samples (cyclone catches and
probe and cyclone rinses) were obtained by drying the samples
to constant weight in tared evaporating dishes at 50°C and
cooling to room temperature in a desiccator.
b. Soxhlet Extractions
All extractions were carried out for a 24-hour period using high
purity methylene chloride (Burdick and Jackson, distilled-in-
glass) . The following procedures were used:
i. XAD-2 Resins - extracted with about 2500 mL of methylene
chloride.
ii. lOy and 3y cyclone catches - weighed individually and
then combined. Portions of the combined particulates
were removed for microscopy and inorganic analysis and
the remainder extracted with 200-400 mL of methylene
chloride.
iii. ly cyclone catch and filter samples - same procedure
as above.
c. Total Chromatographable Organics Analysis (TCO)
The quantity of the total organic material with boiling points
in the range of 100-300°C was determined by gas chromatography,
using a flame ionization detector. The concentration of each
sample was calculated from the ratio of the peak areas of the
sample to that of the known standards. The following instrument
conditions were used:
Column: 10% OV-101 on 100/120 mesh Supelcoport
Injector temperature: 270°
Detector temperature: 305°C
Temperature Program: Room temperature for 5 minutes, then
programmed at 20°C/min up to 250°C
Gas flow rates: He at 30 mL/min
H2 at 30 mL/min
Air at 300 mL/min
17
-------
d. Gravimetric Analysis (Grav)
The amounts of organic material with boiling points higher than
300°C were determined by the gravimetric analysis method (Grav);
one or five mL samples were pipetted into precleaned, dried,
and weighed aluminum dishes, and were dried at room temperature
in a desiccator to constant weight.
e. Infrared (IR)
The IR spectra of all samples as potassium bromide micro pellets
were obtained on a Perkin-Elmer 521 grating spectrometer.
Spectra were interpreted with the aid of references 7-10.
f. Liquid Chromatographic (LC) Separation
Samples for liquid chromatography were initially concentrated
to 10 mL using Kuderna Danish apparatus followed by concentration
to 1 mL under a nitrogen stream and then subjected to three con-
secutive solvent exchanges with cyclopentane. The resultant cyclo-
pentane solutions were chromatographed on a silica gel column,
collecting seven fractions by elution with solvent mixtures of
increasing polarity.
g. Low Resolution Mass Spectroscopy (LRMS)
LRMS analysis was carried out on a Dupont 21-110B spectrometer.
Both batch inlet and direct insertion probe techniques were
used depending on the TCO content of the samples. Sample sizes
varied from 20 uL to 50 uL. Typically, a sample was run at 15 ev
and 70 ev ionization potentials over a temperature range of
70-350°C. Interpretation of the mass spectra was based on
references 11-14.
2. Polycyclic Organic Matter (POM)
The polycyclic organic matter (POM) of each extract was analyzed by
gas chromatography/mass spectrometry (GC/MS). A Finnigan Model 400
GC/MS with data system was used. The microprocessor controlled GC
18
-------
(3% Dexsil 400 on 100/120 Supelcoport) was programmed from 170°C to
300°C after 1 minute of Isothermal operation at 110°C and then held
isothermally at 300°C for 30 minutes. Quantitation was based upon
the selected ion chromatograms for each of the POM molecular
ions. Calibration was done using a reference mixture containing
selected POM compounds for specific molecular weight regions. (15-19)
3. Level 1 Inorganic Analysis
Elemental analysis was done on each sample after the appropriate
sample preparation (described below) using an MS-7 Spark Source Mass
Spectrometer and photographic detection system. Experiments were
conducted by Commercial Testing and Engineering Co.
Particulates: Refluxed with concentrated HNC>3 and
concentrated HC1 mixture for six hours.
XAD-2 resin, coal,
coke: Parr Bomb combustion over HNOs
Impinger solutions: Acidified with HC1
Arsenic, mercury and antimony were determined by atomic absorption
spectroscopy. A Perkin-Elmer 503 Spectrophotometer was used.
4. Microscopic Analysis
The particulates from the two SASS trains were examined under a Zeiss
standard polarizing microscope. Photomicrographs were made on Ekta-
chrome High Speed film, with samples immersed in a medium of 1.44
index to provide good contrast.
E. Problems Encountered
Despite extensive pre-test planning and preparation, several diffi-
culties were encountered during these field tests. These are dis-
cussed briefly below.
19
-------
1. Process
A problem that had a significant impact on the test program was that
a major process change, from silicomanganese production to ferro-
manganese production, occurred between the two Monsanto Research
Corporation sampling runs. This situation resulted from a combina-
tion of some plant scrubber system down time during the first
Monsanto Research Corporation sampling trip, and limitations imposed
on the two subsequent sampling trips by the time, schedule, and
budget constraints of the Monsanto Research Corporation program.
2. Sampling System
a. Steam heating system
The steam heating system designed to control the probe and
oven temperature, was found to heat the oven to about 80°C,
rather than the specified 200°C. It was decided to use the
electrical oven heater with a nitrogen blanket. Steam heat
was used for the probe until the steam generator failed
part way through the first run. It was decided that probe
heating was not essential, since only about one linear foot
of the probe was exposed to the ambient air.
b., Sampling for on-site analysis
Monsanto Research Corporation field crew members were unable
to acquire grab gas samples for analysis of carbon monoxide,
oxygen and carbon dioxide or nitrogen oxides. During one
attempt to acquire a sample for nitrogen oxides analysis
a sampling crew member was injured and required first aid.
The plant control room data were used to estimate the con-
centrations of carbon monoxide, oxygen and carbon dioxide
for Run 1: the same values were used for Run 2 calculations.
Samples for analysis of sulfur gases and organic gases
were taken as planned.
20
-------
c. Sampling at the bypass stack
The port on the bypass stack had to be bored out before the
probe could be inserted. During a velocity traverse on this
stack, the stack was "on fire" for a time and the probe and
pitot were damaged. An electrical overload, causing impinger
backup, occurred when two electrical outlets were misidentified
as being on independent circuits. Finally, during the sampling
run the filter was found to clog in 15 minutes or less. Sample
collection was stopped after the third filter had plugged; the
total volume of gas sampled was 1.36 m3 instead of the intended
30 m3.
21
-------
III. Test Results
A. On-Site Analyses
Data described in this section were acquired by Monsanto Research Cor-
poration personnel.
Table 5 summarizes the sampling data acquired during the two runs
with the SASS train. Sampling rates exceeded isokinetic flow by 197%
in run 1 and 278% in run II, because stack gas flow rates were lower
than had been expected.
Table 6 summarizes the results of the on-site analyses of stack gases.
As noted in Section II.E, problems were encountered in acquiring some
of the Intended grab samples. There are several interesting features
of the data that were acquired.
The concentrations of the major gaseous species, determined at the
scrubber outlet, were somewhat different than had been expected. The
abundance of the reduced species, hydrogen and carbon monoxide, was
about 85% higher than anticipated, while oxygen and carbon dioxide
levels were correspondingly lower. This may be due in part to prefer-
ential absorption of the oxidized components in the scrubber water.
The levels of gaseous organic species in the -160° to -50°C boiling
point range (GCl plus GC2) were three times higher downstream of the
scrubber during silicomanganese production than they were upstream of
the scrubber during ferromanganese production. This observation shows
that the process change between runs I and II resulted in a significant
change in the emissions from the facility. For this reason, the data
acquired in these tests cannot be used to quantify the performance of
the Venturi Scrubber.
Concentrations of sulfur gases were low and approximately the same in
the two sampling runs.
22
-------
Table 5
Summary of Sampling Data
Sample Series
Process
Sampling Point
Silicomanganese
Outlet of Venturi
Scrubber
II
Fe rromanganese
Bypass
Volume of Gas sampled,'
m3
(SCF)
Test period, minutes
Stack temperature,
°C
Stack gas velocity
m/sec
(ft/rain)
Stack gas volumetric
flow rate:
m/sec
(SCF/min)
32.1
(1130)
273
1.51
(3200)
1.36
(48.0)
20
47
(117)
0.0715
(14.1)
388
(730)
0.0852
(16.8)
1.20
( 2550)
Gas volumes are corrected to standard conditions of 101 KPa
(29.9" Hg) and 21.1°C (70°F).
23
-------
Table 6
Results of On-Slte Analyses
Sample Series
Process
Sampling Point
Species
Carbon Dioxide
Carbon Monoxide
Oxygen
Hydrogen
Water
Organic Gases:
GC1 Range
GC2 Rangef
Sulfur Gases:
Hydrogen Sulfide
Carbon Oxysulfide
Sulfur Dioxide
Silicomanganese
Outlet of Venturi
Scrubber
II
Ferromanganese
Bypass
Concentration (v/ v)
9.0%*
76.0%*
0.2%*
14.8%*
12.5%
3000 ppm
90 ppm
1.5 ppm
2.47 ppm
0.20 ppm
not analyzed
not analyzed
not analyzed
not analyzed
35.6%**
1000 ppm
30 ppm
0.95 ppm
2.11 ppm
<0.05 ppm
From readouts of plant on-line instrumentation.
**
Monsanto Research Corporation believes this value to be in error;
the expected value was 4-5%
fOrganic gases boiling in the range of -50° to +90°C (GC3 to GC6)
were not found. Those species would have had very long retention
times under the GC conditions used (50°C Isothermal, Porapak Q).
24
-------
During the sampling of the source, the opacity was never observed to
be less than 100%. There was a heavier smoke during ferromanganese
production than during silicomanganese production according to the
Monsanto Research Corporation job log.
B. Results of Comprehensive Analysis
Data presented in this section are the results of analyses performed
at Arthur D. Little, Inc.
1. Total Particulate Loading
The total mass of emitted particulates as well as the concentration
data for the particulates in the source for both the silicomanganese
and the ferromanganese processes are given in Table 7. In the effluent
gas from the silicomanganese process, 88% of the particulate matter
is in 3-10y size range. The total particulate loading in this series
was found to be 64 mg/m . Extremely high quantities of particulate
matter was collected at the bypass from the ferromanganese process.
A concentration of 68,000 mg/m3, relatively uniform distribution over
all size ranges, was found for this stream.
Unfortunately, due to the different processes in the two series, these
upstream and downstream data dannot be directly compared to reveal the
efficiency of the Venturi Scrubber gas cleaning system. It is inter-
esting to note the relatively small proportion of mass emissions in
the large (lOu) and small (filter) size ranges from the silico.-
manganese sample after the Venturi Scrubber.
25
-------
Table 7
Total Mass of Emitted Participates
Series No.
Process
Sampling point
Volume of gas sampled
Silicomanganese
Outlet of Venturi
Scrubber
32.12 m3
II
Ferromanganese
Bypass Stack
1.36 m3
Total partlculates
lOy cyclone 0.0111 g
3y cyclone 1.8218
ly cyclone 0.0684
filter 0.0319
probe and cyclone rinses 0.1411
Total
2.0743
38.4706 g
12.6509
10.1065
19.3515
11.9077
92.4872
Total concentration
lOy cyclone 0.34 mg/m3
3y cyclone 56.
ly cyclone 2.13
filter 0.99
probe and cyclone rinses 4.4
Total 64. mg/m3
28,000 mg/ra3
9,300
7,400
14,000
8,800
68,000 mg/m3
26
-------
2. Level 1 Organic Analysis
-i. SASS Samples
Data on the total extractable organic material for the various SASS
train components from both processes are summarized in Table 8, Very
little organic matter was extracted from the participates collected
from the silicomanganese process. About 94% of the total organics
was found in the XAD-2 extract, 96% of which falls into the TCO
range (boiling point between 100 and 300°C). Although the concentra-
tion of organics in the sorbent condensate extract was not high, it is
interesting to note that more high boiling material is present in this
component.
Much larger amounts of organic matter were found in the extracts of
all SASS train components, except the sorbent condensate extract, from
the ferromanganese process. About 92% of the material is found in
the XAD-2 extract in this case, of which about 82% was found to be
high-boiling (b.p. >300°C) material.
The five extracts containing more than 0.5 mg/m^ of total organic were
taken through LC separations, and the seven LC fractions collected
from each extract were analyzed for TCO and Grav as well as by IR and
LRMS. The LC, IR, and LRMS data are given in the Appendices. From
these data, the organic species in each extract were classified into
compound categories based on the results of the Level 1 analysis and
the concentration of each category was estimated using the method pro-
posed by Arthur D. Little, Inc. (20) Tables 9 to 13 show these results
Some interesting aspects of these data are pointed out below:
i. Table 9 shows that aromatic hydrocarbons and fused aromatics
having MW <216 are the major species in sample IX. Since the TCO
values are much greater than the Grav values for all LC fractions,
27
-------
Table 8
Total Extractable Organics, mg/m3
Process
Particulates extract
10 + 3p
1 + filter
probe and cyclone
rinse extract
XAD-2 extract
Sorbent condensate
extract
Silicomanganese
TCO GRAY TOTAL
— M3.03 ^0.03
— ^0.03 ^0.03
0.47 0.47
45
0.57
2.18
2.02
47
2.59
II
Ferromanganese
TCO GRAV TOTAL
6.6
— 48.
37.
205
0.41
910
6.6
48.
37.
1110
0.41
28
-------
these species are relatively volatile materials and do not repre-
sent the major known carcinogenic POM.
ii. The major category of compounds found in the sorbent condensate
extract (ISC) is non-volatile fused aromatics having MW <216, col-
lected mainly in LC3.
iii. Extremely high quantities of fused aromatics over all molecular
weight ranges were found in II X, especially non-volatile species.
Also present in this sample were: heterocyclic nitrogen and sulfur
compounds, polycyclic aromatic ketones, and a trace amount of esters.
The LC separations between aromatic and polar species were very
good. (Table 11)
iv. Tables 12 and 13 show that the most abundant organic species present
in the particulate extracts (II GIF and IIPW) were similar to those
found in the XAD-2 extract (II X), i.e., fused aromatics in LC 3 and
heterocyclic nitrogen compounds and ketones in LC 6.
The five extracts that had insufficient organic material for LC separa-
tions and subsequent analysis were examined by infrared only. By com-
bining the IR data with the TCO and Grav results, the organic materials
in each extract were very roughly categorized and approximate concentra-
tions estimated. The data from this process, along with the data in
Tables 9-13, were integrated to construct summary tables describing
the concentration distribution of compound categories from each SASS
train. (Tables 14 and 15)
b. Coal and Coke
Coal and coke were also extracted and analyzed. The organic species
found in these samples were categorized and summarized in Tables
16 and 17. The most abundant species in coal extract were found to
be elemental sulfur, aliphatic hydrocarbons, ketones, heterocyclic
nitrogen compounds and fused aromatics with "low" molecular weights.
Relatively small amounts of the high molecular weight fused aro-
matics were detected.
29
-------
Table 9
ORGANIC EXTRACT SUMMARY TABLE
Sample IX> XAD-2 Extract. Silicomanganese
*>
Total Organics, mg/m
TCO. rog
GRAV, mg
LC1
2.32
74.
<0.1
LC2
15.
480.
0
LC3
19.
620 .
5,0
LC4
0.03
1.1
<0.1
LC5
0.17
5.6
<0.1
LC6
2.93
44.
50
LC7
0.74
23.
<0.1
2
41.
1260
65
Category
Int/mg/rtT
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics <216
Heterocyclic S Compounds
Ketones
Esters
Carboxylic Acids
Alcohols
Heterocyclic N Compounds
Ethers
100/2.3
~
100/14
10/1.4
1/0.1
100/9.4
100/9.4
10/0.9
10/«0.1*
10/«0.1<
10/0. 01*
10/0. 01^
10/0.7
10/0.7
10/0.7
10/0.7
1/0.1
1/0.1
1/0.1
1/0,1
1/0.1
2.3
23.
11.
1.7
0.8
0.8
0.7
0.1
0.1
0.1
UJ
o
*Concentration estimated from LC.IR data, with reference to LRMS data of LC3 and LC6
-------
Table 10
ORGANIC EXTRACT SUMMARY TABLE
Sample ISC. , Sorbent Condensate, Silicomanganese
Total Organics, mg/m
TCO, mg
GRAV, mg
LCI
0.26
0.03
8.4
LC2
0.05
0.01
1.5
LC3
2.70
18.
68
LC4
0.002
0.06
<0.1
LC5
0.008
<0.1
0.25
LC6
0.008
<0.1
2.75
LC7
0.008
0.02
0.25
2
3.0
18.
81.
Category
o
Int/mg/m
Sulfur (SK)
Aliphatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Nitrites
Ketones
Esters
Ethers
Sulfides
Amides
Alcohols
Amines
100/0.2
1/0.002
-
100/0.05*
100/2.7
1/0.02
**
.00/0.001
**
.00/0.001
**
.00/0.004
100/0. §0-
100/0.00-
00/0.007
100/0. oo;
- ;.
100/0. 0&
100/0. oo'
100/0. 0(
100/0. 00^
100/0.00^
100/0. C$
0.2
0.05
2.7
0.02
0.004
0.01_
4 0.01
0.005
0.005
0.004
0.004
0.004
Concentration estimated from LC,IR data with reference to LEMS data of LCI
Concentration Estimated from LC,IR data only
-------
Table 11
ORGANIC EXTRACT SUMMARY TABLE
Sample IIX» XAD-2 Extract, Ferromanganesg
Total Organics, mg/m
TCO.mg
GRAV, mg
LCI
3.9
2.25
3.0
LC2
7.0
9,4
<0.1
LC3
780
195
870
LC4
36.
1.21
4.8.
LC5
6.7.
6.2
vn
LC6
88
10
90
LC7
17
11
12
2
940
255
940.
Category
Int/mg/m"
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Heterocyclic S compounds
Heterocyclic N 'compounds
Ketones (polycyclic aromatic")
Carboxylic acids
Esters
100/3.9
10/3.5
10/3.5
100/372
100/372
10/37
10/1.7
100/17
100/17
lOp/3.3
IOC/3.3
100/42
100/42
10/4.2
10/8.1
10/8.1
1/0.8
3.9
3.5
380
^390
37
70
53
4.2
0.8
u>
ho
-------
Table 12
ORGANIC EXTRACT SUMMARY TABLE
Sampie HCIF, Particulates 216
Ketones (polycyclic aromatic)
Heterocyclic N compounds
Esters
Carboxylic Acids
«0.2
-
«0.2
1/0.2
100/23
10/10
«0.2
«0.2
100/6.4
100/6.4
1/C.G6
1/0.06
1/1.5
«0.2
«0.2
0.2
33
6.4
7.9
0.06
0.06
U)
-------
Table 13
ORGANIC EXTRACT SUMMARY TABLE
Sample ** PW» Probe Wash, Ferroroanganese
*J
Total Organics, mg/m
TCO, mg
GRAV, mg
LCI
1.95
-
2,65
LC2
<0.1
-
<0.1
LC3
28
-
39
LC4
7.8
-
11
LC5
0.54
-
0.73
LC6
7.2
-
9.8
LC7
1.44
-
1.96
2
47
-
65
Category
Int/mg/m*
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Heterocvclic K compounds
Ke tones (polycyclic aromatic)
Esters
Alcohols
1/1.9
«
«0,2
100/14
100/14
1/0.07
100/7.7
1/0.07
100/0.2*
100/0.2*
10/0.02*
10/0.02*
10/0.6
100/6.5
1/0.06
1/0.1
10/1.3
1.9
«Q.2
14.
22
0.8
7.8
0.08
0.02
Concentration estimated from LC,IR data with reference to LRMS data of LC4 and LC6
-------
Table 14
Total Organics (mg/m3) for SASS Train Samples (I)
Outlet of
Compound Categories
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Ether
Ketone
Alcohol
Ester
Amine
Heterocyclic N
Heterocyclic S
Carboxylic Acid
Sulfides
Amide
Sulfur
Nitrite
Silicone Compounds
Scrubber, Silicomanganese Process
Particulates Sorbent
>3u* >3y* Rinses Resin
0.2 2.3
0.2 23
11
0.1
0.8
^.01 ^0.01 0.2 0.1
0.2 0.8
0.1
1.7
0.7
^ 0.01 ^0.01 0.2
Module
Condens
0.05
2.7
0.02
0.005
0.01
0.004
0.01
0.004
0.005
0.004
0.2
0.004
Total
2.5
23
14
0.02
0.1
0.8
^0.3
1.8
-\-0.1
0.1
1.7
0.7
0.2
0.1
0.004
Concentrations estimated from IR and total TCO and Grav data only.
35
-------
Table 15
Total Organics (mg/m3) for SASS Train Samples II
Bypass, Ferromanganese Process
Compound Categories
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Heterocyclic S
Heterocyclic N
Ke tones
Alcohols
Esters
Carboxylic Acids
Particulates
Sorbent Module
Total
>3u*
Rinses Resin Condens.*
4.5
1.1
0.8
^.1
'vo.i
0.2
33
7.9
6.4
0.06
0.06
1.9
M).l
14
22
0.8
7.8
0.02
0.08
3.9
3.5
370
390
37
70
53
0.8
4.2
6.9
3.7
380
0.3 450
37
0.07 80
0.05 67
'VO.l
0.9
4.3
Concentrations estimated from IR and total TCO and Grav data only.
36
-------
Table 16
ORGANIC EXTRACT SUMMARY TABLE
Sample Coal (CL)
Total Organ ics, mgjkg
TCO, mg
GRAV, mg
LC1
286
0.36
24
LC2
24.
<0.01
2.0
LC3
101
0.80
7.7
LC4
35.
0.014
2.9
LC5
13.
<0.01
1.1
LC6
62.
0.29
4.9
LC7
10.
<0.01
0.86
2
530
1.2
43.
Category
Int/mg/Kj
Sulfur
Aliphatic Hydrocarbons
Fused Aromatics <216
Fused Aromatics >216
Heterocyclic Sulfur
Heterocyclic Nitrogen
Esters
Re tones
100/143
100/143
-
100/12*
100/12*
10/7.8
10/7.8
100/78
10/7.8
1/0.17
1/0.17
100/17
100/17
1/0.17
1/0.06
1/0^06*
100/6.4
,100/6.4*
1/0.06*
10/5.6
1/0.56
100/56
10/0.90*
1/0.09*
100/9.0*
160
160
8 0
100
7.8
30
0.88
65
CO
*Estimated from LC and IR data, with LRMS data of adjacent LC fractions.
-------
Table 17
Sample
ORGANIC EXTRACT SUMMARY TABLE
Coke (CK)
Total Organics, mgjfcg
TCO. mg
GRAV, mg
LC1
158
0.36
10.
LC2
<1.5
<0.01
<0.01
LC3
16
0.14
0.86
LC4
14
<0.01
0.86
LC5
22
<0.01
1.4
LC6
10
<0.01
0.6
LC7
10
<0.01
0.6
z
230
0.50
14.3
Category Int/mg/kg
Sulfur
Aliphatics
Halogenated Aromatics
Aromatic Hydrocarbons
Heterocyclic N, 0, S
Sul fides, Disulfides
Nitriles
Ethers
Alcohols
Aldehydes, Ke tones
Nitroaromatics
Amines
Phenols
Esters, Amides
Carboxylic Acids
Sul f oxides
100/156
1/2.0
100/13**
10/1.3**
10/1.3**
10/1.4**
10/1.4
10/1.4
10/1.4
10/1.4
LOO/7.0
LOO/7.0
10/2.2
10/2.2
10/2.2
10/2.2
10/2.2
10/2.2
**
10/2.2
10/2.2
100/5.0
100/5.0
**
10/1.0
10/1.0
10/1.0
10/1.0
100/5.0.
10/1.0
100/5.0
10/1.0
A*
10/1.0
100/5.0
10/1.0
10/1.0
acrap-
10/1.0
10/1.0
160
15
2.7
2.7
3.6
3.6
3.6
9.2
19
8.2
4.2
8.2
2.0
2.0
6.0
2.0
U)
co
**
Estimated from LC and IR data, no LRMS data available.
-------
The total amount of organics extracted from coke is low. The major
portion of this seems to be elemental sulfur. The IR data indicated
that aliphatic hydrocarbons, alcohols, and amines could be present
as minor species.
Blanks
Solvent Blank (ADL Methylene Chloride): very clean, negligible
amount of organic material was detected .
Methylene chloride blank (from the field) ; mostly aliphatic
hydrocarbons, trace of silicdne grease was also detected.
Blank methylene chloride/methanol: very little organic material,
the non-volatile species present seem to be inorganic.
The LC data of the three blanks are given in the Appendices.
39
-------
3. Polycyclic Organic Matter (POM) Analysis
The results of GC/MS POM analysis of the ferroalloy samples, expressed
in terms of their concentration at the sample source, are summarized in
Tables 18 and 19. The Reconstructed Gas Chromatograms are attached in
Appendix A.
For the samples after the air-cleaning system (venturi scrubber) from a
silicomanganese process (Series I), a total of 4.2 mg/m3 of POM was
found, 51% of which was anthracene/phenanthrene. Less than 1 mg/m3 of
fluoranthene, pyrene, chrysene and their derivatives were detected.
Most of these species were found in the XAD-2 sorbent module and the
sorbent condensate extracts. Even at the high sensitivity of the GC/MS
method used, no POM with molecular weight over 228 was detected.
Very high concentrations of POM were found for the Series II samples
which were collected at the bypass to the air-cleaning system during a
ferromanganese process. A total of 633 mg/m3 of POM was found in these
samples, 70% of which was anthracene/phenanthrene and fluoranthene, 16?
of which was chrysene/benzoanthracene, benzofluoranthene, and benzo-
pyrene.
Other species such as carbazole, dibenzocarbazone, perylene, indeno
(1,2,3-cd) pyrene, and coronene were also found in these samples. It
is interesting to note that most of the POM was in the sorbent module
and very little of it was in the sorbent condensate, and also that most
of the high molecular weight species were found in the particulate
extracts, especially in the probe and cyclone rinses.
The substantial differences between the POM concentrations for the two
series of samples shown here could be considered as an indication that
the air-cleaning system used is highly effective in removing POM from
effluent gases. Unfortunately, these data cannot be used as firm evi-
dence for this, due to the different processes in the two series.
-------
TABLE 18
GC/MS Polycyclic Organic Matter (POM) Analysis
Sainple Series: 1, Silicomanganese, after scrubber
Concentration:
mg/nr
Species -^Sample
Fluor en e
An th racene / Phenan th.rene
Carbazole
Methyl— Anth racettes
Isomers
Fluoranthene
Pyrene
Methyl Pyrene /Methyl Fluoranthene
Chrysene/Benzo (a) anthracene/etc.
Methyl Chrysenes
7, 12- Dimethyl Benz (a) anthracene
Benzof luoranthene, BenzoCe) pyrene
Benzo(a) pyrene
Perylene
Methyl Benzopyrenes
3-Methylcholanthene
Indeno (1,2,3-cd) Pyrene
Benzo(ghi) Perylene
Dibenzo ( a , h) anthracene
Dibenzo (c,g) carbazole
Dibenzo (ai & ah)pyrenes
Coronene
TOTAL
m/e
165+6
178
167
192
192
202
202
216
228
242
256
252
252
252
266
268
276
276
278
267
302
300
I C310
*
0.00016
0.000058
0.000042
0.00026
I GIF
0.00039
0.00019
0.00015
0.00073
I PW
0. 00012
0.00064
0.00049
0.00017
.
0.0014
I X
0.86
0.83
0.42
0.044
0.046
1.82
I SC
0.62
1.30
0.028
0.018
0.20
0.17
0.005
0.016
2.40
Total
1.5
2.1
0.070
0.018
0.24
0.22
0.005
0.016
4.2
*A11 blanks are items not detected, detection limlc 0.01 ug/ro3
-------
TABLE 19
GC/MS Polycyclic Organic Matter (POM) Analysis
Sample Series: II, Ferromanganese, bypass
Concentration: mg/nr
Species^^^-^Sample
Flaorene
Anthracene/Phenanthrene
Carbazole
lethyl— Anthracenes
Isomers
fluoranthene
'yrene
Methyl Pyrene/ Methyl Fluor an thene
Chrysene/Benzo( a) anthracene/etc.
Methyl Chrysenes
7 , 12-Dimethyl Benz (a) anthracene
ienzofluoranthene, Benzo(e)pyrene
3enzo(a)pyrene
Perylene
Methyl Benzopyrenes
3-Methylcholanthene
Indeno (1,2,3-cd) Pyrene
Benzo(ghi) Perylene
Dibenzo ( a , h) anthracene
Dibenzo(c,g) carbazole
Dibenzo (ai & ah)pyrenes
Coronene
TOTAL
m/e
165+6
178
167
192
192
202
202
216
228
242
256
252
252
252
266
268
276
276
2-78
267
302
300
II C310
0.0014
0.054
*
0.0018
0.034
0.019
0.048
0.00065
0.031
0.036
0.029
0.099
0.0041
0.079
0.15
0.10
0.68
.11 CIF
0.014
0.0055
0.0057
0.026
0.26
0.29
0.026
0.053
0.26
0.55
0.12
0.23
0.29
2.1
II PW
0.62
0.18
2.46
2.28
0.54
3.40
3.13
2.82
0.50
0.34
0.47
0.71
0.16
0.12
17.
II X
16.3
222.
9.6
24.
220.
14.
46.
5.24
0.58
47.
0.67
5.28
0. 78
612.
II SC
0.0077
0.081
0.014
0.0044
0.0034
0.039
0.031
0.0063
0.0041
0.0041
0.19
Total
16.
220.
9.6
24.
0.0034
220.
2.3
14.
49.
5.2
0.58
51.
3.1
1.20
0.39
6.0
1.4
0.90
0.079
0.54
0.51
660.
J
*A11 blanks are items not detected, detection limit 0.3 ug/m3
-------
A comparison of the data on POM concentrations obtained from Level 1
analysis and GC/MS analysis is given in Table 20. In general, the two
seta of data agree with each other within an order of magnitude. In the
cases of samples ISC (Series I, sorbent condensate) and IIX (Series II,
sorbent module), the data are in excellent agreement with each other.
Comparison of the Level 1 and GC/MS analysis data for heterocyclic
nitrogen compounds (Table 20) shows that considerably higher levels are
found by the Level 1 procedure. This is an indication that the two
specific compounds determined in the GC/MS analysis (carbazole and dibenr-
zocarbazole) may constitute only a small fraction of the total hetero-
cyclic nitrogen material. This is confirmed by the Level 1 LRMS data
(e.g., Appendix A, pages A23 to A26), which show that acrldines and
quinolines are the most abundant heterocyclic nitrogen compounds in the
ferroalloy effluent samples. The Level 1 and GC/MS results, therefore,
are in satisfactory agreement for these species as well as for the
polynuclear aromatic hydrocarbons.
-------
Table 20
Total Polycyclic Organic Matter
Series I
Process Silicomanganese
Sampling Location After Scrubber
mg/nH
Polynuclear
Level 1 GC/MS
SASS Sample
C310 ^0.01 0.00026
C1F ^0.01 0.00073
PW ^0.01 0.0014
XAD-2 11 1.8
SC 2.7 2.4
Total 14 4.2
Heterocyclic
SASS Sample
C310
GIF
PW
XAD-2 0.1
SC
Data Comparison
II
Ferromanganese
Bypass
mg/m3
Aromatics
Level 1 GC/MS
4.5 0.60
33 2.1
36 17
760 602
0.3 0.2
840 650
N Compounds
1.1 0.8
7.9
0.8
70. 9.6
0.07 ^.01
Total
0.1
80
9.7
* Carbazole and Dibenzocarbazole were the only two heterocyclic N species
determined in GC/MS analysis.
44
-------
4. Inorganic Analysis
The results of Arsenic, Mercury, and Antimony determinations for both
series of samples, as well as coal and coke, are summarized in Table 21.
IC1F and IPW were not analyzed for As/Hg/Sb due to insufficient samples
received. The Arsenic content of each sample was found to be much higher
than the Mercury and Antimony contents. The high amounts of Arsenic
present in the ferromanganese samples, coal and coke should also be
noted.
The total inorganics detected by spark source mass spectrometry are sum-
marized for each series in Tables 22 and 23. The individual SSMS data
of each SASS sample converted into pg/m^ for series I and mg/m^ for
series II are also given in Tables 24-33. The results of elemental
analysis in coal and coke are shown in Tables 34 and 35. The original
SSMS data for each sample are attached in Appendix B.
45
-------
Table 21
Arsenic, Mercury, and Antimony Determinations
Sample Code
Silicomanganese Series
I C310
I X
I imp 1
I imp 23
Total
Ferromanganese Series
II C310
II C1F
II PW
II X
II imp 1
II imp 23
Total
As
0.018
0.098
0.0062
0.13
0.25
24.
15.
7.7
1.03
0.15
0.08
48.
/ 3
mg/m
Hg
0.000060
0.00050
0.00018
0.016
0.017
0.045
0.025
0.052
0.014
0.11
0.26
0.51
Sb
0.000016
0.001
0.000025
0.00020
0.00012
0.15
0.088
0.038
0.019
0.0013
0.00087
0.30
Sample
Coal
Coke
mg/Kg
As Hg
20. 0.15
20. 0.24
Sb
0.30
0.58
46
-------
Table 22
Total Inorganics, Silicomanganese
Spark Source Mass Spectrometry
Sample No: Series I
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysposium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone,
MC
0.54
MC
MC
0.07
0.20
1.4
2.4
MC
MC
NR
4.0
1.5
MC
MC
1.2
MC
0.34
0.20
0.13
MC
0.27
7.2
1.2
0.001
0.32
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in tig/m3
Cone.
0.21
NR
STD
0.04
MC
3.2
11.
17
0.03
MC
MC
NR
5.5
2.7
MC
2.6
NR
NR
MC
MC
2.1
0.03
Series
Data
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
17.
0.2
1.1
0.15
0.82
MC
0.57
MC
MC
MC
0.04
0.03
0.072
1.2
2.0
0.032
0.94
MC
0.19
2.5
20.
0.14
6.8
MC
21.
NR - Not quantified
All blanks are elements not detected, detection limit 0.1 ppm
MC - Major component, >64 ug/m3
47
-------
Table 23
Total Inorganics, Ferromanganese
Sample No:
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Spark
Series II
Cone.
1.9
MC
MC
0.01
0.56
0.87
19
6.7
MC
NR
0.61
1.3
MC
5.2
10
34
0.05
0,02
0.03
MC
0.05
3.6
0.28
0.002
Source Mass Spectrometry
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in mg/m3
Cone.
0.03
NR
STD
6.0
MC
0.4
MC
1.3
0.005
MC
NR
3.0
0.18
4
0.08
NR
NR
MC
0.07
Series
Data
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
MC
0
0.14
0.05
1.5
1
12
0.7
0.28
0.02
3.0
0.1
0.006
0.3
7.7
1.2
0.19
0.8
0.03
0.14
MC
0.56
NR - Not quantified
$.11 blanks are elements not detected, detection limit 0.1 ppm
MC - Major component , > 68 mg/m3
48
-------
Table 24
Spark Source Mass Spectrometry Data
Sample No: IC310
Concentration in us/™3
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
MC
0.40
22.
MC
0.051
0.17
1.0
0.11
8.0
MC
NR
2.8
1.4
MC
22.
0.74
16
0.28
0.17
0.11
MC
0.23
6.3
1.1
0.28
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Cone.
0.17
NR
STD
0.023
MC
2.3
8.6
14
0.023
MC
MC
NR
2.4
2.4
2.8
2.4
NR
NR
MC
MC
2.0
0.029
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
16.
1.03
0.057
0.45
MC
0.057
MC
MC
MC
0.04
0.034
0.057
1.1
1.6
0.028
0.85
MC
0.11
2.2
18.
0,11
6.3
12
20.
49
-------
Table 25
Spark Source Mass Spectrometry Data
Sample No: ICIF
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
MC
0.034
2.7
MC
0.012
0.012
0.30
0.006
MC
MC
NR
0.75
0.05
0.44
2.4
0.16
0.56
0.028
0.012
0.009
MC
0.016
0.72
0.031
0.019
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in u«/m3
Cone.
0.019
NR
STD
0.002
MC
0.34
0.78
0.91
0.003
MC
MC
NR
0.16
0.14
0.001
0.075
NR
NR
MC
MC
0.066
<0.0006
Element
Rhodium
Rub id ium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
1.1
0.16
0.066
0.05
0.009
MC
0.009
MC
2.1
MC
<0.002
<0.001
0.006
0.069
0.18
0.002
0.028
MC
0.016
0.15
1.0
0.016
0.26
MC
0.84
50
-------
Table 26
Sample No:
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Spark
IPW
Cone.
MC
0.11
MC
MC
0.009
0.022
0.14
2.3
MC
MC
NR
0.39
0.04
MC
MC
0.34
MC
0.031
0.018
0.017
MC
0.026
0.22
0.061
0.001
0.018
Source Mass Spectrometry
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in u.g/m3
Cone,
0.022
NR
STD
0.013
MC
0.57
1.2
1.9
0.0035
MC
MC
NR
3.0
0.184
MC
6.14
NR
NR
MC
MC
0.08
<0.002
Data
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
r\r\r\f*
^*\JH\* •
0.39
0.061
0.04
0.36
MC
0.61
MC
2.7
MC
0.003
0.009
0.70
0.23
0.0022
0.061
MC
0.066
0.19
1.1
0.018
0.22
MC
0.57
51
-------
Table 27
Sample No: Ix
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
NR
tree Mass Spectrometry
Concentration in y.g/m3
Element Cone.
Holmium
Hydrogen
Indium STD
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury NR
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen NR
Osmium
Oxygen NR
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Data
Element Cone
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium MC
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc MC
Zirconium
52
-------
Sample No:
Table 28
Spark Source Mass Spectrometry Data
imp ]_
Concentration in u-
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone. Element Cone.
Holmium
Hydrogen
6 Indium STD
200 Iodine 2
Iridium
Iron 100
Lanthanum
Lead
2 Lithium
Lutetium
NR Magnesium
Manganese 20
Mercury NR
Molybdenum iQQ
70 Neodymium
3 Nickel
Niobium 0.4
Nitrogen NR
Osmium
Oxygen M
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Element Cone
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium 10
Silicon
Silver
Sodium
Strontium
Sulfur 500
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin 1
Titanium 20
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
53
-------
Table 29
Spark Source Mass Spectrometry Data
Sample No: II C 310
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
0.67
MC
MC
0.0037
0.30
0.37
11.
2.8
MC
NR
0.30
0.64
MC
4.9
7.5
17.
0.030
0.015
0.011
MC
0.022
1.6
0.19
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in u.g/m3
Cone.
0.019
NR
STD
2.0
MC
0.19,
140.
1.1
0.0038
MC
NR
1.0
0.11
3.2
0.037
NR
NR
MC
0.037
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
MC
0.075
0.026
0.53
0.34
4.1
MC
0.15
0.0075
2.1
0.075
0.0037
0.19
4.9
0.56
0.075
0.60
0.019
0.075
MC
0.30
54
-------
Table 30
Spark Source Mass Spectrometry Data
Sample No: II C 1 F
Concentration in mR/m3
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
0.87
MC
MC
0.0043
0.11
0.41
6.5
2.8
MC
NR
0.17
0.54
0.13
1.7
10.
0.021
0.0065
0.015
MC
0.022
1,5
0.043
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Cone.
0.0087
NR
STD
3.5
MC
0.11
20.
0.065
<0.002
MC
NR
1.3
0.043
0.065
0.0065
NR
NR
MC
0.022
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
9,7
0.043
0.022
0.35
0.15
7.1
0.086
0.011
0.26
<0.002
0.086
2.8
0.50
0.043
0.17
0.0065
0.043
MC
0.15
55
-------
Table 31
Spark Source Mass Spectrometry Data
Sample No: II pw
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysposium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
0.41
MC
MC
0.0008
0.15
0.087
2.0
1.1
MC
NR
0.14
0.14
0.17
0.70
7.1
0.0044
0.0026
0.0053
5.5
0.0053
0.53
0.053
0.0017
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in mg/m3
Cone.
0.0026
NR
STD
0.44
MC
0.096
MC
0.22
<0.0008
MC
NR
0.59
0.026
0.44
0.0018
NR
NR
MC
0.0088
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
5.2
0.026
0.0026
0.23
0.096
0.53
0.044
0.0017
0.57
0.017
< 0.0008
0.017
0.070
0.13
0.070
0.070
0.0026
0.017
MC
0.11
56
-------
Table 32
Sample No: II x
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
NR
iurce Mass Spectrometry
Concentration in mg/m3
Element Cone.
Holmium
Hydrogen NR
Indium STD
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury NR
Molybdenum
Neodymium
Nickel
Niobium
Nitrogen NR
Osmium
Oxygen NR
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Data
Element Cone.
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium HC
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
57
-------
Table 33
Sample No:
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysposium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Spark Source Mass Spectrometry
II imp 1
Concentration in mg/m3
Cone. Element Cone.
Holmium
Hydrogen NR
.1 Indium STD
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
NR Magnesium
Manganese o . 7
Mercury NR
Molybdenum
Neodymium
Nickel u . 5
Niobium 0 . 04
Nitrogen KR
Osmium
Oxygen NR
MC Palladium
Phosphorus
0,05 Platinum
Potassium MC
Praseodymium
Rhenium
Data
Element Cone.
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium o . 4
Silicon
Silver 0.4
Sodium
Strontium
Sulfur 0.7
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
58
-------
Table 34
Spark Source Mass Spectrometry
Sample No: coal
Data
Concentration in rag/Kg
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Cone.
>110
0.9
11
810
0.1
220.
2
2
860
NR
7.
0.1
26
2
12
0.2
0.3
2
<2.
Element
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Needy mium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
Cone.
NR
STD
0.2
MU
5
9.
40
350
MC
NR
6
1
12
1
NR
NR
780
120.
MC
1
Element Cone.
Rhodium
Rubidium 1
Ruthenium
Samarium 0 . 8
Scandium 1
Selenium 3
Silicon 39
Silver 1
Sodium MC
Strontium 37
Sulfur MC
Tantalum
Tellurium
Terbium 0 . 1
Thallium
Thorium <1
Thulium
Tin 3
Titanium 300
Tungsten
Uranium <0.8
Vanadium 9
Ytterbium
Yttrium 4
Zinc 33
Zirconium 74.
NR - Not quantified
All blanks are elements not detected, detection limit 0.1 ppm
MC - Major component, >1 g
59
-------
Table 35
Sample No:
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Carbon
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Dysp'osium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
spars
coke
Cone.
MC
1
14
240
0.5
3
6
3
MC
NR
10
1
38
10
30
0.3
0.5
5
2
Source Mass Spectrometry
Concentration
Element
Holmium
Hydrogen
Indium
Iodine
Irldium
Iron
Lanthanum
Lead
Lithium
Lute ti urn
Magnesium
Manganese
Mercury
Molybdenum
Needy mium
Nickel
Niobium
Nitrogen
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Potassium
Praseodymium
Rhenium
in H»S/KK
Cone.
NR
STD
0.3
MC
14
7
46
MC
560
NR
12
4
17
7
NR
NR
710
0.8
MC
2
Data
Element
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium
Cone.
14
2
4
1
MC
3
MC
110
MC
<0.8
0.1
3
5
MC
4
41
5
110
210
NR - Not quantified
All blanks are elements not detected, detection limit 0.1 ppm
MC — Major component, >1 g
60
-------
5. Microscopic Analysis
The photomicrographs of IC310 and IC1F were made at 1/10 second and
those of IIC310 and IIC1F were made at 1/5 second.
The observations on the four particulate samples examined are as
follows:
IC310 - Consisting mainly of isotropic spheres ranging in sizes from
3 to 10 ym, with a few larger, up to 30 ym. While predominan-
tly colorless, the spheres did include some that were opaque,
red, green, and yellow. A few non-spherical birefringent
particles were also present. All particles had refractive
indices greater than 1.515.
IC1F - Appearing to be identical to IC310, except that the spheres
were less agglomerated.
IIC310 - Containing mostly opaque particles mostly less than 1 ym
diameter, "but some up to 6 ym in diameter. The larger particles
might have been agglomerates of smaller particles. A few
birefringent needle like particles were also seen. The re-
fractive indices were greater than 1.515.
IIC1F - Appearing to be the same as IIC310 except very few particles
larger than 1 ym.
61
-------
IV. Conclusions
These tests at a closed metallurgical furnace ferroalloy production
facility were directed towards determination of emissions of particu-
late and polycyclic organic material.
The particulate emission data acquired during these tests are pre-
sented in Table 36. An appropriate reference point for evaluating
the particulate loading in the effluent is provided by the new source
performance standards for ferroalloy production facilities. These
specify that emissions of particulate matter from a control device
shall not exceed 0.23 kg/mw-hr while standard ferromanganese or
silicomanganese is being produced, and that opacity shall not exceed
15% (21). Observations made by the sampling team indicate that
opacity exceeded the U.S. new source performance standard. The
measured loadings of 17 kg/mw-hr upstream of the scrubber during
ferromanganese production indicate that an efficient particulate
control device (>98.6% removal) is required in order to meet the
standard. Measurements made downstream of the Venturi scrubber
during silicomanganese production show a particulate loading of 0.016
kg/mw-hr. This is well within the new source performance standards.
Because of the process change, these data cannot be used to obtain a
quantitative estimate of scrubber efficiency for particulate control.
At least part of the observed thousand-fold difference in particulate
loading between the two tests may be due to the process change.
However, it is also quite probable that the Venturi scrubber did
have sufficient capacity to control the ferroroanganese production
particulate emissions at or below the 0.23 kg/mw-hr performance
standard at the scrubber exit.
The results of the organic analysis are summarized in Table 37, which
lists all categories of compounds found to be present at concentrations
of 0.5 mg/m3 or higher. Extremely high quantities of organic materials
were found in the ferromanganese effluent gas at the bypass to the gas
cleaning system, upstream of the Venturi scrubber. Fused aromatic
62
-------
Table 36
Summary of Particulate Emission Data
Sampling Site
Process
Effluent Flow Rate
m3/sec
m3/hr
Particulated Concentration
ffig/m3
Particulate Emissions
kg/hr
Average Furnace Power
MW (megawatt)
Particulate Emissions
kg/MW-hr
Upstream of
Venturi
Ferromanganese
1.20
4300
68000
290
17.3
17
Downstream
of Venturi
Silicomanganese
1.51
5400
64
0.35
22.5
0.016
63
-------
Table 37
Summary of Organic Analysis Results; Major Components
Concentration, mg/m3 *
Process
Sampling Site
Compound Categories
Aliphatic Hydrocarbons
Aromatic Hydrocarbons
Fused Aromatics < 216 MW
Fused Aromatics > 216 MW
Heterocyclic N
Heterocyclic S
Ketones
Esters
Carboxylic Acids
Organic Gases
(GC1 & GC2)
Ferromanganese
Upstream of
Venturi
6.9
3.7
380
450
80
37
67
0.9
4.3
l,030ppm
Silicomanganese
Downstream of
Venturi
2.5
23
14
0.02
0.1
1.7
0.8
1.8
0.7
3,090opm
Gas volumes are corrected to standard conditions of 101 KPa
(29.9" Hg) 2nd 21.1°C (70°F).
64
-------
hydrocarbons having a wide range of molecular weights were identified.
The presence of fused aromatics of molecular weight greater than 216
at 450 mg/m3 is of particular concern, since this compound category
includes some polycyclic aromatic hydrocarbons recognized as
carcinogens. Moderate amounts of heterocyclic nitrogen and sulfur
compounds as well as polycyclic aromatic ketones were also found in
these samples. The concentration of carcinogenic material could be
very high in this unscrubbed gas stream.
On the other hand, the major organic compound categories found in
the silicomanganese effluent gas after it had passed through a
Venturi Scrubber were simple aromatic hydrocarbons and "low" molecular
weight fused aromatics, both in the TCO range. The concentration of
carcinogenic species appears to be low.
It is significant to note that the Level 2 GC/MS analysis gave results
that were in very good agreement with the qualitative and quantitative
data generated in the Level 1 organic analysis. (See Tables 18-20).
Because of the different processes sampled, one cannot use these data
to quantify the effectiveness of the gas cleaning system for removal
of potentially harmful organic species from the effluent. However,
examination of the process data allows some inferences to be drawn.
The major sources of polycyclic organic material in the ferroalloy
process effluents are the self baking carbon electrodes and the coal
and coke added to the feed. Table 38 summarizes process data which
show that these two potential sources of polycyclic organic material
were of comparable magnitude in the two tests. It is reasonable to
hypothesize, therefore, that comparable quantities and types of POM
compounds were produced in the two ferroalloy processes. The emissions
data, also summarized in Table 38, show that total organics collected
by the SASS train and aromatic hydrocarbon levels are lower by more
than an order of magnitude for the samples collected downstream of the
05
-------
scrubber. Furthermore, the emissions of high molecular weight POM
are lower by more than four orders of magnitude for samples collected
at the Venturi exit. These reductions in POM emissions are almost
certainly too large to be accounted for by the process change alone.
The Venturi scrubber appears to be effective for POM removal and
especially efficient for species in the molecular weight range
(MW>216) that includes the recognized carcinogenic POM This is
consistent with the fact that the higher molecular weight POM have
lower volatility, are more condensable, and are probably scrubbed
from the quenched gas stream as particulate material (condensed,
or adsorbed on solid particuate).
The on-site gas analysis data indicated that emissions of gaseous
hydrocarbons (GC1 and GC2, b.p. < 50°C) were higher in the silico-
manganese test than in the ferromanganese test, by a factor of
three. Levels of these gaseous species would of course be essen-
tially unaffected by the wet scrubber. It could be possible that
these results indicate a significant shift in the chemical com-
position of the organic emissions, with the silicomanganese process
yielding a much higher gas-to-POM ratio than the ferromanganese
process. This seems unlikely in view of the general similarity of
the two ferroalloy process chemistries. The most plausible conclusion
from these results is that total organic emissions (gases plus SASS)
may have been somewhat higher in the silicomanganese test than in the
ferromanganese, and that the scrubber was even more effective for POM
removal than the data in Table 38 imply.
Inorganic chemical emissions from ferroalloy plants were not the
major focus of these tests. However, two features of the inorganic
analysis data are worthy of comment. First it should be noted that,
while trace metal levels in the effluent from the Venturi scrubber
during silicomanganese production were low (generally «1 mg/m3),
the estimated arsenic emission level is 250 yg/m3 (Table 21).
66
-------
Comparison of this estimate with the EPA Multimedia Environmental
Goals - Minimum Acute Toxicity' Effluent (MEG-HATE) criterion of 2 yg/tn3
for arsenic and its compound^ (22), suggests that more extensive,
Level 2 analyses of arsenic in ferroalloy plant emissions may be
warranted.
Second, it is interesting to compare the results of the atomic
absorption spectroscopic (AAS) and spark source mass spectro-
scopic (SSMS) analyses for the two elements that were determined
by both techniques. Table 39 presents the results of the arsenic
and antimony determinations for a number of the SASS train sample
components. (Samples for which the SSMS result was "major
component" are generally omitted from the table). The agreement
between the AAS and SSMS data for arsenic is surprisingly good.
In fact, the agreement is generally much better than could be
expected, considering that individual SSMS determinations are
uncertain within a factor of two or three. The agreement between
AAS and SSMS for antimony is not quite so good. Note, however,
that the antimony concentrations are low about 103 times lower
than arsenic levels. The two sets of antimony data do agree,
within a factor of ten, for the two samples corresponding to concen-
trations of about 100 yg/m3. Since the MATE value for antimony is
500 yg/m3 (22), these results suggest that SSMS analysis may be as
adequate for both antimony and arsenic, as it is for analysis of
other trace inorganics at Level 1.
67
-------
Table 38
Summary of Process and Effluent Parameters
Sampling Site
Process
Upstream of
Venturi
Ferromangane.se
Downstream
of Venturi
Silicomanganese
Electrode Consumption
Ib/day* 6,150
lb/m3 of stack gas ** 0.059
Coal/coke content of 14.5
Feed, %*
Emissions, mg/m3
Total Organics (SASS train) 1,200
Total Aromatics 830
Aromatics of MW> 216 450
Volatile Organics (GC1 & GC2) 1'030
9,000
0.069
14.9
50
26
0.02
3,090
* Calculated from data in Table 1
** Calculated from data in Tables 1 and 6
68
-------
Table 39
Comparison of AAS and SSMA Data for
Sample
Particulates
I C 310
II C 310
II C IF
Impingers
I Imp I
II Imp I
Solids Parr
I X
II x
Coal
Coke
Arsenic and
Arsenic
mg/m^
AAS
0.018
24
25
0.0062
0.15
Bombed for SSMS
0.098
1.03
20 rag /kg
20 mg/kg
Antimony in Selected Samples
Antimony
yg/m3
SSMS AAS
0.022 0.02
MC* (>27) 150
MC* (>21) 88
0.0068 0.025
0.15 1.3
**
n.d. 1.
**
n.d. 19.
11 mg/kg 0.3 mg/kg
14 mg/kg - 0.6 mg/kg
SSMS
n.39
660
840
**
n.d.
A **
n,d.
**
n.d.
**
n.d.
O.P mg/kg
1 mg/kg
**
Major Component
Not detectable, or < 0.1 ppm weight in sample analyzed
69
-------
IV. REFERENCES
1. R.G. Ratzlaff, "Construction and Operation of a New Ferromanganese
Facility," paper presented at the 32nd Electric Furnace Conference
of the Metallurgical Society of AIME, Dec. 1974, Pittsburgh.
2. J. W. Hamersma, S.L. Reynolds, and R.F. Maddalone, IERL-RTP
Procedures Manual: Level 1 Environmental Assessment EPA-600/2-76-
160a, p. 8, 257-850/AS
3. Federal Register, June 8, 1976, pp. 23063-23069.
4. Federal Register, June 8, 1976, pp. 23069-23070.
5. Federal Register, June 8, 1976, pp. 23072-23076.
6. Revised Organic Analysis Procedures for Level 1 Environmental
Assessment, under Sub-case T.D. 10102, ADL Monthly Report to EPA
68-02-2150, Oct. 1977.
7. Rao, C.N.R., "Chemical Applications of Infrared and Raman Spectro-
scopy," 1st. Ed., Academic Press, London, England, 1963, 683 pp.
8. Colthop, N.B., Lawrence, H.D., and Wiberley, S.E., "Introduction to
Infrared and Raman Spectroscopy," 1st. Ed., Academic Press, London,
England, 511 pp.
9. Cross, A.D., "An Introduction to Practical Infrared Spectroscopy",
1st. Ed., Butterworth, Inc., Washington, D.C., 1964, 86 pp.
10. Kendall, D.N., "Applied Infrared Spectroscopy," 1st. Ed., Reinhold
Publishing Corporation, New York, N.Y., 1966, 560 pp.
11. Reed, R.I., "Applications of Mass Spectrometry to Organic Chemistry,"
Academic Press, New York, 1966.
12. Budzikiewicz, H., Djerassi, C., and William, D., "Mass Spectrometry
of Organic Compounds," Holden Day, Inc., San Francisco, Calif., 1976.
13. "Eight Peak Index of Mass Spectra," Mass Spectrometry Data Centre,
AWRE, Aldermaston, Reading RG74PR, U.K., 1970, 1st. Ed.
14. API Research Project 44, "Selected Mass Spectral Data," Thermodyna-
mics Research Center, Texas A & M University, College Station,
Texas, 1975.
continued....
70
-------
REFERENCES (Continued)
15. W. Giger and C. Schaffner, "Determination of Polycyclic Aromatic
Hydrocarbons in the Environment by Glass Capillary Gas Chromotogra-
phy," Anal. Chem 50, 243 (1978).
16. R. C. Lao, R. S. Thomas and J.L. Monkman, "Application of GC-MS to
the Analysis of PAH in Enviornmental Samples" in Carcinogenesis, Vol.
1. Polynuclear Aromatic Hydrocarbons: Chemistry, Metabolism and
Carcinogenesia, edited by R.I. Freudenthal and P.W. Jones, Raven
Press, New York (1976).
17. A. Hase, P. H. Lin and Ronald A. Hites, "Analysis of Complex Poly-
cyclic Aromatic Hydrocarbon Mixtures by Computerized GC-MS", ibid.
18. M. L. Lee, Milos Novotny and K. D. Bartle, "Gas Chromatography/
Mass Spectrometric and Nuclear Magnetic Resource Determination of
Polynuclear Aromatic Hydrocarbons in Airborne Particles," Anal.
Chem. 48, 1566 (1976).
19. P. Jones, J. Wilkinson and P. Strupp, personal communication.
20. "Suggested Report Format for Level 1 Organic Analysis Data" EPA
Contract 68-02-2150, ADL Report October 1977.
21. CFA Title 40, Part 60, Subpart Z.
22. Cleland, J.G., and G. L. Kingsbury, "Multimedia Environmental Goals
for Environmental Assessment", Vol. 1, November 1977, EPA-600/7-77-
136a.
71
-------
APPENDIX A
LEVEL 1 ORGANIC ANALYSIS DATA
Ai
-------
TABLE OF CONTENTS
A. LEVEL 1 ORGANIC ANALYSIS DATA
1. IX, LC Report Al
LRMS Report A1-A6
IR Report A7-A10
2. ISC, LC Report All
LRMS Report A12-A14
IR Report A15-A18
3. IIX, LC Report A19
LRMS Report A20-A26
IR Report A27-A30
4. IIC1F, LC Report A31
LRMS Report A32-A38
IR Report A39-A42
5. IIPW, LC Report A43
LRMS Report A44-A49
IR Report A50-A53
6. IR Report of Concentrated Extracts Before LC
IC310 A54
IC1F A55
IPW A56
IX A57
ISC A58
IIC310 A59
IIC1F A60
IIPW A61
IIX A62
IISC A63
7. Coal, LC Report A64
LRMS Report A65-A68
IR Report A69-A72
8. Coke, LC Report A73
LRMS Report A74
IR Report A75-A78
continued. ..
Aiii
-------
TABLE OF CONTENTS (continued)
Page
9. LC Report
Solvent Blank (ADL Methylene Chloride) A79
Methylene Chloride Blank (from field) A80
Blank, Methylene Chloride/Methanol A81
10. Reconstructed Gas Chromatograph
IC310 A82
IC1F A83
IPW A84
ISC A85
A86
A87
IX A88
IISC A89
Aiv
-------
LC REPORT
SAMPLE: -X X .-
Total Sample 1
Taken for LCZ
Recovered3
Fraction
1
2
3
4
5
6
7
TCO
mg
IV-
^3
GRAV4
mg
A)D
10.
A^P
^TO.
/op
Total4
mg
?*•
<^^.
/
693
t '°
r.&i
1*,
3t3.
Concentration^
mg/M3
*•?
Concentration5
mg/M3
.2.32.
/r, «.
/
-------
LRMS REPORT
SAMPLE: _'-- A i . r\r* r «*• «L»K tr »"->»^> ^ «-^ < < • *— ^ ' * «" — K"^ • -«• , .
Via jo r Categories
Intensity
te>o
1
Category MW Range
- ite <»
ff
Sub-Categories, Specific Compounds
Intensity
10
I O
I 0
\ L>
/ O
^ C-O »A.
Other
Category
Q^r» ^C^^-fi—
/
y i/^o
^ f^t t /MtfL 0 fM«tAA*n.4+
A 2' V ^ /"^*^
A/A« V*L^JL«L \A*r*A
W
-------
LRMS REPORT
SAMPLE:
Major Categories
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
/OQ
Ll ff^Vl
(-0.
.vWy- ? -
'-LJ~
— Aif^rti ***-Jt^*M _
» 0
AUfu?
1 Qit
eusttt
Other
-------
LRMSREPORT
SAMPLE:_
Major Categories
Intensity
Category
MW Range
toO
U2-
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
foo
TJLA.
ro HA
J£*L
M^
i o
( o
JX
6
'.<•: £f.
_L?_
?T
_L2_
Uv^
J-B-
(0
Other
-------
LRMS REPORT
SAMPLE:.
Major Categories
' I'
// fin tn
/frn.
Intensity
Category
MW Range
IQ.
(Q.
-S
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
?
rv
//.
O,
H» £. &
Other
AS*
-------
LRMS REPORT
SAMPLE: t
c /. t,Q
Major Categories
Intensity
Category
MW Range
, C
/*«-
/>*-
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
fltJk
6* yl ( »jJby
*±
J
+*
f
lt- *J
H,, tJ
o
li-
Other
-------
IR REPORT
SAMPLE:
- /
Frequency
(cm'1 )
Intensity
Aiiignment
Comments
IA)
II
IR REPORT
SAMPLE: ty-3 J LC.?- r XAt> fc*tvtVcA~ , \)Q.*\^f\ ^CAM^er
Frequency
(cm'1 )
Intensity
Attignment
Comments
/I-7
-------
IR REPORT
SAMPLE :
>• 3
Frequency
(cm'1 )
X,lt>o- 3cot>
tLoo- , t*J
S
Assignment Comments
• /
autpv**/nc- jnx ofe.t\»le^ L,H
V>tX^«.r»Ki <^\M^Y p i>AwJi C^K./ 4t>
A/eKXAjf.c virtflA
VY\KAl4. »fa^ /Ji. 4 C rfV^> "f I *^» f SX(A0 JL to
A* v trv^s A *Y i r ^ »' w-^ &
5
IR REPORT
SAMPLE: T. Y —
.
9 V ^-
Intensity
tl p K'I /< i" t /A*^ ^
*r f
Assignment Comments
^*ft ^L U {• V^Sfo'fl t~* S
•^ f
-------
IR REPORT
SAMPLE:
Frequency
Icm'1 )
Intensity
Assignment
Comments
rt-
|R REPORT
SAMPLE..
Frequency
(cm'1 )
A),
Intensity
4- / A.' / ;/**
(• T
Assignment Comments
-»x,.-f --7.^ «* (^ ««-/>/• **» -f
^ T
-------
IR REPORT
SAMPLE:
Frequency
(cm-' )
Intensity
Assignment
Comments
w
/ *K
.occ ,18*0
Vn
f. H .
~ZoOQ -
i/J
(11'-
w\
£•=..
/A
- me
5
' /** * jt
*^*i
5,
J^L
Hyk"^
/ b 1 o ( / y o o
ft&O
and -
-tr A^ '
A 10
-------
LC REPORT
SAMPLE: -
f
Total Sample1
Taken for LC2
Recovered3
Fraction
1
2
3
4
5
6
7
TCO
mg
1*.*
IU-.T
/4-,7
TCO4
mg
0. 03
9. 0 1
/a. 3
o.o L>
/OP
r/D
o. o z.
GRAV
mg
4r
<•».
^r.3
Total
mg
££.d
^7
5-^J.
Concentration
mg/M3
^.5-^
^*» > ^* — |
GRAV4
mg
Z, 0.^
/.r»
*s.r
A>0.
O.^r
2 7SI
*!•
1 /
*. 0 to
19. »'^'
a,7r
o.»-7
Concentration
mg/M3
A
-------
LRMS REPORT
SAMPLE: M
V
erro
m\o
Major Categories
Intensity
Category
MW Range
10O
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
-------
LRMS REPORT
SAMPLE:_
Major Categories
U
l-SC-3
Sub-Categories, Specific Compounds
Intensity
loo
Category
m/e
Composition
10
10
-V'i
A
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
/ o
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
loo
/?•***
10
10
rHlO
ft?
ft t>
//
Other
-------
IR REPORT
SAMPLE.
Frequency
(cm'1 )
Intensity
Assignment
Comments
5
IR REPORT
SAMPLE:
LL1-
Frequency
(cm'1 )
Intensity
Assignment
Comments
CJL
-------
IR REPORT
SAMPLE:
Frequency
(cmM )
Intensity
Assignment
Comments
en
/c.
10 .
<— r>
IR REPORT
SAMPLE;
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
-yio $.
(j
Intensity
'-b ' eA /**»+-
T
Assignment Comments
^e ba~Jz
R REPORT
SAMPLE: T ^ £ - j£ Lc, £ > ff^-t*- » t ' ( (^ . ^ ^'t $ C*~> tft*^...
Frequency
(cm'1 )
Intensity
Assignment
Comments
1rr\
JL±L
«.^
J O&O-
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
Intensity
Assignment
Comments
Ctf
Cs-e
A t-<
IR REPORT
SAMPLE:
Frequency
(cm'1)
Intensity
Assignment
Comments
-------
LC REPORT
SAMPLE:
f 0/1*0M&vt
Total Sample 1
Taken for LC*
Recovered^
TCO
mg
^7?
, O /
/ O » (0
n , o
GRAV
mg
IJ.ZO
7*,*
^, 2-
Total
mg
/^-/A
^W'. 2-
Concentration5
mg/M3
/// 0
Fraction
1
2
3
4
5
6
7
TCO4
mg
*.*£
3. <*.£
1 °l £ •
tt*i
A. IS
7-°i ,-)
tt .
GRAV4
mg
3.0
b
s 67
^-fi
3.0
Total4
mg
£•, >^
9 4t^
/O ^i
^_fl
^ t£
IS. 0
3-3
Concentration
mg/M3
3.06
£ ^
-78 /
t> 73
88
/?,
1. Quantity in entire sample, determined before LC
2. Portion of whole sample used for LC, actual mg
3. Quantity recovered from LC column, actual mg
4. Total mg computed back to total sample
5. Total mg divided by total volume
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
/ oo
i
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
A
-------
LRMS REPORT
SAMPLE:_ J X -.2
/'
Major Categories
Intensity Category MW Range
/z? A'KM^A^Lct po^L*~diitt* n. AA, tSH^+Ji Cxa a./>o- »x>^
/O -TXv^lAu?! A.^o>
Composition
^ ///«
w t> ff /fl
Other
-------
LRMS REPORT
*j-UTir •-»-• jlf— •* V « * — : — "• f xf
Major Categories
Intensity
/ O 9
i o 0
f a f
/ O
Category
r^lV A-rrmJi^
V^ ^ « ^ A^n^^fii^ r>*-i£>
n J
d '
MW Range
l*2,-*40
-*<6-3JTO
!&-(*-
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
(00
£«J
C\MTiMiL
ft^jjC.
J_^-
Other
(?A-H-
aJT
^^g *-.
pA-H
tJC
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
^L
A)
/QO
/ 0
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
/ &e
Ct* H* /J
)
JtLa.
M^L
U2-
(0
JL
10
to
C
J-£-
*Z±
7 A/||r>J
-U2-
-/£-
Ifc^VVA^
^^^/.
^2-
-M2-
Other
-------
LRMS REPORT
SAMP LE: tL X
Major Categories
Intensity
Category
MW Range
(00
IG-
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
/£-
ia_L
**ff
-02-
V
_L£_
f
T
J-Q-
.E
/.£-
^
H..
t4.f^\
n O
Other
/£_
fAH
j_£.
0 x
M^ex>
fir*
f
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
100
/\ }
(00
r"
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
/gg>
/c?o
"ft
M
0 O
„
y 'v
L,tr H* O
H>, A
Ht,
to
Ctu. Htt H.
10
rr\
to
10
lO
CtLHn
10
I 0
Other
-(-CL
PAH
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
/ o
/I/
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
4-0-
4
i O
/\J
f 0
r5 \ -
fJ
•*—r t-*-*K—T-
,*> H,, (J
(0
o LM^» * £• ^^
,0/J
^4
jLi2_
Z£L
^
u\
' U. ^/»
Other
-------
R REPORT
SAMPLE: fiX" 1 Lf^l . XA? £xfr*,ct" . T=^VU> fJL&O<~\
Frequency
(cmM )
*(?C*--*S'»
'£00- Ufa
4
' ' Q
Intensity
^
Y*
Assignment Comments
£ ^ s f(jt tff /L-* 1 ^ —
|R REPORT
SAMPLE: JI X - 2- . L <-
Vfto
t
Frequency
(cm'1 )
Intensity
Assignment
Comments
S
-u-
-------
IR REPORT
SAMPLE: 1L* -
X frfr
Frequency
(cm'1 )
Intensity
Assignment
Comments
I&OO -
* ™*rf
--7* +
IR REPORT
SAMPLE:
3±
Frequency
(cm'1 )
Intensity
Assignment
Comments
^H-
ltlf-0
JL
f", '>*»
JV/
/
•9-
Luii^
^f
i»jO
A a-8
-------
|R REPORT
SAMPLE:
. *AP
Frequency
(cnf1 )
Intensity
Assignment
Comments
vO
0
u)
•0
A,
(leo
\f^h
|R REPORT
SAMPLE:
Ur-Ct ,
+
Frequency
(cm'1 )
Intensity
Assignment
Comments
Vvj
IA)
n« y
^•?^
Lkl
u>
IA)
.7 fro. 7*^
-------
IR REPORT
SAMPLE: J^X-OJ LC J
XAQ LK4ra.Ct . f-tVLo^A^L.
<&^ex-*~
Frequency
(cm"1 )
Intensity
Assignment
Comments
Y\r
£±
IR REPORT
SAMPLE:
Frequency
(cm"1 )
Intensity
Assignment
Comments
-------
LC REPORT
SAMPLE: -
Total Sample1
Taken for LCZ
Recovered3
Fraction
1
2
3
4
5
6
7
TCO
mg
—
—
—
TCO4
mg
—
—
—
—
—
—
—
GRAV
mg
u.
t 3.*.
t*^
GRAV4
mg
AJO
AJ D
52
/tt.
A>D
/*
». »
Total
mg
&(,.«.
/3. *.
/3. a.
Total4
mg
/UD
Av>D
^0.
/ **•
AfJl
,8
1. Quantity in entire sample, determined before LC
2. Portion of whole sample used for LC, actual mg
3. Quantity recovered from LC column, actual mg
4. Total mg computed back to total sample
5. Total mg divided by total volume
(,. root P^4«e- -U-Uo.
Concentration^
mg/M3
^^,8
Concentration5
mg/M3
fc/O
^P
^i
f g
tJ D
/3
l.&f
-------
LRMS REPORT
SAMPLE: P
Major Categories
Intensity
Category
MW Range
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
\9H
Other
-------
LRMS REPORT
SAMPLE: N\ Qr\Sa/\\Q
A\\Q
Major Categories
Intensity
1
1_
Category
U \ i • C toO fl f\
HeA-e-x-CKLucAAc ouJlW-r V.<»f^pc)uo^Jiv
MW Range
\?^
£ Z90
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
U \o
Other
-------
LRMS REPORT
SAMPLE:
(\\\0 u
M«)or Categories
TL-C1F-3
Intensity
Category
MW Range
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
loo
D
too
\00
H H
\0
^
^t£.
10-L
U
SHX
/
-------
LRMS REPORT
SAMPLE: I^Aovx ^(Xv\Vo Ferro f\ \\O c^ TL ~C1_F - H
Major Categories
Intensity
10
J • .
Category
^
MW Range
>aib
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
\Q
302.
I 0
10
U
10
asa.
C-toU
ii.
Oev\1
Other
Vo yrsife
-------
LRMS REPORT
SAMPLE:
TL- CIF-5T
Major Categories
Intensity
Category
MW Range
10
10
301
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
V \
3031
O
Other
-------
LRMS REPORT
SAMPLE:
T
(\\\<
Major Categories
Intensity
400
Category
MW Range
Zoo-
C
ur
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
loo
K)
U - v v\ O (
lo
iO
10
10
10
(W\-Wa.qUi ftpUne^ti
10
130
10
10
10
itv
Other
-------
LRMS REPORT
•\Vta r*e,rco
II -
-------
IR REPORT
SAMPLE:_JLCJjfnL
_£&
ftJjL*. < / 4A.
"^m*>Vfl**>j4L*44*-
Frequency
(cm'1 )
Intensity
Assignment
Comments
|R REPORT
SAMPLE:
<-/ 4JL .
-T^t^o fnA^\J,
Frequency
(cnV1 )
\\0 <>'[
I
Intensity
p\L\{£iLvC[ "X.
Assignment Comments
S /tti«o*> •/•'«> n_
'
-------
I R REPORT
SAMPLE:
J-
< 1
Frequency
(cm'1 )
Intensity
Asiignment
Comment!
'JL
. Mo
tj
-C-o
it
IR REPORT
SAMPLE:
r
Frequency
(cm"1 )
Intensity
Assignment
Comments
-vn-
-------
|R REPORT
SAMPLE:
|R REPORT
c AMPLE: HUf
-f&U
Frequency
(cm"1 )
Intensity
Assignment
Commdnts
Cff
1 C
s
S
&
-------
IR REPORT
SAMPLE:
Frequency
(cmM I
-V\tf 2
Intensity
i« f >Vii / i tAWT"
/ T
R REPORT
SAMPLE:
Assignment Comments
-Lit CLMtMf?t>*&
Frequency
(cm"1)
Intensity
Assignment
Comments
-------
LC REPORT
SAMPLE: _JZ-^
Total Sample 1
Taken for LC*
Recovered3
Fraction
1
2
3
4
5
6
7
w . »».
TCO
mg
—
—
—
TCO4
mg
-
•—
—
—
— "
»«L VOASA
GRAV
mg
£•/
a-C*
3*
GRAV4
mg
.», ^-T
AVp *
^ *?
— 1 1 .
/,16
-p^m^ .
^
Total
mg
J-/
j,^-
3A
Total4
mg
J A^"
vo
59
^
ff. 73
/.^^
' "~ 1
Concentration5
mg/M3
37.
Concentration5
mg/M3
•£
O-A
o re-
7 * 1
/. V-V-
1. Quantity in entire sample, determined before LC
2. Portion of whole sample used for LC, actual mg
3. Quantity recovered from LC column, actual mg
4. Total mg computed back to total sample
5. Total mg divided by total volume
-------
LRMS REPORT
K
>*o F
g-x-y-Q
ftV\OH
Major Categories
Intensity
Category
Range
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
-------
LRMS REPORT
SAMPLE: KcmSQurAo £e.<-ro ft\Vo «^ ~^TL - *? LO - ,Q
Major Categories
Intensity
10
nx"Ofrr\Q>\t. n u JvToca-r^oowi 7 7 «Mu*id) ^^ AvnWVic eV^f^ ^-^ ^i.^rv
• •«..... IB — ae : "**la- *— \
-------
LRMS REPORT
SAMPLE:_ ^
Major Categories
Intensity
Category
MW Range
yoo
yoo
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
loo
Z01
IOQ
loo
ro
10
1P_
10
10
10
_10_
10
3o^
.10.
Other
-------
LRMS REPORT
SAMPLE: KgmSOurVo
Major Categories
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
loo
loo
VO
U i
10
10
10
ayg
r
a op.
Cvutt.
Other
^90 ^
-------
LRMS REPORT
SAMPLE: (l
,rro
TL -
Intensity
Y&o
vo
1
Category
/^a.+t> n«..$
UtAerO C.^cJn'c KKWOQ«». Cfrr^QQV*-*^-*
r Efw* .
MW Range
300+
zoo - 300'*'
Sub-Categories, Specific Compounds
-------
LRMS REPORT
SAMPLE: Hor\Sa*vVo YC-tro A\\oM *\V. ~ T^ljJ - ^
Major Categories
Intensity
\o
. 1
(1
Category MW Range
\\J8.
\t°(
TJt>T>
l&u
^^<\
^s•3
z $y
a^ mJ£ a j&
o si \
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
?000- *&ot>
/tOO . &00
Intensity
s
Viv
Assignment Comments
C-H • Oil i phfJi i c. — .
CM t M
R REPORT
SAMPLE: 3L i? \tf ' 3 //'i. PtP^C. ftWA. . f^LK) MS^H [&* £-±3.
' ' < Q
Frequency
(cmM )
Intensity
Assignment
Comments
UJ
f\s*
-------
IR REPORT
SAMPLE:
3 . L(L
-------
IR REPORT
SAMPLE:
Frequency
tern'1 )
Intensity
Assignment
Comments
C ft-
^ia
. <
JL
-m
IR REPORT
SAMPLE:
, /
Frequency
(cm'1 )
Intensity
Assignment
Comments
OH
C -0 . C*L\Jl
. Jo .
J1L
£>
-------
IR REPORT
SAMPLE:
•p&vvo ***~4 i**A
f
Frequency
(cmM )
Intensity
Assignment
Comments
QH a,
loo- 1 oeo
:ri*>:
t
r^
-
<^±
IR REPORT
SAMPLE:
Frequency
(cm'1)
Intensity
Assignment
Comments
-------
IR REPORT
SAMPLE:
titnm.^u*a
Frequency
(cm-1 )
Intensity
Assignment
Comments
OH
-------
IR REPORT
SAMPLE:
Q
Frequency
(cm'1 )
Intensity
IA)
Assignment
Comments
£>// SL,
-££$
f \JtLA**
^0
C'fv/**!
-------
IR REPORT
SAMPLE:
Frequency
(cm-1 )
Intensity
. onLe
Assignment
.t c)
Comments
iff tVH
-&&*-
S
^
-------
|R REPORT
SAMPLE:
X
Frequency
(cm'1 )
Intensity
Assignment
Comments
u)
in. a
-------
IR REPORT
SAMPLE: IXC
Frequency
(cm"1 )
'3 000
boo "ooo
£di
'//
Intensity
¥
<> />
Assignment
Comments
Lti
f
'
ifl, &tftl'*t
c __
Itf
-------
IB REPORT
SAMPLE: jrf f_.
Frequency
(cmM )
^0-3(06
f?0*
t,0
Intensity
vO
s
•V«
t
Assignment
Comments
!£L
it-
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
3 &00-
Intensity
m
Assignment
r>H
-L4L
L*L
t
HM*S*A^*J^
Comments
n
-------
|R REPORT
SAMPLE: TL f>UJ } ^fnLtiL idat/L
FQrr* tYLayy^f^lA^l-A,
-------
IR REPORT
SAMPLE:
tttv\
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
4"
Intensity
Assignment
.
C
.A)
t —
YVMAjLfc. - kdLVL.
O
0
Comments
-------
LC REPORT
SAMPLE: C.OOL-
Total Sample 1
Taken for LC*
Recovered^
Fraction
1
3
4
5
6
TCO
mg
4.0
2.H
l.n
TCO4
mg
O.36"
Wt><*
O,
n.lQ
-
GRAV
mg
:^K
ax
3o
GRAV4
mg
24.
2..O
?.?
z.q
1 . J
^-.
Total
mg
39
2ft
1 a*
Total4
mg
24
2.0
firS
^,g
1 - '
S 2,
O.&tn
Concentration5
mg/Kg
m**4
Concentration
mg/Kg
2.06
24
| Q j
3^;
13
(a 2-
'Q
1. Quantity in entire sample, determined before LC
2. Portion of whole sample used for LC, actual mg
3. Quantity recovered from LC column, actual mg
4. Total mg computed back to total sample
5. Total mg divided by total volume
6.
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
yo
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
-------
LRMS REPORT
SAMPLE:
2L-3
Major Categories
Intensity
Category
MW Range
/&>
ti/c
1?L
/o
2SC,
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
(0
/o
t*
202-
A
. e-rc.
22?
ere.
252-
/ 1-
Other
fa
y
-------
LRMS REPORT
SAMPLE:
Major Categories
Intensity
Category
MW Range
100
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
T£W
/D
.252,
v^
/*.
J&C,
Other
-------
LRMS REPORT
M 0N S/WT
Major Categories
Intensity
id)
10
/a
Category
Kg-ftnOS-S
hfc.r&&>CfCLtC M/T^G-EfiJ CfaPffituJiS
"KT&&S
MW Range
/?& -n«<3So
m *> 223
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
10
-------
|R REPORT
SAMPLE: LI - I f
Frequency
Intensity
cn
Assignment
Comments
(.A\ .
|R REPORT
SAMPLE: Ci-ZL
Frequency
(cm'1 )
S*>000~3j'OQ
/at»/ ,*>~)o
Intensity
17)
IA)
Assignment Comments
(M . cd\AJJ'\t-~
CM 'n
-------
IR REPORT
SAMPLE: /-C
Frequency
-------
IR REPORT
SAMPLE:
Frequency
(cm'1 )
^ £00 -
Intensity
Aitignment
Comment*
ro_
JA!
- M
I/O
py f:<*'
_ii_
IR REPORT
SAMPLE:
C0A.1
A -71
-------
IR REPORT
SAMPLE: C L - "|
Frequency
(cm'1 )
Intensity
Asiignment
Comments
u-pb
_/sZfcL
JLJL
n »o
V
Vrv
&»-o
-1M2-
VAi
IR REPORT
SAMPLE:
Frequency
(cm'1)
Intensity
Assignment
Comments
-------
LC REPORT
SAMPLE: _
Total Sample1
Taken for LCZ
Recovered3
TCO
mg
n.^n
0.2LI
0.570
GRAV
mg
)*.
IZ.
1 I.
Total
mg
/*
/ 2..
I 2.
Concentration
mg/Kg
2.?n
Fraction
1
2
3
4
5
6
7
TCO4
mg
0. ^
f«D
o. m
*/Dk
WP
WO
^O
GRAV4
mg
10. '
rV£>
n.P/,,
O.fi/'o
i .^/
n. 6,
O. (^
Total4
mg
10.
ftp
i.n
n.R^,
1,^4
0.6,'
^) 6s
Concentration
mg/K3
1 Kft
r*P
l(n
14
2.Z,
1 0
/G
1. Quantity in entire sample, determined before LC
2. Portion of whole sample used for LC, actual mg
3. Quantity recovered from LC column, actual mg
4. Total mg computed back to total sample
5. Total mg divided by total volume
fa. HOT
-------
LRMS REPORT
SAMPLE:_
c/c
Major Categories
Intensity
/l>0
I
Category
OOU FU»€-
/>UI PHOTIC 5
MW Range
25^3
3to-HVO
Sub-Categories, Specific Compounds
Intensity
Category
m/e
Composition
Other
-------
IR REPORT
SAMPLE: £OK£
Frequency
(cm'1 )
^^O^S^TO
1450 >^^0
Intensity
m
m
IR REPORT
SAMPLE: &O KE LC.-2-
Assignment Comments
ClH-j (\H-^ Clliph^rhC-
/
Pu-z ,0 HT, ol'tp^x^Wr.
Frequency
pqoo atf<^)
\i\ /}£>, | "3* ~^-(^
Intensity
no
Assignment Comments
0.*f? ^^i oDpf-v-ir^'r.
P.H-., ;P M^a, Ollplna-j^'d.
-------
I R REPORT
SAMPLE:
F
Frequency
(cmM )
Intensity
Assignment
Comments
IR REPORT
SAMPLE:
Frequency
(cm'1 }
Intensity
Assignment
Comments
-------
IR REPORT
SAMPLE:
IR REPORT
SAMPLE:
L£L-
Frequency
(cm'1 )
2q2_n
Intensity
U)
Assignment Comments
dH* ,£^-5 al;phf>h'C-
ICE
Frequency
(cm'1 )
Intensity
Assignment
Comments
LO
OU-j UR
S
UP
Qflid,
A "71
-------
IR REPORT
SAMPLE: COk £ L(L~1~
Frequency
(cm'1 )
A4tor>
^Q^og.^ft,
II TO
ti Do
Intensity
s
6O
UJ
LO
IR REPORT
SAMPLE:
Assignment Comments
OU f KJ H ( \prnnA }
Q\(\tohp(
fllflnho/ CkfOad}
Frequency
(cm'1 )
Intensity
Assignment Comments
A 18
-------
LC Report
Sample: Solvent Blank, B, (ADL Methylene Chloride, 2500
Taken for
Recovered
Fraction
LC
1
2
3
4
5
6
7
TCP. me
0.007
0.02
« 0.01
« 0.01
0.02
« 0.01
« 0.01
« 0.01
« 0.01
GRAY, mg,
0
2.4
< 0.1
< 0.1
0.6
< 0.1
< 0.1
0.8
1.0
-------
LC Report
Sample: Blank, Methylene Chloride (from field, 828 mL)
TCO.
Taken for
Recovered
Fraction
LC
1
2
3
4
5
6
7
0.15
0.14
« 0.01
« 0.01
0.01
« 0.01
0.02
0.01
0.1
, — ,_,
2.1
2.1
0.5
< 0.1
0.4
0.6
< 0.1
< 0.1
0.6
-------
LC Report
Sample: Blank, Methylene Chloride/Methanol (from field, 541 mL)
GRAV. mg
Taken for
Recovered
Fraction
LC
1
2
3
4
5
6
7
2.1
2.1
0.25
< 0.1
< 0.1
0.2
< 0.1
< 0.1
1.6
-------
Ffn2:FER.flL.IIC-310.4/10/78.1N6JS,D400
RGC
sfco 'sbo
efeo
-------
FH28:2tJClF-i-lNGIS).D40a, 170-300/15. laflOV, 4/14
.-!SC
180
A,
pw.X-~"'
/•»
.r--:'
I •«"••" -I
50 100 ISO 200 250 300 350 400 450
100
I I I I ' I ' I ' I ' I' I ' I ' I ' I ' M 1 M I I II I II I > I I | I | I i I | I | I | I | I I M I I M M I 1 M I M I ' I I M I ' I M I I ' I
600 650 700 750 -L- -u- J— ~u~
I i I I II I M i I i I ' I I I i I i I I M I '
850 9130 950
-------
FH22: IPW-f 1NGIS .D400,170-300/15,1800V ,4/13/78
RGC
too 1(>w
\ '''''' ' ' ' I ' ' ' i ' i '' 'I'i'i'i ' i ' I ' i ' i ' i ' i ' i 'i'iiini | i i n 11 i i 11 11 11 i i ii111111
> 50 100 150 200 250 300 350 400 450
oo
*" 100
580 550 600 650 700 750 800 850 "" 900 950 '
-------
FR15:FER.RL. ISC. 4/10/78.INGIS.D400 170-300/15
RGC
100 ISC
1
> 50 100 150 200 250 300 350 400 450
lOO
500 550 600 650 700 75IJ«?00 850 900 950
-------
FR26:llClF+;NGIS.D400,170--3Cn/15,ianQV, 4/14/78
:Sr..?flSEl
ICO
EC I
04 .00
"I"
100
' I I I I 1 I I ' I I 1 I [ M M I I ' I I I M ' I ' I ' I ' [ I I I I I I I I I I I I ' I ' I I I I I I I ' I I I I I I I I I I I I I I I ' I
150 200 250 300 350 400 450
^
SBO 550 6DO 650 7DO 750 " SDO ' 850 SBO ' 950
-------
FR3D:IlPH+lNG]S,D40n,170-3QD/l5,iaOQV,4/14/78
rlSC.PflSEl
loo
IpvO
"I I ' M I 1 I ' | I 1 I
50
~1 [-1 M
100
>
00
ISO
200
250
300
350
400
450
100
>] I ; I I I I I I I I ' I ' I M ' I I I I I ' I ' I ' T I I ' I I I T M I 1 I I I I I I 1 ' I I I I I I 1 I I I 1 I 1 < I •< I I I I I I 1 I 1 ' I I I I I I I I I I I I I I I
5130 550 600 650 71QO 750 800 850 9tJO
-rrrr,
-------
>
00
00
iQO
t
FB4 :FER .RLl.lI-X,3aC: I. IUUEX40Q,170-300/15,1800
7273!. RGC 4.'4/78
iaa
1
1
!*
«!»-
, r ,,,,,,,,,,,,,,
50
MIIIM-«
100
1 1 1 1 i'i p i « t » i
ISO
""1""
200
i i-i 1 1 1 [ 1 1 1 1 1
250
300
350
""1
400
450
.. i • 111111 l > 111»i • i»I • i-"-i-^i • i'1 jp »• < • «"* • -i •'% • •' •' LLTT1
5DO 550 600 650 TOT 750
i Ttl T I 1 I I I l~l f
» 1 l I » I H ' I ' I '"I l I » I ' I l M I"1
850 9QQ 350
-------
FR14:FER.RL.JISC.4/10/78.1NB1S.D40D 17B-30D/15
100
|l|l|MI|H'TMmi»1«'|*-|n'1'TJ'T'T«-|'1']'l'1'»'M|'1'|l|'1IJIl'1'l'TI|n'1IIM'|'|l
50 100 150 200 250 300 350 400 450
100
51)0
-------
APPENDIX B
INORGANIC ANALYSIS DATA
Bi
-------
TABLE OF CONTENTS
B. INORGANIC ANALYSIS DATA
Original SSMS Data Bl
IC310 B2
IC1F B3
IPW B4
IX B5
I imp 1 B6
IIC310 B7
IIPW B8
IIX B9
II imp 1 BIO
XAD-2 Blank Bll
Imp. Blank B12
Coal B13
Coke B14
Bill
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 313 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
TO:
Ms. Julie Rudolph
Arthur D. Little, Inc.
25 Acorn Park
Cambridge, MA 02140
p. o. No.: 540530
Sample No.: I CIO + 3
Date. March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPAA WEIGHT
ELEMENT
Uranium
Thorium
Bismuth
Lead
Thallium
Mercury
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
CONC.
39
29
3
150
20
NR
£0.5
2
£0.7
5
0.4
2
0.5
3
3
5
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymium
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodium
CONC.
1
4
2
18
42
35
50
40
MC
25
0.4
0.6
7
15
STD
140
1
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
42
43
360
110
MC
290
2
8
390
19
110
220
280
50
13
MC
MC
380
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
320
MC
1
MC
MC
MC
MC
MC
MC
MC
MC
MC
MC
NR
NR
NR
18
0.9
>240
NR
NR - Not Reported
All elements not reported
MC - Major Component
<0.1 ppm weight
Approved-.
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-952)
To: Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: I C 1 + F
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT
Uranium
Thorium
Bismuth
Lead
Thallium
Mercury
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
CONC.
48
59
4
250
22
NR
£0.2
5
<0.9
6
1
5
0.7
4
6
9
ELEMENT
Terbium
Gadol inium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodium
CONC.
2
5
3
21
46
21
240
110
MC
15
0.5
£0.3
11
9
STD
MC
3
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
51
24
270
85
661
360
2
3
860
10
230
MC
180
0.3
52
MC
MC
780
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
310
MC
15
MC
MC
140
MC
MC
MC
MC
MC
MC
MC
NR
NR
NR
97
4
>290
NR
NR - Not Reported
All elements not reported
MC — Major Component
<0.1 ppm weight
Approved:
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 728-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
TO:
Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
p. o. No.: 540530
Sample No.: I PW
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
~~ ELEMENT
Uranium
Thorium
Bismuth
Lead
Thallium
Mercury
Gold
Platinum
Iridium
Osmi urn
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
CONC.
43
52
5
280
16
NR
0.2
<0.4
15
4
0.8
4
0.5
4
5
7
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmi urn
Silver
Palladium
Rhodium
CONC.
2
6
4
14
42
18
88
130
MC
9
3
0.7
24
14
STD
MC
140
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
680
31
130
50
610
88
530
83
MC
14
50
MC
MC
MC
77
MC
MC
MC
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
250
MC
9
MC
MC
MC
MC
MC
MC
MC
MC
MC
MC
NR
NR
NR
32
2
430
NR
NR - Not Reported
All elements not reported <0.2 ppm weight
MC — Major Component
Approved:
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60801 • AREA CODE 312 728-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To:
Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: j XAD Parr Bombed
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Uranium <3
Thorium
Bismuth 3
Lead 3
Thallium
Mercury NR
Gold
Platinum 4
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium 2
Lanthanum 2
Barium 9
Cesium
Iodine 0.4
Tellurium
Antimony
Tin 3
Indium STD
Cadmium 6
Silver 0.4
Palladium
Rhodium
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
4
82
3
4
0.3
4
0.7
8
0.3
100
10
16
<0.6
73
5
4
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
CONC.
0.4
59
10.4
210
520
CONT
24
29
52
470
17
>970
CONT
NR
NR
NR
CONT
NR
NR - Not Reported
All elements not reported <0.4ppm weight
MC - Major Component CONT-Contami nation
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
TO- Ms. Julie Rudolph
Arthur D. Little Inc.
25 Acorn Park
Cambridge, MA 02140
Date: March 9, 1978
p. O. No.: 540530
Sample NO.: Impinger I
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN
ELEMENT CONC.
Uranium 0.1
Thorium
Bismuth
Lead 0.03
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Haf ni urn
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymium
Praseodymium
Cerium
Lanthanum
Barium 3
Cesium
Iodine 0.02
Tellurium
Antimony
Tin 0.01
Indium STD
Cadmium 0.02
Silver 0.006
Palladium
Rhodium
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
2
0.004
0.02
0.04
0.003
0.06
0.2
0.07
0.2
0/i
2
0.04
2
0.2
0.7
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.005
0.3
<0.001
2
4
0.4
5
0.2
1
0.3
0.7
0.9
-0.5
NR
NR
NR
0.01
0.02
NR
NR - Not Reported
All elements not reported <0.003yg/ml
MC - Major Component
Approved:
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: II CIO + 3
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.; 97-A981-110-12
CONCENTRATION IN PPAA WEIGHT
ELEMENT CONC.
Uranium 2
Thorium 2
Bismuth 8
Lead 380
Thallium 55
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten 15
Tantalum
Hafnium
Lutetium 0.1
Ytterbium 0.5
Thulium 0.1
Erbium 0.4
Holmium 0.5
Dysprosium 0.8
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymium
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodi urn
CONC.
0.2
0.6
0.3
2
3
1
8
5
MC
17
54
4
18
5
STD
75
9
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
26
1
8
2
110
MC
300
14
MC
5
43
MC
460
85
200
MC
MC
130
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Sil icon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
16
130
0.7
MC
MC
MC
MC
MC
MC
MC
MC
MC
MC
NR
NR
NR
10
0.1
29
NR
NR - Not Reported
All elements not reported
MC — Major Component
<0.1 ppm weight
Approved:
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 328 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 806O1 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To:
Ms. Julie Rudolph
Arthur D. Little, Incorporated
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: II Cl +
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Uranium 2
Thorium
Bismuth 5
Lead 940
Thallium 120
Mercury NR
Gold
Platinum
Indium
Osmium
Rhenium
Tungsten 23
Tantalum
Hafnium
Lutetium <0.1
Ytterbium 0.3
Thulium <0.1
Erbium 0.3
Hoi mi urn 0.4
Dysprosium 1
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodium
CONC.
0.5
1
0.7
2
2
1
8
5
MC
25
160
4
40
4
STD
130
7
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
60
0.3
7
2
330
450
300
16
MC
2
68
MC
460
3
80
MC
MC
6
ELEMENT
Vanadium
Titanium
Scandi urn
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
8
130
1
MC
MC
MC
MC
MC
MC
MC
MC
MC
MC
NR
NR
NR
19
0.2
30
NR
NR - Not Reported
All elements not reported
MC — Major Component
<0.1 ppm weight
Approved:
c
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 80601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION. U335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Ms. Julie Rudolph
Arthur D. Little, Inc.
25 Acorn Park
Cambridge, MA 02140
p. o. No.: 540530
Sample No.: 11 P
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT
Uranium
Thorium
Bismuth
Lead
Thallium
Mercury
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
CONC.
8
2
17
MC
65
NR
15
0.2
<0.1
0.3
<0.1
0.3
0.3
0.5
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodium
CONC.
0.2
0.6
0.6
3
3
1
16
11
MC
16
50
5
47
2
STD
130
11
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
67
0.9
12
2
60
590
230
27
MC
6
60
MC
810
50
80
MC
MC
20
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
-' ••?
CONC.
8
80
0.3
MC
MC
MC
MC
MC
MC
MC
MC
MC
=630
NR
NR
NR
10
0.1
25
NR
NR - Not Reported
All elements not reported
MC — Major Component
<0.1 ppm weight
fc*
Approved:
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 80601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION. 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
TO: Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
P.O. No, 54053°
Sample No.: II XAD Parr Bombed
Date: March 9, 1978
Analyst: S. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPAA WEIGHT
ELEMENT CONC.
Uranium 2
Thorium
Bismuth 8
Lead 3
Thallium
Mercury NR
Gold
Platinum 1
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium 0.3
Cerium 0.9
Lanthanum 1
Barium 5
Cesium
Iodine 0.4
Tellurium
Antimony
Tin 0.9
Indium STD
Cadmium ±0.9
Silver 0.4
Palladium
Rhodium
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
6
59
0.3
5
0.1
2
1
5
0.1
0.2
12
3
13
0.2
44
5
5
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryl 1 i urn
Lithium
Hydrogen
CONC.
0.3
27
^0.3
260
140
CONT
7
16
310
^230
26
MC
CONT
NR
NR
NR
CONT
NR
NR - Not Reported
All elements not reported <0. 2 pprn weight
MC - Major component CONT-Contaminati on
Approved:
rt-'
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS tsl',601 • AREA CODE 312 728-8434
INSTRUMENTAL ANALYSIS DIVISION. 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Ms. Julie Rudolph
Arthur D. Little Inc.
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: Impinger II
Date: March 9, 1978
Analyst: S. Sweeney
lADNo.:97-A981-110-T2
CONCENTRATION IN
ELEMENT CONC.
Uranium
Thorium
Bismuth 0.006
Lead 0.03
Thallium
Mercury NR
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
NR - Not Reported
All elements not reported
MC — Major Component
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymium
Praseodymium
Cerium
Lanthanum
Barium O.Oj
Cesium
Iodine
Tellurium
Antimony
Tin
Indium STD
Cadmium
Silver 0.2
Palladium
Rhodium
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60801 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 60401, PHONE: 303-278-9521
To:
Ms. Julie Rudolph
A. D. Little, Inc.
25 Acorn Park
Cambridge, MA 02140
P. O. No.:
Sample No.: parr Bombed XAD Resin Blank
(Sample was received broken) CONCENTRATION
Date: April 4, 1978
Analyst: s> Sweeney
IAD No.: 97-B085-110-01
IN PPM WEIGHT
ELEMENT CONC.
Uranium 3
Thorium <2
Bismuth
Lead 90
Thallium
Mercury NR
Gold
Platinum 780
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT CONC.
Terbium
Gadolinium
Europium
Samarium
Neodymium
Praseodymium <0. 1
Cerium 1
Lanthanum 0.5
Barium 79
Cesium
Iodine
Tellurium
Antimony 0.4
Tin 1
Indium STD
Cadmium l0.4
Silver 0.5
Palladium
Rhodi urn
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
3
72
£0.7
5
0.2
4
<0.7
1
0.3
7
37
10
0.2
180
2
25
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.4
13
<0.1
210
170
CONT
23
8
95
>110
51
>280
CONT
NR
NR
NR
CONT
0.6
NR
NR - Not Reported
All elements not reported
MC — Major Component
<0.1 ppm weight
CONT-Contamination
Approved
: \\.V_
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAQO, ILLINOIS 80601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Ms. Julie Rudolph
A. D. Little, Inc.
20 Acorn Park
Cambridge, MA 02140
Date.-
j 1978
Analvst: S. Sweeney
P. O. No,
Sample No,
ELEMENT
Uranium
Thorium
Bismuth
Lead
Thallium
Mercury
Gold
Platinum
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
Blank Imp.
CONCENTRATION IN vg/m'\
CONC. ELEMENT CONC.
0.09 Terbium
Gadolinium
Europium
0.04 Samarium
Neodymi urn
NR Praseodymium
Cerium 0.02
Lanthanum 0.01
Barium 0.03
Cesium
Iodine
Tellurium
Antimony
Tin
Indium STD
Cadmium
Silver
Palladium
Rhodium
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
IAD No,
CONC.
0
0
0
1°
0
.1
.004
.04
.002
.02
10.004
<0
0,
0.
0.
<0.
0.
0.
0.
.002
.08
.04
01
002
2
006
007
97-B089-110-01
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
0.003
0.03
10.002
2
1
0.4
0.08
0.09
0.9
0.09
0.3
17
-0.2
NR
NR
NR
0.05
<0.002
NR
NR - Not Reported
All elements not reported
AAC — Major Component
<0.002 yg/ml
Approved: T ^ _\^ \
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 226 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 6060t • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, U335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
To: Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
Date: March 9, 1978
Analyst-. S. Sweeney
P. O. No.: 540530
Sample NO.: Coal Parr Bomb
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Uranium <0.8
Thorium <1
Bismuth 220
Lead 9
Thallium
Mercury NR
Gold
Platinum 120
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Holmium
Dysprosium
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodi urn
CONC.
0.1
0.3
0.2
0.8
1
1
7
5
810
0.1
0.2
0.9
3
STD
2
1
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromi ne
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromi urn
CONC.
6
1
74
4
37
1
2
3
11
<2
2
33
12
12
2
MC
MC
26
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Nitrogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
9
300
1
860
MC
CONT
MC
780
39
>110
350
MC
CONT
NR
NR
NR
CONT
0.1
40
NR
NR - Not Reported
All elements not reported <0.1 ppm weight
MC - Major Component CONT-Contami nati on
Approved: /
-------
Reply to
COMMERCIAL TESTING & ENGINEERING CO.
GENERAL OFFICES: 228 NORTH LA SALLE STREET, CHICAGO, ILLINOIS 60601 • AREA CODE 312 726-8434
INSTRUMENTAL ANALYSIS DIVISION, 14335 WEST 44TH AVENUE, GOLDEN, COLORADO 80401, PHONE: 303-278-9521
TO:
Ms. Julie Rudolph
Arthur D. Little Company
25 Acorn Park
Cambridge, MA 02140
P. O. No.: 540530
Sample No.: Coke parr Bombed
Date: March 9, 1978
Analyst: s. Sweeney
IAD No.: 97-A981-110-12
CONCENTRATION IN PPM WEIGHT
ELEMENT CONC.
Uranium 4
Thorium 3
Bismuth 3
Lead 7
Thall ium
Mercury NR
Gold
Platinum 0.8
Iridium
Osmium
Rhenium
Tungsten
Tantalum
Hafnium
Lutetium
Ytterbium
Thulium
Erbium
Hoi mi urn
Dysprosium
ELEMENT
Terbium
Gadolinium
Europium
Samarium
Neodymi urn
Praseodymium
Cerium
Lanthanum
Barium
Cesium
Iodine
Tellurium
Antimony
Tin
Indium
Cadmium
Silver
Palladium
Rhodium
CONC.
0.1
0.5
0.3
2
4
2
10
14
240
1
0.3
<0.8
1
5
STD
3
3
ELEMENT
Ruthenium
Molybdenum
Niobium
Zirconium
Yttrium
Strontium
Rubidium
Bromine
Selenium
Arsenic
Germanium
Gallium
Zinc
Copper
Nickel
Cobalt
Iron
Manganese
Chromium
CONC.
12
7
210
5
110
14
6
1
14
2
5
110
30
17
10
MC
560
38
ELEMENT
Vanadium
Titanium
Scandium
Calcium
Potassium
Chlorine
Sulfur
Phosphorus
Silicon
Aluminum
Magnesium
Sodium
Fluorine
Oxygen
Ni trogen
Carbon
Boron
Beryllium
Lithium
Hydrogen
CONC.
41
MC
4
MC
MC
CONT
MC
710
MC
MC
MC
MC
CONT
NR
NR
NR
CONT
0.5
46
NR
NR - Not Reported
All elements not reported <0.1 ppm weight
- Major component CONT-Contamination
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
. REPORT NO.
EPA-600/2-79-045
3. RECIPIENT'S ACCESSION-NO.
TITLE AND SUBTITLE
Ferroalloy Process Emissions Measurement
REPORT DATE
February 1979
6. PERFORMING ORGANIZATION CODE
. AUTHORtS)
J.L.Rudolph, J.C.Harris, Z. A. Grosser, and
P. L. Levins
8. PERFORMING ORGANIZATION REPORT NO.
. PERFORMING ORGANIZATION NAME AND ADDRESS
Arthur D. Little, Inc.
Acorn Park
ambridge, Massachusetts 02140
10. PROGRAM ELEMENT NO.
INE624
11. CONTRACT/GRANT NO.
68-02-2150, T.D. 21502
2. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final: 11/77 - 3/78
14. SPONSORING AGENCY CODE
EPA/600/13
is.SUPPLEMENTARYNOTESIERL_RTp project officer is Larry D. Johnson; however, assis-
tant project officer Robert V. Hendriks (MD-62, 919/541-2733) is to be contacted
'or technical details concerning the ferroalloy process or industry.
16. ABSTRACT
The report gives results of sampling and analysis to characterize and quan
tify particulate, organic, and inorganic chemical emissions in effluents from a tot-
ally sealed metallurgical furnace at a ferroalloy plant. Effluents were sampled
downstream of a venturi scrubber during silicomanganese production (Test I) and
upstream of the scrubber during ferromanganese production (Test II). Sampling and
analysis methodology was essentially that of EPA's Level 1 Environmental Assess-
ment procedure, supplemented by a specific analysis of polynuclear aromatic hydro-
carbons (PAH). Good agreement was observed between the results of Level 1 organic
analysis and the specific analysis of PAH. Good agreement was also found between
the atomic absorption and spark source mass spectroscopic analyses of As and Sb.
Because the tests involved different ferroalloy production processes, their results
are not a quantitative measure of venturi scrubber efficiency. However, the data
imply good particulate removal efficiency. The venturi scrubber also appears to be
effective for removal of polynuclear aromatics, especially species in the higher
molecular weight range.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
. COSATI Field/Group
Pollution Dust
Ferroalloys Organic Compounds
Metallurgical Furnaces
Measurement Inorganic Com-
Sampling pounds
Analyzing Ferromanganese
Pnlyryp.lio Hydrocarbons
N STATEMENT
Pollution Control
Stationary Sources
Particulate
Silicomanganese
13 B
11F
131,13A
14 B
Q7C
11G
07B
18. DISTRIBUTION STATEMENT
Unlimited
19. SECURITY CLASS (This Report)
Unclassified
21. NO. OF PAGES
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
B15
------- |