GUIDELINE  SERIES
           OAQPS NO. 1.2-017
                       (Revised 5/74)
     A DESCRIPTION OF THE ANALYTICAL TECHNIQUES
     AND ASSOCIATED SAROAD METHOD CODES USED IN
     STORING DATA IN THE NATIONAL AEROMETRIC
                DATA BANK
    US. ENVIRONMENTAL PROTECTION AGENCY
       Office of Air Quality Planning and Standards


         Research Triangle Park, North Carolina

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               UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
             Office of Air Quality Planning and Standards
             Research  Triangle Park,  North Carolina  27711
       [Description of the Analytical Techniques     DATE:  3 1 MAY W4
        and Associated SAROAD Codes Used in Storing
        Data  in the National  Aerometric Dat^uBank
FROM:    OAQPS #1.2-017             j M
                                                              n

                                                            T
                                                             '
        Robert E.  Neligan, Director ^
T       Monitoring and Data Analysis Division
        Surveillance and Analysis Division Directors, Regions I-X
        Air and Water Analysis Division Directors, Regions I-X

            Enclosed is a copy of guideline document OAQPS #1.2-017.
        The previous draft has been revised based on comments from
        the Regional Offices and NERC-RTP.  The document relates
        SAROAD pollutant method codes with analytical1 techniques
        for which data have been submitted since 1969.

            The principal purpose of this guidance is to establish
        uniformity in reporting data to 'the NADB as well as to
        prevent data from being reported under the wrong code .  It
        is extremely important that air quality data be reported
        under the correct code number because all of our analyses
        and air quality trend statistics are derived.. from these     :-
        code numbers.  Incorrectly coded data may" l4ad to incorrect
        statements that a site has. exceeded standards.
                ."* '-"' •''"'.      -             i
            The Regional Office must take the lead and supervise a
        survey of the various monitoring techniques and SAROAD method
        coding used at each site under their jurisdiction to verify
        if they differ from those described in this guideline.  We
        would appreciate a reply from your office when you have
        surveyed the sites under your jurisdiction.

            Should a technique or code be usedvthat is not described
        in this document, please follow the instructions found on
      .  page 2 and report any differences to the Chief of the Data  .
        Processing Section, NADB, Durham, North Carolina (919/688-8247)

            If there are any further questions or comments, please
        contact Mr. William Cox of the Monitoring and Reports Branch
        (919/688-8312) .
                                     Robert E. Neligan

        Enclosure
EPA Form 1320.6 (R»». 6-72)



                                                                        A

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      A nnrCP.IPTTON' OF THE .MIALYTICAL  TECIII-riQUIiS AND
          AHSCCIAT-JD SAROAD METHOD  COIDJ:S ucr-iv in
  STORING DATA  III THE NATIONAL AERCMETRIC DATA BANK
                       OAQPS 1.2-017
                          J4arch 1974
                           Revised
                         May 30,  1974
               Monitoring and Reports  Branch
       Office  of Air Quality Planning and Standards
                            and
Quality Assurance and Envirc:
             Office; o.~. P.oqcarc
          I-,Ta t i en a 1 !;:; v ir crjru..-1
r.ontal Monitoring Laboratory
        arcii  Center
           U.  S.  Envi::o:vnantal 1'rotection Agency
      Research Triangle Park, :,'orth Carolina  27711

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                  TABLE OF CONTENTS

                  • '  •  • '••.'      '  ":-••••             Page
Introduction                         •'               1
Suspended Particulates                              3
Benzene Soluble Organic                             3
Soiling Index                                       4
Light Scatter                                       4
Radioactivity                                       4'
Metals, by Hi-Vol, AA, Emission Spectra             6
Arsenic                                             9
Mercury                                             9
Water Soluble Particulates                         10
Benzo(A)Pyrene                                     15
Dustfall Procedures                                16'
Carbon Monoxide                                    23
Sulfur Dioxide                •                     24
Hydrogen Sulfide               .                    27
Sulfation Rate Procedures  •  '                      28
Fluoride Ion                                       31
Nitrogen Oxides        .                            32
Ammonium                                           36
Hydrocarbons                                       38
Aldehyde       .                              .      39.
Oxidants                                           40
Ozone                                              43

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     The  purpose of  this  document is  to  bring  together  for
 the  first time a SAROAD  code number  with a description of
 the  analytical technique used in gathering data stored in  the
 National Aerometric Data Bank (NADB).   It has long  been
 needed.   The SAROAD code numbers and methods  in this
 compilation are only those for which data have been sub-
 mitted since 1969.   The  titles of the methods (in capital
 letters  following the code number) are  those  v/hich  were
 assigned in the past and which appear  in the  computer
 printout of Common  Parameters and Methods (the "Farm File"),
 similar  to Code Table 4  of the SAROAD  Users Manual.
     It is to be emphasized that we do  not endorse all  of
 the  procedures described herein.  Some  are known to yield
.erroneous or misleading  data.  Nor do  we endorse a  par-
 ticular  manufacturer's instrument even though the name is
 referred to in a title..  The rule governing the compilation
 was:  every method  used  since 1969 together with its Farm
 File title is to be included for the purposes of completeness.
     Beneath each SAROAD  number and title there is a brief
 description of the  sampling and analysis principles followed
 by references which the  reader should  consult fcjr details.
 Whenever possible,  we have given references to those pub-
 lications which we  think should be readily available to
 field workers.  In  no case have we included enough  details
 for a worker to start an analysis program which will produce
 valid data.  The references must be  consulted.
     Instrumental techniques have not been thoroughly re-
 ferenced and the instrument user should, consult the pro-
 cedure prepared by the manufacturer.

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    Through this publication we hope to achieve some degree
of uniformity in reporting data to the NADB.  If, for example,
data have been submitted to the Bank under a given code number,
but the description of that method as found in this compilation
is different from the method which was actually used to obtain.
the data/ then the reporter must do one of three things:

    a.  he must begin submitting data under the proper
        code number which agrees with the method actually
        used; (data previously reported must be re-reported
        under the correct code);

    b.  the reporter must change his methodology to agree
        with the method described and data then submitted
        using that code number; or

    c.  a nev; code number must be applied for.

    We encourage the persons who submit data to the NADB
to verify with the laboratory personnel that the SAROAD codes
used agree with the analytical procedures described herein.
If there are problems or questions, we urge you to call the
chief of the data processing section, NADB, Durham, N.C.
(FTS 919/688-8247); or your SAROAD contact or quality control
coordinator in the Regional Office.  Also, we will welcome
your pointing out any errors and/or omissions in the text.
There are a few blanks which we have not been able to fill
in.

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 11101 91  SUSPENDED PARTICULATE - HI-VOL - GRAVIMETRIC
           Air is drawn at 40 to 60 ft-.3/rain through a glass
           fiber filter, by means of a blower, and the sus-
           pended particles having a diameter between 100
           and 0.1 ym are collected.  The suspended particulate
           is calculated by dividing the net weight. o:f the
           particulate by the total air volume'sampled and
           reported in density units as yg/m^.  Heavy
           loading of suspended particulate, oily particulates,
           or high humidity can cause reduced air flow
           through the filter.  Therefore, flow rates should
           be measured before and after the sampling period.
           1.  "Rules and Regulations," Federal Register,
           Vol 36, No. 228, U.S. Government Printing Office,
           Washington, D.C.,  (Nov. 25, 1971), p 22388.
           2.  Intersociety Committee, "Methods of Air
           Sampling and Analysis," American Public Health •
           Association, Washington/ D.C., 1972, p 356.
           3.  "Air Quality Data for 1967," EPA-APTD-0741, :•'
           Office of Technical Information and Publications,
           Research Triangle Park; North Carolina, 1971,
           p 17.
11103 91  BENZENE SOLUBLE ORGANICS - HI-VOL BENZENE EXTRACTION
          An 8% aliquot of the filter is placed in a soxhlet
          extractor and extracted with 75 ml of benzene for 6 h.
          The benzene is evaporated and the residue is weighed and
          reported in aerometric units; yg/m^.  Errors may result
          from non-volatile material in the benzene used for
          extraction.
          1.  Stanley, T. W., J. E. Meeker and M.  J.  'Morgan, (1967),
          Environ. Sci. and Tech. 1, (11), 927.
          2.  "Air Quality Data for 1967," EPA APTD-0741, Office
          of Technical Information and Publications,  Research
          Triangle Park, North Carolina, 1971, pp 17-18.

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11201 81  SOILING INDEX CCOH) - TAPE SAMPLER   TRANSMITTAMCE
          Air is drawn through a 1 in. diameter spot on a con-
          tinuous strip of filter paper.  The measurement is based
          on light transmission through the spot having the col-
          lected matter on it,- and reported in COH's (coefficient
          of haze) per 1000 linear foot of sampled air.  The
          standard is a clear spot on the paper.  The inlet air
          funnel must be kept upside dovm, and sampling lines
          must be kept short.
          1.  Water, Atmospheric Analysis, (1971) , "Annual Book-
          of ASTM Standards," American Society for Testing and
          Materials, Philadelphia, Pa., Part 23, p 420.
          2.  "Air Quality Data for 1967," EPA APTD-0741, Office
          of Technical Information and Publication, Research
          Triangle Park,--North Carolina, 1971, p 20.

11202 91  SOILING INDEX (RUD) - TAPE SAMPLER - REFLECTANCE
          The sampling procedure is similar to that of 11201 81.
          Measurement of the soiling is based on light reflectance
          from the spot and is reported in RUD's  (reflectance
          unit density) .
          1.  Water, Atmospheric Analysis, (1971), "Annual Book
          of ASTM Standards," American Society for Testing and
          Materials, Philadelphia, Pa., Part 23, p 420.

11203 11  LIGHT SCATTER  NEPHELOMETER         .    •
          Air enters an optically black metal tube at 5 cfm.  Light
          of 410 nm is scattered from particles in the air stream.
          The amount of light scattered at 90° from the main beam
          is measured by a phqtomultiplier tube.     '
11302 91  RADIOACTIVE-GROSS-BETA-HI-VOL  PROPORTIONAL COUNTER
          The radioactive matter on a filter paper is counted with
          a beta sensitive detector to establish the gross concen-
          tration of beta emitters in the sampled ambient air.  The
          daughter products of natural radon and thoron in the at-
          mosphere can be minimized by waiting three days until they

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have decayed.  A self-absorption correction must be made
if inert matter on the filter interferes.
1.  Intcrsociety Committee, "Methods of Air Sampling and
Analysis/" American Public Health Association, Wash., D.C.,
1972, p 379. '           '   •
2.  Settler, L. R. and G. I. Coats,  (1964), "The Determi-
nation of Airborne Radioactivity,"' Amer. Tnd.' Hygiene
Assoc., J. 22, 64.
.3.  Schulte, H. F., Monitoring Airborne Radioactivity,
"Air Pollution," Vol II, 2nd Ed., A. C. Stern, Ed.,
Academic Press, New York, N. Y., 1968, p 393.

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12101-12185           ATOMIC ABSORPTION  (AA)
         Aliquots of samples from the low temperature ashing
         procedure are sprayed into a reducing flame by an
         atomizer,  where metal ions are reduced to the atomic
         state.   The atoms absorb monochromatic light pro-
         duced by a lamp having a cathode made of the element
         to be measured.  The light absorbed by the atoms in
         the flame is a measure of their concentration.  The
         influence of one element on the excitation potential of
         another does not interfere.  The analysis of Al, Sb,
        i
         l\s, Be, Bi, Ba, Cd, Ca, Cr, Co, Cu, Fe, Pb, Mn, Mo,
         Ni, Hg, Sn, Ti, V, and Zn is. done by AA. .The AA
         is more sensitive than emission spectra for most
         metals.
         1.  W.  Slavin,   "Atomic Absorption Spectroscopy,n
         Interscience Publishers, New York, 1968, pp 69-74.
         2.  Perkin Elmer Corp., Methods Manual-Analytical
         Methods for Atomic. Absorption Spectrophotometry,
         The Perkin Elmer Corp., 1968.
         3.  F.  J. Welcher, Standard Methods of Chemical Analysis,
         D. Van  Nostrand Company, Inc., Princeton, New Jersey,
         1966, p 105.
         4.  Thompson, R. J., G. B. Morgan, and L. J. Purdue,
         (1970), "Analysis of Selected Elements in Atmospheric
         Particulate Matter by Atomic Absorption," Atomic•
         Absorption Newsletter 9,  (No. 3), 55.

L2102-12185              EMISSION SPECTRA
         A solution containing metallic ions is placed between
         two electrodes and subjected to 13-15 kilovolts AC
         discharge.  The spark so created generates enough
         heat to atomize the ions and the high voltage excites
         many electrons per atom.  Spectra characteristic of
         each element are fprraed when the electrons return to

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        their  normal energy levels.  Internal standards are
        used to reference a knovm spectral line so that other
        lines  can be located.. NASN uses indium and yttrium
        as  internal standards:  Metals .as Sb, Be, Bi,  Ba,
        Cd, Cr, Co, Cu, Fe, Pb,'Mn, Mo, Ni,  Sn, Ti, Siu, V,
        and Zn are analyzed by emission spectra.
        1.   H. H. Willard, L. L. Merritt, J. A. Dean,  "In-
        strumental Methods of Analysis," D.  Van Nostrand
        Company, Inc. 4th Edition,  1965, p  280.
         2.   P. J. Welcher,"Standard Methods-of Chemical Analysis,"
         D.  Van Nostrand Company, Inc., Princeton,  New Jersey,;'
         1966,  p 141.    ...                     '                   ' •
         3.   "Air Quality Data for  1967,"  EPA-APTD 0741, (1971),
         Office of  Technical  Information  and Publication, Research
         Triangle Park, N.C.,. 1971, p 19.     v  ,

12102-12185  "   .  .LOW TEMPERATURE  ASHING PROCEDURE        /:<-
     i.'           • ''           .'       .     .-•;        '"' - '     '    '.
         Particulates are^ashed to  remove organic matter.  A/1'..o'r
        ^2-an.  ,by^,7  in. strip,.of the exposed glass filter  (orv\.a  .
         cprnposit'e1 of, 5-8/MS'trips)  is heated' at 150°C for 1 hr;'"at:
         1 torr with an 02  flow of  3000 ml/h. ,The .ashed filter.
         ,is fluxed  for  3  h. with 8  ml 'of  20%-^HCl and 32 ml of
         40% HNO-,:   The acid  extract is * concentrated to 1 or-2 ^
           '  y'3. '       •             •'.     ,n   •'•         •  •- '"•'  •
         ml-by evaporation, centrifuged,  "and the .residue is
            v1'.      h'   '        '      -i\ ,• "•..       '
        .washed  three times with dilute' HCl.  'Samples  from non-  :
         urban air  are  then diluted w,i'£Ji dis^til,led H^O to 3 ml/2
         in. strip  and  samples from urban air are diluted to XL4"
            j      *5   *   '.^                      •   ...           .- -
         ml/9-  in.  .of filter  taken. ,Samples- so prepared are''',
         .rfady ;foir  emission spectra analysis, but must be diluted
        '10 .fold  for'AA analysis. '  •              '..     ;.    *•'.*'•-;&•"
         1.  Thompson,  R. J.,  G.  B. Morgan and L.  J:. Purdue,
         (19'70)  "Analysis of  Selected Elements in Atmbspheric
                        \      .           -••••.  r
         Par,ticulate Matter by Atomic Absorption," Atomic
         Absorption newsletter 9,  54.

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12102-12185           MUFFLE FURNACE PROCEDURE
          Prior to the invention of the low temperature asher,
          organic material was removed by .heating samples to
          500°C for 1 h. in a muffle furnace.  Samples are then
          extracted twice for 1 h. with 40 ial of 1:1 redistilled
          HNO., at a temperature just below boiling.  The solution
          is filtered, evaporated to 4 ml and diluted to 10.4
          ml with H20.  The samples are then analyzed by the
          emission spectrograph.  Metals as Sb, As, Be, Bi, Cd,
          Cr, Co, Cu, Fe, Pb, Mn, Mo, Ni", Sn, Ti, V, and Zn are
          measured by this procedure.  This procedure may volatilize
          some portion of some.of the metals and thus result in
          an unknown fraction recovered.

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12103 93  ARSENIC - HI-VOL   NASN-ARSINE-COLORIMETRIC
          The arsenates arid oxides of arsenic are extracted from a
          2 in. square opposed filter by digestion for 1 hr with .
          30 ml of 6 N HC1 at 90°C,.and then reduced to the trivalent
          state with KI and SnCl,.  Arsine is then generated by Zn
          and HC1 Gutzeit procedure.  The evolved arsine passes
          through a H^S scrubber and into an absorber containing silve
          diethyldithiocarbamate.  The resulting red complex is
          measured spectrophotometrically at 535 nm.  Antimony like-
          wise forms stibine which also complexes with the-carbamate
          but at low concentrations does not interfere with arsenic
          determination.  High concentrations of Ni/ Cu/ Cr, and
          Co interfere with arsine formation.  Many interferences
          can be minimized by using an internal standard of added
          arsenic.
          1.  Inter society Committee, ".Methods of Air Sampling and
          Analysis," American Public Health Association,• Wash., D.C.,
          1972, p 289.

12142 92  MERCURY - ACID IC1   ATOMIC ABSORPTION
          This is a flameless AA technique.  The total mercury is
          collected through a glass impinger in 30 ml of 0.1N
          acidic iodine monochloride at a flow-rate of 200 ml/min.
          Hgl^ is reduced to elemental mercury by hydroxylamine
          hydrochloride in basic solution which is aerated to
          vaporize the mercury.  The vapor is passed into a quartz
          absorption cell where it absorbs light at 253.7 nm.  This
          method is not applicable to atmosphere containing less than
          50 ng Hg/m  of air due to high and erratic-blanks.
          1.  Hatch, R. W. and W. L. Ott,  (1968), "Determination
          of Sub-Microgram Quantities of Mercury by Atomic Absorption.
          Spectrophotometry," Anal. Chem. 40, p 2085.
          2.  Lynch, A. L., R. F. Stalzer, and D. T. Lefferts,  (1968),
          "Methyl and Ethyl Mercury Compounds — Recovery from Air
          and Analysis," Am." Ind. Hygiene Assoc. JV, 79.

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                                 10
12202 Dl  FLUORIDE-III-VOL NILLARD-V.TNTER/SPECIFIC ION ELECTRODE
          The Willard-V.'intcr distillation is carried out to remove
          interfering ions.  Two 1 3/4 in. diameter circles of the
          filter are placed in a platinum dish, covered with 10 ml of
                                       » .     .          *
          Ca(OII)2 suspension  (2.55 Ca by weight), and evaporated to
          dryness over a steam bath.  The residue is heated for
          30 min. in an oven at 150°C, and ignited in a muffle
          furnace at 550°C for 5-6 h.  The ash is mixed with
          Ig AgC104 and steam distilled using 10 ml of 60% HCiq4
          at 135°C.  A total of 190 ml of distillate is collected.
          The fluoride ion concentration is then measured with a
          specific ion electrode.  See 42513 91.
          1.  M. B. Jacobs, (1960), "The Chemical Analysis of Air
          Pollutants," Chemical Analysis,  Vol 1U •, Interscience
          Publishers, Inc., New York, N.Y., p 200.
12203 91  CHLORIDE-HI-VOL-THIOCYANATE
          Chloride  in  the aqueous extract of  the hi-vol particulate
          sample  forms mercuric  chloride and  liberates SCN   ion
          from mercuric  thiocyanate.   The SCN~~ ion  forms  a  colored
                         +4*+                                     • • • —
          complex with Fe     ion from  ferric  ammonium sulfate.   The
          complex is measured colorimetrically at 416 nm.
          1.  R.  B. Fisher, "Quantitative Chemical  Analysis,"
          W. B. Saunders Co.,  Philadelphia, Pa.  1957, p 238.
          2.  Morgan,  G. B.,  E.  C.  Tabor, C.  Golden,  and  H.  Clements,
          Automated Laboratory Procedure for  the Analysis of Air
          Pollutants 66-p 103B,  Technicon Industrial  Systems,
          Tarrytown, N.Y., p  536.

12301 91  AMMONIUM  - HI-VOL    NESSLER  *
          Ammonium  ion is removed from an 8%  aliquot  of the filter by-
          fluxing the  filter  in  50  ml  of- II20  for 30 min,  then  placed
          in a Nessler tube with 4  ml  of Nessler reagent.  Should

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                                 11

          the solution become cloudy, Rochclle salt solution (lOy oC
          KNaC4II406.4H20 in 20.0 ml of .01N NaOH) is added dropv/iao
          with shaking.  The absorption is read using a No. 54  filter
          with a 50 ml glass cell, using a reagent blank as reference.
          (Rochelle salt prevents Ca and Mg precipitation at the high
          pH of the Nessler reagent).
          1.   M.  B.  Jacobs,  (I960),  "The Chemical Analysis of Air
          Pollutants," Chemical Analysis,  Vol 10, Interscience
          Publishers,  Inc.,  New York,  p  216.
          2.   G. B. Morgan, E. C. Tabor, C. Golden, and H. Clements
          Automated Laboratory Procedures for the Analysis of Air
          Pollutants 66-p 108B, Technicon Industrial Systems,
          Tarrytown, N. Y., p 536.

12301 92  AMMONIUM-HI-VGL   SODIUM PHEMOLATE
          Ammonium ions are extracted from a 3/4 in. by 8 in. strip
          of the exposed filter by fluxing with  25 ml of H20.  The
          filtrate is diluted to 50 ml and sodium phenolate and
          sodium hypochlorite are added producing a blue complex v:hcn
          pH is above 7.0.  The absorbance is read spectrophotometrica
          at 626 run.
          1.  Russell, J. A.,  (1944), "The Colorimetric Estimation
          of Small Amounts of Ammonia by the Phenol-Hypochlorite
          Reaction," J. Biol. Chem. 156, 457.
          2.  Morgan, G. B., E. C. Tabor, C. Golden, and H. Clements,
         . Automated Laboratory Procedure for the Analysis of Air
          Pollutants  66-p 1083, Technicon Industrial Systems,
          Tarrytown, N. Y., p 536.
          3.  "Air Quality Data for 1967," EPA-APTD 0741,
          Office of Technical Information and Publication,  Research
          Triangle Park, N.C., 1971, p 18.

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                                 12

123oc 91 "nrrrj\TE-ni-voL   2,4 XVLENOL
          Nitrate nitrates 2,4-xylenol.  The nitrated 2,.4-xylcnol
          is separated from other water soluble colored substances
          by NaOH and toluene.  A 3/4 in. strip of the filter is
          fluxed in 25 ml of H20, filtered  (Whatman No. 1) , and washed
          until 50 ml of filtrate is obtained..  A 5 ml sample and
          15 ml of 85% H-SO are mixed, cooled, and 1 ml of 1% xylenol
          is added.  The solution is heated at 60°C for 0.5 h and
          diluted to 80 ml.  Then, 10 ml of toluene is added and the
          mixture is shaken for 2 min. in a separatory funnel.  The
          lower layer is discarded, 10 ml of 0.4N NaOH added, and
          the funnel again shaken for 5 min.  The lower aqueous layer
          is drawn through cotton into a cuvette.   The absorbance
          is measured at 435 run.
          1.  "Selected Methods for the Measurement of Air Pollutants,
          U.S. Department of Health, Education, and Welfare "999-AP-
          11, Robert A. Ta'ft Sanitary Engineering Center, Cincinnati,
          Ohio, May 1965, p 1-1.           '  .
          2.  Pate, J. B., E. C. Tabor,  (1962), "Analytical Aspects
          of Glass Fiber Filters,."'Am. Ind. Hyg. Assoc. J. 23.
          3.  Barnes, H.,  (1950), "A Modified 2,4-Xylenol Method for
          Nitrate Estimation," Analyst 75,  388.

12306 92  NITRATE-HI-VOL   REDUCTION-DIAZO COUPLING
          The nitrate is reduced to nitrite by alkaline hydrazine,
          converted to HNO^ which diazotizes sufanilamide,. and couplet
          with N  (l-naphthyl)-ethylenediamine dihydrochloride which
          absorbs light at 535. nm.
          1.  Morgan, G. B.,  E. C. Tabor, C. Golden and H. Clements,
          Automated Laboratory .Procedure  for the Analysis of Air  .
          Pollutants  66,. ? 10S3, Technicon  Industrial System,
          Tarrytown,  N. Y., p 536.
                                                                   1(1

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                                 13
          2.   "Air Quality Data for 1967," EPA-APTD 0741,
          Office of Technical Information and Publication,' Research
          Triangle Park, N.C., 1971, p 18.

12306 93  NITRATE-III-VOL   SPECIFIC ION'ELECTRODE
          The aqueous extract of a hi-vol glass 'fiber filter is
          analyzed for nitrate ion by means of a specific ion
          electrode.

12345 91  PHOSPHATE - HI-VOL-KOLYBDATE • STANNOUS CHLORIDE
          Phosphate ions in the water extract of the filter are
          precipitated as ammonium molybdophosphate in an acid
          medium, which is then reduced to a molybdenum blue com-
          plex with stannous chloride.  The absorbance is read at
          650 nra.
          1.  Water, Atmospheric Analysis,  (1971),  "Annual Book  of'
   *
          ASTM Standards," American  Society for Testing  and Materials,.
          Philadelphia, Pa., Part  23, pp  41-49.
          2.  Lundell,  G.' E. and J.  I.  Hoffman,  (1923),  "Notes on
          the Determination  of Phosphate,"' Ind. and Eng', Chem. Anal.
          Ed. 15,  71.

 12403  91  SULFATE - HI-VOL   COLORIMETRIC
          Water  soluble sulfate  is reacted with excess  reagent con-
          taining equivalent amounts of methylthymol  blue  and BaCl2.
          Ba++  and SO? ions  form BaS04  leaving a  [SO^]  equivalent
          of free methylthymol blue.  If  the  pH  is changed from  2.8
          to 12.4 by  KOH,  Ba4"*" ion forms  a  chelate with the free dye.
          The unchelnted  dye is  yellow and  absorbs light at 460  nm.
           1..  Morgan,  G.  B., E.  C» Tabo-r, C.  Golden and H. Clements
          Automated Laboratory Procedure  for the Analysis of Air
           Pollutants  66,  p 10SB, Technicon  .Industrial Systems
           Tarrytown,  N. Y.,  p 538.

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                                 14
          2.  A. L. Lazrus, K. C. Hill and J. P. Lodge, "A New,
          Colorimctric Microdetermination of Sulfate Ion in Rainv.-atcr,"
          personal communication, Division of Atmospheric Sur-
          veillance, Research Triangle Park, N.C., 1965.
          3.  "Air Quality Data for 1967," EPA-APTD ;0741,  .
          Office of Technical Information and Publication, Research
          Triangle Park, N.C., 1971, p 19.

12403 92  SULFATE-HI-VOL   TURBIDIMETRIC
          The water soluble sulfate'extract of the filter forms BaSO,
          in a BaCl2 solution.  Suspended BaS04 particles scatter
          light, and the diminished intensity of a light beam is
          measured by a turbidimeter.
          An aliquot of the filter extract is chosen so that the
          sample contains- the equivalent, of 1 to 20 yg/m  of SOT.
          To the sample diluted to 20 ml, 1 ml of ION HCl is'added,
          followed by 4 ml of a glycerol/absolute ethanol solution
          (l:2v/v).  After mixing, the absorbance is measured at
          500 nm and compared with HjO.  Then 0.25g of BaCl2 crystals
          are added and shaken to dissolve the crystals.  After
          standing for 40 min. at 20°.C, the absorbance is measured
          again.
          1.  "Selected Methods for the Measurement of Air Pollutants,"
          U.S. Department of Health, Education, and Welfare 999 AP-11,
          Robert A. Taft Sanitary Engineering Center, Cincinnati, Ohio,
          May 1965, p 1-1.
          2.  Water, Atmospheric Analysis,  (1971), "Annual Book of .
          ASTM Standards," American Society for Testing and Materials,
          Philadelphia, Pa., Part 23, pp 50-53.

12602 91  .HYDROGEN. ION CONCENTRATION - HI-VOL   pH METER
          The. water soluble extract of the filter is tested by a
          pH meter and the hydrogen ion is calculated from the pH
          value.

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17242 9.1  BF.IIZOCMPYRENE - HI-VOL   THIN LAYi:K CHRO.MATOGRAPIIY
          This io a technique whereby  the  benzene soluble organic:;
          are separated by means of  thin layer  chromatography.   The
          isolated benzo(A)pyrene  as indicated  by comparison with a •
          standard is removed from the thin layer plate and.excited
          with radiant energy of 470 run.   The fluorescence is .neasurod
          at 540 ran.
          1.   Intersociety Committee, "Methods of Air Sampling and
          Analysis," American Public Health Association, Wash., D.C.,
          1972, p 159.

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                                 16
21101 51  TOTAL DUSTFALL - BUCKET   GRAVIMETRIC
          A 1 gallon container having a mouth diameter of 4.4 in.
          is placed in a copper can (5 in.  high and 5 in. diameter) on
          stand,(4 ft. above a roof  and four stories from the ground).
          Five hundred to 1500' ml of antifreeze-treated water is placec
          in the container.  The collected sample is filtered using
          Whatman No. 4HI paper which is then dried and weighed.
          The filtrate is evaporated at 105°C, the residue weighed,
          and both weights added for total dustfall.
          1.  M. B. Jacobs, "The Chemical Analysis of Air Pollutants,"
          Chemical Analysis, Vol 10, Interscience Publishers, Inc.,
          New York, N.Y.,  (1960),  p 37.   •

21101 71  TOTAL DUSTFALL - BUCKET. - GRAVIMETRIC  (APCA)
          The dust falls into a glass or stainless steel container,
          5 in. in diameter and 10-15 in. high.  The top of the con-
          tainer is maintained at from 8 to 50 ft. above the ground
          and 4 ft. above any surface.  Neighboring roof surfaces
          must subtend an angle of 30° or less from the horizontal.
          Distilled water should be maintained in the container and
          a quaternary ammonium salt is added  (1 to 2 mg/1) to suppress
          algal growth.  Isopropyl alcohol may be added as antifreeze.
          The 30 day sample is filtered through a 20 mesh screen to
          remove extraneous material and treated as method 21101 51
          except that samples having antifreeze are evaporated to
          dryness at 105°C, 300 ml distilled water is added, and the
          sample again evaporated to dryness.
          1.  "Recommended Standard Method for Containing Dustfall
          Survey  (APMI-a)," (Nov. 1955), APCA Journal 5,  (No. 3),
          P 176-                       .    •  •

21101 81  DUSTFALL - BUCKET   GRAVIMETRIC  (ASTM)
          A 6 in. diameter, 12-18 in. high, glass, plastic/ or
          stainless steel cylinder, mounted with a bird ring, is

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                                 17
          ucc to collect the dustfall.   The analysis is the same as
          method -21101 71.    .
          1.   Water,  Atmospheric Analysis, (1971),  "Annual Book of  -
          AGTM Standards,"  American Society for Testing and Materials,
          Philadelphia, Pa., Part 23, p 425.
          2.   Nader,  J. S., (1958), "Dust Retention Efficiencies
          of Dustfall Collector," APCA Journal' 8,  p 35.

21102 81  ORGANIC FRACTION - BUCKET   GRAVIMETRIC (ASTM)
          The water insoluble residue and the filter from method
          21101 81 are dried, weighed,  placed in a soxhlet apparatus,
          and extracted for 2 h using 50.ml of benzene.  Benzene
          should remain in the flask at all times.   The remaining
          residue and paper are dried at 105*C and weighed to
          report the weight loss as organic fraction, BSO  (benzene
          soluble organics).          "                     •
          1.   Water,  Atmospheric Analysis, (1971),  "Annual Book of
          ASTM Standards," American Society for Testing and Materials,
          Philadelphia, Pa., Part 23, p 427.

21113 71  INORGANIC FRACTION - BUCKET   GRAVIMETRIC  (APCA)'

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                                 JLtf
21113 81  IMORCANIC FRACTION - BUCKET   GRAVIMETRIC (ASTM)
          The combined wo.ight of water insolublcs and soluble
          matter corrected for any solid present in a distilled water
          blank.
          1.  Water, Atmospheric Analysis, (1971), "Annual Book of
          ASTM Standards,." American Society for Testing and Material/
          Philadelphia, Pa., Part 23, p 428.

21114 71  WATER SOLUBLE WEIGHT - BUCKET   GRAVIMETRIC (APCA)
          The sample is filtered through a 20 mesh screen to remove
          extraneous material and if antifreeze was used, the filtrate
          is evaporated to dryness over a steam bath or in an oven
          at 105°C.  Thirty ml of distilled H20 is added, heated to
          boil, and the sample filtered through an alundum crucible.
          If no antifreeze was used, the sample is adjusted to 300
          ml and filtered through the crucible.  The filtrate is
          evaporated to a small volume.  The filtrate is placed in
          a weighed platinum crucible  (if fluoride is present)' or
          else a borosilicate dish and evaporated to 25 ml.  It is
          evaporated slowly to dryness on a steam bath or in an oven
          at 105°C.  Dryings are repeated for 3 h periods until
          constant weight is obtained.
          1.  "Recommended Standard Method for Continuing Dustfall
          Survey,  (APMI-a)," (Nov. 1955), APCA Journal 5  (No. 3), 17.7.

21114 81  WATER SOLUBLE WEIGHT - BUCKET   GRAVIMETRIC (ASTM)
          The soluble material, described as the v/ater soluble weight
          in method 21101 81,is evaporated in a tared platinum dish if
          fluoride or caustic materials are' present or else a boro-
          silicate dish.  The dish is heated slowly until 25 ml
          remain.  Then a steam bath or a thermoregulated hot plate
          is used to evaporate to dryness at a temperature of 99°C.
          Drying is continued in an oven at 105°C until a constant

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                                 19
          weight is obtained.  The water soluble we if; lit: is the
          difference bctv;een this constant weight am! uare.
          1.  Water, Atmospheric Analysis, (1971), "Annual Book
          of ASTJl Standards," American Society for Testing and
          Materials,. Philadelphia, Pa., Part 23, p 427.

21115 51  WATER INSOLUBLE WEIGHT - BUCKET   JACOBS METHOD
          The collected sample is filtered through a 20 mesh sieve,
          and the coarse material discarded.  The insoluble material
          in the sample is collected on a 9 cm Whatman No. 41 H
          filter.  Alternatively, a tared gooch crucible equipped with
          a light asbestos mat or an alundum crucible could be used.
          The weight of the dry solid is reported as water in-
          soluble weight.
          1.  M. B. Jacobs,  (1960), "The Chemical Analysis of Air
          Pollutants," Chemical Analysis, Vol 10, Interscience Publishc
          Inc., Mew York, N.Y., p 38.

21115 71  WATER INSOLUBLE WEIGHT - BUCKET   GRAVIMETRIC  (APCA)
          The water soluble weight was obtained to report the total
          dustfall, method 21101 71.  The sample is filtered
          through a 20 mesh screen, the volume made to 300 ml, boiled,
          and filtered through a weighed 35 ml alundum filter crucible.
          The crucible is dried in an oven at 105°C for 3 h, cooled,
          and the drying is repeated to constant weight.  The increased
          weight of the crucible is reported as water insoluble weight.
          1.  "Recommended Standard Method for Continuing Dustfall
          Survey  (APMI-a) ,  (Nov. 1955), APCA Journal 5  (No. 3), 176.
21115 81  WATER INSOLUBLE WEIGHT - BUCKET   GRAVIMETRIC  (ASTM)
          The. material collected on a dried and weighed  filter  from
          method 21101 81, is dried in a weighing bottle overnight
          at  105°C.  The net weight less the weight of the  filter
          paper and weighing bottle is the water insoluble  weight.

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                                20

          1.   ,;ntar, Atnosphcric Analysis,  (1971) , "Annual Book
          oi  .\STJ-1 Standards," American Society for Testing and J-Jatcria
          Philadelphia, Pa., Part 213, p 427.

2111C 71  TOTAL WEIGHT ASH - BUCKET   GRAVIMETRIC  CAPCA.)      '   .
          The water insolubles and the water solubles are ignited
          in a dish at red heat for 20 to 30 min, cooled in a
          desiccator, reheated and cooled until a constant weight
          is obtained.  The dish must have been pretreated in the
          same manner.  The excess weight is the total weight ash.
          1.   M. B. Jacobs,  (1960), "The Chemical Analysis of Air
          Pollutants," Chemical Analysis, Vol 10, Interscience
          Publishers Inc., New York, N.Y., p 47.
21116 81  TOTAL WEIGHT ASH - BUCKET   GRAVIMETRIC  (ASTM)
          The total weight ash is the weight of the insoluble and
          soluble materials after the removal of BSO and the com-
          bustible materials.

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223 .1 ;  32, 2212C 92, 22132 92, and 22136 92
          COPPER, IKON, MANGANESE, NICKEL - BUCKHT   ATOMIC ABSORPTION
          Thirty ml of IIN03/II20 (1/1) is added to the due tf all
          in a beaker, heated below boiling for 1 h, and concentrated
          to remove excess UNOy.  The solids are removed by
          centrifuging.  The solution is 'analyzed by AA. •'
          1.  Water, Atmospheric Analysis,  (1971) ,  "Annual Book of
          ASTM Standards/ " American Society for Testing  and Materials,
          Philadelphia, Pa., Part 23, p 678.

22403  81  SULFATES - BUCKET   TURBIDIMETRIC  (ASTM)
          Turbid samples are filtered and the temperature adjusted
          to between 15 and 30°C.  Ten ml glycerin  solution  (glycerin/
          II20, 1/1), and 5 ml of NaCl solution  (240g of NaCl and  20 ml
          cone. HCl/liter) are added to 50 ml of the sample.  A 40 mm
          cell filled with" the treated sample is used as the blank
          sample by setting the colorimeter to  zero absorbance at 380-
          400 nm.  The cell sample is combined with the remaining
          treated sample, 0.3g of BaCl2.2H20 crystals added, and  the
          mixture stirred 'for 1 min.  After standing for 4 rain the
          mixture is stirred again for 15 sec*  The cell is then
          filled with the turbid solution and absorbance measured
          again at the same wavelength as the blank sample.
          1.  Water, Atmospheric Analysis,  (1971) ,  "Annual Book of .  . •
          ASTM Standards/1 American Society  for  Testing  and Materials,
          Philadelphia, Pa., Part 23, p 51.
22G02 -81  pH  (DUSTFALL)i .- 'BUCKET   pH METER V
          Total acidity of the water soluble portion of  the total dust-
          fall is obtained by using a pH .meter,  or  less  accurately
          by use of pH  test paper.  .   *.""             .
          1>-  M. B. Jacobs^ (1960), "The Chemical Analysis  of •Air
          Pollutants,^! .Chemical/Analysis, Vol 10, Interscience .Publishe:
          Inc., New York, N.Y., p 40.

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                                 22

25101 81  DUfJTFALL CO:-:',USTIDLE-BUCKET   GRAVIMETRIC - 500-DEG.
          C. LOSS (ASTM1
          After the DSO has been remove, from the water insoluble
          material/  the material and the filter paper are ashed at"
          500°C in a tared crucible and the weight loss is reported as,
          "Combustibles and volatile particulates other than benzene
          soluble."
          1.  Water, Atmospheric Analysis, {1971}, "Annual Book of
          ASTM Standards," American Society for Testing and Materials,
          Philadelphia, Pa., Part 23, p 428.

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42101 12
42101 21
  INFRA-RED                   /
1  The non-diisperive infrared instrument has a sample
  cell, a reference, cell, and a detector;   The detector
  is divided by a flexing diaphragm into two equal
  cells filled with equal concentrations of CO.  The
  reference cell is. filled with a CO free air.
  When infrared radiation is passed into the sample
  cell some of the radiation is absorbed by CO
  in this cell in proportion to the concentration
  of CO and the rest  is  transmitted to the detector.
  In the detector,  the radiation causes the CO to
  expand flexing the  diaphragm in proportion to the
  transmitted infrared radiation.   Since the reference
  cell is filled with zero CO air,, the reference cell
  side of the detector exerts a  constant pressure on  the
  diaphragm,-  When the CO is introduced into the sample
  cell,  unequal amounts  of residual radiation reaches
  the two compartment of the detector  causing an unequal
  expansion of the detector gas.   This unequal expansion
  causes the diaphragm to deflect, creating a change  of
 ...electrical capacitance in an external circuit, and
  ultimately  an amplified signal which is suitable for
  input to a servo-type  recorder.   The detector is calibrated
  by placing CO standards in the sample cell and recording
  the electrical signals.
  1.   "Rules and Regulations," Federal Register, Vol  36,
  No.  228,  (Nov.  25,  1971),  p 22391.
 CARBON MONIXIDE - INSTRUMENTAL - COULOMETRIC
 Atmospheric air is drawn through a heated ^Oc column
 where Ij is liberated.   The ^ is directed
 into an electrochemical cell where I2, is measured
 coulometrically.             *
 1.  Beckman Instrumention', Bulletin  3000 4411-4,
 Beckman Instruments, Inc., Fullerton, California.
 CARBON MONOXIDE - INSTRUMENTAL -'FLAME IONIZATION   /
 Ambient air is. passed through two gas chromatograph-ic
 columns in series, the  first retains  most pollutants
 but passes CO nnd Cllq,  and the second passes only
 CO.   The CO then Clows  through a Ni catalyst where

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          it is converted to CH4 which is measured by a flame
          ionization dctoccoi.   The re.-jult.inn measured current
          is related to the CO concentration of the input
          ambient air by dynamic calibration with Known CO
          concentration standards.
          1.   Rotterdam, Warsaw, and Bucharest/ "The Status
          of Instrumentation in Air Pollution Control," Environ-
          mental Control Sorninar Proceeding, U.S.  Department
          of Commerce,  (May 5-June  4,  1971), p 217.
42102 11  CARBON DIOXIDE-INSTRUMENTAL   IMFRAR5D ABSORPTION
          This procedure is similar to the NDIR procedure for carbon
          monoxide, 42101 11, except that water does not have to
          be removed from the air stream.

42401 11  SULFUR DIOXIDE-INSTRUMENTAL-WEST CAEKE-COLORIKETIC
          A continuous analyzing system is setup such that
          the ambient sir flows through a glass beaded absorp-
          tion column concurrently with 0.02M  sodium tetrachloro-
          mercurate.  Dichlorosulfitomercurate  ion is formed
          reacted with acid-bleached pararosaniline and
          formaldehyde to produce  a red-purple  pararosaniline
          methylsulfonic acid which is quantitatively measured
          colorimetrically.  The zero  (100%T)   baseline  is
          established with  pure reagents  for  1  h and the  in-
          strument  is then  dynamically calibrated with known
          S02  concentration standards.   Air flow rate  and
          reagent  flow  rate must be calibrated and maintained
          accurately.

 42401  13  SULFUR DIOXIDE-INSTRUMENTAL-CONDUCTIMETRIC
          Sulfur dioxide is absorbed  in  acidic ^02  whi^-h
          oxdizes  the  S02  to H'2S04.   The resulting  change
          in conductivity  can  be measured,  compensated for
         . temperature,  and related to the input S02  concentration
          by dynamic calibration with known S02 concentration
          standards.   However,  specificity is poor  because any
          materials that alter the conductivity of  the reagent
          are potential interfering agents.
          1.   Bcckman  Air  Quality  Acralyzer Operating  and
          Service  Manual,  Scientific  and Process  Inst.  Div. ,        ,/,(

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          Fullcrton, California, 1GTW352,  (Aug. 1966).
          2.  Thomas, M.D.,  (1932)/ "Automatic Apparatus for
          the Determination of Small Concentrations of Sulfur
          Dioxide in Air," Anal. Chem. 5,  253.
          3.  M. B. Jacobs,  "The Chemical  Analysis of Air .
          Pollutants/1 Chemical Analysis,  Vol 10, Interscience
          Publishers, Inc., New York, N.Y..,  (I960), p 394.
          4.  Water, Atmospheric Analysis,  (1971), "Annual Book
          of ASTM Standards," American Society for Testing and
          Materials, Philadelphia, Pa., Part 23, p 272.

42401 14  SULFUR DIOXIDE-INSTRUMENTAL-COULOMETRIC
          The air to be measured is passed through a cell
          containing a neutral buffered iodide or bromide
          electrolyte where an electrical current or potential
          maintains a constant concentration of free 12 or Br2.
          When S02 in the input air reacts with the I2 o'r Br2,
          the change in electrical current or potential necessary
          to restore or maintain the original concentration of
          12 or Br2 (coulometric titration) is £ quantitative
          measure of the S02 input.  If the input flow i?ate is
          constant, the S02 concentration  can be related to
          the electrical signal by' dynamic calibration with
    \ •
          known SO, concentration standards/
42401 15  SULFUR DIOXIDE-INSTRUMENTAL-THOMAS AUTOMETER
          The Thomas Autometer is a conductimetric analyzer
          developed in 1929.  There are later models.  The
          method is similar to method 42401 13.
42401 16  . SULFUR  DIOXIDE-INSTRUMENTAL-GC FLAME PHOTOMETRIC
          Chrorr.atographic  columns  are used to  separate S02,
          H2S,  CS2,  and  CH3ca.  Effluent  from  the columns is
          burned  in  a hydrogen-rich flame. A photcmultiplier
          tube  is used to  detect  the  395  nm emission  band
          characteristic of sulfur 1   The  electrical  signal is
          related to the input concentration by dynamic  cali-
          bration with known SO2,  H2S, CS2,  or CJUSH  concen-
          tration standards..
          1.  H.  H.  Willard,  L. L. Merr'itt,  and J. A. Dean,
          "Instrumental  Methods of Analysis,"  D. Van  Mostrand
          Company, 'Inc., 4th Edition, 1965,  p  309.

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 /12.101 Jl  f.Ul.riJR DIOXIDH-DAVIS INSTRUMENT-HYDROGEN  PEROXIDE
           T'r.c novin instrunont is a conductimetric  instrument,
           and Co uuch, it  vs ir.uch like method  42<101 13.
 42-101 33  SULFUR DIOXIDE-DAVIS INSTRUiMENT-SEQUENTIAL-CONDUCTIK'-JT.V.:;
           Water is deionized by passage through an  amberlite
           resin column, then its conductivity  is measured.
           Ambient air, having first passed through  n scrubber
           of amberlite ro.sin and soda-lime to  remove C02/ is
           next passed through the deionized water- where the S02
         .  is absorbed..  The increased conductivity  of the water •
           is a measure of the S02 concentration of  the air.
                 i
         '  1.  Thomas,  M.D.  and J. N.  Abersold,  (1929), "Automatic
           Apparatus for the Determination of Small Concentrations
           of Sulfur Dioxide in Air,"  Anal.  Chem.  1,  14.

42401 91. SULFUR DIOXIDE-GAS"BUBBLSR-WEST-GAEKE-SULFAMIC ACID
           Sulfur dioxide  is  collected  in  a ''tetrachlorcmercurate
           solution,  forming'a  stable dichlorosulfitomercurate
           complex.   When  acid  bleached pararosaniline is  added
           to the collected  S02  together with formaldehyde,
           the amino groups  (-NHt)  form a  red violet  compound
           called pararosaniline methylsulfonic  acid  which is
           measured  spectrophotometrically.   The method is des-
           cribed in the Federal Register.   (The NAS'N procedure,
           however,  uses 1.725  g/1 sulfamic  acid rather than
           6  g/1  and does  not use  EDTA).   The sulfamic acid
           eliminates interference from oxides of  nitrogen.
           1.   "Rules and  Regulations," Federal  Register,  Vol  36,
           No.  228,  U.S. Government Printing Office,  Washington, D.C
           (Nov.  25,  1971),  p 22385.
           2.   tvcst,  P.  W.  and  G.  C. Gaeke,  (1956),  "Fixation
           of Sulfur Dioxide as Disulfito-Morcurate  (II)  and
           Subsequent Colorimetric Estimation,"  Anal. Chem.  23,
           1819.
           3.   Intcrsociety Coinmittee,  "Methods  of Air Sampling
           and Analysis,"  American Public  Health Association,
           Washington,  D.C.,  1972, p  447.
           4.   "Air  Quality  Data for 1967,"  EPA-APTD  0741,  Office of

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           Technical  Information and Publication, Research .Triangle
           Park,  N.C.,  1971,  p 20.

42401  92   SULFUR DIOXIDE-GAS BUBBLER-WEST-GAEKE
           This method,  is  similar to method 42401 91 except
           that the sample absorbing reagent is O.lM TCM,
           the starch which is used  for standardization is
           made without mercuric iodide,  and sulfamic acid
           is not used  except when high concentrationsof NO-
           are expected.   The sulfamic acid is added to the
           sample after collection.
           1.  "Selected Methods for the  Measurement of Air Pollutants'
           U.S. Department of Health,  Education,  and Welfare  999  AP-
           11, Robert A. Taft Sanitary Engineering Center, Cincinnati,
           Ohio,  May  1965, p  A-l.
           2.  Nauman,  R.  V., et al.,  (1960) ,  Anal Chem. 32,  1307..
           3.  West,  P.W.  and F. Ordoveza,  (1962), "final. Chem.  34,
           1324.
42401  93   SULFUR DIOXIDE-GAS BUBBLER-CONDUCTIMETRIC
           This manual  conductimetric  method uses the same
           principle  as the instrumental  conductimetric
           method.  The absorber is  a  multiple jet bubbler
           system and the  sampling is  not continuous.   The
           details are  described in  the reference.
           1.  Intersociety Committee, "Methods of Air  Sampling
           and Analysis,"  American Public Health Association,
           Washington,  D.C.,  1972, p .456.
42402 71  HYDROGEN SULFIDE-TAPE SAMPLER  AISI LEAD ACETATE PAPER
          Filter paper (Whatman, No. 1} is cut into 2 by 4 in.  strips,
          impregnated with Pb(C2H.,O2)  (10g/10C ml H20 plus 5  ml
          CH3COOH) and dried in H2S  free air.   Air is pumped  over the
          strips.  A concentration of 0.025 mg/1 of H2S gives a
          positive test for H2S.  The stain on the paper is com-
          pared  with a color chart  for II-S concentration.
          1.^ M.  B. Jacobs, (19GO),  "The  Analytical Chemistry of  Indus
          trial Poisons, Hazards, and Solvents,"  Chemical  Analysis,
          Vol 1,  Intorsciencc Publishers, Inc.,  Now York,  N.Y.,
          P 103.

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 24 02 9.1  HYDROGEN SULFIDE-GAS BUBBLER   METHYLENE BLUE
          (100 Mj  tube -t- orifice)
          Air is bubbled through a Cd(OH)2 solution in a large inn-
          pincjor at 1 cfm for 30 min.  Ferric chloride solution and
          p-aminodimethylaniline test solution are added to the im-
          pinger and agitated.  The sample is diluted and allowed to
          stand for 30 min.  The sulfide ion forms a methylene blue
          complex.  The absorbance of the sample is compared with a
          standard which consists of 45 ml of the Cd(OH)2 solution,
          amine test solution, and.the ferric chloride.
          1.   Inter society Committee, "Methods of Air Sampling
          and Analysis," American Public Health Association,
          Washington, D.C., 1972, p 426.
          2.   M.  D. Jacobs, (1960), "The Chemical Analysis of Air
          Pollutants," Chemical Analysis, Vol 10, Interscience
          Publishers, Inc, New York, N.Y. , p 185.
          3.   Lodge, J. P., et al.,  (1966), "The Use of Hypodermic
          Needles as Critical Orifice," J. Air Poll. Control Assoc.
          16_, 197.
          4.   Scaringelli, F. P., S. A. Frey, B. E. Saltzman,  (1967),
          "Evalxiation of Teflon Permeation Tubes for use with
          Sulfur Dioxide," Am. Ind. Hyg. g^jfoc.' J. 28, 260.
42410 71  SULFATION RATE-LEAD PLATE   GRAVIMETRIC (HUEY)
          The PbO2 is converted to PbSO4 by the S02 in the ambient
          air and the SOT is removed by Na2CO., and .boiling H20.
          Barium chloride is used to precipitate the SOT as BaS04 .
          The dried BaS04 is weighed and the SO- equivalence is
          reported.

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                                  29
42'ilO 72  SuLFATION jRATE-L'K/vD PL.Y.E   COLORIMETRIC  (HUEY)
42410 73  SULFATION RATE-LEAD PLATE   TURBIDIMETRIC  (HUEY)
          Sulfur dioxide reacts with lead peroxide to  form  lead
          sulfate.  The amount of SOj formation per  unit  time  is
          the sulfation rate.  The SOJ  is removed from the  plate
          by boiling Na-CO., solution and the  pll is adjusted between'
          2.5 and 4.0 so that sulfaspend or sulfaver precipitates
          the SO^.  The absorbance of the stirred precipitate  is
          read at 450 nm, turbidimetrically.
          1.  Intersociety Committee/ "Methods of Air  Sampling and
          Analysis," American Public Health Association,  Wash., D.C./
          1972, p 442.
          2.  Huey, N. A., M. A. Wallar, and  C. D. Robson,
           (June 1969) "Field Evaluation of an Improved Sulfation
          Measurement System."  Paper No. 69-133, Air  Pollution
          Control Association Annual Meeting.
          3.  Hickey, H. R., and E. R.  Hendrickson,  (1965), "A
          Design Basis for Lead Dioxide Cylinder," J.  Air Poll.
          Control Assoc. 15, 409.

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42'".10 ?:*  r.uLFATiou RATE-LEAD pL.v.r:   COLORIMETRIC  (HUEY)
42410 73  SULFATION RATE-LEAD PLATE   TURBIDIMETRIC  (HUEY)
          Sulfur dioxide reacts with lead peroxide to form lead
          sulfate.  The amount of SO^ formation per unit time  is
          the sulfation rate.  The SCc is removed from  the plate
          by boiling Na-CO., solution and the pH is adjusted between
          2.5 and 4.0 so that sulfaspend or sulfaver precipitates
          the SO^.  The absorbance of the stirred precipitate  is
          read at 450 nm, turbidimetrically.
          1.  Intersociety Committee, "Methods of Air Sampling and
          Analysis," American Public Health Association, Wash., D.C.,
          1972, p 442.
          2.  Huey, N. A., M. A. Wallar, and C. D. Robson,
          (June 1969) "Field Evaluation of an Improved  Sulfation
          Measurement System."  Paper No. 69-133, Air Pollution
          Control Association Annual Meeting.
          3.  Hickey, H. R. , and E. R. llendrickson,  (1965),  "A
          Design Basis for Lead Dioxide Cylinder," J. Air Poll.
          Control Assoc. 15, 409.

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                                 31
          1.   WilccJdn, D. II. and F. J. J-lcConncl,  (1934) ,  "-The
          Measurement of Atmospheric Sulfur Pollution by  Means
          of Lead Peroxide, J.' Soc. .Chem.... Ind. 53, 385.
          2.   Kainzcr, A.,  (1957) , Zemcnt-Kalh-Gyis 10, 281.
          3..  "Standard Methods for the Examination of  t:7ater and
          Waste-water," 12th Ed., American Pvblic Health  Assoc.,
          Inc., New York, N. Y., 1965, p  147-151.

42410 94  SULFATION RATE-LEAD CANDLE   POTASSIUM CARBONATE  (NASN)'
          This metlK
          42410 91.
          This method substitutes I^CO^ for Na2C03 in method
42410 95  SULFATION RATE-LEAD CANDLE   TURBIDIMETRIC
          Gaseous and particulate fluoride in ambient  air  are
          collected by filtration and chenisorption on filter
          paper impregnated with sodium -formate.  Water  soluble
          fluorides are extracted from the filter, made  basic
          with Na^CO^, and coinplexed with citrate ion  to reduce
          the iron and aluminum interference.  The fluoride  ion
          concentration is measured with a specific ion  electrode.
          1.  Thompson, R. J., T. B. McMullen'and G. B.  Morgan,
          (1971), "Fluoride Concentrations in the Ambient  Air,"
          J. Air Poll. Control AGSOC. 21, 484.

42513 91  FLUORIDE HI-VQL   SPECIFIC ION ELECTRODE
          The concentration of fluoride in an aqueous  sample is
          measured by means of the fluoride-specific ion electrode.
          1.  Elfcrs, L. A. and Decker, C. E.,  (1968), Anal. Chem.,
          Vol. 40, p 1G58.
          2.  Frant, M. S. and J. w. Ross, Jr.,  (1966) ,  "Kloctro-Ja for
          Sensing-'Fluoride Ion Activity in Solution," Science 154,
          1553.

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                                 •32
42C01 11  NITRIC OXIDE-IHSTRU-i.^T.-.L   COLORI.METRIC
          NO is; convGrtccl to 1J02 by passing the ambient  air  through
          an aqueous i'v'Mn04 solution.  The  resulting  riO^  is measured
          colorimctrically.  An independent •measurement  of tlie  ar.bicr.
          N02 concentration is required,.   This value,  subtracter!
          from the first, gives a value  for the MO concentration.  Sc
          Methods 42602 11 and 42602  12  for MO2 measurer.en*:  nrocc^u.ra
          1.  Water, Atmospheric Analysis,  (1971), "Annual Book
          of ASTM Standards," American Society for Testing and
          Materials," Philadelphia, Pa., Part 23, p  523.
          2.  Rogers, L. M., (1958),  "Nitric Oxide and Nitrogen
          Dioxide in the Los Angeles  Atmosphere," J. of  Air  Poll.
          Control Assoc. 8, 124.
          3.  Saltzman, B. E. , (1954), "Colorimetric Micro-Detsrmina-.:i
          of Nitrogen Oxide in the Atmosphere, Anal. Chem., 26,  1949.
          4.  Thomas, M. D., et.al.,  (1956), Automatic Apparatus
          for Determination of Nitric Oxide and Nitrogen' Dioxide
          in the Atmosphere, Anal. Chem. 28, 1810.
42601 14  NITRIC OXIDE-INSTRUMENTAL
          When O, reacts with NO to form NO-,
                            CHEMILUMINESCEHCE
                                     some of  the  liberated
energy appears in the form of light  of  600-875 nm.   The
reaction is extremely rapid.  The instrument generates
an excess of 0^ such that the quantity  of  light  emitted
from the reaction and measured by the .instrument,  is a
direct measure of the NO concentration  in  the sampled
air.  See also 42602 14.
1.  Fontijn, A., A. J. Sabadell and  J.  R.  Ronco, (1970),
Anal. Chem. 42, 575.
2.  Stevens, R. K., et.al., "Field Performance Characterise.:
of Advanced Monitors for Oxides of Nitrogen, Czonc,  Sulfur
Dioxide, Carbon I-Ionoxide, Methane, and  Nonmethane  Hydro-
carbons," Environmental Protection Agency, Research  Triangle
Park, N.C., presented at the APCA Meeting, June  1972.
                                                                    <7

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                                 33
4/!Goi
          :;i'i'.iuc o;:iD!>GAS
42602 11
                                     SALTZIIAH (100 in TUDJ: + ORIFICJ ;
                                                 lnO  and the
          Nitrogen o;:ide is oxidized to tI02 by ISln
          Method 4 2 CO?. 72 is followed.
          1.   Intersocicty Committee, "Methods of Air Sampling
          and Analysis," American Public Health Association,
          Wash. , D.C., 1972, p 329.

          NITROGEN DIOXIDE-INSTRUMENTAL   COLORIMETRIC
          The Lyshkow modification of the Griess-Saltzman reagent
          is used in various continuous NO2 analyzers.  Users
          should consult the manufacturer's literature for  details
          of reagent preparation.
          1.  "Rules and Regulations" Federal Register, Vol 38,
          No. 110, USGPO Wash., D.C.,  (June 8, 1973), p 15176.
          2.  Lyshkov/, ft. A.,  (1965), "A Rapid Sensitive Colorirr.etric
          Reagent for Nitrogen Dioxide in Air" J. Air Poll. Control
          Assoc. 15  (No. 10). 481.
42602 12  NITROGEN DIOXIDE- INSTRUMENTAL-COLORIMETRXC
          The original Griess-Saltzman reagent  is used  in
          various continuous N02 analyzers.  Users  should
          consult the manufacturer's literature for details
          of reagent preparation.
          1.  "Rules and Regulation," Federal Register, Vol 38,
          No. 110, USGPO, Wash., D.C., (June 8, 1973) p 15176.
          2.  Saltzman, B. E.,  (1954) "Colorimetric Micro
          Determination of Nitrogen Dioxide in the Atmosphere"
          Anal.  Chem. 26, 1949.

42602 13  NITROGEN DIOXIDE-INSTRUMENTAL-COULOMETRIG
          Air' to be measured is passed through a cell containing
          neutral buffered iodide-iodine solution causing an
          established equilibrium between iodine and iodide

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           to be  unbalanced.   The  current required to re-
           establish  the  equilibrium (coulometric titratiqn)
           is a measure of  the input NO?  concentration.   If
           the input  flow rate is  constant,  the NO2 concentration
           can be related to  the electrical  signal by dynamic
           calibration with known  N02 concentration standards.

42602 14  NITROGEN DIOXIDE-INSTRUMENTAL-CHEMILUMINESCENCE
          The ambient air  to  be measured is  drawn over  a heated
          catalytic  converter which reduces  N02  to NO.   The
          NO is  then analyzed by method  42601  14,  and the
          original N02 concentration is  obtained by subtracting
          the concurrent NO concentration.
          1.  "Rules and Regulation,"  Federal  Register,  Vol  38,
          No. 110, USGPO,  Wash., D.C.,  (June 8,  1973) p  15176.
          2.  NO/NOX/M02 Analyzer Bulletin,  Bulletin 4133,
          Beckman Instruments, Inc.,  Fullerton,  Calif.
42602 71  NITROGEN DIOXIDE-GAS BUBBLER-JACOBS-HOCKHElSER-
          50 Ml TUBE + ORIFICE
          Ambient air to be measured  is  bubbled  through  a
          sodium hydroxide solution where N02  forms  a stable
          solution of sodium  nitrite.  The nitrite ion pro-
          duced  is reacted with phosphoric acid,  sulfanilaraide,
          and N-l naphthylethylenediamine dihydrochloride,
          and measured colorimetrically'  at 540 nm

42602 72  NITROGEN DIOXIDE-GAS BUBBLER-SALTAIAN  (50  Ml TUBE +
          ORIFICE)
          The sample'1 is  absorbed in  the  Griess-Saltzman .reagent
          and after  15 min the stable  pink color is  measured
          colorimetrically at 550 nm>                   •

          1.  Intcrsociety Committee,  "Methods of  Air Sar.ipl.ing
          and Analysis," American Public Health  Association,
          Washington, D.C., 1972', p  329.
          2.  f.alli'iruin,  U. E. ,  (195-1), "Co.! or i me trie Micro-
          Determination  oi llitroqon -in the ALmosphorc,"  ArKO._.
          Chcm.  26,  1949.                                        n

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•12602 BA  NITROGEN'DIOXIDE-GAS 13UBBLER-NASN SODIUM ARSENITE-
          ORiriCE
          The method is much like method -12602 71 except for
          the absorber'1. Ocj/1 of NaAs02).   Ambient ;air is in-
          troduced into ':.he absorber by means of an orifice
          in the bubbler.  The orifice is usually not cali-
          brated.
          1.  "Rules and Regulation," Federal Register, Vol 38,
          No. 110, USGPO, Wash., D.C., (June 8, 1973), p 15175.
          2.  Christie, A..A., R. G. Lidzey, and D. W. F. Radford
          (1970) , "Field Methods for the Determination of Nitrogen
          Dioxide in Air."  Analyst 95, 519.
          3.  Merryman, E. L., et.al., "Effects of NO, C02,
          CH4,  H20 and Sodium Arsenite.on N02 Analysis,"
          presented at the ..Second Conference on Natural Gas
          Research and Technology.  Atlanta, Georgia, June 5, 1972.

42602 91  NITROGEN DIOXIDE-GAS BUBBLER-JACOBS-HOCHHEISER (100
          Ml TUBE + FRIT)
          This method  is identical to method 42602 71, except
          that a fritted bubbler .is used instead of an orifice
          bubbler and  the volume of the absorbing solution is
          doubled.
          1.  "Selected Methods for the Measurement of Air
          Pollutants," U.S. Department of Health, Education,
          and Welfare  999-AP-ll, Robert A. Taft Sanitary
          Engineering  Center, Cincinnati, Ohio, May 1965, p C-4.
          2.  Purdue,  L. J. , et.al..,  (1972),  "Reinvestigation
          of the Jacobs-Hochhoiser Procedure  for Determining
          Nitrogen Dioxide  in Ambient Air," Environ.  Sci.
          and Tech. 6, 152.

42602 94  NITROGEN DIOXIDE-GAS  BU3BLER-NASN-SODIUM ARSENITE-
          FRIT
          This method  is  identical  to method  42602 '71 except.
          that  l.Og/1  of  NaAs02  is  added  to the absorbing
          solution, and  a  fritted bubbler is  used  instead of
          an orifice  bubbler.

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          1.   Christie,  A.  A., R. G. Lidzcy, and D. V7. F. Raclforcl,
          (1970),  "Field. Methods for the Determination of Nitror/cn
          Dioxide  in Air."  Analyst 95, 519.
          2.   Merryman,  E.  L., et.al., "Effects of MO, C02,
          CH4, H20 and Sodium.Arsenite on N02 Analysis/"
          presented at the Second Conference on Natural Gas
          Research and Technology.  Atlanta, Georgia, June 5, 1972.
          3.   "Selected Method for the Measurement of Air
          Pollutants," U.S. Department of Health, Education,
          and Welfare 999-AP-ll, Robert A. Taft Sanitary
          Engineering Center, Cincinnati, Ohio, May 1965,
          p C-4.
42G03 11  OXIDES OF NITROGEN-INSTRUMENTAL   COLORIMETRIC
          The total oxides of nitrogen   (NO + N02) are measured
          by the methods- 42601 11 and 42G02 12.  The instrument
          reports the total as NOX  (total oxides of nitrogen).
          1.   Intersociety Committee, "Methods of Air Sampling
          and Analysis," American Pxiblic Health Association,
          Wash., D.C., 1972, p 325.

42604 91  AMMONIA-GAS BUBBLER-   N33SSLER R5AGCNT-50 Ml TUBS +  ORIFIC':
          Ammonia reacts with the alkaline HgI2.2KI solution
          (Nessler reagent) to produce an crange colored complex
          that is measured colorimetrically at 400 to 425 run.  The
          absorbing solution  (3.27N H2S04) is returned to the
          laboratory after the siir.pling period and Nessler reagent
          added' .   Rochelle salt  is  added  to pravent Ca and Mg pre-
          cipitation.
          1.   M. B. Jacobs,  (1960), "The Chemical Analysis of Air
          Pollutants," Chemical Analysis, Vol 10, Interscience
          Publishers, Inc., New York, N. Y., p 216.
          2.   Morgan, G. B., E. C. Tabor, C. Golden, and H. Clements
          Automated Laboratory Procedure for the Analysis of  Air
          Pollutants GG-p  108B, Technicon Industrial System,
          Tarrytown, N." Y. , p 538,

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                                 37
          3.   Water,  Atmospherjc Analysis,  (1971), "Annual
          nook of  ASTM Standards,"  American Society for Testing
          ami  Materials,  Philadelphia,  Pa., Part 23,  p 236-331.
42GO4 92  AMMOIJIA-GAS BUBBLER-SODIUM PIIEIJOLATE
          The chemical principle used is the same as method
          12301 92.  Ammonia is collected in 0.0504' N H-SO, as
          (NH.JpSO. producing a blue complex with sodium
          ph.enolate and sodium hypochlorite.
          1.  Russell, J.  A., (1944), "The Colorimetric Estimation
          of Small Amounts of Ammonia by the Phenal-Hyppchlorite
          Reaction," J. Biol. Chem., 156, 457.

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                                30
43.101 11  TOTAL ItYDnOC^P^ON'S-^ISTRU^&iTAL   FLAMS:
          Ambient air is passed into the. instrument where tho
          organic compounds present are burnecT in a hydrogen-rich
          flame.  A sensitive, electrometer coupled with a
          recorder measures the current resulting from the
          ions produced in the flame.  The response is
          approximately proportional to the number of carbon
          atoms in the sample.  The analyzer is calibrated using
          methane and the results are reported as methane
          equivalents.
          1.  Intersociety Committee, "Methods of Air Sampling
          and Analysis," American Public Health Association,
          Wash., D.C., 1972, p 184.
          2. "Rules and Regulations," Federal Register,
          Vol 36, No. 228, U.S. Government Printing Office,
          Wash., D.C., (Nov. 25, 1971), p 22394.
43102 11  NONMETHANE HYDROCARBONS-INSTRUMENTAL   FLAME IONIZATIOM
          Measured volumes of air are delivered semicontinuously
          (4-12 times per hour) to a hydrogen flame ionization
          detector to measure its total hydrocarbon  (THC) content.
          An aliquot of the same air sample is introduced into
          a stripper column which removes H20, C02 and hydro-
          carbons other than CH..  CH. and CO are passed
          to a gas chromatographic column where  '
          they are separated.  The CH^ is eluted first, and
          is measured by the flame ionization detector.  This
          value subtracted from that for THC results in a
          measure of the non-methane hydrocarbon  (HMHC) concen-
          tration of the sampled air.  See also 42101 21.
          1.  "Rules and Regulations," Federal Register, Vol 36,
          No. 228,  (Nov. 25, 19711, p 22394.

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                                 39
••I3>:oi ii.  i-yr.'i'iLMir.-i-.'.'-n'KUMEiiTAL-   FLA:in. 10:3.1NATION ..
          A ntripper chroma t.otjro.nhic column  (charcoal)  is used to
          remove H20, C02• and hydrocarbons, other than CH,.
          Ilothane and CO arc then  separated  by a gas chromato-
          graphic column and the CH. measured by a hydrogen
          flame ionization detector.
          1.  Water, /vtmospheric Analysis,  (1971) , "Annual .Book
          of ASTM Standards," American Society for Testing
          and Materials, Philadelphia,  Pa.,  Part 23, p 783.
          2.  "Rules and Regulations," Federal Register, Vol 36,
          No. 228, U.S. Government Printing  Office, Wash., D.C.,  ' •
          (Nov. 25, 1971) , p 22394.
          3.  Ortman, G. C.,  (1966) / Anal.  Chem. 36;, 644.

43501 11  ALDEHYDE-INSTRUMENTAL    COLORIMETRIC
          This method is an automated  1-IBTH  technique.  See 43501 91.

43501 91  ALDEHYDE-GAS BUBBLER   MBTH
          VJater soluble aliphatic  aldehydes (measured as fcrmalydchya
          HCIIO) in the ambient air are measured, using an aqueous
          3- methyl - 2- benzothiazolone hydrazone hydrochloride
          (MBTH) v;hich forms an  azihe.  The excess MBTH is
          oxidized with ferric chloride and reacts with the azine
          to form a blue cationic  dye  in acidic media, measurable
          at 628 nm, colorimetrically.
          .1.  "Selected Methods  for the Measurement of Air Pollutants
          U.S. Department  of Health,  Education, and Welfare, 999-AP-l]
          Robert A. Taft  Sanitary  Engineering Center, Cincinnati,  Oh:.
          May 1965, p F-l.
          2.  Sawicki, E. , et.al., (1961),  Anal. Cljiem. 33, p 93.
          3. . Hauser, T.  R. and  R. L.  Cunrr.ins,  (1964) ibid..- 36,  679.
          4.  "Air Quality Data  for 1967,"  EPA-APTD-0741, Office
          of Technical Information and Publication,, Research Triang.'.-
          Park, N.C., 1971, p  20.

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                                40

44101 11  TOTAL OXIDANT-i::STRUM2XTAL-ALKALT.NE KI
          Identical to method 44101 14 except 1 N sodium-
          hydroxide is used instead of the phosphate buffer
          in the absorbing solution.
44101 13  TOTAL OXIDANTSr-INSTRUMEMTAL-MAST MODEL 742-2   .
          Identical to method 44101-15.
          1.  Mast, G. M. and H. E. Saunders, (Oct. 1962), "Research
          and Development of the Instrumentation of Oxone Sensing,"
          Instrument Soc. of Amer. Trans., 1, 375.
          2.  Bufalini, J. J.,  (1963), "Gas Phase Titration of
          Atmospheric Oxone," Environ Sci Technol 2, 703.
          3.  Wartburg, A. F., and B. E. Saltzman,  (1965),
          "Absorption Tube for Removal of Interfering S02 in
          Analysis of Atmospheric Oxidant" Anal. Chem. 37, 779.
44101 14  TOTAL OXIDANT-INSTRUMENTAL-COLORIMETRIC-NEUTRAL KI
          Air to be measured is contacted with neutral
          phosphate buffered potassiun iodide.  Oxidants
          convert the  KI  to  12  or  KI3  which is measured
          spectrophotometrically at 352 run.   If the input
          air flowrate is constant, the color density can
          be related to the oxidant concentration.  Analyzers
          are calibrated dynamically with known standard
          concentrations of ozone.  Sulfur dioxide inter-
          ference may be minimized by use of  a CrO^ pre-
          scrubber, which also causes an NO interference.
          1.  Intersociety Committee, "Methods of Air
          Sampling and Analysis,"  American Public Health
          Association) Wash., D.C., 1972, p 356.
          2. .Water, Atmospheric Analysis, (1971), "Annual
          Book of ASTM Standards," American Society for Testing
          and Materials, Philadelphia, Pa.,  Part 23, p 518.
          3.  Wartburg, A. F., and B. E.  Saltzman,  (1965),
          "Absorption Tube for Removal of Interfering S02
          in Analysis of Atmospheric Oxidant" Anal. Chen.  37,
          779.

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                                 40

44101 11  TOTAL OZIDAMT-IilSTRUMEriTAL-ALKALINE  KI
          Identical  to method  44101  14  except  1 M sodium
          hydroxide  is used  instead  of  the  phosphate  buffer
          in  the  absorbing solution.
44101 13  TOTAL OXIDANTS-INSTRU:-1SKTAI>MAST MODEL 742-2
          Identical  to method 44101-15.
          1.  Mast,  G. M. and H. E.  Saunders,  (Oct. 1962), "Research
          and Development of the Instrumentation of Oxone Sensing,"
                                                                    •
          Instrument. Soc. of Araer. Trans.,  1,  375.
          2.  Bufalini, J. J.>  (1968),  "Gas Phase Titration of
          Atmospheric Oxone," Environ Sci Technol 2,  703.
          3.  Wartburg, A. P.,  and B. E. Saltzman,  (1965),
          "Absorption Tube for  Removal  of Interfering S02 in
          Analysis of Atmospheric  Oxidant" Anal. Ch;em. 37, 779.
44101 14  TOTAL OXIDANT-SNSTRUMENTAL-COLORIMETRIC-NEUTRAL KI
          Air to be measured is contacted with ne-utral
          phosphate buffered potassiun  iodide.  Oxi.dants
          convert the KI  to  12  or Kl3 which is  measured
          spectrophotometrically at 352 nm.  If the input
          air flowrate is constant, the color density can
          be related to the oxidant.concentration.  Analyzers
          are calibrated dynamically with known standard
          concentrations of ozone.  Sulfur dioxide inter-
          ference may be minimized by use of a CrO-^i pre-
          scrubber, which also causes an NO interference.
          1.  Intersociety Committee, "Methods of Sir
          Sampling and Analysis," American Public Health
          Association, Wash., D.C., 1972, p 356.
          2.  Water, Atmospheric Analysis,  (1971), "Annual
          Book of ASTM Standards," American Society for Testing
          and Materials,  Philadelphia, Pa., Part 23, p 518.
          3.  Wartburg,  A. F.,  and B. E. Saltzraan, (1965),
          "Absorption Tube for Removal of Interfering S02
          in Analysis of  Atmospheric Oxidant" Anal,, Chen. 37,
          779.

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                                •41
44.101 15  TOTAL OXIDArrr-INSTKUMEXTAL-COULOMETUIC-NEUTK/vL KI
          Air to be measured is passed  through a  cell containing
          potassium iodide and two electrodes.  Oxidants
          convert iodide ions to I2 which is reduced at the
          cathode of the cell.'causing a current to flow thru
          an external circuit.   If the  flow rate  is constant,
          this electrical signal can be related to the input
          concentration of oxidants.  Analyzers are calibrated
          dynamically with known standard concentrations of
          ozone.
                                                      • A
44101 51  TOTAL OXIDANT-GAS BUBBL.ER-PHENOLPHTHALIN
          Phenolphthalin, in the presence of CuS04 is
          oxidized to phenolphthalein by ambient  air oxidants.
          Air is passed through 10 ml of reagent  at 800
          ml/min for 10 min.  The color is read using a
          colorimeter and a green filter.
          1.  M. B. Jacobs,  (1960), "The Chemical Analysis
          of Air Pollutants," Chemical  Analysis,  Vol 10,
          Interscience Publishers, Inc., New York, N. Y.,
          p 225.

44101 81  TOTAL OXIDANT-GAS BUBBLER-ALKALINE KI
          Oxidants in sampled aiobient air are absorbed in
          an alkaline KI solution in a  buboler.   A stable
          product is formed which can be stored with little
          loss for several dcys.  Analysis is completed
          by addition of phosphoric acid-sulfuric acid
          reagent, liberating iodine, which is then determined
          spectrophotometrically at 352 nm.
          1.  Selected Methods for the  Measurement of Air
          Pollutants U.S. DHEW 999-AP-ll, RATSEC  Cincinnati,
          Ohio, 1965, p E-l.
          2.  Water, Atmospheric Analysis,  (1971), "Annual
          Book of ASTi-1 Standards," American Society for Testing
          and Materials, Philadelphia,  Pa., Part  23, p 391.
          3.  M. B. Jacobs,  (1960) , "The Chemical Analysis of
          Air Pollutants," Chemical Analysis, Vol 10, Inter-
          scioncc Publishers, Inc., New York, N.  Y., p 219.

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44101 C2  TOTAL OXIDANT-GAS BUBBLER-FERROUS OXIDATION
          Air to be measured is filtered through a
          No. 4 paper at 1 cfia then bubbled through two
          impingers in series containing acidified ferrous
          ammonium sulfate absorbing solution.  Alter sampling
          ammoniuru thiocyanate is added, and the resultant
          color is measured with a colorimeter and green filter.
          1.  M. B. Jacobs/  (1960) / "The Chemical Analysis'of
          Air Pollutants," Chemical Analysis, Vol 1,0, Inter-
          science Publishers, Inc., New York, N. Y., p 228.

44101 83  TOTAL OXIDANT-GAS BUBBLER   NEUTRAL BUFFERED KI
          This is the reference method for standardization and
          calibration of total oxidant and ozone measuring
          techniques.  Maximum sampling time is 30 minutes.
          Sulfur dioxide interferes.

          1.  Intersociety Committee, "Methods of Air Sampling
          and Analysis/1 American Public Health Association/
          Wash., D.C., 1972, p 351,
          2.  "Rules and Regulations" Federal Register, Vol 36,
          No, 228, U.S. Government Printing Office, VJash., D.C.,
           (Nov. 25, 1971), p 22392.
          3.  "Selected Methods for the Measurement of Air Pollutant.
          U.S. DIIEW, 999-AP-ll, R. A. Taft Sanitary Engineering
          Center, Cincinnati, Ohio, May 1965, p D-l.

44103 11  INSTRUMENTAL - TOTAL OXIDANT - 0.2(NO

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                                43

44201 11  OZONE - i;JSTRfj:-:"r-:TAL-CIIEMILUMINESCI3MCE
          Ambient air to be ii.easurcd and ethylene  are
          delivered siraU3.tr.n-.:ously to a mixing cell where
          ozone reacts with the ethylene to emit light which
          is measured by a nhotomultiplier tube.   If  the  air
          and ethylane flov/ratcs arc constant, .the resulting
          photomultiplier signal can be related to the input
          ozone concentration.  Analyzers are calibrated with
          known ozone concentration standards.
          1.  "Rules and Regulations," Federal Register Vol 36,
          No. 228, U.S. Government Printing Office, Washington,
          D.C.,  (Nov. 25, 1971), p 22392.
          2.  "A ChGiailuminescence Detector for Ozone Measure-
          ment," Bureau of Mines Report of Investigation  RI-7650,
          United States Department of the Interior, U.S.  Government
          Printing Office, Washington, D.C., 1972.

44201 13  OZONE - INSTRUMENTAL - COULOMETRIC
          This method is identical to method 44101 15.
          1.  Mast, G. M. and H. E. Saunders, (Oct. 1962),
          "Research and Development of the Instrumentation of
          Ozone Sensing," Instrument Soc. of Amer. Trans.,
          1., 375.
          :.  Bufalini, J. J.,  (1968), "Gas Phase  Titration of
          Atmospheric Ozone," Environ. Sci. Tech.  2,  703.
          3.  Wartburg, A. F., and 3. E. Saltzman, (1965),
          "Absorption Tube for Removal of Interfering S02 in
          Analysis of Atmospheric Oxidant" Anal. Chem. 37, 779.

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