TRW DOCUMENT NO.
                          28055-6004-RU-OO
PROCESS MEASUREMENT
      PROCEDURES

 SULFURIC ACID

     EMISSIONS
         February 1977
           Prepared for


  INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
     OFFICE OF RESEARCH AND DEVELOPMENT
     ENVIRONMENTAL PROTECTION AGENCY
  RESEARCH TRIANGLE PARK, NORTH CAROLINA 27711
        CONTRACT NO. 68-02-2165
         TASK NUMBER 13
           TRW
      OM6 SPACE PARK • REQOINOO BEACH •

-------
                         TRW DOCUMENT NO.
                           28055-6004-RU-OO
                         6OOR77O1O
PROCESS MEASUREMENT
      PROCEDURES

 SULFURIC ACID
     EMISSIONS
          February 1977
           Prepared for

  INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
     OFFICE OF RESEARCH AND DEVELOPMENT
     ENVIRONMENTAL PROTECTION AGENCY
  RESEARCH TRIANGLE PARK, NORTH CAROLINA 27711
        CONTRACT NO. 68-02-2165
          TASK NUMBER 13
            TRW
          DEFENSE AND SPACl SYSTEMS GROUP
      ONE SPACE PARK • REOONOO BEACM • CALIFORNIA

-------
       PROCESS MEASUREMENT PROCEDURES

          SULFURIC ACID EMISSIONS
                February 1977
              By:  R.  Maddalone
                   N.  Garner
EPA Project Officer:   Dr. Robert M.  Statnick
                Prepared for
Industrial Environmental Research Laboratory
     Office of Research and Development
       Environmental  Protection Agency
     Research Triangle Park, N. C.   27711

           Contract No. 68-02-2165

                 Task No. 13
                      Approved by:
                                   R.' F. Maddalone
                                   Task Order Manager
                      Approved by:
                                   C. A. Flegal^J
                                   Program Manager

-------
                              ACKNOWLEDGMENT

      This document describes the procedures developed on Task 13, Under-
standing S03 Data on EPA Contract No. 68-02-2165, Sampling and Analysis of
"Reduced" and "Oxidized" Species in Process Streams.  The Chemistry and
Materials Laboratory Applied Technology Division was responsible for the
work performed on this task.  The work was conducted under the EPA Project
Officer Dr. R. M. Statnick, Environmental Research Center, Research Triangle
Park, North Carolina.  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.  I 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 Bechtel, and Mr. Steven Newton and Mr. John
Lawton of the TVA has been greatly appreciated.

-------
                                 CONTENTS
                                                                      Pac
ACKNOWLEDGMENT 	      ii
INTRODUCTION 	       1
1.0  SCOPE	       2
     1.1  Documents	       2
     1.2  Equipment and Materials  	       2
          1.2.1  Sampling Materials  	       2
          1.2.2  Reagents and Apparatus for H,,S04 Titration  ...       6
     1.3  Requirements 	       8
          1.3.1  System Design 	       8
          1.3.2  Sampling	       8
          1.3.3  Handling of Glassware	      12
          1.3.4  Calibration and Maintenance 	      12
          1.3.5  Cleanliness	      12
          1.3.6  Safety	      12
     1.4  Procedure	      14
          1.4.1  Probe Manufacture 	      14
          1.4.2  Filter Holder Fabrication 	      17
          1.4.3  Site Equipment Setup and Operation	      17
          1.4.4  Analysis Procedures 	      23
     1.5  Data Monitoring Procedures	      27
          1.5.1  Acid Base Titration	      28
          1.5.2  Data Monitoring by Statistical  Quality Control   .      29
     1.6  Maintenance Schedules  	      29
     1.7  Troubleshooting and Repair Procedures   	      29
                                    m

-------
                                INTRODUCTION
      This manual has been prepared for the Industrial and Environmental
Research Laboratory of the Environmental Protection Agency, Research Triangle
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
(HpSO. vapor) within a precision of +10%, but not to exceed a precision of
+20%.  The method chosen on the basis of previous experience (Task 02 of
this program) was the Controlled Condensation System (CCS).  A test program
was then established to evaluate the CCS under simulated stack conditions.
      The project test program had three phases:
           •  Test the efficiency of the CCS under varying concentrations
              and mixtures of ^$04, S02, 02, H20, and COp with and with-
              out fly ash present on the filter.
           •  Evaluate the CCS versus the EPA HgSO^ methods.
           t  Test the CCS inlet and outlet of an ESP at a coal-fired
              utility.
      As a result of this test program these facts were ]earned about CCS:
           •  The average laboratory coefficient of variance was +6%
           •  Fly ash at the level of 0.3 g on the surface of the filter
              can reduce the amount of H2S04 recovered by 12% when 10 ppm
              gas stream of ^504 is passed through the system.
           •  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 HUSO* can be detected.
           t  The coefficient of variance for the percentage removal of
              H2S04 by wet scrubbers at a coal-fired utility was found to
              be +_18%.  This value compares well with the +11% for the
              estimated field accuracy.
           •  Oxidation of S02 at the recommended filter holder temperatures,
              4000 ppm S02 and 8% 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.
      As a result of this intensive laboratory and field test program, we
feel that this H2SO. measurement system offers the best method available to
monitor FSO- emissions from combustion sources.

-------
                                 1.   SCOPE

     The Controlled Condensation System (CCS) is designed to measure the
vapor phase concentration of SO, as  HUSO,  in controlled or uncontrolled
flue gas streams.  This method is specifically designed to operate at temper-
atures up to 250°C (500°F) with 3000 ppm S0?, 8-16 percent H?0, and up to
     -                                     <-                t-
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 S03 (H-SO. vapor) condenses.  The temperature of the
gas is kept above the water dew point to prevent an interference from S02
while a heated quartz filter system removes particulate matter.  The con-
densed acid is then titrated with 0.02 N NaOH using Bromphenol  Blue as the
indicator.
1.1  DOCUMENTS
        1-1     Federal Register, Volume 41, No. Ill, pages 23061-23063.
        1-2     Goksoyr, H. and K. Ross, J. Inst. Fuels, 35, 177 (1962).
        1-3     Lisle, F.S. and J.D. Sensenbaugh, Combustion. 1, 12 (1965).
        1-4     Nacovsky, W., Combustion,  1. 35 (1967).
        1-5     Standard Methods for the Examination of Water and Waste-
                 water,  13th  Ed.,  pages 52-56 (1971).
        1-6     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.
        1-7     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.
1.2  EQUIPMENT AND MATERIALS
     The following sections list the materials required to fabricate dup-
licate CCS's.
1.2.1  Sampling Materials
1.2.1.1  Probe construction materials.  (Note:  These materials are for a
3-foot probe.  Longer probes can be made for increasing the dimensions
presented.)

-------
        1)  Three Vycor tubes 0.5 inch OD x 36 inch with a 18/9 female ball-
            and-socket joint placed on one end (special  order, A.  H.  Thomas
            or Ace Glass, see Figure 1).
        2)  Three glass insulated heating tapes - 1/2 inch x 72 inch; 288
            watts (Fisher Sci.  Co., No.  11-463-50C or equivalent).
        3)  Three 33 inch x 1 inch OD x 0.065 inch wall  304 SS tubes  used
            as :probe sheaths.
        4)  One dozen silicone  rubber No. 6 stoppers (A.H. Thomas, No.
            8747-E65).
        5)  Glasstape (Scotch glassfiber electrical tape).
        6)  Four Omega (Stanford, Conn.)  shielded thermocouples (I/C),
            (TJ36-ICSS-18G-12)  with 8-foot lead.
        7)  Four Omega (Stanford, Conn.)  unshielded thermocouples  (I/C),
            (IRCO-032 with 8-foot lead).
        8)  Six Omega male connectors (ST-ICRO-M).
                                    i
        9)  Two six-foot heavy  duty ( - 20A) electrical  cords.
       10)  Four 1-1/2 inch hose clamps.
       11)  Two square yards of asbestos  cloth (VWR, Atlanta,  Georgia,
            No. 10930-009).
       12)  Three adaptors for  connecting hoses (Ace Glass, No. 5216-23).
       13)  Two Teflon Swagelok Union (T-810-6).
1.2.1.2  Two pumps capable of pulling 1  cfm of free air (Brink impactor
pump may be used).
1.2.1.3  Two bath controller-circulators  (A.H. Thomas,  No. 9840-B15 or
equivalent).
1.2.1.4  Fifty feet of 1/2 inch x 1/4 inch rubber tubing (A.H. Thomas,
No. 9544-R57).
1.2.1.5  Three Graham condensors (Controlled Condensation Coils -  CCC)
modified to hold an enclosed 60 mm medium frit (special  order  from Ace
Glass, Louisville, Ky., see Figure 2).
1.2.1.6  Two insulated chests capable of holding  a two-gallon  bucket.

-------
                        THERMOCOUPLE WELL
0.5"
T
                                                                18"
                                           36"
18/9
THERMO-
COUPLE
WELL
                                    Figure  1.   Vycor sampling liner.

-------
en
       THERMOCOUPLE
           WELL
        18/9
      3 CM-
               60 MM MEDIUM
                  FRIT
                                                                                                   18/9
                                        THERMOCOUPLE
                                            WELL
«•	 4.0 CM-
23.8 CM
-4CM-
                                     Figure  2.   Controlled condensation coil.

-------
1.2.1.7 Three glass insulated heating tapes,  3/8  inch  x  24 inch,  96  watts
(A.H.  Thomas, No.  5954-H22 or equivalent).
1.2.1.8  Four autotransformers,  variable,  10  amp.  (A.H.  Thomas,  No.
9461-D10 or equivalent).
1.2.1.9  One hundred Tissuequartz filters, 37 mm  diameter (PalIflex  Corp.,
Kennedy Drive, Putnam, Conn.  06260).
1.2.1.10  Eight pinch clamps  (A.H.  Thomas, No. 2841-21 or equivalent).
1.2.1.11  Six Greenburg-Smith type impingers  or equivalent.
1.2.1.12  Sodium Carbonate, technical grade.
1.2.1.13  Indicating silica gel  (1C) Ib).
1.2.1.14  Stopcock grease (Ace Glass  Co.,  No. 8229-10).
1.2.1.15  Two three-inch  bushings with a 1-1/8 inch hole drilled in  the
center.
1.2.1.16  Two RdF digital temperature indicators-series-2000 with iron/
constantan sensors.
1.2.1.17  Two vacuum gauges (A.H. Thomas,No.  5654-B10).
1.2.1.18  Two 0 to 100 ml/min flowmeters (Fisher  Scientific  Co.,  No.
11-164-50 or equivalent).
1.2.1.19  Two Glass-Col heating  mantles for filter system (Glass-Col, 711
Hulman St., Terre Haute,   Ind., special  order  to fit filter holder).
1.2.1.20  Two quartz filter holders (see Section  1.4.2 for design
fabrication).
1.2.2  Reagents and Apparatus for H2S04 Titration
1.2.2.1  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.
                                   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.

-------
1.2.2.2  NaOH pellets - Reagent grade.
1.2.2.3  Stock 1.0 N NaOH - Dissolve 40 g of reagent grade NaOH in 1  liter
of C02 free distilled water.  Store in a pyrex glass container with a tight-
fitting rubber stopper.
1.2.2.4  0.0200 N NaOH - Dilute 20 ml of 1 N NaOH with C02 free distilled
water to 1 liter.  Store in a tightly rubber stoppered pyrex glass bottle
protected from atmospheric C02 by a soda lime tube.  For best results, pre-
pare daily.  This solution will be standardized against potassium biphthalate
(see Section 1.4.3.2).
1.2.2.5  Potassium biphthalate (KHCgH^)-Anhydrous - Reagent grade.
1.2.2.6  0.0200 N potassium biphthalate (KHP) solution - Dissolve 4.085 g
of dry (110°C for 1 hour) KHP into 1 liter of C02 free distilled water.
                                   NOTE
          The normality of the KHP solution equals (wt. KHP)/204.2.
1.2.2.7  Anhydrous ethyl alcohol - U.S.P. or equivalent.
1.2.2.8   Phenolphthalein indicator solution  - Dissolve  0.05 g of reagent
grade phenolphthalein in 50 ml ethyl alcohol and dilute to 100 ml with
COp free water.
1.2.2.9  Bromphenol 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.
1.2.2.10  Ten milliliter micro-buret, Kimble 17132F  (A.H. Thomas, No.
1993-M-30 or equivalent).
1.2.2.11  Desiccator (A.H. Thomas, No. 3751-H10 with cover and plate to fit).
1.2.2.12  Drierite desiccant - 5 Ib. Drierite (A. H. Thomas, No. C288-T49).
1.2.2.13  Four Erlenmeyer flasks with 28/15 ball-and-socket joint, 125 ml
(Ace Glass Co., Louisville, Ky., No. 6975 or equivalent).
1.2.2.14  Four stoppers for 28/15 ball-and-socket joint (Ace Glass Co.,
No. 8263-08 or equivalent).
1.2.2.15  Four 50 ml volumetric flasks.
1.2.2.16  Dowex 50W-X8 cation exchange resin 20 to 50 mesh.

-------
1.2.2.17  Barium perchlorate trihydrate.
1.2.2.18  0.01  N Ba(C104)2 - Transfer approximately 3.9 g of reagent grade
barium perchlorate trihydrate into a one  liter reagent bottle.   Add enough
D.I. H20 to dissolve the salt and then dilute to the mark.
1.2.2.19  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.
1.3  REQUIREMENTS
1.3.1  System Design
     The SO- (HUSO, 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).
1.3.2  Sampling
     Since a gas, or a small aerosol is being sampled, no traverse
will be performed in the stack.  It can be shown (Reference 1-7) that the
average degree of stratification in the duct is £15 percent of the mean
concentration.   Because of the large fluctuation in source emission rates
(-50 percent),  elimination of the error due to stratification will not
significantly improve the sampling accuracy.  Thus, 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 hLSO,  determined
from a sample of D days and H samples per day is given by:
                                    2      2
                             2     aD  .   °H                          m
                            a-  -  T  +  DH                          (1)
                             /\
        2                                    2
where o-   is the variance between days and
-------
                                                                                       RUBBER VACUUM
                                                                                          HOSE
STACK
             ADAPTER FOR CONNECTING HOSE

                              TC WELL
           GLASS-COL
           HEATING
           MANTLE
                       ASBESTOS CLOTH
                        INSULATION
DRY TEST
METER
                                                                                                    [REE WAY
                                                                                                    VALVE
                                                   STYROFOAM
                                                   ICE CHEST
                            Figure  3.   Controlled  condensation system setup.

-------
TABLE 1.    CRITICAL  CHECKPOINTS  FOR  G/R  H2$04 SAMPLING  SYSTEM
           Checkpoint
                                                    Initials
                                            Supervisor
                                                                   QA  Inspector
                                                                                       Remarks
I.   Laboratory Preparation
        Inspect and  clean G/R coil.  Both fil-
    1    ter holder and G/R are cleaned with
        hot chromic  acid solution and D.I.  H-0
    -   Rinse with acetone and air dry G/R
        coil.
    -   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 0.003 cfm
        or 30 ml/inin.
    -   Zero Magnehelic gauges.
    -   Thermocouple leads attached  to probe
        and filter.
    -   G/R water bath held at 140°F  (+2°F)
    -   Leak test train.
        Probe temperature maintained  at  600 F
        (+30°F).
    -   Gas temperature out of
        held at 5bO°F (+10°F)
    -   Fresh solutions placed in impingers.
    -   Fresh absorbarit replaced in  final
        impinger.
    -   Adjust flowrate in system to  8 1pm.
Ill. Sampling Run
        Turn vacuum  pump on just before  insert-
        ing probe in the stack.
    -   Check seal between probe and  port to
        prevent any  outside air entering the
        stack.
    -   Run test for 1 hour or until  coils are
        frosted to 1/2 to 2/3 of their length.
    -   After run cap both ends of the probe
        and lay in horizontal position.
    -   Rinse the G/R coil into the modified
        Erlenmeyer flask with a maximum  of
        40 ml of D.I.  H20.
    -   Was any of the solution lost  (    ml
        estimated)?
        Handle hot glassware carefully to
        prevent personnel injury and  damage
        to equipment.
                  of filter holder
                                                                                       (continued)
                                             10

-------
                                          TABLE  1.    (continued)
                   Checkpoint
                                                              Initials
                                                     Supervi sor
                                                                     QA Inspector-
                                                                                                  Remarks
     -   After probe has cooled, the probe  is
        rinsed with a maximum of 40 ml.   O.I.
        H-0  into a 125 ml Erlenmeyer.

     -   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  liromphenol Blue indicator.

        Is the HaOH buret protected with a
        C02  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. H.O equal to sample aliquot
        used.    i
     -   Indicator blank added to H-SCL milli-
        equivalents found.
     -   Perform all analyses in triplicate.

     Data Analysis Verification

     -   Obtain and titrate test samples  from
        main laboratory.
                                                         11

-------
From previous experience for a coal-fired utility, the CVH was determined
to be ±32.4 percent and CVD 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 H2SO,  within 20 percent, a sampling plan
of five days with five samples per day, or six days with two samples per
day, or seven days with one sample per day is required.
                                                         f
1.3.3  Handling of Glassware
     Because of the corrosive nature of SCL (HpSCL 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.
1.3.4  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  1.6 and 1.7 for  the recommended
schedule of maintenance and troubleshooting  activities.
1.3.5  Cleanliness
     Contamination of the  condensation coil  rinse solutions must be avoided
to prevent neutralization  of the H2S04.   Keep the rinse solutions in a
covered flask.

1.3.6  Safety
     OSHA safety requirements with regard to working environment and operator
safety must be met at all  times.  The reagents mentioned in the procedure
are  not extremely toxic, but misuse of any chemicals can be harmful.
                                     12

-------
40
                     234

                      SAMPLES PER DAY
    Figure 4.   Expected coefficient  of  variance  (CV)
               of the H2S04 measurement based on the
               number of samples  taken.
                             13

-------
1.4  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
overview of the procedure.  This critical item consists of:
        •  Recommended flowrates, temperatures and sampling times
        •  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 an on-site checklist for the supervisor and quality assurance
personnel during the run.   During a test audit the supervisor or QA rep-
resentative 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
during the execution of the test run.  Copies can be posted in the labora-
tory and sampling site for this purpose.
1.4.1  Probe Manufacture (Refer to Figure 5)
     The necessary equipment is listed in Section 1.2.1.1.  Follow correct
electrical safety procedures at all times.   Be sure that no sharp pieces of
metal abrade  any of the electrical wires.
1.4.1.1  Cut the 304 SS one-inch tubing into 32-inch lengths.
1.4.1.2  Align the shielded thermocouple (TC) as shown in Figure 5.  Using
the glasstape, secure the shielded thermocouple to the Vycor probe.  Place
the unshielded thermocouple in the thermocouple well and secure with the
glasstape.  Continue down the probe, securing both thermocouple leads
simultaneously against the tube.
                                   NOTE
          Be careful never to kink the thermocouple or thermocouple
          leads.
                                    14

-------
                                                                           PROBE T.C.
                                18/9
                  SILICONE
                  STOPPER
                     I
      VYCOR TUBE

TEFLON UNION


 6 MM
                      SHIELDED
                      T.C.
                                                           SILICONE
                                                           STOPPER
                                                      ASBESTOS
                                                      CLOTH WRAP
HEATING TAPE
                                     GLASS HEATING
                                     TAPE LEAD
                                                                                      STACK
                                                                                      T.C.
  (?) STOPPERS SHOULD BE AWAY FROM HEATING TAPE

  fT) ASBESTOS COVER SHOWS SLIGHT OVERLAP
                           Figure 5.   Controlled  condensation  system probe  design.

-------
1.4.1.3  Take the 72-inch glass heating tape and fold it in half.
1.4.1.4  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 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.
1.4.1.5  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.
1.4.1.6  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 glasstape.
1.4.1.7  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.
1.4.1.8  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.
1.4.1.9   Place the male quick connects on the end of the TC leads.  The
red TC lead goes to the negative terminal.
1.4.1.10  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.
1.4.1.11  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.
                                    16

-------
1.4.2  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
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.
1.4.3  Site Equipment Setup and Operation
1.4.3.1  In the 3-inch port, insert a 3-inch plug with 1-inch hole.
1.4.3.2  Use a table or another suitable device to support the CCS (see
Figure 3).
1.4.3.3  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.
1.4.3.4  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).
1.4.3.5  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. Hq).
                                     17

-------
          18/9
          BALL
                                 SPRING
                                 ATTACHMENT
                                 HOOKS
TISSUE QUARTZ
FILTER
                                 18/9
                                SOCKET
                THERMOCOUPLE
                  / WELL
00
                               STANDARD
                               TAPER QUARTZ
                               40/50
 SEAL
 EXTENTION
 TO STD.
 TAPER JOINT
EXTRA COARSE
QUARTZ FRIT
                                    Figure 6.  Quartz filter holder.

-------
1.4.3.6  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 further information.
1.4.3.7  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.
1.4.3.8  Begin heating the probe arid 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
          2880C (55QOF).
1.4.3.9  After leak testing, the pump is again turned on and the flowrate
adjusted to 8 £pm (0.3 cfm;.  The pump is turned off without  readjusting
the valve settings.
1.4.3.10  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
          discriminated against because of their extremely small size,
          which allows them to follow the flow lines into the nozzle.
1.4.3.11  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).
1.4.3.12  Sample for one hour or until 1/2 to 2/3 of the length of the coils
are frosted with H^SO..
                                    19

-------
Sample  Location^
Run #     	
Run Date/Time_
Operator	
Flowrate  (cfm)
Ambient  Pressure (P)
                                    AEROSOL S03
                               (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.
                                        20

-------
                                   NOTE

          If the coil is operating properly, the f^SCty 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 per-
          centage moisture has  exceeded 16 percent or the tempera-
          ture of the water bath has dropped below 60°C.   Abort the
          run and check the water bath temperature with a Hg thermom-
          eter and confirm the percentage moisture in the gas stream.
          If the water bath is below 6CrC, recalibrate the temper-
          ature bath control.  For every percent above 16 percent H?0,
          adjust the CCC temperature 2°C upward.  Clean and dry the
          CCC, and replace the reagents in the impingers  prior to
          restarting the run.

1.4.3.13  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 for analysis.

                                   NOTE

          Multiple rinses are recommended to ensure a quantitative
          wash of the coil.

1.4.3.14  Rinse the probe with 30-40 ml of D.I. H20 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
C02~free water.

                                  CAUTION

             Wait until  the  filter  has  cooled  before  proceeding.

1.4.3.15  Remove the filter and any debris from the filter holder and place

it into a beaker.  Add 30 ml of D.I,. hLO 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. H20 until the volumetric is filled to the mark.
                                    21

-------
                                                 PIPET  BULB
                                                  ADAPTER
                                               DJ. H2O

                                               SOLUTION
                                             POSITIONING
                                                DRAIN
                                            STOPCOCK VALVE
                                              125 ML ERLENMEYER FLASK
D.I.

FROM COIL
Figure 8.   Controlled condensation  coil  rinsing apparatus.

                               22

-------
1.4.4  Analysis Procedures
     Two procedures can be used to determine the amount of HUSO, collected:
        1)  An acid/base titration using Bromphenol  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 obtain the most accurate data, the following techniques should be employed
in all titrations:
        •   Always add the same number of drops of indicator.
        •   Have the same operator do 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.
        t   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
section 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).
1.4.4.1  Sulfate Titration Using Sulfonazo III.  This procedure is similar
to the sulfate procedure developed for liquors (Reference 1.6).  There are
important changes, however, so these instructions must be followed or the
resultant calcuations will be incorrect.
        1)  Wash 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 CIQ H2(OH)2] (N:NC6 H4S03H)2 to a 25 mi-bottle, add
            water to dissolve the indicator, and fill to the mark.
                                     23

-------
Run #
Run Date/Time_

Analyst	
                                 AEROSOL
                           (CONTROLLED COUDEIISATIOH)
                           LABORATORY DATA SHEET
Sample Location
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)
Atmospheric Pressure (P)
ppm H2SO. (vol/vol).
(ml)
(eq./Ji)
(ml)
(ml)
(ml)
Avg. (ml)
(ml)
(ml)
(°R)
(ft3)
(in. Hg)


Normality  of acid used to titrate blank
(if used)
ppm H2S04 =1202.52  X
                       HVT.
                       AVmP
                    Figure 9.   Laboratory data  sheet.

                                     24

-------
3)  Transfer approximately 3.9 g of reagent grade barium perchlorate
    trihydrate [Ba(C104)2-3H20] 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(C10, ) by titrating sodium sulfate.  Dry
    the Na2S04 in an oven for two hours at 125°C and allow to cool
    to room temperature in a desiccator.   Weigh  out accurately in
    triplicate 12 to 16 mg of the Na2S04 from a  weighing 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.

5)  Repeat this procedure in triplicate for the  sample and blank
    (D.I. H20):
                      N =
                          (142) (V-va)

    Where:  N = Normality of the barium perchlorate solution,
                equivalents/liter

            W = Weight of sodium sulfate titrated, mg

            V = Average volume of barium perchlorate solution
                required for titration of sodium sulfate, ml

           vg = Average volume of D.I. water blank titration.

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 N 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 5-10 minutes.  Record
    the volume of 0.01 N Ba(C104)2 used to reach the end point and
    calculate the average titration volume.  Titrate a 10 ml  aliquot
    of D.I. water in the same fashion to obtain the titration blank.
                            25

-------
1.4.4.2  Acid/Base Titration.   The preferred method of analysis is the
acid/base titration using Bromphenol  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.
     Each acid/bare indicator in this procedure will  change color over a
different pH range.  For example:
        Indicator               pH range              Color Change
     Bromphenol Blue            3.0-4.6 i            yellow to blue
     Phenolphthalein            8.2-10.0            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 Bromphenol.Blue is chosen for the
NaOH + H^SO. titration, since the equivalence point occurs at about pH 3.
Phenolphthalien 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 possible
to the actual end point, a small difference still exists and is called the
indicator blank.  The indicator blank for phenolphtalein is the amount of
NaOH required to change a specific amount of water containing a known number
of drops of phenolphtalien pink.  This value is subtracted from the milli-
liters used to titrate the sample.
     The indicator blank from Bromphenol Blue is determined in the same
way (known volume and number of drops) except that a standard acid ^SO.)  .
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.
                                     26

-------
     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 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.^O (blank).

        3)  Average the volume used to titrate the KHP solution.  The  true
            normality of the standard NaOH solution equals:

                   N _ (0.0200) (ml  titrant - ml  blank)
                   n ~              10 ml

        4)  To titrate the H2S04 in the condensation coil, probe, and  filter
            rinses, pipet 10 ml of one of these solutions into a 125-ml
            Erlenmeyer flask.  Add three drops of the Bromphenol Blue  indi-
            cator to the solution and titrate to the blue end point.   Trip-
            licate analyses should be performed as well as an indicative
            blank.  Be sure to use the same size aliquot and number  of drops
            during the blank test titration.   (See Paragraph 1.4.4.2)
            Remember this Bromophenol Blue sample blank is added to  the
            sample value.

1.4.4.3  Calculation of the H2$04 ppm (v/v) Concentration.  Using either
the sulfate or acid/base titration,  the concentration of SO., as HpSO.  in the

flue gas stream can be calculated.

        1)  From the Field Data Sheet (Figure 7) obtain the average  dry
            test meter temperature,  volume of gas sampled and atmospheric
            pressure.  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\
                         ppm H?S04 = 1202.52 Uy-^ I
                              *              \  m /

             The result is ppm (v/v)  H2S04 at STP.

             NOTE:  this  value can be 12%  low due to  fly ash present on
                    the filter (See  Introduction).

 1.5   DATA MONITORING PROCEDURES

      The  data monitoring procedures  for the  G/R  system are devoted mainly

 to the acid-base titration performed in the  laboratory and to the monitor-
 ing  of the H2S04 ppm values  calculated.
                                     27

-------
1.5.1  Acid Base Titration
     In order to check the accuracy of the titrations performed on the G/R
samples, an independent check of the NaOH solution and titration method is
required.  An unknown standard sample of H^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 Z).   Analysis 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 Bromphenol Blue to the blue end
            point and record the number of milliliters used.
        3)  Determine the normality of the solution from:
where
        N. = Normality of the acid
        VA = Volume acid aliquot taken (ml)
        ND = Normality of the base
         D
        VD = Volume of the base used to titrate the sample (ml)
         D
     The results of the determination should not differ by more than
percent within the triplicate numbers nor should the determined normality
be off by more than jJO percent.
     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.
                                    28

-------
1.5.2  Data Monitoring by Statistical  Quality Control
     In many cases where inlet and outlet information  in ^SO.  values are
measured, it was possible to monitor the SCL results by plotting the inlet
and outlet SO- 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 -2 a
and +2crlimits should contain, in the  long  run, 95 percent of all future
paired measurements.  The region between the -3 a and the +3 a limits should,
essentially, contain all future paired measurements of inlet and outlet con-
tamination.  A point falling outside of the 3 a limits indicates that the
measurement system is out of control.
     The o- 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:
        •   Check with the power plant of scrubber control room to find
            out if any mechanical problems  occurred during the run.
        t   Verify that all  the  laboratory  numbers  are correct  and repeat the
            analysis if solution is left over.
1.6  MAINTENANCE SCHEDULES
     Table 2 details the recommended maintenance schedule.  Following
this schedule is imperative to prevent breakdown and to maintain the high
accuracy required in the program.
1.7  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.
                                    29

-------
                                                                                                 -20


                                                                                                 -30
       us

       4->
       C
       
-------
                                                   TABLE  2.    GENERAL  MAINTENANCE  SCHEDULE
                           Component
                       Probe nozzles
                       Quartz probe
                        Impingers
CO
                       Pump
                        Swagelok fittings
                       CCS filter Holder
                       CC coil
                        NaOH solution
                                                                         Maintenance Schedule By:
                                                       Run
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
Kreon until  rinse is clean.

Rinse out  after each run
with DI  water.

Inspect  and clean seal
area ar.d 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
aach run.   Replace filter
after each  run.
                                            Inspect and clean after
                                            each run
                                                                                  Week
Clean frit  each week in hot
chromic  acid  for 12 hours.
Rinse to neutral pH with
DI HpO.

Clean coils and frit each
week in  hot chromic acid
for 12 hours.  Rinse to
neutral  pH  with DI HjO.

Standardize the NaOH with
KHP weekly.
                                                                                                                Month
                              Inspect vanes on diaphragm.
                              Inspect and clean motor
                              brushes.
                                                                                                                                        Calibration Procedure
                                                                                                                                   Measure  nozzle ID with micrometer.
                                                                                                                                   N/A
                                                                                                                                   N/A
Leak test at  380 torr (15" Hg)
and verify that a leak rate of
<0.3 1pm (0.02 cfm) is maintained.

Depending on  the system, a leak
rate must be  .less than a certain
value.   See specific critical
checkpoint table for information
on recommended maxinum leak rates.

N/A
                                                                                                                                   N/A
                                                                                                                                   N/A
                                                                                                                                                             (continued)

-------
                                                                  TABLE  2.    (continued)
             Component
                                                           Maintenance  Schedule  By:
                                         Run
                                                                     Week
                                                                                                    Month
                                                                                                                    Calibration Procedure
         Thermocouples
         Temperature
         Indicator
                     Inspect lines  for wear and
                     kinks.
                              Clean  readout  of all dust.
                               Clean  tips  of  shielded TCs.

                               Clean  connector prongs
                               with steel  wool.
GO
ro
Connecting
lines
         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
                                                            recalibration.

-------
                                                              TABLE  3.    TROUBLESHOOTING  AND REPAIR
                            Component
                        S-Pitot Nozzles
                        Probe Nozzles
oo
CO
Quartz Probes
                         Impingers
                                                         General  Remarks
                      Alignment of pilot  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  insure good seals,
keep the impinger seals clean.
                                                                                                         Problem
                                                                                           Misaligned  nozzle
                                                                   Damaged edge


                                                                   Nozzle wear or damage

                                                                   Misalignment
                                                                                           Normal wear and  cleanliness
                                                                                           Normal wear and cleanliness
                                                                                           Leakage in impinger system
                                                                                                                                     Repair Sequence
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 to insure
it is not dissolved by  the acetone).
                                                                                                    Rinse out with DI water after each use.
                                                                                                    Dry  impinger to be used for  moisture
                                                                                                    trap.

                                                                                                    Clean sealing edges and 0-ring  of
                                                                                                    impinger.

                                                                                                    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
                                                                                                    loak.
                                                                                                                                                                (continued)

-------
                                                                            TABLE  3.    (continued)
                               Component
                           Thermocouples
CJ
                           Temperature
                           Indicator
                           Mantle  or  probe
                           heatur
                           Connecting  lines
                           Furap
                                                            General  Remarks
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 thermocouple.

Store  in Just-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.  The
Aerotherm lines  should  never be
kinked to cut off  flow.

Care must be taken in  shutting the pump
off after a run.   Rapid shutdown with-
out bleeding air into  the pumping sys-
tem will  cause  the impingers to
back up towards  the filter.
                                                                                                          Problem
Temperature indicator  fluctu-
ating over wide  range
Temperature readings  fluctu-
ating 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)
                                                                                        Repair Sequence
                                                                                                                               Locate possible short in TC wire  or
                                                                                                                               connectors.  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 manufacture 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
                         Pump
                         (Continued)
                         Swage!ok fittings
CO
tn
                                                           General Remarks
Swaqelok fittings  are designed to seal
with a minimum of  tightening.  Exces-
sive torque applied  to  the fitting
will eventually cause leakage.
                                                                                                        Problem
                                             Leakage  (diaphraqn)
                                                                                             Installation
                                                                                             Reinstallation
                                                                                                                                       Repair Sequence
Kor leakage  or  low flow in diaphragm
pumps check  the diaphragm cover to
ensure it  has not vibrated loose.

Remove face  plate and  inspect dia-
phragm for signs of wear or pinholes.
Check the  diaphragm gasket for wear;
replace if necessarv.

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 dia-
meters, 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 fit-
ting.  At  this  point,  scribe the nut
and body a.t  the 6 o'clock position of
the fitting. Now while holding 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
                          Dry  Test Meter
                          CCS  filter holder
CO
                          CC  coil
                                                           General  Remarks
These meters are very sensitive  to
mechanical  shock and  should  he handled
with care.   Corrosive gas  from the stack
should never be passed through the
meter without prescrubbing.

The G/R filter holder is made out of
quartz and,especially when it is hot,
mechanical  shocks will cause breakage.
The filter  holder is  designed to
always be run with a  filter  on the
guartz 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, so main-
                                                tain the water jacket's cleanliness.
                                                                                                         Problem
Incorrect  volume  readings
                                                                                                seal to filter
                                                                                              Gas  leakage
                                                                                              Plugged  frit
                                             Gas leakage
                                                                                                                                         Repair  Sequence
Check meter  for  blockage.

Check mechanical  linkage  for wear.

Recalibrate  meter.

Check extension  tube.   If it is not
making 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 1-2  hours.  Rinse with DI
H-0 till neutral.

Check thermocouple well for pinhole
leak.

Check alignment  of ball-and-socket
joints.   Try to maintain  linearity.

Check seal at joints,  cle?n joint,
and  retest.

Check joints for thermal  warping.
Replace.

Soak in hot chromic  acid  cleaning
both for  12 hours.  Rinse with 01
HJ)  till neutral.

-------