United States Industrial Environmental Research EPA-600/7-79-156
Environmental Protection Laboratory July 1979
Agency Research Triangle Park NC 27711
Process Measurement
Procedures:
Emissions
Interagency
Energy/Environment
R&D Program Report
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the INTERAGENCY ENERGY-ENVIRONMENT
RESEARCH AND DEVELOPMENT series. Reports in this series result from the
effort funded under the 17-agency Federal Energy/Environment Research and
Development Program. These studies relate to EPA's mission to protect the public
health and welfare from adverse effects of pollutants associated with energy sys-
tems. The goal of the Program is to assure the rapid development of domestic
energy supplies in an environmentally-compatible manner by providing the nec-
essary environmental data and control technology. Investigations include analy-
ses of the transport of energy-related pollutants and their health and ecological
effects; assessments of, and development of, control technologies for energy
systems; and integrated assessments of a wide range of energy-related environ-
mental issues.
EPA REVIEW NOTICE
This report has been reviewed by the participating Federal Agencies, and approved
for publication. Approval does not signify that the contents necessarily reflect
the views and policies of the Government, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/7-79-156
July 1979
Process Measurement Procedures
Emissions
by
R. Maddalone and N. Garner
TRW Defense and Space Systems Group
One Space Park
Redondo Beach, California 90278
Contract No. 68-02-2165
Task No. 202
Program Element No. INE624
EPA Project Officer: Robert M. Statnick
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, NC 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
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ACKNOWLEDGMENT
The work was originally conducted under the FPA Project Officer
Dr. R. M. Statnick, Environmental Research Center, Research Triangle Park,
North Carolina. The current EPA project officer is fir. Frank Briden.
Dr. C. A. Flegal was the Program Manager and the Task Order Manager was
Dr. R. F. Maddalone. The laboratory tests during the development of these
procedures were done by Mr. Morton L. Kraft, Mr. David R. Moore and
Mr. Maynard D. Cole. We wish to thank Mr. Steve Newton of the TVA and
Mr. Ray Grote of the EPA for their review of the document. The overall
review and support, during the field test program, from Mr. Richard G.
Rhudy of EPRI, and fir. Steven Newton and fir. John Lawton of the TVA
has been greatly appreciated.
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CONTENTS page
ACKNOWLEDGEMENT. . ii
TABLES & FIGURES IV
1. INTRODUCTION 1
2. EQUIPMENT AND MATERIALS 3
2.1 Sampling Materials 3
2.2 Reagents and Apparatus for H?SO. 5
3. REQUIREMENTS 9
3.1 System Design 9
3.2 Sampling 9
3.3 Handling of Glassware 12
3.4 Calibration and Maintenance 12
3.5 Cleanliness 12
3.6 Safety 12
4. PROCEDURE 13
4.1 Probe Manufacture 13
4.2 Filter Holder Fabrication 17
4.3 Site Equipment Set-Up and Operation 19
4.4 Analysis Procedures 22
5. DATA MONITORING PROCEDURES 29
5.1 Acid Base Titration 29
5.2 Data Monitoring by Statistical Quality Control 30
6. MAINTENANCE SCHEDULES 32
7. TROUBLESHOOTING AND REPAIR PROCEDURES 35
8. REFERENCES 40
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TABLES
Page
1. Critical Checkpoints for Controlled Condensation H?SO.
Sampling System 14
2. General Maintenance Schedule 33
3. Troubleshooting and Repair 36
FIGURES
1. Vycor Sampling Liner 4
2. Controlled Condensation Coil (CCC) 6
3. Controlled Condensation System Set-Up 10
4. Expected Coefficient of Variance (CV) of the HpSCL Measurement
Based on the Number of Samples Taken 11
5. Controlled Condensation System Probe Design 16
6. Quartz Filter Holder 18
7. Controlled Condensation Field Data Sheet 21
8. Controlled Condensation Coil Rinsing Apparatus 23
9. Laboratory Data Sheet 25
10. Statistical Quality Control Chart for Contamination
Measurements 31
IV
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1. INTRODUCTION
This manual has been prepared for the Industrial and Environmental
Research Laboratory of the Environmental Protection Agency, Research Tri-
angle Park, North Carolina, as part of Task 13 of Contract No. 68-02-2165.
The technical objective of this task was to develop a stack sampling
procedure for the measurement of the mass emission rate of sulfur trioxide
(H?SO. vapor) within a precision of ±10 percent, but not to exceed a pre-
cision of ±20 percent. The method chosen on the basis of previous expe-
rience (Task 02 of this program) was the Controlled Condensation System
(CCS).
The Controlled Condensation System (CCS) is designed to measure the
vapor phase concentration of SOo as H^SO. in controlled or uncontrolled
flue gas streams. This method is specifically designed to operate at tem-
peratures up to 250°C (500°F) with 3000 ppm S09, 8-16 percent H90, and up
3
to 9 g/m (4 gr/cf) of particulate matter.
By using a modified Graham condenser, the gas is cooled to the acid
dew point at which the SO- (hLSO. vapor) condenses. The temperature of
the gas is kept above the water dew point to prevent an interference from
SOp while a heated quartz filter system removes particulate matter. The
condensed acid is then titrated with 0.02 N NaOH using Bromophenol Blue as
the indicator.
The CCS was evaluated under simulated stack conditions in the labora-
tory. This test program had three phases:
• Test the efficiency of the CCS under varying concentrations
and mixtures of HgSO^ S02, 02, H20, and C02 with and without
fly ash present on the filter.
• Evaluate the CCS versus the EPA H^SO. methods.
• Test the CCS inlet and outlet of an ESP at a coal-fired utility.
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As a result of this test program these facts were learned about CCS:
t The average laboratory coefficient of variance was ±6 percent.
t Fly ash at the level of 0.3 g on the surface of the filter
can reduce the amount of 1^04 recovered by 12 percent when a
10 ppm gas stream of ^804 is passed through the system.
. o
• Extensive field evaluation under high (11 g/m ) mass loading
and high S02 (4000 ppm) concentrations showed that as little
as 0.1 ppm of H2S04 can be detected.
• The coefficient of variance for the percentage removal of
H2S04 by wet scrubbers at a coal-fired utility was found to
be ±18 percent. This value compares well with the ±11 percent
for the estimated field accuracy.
• Oxidation of SO? at the recommended filter holder temperatures,
4000 ppm SOp and 8 percent 02 did not occur. When fly ash from
a coal-fired utility was placed on the filter, it did not have
a catalytic effect under those conditions.
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2. EQUIPMENT AND MATERIALS
The following sections list the materials required to fabricate
duplicate CCS's.
2.1 SAMPLING MATERIALS
2.1.1 Probe Construction Materials. (Note: These materials are for a
91 cm (3-foot) probe. Longer probes can be made by increasing the dimen-
sions presented).
• Three Vycor tubes 1.3 cm (0.5 in.) OD x 91 cm (36 in.) with a
18/9 female ball-and-socket joint placed on one end (special
order, A. H. Thomas or Ace Glass, see Figure 1).
• Three glass insulated heating tapes - 1/2 inch x 72 inch; 288 watts
(Fisher Sci. Co., No. 11-463-50C or equivalent).
• Three 33 inch x 1 inch OD x 0.065 inch wall 304 SS tubes used as
probe sheaths.
• One dozen silicone rubber No. 6 stoppers (A. H. Thomas, No. 8747-
E65).
• Glass tape (Scotch glass-fiber electrical tape).
• Four Omega (Stanford, Conn.) shielded thermocouples (I/C),
(TJ36-ICSS-18G-12) with 8-foot lead.
• Four Omega (Stanford, Conn.) unshielded thermocouples (I/C),
(IRCO-032 with 8-foot lead).
• Six Omega male connectors (ST-ICRO-M).
• Two six-foot heavy-duty (^ 20A) electrical cords.
• Four 1-1/2 inch hose clamps.
• Two square yards of asbestos cloth (VWR, Atlanta, Georgia,
No. 10930-009).
• Three adaptors for connecting hoses (Ace Glass, No. 5216-23).
• Two Teflon Swagelok Unions (T-810-6).
2.1.2 Train Components
• Two pumps capable of pulling 1 cfm of free air.
• Two bath controller-circulators (A. H. Thomas, No. 9840-B15 or
equivalent).
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1.3 cm
T
THERMOCOUPLE WELL
46 cm
91 cm
18/9
THERMO-
COUPLE
WELL
Figure 1. Vycor sampling liner.
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• Fifty feet of 1/2 inch x 1/4 inch rubber tubing (A. H. Thomas,
No. 9544-R57).
• Controlled Condensation Coils (CCC) — Three Graham condensers are
modified to hold an enclosed 60 mm medium frit (Figure 2).
• Two insulated chests capable of holding a two-gallon bucket.
• Three glass insulated heating tapes, 3/8 inch x 24 inch, 96 watts
(A. H. Thomas, No. 5954-H22 or equivalent).
t Four autotransformers, variable, 10 amp. (A. H. Thomas, No. 9461-
D10 or equivalent).
• One hundred Tissuequartz filters, 37 mm diameter (Pallflex Corp.,
Kennedy Drive, Putnam, Conn. 06260).
§ Eight pinch clamps (A. H. Thomas, No. 2841-21 or equivalent).
• Six Greenburg-Smith type impingers or equivalent.
• Sodium Carbonate, technical grade.
t Indicating silica gel (10 Ibs).
• Stopcock grease (Ace Glass Co., No. 8229-10).
• Two three-inch bushings with a 1-1/8 inch hole drilled in the
center.
• Two RdF digital temperature indicators-series-2000 with iron/con-
stantan sensors.
• Two vacuum gauges (A. H. Thomas, No. 5654-B10).
• Two 0 to 100 ml/min flowmeters (Fisher Scientific Co., No. 11-164-
50 or equivalent).
• Two Glass-Col heating mantles for filter system (Glass-Col, 711
Hulman St., Terre Haute, Ind., special order to fit filter holder).
t Two quartz filter holders (see Section 4.2 for design fabrication).
2.2 REAGENTS AND APPARATUS FOR H2S04 TITRATION
t Carbon dioxide-free distilled water - Prepare all stock and standard
solutions, and dilution water for standardization procedure, using
distilled water which has a pH of not less than 6.0. If the water
has a lower pH, it should be freshly boiled for 15 minutes and
cooled to room temperature.
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CTl
THERMOCOUPLE
WELL
18/9
3 CM-
60 MM MEDIUM
FRIT
18/9
THERMOCOUPLE
WELL
4.0 CM-
23.8 CM
-4 CM-
GAS
FLOW
Figure 2. Controlled condensation coil (CCC).
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NOTE
Deionized water may be substituted for distilled water provided
that it has a conductance of less than 2 micro-ohms/cm and a pH
greater than 6.0.
f NaOH pellets — Reagent grade.
• Stock 1.0 N NaOH - Dissolve 40 g of reagent grade NaOH in 1 liter
of COp free distilled water. Store in a Pyrex glass container with
a tignt-fitting rubber stopper.
• 0.0200 N NaOH - Dilute 20 ml of 1 N NaOH with OL free distilled
water to 1 liter. Store in a tightly rubber stoppered Pyrex glass
bottle protected from atmospheric (XL by a soda lime tube. For
best results, prepare daily. This solution will be standardized
against potassium biphtalate (see Section 4.4.2).
t Potassium biphthalate (KHCoH^O,) -Anhydrous, reagent grade.
t 0.0200 N potassium biphthalate (KHP) solution - Dissolve 4.085 g
of dry (110°C for 1 hour) KHP into 1 liter of (XL free distilled
water.
NOTE
The normality of the KHP solution equals (wt. KHP)/204.2.
• Anhydrous ethyl alcohol — U.S. P. or equivalent.
§ Phenolphthalein indicator solution — Dissolve 0.05 g of reagent
grade phenol phthalein in 50 ml ethyl alcohol and dilute to 100 ml
with C02 free water.
• Bromophenol Blue indicator solution — Dissolve 0.1 g in 7.5 ml of
0.02 N NaOH. Dilute to 250 ml with C02-free distilled water.
• Ten milliliter micro-buret, Kimble 17132F (A. H. Thomas, No.
1993-M-30 or equivalent).
• Desiccator (A. H. Thomas, No. 3751-H10 with cover and plate to fit)
• Drierite desiccant -5 Ibs. Drierite (A. H. Thomas, No. C288-T49).
§ Four Erlenmeyer flasks with 28/15 ball-and-socket joint, 125 ml
(Ace Glass Co., Louisville, Ky., No. 6975 or equivalent).
• Four stoppers for 28/15 ball-and-socket joint (Ace Glass Co.,
No. 8263-08 or equivalent).
• Four 50 ml volumetric flasks.
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Dowex 50W-X8 cation exchange resin 20 to 50 mesh.
Barium perch]orate trihydrate.
0.01 f1 Ba(C10J2.3 H20 - Transfer approximately 3.9 g of reagent
grade barium perchlorate trihydrate into a one-liter reagent bottle.
Add enough D.I. HpO to dissolve the salt and then dilute to the mark.
Sulfonazo III Solution, 0.1 percent W/V -Transfer 0.025 g of
Sulfonazo III into a 25-ml bottle, add water to dissolve the
indicator and fill to the mark.
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3. REQUIREMENTS
3.1 SYSTEM DESIGN
The SOo (HpSO. vapor) Controlled Condensation System (CCS) consists
of a heated Vycor probe, a modified Graham condenser (condensation coil),
impingers, a pump and a dry test meter (see Figure 3).
3.2 SAMPLING
Since a gas or a small aerosol is being sampled, no traverse will
be performed in the stack. It can be shown (Reference 7) that the aver-
age degree of stratification in the duct is ±15 percent of the mean con-
centration. Because of the large fluctuation in source emission rates
(±65 percent), elimination of the error due to stratification will not
significantly improve the sampling accuracy. For these reasons, the
sample probe will be positioned at the center of the duct or stack.
It is possible to predict the expected variance in the average H?SO.
value. The sampling variance of an estimated average of I^SCL determined
from a sample of D days and H samples per day is given by:
x D H
9 9
where OQ is the variance between days and o^ is the variance per sample
within a day. Converting this equation to terms of the coefficient of
variation (CV) we have:
cv2
From previous experience for a coal-fired utility, the CVU was determined
rl
to be ±32.4 percent and CVn was determined to be ±57.9 percent. Using these
values, Figure 4 is generated from equation 2. Thus, if it is desired to
estimate the average H^SO, within 20 percent, a sampling plan of five days
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RUBBER VACUUM
HOSE
ADAPTER FOR CONNECTING HOSE
TC WELL
STACK
ASBESTOS CLOTH
INSULATION
GLASS-COL
HEATING
MANTLE
RECIRCULATOR
THERMOMETER
DRY TEST
METER
THREE WAY
VALVE
SILICA GEL
Figure 3. Controlled Condensation System Set-up.
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•"fr
o
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with five samples per day, or six days with two samples per day, or seven
days with one sample per day is required.
3.3 HANDLING OF GLASSWARE
Because of the corrosive nature of SCL (HLSCL vapor), only Vycor and
Pyrex glassware are used. Severe mechanical shocks are to be avoided,
especially when the probe is heated to 316°C (600°F). Never place any
strain on glass ball joints. Clean the ball joints of grease and dirt
after each run.
3.4 CALIBRATION AND MAINTENANCE
After each run the probe, connecting lines, controlled condensation
coil, filter holder, and impinger system must be cleaned. The probe and
connecting lines can be cleaned with a long-handle test tube brush and
backflushed with high pressure air. If particulate matter adheres to the
inside of the probe, rinse with D.I. water followed by acetone (or
isopropyl alcohol). The impinger system is flushed out and the proper
solvents are then replaced in the impinger bottles prior to the next run.
The filter holder is inspected and cleaned before the next run and the
filter pad is replaced. See Sections 6.0 and 7.0 for the recommended
schedule of maintenance and troubleshooting activities.
3.5 CLEANLINESS
Contamination of the condensation coil rinse solutions must be avoided
to prevent neutralization of the hLSO^. Keep the rinse solutions in a
covered flask.
3.6 SAFETY
OSHA safety requirements with regard to working environment and opera-
tor safety must be met at all times. The reagents mentioned in the proce-
dure are not extremely toxic, but misuse of any chemicals can be harmful.
12
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4. PROCEDURE
This section contains the necessary information to build, set-up, and
operate the CCS. Table 1 is a checklist of critical items giving an over-
view of the procedure. These critical items consist of:
• Recommended flowrates, temperatures and sampling times
t Reminders on laboratory and sampling techniques
• Specific equipment checks
While this list is provided for review prior to the sampling run, its
best use is as an on-site checklist for the supervisor and quality assurance
personnel during the run. During a test audit the supervisor or QA repre-
sentative should initial each item successfully completed, and the entire
list should be included with the documentation of that test run. The oper-
ating personnel should also have copies of the checklist for reference dur-
ing the execution of the test run. Copies can be posted in the laboratory
and sampling site for this purpose.
4.1 PROBE MANUFACTURE (Refer to Figure 5)
The necessary equipment is listed in Section 2.1.1. Follow correct
electrical safety procedures at all times. Be sure that no sharp pieces of
metal abrade any of the electrical wires.
a) Cut the 304 SS one-inch tubing into 32-inch lengths.
b) Align the shielded thermocouple (TC) as shown in Figure 5. Using
the glass tape, secure the shielded thermocouple to the Vycor probe. Place
the unshielded thermocouple in the thermocouple well and secure with the
glass tape. Continue down the probe, securing both thermocouple leads
simultaneously against the tube.
NOTE
Be careful never to kink the thermocouple or thermocouple
leads.
cj Take the 72-inch glass heating tape and fold it in half.
d) Beginning 5 inches from the probe tip, wrap the probe with the glass
heating tape. Make sure the heating tape is snugly up to the probe and
secured every 6 inches with a wrapping of glass tape. Wrap the coils close
13
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TABLE 1. CRITICAL CHECKPOINTS FOR CONTROLLED CONDENSATION
H2S04 SAMPLING SYSTEM
Checkpoint
Initials
Supervisor QA Inspector
Remarks
I. Laboratory Preparation
- Inspect and clean CCC. Both filter holder and CCC are
cleaned with hot chromic acid solution and D.I. FUO.
- Rinse with acetone and air dry CCC.
- Place Tissuequartz filter in filter housing.
- Check seal between end of joint and filter.
- Do not use grease on joints.
- Inspect and clean all glass joints.
II. Site Setup
- Rinse the inside of probe prior to run.
- Rinse probe with acetone until rinse solution is clear.
- Perform leak test.
- Leak rate must be less than 80 ml/min (0.003 cfni).
- Thermocouple leads attached to probe and filter.
- CCC water bath held at 60°C (140°F) il°C.
- Leak test train.
- Probe temperature maintained at 316°C (600°F) !17°C.
- Gas temperature out of filter holder held at 288°C (550°F).
- Fresh solutions placed in impingers.
- Fresh absorbent replaced in final impinger.
- Adjust flowrate in system to 8 1pm.
III. Sampling Run
- Turn vacuum pump on just before inserting probe in the stack.
- Check seal between probe and port to prevent any outside air
from entering the stack.
- Run test for 1 hour or until coils are frosted to 1/2 or
2/3 of their length.
- After run cap both ends of the probe and lay in horizontal
position.
- Rinse the CCC coils into the modified Erlenmeyer flask with a
maximum of 40 ml of D.I. H20.
- Has any of the solution lost ( ml estimated)?
- Handle hot glassware carefully to prevent personnel injury
and damage to equipment.
- After probe has cooled, the probe is rinsed with a maximum
of 40 ml. D.I. H20 into a 125 ml Erlenmeyer.
(continued)
14
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TABLE 1. (continued)
Checkpoint
- Was any solution lost ( ml estimated)?
- Clean support equipment prior to next run.
- Save filter for titration.
IV. Laboratory Analysis
- Clean glassware prior to titration.
- Use Bromphenol Blue indicator.
- Is the NaOH buret protected with a CO,, absorbent tube?
- When was NaOH standardized last (Date )?
- Filter any solution that has suspended particulate.
- Use same number of indicator drops for each titration.
- Perform indicator blank on a volume of D.I. H20 equal to
sample aliquot used.
- Indicator blank added to HpSO. milli-equivalents found.
- Perform all analyses in triplicate.
V. Data Analysis Verification
- Obtain and titrate test samples from main laboratory.
Initials
Supervisor
QA Inspector
Remarks
15
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PROBE T.C.
18/9
SILICONE
STOPPER
ASBESTOS
CLOTH WRAP
cr>
SILICONE
STOPPER
VYCOR TUBE
TEFLON UNION
6 MM
HEATING TAPE
SHIELDED
T.C.
GLASS HEATING
TAPE LEAD
STACK
T.C.
(?) STOPPERS SHOULD BE AWAY FROM HEATING TAPE
(T) ASBESTOS COVER SHOWS SLIGHT OVERLAP
Figure 5. Controlled condensation system probe design.
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enough so that the heating wire is completely used up 2 inches from the
ball joint. Secure the end of the heating tape with a final wrap.
e) Bore a 9/16-inch hole into two No. 6 silicone rubber stoppers, then
cut a slit vertically down one side of the stopper into the 9/16-inch hole.
The slit will allow easy assembly.
f) Cut a piece of asbestos cloth approximately 30 inches long and wide
enough to wrap the probe and heating tape with a 1/2 turn overlap. Tightly
wrap the probe and secure the asbestos cloth with glass tape.
g) Slide the 304 SS sheath over the Vycor probe. Avoid scratching the
insulation on the electrical leads. Position the sheath so that the end
near the tip extends one inch past the start of the heating tape.
h) Spread the stopper open, slip it over the tip of the probe, and
slide it into the 304 SS sheath. The stopper is then wired to help hold
it in place. Repeat this procedure for the other end, only use a hose
clamp to hold the back stopper in place.
i) Place the male quick connects on the end of the TC leads. The red
TC lead goes to the negative terminal.
j) The probe should be tested in the laboratory to ensure that all
parts are in order. Simply connect the heating wire to the Variac and
allow the probe to heat up. Monitor the temperature to verify the TCs are
functioning.
NOTE
Whenever heating up the probe, start off with very low
power inputs (^5 percent) until heating starts.
k) The 0.25-inch nozzle and Teflon union (Figure 5) are attached prior
to the test run. The nozzle consists of a 0.5-inch diameter quartz tube
tapered to 0.25-inch at one end and a 90° bend placed in the center of its
2.5-inch length.
4.2 FILTER HOLDER FABRICATION
Figure 6 details the recommended design for the quartz filter holder.
This filter holder consists of a modified 40/50 standard taper quartz joint.
The modifications included adding a coarse quartz frit and an extension tube
17
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18/9
BALL
SPRING
ATTACHMENT
HOOKS
TISSUE QUARTZ
FILTER
18/9
SOCKET
00
THERMOCOUPLE
WELL
STANDARD
TAPER QUARTZ
40/50
SEAL
EXTENTION
TO STD.
TAPER JOINT
EXTRA COARSE
QUARTZ FRIT
Figure 6. Quartz filter holder.
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to the male joint to act as a pressure seal when the Tissuequartz filter
pad is in place. Ball-and-socket (18/9) joints are used to connect the
filter holder to the probe and controlled condensation coil.
NOTE
Be sure the extension tube seals on the Tissuequartz filter.
If there is not a tight seal, carefully cut a washer out of
a spare Tissuequartz filter to make a seal. Do not use two
filters.
4.3 SITE EQUIPMENT SETUP AND OPERATION
a) In the 3-inch port, insert a 3-inch plug with 1-inch hole.
b) Use a table or another suitable device to support the CCS (see
Figure 3).
c) Prior to use, be sure the controlled condensation coil (CCC) is
clean and dry. Carry the CCC to the site with each end stoppered. If any
condensation appears because of temperature changes, connect the CCC to the
water bath and start the circulation of the 60°C (140°F) water. This should
evaporate any premature condensate.
d) With the probe still out of the stack, assemble the train as shown
in Figure 3. Be sure that each ball joint is completely clean and free of
dust. Because of the possibility that the greases will freeze at the tem-
peratures employed, it is not recommended that any grease be used. Proper
care of the ground glass fittings will ensure that vacuum seals are main-
tained. Should any ground glass fitting not seal vacuum-tight, a small
amount of Apiezon H grease may be used for emergency repair. As soon as
it is possible, the joint in question should be returned to the glass shop
for regrinding (see Tables 2 and 3 for further suggestions).
e) Connect the flowmeter to the vacuum pump exit. Be sure that the
flowmeter is vertical. Close off the end of the probe with a stopper, turn
on the vacuum pump and adjust the vacuum to read 380 torr (15 in. Hg).
f) Begin measuring the flowrate with the flowmeter. If the leak rate
is less than 80 ml/min (0.003 cfm), then the system is ready for use. If a
leak rate greater than 80 ml/min is found, the system should be checked for
loose joints and connections. The pump should also be checked and any worn
parts replaced. See Tables 2 and 3 for corrective action.
19
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g) Once the vacuum test is completed, slowly turn the three-way valve
to the vent position and allow the air to bleed into the system. This
must be done carefully to prevent a pressure surge from backing up the
impingers. Remove the flowmeter from the system and unstopper the probe.
h) Begin heating the probe and the filter holder to 316°C (600°F) and
288°C (550°F), respectively. The heating bath should already be at 60°C
(140°F). Once the skin temperatures reach these values, the run can
commence.
NOTE
During the course of the run, the filter temperature will
be controlled by the gas out temperature which should be
288°C (550°F).
i) After leak testing, the pump is again turned on and the flowrate
adjusted to 10 1pm (0.33 cfm) using the dry test meter and a stopwatch.
The pump is turned off without readjusting the valve settings.
j) Pinch the hose at the end of the controlled condensation coil and
insert the heated probe into the duct with the nozzle pointed downstream.
NOTE
The downstream orientation of the probe nozzle will reduce
the gross amount of particulate collected in the probe and
filter section. Sulfuric acid aerosols should not be dis-
criminated against because of their extremely small size,
which allows them to follow the flow lines into the nozzle.
k) Turn on the pump, release the pinched hose, and obtain an initial
dry gas meter reading. Throughout the run, collect the data required (see
Figure 7).
1) Sample for one hour or until 1/2 to 2/3 of the length of the coils
are frosted with HoSO..
NOTE
If the coil is operating properly, the ^04 will cover
the inside of the coils as a thin gray-white film. If
large drops of a clear liquid form and begin to block
the coil, then moisture is being condensed. Either the
percentage moisture has exceeded 16 percent or the tem-
perature of the water bath has dropped below 60°C. Abort
the run and check the water bath temperature with an Hg
20
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Sample Location_
Run #
Run Date/Time_
Operator
Flowrate (cfm)
Ambient Pressure (P)
AEROSOL SOs
(CONTROLLED CONDENSATION)
FIELD DATA SHEET
Reheater Air Flow Rate, acfm_
Inlet Gas Rate, acfm
Sample Location S02 (ppm]_
Boiler Load (mw)
Leak Rate
Time (Min)
AVG.
Temperature (°F)
Stack
Probe
Filter
Skin
Out
Recirc.
Water
Exit
Coil
Dry Gas
Meter
In
Out
Gas Meter
Reading,
cu. ft.
Figure 7. Controlled condensation field data sheet.
21
-------
thermometer and confirm the percentage moisture in the
gas stream. If the water bath is below 60°C, recalibrate
the temperature bath control. For every percent above
16 percent h^O, adjust the CCC temperature 2°C upward.
Clean and dry the CCC, and replace the reagents in the
impingers prior to restarting the run.
m) At the end of the sampling period, remove the probe from the duct
and slowly shut off the pump. After the pressure drops, remove the CCC
from the system without removing the water bath hoses. Carefully connect
the G/R coil (Figure 8) to the Erlenmeyer flask without spilling any con-
densate in the tube. In 10 ml increments (up to 30 ml), use D.I. water to
rinse out the CCC. Be careful to avoid introducing any dust or grease into
the rinse solution. Take the rinse solution in the stoppered Erlenmeyer to
the laboratory, dilute to 50 ml with ^-free water prior to analysis.
NOTE
Multiple rinses are recommended to ensure a quantitative
wash of the coil.
n) Rinse the probe with 30 to 40 ml of D.I. H^O after it has cooled.
Take this solution back to the laboratory, and filter it through a Whatman
number 1 filter into a 50 ml volumetric. Dilute this solution to 50 ml
with COp-free water.
CAUTION
Wait until the filter has cooled before proceeding.
o) Remove the filter and any debris from the filter holder and place
it into a beaker. Add 30 ml of D.I. H^O and swirl the beaker. Filter the
solution through a Whatman number 1 filter into a 50 ml volumetric. Repeat
with 10 ml portions of D.I. HLO until the volumetric is filled to the mark.
4.4 ANALYSIS PROCEDURES
Two procedures can be used to determine the amount of H-SO* collected:
1) An acid/base titration using Bromophenol Blue indicator or
2) A sulfate titration using Sulfonazo III as the indicator.
Since the end points for titrations are very color dependent, the end
point will probably vary slightly for each operator's sense of color. To
22
-------
PIPET BULB
ADAPTER
SOLUTION
POSITIONING
DRAIN
STOPCOCK VALVE
125 ML ERLENMEYER FLASK
D.I.
FROM COIL
Figure 8. Controlled condensation coil rinsing apparatus.
23
-------
obtain the most accurate data, the following techniques should be employed
in all titrations:
• Always add the same number of drops of indicator.
t Have the same operator do the blank and sample.
• Always titrate to the same color intensity.
• Avoid parallax errors - keep eyes at the same level as
the liquid meniscus and hold a white piece of paper
behind it with a dark line horizontal to the table top.
• Remove air bubbles from buret tip prior to use.
• Never store reagent in buret. Always rinse out buret
with a slight amount of titrant.
• Always record titrant type and volume used.
Because of the simplicity and sensitivity of the acid/base titration, it is
the recommended procedure. The sulfate procedure is included in this sec-
tion to act as a backup or total sulfate method if the need arises. In
either case all the titrations should be done in triplicate and the results
recorded on the laboratory data sheet (Figure 9).
4.4.1 Sulfate Titration Using Sulfonazo III. (References)
1) Hash the Dowex 50 W-X8 cation exchange resin with 10 percent
V/V HC1 . Fill a 1/2-inch I.D. ion exchange column to a
3-inch bed depth and place glass wool pads at the bottom
and top of the bed. Rinse the column with deionized water
until the elutant tests neutral with pH paper.
2) Transfer 0.025g of chemically pure Sulfonazo III indicator
[(NaS02)2 C10 H2 (OH)21 (N:NC§ H4S03H)2 to a 25 mi-bottle,
add water to dissolve the indicator, and fill to the mark.
3) Transfer approximately 3.90 q of reagent grade barium per-
chlorate trihydrate [BatClO.lL.SHpO] into a one-liter
reagent bottle, add a small amount of distilled water to
dissolve the salts, and then fill to the mark. Mix the
contents of the bottle.
4) Standardize the Ba^lO.K by titrating sodium sulfate. Dry
the iJa9SO» in an oven for two hours at 125°C and allow to
cool t& room temperature in a desiccator. Weight out accu-
rately in triplicate 12 to 16 mg of the Na2S04 from a weigh-
ing bottle into 125 ml Erlenmeyer flasks, dissolve with 10 ml
deionized water, add 10 ml acetone and three drops Sulfonazo
III indicator solution, and titrate with the barium perchlorate.
24
-------
AEROSOL S03
(CONTROLLED CONDENSATION)
LABORATORY DATA SHEET
Run #
Sample Location
Run Date/Time_
Analyst
Date Lab Analysis Completed
Variable
Value
Aliquot Size (A)
Normality of titrant (N)
ml of titrant used to titrate G/R coil
rinses (v)
Blank (equivalent NaOH)
Net titration volume (V)
Absolute dry gas meter temperature (Tm)
Volume of gas sampled (Vm)
Meter Pressure (P )
ppm HpSO. (vol/vol)
(ml)
(eq./O
(ml)
(ml)
(ml)
Avg. (ml)
(ml)
(ml)
(°R)
(ft3)
(in. Hg)
Normality of acid used to titrate blank
(if used)
Figure 9. Laboratory data sheet.
25
-------
5) Repeat this procedure in triplicate for the sample and blank
(D.I. H20):
M =
(142) (V-va)
Where: M = Molarity of the barium perchlorate solution,
moles/liter
W = Weight of sodium sulfate titrated, mg
V = Average volume of barium perchlorate solution
required for titration of sodium sulfate, ml
v3 = Average volume of D.I. water blank titration.
a
6) Take a 10 ml aliquot of the rinse solution and pass it through
the ion exchange column at 3 ml/min. Rinse the column with
30 ml deionized water and collect the elutant and rinsings in
a 50-ml volumetric flask and dilute to the mark with deionized
water.
7) After every tenth use of the column, regenerate it with 100 ml
of 10 percent W/V HC1 at 3 ml/min flowrate and rinse until the
elutant tests neutral to pH paper. Rinse the column with 50 ml
of D.I. water.
8) Add 10 ml acetone and three drops of the Sulfonazo III indicator
to a 10 ml aliquot of the ion exchange elutant.
9) Titrate with 0.01 M Ba(C104)2 using a magnetic stirrer and back
lighting. The color will change from purple to blue. The end
point is the point at which an additional drop of titrant does
not change the color of the solution. The end point should not
fade unless left standing for more than 5 to 10 minutes. Record
the volume of 0.01 M Ba(C10»)~ used to reach the end point and
calculate the average titration volume. Titrate a 10 ml aliqout
of D.I. water in the same fashion to obtain the titration blank.
4.4.2 Acid/Base Titration
The preferred method of analysis is the acid/base titration using
Bromophenol Blue indicator. Carefully handle and store the samples in clean
glassware and analyze them as soon as possible. Record all results on the
laboratory data sheet.
26
-------
Each acid/base indicator in this procedure will change color over a
different pH range. For example:
Indicator pH Range Color Change
Bromphenol Blue 3.0 to 4.6 yellow to blue
Phenolphthalein 8.2 to 10.0 colorless to pink
The point measured by the indicator is simply the point at which the
color change occurs. The actual end point where exactly the right amount
of acid and base have reacted (equivalence point) can be close to or far
away from the indicator end point. Thus Bromophenol Blue is chosen for the
NaOH/H2S04 titration, since the equivalence point occurs at about pH 3.
Phenolphthalein is used for the KHP/NaOH standardization titration because
the equivalence point is near pH 7.
Even though the indicators have been selected to be as close as pos-
sible to the actual end point, a small difference still exists and is
called the indicator blank. The indicator blank for phenolphthalein is
the amount of NaOH required to change a specific amount of water contain-
ing a known number of drops of phenolphthalein pink. This value is sub-
tracted from the milliliters used to titrate the sample.
The indicator blank from Bromophenol Blue is determined in the same
way (known volume and number of drops) except that a standard acid (H2$OJ
is used to backtitrate the indicator in distilled water to a yellow color.
The number of milliequivalents used is added to the amount found titrating
the sample.
NOTE
Blanks can vary with sample size and number of drops
of indicator; therefore determine the indicator blank
under the same conditions in which the sample is
titrated.
The procedures for standardization and sample analysis follow:
1) Pipet 10 ml of the 0.0200 N KHP solution into a 125 ml wide-
mouth Erlenmeyer flask.
2) Add 3 drops of the Phenolphthalein indicator. With a swirling
action of the flask, titrate with 0.02 N NaOH solution until the
first pink color stays. Record the volume and repeat from (1)
in triplicate. Repeat this procedure using D.I. H^O (blank).
27
-------
3) Average the volume used to titrate the KPH solution. The
true normality of the standard NaOH solution equals:
(0.0200) (10 ml)
N =
(ml titrant - ml blank)
4) To titrate the H?SO, in the condensation coil, probe, and
filter rinses, piper 10 ml of one of these solutions into
a 125-ml Erlenmeyer flask.
5) Add 3 drops of the Bromophenol Blue indicator to the solution
and titrate to the blue end point with standard NaOH. Trip-
licate analyses should be performed as well as an indicator
blank during the blank test titration. (See Paragraph 4.4.2).
Remember this Bromophenol Blue sample blank is added to the
sample value.
4.4.3 Calculation of the H^SO. ppm (v/v) Concentration
Using either the sulfate or acid base titration, the concentration of
SO- as H?SO, in the flue gas stream can be calculated.
Note: The formula is based on a 50 ml original sample volume.
1) From the Field Data Sheet (Figure 7) obtain the average dry
test meter temperature, volume of gas sampled and the pressure
at the meter box. Record these values on the Laboratory Data
Sheet. (Figure 9).
2) Using the Laboratory Data Sheet, insert the correct numbers into
the following formula
/NVT \
for acid/base titration: ppm H2SO. = 1,201.9 1 ... p I
\ m m/
for sulfate titration: ppm H?SO, = 12,019
The result is ppm (v/v) H2S04 at 70°F and 29-92 in Hg.
Note: This value can be 12 percent low due to fly ash present
on the filter (See Introduction).
28
-------
5. DATA MONITORING PROCEDURES
The data monitoring procedures for the CCS are devoted mainly to the
acid-base titration performed in the laboratory and to the monitoring of
the H2S04 ppm values calculated.
5.1 ACID BASE TITRATION
In order to check the accuracy of the titrations performed on the CCS
samples, an independent check of the NaOH solution and titration method is
required. An unknown standard sample of f^SO, approximately 0.01 N should
be analyzed by the lab personnel every couple of weeks. Analysis of the
sample should be in triplicate and reported to 3 places (O.X Y I). Analy-
sis of this sample will provide information on the precision of the CCS
titrations and accuracy of the results.
The procedure follows:
1) Take a 10 ml aliquot of the unknown standard.
2) Titrate in triplicate with Bromophenol Blue to the blue
end point and record the number of millilHers used.
3) Determine the normality of the solution from:
Vfl
where: N. = Normality of the acid
V. = Volume acid aliquot taken (ml)
NB = Normality of the base
VB = Volume of the base used to titrate the sample (ml)
The results of the determination should not differ by more than ±10
percent within the triplicate numbers nor should the determined normality
be off by more than ±10 percent.
29
-------
If the values differ by more than 10 percent:
• Check the calculations and be sure the correct values
have been used.
• Repeat the analysis.
• If the value is still off, restandardize the NaOH with KHP.
• Repeat the test.
5.2 DATA MONITORING BY STATISTICAL QUALITY CONTROL
In many cases where inlet and outlet information in h^SO* values are
measured, it was possible to monitor the SO., results by plotting the inlet
and outlet S03 values. Since there is a direct correlation between outlet
and inlet concentrations, a simple control chart using regression analysis
can be used (Figure 10) to evaluate the data. The area between the 2 and
3a limits is the warning zone. A point falling in this area indicates
that the measurement system may be out of control. The region between the
-2a and +2a limits should contain, in the long run, 95 percent of all
future paired measurements. The region between the -3o and the +3a limits
should, essentially, contain all future paired measurements of inlet and
outlet contamination. A point falling outside of the 3o limits indicates
that the measurement system is out of control.
The a limits should be based on a "large sample", say >30, of paired
measurements. If, for a particular environmental situation, the sample
size is less than 30, interim charts will be established using tolerance
limits. Thus, the warning limits will be the (90,90) limits. That is,
it is expected that 90 percent of the future observations will lie within
such limits, 90 percent of the time. The rejection limits, or the limits
that indicate that the system is out of control will be the (90,95) limits.
That is, it is expected that 95 percent of the future observations will be
within these limits 95 percent of the time. At all times:
t Check with the power plant of the scrubber control room to find
out if any mechanical problems occurred during the run.
• Verify that all the laboratory numbers are correct and
repeat the analysis if solution is left over.
30
-------
re
s-
o>
(J
c.
o
d)
CO
+30 limit
+2
-------
6. MAINTENANCE SCHEDULES
Table 2 details the recommended maintenance schedule. Following this
schedule is imperative to prevent breakdown and to maintain the high accu-
racy required in the program.
32
-------
TABLE 2. GENERAL MAINTENANCE SCHEDULE
Component
Maintenance Schedule By:
Run
Week
Month
Calibration Procedure
Probe nozzles
Quartz probe
Impingers
oo
GO
Pump
Swage!ok fittings
CCS filter holder
CCC
NaOH solution
Inspect nozzle for damage.
Brush nozzle before and
after run to remove inside
particulate.
Before and after each run
brush and rinse with rea-
gent grade acetone or
Freon then D.I. ^0 until
the rinse is clean.
Rinse out after each run
with D.I. water.
Inspect and clean seal
area and 0-rings.
Leak test before each run.
Before each run check leak
rate in pumping system.
Inspect fitting, espe-
cially ferrule and seat
for wear and dirt. Clean
or replace fitting as
required.
Inspect and clean after
each run. Replace filter
after each run.
Inspect and clean after
each run
Inspect vanes on diaphragm.
Inspect and clean motor
brushes.
Clean frit each week
in hot chromic acid
for 12 hours. Rinse to
neutral pH with D.I. H20.
Clean coils and frit each
week in hot chromic acid
for 12 hours. Rinse to
neutral pH with D.I. H20.
Standardize the stock NaOH
with KHP weekly.
Measure nozzle ID with micrometer.
N/A
N/A
Leak test at 380 torr (15" Hg)
and verify that a leak rate of
<80 ml (0.003 cfm) is maintained.
Total leak rate in system at
380 torr (15" Hg) must be less
than 80 ml/min (0.003 cfm).
N/A
N/A
N/A
(Continued)
-------
TABLE 2. (continued)
Component
Maintenance Schedule By:
Run
Week
Month
Calibration Procedure
Thermocouples
Temperature
Indicator
OJ
-p.
Connecting
lines
Inspect lines for wear and
kinks.
Clean readout of all dust.
Clean tips of shielded TCs.
Clean connector prongs
with steel wool.
Dry test meter
Blow out connecting lines
with air.
Visually inspect exterior
for wear. Especially
inspect hose to fitting
connections.
Clean exterior.
Flush with water and dry
with clean plant air.
Calibrate thermocouples.
Have electronics shop
remove the back and clean
the inside of the unit.
Check indicated tempera-
ture with calibrated
thermocouple.
Calibrate versus wet test
meter every 3 months.
Calibrate TC at two points (ice-
water and near boiling). Compare
TC readings to mercury thermometer.
Replace TC if agreement is not
within 3°C (6°F).
Perform thermocouple calibration
with readout unit using indepen-
dently calibrated thermocouple.
Check indicated temperature read-
ings with calibrated thermocouple.
N/A
Run wet and dry test meters in
series; note temperature and
pressure. If dry test meter is
>3% off, send to factory for
recallbration.
-------
7. TROUBLESHOOTING AND REPAIR PROCEDURES
Table 3 lists possible problems that can be encountered with the
equipment used in the test program. This list should be updated by the
field personnel as new problems are encountered and solved.
35
-------
TABLE 3. TROUBLESHOOTING AND REPAIR
Component
General Remarks
Problem
Repair Sequence
S-Pitot Nozzles
Probe Nozzles
CO
en
Quartz Probes
Impingers
Alignment of pitot tubes is critical.
The tubes must be facing 180° with
respect to each other and parallel
to gas flow in the duct.
A smooth circular edge is required
for accurate sampling. Alignment
of nozzle face must be perpendicular
to gas flow.
Avoid mechanical shocks especially
when probe is hot. Before cleaning
probe with liquids, allow the probe
to cool to air temperature.
Impingers, should be cleaned with soap
and water. Deposits should not be
allowed to build up inside impinger.
All nozzles should reach to within
±1.3 cm (0.5") of the bottom of the
impinger. To ensure good seals,
keep the impinger seals clean.
Misaligned nozzle
Damaged edge
Nozzle wear or damage
Misalignment
Normal wear and cleanliness
Normal wear and cleanliness
Leakage in impinger system
Return S-Pitot tubes to original 180°
alignment.
Align nozzles to be parallel to gas
flow.
Position face of nozzle to be perpen-
dicular to gas flow.
File and buff edge to smooth oval -
repeat alignment checks.
Loosen Swagelok fitting and realign
(x-axis) nozzle face to perpendicular
to gas flow.
Bend nozzle neck (y-axis) so that
nozzle face is perpendicular to gas
flow.
Brush and rinse with acetone after
each run (Note: Test brush tc ensure
it is not dissolved by the acetone).
Rinse out with D.I. water after each use.
Dry impinger to be used for moisture
trap.
Clean sealing edges.
Check all Swagelok fittings.
Inspect impinger seal area for dirt or
damage. Clean area if dirt found.
Use larger 0-ring.
If all other measures fail to locate leak,
pressurize and immerse in water to find
leak.
(continued)
-------
TABLE 3. (continued)
Component
General Remarks
Problem
Repair Sequence
Thermocouples
Temperature
Indicator
GO
Mantle or probe
Connecting lines
Pump
Thermocouple (TC) leads and wire are
fragile and require care in arranging
the equipment set-up to prevent kink-
ing and stripping of leads. Never
pull a TC apart by pulling on the
lead. Verify that the polarity is
not reversed anywhere in the system.
Be sure that the same type of TC
wire and connectors are used in the
system (Iron-constantan or chromel-
alumel). Do not bend casing of
shielded thermocuople.
Store in dust-free area.
Never exceed maximum temperature as
stated in the manufacturer's manual.
While these lines are either heavy
vacuum hose or steel-braided Teflon
lines, care should be taken to mini-
mize weight supported by the lines
and excessive mechanical abuse.
Care must be taken in shutting the
pump off after a run. Rapid shut-
down without bleeding air into the
pumping system will cause the
impingers to back up toward the
filter.
Temperature- indicator fluctuat-
ing over wide range
Temperature readings fluctuat-
ing on one channel
No temperature readout or fluc-
tuating temperatures on all the
channels with thermocouples
attached
No temperature rise with current
on
General maintenance
Leakage (oil-free)
Locate possible short in TC wire or con-
nectors. Once portion of wire with short
is located, mark and have the wire
replaced.
Have readout checked by electrical
shop if no external short can be found.
Check thermocouple for short in lead or
connectors.
Return to electronic shop for repair.
Return to manufacturer if problem cannot
be found.
Check electrical connections.
Check main power.
Check fuses and circuit breakers.
Verify thermocouple connected.
Replace any worn or corroded parts.
Check all valve and hosing connections
leading to pump.
If the leakage has been isolated in the
pump, disassemble pump and inspect vanes
for wear and replace if necessary.
(continued)
-------
TABLE 3. (continued)
Component
General Remarks
Problem
Repair Sequence
Pump
(Continued)
Leakage (diaphragm)
Swagelok fittings
Swagelok fittings are designed to seal
with a minimum of tightening. Exces-
sive torque applied to the fitting
will eventually cause leakage.
Installation
OJ
CO
Reinstallation
For leakage or low flow in diaphragm
pumps check the diaphragm cover to ensure
it has not vibrated loose.
Remove face plate and inspect diaphragm for
signs of wear or pinholes. Check the dia-
phragm gasket for wear; replace if
necessary.
Insert the tubing in the service.
Insert the tubing into the Swagelok tube
fitting. Make sure that the tubing rests
firmly on the shoulder of the fitting and
that the nut is finger-tight.
Due to the variation of tubing diameters,
a common starting point is desirable.
Therefore, use a wrench to snug up the
nut until the tubing will not turn (by
hand) in the fitting. 'At this point,
scribe the nut and body at the 6 o'clock
position of the fitting. Now while hold-
ing the fitting body steady with a backup
wrench, tighten the nut one-and-one
quarter turns. Watching the scribe mark,
make one complete revolution and continue
to the 9:00 o'clock position.
Tubing with preswaged ferrules inserted
into the fitting until front ferrule
seats in fitting. Tighten nut by hand.
Rotate nut about one-quarter turn with
wrench (or to original one-and-one
quarter tight position), then snug
slightly with wrench.
(continued)
-------
TABLE 3. (continued)
Component
General Remarks
Problem
Repair Sequence
Dry Test Meter
CCS filter
oo
10
ccc
These meters are very sensitive to
mechanical shock and should be handled
with care. Corrosive gas from the
stack should never be passed through
the meter without prescrubbing.
The 6/R filter holder is made out of
quartz and especially when it is hot,
mechanical shocks will cause break-
age. The filter holder is designed
to always be run with a filter on the
quartz frit. Because of the high
temperatures employed, greasing the
joints is not recommended.
The coil is an especially delicate
piece of equipment. Clear visibility
of the coils is necessary to main-
tain the water jacket's cleanliness.
Incorrect volume readings
No seal to filter
Gas leakage
Plugged frit
Gas leakage
Check meter for blockage.
Check mechanical linkage for wear.
Recalibrate meter.
Check extension tube. If it is not mak-
ing a seal, have the glass blower repair.
As a temporary repair, a washer out of
Tissuequartz can be used to promote a
seal.
Check thermocouple well for pinhole leak.
Check alignment of ball-and-socket joints.
Try to maintain linearity.
Check seal at joints, clean joints, and
retest.
Check joints for thermal warping. Replace.
Soak in hot chromic acid cleaning bath for
12 hours. Rinse with D.I. H20 till
neutral.
Check thermocouple well for pinhole leak.
Check alignment of ball-and-socket joints.
Try to maintain linearity.
Check seal at joints, clean joint, and
retest.
Check joints for thermal warping. Replace.
Soak in hot chromic acid cleaning bath for
12 hours. Rinse with D.I. H2<3 till
neutral.
-------
8. REFERENCES
1. Federal Register, Volume 41, No. Ill, pages 23061-23063.
2. Goksoyr, H. and K. Ross, J. Inst. Fuels, 35, 177 (1962).
3. Lisle, F.S. and J.D. Sensenbaugh, Combustion, 1, 12 (1965).
A. Nacovsky, W., Combustion, J, 35 (1967).
5. Standard Methods for the Examination of Water and Wastewater,
13th Ed., pages 52-56 (1971).
6. Maddalone R., C. Zee, and A. Grant, "Procedure for Titrimetric
Determination of Sulfate Using Sulfonazo III Indicator," TRW
Systems, EPA Contract No. 68-02-1412, Task 6, February 14, 1975.
7. E.F. Brooks and R.L. Williams, "Technical Manual for Process
Stream Volumetric Flow Measurement and Gas Sample Extraction
Methodology," TRW System, EPA Contract 68-02-1412, Task 13,
November 1975.
40
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/7-79-156
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Process Measurement Procedures: H2SO4 Emissions
5. REPORT DATE
July 1979
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
R. Maddalone and N. Garner
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
TRW Defense and Space Systems Group
One Space Park
Redondo Beach, California 90278
10. PROGRAM ELEMENT NO.
INE624
11. CONTRACT/GRANT NO.
68-02-2165, Task 202
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final; 6/76 - 2/77
14. SPONSORING AGENCY CODE
EPA/600/13
15. SUPPLEMENTARY NOTES EPA project officer R.M.Statnick is no longer with IERL-RTP;
for details, contact F.E.Briden, Mail Drop 62, 919/541-2557.
16. ABSTRACT Tne report gives procedures to measure H2SO4 vapor or aerosols in con-
trolled or uncontrolled flue gas streams. The method was designed to operate at
temperatures up to 250 C with 3000 ppm SO2, 8-16% H2SO4, and up to 9 g/cu m of
particulate matter. The basis of the method is the clean separation of particulate
matter, H2SO4 vapor, and SO2. A heated (>250 C) quartz filter system removes
the particulate matter, but passes most of the H2SO4 vapor to a modified Graham
condenser. There the gas is cooled to about 62 C to condense and collect the H2SO4
vapor while passing the SO2 and H2O vapor. The condensed acid is titrated with
either NaOH using bromophenol blue indicator or Ba(ClO4)2 using Sulfonazo HI as
the indicator. The laboratory coefficient of variance is + or - 6% and the estimated
field accuracy is + or - 11%. Flyash on the filter was shown to reduce the recovery
of H2SO4 by 12% at the 10 ppm H2SO4 level. Field experiments showed that as little
as 0.1 ppm H2SO4 could be detected.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
c. COS AT I Field/Group
Pollution
Sulfuric Acid
Vapors
Aerosols
Sulfur Dioxide
Dust
Flue Gases
Pollution Control
Stationary Sources
Particulate
13B
07B
07D
11G
2 IB
3. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
45
20. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
41
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