Volume 1, Number 1
        Research Triangle Park, N.C. 27711
                                                                 First Quarter, 1978
                       PMB SYMPOSIUM:
                       ADVANCES  IN
                       PARTICLE SAMPLING
                       AND MEASUREMENT
  The Process Measurements Branch (PMB) of
the  EPA Industrial Environmental Research
Laboratory (IERL/RTP) is responsible for the
development, assessment, and application of
measurement techniques for the energy and in-
dustrial process research  and development
programs conducted by the IERL/RTP. The
PMB program is twofold, addressing both en-
vironmental assessments and  control  tech-
nology  applications.  The  Process  Meas-
urements Review,  published quarterly, will
report on items of interest in these areas.
  Articles  describing advances in sampling,
analysis, quality assurance, and on-line process
control will be featured. While this first issue
is primarily based on work sponsored by PMB,
future issues will feature articles submitted by
other organizations. Suggestions for  future
articles are actively solicited (see page 8).
  The  Process Measurements  Review  is
available to anyone involved in or interested in
measurement techniques applicable to the
characterization and evaluation of energy and
industrial processes and control equipment. If
you  would  like  to   be  on  the  Proc-
ess  Measurements Review  mailing list, com-
plete and return the request form on page 7.
                         "Advances  in  Particle Sampling  and
                       Measurement," a symposium sponsored by the
                       IERL/RTP Process Measurements Branch will
                       be from May 15 through May 17, 1978 at the
                       Grove Park  Inn in Asheville, North Carolina.
                       The symposium will be a gathering of experts
                       in the areas of particle sampling and measur-
                       ing technology. Eighteen invited speakers will
                       discuss the  status  of current research and
                       development in this science, with ample time
                       allotted for  questions, discussions, and infor-
                       mation exchange. Take this opportunity to talk
                       with the experts in this field. For further infor-
                       mation please contact Kenneth M. Gushing at
                       Southern Research Institute, (205) 323-6592.
                            The views expressed in the Process
                          Measurements Review do not necessarily
                          reflect the views and policies of the En-
                          vironmental Protection Agency. Mention of
                          trade names or commercial products does
                          not constitute endorsement or recommenda-
                          tion for use by EPA.

Process Measurements Review
                                                          Volume 1, First Quarter, 1978
                                             MEASUREMENT PROGRAMS
  The  Industrial Environmental  Research
Laboratory of the U.S. Environmental Protec-
tion Agency has the responsibility of develop-
ing control technology for energy  and  in-
dustrial processes.  Within IERL/RTP, the
Process Measurements Branch is responsible
for all measurement programs. Major areas of
responsibility include:
     Methods evaluation and development
     Review of test programs
     Review of proposals
     Evaluation of results
     On-site troubleshooting
     Special field studies
  In addition to the permanent technical staff,
which includes chemists, engineers, and techni-
cians, other professionals are on staff by ap-
pointment from  universities. As  indicated
below, these professional staff members have
been  assigned select areas of measurement
technology responsibility.
                Organic Sampling and
                Bioassay Procedures

                Manual Particulate Mass
                and Size,

                High Temperature
                Sampling, Quality
 Frank Briden    Inorganic Analysis,
                Computer Facilities

  PMB  staff members can be contacted  at
Larry Johnson
Ray Merrill
Bruce Harris
Bill Sensing
BUI Kuykendal
Ben Smith
  Presently, much emphasis within the PMB is
being placed  on. measurements for the  en-
vironmental  assessments  program. The
ultimate goal of this program is to assure that
effluent streams from  industrial or energy
processes are environmentally acceptable or
that adequate control technology either exists
or  can  be developed  for those processes.
Twelve major contracts have been funded by
the engineering  branches in  IERL/RTP to
develop engineering, industrial, and energy
processes data. These methodology programs
are described in the "Current Status Guide to
IERL/RTP  Environmental   Assessment
Methodology" (draft).
  To characterize the effluent streams from in-
dustrial or energy processes, two different ap-
proaches to a sampling  and analysis program
were considered by the PMB. Because of its
cost effectiveness,  a three-level phased  ap-
proach was selected. In  a program employing
this phased approach, all streams would be in-
itially characterized during Level  1 using
generalized screening  methods. This  would
allow the ranking of the streams on the basis of
their relative hazard.
  The most hazardous streams would then be
subjected to the more complex  sampling and
analytical methods of Level 2 to identify and
quantify specific organic and inorganic species.
Finally, during Level 3, continuous monitoring
of certain indicator compounds in the streams
would take place to provide data for use in the
design and development of control devices.
  To provide technical assistance and support
in the administration  of  the environmental
assessments  program,  an Environmental
Assessments  Steering  Committee  has  been
formed. The Committee is composed of experts
in  environmental  measurements from  the
government and the private sector. Within the
Committee there is a Bioassay Subcommittee,
which addresses biological measurement of en-

.Process Measurements Review
             Volume 1, First Quarter, 1978
vironmental pollutants  and  bioassay inter-
pretation problems. The Steering Committee's
objective is to evaluate  the  concept  of the
phased approach and to  correlate  biological,
chemical, and  engineering data to  provide a
meaningful assessment of the effect a pollutant
has on the environment.
  In June of 1976, the PMB issued a  document,
EPA-600/2-76-160a, delineating sampling and
analysis procedures for Level 1 Environmental
Assessment Studies. Since that time, PMB has
been reviewing these methods and evaluating
alternatives in an attempt to simplify data ac-
quisition and optimize information recovery.
While examining, among  other things, actual
field experiences, this investigation has iden-
tified several modifications that will improve
the original procedures. The evaluation of the
original procedures will continue and further
modifications are expected. Brief descriptions
of changes are on page 5 of this issue.

  Three key manuals describe the phased ap-
proach in detail. They are:

  1. IERL-RTP Procedures Manual: Level 1
     Environmental Assessment (EPA-600/2-
     76-160a, PB 257-850/AS).
  2. IERL-RTP Procedures Manual: Level 1
     Environmental  Assessment   Biological
     Tests   for Pilot Studies  (EPA-600/-
     7-77-043, PB 268-484/AS).
  3. Environmental  Assessment  Sampling
     and Analysis:  Phased  Approach  and
     Techniques  for Level   1  (EPA-600/-
     2-77-115, PB 268-563/AS).

  These documents are available from the Na-
tional Technical Information Service.

   The phased approach to the environmental
assessment of energy and industrial processes
is based on the use of specified procedures for
sampling and  analysis. Research Triangle In-
stitute (RTI) at Research Triangle Park (RTF),
N.C. is  under  contract to the EPA Industrial
Environmental Research Laboratory to inter-
pret and supplement these Level 1 procedures.
This service is intended to provide current in-
formation on the phased environmental assess-
ment technology to those involved in sampling,
analysis, and technical support. RTI will act as
a receiving agent for questions, comments, and
problems. Matters that cannot be resolved in-
house will be transmitted to the appropriate in-
dividual in the Process Measurements Branch,
IERL/RTP, for resolution. Problems of general
concern will be studied and could result in pro-
cedural revisions. Questions and comments of
general interest  will be reported in future
issues of the Process Measurements Review.
  For assistance  from the User's Update Ser-
vice,  please  contact Ann  Turner  at  RTI,
(919)541-6893.  We encourage your participation
in this information exchange process.

  The  Process  Measurement  Branch  of
IERL/RTP held a symposium for environmen-
tal  assessment measurements  in Atlanta on
February 13-15, 1978. The  first  day's  pro-
ceedings consisted of an overview of the En-
vironmental Assessment program, including
presentations  of  its  concepts and  uses by
various groups both within and outside of the
Environmental  Protection  Agency.  The
highlight of this session was the keynote ad-
dress by  Stephen J. Gage,   Assistant Ad-
ministrator for Research and Development  of
the EPA.
  Included in  Tuesday's session on Measure-
ment Technologies were presentations on the
measurements of inorganic,  organic,  and
fugitive emissions, the field evaluation of the
SASS train  and Level 1 procedures, and the
sampling of high-temperature, high-pressure
  The final day of the symposium  focused on
Industrial and  Energy Processes Applications.
Among the  processes discussed were petro-
leum refining, textile industries, nonferrous
metal  processing, conventional  combustion
systems, fluidized-bed combustion, glass in-
dustries, gasification and synthoil/synthane
processes,  waste-as-fuel  processes,  and oil
shale processes. Proceedings of the symposium
will be published in June.

Process Measurements Review                              Volume 1, First Quarter, 1978


  To improve the quality of data derived from environmental assessment and control technology
studies, IERL/RTP has included a comprehensive program of quality assurance (QA) activities within
the structure of the Laboratory's measurement program. In addition to improving data quality, the
goals of the QA program include assuring, assessing, and documenting the quality of data derived.
IERL/RTP, in cooperation with the quality assurance contractor, Research Triangle Institute, expects
several benefits from the QA program. Perhaps one of the most important benefits is the increased
acceptance and use of program-generated data, which is due to increased credibility. Other benefits
include identification of potential sources of error in measurement systems, establishment of an in-
creased awareness of common data quality problem areas, and establishment of a central location for
documentation  of measurement methods  and data quality.
  Currently, several QA activities are available to environmental assessment/control technology con-
tractors. These are  intended to  assess and document their  measurement data quality.  Research
Triangle Institute is performing both performance and systems audits on field and central laboratory
operations. Performance audits are quantitative and involve challenging analyzers or other measure-
ment systems  with  audit standards  or  devices built around or  traceable to National Bureau of
Standards-Standard Reference Materials (NBS-SRM). Such audits are conducted routinely for various
parameters and measurement systems, many of which are listed below.

                Gaseous Parameters
                  •  Oxides of nitrogen
                  •  Sulfur species
                  •  Low molecular weight alkanes
                  •  Fixed gases

                Liquid Parameters
                  •  Various nutrients  in water
                  •  Various minerals in water
                  •  Various physical parameters of water solutions
                     (e.g., pH, conductivity, turbidity)
                  •  Extraction of organics

                Measurement Systems
                  •  Volumetric flow, velocity, etc.
                  •  Parr bomb combustion-spark source mass spectroscopy
                  •  Infrared analysis
                  •  Low resolution mass spectroscopy
                  •  Liquid chromatography
                  •  Temperature

  Systems audits, conducted by experienced personnel, consist of on-site evaluations of an organiza-
tion's ability to perform a specific measurement. The audit is based on a review of facilities, equip-
ment, recordkeeping, personnel training  procedures, etc. The scope of this audit can vary, covering
anything from a laboratory's ability to conduct Level 1 analyses to a team's ability to properly use a
SASS train.
  The result of these audits is a report documenting the quality of data being produced by a particular
measurement process. This report also identifies any problem areas incurred, thus enabling project
personnel to remedy the problem(s) and thereby improve data quality.
  Contractors  desiring these services should ask their EPA project officers to contact William B.
Kuykendal, the IERL/RTP quality assurance coordinator and project officer for the QA contract.

Process Measurements Review                               Volume 1, First Quarter, 1978
    Change 1 -  "Silica Gel Drying in Fourth SASS Impinger"
               Chapter III, Page 39
               Date Accepted: December 15, 1977

     The original procedure specified the use of Drierite in the fourth SASS impinger for gas
    drying. However, Drierite, in some cases, had to be renewed frequently during a sampling run
    due to limited capacity. Silica gel has been found to have a greater capacity than Drierite and,
    accordingly, reduces the workload on the field sampling team.

    Change 2 •  "Hydrogen Peroxide for First SASS Impinger"
               Chapter III, Page 39
               Date Accepted: December 15, 1977

     Oxidizing conditions must be maintained in the first SASS impinger to neutralize reducing
    gases before the sample is scrubbed in the trace metals collection solutions. The 6M hydrogen
    peroxide originally specified for use in the first impinger did not always provide sufficient ox-
    idizing potential  and has been replaced by 750 ml of a 30 percent solution of nonstabilized
    hydrogen peroxide.

    Change 3 -  "Passivation of Series 300 Stainless Steel"
               Chapter HI, Page 36
               Date Accepted: December 15, 1977

     The SASS stainless steel components require  initial cleaning and  periodic  cleaning
   thereafter whenever the system is placed in operation. However, the 1:1 nitric acid originally
   specified for cleaning and passivation is a more rigorous procedure than required, sometimes
   resulting in excessive  corrosion. Therefore, the cleaning specification has been changed to
   state that contact with 15 percent nitric acid for 30  minutes is sufficient.

   Change 4 •  "Cooling of Liquid Chromatography Columns"
               Appendix C, Page 127
               Date Accepted: January 19, 1978

     Sufficient heat of adsorption is generated during the LC analysis to warrant external cool-
   ing of the column. The  original procedure specified the use of towels soaked with acetone to
   accomplish this. However, this cooling is not efficient and the procedure has been modified to
   require that all columns be water jacketed. The water coolent must remain between 18-22° C
   and at a flow rate of 5  ml/min.

   Change 5 -  "Deletion  of Liquid Chromatography Fraction 8"
               Chapter VIII, Page 101
               Date Accepted: January 27, 1978

     Elution of samples from the silica gel liquid Chromatography column currently involves the
   use of eight solvent fractions. Laboratory data indicate that silica gel is dissolved by the
   eighth fraction of this solvent system. Data also indicate that no organics are desorbed from
   the column by this fraction. Therefore, use of the eighth fraction is deleted. The first seven
   fractions only will be used for separation of sample components.
          Revisions appear in condensed form. For complete change notices, contact Ann Turner at RTI.

 Process Measurements Review
             Volume 1, First Quarter, 1978
   The  following  abstracts  of  publications
 report  on  developments in  the  field  of
 measurements for control technology. In this
 and future issues, the Process Measurements
 Review will be focusing on such pertinent ad-
 vances  in this, as well as the environmental
 assessments   field.  These  publications  are
 available from the National Technical Informa-
 tion Service.
 A. C. Eckbreth, P. A. Bonczyk, and J. F. Ver-
 dieck,   Review  of  Laser  Raman  and
 Fluorescence  Techniques for Practical Com-
 bustion  Diagnostics,  EPA-600/7-77-066,  PB

   This report reviews various laser techniques
 potentially suitable  for  "point" temperature
 and concentration  measurements  in flames.
 From these, four techniques are selected for
 detailed  evaluation  including: (1) spontaneous
 Raman   scattering,  (2) near-resonant Raman
 scattering,  (3)  laser  fluorescence,  and (4)
 coherent  anti-Stokes  Raman  scattering
 (CARS).  The spectroscopy of species of interest
 in combustion monitoring is discussed and the
 application  of the  foregoing techniques to
 detection of these species is examined.
  The basic principles of physics employed in
 the operation  of these techniques as well as
 characteristics  of the method such as sensi-
 tivity and signal-to-noise ratio are discussed.
 Problem  areas are examined and variations on
 the basic technique  introduced. Practical con-
 siderations are  reviewed with emphasis on
 noise sources, medium perturbations, laser and
 signal transmission,  and signal averaging in
 temporally fluctuating media.  Measurement
 systems  are described  including  cost  esti-
 mates, probability of success assessments, and
 risk  assignments. Application of these tech-
 niques   to  temperature  measurement is
presented.  General  conclusions,  suggesting
 future research efforts required for the evalua-
 tion  and development of the  more promising
 diagnostic approaches, are given.
W. B. Smith, P. R. Cavanaugh, K. M. Gushing,
W. Farthing, and  R. R. Wilson, Technical
Manual: A Survey of Equipment and Methods
for Particulate Sampling in Industrial Process
Streams, Southern Research  Institute,  draft
report, SORI-EAS-78-51 3630-19TM, (EPA Con-
tract 68-02-2131).

  This  technical manual describes  the  in-
struments  and  techniques  available  for
measuring the concentration  or size distribu-
tion of particles suspended in process streams.
The standard (or well established) methods  are
described,  as  well  as  some  experimental
methods and prototype instruments. To the ex-
tent that  the information could  be found,  an
evaluation of the performance of each instru-
ment is included.
  The  manual  contains  descriptions of  in-
struments and procedures for  measuring  mass
concentration,  opacity,  and particle  size
distribution.  Procedures for planning and  im-
plementing tests for control device evaluation
are discussed. A glossary and an extensive
bibliography are also included.
W. B. Smith, K. M. Gushing, and J. D. McCain,
Procedures  Manual  for  Electrostatic
Precipitator Evaluation, EPA-600/7-77-059, PB

  This manual describes methods to be used in
characterizing the performance of electrostatic
precipitators for pollution control. A detailed
description of the mechanical and  electrical
characteristics  of these  control devices  is
given. Procedures are described for measuring
the particle size distribution, the mass concen-
tration,  and  the  concentrations  of  major
gaseous components of flue gas-aerosol mix-
ture. Also given are procedures for measuring
the electrical  resistivity of the  particles. A
discussion and  outline,  which  describe the
development of a test plan for the evaluation of
a precipitator,  are also included.

Process Measurements Review
                          Volume 1, First Quarter, 1978

N. Zimmerman,  D.  C. Drehmel, and  J.  H.
   Abbott, Characterization and Generation
   of Metal Aerosols, EPA-600/7-78-013, NTIS
   No. PB 277013, (2/78).

L.   M.  Schalit   and   K.   J.   Wolfe,
   SAM/IA: A Rapid Screening Method for
   Environmental  Assessment of  Fossil
   Energy  Process Ef'fluents,EPA-600/
   7-78-015, NTIS No. PB  277088, (2/78).

R. Stone and  R. Kahle,  Environmental  As-
   sessment of Solid Residues From Fluid-
   ized-Bed  Fuel  Processing, EPA-600/
   7-77-139, NTIS No. PB  276879, (12/77).

K. J. Bombaugh, Analyses of Grab Samples
   From Fixed-Bed Coal Gasification Proc-
   esses,  EPA-600/7-77441,  NTIS  No.  PB
   276608, (12/77).

R. E. Barrett, W. L. Margard, J. B. Purdy, and
   P. E. Strup,  Sampling and Analysis  of
   Coke-Oven  Door  Emissions,  EPA-600/
   2-77-213, NTIS No. PB  276485, (10/77).
             G. T. Brookman, J. J. Binder, and W. A. Wade
                III, Sampling and Modeling of Non-Point
                Sources at a Coal-Fired Utility, EPA-600/
                2-77-199, NTIS No. PB 274-369, (9/77).

             L. G. Felix, G. I. Clinard, G. E. Lacey, and J. D.
                McCain,  Inertial  Cascade  Impactor
                Substrate Media for Flue Gas  Sampling,
                EPA-600/7-77-060, NTIS No. PB 276583,

             J.  Adams,   K.  Menzies,  and P. Levins,
                Selection  and  Evaluation  of  Sorbent
                Resins for the Collection of Organic Com-
                pounds,  EPA-600/7-77-044, NTIS No. PB
                268-559, (4/77).

             D. B. Harris, Procedures for Cascade Impactor
                Calibration  and Operation in  Process
                Streams, EPA-600/2-77-004, NTIS No. PB
                263-623, (1/77).
              Copies of these publications may be ordered
                  National Technical Information Service.
                  U.S. Department of Commerce
                  5285 Port Royal Road
                  Springfield.Virginia 22151
                      Request for the Process Measurements Review
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                    Return to:
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Research Triangle Institute
P.O. Box 12194, Building 6
Research Triangle Park, N.C. 27709
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        Process Measurements Review
                                          Volume 1, First Quarter, 1978
         The Process Measurements Review is prepared by the Research Triangle Institute, P.O. Box 12194,
       Research  Triangle  Park,  N.C. 27709 for  the U.S. Environmental Protection Agency, Industrial
       Environmental Research Laboratory, Process Measurements Branch, Research Triangle Park, N.C.
       27711 under EPA Contract No. 68-02-2156. The EPA Task Officer is James A. Dorsey (919-541-2557)
       and the RTI Editor is Raymond M. Michie, Jr. (919-541-6492). Contributors to this issue were Nancy H.
       Gaskins, Donald E. Lentzen, Ann R. Turner, and Eva D. Estes. Comments on this issue and sug-
       gestions for future topics are welcome and may be addressed to either the Task Officer or the Editor.
United States
Environmental Protection
Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, N.C. 27711
Official Business
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