, 1980
           MEASUREMENTS OF
HIGH-TEMPERATURE PROCESSES
          A SUMMARY  REPORT
                     Prepared by
                L. Cooper, M. Shackleton
                  Acurex Corporation
              Energy & Environmental Division
                   485 Clyde Avenue
              Mountain View, California 94042
                  Contract 68-02-2153
                    Project Officer
                    W. Kuykendal
                     Prepared for
            U.S. Environmental Protection Agency
          Research Triangle Park, North Carolina, 27711
     INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
          OFFICE OF RESEARCH AND DEVELOPMENT
         U.S. ENVIRONMENTAL PROTECTION AGENCY
                CINCINNATI, OHIO 45268

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                                                   June 1980
MEASUREMENTS OF HIGH-TEMPERATURE HIGH-PRESSURE
        PROCESSES - A SUMMARY REPORT
                      by
           L. Cooper, M. Shackleton
              Acurex Corporation
       Energy & Environmental Division
               485 Clyde Avenue
       Mountain View, California  94042
             Contract 68-02-2153
               Project Officer

                 W. Kuykendal




                 Prepared for

     U.S. Environmental Protection Agency
Research Triangle Park, North.Carolina  27711
 INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
      OFFICE OF RESEARCH AND DEVELOPMENT
     U.S. ENVIRONMENTAL PROTECTION AGENCY
            CINCINNATI, OHIO 45268

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                                   DISCLAIMER
     This report has been reviewed by the Industrial Environmental Research
Laboratory, U.S. Environmental Protection Agency, and approved for
publication.  Approval does not signify that the contents necessarily reflect
the views and policies of the U.S. Environmental Protection Agency, nor does
mention of trade names or commercial products constitute endorsement or
recommendation for use.

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                                    FOREWORD
     New energy conversion processes are being developed to utilize coal.  The
best time to examine these processes for potential damage to the environment
is during their development cycle.  The Industrial Environmental Research
Laboratory is engaged in work which examines pollution potential for emerging
coal conversion technologies.

     Several of these emerging technologies, for example pressurized fluidized
bed combustion and gasification processes, involve gas streams at high
temperature and pressures which contain particulates.  Since these
particulates generally must be removed from the gas stream, hot gas cleaning
devices are also under development.  In order to evaluate the effectiveness of
these hot gas cleaning devices, particle measurement and sampling equipment is
needed which can operate in these severe environments.  This report examines
some of the problems associated with particle sampling in high temperature and
pressure environments.
                                      11 i

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                                    ABSTRACT

     The major focus of this program under EPA contract 68-02-2153 was that of
particulate sampling in advanced coal conversion technologies.  Work performed
was to assess and develop the technology required to perform high-temperature
high-pressure particulate sampling.  In addition to the effort denoted to
development and testing of an HTHP sampler for the EPA/Exxon Miniplant,
experience was gained in design aspects of HTHP sampling equipment and testing
procedures and is highlighted in this report.  A background study and planning
effort was directed toward possible future sampling efforts in a coal
gasification facility.  A state-of-the-art review of HTHP sampling was also
performed.  As a means of documenting the materials collected, a bibliography
of articles, reports and books relating to HTHP sampling was compiled.
Further a mailing list of persons interested in this technology is included in
the report.
                                      iv

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                                    CONTENTS
Foreward	     iii
Abstract	      iv
Figures	     vii
Tables	      ix

   1.  Executive Surrmary	       1
           1.1  An Overview of the Problem	       1
           1.2  Summary of Work Performed	       2
           1.3  General Findings and Recommendations 	       4
   2.  Introduction  	       6
           2.1  Program Work Activities  	       6
                2.1.1  PFBC Sampler Hardware Development and
                         Demonstration Tests	-.       6
                2.1.2  Gasifier Sampling Site Survey 	      13
                2.1.3  Source Assessment Sampler Development
                         (SASS)	      13
                2.1.4  Special Purpose Probes  	      16
                2.1.5  State-of-the-Art Review 	      16
           2.2  Near and Far Term Needs for HTHP Sampling  ....      16
                2.2.1  Pressurized Fluidized Bed Combustor ....      18
                2.2.2  Coal Gasification Sampling Development  .  .      20
                2.2.3  Other HTHP Particulate Sampling Needs ...      28
   3.  Survey of Facilities and Equipment	      35
           3.1  Objectives of Survey	      35
           3.2  General Findings of the Survey	      36
   4.  Approaches to HTHP Sampling	      49
           4.1  Continuous Versus Noncontiguous Sampling 	      49
                4.1.1  Optical Systems	      49
           4.2  Approaches to Extractive Sampling   	      51
                4.2.1  Fixed Probe Concepts  	     -51
                4.2.2  Traversing Probe Concepts .  ."	      51
                4.2.3  Prototype Designs	      55
           4.3  Particulate Collection Devices 	      55
                4.3.1  Impactors, Cyclones, and Filters  	      55
                4.3.2  Suitable for HTHP Application   	      63
                4.3.3  Operation at High-Temperatures and
                         -Pressures	      68
           4.4  Sampling Handling and Flow Measurement 	      68
                4.4.1  Isokinetic Sampling Considerations  ....      68
                4.4.2  Automatic Isokinetic Sampling 	      69
                4.4.3  Other Considerations  	      69

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                            CONTENTS (Concluded)
           4.5  General Findings and Experiences Derived from
                  Exxon Tests	      71
                4.5.1  Test Results ~ Phase I and II	      71
                4.5.2  Experiences Derived from Exxon Testing  .  .      80
           4.6  Beyond Prototype Systems 	      82
                4.6.1  Generalized Sampling Systems  	      82
                4.6.2  Modular Approach  	      83
                4.6.3  Other Desirable Features  	      84
   5   Review of Particular Problems Associated with HTHP
         Sampling	      85
           5.1  PFBC Sampling	      85
           5.2  Gasifier Sampling  	      85
           5.3  Other Applications 	      86
   6   Conclusions and Recommendations 	      87

References	      89
Appendices

   A.  High-Temperature, High-Pressure Mailing List  	   -       91
   B.  Survey of Continuous Particulate Measurement
          Devices	         110

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                                  FIGURES
Number                                                                 Page

   1       High-temperature, high-pressure (PFBC) sampling
             system  	       8
   2       System schematic  	       9
   3       Exploded view of HTHP probe	      11
   4       HTHP sampling probe and duct interface valve  	      12
   5       Cyclone test apparatus  	      15
   6       Liquid cooled sampling probe  	      17
   7       Tar yield as a function of coal volatile matter ~
             pilot gas producer	      24
   8       Gasification process sampling scheme  	      27
   9       Alternative approaches to tar collection for
             gasification sampling system  	      29
  10       Westinghouse fluidized bed gasification process ....      31
  11       DOE MERC stirred-bed gasification system  	      32
  12       Fixed probe concepts  	      52
  13       Traversing probe  	      53
  14       Schematic of sliding seal sampling system 	      57
  15       Schematic of concentric tube sampling system  	      58
  16       Schematic of total enclosure sampling system  	      59
  17       Schematic of gasifier sampling system 	      60
  18       Conceptual design of gasifier sampling system 	      61
  19       Generalized cyclone design  	      64
  20       Comparison of cascade impactor stage with cyclone
             collection efficiency curve 	      65
  21       Sampling time determination for total mass
             collection of 25 milligrams	      66
  22       Automatic isokinetic sampling probes  	      70
  23       Particle size distribution r- Phase I tests 	     -75
  24       Impactor substrates ...........	      76
  25       Impactor substrate Run 3, Stage 5	._ .      77
  26       Particle photomicrographs, Stage 4  	      78
                                     vn

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                               LIST OF TABLES
Number                                                                Page

   1      Sampling system capabilities 	      7
   2      Potential Gasifier Sampling Sites  	     14
   3      Summary of Coal Gasification Processes ... 	     21
   4      Typical Coal and Gas Analysis	     23
   5      Primary Converters-Distribution of Energy into
            Products and Byproducts  	     25
   6      Grand Forks Slagging Lurgi Tar Analysis  	     26
   7      Development Problems of HTHP Gasification Samplers ...     30
   8      Westinghouse PDU Gas Stream Characteristics  	     33
   9      Morgantown Stirred-Bed Gas Stream Characteristics  ...     33
  10      Survey of Coal Conversion Demonstration Facilities
            and Sampling Equipment 	     37
  11      Summary of Traversing Probe Concepts 	     56
  12      Size Fractionating Points of Some Commercial Cascade
            Impactor for Unit Density Spheres  	     62
  13      Phase I Test Conditions  	     73
  14      Structure Temperatures 	     73
  15      Particulate Content	  .     74
  16      Particle Size Distribution	     74
  17      Concentration of Elements in Flyash SSMS Analysis
            (Partial)  	     79
  18      Partial Comparison of Front and Rear Particulate
            Catches from Exxon Test Series I and II	     81

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                                   SECTION 1

                               EXECUTIVE SUMMARY
1.1  AN OVERVIEW OF THE PROBLEM

     Sampling for participate matter in hostile environments is a technology
that is still in the early stages of development.  The need for these
techniques, however, is yet to be fully realized.  High-temperature or
high-pressure (HTHP) sampling is integral to the resolution of environmental
concerns resulting from the development of immerging energy conversion
technologies.  There are also potential applications for HTHP sampling in
current technologies, including those in the petrochemical industry.

     The major focus in this program under EPA contract 68-02-2153,
"Measurements of High-Temperature, High-Pressure Processes," was that of
particulate sampling in advanced coal conversion technologies.  Those
technologies of particular interest were pressurized fluidized bed combustion
(PFBC) and coal gasification (CG).  Although coal gasification received
attention during this program, far more effort was devoted to PFBC.

     At present it has become more and more evident that the successful
development of a pressurized fluidized bed combined cycle power system hinges
on the ability to produce a clean gas stream.  The reasons for providing a
clean gas stream are two-fold.  First, from an environmental point of view,
low levels of particulate emissions must be achieved so that limits set by the
EPA and state regulatory agencies can be met.  Secondly, and more importantly
to the power system developer, the hot gas stream must be sufficiently free of
particulate matter to allow for long turbine life (References 1 and 2).  In
general, it cannot be conclusively stated that meeting one criteria
automatically satisfies the other in alt cases.  A lot depends on the required
control level of environmental emissions in a given location and the
particular design constraints of the turbine in question.  Nevertheless, this
all points to the fact that high-temperature, high-pressure partfculate and
gaseous cleanup systems must be developed to provide for high thermodynamic
efficiency (by cleaning at elevated temperatures and pressures) and long
system life (by maintaining low levels of erosive and corrosive materials).
This report focuses predominately on those aspects related to particulate
collection.

     To develop cleanup systems to meet environmental and turbine standards,
it is necessary to perform stream sampling both upstream and downstream of
each cleanup stage.  In so doing, the removal efficiency of each stage can be
determined.  The measurements must be accurate and comprehensive.  Not only

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must total stream participate loading be measured but particle size
distribution must be determined.  It is well known that the overall efficiency
of various particulate cleanup devices is sensitive to the upstream size
distribution.  It is also well known that the particle size distribution
strongly effects the erosion and deposition of turbine components.  In
addition, the chemical composition of the particulate is important from the
standpoint of corrosive reactions that can occur within the cleanup system and
on turbine surfaces.

     Hence, it is clear that the sampling system must be accurate,   reliable,
and allow for post examination of the sample.  The system should provide the
capability to survey across the duct to determine nonuniformities in
particulate concentrations and particle size stratification.

     The system constraints defined above all point to the selection of an
extractive sampling approach for the purpose of developing advanced power
systems.  In situ, laser/optical approaches to particulate measurement are
currently under development (References 1 and 3).  Most of these methodologies
are yet to be proven in high-temperature, high-pressure environments.  Once
they are fully developed they will be extremely useful tools, but in many
applications their primary function will be for monitoring system upsets on an
operational power system.  In addition, their operation is general-ly based on
the principle of optical light scattering to determine an optical diameter.
The more conventional extractive approaches discussed in this report collect
and size particulate matter on the basis of particle aerodynamic diameters.
This parameter directly correlates to the operational function of inertia! and
noninertial cleanup devices (cyclones, barrier filters, and granular beds) and
the turbine itself.  In the case of laser/optical devices, the optical
diameter is often difficult to correlate with the aerodynamic particle
diameter.  Optical devices offer less flexibility for instance, duct surveys
are more difficult and no portion of the particulate is available for chemical
analysis.  Operation of some optical devices depends on maintaining a clean
window in the duct.  This can be difficult to sustain for long periods of
operation.

     The arguments delineated previously for the selection of an extractive
approach to particulate sampling for the development of PFBC power systems can
easily be extended to the .development of other coal conversion technologies
currently under development such as low-Btu gasification combined power cycle
and magnetohydrodynamic (MHD) coal conversion technologies.

1.2  SUMMARY OF WORK PERFORMED

     The purpose of the work performed under EPA Contract 68-02-2153 was to
assess and develop the technology required to perform high-temperature,
high-pressure sampling.  Efforts were put forth in several directions.  The
major emphasis of this program as mentioned earlier, was upon the development
of HTHP sampling hardware for coal energy conversion technologies.  Other
activities included the development of special purpose sampling hardware for
coke oven sampling, a versatile probe for sampling conventional/combustion
processes at the Research Triangle Park, Environmental Protection Agency,
Industrial Environmental Research Laboratory (RTP EPA/IERL) experimental

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facilities and the high-temperature calibration of  series cyclone  trains  for
the  EPA Source Assessment Sampler  (SASS).  A detailed description  of  these
activities can be found  in References 4 and 5.  Hence, the  information  in this
report concentrates on the findings of those activities related to coal
conversion technologies.

     The major portion of work performed under this contract  included the
development of sampling  hardware and subsequent testing in  a  PFBC  test  rig.
These efforts were eventually brought to fruition at the Exxon Miniplant  in
Linden, New Jersey in March 1977.  Two test series  were performed  at  duct
conditions of 9 atm and  1350°F.  The detailed results of these tests  are
described in References  6 and 7.

     Valuable experience was gained in the design aspects of  HTHP  sampling
equipment and testing procedures.  These related to probe design,  sampling
procedures, and data analysis.  The highlights of the information  obtained are
explained in more detail in other portions of this  report.

     In addition to the  emphasis placed on PFBC sampling, a background  study
and  planning effort was  directed toward possible future sampling efforts  in a
coal gasification facility.  A survey was performed to identify likely  test
sites and determine what sampling requirements and  problem  areas would  be
encountered.  This, in turn, led to a study of how  best to  sample  gas streams
containing tar vapors.   Several methods were proposed for separating  and
collecting these tars from the solid particulate matter present.   A design
exercise led to a proposed system for sampling in a coal gasification process
stream.

     Concurrent with the experimental tasks performed at the  Exxon Miniplant,
a state-of-the-art (SOA) review of HTHP technology  was performed.  The
activities carried out under this portion of the program were also varied.
This included a study of practical techniques for measuring stream variables
such as pressure, temperature, and velocity.  A comprehensive telephone survey
was  carried out to determine the possible future applications and  requirements
for  HTHP sampling.

     The survey also included attention to special  sampling problems  that
might be expected to occur in practice.  The highlights of  all of  the SOA
efforts are discussed in other sections of this report.

     Other SOA review activities included a detailed study  of problems
associated with the selection of materials for HTHP probes.  Material problems
occurring in the reducing atmospheres found in gasification systems present a
much more severe problem than those associated with oxidizing environments
such as those in fluidized bed combustion applications.  Highly corrosive
gases, such as H2S, present at elevated temperatures pose substantial
problems to the HTHP probe designer in selecting metals capable of
withstanding these exposures.  A detailed discussion of these problems  and
recommended solutions can be found in Reference 4.

     Finally as a means of documenting the materials collected, a  bibliography
of articles, reports, and books relating to HTHP sampling technology  and

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selected coal conversion technologies was assembled and is contained as one of
the appendices of this report.  In addition, through the various contacts
established in the course of the entire project, a mailing list of interested
persons was prepared.  This mailing list is also contained in one of the
appendices of this report.

1.3  GENERAL FINDINGS AND RECOMMENDATIONS

     The major effort conducted under this contract was, as mentioned
previously, a demonstration of the extractive HTHP sampling approach conducted
at the Exxon Miniplant.  Test conditions were 9 atm and 1350°F.  The major
findings of this portion of the program are summarized as follows.

     During the first of two test series, it was demonstrated that the PFBC
test stream could be successfully contained using a concentric tube sliding
seal approach in conjunction with a double gate valve arrangement for sampler
isolation while not in use.  Procedures for probe insertion, sampling, and
withdrawl were successfully demonstrated during the different test runs.

     Test gases were cooled using a Dowtherm cooling system to a nominal
temperature of 450°F and conventional impactor and filter designs were
used.  During the demonstration tests, particulate samples were co-llected both
on a series of seven impactor plates (two runs) and also on a thimble filter
(one run).  Repeatability of test data using the two impactor test runs was
judged as good to excellent.  Particulate matter was collected during the two
impactor runs over a size range of 0.3 ym to 30 m.  This material was
subsequently examined photomicrographically and analyzed chemically.  Results
of this analysis yielded no unexpected results.

     A second test series was conducted to examine the possible occurrence of
alkali metal condensation during sample cool down prior to collection.  The
sampling probe was reconfigured so that the sample first passed through a
scalping cyclone and total filter combination at test stream conditions.
Subsequently, the sample was cooled by the Dowtherm cooling system followed by
a second total filter.  If alkali metal condensation had occurred then it was
expected that the downstream filter catch would show a larger alkali metal
content.  Chemical analysis failed to show any significant alkali metal
condensation effects although these limited results were by no means
conclusive.

     The Exxon results demonstrated that the methods developed and the results
produced proved wholly satisfactory for this application.  Had the technology
been demonstrated at the time, cyclones calibrated for high-temperature,
high-pressure operation would have proven more versatile and eliminated the
need for cooling prior to collection.

     The experience of the Exxon sampling program especially with regard to
hardware development and the results of the SOA survey pointed to various
conclusions regarding the universality of future sampler designs.  Owing to
the wide range of test stream conditions including temperature, pressure, gas
composition, particulate loading, stream velocity, and duct diameter the
impact upon standardization of design is great.  It was found that design

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requirements tend to be nonstandard, thus sampler designs require custom
design approaches in response to the particular set of above mentioned
parameters.

     These broad design requirements inevitably lead to new engineering
problems and a consequential custom engineered system.  Based on experience
gathered during this program, the costs of engineering, designing,
calibrating, and acceptance testing of these systems is deemed to be high.  As
a result, the development costs of one-of-a-kind systems are high with
subsequent cost reduction occurring on duplicate systems if they are required.

     Some new approaches to HTHP sampling system design were identified.
Future systems can conceivably be built at lower cost with greater versatility
and safety by using a "total enclosure" design approach in which the traveling
probe is totaly isolated, thus eliminating the need for sliding seals.  As
mentioned previously, it was concluded that HTHP cyclones need to be developed
and tested as a means of increasing the allowable sampling time over that of
impactors.  Where a cooling system may be required to condense water and acid
constituents, a water mist approach may prove simpler and less subject to
maintenance problems than the Dowtherm system used at Exxon.

     In addition to these improvements, new forefronts of research- and
development were identified.  The next challenging problem confronting HTHP
sampler developers is that of coal gasification emissions sampling.  Problems
such as separation and collection of tars, selection of probe materials
compatible with corrosive, reducing atmospheres, and explosion hazards must be
overcome.

     These aforementioned problems are not simple and will be overcome only
through diligent research and development programs.  It is difficult to
foresee the process developers or other members of the private sector bearing
the full costs of development for advanced HTHP sampling systems.  The burden,
therefore, falls on government agencies to provide the necessary research and
development funds that are required to bring these systems into common
application.

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                                   SECTION 2

                                  INTRODUCTION
     This section describes the work performed under this program and
identifies the near and far term needs for HTHP sampling in the future.

2.1  PROGRAM WORK ACTIVITIES

     The primary purpose of the program conducted under EPA Contract
68-02-2153 was to develop techniques and evaluate problems associated with
sampling at high temperature and pressure.  Strong emphasis was placed upon
techniques required for sampling in coal conversion systems such as PFBC and
low- and high-Btu CG systems.  The results of all contracted efforts are
described in References 4, 5, 6, and 7.  The paragraphs that follow provide a
brief explanation of the various tasks undertaken during this 3-year program.
The reader is encouraged to consult the aforementioned references to obtain
detailed descriptions of these activities.

2.1.1    PFBC Sampler Hardware Development and Demonstration Tests

     During the period of performance of this program, a major .effort was
devoted to engineering, designing, and building a prototype sampling system
for primary application in a PFBC.  The design and engineering of such a
system is by no means simple, and constituted a major portion of the efforts
put forth by the project team.

     Table 1 shows the general capabilities of the PFBC probe designed to
operate at the Exxon Miniplant at Linden, New Jersey.  The nominal operating
conditions at Exxon were 9 atm and 1350°F.  The general configuration of the
sampling system is shown in Figure 1.  Here the following components shown
schematically in Figure 2 include:     .

     •   The sample probe assembly including the sample collection system (a
         choice of a seven-stage University of Washington Mark III cascade
         impactor and final filter or a thimble filter assembly alone)
     •   A Dowtherm cooling system used to cool the sample to a nominal
         temperature of 450°F so that a conventional impactor design could
         be used since no SOA high-temperature, high-pressure collection
         device was available

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               TABLE 1.    SAMPLING  SYSTEM  CAPABILITIES
Sample Environment

    •    Temperature

    •    Pressure

    t    Gas  Constituency
            CO
            C02
            NO
            S02
            H20
            NOX
            H2S
            trace organics
            trace inorganics

    •   Stream Velocity

    •   Particulate Grain Loadings
    •   Particulate Size Range
        (for classification)
        Duct Size
 Sampling System Configuration
 Traverse Capability or Penetration
 of Nozzle into Duct or Vessel
Access  Process Port Requirements
 650'C - 1000°C (1200°F - IBOO'F)

 300 - 2000 kPa (3 - 20 atm)

 Concentrations- subject to further
 investigation, dependent on process
 sampled
Stream Constituency Analysis
 2-46 m/s (8 - 150 fps)

 0-34.3 g/rr,3 (0-15 gr/ft3)
 (subject to further consideration
 and actual process  characteristics)

 0.2 - 26 microns (Notes:   Larger
 particulates may be acceptable  in
 most cases of total mass  determination.
 or if classified,  they may be amenable
 to "scalping" anead of classification
 device)

 Variable depending  on probe;  std.
 is 20.3 cm (8 in.)  l.D. minimum

 Modular, so as to  allo* in-situ or
 extractive sampling by cool eel probe

 Approximately 46 cm (18 in.) either
 in-situ or extractive configuration
 (some dependence on internal config-
 uration of duct or  vessel).  Can be
 extended by relatively minor hardware
 modification (longer probe, chamber
 extension, spool piece, etc.)

. Standard:  10.2 cm  (4 in.) IPS
 minimum, 136 kg (300 It.)  flange
 access through 10.2 cm (4  1n.)
 IPS alloy gate value (Note:
 Smaller ports may  be acceptable
 if special probe assembly  is used)

 Particulates, gases (inorganic  and
 organic, trace elements,  trace
 organics)

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00
      Probe Drive
      Hydraulic Cylinder
                     Microswitches For
                     Transverse Control
                      Dowtherm Coolant
                    Systems And Controls
                                Inner Tubular Housing
           i  V
                    Hydraulic Lines
   Outer Tubular  control Umbilical
   Housing
                         Dowtherm Coolant
                         Supply And Return
                    Sample Line
             Control Console
Hydraulic
Supply System
                                               Control Valve
                                               And Operator
                 Figure 1.  High-temperature, high-pressure (PFBC) sampling system.

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                                   Enclosure
                     1         (valves R  housings)
                     L__
               Motor
.—	1     driven
         |      valve
                                                                                      Hand
                                                                                      valve
       5
      Sample
      Inlet
                                                                                                       Heat
                                                                                                     tracing
1 _____ J
To vent
                  Impinqer
                   train
                                                                        To vent
                                                                                     Back
                                                                                   pressure
                                                                                   regulator
                                                                Flov/ control
                                                                    oven
                                     Figure  2.   System schematic.

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     0   A hydraulic actuator system that was required to overcome the  blowoff
         loads created by use of the concentric traversing tube design  (see
         Section 4)
     •   A flow control oven that includes orifice and metering valves  to
         maintain the flow at 450°F
     •   A trace organic module containing a chemical solvent  (XAD-2) to
         remove trace organics present
     •   Trace metal impinger train that contains selected chemical reactants"
         to condense out various trace species
     •   Various control consoles to monitor the systems and measure stream
         and system parameters
     The fully assembled probe is depicted in Figure 3.

     Field tests were first conducted during March and early April 1977 at the
Exxon Miniplant.  The sampling location for demonstration purposes was
downstream of the secondary cyclone and upstream of the final  cleanup device
which at that time was proposed to be a Ducon granular bed filter.  Test
procedures were developed to ensure safety for the operators and good data
reproducibility.  Standard EPA Level 1 Environmental Assessment cleaning
procedures were utilized for the purpose of post-test washing  of all probe
components to collect deposited materials.

     Two test series were conducted.  The first test series began in March
1977 with the second series taking place several weeks later after some
modified internal parts were fabricated.  The purpose of the first series
(which consisted of three test runs) was to demonstrate that the general
approach taken with respect to stream containment and sample collection was
viable.  The second test series was conducted to investigate whether alkali
metal compounds present in the flyash could have been condensing out of the
extracted flow due to the gas stream cooling to 450°F prior to collection.
Alkali metal compounds are particularly corrosive to turbine blades.

     During the first test series the probe was configured as  shown in
Figure 4(a) (where a thimble filter could be substituted for the cascade
impactor also).  In the second test series the probe was configured as  shown
in Figure 4(b).  Here a scalping cyclone and high-temperature  filter (saffil
alumina) were used to capture the bulk of particulate material present  in the
test stream.  The sample stream containing gaseous components  and fines then
passed through the cooler and a multiple choke system designed to reduce the
pressure while minimizing stream cooling due to super-sonic expansion.  The
sample line was then heat traced before entering a backup filter located
external to the main housing.  The objective was to chemically analyze the
trace metal composition of the high- and low-temperature filters to determine
if condensation had occurred.  The pertinent results of both test series are
discussed in Section 4.5 of this report.  The reader is referred to
Reference 2 for a detailed discussion of the hardware and the  test results.

2.1.2    Gasifier Sampling Site Survey

     During the early phases of the program a potential secondary sampling
demonstration was identified namely at a pilot-scale coal gasification  site.
At that point in the program the purpose was to identify particular problems

                                      10

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Figure 3.   HTHP sampling probe and duct interface valve.

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Normal
                   Cooler
£
       Process  Flow
Condensation Test

  Scalping  732° C
  Cyclone   Filter
    u
   Process Flow
                                Impactor
                                                      Sample Flow
                                 (a)
                                   (Or Filter)  Throttling
                                                Valve
                             Choked
                             Orifices
                                  (b)
                                            Control
                                            Valve
I
1


Cooler
•^

i
i
 204° C
(400° F)
 Filter
Sample
 Flow
                         Figure 4.  Probe configuration.

-------
 associated with  sampling  in  a  coal  gasification  facility.   It  was  conceived  at
 that  time that  if  sampling requirements  could  be met with  a new  or modified
 probe, preparations for gasification  sampling  could be  started under  this
 program.

      A site survey as well as  a telephone  survey was conducted to  identify
 potential sampling locations,  determine  what the sampling  requirements  are,
 and to identify  what special problems require  solutions.   After  the survey was
 completed a work plan was prepared  outlining a proposed program  for sampling
 at alternative sites yet  to  be determined.  Several potential  sites suggested
 are shown in Table 2.

      Upon completion of the  survey  it became evident that  the  scope of  a
 complete program for building  a gasifier sampling probe and  conducting  a
 sampling demonstration test  would be  beyond the  funds available  under the
 existing program.  The problems identified with  sampling at  a  gasifier  require
 a major engineering and design effort to construct a new probe system.  A
 major problem in terms of sampling  at a  gasifier is that of  developing  a means
 of condensing vaporous tars  for analysis while keeping them  separate  from  the
 particulate material.  Other problems peculiar to sampling  in  a  gasifier
 include the selection of materials  that will be  compatible  with  a  highly
 corrosive, reducing atmosphere and  that of producing an explosion-proof
 sampling system.

      Since such an air ambitious program was not possible within the  funds
 available, it was  decided that two  of the problem areas be  addressed  under the
 SOA review portion of this program.  A study was conducted  to  explore various
means of collecting and separating  tars from a gasification  stream.   Some  of
 these findings are discussed elsewhere in this report.  A second effort
 undertaken in the  SOA review was that of examining the problems of  material
 compatibility in a gasification environment.   This study was performed  from a
metallurgist point of view.  The complete findings of both of  these studies
 are found in Reference 4.

 2.1.3    Source Assessment Sampling System Development (SASS)

     A development task was  undertaken to make improvements  to the  EPA's
 recognized Level 1 Environmental Source Assessment Sampling  System, the SASS.
 Several modifications were made that gave improved performance, better
maintainability, and extended cyclone operating  range.  The  aspect  that most
 related to HTHP technology was that of the development of a  calibration test
facility designed  to calibrate cyclones at elevated temperatures up to
400°F.  A rotating dust table, dust pickup mechanism, and dispersion  system
was conceived and  developed  under this task.   A  standard SASS  cyclone train
consisting of three cyclones was calibrated at a temperature of 400°F.  A
 schematic of the test rig is shown  in Figure 5.  The complete  details of this
effort are discussed in References  4 and 5.

 2.1.4    Special Purpose Probes

     Two special purpose probes were constructed for particular applications.
Both of these probes were based upon the basic SASS design and were modified


                                      13

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                    TABLE 2.    POTENTIAL  GASIFIER SAMPLING SITES
Category
      Facility
Developers/Sponsors      Gasifier  Type
Temperature  Pressure
    (F)       (psia)
  1.      P<300 psia,  T<1800  F,
          gas composition  re-
          latively  low tar con-
          centrations

          t  Westinghouse
             Waltz  Mill
          •  C02  Acceptor
          P<300 psia,  T<1800  F,
          higher tar,  particu-
          late, sulfur loading
          in product gas

          •  Stirred bed


          •  G.E.  Gas
             Schenectady,  N.Y.


          t  Union Carbide
             Ash Agglomer-
             ation

          P>300, T<1800
                         ERDA
                        Consolidation Coal
                        CO./ERDA, AGA
                        U.S. Bureau of
                        Mines

                        G.E./EPRI
                        Battelle/ERDA
                     Multiple fluid
                     beds with dolo-
                     mite regenera-
                     tor step

                     Fluidized bed
                     using dolomite/
                     limestone as
                     acceptor for C0?
                     and H2S
 1400-1800   150-240
 1500-1550   150-300
                                          1000
             300
Fixed bed reactor
with agitator

Moving fixed bed     1000-1100    170-350
reactor with coun-
tercurrent flow

Two fluidized beds    1600-1800    120
  4.
          t  Bi-Gas
             Homer City

          •  Hi-Gas
•  Synthane

•  Grand Forks
   Energy Research
   Center

P>300, T>1800

t  U-Gas
                         Bituminous Coal Re-
                         search/OCR-AGA

                         IGT/ERDA
                                  U.S. Bureau of
                                  Mines
                                  ERDA
                                  IGT/ERDA
                     Two-stage entrained  1800
                     beds, upflow con-
                     figurations
            1000-1500
                     Two-stage fluid bed
                     hydro-gasifier;
                     electrothermal/
                     Oxygen/steam-iron/
                     steam-air bed char
                     gasifier for H^

                     Fluid bed reactor


                     Lurgi-slagging
                     design
                      Fluidized bed re-
                      actor, ash-
                      agglomeratino
                      gasifier
  600-1200  1000-1500
 1100
                                 500-1000
  400-1500   400
 1900
                                300-350
                                               14

-------
en
         AIH
         M1IO-
         MIN
                                                                                                                  CVO.OCM
                                                                                                             COlLtCTKM
                                                                                                             CUP
                                                                                                             CONTROL PANEL
                                                Figure 5.   Cyclone  test  apparatus.

-------
to operate at elevated temperatures.  Both probe designs utilized  a water
cooled jacket to maintain probe integrity.  One of the probes shown in
Figure 6 was designed to operate in a variety of applications on experimental
combustion facilities located at the EPA Industrial Environmental  Research
Laboratories at Research Triangle Park, North Carolina.  A description of the
probe itself and operational procedures are contained in Reference 4.

     The second probe was of a similar but simplified water-cooled design and-
was specifically developed to evaluate the environmental pollutants emanating
from coke ovens during open door conditions.

2.1.5    State-of-the-Art (SOA) Review

     Whereas the primary focus of the overall program was upon the PFBC
sampling effort, the secondary emphasis was placed upon the SOA review.  The
major elements of the SOA review included:

     •   A survey of facilities to determine near and far term HTH? sampling
         needs
     •   A study of techniques for measuring pressure, temperature, and
         velocity in a particle laden stream
     •   A study of means for collecting and separating tars and solid
         particulate in a coal gasification stream
     •   A survey of problems related to selection of materials compatible
         with coal conversion environments
     •   A bibliography of information relating to HTHP sampling system
         technology

     Most of the detailed findings for the second, third, and fourth studies
are contained in Reference 4.  Some aspects, particularly related to tar
separation, are updated in this report.  The results of the facility survey
are contained in Section 3 of this report.

     In summation, the various elements that comprise the entire program were
very comprehensive in nature.  The major thrust of the program was directed
toward PFBC probe development and field demonstration and comprised about 60
percent of the total effort.

2.2  NEAR AND FAR TERM NEEDS FOR HTHP SAMPLING

     There is a current need for sophisticated extractive particulate sampling
equipment.  Because this equipment is not generally available the-required
sampling is accomplished using modifications of equipment designed for
conventional  environments and through simplified "homebuilt" devices which may
not yield accurate results.  These approaches can provide order-of-magnitude
results that may be adequate for obtaining preliminary data but will not serve
for the more refined development of coal conversion technologies that will be
attempted soon.
                                      16

-------

Figure 6.   Liquid cooled sampling probe.

-------
     The primary reason the required sampling equipment  is not currently
available is that developing precision equipment for application  in the severe
environments of the coal combustion zone is extremely expensive.  Furthermore,
applications of this sampling equipment are generally limited to  those few
test sites doing research on advanced coal conversion processes.  Thus, there
is no viable current market for the equipment.  For these reasons industry
will not sponsor development and, therefore, if it is to be available its
development will have to be sponsored by the government.

2.2.1    Pressurized Fluidized Bed Combustion

     One of the most significant application areas for HTHP extractive
particle sampling equipment is associated with the development of pressurized
fluidized bed combined cycle powerplants.  Potentially the process can utilize
a wide variety of coal types at high thermodynamic efficiency (40 percent) and
do so while controlling SOX and NOX without expensive add-on devices.

     Major test facilities operating research PFBC systems are the CURL
facility in Leatherhead, England, the EPA/Exxon Miniplant in Linden,
New Jersey and the PFBC installed at Curtiss Wright Corporation in Woodbridge,
New Jersey.  A new and larger facility is being built under International
Energy Association (IEA) sponsorship at Grimethorpe in England.  American
Electric Power Corporation, in conjunction with Stal Laval, a Swedish turbine
manufacturer, is preparing preliminary designs for a utility-sized PFBC to be
built in Ohio.  Each of these facilities will have continuing needs for
reliable extractive particle sampling equipment as process development
continues and the hot gas cleaning problem is addressed over the next several
years.

     In the combined cycle process, coal is burned in a pressurized, fluidized
bed of sorbent material such as dolomite or limestone.  The bed is fluidized
by injecting compressed air under and through the bed.  The dolomite or
limestone is injected into the bed in sufficient quantity to react with the
sulfur gases released through this combustion of coal.  Steam tubes are
located within the bed and water is passed through these tubes at a rate such
that the combustion temperature is controlled at 800 to 900°C.  This
relatively low combustion temperature limits production of thermal NOX.

     Most proposed PFBC systems are designed to operate at between 10 and
20 atm of pressure.  The hot, high-pressure gases leaving the bed contain the
gaseous combustion products and large quantities of particulate flyash.  This
HTHP gas stream is expanded across a gas turbine to drive the compressor and
generate electrical power in the second of the two cycles comprising the
combined cycle system.  Development of methods to protect the gas turbine from
particulate erosion and corrosion represent the major tasks required before
commercialization of this advanced coal combustion technology can take place.
Reference 1 discusses the levels of cleanup required by various turbine
manufacturers.

     To more fully understand the system, particle sampling is needed at
several locations within the process.  These locations include sampling within
the bed, before and after one or more stages of cyclone separation, upstream


                                      18

-------
and downstream the fine particle removal device, and downstream of the
turbine.  Commercially available low-temperature, low-pressure equipment  is
suitable only for sampling downstream of the turbine.

     The high temperatures and pressures combined with erosive and corrosive
contaminants present in the operating environment create severe design and
materials limitations to the design of the sampling system.  These factors
create problems in construction, sealing, cooling, and require the use of high
performance materials.  Major design constraints for an HTHP particle sampler
are listed:

         Severe environment — Temperature, pressure, corrosives
         Flow stream problems -- Tortuous paths
         Confined space — Limits work space
         Variation in particle concentration -- Affects sampling time and
         capacity
         Safety — For operators
         Cost -- Must be affordable

     As a result of the high pressure and temperature conditions, gas
distribution piping is costly and long straight sections ideal for particulate
sampling are seldom available.  In addition, the sampling locations are often
cluttered with other equipment, structures, and piping.  These conditions
require that the sampler be capable of isokinetic operation while also being
compact so that it can be installed where needed.  For isokinetic sampling at
locations with a less than ideal flow distribution, the sampler must have the
capability to sense and be adjusted to changes in flow velocity and must
posses a high degree of transverse and angular mobility.

     At the locations where sampling is needed, the particle mass
concentration can vary over several orders of magnitude.  This means that the
sample quantities collected, the collection time, and the volume sampled or a
combination of these parameters must be capable of being varied if a single
design is to be used at different locations.

     A gas leak failure of the system could pose a potentially lethal hazard
to nearby operating personnel.  For this reason, the sampler must be rugged,
reliable, and be designed with operator safety as a major consideration.  It
is highly desirable, if not mandatory, that the sampler be capable of remote
operation.  This is probably the least expensive and most positive way to
ensure operator safety.

     Cost is another design constraint.  A review of the technical constraints
above should provide some understanding of why estimated costs of this
equipment have been high.  This is especially true when the order quantities
are limited to one or two prototypes.  As a result of several design efforts
to date at Acurex, the predicted costs for HTHP samplers have been reduced.
These reductions are a result of refinements in design concepts leading toward
simplification of hardware.  Once the initial development costs are completed
and the design concept is demonstrated, additional copies of the most simple
probes should find application in other PFBC facilities at costs only somewhat
above those of more conventional sampling equipment.


                                      19

-------
2.2.2    Coal Gasification Sampling Development

     Coal gasification is basically an old technology that is receiving
renewed attention as an efficient means of extracting a gaseous fuel from coal
and using it either to the site of gasification or transporting the gas via
pipeline to be burned offsite.  Gaseous fuel burned onsite in turbines or
boilers is usually of the low-Btu variety (100 to 300 Btu/scf) while high-Btu
gas (800 to 1000 Btu/scf) produced through a methanization process would be   ~
used as a substitute pipeline fuel for natural gas.

     The basic differences between the two process types is governed by the
operating temperatures and pressures and by whether the gasification bed is
air blown or oxygen blown.  High-Btu gasification processes tend to be oxygen
blown and operate at extremely high temperatures and pressures.  Reference 8
presents the significant features of more than 20 operating coal gasification
processes located in the U.S.  Table 3, taken from Reference 9, presents a
comparision of 19 coal gasification processes.  The typical operating
temperatures and pressures for each facility are shown.  The operational
ranges for gasification system dictate the need for high-temperature,
high-pressure or at the least, high-temperature sampling approaches.

     Operating pressures for some high-Btu gasification processes are enormous
even compared to PFBC sampling applications and dictate that special means of
pressure containment be used.  For example, it is highly unlikely that a
pressure housing such as that used at the Exxon PFBC, (concentric tubes
separated by a sliding seal) be applicable at pressures as high as 1200 psi.
Sealing requirements would be untenable in any event.  Also, the blowoff loads
would be extreme and would require a very large hydraulic actuation system to
traverse the probe.  Alternatives to these approaches are discussed in
Section 4 of this report.

     The needs for using in process HTHP particulate sampling systems in
gasification processes with which the authors of this report concur are
identified by the authors of Reference 8.  They are as follows:

     •   To measure particulate carryover from the reactor bed
     •   To determine the chemical composition of the particulate leaving the
         bed
     •   To determine the concentration of mositure, tars, trace elements,
         etc., at various points in the'process
     •   To determine particulate levels prior to the methanization step (for
         high-Btu applications) to prevent catalyst poisoning
     •   To determine particulate level and composition upstream of the
         turbines (for low-Btu applications)
     •   To evaluate the performance and aid in the design of particulate
         cleanup devices

     Many of the above needs and requirements are shared with PFBC
applications.  One requirement that is unique to sampling applications in coal
gasifiers is that of sampling tars.
                                      20

-------
TABLE 3.  SUMMARY OF COAL GASIFICATION PROCESSES
IDENTIFIER
BATTELI-E
CLEHCF.RY
WILPUTTE
NLiS
R-M
HERC
CE
1CT
FMC
BATTELLE
8CR
UF.ST
PERC
CONOCO
BI.W

CE
OCCIDENTAL
TEXACO
BCR
LOCATION
Rtchland, Wash.
Shoemakersvl 1 le , Pa.
Klngaport, Tenn.
Carey, Ohio
Worcester, Mass.
Morgantovn. U.Va.
Schenectady. N.Y.
Chicago. 111.
Prlncetovn, N.J.
Columbus, Ohio
Monroevllle. Pa.
Madison, Pa.
Brucetown, Pa.
Rapid City, S.D.
Alliance, Ohio

Windsor, Conn.
Lave me, Ca 1 .
Hont e Bel lo , Ca 1 .
Homer City, Pa .
TYPE OK
BED
Fixed
Fined
Fixed
Fl>ed
Fixed
Fixed
Fixed
FluldUed
FluldUed
FluldUed
Fluldlzed
Fli.'ldUed
FluldUed
FluldUed
F.n t ra Ined

Entrained
Entrained
Entrained
Ent ra Incd
TEMP.
°F
1500
1000
1200
10)0
1050
1200
1200
1200
1500
1800
laoo
1750
1750
1500
1 700

1700
1500
I5DO
1750
PRFSS:
psn:
5
1
15
1
1.5
125
100
1000
30
100
300
175
100D
150
35

15
50
300
1700
AIR OR
°7
Air
Air
Air
Air
Both
Air
Air
°2
Air
Air
Roth
Air
°2
(Air)
Bot h

Air
Air
°2
°2
i.n. COM.
FT TON /DAY
3
10 24
-
-
10.5 90
3.S 27
3
2.5 72
6 2.5
3 25
-
3 15
5 75
3.3 30
9 850

30 2840
1
2
9
O /AIR STTAM
I.B/IIR TOM/MR SAKl'I.lNi:
- Impart" r
Nu
No
Only to Satisfy P.PA
11.5 T/Hr 1.35 From Cyclone
3037 0.25 High Temperature Filter
No
1720 0.21 Crab Sample
No
No
- Planning
Yes
From Scruhber
n 1 .6 From Cyclone
30 T/llr 30 Tried, Filter Plugged
with Tar
372 T/Hr 35 No
No
No
Planning
OPERATING
Yes
Yen
Yes
Yes
Nu
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Mid '76
Yea
Yes

Designing
Yes
Yes
I-ate '76

-------
     During the gasification process trapped volatile materials  in  the  coal  is
released.  Foremost among the variables affecting  the quantities  of tars  and
other volatiles released are the operating pressure  and temperature and the
coal type.  Table 4 shows the relative quantities  of tars and  ash present in
four different coal types.  Also as shown in Figure  7 the tar  yield is
directly related to the percentage of volatiles present.  It has  also been
shown that in practice prolonged exposure to high  temperatures in the bed
increases the tar yield.  Table 5 shows the relative yield of  gas,  volatiles,-
and solids that are produced in several operating  gasifiers.   Acurex conducted
a separate survey of gasification facilities to determine process development
problems relating to tar production.  These are discussed in further detail  in
Section 3 of this report.

     Basically, tars in the off gas present two major problems.   First, as
system pressures and temperatures drop the tars may  condense on the walls of
the process ducts or clog turbine passages.  In addition, the  tars  themselves
present a health hazard to those who are exposed,  whether at the  process  plant
or through pipeline application.  These tars are known to be highly carcinogenic
and breathing their vapors or skin contact should  be avoided entirely.  On the
positive side, these tars are combustible; hence,  their energy content  cannot
be ignored.

     Consequently, the presence of tars in the gasification process requires
measuring systems to identify their relative quantities and properties within
the process.  At the same time, the process developer needs to understand the
quantities and size distributions of particulate to  satisfy the needs and
requirements stated earlier.  These simultaneous requirements  demand that a
HTHP sampling system designed for gasifier application have the capability of
collecting and separating tars and particulates simultaneously.   This is  a
difficult requirement to fulfill in that throughout most of the gasification
process the tars are in a vapor phase.  This means that if the tars are in a
vapor phase in the process duct they must first be condensed into a liquid
phase within the sampler.  Unfortunately, the tars present in  coal
gasification processes are very complex in molecular structure and  do not
possess a single condensation temperature.  Table  6  shows a percentage
breakdown of tars from the Grand Forks gasifier.   Bear in mind that these are
broad classifications and that literally thousands of different molecular
species are present.

     Condensation of the tar vapors forms a tar mist .of very fine particles.
The condensation of tar mist must take place downstream of the solid
particulate collection device otherwise one will obtain clogging  in the probe
cyclones and a resultant catch which is a combination of tars  and solid
particulates.

     The proposed sequence of events that must take place within  the probe are
shown in Figure 8.  Here the solid particles are collected at  the system
temperature and pressure so that the tars remain in a vapor phase.  After the
solid particulate is removed the temperature is reduced below  the condensation
temperature of the lowest fractions to be collected.
                                       22

-------
TABLE 4.  TYPICAL COAL AND GAS ANALYSIS
Coal rank

Origin
Dry coal analysis,
wt, %
C
N
0
H
S
Ash
Volatile matter
Fired carbon
Heating value
Btu/lb
Free swelling
Index
Coal ash softening
Temp, °F
Typical gas analysis
CO
N2
CO 2
CH4
Higher H/C
H2S
NH3
N2 + inerts
HHV. Btu/Scf
Anthracite

Pennsylvania


85.5
2.0
1.7
0.9
0.7
9.2
4.8
86.0

13,450

0

+2,700
Air 02
24.1 38.4
18.4 41.9
6.6 18.6
0.5 0.7
.0.5
0.1
—
50.3 0.4
142 266
Low vol . A
bituminous
Pocahontas


80.5
4.1
2.8
1.0
0.7
10.9
16.4
72.7

13,850

3

*~
Air
25.4
14.6
6.8
0.9
0.1
0.11
0.27
51.8
141
High vol . A
bituminous
W. Virginia


83.8
5.2
4.1
1.5
0.7
4.7
30.1
65.2

14,855

8

+2,700
Air
25.6
13.8
6.4
1.8
0.3
0.12
• 0.05
51.9
152
High vol. C
bituminous
Ohio


67.0
4.7
6.3
1.1
4.0
16.9
37.1
- 46.0

12,195

4

2,360
Air 02
25.4 39.2
12.3 31.4
4.6 16.2
1.7 3.3
0.1 0.8
0.30 1.1
0.05 0.1
55.3 7.9
139 286
                   23

-------
    14
    12
O>
O>
^   10
O
u
c
c
O
en
oi
QJ
S_
fO
           Legend

D Anthracite  (1P1)
O LVA bituminous  (1P1)
O HVC bituminous  (3  pts)
A HVA bituminous  (14 pts)
                  10            20       '    30
                   Coal  volatile matter, % by wt.
                           40
      Figure  7.   Tar yield as a function of coal  volatile
                 matter -- pilot gas producer.
                               24

-------
TABLE 5.   PRIMARY CONVERTERS -- DISTRIBUTION OF ENERGY
          INTO PRODUCTS AND BYPRODUCTS



?ro:e 6 «
Koppe ri-Totze'*
Texaco
U-CAS
BI-GA3
CCj-Acceptsr
KYGAS-Oxyger.
Syr.ihane

Union Carbide •' Eartelle
W i rif. 1 e r
V.' e 1 1 r~, a ~ - G il u e h a
Lu.-f i
COED
TO5COAL
Carre::
ri-COAL
csr
SCR



Ca 9
95
95
96
95
94
95
71
96
96
80
72
• • 65
25
6
35
10
10
20

Percent o! Ounsut

Tan J. Oils

• -
--
--
--
3
4


--
18
16
2C
IS
15
"5
7 i
55

Enerrv
Char*. Ash.
i> Fe siiue
5
5
4
5
6
•>
25
4
4
20
10
15
i c.
76
60
15
5
25 .
                           25

-------
TABLE 6.   GRAND FORKS  SLAGGING  LURGI TAR ANALYSIS3
           Constituents                 Pet
     Saturated  hydrocarbon             10.3
     Nonvolatile  residue               7.7
     Phenol/cresol/xylenol             22.4
     Indanol                           1.0
     Dibenzofuran                      3.78
     Hydroxyanthracene                 1.01
     Indanes                           0.22
     Naphthol                          3.93
     Indenes                           0.96
     Pyridines                         1.81
     Quinolines                       1.35
     Naphthalene                       4.76
     Acenaphthene/biphenyl             0.37
     Fluorene/acenaphthalene           1.76
     Phenanthrene/anthracene           0.85
     Oihydropyrene                     0.81
     Pyrene/fluoranthene               0.49
     Chrysene                          0.49
     Benzenes                          1.78
     Indole       .                     0.23
     Carbazole                         0.21
     Benzocarbazole                    0
     Benzofuran                       5.16
     Benzonapthofuran                  2.30
     Performed  by  mass  spectrometry
                        26

-------
         SAMPLE EXTRACTION FROM
               PROCESS DUCT
            SOLID PARTICULATE
               COLLECTION
        APPROPRIATE TEMPERATURE
         AND PRESSURE REDUCTION
                   TAR
                COLLECTION
              LIGHT OIL AND
            WATER COLLECTION
                SAMPLE GAS
            VENTING OR ANALYSIS
Figure 8.   Gasification process sampling scheme.

                    27

-------
     This forms a fine tar that is difficult to coalesce by  impingement  or
other inertia! approaches (see Reference 4).  Consequently,  other means  must
be used to collect the tars.  Several approaches to tar collection were
studied during this program.  A detailed discussion of these methods  is
presented in Reference 4.  A further discussion of these approaches is also
contained in Section 5 of this report.  These approaches included:

         Inertia! separators
         Filters
         Electrostatic precipitators
         Packed beds
         Scrubbers

     The selection and development of one of these tar collection devices is
critical to the development of a HTHP sampling system for gasification
application.  The suggested approach (recommended by University of California
at Berkeley researchers) is to use a packed bed of inert ceramic material
filled with pyridine, CH(CHCH)2N, as a tar solvent.  The pyridine can later
be evaporated away.  Several collection schemes seem viable  using both an ESP
and/or a packed solvent bed.  Figure 9 shows three possible  tar collection
schemes.  The configuration upstream of the tar collectors is the same in all
three cases.  It consists of collecting the particulate at high temperature
and pressure and then rapidly chilling the gas to condense the tar vapors to
form a mist.  Chilling to a point just above the condensation temperature for
water (at the local P) should be sufficient.  Scheme 1 uses  a packed  bed
scrubber in series with an ESP to collect the tars.  This arrangement presumes
that a packed bed will not be able to remove all the submicron tar mist.
Thus, the ESP design effort will be simpler since the operating regime is
confined to submicron particles.  The filter downstream will collect  any
residual materials.  The gas can then be passed through an impfnger train (not
shown) to remove any condensibles not removed upstream such  as light  oils.  In
Scheme 2 the ESP is replaced entirely by the packed bed.  Finally, Scheme 3
shows the ESP as the primary collection device and would be  used along only if
the packed bed approach proved ineffective.

     Other problems that must be overcome in developing the  entire system are
highlighted in Table 7.  Finally, to illustrate typical sampling conditions
Figures 10 and 11 and Tables 8 and 9 are presented.  These figures and tables
present the operating conditions and required sampling locations at the
Westinghouse fluidized bed gasification'process and the DOE  Morgantown stirred
bed gasification system.

     In summary, there exists the requirement to develop gasification sampling
systems and difficult development problems lie ahead.

2.2.3  Other HTHP Particulate Sampling Needs

     Applications for special purpose high-temperature, high-pressure samplers
exist in a few areas other than PFBC and gasifiers.  Two applications recently
identified were sampling in the exhaust of an MHD channel and an application
at a catalytic cracking plant to determine interstage cyclone efficiency
                                      28

-------
       r
SAMPLE
       L.
            LJ    i_f   i— r
                           =ffl=K
              CYCLONE TRAIN
V   !c
/    i
                                   CONDENSER
                          FINAL
                       PARTICULATE 1
                         FILTER    1
                                 1
                                                 1.
                                                  PACKED BED/
                                                 SOLVENT BATH
                       2.
                                                                 ESP
                                                                  OR
    T^^TN333*" ANALYSIS
       FILTER     IF REQUIRED
 €=
FILTER
                                                                         A-19005
 €]=
FILTER
                                                 3.
                                                     ESP
                                                                 €>==
                                                                FILTER
      Figure 9.  Alternative approaches to tar collection  for gasification sampling  system.

-------
           TABLE  7.   DEVELOPMENT  PROBLEMS  OF  HTHP GASIFICATION  SAMPLERS
          Problem
           Reason
            Solution
•  Cyclones must be operated
   at high temperature and
   pressure (1000°F, 25 atm
   typ.)
•  Cyclone size variations
   with temperature, pres-
   sure, flowrate
•  Isokinetic sampling
•  Cyclone accessability
t  Maintain pressurized
   environment exterior
   to cyclone bodies

•  Maintain cyclone train at
   hiqh temperature (1000°F)
•  Collection of heavy
   hydrocarbon species (tars)
•  Sample pressure, temper-
   ature reduction prior to
   adsorption cartridge
•  Flowrate control
•  Determination of actual
   cyclone and sample gas
   flow rates
t  Sample transport
t  Coolant requirements
•  Variations in impinger
   flowrate

•  In-probe catalytic
   effects
•  Corrosion,  erosion at
   high temperature and
   pressure
 Particulate removal must be
 performed initially.  Tempera-
 ture and pressure reductions
 allow heavy HC species to
 condense

 Require a known cut size for
 modified cyclone designs
 Isokinetics must be maintained
 for particulate sampling

 Cyclone system integral to the
 probe must be accessible for
 disassembly/sample collection

 Avoid large pressure differ-
 tial between outside and in-
 side of cyclones

 Avoid condensation of heavy
 hydrocarbon species (tars)
 in cyclones
Collection must be performed
prior to XAD-2 adsorption
XAD-2 must be operated at
20°C, atmospheric pressure
Control gas flows to cyclones
and absorber/impinger com-
ponents

Maintain proper cyclone flow-
rates.  Knowledge of total
sample volume
Maintain sample flow through
the system

Maintain probe structural
integrity

May affect chemical absorp-
tion efficiency

Maintain sample chemical
integrity between process ex-
traction and final analysis

Effects on final  design may be
different than at lower temper-
atures and pressures
Smaller actual  flow rate require-
ments (due to increased pressure
allow smaller cyclone sizes.
Cyclone train can be made inte-
gral to the probe body

Calculations available to demon-
strate cut size variation with
pressure (none), temperature
(small), and flowrate (moderate)

Isokinetics achieved as in present
system with change of probe nozzle

Provisions made for probe dis-
assembly and cyclone removal.
Time requirements are not critical

Utilize exterior pressure system
or pressure equalization line  to
sample source

Requires possible heating/cooling.
Electrical heating probably most
applicable in contained pressur-
ized environment

Collection by temperature reduc-
tion at high pressure.  Efficient
collection chamber design is  re-
quired

Throttle valve, pressure regulator,
critical orifice utilized for  pres-
sure reduction.  Temperature  re-
duction by oven and gas cooler

Utilize flow control valve and
critical orifice in controlled
temperature environment

Use of orifices and/or gas flow
meter with temperature and pres-
sure measurement taken to compute
other system location flowrates

Source pressure adequate - no
pumping required  -

Coolant circulation in probe  body
may be required

Impinger bottle nozzle size
variation may be required

Study warranted to determine
probe/sample interactions at
HTHP

Choose appropriate materials  to
alleviate corrosion.  Analyze
erosion problems at HTHP
                                               30

-------
                       200-3'>i) Ib/hr
                       part Kuldte
OEVOLAIlLl/tK
       coj)
               I ,600"f
               IS  Aim
   Sjniple _UKdl ion ?

   \ ,400"F  -  1 .600 F, IS Aim
                           Chjr
?.000CF
IS Atm
                S It."din ,ini1 .11 r
                                       Gasifier
                            \
                                                                         Ic Loc.it ion  I
                                                                     I .41)0 'F -  I .600'
                                                                     15 Atm
                                     Cyclone
        Product q.is
        6.000  Ib/hr
        ISO Btu/itf
Quench
vessel
                                                            f MIL'S
                                                                                      tar. 011
                                                                                      f mes
                                                                             Typical transport duct
                                                                 Kl'f rjc tory
                                                                                                18" Sch 80 pipe
                                                                                                6"  10
                                 Ash
                      Figure 10.   Westinghouse fluidized  bed gasification process.

-------
                                                           Primary sample location 1     Alternate lample location 2
      £>S\  Crushed coa
CO
ro
                                                                                   Cyclone
                                                                 Ash
                                                                                                  Pressure

                                                                                                  letdown

                                                                                                  orifice
                                                                                                            Mufflers
To stack
                                       Figure 11.   DOE MERC stirred  bed  gasification  system.

-------
          TABLE 8.  WESTINGHOUSE PDU GAS STREAM CHARACTERISTICS
             Characteristic
                Value
          Temperature

          Pressure

          Stream velocity

          Approximate gas
            composition

          Particulate loading

            Cyclone outlet
            Cyclone inlet
   1,400 °F to 1,600°F

   225 psig

   22 to 23 fps

   CO: 17.5%, C02:9%, H2:13r0
   H20:8%, CH4:2.5%, N2:50% (mole %)
   8 gr/acf to 20 gr/acf
   100 gr/acf
       TABLE 9.  MORGANTOWN STIRRED BED GAS STREAM CHARACTERISTICS
      Characteristic
                 Value
Temperature

Pressure

Stream velocity

Approximate gas composition
  (dry basis, mole percent)


Particulate loading:

  Gasifier outlet
  Cyclone outlet

Tar and oil loading

  Gasifier outlet

Moisture content
1200°F nominal with excursions to 800°F

150 psig nominal, 300 psig maximum

29 to 40 fps

CO:    16:2 percent, C02:  13.5 percent,
H2:    16.7 percent, H2S:   0.5 percent,
CH/j:    2.5 percent, N2:     50 percent
10 gr/acf
 1 gr/acf
17 gr/acf

10 to 20 percent
                                   33

-------
where a cyclone train was specified for catalyst removal upstream of a turbine
gas expander.

     Particle sampling in the MHD gas stream does not involve high pressures
but does involve high temperatures.  At the sampling location, temperatures
were stated to be as high as 1370°C.  The MHD exhaust also contains
corrosive alkali seed material in addition to the gaseous and particulate
products of coal combustion.  These corrosives in combination with the extreme
temperatures, present severe material selection problems for sampler design.
One must be concerned about contaminating the sample collected through contact
with the sampler probe itself.  As MHD development continues, particle
samplers will need to be adapted so that characteristics of particles in the
MHD gas stream can be characterized.

     Catalytic petroleum crackers operate at pressures of 2 to 3 atmospheres
and exhaust temperatures of nominally 600°C.  In the process the hot,
high-pressure gas stream containing particles of catalyst is passed through a
turbine device known as an expander.  This step removes a portion of the
energy in the gas stream and contributes in large part to making the process
cost effective.

     Catalyst contained in the gas stream is removed using several, stages of
cyclone separation.  This removal recovers some of the catalyst material and
is needed to protect the expander from erosion.  Since the catalyst particles
are originally large ( 1000  m) those small particles that leave the cracker
are generated by grinding action between each other.  Thus, they tend toward a
larger size fraction capable of removal by inertia! separation.  Even so, such
separation requires good cyclone performance to ensure turbine expander life
of greater than 2 years.

     To obtain the needed level of performance up to four cyclones in series
are used.  To monitor performance of these cyclone stages and help in
improving designs to lower the fraction of particles released to the
atmosphere through the turbine expander it is desirable to be able to measure
particle concentration in the HTHP region of the ducting.  A small market
would exist for inexpensive general purpose samplers capable of operation in
this application.  However, the incentive for the petroleum industry or for
cyclone manufacturers to pay for development of such equipment is lacking.
                                     34

-------
                                   SECTION  3

                       SURVEY OF FACILITIES AND EQUIPMENT
     As a part of the SOA review task of the overall program, a survey of
potential HTHP sampler users was conducted.  The reasons for conducting this
survey were several.  In the paragraphs that follow, the objectives of the
survey will be discussed along with a discussion of the general findings.

3.1  OBJECTIVES OF SURVEY

     The formal telephone survey was conducted over a period of 1 year
beginning in April 1976.  This formal survey was followed by more informal
inquiries which continued until the end of the program; however, only the
formal portion is reported here."

     The first objective of the survey was to contact facilities involved in
advanced coal conversion technologies to learn the goals and objectives of
each of these programs from the standpoint of process development.  Included
in the inquiries was a determination of the operational environmental
conditions at the locations where particulate sampling would be likely to
occur.  This included information such as the range of temperatures,
pressures, and velocities that could be encountered.

     Another objective was to determine what need, if any, currently existed
or would exist in the future for particulate sampling within the process
stream.  In addition, information was sought as to whether particulate
sampling would (1) be a necessity in terms of a tool for process development
or (2) a means of acquiring additional information for determining process
mass and energy balances.  Inquiries relating to ground rules that might be
imposed for sampling at a particular facility were also made.  This would
relate to safety requirements such as explosion proofing, typical constraints,
and allowable shutdown periods for operation of the facility.  Questions were
posed as to whether any special problems such as sampler plugging and
corrosive and/or erosive conditions that might inhibit sampling attempts.

     Another objective was to determine what types of sampling had been done
to date, the results that were obtained, and where the sampling equipment was
obtained.  Also, if sampling had actually be done (whether gaseous or
particulate), what problems had occurred.  If types of equipment were
suggested or identified, inquiries were made to the manufacturers to determine
their applicability to HTHP sampling conditions.  General inquiries to experts
in the field of coal conversion instrumentation were also made.
                                     35

-------
     Finally, inquiries were made to identify process developers that might
have an immediate sampling need which could be filled as part of the EPA
program.  This included inquiries to coal gasification developers who might
have provided the opportunity to sample at their facility.

3.2  GENERAL FINDINGS OF THE SURVEY

     Several members of the Acurex staff were involved in conducting the
survey.  The complete survey results are too extensive to cover in detail.
Each phone contact was documented with a typewritten telephone memorandum and
filed chronologically.  These memorandum fill four 1-inch loose leaf
notebooks.  To condense this voluminous quantity of material, Table 10 was
constructed.  In this table, an effort was made to summarize some of the high
points of the information that was collected.  In addition to Table 10, a list
of contacts was established that includes some persons that were not contacted
directly during the survey, but who contacted us or attended conferences
related to HTHP technology.  This list is presented in Appendix A.

     Without going into details of specific contacts, the results of the
survey can be summarized as follows.

     At the time of the survey, .very few of the process developers, were aware
of the EPA-sponsored HTHP program that is the subject of this report.  Most
became interested, however, once the purpose of the program was explained.
Many asked to receive additional information regarding the equipment that was
under development.

     During the period of the survey, most of the process developers were in
the early stages of shaking down their facilities and bringing the systems up
to desired performance specifications.  In most cases, the processes had not
been developed to the point where final stage cleanup devices had been brought
online.  In a few cases, the process was currently operating on a substitute
fuel such as fuel oil or natural gas to test various operational characteristics
of the process.  In these specific instances, there was little immediate interest
in performing in-process HTHP sampling.  They did express the desire to perform
particulate sampling at some point in the future once the final cleanup devices
had been installed.  This would naturally become a necessity to evaluate the
performance of the final cleanup systems before the turbine stage could be
installed.

     Evaluation of final cleanup devices was the primary use to which HTHP
sampling would be put as expressed by the developers.  The second most often
cited need for HTHP sampling was stated to be to establish mass and energy
balances within the process.  Where the latter need was expressed, HTHP
sampling was of more near term importance to the process developer.  For
example, the viability of some processes depends upon the return of
particulate captured in the first and second stage process cyclones to the
reactor bed.

     Naturally, one means of establishing quantities of particulate leaving
and returning to the reactor is by virtue of particulate sampling.  A few
process developers even expressed the desire to be able to sample particulate


                                      36

-------
                     TABLE 10.   SURVEY  OF COAL  CONVERSION  DEMONSTRATION  FACILITIES AND  SAMPLING EQUIPMENT
       Date
      Facility
     Person
    Contacted
       Subject
                  Summary
      4/12/76    A. D.  Little
      4/12/76    ERDA
      4/16/76


      4/20/76
Radian


Exxon/Linden
00
       4/22/76    ERDA
       4/23/76    ERDA
       4/27/76    Mitre
       4/30/76    EPRI
P. Levins




G. Manning





Gene Cavanaugh


R. Hoke
                        F. Crim
                        G. Manning


                        M. Sluyter
                        J. Shang
                        M. Gluckman
       4/30/76
Gilbert Associates       W. Szwab
                                             EPA in-house sampling
                                               task
                                              Telecon  to get acquainted
                                               with George Manning of
                                               Advanced Power Group of
                                               ERDA
Low Btu Gasification  EA
Exxon pretest survey
                      HTHP  Sampling
                        (Acurex-funded)
                      HTHP  Sampling
                        (Acurex-funded)
                      Combustion  Power Granular
                        Bed  Filter  program
                      Telecon  to  identify
                        potential  coal  sampling
                        sites

                      ERDA Sampling  Survey
P.  Levins  will  discuss  the ADL role  in the
  EPA In-house  sampling program during a visit
  to RTP during week  ending 5/16.  Suggested
  a mutual visit.

Manning Interested In capability of  sampling
  inlet conditions to turbines.  Would like to
  be Invited to second  sampling session at
  Exxon.  Will  assist Acurex  1n getting into  a
  gasifier plant.

Radian has not  gotten Into their EA  to any
  great extent.  Favors open  communication.

Pretest survey  to be  held  at  end of  May.
  Facility available  for sampling on
  December 1976.

  Interested In continuous mass monitor In
  HTHP environment for  process control to
  protect turbine

Involved In MHD development.  Must sell
  uniqueness of HTHP  sampler  over conventional
  sampler.  Suggest visit  to  John Dlx, Coal MHD
  program at UTS I.  Suggests  we keep Sluyter
  informed of HTHP progress.

Chairman of Panel reviewing Combustion Power
  GBF program.   Interested in hot particle
  collection.  Indicates other possible
  sampling sites (FBC program at Rivesville,
  West Virginia, and  PFBC  program at Argonne).

"No operational full  scale gasifier  In the
  U.S.A. at present."  Gave  list of  small
  scale gasification  plants  and contacts.

  Briefed him on HTHP program
                                                                                                                                (continued)

-------
                                                             TABLE 10.    (continued)
         Date
Facility
 Person
Contacted
Subject
Summary
        4/30/76     ERDA
        4/30/76    Radian
        5/3/76      ERDA
        5/3/76      EPA/North Carolina
co      5/4/76      Westinghouse/
0°                  Waltz Mill
        5/5/76      Westinghouse/
                    Waltz Mill
        5/5/76     Radian
        5/6/76      Westinghouse
                     Research Labs
        5/11/76     Radian


        5/12/76     ERDA/Pittsburgh


        5/12/76     Spectron
                   T.  K.  Lau


                   G.  Cavanaugh





                   G.  Weth



                   W.  Kuykendal


                   D.  Keairns



                   D.  Archer



                   G.  Cavanaugh



                   Brian  Lancaster



                   F.  Mesich


                   D.  Nakles


                   M.  Fanner
                  Instrumentation  for
                    gasifiers  and  FBC's

                  Followup  on  Cavanaugh1s
                    visit to RTP
                  Recent progress  related
                    to HTHP work
                  More info on Weth  call
                  Westinghouse gasifier
                    facility at Waltz  Mill
                  Westinghouse gasifier
                  Radian's ERDA contract  to
                    make gasifier
                    measurements

                  Status of
                    gasification plant and
                    sampling

                  Radian's ERDA and EPA
                    contracts

                  Inquiry about HTHP program
                  Laser-doppler velocimeter
                      Brief discussion of HTHP program
                      Radian's Low Btu/EA still  in planning stage.
                        Discussed manner by which Acurex HTHP-TLE
                        will  interact with Radian's EA Radian
                        experts to work with Lurgi plant in
                        Yugoslavia.

                      Curtiss Wright and GE have turbine cleanup
                        contracts — Leeds and Northrup and Spectron
                        are developing particulate instrumentation

                      Bill gave some background on L & N and
                        Spectron contracts

                      Operates at 225 psi and 1600°F to 2100°F.
                        They are interested in sampling for gases
                        and particulates

                      Interested in sampling upstream of cyclone
                        — gave physical data ~ will relay needs to
                        ERDA

                      Got organization roles straight -- any future
                        work should be coordinated with Rhodes and
                        Kuykendal

                      They will be using a simple approach but want
                        to consider Acurex technology
                      Have interest in SASS train — general info
                        on ERDA activities

                      He was interested in finding out more about
                        HTHP work

                      Description of apparatus — will be testing
                        at Argonne FBC
                                                                                                                                   (continued)

-------
                                                          TABLE  10.    (continued)
        Date
      Facility
     Person
    Contacted
       Subject
                  Sumnary
OJ
       5/13/76     Leeds & Northrup         S. Katy
       5/14/76    Westinghouse/            D. Archer
                   Waltz Hill

       5/19/76    GE  Schenectedy           J. Peterson
       5/20/76     Curtiss-Wright           C. E. Irion
       5/21/76     Leeds & Northrup         Or. Muly
       5/27/76     Caltech                  R. Flagin
       5/28/76    MIT                      J. Howard
       5/28/76     ERDA/Pittsburgh          J. Biordi
       6/1/76      Univ.  of North Dakota    Gene Baker
       6/1/76

       6/1/76
EPRI

Caltech
       6/1/76      Exxon Miniplant
Don Teixeria

George Gavales


M. Nutkis
                                              Laser device to measure
                                                particulate size
                                                distribution

                                              Arrangements for trip
                                              ERDA hot gas cleanup
                                                contract
                                              ERDA hot gas cleanup
                                                contract
L & N ERDA contract
  to measure particulates


Discuss Academic contacts


Discussion of MIT coal
  gasification work


Probe sampling reports


Project Liquite


HTHP sampling problems

Cool Pyrolysis Research


Field sampling
                                                   General  info  on  program  —  suggested  a  call
                                                     to Dr. Muly
ERDA not very interested in joint program
  with EPA

Will be testing at Exxon — interested in
  sampling during tests ~ suggested we talk
  to GE gasifier people

Will be using CW PFBC, 6 atm, 1350°F to
  1700°F, using Rover turbine — interested
  in HTHP work

Will be testing at Argonne Labs — can
  measure to lu size over a 2-foot path —
  testing to begin in 8 to 9 months

  Suggested I call Howard (MIT), Gavoles
  (Caltech), England (JPL) and Teixeira (EPRI)

Has been doing sampling using water injection
  -- plans to sample at 100 atm - suggested
  call to J. Biordi at ERDA, Pittsburgh

They will send reports — interested in
  Acurex flame sampling work

General info on operating conditions
  2500 psi, 950°F high grade solid fuel

Suggested we call KVB or UCB

Doing sampling at one atm.  Using gas
  chromatograph and spectograph.

Discussed details of dimensions and valves
  required
                                                                                                                                  (continued)

-------
                                                TABLE  10.    (continued)
Date Facility
6/4/76 JPL
Person
Contacted
E. England
Subject
Sampling data
Sumnary
Flame and Combustion, and Coal-Fired

atm
6/4/76     G.  E.  Schenectedy
6/8/76     Pitsburgh  &  Midway
6/8/76     Acurex/EPA
6/10/76    PAMCO
6/14/76    Stone  &  Webster
             Boston,  MA
6/17/76    Texaco Res.  Lab.,
             Montebello,  CA

           Texaco Develop. Corp.
             New York,  NY

6/17/76    Bureau of Mines,
             Morgantown,  W.VA
6/17/76    Atomics International
             Div/Rockwell
             International  Corp.
P. Palmer,  Project
  Engineer, Power
  Cycles and fuel
J. Piatt,  Tech.
  info officer
N. Jaffe



J. Ward, Plant Mgr.




R. C. Stone



Dr. Slinger


J. Moranque, V.P.
R. Casmer,
  Hardware Eng.
A. Kohl
GE/EPRI Gasifier Project:
  GE-GASD
PAMCO's fuel processing
  plant to process low
  sulfur solid fuel from
  coal and liquid
  feedstock

Additional info on PAMCO
  fuel processing plant
  from H. Fisher, ERDA

Obtain sampling
  information for PAMCO's
  solvent Refined Coal
  Pilot Plant

Curtis Wright Fluidized
  Bed Combustor Gas-
  Turbine Project

Pilot Scale Gasifiers
  at Montebello
BuMines gasifier
Pilot Coal Gasification
  Plant at Morwalk Harbor
  Station, CO, Light &
  Power Company
  furnace sampling.  Problems with fuel rich
  regions, NO reduced by C.

Lurgi type gasifier operational, 170 psia
  1100°F, eventually 350 psia and 300°F with
  spray part.  Add-on.  Receptive to
  sampling-ports available at top of bed.

50 to 100 ton/day plant operating at
  1500 psig and 850°F.  Have sampled using
  refinery techniques (grab).
Obtained Project Report and Fisher suggested
  contact J. Ward, PAMCO regarding sampling
  techniques

Sampling for process control, sample gases
  passed thru gas chromotograph.  Liquids
  filtered and fractional distillation
  performed; interim reports forwarded.

Curtis to build small g.t. rig to test
  blade material also conceptual design
  (1977) for 500 MW utility.

No technical information published on
  gasifiers pressure and temperature as high
  as 2500 psia and 3000°F
ERDA funded.  100 to 300 psig, 1100°F to
  1300°F.  Sampling with Lear Siegler and
  Bendix gas chromatograph.

Project stopped but smaller scale plant to
  be built at Rockwell test facility, Canoga
  Park, CA in preliminary design
                                                                                                                           (continued)

-------
                                                             TABLE 10.   (continued)
Date
Facility
Person
Contacted
Subject
Sumnary
       6/18/76    U.S. Bureau of Mines,    H. Chambers
                    Pittsburgh, PA
       6/18/76     Fluor Eng.,              J. M. Moe
                    Los Angeles, CA
       6/18/76    Atomics  International    C. Trilling
                    Div./Rockwell
                    International Corp.
—'     6/22/76    Argonne  Labs
       6/29/76    Radian  Corp.
       7/2/76     U.S.  Bureau of Mines
                    Synthane Coal
                    Gasification Plant
       7/2/76     Battelle
Dr. N. O'Fallon





G. Cavanaugh


Dr. J. Strakey





W. Corder
       7/2/76     USBM Synthane  Plant      Dr. J. Starkey
                      Hydrane Gasification
                        Plant
                      Texas Eastern Transmission
                        Co. Coal  Gasification
                        years plant at
                        Four Corners,  NM

                      Molten Salt Gasification
                        Plant
Article "Monitoring Coal
  Energy Processes" in
  Processes" in Industrial
  Research, June 1976,
 . co-authored by O'Fallon

Six Lurgi gasifiers
  installed in Yugoslavia

Synthane Coal Gasification
  Plant
Ask Agglomeration Gasifier
                      Interest in sampling
                        program and fact finding
                             One  stage  process  operating  at  1000 psi  and
                               900°C.   Gas  chromatograph  of  H2,  CH4,  CO,
                               C02,  C2Hs, H20,  H2S,  C3H8.  Problems  with
                               particulate  plugging  report to be sent.

                             Design  of  26 units at 500  psia,  700°F
                               completed.   Construction delayed  2 to 3
                               due  to funding problems.
Intermittent operating experience with pilot
  plant 1 atm at 1700°F to 1900°F under
  contract to ERDA to build 5-ton/hr pilot
  plant (startup late 1977) at 1 to 20 atm
  and 1700°F to 1900°F

To send copy of Argonne report to be
  completed in next few months
Plant operates at 300 to 350 psi, interested
  in sampling (grab)

Plant to produce high-Btu pipeline gas from
  coal.  Gas cleanup by cyclones followed by
  scrubbers sampling with gas chromatograph
  downstream of scrubbers.  No interest in
  outside help with sampling.

Plant has two fluidized beds; one gasifier
  and one combustor at 100 psi and 1600°F.
  Interested in both gaseous and particulate
  sampling.

Had not started to gasify coal.  Doing their
  own sampling.
                                                                                                                                  (continued)

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                                                          TABLE  10.   (continued)
 Date
Facility
 Person
Contacted
Subject
Summary
7/2/76     Battelle ash            W. Corder
             agglomeration  gasifier
7/2/76     Morgantown Energy        A. Liberatore
             Research Center
7/2/76     Curtis-Wright            E. Garruto
7/6/76     C02 Acceptor Plant       T. Holen
7/6/76     Bi-gas                   D.  Hull
7/9/76     Radian                  6. Cavenaugh
7/9/76     McDowell-Wellman         R. Wellman
7/23/76    GE Gasifier              J.  Wang
             Schenectady

7/26/76    U.C. Berkeley            B.  Macknick
8/3/79     C02 Acceptor             T.  Holen
8/3/76     Energy Research Center    R.  Ellman
             Grand Forks
8/5/76     Curtiss-Wright
                   D.  Weller
                                         Interest in sampling
                                          program and fact finding
                                         Interest  in sampling
                                          program and fact finding
                                        Guidance  in sampling at CW
                                         Interest  in sampling
                                          program and fact finding
                                         Interest  in sampling
                                          program and fact finding

                                         Plans to  sample at CO2
                                          acceptor

                                         Wellman-Galusha gasifiers
                                        HTHP Sampling
                                         ERDA-sponsored tar
                                           characterization program
                  Sampling interest and
                    sampling plans by Radian

                  Interest in sampling
                    program

                  Sampling interest
                      Will  be fully operational  in about 2 months
                        —  1800°F and 100 psi  have been doing gas
                        sampling themselves;  will be interested in
                        sampling ahead of turbine

                      Are currently sampling  at  four locations for
                        particulate and gases — having problems
                        with tar condensates

                      Receptive to an EPA-funded sampling program
                        (95 psia, 1700°F)

                      Have done some sampling at 150 psi and 1500°F
                        particulate clogging  problems — interest in
                        gasifier overhead sampling

                      Sampling for gases, 1500 psi, 1700°F.
                        Interested in method  of  measuring char.

                      Under ERDA contract --  not sure if they will
                        be sampling at C02 acceptor

                      Identified three operational units in
                        Penn/Ohio region

                      Sampling for condensed  tars, 10 to 20 atm,
                        300°F to 600°F

                      Discussed funded program to determine vapor
                        pressure and condensation temperatures of
                      CO tars

                      Radian will make trace  element mass balances
                        for process streams under ERDA contract

                      GFERC has interest in particulate sizing on
                        the four-stage condenser

                      Desire opacity, NOX, SOX,  particulate,
                        etc., measurements
                                                                                                                           (continued)

-------
                                                             TABLE 10.   (continued)
        Date
Facility
 Person
Contacted
Subject
Summary
       8/26/76    Energy Research  Center   R. Ellman
                    Grand Forks
CO
       8/30/76    U.C.  Berkeley
       9/3/76     Environmental
                    Systems Corp.

       9/9/76     Steams-Rodger
       9/10/76    Riley-Stoker
       9/10/76    GFERC
       9/15/76    Bi-gas
       9/20/76    GFERC
       9/20/76    C02 Acceptor
       9/20/76    Westinghouse/Waltz
                    Mill Gasifier
       9/23/76    Sandia Corp
       9/24/76    Riley-Stoker
                   B.  Macknick



                   B.  Nuspliger


                   B.  Scheck


                   S.  Johnson


                   R.  Ellman


                   0.  Hull


                   R.  Ellman


                   T.  Holen


                   Suresh Tendulkar



                   D.  Hartley



                   B.  Lisauskas
                  GFERC operational  status
                    and Ellman contact with
                    ERDA

                  Tar characterization
                    study for ERDA
                  PILLS devices
                  ERDA, FBC award
                  Tar collection techniques
                  Interest in HTHP
                  Progress update on Bi-gas
                  Sampling in GFERC
                  Status of C02 acceptor
                  Tar collection at Waltz
                    Mill
                  Sandia ERDA Project
                  Tar properties
                      ERDA has  not responded to Ellman yet.   GFERC
                        currently operating at 200 psi.   Current
                        sampling needs are low.

                      Methods of tar collection, storage, and
                        handling summarized.  Possible consulting
                        arrangement discussed.

                      General discussion of product line
                      Followup call  to determine HTHP sampling
                        needs

                      Tars form fine mists they used millipore
                        filters to remove them

                      They have run  for 3 to 4 hours on lignite at
                        200 psi — will go to 400 psi in October

                      Still not operating on coal; expects to be
                        coal fired in late October

                      Ellman to call Grua for impact to his
                        decision

                      Discussed sampling operational problems tar
                        problems

                      Tars are in the 8 to 10 percent of coal feed
                        range — ESP's are effective in removing
                        mist from CG lines; property data lacking

                      Funded to provide diagnostic equipment
                        assessment for coal-fired combustion
                        processes

                      Separate by size using cascade impactors;
                        molecular wts = 300 to 800 Ib/lb-mole; also
                        gave gas properties
                                                                                                                                  (continued)

-------
                                                         TABLE 10.   (continued)
  Date
      Facility
     Person
    Contacted
       Subject
                  Summary
10/4/76
10/6/76
10/6/76
Energy Research  Center   Dr. M. F. Scharff
  Morgantown
Energy Research  Center   R. Ellman
  Grand Folks
ERDA
  Oak Ridge
10/7/79     U.C.  Berkeley
10/12/76    ERDA
11/22/76    GFERC


11/30/76    GFERC
A. Sidparo
                        B. Macknick
                        C. Grua
10/26/76    Energy Research Center   R. Ellman
              Grand Forks
10/28/76    Energy Research Center   R. Ellman
              Grand Forks
                        R.  Ellman


                        R.  Ellman
Instrumentation
  development for
  Morgantown FBC

Ellman discussions with
  with Grua re Acurex
  sampling

ERDA funding of FBC unit
  to be built at Univ.  of
  West Virginia by
  Reynolds, Smith, and
  Hills Co.

Support of gasifier tar
  studies

Acurex sampling at GFERC
                                              C. Grua's comments to
                                                N. Jaffe re HTHP
                                                sampling with EPA
                                              Sampling at GRERC
                      Sampling work
                        recommendation

                      Tar problems  at GFERC
                                                   In-bed  measurements  of  specie,  flow,  and
                                                     thermodynamic  data are  critical  to  FBC
                                                     development

                                                   Not  currently  feasible  due  to  intermittent
                                                     operation
Unit is 500 psi, 700° to 1000° steam
  produced by 10 to 90 tons/hr coal.
  system design is preliminary.
                                                                                                                             Cleanup
                                                   Macknick  to  provide  state-of-art  exchange
Inquired as to availability by GFERC site by
  sampling

ERDA/EPA expected to be cooperative.  Acurex
  should submit a WR which addresses:
  (1)  Design and (2) sampling locations of
  HTHP

Sampling spec:  200 psi, producer gas 300°F
  to 400°F, no evidence of tar (may be a
  fine mist).  Relocate sampling equipment for
  convenience.

Agreed that it did not make sense to submit
  a work recommendation at this time

Compared the effectiveness of scrubber and
  side stream sampler.  Will be making another
  run at 200 psi, if successful will run at
  400 psi.
                                                                                                                            (continued)

-------
                                                             TABLE  10.    (continued)
        Date
Facility
 Person
Contacted
Subject
Summary
      12/15/76    Molten Salt              C.  Trilling
                    Gasification Plant
       12/22/76    GFERC
en
                   0.  Mioduzewski
       12/27/76    Battelle, Ash            W.  Corder
                    Agglomeration Gasifier
       12/28/76    Bi-Gas
       12/29/76    Jaycor
       12/30/79    Westinghouse/Waltz
                    Mill Gasifier
        1/4/77     GE (Schenectedy)
        1/13/77    McDowell-Wellman
                   D.  Hull
                   M.  Scharff
                   S.  Tendulkur
                   Dr.  Ralph Wood
                     Dr.  Steven
                     Brzozowski
                   Wallace Hamilton
        1/18/77    Magna Corp, Santa Fe     Jerry Lambert
                    Springs, CA
                  Tar problems





                  HTHP update



                  Tar problems


                  Tar problems




                  Instrument developments


                  Tar problems
                  Development of a Particle
                    Impact Probe
                  Wellman-Galusha Gasifiers
                                         Corosometer
                      They don't  think  they have  a tar  problem at
                        operating temps (1700°F to 1900°F)  yet
                        they nave seen  some evidence  of tar
                        accumulation.   He  was  interested in
                        particulate  plugging problems.

                      Particularly interested  in  production rates
                        of water, tars, particulates, and gases.
                        Will provide us with tar  samples.

                      Haven't started operating gasification leg
                        yet.  Not sure  if  a tar problem exists.

                      Have just  started operating on  coal.   No tar
                        problems  observed  yet.  Feels that  high temps
                        will crack tars (1700°F/3200°F  reactor
                        temperatures).

                      Suggested  we contact GE  on  impact probe and
                        Magna Co. on corosometer

                      Currently  accumulating tars in  quench phase.
                        They are  interested in being  able to sample
                        for tars  —  especially after  combustor/
                        gasifier  leg is operational.

                      Can measure velocity and momentum of
                        particles down  to  635  micrometers.   In
                        erosion  field 15,000 to 20,000  impacts per
                        second.

                      Attempts to sample producer gas derived from
                        bituminous coal in Wellman-Galusha  gasifiers
                        have failed  due to tar accumulation

                      This instrument measures corrosion and
                        erosion  in gas  and liquid streams.   Widely
                        used; including coal gasification units.
                                                                                                                                  (continued)

-------
                                                             TABLE  10.   (continued)
        Date
Facility
 Person
Contacted
Subject
Summary
cr>
       1/18/77    Riley-Stoker             Tom Walsh
       1/19/77    Morgantown Energy        C.  C.  Shale
                    Research Center
       1/20/77    Holstein Army Arsenal     Clarence  Berryman
                    Gasifier, Kingsport,
                    Tennessee
       1/20/77    American Natural  Gas-    Dr.  Fred  Jones
       1/21/77    Stearns-Rodgers
                    (Denver)
                   Bob  Scheck
        1/25/77    Fluidynamic Devices,      Richard Wirth
                    Limited
       1/26/77    U.C. Davis               Bob Williams
       1/26/77    Pittsburg and            Dr.  Perussel
                    Midway Coal Co.
                                        Information on their
                                          gasifier
                                        Sampling of Stirred Bed
                                          Producer Gasifier
                                        Gasifier Sampling
                                        American Natural Gas Test
                                          Program at Riley-Stoker
                  HTHP Sampling and Gas
                    Cleaning
                                        Sampling at Exxon
                                        Blue Diamond Gasifier
                                        Sampling needs at SRC
                                          plant
                      The unit is a full  scale Riley-'-Morgan design.
                        7500 Ibs/hr with air and 1300 Ib/hr with
                        oxygen.   Cleanup train will  be required to
                        clean up tars.

                      Sampling attempts thus far have been
                        unsuccessful due to the inability of their
                        system to maintain high enough temperature
                        to avoid tar plugging.  Biggest problem is
                        between  cyclone and two-stage venturi
                        scrubber.

                      They own a Chapman (Wilputte)  gasifier for
                        producing low Btu gas.  They do in-house gas
                        sampling periodically.  Unit has been
                        operating for 25 years.

                      Evaluating the performance of  lignite coal.
                        Sampling will be done at 600°F.  Radian
                        involved.  American Natural  Gas is also
                        involved in an FBC test at Foster-Wheeler.

                      Stearns-Rodgers is doing E&A at Argonne Labs
                        PFBC.  He wants to be kept Informed on HTHP
                        sampling and gas cleaning.

                      A special  probe has been developed to measure
                        accurately low velocity flows (8 fps).
                        Operates on fluidic amplification principle.

                      Their walnut shell  gasifier produces complex
                        tar/matter.  Other fuels are corn cobs, tree
                        pruning  and wood chips.  Efforts to sample by
                        condensing and filtering the tars have been
                        unsuccessful.

                      They currently use a powdered coal slurry and
                        are in the process of converting to coal
                        liquifaction operation.  Perussel indicated
                        they are "clean" from an EA standpoint since
                        they have a closed system.
                                                                                                                                   (continued)

-------
                                                       TABLE  10.   (concluded)
Date
2/1/77
2/8/77
Facil ity
Hydrocarbon Research
Grand Forks Research
Person
Contacted
Harold Stotler
Robert Ellman
Subject
Sampling work on new
EPA program
Slagging Lurgi gasifier
Summary
Evaluating fuel conversion cleanup.
volve sampling in about a year.
A recent run at 400 psi resulted in

May
slagging
             Center
2/9/77     Synthane
2/11/77    Morgantown Energy
             Research Center
2/14/77    GE (Schenectedy)
2/17/77    U.C.  Berkeley
2/17/77    EPA
3/4/77


3/11/77


3/14/77


3/14/77
                        Robert Lewis
                        Al Moore
                        Clem Thoennes
                          Walt Jiles
                        Brian Macknick
                         Bruce Henshel
                      Facility  sampling  plans
                      Gasifier  stream
                        characteristics
                      HTHP  samplings  and  hot
                        filtration  application
                      Concept  evaluation  on  tar
                        collection
                      Exxon PFBC  Sampling  plans
Bi-gas,  Homer City,  PA    D.  E. Hull, et al.    Sampling requirements
Stearns-Rodgers
Argonne Labs
MERC
R. Crawford, et al.    Sampling requirements
J. Montagna
A. Moore
Sampling of Steams-
  Rodger s PFBC unit

ERDA sampling of alkali
  metals in MERC
  16" gasifier
  problems.  Their sampling system is producing
  good results without tar plugging.

Early design stage for sampling system by
  Lummis Co. based on a lab scale system.
  Anticipate tar problems.

Varying particulate loadings may make
  measurement difficult.  Light oil separation
  from water may not be possible.

They are presently reviewing HTHP sampling
  capabilities.  Current materials evaluation
  work is being performed at Exxon.

Throttling was identified as a viable
  technique for condensing tars.  A light oil/
  water separation technique was identified.
  Tar collection concepts were reviewed.

Cyclones will be used to evaluate the
  granular bed with three cut sizes below 1 urn.
  Particulate to be removed at 1600°F, 10 atm.

Present interest in solid sampling process.
  Sampling activities will come later.

PFBC facility for Argonne will require
  sampling hardware yet to be developed.

An RFP for bed and process sampling will be
  issued for the unit to be completed in 1980.

Sampling to be performed downstream of
  scrubber and hot gas cleanup atomic emissions
  spectrometer to be used for sodium and
  potassium detection.  Currently need a
  technique to separate particulate and tars.

-------
and slag in the reactor itself, a task that is beyond the current  state of  the
art.

     Several process developers mentioned problems that they anticipated would
occur or had actually occurred during sampling attempts.  A very limited
number of developers had attempted particulate sampling using very rudimentary
devices such as fixed probes and single filter traps.  At the time of the
survey, no one had produced an operational particulate sampling system of the
nature of that developed under this EPA-sponsored program.  The results that
had been obtained by the process developers in their attempts to sample were
not clearly definitive.  Most of those who attempted sampling had  encountered
problems associated with particulate plugging, tar condensation (in
gasifiers), and acid gas condensation.  Some of the gasifier developers who
had not yet attempted in-process sampling at the time did express  deep concern
about the problems that they anticipated once sampling was a requirement to
continue process development.  Most of their concern centered about problems
relating to tar condensation, probe material survival, and safety
considerations.  Many mentioned problems of tar condensation that  had occurred
within the process itself during normal operation.

     Finally, the conversation often got to the point where the process
developers asked the approximate cost of developing a sampling system that
would meet the needs of their particular process.  The response to the high
cost of HTHP probe development was generally that the process developer would
not be able to provide the required funds.  In nearly all cases the developer
responded that they would need to request the funds from the funding agency.
That is to say, the cost of sampler development had not been anticipated or
included in the development funds that were currently available.
                                      48

-------
                                    SECTION  4

                          APPROACHES TO  HTHP  SAMPLING
      In this section we will consider some of the  general aspects of  selecting
an HTHP sampling system and  its requisite components.  These discussions  are
based upon  information surveyed from the literature from direct contact with
manufacturers and other users and from experience  gained from direct  sampling
activities  during this program.

4.1  CONTINUOUS VERSUS NONCONTINUOUS SAMPLING

     In selecting a sampling system for application to a high-temperature,
high-pressure technology the first question that must be posed is that of the
exact purpose and intent for which the sampler is  to be used.  At "the present
time all of the coal conversion technologies discussed in this report
(fluidized  bed combustion, coal gasification, and  MHD) are in a state of
development.  Many different problems are yet to be resolved; however, one
very significant problem that has come to the forefront in all of these
technologies is that of particulate control.

     In the evaluation of particulate collection devices for coal conversion
systems it  is necessary to take samples both upstream and downstream of the
collection  system to establish its performance.  The information most
frequently  desired is that of total particulate concentration, particulate
size distribution, and particulate matter chemical composition.

     Two general classes of particulate sampling systems are available, those
that operate on a continuous basis (more commonly referred to as monitoring
devices) and those that operate noncontinuously or intermittently.  Monitoring
devices generally do not possess the capability of physically extracting a
sample of the particulate for chemical  -analysis.  Continuous devices tend to
be nonintrusive or in situ devices while noncontinous sampling systems tend to
be intrusive or extractive devices.  That is, they are inserted into the flow
and physically remove a sample.  A good example of a noncontinuous extractive
sampling system would be the one developed under this program for use at the
PFBC at Exxon.   Similarly, a good example of a continuous in situ monitoring
device would be an optical sampler based upon laser optical  scattering.

4.1.1    Optical Systems

     Several optical systems are currently under development by both the EPA
and DOE.  At this point in their development, these optical  devices have not
been useful as  instruments for evaluating the performance of particulate


                                     49

-------
collection systems and other portions of advanced coal conversion systems,  but
may adequately serve as monitors to determine system upsets and perform
estimates of particulate loading levels and size distribution.  A brief survey
was performed under this contract to evaluate the availability of SOA
particulate monitoring systems for application to HTHP systems.  The purpose
of the survey was, in part, to determine if any of these systems could have
been used in conjunction with the PFBC probe during the Exxon tests to compare
the performance of both.  No such attempt was made however.  The results of
this survey are presented in Appendix B.  A more detailed discussion of
optical systems for use in HTHP stream can be found in Reference 3.

     For particle size distribution determinations, extractive samplers
separate the particulate using inertial devices (cyclones or impactors) that
directly correlate to the so-called aerodynamic diameter of the particles.
Size classification by aerodynamic diameter is particularly useful in
evaluating particulate collection devices that depend upon aerodynamic
impaction behavior as their means of particle capture.  Consequently,
correlations between the operation of these particle collection devices and
particulate sampling by an extractive sampler are direct.

     On the other hand, optical systems tend to measure an effective optical
diameter.  This diameter depends, upon the optical light scattering properties
and the shape of the particle.  The particle diameter that is measured is not
aerodynamic, and some assumptions must be made to compare optical aerodynamic
data (Reference 16).  Consequently, the usefulness of optical diameter as a
means of determining particulate removal system performance is of less than
optimum value.

     Other problems must be resolved before optical systems will come into
more general usage as monitoring devices.  The operation of these systems
often depends upon the use of one or more optical windows located on the side
of the duct through which a laser beam and scattered light must pass.  The
successful operation of the device depends upon keeping the windows optically
clean.  This may be a significant problem over long operational periods with
constant exposure to corrosive gases, slag, tars, and sticky particulate
matter.  The windows can be recessed from the duct wall and a purge stream
applied as a possible means of keeping them clean.

     Another problem associated with optical monitors operating in
high-temperature streams is that the background radiation of the hot gases may
interfere or tend to mask the optical signals received by the monitoring
system.  Also optical systems may be limited to use in situations" with light
particulate loadings.  If more than a single particle occupies the measurement
volume at one time the measurement is invalid.  Also high dust loadings can
attenuate the light beam and thus limit its use.

     In summary, optical systems and extractive systems tend to be
complimentary and not competitive measurement devices at present.  The
extractive approach allows physical and chemical analysis of the sample while
optical monitors can provide process developers with on-line evaluation of
system upsets and approximate particulate loadings and size distributions.
                                      50

-------
 Future  improvement  of extractive  and  optical  systems  will  determine  whether
 the  two  approaches  will  tend  to become more competitive  as  analytical  aids  in
 process  component development.

 4.2  APPROACHES TO  EXTRACTIVE SAMPLING

     This  section discusses two topic areas:   the  design concepts  appropriate
 to fixed position sampling and, secondly,  various  means  of  designing the
 pressure containment vessel for traversing probe applications.

 4.2.1    Fixed Probe Concepts

     The question of whether fixed or movable  probes  are used depends  upon the
 application.  For most R&D work the flowfield  must be surveyed, consequently,
 traversing probes are required, whereas, fixed probes may be used  where
 surveys  are not required.  Figure 12  shows two different fixed probe designs.
 Figure 12  illustrates a  probe which is truly fixed  into  a port plate at one
 position in the duct.  It will be shown that such  an  arrangement has limited
 application.  Since the  probe is continuously  exposed to the duct  environment
 it is subject to erosive and corrosive attack, and  such failure of the probe
 may  lead to damage of downstream components.

     In  addition, some means of keeping the probe  free of particulate matter
 while not  in use must be provided or probe clogging will occur.  Two possible
methods of accomplishing this include maintaining  a constant external gas flow
 purge while the probe is not in operation.  This requires large quantities of
 purge gas.  A second approach is to turn the probe  using a  rotating  seal, so
 that the probe is facing downstream while  it is not in operation.  An external
 valve must be provided to allow a sample to be withdrawn.   After some period
 of probe use, the sample tube should be cleaned which would require  shutdown
 of the process stream for probe removal.  Consequently, the completely fixed
 probe, although simplest in concept,  lacks practicality for particulate
 sampling.  Is is more appropriate for gas  sampling  systems  free of particles.

     A retractable-fixed probe design is shown in  Figure 12(b).  In  this
 design the probe is either entirely withdrawn from  the duct or fixed at a
 single point in the duct when in use.  Once inserted  into the duct,  positive
 sealing occurs.  Purge gas is only required during  probe insertion and
 extraction.  When the probe is not in use and retracted, it is protected from
 the hot gases by the closure of a gate valve.  This type of fixed probe is
much more practical than a completely fixed version yet is  somewhat  less
 costly than a traversing system.

     When  it is necessary to survey the duct a traversing system must be
used.  Various approaches to a traversing design are considered in the
following paragraphs.

4.2.2    Traversing Probe Concepts

     Several approaches to traversing probe systems were considered  during the
course of this program.  Three basic alternatives  are shown in Figures 13,(a)
 (b), and (c).


                                      51

-------
        I
         I
                                             (a) Completely  fixed  probe
                                                                                       To particulate
                                                                                       collection  device
en
ro

                                Gate  valve





1
1 1
A
T



/'
Vt





n
'/>
i


'//tt///





T/f/f/i/,


/
. j
\f
r\



V
A
/ >

1

'/////f////f/ff/i





7J////fff/Jf//f/l




'fff//lff///ffff///
m
m\ \

nj 1
xfl-'
m\f////ff////////
\
^ s








IN

6c


'ff////ff//////fffi
i
b2

i

* f//i //(ll/f //(*/i

il
/- Seal
/
/
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1 1

II
1 r
vf/f//rr/if////\ i//r//f/ff//rr///\
y *"
/
•^- Drive mechan
                                            (b) Retractable-fixed probe
                                                                                    To particulate
                                                                                    col lection device
                                            Figure  12.   Fixed  probe  concepts.

-------
                         Closure plate
                            Sliding seal     ^ j-jple collection
                                    Traverse
                                                         Valve
               Gate  valve
Gas stream
                                                          Closure
                                                          plate
                  Probe
Sample collection
device
                                                               Valve
                         (b)
                                             Closure plate
                                                   Flexible  line
                                                 Sample  collection
                                                 device
                                                      Traverse  track
                                                      (internal)
                               Pressure containment
                               vessel
                         (O
          Figure  13.   Traversing  probe.
                         53

-------
Sliding Seal

     Figure 13(a) shows a traversing probe concept termed the sliding  seal
concept.  The principal advantage of this approach is that the physical  size
and weight of the system are considerably reduced over that of other
approaches considered.  The main .pressure housing can be made of minimum
size.  The sample probe tube must be rigid and straight to its juncture  with
the particle collection device to avoid particle deposition.
This requires that the particle collection device slide with the probe.
Having the particulate collector external permits easy access.  The sample
collection enclosure can be a pressure vessel itself or the walls of the
sample collectors can act as the pressure vessel.  Also, because the diameter
of the sliding tube is likely to be small, the blowoff loads and the actuation
requirements are minimized.

     On the negative side, the sliding tube and seal are exposed to hot
corrosive gases and particulate matter.  Sealing surfaces can quickly  degrade
under such conditions leading to a system leak.  Various means can be  devised
to protect the seal and metal surfaces such as purge systems and telescoping
shields over the sample tube.

Concentric Tube

     The traversing probe concept shown in Figure 13(b) is termed the
concentric tube.  In some respects it is similar to the sliding seal concept.
In this configuration, the sample collection device is contained within  the
inner shell that acts as the pressure vessel.  The sliding metal to seal
surface is easier to maintain in that a wiper can be employed at the forward
end of the inner tube to keep particulate and corrosive materials off  of the
outer surface of the inner shell.  The concentric tube type of design  was
employed for the Exxon PFBC probe.

     The principal disadvantages of this design are that the size and  weight
of the system tend to be large.  Also, because of the relatively large
diameter of the inner shell the blowoff loads generally will require the use
of a hydraulic or motor driven traversing mechanism.

Total Enclosure

     The third approach shown in Figure"13(c) is called the total enclosure
concept.  Here the pressure vessel is fixed and the sample tube and collection
device move on a track within the vessel.  No sliding seals are required and
since no movable surface passes through the pressure vessel, there are no
blowoff loads to overcome during traverse.  Consequently, the traversing can
be done manually using a chain drive or rack and pinion mechanism.

     The major disadvantage of the third concept is that of size and weight.
Since the vessel diameter is the largest of the three, the wall thickness and,
therefore, overall weight may be the largest.  In general, however, the  total
enclosure concept will be shorter than the concentric tube concept.
                                      54

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     Table  11 summarizes the  various  advantages  and disadvantages  of  each  of
the three concepts.  Depending upon the particular application  each of  the
three  approaches may be most  advantageous  in  a given circumstance.  In
general, however, the total enclosure approach seems to offer several
attractive  advantages.

4.2.3    Prototype Designs

     To illustrate the application of each of the design concepts  Figures  14,
15, and 16  are presented.  These schematics show three different PFBC
applications in which each of the respective  design concepts was selected.
All major system components are identified.

     In addition, Figure 17 is presented to show a schematic of the total
enclosure approach applied to a gasifier sampling system.  Figure  18  shows a
conceptual  design of the same gasifier sampling system.

     In summary, the total enclosure approach seems to offer the most
flexibility in design concept.  Internal components may be selected so  that
different sampler configurations can be achieved depending upon the
application.  For applications where sampling at a fixed location  is
permissible the semifixed concept offers the most practical approach.

4.3  PARTICULATE COLLECTION DEVICES

     Several techniques are available for use in a sampling probe  to  collect
and classify the particulate by size.  These methods include cyclones,
impactors, filters, impingers, diffusion batteries, and electrostatic
precipitators (ESP).  In designing a sampling system for use in a  HTHP
application, a selection of the most appropriate particulate collection device
must be made.  The discussion that follows is limited to the first three
devices, in that they are most commonly used  in conventional extractive
samplers and can be adapted to use at HTHP conditions.  This is not to  say
that the other devices mentioned or others not mentioned might not be
appropriate in a given situation.  For example, the ESP may provide the best
means of collecting fine tar mist when sampling at a coal gasification
facility.  This is discussed further in Section 5.3.  The reader is referred
to Reference 9 for a discussion of particulate collection devices  applied to
HTHP sampling conditions.

4.3.1    Impactors, Cyclones, and Filters

     As mentioned previously, three different types of particulate collection
devices will be considered here as the most likely to be selected for near
term HTHP sampling systems.

     Impactors generally consist of multiple stages of plates, each containing
a number of progressively smaller holes arranged in series for collection of
particles by aerodynamic diameter.  Each plate contains a number of holes
through which the particulate laden stream flows in a jet-like manner.  The
gas jet impinges perpendicular upon the plate immediately downstream of the
orifice plate.   As the flow continues downstream, the holes in each stage are


                                      55

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               TABLE 11.  SUMMARY OF TRAVERSING PROBE CONCEPTS
     Concept
       Advantages
     Disadvantages
Sliding seal
Concentric tube
•   Simple in concept

•   Light weight

•   Smallest envelope
      required for probe
      insertion/removal
    Seal is on a cold
    clean surface

    Sample collection
      device can be en-
      closed in pressure
      environment
Total enclosure
    No sliding seals
      required

    No power assisted
      transverse required

    Reasonable envelope
      required for probe
      insertion/removal
o   Seal is on probe; it
      sees the hot corro-
      sive environment.
      Not practicable for
      high temperature
      environments, there-
      fore seal must be
      protected and cooled.

•   Heavy pressure chamber

•     Requires long envelope
      for probe extraction
      extraction and removal

•   Seal diameter relatively
      large -- blow-off
      loads significant
      requiring power
      assisted traverse
      (hydraulic, or
      electric drive)

•   Pressure chamber may be
      larger in diameter
      than concentric tube

•   Overall weight large
                                     56

-------
tn
Probe rotational lever
with slip  seal
                                                             Heating/cool ing
                                                             element
                                                                                            Flow control valve

                                                                                               niter
                                                                                                       Gas
                                                                                                       environmental
                                                                                                       cell
                                                                                                    Orifice
                                                                                                    flowmcter
                                                      To Staub tube  and
                                                      thermocouple measurement
                                                      Systems (control module)
                 Probe
                 (see detail)
                                                                                         1)1tlr
                                                                                                    Traverse screw and motor
                                                                                            Quick break-down sample
                                                                                            environmental chamber,
                                                                                            cyclone and filter (with
                                                                                            heating and cooling capability)
                                       Figure 14.   Schematic of sliding  seal  sampling  system.

-------
                         . Process Duct
en
oo
                                              Enclosure
                                              (Pressure Boundary)
                                                                 Control Valves
                                                                         Flexible Line
                               rmrinnmnnnnr
                               1Heater
           Heat Tracing
                                                                                       Vent
                                                   Flow
                                                 Controls
 Organic
Collector
  Trace
  Metals
Impingers
                           Figure 15.  Schematic of concentric tube sampling system.

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                       S-type nitot tube
 Oven
heat inn
clement.
CJl
UD
                                               Heatinn element (oven)
                                                                                     Flow control' valve


                                                                                             Filter
                                                                                                            Backpressure  regulator


                                                                                                                            Oven  temp.
                                                                                                      -&«
                                                                                                                      ^-
                                                                                    —£.     -%—J$ —ff-	!
                                                                                      /^      -/      71     /
                                                                                                                                    flri rii-p I In'.-jniPi f-r
                                             Flnw con Irul oven
                                                                                                                            Disconnects
                                                                                           To nas  samnlo  01 rt,
                                                                                               ris  rouuirod
                                                                                             seo I inure
                                         Figure  16.   Schematic  of  total  enclosure sampling system.

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                                                               Shutoff valves
                                                                                Tar collector (ESP)
                                                                                   Guide rail  and trans-
                                                                                              verse drive
                                                                  Cyclone package

                                                                         Cooler
                                      Heaters and Insulation
          Heat trace


Keter valve (throttle)


   N2 purge J—IX}—O—
                    Secondary
                     tar and
               moisture collector
To vent system
                       Figure  17.   Schematic of gasifier  sampling system.

-------
                                                     -countcion noatxcT otf
           *-LOC« •*• \  \    ^—njCTCLONE P«CH«,E  \     \-t»» COLLECT
Figure 18.   Conceptual  design of gasifier  sampling system.

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made progressively smaller and the jet velocity becomes progressively
greater.  In this manner, particulate of smaller size are collected on each
stage.  A filter is usually placed downstream of the final stage to collect
the residual particulate.  Table 12 presents a list of commercially available
impactors designed for conventional operation.  The 059* cut points of each
stage are shown.

        TABLE 12.  SIZE FRACTIONATING POINTS OF SOME COMMERCIAL CASCADE
                   IMPACTORS FOR UNIT DENSITY SPHERES
                       Modified    Andersen    U. of W.    E.R.C.
                        Brink      Mark III    (Pilat)      Tag
            Stage    	
                       0.85 LPM    14 LPM      14 LPM     14 LPM
           Scalping    18-.0 ym
             cyclone
0
1
2
3
4'
5
6
7
8
11.0
6.29
3.74
2.59
1.41
0.93
0.56



14.0 ym
8.71
5.92
4.00
2.58
1.29
0.80
0.51

39.0 ym
15.0
6.5
3.1
1.65
0.80
0.49

11.1 ym
7.7
5.5
4.0
2.8
2.0
1.3
0.9
0.6
         Cyclones are also inertial collection devices.  A cyclone works
on the principle of selective sizing through the use of centrifugal
forces.  In fact, impactors also use the same effect.  In a cyclone, a jet
of particle laden gas is directed to enter the cylindrical body of the
device in a tangential fashion.  The momentum of the stream causes the jet
to form a spiraling vortex that travels down the inner surface to the
funnel-like bottom of the device.  The vortex then reverses direction and
*Particle diameter for which the collection efficiency of a given stage is
 50 percent

                                      62

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spirals upward along the centerline with the flow exiting  at  the  top.  A
sketch of a typical cyclone  is shown  in Figure  19.

     The largest of the particles present are thrown to the outer walls and
fall to the bottom of the funnel and  are collected  in a cup.  The fact that
large quantities of particulate matter can be collected in the cap  is
one of the principal advantages of cyclones over impactors.   A series of
cyclones that are progressively smaller in size can be used to size
particles.  In general, cyclones are  not capable of as small  size cuts as
impactors and also the size, cut collection efficiency characteristics are
generally not as sharp as impactors.  A comparison of cyclone and impactor
collection efficiency are shown in Figure 20.  Again, a final filter is used
downstream of the last cyclone stage  to collect the residual material.

     In some applications, it may not be necessary to classify particulate by
size during the test.  Filters can be used in cases where only the particulate
loading is desired, or when  the particulate is of such character  that it can
be sized optically after collection.  Two problems can result in  using filters
for particulate collection:  "blinding" of the filter due to  overloading and
lack of a suitably efficient filter which can survive at high temperatures.
These problems will be discussed further in the following paragraphs.

4.3.2    Suitability for HTHP Application

     In some instances, the  selection of a particular collection device may
not be wholly governed by the collection efficiency or sharpness of the size
cut of the device.  For example, the  pressure housing design of the sampler
may dictate the use of a small diameter device such as an impactor or filter
instead of a bulkier multiple cyclone system.  For example, for the type of
sampler design used in the Exxon tests described here, the blowoff loads are
proportional to the I.D. of  the outer sampler housing.  This demands the use
of a small diameter device such as an impactor train.

     Another important factor governing the selection of a sample collection
device is that of the quantity of sample required.  For instance, the quantity
of particulate that can be collected with an impactor is limited.  Once the
impactor becomes overloaded with particulate matter, the data can become
obscurred by various phenomena.  If the stage loading becomes too great, the
particulate already collected can become scoured away by the action of
particulate continuing to impact the previously collected material.  This
scouring action can also cause fracture of the already collected material, and
the smaller fractured particles can become reentrained back into the system
and be collected on lower size cut stages.

     Similarly, the use of filters limits the length of time  (or amount of
sample collected) by virtue of the filter becoming overloaded with
particulate.  As more particulate is collected, the pressure drop across the
filter rises abruptly until  the flow  is essentially stopped.  Once such a
condition is reached, there  is a great danger of tearing the filter element.

     The nonograph presented in Figure 21 is useful in quickly calculating the
time required to collect 25 milligrams of material.  At heavy dust loading


                                      63

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                   Gas out
Gas
   Bc=Dc/4




   De=Dc/2



   Hc=Dc/2


   L =2D
    C   C


   s =D /e



   Z =2D
    c   c
   J =arbitrary,

      usually D /4
      Section A-A
                     Dust ou
 Figure 19.  Generalized  cyclone  design.
                    64

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  X
  u
  z
  z
  o
                      1.0      1.5      2.0




                         PARTICLE DIAMETER / D50
3.0      3.5




   3630236
Figure 20.   Comparison  of cascade impactor stage with  cyclone

             collection  efficiency curve  (Reference  16).
                              65

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  0.001
1000
                     0.01
                                         GRAIN LOADING (GRAINS/ACF)

                                          O.'l             !)     I
                                                                           5     10
5      100
                                                      1.0   0.50.40.3  0.2     O.I 0.05 ° °4 0. 03°'°2   0.01

                                          SELECTED FLO* RATES (ACFM)
   Figure 21.   Sampling  time determination  for  total  mass collection  of 25  milligrams.

-------
conditions, the use of a filter or  impactor may be severely  impaired  by  the
very short sampling time to reach an overloaded condition.   That  is to say,  to
make the sampling time of reasonable length in a high dust loading condition,
some means of reducing the loading  to the  impactors or filters must be found.
One approach is to utilize a "scalping" cyclone ahead of the  impactor train  or
filter.  The cyclone is designed to take out  large size particulate and  reduce
the particulate loading seen by the collection device.  Such  an approach  is
effective in reducing an overloading condition in the upstream stages of  an
impactor train.

     Another criteria for selection is the ability of the device  to be
insensitive to changes in flowrate  through the sampling system.   Depending
upon the local duct velocity, to maintain  isokinetic conditions,  the  flow
through the sampler may be adjusted.  Changes in flowrate will affect the
performance or any inertial collection device.  That is to say, if the device
has been designed and calibrated at a given operational flowrate, then
excursions from that flowrate will  change  the size cuts of each impactor  or
cyclone stage.  In general, cyclones are more sensitive to deviations in
flowrate, and therefore such changes should be avoided (Reference 16).  One
means of keeping the flowrate constant'while maintaining isokinetic sampling
conditions is to change the inlet size.  This is most commonly done by using
inlet nozzles of various sizes.

     Another criteria for selection of a particulate collection device for an
HTHP application is its suitability for use based upon environmental
considerations.  For example, it is common practice to coat  each  stage of an
impactor train with a substrate material (such as grease) to  ensure initial
adhesion to the collection surface.  Most  of these materials  cannot be used  at
temperatures much beyond 400°F.  Therefore, if one were to attempt to sample
at high temperature conditions, the selection of a suitable  substrate material
may become problematic.

     Another example is the selection of a filter material that can survive  at
high temperatures.  It is difficult to find a commercially available filter
material that can be used at temperatures  above 1000°F.  On  the other hand,
if the stream is cooled prior to particulate collection, certain  species may
condense.  Depending on the stream  sampled, the amount of cooling, and the
pressure level, condensation of water vapor, alkali metal compounds,  and  acid
gases can result.  The presence of these materials in the particulate
collection device can obscure the chemical composition of the sample, plug the
collection device, or destroy the collector.

     A variety of ceramic fiber insulation materials have been tested for
filtration applications.  Most of those available in mat form are capable of
high efficiency collection of fine particles.  This is true  also of the
ceramic paper materials.  Properly supported, the fine diameter ( ~3vim)
fibers in these materials will provide absolute filter performance if suitable
thickness is used in the filter.  Most of the materials contain binders which
should be burned out prior to weighing the filter before use  to collect a
sample.  Some also contain shot or beads of ceramic material  that remain from
the fiber manufacturing process.  These beads do not impair filtration
performance but may interfere with microscopic interpretation of  the dust


                                     67

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sample.  Of the materials which are commercially available, those produced  by
ICI and known as SAFFIL fibers tend to contain the least amount of ceramic
shot and are therefore a first choice as high temperature absolute filter
materials.  Sufficient data to select candidate filter materials for test
applications is contained in Reference 18.

4.3.3    Operation at High-Temperatures and -Pressures

     Cyclones offer the greatest promise for operation at duct conditions
in HTHP applications.  Experience in calibrating cyclones or impactors at HTHP
conditions is lacking, however.  Systems must be constructed to calibrate
these devices at typical temperature and pressure conditions to fully define
their expected performance.  There are existing test facilities that have been
used for hot filtration testing (at Acurex and Westinghouse) that could be
used to perform both high-temperature and high-pressure calibration of sampler
collection devices.

     Operation at off-calibration conditions can be predicted based upon
theoretical considerations of the.variations in collection mechanisms with
temperature and pressure.  Properties of gases at high temperatures and
pressures can be found in Reference 9.

4.4  SAMPLE HANDLING AND FLOW MEASUREMENT

     In this section source general considerations regarding the choice of
design features upon sample collection are discussed.  These include the
effects of isokinetic sampling, flowfield measurement, flow conditions within
the probe, and material compatibility.

4.4.1    Isokinetic Sampling Considerations

     To accurately sample in a particulate laden stream, a representative mass
of particles must be withdrawn from the gas at the same velocity as the
particles are flowing in the gas stream.  This condition, where the velocity
at the probe inlet face is equal to the local stream velocity, is known as
isokinetic sampling.  The theoretical aspects of isokinetic sampling are
discussed in- References 10 and 11.

     To sample under isokinetic conditions, two approaches have been used.
The first is to use inlet nozzles of various sizes for different stream
velocities while the flowrate through the sampler remains constant.  In
addition, a continously variable two-dimensional inlet nozzle could be used to
avoid changing the nozzle size every time a new location in the duct is to  be
sampled.  This approach has not be in common use.  Cyclone performance is
particularly sensitive to changes in flow and individual cyclone cut points
vary with velocity, therefore, the rate of sample extraction should be nearly
constant.

     The second approach to maintaining isokinetic conditions is to use a
fixed inlet nozzle and vary the flowrate through the sampler.  Within a narrow
range this can be done even for cyclone operation, but if the flowrate
variation is considerable cyclone operation will be affected.  This can be


                                     68

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overcome by using a bypass flow system so that the cyclone always  receives  a
constant volume flow.  This becomes complex and difficult in that  each  leg  of
the bifurcated stream must be measured individually and particulate biasing
could occur.  For high-pressure applications no pump  is required,  instead an
orifice/valve combination can be used to throttle the flow to atmospheric
conditions.

4.4.2    Automatic Isokinetic Sampling

     To determine the stream velocity for isokinetic  sampling by ordinary
means it is necessary to determine the stream dynamic pressure differential,
stream static pressure and temperature.  The latter two quantities, along with
gas composition information, are necessary to determine the gas density so
that the velocity can be obtained through the Bernoulli equation.

     Potentially, there are automatic approaches to sampling isokinetically.
Figure 22 shows three of these approaches.  In Figure 22(a), the approach is
conventional in that the stream differential pressure, pressure, and
temperature are obtained.-  These are input to an analog logic circuit or
minicomputer that determines the required sampler flowrate and the flow
controller is set accordingly.  The approaches shown  in Figure 22(b) and 22(c)
do not require that the stream density be determined.  The principal of
operation requires that the static pressure of the stream be determined by  a
field probe.  At the same time the static pressure at the inlet port is also
measured.  When the static pressures at each location are equal, the
velocities are also equal and isokinetic conditions will exist.

     In developing an isokinetic flow control system, whether manual or
automatic, it is necessary to select differential pressure transducers that
are sufficiently precise to maintain isokinetic conditions to within 10
percent.  One can compute the required transducer sensitivity by calculating
the allowed error signal which will produce a predetermined error  in the
velocity.

4.4.3    Other Considerations

     When making measurements near bends in ducts or downstream of sudden
expansions or contractions, care should be taken in locating the sample
extraction site.  Ideally, the sampling location should be 8 to 10 duct
diameters downstream and two diameters upstream of such flow disturbances to
ensure that the stream is nearly uniform and well mixed.  As piping costs are
high, long straight runs ideal for particulate sampling may not be available.
When this is the case, flow baffles followed by flow straighteners may be used
to promote uniform distribution of the velocity and particulate fields.

     In designing the internal flow system of the sampler, care should be
taken to examine the distribution of temperature and pressure.  That is, as
the gas flows through the probe it should not be subjected to any sudden
changes of temperature or pressure.  For example, if locally within the probe
the flow undergoes an abrupt pressure drop, local supersonic flow conditions
might occur.  Should this occur the flow will expand locally to supersonic
Mach numbers and a sharp drop in local stream static temperature will occur.


                                      69

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            Thermocouple
 Isokinetic
 Capture
 Stream tube
                                           rzi
                                                   S-Type Probe
Sampling
Probe

  a) Analytical feedback
                                        Static Ports
         Sampling Probe
                Static Ports
                                               Field Probe
                           b)  Null  balance
  Pneumatic Pressurization
    Two-Dimensional
    Sampling Probe
                        Static Port

                          c) Variable  inlet
                                                  Static Ports
                                                          • Field Probe
Figure 22.   Automatic  isokinetic  sampling  probes.

                               70

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This may cause a phase change of some of the chemical species which may  be
present.  Such design precautions require careful calculation and examination
of the flow system in the design phase.

     Finally, in selecting materials for the probe care should be taken  that
they are compatible with the gaseous species present.  For example, special
care should be taken in selecting nonmetallic materials for seals and valve
seats.  Many of these nonmetallic materials are subject to attack by various
gases present or acids formed through the combination of acid gases and
condensed water vapor.  Reference 17 discusses materials for use in HTHP
environments.

4.5  GENERAL FINDINGS AND EXPERIENCES DERIVED FROM EXXON TESTS

     The following discussion presents a review of the test results obtained
from the two test series conducted at the Exxon Miniplant.  A more detailed
discussion of the entire test program is contained in Reference 6.  After
reviewing the" general results of the sampling tests performed at the Exxon
PFBC at Linden, New Jersey, a discussion follows that points to some
experiences that were encountered prior to and at the time of the tests.  This
discussion is presented in an effort to show the types of problems that may be
encountered in future HTHP testing so that others may learn from our
experiences.

4.5.1    Test Results -- Phase I and II

     In Section 2.1 of this report the activities and hardware development
leading to the actual testing was discussed.  A detailed discussion of the
equipment, including drawings, is contained in Reference 6.

     To reiterate, two different test series were conducted:  Phase I and
Phase II.  During the Phase I tests the objectives were to demonstrate that
the sampling approach taken was a viable one from the standpoint of data
accuracy and repeatability and that the sampling system was safe and reliable
in use.  During test Phase I three sampling runs were made:  one (Run 2) using
a thimble filter to collect the total particulate catch and two additional
tests (Runs 2 and 3) using a cascade impactor -(containing seven stages)
followed by a final filter.  The following types of data were recorded during
the Phase I tests:

         Particulate size distribution
         Particulate chemical composition
         Particulate shape
         Particulate concentration
         Process temperature and pressure
         Moisture content
         Structural temperatures (valves and probe housing)
         Trace element samples
         Organic samples
                                      71

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Phase I Tests

     Table 13 shows the test conditions present during the three runs
comprising Phase I testing.  The bed temperature was typically 300°F higher
than the duct temperatures at the sampling location.  Typical wall
temperatures recorded during Run 1 are shown in Table 14.  The total
particulate concentration from the other test runs are shown in Table 15.
Here the most accurate reading (1.58 g/m^) comes from Run 1 where the bulk
filter was used.  This is because a longer sampling period was used and bulk
filter catches are less subject to cumulative errors associated from weighing
the catches from the eight stages of particulate catch in test Runs 2 and 3.
A weight breakdown by impactor stage plus final filter particulate collected
during Runs 2 and 3 is presented in Table 16.  A cursory examination of this
table shows that the predominance of particulate collected was in the 1-10 ym
range.

     Figure 23 summarizes the results of Runs 2 and 3 of Phase I testing.
Particulate distributions ranged from 0.3 to 30 ym in aerodynamic diameter.
These curves were constructed directly..from the D$Q cut points of the series
impactors used.  A temperature correction for the operating temperature of
450°F was applied based on theoretical considerations.  The effect of
pressure on the operation of the series impactors was determined to be small
based on theoretical considerations.  The repeatability of the data as
exhibited by Figure 23 was deemed to be good for a first demonstration.
Figure 24 shows the particulate collected on the substrate material during
Run 3.  A closer examination of stage 3 in Figure 25 shows the classic
"pyramids" of particulate collected.

     The particulate sample from Run 2 was subsequently examined using a
scanning electron miscrscope.  An example of the particulate is shown in
Figure 26.  From this photo it is evident that the particulate is somewhat
fused together so it is difficult to correlate the physical size to the
impactor cut size.  The samples were chemically analyzed using a dispersive
X-ray fluorescence analyzer.  Later a SSMS examination was performed in the
analysis of Phase II results and Phase I, Run 1, results as will be explained
below.

Phase II Tests

     A total of four test runs were made during Phase II of testing.  The
samples from Run 3 of Phase II were retained for SSMS analysis.  Table 17
shows the results of the SSMS analysis from Run 3 of Phase II.  Examination of
the table shows that the quantities of material obtained on the downstream
filter were inadequate to make a meaningful comparison to the quantities
contained in the scalping cyclone and upstream filter.  This was because the
upstream filter removed a great bulk of particulates.  In addition the
downstream filter was subject to some contamination as will be discussed
later.  To resolve the problem of lack of sufficient sample quantity a
comparison was made with the chemical composition of the bulk filter catch
from Run 1, Phase I.  Since the test conditions were virtually identical the
results should be, it was reasoned, equally valid.
                                      72

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TABLE 13.   PHASE I  TEST CONDITIONS

Date
Time
Ambient temperature
Bed Conditions
Temperature
Pressure (gage)
Ca/Sulphur Ratio
Excess Air
"Coal
Dolomite
Flowrate - sm /m1n (scfm)
Average Duct Velocity -
m/s(ft/sec)
Run: 11
3-31-77
3:30 p.m.
18°C (64DF)
900°C (1650°F)
912 kPa (9 atm)
1.25
301
Champion
Pfzlzer
14(544)
2.0(6.7)
12 13
4-1-77 4-1-77
10:30 a.m. 2:40 p.m.
2TC (70'F) 19°C (67eF)
900eC (1650°F) 900'C (1650°F)
912 kPa (9 atm) 912 kPa (9 atm)
1.25 1.25
30t 30S
Champion Champion
Pfzlzer Pfzlzer
14(546) 14(546)
1.9(6.3) 2.0(6.7)

TABLE 14. STRUCTURE TEMPERATURES
Time
0
10 min
20 min
60 min
Valve-
Probe
Side
64°C(147°F)
71°C(159°F)
69°C(157°F)
88°C(190°F)
Inner Outer
Probe Probe
Housing Housing
56°C(133°F) 56°C(133°F)
55°C(131°F) 68°C(154°F)
56°C(133°F) 75°C(167°F)
N/A N/A
               73

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TABLE 15.   PARTICULATE CONTENT










Date:
Time:
Particle Catch:
(grams)
Filter
Impactor
Residue
.Total
Sample Volume:
m'tscf)
Particle Content:
(g/m'Mgr/scf)
Particle content:
(g/rr'Kgr/scf)
(Anisokinetic
Correction Applied)
TABLE 16.
Run 11
3-31-77
1530

3.2515
-
1.8565
5.108
3.22(122.5)
1.58(0.64)
1.60(0.65)
PARTICLE SIZE
Run 12
4-1-77
1030

-
0.0554
0.0334
0.0884
0.082(3.13)
1.06(0.43)
1.08(0.44)
DISTRIBUTION
Run 12
Stage
1
2
3
4
5
6
7
Filter

°50 Weight
Microns Collected
26.0 0.0076
12.0 0.0080
4.3 0.0171
2.1 0.0139
1.2 0.0022
0.6 0.0036
0.3 0.0020
(LOOK)
0.0554 grams
I Total I Weight
Weight Smaller Collected
13.7 86.3
14.4 71.8
30.9 41.0
25.1 15.9
4.0 12.0
6.5 5.4
3.6 1.8
1.8
0.0093
0.008
0.0221
0.0215
0.0135
0.0081
0.0039
0.0028
Run 13
4-1-77
1500

-
0.0892
0.0595
0.1497
0.132(5.03)
1.13(0.46)
1.16(0.47)

Run 13












I Total I
Weight Smaller
10.4
9.0
24.8 .
24.1
15.1
9.1
4.4
3.1
89.6
80.6
55.0
31.7
16.6
7.5
3.1

0.0892 grams
             74

-------
   100
   to
   60

   40
   20
                10
                       PERCENTAGE UNDERSIZE (BY WEIGHT)
                       20   30   40   SO  60   70   60
                                                     •90
5
5
   1.0
   06

   0.6

   04
   o.:
                00     60   TO   60  SO  40   30
                           PERCENTAGE OVERSIZE
                                                20
                                                      10
 Figure  23.   Particle  size distribution  --  Phase I tests,
                                   75

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                 j EXXON-HTHP
                 I    4/1/77   j
                     RUN 3
                   | EXXON-HTHP j
                   I    4/1/77   j
                      RUN 3
Figure  24.   Impactor  substrates,
                76

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Figure 25.  Inipactor substrate  Run  3,  Stage 5.

-------
                     1000X
                   •!  10 microns
                     3000X
             '-«—«-l  3 microns
Figure 26.  Particle photomicrographs, Stage  4.
                     73

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                         TABLE 17.   CONCENTRATION OF  ELEMENTS  IN FLYASH SSMS ANALYSIS  (PARTIAL)
ID

Element
K
Na
Rb
A1
SI
Fe
Ca
Mg
T1
Sr
Ba
An
All
P
Cu
Zr
Nt
Cr
Pb

Cyclone
(ppm)
8.200
1.310
< 70
67
. /
164.000
94.000
30.000
20.000
11.400
2,430
810
710
276
248
160
120
< 90
85
TEST i
Front
(ppm)
8.850
2.500
< 68
94.000
82.600
13.400
19.000
17.800
1,950
555
694
223
165
140
100
< 140
75
n - PHASE II
Rear
(ppm)
15.1
< 135. *
< .43 *
< 62 *
64.2
<2510. *
60.
< 6.6 *
38.
7.1
.6
< 5.0
( 1 A
^ 1 . H
< 224. *
< 1.5 *
< 2.1 *
5.8
< 13.1
< 4.0 *

Rear Blank
(ppm)
5.4
91.
.13
6.4
1210.
2.36
7.3
5.9
3.1
1.15
1.5
68.
.91
.64
.29
6.4
1.2
PHASE I
Bulk Filter
(ppm)
16.250
3.560
866
8 a
• o
Major
310.000
36.300
44.000
28.600
10.600
1.320
1.080
213
C 1 J
1.880
142
334
348
366
86
                 Notes:  < - natural background limited detection limit
                        <* - blank limited detection limit

-------
     To reiterate the major objective of the Phase  II tests was  to  determine
if alkali metal compounds would condense out of the stream if the sample was
cooled to 450°F.  Table 18 shows a summary of the results obtained  from
Phase II tests.  The results are shown in a dimensionless form,  normalized by
the iron and magnesium content of the coal.

     A comparison is made of the ratio of nondimensional quantities caught
"hot" and caught "cold."  These results showed no consistent evidence of
alkali metal condensation occurring as a result of  sample cool down.  The
results are not totally conclusive, however, and the amount of data is
limited.  To avoid future uncertainties arising over whether the sample can be
cooled prior to collection, it is advised that in most future test  programs
the particulate be collected at duct conditions.  This will require the
development of particulate collection devices that can be operated  and
calibrated at high-temperature and -pressure.

     In summary, the Exxon tests produced good results and demonstrated that
the sampler design worked well.  In the course of obtaining these positive
results several considerations and experiences were identified that require
discussion.

4.5.2    Experiences Derived from Exxon Testing

     In the course of planning and performing the tests at the Exxon Miniplant
the following problem areas were identified.

     Probe alignment problems were encountered during the first  test phase.
Such problems can be expected when the probe is very long and the clearances
through the isolation valves are tight.  The S-type pitot probe  tube was
damaged during insertion.  Hydraulic actuation makes the danger  of  such damage
greater since all "feel" is gone.

     Double gate valves were used for probe isolation during the Exxon tests.
It is felt that a double valve approach is safer and increases system
reliability.  During Phase I testing, some problems were encountered from the
leakage past the valves.  The problem was narrowed down to the fact that
particulate was accumulating in the bottom of the value seat with the gate
moving down vertically into the seat.  The problem was solved by rotating the
valve so that the particulate did not accumulate in the bottom of the valve
seat.

     During the condensation tests (Phase II), a flow control valve was
located upstream of the downstream (cold) filter which was outside of the
probe housing.  A problem was encountered when the heat tracing  on  the tube
downstream of the valve was unable to compensate for temperature reduction due
to the throttling effects of the valve.  As a result, the catch  in the
downstream filter was contaminated with sulfuric acid condensate because of
the sudden drop in temperature.  A subsequent analysis of sulfuric  acid
condensation limits bore out this conclusion.  In addition, the  throttling
valve seat material was apparently attacked by the sulfuric acid that further
contaminated the downstream filter.  As a result in future tests care should
be taken to ensure that abrupt temperature drops do not occur and that all


                                      80

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TABLE 18.   PARTIAL COMPARISON OF FRONT AND REAR PARTICULATE
           CATCHES FROM EXXON TEST SERIES I AND II

K
Fe
Na
?₯
S1
Fe
Ca
FT
Ma
Fe
Sr
Fe
Ba
FT
K
Rg
Na
Mg
SI
Hg
Fe
Mg
Ca
Mg
Sr
Ba
M?
Phase I Tests
Bulk Filter
0.45
0.10
8.54
1.23
0.79
0.04
0.03
0.57
0.12
10.84
1.27
1.56
0.05
0.04
Phase II Tests
Cyclone Front Filter
0.27
0.04
3.13
0.67
0.38
0.03
0.02
0.72
0.11
8.25
2.63
1.75
0.07
0.06
0.66
0.19
6.16
1.42
1.33
0.04
0.05
0.50
0.14
4.64
0.75
1.07
0.03
0.04
Ava.
0.47
0.12
4.65
1.05
0.86
0.04
0.04
0.61
0.13
6.45
1.69
1.41
0.05
0.05
Ratio
0.96
0.83
1.84
1.17
0.92
1.00
0.75
0.93
0.92
1.68
0.75
1.11
1.00
0.80
                           81

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valve seat materials be carefully selected for compatibility with the  species
present.

     Finally, the question of safety cannot be overemphasized in HTHP
sampling.  Fortunately, no severe safety problems occurred during the  Exxon
tests.  It should be recalled that if large system leaks were to occur the
gases escaping would accelerate to supersonic velocities upon expansion.  Not
only are the hot escaping gases dangerous but the erosive effects of the
particulate exiting at these high velocities could be disastrous to persons or
equipment in the area.

     In future tests at coal gasification facilities, the safety problems are
even greater.  In addition to the problems already mentioned, if a leak
occurred the danger of an explosion is very real.  Also, many of the
constituents present may be carcinogenic depending upon the sampling location
in the process.

4.6  BEYOND PROTOTYPE SYSTEMS

     The sampling system designed and tested in this program exemplified the
prototype approach.  The design of the probe hardware utilized approaches
employed to ensure proper operation in a first-of-a-kind sampling exercise.
Now that the general approach has been demonstrated at least at an PFBC
facility we can look to some of the questions affecting the development of
more general purpose sampling equipment designed to meet a wider variety of
applications.  It should be emphasized that to some extent this discussion is
premature in that prototype sampling systems have not yet been demonstrated in
coal gasification or MHD applications.

4.6.1    Generalized Sampling Systems

     One might conjecture that it would be valid to assume that a general
purpose HTHP sampling system could be constructed that would serve a wide
variety of purposes.  Indeed such systems as the SASS are used in a variety of
ways in conventional sampling applications.  This approach is not entirely
viable for HTHP coal conversion system applications.

     For example, temperatures and pressures may vary from 1000 to 3000°F
and 1 to 100 atm depending upon the application.  The wide range of
temperatures (and for that matter pressures) will dictate when the probe
surfaces must be protected by cooling, since the temperature, pressure and
velocity strongly affect the heat transfer coefficient.  Therefore, over a
wide range of conditions the cooling requirements may be drastically
different.  Also the pressure level (and for that matter temperature) will
dictate the pressure vessel design considerations.  Consequently, from the
standpoint of pressure and temperature, the system would have to be
considerably overdesigned with respect to cooling (if required at all, in many
applications) and pressure vessel strength.
                                      82

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     Gaseous constituents would greatly dictate the choice of materials.
Gases present  in reducing environments are considerably more corrosive to
metal parts than those found in oxidizing environments.  These also combine
with operating temperature and pressure levels in selecting probe materials.
Consequently, material for a generalized probe would be of an exotic nature to
cover the most extreme conditions.

     Other considerations would tend to thwart the design of a general purpose
sampling system.  If a general purpose sampler is designed it must be capable
of traversing over a wide variety of duct sizes ranging from a few inches to
several feet.  This is a particularly awkward situation that confronts a
generalized system approach.  If a probe is designed to traverse a maximum
5-foot duct it is likely to be oversized to sample in a one foot duct.
Constraints such as the total available external operating envelope are likely
to restrict the use of an oversized probe system in many applications.

     Duct velocity and particulate loading are other parameters which make the
generalized design approach difficult.  If the probe and particulate
collection devices are designed for some maximum anticipated condition then
when sampling conditions at the opposite end of the spectrum, nozzle sizes,
isokinetic considerations, and sampling times are likely to become untenable.
For example, if the particulate collection device is designed to collect
particulate at a high dust loading and high velocity condition in a matter of
a few minutes of sampling time, then it might take hours to collect a
representative sample at a low dust loading, low velocity condition.

     Based upon the arguments delineated above it is easy to see why each HTHP
sampling application demands a custom approach to some extent.  It is
therefore unlikely that a single sampling system can be used in all or even
most PFBC applications for example.  This is not to say that a given probe
design can only be used in a single application, facility, or location in the
process stream.  It is also likely that a given design can have multiple
uses.  But it is impractical to consider the generalized design approach for
HTHP applications.  This explains one of the inherent reasons that costs for
producing a HTHP sampling system are high.

4.5.2    Modular Approach

     There is another approach to the design and fabrication of HTHP sampling
systems that offers a means of reducing costs.  Rather than consider a
generalized design approach, a modular approach can be taken.  In the modular
approach the design aspects of each of the major sampling system components
(probe housing, traversing mechanism, collection devices, cooling system, flow
control  system, etc.) can be refined to a point where sampler design can be
simplified.

     Design guides for each of the major systems would be developed,
calibrated, and tested separately.  Principals would be defined for
extrapolating these designs to other situations.  For example, a comprehensive
program to develop and calibrate HTHP cyclones over a wide range of operating
conditions would allow the designer to quickly select a design applicable to
his particular set of conditions.  Similarly, for coal gasification


                                      83

-------
applications a program could be developed to perfect a tar collection device
with design parameters identified so that the probe designer could match his
application.  In this manner, each new application would become  less of a new
development program and more of a predictable design exercise.   A modular
approach could not be full proof to the point where acceptance tests would not
be required, however.

     To some extent the modular approach was demonstrated during the Exxon
tests.  The internal and external configuration of the probe was modified from
the original using the impacter train to the Phase II configuration that
employed the scalping cyclone and dual filter arrangement.  This was a good
example of the versatility of the modular approach.

4.6.3    Other Desirable Features

     In the course of the period of performance of this contract at least two
process developers expressed the desire to have one or both of two automatic
features.  These were (1) an automatic isokinetic capability and (2) an
automatic traversing capability.  In both cases the reasons for  these desired
features were to (1) improve system accuracy (2) lessen sampling time and (3)
reduce the number of required operators.

     For long term process development situations at least one process
developer felt that the trade of the cost of automatic systems would be cost
effective in terms of reducing the operator labor required.  This will not
always be the case.  But once the automatic systems are developed their use
may become cost competitive in a wider variety of applications.
                                      84

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                                   SECTION 5

          REVIEW OF PARTICULAR PROBLEMS ASSOCIATED WITH HTHP SAMPLING
     In the previous sections several problem areas pertaining to HTHP
sampling were discussed.  In this section a few of those areas will be
reviewed and elaborated upon.  Based upon the current state of HTHP sampling,
some recommended solutions to these problems are offered.

5.1  PF3C SAMPLING

     Two areas defined as potential problem areas based upon direct experience
gained in this program are (1) pressure containment and (2) condensation
effects.

     A satisfactory means of containing high pressure levels ensuring safety
and ease of operation remains a problem.  Based upon the experience gained  in
actual tests and studies performed during the period of this contract, a
proposed means of pressure containment has evolved.  In future sampler designs
where traversing is required, it is proposed that the best means of containing
high pressures is by use of the total enclosure concept as discussed in
Section 4.2.  The elimination of all sliding seals and power-driven traversing
mechanisms make this approach very attractive.  The technique remains to be
proven in practice, however.  There are potential problems relating to
maintenance of the internal components, and these must be put to test in
practice.

     Some problems of probe condensation effects were encountered during the
Exxon tests.  At times, controlled condensation might be desirable to remove
water vapor or acid gases.  The question of alkali metal condensation remains
open to discussion.  Special care should be taken in analyzing and designing
the internal flow system so that pressure and temperature distributions can be
determined beforehand.  If abrupt temperature drops are unavoidable, then flow
passages should be adequately heat traced to avoid condensation.  The best
approach is to collect the particulate at stream conditions then drop the
pressure and temperature after collection.

5.2  GASIFIER SAMPLING

     The problem areas discussed in Section 5.1 pertain equally to gasifier
sampling.  In fact, these problems are accentuated in some gasification
processes.  As discussed earlier, the operational pressure levels in some high
Btu gasification processes far exceed those in PFBC processes.  Therefore,
                                     85

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pressure containment is a very difficult problem for sampling  in gasification
facilities.

     In addition, as discussed previously, condensation of volatiles from the
gasification process presents a problem not only from the standpoint of
collecting samples, but also as it relates to the pressure containment
problem.  For example, sliding seal approaches (see Section 4.2) may prove
untenable in gasifier environments.  The seals would be subject to attack from
the acid gases present, and tar condensation could foul sliding seal
surfaces.  Hence, it appears that the best approach to pressure containment
for gasifier sampling is the total enclosure approach.  Again, this
recommendation is subject to verification by test.

     Of course the other major problem confronting the design of a gasifier
sampling system is that of collecting tar mist separate from the solid
particular matter.  Some of these problems were discussed in Section 2.2.
Reference 4 discusses the various approaches considered to collect the tar
mist once it has been condensed from the stream.  Again, the approach would be
to maintain the sample at the process stream temperature and pressure where
the volatiles are in a vapor state, collect the solid particles, then drop the
temperature and pressure to form a tar mist and subsequently collect the tar
mist.  Most of the devices (scrubbers, impingers, cyclones, filters, etc.) for
collecting the tar mist mentioned in Section 2.2 and discussed in detail in
Reference 4 are not efficient and are subject to plugging.  The exception
would be the ESP that has been successfully used to collect tars in large
industrial applications.  The condensation properties of tars must be better
defined to properly design a small ESP collector.  Work sponsored by DOE has
been underway for some time at the University of California at Berkeley to
characterize the chemical and condensation properties of gasification tars
(DOE Contract DE-AC01-79ET14-884, Dr. J. M. Prausnitz -- UCB).

5.3  OTHER APPLICATIONS

     Two other possible applications for HTHP sampling were mentioned in this
report:  MHD exhaust sampling and catalytic cracker sampling.  Both of these
areas present new challenges for HTHP sampling technology.

     For MHD sampling the major problem is sampling at high temperature
(2200°F) in an erosive environment.  Also the application calls for a fixed
probe approach.  The recommended solution was to make the sample tube and
cyclone collection device of ceramic material.  The ceramic would be
temperature and erosion resistant.  The ceramic fabrication approach offers
promise for other applications also.  However, ceramics are subject to thermal
shock failure and means must be devised to avoid such a consequence.  Again,
prototype development of a ceramic system should go far to prove the concept.

     The other application, sampling at a catalytic cracker, is a lower
temperature application.  Here ceramic fabrication techniques are not
required.  Although fixed point sampling is the only requirement the high
velocity erosive environment dictates that the probe be removed from the
stream while not in operation.  Here the proposed solution as discussed in
Section 4.2 is to use the semifixed housing design approach.

                                     86

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                                   SECTION 6

                        CONCLUSIONS AND RECOMMENDATIONS
     The scope of the program undertaken was very comprehensive.  The major
effort that of the demonstration of HTHP sampling at the Exxon Miniplant was
successful.  The design and testing of this apparatus provided valuable
insight into some of the problems of HTHP sampling.

     The design, analysis, and testing of an HTHP sampling system can be an
expensive proposition.  The system components are complex and constant
attention must be placed upon compatibility the process stream constituents
and safety aspects.  Short cut approaches to HTHP sampling are not advised.

     In addition to the conclusions drawn above, the other portions of the
program especially the SOA review led to several conclusions.  At the time of
the survey of process developers not many had begun to consider their needs
for HTHP particulate sampling.  As their systems approach further states of
development especially with respect to cleanup devices, a clearer list of
sampling requirements will develop.

     Some special problems were identified during the SOA review.  One problem
that must receive further attention is that of development of system
components for coal gasification sampling.  The selection of materials
compatible with gaseous constituents poses only one problem.  Tar separation
and collection presents another problem area which must be addressed prior to
taking the next big step to coal gasification sampling.  Perhaps a
conservative approach would be to develop a sampling system designed for
operation at an atmospheric gasifier.  After a successful demonstration
further development for sampling at both high temperature and pressure could
be considered.  Safety considerations for gasifier sampling should receive
foremost attention to ensure the safety of the operators and the plant
equipment.  Perhaps a separate program aimed at the issue of safety for this
application is appropriate.

     Another area that requires further attention is that of modularization of
design.  For most applications the HTHP sampler design tends to be customized
to the particular application.  However, certain components such as pressure
vessels, impactors, cyclones filters, ESPs, etc., could be designed and
laboratory tested as individual components.  Once these basic components are
developed, deviations for particular applications would become more routine.
This modular approach in which separate components would be designed, proof
tested, and calibrated offers the best solution towards reducing total system
costs to future users.
                                     87

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     To bring HTHP sampling into more common usage, further cost reductions
must be achieved.  Although process developers may decide to develop sampler
technology and carry the burden of the system development costs government and
private research agencies (DOE, EPA, EPRI, IEA, etc.) also have specific needs
for such equipment.  These organizations will probably carry out the
technological development of these systems to the point where most of the
costs have been absorbed prior to sale to the user.

     Finally, there appears little doubt that emerging coal conversion
technologies (PFBC, coal gasification and liquification, MHD, etc.) will
require on-line HTHP extractive particulate sampling within the next 1 to 2
years.  Development of advanced HTHP sampling systems need to get underway now
so that they will be available at the time they are needed.  The corresponding
development of particulate cleanup systems are the pacing item with regard to
when these sampling systems will be needed.  The completion of this program is
only the beginning of the development path outlined above.
                                     88

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                                   REFERENCES
i.   Meyer, Jr., P., and M. S. Edwards.  Survey of Industrial Coal Conversion
     Equipment Capabilities:  High-Temperature, High-Pressure Gas
     Purification.  ORNL/TM-6072, June 1978.

2.   Sverdrup, E. F., P. H. Archer, M. Merguturic.  The Tolerance of Large Gas
     Turbines to 'Rocks,1  'Dusts,' and Chemical Corrodants.  EPA-600/9-78-004,
     March 1978.

3.   Coleman, H. W., et al.  U.S. Environmental Protection Agency Interim
     Report: Diagnostic Assessment for Advanced Power Systems, SAND 77-8216,
     March 1977.

4.   Cooper, l., et al.  Measurement of High-Temperature, High-Pressure
     Processes:   Annual Report, EPA-600/7-78-011, U.S. Environmental
     Protection  Agency, January 1978.

5.   Blake, D. E.  Source Assessment Sampling System:  Design and
     Development.  EPA-600/7-78-018, U.S. Environmental Protection Agency,
     February 1978.

6.   Masters, W., R. Larkin, L. Cooper, and C. Fong.   Sampling System for
     High-Temperature,  High-Pressure Processes.  U.S. Environmental  Protection
     Agency, EPA-600/7-78-158, August 1978.

7.   Masters, W., R. Larkin, and L. Cooper.  A Particulate Sampling  System for
     Pressurized Fluidized Bed Combustors.   Paper presented by L. Cooper at
     the West German Workshop on Particulate Technology in March 1978.

8.   Dravo Corporation.  Handbook of Gasifiers and Gas Treatment Systems.
     FE-1772-11, Pittsburgh, Penn., February 1976.

9.   Szwab, W.,  W.  H. Fisher, and B. N. Murthy.  Technical Support for  Coal
     Conversion  and Utilization:  Techniques for Particulate Sampling and
     Measurement from Gasifiers at High-Temperatures  and High-Pressure.
     FE-2220-5,  December 1976.

10.   Vitols, V.   Theoretical Limits of Errors Due to  Anisokinetic Sampling of
     Particulate Matter.  IAPCA Journal,  February 1966.

11.   Parker, G.  J.   Some Factors Governing  the Design of Probes for  Sampling
     in Particle and Drop Laden Streams.   Atmospheric Environment, 1968.

12.   Survey of Coal Conversion Demonstration Facilities and Sampling Equipment
     - Telephone Survey conducted in 1976 and 1977 documented in this report.

13.   O'Fallon, N. M., and L. G. LeSaye.  Coal Conversion Instrumentation.
     Industrial  Research/Development, June  1978.
                                     89

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14.  Cooper,  B.  R.   Research Challenge:   Clean Energy from Coal.   Physics
     Today,  August  1978.

15.  Kuykendal,  W.  B.   Instrumental  Techniques for  Industrial  Source
     Particulates.   Presented at the West German  Workshop on  Particulate
     Technology, March,  1978.

16.  Smith,  W.  B.,  P.  R.  Cavanaugh,  R.  R. Wilson.   Technical  Manual:   A Survey
     of Equipment and  Methods for Particulate Sampling in Industrial  Process
     Streams.   EPA  600/7-78-043, U.S.  Environmental  Protection Agency, March
     1978.

17.  Hull,  J.   Materials  for Use in  High-Temperature/Pressure  Hostile
     Environments.   EPA  600/9-78-004,  U.S.  Environmental  Protection  Agency,
     September  1977.

18.  Shackleton, M. A.  High-Temperature, High-Pressure  Particulate  Control
     with Ceramic Bag  Filters.   EPA  600/7-78-194, U.S. Environmental
     Protection  Agency,  October  1978.
                                     90

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                 APPENDIX A



HIGH-TEMPERATURE, HIGH-PRESSURE MAILING LIST
                      91

-------
          HTHP MAILING LIST
N. Abuaf
Brookhaven National
Upton Long Island
New York,  11973
Laboratory
Richard L. Adams
Wheelabrator-Frye Inc.
600 Grant Street
Pittsburgh, PA  15219

Jeffery C. Alexander
M.I.T.
Room 36-323
Cambridge, MA  02139

Gerald L. Anderson
Institute of Gas Technology
3424 South State Street
Chicago,  IL  60616

Herman B. Anderson,  Jr.
General Services Administration
Region 3, PBS
Technical Field Office
7th & D Streets, S.W.
Washington, D.C.  20407

Dr. John W. Anderson
Rexnord,  Inc.
1914 Albert Street
Racine, WI  53404

Larry W. Anderson
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA  94042

Stig Andersson
STAL Laval
S-61320 Finspong
Sweden

Francis M. Alpiser
Chemical Environmental Engineering
EPA III - AHMD-SIP
Sixth and Walnut
Curtis Building MS-3A-H11
Philadelphia, PA  19106
Jim Abbott
EPA
IERL-RTP
Research Triangle Park, NC

D. H. Archer
Westinghouse
Beulah Road
Pittsburgh, PA  15235

Ted Atwood
Process Engineering
Department of Energy
Room 504
20 Massachusetts Avenue
Washington, D.C.  20545
                                      - B -

                      W.  D.  Bachalo
                      Spectron Development Labs
                      3303 Harbor Blvd.
                      Costa  Mesa, CA  92626

                      Roland Beck
                      Department of Energy
                      7374 S.  Forest
                      Whittier, CA  90602

                      Robert W. Bee
                      Consultant
                      126 Hopeland Lane
                      Sterling, VA  21170

                      Albert J. Bevolc
                      Associate Physicist
                      US  Department of Energy
                      Ames Laboratory
                      A205 Physics
                      Ames,  IA  50011

                      Dr. Suresh P. Babu
                      Institute Gas Technology
                      3424 S.  State Street
                      Chicago, Illinois  60616

                      E.  T.  Barrow
                      Ministry of the Env.
                      Air Resources Branch
                      44880  Bay Street
                      Toronto, Ontario MS5 128
                      Canada
27711
                                     92

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Walter A. Baxter
Environmental Elements Corp.
P. 0. Box 1318
Baltimore, MD  21230

K. Bekofske
General Electric Co.
CR&D  -
P. 0. Box 8
Schnectady, NY  12301

Michael Beltran
Beltran Assoc., Inc.
1133 E. 35th Street
Brooklyn, NY  11210

Paul A. Berman
Westinghouse Electric Corp.
P. 0. Box 9175, Lester Branch
Philadelphia, PA  19113

Dr. Samuel Bernstein
Flow Research Co.
P. 0. Box 5040
Kent, WA  98031

Prem Sagar Bhardwaja, PhD
Lawrence Berkeley Laboratory
University of California
Berkeley, CA  94720

Charles E. Billings
Environmental Engineering Science
740 Boylston Street
Chestnut, MA  02167

Samuel 0. Biondo
Federal Power Commission
825 N. Capitol Street, N.E., Room 5008
Washington, D.C.   20426

David Blake
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA  94042
Dale Blann
Acurex/Aerotherm
3301 Woman's Club Drive
Raleigh, NC  27611
Frederic L. Blum
Research-Cottrell Inc.
P. 0. Box 750
Bound Brook, NJ  08805

B. H. Bochenek
U. S. EPA
401 M. Street, S.W. (A-134)
Washington, D.C.  20460

Dr. R. Boerieke
General Electric Co.
Building 2, Room 712
One River Road
Schnectady, NY  12345

Dr. R. H. Boll
Babcock and WiIcox
Research Center
P. 0. Box 835
Alliance, OH  44601

Mr. Wi Hi am L. Brangers
U. S. Army  Environmental
Hygiene Agency
Abeerdeen Proving Grounds, MD

Ed Brooks
TRW
One Space Park Drive
Redondo Beach, CA  90278

Robert F. Brown
Research-Cottrell
P. 0. Box 750
Bound Brook, NJ  08805
         21010
Warren L. Buck
Argonne National Lab.
9700 S. Cass Avenue.,
Argonne, IL  60439
Building 308
Charles L. Burton
Combustion Engineering
1000 Prospect Hill Road
Windsor, CT  06095
John R. Bush
Research-Cottrell
P. 0. Box 750
Bound Brook, NJ  08805
                                      93

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Chris Busch
President
Spectron Dev. Lab.
3303 Harbor Boulevard
Costa Mesa, CA  92606

Jeffery Bradley
Researeh Associate
University of Wisconsin
 at MiIwaukee
3200 N.  Cramer Street
Milwaukee, WI  53201

Beth A.  Brown
Aspen Systems Corporation
20010 Century Blvd.
Germantown, MD  20767
Bruce Boggs
Amax
5020 S. Atlanta Rd.
Smyra, GA  30080
S.E,
Walt Badalski
Argonne National Lab.
9700 Cass Avenue
Argonne, IL  60439

Joan Biodi
PERC
4800 Forbes Avenue
Pittsburgh, PA  15213

Eugene Baker
Univ. of N. Dakota
Grand Forks, ND  58201
                - C -

John J. Casey
Sr. Marketing Engineering
Fluidyne Engineering Corp.
5900 Olson Memorial Highway
Minneapolis, MN  55422

Gilbert K. C. Chen
Monsanto
800 North Lindbergh Blvd.
St.Louis, MO  63166
John F. Cobianchi
J. P. Stevens & Company, Inc.
1185 Avenue of the Americas
New York, NY  10036

Dr. Hugh Coleman
Sandia Laboratories
P. 0. Box 5800
Albuquerque, NM  87115

John Colton
TRW
7600 Colshire Drive
McLean, VA  22101

James Colyar
Process Engineering
Cogas Development Company
P. 0. Box 8
Princeton, NJ  08540

Peter Costanza
Staff Scientist
Textile Research Inst.
P. 0. Box 65
Princeton, NJ  08540

Steven R., Cross
Buell-Envirotech
253 N. Fourth Street
Lebanon, PA  17042

Robert A. Chronowski
MITRE Corporation
Westgate Research Park
McLean, VA  22101

Robert Carlson
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA  94042

Captain Jesse B. Cabellon
U. S. Army Environmental
Hygiene Agency
Abeerdeen Proving Grounds, MD

Dr. Seymour Calvert
Air Pollution Technology, Inc.
4901 Morena Blvd, Suite 402
San Diego, CA  92117
                                                     21010
                                      94

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Dr. R. L. Carpenter
Lovelace Biomedical and Environmental
Research Institute
P. 0. Box 5890
Albuquerque, NM  87115

Captain James W_. Carroll
U. S. Army Environmental
Hygiene Agency
Abeerdeen Proving Grounds, MD  21010

Gregory H.  S. Cheng
Environeering, Inc.
4233 N. United Parkway
Schiller Park, IL  60176

C.K.H. Choi
TRW Energy Systems Group
Building R4/Room 2136
One Space Park Dr.
Redondo Beach, CA  90278

Dr. David F. Ciliberti
Westinghouse R&D Center
Beulah Road, Bldg. 501-3E29
Pittsburgh, PA  15235

Neil H. Coates
Mitre Corp./Metrek Div.
1820 Dolly Madison Blvd.
McLean, VA  22101

Leland Collins
Mech. Eng.  Dept.
Stanford University
Stanford, CA  94305

Steven D. Colome
Harvard School of Public Health
665 Huntington Avenue
Boston, MA  02115

Glenn Coury
Coury & Associates, Inc.
7400 W. 14th Avenue
Lakewood, CO  80214

Rufus Crawford
Steams-Roger Eng. Co.
P. 0. Box 5888
Denver, CO  80217
T. E. Ctrvtnicek
Monsanto-Dayton Labs
1515 Nicholas Road
Dayton, OH  45407

John S. Cvicker
Foster-Wheeler Energy Corp,
110 S. Orange Avenue
Livingston, NJ  07039

Fred Cox
Menardi Southern
1201 W. Francisco Blvd.
Torrance, CA  90502

Irving Carls
Argonne National Lab.
9700 Cass Avenue
Argonne, IL  60439

ton. Corder
Battelle-Columbus
505 King Avenue
Columbus, OH  43201

Dr. Stanley Canada
G.E.
P.O. Box 8
Schnectady, NY  12301
John C. Dempsey
Program Manager
U.S. Department
WPR Division
Washington, D.C,
                - D -
of Energy

  20545
Mark N. Director
Head, Gas Physics Section
Atlantic Research Corp.
5390 Cherokee Avenue
Alexandria, VA  22314

Thomas Donnelly
Donaldson Company, Inc.
P. 0. Box 1299
Minneapolis, MN  55440
                                      95

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Frederick J. Dudek
UOP, Inc. Air Correction Div.
P. 0. Box 1107, Tokeneke Road
Darien, CT  06820

John M. Ducan
Shell Development
P. 0. Box 2463 -- One Shell Plaza
Houston, Texas  77001

Alberta M. Dawson
Sala Magnetics, Inc.
247 Third Street
Cambridge, MA  02142
                - E -

Sally Edler
Bendix Environmental & Process
Instruments Division
1400 Taylor Avenue
Baltimore, MD  21204

Heinz L. Engelbrecht
Wheelabrator-Frye Inc.
600 Grant Street
Pittsburgh, PA  15219
Joseph Epstein
MHD Division
U.S. Department of Energy
20 Massachusetts Avenue,  N.W.
Washington, D.C.  20545

George Erskine
Mitre Corp./ Metrek Division
1820 Dolly Madison Blvd.
McLean, VA  22101

Robert Ellman
Department of Energy
Grand Forks Energy Res. Ctr.
Grand Forks, ND  58202
                - F -

H. N. Frock
Leeds & Northrup
Dickerson Road
North Wales, PA  19454
B. P. Faulkner
Allis-Chalmers Corp.
P. 0. Box 512
Milwaukee, WI  53201

William Fedarko
U.S. Department of Energy
20 Massachusetts Avenue, NW
Washington, D.C. 20545

Paul L. Feldman
Research-Cottrell
P. 0. Box 750
Bound Brook, NJ  08805

Lewis K. Felleisen
EPA, Region III
Curtis Building
Sixth and Walnut Streets
Philadelphia, PA  19106

Paul E. Fredette
Midland-Ross Technical Center
P. 0. Box 907
Toledo, OH  43691

Max Friedman
Chemico Air Pollution Control Co,
One Penn Plaza
New York, NY  11801

David Ferrell
CE Power Systems
1000 Prospect Hill Rd
Windsor, CT  06095

Dale Furlong
Buell Emission Control Division
Envirotech Corp.
200 N. Seventh Street
Lebanon, PA  17042

James Facet
Facet Enterprises
434 W. 12 Mile Road
Madison Hts., MI  48071

Robert Frumerman
Frumerman Associates
5423 Darlington Road
Pittsburgh, PA  15217
                                      96

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Oliver Foo
Mitre/Metrek Division
Westgate Research Park
McLean, VA  22101
             -  - 6 -

John A. Garbak
Montgomery County
Dept. of Env. Protection
6110 Executive Blvd., Room 340
Rockville, MD  20852

Peter Gelfand
Buell Emission Control Div.
Envirotech Corp.
200 N.  Seventh Street
Lebanon, PA  17042

James A. Gieseke
Battelle-Columbus Labs.
505 King Avenue
Columbus, OH  43201

W. Giles
General Electric Co.
Corporate R&D
P. 0. Box 8
Schenectady, NY 12301

Dr. Simon L. Goren
National Science Foundation
Engineering Division
Washington, D.C.  20550

John S. Gordon
TRW.
Energy Systems Planning Div.
7600  Colshire Drive
McLean, VA  22101
Eugene Grassel
Donaldson Company
P. 0. Box 1299
Minneapolis, MN  55440

Michael W. Gregory
Exxon Res. & Dev.
1600 Linden Avenue
Linden, NJ  07036
Ulrich Grimm
MERC
U.S. Department of Energy
P. 0. Box 880
Morgantown, WV  26537

Robert Gugger
Curtiss-Wright Corporation
One Passaic Street
Wood Ridge, NJ  07075

Nigel Guilford
Ontario Res. Foundation
Sheridan Park
Mississauga, Ontario L5K 1B3

Michael Gurevich
U.S. Department of Energy
1900 S. Eads Street
Arlington, VA  22202

Karl-Axel Gustavsson
Bahco Ventilation
Bahco Systems, Inc.
P. 0. Box 48116
Atlanta, GA  30362

Adi R. Guzdar
Foster-Miller Association
135 Second Avenue
Waltham, MA  02176

John A. Garbak
Environmental Engineering
Montgomery County
1909 Hyannis Ct.  No. 202
McLean, VA  22101

John Gefkin
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts Avenue, N.W.
Washington, D.C.  20545

Gerald M. Goblirsch
Mechanical Engineering
Department of Energy
Grand Forks Energy Research Center
Box 8213 University Station
Grand Forks, ND  58202
                                      97

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Masood Ghassemi
TRW, Bldg. R4., Rm. 1128
One Space Park Dr.
Redondo Beach, CA  90278

Stanely S. Grossel
Process Design Section
HoffmaR-LaRoche, Inc.
Nutley, NJ  07110

Edw. Garruto
Curtiss-Wright Corp.
One Passaic Avenue
Wood Ridge, NJ  07075

Dr. Wn. Goldberger
Battelle-Columbus
505 King Avenue
Columbus, OH  43201

Michael Gluckman
EPRI
3412 Hillview Avenue
Palo Alto, CA  94306
                - H -

H. J. Hall
H. J. Hall Associates
Cherry Valley Road
Princeton, NJ  08540

Mark S. Hanson
Battelie-Northwest
P. 0. Box 999
Rich land, WA  99352

Michael J. Hargrove
C-E  Power Systems
1000 Prospect Hill Road
Windsor, CT  06095
G. 0. Haroldsen
Allied Chemical Corporation
550 Second Street
Idaho Falls, ID  83401

Andrew Harvey
Foster-Miller Associates
135 Second Avenue
Waltham, MA  02154
Wi Hi am J. Havener
Waltz Mill Site Box
Westinghouse
Madison, PA  15663
158
J. H. Hedberg
Aerojet Energy Conversion Company
P. 0. Box 13222
Sacramento, CA  95813

K. H. Hemsath
Surface Division
Midland-Ross Corporation
P. 0. Box 907
Toledo, OH  43691

Howard E. Hesketh
Southern Illinois University
School of Eng.
Carbondale, IL  62901

R. C. Hoke
Exxon Research and Engineering
P. 0. Box 8
Linden, NJ  07036

D. G. Ham
Battelie-Northwest
Battelle Blvd.
Rich land, WA  99352
John D. Holmgren
Westinghouse
Waltz Mill Site, Box
Madison, PA  15663
 158
Dr. Donald J. Holve
Stanford University
Mechanical Engineering
Stanford, CA  94305

Dr. Chao-Ming Huang
TVA Energy Research
1320 Commerce Union Bank Bldg.
Chattanooga, TN  37401
Gordon Huddleston
Montana Energy and MHD
Research and Dev. Inst.,
P. 0. Box 3809
Butte, MT  59701
     Inc.
                                      98

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Jacques Hull
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA
94042
Don Holve
Stanford University
MechanJcal Engineering
Stanford, CA  94305

C. Frederick Hansen
Ames Research Center
NASA, Div. 229-3
Moffet Field, Ca  94033

Robert Hosemann
PG&E
77 Beale Street
San Francisco, CA  94106

Francine Hakimian
Librarian
Mcllvaine Co.
2970 Maria Avenue
Northbrook, IL  60062

Daniel  Hartley
Sandia Laboratories
Livermore, CA  94550

Donald Hull
Phi Hips Petrol euro
P.O. Box 25
Homer City, PA  15748

Thomas Ho Ten
Stearns-Roger
Conoco Coal Dev. Co.
Rapid City, SD  57701

Herbert I. Hollander
Gi Ibert Associates
P.O. Box 1498
Reading, PA  19603
                - J -

Albert A. Jonke
Argonne National Lab.
9700 S. Cass Avenue
Argonne, IL  60439

I. L. Jashnani
Arthur D. Little, Inc.
One Acorn Park
Cambridge, MA  02140

Dr. Fred Jones
American Natural Service Co,
One Woodward Avenue
Detroit, MI  48226
                                       - K -

                       Yale G.  Kardish
                       Peabody  Air Resources Equip.  Co,
                       P.  0.  Box 5202
                       Princeton,  NJ  08540

                       William  M.  Kelly
                       Environmental Elements  Corp.
                       P.  0.  Box 1318
                       Baltimore,  MD  21203

                       Richard  A.  Kennedy
                       Mitre/Metrek Division
                       1820 Dolly Madison Bovd.
                       McLean,  VA  22101
C. E. Irrion
Curtiss-Wright Corp.
One Passaic Avenue
Wood Ridge, NJ  07075
                       Frank J.  Kiernan
                       Aerojet Energy Conversion
                       99 Clinch Avenue
                       Garden City,  NY  11530

                       Richard N.  Kniseley
                       Department  of Energy
                       Ames  Laboratory, DOE
                       Iowa  State  University
                       Ames, IA  50011

                       Dr.  Charles E.  Knox
                       Uniglass Industries
                       1440  Broadway
                       New York, NY   10018
                          Co
                                      99

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Arthur L. Kohl
Rockwell International/
Atomics International Division
8900 DeSoto Avenue
Canoga Park, CA  91304

John J. Kov.ach
MERC  -
Department of Energy
P. 0. Box 880
Morgan town, W. VA  26505

William Krisko
Donaldson Co., Inc.
P. 0. Box 1299
Minneapolis, MN  55440

Andres Kullendorff
Atal-Laval Turbin AB
S-61220 Finspong, Sweden

T. Kumar
Occidental Research Corporation
1855 Carrion Road
LaVerne, CA  91750

William B. Kuykendal
IERL-RTP
Environmental Protection Agency
Research Triangle Park, NC  27711

Henry F. Keller
Carrier Corporation/
Research Division
Carrier Parkway
Syracuse, NY  13201

Mike Klett
Process Engineering
Gilbert Associates
P. 0. Box 1498
Reading, PA  19603

Harry Krokta
The Ducon Company, Inc.
147 E. Second Street
Mineola, NY  11501

Hank Kolnsberg
TRC, Inc.
125 Silas Deane Hwy.
Wethersfield, CT  06109
Dale Keairns
Westinghouse
Waltz Mill Site Box
Madison, PA  15663
    158
T. Kalina
G.E.
P.O. Box 8
Schnectady, NY
12301
                - L -
Norman R. LaMarche
General Electric
1 River Road
Building 23, Room 355
Schenectady, NY  12345

George Lamb
Textile Research Institute
P. 0. Box 625
Princeton, NJ  08540

William T. Langan
Buell Emission Control Division
Envirotech Corporation
200 N. Seventh Street
Lebanon, PA  17042

Robert Langley
Inex Resources, Inc.
7475 W. Fifth Avenue
Lakewood, CO  80226

C. E. Lapple
Chemical Engineering Department
SRI International
333 Ravenswood Avenue
Menlo Park, CA  94025

Benjamin Linsky
A Different Air — Skyline
1360 Anderson
Morgantown, WV  26505

C. E. Lombardi
Teller Environmental Systems, Inc.
10 Faraday Street
Worcester, MA  01605
                                     100

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£. T. Losin
A11 is-Chalmers
MiIwaukee, WI
Corporation
53201
F. E. Lukens
Western Arcadia
4115 W. Ogden Avenue
Chicago, IL  60623

Bruno Loran
Ralph M. Parsons co.
100 W. Walnut Street
Pasadena, CA  91124

Vance Leak
U.S. Dept. Interior
P.O. Box 1660
Twin Cities, MN  55111

Dr. Phi lip Levins
Arthur D. Little, Inc.
One Acorn Park
Cambridge, MA  02140
                - M -

Andrej Macek
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts Avenue, N.W.
Washington, D.C.  20545

Dr. Ray F. Maddalone
TRW Defense and Space Systems Group
Building 01/2020
One Space Park Drive
Redondo Beach, CA  90278

Dr. Lidia Manson
TRW
Bldg. 01-2161
One Space Park Drive
Redondo Beach, CA  90278
William Masters
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA
    94042
I. Matsunga
Mitsubishi Heavy Industries
875 North Michigan Ave., Ste.
Chicago, IL  60611

Sigvard Mats
Flakt Inc.
1500 E. Putnam Avenue
Old Greenwich, CT  06870

Mike May
Babcock and Wilcox Company
20 S. Van Buren
Barberton, OH  44203

J. T. McCabe
Mechanical Technology
968 Albany-Shaker Road
Latham, NY  12110

J. D. McCain
Southern Research Institute
2000 9th Avenue
Birmingham, AL  35205

Joseph E. McGreal
United States Steel Research
"B" Street
Penn Hills, PA  15235

James R. Melcher
MIT
Room 36-313, 50 Vassar Street
Boston, MA  02139

Dr. Arthur G. Metcalfe
Solar Turbines International
Mail Zone R-l, Box 80966
San Diego, CA  92138

Richard Mitchell
Inex Resources, Inc.
7475 W. Fifth Avenue
Lakewood, CO  80226

Mark H. More Hi
Amax Coal Company
105 S. Meridian Street
Indianapolis, IN  46225
2100
                                     101

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John M. Morris
Air Pollution Division
Rexnord Inc.
P. 0. Box 13226
Louisville, KY  40213

Andy Murphy
Acurex/Aerotherm
3301 Woman's Club Drive
Raleigh, NC  27611

Keshava S. Murthy
Battelie-Columbus Labs.
505 King Avenue
Columbus, OH  43201

Ron Miller
PSM Sales — Rexnord
7675 Maple Avenue
Pennsauken, NJ  08109

Wi lliam McCarthy
Chemical Engineering
US/EPA - OEMI
Waterside Mall
Washington, D.C.  20460

George B. Manning
Department of Energy
20 Massachusetts Avenue
Washington, D.C.  20545

Dr. Jim Meyer
Research Engineering
Oak Ridge National Lab.
P. 0. Box "X"
Oak Ridge, TN  37830

M. Miller
Fluidyne Engineering Corporation
5240 Port Royal Road
Springfield, VA  22151

John C. Montagna
Argonne National Lab.
9700 S. Cass Avenue
Argonne, IL  60439

R. H. Moore
Battelie-Northwest
Battelle Boulevard
Rich land, WA  99352
Samuel J. Moore
Carrier Corp/Research
Carrier Parkway
Syracuse, NY  13201
Div.
William E. Moore
Fossil Energy/Adv. Power Systems
Department of Energy
20 Massachusetts Avenue
Washington, D.C.  20545

Tom Mosure
US/EPA
Environmental Research Inf. Center
26 W. St. Clair
Cincinnati, OH  45268

Larry Micha lee
Code 64270 NARF
NAS North Island
San Diego, CA  92135

Henry Modetz
EPA, Region IV
230 S. Dearborn
Chicago,  IL  60604

M. MacCafferty
IEA Coal Research
Technical Information Service
14/15 Lower Grosvenor Place
London SWIW OEX
England

Capt. Joseph A. Martone
USAF, BSC
DET 1, HC ADTC
Tyndall AFB, FL  32403

John Miles
Phillips Petroleum
P.O. Box 25
Homer City, PA  15748

Rich McMillan
Foster-Wheeler Energy Research Ctr.
12 Peach Tree Hill Road
Livigston, NJ  07039
                                     102

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                 -  N -

 Leonard  M.  Naphtali
 Department  of  Energy
 Fossil Energy/CCN
 20  Massachusetts Avenue
.Washington,  D.C.   20545

 Charles  K.  Neulander
 General  Electric Company
 P.  0.  Box 8,  Building  K-l
 Schnectady,  NY  12301

 G.  S.  Newton
 Lovelace Biomedical
 Environmental  Research Institute
 P.  0.  Box 5890
 Albuquerque,  NM  87115

 James  C. Napier
 Solar  Turbines International
 P.  0.  Box 80966
 2200 Pacific  Highway
 San Diego,  CA  92138

 David  V. Nakles
 Carnegie-Mellon  Univ.
 Schenley Park
 Pittsburgh,  PA  15213
                 -  0  -

Thomas  E.  O'Hare
Brookhaven National  Laboratory
Upton,  Long Island,  NW   11973

Dr.  Morris S.  Ojalvo
National Science Foundation
Engineering Division
Washington,  D.C.   20550

John M. Ondov
Lawrence Livermore Lab.
P. 0. Box  808
Livermore, CA   94550

Dr.  H.  H.  Osborn
C-E  Air Preheater  Co.
P. 0. Box  372
Wellsville,  NY   14895
Dr. Nancy O'Fallon
Argonne Natl. Lab.
Applied Physics Dept., Bldg. 316
9700 Cass Avenue
Argonne, IL  60439
                - P -

Subhash S. Pate!
Hittman Associates, Inc.
9151 Rumsey Road Building
Columbia, MD  21045

Dr. Ronald G. Patterson
Air Pollution Technology, Inc.
4901 Morena Boulevard, Suite 402
San Diego, CA  92117

Dr. Richard D. Parker
Air Pollution Technology, Inc.
4901 Morena Blvd., Suite 402
San Diego, CA  92117

Walter Podolski
Argonne National Lab.
9700 S. Cass Avenue
Argonne, Illinois  60439

James B. Padden
Facet Filters
434 W. 12 Mile Road
Madison Heights, MI  48071

Joseph R. Polek
Catalytic, Inc.
1500 Market Street, CSW-10
Philadelphia, PA  19102

Duane H. Pondius
Southern Research Inst.
2000 9th Avenue S.
Birmingham, AL  35205

Wm Penson
Battelle-Columbus
505 King Avenue
Columbus, OH  43201

Jerry Peterson
G.E.
P.O. Box 8
Schnectady, NY  12301
                                      103

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Lyle Pollack
Phi Hips Petroleum
154 RB 1
Bartlesville, OK  74004

John Piatt
Pittsburgh and Midway Coal Company
(PAMCO)
P.O.  Box 199
DuPont, WA  98327
Peter Palmer
G.E.
P.O. Box 8
Schnectady, NY
12301
                - Q -
Sandra Quinlivan
TRW
Bldg. R4, Rm. 1120
One Space Park Drive
Redondo Beach, CA  90278
                - R -

Ronald Renko
Development Engineering
C-E Air Preheater
Wellsville, NY  14895

D. L. Reid
Battelle-Northwest
P. 0. Box 999
Rich land, WA  99352

George Rey
Office of R & D (RD-681)
Env. Protection Agency
Washington, D.C.  20460

George Rinard
Research Engineer
Denver Research Inst.
Denver, CO  80208

Stephen N. Rudnick
Harvard School of Public Health
665 Huntington Avenue
Boston, MA  02115
E. Radhakrishnan
Battelle-Columbus Labs.
505 King Avenue
Columbus, Ohio  43201

Madhav B. Ranade
Research Triangle Institute
P. 0. Box 12194
Research Triangle Park, NC  27709

David L. Raring
Sonic Development Corporation
3 Industrial Avenue
Upper Saddle River, NJ  07458

Dr. Richard Razgaitis
Ohio State University
206 W. 18th Avenue
Columbus, Ohio  43221

R. B. Reif
Battelle-Columbus Labs.
505 King Avenue
Columbus, Ohio  43201

Frank G. Rinker
Midland-Ross
P. 0. Box 907
Toledo, Ohio  43691

Thomas 0. Robertazzi
Facet Enterprises
6521 Arlington Boulevard
Falls Church, VA  22042

David R. Rubin
U.S.D.A., Rural Electrification Admin
Agriculture South Building
14th and Independence Avenue, S.W.
Washington, D.C.  20250

Mr. Jean V. Remillieux
Air Industrie
19, Avenue DuBonnet
92401 Courbevoie
France

George L. Roberts
Vice President
Universal Transport Systems, Inc.
2665 Marine Way
Mountain View, CA  94040
                                     104

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James Ronning
Curtiss-Wright Corp.
One Passaic Avenue
Wood Ridge, NJ  07075
                - S -

William A. Standstrom
Institute of Gas Technology
3424 South State Street
Chicago, IL  60616

Gene Schaltenbrand
C-E Preheater Company
P. 0. Box 387
Wellsville, NY  14895

Robert Scheck
Steams-Roger
P. 0. Box 5888
Denver, CO  80217

Martin Schi Her
CSI Engineering
P. 0. Box 1515
Fairfield, CT  06430

J. W. Schindeler
John Zink Company
P. 0. Box 7388
Tulsa, OK  74105

Dr. Schnittgrunt
Consolidated Aluminum
2302 Wei don Way
St. Louis, MO  63178

H. F. Schulte
Rexnord, Inc.
1914 Albert Street
Racine, WI  53404

Gernot Mayer Schwinning
Lurgi Apparate-Technik GmbH
Postfash 1, Gwinner Street
6000 Frankfort am Main-2
West Germany
Dr. David S.  Scott
Dept.  of Mech Engineering
University of Toronto
Toronto, Ontario M5S 1A4
Canada

Stanley J. Selle
Grand Forks Energy Res. Ctr.
Department of Energy
P. 0.  Box 8213, University Station
Grand Forks,  ND  58202

Michael Shackleton
Acurex/Aerotherm
485 Clyde Avenue
Mountain View, CA  94042

J. K.  Shah
Surface Division
Midland-Ross  Corporation
P. 0.  Box 907
Toledo, OH  43691

Jer-Yu Shang, Ph.D
Mitre Corp./Metrek Division
Westgate Research Park
McLean, VA  22101

W. J.  Sheeran
General Electric Company
Corporate R&D
P. 0.  Box 43
Schenectady,  NY  12301

Dr. Thomas S. Shevlin
3M Company
3M Center, P. 0. Box 33221, Bldg. 230
St. Paul, MN  55138

Dr. Gajendra H. Shroff
Bechtel Power Corporation
15740 Shady Grove Road
Gaithersburg, MD  20760

Dr. A. P. Sikri
U.S. Department of Energy
Gas & Shale Technology
20 Massachusetts Avenue
Washington, D.C.  20545
                                      105

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A. A. Smith
Babcock and Wilcox Ltd.
Woodall-Duckham House
Crawley, Sussex,
United Kingdom

Dr. Donald W.  .Smith
HAVEG Industries
900 Greenbank  Road
Wilmington, DE  19808

Wallace B. Smith
Southern Research Inst.
2000 9th Avenue
Birmingham, AL  35205

John H. Smith son
Department of Energy
20 Massachusetts Avenue
Washington, D.C.  20545

Herbert W. Spencer, III
Western Precipitation Division
Joy Manufacturing
4565 Colorado Boulevard
Los Angeles, CA  90039

John  Spriggs
Donaldson Company, Inc
P. 0. Box 1299
Minneapolis, MN  55440

Dr. C. J. Stairmand
Babcock and Wilcox Ltd.
Woodall-Duckham House
Crawley, Sussex
United Kingdom

Richard C. Stone
Stone & Webster Engineering Company
P. 0. Box 2325
Boston, MA  02107

William M. Swift
Argonne National Laboratory
9700 S. Cass Avenue, Bldg. 205
Argonne, IL  60439

Ronald D. Synder
Buell Emission Control Division
Envirotech Corporation
200 N. Seventh Street
Lebanon, PA  17042
Robert K. Schaplowsky
Chemist
Aerojet
7767 LaRivera Drive No.
Sacramento, CA  95826
   219
David Shaw
Professor
State University of NY/Buffalo
4232 Ridge Lea Road
Buffalo, NY  14226

G. F. Schiefelbein
Battelle-Northwest
Battelle Boulevard
Rich land, WA  99352

Jer Yu Shang
Professional Engineering
4524 Andes Drive
Fairfax, VA  22030
Kevin J. Shields
Hittinaw Associates,
9190 Red Branch Road
Columbia, MD  21045
Inc.
Jack Siege!
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts Avenue
Washington, D.C.  20545

Theodore B. Simpson
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts Avenue
Washington, D.C.  20545

Gregory W. Smith
Argonne National Lab.
9700 S. Cass Avenue
Argonne, IL  60439

Walter Steen
Chemical Engineering
US EPA
IERL-RTP
Research Triangle Park, NC  27711
                                      106

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G. E. Stegen
Battelle-Northwest
Battelle Boulevard
Rich land, WA  99352

David Stelman
Rock well/Atomies Int. Div,
8900 DeSoto Avenue
Canoga Park, CA  91304

Ed Stenby
Project Engineering
Stearns-Roger
P. 0. Box 5888
Denver, CO  80217

E. F. Sverdrup
Westinghouse
Beulah Road
Pittsburgh, PA  15235
Dean Simeroth
California Air
P.O. Box 2815
Sacramento, CA
Resources Board

 95812
A.V. Slack
SAS Corporation
Wilson Lake shores
Sheffield, AL  35660

Richard A. Schwartz
Koch Engineering Co., Inc.
161 East 42nd Street
New York, NY 10017

Franklin Smith
Research Triangle Institute
P.O. Box 12194
Research Triangle Park, NC  27709

W. Szwab
GiIbert Associates
P.O. Box 1498
Reading, PA  19603

Max Souby
Univ. of N. Dakota
Grand Forks, ND  58201
                           Harold Stotler
                           Hydrocarbon Res.,  Inc.
                           334 Madison Avenue
                           Morristown, NJ  07960

                           A. G.  Sliger
                           Pullman-Kellogg
                           16200 Park Row
                           Industrial Park Ten
                           Houston, TX  77079
                - T -

F. Gale Teats
Argonne National Lab.
9700 S. Cass Avenue
Argonne, IL  60439

Yung Kwang Ti
Research Associates
University of Wisconsin
3200 N. Cramer Street
Milwaukee, WI  53201

C. Tien
Syracuse University
Syracuse, NY  13210

R. F. Toro
Recon Systems, Inc.
Cherry Valley Road
Princeton, NJ  08540
                           Richard H.  Tourin
                           NY State Energy Research
                           and Development Authority
                           230 Park Avenue
                           New York, NY  10017

                           Norman R. Troxel
                           Research-Cottrell,  Inc.
                           P. 0.  Box 750
                           Bound  Brook, NJ  08805
                                                   at Milwaukee
                           Keh C.  Tsao
                           University of Wisconsin
                           College of Engineering
                           3200 N. Cramer Street
                           Milwaukee, WI  53211
                        at MiIwaukee
                                      107

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Alex lurchine
Proctor and Gamble
7162 Reading Road
Cincinnati, OH  45222

Suresh P.  Tendulkar
Westinghouse  .
Waltz Mill Site, Box 158
Madison, PA  15663

C. M. Thoennes
General Electric Company
Building 2, Room 712
One River Road
Schnectady, NY  12345

Dr. Jim Trolinger
Spectron Development Labs
3303 Harbor Boulevard
Costa Mesa, CA  92626

S. I. Taub
IU Conversion Systems, Inc.
Joshua Road and Stenton Avenue
P.O. Box 331
Plymouth Meeting, PA  19462

Charles Trilling
Rockwell/Atomics International
P.O. Box 319
Canoga Park, CA  91304
F. Munro Veazie
Owens-Corning Fiberglass Corporation
Technical Center
Granville, OH  43023

Geza Verities
Westinghouse
1500 Chester Pike, Building A703
Eddystone, PA  19013

John A. Verrant
Donaldson Company, Inc.
P. 0. Box 1299
Minneapolis, MN  55440

S. N. Vines
University of VA, Chemical Eng. Dept,
Thornton Hall
Charlottesville, VA  22901

G. J. Vogel.
Argonne National Lab.
9700 S. Cass Avenue
Argonne, IL  60439

D. V. Vukovic
Faculty of Technology and Metallurgy
Belgrade University
1100 Beogard, Karnegijeva 4,
P.O.B. 494
Yugoslavia
                - U -

V. S. Underkoffler
Manager, Combustion and Advanced Power
Gilbert Associates, Inc.
525 Lancaster Avenue
Reading, PA  19603
                - V -

V. A. Varady
UOP Process Division
UOP Plaza
Des Plaines, IL

E. S. Van Valkenburg
Leeds and Northrup Company
Dickerson Road
North Wales, PA  19454
                - W -

Gordon L. Wade
Combustion Power Company
1346 Willow Road
Menlo Park, CA  94025

Donald E. Wambsgans, II
District of Columbia
Dept. of Environmental Services
Room LL-3
614 "H" Street N.W.
Washington, D.C.  20001

Walter Wolowodivk
Foster-Wheeler Dev. Corp.
12 Peach Tree Hill Road
Livingston, NJ  07039
                                      108

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Peter Waldstew
Physical Chemist
RDR
P. 0. Box 33128
District Heights,
   MD  20028
Andrew Wallo
Env.-Scientist
1605 Craig Street
Sterling, VA  22170

Phillip C. White
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts Avenue, N.W.
Washington, D.C.  20545

Stephen Wander
Department of Energy
400 First Street, N.W.
Washington, D.C.  20545

Val E. Weaver
Department of Energy
Fossil Energy/Advanced Power Systems
20 Massachusetts. Avenue, N.W.
Washington, D.C. 20545

Frank Weiskopf
Environmental Elements Corp.
P. 0. Box 1318
Baltimore, MD  21203

Clyde L. Witham
SRI International
333 Ravenswood
Menlo Park, CA  94025
Thomas Walsh
Riely-Stoker
P.O. Box 547
Worcester, MA
01613
David Weller
Curtiss-Wright Corp.
One Passaic Avenue
Wood Ridge, NJ  07075

D. E. Woodmansee
G.E.
P.O. Box 8
Schnectady, NY  12301
                           Dr. John S.  WiIson
                           Department of Energy/MERC
                           P.O.  Box 880
                           Morgantown,  WV  26505
                                           - Y -

                           Dr.  H.  C.  Yeh
                           Lovelace Biomedical and Environmental
                           Research Institute
                           P.  0.  Box  5890
                           Albuquerque,  NM  87115
                                           - Z -
                           Dr.  Karim Zahedi
                           President
                           EFB, Inc.
                           94 Francis
                           Brook line,
           Street
           MA  02146
John H. Zarnitz
N.Y.C. Dept. of Air Resources
7044 Manse Street
Forest Hills, NY  11375

Dr. F. A. Zenz
The Ducon Company
147 East Second Street
Mineola, LI, NY  11501

August H. Zoll
Curtiss-Wright Corporation
Power Systems
Wood Ridge, NJ  07075

Stephen H. Zukor
Department of Energy
OGST
20 Massachusetts Avenue, N.W.
Washington, D.C.  20545

Irena M. Zuk
Interdevelopment, Inc.
Suite 104,
Rutherford B. Hayes Bldg.
2361 South Jefferson Davis Hwy.
Arlington, VA  22202
                                     109

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                                   APPENDIX 8

              SURVEY OF CONTINUOUS PARTICULATE MEASUREMENT DEVICES
B.I  SUMMARY

     This investigation surveys the state-of-the-art of continuous particulate
monitoring devices applicable to high-temperature and high-pressure (HTHP)
processes.  The study determined that continuous particulate monitoring of
HTHP-process streams, involving fluidized bed combustion and coal
gasification, are relatively new frontiers for particulate sampling
technology.  No commercial monitoring device is currently available that can
meet this need; however, research efforts are underway to develop the
technology.

     Instrumentation based on electro-optics is very attractive for this
future need.  In addition to the electro-optical devices, the IKOR continuous
monitor, based on the principle of contact charge transfer, also .is a
potential candidate for HTHP monitoring.

B.2  INTRODUCTION

     The deficiencies of existing monitoring equipment is a hindrance to
process control and environmental protection in the development of advanced
coal and energy conversion systems, (e.g., fluidized bed combustors and coal
gasifiers).

     In particular, Argonne National Laboratories has concluded (Reference
3-1) that coal-fired processes (both existing and proposed) require
instrumentation development for the monitoring of:

     0   Mixed phase flowrates of dense phase solids mass flow, dilute phase
         solids mass flow, and dirty gas flow
     •   On-line composition of streams (containing solids, liquids, and
         gases) and vessels (containing solids and liquids)
     •   Level detection of oil/water interfaces occurring in coal conversion
         processes and of fluidized-bed heights
     •   Rapidly fluctuating temperatures, in the 1500°F to 3000°F range

     Continuous particulate sampling is also essential to the determination of
on-line process conditions.  The importance of this sampling is underscored
for HTHP streams, which can corrode or erode exposed equipment surfaces such
as turbine blades.
                                     110

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     This investigation presents a brief survey of the state-of-the-art of
continuous particulate monitoring equipment.  Information sources  include
current literature and equipment manufacturers.

     The coal energy conversion industry encompasses a variety of  processes
which can span a wide range of operating conditions.  This survey  considers
the sampling environment defined below, which is representative of technology
currently under development.

         Temperature:  1200°F to 2000°F
         Pressure:  3 to 100 atm
         Flow velocity:  10 to 100 ft/sec
         Particulate size:  <60ym
         Particulate loading: 0.04 to 4.4 gram/m^

Factors which create hostile environments for particulate monitoring equipment
are:

     •   The existence of high temperature and high pressure
     •   Corrosive, abrasive, and highly flammable nature of the constituents,
         while nonuniform flow profiles complicate the determination of
         particulate loading.

B.3  DISCUSSION

     The current state of particulate detection technology is comprised of
continuous monitoring and noncontinuous sampling.  Virtually all of the
hardware for measurements at modest temperatures and pressures falls in the
latter category.  Typical techniques consist of sample extraction, sample
conditioning, sample collection (filters, impactors and cyclones)  and
subsequent weighing of this sample in a gravimetric balance.  Reference 2
presents a survey of the existing noncontinuous HTHP sampling techniques.

     As mentioned previously, the requirement for continuous monitoring
equipment is critical to the development and subsequent commercialization of
advanced coal energy systems.  This document presents an overview of the
state-of-the-art of continuous particulate monitoring at HTHP, which is still
in the very initial stages of development.  As such, the approach here looks
at the existing continuous particulate monitoring techniques and presents
their status for HTHP application.  The field of continuous monitoring divides
into two categories:   extractive and nonextractive sampling.  A discussion of
these is presented below.

B.3.1    Extractive Continuous Monitoring

     The methods studies using the extractive monitoring approach were based
upon:
     •   The Piezo-electric effect
     •   'Beta wave attenuation
     •   Contact charge transfer (tribo-electric effect)
                                      111

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B.3.1.1  Piezo-Electric Effect

     Instruments using this method are called piezo-electric microbalances.
The heart of the microbalance is a quartz crystal, which acquires a
particulate sample deposition by impaction (see Figure B-l).  This alters the
natural frequency of vibration of the crystal, and the shift in frequency
correlates with the particulate mass.  Reference 3 presents a detailed
discussion of this technique.

     At the particulate loadings of interest for HTHP process stream
measurements, this technique is essentially a noncontinuous one.
Piezo-electric microbalances monitor low concentrations at ambient
conditions.  Dr. Wallace of Berkeley Industries (Reference 4) advised that the
current limit for these instruments is a frequency shift of 2000 Hz.  This
implies a mass concentration of about 150 pg/m3 for 30 minutes without
overloading the crystal.  In addition, the frequency response of the crystal
is very sensitive to both pressure and temperature, an undesirable trait for
HTHP application.  As such, this technique was deamed not suitable for HTHP
process steam monitoring.

3.3.1.2  Beta-Wave Attenuation

     Figure B-2 presents a Beta-wave radiation attenuation instrument and its
use as an emissions mass monitor.  Differences in Beta-wave transmission
between the clear and loaded portions of a filter tape determine the radiation
attenuation due to the presence of particulate.  The particulate mass is
directly related to this attenuation.  A detailed discussion of this technique
is presented in Reference 3.

     A recent investigation conducted by C. H. Gooding (Reference 5) found the
GCA instrument based on Beta-attenuation to be inaccurate.  He, along with
others, have stressed that further work is needed to improve conversion from
Beta-attenuation to particulate mass.  Besides this, the current temperature
limit for filter tapes is about 600°F, and the high pressure is likely to
pose a serious gas leakage problem.  Hence, this method was also judged
unsuitable for HTHP requirements.

8.3.1.3  Contact Charge Transfer (Tribo-Electric Effect)

     If a particle can be made to hit or slide along a surface, it will
usually transfer electrical charge to the surface.  This creates a voltage
potential which will cause a current (10"7 to 10~8 amps, typically) within
conducting materials.  This is one example of the tribo-electric effect
(Reference 3).  Figure B-3 illustrates the use of the IKOR continuous monitor,
which is based on this principle.

     Two companies produce(d) particulate sampling equipment based on this
principle:  IKOR and KONITEST* (German).  IKOR markets both an extractive and
a nonextractive sampler.  This type of monitor holds promise for application
to HTHP process stream monitoring.
                                     112

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                   Appro x irately
                  150 1 i ters/minute
                                             Approximate!/
                                             1 liter/-inute
Figure  B-1.
Piezo-electric microbalance  (quartz) particulate
sampling  train.

                113

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                                                 Approximately
                                                60 liters/-inute
                                Valve
Flowreter    Puro
Figure B-2.   Beta-wave  attenuation particulate sampling train.

                               114

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Figure B-3.
IKOR continuous particulate mass  monitor
based on contact charge.
                         115

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     According to the equipment specifications, the IKOR probe can detect mass
concentrations from 1 x 10'4 grains/scf to 100 grains/scf for particles
between 0.1 and 100 ym in size.  Mr Gruber of IKOR (Reference 6) stated that
the IKOR samplers have been used at high temperatures (2000°F) and low
pressure (ambient) and low temperatures and high pressures (350 psi).  He
further indicated that the corrosive environment of these process streams
interest will not damage a suitable probe material, such as Titanium.
of
     Studies recently conducted (Reference 7) show that with the IKOR
continuous monitor particulate concentration readings are a strong function of
flow velocity.  Further testing and evaluation are needed to resolve this
problem.

B.3.2    Nonextractive Continuous Monitoring

     Since HTHP process streams are corrosive, abrasive and volatile in
nature, nonextractive monitoring is preferable to minimize the potential of
system leaks, which could be hazardous.  In this category the discussion will
center on methods using electro-optics.

8.3.2.1  Electro-Optical Methods

     This field of the particulate sampling technology is currently receiving
much attention.  A variety of instrumentation is under development to
determine the size, number density, mass concentration and velocity of the
particulates.  These techniques, in which the particulates are illuminated by
a beam of light (e.g., laser or LED), divide into the two categories listed
be 1 ow:

     •   Light absorption
     •   Light scattering

Instruments based on the former principle are opacity meters, or
transmissometers.  They rely upon correlations of opacity versus mass
concentration, and are classified as "crude" techniques; hence, this
investigation did not concentrate on them in detail.  However, they appear to
be useful for determining relative changes in particulate loading as an aid to
process control.

     Instrumentation based on light scattering are sophisticated diagnostics
approaches that may be capable of resolving particulate size distributions as
well as loading densities.  These devices rely on application of the MIE
Theory (References 8 and 9), which describes the scattering of electromagnetic
radiation from particles.  For a description of the theory and its
applications, the reader is referred to recent investigations by Coleman,
et al., (Reference 10).
*Not in production since 1968.
                                     116

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      Applications  of  light  scattering  for  diagnostics  has  burgeoned  into  a
 vast  technology  which  continues  to  expand.   It  is  neither  possible nor
 desirable  to  present  a comprehensive review  in  this  study.   What  is  presented
 is  a  discussion  of techniques  which have  the greatest  potential  application  to
 HTHP  processes.  These are  based  upon

         Photography
         Holography
         Visibility
         Intensity Ratio
         Diffraction

      Photography is the simple camera  technique  using  a  spark or  pulsed laser
 light  source  (Figure B-4).  References  11  and 12 provide details  of  specific
 systems.   Advantages of the photographic technique are insensitivity to
 refractive index,  applicability  to  heavy particle  loading densities,  optical
 simplicity, the  ability to  resolve  size and  shape  for  particles greater than 2
 micrometers in diameter,  and real time  information gathering.  However, the
 method suffers from a  limited  sensitivity  to  small particles and  narrow
 depth-of-  fields at large magnifications.  Furthermore, data reduction is  an
 extremely  time-consuming  process.

      Figure B-5  illustrates the  formation  of  a  hologram by  the splitting  and
 subsequent coalescence of a laser beam.  Light  scattering causes  a phase  shift
 in  the light  passing through the  flowfield.   Hence, when this beam recombines
 with  the reference  beam,  the phase  difference creates  an interference
 pattern.   McCreath  and Beer (Reference  13) present the analysis relating  this
 pattern to particle size.  Holography has  little or no depth-of-field
 restriction and  assures that magnification of particles along the optical  axis
 is  uniform.   It can measure particle sizes >5ydiameter.  However, this method
 requires complex equipment  and painstaking adjustment; moreover,  size
 information cannot  be  obtained in real  time.

     The visibility technique  is  an application  of the fact that  a particle
 will modulate as well  as cause a  Doppler-shift  in  the frequency of a  laser
 beam.  Figure B-6  shows a typical system used to obtain visibility
 information.  A  laser  beam  is split into two equal beams, which are  focused
 and intersect in the region of interest (called  a measurement volume).
 Interference  of these  beams form  a  fringe  pattern, which produces a  modulated
 and shifted signal when perturbed by a particle  traversing  this volume.  The
 particle diameter  determines the  maximum and minimum of this signal
 (Reference 14).

     Hodkinson (Reference 15) first proposed to  determine particle size by
 using  the  scattered light intensities from two,  or more, directions  (i.e.,
0]_, £'2, ..., On; Figure B-7).  In particular, this method  (the intensity
 ratio  technique) is an application  of the  relationship between the ratio of
 two such intensities,  their 3-j's, and the  particle size.  Gravatt
 (Reference B-16) extended this technique to  cover  a range of refractivities,
 while  Hirleman, et  a!., (Reference  7) have developed a two-ratio  modification
 of  the technique.  The intensity  ratio(s)  technique is able to provide real
                                     117

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        ..,• •. -a..'..
       ••'. a ••••••••
       •.• • .• •. ••;••• -\
        •  . •  •. • V • • <
         *  •••
                                             Camera
    Process

    Stream
Figure  B-4.   Photography technique.
                 118

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Laser Beam
                      •.'.;•:••/.;•: Flow
                      .'.- •'..'••" Cross-section
                                                Reference Beam
                  Figure B-5.   Holographic  technique.
                                    119

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                                Transmitter
                                  Optics
Collection
  Optics
Photodetector
               Laser
ro
CD
                         Signal Processor
                         (determines Doppler
                         Frequency of
                         Scattered  Li«jht)
                                    Measurement
                                      Volume
                                                                         c
                                                                         
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   PARTICLE
   Z — direction of propagation of linearly polarized
       incident light
   E - direction of electric vector
   K — direction of magnetic vector
   F—direction of scatter to the point of observation  (P)
Figure B-7.   Scattering of electromagnetic radiation.
                         121

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time information and apparently is not overly sensitive to either particle
shape or refractivity.  However, it is limited to loading densities  low enough
to provide single-particle signals.

     The diffraction technique determines the size distribution of particles
within the cylindrical volume formed by a laser beam passing through a
flowfield; this method uses the total Fraunhofer diffraction pattern from the
particles within the volume.  McCreath and Beer (Reference 13) and
Swithenbank, et al.5 (Reference 18) describe the technique and present
experimental results.  The method is optically simple, provides real time
information, and is insensitive to particle shape.  Its drawbacks are that it
is limited to particle diameters >2y, requires large measurement volume, and
is a line-of-sight rather than a point measurement technique.  This method
also requires a prior assumption as to the shape of the size distribution
curve.

     With the exception of the diffraction technique, any of the above methods
can supply information to determine loading densities.  Number densities are a
function of size distribution and flowrate through a known volume.  However,
since particles may be porous or hollow, conversion of number densities to
mass densities is uncertain.  In fact, the only reliable method to determine
mass loadings is to withdraw a sample arid weigh it.

     The electro-optical monitoring technology is an attractive candidate for
HTHP application.  However, there are some challenging hurdles to be
overcome.  The "window" concept is a key issue and its applicability needs to
be demonstrated in terms of sealing the window area for leaks and for keeping
the window clean from tar and slag deposits.  One current proposal is to use
either a quartz or sapphire window.*

     Another method proposed is to eliminate the window altogether.  Instead,
the light source is housed in a sealed containment vessel outside of the flow
duct.  A hole is cut in the duct wall to allow for beam transmission.  Hot
gases are kept from entering the containment vessel by continuously
pressurizing the vessel with an inert gas.

     Secondly, the ability of these techniques to overcome some of the HTHP
sampling environment aspects must be demonstrated, especially to background
light radiation** interference from the hot gases, and the opacity of the
stream itself.
 *These windows are well known to "fog-up" (crystallize) at high
  temperatures; however, this is not likely to be a serious problem
  for this application if sapphire is used.  Quartz is not recommended
  over 1500°F.
**Initial estimates show that gas radiation is not likely to be a
  problem but wall radiation is a potential source of interference.
                                    122

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8.3.2.2  Manufacturers

     There are currently four major manufacturers of this type of equipment,
all of whom were contacted during this study.

     1.  Environmental Systems Corporation  (ESC), Knoxville, Tennessee,
         Dr. Hal Schmitt (PILLS System).
     2.  Particle Measuring Systems, Inc.  (PMS), Boulder Colorado.  Dr. Bob
         Knollenberg  (ASAS System).
     3.  Spectrom Development Labs (SDL), Tullahoma, Tennessee.  Dr. Mike
         Farmer (MORPHOKINETOMETER System).
     4. . Leeds and Northrup Company (L&N), North Wales, Pennsylvania.
         Dr. Emil C. Muly (Microtract System).

     All of these manufacturers produce equipment which have the capability to
monitor particle size and mass density in the range of interest.  In addition,
the Spectron device has the capability of measuring particle velocity using
the laser doppler system.  However, at this time all of these manufacturers
lack experience in applying their technology to the problem of HTHP process
stream monitoring.  Both Spectron Labs and Leeds & Northrop are currently
under contract to DOE to develop a suitable optical system under test
conditions at Argonne National Laboratory.  Sandia Laboratory (Livermore,
California) is also under contract to DOE to evaluate several optional devices
under bench test conditions.  However, work is just getting underway at the
time of this study.*

B.4  CONCLUSIONS

     This state-of-the-art survey indicates that continuous particulate
monitoring of high temperature and pressure process streams is a new frontier
for sampling technology.  No commercial particulate monitoring instrument is
currently available which can meet this need.  However, efforts are underway
to develop the technology.

     This investigation indicates that the optical  particulate monitoring
technique appears to be very attractive for this need.   Some of the key issues
that need to be addressed are:

     •   Applicability of the "window" concept
         --  Sealing the window area for leaks
         --  Keeping the window clean from slag and tar deposits
             Integrity of window glass (quartz or sapphire) under the
             HTHP environment
*Significant testing has occurred since this section was written.
 The reader should contact the manufacturers for the status of
 their development program.

                                     123

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       •   Ability to accurately monitor in the presence of
           --  High velocity and high levels of opacity
           --  Radiation interference from the walls

The results of current DOE contract efforts of Spectron Labs, Leeds, &
Northrup, and Sandia Laboratories should provide answers to some of these
questions.  In addition to the optical techniques, the IKOR continuous
monitor also appears to be a potential candidate for HTHP monitoring.  The
key issues that need to be resolved for this device are:

       •   Choice of probe material
       •   Dependence of mass concentration readings on flow velocity

Here again some actual tests should be undertaken to address these
issues.  It is also recommended that light transmissometer technology be
looked at in greater detail for possible application to HTHP monitoring
needs.
                                     124

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                           REFERENCES FOR APPENDIX B
 1.  O'Fallon, N. M., et al.   Monitoring Coal Energy Processes.
     Industrial Research, June 1976.

 2.  Blann, D. H.  Measurement Methods at High-Temperature and Pressure.
     Paper presented at the Symposium on Particulate Control in Energy
     Processes, San Francisco, California, May 11-13.

 3.  Instrumentation for Environmental Monitoring.  Air, Part 2, Lawrence
     Berkeley Laboratory, U.S., Berkeley, July 1976.

 4.  Personal communications  with Dr. Don Wallace of International
     Biophysics Corporation (Celesco), Irvine, California, August 1976.

 5.  Gooding, G. H.  Wind Tunnel  Evaluations for Particulate Sizing
     Instruments.  EPA/2-76-073,  U.S. Environmental  Protection Agency,
     March 1976.

 6.  Personal communications  with Mr. Arnold Gruber  of IKOR Incorporated,
     Burlington, Massachusetts, August 1976.

 7.  Gotterba, J.  Characterization and Optimization of the EPA High Mass
     Flowrate Aerosol Generator.   Aerotherm Report 75-209, Acurex
     Corporation, July 1976.

 8.  Van de Hulst, H. C.  Light Scattering by Small  Particles.  John Wiley
     and Sons, 1957.

 9.  Kerker,  M.  The Scattering of Light and Other Electromagnetic
     Radiation.  Academic Press,  1969.

10.  Coleman, H. W., et al.  Interim Report:  Diagnostics Assessment for
     Advanced Power Systems.   SAND 77-8216 (UC-90f), Sandia Laboratories,
     Albuquerque, New Mexico,  March 1977.

11.  Cadle, R. D.  The Measurement of Airborne Particles.  John Wiley and
     Sons, 1975.

12.  Hotham,  G. A.  Sizing  Aerosols in Real Time by  Pulsing UV Laser
     Machine.  Aerosol Measurements, NBS Special Publication 412, p.
     97-126,  1974.

13.  McCreath, C. G. and J. M. Beer.  A Review of Drop Size Measurement  in
     Fuel Sprays," Applied  Energy 2:  3-15, 1976.

14.  Farmer,  W. M.  Measurement of Particle Size, Number Density and
     Velocity Using a Laser Interferometer.  Applied Optics 11:  2603,
     2612, 1972.
                                     125

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15.  Hodkinson,  J.  R.   Particle Sizing by Means of the Forward Scattering
     Lobe.   Applied Optics  5:   839-844,  1966.

16.  Gravatt,  C.  C.  Light  Scattering Methods  for the Characterization of
     Participate  Matter in  Real Time.  Aerosol  Measurements,  NBS Spee-ial
     Publication  412,  p.  21-32, 1974.

17.  Hirleman, E. D.,  et  al.   Development and  Application  of  an Optical
     Exhaust Gas  Particulate  Analyzer.  Laboratories for Energiteknik  Resport
     RE76-3, Technical  University of Denmark,  1976.

13.  Swithenbank, J.,  et  al.   A Laser Diagnostic Technique for the Measurement
     of Droplet  and Particle  Size Distribution, AIAA Paper No. 76-69,  1976.
                                     126

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                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
1. REPORT NO.
                              2.
                                                           3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
  Measurement of High-Temperature
  High-Pressure Processes -- A  Summary Report
             5. REPORT DATE
                    June 1980
             6.-PERFORMING ORGANIZATION CODE
              Final  Reoort 79-353
              Pro.iect  723"
7. AUTHOR(S)

   L.  Cooper and M. Shackleton
                                                           8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
  Acurex  Corporation
  Energy  & Environmental Division
  485  Clyde Avenue, Mountain  View,  CA 94042
                                                            10. PROGRAM ELEMENT NO.
             11. CONTRACT/GRANT NO.

              Contract  68-02-2153
12. SPONSORING AGENCY NAME AND ADDRESS
                                                            13. TYPE OF REPORT AND PERIOD COVERED
   Industrial  Environmental Research  Laboratory
   Office  of Research & Development
   U.S.  Environmental Protection  Agency
   Research Triangle Park, NC  27711	
             14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
   The major  focus  of this program under  EPA  contract 68-02-2153 was  that of
   particulate  sampling in advanced coal  conversion technologies.  Work  performed
   was to assess  and  develop the technology required to perform high-temperature
   high-pressure  particulate sampling.  In addition to the effort denoted to
   development  and  testing of an HTHP sampler for the EPA/Exxon Miniplant,
   experience was gained in design aspects of HTHP sampling equipment and testing
   procedures and is  highlighted in this  report.   A background study  and planning
   effort was directed toward possible  future sampling efforts in a coal
   gasification facility.   A state-of-the-art review of HTHP sampling was also
   performed.   As a means  of documenting  the  materials collected, a bibliography
   of articles, reports and books relating to HTHP sampling was compiled.
   Further a  mailing  list  of persons interested in this technology is included in
   the report.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                              b.IDENTIFIERS/OPEN ENDED TERMS
                           c. COSATl P'ield/Croup
                                               Particulate  samp!ing
                                               High-temperature
                                               High-pressure
                                               Extractive sampling
                                               Pressurized  fluidized
                                               combustion
                                               Gasification
                        bee
18. DISTRIBUTION STATEMENT

  Release Unlimited
19. SECURITY CLASS (This Report}
 Unclassified
21. NO. OF PAGES
     13"
20. SECURITY CLASS (This page)

 Unclassified
                                                                         22. PRICE
EPA Form 2220-1 (Rev. 4-77)
                      PREVIOUS EDI TION IS OBSOLETE
                                            127

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