EVALUATION OF A COATED BAGHOUSE
AT A SECONDARY ALUMINUM SMELTER
by
R.A. Baker, P.E.; A.A. Linero; J.D. Riggenbach
Environmental Science and Engineering, Inc.
P.O. Box 13454, University Station
Gainesville, Florida 32604
Contract No. 68-02-1402
EPA Project Officer: M. Scasikawski
Industrisl Environmental Research Laboratory
Metals and Inorganic Chemicals Branch
Cincinnati, Ohio 45268
Prepared for
U.S. Environmental Protection Agency
Office of Research and Development
Washington, D.C. 20460
October 1976
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RESEARCH REPORTING SERIES .
Research reports of the Office of Research and Development, U.S. Environ-
mental Protection Agency, have been grouped into five series. These five
bread categories were established to facilitate further development and ap-
plication of environmental technology. Elimination of traditional grouping
was consciously planned to foster technology transfer and a maximum inter-
1. Environmental Health Effects Research
2. Environmental Protecton Technology
3. Ecological. Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
This report has been assigned to the ENVIRONMENTAL PROTECTION TECHNOLOGY
series. This series describes research performed to develop and demon-
strate instrumentation, equipment, and methodology to repair or prevent
environmental 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.
ifiis document' is available to the public through the National Technical
Information Service, Springfield, Virginia 22161.
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ABSTRACT
This report assesses the use of a coated baghouse to control emissions
from charging and demagging operations at a secondary aluminum smelter.
On-site sampling was conducted for characterization of the emissions gen-
erated by specific tests for total particulates, particle sizing, elemental
analysis of particulates, polynuclear aromatics, sulfur dioxide, sulfur
trioxide, total methane hydrocarbons, total chlorides, and total fluorides.
Operating data supplied by the smelter is evaluated as to the system's
reliability.
The coated bahouse system was found to be reliable and very effective
for reducing emissions of particulate matter, sulfur trioxide, chlorides,
and fluorides. It had no effect on the total methane hydrocarbon emis-
sions. Particulate emissions from the baghouse are characterized as con-
taining small quantities of copper, aluminum, sodium, potassium, and zinc.
This report was submitted in fulfillment of Contract No. 68-02-1402 by
Environmental Science and Engineering, Inc., under the sponsorship of the
U.S. Environmental Protection Agency. This report covers a period from
10/17/76 to 10/22/76, and work was completed as of 10/22/76.
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CONTENTS
Abstract [[[ i
Figures ..................... ............................................ iii
Tables [[[ iv
1 . Introduction [[[ 1
2. Conclusions [[[ 2
3. Process Description ................... .......................... 6
4. Testing Methods ................................. ................ 1A
5. Results and Discussion .......................................... 27
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LIST OF FIGURES
Figure 3-1. Chlorination "Bell" In-Place at. Charging Well 7
Figure 3-2. Typical Reverbatory Furnace at Rochester Smelting
and Refining 9
Figure 3-3. Sketch of Charging Well Exhaust System - Part 1 11
Figure 3-4. Sketch of Charging Well Exhaust System - Part II 12
Figure 4-1. Sketch of Inlet Sampling Location 16
Figure 4-2. Sketch of Outlet Sampling Location 17
Figure 4-3. U.S. EPA Method 5 Particulate Collection Train 18
Figure 4-4. U.S. EPA Method 6 Sulfur Dioxide Collection Train 24
Figure 4-5. Chlorine and Hydrogen Chloride Collection Train 25
Figure 4-6. Andersen Mark III Cascade Impactor Collection
Train 21
Figure 4-7. Three Stage Cyclone Sampling Train 22
Figure 5-1. Inlet Particle Size Distributions at Rochester
Smelting and Refining 42
Figure 5-2. Outlet Particle Size Distributions at Rochester
Smelting and Refining 43
Figure 5-3. Average Inlet and Average Outlet Size Distributions
at Rochester Smelting and Refining 44
iii
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LIST OF TABLES
Table 2-1. Summary of Testing Results 3
Table 2-2. Summary of Process Data 5
Table 3-1. Summary of Expected Emissions from a Secondary
Aluminum Reverbatory Furnace 10
Table 4-1. Testing Methods and Analytical Procedures 15
Table 5-1. Schedule of Field Testing 28
Table 5-2. Summary of U.S. EPA Method 5 Results - Combined
Baghouse Inlet . . 30
Table 5-3. Summary of U.S. EPA Method 5 Results - Baghouse
Outlet 3.1
Table 5-4. Summary of U.S. EPA Method 5 Results - Baghouse
Collection Efficiencies 32
Table 5-5. Summary of Overnight U.S. EPA Method 5 Results 34
Table 5-6. Summary of Andersen Impactor Results 35
Table 5-7. Summary of Three-Stage Cyclone Results 36
Table 5-8. Summary of Particulate Emission Results - All
Sampl ing Trains 3'>7
Table 5-9. Summary of Total Fluoride Results i 39
Table 5-10. Summary of Andersen Impactor Sizing Results 41
Table 5-11. Summary of Elemental Analysis of Particualte Catch
from Three-Stage Cyclone Sampler 45
Table 5-12. Summary of Sulfur Dioxide and Sulfur Trioxide
Resul ts 47
Table 5-13. Summary of Chlorine and Hydrogen Chloride Results 48'
Table 5-14. Summary of Tonal Methane Hydrocarbon
Determinations 50
IV
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SECTION 1
INTRODUCTION
In 1973, Rochester Smelting and Refining Co. installed a coated bag-
house, designed by Teller Environmental Systems, Inc., in order to reduce
particulate and gaseous emissions from the charging wells on their three
reverbatory furnaces. Subsequently, a U.S. EPA demonstration contract was
obtained by the smelter to show the effectiveness of this control facility
during their charging and demagging operations. In 1974, Clayton Environ-
mental Consultants, Inc., was contracted by EPA to conduct a series of
emission tests on the facility in order to characterize its major parti-
culate and gaseous emissions during operations of fluoride fluxing and
chlorine demagging. However, the chlorine demagging equipment was not
installed, therefore, that aspect of the testing program could not be
c omp1e t e d.
In August of 1976, Environmental Science and Engineering, Inc. (ESE)
was assigned Task Order #015 of EPA Contract No. 68-02-1402 to perform a
testing and evaluation program of the coated baghouse. The sampling was to
be performed during demagging operations using chlorine and to include the
following parameters:
1) Particle size distribution at the inlet and outlet of the
baghouse,
2) Simultaneous measurement of average particulate loading at the
baghouse inlet and outlet,
3) Velocity, temperature, moisture, flue gas composition, sulfur
dioxide and sulfur trioxide determinations as required,
4) Characterization of the particulate and gas composition
(chlorides, polynuclear aromatics, chlorine, etc.), and
5) Analyze and evaluate the testing and operating data (compiled by
Rochester Smelting and Refining Co.) and prepare a final report
of the systems performance and reliability.
During ESE's preparation of the work plan, the scope of work was ex-
tended to include possible sampling 'during charging and fluorine demagging
periods if chlorine dejagging could not be performed continuously. The
field testing work was to be performed during the week of October 10th,
1976. However, it was postponed until the week of October 17th due to a
malfunction of an electrical transformer at the plant.
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SECTION 2
CONCLUSIONS
The results of the testing program have demonstrated that the use of
a coated baghouse is very effective for reducing certain emissions from a
charging well of an aluminum reverbatory furnace. As shown in Table 2-1,
the total particulate emissions were reduced 84 percent, sulfur trioxide
emissions were reduced 83 percent, chlorine emissions reduced 84 percent,
hydrogen chloride emissions were reduced 97.4 percent and total fluoride
emissions were reduced 75.4 percent.
The particulate emissions were sized with an in-stack impactor and
found to have an average particle size of .4 microns at both the inlet and
outlet locations. The particulate control efficiency of 84 percent is
xcithin the expected range for a typical baghouse when the exhaust gases
have particles of this size range. Therefore, the coating on the bags does
not appear to affect the overall collection efficiency.
Surprisingly, the records of Rochester Smelting and Refining do not
report a significant weight gain when collecting the used coating material.
This is interesting since the average inlet emission rate was 11.75 Ibs/hr
and the bags are used from several days to more than a week without
recoating.
The sulfur dioxide emissions at the inlet and outlet were consistently
below the test method's stated detection limits. So, the sulfur dioxide
collection efficiency of the coated baghouse was questionable.
The outlet levels of sulfur trioxide were found to be below the test
method's detectable limit while inlet levels were much higher. Therefore,
the calculated efficiency of 83 percent may be lower than actual. In any
case, the control system appears to be effectively reducing sulfur trioxide
emissions.
The efficiencies determined for chlorine and hydrogen chloride were 84
percent and 97.4 percent, respectively. These results show that the coated
baghouse is very effective for emissions during chlorine deraagging. It was
noted that the charging well hoods and chlorination well designs were in-
adequate to prevent severe in-plant ventilation problems during chlorine
cema;:s,ing. The "bell" would leak some emissions around the sides of the
well where the heavier-than-air gases would not be captured by the hoods'
inlet f1ow.
A reduction of 75.4 percent for total fluorides was demonstrated by
ESE's tests. While this is not as high as some efficiencies for other
contaminants, it does show a significant reduction by passing through the
coated baghouse.
Other than sulfur dioxide, the only other contaminant not positively
shown to be effectively controlled by the system was total methane hydro-
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Table 2-1. Summary of Testing Results
Parameters
Results* (Averages)
Total Particulate
Particle Size
Sulfur Dioxide
Sulfur Trioxide
Total Hydrocarbons (as Methane)
Chlorine
Hydrogen chloride
Polymiclear Aromatic
Hydrocarbons
Total. Fluoride
Baghouse is 84% efficient [11.75 Ibs/hr in vs. 9.95 Ibs/hr out]
Size distribution is approximately the same at inlet and outlet
[D50 In = 0.4v vs. D50 Out = 0.4y]
Baghouse is 54% efficient [0.71 Ibs/hr in vs. 0.43 Ibs/hr out]
Baghouse is 83% efficient [1.81 Ibs/hr in vs. 0.63 Ibs/hr out]
Baghouse has little or no effect on gaseous hydrocarbons [46 ppm in
vs. 40 ppm out]
Baghouse is 84% efficient [7.66 Ibs/hr in vs. 1.29 Ibs/hr out] '
Baghouse is 97.4% efficient [5.06 Ibs/hr in vs. 0.28 Ibs/hr out]
None found in the par I. i cu I ate s.-.impl es .
Baghouse is 75.4% efficient: [1.23 Ibs/hr in vs. 0.23 Ibs/hr out] f
Elemental Analysis of
Outlet. Dust
SiO
Na
K
Al
50%
2.0%
2.0%
3.5%
Fe ""
Cu
Pb
Zn
20%**
7.5%
0.3%
1.0%
Sr
Cd
Mg
Ca
0.0%
0.5%
0.6%
0.3%
* The average emission rates are from all test runs while the average efficiencies are only from
chose runs performed sironUaneously,
** Suspect, rust containing!: ion.
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carbon. A comparison on strip-chart data shows no difference in peak
magnitudes or frequency between the inlet and the outlet.
The elemental analysis of the outlet dust reported quantities of Iron
(20%), Copper (7.5%). Aluminum (3.5%), Sodium (2%), Potassium (2%), Zinc
(1%), and all other metals (less than 1%). The high quantity of Iron is
believed to be from contamination from the sampler.
Samples of the particulate catch were analyzed for polynuclear
aromatics, however none were detectable.
Table 2-2 is a summary of the operation log books of the four furnaces
during the testing program. Each furnace was operated on its own schedule
due to specific product requirements. Except for the time during fluoride
and chloride testing, no attempt was made to adjust production with
sampling. In fact, fluoride demagging, charging and idle periods of
operation were randomly occurring during all sampling periods.
A review of the monthly operating reports showed no serious main-
tenance problems with the baghouse system. Some bags have been replaced
over the last year but this is expected with any baghouse system.
A problem of in-leakage was apparent during our testing period since
flows were up to 16,000 DSCM greater at the outlet. This is only signifi-
cant in that it reduces the effective capture zone of the exhaust hood at
charging wells.
In summary, the coated baghouse system proved to have very effective
collection efficiencies for particulate emissions, sulfur trioxides,
chlorides, and fluorides. It was not shown to have good collection
characteristics for total methane hydrocarbons. Particualte emissions
contained small quantities of Copper, Aluminum, Sodium, Potassium, and
Zinc. An overall assessment of the system's reliability is that it is very
good and its effectiveness on reducing the emissions of most test contami-
nants is also very good.
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Table 2-2. Summary oO Process Data
Furnace
No. 1
Clean Scraps & Main; rial (Ibs)
Dirty Scraps (Ibs)
Flux (Ibs)
Skimmed (Ibs)
Finished Product (Ibs)
Demagging Type
NO . /
No. 3
Clean Scraps & Material (Ibs)
Dirty Scraps (Ibs)
Flux (Ibs)
Skimmed (Ibs)
Finished Product (Ibs)
Demagging Type
No. 4
Clean Scraps & Material (Ibs)
Dirty Scraps (Ibs)
Flux (Ibs)
Skimmed (Ibs)
Finished Product (Ibs)
Demagging Type
10/18/76
13,018
24 , A 1 1 .
6,000
10,300
38,554
Fluorine
10,496
6,018
4,000
1,736
16,650
Fluorine
52,292
8,546
6,000
7,341
46,780
Fluorine
10/19/76
15,386
31,851
6,000
5,405
39,374
F luorine
5,393*
11,982
4,000
2,330
13,440
Fluorine
Chlorine
46,629
11,254
6,000
8,842
54,084
Fluorine
10/20/76
25,121
17,321
6,000
3,274
39,948
None
- Not operat ing
6,642
7,976
4,000
5,394
15,740
Fluorine
Chlorine
47,622
5,842
44,268
Fluorine .
10/21/76
27,278
15,352
6,000
9,090
40,024
None
11,474
6,516
4,000
5,599
14,280
Fluorine
39,411
14,420
6,000
9,718
51,784
Fluorine
1.0/22/76
27,822
15,927
6,000
7,274
29,716
None
9,745
5,010
4,000
2,294
19,970
Fluorine
Chlorine
43,319
'\15.453
6,000
5,531
56,182
Fluorine
*A1l added during nigh I. shift
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SECTION 3
PROCESS DESCRIPTION
General
The operation of a typical secondary aluminum reverbatory furnace,
similar to those at Rochester Smelter and Refining, Inc., consists of
charging scrap metals with a high aluminum content; melting the scrap by
firing fuel oil; fluxing for removal of impurities; alloying, mixing, de-
magging and degassing to achieve specifications, and skimming of floating
impurities. Finally, the furnace is tapped to obtain molten aluminum. A
secondary smelter utilizes metal wastes which contain a high percentage of
aluminum and impurities of magnesium, copper, silicon, zinc, iron, and
other metals. These are classified as clean or dirty depending on their
physical state; oil coated, painted, etc. The dirty scraps are not usually
pretreated on-site, except that some of the oily scraps are degreased by
passage through a direct fired rotary kiln.
The charge is introduced into the furnace through a charging well,
where it melts and flows through a bottom connection into the combustion
zone of the furnace. A flux is applied to float some o,f the impurities and
also to create a cover to help prevent oxidation with air. The molten
metal is analyzed for coinppsition and is adjusted to specifications by
alloying, mixing, demagging and degassing. The demagging process which
reduces the content of magnesium in the melt is of interest for this test-
ing project. Essentially, there are two primary methods of demagging in
use. The more common deir.agging procedure is to add- fluorine, in the form
of aluminum fluoride, to form magnesium fluoride which floats to the top of
the molten metal. This is a relatively simple operation which requires no
additional process equipment.
The other demagging operation is performed by lancing gaseous chlorine
into the lower portion of the charging well to form magnesium chloride.
Chlorine demagging is susceptible to over-chlorination which creates venti-
lation problems within the plant as well as odors outside the plant. Due
to the toxic nature of chlorine gas, a special charging well bell and
scrubber system is required to try to contain the excess chlorine gas and
chloride emissions, as shown in Figure 3-1.
The semi-solid impurities formed by the above mentioned steps are man-
ually skimmed with ladles and put into containers. The final step is to
tap the furnace and to pour the molten metal into a "shot" machine (vibra-
tion disc) or a billet log machine or a refractory lined container for
transfer to a nearby foundry. Production records are maintained to indi-
cate the amount and type of materials in the charge as well as the amount
of flux, skimmingsj and the molten metal tapped.
Specific
Rochester Smelting and Refining Company operates four reverbatory
furnaces for smelting of aluminum scraps. Each furnace has two separate
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HOOD
CHLORINE
GAS
TO SEWER
Figure 3-1. Chl.rrj n.-il ion "Bell" Jn-I'l ;iro ;ii-. Ch.-i r;.',1 UK
-------
exhausts as shown in Figure 3-2; The combustion gases from firing fuel oil
are exhausted through the combustion zone stack. Due to the impingement of
the flame through part: of the stack, these exhaust gases do not appear to
present a significant particulate emission problem. The charging well is
separated from the combustion zone as are its emissions which are vented
through an adjacent hood. The major emissions from the charging well are
caused during the charging and demagging phases of the operation. Based on
recent EPA contracts studying this process, emissions during charging are
generally related to aerosols of unburned hydrocarbons, while emissions
caused by demagging can be a mixture of many different gases and
aerosols. A summary of the expected emissions is presented in Table 3-1.
In 1973, a coated baghouse system, designed by Teller Environmental
Systems, Inc., was installed. The bag coating known as TESISORB was
reported by Teller to act as an acid gas absorber and neutralizer as well
as a precoat filter. Once the coating is applied, the baghouse is operated
without a shaking cycle to clean the bags until the pressure drop across
the baghouse approaches 18" W.C. Depending on specific operational
parameters such as type of charge (dirty or clean), number of furnaces
on-line and type and amount of demagging operations, it may take from
several days to more than a week before a cleaning cycle is needed.
The entire system is a very unique arrangement of charging hoods, flow
combiners, flow splitterSj dampers, water sprays, an evaporator chamber,
baghouse modules and exhaust fans. Figues 3-3 and 3-4 show the essential
components.
The charging hoods of the four furnaces are ducted to above the roof,
where the original stacks are dampered closed and a horizontal manifold
connects all the stacks. However, the present capacity of the cleaning
system allows for only three furnaces to be vented at a time. The combined
exhaust gases are passed through a water quench duct (sprays are only used
when gas temperature is above 260°F) and a large baffled evaporator chamber
for water evaporation and larger particulate matter removal. A 2-foot
diameter damper is mounted in the side of the evaporator for emergency
temperature reduction by mixing ambient air with the exhaust gases. Next
the flow is divided for entry into three separate baghouse modules; each
has separate inlet and outlet dampers for flow control and contains 504
Dacron tubular bags. When coated, the bags are reported to have an oper-
ating range up to 250°F. A hopper collects the spent coating and larger
particles during normal operation and the remainder of the coating plus
captured particulat.es and absorbed gases during the bag shaking phase.
This material is passed through a rotary valve into a flexible discharge
hose for collection into containers for weighing and removal. During coat-
ing operations, the module inlet damper is closed and the coating is pulled
up a flexible hose and through a special 'inlet duct into the dirty side of
the baghouse by the fan system. The three modules are usually coated with
R total of 3,000 pounds of material. It has been reported by Rochester
Smelting and Refining Co. that material collected after the cleaning cycle
is approximately the same weight.
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CHARGING WELL
EXHAUST
COMI'.USTTON
EXHAUST
HOOD
CHARGING WELL
II
II
A
COMBUSTION
ZONE
MOLTEN METAL
BURNER
Figure 3-2. Typical. Keverbntory Furnace at Rochester Smetling
and Refining
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Table 3-1. Summary of Expected-Emissions from a Secondary Aluminum
Reverbatrory Furnace.
Process Step
Compos ic ion
Remarks
Charging
Fluxing.
alloying
and
mixing
(N9)
Degassing
(N2, C12,
or N2 -C12
IT: i :•: t u r e)
Fumes and smoke from
volatization and/or combus-
tion of scrap contaminants.
Gases: Nitrogen, hydrogen
fluoride, hydrogen chloride,
combustion gases, and other
volatile components.
Particulate: Major consti-
tuent when fluxing with
salt-cryolite mixture is
sodium chloride with minor
amounts of aluminum and
magnesium compounds. Addi-
tional compounds of Na, Al,
Mg, Ca, Fe, Pb, Mn, K, Cr,
Zn, and Ni may also be
presented.
Gases: Chlorine, hydrogen.
halides, volatile metal
chlorides, combustion gases
(if there is not a separate
chlorination chamber).
Particulate: Aluminum
chloride, aluminum fluoride,
aluminum oxide, magnesium
chloride, magnesium fluoride,
magnesium oxide, calcium
chloride, calcium fluoride,
sodium chloride, plus addi-
tional compounds of Cu, Ni,
Cd, and other metals.
Severe fuming results only
with C12 or N2-Cl2 mixtures.
Emissions are similar to
those from demagging.
Skimming
Pouring
Minor fugitive emissions.
Minor atmospheric emissions.
Fluxing fume samples collected
by thermal precipitation were
found to contain particles
smaller than 2 microns with
most of the particles 0.1
micron. The fumes were
characterized as corrosive par-
ticularly when collected wet.
These emissions are converted
to air pollution control
residuals (either wastewater,
sludge, or solid waste) at
plants where such systems are
implemented. See gas cleaning
processes below.
The parameters which determine
quantities of emissions frorr,
demagging are:
- metal temperature •
- chlorine flow rate
- magnesium content of alloy
- depth of chlorine injection
- thickness and composition
of dross
Air pollution and control
systems are usually used to
process demagging effluent
gases. See below.
The results of one study showed
that all fume particles from
degassing with chlorine were
under 2 microns and 90-95% were
less than 1 micron. Mean
particle size appeared to be
0.7 microns. Refer to gas
cleaning processes below.
Can be controlled by hood.
Can be controlled by hood.
10
-------
DAMPER
ROOF LINE
-------
A A ii
FROM
QUENCH
CHAMI5ER
I
ROOF LINE
___. 3 STACKS
\
FAN
ROOM
(3 FANS)
!•'ifMire 3-4. Skt'trli of c;li.-i rj>, inj1, We.l.l Exh.-itist System - Part IT
-------
The clean air side of the baghouse modules are manifolded together and
the flow is imrrv?diate 1 y divided for entrance into the three fan exhaust
?ysten. This was designed to maintain a constant flow throughout the cycle
of ooeration by dampening the inlet to the fans at the initially low pres-
sure drop across the baghouse and compensating for increased pressure droos
by opening the fan dampers. Each fan is followed by a stack for discharg-
ing the cleaned charging well exhaust gases into the ambient air.
13
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SECTION 4
TEST METHODS'
The specific testing rn«rhods and analytical procedures followed in
rhi? project are curlino-rl in Table 4-1 and are individually described
below'.
Samp] ing Locar.ions
The sarr.pl ing nor'.: locations were chosen based on availability of
•_::;;••: n:: locations, flow d is r.r ibut ions and practicality of sampling. The
cc-'riTec inlet due;, paneling location was modified with additional ports to
accor.r.:'5date several different sampling trains at the same time. Figure A-l
s ••>.-••«<:• rh? geo;-.v.?t r ic? of this location. It is termed "inlet" (all exhausts
fro- charging well hood? are combined before reaching this poinr.) through-
•:»,:: i.hi? reporr and repres?nrs the only baghouse inlet sampling locar.ion
\ o ~: this t e s \: i n g n r o \ ? c;..
~"i; baghousir outl?:' had no convenient combined sampling location, so
:';••- i hrtfc- onr.lc-t clue r 5 rrid stacks were investigated for testing purposes.
'. "•- pv' vioi.'ply estr.V. i ;-•'.-.••.;•: ranplinp locations on the rectangular ducr.s
"•:r--v:.".'': ro r.hc. far-? •.'•ri't: f?\.;;;d ;o be unacceptable due to a high duct vacuu:a
r~'~. i:-.;: ninrl-?? o:- :h-:; r::'r r which would have interfered with our tesuirij;
rr"hocs and equiunenr. A r^re convenient location was found on each of the
f"" v=:i':".r.i1 ?' s~ z.i~\\£ !.'.- !:'':ow: in Figure 4~2.
? v/ere sanpled bv following U.?. E?.-'.
--..\ •'. r- -.- .. :•••; :.wo axes located ac 90 degree? co each
or -- sarr.i;':ing ooincs. Samplinr rime oer Doinr.
1.5 r. o 3.0 rni nu r.e s .
1' .:'••• of i:n.> i :::•-.-•. .••::.".;•: sracks hsd rwo campling pores se;: r.:: 90 r^-
" (.. -.f.c . oilier. .-.: '>.:•::•:? locsrions, the pores were only 1.4 dia::;e::--r:
rn-r.- rrrr.- ?!•-. ".c .- . !•-. .-.c: and were nor acceptable according ro Mer.hcc'
. r-.'t I•;.'£.•; i.ban .1' :. iar.-..-: ers). However, in was decided to sample £r
: oca r. ions sfrc-r a:\ i r. i r. i a 1 i:rsverse was perforir-ed which shoved r.ne
: •> be- fairiv ur.: :".or:r.. V^s;: run r:l was performed on onlv one c~.'. !•::
••l;.r. ;: F-::>; rr. i-• ^c uip:r-v-:r. ;:rsir: an each port. This was do-ic- i." or:o:
•r r:..i r;c- c. F,a~;'> 1 i v. • ,?-•"..•:-.".u": i which would alio\7 for s imu i i:ant .'us inl'.r
."let si. ;.;iir.!. . f i- we 1 • at: obcain two particulate test: runs per cay.
: s found thar c:':- ou:le: train sampling 24 points per stack at £ rcr-;
• minur.es per noinr: vrou", d be acceptable. Thereafter, simultaneous
.-.; across th-? :ora 1 ;:-;:;aus;: flow was conducted. The sampling rrair.
. ? siio-,:n in Figurve 4.3.
.f:er com-jl •..•: i or: :•: <:ach particulate test run, the filter was recov-^-r-
:.: the Di'efilr.er ccroonenr.s of the test train were brushed and washed
•cerone. and the effluenr collecred. The filters were scored in n'nei:
-------
Table 4-1. Testing Methods and Analytical Procedures
Parameter
Test Method
Ana Ivsis
USEPA Methods 1, 2, 3,
5--simultaneous inlet
and outlet sampling'
US^PA Method ISA--
simultaneous inlet and
outlet sampling
Gravimetric de-termination
of filter and probe wash
Specific ion electrode
,-n.f. CI-)
Decker and Hagar
"vthod with alkaline
arsenite absorbing
rt'agent for Clo and
.-odium liydroxi.de for
liG i -~s imul t aneous inlet
snd outlet sampling
Sample with Teflon
tubing from inlet; and
outlet location--
vi•;• rfor:ned alteriiately
Volhard tit ration —
performed on-site
Becknann Model 400
Flame Ion isat ion
Detector—performed
a 1 ternsfelv
".'?EP.'. Method 6--
;- i~j. 11aneou? inlet- and
.• :' ",et samp i inp
Modified USEPA Method
{—Isopropanol reagent
iT save for analvsis.
.:.i~-.i 11.aneous inlet, and
out let sarnnling
••.r> ci Q r s e n Mp. r!•; Ill
Ca=cade Impsctor--
r-crfor:?.ed alternately
•-'• inlet and outlet
i 1.1 r a 11. on ? c;-. ? i; e
Tit rat ion? on s111
Filters weighed on-si
witn electron L->£ ^s•'.•:•:•
ihree Cyclone Parti-
culate sampling train
v.-Lth backup filter--
performed alternately
sr inlet and outlet
Spark Source Spec, t ros
and Atomic Absorption
Analyzer
Used filters from
Total Particulate
Sarnnl ins
Gas Chromstograph r. lectron
Capture Detector
15
-------
2. A D.IAMliTKKS
1.2 DTAMI'TI'iRS
STRAYS
O
5 FT
8.(, I "I.1
'\-\. SI.C/I ell u! Illli-i S.iliip I i II;', I.(M-,I (' i ml
QIIL'NCII
CHAMBER
-------
'ORTS
r
30"
1
*
j
1
, !
30"
\N i-.noi-i
30"
!
i
i
J
;'!
s
j
*
i
1 A DIAMETERS
-------
00
7.
8.
9.
10.
11.
12,
13,
14.
15.
16.
17.
18.
19.
Glass lined,
1. Nozzle
2. Probe ,
3. Filter
4. Heated Box
5. Impinger with 100
distilled water,
ML
modified
6. Impinger with 100 ML
distilled water,
Impinger, dry
Impinger, silica gel
Ice Bath
Flexible Sampling Line
Vacuum gauge
Main Flow Valve
Vacuum Pump.
Fine Control Valve
Dry Gas Meter
Thermometers
Manometer
Orifice
"S"-type Pilot Tube
standard
17
Figure 4-3. U.S. EPA Method 5 Particulate Collection Train
-------
original plastic containers while the acetone washes were rinsed into clean
borosilicate glass bottles with Teflon-lined tops. Samples were labeled,
logged and stored for gravimetric analysis in ESE's Gainesville laboratory.
Overnight Particulate Emission
In an effort to obtain a larger catch for the elemental analysis of
the baghouse's particulate emission, a series of four overnight test runs
were performed. The sampling trains were started in the evening just be-
fore leaving the plant and stopped the next morning. Only one sampling
point was used, however the initial sampling rate was established for cor-
rect isokinetic conditions. Samples were recovered in the normal manner.
The probe and box heaters were "off" for these runs to prevent electrical
complications with the inclement weather. Overnight runs 3 and 4 were con-
ducted simultaneously; the train for run 4 did not contain a filter in
order for the impingers to catch the total solid and condensed particu-
late matter without clogging a filter. The total impinger catch as well as
probe was analyzed with the other samples.
Total Fluorides
The total particulate test runs 1 and 5 were also used for total'
fluorides determination per U.S. EPA Method 13B of 40 CFR 60, Appendix A.
The normal Method 5 testing trains were modified on these runs by using
Whatman filters instead of fiberglass filters and the recovery procedures
altered by saving the impinger catch along with a preliminary water wash
(no brushing) of the prefilter components (probe and filter holder). A
normal brushing and an acetone wash were- performed after the water wash;
the filter and acetone wash were stored for analysis with the other U.S.
EPA Methods test runs. After the filter had been analyzed for weight gain,
it was put into the container with its water wash and impinger catch for
the total fluoride determination per Method 13B. While it is recognized
that some particulate matter may have been lost due to the preliminary
water wash, it is not felt to be significant enough to effect the total
particulate results.
Particle Sizing
Particle size distribution of the particulate matter in the inlet and
outlet gases was measured with an Andersen Mark III Cascade Impactor.
The apparatus used had a ore-cut cyclone, eight impaction stages, and a
back-up filter. Dessicated fiberglass filters were weighed before and"
after sampling using a Cahn Model 4400 electrobalance (sensitivity to 0.001
rug). The testing locations were the same as those used for total
particulate emission tests, however, only one sampling point at each
location was used.
The assembled impactor was inserted into the stack and allowed to
reach thermal equilibrium with the gases. The nozzle of the impactor was
then turned into the gas stream and immediately sampling was begun.
Near isokinetic sampling was achieved by sampling at a rate based on a
previous velocity measurement at the single point where the sample was
taken. However, changes in the sampling rate were not made to accommodate
19
-------
changes in the gas velocity as this would change the cut points of the
impactor stages. Figure 4-6 shows a schematic of the sampling train.
After sampling, the impactor was taken back to the weighing room for sample
recovery. This was performed by disassembling the impactor, removing the
glass-fiber substrates and brushing the remaining particulate matter from
each stage into the sample container with the substrate. Due to the
difference in grain loadings between the inlet and outlet locations, the
impactor was able to sample for much longer periods at the outlet (4 to 5
hours) than at the inlet (20 to 60 minutes).
Gross Sized Particulates
The sample weight of the particulate matter captured in the Andersen
Mark III Cascade Impactor is so small as to preclude elemental analysis on
the emissions from the coated baghouse. Therefore, gross samples were
obtained through the use of a three-stage cyclone sampler shown in Figure
4-7. This sampler was borrowed from the U.S. EPA Industrial Environmental
Research Lab in Raleigh, North Carolina. The nominal sampling rate of
the cyclones is 1.0 CFM which requires sampling for fairly long periods to
obtain large enough samples for analysis. At the baghouse inlet, the
sampling period ranged from 20 to 60 minutes, while the outlet sampling
period ranged from 360 to 899 minutes. The outlet test runs #2 and #3 were
conducted overnight in order to have sufficient time to obtain an adequate
sample. Tests were run during the day at the inlet location for possible
comparison.
After the sampling run, the sampler, was taken to the weighing roon and
disassembled. Each stage was brushed clean and the captured particulates
placed into containers. A backup filter was used to obtain a cummulative
relationship of the sample weights. These samples were dessicated -and
weighed on a Cahn Model 4700 electrobalance having a sensitivity of .0001
mg.
In conjunction with the elemental analysis of the emitted particu—
late matter, a sample of the baghouse hopper dust was obtained for analysis
by spark source spectroscopy. The composition of the TESISORB was obtained
iron Teller Environmental Systems, Inc., and compared with that of the
hopper dust. A final selection of 11 elements was made for quantification
of the metals contained in the baghouse emissions. This was performed by
using an Atomic Absorbtion Analyzer and using the particulate catches from
the three-stage cyclone sampler's outlet runs #1 and #3. Due to problems
of high blank values from fiberglass, the results are limited to samples
not collected on a filter.
Sulfur Oxides
Sulfur dioxide and sulfur trioxide were samples in accordance with
U.S. EPA Method 6 in CFR 60, Appendix A. The method is based on the
principle that sulfur trioxide is separated from sulfur dioxide by its
selective absorption in isopropyl alcohol. The sulfur dioxide is
subsequently absorbed in hydrogen peroxide. Although the method was
written specifically for sulfur dioxide determination, it was extended to
20
-------
modified
ML
standard
gel
1. Nozzle
2. Probe
3. Cyclone
4. Anderson Irnpactor
5. 'Impinger with TOO ML
distilled water,
6. Impinger with 100
distilled water,
7. Impinger, dry
8. Impinger, silica
9. Ice Bath
10. Flexible Sampling Line
1 1 . Vacuum gauge
12. Main Flow Valve
13. Vacuum Pump
Kl, Fine Control Valve
1$. Dry Gas Meter
16. Thermometers
17. Manometer
18. Orifice
19. "S"-type Pi tot Tube
17
Figure 4-6
Anderson MarK III Cascade Impactor Collection Train
-------
to
to
.C;
19
1. Nozzle
2. Probe
3. Filter
4. Three..stnae Cyclone
5. Impinger with 100 ML
distilled water, modified tip
6. Impinger with 100 ML
distilled water, standard tip
7. Impinger,, dry
8. Impinger', silica gel
9. Ice Bath
10. Flexible Sampling Line
11. Vacuum gauge
12. Main Flow Valve
1.3. Vacuum Pump
14. Fine Control Valve
15. Dry (jas Meter
16, Thermometers
17. MiUioiiieter
18. Orifice
19. "5"-type Pi tot Tube
17
Fioure 4-7 Three stage Cyclone Sampling Train
-------
include sulfur trioxide determination by recovery of both absorbing re-
agents and associated washes. A schematic of the sampling apparatus is
presented in Figure 4-4. Sulfur trioxide is scrubbed from the gas stream in
the first impinger which contains 15 ml of 80 percent isopropanol; the
sulfur dioxide is then removed in two impingers each of which contain 15 ml
of three percent hydrogen peroxide. The sulfur dioxide is oxidized and
subsequently analyzed by titration with barium perchlorate .using thorin as
an indicator. Similarly, the glass-wool mist trap, probe washings, and the
first impinger's catch and wash are titrated with the barium perchlorate
and thorin indicator. The samples were analyzed on-site after completion
of a 15 minute purging with ambient air. Each test run was performed at
the same sampling location as were the particulate determinations but only
at one sampling point.
Chlorides
Concentrations of chlorine and hydrogen chloride were measured at both
the inlet and outlet of the baghouse to determine the control efficiency of
these two chemical species. The method used was that proposed by C.E.
Decker and C.B. Hagar in 1968, "Determination of Hydrogen Chloride and
Chlorine in Stack Gas." Gas samples were extracted frora the appropriate
location and passed through a midget impinger containing 15 ml of alkaline
arsenite absorbing solution. The gas volume sampled was then determined by
passing the clean sample gases through a vacuum pump and dry gas meter as
illustrated in Figure 4-5. After a sufficient volume of gas was sampled,
the impinger contents were recovered and analyzed for C1-/HC1 per the
method. Chlorine was determined by analyzing the sample for unconsumed
arsenite wich reduces the Cl? to HC1. The total HC1 was then measured
using the Volhard titration. The Cl2 determined in the first titration was
then subtracted from the total chlorine found by the VoBiard titration r.o
give the free chlorine concentration. As with the sulfur oxides, each test
run was conducted at the same locations as were the particulate tests but
at only one sampling point.
Gaseous Methane Hydrocarbons
A Beckman Model 400 hydrocarbon analyzer was employed for Total
Gaseous Hydrocarbon Determinations as Methane. Separate sampling lines
(teflon) were employed for inlet and outlet sampling and were located at
the same duct and stack locations as for the particulate sampling. The
sample lines were alternately purged and connected to the instrument for
approximately 45-minute periods. A chart recorder was connected to the
instrument's electrical terminals and the data were redrac-ed on a time
weighed basis at a later time. The sampling times were' essentially
continuous throughout the work hours of the testing program except for
periods of checking the zero and span and purging sample lines.
Polynuclear Aromatic Hydrocarbons
Filters from the three-stage cyclone sampler's outlet run #2 and U.S.
EPA Method 5 outlet runs #4 and #7 were analyzed for polynuclear aromatic
hydrocarbons (PNA). The particulate catch was extracted' with methylene
chloride, concentrated to 1 ml and analyzed by a gas chromatograph with a
23
-------
1. Glass-wool plug
2. Glass-lined probe
3. Glass-wool mist trap
4. Glass impinger with 100 ml
5. Glass impinger with 100 ml
6. Glass impinger with silica
7. Flexible tubing
8. Ice bath
9. Main flow valve
10. Fine control valve
11. Vacuum pump
12. Thermometer
13. Dry gas meter
14. Rotometer :
15. Inclined manometer
16. "s" type Pi tot tube
16
80% isopropanol
3% hydrogen peroxide
gel
14
Figure 4-4. ILS. EPA Method 6 Sulfur Dioxide Collect-ion Train
(used also for Sulfur Trioxide collection)
-------
NJ
Ln
16
1. Glass-wool plug
2. Glass-lined probe
3. Glass-wool mist trap
4. Glass impinger with 15 ml absorbing
5. Glass impinger with as dry trap
6. Silica gel
7. Flexible tubing
8. Ice bath
9. Main flow valve
10. Fine control valve
11. Vacuum pump
12. Thermometer
13. Dry gas meter
14. Rotometer ;
15. Inclined manometer 14
16. "s" Type Pitot tube
reagent
Figure 4-5. Chlorine and Hydrogen Chloride Collection Train
-------
flame ionization detector. The three chromatographs were compared with the
chromatograph for ct-Naphthyl Amine a P.N.A. hydrocarbon. This was to
determine if additional analyses on a gas chromatograph-mass spectroscopy
unit would be beneficial.
Copies of all the testing and/or analytical procedures are in
Appendix B.
26
-------
SECTION 5
RESULTS AND DISCUSSION
The testing program was conducted on October 18th, 19th, 20th, 21st,
and 22nd of 1976 with the assistance of personnel from Rochester Smelting
and Refining Company. The scheduled work plan was modified_in the field to
obtain that which is shown in Table 5-1. The overall consideration was to
perform the various tests (except for Total Chlorides) on a regular basis
regardless of the furnace operations. A review of the process data pre-
sented in Section 2, shows that only furnaces #1, #3, and #4 were operated
during our testing schedule. However, for production reasons, a definite
pattern of all furnaces performing the same operation could not be
established. For example, on the second and fifth day, chlorine demagging
was performed on furnace #3 while the other two furnaces were charging,
using fluorine for fluxing and demagging, and were idle at various times
during the day. Throughout the week of testing, this pattern of random and
different operation on each of the furnaces continued. Therefore, it would
be in error to interpret the following data as anything but as emissions
occuring from three charging wells during various phases of operation.
Particulate Emissions
The total particualte results from the U.S. EPA Method 5 sampling are
shown on Tables 5-2, 5-3, and 5-4.
The inlet emission rates varied from 5.56 Ibs/hr to 17,06 Ibs/hr while
the outlet emission rates ranged from 0.19 Ibs/hr to 26.85 Ibs/hr. Several
runs had higher emission rates at the outlet than at the inlet during the
same time period. A review of the individual filter and probe-wash gravi-
metric results show that for the inlet samples most of the particulate
matter collected came from the filter, while this was not true for the
outlet samples. Outlet runs #1 and #8 had larger net weight gains in. their
washes while runs ^2, -:-5, and #7 had almost all the catch found on the
filters. A green coloration of the filters was noticed after outlet runs
v5 and -;!-7 (conducted in the morning) and the preceding overnight runs -;>1
and =,-2. The cause of this coloration was not identified but is suspected
to be related to overnight plant operations. Outlet run #2 was immediately
following a cycle of cleaning and recoating of the bags, and demonstrated a
higher outlet than inlet emission rate.
Another factor to consider when comparing the emission rates is that
stack gas flow (DSCFM) has a direct relationship to emission rates. In all
but the first run, the outlet flow exceeded the inlet by from 9,000 to
16,000 DSCFM depending on the specific run. The fan system is rated at
39,000 SCFM at a pressure drop of 10 to 22 inches water column. This.
corresponds favorably with the average outlet flow of 43,202 DSCFM bu-t not
with the average inlet flow of 32,064 DSCFM. It is suspected that: a
in-leakage existed between the two sampling locations and probably was from
the evaporating chamber's emergency damper or baghouse pre-coat inlet
due ts.
27
-------
Table 5-1. Schedule oE Field Testing
CO
Type Local: ion
P 3 r r i c u 1 a t P s I n 1 o t
Out If.- 1
Fluorides
(in particu- Inlet
late trains
on Runs Out: lei:
#1 and #5
Chlorides Inlet
Outlet
Total Methane
Hydrocarbons
(Test: Loca- Inlet
tions alter-
nately sampled Outlet
throughout the
days indicated)
Monday Tuesday Wednesday
10/18/76 10/19/76 10/20/76
#1 14:55-16:40 #2 11:05-14:1.1 #3 10:34-13:06
#4 13:58-16:55
//! 15:22-16:06 #2 11:06-14:30 #3 10:45-13:22
#4 14:08-16:42
#1 14:55-16:40
#1 15:22-16:06
#1 12:06-12:46 #2 11:35-12:00
#3 14:05-15:30
#1 13:50-14:30 #2 10:55-11:55
#3 14:05-15:30
193 minutes 264 minutes
171 minutes 184 minutes
Thursday
10/21/76
#5 10:27-12:56
#6 14:30-15:36
#5 10:28-13:02
#6 14:26-15:48
#2 10:27-12:56
#2 10:28-13:02
200 minqtes
190 minutes
Friday
10/22/76
#7 08:39-10:54
#8 13:43-16:05
#7 08:38-11: 12
#8 13:46-16:22
#4 13:40-15:30
#5 17:10-18:10
#4 13:45-15:3:0
#5 17:10-18:10
200 minutes
260 minutes
-------
Table 5-1. Schedule oC Field Testing (CONTINUED)
J
Type Location Monday Tuesday Wednesday
10/18/76 10/19/76 10/20/76
Sulfur Oxides Inlet #1 15:10-16:18 #2 1.3:44-1.4:50 #3
#4
#5
Sulfur Oxides Outlet #1 15:49-16:14 #2 11:55-13:05 #3
#4
#5
Particle Sizing Inlet #1 14:58-15:23 #2 11:23-12:13 #3
Outlet #1 12:57-16:58 #2
Thursday
10/21/76
10
12
14
10
11
14
12
12
:32-ll
:35-13
: 25-14
:40-11
:45-12
:30-15
:27-13
: 10-17
:42
:05
:55
:14
:15
:00
:41
:00
Friday
10/22/76
#6 09:00-09:35
#7 10:55-11:25
#6 08:55-09:30
#7 11:00-11:30
#4 14:35-17:05
#3 09:45-17:00
Cyclones
Inlet
#1 11:27-11:47
#2 14:20-15:20
#3 09:55-10:47
#4 13:35-14:10
Over nigh t
Outlet
Outlet
#1 11:00-17:00
#2 18:05
17:20-
-09:04
—09:04
#2 16:40-
#3 17:40 7:2
10/23/76
—07:30
#3 17:40 7:1
10/23/76
#4 17:45 7: l<
10/23/76
-------
Table 5-2. Summary of U.S. KPA Method 5 Results - Combined Baghouse Inlet
u>
o
Run
1
2
3
4
5
6
7
8
Date
10/18/76
10/19/76
10/20/76
10/20/76
10/21/76
10/21/76
10/22/76
10/22/76
Time
14:55-16:40
11:05-14:11
10:34-13:06
13:58-16:55
10:27-12:56
14:30-15:36
08:39-10:54
13:43-16:05
Average
Stack Temp
(°F)
86.7
112.6
115.9
132.7
103.6
96.6
115.3
92.8
107.0
Flow1
(SCFMD)
43,572
35,217
38,779 .
33,469
24,673
26,303
26,419
28,078
32,064
Filter
We i gh t
(mg)
45.0
164.0
170.6
267.8
170.4
90.7
240.6
177.5
Wash
Weight
(mg)
16.5
22.7
25.1
31.7
16.4
56/1
75.6
30.8
Total
We i gh t
(mg)
61.5
186.7
195.7
299.6
186.8
146.8
316.2
208.3
Emiss ions
Ubs/hr)
5.56
10.52
11. 16
16.92
10.29
10.77
17.06
11.74
11.75
1. Dry Standard conditions of 68°F and 29.92 inches Hg
-------
Table 5-3. Summary of U.S. EPA Method 5 Results - Baghouse Outlet
Run
I
2
3
4
5
6
7
8
Aver
Date
10/18/76
10/19/76
10/20/76
10/20/76
10/21/76
10/21/76
10/22/76
10/22/76
age
Time
15:22-16:06
11:06-14:30
10:45-13:22
14:08-16:42
10:28-13:02
14:26-15:48
08:38-11:12
13:46-16:22
Stack Temp
(°F)
70. O2
89.5
98.4
108.4
86.0
91.4
100.8
73.2
89.7
Flow1
•(SCFMD)
45 ,689 2
45,150
47,765
45,617
41,019
42,002
40,015
38,360
43,202
Filter
Weight
(mg)
35.7
124.2
46.6
4.8
lll.O
NEC3
255.5
4.3
Wash
We igh t
(mg)
105.7
2.2
1.2
2.8
NEC3
0.9
9.0
14.1
Total
We igh t
(mg)
141.4
126.4
47.8
7.6
lll.O
0.9
264.5
18.4
Emiss ions
(Ibs/hr)
20.86
12.94
4.93
0.77
11.21
0.19
26 ."85
1.82
9.95
1. Dry Standard conditions of 68 F and 29.92 inches Hg
2. Estimated from traversing only one outlet stack
3. Neg - Negative weight gain
-------
Table 5-4. Summary of U.S. F,PA Method 5 Results - Baghouse Collection Efficiencies
OJ
K3
Run
1
2
3
4
5
6
7
8
Date
10/18/76
10/19/76
10/20/76
10/20/76
10/21/76
10/21/76
10/22/76
10/22/76
T ime
14:55-16:40
11:05-14:30
10:34-13:22
13:58-16:55
10:27-13:02
14:26-15:48
08:38-11:1.2
13:43-16:22
Em iss ion
Inler
(Ib/hr)
5.56
10.52
11.16
16.92
10.29
10.77
17.06
11.74
Rates
Outlet
(Ib/hr)
20.86
12.94
4.93
0.77
11.21
0.19
26.85
1.82
Baghouse Efficiency (%)
Preliminary run - inval
compar is ton.
Immediately after bags
coated. Suspect coating
through.
55.8
95.4
id for
re-
bleed
Biased run due to green
coloration of outlet filter;
high weight gain.
98.2
Biased run due to green
cglgr-adtQa og gytilee fi
high weight gain.
84.5
UQP;
Average 83.5
-------
The particulate control efficiencies ranged from 55.8 percent to 98.2
percent with an average of 83.5 percent. This is somewhat lower than
expected for a baghouse but does agree with previous testing on. this unit
by Clayton Environmental Consultants, Inc.
Table 5-5 presents a summary of the overnight particulate sampling at
the outlet and shows a lower average emission rate, 2.47 lb_s/hr, than, found
during the daytime. This may relate to reduced furnace operations dosring
the night, when usually two furnaces were idle and the other furnace was
charged.
The emission rates from the one point sampling methods used for the
Andersen Mark III Cascade Impactor and the three-stage cyclone sampler are
presented in Tables 5-6 and 5-7, respectively. The Andersen impac:tor's
results show an average of 8.78 Ibs/hr at the inlet and 0.26 Ibs/hr at: the
outlet. Likewise, the three-stage cyclone sampler had results of average
emission rates of 8.19 Ibs/hr and 0.09 Ibs/hr for the inlet and outlet,
respectively.
A summary of all the particulate sampling train results is presented
in Table 5-8. The Andersen impactor and three-stage cyclone sampler" gave
lower results at both the inlet and outlet locations, but the degree of
difference was much greater at the outlet. This may mean that the oistlet
emission levels are somewhat lower than reported by the U.S. EPA Me-tfeod 5
test runs; outlet runs #5 and #7 mentioned before, show the greatest:
differences but this may be explained by the absence of the green
coloration on the filters from the Andersen Impactor and three-stage
cyclone sampler. It is important to note the difference in the meth-ods of
sampling (in-stack filters vs out-of-stack hot box, one point vs- multiple
points), sample recovery (no wash vs probe wash, dry brushing of stages vs
brushing and acetone rinse) and analyses (on-site weighings vs off.-si.te
weighings) that exist between the Andersen Impactor and three stage cyclone
sampler, and U.S. EPA Method 5. Therefore, 'direct numerical comparisons of
the results may be erroneous. However, "ballpark" estimates and1 comparisons
can be made to determine the possibility of gross errors or sample bias.
For example, on October 21, 1976, the inlet runs show the same "ballpark"
of emission rates even though two of the values (Impactor #3 and Cyclone
v2) differ from the other three values by a multiple of 3. On the same
day, the outlet runs differ significantly due to the green coloration on
U.S. EPA Method 5 filters on runs #5 and overnight #2.
Total Fluorides
The results of the fluoride determination on the samples obtained from
the U.S. EPA Method 5 runs #1 and #5 are presented in Table 5-9. The
average emissions were found to be 1.23 Ibs/hr at the inlet and 0.23 Ibs/hr
at: the outlet with an average collection efficiency of 75.4 percent. Both
of these test runs had higher outlet total particulate emission rates' than
found at the inlet, but showed a large removal of fluorides by passing
through the coated baghouse system. These emission results are slight:ly
33
-------
Table 5-5. Summary of Overnight U.S. L?,PA Method 5 Results
Run Date
Outlet- 1 10/20/76
2 10/21/76
3 10/22/76
4* 10/22/76
Average
Time Stack Temperature Flow**
(°F) (SCFM)
17:20-09:04 100 43,318
16:40-07:30 75 38,360
17:40-07:17 79 41,009
17:45-07:10 100 38,360
Emiss ions
(Ibs/hr)
3.35
6.01
0.46
0.04
2.47
*No filter used
**Based upon an average of flows from the first full traverse particulate test runs before and after
the overnight test.
-------
Table 5-6. Suiiimnry of Anrlersen Impnctor Results.
U>
Ln
Run Date Time Stack D50
Temperature (u)
Inlet 1 10/19/76 14:58-15:23 117.2 0.3
2 10/20/76 11:23-12:13 117.7 0.4
3 10/21/76 12:27-13:41 96.7 3.6
4 10/22/76 14:35-17:05 95.4 0.4
Outlet 1 10/20/76 12:57-16:58 100.1 0.2
2 10/21/76 12:10-17:00 80.0 2.5
3 10/22/76 09:45-17:00 80.7 0.3
Flow*
(DSCFM)
35,217
38,779
24,673
28,078
Average
47,765
42,002
39,187
Average
Emi. ss ions
(Ibs/hr)
13.43
15.03
3.65
3.02
8.78
0.10
0.56
0.13
0.26
VfFlows taken from particulate sampling.
-------
Table 5-7. Smmiuiry of I'll nji.'-Si.uge Cyclone Results
OJ
ON
Run
Inlet: 1
2
3
4
Average
Outlet 1
2
3
Average
Date Time
10/21/76 11:27-11:47
10/21/76 14:20-15:20
10/22/76 09:55-10:47
10/22/76 13:35-14:10
10/20/76 11:00-17:00
10/20/76 18:05-09:04
10/22-23/76 17:40-07:20
Cyclone D50's Flow* Emissions
1st: 2nd 3rd (DSCFM) (Ibs/hr)
(u) (u) (u)
2.05 0.75 0.40 38,779 11.45
2.01 0.73 0.39 33,469 2.82
2.43 . 0.89 0.47 24,673 10.64
2.26 0.83 0.44 26,303 7.84
8.19
2.02 0.74 0.39 45,150 0.11
2.03 0.74 0.39 46,458 0.08
2.13 0.78 0.41 38,360 0.08
0.09
* Flow taken from particulate sampling.
-------
Table 5-8. Summary of Part: i.cul ?ii e Emission Results - All Sampling Trains
u>
Date
10/18/76
10/19/76
10/20/76
10/21/76
14
15
11
11
14
10
10
11
11
12
13
14
17
18
10
10
11
12
12
14
14
14
16
Time
: 55-1 6
:22-l6
: 05-14
: 06-14
:58-15
:34-13
:45-13
:00-17
:23-l2
:57-16
:58-16
:08-16
: 20-09
:05-09
:27-12
:28-13
:27-ll
: 10-17
:27-l3
: 20-1 5
:26-15
:30-15
:40-07
:40
:06
: 1 1
:30
:23
:06
:22
:00
:13
:58
:55
:42
:04
:04
:56
:02
:47
:00
:41
:20
:48
:36
:30
Method
Inlet:
Oul-.le'i:
Inlet
Out. lei:
Inlet
Outlet
Inlet
Outlet.
Train and Run
5 Impactoi: Cyclone
#1
#1
#2
#2
Inlet: #1
#3
#3
Outlet #1
Inlet #2
Outlet #1
#4
#4
Inlet Emissions
(Ibs/hr)
5
10
13
11
15
16
.56
. 52
.43
.16
.03
.92
Overnight #1
Inlet:
Outlet:
Ou t: 1 e t
Inlet:
Overnif
Outlet #2
#5
#5
Inlet #1
Outlet #2
Inlet #3
Inlet #2
#6
#6
;ht #2
10
11
3
2
10
.29
.45
.65
.82
• 77
Outlet EIT
liss
(Ibs/hr)
20.
12.
4.
0.
0.
0.
3.
0.
11.
0.
0.
6.
86
94
93
11
10
77
35
08
21
56
19
01
-------
T.->M." 5--8. Kiinnni-y of l-'.-iri i cnl .n i c Ei'i i :;:-, i on
All Samp I ing T ra ins (CONTINUED)
OJ
CO
Date
10/22/76 08
08
09
09
13
13
13
14
17
17
17
T i.me
:38-ll
:39-10
.-45-17
:55-10
:35-14
:43-16
:46-16
:35-17
:40-07
:40-07
.-45-07
:12
:54
:00
:47
: 10
:05
:22
:05
:20
Method
Ou 1 1 e t
Inlet--
Inlet
Ou 1 1 e t
Tr.iin and Run
5 Impact or Cyclone
#7
if 7
OU t 1 <:' 1 #3
Inlet #3
Inlet #4
#8
#8
Inlet #4
Outlet #3
Inlet Emissions
(Ibs/hr)
17.
10.
7.
11.
3.
06
64
84
74
02
: 17 Overnigh t: #3
: 10 Overnight #4
Outlet Emissions
(Ibs/hr)
26.
0.
1.
0.
0.
0.
85
13
82
08
46
04
-------
Table 5-9. Summary of: Toi:al Fluoride Results
Location Date
Inlet: #1 10/18/76
Outlet: #1 10/18/76
Inlet: #2 10/21/76
Outlet #2 10/21/76
Average**
Inlet
Ou 1 1 e t
Time
Concentration
(Ibs/ft 3 xlO~7)
14:55-16:40 6.23
15:22-16:06 0.45
10:27-12:56 3.35
10:28-13:02 1.39
4.79
0.92
FLUORIDE
Emiss ions
(lbs/hr)*
1.63
0.125
0.825
0.343
1.23
0.234
Ef f ic iency
92.3
58.4
75.4
* Calculated based on the stack flow data from a concurrent full traverse particulate test run.
** Averages based on all test runs except that efficiencies are based on only those runs performed
simultaneously.
-------
higher than that reported by Clayton Enivornmental Consultants, Inc., but
the average efficiency is similar. However, it should be noted that the
previous test and analysis methodologies are unknown and the results may
not be comparable.
Particle.Sizing
The results of the Andersen Impactor test runs are summarized in Table
5-10. The D50 is the calculated particle diameter in microns at which 50
percent of particles will be larger than -and 50 percent will be smaller
than this size. The "percent less than" is the cumulative percentage of
the total weight caught during each test run, for a particular stage and
all the stages located downstream of it in the impactor, and includes the
back-up filter.
The average D50 for each test run and for all test runs at the inlet
and outlet are presented. The average D50 for all the inlet test runs was
determined to be 0.4 microns. Interestingly, the average D50 for all the
outlet tests was also 0.4 microns. These run averages were obtained by
plotting the results on log-probability paper and finding the size for each
test run at the 50 "percent less than" value as shown in Figures 5-1, 5-2,
and 5-3. Based on a weight relationship, these D50 run averages and D50
inlet and outlet averages represent that particle size at 50 percent of the
cumulative weight.
Inlet run #3 and outlet run #2 were performed during the same time
period on October 21, 1975, and show much higher average D50's (3.6 and 2.5
microns respectively) than the other runs.
The major aspect of the particle sizing results is that the average
particle found at the inlet is the same size as the average particle found
after the coated baghouse. In view of this and the average particulate
collection efficiency of 83.5 percent (Table 5-4) of the baghouse, the
system appears to be operating in the expected range for a normal baghouse
with the same D50 particle size. The higher efficiencies (99% +) usually
associated with baghouses is for collecting particles larger than 5 microns
Three-Stage Cyclone Sampler
Elemental analysis of the particulate samples collected in the three
cyclones was performed on outlet runs #1 and #3 (run #2 was retained for
possible crystaline analysis). Table 5-11 presents a summary of 11
separate analyses performed with an atomic absorption unit on the three
stages of both test runs. These 11 were chosen for further investigation
following review of a qualitative analysis of a sample of the baghouse
hopper dust by spark source spectroscopy. The metals of interest and their
average percentage in the outlet dust samples is given on the bottom of the
table. The iron results are apparently in error due to rust contamination
from the sampler. The contamination was apparently less severe on run #3
which concurs with visual observations during sample recovery.
40
-------
5-10. Summary for An°^r
7.79
6.56
4.53
3.34
1.58
1.01
0.53
0.26
Percent:
Less Than
89.
89.
88.
86.
85.
77.
67.
51.
88.
79.
79.
79.
77.
65.
58.
53.
3
1
2
7
8
3
6
9
2
3
3
3
5
7
0
3
Run 2
D50
(u)
7.97
6.72
4.63
3.41
1.62
1.03
0.54
0.26
0.4
7.97
6.72
4.63
3.42
1.62
1.03
0.55
0.26
Percent
Less Than
94.9
93.3
91.5
88.8
85.4
78.8
63.0
42.6
84.4
74.2
62.4
54.4
45.7
41.2
44.2
40.7
Run 3
1)50
(u)
8.33
7.02
4 . 84
3.57
1.69
1.08
0. 57
0.28
3.6
8.04
6.78
4.68
3.45
1.63
1.04
0.55
0.27
Percent
Less Than
55.8
54.3
52.4
49.5
46.4
41.8
36.0
. 29.4
97.7
95.1
87.8
79.5
78.4
76.2
65.0
49.0
Run 4
D50 Percent
Less Than
(u) (%)
8.
7.
5.
3.
1.
1.
0.
0.
0.
75 85.8
37 85.4
09 84.0
75 82.0
78 79.6
14 73.9
60 60.0
29 44.9
4
Average
D50
(u)
8.42
7.10
4.89
3.61
1.71
1.09
0.57
0.28
0.4
7.93
6.67
4.61
3.40
1.61
1.03
0.54
0.26
Percent
Less Than
81.4
80. 5 .
79.0
76.7
74.3
67.9
56.6
42.2
90.1
82.9
76.5
71.1
67.2
61.0
54.7
47.7
D50 Average
2.5
0.3
0.4
-------
FIGURE 5-1. INLET PARTICLE SIZE DISTRIBUTIONS AT ROCHESTER SMELTING
AND REFINING
10 ..a
I
m
A
GO
00 A
2
1..0
-! 0.1
KEY
RUN #1
RUN ;/2
RUN f-3
RUN f-4
10/19/76
10/20/76
10/21/76
10/22/76
o
A
H
0
1
_! o.oi
100
10 20 30 40 50 60 70 80
PERCENT SMALLER THAN STATED SIZE
90
-------
FIGURE 5-2. OUTLET PARTICLE SIZE DISTRIBUTIONS AT ROCHESTER SMELTING
AND REFINING
I T I 1 I I I
10.0
a
A
0 E3
_
KEY
RUN #1 10/20/76 0
RUN #2 10/21/76 A
RUN #3 10/22/76 JTJ
A
A 0
A
0
A E30
Q
1.0
CO
§
U
M
s
N3
M
CO
M
H
OS
<
PH
-i 0.1
j I
0.01
10
20 30 40 50 60 70 80
PERCENT SMALLER THAN STATED SIZE
43
90
100
-------
FIGURE 5-3. 'AVERAGE INLET AND AVERAGE OUTLET SIZE DISTRIBUTIONS AT
ROCHESTER SMELTING AND REFINING
l T
1 I1 \
A 0
10.0
KEY
Average Outlet
Average Inlet
©A
©
©
A
•; 1.®
A
to
ai
^-1
I
o
0.1
J
i
0.01
10 20 30 40 50 60 70 80
PERCENT SMALLER THAN STATED SIZE
44
90
100
-------
Table 5-11. Summary of E1 .emonfal Ana!y;:i.3 of Particu late Catch From 3 Stage Cyclone Sampler
Run
Out: lei:
#1
Outlet
#3
T 0
Cyc lone
Date Time Run
10/20/76 11:00-17:00 1
2
3
Average
10/22 + 17:40-07:20 1
10/23
2
3
Average
T A L AVERAGE
Percentage of
Na
1.2
0.4
1.6
I. I
0.7
4.2
3.4
2.8
2.0
K
0.7
0.2
0.8
0.6
1.0
4.2
5.1
3.4
2.0
Al
2.0
0.8
3. 1
2.0
1.7
6.5
6.4
4.9
3.5
Sr
0
0
0
0
0
0
0
0
0
Fe*
21.5
34.5
34.2
30.1
19.0
6.5
4.2
9.9
20.0
Cu
0.1
O.I
1.6
0.6
0.3
0.7
1.7
0.9
7.5
Total
Pb
0.2
0.1
0.2
0.2
O.I
0.7
0.4
0.4
0.3
Weight
Zn
0.5
0.2
1.6
0.8
0.5
1.0
2.1
1.2
1.0
Mg
0.3
0. 1
0.2
0.2
0.2
1.3
1.1
0.9
.0.6
Cd
0.4
0. 1
0.3
0.3
0.1
1.3
0.4
0.6
0.5
Ca
0.0
0.2
0.6
0.3
0.3
0.7
0.0
0.3
0.3
* High levels of: PC probably duo Co special connoci'.iona betrween cyclones; appeared rusty but were not:
accessible for cleaning.
-------
Sulfur Dioxide and Sulfur Trioxide
The results for sulfur dioxide and sulfur trioxide sampling are: pre-
sented in Table 5-12. The average sulfur dioxide emission rates were 0.07
Ibs/hr and 0.05 Ibs/hr for the inlet and outlet, respectively. The average
efficiency of the coated baghouse was found to be 54 percent for sulfur
dioxide removal.
The sulfur trioxide emissions were determined to have an average inlet
rate of 1.81 Ibs/hr and an average outlet rate of 0.6 Ibs/hr. The system
had an average collection efficiency of 86 percent.
The results show some higher emission rates at the outlet than at the
inlet. This may be due to a chromographic effect of the bag coating where
inlet concentrations may be delayed or retained by the coating before being
released sometime later. Also, the U.S. EPA Method 6 is reported to have a
detectable limit of 2.1 x 10 ~7 Ibs/DSCF for sulfur dioxide, and an equiva-
lent detectable limit of 2.63 x 10~7 Ibs/DSCF for sulfur trioxide.. Since
Table 5-12 shows that all the sulfur dioxide inlet and outlet results and
most of the sulfur trioxide outlet results are considerably below these
limits, the results may have a degree of lower limit "bounce". However,
sample volumes were approximately four times the usual requirements of the
method (~3.0 DSCF to 0.71 DSCF) which might have a lowering effect on the
detection limits.
-N
The important points of the results are that sulfur dioxide is emitted
at both the inlet and outlet in very l,ow .concentrations and that sulfur
trioxide concentrations are reduced effectively by the coated baghousje.
Hydrogen Chloride and Chlorine
The aspect of the possible reduction of chlorine gas and chloridles was
the primary goal of this testing program. Table 5-13 presents the results
of chlorine and hydrogen chloride testing and reports on the collection
efficiencies. The average chlorine.emission rates were 7.66 Ibs/hr ax the
inlet and 1.29 Ibs/hr at the outlet; .the average chlorine collection, effi-
ciency was 84.4 percent. The average hydrogen chloride emission rates were
5.06 Ibs/hr and 0.28 Ibs/hr at the inlet and outlet, respectively; thve
average collection efficiency was 97.4 percent.
These results demonstrate that the coated baghouse was effectively
reducing the chlorine/hydrogen chloride emissions.
In order to determine any residual effect of the chlorine demaggfing
process, run #5 was conducted approximately two hours after chlorinatlon
was stopped and the "bell" removed from the charging well. While the
emission rates of both gases decreased during this run, as compared fco run
v4, the outlet levels of chlorine increased and hydrogen chloride was not
detectable. The increase in chlorine emissions may be related to a
chroraatographic effect of the bag coating or its saturation level. Yihe
significant aspects of the results are that chlorine and hydrogen emissions
continued from both the charging well and the baghouse for at least several
46
-------
Table 5-12. Sumn'.iry of Sulfur Dioxide and Sulfur Trioxide Results
Run
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
#1
#1
n
n
#3
#3
#4
#4
#5
#5
#6
#6
#7
#7
Date
10/18/76
10/19/76
10/21/76
10/21/76
10/21/76
10/22/76
10/22/76
Average :
T ime
15:10-16
15:49-16
13:44-14
11:55-13
10:32-11
10:40-11
12:35-13
11:45-12
14:25-14
14:30-15
09:00-09
08:55-09
10:55-11
11:00-11
;1«
:50
:05
:42
:05
:55
:00
:35
:30
:25
:30
Qs
(SCFMD)
43,572
45,707
35,217
45,150
24,673
41,019
24,673
41,019
26,303
42,002
26,419
40,015
26,419
40,015
Inlet
Outlet
SULFUR DIOXIDE
xlO-'/ Ibs
DSCF
0.20
0.45
0. 14
0.55
0.35
0.00
0.39
0.15
0.14
0.00
0.05
0.06
0.44
0.06
Ibs* Efficiency
hr (%)
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
05 Neg
12
03
15
08 100
00
06
04
22 100
00
01 0
01
07 71
02
07 54
05
SULFUR TRIOXIDE
xlQ-7 Ibs
Ibs* E f f ic iency
DSCF hr (%)
5.03
0.00
0.09
5.72
8.98
0.00
1.38
0.00
10.12
0.07
20.27
4.14
25.40
6.83
1.32
0.00
0.19
1.55
2.09
0.00
0.20
0.00
1.60
0.02
3.21
0.99
4.03
1.64
. 1.81
0.6
100
100
99
72
59
86
NOTE: S02 detectable limit of 2.1 x 10~7 Ibs/DSCF; S03 detectable limit of 2.63 x 10~7 Ibs/DSCF.
* Calculated based on the stack flow data from a concurrent full traverse particulate test run.
** Averages based on nil test runs except that efficiencies are based on only those runs performed
s i mu 1 I; n n r> on:; 1 y .
-------
Table 5-13. Summary of Chlorine and Hydrogen Chloride Results
.c-
00
Run Date
T imc
Concentrat: ion
. (lbs/ft:3 xlO~7)
Inlet; #1 10/19/76
Out: let; #1
Inler. #2 10/20/76
Outlet #2
Inlet #3 10/20/76
Outlet #3
Inlet #4 10/22/76
Outlet #4
Inlet #5 10/22/76
Outlet #5
Average**
Inlet
Outlet
12:06-12:46
13:50-14:30
11:35-12:00
10:55-11:55
14:05-15:30
14:05-15:30
13:40-15:30
13:45-15:30
17:10-18:10
17:10-18:10
100.00
2.37
25. 10
2.77
46.90
4.35
86.10
5.94
55.60
10.49
62.74
5.18
CHLORINE
Emissions'''' Efficiency
(Ihs/hr) (%)
22.62
0.64
5.85 86.5
0.79
9.42 87.4
1.19
13.64 89.5
1.43
9.37 74.3
2.41
7.66 84.4
1.29
HYDROGEN CHLORIDE
Concentration
(lbs/ft3 xlO~7;
5.77
0.66
21.76
0.09
20.63
0.00
77.80
5.02
15.04
0.00
28.20
2.16
Emissions* Efficiency
) ubs/hr) (%) :
1.22 ,
0.18
5.06 99.4
0.03
4.14 100
0.00
12.33 90.2
1.21
2.53 100 1
0.00
I
1
5.06 97.4
0.28
* Calculated based on the stack flow data from a concurrent full traverse particulate test run
** Averages based on all test runs except that efficiencies are based on only those runs perfdrmed simultaneously.
-------
hours after chlorine demagging was completed and that the coated baghouse
successfully reduced both of these emissions by 84 percent and 97 percent,
respectively.
Total Methane Hydrocarbons
As summaried in Table 5-14, the emission levels of total methane
hydrocarbons did not differ significantly by use of the coated baghouse.
Simultaneous sampling was not conducted while making this determination,
however, each location was adequately sampled for greater than 800 minutes
during the course of the four days in order to characterize the emission
rates. The inlet and outlet gases were sampled alternately for individual
periods of up to 45 minutes throughout the testing period. This technique
was designed to adequately describe the total methane hydrocarbon
concentrations at both sampling locations.
The time-weighed average concentrations of total methane hydrocarbons
were determined to be 46 ppm at the baghouse inlet and 40 ppm at its
outlet. Due to the lack of a significant difference in concentrations, a
control efficiency is not given.
Polynuclear Aromatics
The filters from the three-stage cyclone outlet run #2 and U.S. EPA
Method 5 outlet runs #4 and #7 were analyzed on a gas chrornatograph for
polynuclear aromatic hydrocarbons (PNA). Based on comparison with a sample
of ot-Naphthyl Amine, a known PNA, none were detectable. Therefore, the
scheduled gas chromatograph-mass spectroscopy analysis was cancelled.
49
-------
T.'ible 5-14. Summary o£ Tot.il Methnno Hydrocarbon Determinations
o
Emissions
Location Date
Inlet 10/19/76
10/20/76
10/21/76
10/22/76
TOTAL
Outlet 10/19/76
10/20/76
10/21/76
10/22/76
TOTAL
Total Sampling
(min)
193
264
200
200
857
171
184
190
260
811
Time Time Weighed Average
(ppm)
44
38
. 71
35
Average 46
34
44
51
32
Average 40
Non-Peak
Maximum
(ppm)
115
111
117
78
110
124
115
107
•
Non-Peak
Minimum
(ppm)
12
20
32
119
12
15
16
15
-------
APPENDIX A
TEST METHODS
-------
ENVIRONMENTAL PROTECTION AGENCY REGULATIONS
ON STANDARDS OF PERFORMANCE FOR NEW STATIONARY SOURCES
(40 CFR 60: 36 FR 24876, December 23. 1971; Effective Auynst P. 1971';
Amended as shown in Code of Federal Regulations. Volume 40, revised as of Ju!v 1.
1975: 40 FR 33152, August 6. 1975: 40 FR 42194. September 11, 1975; 40 FR 43850.
September 23, 1975; 40 FR 45170. October 1. 1975; 40 FR 46250. October 6. 1975: 40
FR 48347, October 15, 1975; 40 FR 507] S, October 31. 1975, 40 FR 53340 November
17, 1975; 40 FR 58415, December 16. 1975; 40 FR 59729. December 30. 1975: 4! FK
1913, January 13. 1976; 41 FR 2232. January 15, 1976:41 FR 3826. January 26. 1976:
41 FR 4263, January 29, 1976: 41 FR 7749, February' 20, 1976: 41 FR 8346, Fobruary
26, 1976; 41 FR 11820, March 22, 1976; 41 FR 17549. April 27, I976;41 FR 18498.
May 4. 1976)
PART GO-STANDARDS OF PER-
FORMANCE FOR NEW STATION-
ARY SOURCES
AUTHORITY: Sees, in or.d 114 of the Clean
Air Act. D.S DT-.cmec!"t>i r.t-c. 4(tt) 'of Pub-. L.
91-eOi. 84 StBt. 1C78 (42 TJ.S.C. 1857C-C.
1G57C-9). Subpurt-B also Issued under sec.
331(a) ol-tlsc Clean Alr Act. us amended by
toe. ISiCif-) o' ^'a'J- L- 01-004. S4 Stat.
1712 (-12 C.S.C. 1C57CJ.
140 FR 53340, November 17. 19751
A — General Provisions
§ 00.1 Applicability.
Except as provided in Subparts B and
C. the provisions of this part apply to
the owner or operator of any stationary
source which contains an afiected facil-
ity, the construction or modification ot,
vrhlch Is .commenced after the date of
publics t-lor. in this part of any standard
(or, ii earlier, the date of publication of
any proposed standard") applicable to
that facility.
(39 FK 20790, June 14, 1974)
(40 FR 46250, October 6, 1975!
0 60. li Definitions.
As used in tills part, all terms not
dL-n.'ic;! licro'.n shall h-.ivc the ir.caning
Civc-r. '.hem in Die Act:
.n;c-nded by
P'.-:/.:<- l.::'.v 'j ': -t-'j't , fi-i SUtl. IGTC.i.
r" means the Ad-
;••,;:::: irri'.or c; the Environir-.i'ntal Fro-
: v': ; -.-:•. /•.•••-•"•:;.• or i:i_ :v.nhc,r:::-?d i c;-.rc-
fc) "Standard" ir.enns a standard of
performance proposed or promoigated
under this part.
(d) "Stationary source" cseross nnj-
building, structure, facility, or installa-
tion which emits or may erait aay'alr
pollutant and which contains any one or
combination of the'f olio—ing:
(i) ASccted.facilities.
(2) Existing faculties.
(3) Facilities of the type for vhich r,o
etundards have been promulgated! ta this
part.
(40 FR 58415. December 16, 1.975]
(e» "Affected facility" means, with
reference to a stationary scurcc, any ap-
paratus to v:hich a stauriard is sppiiicabic.
(f) "Ov.Ticr or operator" means anj
person v.-ho OT.TIS. leases, operates, con-
trols, or supervises an aflc-ctcd Sacility
or a statienr>ry source of ?,-l;icl:T mi af-
fected facility is a part.
>E> "Cc.'i-'.lniction" niuasis fa.l)rfastion.
erection, or installation of an. aSect.fid
facility.
(h) "Modification" means any phvsi-
cal change in. or change in the method
of operation of, an existing facility •wh'ich
increases Uie arcoiinL ot any air-psllutant
(to v»'hich a standard applies)-., cinilte:;
into the atmosphere by Uiat fEcHity or
which res:'.:;'us in Uie ep.'.'.'sion of ai:y sir
pollutnnt (ID which a standard applies)
into the atmosphere not p-ewouiiy
emitted.
|40 FK SS--1I5. IXM.-cn-.bcr 16. 19753
')> "Cii:ii:r.!.'!X;:u" r.-!!:;:ns, \\itn rc£|JCi-t
to '.ho i.'.!.-:.::.'..or. ol -i:f.v .v/i;r;-e" :r. ruc-
tion iiiia> t'.>) o! the AC;, tnat aiicv.iicT
or opri'alor )':r.s ur'dc
program cf coiv^rDOticn or :,->o'j'.S.~:i: if.n
01 that, an owner or operator has e^tevcd
tako and romnlf'e. within a rea
!:r:-ip. r. f.-o::: :;'-jc.-.:s p:\vci :!.:i» c; c~r:ii.r;-c-
tion or iv.C'iii'icatio".
v.-hi'.-i; ep'.lvu'j:.:. .-v.'JU'.-c the t:-.u:»rrj;-asi:.'r.
[if :!-.-!'.i ;i:ia -..'!)r.-;-j:o *.;v;- vicv.- of an ci^cct
in the b;irk;;ro--ir.J.
'ki "Kilro.Tcr: oxick-s" mo :-.:':"• s'a «3::-
ides of nitrogen f>:ce;y. r.iiro:^. oxidV1. is-
measured by tc.-i :i:';-t!:'xis cst forSSr i.i
Uiis part.
1 1) "3t:u-.'J:i"d co:;c!:t:-jr.r." inss=r.3 a.
t;-:v.r,erat\;rc o! HO'C 'Ci:'T-> nrai -- jjre>
?ure of 700 ii.::: »;•:' li;; f^C!.S2 in. of £=.:«>.
('mi "Propcnional r,a.T.;)'ir.r;" ssnecns
san'.ijHiifi at a rate thist pioduccrr sa. ccn-
Maiit ratio of i:\riiT.Oir::; ran ic-.'-twcl: 'pas
r.c\v rate-.
(n> "I.sok:iir-r.ic f:un>)!ir:[;" ^ncnns
samjilissr in v.'!i:c!i the linear vetc«:i*.y of
tiie pat; enwi-Uis the Jiii!-.;'':;!!-; nc^^ilc is
equal to that o? the undisturoes! gas
strw!T« at the- s.i;:ii>'.o point.
io> "Siariii:;" tnca.-is 'Jse s;M.iiir)jp in
oiK-raUoii c.r ai: allecleii tacili'.y "sis-
ol
'lor
ri!*.J up.uvi.ivi.-.Lfic I.! 111*!c ot ;:::' t*,*:V.'-ultf.in
cC-:*t«. i\i] fCjLJ'-i-ii':1 •:*!*. or I>!"O'.;C-^N f;u:;.'n".'3"iont
Copyritjiit •;: ',97fi fc/ The [iureuu ol ticlion.u.) V-.!:oiii. Inc.
-------
17.1:0522
FEDERAL REGULATION'S
fl) Method F. for concentration of par-
f'.cu"nt2 matter and associated moisture
content; ' •••
(C) Method 1 for sample find velocity
traverses;
(3) Method 2 for velocity end volu-
metric flow rate: and
(•J) Method 3 for gas analysis.
For Method 5. the sampling time
for each ran shall be at least four hours.
When a single EAF is sampled, the sam-
pling time for each run shall also in-
clude an Integral number of .heats.
Shorter sampling times, when necessi-
tated by process variables or other fac-
tors, may be approved by the Admin-
istrator. The minimum sample volume
shall be 4.5 dscm (160 dscf).
(c) -For the purpose of this subpart,
the ovrner or operator shall conduct the
demonstration of compliance with 60.-
2.72 During any performance test re-
quired under § 60.8 of this part, no gase-
ous~ diluents may be added to the
effluent gas stream after the fabric in
any pressurized fabric filter collector,
unless the amount of dilution is sepa-
rately determined and considered in the
determination of emissions.
(e) When more than one control de-
vice serves toe EAP(s) being tested, the
concentration of participate matter shall
be -determined, using the ' following
equation:
II-I
K'Lerc:
C.=concer.'.r3tion cf pirticubt* mzlltr
in cis.dsera (jr/osc!) as dctcnaincd
Lv s:clhnt! 5.
iV=IotaI number of control devices
trstfd.
Q.=vo:cmctric flow rate of Iho effluent
pas stream iu drcrr./hr (dsctrtir) as
determined by method 2.
(C.Q.). or (Q,).=v2!ae of the cpp'.icablc parameter for
each conuel device tciicd.
• (f> Any control device subject to the
provisions of tliis subpart shall be de-
sirncd and constructed to allow meas-
urement of emissions using applicable
test methods and procedures..
(£) Where emissions from any EAP(s)
are combined with emissions from facili-
ties not subject to the provisions of this
subpart but controlled by a common cap-
ture system and control device, the owner
or operator may use any of the follow-
ing procedures during a performance
test:
(1) Base compliance on control of the
combined emissions.
(2) Utilize a method 'acceptable to
the Administrator which compensates
for the emissions from the facilities not
subject to the provisions of this subpart.
(3) Any combination of 'the criteria
of paragraphs (g) (1) and (g> (2) of this
section.
(h) Where emissions from any EAF(s)
are combined with emissions from facili-
ties not subject to the provisions of
this subpart, the owner or operator may
use any of the following procedures for
demonstrating compliance with § 60.272
(1) Base compliance on control of the
combined emissions.
(2) Shut down operation of facilities
not subject to the provisions of this
subpart.
(3) Any combination of -the criteria
of paragraphs (h) (1) end (h) (2) of this
section.
* • • • •
(Sees. Ill and 114 of the Clean Air Act, as
emended by see. 4 (a) of Pub. L. 61-604, 64
Btat. 1678 (42 U.S.C. 1857C-S. 1857c-9)l
[40 FR 43850, September 23. 1975]
APPENDIX A - REI-ERENCE METHODS
[39 FR 20790, June 14, 1974|
1 — SAMPLE AND Vn-OCTTT
PCS STATIOIJABT 60DBCES
1. Principle and Applicability.
1.1 Principle. A sampling site and the
number cf traverse points ere selected to eld .
Sa the extraction of a representative sample.
14_ Applicability. Tills method, ebould
"be applied only when irieclriod fcy the test
procedures fcrdetcrmfialnK corr.pl lEtice with
the New Source Performance Standards. Un-
less otherwise specified'., this method 1? not
Intended to apply to gzo sucturj other than
those emitted directly to the atmoephcte
grit-bout further processing.
2. Procedure.
2.1 Selection of ft casapHng ill* and mini-
mum number or traverse points.
2.1.1 Select a sampling site taat IB nt Icvst
eight Etacfc or duct c*arneters downstream
and two diameters upstream from any Eow
disturbance such as a-bend, expansion, con-
traction, or visible Stone. Fcr rectangular
cross section, determine an equivalent diam-
eter frora the-followlng equation:
_ . , .. ^(length) (width)\
Equwlent diameter-2^ lcGgtfa+wi(jth )
equation 1-1
2.1.2 When the sfflsore campling site
criteria can be met,, t&o minimum number
of traverse points 13 twelve (13).
2.1.3 Some sampling; Situations render the
above sampling site; criteria Impractical.
When this Is tbe case., choose a convenient
sampling location end! ^se Figure 1-1 to de-
termine the minimum number of traverse
points. Under no coniHiiaons should a sam-
pling point be selected within 1 Inch of the
stack wall. To cbtalm tJns number of traverse
points for stacks 'or ctacts with a diameter
less than 2 feet, muBSiply the number of
points obtained from Figure 1-1 by 0.67.
2.1.4 To use Figure* E-l first measure the
distance from the cltossn sampling location
to the nearest upstream and downstream dis-
turbances. Determine: the corretpondlng
number of traverse polaats for each distance
from Figure 1-1. Select the higher of the
two numbers of traverse points, or a greater
value, such that for. circular stacks the num-
ber Is a multiple of. 4L and for rectangular
stacks the number JcSLpws the cr.tcrla of
section 22.2.
2.2 Cross-secUonci: 1'sxycut sad location or
traverse poluts.
25.1 For circular sSacks locate the tra-
verse points on at lessx two diameters ac-
cording to Flgur» Jt-2 nal Table 1-1. The
traverse ares sr.iU, dSsJno the stacfc crcsa
Bcctlon into equal' parss.
-------
STATIONARY SOURCES
S-305
12:1:0423
NUMBER OF DUCT DIAMETERS UPSTREAM'
(DISTANCE A)
FROM POINT OF ANY TYPE OF
DISTURBANCE (BEND. EXPANSION. CONTRACTION. ETC.)
NUMBER OF DUCT DIAMETERS DOWNSTREAM'
{DISTANCE B]
figure 1-1. Minimum number of traverse points.
Table 1-1. Lc-:it!i>n of traverse potrts in circu'sr
•~?rce-t of stac'< direter frn ^c'.ide voll f> traverr
Figure 1-2. Cross section of circular stac'k divided into 12 equal
areas, showing location of traverse points at centroid of each area.
O
_
O
o
i
1
o \ 9
i
r ' |
i
O 1 O
1
, -J
1
O 1 O
1
I
o
o
r
0
1-3. Cross section of rectangular stack divided into 12 equal
, v.-iiii traverse points at ccnlrpid of each area.
Traverse '
r.-rter : .
en 6 , ' "
cijro'.or. 2.4 6
; ; 14.6: 6.7 ; 4.4
•ter of trj.erse toir.ts on i dijreter
a •: :: > 12
3.3: 2.5 2.1
2 E5.4 25. 0; '.4.7 ; 10.5 ' S.2 6.7
3 •! 75.0: 29.5 . 13.4 | 14.6 11.5
4 53.3; 70.5 j 32.3 . 22.6 17.7
5 f S5.3
6 , 55.5
67.7.34.2 25.0
£3.6 65.8 J5.5
7 ! : £3.5:77.4 £;.5
8 1
9
10
1,
12
13
14
15
16
17
13
19
20
21
22
23
24
96.7 85. « 75.0
! SUE E2.3
i i 97. 5 I S3. 2
i |
i
M.3
97.9
;4
16
1.8 1.6
'4 20 :: ;.~
1.4
1.3.J
5.7 4.9 4.4 3.9.:
9. 9! '6. 5 7.5
20.1
ZJ.9
6.7
12.5 !0.9 9.7
16.5 U.6!l:.9 •
22.0 1S.8| 15.5 1
Ji.6125.3 23.5
63.4 37.5 25.6
73.1
62.5 33.2
20.4 1
25.0 <
20.6 :
79.9 ! 71.7 61. 8 1 3a.8- 3
61.4
90.1
7S.O 70.4
r.i :_-.
i.s .:••_:
5 ; S.S
° » "^ 3
:..£ !tr.5
4'.5 13-2
o'.O, '-S.1
i'.2 !;3..4
-:.: rs.c
61.2 33.3 :-~.3
33.1 76.4 1 69.4' (
54.3 37.5
53.2
91.5
95 1
53.4
D.7 2.S.'3
31.2 j 75.0 63.S £:._?
35.4
83 1
52.5
55.6
53.6
73.S 7
S3 5 <
2.S :J..7
c ^ ~v 9
£7.1 £2.0 ".3
90.3 c
93.3 E
95.1 S
sa.7 s
S
!
5.4,- cJ.,5
3.4 SJ13
1.3: cs.3
J.O C.KS
5.5 E2.T
3.5 K'..S
•S3u3
! J3-.3
6-25-76
Copyright ? 1976 by The Bureau of Notional Affairs, Inc.
[Appendix Ai
-------
121:0424
FEDERAL REGULATIONS
2.2.2 For rectangular stacks divide the
cross section into as many equal rectangular
areas as traverse points., such that the ratio
cf the length to the width of the elemental
areas is between one and two, I/ocate the
traverse points at the centroid of each equal
area according to Figure 1-3.
3. References.
Determining Dust Concentration In a Gas
Stream, ASME Performance Test Code £27,
New York, N.Y., 1957.
Devorkin, Howard, et al.. Air Pollution
Source Testing Manual, Air Pollution Control
District, Lcs Angeles, Calif. November 1963.
Methods for Determination of Velocity,
Vvlume, Dust and Mist Content of Gases,
Western Precipitation Division of Joy Manu-
facturing Co., Los Angeles, Calif. Bulletin
\VP-50. 1963.
Standard Method for Sampling Stacks fnr
Paniculate Matter. In: 197l" Book of ASTM
Standards, Part 23. Philadelphia, Pa. 1971,
ASTM Designation D-2928-71.
METHOD 2 DETERMINATION OF STACK CAS
VELOCITY AND VOLUMETRIC FLOW BATE (TYPE
S PITOT TUBE)
1. Principle and applicability.
1.1 Principle. Stack gas velocity is deter-
mined from the gas density and frcm meas-
urement of the velocity head using a Type S
(Stauscheibe or reverse type) pitot tube.
i.z Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with the
New Source Performance Standards.
2. Apparatus.
2.1 Pitot tube—Type S (Figure 2-1), or
equivalent, with a coefficient within ±5%
over the working range.
^ 2.2 Differential pressure gauge—Inclined
•nanometer, or equivalent, to measure velo-
Pcity head to v.nthin 10% of the minimum
vaiue.
2.3 Temperature gauge—Thermocouple or
equivalent attached to the pitot tube to
measure stack temperature to within 1.5% of
the minimum absolute stack temperature.
2.4 Pressure gauge—Mercury-ailed D-tube
manometer, or equivalent, to measure stack
pressure to within 0.1 in. Hg.
2.5 Barometer—To measure atmospheric
pressure to within 0.1 In. Hg.
2.6 Gas analyzer—To analyze gas composi-
tion for determining molecular weight.
2.7 Pitot tube—Standard type, to cali-
brate Type S pitot tube.
3. Procedure.
3.1 Set up the apparatus as shown In Fig-
ure 2-1. Make sure all connections are tight
and leak free. Measure the velocity head and
temperature at the traverse points specified
by Method 1.
3.2 Measure the static pressure in the
stack.
3.3 Determine the stack gas molecular
weight by gas analysis and appropriate cal-
culations as indicated in Method 3.
4. Calibration.
4.1 To calibrate the pitot tube, measure
the velocity Jread at some point in a flowing:
gas stream with both a Type S pitot tube and
a standard type pitot tube with known co-
efficient. Calibration should be done in the
laboratory and the velocity of the flowing gas
stream should be varied over the normal
working range. It is recommended that the
calibration be repeated after use at each field
site.
4.2 Calculate the pitot tube coefficient
using equation 2-1.
P =C /AP'.'J-
"'"' """A'Ap,,., equation 2-1
where:
C,,,c,, = Pitot tube coefficient of Type S
pitot tube.
CP>IJ=Pitot tube coefficient of standard
s type pitot tube (if unknown, use
0.59).
<4p,id = Velocity head measured by stand-
ard type pitot tube.
Ap,,,t = Velocity head measured by Type S
pitot. tube.
4.3 Compare the coefficfents of the Type S
pitot tube determined fires with one leg and
then the other pointed downstream. Use the
pitot tube only if the two coefficients differ by
no more than 0.01.
5. Calculations.
Use equation 2-2 to calculate the stack gas
velocity.
Equation 2-2
where:
(V,)«,,.=Stack gas velocity, feet per second (f.p.s.).
E°=Si-4<.4(lb.moic-°H)i'w"ent''cs''unlts
are used.
CB=Pitot tube coefficient, dimensionless.
(T.).,,.=AvcraEe absolute flack gas temperature,
(Vip)avc.=Averape, velocity head ot stack pas, inches
JlsO (see. Fir. 2-2J.
P,=Absolute stack pas pressure, inches He.
M.=.Molee\ilar weight of stack gas (wet basis),
Ib./lb.-molc.
Md=Dry molecular weight of slaek cas (from
Method 3).
B,0=rroportion by volume of water vapor in
the gas stream (from -Method 4).
Figure 2-2 shows a sample recording sheet
for velocity traverse data. Use the averages
in the last two columns of Figure 2-2 to de-
termine the average stack gas velocity from
Equation 2-2.
Use Equation 2-3 to calculate the stack
gas volumetric flow rate.
Q, = 3600
-------
STATIONARY SOURCES
S-305
121:0425
6. References.
Mark, L. S., Mechanical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1951.
Perry, J. H., Chemical Engineers' Hand-
book, McGraw-Hill Book Co., Inc., New York,
N.Y., 1960.
Shigehara, R. T., W. F. Todd, and W. S.
Smith, Significance ol Errors in Stack Sam-
pling Measurements. Paper presented at She
Annual Meeting of the Air Pollution Control
Association, St. Louis, Mo., June 14-19; 1STO.
Standard Method for Sampling Stacks. Jor
Particulate Matter, In: 1971 Book of AS'TM
Standards, Part 23, Philadelphia, Pa., IST71.
ASTM Designation D-2928-71.
Vennard, J. K., Elementary Fluid' Mechooi--
!cs, John WUey £: Sons, Inc., New York, N,75T.,
1947.
PLANT_
DATE
RUN NO.
STACK DIAMETER, in.
BAROMETRIC. PRESSURE, in. Hg.
STATIC PRESSURE IN STACK (P ), in. Hg.
OPERATORS
SCHEMATIC OF STACK
CROSS SECTION
Traverse point
number
Velocity head,
in. H,0
Stack Temperature
S
AVERAGE:
Figure 2-2. Velocity traverse data.
6-25-76
Copyright £. 1976 by The Bureou of Notionoi Aitoirs, inc.
[Appendix A)
-------
121:0426
FEDERAL REGULATIONS
METHOD 3 - CAS ANALYSIS FOP. CARBON DIOXIDE,
EXCESS AIF., AKD DRY MOLECULAR WEIGHT
1. Principle and applicability.
l.l Principle. An integrated or grab gas
is extracted from a sampling point
and "analyzed for its components using an
Orsat analyzer.
1.2 Applicability. This method should be
applied only when specified by the test pro-
cedures for determining compliance with the
New Source Performance Standards. The test
procedure will indicate whether a grab sam-
ple or an integrated sample is to be used.
2. Appcra.i-^3.
2.1 Grab sample (Figure 3-1 } .
2.1.1 Probe — Stainless steel or Pyrex *
glass, equipped with a filter to remove partic-
ujste matter.
2.1.2 Pump — One-way squeeze bulb, or
equivalent, to transport gas sample to
analvzer.
2.2 Integrated sample (Figure 3-2).
2.2.1 Probe—Stainless steel or Pyrex'
glass, equipped with a filter to remove per-
ticulate matter.
2.2.2 Air-cooled condenser or equivalent—
To remove any excess moisture.
2.2.3 Needle valve—To adjust flow rate.
2.2.4 Pump—Leak-free, diaphragm tj-pe,
or equivalent, to pull gas.
2.2.5 Hate rneter—To measure a flow
range from 0 to 0.035 cfm.
2.2.6 Flexible bag—Tedlar,1 or equivalent,
with a capacity of 2 to 3 cu. ft. Leak test the
bag iu the laboratory before using.
2.2.7 Pltot tube—Type S. or equivalent,
attached to the probe so that the sampling
flow rate can be regulated proportional to
the stack gas velocity when velocity is vary-
ing with time or a sample traverse is
conducted.
2.3 Analysis.
2.3.1 Orsat analyzer, or equivalent.
PROSE
FLEXIBLE TUBING
TO ANALYZER
FILTER (GLASS WOOL)
SQUEEZE BULB
Figure 3-11 Grab-sampling train.
RATE METER
AIR-COOLED COMDEUSER
::LTER (GLASS WOOL)
QUICK DISCONNECT
.BAG
3. Procedure.
3.1 Grab sampling.
3.1.1 Set up the equipment as shown In
Figure 3-1. making sure all connections are
leak-free. Place the probe in the stack at a
sampling point and purge the sampling line.
3.1.2 Draw sample into the analyzer.
3.2 Integrated sampling;.
3.2.1 Evacuate, the flexible bag. Set v.p the
equipment as shown in Figure 3-2 with the
bag disconnected. Place the probe in the
stack and purge the sampling line. Connect
the bag, making sure that all connections are
tight and that there are rro leaks.
3.2.2 Sample at a rate proportional to the
stack velocity.
3.3 Analysis.
3.3.1 Determine the CO., O... and CO con-
centrations as soon as possible.'Make ?..? many
passes as are necessary to give constant, renc!-
ings. If more than ten passes are necessary.
replace the absorbing solution.
3.3.2 For grab sampling-, repeat the sam-
pling and analysis until three consecutive
samples vary no more than 0.5 percent bv
volume for each component; being analyzed'.
3.3.3 For integrated sampling, repeat the
analysis of the sample unto three consecu-
tive analyses vary no more liian 0.2 percent
by volume lor each component being
analyzed.
4. Calculations.
4.1 Carbon dioxide. Average the three con-
secutive runs and report trte result to the
nearest 0.1 C0 CO..
4.2 Excess air. Use Equation 3-1 to calcu-
late excess air. and averag.»> ttlse runs. Report
the result to the nearest 0.1 rb excess air.
%EA =
Figure Z-2, Integrated gas -sampling Iraitii
N;)-(Tc 0,)-rO.:i('-c CO)
equation 3-1
where :
<;;,EA = Percent excess air.
7tO., = Percent, oxygen by vclume. dry basis.
%N3 — Percent nitrogen b*- volume, dry
basis.
TrGO = Percent carbon n:c3:ox:de by vol-
ume. dry ba?:?.
0.264 = Ratio of oxygen to ziitrogen in tv.r
by volume.
4.3 Dry molecular weight. TJse Equation
3-2 to calculate dry molecvJjir weight and
average the runs. Report t£e result to the
nearest tenth.
Ma = 0.«C"£CO. 1 -0.32, ' ; O. l
rC I'M ,X.- --CO.
equation 3-2
where :
Md=Dry molee»'''/ir weight. Ib./lb-mole.
7eCO^=Percent csriw. cticxkJe by volume,
dry basis.
TcO— Percent ^A/gen few volume, dry
basis.
%N~Percent nitrogen by volume, ary
basis.
0.44=Molecular weight a* •carbon dioxide
divided by 100'.
0.32=Molecular weight o* oxygen divided
by 100.
0.28=Molecular weight el nitrogen and
CO divided by 1OO.
Environment Reporter
[Appendix A]
26
-------
K)
S"
n
:r
&
+0
*-J
o
•O
•V"
5. llc/craiccs.
Altshuller, A. P.. ct nl., Storage of Oiir.cs
and Vapors In Plastic Dags, Int. ,1. Air &
V.'iUnr Pollution, (i:7.r)-81, 1903.
Conner, William D., and J. S. Nader, Air
Sampling with Plastic Uags, Journal of Use
American Industrial Hygiene Assoclntlun,
25:21)1-297, May-Jur.o 1
-------
121:0423
FEDERAL REGULATIONS
4.2 Gas volume.
°R /V P \
17-71in7Hi(-frO
equation 4-2
where:
Vme =rDry gas volume through meter at
standard conditions, cu. ft.
VD =Dry gas volume measured by meter,
cu. ft.
Pm = Barometric pressure at the dry gas
meter, inches Hg.
P.td = Pressure at standard conditions, 29.92
inches Hg.
Tnd = Ab5olute temperature at standard
conditions, 530° R.
Tm = Absolute temperature at meter (°F +
460), -R.
4.3 Moisture content.
-+(0.025)
c
equation 4-3
v,-here:
Bwo = Proportion by volume of water vapor
in the gas stream, dimensionless.
Vne = Volume of water vapor collected
(standard conditions) , cu. ft.
Vnic =Dry gas volume through meter
(standard conditions) , cu. ft.
Bwii = Approximate volumetric proportion
of water vapor in the gas stream
leaving the impingers. 0.025.
5. References.
Air Pollution Sr.ginee.-ins Manual. Daniel-
Eon. J. A. (ed.), U.S. DKEW, PHS, National
Center' 'or Air Pollution Control, Cincinnati,
Ohio, -PHS Publication No. 999-AP-^O, 1967.
Devorkin, Howard, et a!., Air Pollution
Source Testing Manu?.!, Air Pollution Con-
ol District, Los Angeles, Calif., November
2.1.4 Filter Holder—Pyrex1 glass with
heating system capable of maintaining mini-
mum temperature of 225" F.
2.1.5 Impingers / Condenser—Four impin-
gers connected In series with glass ball joint
fittings. The first, third, and fourth impin-
gers are of the Greenburg-Smith design,
modified by replacing the tip with a >/2-inch
ID glass tube extending to one-half inch
'from the bottom of the flask. The second im-
pinger is of the Greentaurg-Smlth design
with the standard tip. A condenser may be
used in place of the impingers provided that
the moisture content of the stack gas can
still be determined.
2.1.6 Metering system—Vacuum gauge,
leak-free pump, thermometers capable of
measuring temperature to within 5° F., dry
gas meter with 2% accuracy, and related
equipment, or equivalent, as required to
maintain an Isokinetic sampling rate and to
determine sample volume.
2.1.7 Barometer—To measure atmospheric
pressure to ±0.1 inches Hg.
2.2 Sample recovery.
Methods for Determination of Velocity,
Volume, Dust arid Mist Content of Gases,
V.'estem precipitation Division of Joy Manu-
' act urine Co., Los Angeles, Calif., Bulletin
•.YP-50. 1SGS.
MZTKCO 5- — DETTF.MINATTON OF PAP.TICULATE
ELUSIONS Fxo:.: STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. P?.--ticu!ate matter is with-
drav.-n isok!net:ca31y Irom the source and its
••veight :s determined graviraetrically after re-
moval of uncombined water.
1.2 Applicability. This method is applica-
ble- ..'or the determination of participate emis-
sions from stationary sources only when
rpecified by the test procedures for determin-
ing compliance with New Source Perform-'
ance Standards.
2. Apparatus.
2.1 Sampling train. The design specifica-
tions of the particulote sampling train used
'or EPA (Figure 5-i i are described in APTD-
0581. Commercial models of this train are
available
2.1.1 Nozzle — Stainless steel (316) with
sharp, tapered leading edge.
2.1.2 Probe — Pyrex * glass with a heating
cvj'.cm capable of maintaining a minimum
g.is temperature of 250° F. at the exit end
tiuring sampling to prevent condensation
frc.:n occurring. When length limitations
i greater than about. 8 ft.': are encountered at
temperatures less than GOO" F., Incoloy 825 ',
or equivalent, may be used. Probes for sam-
pling gas streams at temperatures in tncess
of 600° F. must have been approved by the
Administrator.
2.1.3 Pitot tube — Type S, or equivalent,
Attached to probe to monitor stack gas
Velocity.
i Trade name.
REVERSE-TYPE
PITOT TUBE
2.2.1 Probe brush—At least as long as:
probe.
2.2.2 Glass wash bottles—Two.
2.2.3 Glass sample storage containers.
2.2.4 Graduated cylinder—250 ml.
2.3 Analysis.
2.3.1 Glass weighing dishes.
2.3.2 Desiccator.
2.3.3 Analytical balance—To measure to
±0.1 mg.
2.3.4 Trip balance—300 g. capacity, to
measure to ±0.05 g.
3. Reagents.
3.1 Sampling.
3.1.1 Filters—Glass fiber, MSA 1106 BH ».
or equivalent, numbered for identification
and preweighed.
3.1.2 Silica g'l—Indicating type, 6-1G
mesh, dried at 175' C. (350° F.) for 2 hours.
3.1.3 Water.
3.1.4 Crushed ice.
3.2 Sample recovery.
3.2.1 Ac;tcne—Reagent grade.
3.3 Analysis.
3.3.1 Water.
IMPINGE!? TRAIN OPTIONAL. MAY BE REPLACED
BY AK EQUIVALENT CONDENSER
HEATED AREA FILTER HOLDER / THERMOMETER CHECK
VALVE
..VACUUN5
LINE
THERMOMETERS'
DRY TEST METER
AIR-TIGHT
PUMP
Figure 5-1. Particulate-sarhplir.g train.
3.3.2 Desiccr.nt--Drierlte,' indicating.
4. Procedure.
4.1 Sampling
4.1.1 After selecting the sampling site and
the minimum 'number of sampling points,
determine the stack pressure, temperature,
moisture, and range of velocity head.
4.1.2 Preparation of collection train.
Weigh to the nearest gram approximately 200
g. of silica gel. Label a filter of proper diam-
eter, desiccate - for at least 24 hours and
weigh to the nearest 0.5 mg. in a room where
the relative humidity is less than 50%. Place
100 ml. of water In each of the first two
Impingers, leave the third impinger empty,
and place approximately 200 g. of preweighed
silica gel In the fourth impinger. Set up the
train without the probe as in Figure 5-1.
Leak check the sampling train at the sam-
pling site by plugging up the inlet to the fil-
ter holder and pulling a 15 in. Hg vacuum. A
leakage rate not in excess of 0.02 c.f.m. at a
vacuum of 15 in. Hg Is acceptable. Attach
the probe and adjust the heater to provide a
gas temperature o'f about 250° F. at the probe
outlet. Turn on the filter heating system.
Place crushed ice around the impingers. Add
1 Trade name.
'Dry using Drierite ' at 70° F.±10° F.
more ice during the run to keep the temper-
ature of the gases leaving the last impinger
as low as possible and preferably at 70s F.,
or less. Temperatures above 70° F. may result
in damage to the dry gas meter from either
moisture condensation or excessive heat.
4.1.3 Paniculate train operation. For each
run, record the data required on the example
sheet shown in Figure 5-2. Take readings it
each sampling pcir.t, at least every 5 minutes,
and when significant changes in stack con-
ditions necessitate additional adjustments
in flow rate. To begin sampling, position the
nozzle at the first traverse point with the
tip pointing directly into the gas stream.
Immediately start the pump and adjust the
flow to isckinetlc conditions. Sample for at
least 5 minutes at each traverse point; sam-
pling time r.iust be the snrne for each point.
Maintain isskhictic sampling throughout the
sampling period. Nomographs are available
which aid in the rapid adjustment of •.:•;*
sampling rats without other computations'.
APTD-0576 details the procedure for usipg
these nomographs. Turn off the pump at the
conclusion of each run and record the final
readings. Remove the probe and nozzle from
the stack and handle in accordance with the
sample recovery process described, in section
4.2.
Environment Reporter
[Appendix A)
28
-------
STATIONARY SOURCES
S-3Q1
121:0429
IXATIOT
OTCUTM
CATt
SXUTU 601 N0^
KliB'tOI N0.
V =V
>w"d ''
D wxsrutt. x_
HtATU BOI SOTINO
MOSE LENGTH. •».
pH^O RT.m Ib.
MH,o P.* 454 gin.
t W>1U StltlNO_
C Of S1ACX CR01S SECTION
IWVERSE POIKT
KUVLtR
SAWPLIfVC
TIME
(•J. mn.
1
t
1
TOTAL
tvfftOE
SIATIC
WitiUJW.
IPj!. in. Hg,
suet
tWKRAIUK
(Ts). 'f
vitocm
HIAO
UFi).
1
1
1
PtiSSjKI
OlfftSfVIIAl.
ACKKS
CRIMCE
UtflR
I*HJ,
IttHjO
GUSUFU
VtXUUE
(vwj. tr
GAS SA*i
OF CM
U«V11C
C»C£»!t« Ot
UUT KPMCU*.
•f
1
equation 5<--2
where:
V»,,4= Volume of water vapor In the gas
sample (standard conditions-}.
cu. ft.
Vie = Total volume of liquid collected, in
•impingers and silica gel (see-Fig-
ure 5-3), ml.
pnao= Density of water, 1 gym!.
MHao = Molecular weight of water, 18 Ib./
Ib.-mole.
R = Ideal gas constant, 21.83 Inches
Hg—cu. ft./lb.-rnole-'R.
T.ld= Absolute temperature at standard
conditions, 530° R.
P.,4= Absolute pressure at standard con-
ditions, 29.92 inches Hg.
6.4 Moisture content.
^-2. Parliculate lie'd daia.
4.2 Sample recovery. E::ercise care in mov-
ing the collection train from the test site to
the sample recovery area to minimize the
loss of collected sample or the gain of
ertraneo-us particulate matter. Set aside a
portion o* the acetone used In the sample
recovery as a blank for analysis. Measure the
•volume" o' water from the first three im-
pingers, then discard. Place the samples in
containers as -follows:
Container Ko. 1. Remove the filter from
its holder, place in this container, and seal.
Container No. 2. Place loose particulate
matter and acetone washings from all
sample-exposed surfaces prior to the filter
in this container and seal. Use a razor blade,
brush, or rubber policeman to lose adhering
particles.
Cc7ife:'?icr A'o. 3. Transfer the silica gel
from the fourth impinger to the original con-
tainer and seal. Use a rubber policeman as
an aid in removing silica gel from the
impinger.
4.3 Anf.lvEis. Record the data required on
the example sheet shown In Figure 5-3.
Handle each sample container as follows:
Container No. 1. Transfer the filter and
any loose participate matter from the sample
container to a tared glass weighing dish,
desiccate, and dry to a constant weight. Re-
port results to the nearest 0.5 mg.
Confci7icr ;Vo. 2. Transfer the acetone
washings to a tared beaker and evaporate to
dryness ot ambient temperature and pres-
sv.re. Desiccate and dry to a constant weight.
Report results to the nearest 0.5 rng.
Container No. 3. Weigh the spent silica gel
and report to the nearest gram,
5. Calibration.
Use methods and equipment which have
been approved by the Administrator to
calibrate the orifice meter, pltot tube, dry
gas meter, and probe heater. Recalibrate
after each test series.
6. Calculations.
6.1 Average dry gas meter temperature
and average orifice pressure drop. See data
sheet (Figure 6-2).
6.3 Dry- gas volume. Correct the sample
volume measured by the .dry gas meter to
standard conditions (70° F_ 29.924nches Hg)
by using Equation 5—1.
AH
"V..ld + V..ld
equation- G
where:
13.6
equation 5-1
where:
Volld= Volume of gas sample through the
dry gas .meter (standard condi-
tions) , cu. ft.
Vn = Volume of gas sample through the
dry gas meter (meter condi-
tions) , cu. ft.
Tiia = Absolute temperature at standard
conditions, 530° R.
Proportion by volume of water vapor in the t_.s
stream, dimcnsionless.
^"•i
-------
121:0430
FEDERAL REGULATIONS
PLANT.
DATE
RUN NO.
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED,
mg
FINAL WEIGHT
;x^.
TARE WEIGHT
^<
WEIGHT GAIN
_
FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME.
ml
SILICA GEL
WEIGHT.
9
g* ml
CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
INCREASE BY DENSITY OF WATER. (1 g. ml):
INHjO=Density of water, 1 g./ml.
R = Ideal gas constant, 21.S3 Inches ITg-cu. fl'./lb.
mole-°R.
MH,O = Molecular weight of water, 18 Ib./lb.-mole.
Vm=Volume of pas sample through the dry gas meter
(meter conditions), cu. ft.
Tm=Absolute average dry gas meter temperature
(see Fij!ure5-2),°R.
Ft,., = Barometric pressure at sampling site, inches-
He.
A|[=Avcragc pressure drop across the orifice (see
Fig. 6-2), inches HiO.
T,=Absolute average stack gas temperature (see
Fig. 5-2). °R.
e=Total sampling time, min.
V,=Stnck gas velocity calculated by Method 2,
Equation 2-2, ft./sec.
r,=Absohne stack gas pressure, inches Hg.
Au = Cross-s
-------
.9'
to
V
n
o
neees.snry only If a snmplo traverso Is re-
qulrccl. or it clack gas velocity varies with
time.
2.2 Sample recovery.
2.2.1 Qlttss wash bottles—Two.
2.2.2 Polyethylene storage bottles—To
store Implngcr samples.
2.3 Analysis.
PROBE (END PACKED
WITH QUARTZ
PYREX WOOL
rz OR ./ ST.'
\_t:
STACK WALL
MIDGET BUBBLER MIDGET IMPINGERS
GLASS WOOL
SILICA GEL DRYING TUBE
I
TYPE SPJTOT TUBE
PITOT MANOMETER
THERMOMETER
'PUMP
DRY GAS METER ROTA'METER
Figure 6-1, SOg sampling train.
2.8.1 Pipettes—Transfer type, 6 ml. and
10 ml. sizes (0.1 ml. divisions) and 25 ml.
Blzo (0.2 ml. divisions).
2.3.2 Volumetric flasks—50 ml., 100 ml.,
and 1,000 ml.
2.3.3 Burettes—5 ml. and BO ml.
2.3.4 Erlenmeyer flask—126 ml.
3. Reagents. .
3.1 Sampling.
3.1.1 Water—Detonlzed, distilled.
3.1.2 Isopropanol, 80%—Mix 80 ml. of Iso-
propanol with 20 ml. of distilled water.
3.1.3 Hydrogen peroxide, 3%—dilute 100
ml. of 30% hydrogen peroxide to 1 liter with
distilled water. Prepare fresh dally.
3.2 Snmple recovery.
3.2.1 Water—Dclonlzed, distilled.
3.2.2 Isopropanol, 80%.
3.3 Analysis.
3.3.1 Water—Delonlzed, distilled.
3.3.2 Isopropanol.
3.3.3 Thorlnl Indicator—l-(o-arsonophcn-
ylazo)-2-naphthol-3.8-dlsulfonlc acid, dlso-
dlum salt (or equivalent). Dissolve 0.20 g. In
100 ml. distilled water.
3.3.4 Barium perchlorate (0.01 N)—^Dis-
solve 1.96 g. of bnrliim perchlorate
|Ba(CIp,),: 311,9] In 200 mj. "distilled water
velocity. Take readings at least every five
minutes and when significant changes in
stack conditions necessitate additional ad-
justments In flow rate. To begin sampling,
position the tip of the probe at the first
sampling point and start the pump. Sam-
ple proportionally throughout the run. At
tho conclusion of each run, turn off the
pump and record tho final readings. Remove
the probe from the stack and disconnect It
from the train. Drain tho Ice bath and purge
the remaining part of the train by drawing
clean ambient air through tho system for 15
minutes.
4.2 Sample recovery. Disconnect tho 1m-
plngers after purging. Discard the contents
of the midget bubbler. Pour the contents of
the midget Implhgers Into a polyethylene
shipment bottle. Rinse tho three midget 1m-
plngcrs and the connecting tubes with dis-
tilled water and add these washings to the
same storage container.
4.3 Sample analysis. Transfer the contents
of the storage container to a 60 ml. volu-
metric flask. Dilute to the mark with de-
lonlzed, distilled water. Pipette a 10 ml.
aliquot of this solution Into a 125 ml. Erlen-
meyer flask. Add 40 ml. of Isopropanol and
two to tout; drops of thorlu Indicator. Titrate
to o. pink endpolnt using 0.01 N barium
perchlorate. Run a blank with each series
of samples.
6. Calibration.
6.1 Use standard methods and equipment
which have been approved by the Adminis-
trator to calibrate tho rotametcr, pltot tube,
dry gas meter, and probe heater.
6.2 Standardize the barium perchlorato
against 25 ml. of standard sulfurlc acid con-
taining 100 ml. of Isopropanol.
0. Calculations.
6.1 Dry gas volume. Correct the sample
volume measured by the dry gas meter to
standard conditions (70' F. and 29.92 Inches
Hg) by using equation 6-1.
1771
1
°R
in. 11 gV. T
equation 6-1
when:
V
tl<>-=> Volume of gas sample through the
dry gas meter (standard condi-
tions), cu. ft.
Vm= Volume of gas sample through the
dry gas meter (meter condi-
tions), cu. ft.
T.ld= Absolute temperature at standard
conditions, 630* R.
Tm = Average dry gas meter temperature,
Pb,r— Barometric pressure at the orifice
meter, Inches Hg.
Ptl. = Absolute pressure at standard con-
ditions, 29.92 Inches Hg.
0.3 Sulfur dioxide concentration.
and dilute to 1 liter with Isopropanol. Stand-
ardize with Bulfurlo acid. Barium chloride
may be used.
3.3.6 Sulfurlc acid standard (0.01 N) —
Purchase or standardize to ±0.0002 N
against 0.01N NaOH which has previously
been standardized against potassium acid
phthalate (primary standard grade).
4. Procedure.
4.1 Sampling.
4.1.1 Preparation of collection train. Pour
15 ml. of 80% Isopropanol Into the midget
bubbler and 16 ml. of 3% hydrogen peroxide
Into each of the first two midget Implngcrs.
Leave the final midget Implngcr dry. Assem-
ble the train as shown In Figure 6-1. Leak
check the sampling train at tho sampling
site by plugging tho probe Inlet and pulling
a 10 Inches Hg vacuum. A leakage rate not
In excess of 1 % of the sampling rate is ac-
ceptable. Carefully release tho probe Inlet
plug and turn off the pump. Place crushed
Ice around the Implngers. Add more Ice dur-
ing the run to keep the temperature of the
gases leaving the last Implnger at 70' F. or
less.
4.1.2 Samplo collection. Adjust the sam-
nlq flow ra^i iaVQnprUpna.1 to "U>9 gtaqk paa
/ ib-i \
CB03=( 7.05X10-'— ~ )
3 \ g.-uil./
m.ld
equation 6-2
where:
C.jo3= Concentration of sulfur dioxide
at standard conditions, dry
basis, Ib./cu. ft.
7.05 X lO-5^ Conversion factor. Including tho
number of grams per gram
equivalent of sulfur dioxide
(32 g./g.-eq.). 463.6 g./lb., and
1,000 ml./l., Ib.-l./g.-ml.
V,= Volume of barium perchlorato
tltrant used for the sample,
ml.
Vlh=>Volume of barium perchlorate
tltrant used for the blank, ml.
JV = Normality of barium perchlorate
tltrant, g.-eq./l.
V.olq = Total solution volume of sulfur
dioxide, 60 ml.
V, = Volume of sample aliquot ti-
trated, ml.
Vnj.ld=-Volume'cf gas sample through
the dry gas meter (standard
conditions), cu. ft., see Eqim-
tjpn (Mi
7. References.
Atmospheric Emissions from Sulfurlc Aclcl
Manufacturing Processes, U.S. DHEW. PHS,
Division of Air Pollution, Public Health Serv-
ice Publication No. 999-AP-13, Cincinnati,
Ohio. 1965.
Corbett, P. P., Tho Determination of SO,
and ,'5O, In Flue Gaues, Journal of the Insti-
tute of Fuel; 24:237-243, 1961.
Matty, R. E. and E. K. Dlchl. Measuring
Flue-Gas SCX and SO,, Power .101:94-97, No-
vember, 1957"
Patton. W. F. and J. A. Brink, Jr., New
Equipment and Techniques for Sampling
Chemical Process Gases, J. A!r Pollution Con-
trol Association, 13, 162 (1963).
METHOD 7—DETERMINATION OF NITaOGEN OXIDH
EMISSIONS FROM STATIONARY SOURCES
1. Principle and applicability.
1.1 Principle. A grab sample Is collected
In an evacuated flask containing a dilute
sulfurlc acldrhydrogcn peroxide absorbing
oplution, and tli'e jiitjogeri exjilcs,
-------
METHOD 13B
DETERMINATION OF TOTAL FLUORIDE EMISSIONS
-------
FEDERAL nEGULA7IOi\'S
»:::i t iswi'ii'Titi iij
»vi«ucicmif»"T
FPOIt Ht»TtMint\
>:icOf 1T1CC C»-"iS M
i
1
!
Lri£4V"
•
,.;;^
„.«
S*i-I
JX
HJO
•
pun>*M:u.
*ciosi
wo'.-a
'
j..i:'.ce \v:*.:i :•.-•-,'.• source pcr-
i'roo::i. :'.ro !:o'. cv.:'.r.ii'.rv'.i-.ciy ro'.leciccl or
i-.^^Mired by t!:is proceciure.
J. Xc-.ne a::?. icnnriMrj'.
T;-.e fluoride specL'ic ion eiertrode ar.nlyti-
oi! nietlioci covers the range of 0.02-2,000 t*S
K. ;r.l; i'.ov.-cvcr. rn;r_aure:-.ients of less tl'.an
0.1 ;:g F/:v.: rcciv.irc txtra ci-.re. Sciwitivity has
r.o'. bfc:i clCiermincd..
. .
During trie laboratory nr.aiysu. nluininuni
in exce-js of 300 mj/liier and silicon dioxide
1:1 fxccss of 300 ; g/iiicr \vi!J prcve:ii complete
recovery of f.ucrioe.
4. Pivctv.'G?!. Accuracy end S.'abi/ity.
T!:e accuracy of fluoride electrode measure-
:-.-.f:'.Hj hrii oeen repcri'.-J \y,' vunous re-
5.e:ir.T!iers 10 be in the range cf 1-5 percent in
a co:icciur::t:C!! rf.iif;e of O.C-- to 80 mp/l. A
< ::.\!.;!C in the iGirspcmfjre of the sample will
c-:.:i:.jV t!ic cicc'.rcdc rf.spc::;e; a c!i:.nge. ol
1'C v.-:!l produce a 1.5 percent relative error
in tjit- ;.':easureir.e;;t. La<.k o! stability in tile
f:ef..or.ii'.cr •-•.;;:- to moasiurc Et'.'.F can intru-
f.ure cvrc". A:v error of 1 ir.ilhvolt in the E."P
r.jeasv.reM-.er.i. produces a relative error of 4
jn'ivf.!'. r^:;?.rc'.'.Cb--'. of '.lie iibsolute ci>:;cor.-
.. '. S..•-;•:••'.(.' irr.ui. 5-e KI^'.KC ICA-l
:.:.-..MLl U.-.): r. :;; :in-..;i\r to t::c Mcil.c.%1 5
^:i2 no;.il;c:i of the 'ilter. Commercial models
,: ;:,.:. ::;i:. sr.-; .'ivc:.:;:.<;p. j;^«:ever. If one.
i:-,-:>;:•.•:•, 10 build !-'.s ov.'n, coir.p'.ctc c.or:-,:ruc-
!:•.•:! ij-l:,:-, ::re <:-.TCr:l'C'J !:i APTD-OJS1; f';r
up.'.rr.t nnj
for nlloivnble modifications to Figure ISA-1,
.•-e.e tuc following subscclions.
The ojvrating and ir.Tintenniire procedures
for ihe sampling train arc described In
APTD-057G. Since correct usa^c Is impor-
tant in obtafn:np valid results, nil v.sers
should read the APTD-C57G document and
adopt the opcrAting and mniKtcnancc pro-
cedures outlined In it. unless otherwise spec-
ified herein,
5.1.1 Probe norr.lc—Stainless steel (316)
•with sh:i:p. tapered Icafiinj; edj;e. Tnc ar.j'le
of taper shall be £30' and the taper shall be
0:1 the outside to preserve a constant hucr-
I'-.ii diameter. T:'.e prolje nc^iie shall '-'C of
the ljuuon-hoo;: or elbov/ dtsijn. v.r.lor;
cthrr\vi;e speciSed l;y t^e Adrr.ir.jr'.rator.
'Hie v:,i'! thickness of the nozzle shall be
ICES tha:; or equr>! to that of 20 caupe f.ib-
iiiy. i.e.. 0.1 G5 cm (O.OC5 in.) and the distance
from the tip of the nozzle to the first bend
or point of disturbance shcil be at least two
times the outside no2z!c diameter. The noz-
zie shall be constructed from seamless stn.in-
1:E3, steel tubing. Other configurations ancl
con.=.tructio:i material rr.ay he used with ap-
proval from the Administrator.
A ranne of sizes suitable for tsokinetlc
sampling shouid be available, e.g.. 0.32 c:n
('.a in.) up to 1.27 cm f'-'., in.) (or larger if
higher volume sair.p'.'.r.g trains are used)
::-.h.irte diameter (ID) no7?.!es in Increments
of O.iC cm (:;.; in.). F.ach ncxr.ie shall be
calibrated according to the procedures out-
lined in the calihri-.lon section.
5.1.2 P.-obc- !::5fr—Ecrosllicr.l? pla.^3 or
stainic-si, s:ec: (31Cj. V.'hcn the :ilter is lo-
cated iiyimedir.tely after 'Oie probe, a probe
tw.Mins sysioin ir.:.y be xued to prevent filter
pr.iL".'.:!!,; vtiuliin^1 ' frovr. moisture cor.clc:i-
saiinn. 7'Me temperature in the probe shall
not OMC-OCU'120-14 C (2-lSrt:25:F).
j.l ?, Piiot -..i'.:;—Ty~.: .••-. or other cievr.-c
a-iirovc-ti by the .•-.T.ir.i'.trati-r. n:taci:eu to
probe to aiiov: tcn:>'-j:.t monitorin-j of tht
s;:icl'. tjas velocity. Ti:c r.'.cc cper.irv.-r, cf tho
pilot t.iDc ai:d :tic prv!:e i,o.~.i'!(.- '.'.ai! !jt r.d-
;;.-.'c:'.' a'.id ;;rii\.'.:c; '. > c-tc:: o:r:c-r. noi ijecr;;-
£.\nly on the sar.ic piaiJO, tiunn;j campling.
The free spa:* iiotwcen ine no/./le :nid pito".
:\::;E MiMi be a: lra;>. 1.9 cm 1'J.Tj in.;. T::u
Iri-L- sp.:cu :.!-.:\!l be set b-jrc:l en u 1.3 cm
Id.'j lit.) ID i;oj^:e. '.v;:.':'!i i:i liie lfir;;rst t:;;e
ItO.'.L'iV Uv-C.I
ThC'pitol ti'''.)C :m:('t air.."- meet th? cr(.:r:'. v
Speclficil In r..>;'-K:i '.):':: '.•";! r -
cording to tho pr/xTtlxirc In the ra;n>:.it:.-:i
action of that rr.ct!iC'd.
5.1.4 DlffTrntlnl prcranrc raupr — in-
clined rr.int'mctor cny.r^Wf of r.irr.r.v.rii'.^
velocity hr-ad In within 10 pcr.'cr.i o( i>.,r
minimum rr.'.v-rrod v.iiuf. rc!:.-v n d'Tc:1::!-
lial prc?:--.:re of in. >V.:TI idf:'. Irj.) \\;\'T
paupc. micrnrn.-:ni.mr-tcr5 uli'u .'•rnr-l'.ivli'.r.--.
of C.013 ir.ni (ti.nc?5 In.) f-'nov.'.d he \:~t:'..
However. r.ilcromanc:iU'trr? arc- V'ot car.ilv
adaptable to field rondllior.s and nrc suit
easy to \ir,? with pulsating flow. Thus, other
inethpds or devices acceptable to ihr Acl-
minl?tratcr may be xiscd whcr. *onti:tic:i"
\varrant.
5.1.5 Filter l:o'.c!er — B.irnsi'.:c.ito (.I.-.'-"
\vilii a plas^ frit f.lior SHppnt!. s:'.': a f :':'i-o:-.!'
riibhcr itaVtiot. Other inateri.ii-. of cov.'trvr-
(ion mnv b? vis^rl with nr-pr-r-val .'rrr.1. •'.>"•
Admini5tr.-itor. c c,. if probe l;rer is s •.?.•• v-
Irss slrrl. ',h?n IViU-r JirU'.cr nisy be j-'i.i::;:o"-'
steel. The holder desijii shall provide n posi-
tive son! against If.iknj.-; fri-.;n t!-.e ou'.5:c:e
or around the filler.
5.1.C Filter l:r.i:inj yvslem — \V;ic:i .-.••:.:.;-
lure condensation is n proWcrn. any lic.\:::<~
sysiein capable of :v.nintnlr.!ii;: a ie.'i'.pprv. ::ro
around the filler lif'.rtcr duri;;:: .e.ir.jpiip.r c'
no {rrcalcr than irf)±M°C (243iC5'Fl. A
temnrr.xtuve pAnjre c,;pahlc of n:or-uri!i£ tT;:-
pcra'.ure to within 3"C (f'.-l'F* r-hall he ir.-
Btallcd so that when the filter hp.v.cr if i:f.'-(l.
the temporal UIT .irounrt the SHtr holder can
he rcpulated and mr-r.ito-cd chiri::j: sarrpl:":-
Hcatins systems other ;lu;i the one slioxvn
in APTO-P58! may be tiFed.
5.1.7 Iiv.pin^-crs — Four Imr.-irrrrs co::-
n.'
to
•( — 5*F). f'ry gns r.ieter v.'ith 2 pcrccri4. r. •-
curacy a", the rccuirf.i sampl.r.;; rr.'.e. ar.rl
related equipment, sr c:;uivalc!;t. or- rco.'.'.:rt*l
to mair.'.air. an lco'i-.:p.et:c Ewr. ;:-'.> up: ri'.e rr.cl
to rietermii'.o sample volume. When fhe
metering system i." u.U'd in cnnjunction wil'i
a pitot ti'.ifi. the r.ys'.','m shall t:ia'jle chec'r.?
of isoklnetic rales.
0.1.9 Barometer — Mi'rctsrv. n'.'iCroiu. < :•
other b.iro.'iieters cr>pa!)l'.' of measii!1::.-:; a:-
mosphcrlc pretsuve to within 2.5 mm J--; (0.1
in Hi;). In m:Lny cr.^es, the t.irorr.t-tric reac;-
iii£ may be obtained from a ncr.roy weather
bureau S'.aucn. in which, car-? ti:e rt2!:o:i
value sha:: i;e :-cn:icK'.ed and a:', adjits.: :i:'.-:: •.
for olevtitiou {lifl'erer.css shali be ritiplioti at n
rate of mir.M.i 2.D ir.jv. Hg |i)-l !"•- 1:21 ;•'•" -•'
m (100 I1.) elevation Increace.
52 San-.pie recovery.
O.'J.l rro'os Inu-i" ni'.cJ p'.obe •.::-.•:..
brushes— Njian bristle.1; \viili ct:.::-:lC5s r'.vil
wire )i.Ti;ti;c.-. The pro!)e brucli sh--.:i l::i'v
cxtf'p.3io:i.". ct- Icoit n.> lo:"-2 as i:.e proV-c. c-^'
Kt:xiiiif:r;s r.:eo!. TC:'.'J:'.. or Eim'.!.\rly ij-.rr: ::.:.••.••
rial. Both brt:shfs JhaSl be propcr'.y si.:c-i :>n:i
?):ap»tl to bv.sli oi;'. the pro!:c lir'.c-:' r^'.j :-.."••/-
f: ?.." Ci: -.'.•. •
O'. tiOE — TV. O
o:iini.icr;. o. .-?:•.;-.. I'M-:':'. volu:*.:v to j'.'r-rc :/::r.
.S •_' f. Gra.!"..;:'.-ci cy'.'-.-.cv-r— LJ; ::.'.
6.2 u l'i;:'.:'.i-: :\:-.u rubber ji:.'.:.-e:i::>:: — '1 «
;:vl ;;: tra...-:\.- tC -r::;c;* (;ci 10 fC'It'.-;;'.'.'. ..... '.
o\v..-;ivy L'. i.;..\t •-(.'. :.-. v.'t i.;i'iC« 1:'. t'-.t- : .-..i
ftl
-------
STATIC\'A.';V SOURCES
rCi-37
5.3.1 J".': -•!•:.-.•!-.:•. r.ppara'.u? — Glara •ab!c cf heating to
furnace— Cr-.pabic of
l-i'-atljis TO OOO'C.
fi.J-T Cr-.:c".-.:<":-— Nirkc!, 75 to 100 rr.l
capacity.
:i.r?5 ' n-:ai:cr— loOn rr,I.
5.3.5 Volumetric flask — f.O ml.
6.3.7 Erienmevcr flask or plastic bottle —
500 ml.
5.3.8 Constant temperature bath — Cap-
able of ir..-.::;;.iinl:j;r n con.nant temperature
of il.O'C in the range of room temperature.
5.3.0 Trip l:a!ance — 300 g capacity to
incnMire to iO.S p.
5.3.10 Fluoride ten activity sensing c'.cc-
trcflc.
5.3.11 reference electrode — Sinple jur.c-
tlon: sleeve type. (A corr.bination-t-ypc eiec-
troclo having the references electrode and
the fluoride-ion sensing electrode built into
one unit may also be used).
5.3.12 Electrometer — A pH meter wl'.h
millivolt SiMlc capable cT ±0.1 rnv resolu-
tion. or .1 specific ion ;r.c;er made specifically
for specif;? !on use.
5.3.13 Magnetic stirrer and TFE fluoro-
c.-.rbon crated stripping barf.
G. ncapCTiif.
6.1 Sampling.
G.I.I Filters — Whatman N'o. 1 filters, or
covjlvalcr,;. sk'.cd to fit Slier holder.
"c.1.2 Silica get— Indicating type. C-16
mesh. If previously xiscd, dry at I75'C
(350.'."i-r::4i!i o: the .A'.'n::n-
:.:T:.'.-. r ll-.at- t'rc .•..-.i-.-.ric; co:-.n::i p::ly \va'«..--
7.1 Ca:np:!nr;. Tlic jr.n:pl:ri;r '.hi'-'.l ci-C'^r-
du.-.tt first be obtained.
7.;3 Preparation of collection train. Dur-
ing preparation and astc-mbly ol the sampling
train, beep all cpcv.iiiRS where contamination
cr.ii occur cf.-vciod until Ju.u prior i<>a£!:e:r)!;!y
or until sampling is about to begin.
Place 10U ml of water in each of the first
tv.o impingers, iea\c the third impinuer
empty, and place approximately 2CO-COO p. or
more, if necessary, of prcweighed silica pel in
t.he fourth impinjer. Record the weight of
tV.o Mlica KC-! :.'.-.(.-. c.',:y.ii;nrr <•..". tho r;..'.:, sr.t-. t.
P;.ire thf empty container in u cifan pliwc
lor later use ir. t!:e s:.:i:>.le rtcovc-ry.
Place a filter 1:1 the liltcr holuer. DC sure
t!:a'. the iil'.or >•: prt.per^y ccr.'.'.vc'J r.tul tr.e
[:.i::':'.(.'t pr.'^por-y iTliuV^ so as *.o ::w' :i'lovv the
sample ga-j stream to cirf.imvcni '.lie niter.
C':::'Ci: '.V.tc-r '.LT •.;•:." alter :-;;i';;,i.-:y u ccn>
Ijji-.-rs -re ur-ed. irisi.'i!; selected
'• V;tni: A O-.';n;.: t!:« Vito:. A
:..l':i".i :-.'• :. :'.:•! \\'. .<-•:•: \.\:r :: •i:.:.'.i;
i> cT:''1-"''.I '•"> .t ,"l'--"~ '!:'': FT .•.p~n-ry:.-
.for detail'. V.'lirr. :r.c"r.l ',.:.<•:•- r,r" ::-<--.•!. i:-,.
ntal! tl-.c r.'..".-:-* r..= a-" •.:•<•• or >-y :, >?.:•-. frro
with hop.', rc'-is'.aiit' t'l-.r-.r nr by r-'-:-.-.o r,!.:-.T
:not.jif>ri t=-> ',-"ic'.c V.'fn* jiT-r-'-r •-•:•<. :n! t':',r v-:-'-.'-.r : ,;-. a:.!!
dcc^; not touch any ••.•.." \:-.'. !•.•• fiMT. •.I'.o'.ilJ
be r^hr.\i! IF to-2?t c~.i 10.7.=- if 1 '.:':. 1 frr?n
tlic pltot tube antf iir«rb«: r.or.r.:'- '.o r.vcid In-
terference- with tho p^is f?n\v.
A..-i!.!j tive f.'.lrr I'fV.vccn
ihc third r-.nd fou.rKh '.mpinrrrs. Alterna-
tively, the f.ltcr i:'.ay Sjr plui-r;! i-.rf.vcer. t;-.o
probe and' first. I mpi :.:.;•>' r. \ filter I'cati:1: r.;. r-
lem may br u.ned to prevent :i:r:«t:ir(- >:c::-
dPr.Rai'.o-.i. b;;t the teznpnrMurc arr>-.iijc! \'r.t
filler he-Icier shall EJT>: exceed JJWiJ-iS'O
(248r:-S F). |(N"otc-r v.'hatman Xo I~'filtrr
decomposes nt 350-C (300F)).| record
filter location nn the <25>.a fhc-et.
Place crushed ice. strounrt the impir.fers.
7.1.4 Leak check -.procedure — After 'tho
;.-.mp!inf: train lias, rjrwji ar^crrb.'ed. turr. o;i
and set (if applies*!*!! t!-.e probe and f.ltcr
heating system(s) t«» re.-.eh o tcm^ernturo
sufficient to avoid corarScnsp i ion in tlic probe.
Allow time for the teaiircr.iUirc to stabill.-e.
Leak check the train* aa the sampling s;te by
plugciug the no".;e. a;nd pui;i.n{r a 3X0 r.i:ri
HR (15 Ir.. Hgv vacvussn. A leaknre rate in ex-
cess of 4rc of the miTracc naniniirr: :-,-.:e of
0.0057 mV'ir.in. (0.02; zim I, whichever is If',
Is unacceptable.
The following leak arhf.-'.: Instrii'-tior. fr-.r
tho ramplme train dira'-ribed !n AV'TD-fi'-TO
and APTD-C581 mrsjr 3jc j:o!pf-.i:. £:.".rt •,:;•>
pump with by-pass waive fu'.'.y <.pcn arrt
coarsu adiur-t valve crainp'.ptely clcroJ. Pr.r-
tiaily open the coarse adjust valvp av.tl jlo-'-
ly close the by-pas-,, v^al'-c u-.n'.l SSO mm Ivj
(15 In. l!gl vacuuni. i; reached. I'm .Vr,; r---
verse direction of VjcHpass valve. ^T.'.E v.-i'.i
cause water to back; ura into the filter l-.o'.ic-r.
K 3EO mm Kr; (15 l:s..23cl is cxccc^c-d. either
leak check at this hr£.5jcr vicuum cr cv.ti tNv
leak check as dcrcririeil fcc'.cv; nr.rt c::'.7t over.
V,T.c:i tile ieak oierk ir. cor.-.p!c-'.ec, f.r^i
tlov.-ly remove the ptes; l.-orr. the in'.ct to ti-.e
probe cr filter hciMtrand i.'i-.nicciir.'.t:'' turn
off the vacuum purnj:. Tliis prevcr.ts t::a
water i:i the impin«??rs from bcir.ft fcn-ccd
backward, into, the; Alter liclaer
-------
FEDERAL REGULATIONS
• i-..r.i- .:-:I:!:r::.-.-. r.Ojurtnor.ts in Sow rate. 3c
vi — to level and ^CTO the tr.anonietor.
C'Titi the porthole; prior to the test run
to .inr.iimi-.-e- chr.ncc c! sampling deposited
::i.v,cr!al. To bcp'.rt sampling, remove the
:-. !j toinnrr.v.urft. ry.irl that, the pilot tube
v.::l probe arc properly posit i-.-ncd. Position
;lic nn-/ie r.: the f:r.-l traverse point with
the* ti;> pointin- directly into the cas stream.
Immediately start the pump and adjust the
:;••>«• to !;okinctic conditions. Komcpraphs are
r-.vailablc for sampling trains using type S
pilot tubes with 0.85^0.02 (coefficients (C-).
.V.K! \vhc-n r:i;r.;Sinc in air or a slack pas with
equivalent density (molecular weight. M.,.
r>;'.ial to C'.'n-1'i. which aid in the rapid ad-
K-.itment of the isc.'.;i:irtic ran-.pliup rate
v:;:hov.t c:le run. except for filter and silica gel
cS\:ir.ge3. Kr.vcver, if approved by the Admm-
r.irc.ior, V.vo or more tiiiins may be used for
a single test run when there ore two or more
tix'.cts or sarr.phn£ ports. The final emission
rfsulti iUr.ll be based on the total of all
.sampling tram catches.
At the end of the sample run, turn oft the
li;i:r.p, reui'vc the- pre-be and ncsrifi from
;;:c i.'..ic:-:. ur.Q r'.-corci ;he final dry gas meter
rcidins- ronorm a leak check.1 Cn'.culavc
perccut ii-okip-eisc (see calculation section) to
(ivUTmir.-j •.'.•:.sihcr a!.o;l;cr test ruii th.ould
'..»! iv.^'.ie. I: thc'.e is Ui!'.-.cii.:y i:i n-.:;-.:;ta:uin™
i.'.oium'.ic ruie-i due to source conditicns, con-
.'.uli. v/i;h tiie Administrator lor possible
\.."••..:!.ce L.:; '.h. .:-;•,• li:r.ci;c rates.
' \vif.i r.-rc-::..':l!'.tv t-f the teit mn to be
7.2 Sample recovery, rror-cr cleanup pro-
cedure, begins ar, s-nn a", the probe is r^-
movcd from the stack at the end of the
sampling period.
When tho proHe can be rafcly handlcil.
wipe off all extern.-1.1. part:culate matter near
the. tip or the probe iv.vzlc an:l pir.rr a r:::i
ovi-r it to keep from i^ri-.-.r r"l of the sam-
ple. Do not cap oft the probe tip t!;;:Uij
while in? sampling train is conh^g down.
as this would create a vacuum in the filicr
holder, thus drawing water from the im-
pin^cr.s into the li'.ter.
Before moving the sample train to the
cleanup site, remove the probe from the
sample -train, wipe off the siliconc prca::?.
and cap tho open outlet of the probe. EC
careful not to lore any conclci'.sate, it pres-
ent. Wipe off the slllcone ftrcase from the
filler inlet where the probe was fastened
nud cap it. Remove the uvr.bil'.ta! cord from
tho last impinrcr and cap the implr.f.c.-. After
wiping ort the silicon" grease, cap ofT the
filter holder outlet and impingcr inlet.
Ground glass stoppers, plastic cans, or serum
caps may be us:d to clos.- these cpenir.ps.
Transfer the probe and filtcr-impingcr as-
sembly to the cleanup p.rca. This area should
be clean and prelected from the wind no that
the chances of contami-.-.aline or losing tho
sample will be minimized.
Inspect the traiu prior to nnd during dis-
assembly and note any abnormal conditions.
Using a graduated cylinder, measure and re-
cord the volume of the water in the first
three impinpcrs, to the nearest inl; any r.on-
dens.atc in the probe should be included In
this determination. Treat the samples a?
follows:
No. 71778. Pauley. J. E.. 8-5-75
7.2.1 Container No. 1. Transfer the ir.i-
plnger water from the graduated cylinder
to this container. Add the filter to this
container. Wash all sample exposed sur-
faces, including the probe tip, probe, first
three irapingers, Impinjcr connectors, filter
holder, and graduated cylinder thoroughly
wit.li Uisl:ilea water. Wash each component
three iepir.-.t-? times with water and clean
the prorte und nozzle with brushes. A rr.ax-
i:r._ru wash of £.03 ml is used, ar.d the wash-
ings arc added to the sample container
which must, be murte of polyethylene.
7.2.2 Container No. 2. Transfer the silica
gel from the fourth impingcr to tills con-
tainer and seal.
7.3 Analysis. Treat the contents of each
sample container as described below.
7.3.1 Container No. 1.
7.3.1.1 filler this container's contents, in-
clutliny the Whitman No 1 tiller, through
Whatman No. 041 filler paper, or cc;uivc.lent
into a 1500 ml bc;-.!:er. NOT:: II fillriV.c vol-
ume exceeds 000 r.-.l rr.a!:e Jillrntt- br.;ic with
NaOH to phenolphthalem and evaporate to
less than 000 ml.
7.3.1.2 Place the Whatman No. 5-!l filler
containing the insoluble matter (Including
vhc Whatman No. 1 filter) lr. a nickel cru-
cible, add a- le-.v ;:il of water a'.id macerate
the filter wu-h a slasr, rau.
Add 100 nig C'aO to the crucible and mix
the cor.ter.ts thcroughly to form a slurry. Add
a couple o? drops o.' plieiiolphthuieiri indi-
cator. The Indicator will turn red in a bac:-:
jr-.idlviin. T"n!> slurry .should remain, basic
dr.rmjj ilia cvavo:'itinn o: the v::'.tcr cr
fli'.cri'.Jo ion v.'il! be lv--. II the i::rii-..tr-r
turns co'.or!e5;3 curir.g the evaporation, an
acidic condition U lr.dic.v.ci. If this happens
add CaO u:iv:i th-.; color tur::::. red ;:^:>::;.
I'lacc Ui'j cruc.blc In a 1:C^1 unct;: In-
frared l.\rnpj or on a hot pi;ue ;.'. low ht.it.
Mo*ij l::trca:e the ;<-rr>j/cr:-'.u:c cn'.il t'.c
paper ehirr.. It may t:i'/.c srvcr.'ii Ixv.'.rs for
com;>'.e'.':i.::') in-vv
t:«.c lcni!i"r:i'ii!p tn r-.":?*C. and m?::i:n:n un'.::
the content:, are rcih'.cc'l to t:i a:-.h. T<-".r.:--:a
the cr\:,-.!blc Irom '.he frrr.are a:"'j .V.!-r>v» it t:i
roM.
7.3.1.3 AJil spprovira.itcij 4 p of crvv.'.'.e.'l
N:-.OH to the rniciliie nnd mi;:. P.cturu t'.'.r
crucible to the nuifii? Jurnacc. ar.U fuse the
sample for 10 mUiutr.% al ROO'C.
r.cniove th.e sr'mpVc from >he lurnnre r.::d
cool t-o aaibicjit 1r::ipcra!ure. Usi:i:: f.:\crAi
rinsings of warm d;Jtillcd vatcr trnr^fcr
the contents c-f the crucible to the l-.rnker
contamini; the fii:r:»l< from cc:ilai"-:r No.
1 (7.3.1). To nw.ire oomplcic sample re-
moval, rinse finally \villi two 20 ml r-orniT.r.
of 2r> perecni. (v.-'v) s-..ilfurlc a.-.:J and circ-
fully iu.ld to the bcakrr. Mix well and trans-
fer to a one-liter volumetric flail:. Dilute
to volume with dii'.mcd water and mix
thoroughly. Allow nr>y u:idissolvcd solids t-o
sct.tle.
7.32 Container No. 2. \Vo!i.i» tV.c .-.pent.
rilic.i jcl and report to tho nearest 0.0 ?..
7.3.3 Adju.itr.icnt ol iv.'.i:!.'wv.fr rr.tio in
clLstillst'on f.ask.—(U'.SliTC 3 proter.tjvc shield
when carryiii; out t&tsprrK-cdurt). P'.ace 400
ml of distilled wa'.er in Die d:;.till!n;t f.as'*
and r.dd 200 n-J of c^'-icc-itrnleti H *O.. C.-.\^-
tion: Observe Ptan'JaTtl precautions wl-.en
rr.ixir:g the H SO, hT slowly ndd'.-.ip the i,-;iJ
to i.hc fl.\sl; with co:>;tar.t swirl::ic. A,'I:! snir.o
soft glass brads and. srvcral sr.ijil pieces of
broken plass tubir.j, and nr."cr.;hlr the ap-
paratus ns shown in Figure 13A-2. Heat, the
fl.islc until it. reirhes a temperarure of IVO'C
to adjust the r.cidV'vUcr ratio :or subso'^usiit
distillations. Disraru Uic eliminate.
7.3.4 Distillation—Cool the conicv.f. o:
tho distilla'.ion fiast to below BO'C. Pipette
art aliquot oi" • sairn-,jl» costaininrt le.%^
than 0.6 rr.r: F cisrecily into i!:e r. i it :U •.:-.;•.
fUisk c.rid add distii'raS •Witcr tc iv.rikc a total
volume of 220 nU added to the d;rv.i':i:-.u
nusk. ITor r.n crt;n-.:ite cl wh;.t .-•;:•-• ;'.:•.•.•.;?•.
does lic-t exceed O.li dj; F, select. a!i ?.;:^ua'-
of the julution aui treat r« ie'.M-riiivd i:\
Section 7.3.6. This vrjll c've fn approxium-
!k.-n of tho iiuorlrte cantcnt. Uti; o."'.y o-i «ip-
proximal ion since ialerfcring ions I'.^XL- T,~J'-
been removed by thedistillatic.D step.)
Piac: a 2io ml volumetric flask, r.: the con-
tler.ser cxb>t. No;* begin distillation nnd
L'.ra'.tually ir.cicasctrjjc jjcat-and colloct all li.-e
OistillMf up to I75-C. Caution: Hc-r.tlnc t^i-
solution abox'o 175'Cvrill cr-USc sul.'itr;. aciii
to distill over.
The p.c;d in the cH.uU!iug f.:.s'.; can be
used until ti-.cre a carryover c: iiiivncrciicc;
or pci'.'.r !iuori'Jc r-vruvcry. An cc j.'t.M'-.'iil
check ol iluor.clt recovery vni: ii:-.:'iS::ril
solutions is auvi£sd. The acid should
bo chunked v.'liej'.cvcr tlu're ;-: li':-3 t;-.;.r. C-J
perceiit, recovery or blank vsiuis arc hirhcr
than 0.1 uc'inl.
7.3.1 L'vUTiMinr.ri.ciu t.t:ui ion—
IJrin;; thi' il!.',:li::..',e ::i x.'-.c CiO :-.; v-:.::r.i'i-;c
J'.ar'i 10 Hit marl:, TO:'! ciislii'.Cu '.vu'.v:' t::d
iv.ix thoi'Oi'i'.hl.v. Pl.piltC u "J") r..! ::::<|\:o'. fri;i«
'lie* cu.^tiliu'.r Add :^a enual \cluii.i o:' 'i Z'iAIi
r.nd r::x. The r:irj};]e sii-iulu be a: the
siur.o tc:i:i:err:t«rij KS llic <:ul.l':-it.:o:; t:a:.r.-
urd.> «l:i:i lhv;i'.r:eiiH':r.:. ^re r.i.T.1;.1. 1'
.v.u.i. t lit- I:.!) t!.:u:-i?r^;;irc: :'. ..•.'.;-.. tc-i i;:":
the c.-1.li:jr.v.!o.i FV.isilarcs v/cvc ;:.•.-. i-'.:rcil,
co!:u:ti".r. s.i:nr.!ej ra:ud star.rl.'.r'.!'. ri a cf%;t-
^tu.".'.. i-.':i'"c:':i'.v.rc l-:...tii ]:i'.:.'.'.:r^:'-'ir:.'- :.'.tr
the r.:inir.'... v.v.r. a. ir.^r.rc'.:: tt:r:i.-r u.••.;.";•
i.-.r.i :•::•.•.:...•:.; '.-• '.•..••..in'-.-": c'.' :tn;cte rc"',':;.:c
Enviionmcnl
A:
-------
STATIONARY SOURCES
12 IS: 044 5
TEMPERAH'RE
.
LX PROBE
1.9cm (0.75
PITOTTUBE ' OPTIONAL
S FILTER HOLDER
V/[ STACK WALL L _LOCATION
THERMOMETER
PROBE
/
fe
W
/
REVERSE-TYPE
PITOTTUBE
V
PITOTMAKOMETtP.
ORIFICE MANOMETER
•i AIRTIGHT
PUMP
r:i,.-!» 13^-1. F Itt
CONKECTIKSTUBE
tl-om 10
f 24 40 V;
THERMOMETER TIP MUST EXTEHD BELOW
THE LIQUID LEVEL
V,1TH J 10/30
HEATING
MANTLE
CONDENSER
250ml
VOLUMETRIC
FLASK
Figure 13A-2. Fluoride Distillation Apparatus
1-14-77
Copyright © 1977 by The Bureau of National Affairs, Inc.
[Appendix A]
57
-------
STATIONARY SOURCES
tlr.'-.r. If t'.-.o ?;i.-;'C.- r;c:-.cr.?tcs csx-nch heat to
ch.inr-e sr/.ut k'li ;cmperaturc, place a. piece
rf ir.^-.'.lntinc; material such as ccrk
brtv.Tcn tho Ftirrer r.nd the beaker. Dili;!e
r.-.rr.p'.es ibcl.vv 10 « I-.! Huorlcle irn content)
:.:'.'!<:M be held in polyethylene or po'.y-
pvpyie^e bra'.icr- iluiin:- mr.rA'.ire:nciit.
!r.:.-rt the fiupridc rod reference, electrodes
ln:o •,::•.' roh:;:."-.. V.'hcn a itca'Jy millivolt
rTi-.l;::- ;'.-. r>!)t-'.;i"d. rec-rd It. This niny take
srvpia: minute.-. Determine concentration
frcm the callbratinn curve. Between clcc-
tr.y:ie •r.cr.'.iii'Ciy.cnts. roa/i tho fluoride .cer,s-
inp electrode, in distilled water for 30 seconds
and ihcn remove and blot dry.
Maintain a laboratory log of all
0.1 Snmplir.n Train.
3.1.1 Probe r.or.;le—LVir.p a micromotor,
rr.o.v.ire the ii>:-ide diameter of tho nozr.lc
to the nearest 0.025 mm (0.001 in.). Make
3 separate nior.surcnicnts «s;:sf; different
diameters each time and obtain the avcranc
of the measurements. The difference between
the hirh and lo'.v numbers shall not exceed
0.1 -.-.m iC.OOJ in.).
V.'hcu iior.:!es be-ccme nicked, dented, cr
corroded, they .'-ball be rcr-hnped. sharpened,
.ir.d recalibrated hc-fcrc use.
Each no.-.-:le fhall be permanently and
uniquely identified.
8.1.2 Pltot tube—Ti-.c pilot tube shall be
calibrr.tca according to the procedure out-
lined in Method 2.
G.1.3 Dry r.is n-.cter and orifice meter.
Both meters shall be calibrated according to
• the procedure outlined in APTD-Q576. When
ciisphretrm pumps with by-pass valves ore
used, chock for proper mcterine; system
deslrm by calibrating the dry pas meter at an
tdcHticnil flo\v rate of 0.0057 mVmln. (0.2
cfni) wi;h the by-paw? valve fully opened
end then with it fully closed. If there is
more th?.n ^2 percent difference in flow
rates when compared to the fully closed posi-
tion of the by-pass valve, the system is not
designed properly and must be corrected.
£.1.4 Probe heater cr.:ibration—The probe
5sta;::ir: system shai", be calibrated according
to the procedure contained In APTD-057G.
Probes constructed accordiRj: to APTD-0581
need cot be calibrated If the calibration
curves Ir. APTD-C57C &re UiC-J.
8.1.0 Tenipcra'-urc gauges—Calibrate dial
mid liquid filled bulb thermometers p.gclirjt
mercury-ia-glass thermomc'.erc. Tbcrrr,o-
couples nc-e by serial dilution of
tue 0.1 ?.t :':uoride standard solution. Pipet
10 tnl of 0.1 M KaF in'.o a 100 ml volumetric
fias'.i ar-.d make up to the marl: with distilled
water for a 10--' M standard solution. Use 10
rr.l of 1U': M ioi-.:i:on to mr.'ie ?. l(j-J M solu-
tion la the same manner, ncapt 10-' and 10-'
r;?6-t CO ml of each standard into a scp-
nr?.tc bealrcr. Acid 50 ml of T1SAB to each
beaker. Place the electrode in the rr.cst dilute
standard eolut;cr.. When n steady millivolt
rcidi.'ij 15 obtamc-.'i, filot. the vr.Uic or, the-
linear p.x:s of semi-leg graph paper versus
concc;itrntio:i or. the log !i:<:s. Plot live
;;:::r:i".'-.! va'nc tor co::c;-:'.'.ratH',:i of the
s'.:.:!C.vj on tl.c- lc^ a:-;::, e.;;., \vi:e:i 50 rii! c:
10-: M siMiflai'd is diix:;o:: v.-jtli DO nil T1SAD,
tlic cor'.centr.v.icn ij s'.:!l dc-Hijiuv.cd "10" M".
:.'-:^.:-.':: c'.i'C'.rcce in d:s:ilio-.l water .'or 20
seco".:;S. r.nd thc-u remove n::d blot dry.
A::ai;'."c tr.o !.!'i!i'.:ard.: £•:.::£ lr...;i, d:!uti; to
br..1.:-.-:: curve >.'::! be i.b::::.';C'J, v.:th ron.i'.-.ul
c-,::•'.•:.tr-.-.-.loi.- (•'• '•'•'•'•• K'f". It1-", K.'r. 10'1
.- .Li-. •.•:•.•.-.••:... .-' '.'-'•'. 10'. l'i- , V.i-'-. 10'1
vrrr.«:s olcctrc-Oc p.vtentlal (In nv,ll:vc'.t = l on
the lir.rnr scale.
C.-.Mbratc ll'ie fluoride' Plectra!" daily, n'.vl
check It hrniriy. Pr»-pnrc frcit calculation.';, retaining at le.v-t
one oxtra clcciii-.al fipure b"yor.d 4>:i:>.t cf the
acrjuired data. Round of! finirrs after final
calculation.
P.l NonienrSature.
.1-. = Cross rectionnl area of nor.rlc. r.i? ift.').
^•li— .Aliquot of total scjiiplc nddcd to still,
ml.
C^-. — Water vapor in tl-c gas strcr.ni, propor-
tion t>y volume.
C. = Concentration o' fluoride In stack pas,
mc-'ni1, corrected to standard conditions
of 20' C. Ton mm Jig (CO' F, 2D.D2 in. lig)
on dry basis.
Fi = Total weight of fluoride In sample, mg.
; = Perccnt of Isokinetic. samplinr;.
.",r = Coiicentration of fluoride from calibra-
tion curve, molarity.
?n» = Total amount of particiilate matter
collected, mg.
,',;» =Molccular weight of water. 18 g-'g-mole
(18 Ib/lb-molc).
nio = Mass of residue of ncetonc after evap-
oration, rr.g.
Pb»t = Barometric pressure at the sampling
site, mm Hg (In. He).
Pi = Absolute stack pas pressure, mm HG (In.
Kg). '
P. tj=: Standard r.bsolute ' pressure. 760 mm
Hg (29.92 in. Hg).
R — Ideal gas constant, 0.0023G mm Hg-m5/
"K-p.-molc (21.83 in. Hg-ftV'R-lb-ciole) .
Tm ^Absolute average dr>' g.ij meter tem-
perature Cec f.g. J3A-3). 'K ('R).
TI-- Absolut? average stack gas temperature
(see fig- !3A-3i.~'K CR).
Ti..i = .Standard absolute temperature. 203*
K (528' P.).
V« — Volume of acetone blank, ml.
V'«v = Volume of acetone used In wash, ml.
Vj — Volume of distillate collected, ml.
V'i« = Total volume of liquid collected In Lm-
plnrjcrs and silica gel, ml. Volume of water
in silica eel equals silica gel weight In-
crease in crnnis times 1 ml/gram. Volume
of liquid collected In lmp!nr;CT equals final
volume minus initial volume.
Vr, = Volume of gas sample as measured by
dry (;as meter, dcui (dcf).
Vt» <.:.])=: Volume of gas sample measured by
the dry gas meicr corrected to £tr_ndard
conditions, dscin (dscf).
Vvnid)=: Volume of water vapor In the gas
cample corrected to standard ccnditicns,
Bern (Ecf).
Vi = To'.al volume of sample, r.il.
ri = St.ii:)i [',\j veiocity. r.tlculiiti'U by Mc'.liO'J
:!, Kc;;i:'.'.:.';n -••'• '-;::•.!; dn:a obtained lru;;i
^!rthcKl 5. r'.TC-c (ft/sec).
Vv'o^v.'oijlit (.' residue in acetone waili, mg.
_\ll ~Av(-r:igfc pi'csiiuro difierentlal iicrois thu
f.rilii-i.1 i'.'.--e ;:j. l:'A-3i, meter, runs J:.O
iin. 11. O|.
/
r.nd r.vc-r.-.^:-? orifice r''''"-'^-'f drcp. .S--r ai\?.
f-\-rr: ti'-.-.v.r" 1HA-C of :.%-'h~! 1.7 -M .
P3 O:v (:.-- vo5t:-i:r. V'-'- 5f.T.: !•%:; 0.? r.'
:.>:;io-.l i."..\.
:• i Vr.:-.:--:'- f : V.':.'T V.-por. U:r .?,•'::..:!•.
n 4 f--:' :.;i-t::,--J :r:.\.
f "i ;.'!.: = • '.ir'- f'cT.^T.: I'T f---'i"r: f- " r'.
Mi :•.-•<) ij.\
f' *•• Or:oT.tr.i!i'c:i
I' G 1 Calculate1 5.?ic r.n-..-;:"f c-.' "'.:Ar:-.:e i:i
the .-ample sccortlinp to cnu.i!ic:i T.''I3-1.
where:
K.-1;: ni7T.i!.
f.C.2 C^'-i-'i'in-aSiJon of finc-rlrir ir. •-•:.';••'•:
pr?. Vre Sv'tior: P.^.2 ol Mr:'::r,-: l.'A.
f 7 JrK-:i:".rtir. varlatiou. r.ce Src\lo:; P7
of Me; heel I3'A..
P.S Acceptable1 rr?ult.=. U:.e Soctl.'.r. O.f. c-T
Method 13 A.
10. Kctrrtn.-ft.
JJcViac'i:. Zrvin.. •1SiiT>.-,)'',if'.rd F'.r.rr'sd'- !>'.''.'.'.-
latlon Method. " Journal ot thr Anr'iccn
Water \\-n-kf A.'rectetir-r. =00; 5ri;l-G OP.vn.
JTacLPOf!. Kathrjrs F... nr.d I!r"var,-| I.. Crir-:.
"Comparisn:'. cf' t:!he .SPADN'f7 — rir-'^'inu: )
Lake and Specific ton Electrode Mot ^Of'.* cf
Fluoride Determ.insalion In Sta^: r.mi^-i'f.
P.implcs." ^nsj.vfiV;c3C.!icr::r/n/ 45: )2T2-:27j
(1P7.1V.
Martin, Robert "tfConstrucUon Details c'
Ir-okisietic FciuririP P.i::ipl;:V-- nr.-.iinmer. '-."
F.nvironmenta! Pncr!ectlon Ar.-cncy. Air T'-'.-
lut.ion Control O:»«E miblic.ition Nc- APTD-
0581.
It73 Jnn-js: noofrof /Sr.V 5:c?i".!r.::
Equipmcr.t." Env3tronnirr.t:-.I rr-'.'.v. i'.::
Agency. Air Polhiltocn Control OIT;cc PuVi'.ira-
tion No. APTD-CK61
Sfcnrfi:rv.-:i
into a permanen.i Effi-'tnplir.r; manifold through
several large nccrV'tts. The iMTiplc i» tr;..-,-.-
portcd from the 5.a:r^jlu:g ni^ni:o!c to f round
level through a d'Uttit. ""lie gas 1:1 the our; is
sampled uslr.a J.tc-sRsnd ?.3A or :TtJ — I5=:';«:r;-
MINATiON OP TOfTAL l-'L'JC:»:TJi; !.:>:::;-
S1ONS FROM STA1T3ONAIJV iiOUJtCC^' F.f-
(luent velocr.y andi Tolunietric :ljV rv.c .".re
deterrmnca wltlii nc;c:v.'.:r:;i.':irs piTHMii.v:.".;';.
located in the roo!'Euomtor.
1 2 >.p;>.'icc!>i!n^. "Jh'.s. rr.c'.hcu •-•; r.:-)>'. ?-•
blc for the cricr'.-.irj.iiion of ii.ic. .•:.:•-• r::;: --
M'jjts 'ro:i. ?'._'..'.:r.i.T.' t-..'jr •;..••: i..:.:;. v,;.-. ..
:.-;;cc;::ed br tiie U'~.t proccJutv.-. f;:r c."r.--
mining compliance- :;i'.it i:0\v sj;;rcc j:tr:or::. -
anre r'.ancari;.
2.1.1 Ar.or.omc'.cns.
tinrrr.ometcr.s v.itl^ ii v.'-'.
!i:rv*i;c;d -Z !cv,' n, ;.'. r .1 '.•.•:
.r:inKC up to it ltr-ii 6;i.M r.'ic'.'.
.'.->r.e t.r pr..ri:-':cr
y :: vr-.iiir1.". *
-.'.:. ..... — : ..
c-.i.-.-'.c. E;n:r.
.:'. ;:y *.-: irC'rcur
to percent.
-------
DETERMINATION OF HYDROGEN CHLORIDE AND CHLORINE
-------
DETERMINATION OF HTDROGEN CHLORIDE AND CHLORINE IN STACK GAS
C. E. Decker
and
C. B. Kagar
U.S. DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE
Public Health Service
Rireau of Disease Prevention and Environmental Control
National Center for Air Pollution Control
Cincinnati, Ohio
April, 1968
-------
DETERMINATION OF HYDROGEN CHDDRIDE AND CHLORINE IN STACK GAS
INTRODUCTION
This method is intended for the determination of hydrogen
chloride and chlorine in stack gases, as would be encountered in
emissions from hydrochloric acid manufacture. Hydrogen chloride
is collected from the gas stream in midget _in
-------
Absorbing Reagent " ~ "
A. Sodium hydroxide (1 N) - Dissolve hO g of sodium hydroxide
• in water and dilute to 1 liter. Use this reagent when the
stack gas concentration of HC1 is less than 1000 ppm.
B. Sodium hydroxide (2.5 N) - Dissolve 100 g of sodium hydroxide
in water and dilute to 1 liter. Use this reagent when the
stack gas concentration of HC1 is greater than 1000 ppm.
C. Alkaline arsenite (l N NaOH - 0.1 N NaAsO-) - Dissolve
lO g cf NaOH and 6.5 g of sodium arsenite (NaAsO-) in
water and dilute to 1 liter in a volumetric flask. Use
this reagent when the stack gas concentration of HC1 and
Cl- is less than 1000 ppm.
D. Alkaline arsenite (2.5 N NaOH - 0.5 N NaAs02> - Dissolve
100 g of NaOH and 32.5 g of KaAsOg in water, and dilute to
1 liter in a volumetric flask. Use this reagent when the
stack gas concentration of HC1 and Cl? is greater than 1000
ppm.
Ferric Indicator
Dissolve 28.0 g of ferric ammonium sulfate [FeNH, (SO, )2'12 HgOj
in 70 ral of hot water. Cool, filter, add 10 ml of concentrated
nitric acid (HNQ ), and dilute to 100 ml in a volumetric flask.
Nitric Acid (8 N)
Prepare NOX free nitric acid by adding 100 ml of HND- to 100 ml
- 2 -
-------
of water and boiling in a conical flask'until the solution is color-
less. Storo in a glass reagent bottle.
Nitrobenzene
Reagent grade.
Sodium Chloride (Primary Standards)
A. KaCl (0.1 N) - Dissolve £.8ii6 g of dried sodium chloride
(KaCl) in vater and dilute to 1 liter in a volumetric
flask.
B. NaCl (0,01 N) - Dissolve 0.58146 g of dried Nad in water
and dilute to 1 liter in a volumetric flask, or dilute
100 ml of 0.1 N NaCl to 1 liter.
AnEioniuia Thiosvanate
A. KH, CNS (0.1 N) - Dissolve 8 g of NH.CNS in water and dilute
to 1 liter in a volumetric flask.
' -B. KHiCNS (0.01 N) - Dilute 100 ml of 0.1 N NHiCSS to 1 liter
in a volunistric flask, or dissolve 0.8 g NH,. CNS in 1 liter
of distilled water.
Silver Nitrate
A. Agio. (0.1 N) - Dissolve 17.0 g of silver nitrate (Ag?\T0~)
in vater and dilute to 1 liter in a volumetric flask.
Transfer to an archer reagent bottle. Standardise this
solution against standard 0.1 N NaCl solutions,, according
to the Volhard Titration.1
- 3 -
-------
3 (0.01 N) - Dissolve 1.7- g-of -AgNO. in water and dilute
to 1 liter in a volumetric flask. Transfer to an amber
•reagent bottle. Standardize this solution against standard
0.01 N NaCl solution, according to the Volhard Titration.
Starch solution (iodine indicator)3 1.0$
Make a thin paste of 1 g of soluble starch in cold water and
pour into 100 ml of boiling water while stirring. Boil for a few
minutes. Store in a glass stoppered bottle.
Standard iodine solution (0.1 N)
Dissolve 12.69 g of resublimed iodine (!„) in 2$ ml of a solution
containing 15 g of iodate-free potassium iodide (Kl); dilute to 1 liter
in a volumetric flask. Standardize this solution against a standard
thiosulfate solution using starch as an indicator. This solution should
be stored in an amber reagent bottle and refrigerated when not in use.
APPARATUS
Absorbers
A. Midget irrpingers - An all glass midget impinger capable of
removing KC1 and Cl from an air sample by using l£ ml of
absorbing reagent. This device should be used when sampling
stack gas containing less than 0.1 percent KG1 or Cl_.
B, Grab sampling flask - A 2-liter glass bottle equipped vith
Teflon stopcocks on either end. This device should be used
when sampling percentage quantities of HC1 or C12. Absorbing
-------
reagent is added to the grab sample flask after the sample
has been collected.
Dispenser (absorbing reagent) - One-hundred milliliter round-bottom
flask, modified with a Teflon stopcock and ball joint extension (see
Figure 2). Use to add absorbing reagent to grab sampling bottle after
the sample lias been collected.
Buret ($0 ml)
Srlenmeyer flasks (2j?0 ml)
ANALYTICAL PROCEDURE
Collection of samples
A. Midget impingers: The apparatus for sampling of HC1 and
Clp consists of a probe (l), impingers (5>> 6, 7, 8), pump
(12), rotameter (lit), and dry gas test meter (16)* (Figure 1.)
The probe (l) is 18" long and made from medium wall pyrex
glass. The first 6 inches is 5/8" OD tube and ifee Last 12
inches is 1/U" OD tube. Nubs are impressed into the larger
tube just before the contraction to act as a s-top for glass
wool which is placed in the end of the probe to.' act as a
filter. The l/lj" end has a male 12/J? ball joint on the end.
The whole glass tube is wrapped with 7 feet of 26 gauge
nichrome heating wire (2). A variable transformer (3) con-
nected to the wire controls the voltage and hence the tempera-
ture of probe. The wire is covered with fiberglass insulation
tape and placed in a stainless steel probe sheath*
-------
A-three-vay~valve-(b) with ball joint connections to the probe
and first impinger allows the ice bath (9) (a plastic bucket)
1 _ . -T, J.1-^
• and ijpinger system to be sealed off and removed after a run
iscoraolcted. This valve is also used to purge the probe prior
to sampling. EUe to the sensitivity of the analytical method,
only a small sample is required; therefore, Tour midget impin-
gers (5, 6, 7) contain 15 ml of the absorbing reagent. The
fourth impinger (8) is left dry to collect ar?r entrained liquid.
This impinger is attached to the umbilical coard. '
The umbilical cord (10) leading from the collection device to
the pump and metering system consists of a 1/1*" OD - 1/8" ID
polyethylene sample line, and an electrical circuit for the
probe. The sample line is first connected to; a drying tube
(11) containing silica gel, which removes moisture from the
sample gas. From the drying tube, the gas passes through a
diaphragm pump (12) to a gross flow control rotameter (lh),
where the sampling rate is maintained at O'.l. CM with a needle
valve (13). The sampled gas then passes thorough a 0.1 CFM per
revolution dry gas test meter (16), where the sample volume is
read with an accuracy of 1 1 percent. A thessaometer (lf>)
placed on the inlet side of the meter measures the temperature
of the gas in the meter. This temperature reading is later
used to correct the sample volume to standard conditions.
The equipment described above is leak tested prior to sampling
by plugging the end of the probe and then le&ting the
- 6 -
-------
create a vacuun-on-the sysiem._ If ..the dry test meter con-
tinues to revolve, the system lias a leak; if the meter does
.not revolve, then the system is tight at operating vacuum
pressures.
VJhen the leak test has been completed, the probe should be
heated to the desired operating temperature (200 to 2|?0 F)
before sampling begins. To sample, simply turn on the pump
and adjust the rotameter via the needle valve to the desired
setting. This setting should be checked at 10 to 15 minute
intervals during the test. Generally, a sampling interval
of 30 to 60 minutes is used; however, this may vary with the
concentration of HC1 present in the source effluent. At *he
end of the test turn off pump and disconnect the sample col-
lection unit.
Cleanup procedure for the midget impinger train consists of
errptying the four impingers into a sample bottle and then
rinsing each one tvrice with distilled water into the sample
bottle.
B. Grab sampling: The apparatus used for purged flasi-: gas
sarpling consists of an accurately calibrated 2-liter glass
bottle with Teflon stopcocks on either end. The flask,
vith both stopcocks in the open position, is placed in the
sa.Tpling line and stack gas (under positive pressure) is
allG-tfed to flow through the flask. (A purge volume 1Q tines
- 7 -
-------
-the"voiume~of -fche~flask should~be used.) After the~flask
has been purged, both valves are shut off.. The flask is
removed from the sampling line and one valve opened to the
atmosphere to allow the flask to come to atmospheric pressure.
Pipet 2$ ml of absorbing reagent into the modified buret and
connect it to the ball joint on one side of the flask. Absorb-
ing reagent is allowed to flow into the flask by opening the
stopcocks. The reaction of HC1 and/or Cl with the appropriate
absorbing reagent creates a negative pressure in. the flask and
pulls more reagent into the flask. After completion of the
reaction, wash all the absorbing reagent into the flask with
a snail quantity of water. This step is important only when
alkaline arsenite reagent is used. Remove the traret and shake
the flask for several minutes to insure complete absorption of
the gases.
Quantitatively transfer the contents of the grab sailing bottle
to a saroxle container, such as a polyethylene bottle, with
deionized-distilled water.
Sample Preparation
Measure the actual volume of the liquid saraple or adjust to a
known volume using a graduated cylinder or volumetric flask.
PROCEDURE A. Analysis of Hydrogen Chloride
Pipet an aliquot of the sample into a 2^0 ml Erlenrueyer flask.
Add 2j ml of water, $ ml of nitric acid and sirirl to mix. Add 0.1 K
- 8 -
-------
or 0.01 N silver nitrate, depending_.on_chloride content, from a buret
until it is in excess. Near the equivalence point, the silver chloride
precipitate will coagulate. YJhen coagulation occurs, add an additional
5> ml of silver nitrate. Add 3 ral of nitrobenzene, 2 ml of ferric indi-
cator, and back-titrate with 0.1 N or 0.01 N ammonium thiocyanate until
the first appearance of the reddish-brown Fe(CN3)7^ complex. A blank.
determination for chloride in the absorbing reagent should be run simul-
taneously and subtracted from the sample results. From the titer of
iJHi CMS solution, as determined previously by titration against standard
AgNO- solution using ferric alum as an indicator, calculate the net
volume of AgNO required for precipitation of the chloride.
•CALCULATIONS
Compute the number of milligrams of KC1 present in the sample by
the following equation:
KC1, mg = net ml AgNO, x T x F
T = hydrogen chloride equivalent of standard AgNO,
(T = 3.6£ mg HCl/ml for 0.1 N AgNOj
(T = 0.365 mg HCl/ml for 0.01 N AgNO )
p c samP-e volume, ml
aliquot volume, ml
Convert the volume of air sampled to the volume at standard condi-
tions of 70°F and 29.92 in. Hg.
yg . y x -L- ~ #0°R
19.92 A (t + W'R)
V » volume of gas sampled, cu. ft.
- 9-
-------
P '^-barometric "pressure, in. Hg
t = temperature of gas sampled, °R
Determine the concentration of HC1 in the air sample by the
following formula:
662 = ul/mg of HC1 at ?0°F and 29,92 in. Hg
C =• concentration of HC1, mg
Vg = volume of gas sailed in cu. ft. at ?0°F and 29.92 in. Hg:
28.32 » liters per cu. ft.
PRQCEUJRS B. Analysis of Hydrogen Chloride in the Presence of Chlorine
Pipet an aliquot of the sample into a 25>0-ml Erlenmeyer flask and
proceed with the Volhard Titration for total chlorides as described
under Procedure A. A blank determination for chloride in the absorbing
reagent (alkaline arsenite reagent) should be run simultaneously and
subtracted from the sample results.
Pipet another aliquot of the sample into a 2^0-ml Erlenmeyer
flask. Add a few drops of phenolphthalein indicator, neutralise
carefully with concentrated hydrochloric acid, and cool. Add suffi-
cient solid sodiun bicarbonate (NaKCO_) to neutralize any excess
hydrochloric acid, then add 2-3 g in excess. Add 2 ml of starch
indicator and titrate with 0.1 N iodine solution to the blue endpoin-t.
For the reagent blank, determine the number of ml of 0.1 N !„ required
to titrate 2£ ml of alkaline-arsenite absorbing reagent, as described
above .
- 10 -
-------
CALCULATIONS"•
Deterniine the number of milliliters of 0.1 N I_ required to
titrate the entire sample by the following formula:
Sample (ml 0.1 N I2) = (ml of 0.1 N I,, 'for aliquot) x F
tr - volume of sample, ml
volume of aliquot? ml
C12, mg = Blank (ml 0.1 N I2) - Sample (ml 0.1 U I2) x 3.516
3.5U6 = chlorine equivalent of 0.1 N IA, mg
Convert the volume of gas sampled at standard conditions of
70°F, 29.92 in. Hg, using the formula in Procedure A, Calculate
the concentration of Cl? in the sample using the following formula:
pom Cl, by volume
^ S
3bO = ul/nig of C12 at ?0°F and 29.92 in. Hg
C = cone antration of C1?J mg
Vq = volume of gas sampled at standard conditions, liters
\~*
Determine the number of milligrams of HC1 present in the sanale
b}r subtracting the number of milligrams of Cl? present, as determined
by the iodine titration, from the total number of milligram^ of
chloride present as determined by the Volhard Titration. Calculate
the concentration of HC1 in parts per million using the formula in
Procedure A.
- 3JL -
-------
DISCUSSION- OF- PROCEDURE _. - .
The estimated error for the combined sampling and analytical
procedure.is _ 10 percent. The precision of the analytical methods
is t 2 percent on standard samples containing NaCl and NaAs00.
The usual volumetric errors are encountered with the Volhard
Titration. Premature endpoints may occur, if the NH, CNS is not
added dropvri.se near the equivalence point and the solution shaken
before the next addition. Nitrobenzene is used to effectively
remove AgCl by forming an oily coating on the precipitate and pre-
2
venting reaction with the thiocyanate. Substances which form
insoluble silver salts and bivalent mercury, which forms a stable
complex ion v;ith the thiocyanate, interfere in the analysis and
must be absent from the sample. Titrations should be made at tem-
peratures below 2£°C, as is customary in other titrations with
thiocyanate."
The chief source of error in the iodine titration of arsenite
is failure to use sufficient bicarbonate to neutralize all the
excess acid. If insufficient bicarbonate is added, serious errors
are incurred due to a fading endpoint. Reducing agents, such as
sulfur dioxide, and oxidizing agents, such as iodine, nitrogen
dioxide, and ozone, if present in the stack gas sample, would inter-
fere with the iodine titration and yield high results.
- 12 -
-------
REFERENCES
1. Standard Methods of Chemical Analysis, D. Van Nostrand Coropany,
Inc., 6th Ed., Vol. 1, 329-330 (1962). .
2. CaldweU, J. R., and Mayer, H, V., Ind. Eng. Chea., Anal. Ed.,
7, 38 (1935).
3. Jacobs, K. B., The Chejuical Analysis of Air Pollutants, Interscience
Publishers, Inc., 10, 199 (I960).
-------
1 2
13
Figure 1. Schematic of sampling apparatus,
-------
APPENDIX B
PROCESS DATA
-------
ROCHESTER SMELTING
AND REFINING CO., INC.
SB SHERER STREET • ROCHESTER, N. Y. 14611
MAILING ADDRESS' P. D. BOX 547 • ROCHE STER, IM. Y. 1<3 6 D 5
February 3, 1977
SIIMCE 1895
TELEPHONE 716/3aB-<37-SO
MR. ROBERT A. BAKER, P. E.
ENVIRONMENTAL ENGINEER
ENVIRONMENTAL SCIENCE AND ENGINEERING, INC,
P. 0. Box 13^
Gainesville, Florida 32604
Dear Mr. Baker:
Enclosed herev;ith is the information that you requested.
If you have any more questions or need any further
information, please do not hesitate to call.
Cordially yours,
_.
STEVEN R. SHENCUP
SRS:rd
Enc.
ALL AGREEMENTS AND SALES ARC CONTINGENT UPON STRIKES ACCIDENTS, DE.LAVS OF CARRIERS AND OTHER DEE. *V1:S .UNAVOIDABLE OR
PE»C\D OU« CQ'-*T~.C: f.i F«('CCS Sl-t-JfCl TO ACCEPTANCE B> RETURN MAIL ALL SUNOGRAPHICAL »A'D ILEHlCAL
fn.--»5 SUb.'f'l '•! '. O'-f'C.V .r>\ t-i tGPiEwtNTS MADC Pv AGtNTS *R£ SUbJECT TO OUH A'F-f'^OV AL
-------
FURNACE //..
ALUMINUM SCRAP INPUT
ALSO ADDED
SKIMMED OFF
FINISHED PK
J0/3P/76
10/19/76
10/20/76
10/21/76
10/22/76
7775#
5'05//
3750//
31H#
5121#
3W6//
60 0#
^256//
988#
1125V/
99W
25859#
1480#
12606#
16106#
5842#
15160#
1000#
8086#
9996#
633V
25^65#
700#
^50//
8199//
12230//
5136//
3703//
725V-/
1777V/
67 6#
550#
300 ALUMINUM INGOT
CAST ALUMINUM (DIRTY)
ALUMINUM BUTTS
6000// FLUX
3550^ SILICON
15 BAGS ALUMINUM FLUORIDE
SILICON
15 BAGS ALUMINUM
FLUORIDE
6000// FLUX
PAINTED ALUMINUM SIDING (DIRTY)
#3-S ALUMINUM SPINNINGS
ALUMINUM CHIPS (CLEAN)
ALUMINUM COPPER RAD. FINS
ALUMINUM BUTTS
CASTINGS
CAST ALUMINUM (DIRTY)
//3-S ALUMINUM SPINNINGS
ALUMINUM CHIPS (CLEAN)
ALUMINUM COPPER RAD. FINS
CLEAN CASTINGS 2750// SILICON
#3-S ALUMINUM SPINNINGS
PAINTED ALUMINUM SIDING (DIRTY)
ALUMINUM CHIPS (CLEAN)
COPPER
ALUMINUM CAST (DIRTY) 6000// FLUX
ALUMINUM BUTTS 2800# SILICON
PAINTED ALUMINUM SIDING (DIRTY)
ALUMINUM CHIPS (CLEAN 20 BAGS FLUORIDE
ALUMINUM COPPER RAD. FINS
ZAMAK DROSS
ALUMINUM CAST (DIRTY)
ALUMINUM BUTTS
3-S ALUMINUM SPINNINGS
3-S ALUMINUM
PAINTED ALUMINUM SIDING (DIRTY)
ALUMINUM CHIPS
Z-5 HARDENER
COPPER
6000# FLUX '
3250// SILICON
19 BAGS FLUORIDE
8842//
9718#
5531//
56.182,/
-------
ROCHESTER SMELTING
AND REFINING CO., INC.
26 SHERER STREET • ROCHESTER, N. Y. 1-4611
MAILING ADDRESS' P.O.BOX 5«37 • Ft OEHE STER. N. Y. ia S OS.
SINCE 1BSS
TELEPHONE 7 1 6 / 3 S S - & 7 -3 O
October 25, 19?6
Mr. Robert A. Baker
ENVIRONMENTAL SCIENCE AND ENGINEERING, INC.
P. 0. Box 13^54
Gainesville, Florida 3260*1
Dear Mr. Baker«
Enclosed is the FURNACE information that you requested.
If you have any further questions regarding this, please
do not hesitate to call me.
Yours very truly,
STEVEN R. SHSNGUF
SRStrd
Enc.
G[M UPO.N ST-^-IS ACCIDENT:- D£LA;£ or cA'-=c£
- i S :. • " TV i tit! - — N C [ Er PtT_f.'\ v.a-L ALL
i ;'O CJHE& DELAVS UNAVOIDABLE OR
TC \OGS AS'HtC AL A',: ' L C f"T ' ^
-------
DATE
10/18/76
10/19/76
10/20/76
10/21/76
10/22/76
NO. 1 FURNACE
ALUMINUM SCRAP INPUT
ALSO ADDED
SKIMMED OFF
FINISHED
PRODUCT
Sheet Aluminum (Dirty)
6166// Loose Aluminum Sheets £
(Sheet was Dirty) Clips
75 ^5$ Big Alum Bricquetten
Hf818# Loose Sheet & Brick Alum
(Sheet was Dirty)
Aluminum Rolls (Clean
6000# Flux
10 Bags Alum Fluoride
(for testing purpose)
10.300//
33,
Sheet Aluminum (Dirty)
Big Aluminum Bricquettes
Loose Alum Sheet & Clips
(Sheet was Dirty)
2158// Aluminum Sheet (Dirty)
13118# Sheet Alum in Bales (Dirty)
7611// Clean bricks & Sheet Aluminum
(Sheet was Dirty)
3535// Clean Alum Spinnings in Bales
618V/ Large Aluminum Bricks
265// Iron
6000// Flux
10 Bags Alum Fluoride
(for testing purpose)
39,37^
15352//
7820//
Contaminated Clips - 90# Iron
720# Clips 6000# Flux
Loose Aluminum Sheets (Dirty)
Bales of Sheet Aluminum (Dirty)
8602# Large Aluminum Bricks & 8718# Aluminum Rolls (Clean)
Aluminum Wire . ,
Loose Sheet 'Aluminum (Dirty) 6000# Flux
Large Aluminum Bricks
Aluminum Chips
Aluminum Rolls '
Aluminum Spinnings
Aluminum Clippings 156# Iron
Loose Aluminum Sheets (Dirty) 6000# Flux
Bricks * ' t
Aluminum Sheet in Bales (DJrty)
Aluminum Can Stock
Alumi)ium Litho Sheet
39,
11236#
3528//
9,090#'
13650#
o
3855#
921//
-------
HAT!;:
10/18/76
10/19/76
NOTE:
10/20/76
10/21/76
10/22/76
ALUMINUM SCRAP INPUT
ALSO ADDED
SKIMMED OFF
FINISHED
PRODUCT
800# Silicon
8 Bags Alum Fluoride
4000# '.Flux
10 Bags Fluoride
60 IB// Cast Aluminum (Dirty)
3S Clippings (Clean)
Aluminum Chips , (Clean)
Alum/Copper Rad.Fms
6110// Cast Aluminum (Dirty)
5072// Painted Aluminum Siding
(Dirty) 50// Magnesium
30/J-3// Mxd. Aluminum Clippings (Clean)'K)00# Flux
~500# Alum/Copper Had/ Fins 1?00# Silicon
100# Copper
On our day shift the only thing we added was the Magnesium.
in the furnace from the midnight shift.
17 36//
16.650//
2330# 13
Everything else was already
Cast Aluminum (Dirty) *K)00# Flux
?890// Painted Alum Siding (Dirty) 1^20# Silicon
4902// Mxd. Alum Clippings (Clean) 9 Bags. Alum Fluoride
300// Alum/Copper Rad. Fins (Clean) 'iO# Magnesium
15,
26l2# Aluminum Butts
6516// Cast Aluminum (Dirty)
6106// Aluminum Chips (Clean
4000# Flux
800# Silicon
10 Bags Alum Fluoride
1956// Mxd. Aluminum Clippings (Clean)
5010// Cast Aluminum (Dirty) 38?0# #38^ Alum Ingot
Aluminum Butts ^000# Flux
Mxd. Aluminum Clippings (Clean)
770# Silicon
100// Copper
1^- Bags Alum Fluoride
25// Magnesium
5599#
-------
(ttaiif'icate itf Analysis
&
Ort/cr No.
Lab No ....... .£.ZZ. .......
Sample Of
Heat
Ship To
..?..'7
%
%
%
%
%
%
%
%
Copper
Tin
Lead
Antimony
Iron
Nickel .......... '.*?...
Zinc .......... .'..%/.
Silicon
Manganese
Magnesium
Aluminum ..j^ZZ...... ............ %
Titanium ....... '..?..¥.. ............. %
Cadmium .................................... %
Sulphur ................................... %
Phosphorous ................................ %
Chromium ........ '.'2. ................. %
Metallurgist
fflaitftcat^ nf Analysis
£
Order No.....
Lab No >1Z.
Sample Of ^..L
Ship To
%
..... .<.*.£... ............ %
%
........ /.<.//. ............... %
....... /.
-------
(ttaitftcate nf JVrta lysis
o..
Ortler No.
l^ib No. /£ "^
Sample Of .. --. :.-^-
Ship To .
Cobber
/ r
Tin
Lead
Antimony .
Iron
Nickel
Zinc
Silicon
Maneanese.
Heat No. . 2-3 "/f
. r? - or
/"
r*Y... %
iff %
?..£/ %
Magnesium £.JL./^. °/o
Aluminum ../..?..<.»..£. ...°/0
Titanium ?£.?r:. ....%
Cadmium °fo
Sulphur %
Phosphorous %
Chromium '..^A %
ijf^^i^^l^^^
^,
(Haitftcate nf Analysis
Order No.
Lab No ......... FA..*?.. ...... Heat No ...... i
Sample Of ..... _...^
-------
k^Sy^^
(Eerltficate nf JVnalgats
Order No....
L*£ No
5rf/w/>/e O/
5/-/> To
%
%
Copper
Tin
Lead
Antimony
Iron
Nickel
Zinc
Silicon
Manganese ...... '...I. J... .................. °/o
Magnesium.../...'...../.. ................. °/o
Aluminum
..:.%
%
%
%
'.%
Cadmium .................................... °/r>
Sulphur ................................... %
Phosphorous ................................ °fa
Chromium ......... ?..{'./.. ................. °fo
Mctallurgiil
Xfi^'*
TiT?1*
¥
r :i
fflairficate uf JVnalysis
a.f tic..
Order No.
Lab No
Sample Of
Ship To
Heat No.....
%
%
%
Copper
Tin
Lead
Antimony ..... . ............................. %
Iron ...... {.
-------
(Herftftcttte of JVnalgsis
o-.r 9
1:
Order Nn.
Lab No j£Z*_ Heat
Sample Of -.21.?..!*^. ^f^L^.. ^
Ship To _
Copper -ZiA/". %
Tin __C?/I_ %
Lead £*.£ %
Antimony %
Iron /j.Lfc. °/0
Nickel t.a?j£.. %
Zinc ../_:£?. %
Silicon /A/.?. % W
Manganese ..f.A.7. %
Magnesium {...?../... % ^f
Aluminum ../&?3.... % •%_
^ ' y^
_, Titanium f. % {f
€C N=
Cadmium ^o
Sulphur %
Phosphorous %
Chromium L°.L % W
Metallurgist
^^^^r^^
-------
^^
Qlcrttftcatc nf
&
On/ir No.
Lab No 7.
Sample Of.
Ship To
Mat
Dale
%
Copper 3;..?J %
Tin ..../."/I %
Lead f.<>.'..l. %
Antimony %
Iron IC(.J.. .°/0
Nickel ... /*>f °7~
Zinc
Silicon
/ -
Manganese i. J...7. %
Magnesium /.././. °/o
Aluminum fizf^.. %
Titanium f.?.J. %
Cadmium nfo
Sulphur , %
Phosphorous °/0
Chromium '
.^/^
Metallurgist
^^'^^'^^^^^^'^
fflaitftcate nf
Sample Of
Date ..... /..<>. ^..t.-.<
Copper J.<-.S.& %
Tin _..../.J Cadmium , %
Sulphur '.. %
Phosphorous °/n
Chromium 'A.I..
<>—£•>
Metallurgist
\c:.
f'
-------
^.^^i^
Cferftftcate of
&
Order No.
Lab No. .......
Sample Oj -.
Ship To ......
Heat No
Copper ....J.f.-J.-L.. %
Tin _.._'_i..£L %
Lead t.*L %
Antimony _ %
Iron L?A %
Nickel /:.f?..^._.._ %
Zinc if...^.. %
Silicon ' ' /£:££l.. %
Manganese !?...•?..(.. _ °fo
Magnesium /...^y?_ %
Aluminum .j&Zfff.... °/o
Titanium ,^L._ °/Q
Cadmium %
Sulphur %
Phosphorous %
Chromium
o-.,
•$£•. -j
Metallurgist
-------
APPENDIX C
ADDITIONAL INFORMATION
-------
U.S. EPA METHOD 5
COMPUTER PRINT OUT
AND
LABORATORY ANALYSIS
-------
t;| A '• T - * '-' F - J u "
? T t C H J n . C C'•' R I K E D IKL F 7
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' *~ ' r • " r ; •
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r-- T i ^ f ; • '
1 f-r L\ i- T | -j f- v r i T- i- f '. '- 1
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Ti
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r: .
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). ^ . 1 it. c f .
1 0 / ? 1 / 7 ft 1 r. / ? 1 / 7 f-
1 0 ? 7 - HJ 3 G
1 ? 5 ft j 5 ?. ft
n?. . *-f .
/-: ^ . i .~ ^-ftc.^0
fc 1 . 0 f ?. 6! 7 . ft 1 s
5 ° . ? r- * /.! 7 . ii ~ *•
1 'c . r 7.5
5.^1 C . 7 •-• 1.2?
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?'.'• ?-r.? ?-^.K?
. r: . ^ ' . r. r • . .-. r
? s , P a 7- >"..= = p K , c- ?
? ?• . ft 5 p P , 7 i.. ? F . 7 fl
A -7 r- .-» *% - •* f
... 7 P. - , p . ,. .-
0.305 i* . u 1 r
? 3 . ^ 1 ? i.- . ? 'e ? •• . 7 P
? 7 ii ^ i . ? *•• ^ ^ i .. ;; i s .'.''•.
? 7 -*:/!. ? ~ s 3 r „ 3 « ; .'.• 7 .
?^ft73. P'-sO'1, ? " j i: f .
3 r- 0 . 7 P 1 c 1 . 1; " :• i ;- . 7 c
0 0 ? ^ <•: 0 r. i ;•• i
<"• .
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» ' *
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« «•
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••* • »
J 7 n . ij r. c « . 7 •-
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3 P r. . F (^ 1 1 * . f.r
C- . ^ ^' ?, ft ^.^33" • . r /• l c
f) . f: i.1 p S ^ , 0 3 =1 P " . ,': fc ft C
1 ''' . ? F c p p . r 5 K ? - .5 4 ^ \ f- ,.
-------
- , r r
r (• /. 7 T .-• i. _ •_" r- r .. r. r 7 r c
/. ' P | ] ,' f. T C A T >.' ^ P « C
-------
I; r f i 7 j r t. - crryrcfFp
5 A " P (. I ^ - T L'' i T »-• - P * P T " C I 1. i T
r ', , r :
7 1 ,71
•"' . I C 5
r - ? r. -
1 / 1 c / 7 r-
i •, r ~
•, /. ~i ,*
~ r .
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!-' | .'. f ~ N .' " r » ] f. > •
J-l .* (>' T r - f L'T 1. F. T
c 4 v P [ It. r; T H i T K - P * c f J f L L * - c c
1 ^ / r 0 / 7 A
0 /.?'•/ 7
i r ? ^
1 ?-0?
1 1 •'.•• .
•7 ?
o r n :r r i c •
C •; C C
•" r n r, «, c i
52 . 1
.0123
.0136
5.3111
1 . C C'
-------
f. r i( 1 r . - " I. T I p. T
L C C i T I f V - * P C ••' F F " '-; c
5 A •'• P L Ik- G T D i T *- - P A R T j c i. I. .'. T - f.
• : • r T T • -
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• " ~ r -• r r. r •' ~ >. T c
r c r i
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' / c. ? / 7 f
A 3 P
1312
t; A .A ^ c
C*^ * ff< r~
•; . ' r c
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5 7
-------
1.0 F i. 1 t- e r
LAHORATORY ANALYSIS - I'ARTT.CULATES
Sample 1
I
Inlet:
9437
9440
9454
9448
9455
9463
9471
9473
Outlet:
9432
9374
9442
9446
9449
9458
9461
9468
9379
Overnight:
9452
9465
9381
km 1
I
2
3
4
5
6
7
8
1A
IB
2
3
4
5
6
7
8
Runs :
1
2
3
F L Iter
No.
375
433
445
413
389
421
448
402
378
379
425
436
417
370
434
418
444
446
435
44 1
Tare
We i gh t
(gm)
.4682
.4274
.3279
.4299
.4656
.4288
.3302
.4265
.4902
.4541
.4315
.4290
.3921
.4869
.4309
.3896
.3266
.3318
.4268
.3984
Co 1 01-
green-gray
die black w/gray
dark black
black
black
b 1 a c k
black w/glass
black w/green
wh i. te
wh i. te
1 t gray in ct r
1 1: gray in ctr
black gray
green
o £ E wh L t e
dk gray green
1 ight gray
green black--
c o IT r o d e d state
green
black gray
1st:
(gm)
.6203
.5970
.5027
.7073
. 6529
.5330
. 5854
.6158
.5244
.4655
.5585
.4765
.3972
. 6042
.4316
.6567
.3340
. 5608
.8798
.4105
2nd
(gm)
.5740
.5939
.4998
. 7040
.6525
.5290
.5858
.6106
.5239
.4651
.5562
.4760
.3975
.6001
.4312
.6542
.3316
.5607
.8796
.4100
3rd
(gm)
.5741
.5951
.4996
.7062
.5264
.6119
.5568
.6025
.6526
.3316
.8796
W I
4th
(gm)
.5698
.5968
.5027
.7052
.6529
.5250
.5749
.6100
.5227
.4649
.5571
.4767
.3974
.6024
.4313
.6549
.3325
.5610
.8910
.4105
SIGH]
5th
(gm)
.5460
.5917
.4984
.7000
.6399
.5225
.5713
.6046
.5187
.4612
.5552
.4751
.3966
.6006
.4304
.6482
.3307
.5528
.8724
.4089
[ N G S
6th
(gm)
.5207
.5968
.5013
.7008
.6457
.5253
.5730
.6112
.5259
.4711
.5574
.4768
.3980
.6140
.4318
.6568
.3319
.5631
.8847
.4088
7th
(gm)
.5165
.5934
.4989
.6992
.6360
.5202
.5718
.6080
.5208
.4618
.5563
.4791
.3975
.5979
.4315
.6465
.3310
.5523
.8698
.4075
8th
(gm)
.5132
.5911
.4980
.6963
.6359
.5188
.5702
.6033
.5187
.4613
.5570
.4799
.3991
.5991
.4312
.6451
,3320
.5490
.8640
.4082
Final 1
(gm)
.5132 .1
.5914
.4985
.6978 .:
.6360
.5195 J
.5708 .:
.6040
.5187 .(
.4613 .(
.5557 .:
.4756 .(
.3969 .(
.5979
.4308 -.1
.6451 .:
,3309 ,(
.5490 .:
.8640 .i
.4079 .(
-------
2.0 Honkers
Sample Run Beaker
Inlet :
9441 I 13
14
9444 2 11
12
9445 3 3
5
9451 4 2
1
9456 5 8
9
9464 6 6
7
9472 7 16
9474 8 15
B 1 ank 1 0
Vol u me
(ml)
85
135
118
146
115
130
11.0
145
130
115
50
140
130
150
50
Tare
(gm)
81.
80.
79.
81.
82.
81.
81.
82.
81.
81.
81.
80.
83.
80.
82.
6445
8667
8626
7659
2915
3906
4655
3022
0174
4521
5212
8630
2780
1897
0571
W
1st
(gm)
81.6543
80.8767
79.8747
81.7804
82.3087
81.4024
81.4856
82.3175
81.0292
81.4603
81.5416
80.9011
83.3556
80.2226
82.0577
E I G H INGS
2nd 3rd 4t:h
(gm) (gm) (gm)
81.
80.
79.
81.
82.
81.
81.
82.
81.
81.
81.
80.
83.
80.
82.
6544
8771
8749
7807
3083
4028
4862 81.4858
3177
0295
4605
5418
9017 80.9019
3558
2231
0580
Final
Weigh t
(gm)
81.
80.
79.
81.
82.
81.
81.
82.
81.
81.
81.
80.
83.
80.
82.
6544
8769
8748
7806
3085
4026
4859
3176
0294
4604
5417
9016
3557
2229
0579
Net; Adjustment
Gain for Blank
(gm) (gm)
.0099
.0102
.0122
.0147
.0170
.0120
.0204
.0154
.0120
.0083
.0205
.0386
.0777
.0332
.0008
.0014
.0022
.0019
.0023
.0018
.0021
.0018
.0023
.0021
.0018
.0008
.0022
.0021
.0024
.0008
Ad jus tec
Net Gair
(gm)
.0085
.0080
.0103
.0124
.0152
.0099
.0186
.0131
.0099
.0065
.0197
.0364
.0756
.0308
-------
2.0 Beakers
Sample Run
Outlet: :
9434 1A
9376 IB
9443 2
9447 3
9450 4
9459 5
9462 6
9469 7
9380 8
Beaker
3
15
15
14
16
1
3
12
7
16
6
9
11
10
4
8
5
Volume
(ml)
145
140
145
25
150
140
145
140
90
110
145
30
140
55
140
140
50
Tare
(gm)
82.
80.
80.
80.
83.
82.
82.
81.
80.
83.
81.
81.
79.
82.
84.
81.
81.
2915
1897
2229
8769
3557
3176
3085
7806
8630
2780
5417
4604
8749
0579
2189
0294
4026
W
1st:
(grn)
82.3447
80.2507
80.2240
80.8713
83.3532
82.3219
82.3120
81.7820
80.8672
83.2830
81.5436
81.4567
79.8782
82.0590
84.2302
81.0464
81.3993
E I G 11
2nd
(gm)
82.3430
80.2507
80.2240
80.8710
83.3532
82.3221
82.3120
81.7816
80.8672
83.2809
81.5436
81.4560
79.8777
82.0581
84.2300
81.0451
81.4002
INGS Final
3rd 4th Weight
(gm) (gm) (gm)
82.3407 82.3407 82.
80.
80.
80.
83.
82.
82.
81.
80.
83.2788 83.2789 83.
81.
81.4565 81.
79.
82.0586 82.
84.
81.0455 81.
81.3988 81.
3407
2507
2240
8712
3532
3220
3120
7818
8672
2789
5436
4564
8780
0586
2301
0457
3994
Net Adjustment
Gain for Blank
(gm) (gm)
.0492
.0610
.0011
-.0057
-.0025
.0044
.0035
.0012
.0042
.0009
.0019
.0040
.0031
.0007
.0112
.0163
-.0032
.0023
.0022
.0023
.0004
.0024
.0022
.0023
.0022
.0014
.0018
.0023
.0005
.0022
.0009
.0022
.0022
.0008
Ad justec
Net Gain
(gm)
.0469
.0588
-.0012
-.0061
-.0049
.0022
.0012
-.0010
.0028
-.0009
-.0004
-.0045
.0009
-.0002
.0090
.0141
-.0040
-------
2.0 Beakers
Sample Run Beaker
Ovorn iph t :
9453 1 54
9467- 2 35
catch
9382- 3 Ace 30
cat ch
9383 Water 52
9470 3* 51
53
Vol nine
(ml)
225
110
200
250
250
225
Tare
(f>m)
96.7278
106.5266
107.4211
87.4415
105.7463
104.7784
W
1st
96.7495
106.5518
107.4300
87.4675
105.7455
104.7835
R I G H
2nd
(gm)
96.7489
106.5517
107.4304
87.4677
105.7450
104.7833
I N
96
106
107
87
105
104
G S
3rd 4th
(gm) (gm)
.7488
.'5517
.4324
.4676
.7451
.7834
Final
Weigh t
(gm)
96.7489
106.5517
107.4302
87.4676
105.7451
104.7833
Net
Gain
(gm)
.0211
.0251
.0091
.0261
-.0012
.0049
Adjustment
for Blank
(gm)
.0036
.0000
.0032
.0000
.0000
Adjusted
Net Gain
(gm)
.0175
.0251
.0059
.0261
-.0012
.0049
* No filter.
-------
TOTALS
3.0 Total
Sample Run
Inlet: 1
2
3
4
5
6
7
8
Our. let 1A
IB
2
3
4
5
6
7
8
Overnight 1
2
3
3
Sample No.
9437
9440
9454
9448
9455
9463
9471
9473
9432
9374
9442
9446
9449
9458
9461
9468
9379
9452
9465
9381
Filter No.
375
433
445
413
389
421
448
402
378
379
425
436
417
370
434
418
444
446
435
441
No filter
Filter
(gm)
0.0450
0. 1640
0.1706
0.2679
0. 1704
0.0907
0.2406
0.1775
0.0285
0.0072
0.1242
0.0466
0.0048
0.1110
-0.0001
0.2555
0.0043
0.2172
0.4372
0.0095
Sample No.
9441
9444
9445
9451
9456
9464
9472
9474
9434
9376
9443
9447
9450
9459
9462
9469
9380
9453
9467
9383
9382
9470
Wash
(gm)
0.0165
0.0227
0.0251
0.0317
0.0164
0.0561
0.0756
0.0308
0.1057
.Neg
0.0022
0.0012
0.0028
Neg
0.0009
0.0090
0.0141
0.0175
0.0251
0.0320
0.0049
Totals
(gm)
0.0615
0.1867
0.1957
0.2996
0. 1868
0.1468
0.3162
0.2083
0.1342
0.0072
0.1264
0.0478
0.0076
0.1110
0.0009
0.2645
0.0184
0.2347
0.4623
0.0415
0.0049
-------
PARTICLE SIZING
COMPUTER PRINT OUT
AND
LABORATORY ANALYSIS
-------
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f.. r- ~ f r 2 •'•i:
^. « -*n *\ ~~* -'r ' "7
i • •••..-
r-. ft f, r: Q 5 ? ]
'.r n51??P
-------
,r- ,c ! ''
'. . r
'_ *
1 /. '•
[.. ./. LV T 7 r I [- " i
- "• '•• T • J '- r. T v |_ r T P i - V /j
"v .. ? . ^. r r: •- / C r
<-<.'• • ^f t; - / A r. r
:• 1
:• r r ^, - :- A : ^
r ! :' t-; i c c;
3 c S ? #• . ^
T; <; 7 c. t ^ p
" ^ " 0 f , 0
7 t C C 5 ^ f:
^?°BI.c
V:- £ ? 5 . ^
• T ;;• T r p r r 5; 5 [; t. r -
c
Pf
-.. ?
fi ?.r- 7-
7?.!^.?
7 7 . S /J
f *.'?
li ,i . C /J
A. T ' s / ? .T r P
!, n n f • o 5 0 f'
. ^f-C'. fi'5
. n r- r 2 i.' *: 5
.rnr^c: = p
. C f 0 7 0 2 1
-, 003 7? J =
•.r n l B 6 7 ij
. r o i p 1 ? ?
-------
LABORATORY ANALYSIS OF ANDERSKN FILTIiRS
Run ID Filter
No.
Inlet #1 416
H
B
G
A
F
E
I
C
14
Stage
Pre-catch
1
2
3
4
5
6
7
8
Final
Tare
(gm)
0.257350
0.179775
0.166850
0.172800
0.170225
0.172750
0.168200
0.178075
0.168900
0.240525
WEIGHINGS
1st
(gm)
0.260050
0.179900
0.167275
0.173200
0.170475
0.174925
0. 170650
0. 182050
0.172825
0.249750
2nd
(gm)
0.260000
0.179775
0.166850
0.173180
0.170425
0.174825
0.170625
0.181925
0.172675
0.249650
Final
Weight
(gm)
0.260030
0.179838
0.167063
0.173190
0.170450
0.174875
0.170637
0.181988
0.172750
0.249700
Net
Ga in
(gm)
0.002680
0.000063
0.000213
0.000390
0.000225
0.002125
0.002437
0.003913
0.003850
0.009175
TOTAL
0.025071
Inlet ir-2
415
T
Y
S
W
R
X
U
V
18
Pre-catch
1
2
3
4
5
6
7
8
Final
0.
0.
0.
0.
0.
0.
0.
0.
0.
258700
173875
170325
179750
169850
178400
170025
175675
167825
0,246100
0.261750
0. 174800
0. 171425
0.181375
0. 17L825
0.182375
0.179400
0.187825
0.179250
0,260050.
0.261750
0.174800
0.171425
0. 181375
0.171825
0. 182375
0. L79AOO
0.187825
0.179250
0.260050
0.003050
0.000925
0.001100
0.001625
0.001975
0.003975
0.009375
.0.012150
0.011425
0.013950
TOTAL
0.059550
-------
LABORATORY ANALYSIS OF ANDliiUSiiN KILTERS (continued)
Run ID Filter Si: age
No.
Inlet #3 407 Pre-catch
25 1
67 2
26 3
66 4
27 5
65 6
28 7
68 8
424 Final
Tare
(gm) If
(*
0.230550
0.174425
0.171775
0.179475
0. 168400
0.176150
0.171100
0.173775
0.163850
0.255050
WEIGHINGS
si. 2nd
^in) (g"i)
0.242100
0. 174825
0. 172275
0.180225
0.169200
0. 177350
0. 172625
0. 175500
0.165375
0.261200
Final
We Lgh t
(gm)
0.242100
0.174825
0.1.72275
0.180225
0.169200
0. 177350
0.172625
0.175500
0.165375
0.261200
He t
Gain
(gm)
0.011550
0.000400
0.000500
0.000750
0.000800
0.001200
0.001525
0.001725
0.001525
0.006150
TOTAL
0.026125
Inlet
628
34
76
33
25
35
74
36
73
17
16
Pre-catch
1
2
3
4
5 .
6
7
8
Final
Final
0. 2 99 SO 0
0. 175950
0. 163400
0.181950
0.172350
0.179800
0.164200
0. 181200
0.170375
0.244450
0.24 400 0
0.305750
0. 176188
0. 163950
0. 182800
0. 173400
0. 182350
0. 170000
1). 187300
0. 176525
0.256800
0.244250
0.305650
0. 176050
0. 163950
0. 182750
0.173300
0. 181950
0.169925
0. 18V6UO
0. 176350
0.256650
0.244300
0.305700
0. 176119
0. 163950
0. 182775
0. 173350
0.182150
0. 1699.63
0. IH7450
0. 176438
O; 256725
0.244275
0.005900
0.000170
0.000550
0.000825
0.001000
0.002350
0.005763
0.006250
0.006063
0.012275
0.000275
TOTAL
0.041421
-------
LA110RATORY ANALYSIS OF ANDEKSl'N FILTI.'.KS (coat: inued)
Run ID
Outlet #1
Out: lei: #2
Filter
No.
409
38
78
37
79
39
80
40
77
427
408
24
61
23
62
21
63
22
64
413
414
Sr.age
Pre-cal'ch
1
2
3
4
5
6
7
8
Final
]' re -catch
1
2
3
4
5 ,
6
7
8
Final
Final
Tare
(gm)
0.230350
0.172825
0.169450
0.173050
0. 172000
0.178950
0.162325
0. 171300
0.169225
0.253700
0.231850
0.174550
0. 172175
0. J 74 5 50
0.162175
0.173225
0.160275
0. 179775
0. 167925
0.254600
0.253550
WEIGHINGS
1 s t 2 n J
(gm) ()','»)
0.230550
0.172975
0.169450
0.173050
0.172025
0.179150
0.162450
0. 171375
0. 169150
0.254600
0.233750
0. 175650
0. 173475
0. 175375
0.163175
0. 173675
0. 162050
0. 179775
0. 168L75
0.256550
0.256050
0.233700
0. 175900
0. L73725
0. 175650
0. 163275
0. 173850
0. 162050
0. 179900
0. 168375
0.256600.
0.256200
Final
VJeLghi:
(gm)
0.230550
0. 172975
0. L69450
0.173050
0.172025
0. L79150
0.162450
0. 171375
0. 169150
0.254600
TOTAL
0.233725
0. 175775
0. 173600
0. 175513
0. 163225
0. 173763
0. 162050
0. 179838
0. 168275
0.256575
0.256125
TOTAL
Net
Gain
(gm)
0.00020
0.00015
0.00000
0.00000
0.00003
0.00020
0.00013
0.00008
-0.00008
0.00090
0.00169
0.00188
0.00123
0.00143
0.00096
0.00105
0.00054
-0.00003
0.00006
0.00035
0.00198
0.00258
0.01206
-------
LABORATORY ANALYSIS OF ANDKRSI'iN FII.TKKS (coiir.iniii.-d)
Run ID Filter
No.
Our. lei: #3 614
J
N
K
0
L
P
M
Q
406
Stage
Pre-c'atch
I
2
3
4
5
6
7
8
Final
Tare
(gin)
0.287600
0.180300
0.172200
0.180150
0.170025
0.181725
0.169275
0.176200
0.170400
0.233400
WEIGHINGS
1st:
(gm)
0.287600
0.180600
0. 172475
0. 180575
0. 170025
0.181775
0.169700
0. 176850
0. 170800
0.234900
2nd
(gm)
0.287800
0. L80525
0.172550
0.180425
0.170125
0.181850
0.169800
0. 176900
0. 170850
0.235200
Final
We igh i:
(gm)
0.287700
0. 180414
0.172513
0.180500
0.170075
0. 181813
0.169750
0.176875
0. 170825
0.235050
TOTAL
Net
Gain
(gm)
0.00010
O.OOOU
0.0003L
0.00035
0.00005
0.00009
0.00048
0.00068
0,00043
0.00165
0.00425
-------
THREE-STAGE CYCLONE SAMPLER
LABO'RATORY PARTICULATE ANALYSIS
-------
LABORATORY ANALYSIS ON CYCLONE CATCH
Run
Inlet 1
Stage
1st
2nd
3rd
Filter 625
Filter 631
Tare
Weight
(nig)
0.000
0.080
0.080
137.425
134.200
Final
Weight
(rag)
12.380
4.130
6.280
157.600
135.750
Net
Gain
(rag)
12.380
4.050
6.200
20.175
1.550
Percentage
of. Total
(%)
27.9
9.1
14.0:
. 49,0
1st
2nd
3rd
Filter 664
Filter 656
0.080
0.210
0.180
134. '075
140.045
22.510
0.610
2.160
147.900
142.150
22.430
0.400
1.980
13.825
1.700
TOTAL 44.355
Inlet 2 1st 0.080 22.510 22.430 55.6
1.0
4.9'
38.5
TOTAL ' 40.33:
Inlet 3 1st 0.160 58.290 58.130 46.9'
2nd 0.250 2.160 1.910 l.,5
3rd 0.230 5.590- 5.360 4.3
Filter 693 138.600 139.425 0.825 47.2
Filter 694 138.275 195.900 57.625
TOTAL 123.850
Inlet 4 1st 0.150 14.800 • 14.650 22.. 1
2.8
11.7
6.3.4
TOTAL 66.410
1st
2nd
i •
j>ra
Filter 616
Filter 612
0.150
0.140
0.160
143.700
144.325
14.800
1.970
7.890
143.450
186.275
- 14.650
1.830
7.730
-0.250
41.950
-------
LABORATORY ANALYSIS ON CYCLONE CATCH (continued)
Run Stage
Outlet 1 1st
2nd
3rd
Filter 612
Filter 613
TOTAL
Outlet 2 1st
2nd
3rd
Filter 692
Filter 619
TOTAL
Outlet 3 1st
2nd
3rd
Filter 615
Filter 609
Tare
Weight
(rag)
0.000
0.027
0.058
141.975
138.300
0.058
0.107
0.082
141. '950
138.500
0.102
0.147
0.120
140.450
143.325
Final
Weight
(mg)
1.024
2.706
1.346
144.125
138.450
2.403
0.710
0.441
149.925
139.825
6.167
0.455
0.592
140.475
148.100
Net
Gain
(rag)
1.024
2.679
1.288
2.150
0.150
7.291
2.345
0.603
0.359
7.975
1.325
12.607
6.065
0.308
0.472
0.025
4.775
Percentage
of Total
CZ)
14.0
3;5.7
17,7
• 31.5
18.6
4.8
2.8
73.8
5-2.1
2.6
4,1
41.. 2
TOTAL
11.645
-------
POLYNUCLEAR AROMATIC HYDROCARBONS
LABORATORY ANALYSIS
-------
POLYNUCLEAR AROMATIC HYDROCARBON ANALYSIS
The outlet filters (#417, Method 5, Run
4; #692, Cyclone Run 2; #418, Method 5,
Run 7) were extracted with methylene
chloride and concentrated to one ml. A
gas chrornatograph with a flame ionization
detector with a Tenex-GC column was used
for the analysis. The sample contained
less than 1 yg (10~7 g) PNA as a-naphthyl
araine, and as such PNA was not detectable
on the gas chromatograph nor would it have
been on the GC/MS.
-------
CHLORINE/HYDROGEN CHLORIDE
LABORATORY ANALYSIS
-------
CHLORINE ANALYSIS
Run
1
1
2
2
3
3
4
4
5*
5*
Date Source
10/19/76 Inlet
Outlet
10/20/76 Inlet
Outlet
10/20/76 Inlet
Outlet
10/22/76 Inlet
Outlet
10/22/76 Inlet
Outlet
Aliquot Titrate
ml Iodine
1/4 sample 11.
12.
12.
12.
11.
12.
11.
12.
11.
12.
["Chlorine lilqu
55,
60,
u,
50,
80,
48,
66,
38,
60,
50,
i v a
11.
12.
12.
1.2.
1 I.
1.2.
11.
12.
11.
12.
1 e n i:
65
61
30
68
89
55
60
46
64
54
n _.
Total ml
Iodine
11.
12.
12.
12.
11.
12.
11.
12.
11.
12.
3.1559]
60
61
21
59
85
52
63
42
62
52
Blank ml
Iodine
12.
12.
12.
12.
12.
12.
12.
12.
12.
12.
64
64
64
64
64
64
64
64
64
64
Total mg
Ch lor ine
13.
0.
5.
0.
9.
I.
12.
2.
12.
1.
130
379
430
631
970
510
750
780
880
510
* Sampled 1 hour after "chlorine demagging"
•"" This value has already be-on multiplied by the F factor
-------
HYDROGEN CHLOKI.DK ANALYSIS
Run
1
I
2
2
3
3
4
4
5*
S ~'
Date Source
10/19/76 Inlet
Outlet
10/20/76 Inlet
Outlet:
10/20/76 Inlet
Outlet
10/22/76 Inlet
Outlet
10/22/76 Inlet:
Outlet
Aliquot ml AgNO3 ml Am.
Added Thio
back
1/4 sample 9.
9.
21 .
15.
25.
15.
25.
20.
25.
10.
00
00
00
00
00
00
00
00
00
00
8.01,
8.41,
16.20,
14.30,
20.52,
14.21,
15.2-5,
17.20,
21.19,
9.50,
8.05
8.55
16.85
14.20
20.56
14.31
15.39
17.32
21.22
9.52
Equ iva lent
Amount
AgNO3
8.
8.
17.
14.
21.
15.
16.
18.
22.
10.
45
92
38
99
61
00
12
16
31
00
Net ml**
AgNO3
2.
0.
14.
0.
13.
0.
35.
7.
10.
0.
20
32
48
04
56
00
32
36
76
00
Blank ml
AgNO3
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
Total mg
I1C1
0.765
O.llt
5.040
0.014
4.720
0.000
12.360
2.560
3.740
0.000
f'T" = 0.3478]
* Sampled 1 hour after "chlorine de-magging"
'*""' This value lins already been multiplied by the F Cacroi"
-------
SULFUR DIOXIDE/SULFUR TRIOXIDE
LABORATORY ANALYSIS
-------
SulLur Dioxide rmrl Suliui' Trioxi.di' Analysis
Run Uar.e
1 10/18/76
1
2 10/19/76
2
3 10/21/76
3
4 10/21/76
4
5 10/21/76
5
6 10/22/76
6
7 1.0/22/76
7
Source
In lee
Outlet:
Inlet:
Outlet
Inlet
Outlet
Inlet
Outlet-
Inlet
Outlet
Inlet
Outlet
Inlet;
Outlet
SULFUR DIOXIDE
Ali.quot Blank
(ml )
Entire Sample 0.00
0.00
11 0.00
" 0.00
0.00
0.00
11 . 0.00
0.00
0.00
" 0.00
0.00
" 0.00
0.00
" 0.00
Sample
(ml)
1.60
0.00
0.02
1.76
2.86
0.00
0.28
0.00
2.96
0.02
6.26
1.70
5.10
L. 78
SULFUR TRIOXIDE
Aliquot Blank
(ml)
Entire Sample 0.00
" 0.00
0.00
" 0.00
0.00
" 0.00
0.00
" 0.00
0.00
0.00
" 0.00
" 0.00
0.00
0.00
Sample
(ml)
0.08
0. 13
0.04
0.21
0. 14
0.00
0.10
0.04
0.5L
0.00
0.02
0.03
0.11
0.02
Normality - 0.0106
-------
ELEMENTAL ANALYSIS OF
BAGHOUSE HOPPER DUST
-------
TnO-CKERIICAL LABORATORY
DIVISION OF COOES PORCELAIN COMPANY
GOLDEK, COLORADO, U.S.A.... .„
303-279-6565 Ext: 3202
Mailing Address:
P.O. Box SOS -
Golden, Cciorsao 8?401
inp Inc.
Gcinesville, FL 32504
LABORATORY
NUMBER 27316-00
j DATE 12-7-76
j CUSTOMER-
! ORDER NO. £1')2
MATERIAL
I
SAMPLE
NUMBER
; ^ || ELEMENT • %
• 1 1
1 j j
n : > 10 j! Gallium (Go) ! 0.00?
i . . . Ij . I .
0.0;: jj Gcrmoniun-L (Ge" \ < 0-005
• i • '
1 < 0.01 .! Inck'rr. (\-\ \ < O.OOS
! i i
i 0.00r i Iron (re-) ! C ,2
• "' i I
"• i •
-'• : < ?.0'~1 JLcojJ-'Fb) ! 0.1
..'••. ."1 i'-'.csriesii-r. --'.--• : " . 1
iMcnrcrx-se i'.v.r. • '
• -• - : , " : ' ' - —
: ,, ._.. iJMercury (HEi |
'• '.
;: j.!, ;',..;! .' |'( : ';
: < :,.•::.. i^iobium <}^--
!:pi,s^r.=r^ •:?-. , .. ,.
ELEMENT
|
Silicon (St)
„_ . .
Stiver (Ag)
i . ....
Strontium (Sr)
Tin (Sn)
... — ....
Titanium (Ti)
Vcncdium (V)
i
Zinc (Zfi/
i
Zirconium (Zr)
Sodium (No)
irpei,,r) f(~O
1 wesi um t.^s;
LithiuT, (Li)
;Pcicss!urr. (K)
%
10
. _ „ . . . .
< 0.001
0.005
.... . ./ .
f^ .f --vr^
U . \J-J i
0 0^
< 0.005
^ .- -•-.
. . .-"•'• '~'-J .
0 . 01
..„..
•*- •- • • -•' . —
i --
ELEME.KT j fi
Rubidium (Rb) 0.005
».!..-. .1— .^ .1 - —
! . 1
Iao"3iiv.-.'.'!7rOi < 0.1
I
i
JTellur:>i.v.^-:"- < 0.05
i
Taoriu-.(^r/' < 0.1
i r^-.. ~ ~ ~ .' ' N--' -•- .' ~
\
i _. ' -. . -.
-^••\_--' '-•- • . ' .' ^~ .••_.
i
f", ., . -*.... ' .- - • ^- " ' • ~:
«-' . - - -..--.
'
Les s than
Greater then
I I Atomic Absc-rpi
Q Opiicoi EmisL;
I I iV'et Chemisrr\
D X-Ray
,;-?.c wp^" Jne conditions that ii is net to be reproduced
•it •:'. v c- • ; ••', > r. ^ c r o • h c f p u r p o L v t £ v o i cur £ i g n c t u r e 6 r~Trr
.'; UT . i >'i i f f'i C U t 5j pO C I C I p fe TfTl! *. i i O P. I .': V,1 r I 1 I fl Q . D 1
CL'SIOMER
Frank B. Scruveilzer, Manager
-------
DIVISIOH OF COORS PORCELAIN COMPANY
GOLDEN, COLORADO, U.S.A.-
303-279-6565 Ext. 3202
Mailing Address:
P.O. Box 500
Golden, Colorado 80401
Science and Engineeringf Inc.
LABORATORY
NUMBER 27316-00
DATE 12-7-76
CUSTOMER
ORDER NO.
2152
Result
jJrbiu-i(Sr 5
<. O.(
< 0.005
< 0.005
< 0,05
< 0.01
< 0.01
-:ez u;-*n J^e condition *> the: :i is no: r^ be reproojcec
, tc,".••:! sing 01 C'r.sf p-jrpc.;c-: ovtr OUT signature or in
i.cm- without speciui f.e[rr.i tsior, in v.-!hir,o.
l&EOPJJOSV
"FrEnk E. Scfrr>:eitse f,^^-^.ev"
-------
COMPOSITION OF TESISORB
-------
TESISORB as supplied by Teller Environmental Systems, Inc.
Silicon as SiC>2 ~ 61%
Aluminum as A1203 - 23.3%
Calcium as CaO - 0.7%
Sodium as Na20 - 9.8%
Potassium as ^0 - 4.6%
Magnesium as MgO - Trace
Iron as F^o^S ~ Trace
Titanium as Ti02 - Trace
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