0-1
                                      February  10,  1973
                                      Revision  0
  Sampling Methods and Analytical
Procedures Manual for PCB Disposal
           Interim Report
          February 10, 1978
                  PREPARED 3Y:   J. Howard Beard,  III
                                 John Schaum
                                 Office of Solid Waste
                                 U.S. Environmental
                                    Protection  Agency
                                 Washington, D.C.   20460

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                           PREFACE
     This manual is a compendium of sampling methods and



analytical procedures which may be referred to and used by



the ?CB disposal facility owner/operators to assist them



with any sampling and analytical testing which may be required



under 40 CFR Part 761, Polychlorinated Biphenyls.  However,



due to the short time period in which this manual was



prepared, the U.S. Environmental Protection Agency is issuing



this manual as an interim document.   (The U.S. EPA believes



ehat a sampling methods and analytical procedures manual



has to be available to PCS disposal facility owner/operators



at the time the regulation is finally promulgated to success-



fully implement the site approval process under 40 CFR



Part 761, Polychlorinated Biphenyls.)  A final version of



this manual is expected to be issued, after undergoing



further review within the U.S. EPA, by early spring of 1978.

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                      Table of Contents








i.0       Introduction




  1.1     Purpose




  1.2     Scope




2.0       Determination of PCB Spill Contamination Levels




3.0       Procedures for Monitoring Feed Rate




   3.1    Liquid PCB Wastes




   3.2    Solid PC3 Wastes




4.0       Procedures for Monitoring Incineration Operations




          and Combustion Products




   4.1    Temperature




   4.1.1  Temperature Monitoring Locations




   4.1.2  Temperature Monitoring Equipment Selection




   4.2    Dwell Time




   4.3    Scrubber Water Monitoring




   4.4    Continuous Stack Monitoring; CO, C02,  02




5.0       Procedures for Conducting and Monitoring A Test B




   5.1    Performance




   5.2    Combustion Products




   5.2.1  CO, C02,  02




   5.2.2  HC1




   5.2.3  RCL (Total Chlorinated Organic Content) and




          PCB (PCB Chemical Substances)




   5.2.4  MOX




   5.2.5  Total  Particulate Matter

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                         Atachments
Attachment: A
Attachment 3
Attachment C
Attachment D
Attachment E
Attachment F
Attachment G
Tentative Method of Testing for Polychlorinatec




Biphenyls in Spilled Material



Tentative Method of Testing for Polychlorinated



Biphenyls in Water



Determination of CO Emissions from Stationary



Sources



Gas Analysis for C0_, 02/  Excess Air, and



Dry Molecular Weight



Determination of Total Polychlorinated



Biphenyl (PCB)  Emissions from Industrial,



Sewage Sludge,  and Municipal Refuse Incinerators



(Draft Method)



Determination of Nitrogen Oxide Emissions



from Stationary Sources



Determination of Particulate Emissions



from Stationary Sources

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1.0  INTRODUCTION




     i.1  Purpose




     The purpose of this manual is to provide guidance to




the PC3 disposal facility owner/operators with any sampling




methods and analytical procedures which may be required




by the Regional Administrator for the parameters specified




in 40 CFR Part 761, Polychlorinated Biphenyls.  The manual




provides a procedure for determining the contamination levels




associated with a PCS spill as required under 761.10 (e)




and provides information on incinerator sampling methods




and analytical procedures as required in the  "Note" under




761.40.




     1.2  Scope



     Section 2 of this manual describes the sampling and




analytical procedures for determining the contamination




levels associated with a PC3 spill.




     Section 3 describes the procedures for measuring the




flow rare of liquid and non-liquid PC3s fed to the combustion




system.  This task is required to be conducted in 40 CFR




761.40(a)(3) of the regulations.




     The next section (Section 4) describes the procedures




for monitoring incineration operations and combustion




products.  The continuous monitoring of combustion temo-




erature during PCS incineration is required as specified




in 40 CFR, 761.40 (a) ( 4) .  Additionally, the continuous




monitoring of CO and C09,  and 02 are required during the




incineration of PC3s as prescribed under 40 CFR 761.40(a) (1"

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 Dwell  time  calculations and procedures for sampling ana.




 monitoring  the  scrubber water effluent are also included




 within Section  4.



     Finally, the procedures for conducting and monitoring




 a  trial  or  test  burn are  included in Section 5.  When an




 incinerator  is  first used  for the disposal of ?CBs, or when



 nodificatons are made that may affect the character of stack




 emission products, several parameters must be monitored,



 as  specified under 40 CFR  761.40 (a) (6) .  Additionally, trial




 burns  may be required of the PCE disposal facility owner/




 operator by  the  Regional Administrator as discussed under




 40  CFR 761.40(d)(2).




 2.0  DETERMINATION OF PCS  SPILL CONTAMINATION LEVEL




     The following procedure describes where and how to




 sample in the event of a PC3 spill  in order to determine




 the extent of contamination.




     A three dimensional plot of the suspected zone of con-




 tamination should first be developed which defines the




perimeter and depth of the suspected area.




     The plot should be defined by  establishing transects




along the suspected perimeter with  sufficient surface samples




taken to define the perimeter.  Transects for subsurface




samples should  also be established  that intersect through




the approximate center of the suspected area with subsurface



samples taken at the perimeter intersection of the transects,



the intersection of  the transects at the approximate center

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of the suspected area, and at the approximate center of each




segment formed by the perimeter and the -ranseczs.   Figure




1 illustrates the designation of sample locations by use




of transects.




     Surface samples should be 500 gram samples taken at




a depth of no greater than 2 millimeters.   For suspected




areas greater than 10 square meters, a surface sample point




should consist of four surface samples taken at the corners




of a one meter square grid with the four samples homogenized




to make one composite sample.




     Subsurface samples should be removed from the core at




the elevation of interest, i.e., 0.3 meters deep, 0.5 meters




deep, etc.  The sample volume should be 100 grain samples




taken at a depth of 0-3 meters or greater.  The samples should




then be prepared and analyzed for PCS content using the




air-dried, 10 percent moisture added soxhlet extraction pro-




cedure  (see Attachment A).  If the analytical results at a




0.3 meter depth are below 500 parts per million PCBs, then




it is presumed that the zone of contamination extends to




0.3 meters for purposes of practical excavation or removal.




If the analytical results exceed 500 parts per million PCBs,




then additional samples must be taken at successive 0.3 meter




levels until the analytical results indicate a concentration




below the 500 parts per million PC3 level.   Successive




samples can be avoided by taking a sample at a depth assumed




to be below the zone of contamination.  If the concentrati- on




of PCBs is below 500 parts per million, then that samcle

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               Figure 1:  Designation of  Sarnie Locations
                          Bv Use of Transects
KEY
                                              BBI1
Perirneter of Suspected Area- ABCD
Subsurface Sanples
  Perimeter Intersection of the Transects- AA, BE, CC, DD
  Intersection of the Transects at the Approximate Center of the
   Suspected Area- II
  Aproximate Center of Tilach Segment ^cmed by the Perioeter and
   the Transects- ABI'ABI', BCT'BCI', CDI'CDI', ADI 'ADI1

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point can be used to define the outer limit of the zone of




contamination.  When excavation activities are believed




to be completed, samples should be taken at the excavated




depth to determine if the excavation process has caused




contamination at depths below the originally defined




contaminated zone.




3.0  PROCEDURES FOR MONITORING FEED RATE




     3.1  Liquid PCB Wastes




     The flow rate of liquids is normally determined by measuring




the pressure drop across an orifice of known size.  The pressure




drop is converted to flow rate via fundamental engineering




calculations.  However, other devices are more commonly used to




measure the liquid flow such as ones based on mechanically




driven propellors or more advanced instruments based on




magnetic measurements. Such devices are used widely and




available commercially.  Information on their installation,




operation,  etc., is supplied and should be obtained from the




various vendors.   No special consideration for PCB wastes




are necessary compared to other liquids; consequently,




detailed procedures are not specified in this manual.




     However, it is recommended that instruments be selected




which provide a continual real-time measurement of the flow-




rate in such a manner that the data can be visually disolaved

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 a .-id automatically  recorded.   It  should  also be pointec



 that the instruments  discussed above, whicn measure trie  _j-




 rate directly,  indicate  the  bulk  flow rate of the entire



 liquid.   If  the flow  rate  of PC3s  is needed, it  is necessary




 to determine the concentration of  PC3s  in the liquid waste



 feed.   Sample preparation  and analytical procedures for  this




 purpose  are  identical  to those specified for scrubber



 water  in Section 4.3  of  this manual.  The bulk flow rate



 is simply multiplied  by  the  percent of  ?C3s  (by  weight)  in




 the feed to  calculate  the  feed rate of  ?C3s.



      3 . 2  Solid PCS Wastes



     The flow rate of  solids is  normally determined by weighing




 loads  and monitoring  the time frequency at which these




 wastes are fed  into the  incinerator.  Conveyor belts or



 other  feed mechanisms  can be equipped with scales  for this




 purpose.   As  with liquid flow measurements, detailed procedures




 are not  needed  for such  site specific techniques.




     Load weights should be  determined  by weighing several




 representative  loads and averaging them.  Typically, in




 batch operations, the  number of  loads in a specific time,




 such as  one hour, are  merely counted by the operator.




Sophisticated time frequency measurements are usually not




practical during normal  incineration operations.  Flow




rates should  be  calculated and recorded at least several

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     As with liquid wastes, if the feed rate of ?C3s is




needed, it is necessary to determine the concentration of




PC3s in the feed material and multiply the % ?C3s by




the bulk feed rate.




4.0  PROCEDURES FOR MONITORING INCINERATION OPERATIONS AND




     COMBUSTION PRODUCTS




     4.1  Temperature




     Temperature should be routinely monitored and recorded




at several locations within the combustion zone of the




chemical waste incinerator, since it is an excellent indicator




of the performance of the combustion process.  The choice of




temperature monitoring equipment and its placement or location




within the combustion zone will vary depending on the particular




design of the incinerator.  Typically, flame temperature,




afterburner temperature, hot duct temperature, and wall




temperatures are monitored.




     Combustion temperature is usually thought of as a value




or range of values which typify the temperature at which




chemical wastes introduced into the combustion chamber are




subjected.  Wastes introduced into the combustion zone are




first heated rapidly to the appropriate flame temperature




and then normally cool over time and distance from the flame.




Temperatures within the combustion zones therefore can varv




over a wide range.

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      In order to insure that ?C3 v:astes are subjected to




 adecua-e -emperature and dwell time conditions,  tne rollowinu




 specific minimum criteria have been specified in the reg-




 ulation (40 CFR Part 761)  as combustion criteria:



      (1)   Maintenance of the introduced ?C3 wastes for a




           2-second dwell time at 1200°C (J:100OC)  and 3




           percent excess oxvgen in  the  stack gas,  or



      (2)   Maintenance of the introduced ?CB wastes for a




           lis-second dwell  time at 1600°C (+ 100°C) and 2




           percent excess oxygen in  the  stack gas.



      4.1.1     Temperature Monitoring Locations




      Compliance with the above criteria can be insured by



 maintaining a temperature  above the required minimum temp-




 erature in the  coldest  portions of  the  combustion chamber.




 Accordingly,  at least one  temperature monitor should be




 located in this area, which  typically is the furthest point




 from  the flame,  such  as  the  point prior to  the combustion




 zone  exit.   Specific  locational requirements and the number and




 type  of temperature monitors  should be  based upon consideration




 of particular designs.   However,  at least two monitors will




 normally be  required, other  than  flame  temperature monitors,




 in order to  insure representative monitoring of  the combustion



chamber.

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     4.1.2     Temperature Monitoring Equipment Selection




     Temperature monitoring wi-hin the conibusiton zone




should be performed with thermocouples which are selected




for the appropriate characteristics, in accordance with ~he




composition, size and construction factors.  To assist in the




seiec-ion of a proper thermocouple, summary tables and




curves are provided in Tables 1 through 4 and Figures 2 and 3




(see Perry's Chemical Engineers Handbook, 4th Edition, for




a more detailed discussion).




     Radiation pyrometers should be used to monitor flame




temperature if the flame is hotter than the practical operating




range of thermocouples.  Combustion temperature should




also be monitored by thermocouples shielded from the flame




in order to detect gas temperatures free of hot surface




radiation effects.  As specified in the regulation  (40




CFR Part 761), the thermocouples should be accurate to




within 100 C of the true temperature.




     The thermocouple equipment choice must take into account




maintenance requirements and operating limitations and




should provide a continuous visual display of combustion




temoerature which automaticallv records the data.

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                 Carmen Types  of  Thermocouples  and Temperature
                 Ranees in Which  Thev  Are  Used
I.S.A. ; p^riv, ;X,.,-.T.| c,.
'
"
ilt'-
=.;. .-i
T-
•C. | 'f.
c : 00 - p,.,G - =h , f.-^.,.. ._ ! o i,,
P- 87--. Pi-l3<- Kb ' ?'.i::-.-:^: 0 to
A
J, V
T


Ch.-0=!i-P .iU-S.
Iron
Coppir
Ch.-oasl.?
—200 to
'.'on- j— 2CO to
Coo-
df'"
s'.aa-.ac
-200 to
-100 to

Uif

nnr
750
350
1000

T •>
^1
->on
— 300
-:oo
-150

t'ra;'
"C. ' 'F.
K 2650 IJOO 3 'JO

to:OOOH200'i200
to M 0
to 650
100011800
|
600JIIOO
to ISOO|IOCoil800
1
                 (Perrv's  Cnernica.1  Engineers'  Handbook,
                  4th  Edition,  p.  22-6)
Table  2:    Corrosion  Characteristics  of  Cannon
               ThernncouDles
                 Type of
                Mnjrn TJ.
              Chr
                  ei-P \
Iron TO, CocstaoUn..
              t.nroTTJ?I-P vs. OiajUatan..
                           InSuencc o: Teaper»turt m
                                Gu AfmM^l.e •«
                         P—tsu^c*1 to o'.iiniog  itsn
                                        r'.A-.inum  corrcxlss   tuilv
                                        lOOC'C. .^aould DI» uj*(i IQ
                                        R^-i-in'^ ro ocdiiai
                                        ff-xxl ;o rerj- p-jod
                                        RrfsistAnr* to r-ducing liziorphers:
                                        poor
                                        AJIertad by sulfur, r-ducin;  or rji-
                                        furoua EOS, 50:. ud 5TiS
                                        Oxjcino; tad rtcurnt s;moe7ic?res
                                        bar? ii;:.e e^fct on  acruracy. £t-Jt
                                        U3sd io dry iC3C"pri-rs»
                                        ?. — i'raD'f to cxjd»;t&o: rood u" to
                                        400'C. out pco: ahore 700*C,
                                        R^3L?tiDCT to r»duco; »E3io3phcr«:
                                        rxwi (up to iOO"C. 1
                                        Protect froa OTVHO. c.oiature, sulfur
                                        Subjec; t« oxiJatiou and  il:?rvtioQ
                                        iboT*-  400aC. due to copp*r, ^hove
                                        600"C. du* to Coojt»Qtan mre. Coo-
                                        tiaiioati.^a of fopp^r tncaa  aJibr*-
                                        lioo sreitly
                                        R.teist3nc* ;o oiidizing
                        . Re*ist»u«  to redurlag »ttn«?h«rt:
                         sood
                         Re^uifrt protfcticu from »cid fumes
                        . Chrosul kltacicei by suL'uroas itir.a*.
                         pher?
                         Resistance tn oiidation: good
                         Rttiftaac-  *o reduciaj a:mo3ph«re:
                         food
                          s  ^e^cal c-ngineers '  Handbook
                 4th  Edition,  p.22-7)

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Table  3:   Methods  of Joining Thermocouple
            1*7-1 T-QC?
            wires
Planer vs, ;ac::u^ii-.-;i>

Cfiocej.p vs. Alurnci	
         •-.m-il-!1 -.j. Cotj'j.3Ur.
                            Ele-.nc-a.-c
                            hlcciric-drc TC!
                            ;i'irrr •n[c-r
                  I silver pold,-r
                   ::••'• sol'j::
                  I "nn»
                                   ' Rcrct
                                   ! PJMID
          (Perry's  Chemical Engineers' Handbook,
           4th Edition,  p.22-7)
Table 4:   Reccnmended Maxinrun  Operating  Temperature o:
            Thermocouple Protecting Tubes
— . , . He :j."jr"e '.-.-'. ruj. tin?.
Met*. Tunes
S* am leu at«l 	
Ca/bon «tpel 	
Cist iron 	
U'roueht iroo 	
1 6 Cr-8 Ni itAialeu stMt. .
28Criro3 	
Chromel T 	
Nichrome 	
20 Cr-32N'i-48 Te aocoloy).-
Inconel 	 - 	
Ctrsmic TL
Fire clay 	
SiUimanitc 	
MulUt« 	
Silic* 	
Silicon txfbici^ ... •
550
550
700
700
?iO
MM
1100
MOO
MOO
MCO
1260
()«
1050
1550
1550 !
1530 |
1600 !
1650 i
I JOO
1000
1000
1300
1300
IHW
2000
2000
2000
2000
2000
2300
1900
2300
2200
2600
2900
3COO
           (Perry's Chenical  Engineers'  Handbook,
            4th Edition,  p.22-7)

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  re  2:   Temperature-thermal E.M. F  Curves for
          Cocnxn Tvoes  of Thermocouples
            70


            60
            40

          1

          - 30

          LU
            10
            -10
                93 pic1 >ni_^",- C r ~; -''JTI v s 0:31. ~jm
               2 £T p'ann^.Ti-!3'"odium vs. piad"-m
               3 C.ircmel vs alurel
               4 CsDier vs. cons':.itan
               5 Iron vs. c"s:c~.'cn
               D.C.^rcmef vs co.^.srcntan
                            i    i   I    i
                        Reference junction ct 0° C.
                        I    I    I   I    I
             -200  0  2CO 4C3 SDO SCO !COO 1200 MOO I€CO
                         Temperalure , °C.


         (Perry's  Chemical Engineers'  Handbook,
          4th Edition, p.22-7)
Lgure  3:   Response of Bare Thermocouples'  of
           Different Size
            100
           s so
           £ 60
             40
                   '\   in siili cir ot 250" F
              0     24     6    8    iO
                       Ti me  mm
         (Perry's Chemical Engineers'  Handbook,
          4th Edition,  p.22-7)

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     4.2  Dwell Time

     Dwell time or residence time is the amount: of rime

in which a waste is subjected within the combustion zone

to the combustion temperatures.  This time should be estimated

on rhe basis of flow rate calculations.

     The least complex calculations for the average dwell time

of combustion gases is equal to the volume of the combustion

chamber divided by the volumetric flow rate of the gas corrected

for temperature and pressure as shown below:

     DWELL   _      Volume of combustion chamber
     TIME           Volumetricflow rate ofgas thru chamber

where,

Volumetric flow = Mass flow rate of fuel +        Atmospheric
rate of gas       mass flow rate of air      x    Pressure
                  Density of Air @ T         "    Combustion
                                                  Chamber Pres-
                                                  sure

and,

     T         =  Temperature of gases in combustion chamber

(Note:  Mass flow rate of fuel includes any combustible
        gases derived from the waste.)

Example Calculation

If an ^ncinerator includes a primary combustion chamber of
100 FTJ and an after burn chamber of 2000 FT3, fuel rate =
10,000£/hour,  air rate = 90,OOOS/hour> primary chamber
temperature - 3000°F, afterburner temperature = 2500°F,
chamber pressure = 5 psig = 20 psia

     Vol Furnace = 100 FT3 + 2000 FT3 = 2lOO FT3 at T = 2500°F

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          Volumetric flow rats = 10,000^ - 90,900= X 15 psia
                              3600 ?ZC X .0134=/FT- X 20 psia
  Dwell Time =   2100 = 1.35 5EC
               T55I

      C-ote: The density of air at various temperatures may be calculated
     using the following formula.)

 Dens if-- =  Ambient Temperature (°K)
           13.1 X Combustion Temperature C"X)

 or iz rray be obtained from precared tables.  Such tables  can be found
 in the "torrh American Combustion Handbook, North ^nierican Manufacturinq,  Inc

      The  above  calculation is a good  technique for estimating

 residence time;  however,  the true residence  time cannot

 be easily calculated  on  a   theoretical  basis since the  effects

 of turbulence  are  difficult to model.  The most  accurate

 technique for determining dwell time  is  via  actual test

 measurements.   Such tests can be made by physically introducing

 a  tracer gas such  as  radioactive argon into  the  incinerator

 and timing the  tracer gas as it passes through the combustion

 chamber.  The state-of-the-art and expensive equipment asso-

 ciated  with such tests may make this  technique impractical

 at  most facilities.

      4.3  Scrubber Water  Monitoring

      Scrubber effluent samples should be taken prior  to,

during,  and  after PCS  incineration.

     Samples  of the quench/scrubber water can be taken from

several  points  depending  on the facility design.  Listed  in

decreasing order of preference for obtaining a composite  sample

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are:  (I) a holding tank for ponds containing all the scrubber




solution used during a burn,  (2) a recirculation cank for




scrubber solutions being recycled, and  (3) a pipe through which




these scrubber solutions are being pumped.  The advantage




of collecting a sample from holding tanks or ponds is that




iz. is a composite sample and, as such, can be obtained




without the requirement for collecting frequent grab samples




or using automated sampling equipment.



     Samples can be collected from valves on tanks or pipes




containing the scrubber solution.  If such valves are not




available, a dip tube or sampling bottle device can be dropped




into the tank or pond and allowed to fill.  If grab samples




are required to be taken, the facility owner/operator should




mix all  samples into a tank or drum.  A composite sample




should then be taken as described above.   (All sample loc-




ations should be noted for consistency when future samples




are taken.)  The scrubber effluent samples should then be




transferred to clean brown bottles equipped with polycetra-




fluoroethylene  (PTFE) lined bottle caps and stored in a cool




area.




     To prepare the sample for analysis, 1.5  liter alicuots




of the scrubber water samples should be extracted for organics




using the separatory funnel extraction process for oil and arease




from water.  This procedure is described in the EPA Handbook




on Methods for Chemical Analyses of Water and Wastes  (EPA

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 526/6-74-003  MERC,  Cincinnati,  Ohio   45263).  Pentane  or

 methylene  chloride  can  be  substituted  for Freon.   The  extrac-s

 should be  dried  by  passing the  sample  through a  200  x  10.5  mm

 glass column  containing a  50 mm bed of  sodium sulfate  which

 has  been ore-extracted  with pentane in  a soxhlet  for 24 hours.

 The  extracts  should then be concentrated to  a 10  milliliter

 sample using  a Kuderna  - Danish concentrating evaporator.

 Characterization of the scrubber  effluent samples should

 also be prepared.

      The prepared sample is now ready  to be  analyzed for

 PCS  content by gas  chromatography-mass  spectography.   (See

 Attachment B.)

      4.4  Continuous  Stack Monitoring

      The PCS  marking  and disposal regulation (40  CFR

 Part 761)  requires  continuous stack monitoring  for CO,  CO-,

 and  02 .  The  purpose  for these  analyses is in part,  to insure

 99%  combustion efficiency,  specified  as:

      Cco9        x   100
      Ceo + Cco2

 Where Ceo and Cco~  are  the  concentrations of carbon  monoxide

 and  carbon dioxide,  respectively.  Additionally,  0->  is

 analyzed to insure  compliance with excess air requirements.

     Carbon monoxide  should be  continuously  measured in the

 stack of incinerators while burning PC3s as  specified  in

CFR 60, Appendix A,  Method  10 (Determination of  carbon

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monoxide emissions from stationary sources).  This method




utilizes a nondispersive infrared  (NDIR) analyzer, and is




included in Attachment C of this manual.




     Carbon dioxide in the stack should also be continuously




monitored using a NDIR analyzer.  The instrument  should




be accurate to ^ 1 percent of full scale.   A Cco2 concentration




of 0.05 - 5% and 0.02 - 20% is needed.  Excess oxygen in




the stack should be continuously monitored  using  paramagnetic




or electrochemical instrumentation accurate to within +_ 1%




of full scale.  A C^ concentration range of 0.05  - 5%,




0.25 -  25% and 1 - 100% are needed.




5.   PROCEDURE FOR CONDUCTING AND MONITORING A TEST BURN



     5.1  Performance




     The test burn should be conducted  under conditions




simulating normal operations.  All effluent .streams should




be carefully monitored so that the environmental  performance




of the  incinerator can be evaluated.  The  test should last




approximately one day, consisting of the following 3 steps:



     1)   Start-up.  The incinerator is fired with fuel




          only to purge the system and  bring it up to steady-




          state at -normal operating conditions.




     2)   Waste burn.  The PCS waste is introduced into




          the incinerator at expected normal feed rates.

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           The  test  should only be as long as necessary  to




           collect sufficient samples for analysis.  A four




           hour  run  will probably suffice.



      3)    Shut-down.  Waste feed is terminated and  the



           incinerator is shut-down per normal procedures.




      Prior to  the -est burn, PCS waste samples should be



 obtained  and analyzed for their ?C3 concentrations, bulk




 waste feed rates should be determined, and feed rates of




 ?C3s  calculated.



      The  incinerator should be equipped with all necessary




 instruments and controls, as specified in 40 CFR Part 761.




 This  should include provisions for continuous monitoring




 of combustion temperature, feed rates, and CO, CCu  and  C>2



 in the stack.   (See Section 4.0 of this manual for  more details.)




 Additionally, stack sampling equipment for non-continuous




 monitoring  for specified pollutant concentrations should




 be installed and prepared as specified in section 5.2 of




 this  manual.  All instruments should be calibrated.




      Prior to start-up,  all ash should be removed from




 the incinerator and the scrubber system should be purged



 and filled with a fresh solution.




     As soon as steady-state conditions are reached during




the start-up phase of the test, conditions should be noted




and samples collected to characterize backcround conditions.

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     When the monitoring equipment is ready for collecting
the next set of samples, the PCS waste should be introduced
into the incinerator.  During the test, samples should
be collected and records kept of the readings of the con-
tinuous monitors.  Visual observation of the plume should
also be made.
     The following safety procedures should be established
and followed:
          Only authorized personnel should be permitted
          in the test area during operations.
          Waste handling must be performed only by personnel
          wearing suitable protective clothing and trained
          in handling such materials.
          Visual observation of the test system must be
          maintained at all times during operation.
          Canister gas masks and emergency oxygen resuscitation
          units must be available in the immediate test
          burn area.
5.2  COMBUSTION PRODUCTS
     Non-continuous  stack monitoring for CO, C0~, 0-,, KC1,
total particulate matter, NO , total chlorinated organic
                            A,
content  (RCL) and PCS chemical substances, should be conducted
as soecified below.

-------
               CO, CO?, O-i




     Stack concentrations of carbon monoxide, carbon




dioxide and oxygen should be determined as specified in




40 C?R 60, EPA Method number 3, which is provided in




Attachment D of this manual.




     5.2.2     HC1




     Stack concentration for hydrogen chloride should be




determined by collecting -he hydrogen chloride in an




impinger  filled with a caustic solution, such as dilute sodium




hydroxide or sodium bicarbonate.




     This solution should then be analyzed for chloride




ion concentrations using the mercuric nitrate method.  This




method is described in Methods of Air Sampling and Analysis,




2nd Edition, and in Standard Methods for the Examination of




Water and Wastewater.  Both are publications of the American




Public Health Association.




     5.2.3     RCL and PCBs




     Samples for analysis of total chlorinated organic content




(which includes PCBs) should be collected on a solid sorbent




trap,  such as XAD-2 Amberlite Resin.  Temperature control




must be maintained since the absorptive characteristics




of the trap change with temperature differences.  The solid




sorbent trap should be located in the sampling train downstream




from the  heated filter and uostream of the first irnsincer.

-------
     The sample is then removed from the solid sorbent trap




via a 24 hour soxhlet extraction with both pentanol and




rnechanol.  The extracts should be dried with sodium sulfate




and concentrated to 10 ml.   (A more detailed description




of this sampling method is provided in Attachment E.)




     Finally, the sample is analyzed for ?C3 and RCL content




by Gas Chromotography-Mass Spectography  (see Attachment 3).




     5.2.4     NOX




     Stack concentrations of nitrogen oxide(s) should be




determined as specified in 40 CFR 60, EPA Method number 7,




which is provided in Attachment F of this manual.




     5.2.5  Total Particulate Matter




     Mass emission rates of total particulars matter should




be determined as specified in 40 CFR 60, Method  5, which




is provided in Attachment G of this manual.

-------
                         REFERENCES
I.    Determination of PC3 Spill Contamination Levels,
     unpublished report.  Available from Hal Snyder,
     EPA/Office of Enforcement.

2.    EPA Handbook on Methods for Chemical Analyses of Water
     and Wastes, EPA publication No. 629/6-74-003, MERC,
     Cincinnati, Ohio, 1S74.

5.    Standard Methods of Air Sampling and Analysis, 2nd edition,
     A?HA, Washington, D.C., 1975.

4.    Standard Methods for the Examination of Water and Wastewater,
     APHA, Washington, D.C., 1977.

5.    Personal, communication.  Robert 3. Burns, President,
     Industrial Hydronics Corporation, Princeton, N.J., to
     J. Howard Beard, III, Office of Solid Waste, U.S. EPA,
     January 1978.

6.    Personal communication.  James Stevens and Joan Berkowitz,
     Arthur D. Little, Inc., Cambridge, Massachusetts, to
     J. Howard Beard, III, Office of Solid Waste, U.S. EPA,
     January, 1978.

7.    Personal communication.  Carol A. Zee, TRW,  Inc.,
     Redondo Beach, California, to J. Howard Beard, III,
     Office of Solid Waste, U.S. EPA, January, 1978.

8.    Analysis of Pesticide Residues in Human and  Environmental
     Samples, EPA unpublished manuscript prepared by Pesticides
     and  Toxic Substances Effects Laboratory, National
     Environmental Research Center, U.S. EPA, Research Triangle
     Park, N.C., 1974.

9.    Personal communication.  Christopher C. Shih, TRW,
     Redondo Beach, California, to J. Howard Beard, III,
     Office of Solid Waste, U.S. EPA, January 1978.

10.  Destroying Chemical Wastes in Commercial Scale Incinerators,
     EPA  Contract No.  68-01-2966, Facility Report =6, Office
     of Solid Waste, U.S. EPA, Washington, D.C.,  1977.

11.  Disposal of Organochloride Wastes by Incineration at  Sea
     (EPA - 430/9-75-014), Washington, D.C., July 1975.

-------
                Attachment
      Tentative Method of Testing for
Polychlorinated Biphenyls in Spilled Material

-------
  Ten-ative Method of Testing for Polychlorinated Biphenyls




                  (?C3s)  in Soilled Material
     Any excess liquid is decanted and the sample is spread



in a pyrex dish (8" wide x 12" long x 2" deep).  The sample




is air dried at room tempera-cure for about. 4 to 5 days in a



contaminate free area.  The dried sample is then ground wich



a procelain mortar and pestle to a uniform particle size.



     The sample is then divided by mixing and quartering



until  a sub-sample of about 100 grams is obtained  (for



surface samples only).  The sample is weighed  in a  100-ml



beaker.   (Add 10—20  % water, seal and thoroughly mix by



tumbling, and equilibrate  (minimum 2 hours) prior to extraction,



     The extraction is then carried out: in a soxhlet extractor



 (see Figure  ).  Glass wool  (about 1 inch deep) is  packed



in the bottom of the  extraction chamber  (40 x  150 mm).



The weighed sample is added and an additional wad of glass wool



is placed on the top.  The sample is then extracted using



200 ml of hexane-acetone  (9:1) for about 8 hours.   The



extraction may be carried out overnight or longer as mav be



necessary for heavily contaminated samples.



     The .extract  (approximately 200 ml) is then transferred



to a Kuderna-Danish  (K-D) evaporator and concentrated to



6 - 10 ml on a warm water bath at approximately 70  C.



(The remainder of the procedure is described in Method  3



(Method for Polychlorinated Biphenyls  (?C3s) in Industrial  '




Effluents) becinninc with Section 9.4.)

-------
"~~-f- !P^^^f?§^^iS^-': f f ~-~^~-~'^&^^r-e^i'\ •.   ^^S^^fd^'f-?^  If^'—SSr'^'t?:




'~^^^^^^^<^'-^^A^^^AS:lf-'-'-'-"~^^^'^r '~J^KJ?' -   ^°lpl "'"v-.^^-f^^-j  Z^'^^^VJ-^?
,1^1^-C;^-^^;--- -—_-,&-p^^-,.- ._, ^'-<>=i ' -     ™';i^_ ^,'-l'^^'?%,.J ~^--'^^^^i1 f i5^-^-_7 ^Ss-t^r^''^  ^^rZ'.^-rrj^'jSl-,"^!
                                            "•rucl-lon of Boilofn Samples
                                             26

-------
9.4  Qualitatively analyse the sample by gas chromatography with an




     electron capture detector.  From the response obtained decide:




     a.  If there are any organochlorine pesticides present,




     b.  If there are any PCB's present,




     c.  If there is a combination of a and b,




     d.  If elemental sulfur is present,




     e.  If the response is too complex to determine a, b, or c.




     f.  If no response, concentrate to 1.0 ml or less, as required,




         according to EPA Method (4), pg. 23 and repeat the analysis




         looking for a, b, c,  d, and e.  Samples containing Aroclors




         with a low percentage of chlorine, eg. 1221 and 1232, may




         require this concentration in order to achieve the detection




         limit of 1 yg/1.  Trace quantities of PCB's are often masked




         by background which usually occur in the samples.




9.5  If  condition _a exists, quantitatively determine the organochiorine




     pesticides according to  (1].




9.6  If  condition b exists, PCS's only are present, no further separation




     or  cleanup is necessary.  Quantitatively determine the PCB's according




     to  11.below .




9.7  If  condition £ exists, compare peaks obtained from the sample to




     those of standard Aroclors and make a judgment as to which Aroclors




     may be present.  To separate the PCB's from the organochiorine




     pesticides, continue as outlined in 10.4.




9.S  If  condition d_ exists separate the sulfur from the sample using the




     method outlined in (10.3) followed by the method in  (10.31




9.9  If  condition e_ exists then the following macro cleanup and separation




     procedures (10.2 and 10.3) should be employed and, if necessarv




     followed by the micro separation procedures (10.4 and 10.5).

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                                      3-8





LO.   Cleanup  and Separation Procedures




     10.1   Interferences in the fora of distinct peaks and/or high background




           in  the initial gas chromatographic analysis, as well as,  the




           physical characteristics of the extract (color, cloudiness,




           viscosity) and background knowledge of the sanple will indicate




           whether cleanup is required.  When these interfere with measure-




           ment of the pesticides, or affect column life or detector sen-




           sitivity, proceed as directed below.




     10.2   Acetonitrile Partition - This procedure is used to remove fats and




           oils from the sanrple extracts.  It should be noted that not all




           pesticides are quantitatively recovered by this procedure.  The





           analyst must be aware of this and demonstrate the efficiency of




           the partitioning for the compounds of interest.




           10.2.1  Quantitatively transfer the previously concentrated extract




                  to a 125 ml separatory funnel with enough hexane to bring




                  the final  volume to 15 ml.  Extract.the sample four times




                  by shaking vigorously for one minute with 50 ml portions




                  of hexane-saturated acetonitrile.




           10.2.2  Combine and transfer the acetonitrile phases to a one-liter




                  separatory funnel and add 650 ml of distilled water and




                  40  ml of saturated sodium chloride solution.  Mix thor-




                  oughly for 50-35 seconds.   Extract with two 100 ml portions




                  of  hexane  by vigorously shaking about 15 seconds.




          10.2.3  Combine the hexane extracts in a one-liter separatory funne.




                  and wash with two 100 ml portions  of distilled  water.   Dis-




                  card the water layer and pour the  hexar.e layer  through  a




                  5-4 inch anhvdrous sodiua sulfate  colirnn  into a 500  ml  K-D

-------
                                 3-9





              flask equipped with a 10 al ampul.   Rinse the separator/




              funnel and column with three 10 ml  portions of hexane.




      10.2.4  Concentrate the extracts to 6-10 ml in the K-D evaporator




              in a hot water bath.




      10.2.5  Analyze by gas chromatography unless a need for further




              cleanup is indicated.




10.3  Florisil Column Adsorption Chromatography




      10.3.1  Adjust the sample extract volume to 10 ml.




      10.3.2.  Place a charge of activated Florisil (weight determined




              by lauric-acid value, see Appendix  I)  in a Chrcmaflex




              column.  After settling the Florisil by tapping the column




              add about one-half inch layer of anhydrous granular sodium




              sulfate to the top.




      10.3.3  Pre-elute the column, after cooling, with 30-60 ml of




              petroleum ether.  Discard the eluate and just prior to




              exoosure of the sulfate layer to air,  quantitatively




              transfer the sample extract into the column by decantation




              and subsequent petroleum ether washings.  Adjust the




              elution rate to about 5 ml per minute  and, separately,




              collect up to three eluates in 500  ml  K-D flasks equipped




              with 10 ml ampuls.   (See Eluate Composition below).




              Perform the first elution with 200  ml  of 6?6 ethyl ether




              in petroleum ether, and the second  elution with 200 ml of




              15?i ethyl ether in petroleum ether.  Perform the third




              elution with 200 ml of 50?o ethyl ether - petroleum ether




              and the fourth elution with 200 ml  of 100% ethvl ether.

-------
                                   5-10

             Eluate Composition - By  using an equivalent quantity of any

             batch of Florisil as determined by its  lauric acid value,  the

             pesticides will be separated into the  eluates indicated below:

                                   6% Eluate

             Aldrin             DDT                 Pentachlcro-
             BHC                Heptachlor           nitrobenzene
             Chlordane          Heptachlor EpoxLde   Strobane
             ODD                Lindane             Toaaphene
             DDE                Methoxychlor        Trifluralin
                                Mirex               PCB's

                     15% Eluate               50% Eluate
                     Endosulfan 1              Endosulfan II
                     Endrin                   Cap tan
                     Dieldrin
                     Dichloran
                     Phthalate esters

             Certain thiophosphate  pesticides  will  occur in  each of the

             above fractions  as well  as  the  100% fraction.   For additional

             information regarding  eluate  composition,  refer to the FDA

             Pesticide  .Analytical Manual (6).

     10.3.4  Concentrate the  eluates  to  6-10 ml  in  the  K-D evaporator

             in a hot water bath.

     10.3.3  Analyze fay gas chromatography.

10.4 Silica Gel Micro-Column  Separation  Procedure  (7)

     10.4.1  Activation for Silica  Gel

             10.4.1.1  Place  about  20 gm of  silica  gel  in a  100 ml  beaker.

                       Activate at  180 C for approjdmately  16 hours.   Transfer

                       the  silica gel  to a 100 ml  glass stoppered bottle.

                       When cool, cover  with about  55 ml of  0.50% diethyl

                       ether  in ben:ene  (volume : volume ).  Keep  bottle

                       well sealed.   If  silica gel  collects  on  the  ground

                       glass  surfaces, wash  off  with the  above  solvent

-------
                              3-11




                  before resealing.  Always maintain an excess




                  of the mixed solvent in bottle  (appro-ximately 1/2 in.




                  above silica gel).  Silica gel  can be effectively




                  stored in this manner for several days.




10.4.2  Preparation of the Chromatographic Column




       10.4.2.1   Pack the lower 2 mm ID Section  of the microcolLmn




                  with glass wool.  Permanently mark the column




                  120 mm above the glass wool.  Using a clean rubber




                  bulb from a disposable pipet seal the lower end




                  of the microcolunn.  Fill the microcoluzm with




                  0.50% ether in benzene Cv:v) to the bottom of




                  the 10/30 joint  (Figure  1).  Using a disposable




                  capillary pipet, transfer several aliquots of the




                  silica gel slurry into the microcolunn.  After




                  approximately 1  cm of silica gel collects in




                  the bottom of the microcolumn,  remove the rubber




                  bulb seal, tap the column to insure that the




                  silica gel settles uniformly.   Carefully pack




                  column until the silica  gel reaches the 120 ; 2




                  mm mark.  Be sure that there are no air bubbles




                  in the column.   Add about 10 mm of sodium sulfate




                  to the top of the silica gel.   Under low humidity




                  conditions, the  silica gel may  coat the sides of




                  the column and not settle properly.  This can be




                  minimi led by wiping ths  outside of the column




                  with an anti-static solution.

-------
                 5-12




10.4.2.2  Deactivation of the Silica Gel




          a.   Fill the microcorumn to the base of




              the 10/50 joint with the 0.50% ether-




              benzene mixture, assemble reservoir




              (using spring clasps)  and fill with




              approximately 15 ml of the 0.50% ether-




              benzene mixture.  Attach the air




              pressure device (using spring clasps]




              and adjust the elution rate to approxi-




              mately 1 ml/min. with  the air pressure




              control.  Release the  air pressure and




              detach reservoir just  as the last of




              the solvent enters the sodium sulfate.




              Fill the column with n-hejcane (not nixed




              hexanes) to the base of the 10/50 fitting.




              Evaporate all residual benzene from the




              reservoir, assemble the reservoir section




              and fill with 5 ml of n-hexane.   Apply




              air pressure and adjust the flow to 1




              ml/min.  (The n-hejcane flows slightly




              faster than the benzene] .   Release the air




              pressure and remove the reservoir just as




              the n-he-xane enters the sodium sulfate.




              The column is now ready for use.




          b.   Pipet a 1.0 ml aliquot of the concentrated



              sample extract (previously reduced to a




              total volume of 2.0 ml)  on to the  column.

-------
                           3-13





                      As  the last  of the sample passes  into




                      the sodium sulfate layer, rinse dour.




                      the internal wall  of the column twice




                      with 0.2S ml of n-hexane.  Then assemble




                      the upper section  of the column.   As the




                      last of the  n-hexane rinse reaches the




                      surface of the sodium sulfate,  add enough




                      n-hexane (volume predetermined, see




                      10.4.3 below)  to just elute all of the




                      PCB's present  in the sample.   Apply air




                      pressure and adjust until the  flow is




                      1 ml/min.  Collect the desired volume of




                      eluate (predetermined, see 10.4.3 below)




                      in an accurately calibrated ampul.  .As the




                      last,of the  n-hexane reaches  the  surface




                      of the sodium sulfate, release the air




                      pressure and change the collection ampul.



                  c.   Fill the column with 0.50% diethyl ether




                      in benzene,  again  apply air pressure and




                      adjust flow to 1 ml/min.  Collect the




                      eluate until all of the organochlorine




                      pesticides of interest have been eluted




                      (volume predetermined, see 10.4.3 below).




                  d.   .Analyze the eluates by gas chromatograrhy.




10.4.3  Determination of Elution Volumes




        10.4.3.1  The elution volumes for the PCB's  and the




                  pesticides depend upon a number of factors which

-------
                      5-14




          are difficult to control.   These  include




          variation in:




          a.   Mesh si:e of the silica gel




          b.   Adsorption properties  of the  silica gel




          c.   Polar contaminants  present in the  eluting




              solvent




          d.   Polar materials  present in the sample and




              sample solvent




          e.   The dimensions of the  microcolumns




          Therefore, the optimum  elution volume  must




          be  experimentally determined each time  a factor




          is  changed.  To determine  the elution  volumes,




          add standard mixtures of Aroclors and  pesticides




          to  the column and serially collect 1 ml elution




          volumes.   Analyze the individual  eluates by gas




          chromatography and determine the  cut-off volume




          for n-hexane and for ether-benzene.   Figure 2




          shows the retention order  of the  various PCS




          components and of the pesticides.  Using this




          information, prepare the mixtures required for




          calibration of the microcolumn.




10.4.0.2  In  determining the volume  of hexane required to




          elute the PCB's the sample volume (1 ml) and the




          volume of n-hexane used to rinse  the column wall




          must be considered.   Thus, if it  is  determined




          that a 10.0 ml elution volume is  required to




          elute the PCB's, the volume of heaane to be added

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                                 5- 15





                        in addition to the sample voluae but including




                        the rinse volume should be 9.5 ml.




              10.4.5.5  Figure 2 shows that as the average chlorine




                        content of a PCS mixture decreases the solvent




                        volume for conrrjlete elution increases.  Quali-




                        tative determination [9.4) indicates which




                        Aroclors are present and provides the basis




                        for selection of the ideal elution volume.  This




                        helps to mininiire the quantity of organochlorine




                        pesticides which will elute along with the low




                        percent chlorine PCB's and insures the most




                        efficient separations possible for accurate




                        analysis.









              10.4.5.4  For critical analysis where the PC3's and




                        pesticides are not separated ccnrpletely, the




                        column should be accurately calibrated according




                        to (10.4.5.1) to determine the percent of




                        material of interest that elutes in each  fraction.




                        Then flush the colunn with an additional  15 nil  of




                        0.50?i ether in benzene followed by 5 ml of n-




                        hexane and use this reconditioned column  for




                        the sample separation.  Using this technique  one




                        can accurately predict the amount ("O of  materials




                        in each micro column fraction.




1C.5  Micro Colunn Separation of Sulfur, PCB's, and Pesticides




      10.5.1  See procedure for preparation and packing T.icro colu-m  in




              ?C3 analysis section {1C.4.1 and 1C.-.2).

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                       3-16




10.5.2  Microcolumn Calibration




        10.5.2.1  Calibrate the microcolumn for sulfur and




                  PC3 separation by collecting 1. 0 al fractions




                  and analysing them by gas chromatography to




                  determine the following:




                  1)  The fraction with the first elating ?C3's




                      (.those present in 1260),




                  2)  The fraction with the last eluting PC3' s




                      (those present in 1221),




                  3)  Tne elution volume for sulfur,




                  4)  The elution volume for the pesticides of




                      interest in the 0.30% ether-bentene fraction




                  From these data determine the following:




                  1)  The eluting volume containing only sulfur




                      (Fraction I).




                  2)  The eluting volume containing the last of




                      the sulfur and the early eluting PCS's




                      (Fraction II),




                  3}  The eluting volume containing the remaining




                      PCB's (Fraction III),




                  4)  The ether-benzene eluting.volume containing




                      the pesticides of interest (Fraction IV).




10.5.3  Separation Procedure




        10.3.3.1  Carefully concentrate the 6% eluate from the




                  florisil column to 2.0 ml in the graduated




                  ampul  on a warm water bath.




        10.5.3.2  Place  1.0 ml (50!s)  of the concentrate  into




                  the  microcolumn with a 1 ml  pipet.   Be  careful

-------
                 J-l /






          not to get any sulfur crystals into the pipet.




10.5.3.3  Collect Fractions I and II in calibrated centri-




          fuge tubes.




          Collect Fractions III and IV in calibrated ground




          glass stoppered ampules.




10.5.3.4  Sulfur Removal (9) - Add 1 to 2 drops of mercury




          to Fraction II stopper and place on a wrist-action




          shaker.  A black precipitate indicates the presence




          of sulfur.  After approxiately 20 minutes the




          mercury may become entirely reacted or deactivated




          by the precipitate.  The sample should be quantita-




          tively transferred to a clean centrifuge tube and




          additional mercury added.  When crystals are present-




          in the sample, three treatments may be necessary to




          remove all the sulfur.  .After all the sulfur has




          been removed from Fraction II (check using gas




          chromatography) combine Fractions II and III.




          Adjust the volume to 10 ml and analyze gas chroma-




          tography.  Be sure no mercury is transferred  to




          the  combined Fractions  II and III, since it  can




          react with certain pesticides.




          By combining Fractions  II and III, if ?C3's  are




          present, it is possible to identify the Aroclor(s)




          present and a quantitative analysis can be oer-




          foraed accordingly.  Fraction I can be discarded




          since it only contains  the bulk of the sulfur.




          Analyze Fractions III and IV for the PCB's and

-------
                                      3-18


                             pesticides.   If  DDT  ana  its  hoaologs,  aldrin,

                             heptachlor,  or technical  chlordane  are present

                             along  with  the PCB's,  an  additional micro -

                             column separation  can  be  performed  which nay help

                             to  further  separate  the  PCB's  from  the pesticides

                             (See  10.4).

11.   Quantitative  Determination

     11.1   Measure  the  volume of n-hexane eluate, containing  the PCB's and

           inject  1  to  5  ul  into the gas  chromatograph.   If necessary, adjust

           the  volume of  the  eluate to give linear  response to  the  electron

           capture  detector.   The raicrocouloraetric  or  the electrolytic detector

           may  be  employed to improve specificity for  samples having higher

           concentrations of  PCB's.

     11.2   Calculations

           11.2.1   When a single Aroclor  is present,  compare  quantitative

                   Aroclor reference standards  (e.g.,  1242, 1260)  to the un-

                   known.  Measure  and sun the  areas  of  the unknown and the

                   reference  Aroclor and  calculate  the result as follows:

                                          [A]  [B]  [V  ]
                        Microgram/liter  =  f(VJ  (v }j  ~ [N]


                        A   - "g.of Standard Injected
                              Z of Standard Peak  Areas  ~  ^j
                                                           mm"
                                                           •)
                         B   = E of Sample Peak  Areas =  (ma'1)

                        V.  = Volume of  sample injected  (yl)

                        V   = Volume of  Extract  (ul)  from  which sample
                              is injected into gas  chromatograph

                        V   = Volume of  water  sarnie  e-xtracted  (ml)
                         s
                        N   = 2 when micro column  used
                              1 when micro column  not used

-------
                       3-12



             Peak Area = Peak height (an .x Peak Width at

                         1/2 height



11.2.2  For complex situations,  use the calibration method



        described below.  Small variations in components between



        different Aroclor batches make it necessary to obtain



        samples of several specific Aroclcrs.   These reference



        Aroclors can be obtained from Dr. Ronald Webb, Southest



        Environmental Research Laboratory, EPA, Athens, Georgia



        30601.  The procedure is as follows:



        11.2.2.1  Using the OV-1 column, chromato graph a known



                  quantity of each .Aroclor reference standard.



                  Also chromatograph a sample of p,p'-DDE.



                  Suggested concentration of each standard is



                  0.1 ng/ul for the Aroclors and 0.02 ng/ul for



                  the p,p'-DDE.



        11.2.2.2  Determine the relative retention time  (KRT} of



                  each PCS peak in the resulting chroma to grams



                  using p,p'-DDE as 100.  See Figures 3 through 5.



                        RT  x  100
                  RRT
                          RTDDE
                  RRT = Relative Retention Time



                  RT  = Retention  tiae of peak of interest



                  RT
                    DDE = Retention  time of p,p'-DDE



                  Retention time is  measured as  that  distance  in



                  nm between  the first appearance of  the  solvent



                  peak and the maximum for the coiroounc.



        11.2.2.5  To calibrate the instrument  for each  PC3



                  measure the area of each peak.

-------
          Area * Peak height  CUED) a Peak width  at  1/2

          height.  Using Tables  1 through  6 obtain the

          proner mean weight factor, then  determine
                                   -?
          the response factor ng/nm".

                   (ng• ) (me_an weight percent)
             ,  :        	    100
          ng/mm  =	Q—^	

          ngj_ = ng of Aroclor Standard Injected

          Mean weight percent = obtained from Tables 1
                                through 6.

11.2.2.4  Calculate the RRT value and the  area for each

          PCB peak in the sample chromatograjn.  Compare

          the sample chromatogram to those obtained for

          each reference Aroclor standard.  If it  is

          apparent that the PC3 peaks present are  due to

          only one Aroclor then calculate  the concentration

          of each. PCB using the following  formula:

          ng PCB = ng/mm  .x Area

          Where Area = Area (jm ) of sample peak

          ng/mm" = Response factor for that peak measured.

          Then add the nanograms  of PCB's present  in the

          injection to get the total number of nanograms

          of PCB's present.  Use  the following formula to

          calculate the concentration of PCB's in  the sacple

                             In&J  JV.J
          MicrogranLS/Liter = JTT-T	rrrr x INJ
                             lvsJ  lviJ

          Vs = volume of water extracted (al)

          Vt = volume of extract

-------
                                     3-21




                                V. = volume of sample injected  (j-1)




                                Ing = SUE of all tits PCB's in nanogranis  for




                                      that Aroclor identified




                                N = 2 when nicrocolunn used




                                N = 1 when aicrocolunr. not used




                                The value can then be reported  as Micrograns/




                                Liter PCS's reported as the Aroclor    For




                                samples containing nore than one .-.rocior, use




                                Figure 9 chronatogras divisional flow  chart




                                to assign a proper response factor to  each




                                peak and also identify the "most likely"




                                Aroclors present.  Calculate the ng of each




                                PCB isomer present and sun them according




                                to the divisional flow chart.   Using the




                                forrrula above, calculate  the concentration of




                                the various Arociqrs present in the sairnDle.




12.   Reporting Results




     12.1  Report results in micrograms per liter without correction for




           recovery data.  When duplicate and spiked samples are analysed,




           all data obtained should be reported.

-------
                          Table 1

                Comoosition of Aroclor 1221 (&)

RRTa
11
14
16
19
21
28

32

[37
[40
Total
Mean
Weight
Percent
31. 8
19.3
10.1
2.8
20.8
5.4

1 .4

1.7

93. 3

Relative
Std. Dev.b
15.8
9.1
9.7
9.7
9.3
13.9

30-1

48.8



Number of
Chlorines0
1
1
2
2
2
2l 85%
3J 15%
2] 101
3j 90%
3
3

    aRetention ti^ie relative to p ,p ' -DDE=100 .   Measured from
irst appearance of solvent.   Overlapping peaks that are
quantitated as one peak are bracketed.
     bstandard deviation of seventeen results
of the mean of the results.
     CFrorn GC-MS data.  Peaks containing mixtures
of different chlorine numbers are bracketed.
                                             as a percentage
                                                 of isoners

-------
                            Table 2

                 Composition of Aroclor 1232 C8)


RRTa
11
14
16
f20
Ul
28

32
37
40
47
54

58
70

78
Total
Mean
Weight
Percent
16.2
9 .9
7.1
17.8

9.6

3.9
6.8
6.4
4.2
3,4

2.6
4.6

1.7
94.2

Relative
Std. Dev.b
3.4
2.5
6.8
2.4

3. 4

4.7
2.5
2.7
-4.1
3.4

3.7
3.1

7.5


Number of
Chlorines0
1
1
2
2
2
21 40%
3J 60%
3
3
3
4
3] 33%
4J 67%
4
4] 90%
s] 10%
4

     aRetention time relative to p ,p'-DDE=100.   Measured fron
first appearance of solvent.  Overlapping peaks that are
guantitated as one peak are bracketed.
     ^Standard deviation of four results as a mean of the
results.
     CFrom GC-MS data.  Peaks containing mixtures of isomers
of different chlorine numbers are bracketed.

-------
                           Table  3

                 Composition of Aroclor  1242 C3)


RHT£
11
16
21
28

32
37
40
47
54

58
70

78
84
98
104
125

146

Total
Mean
Weight
Percent
1. 1
2.9
11.3
11.0

6.1
11.5
11.1
8. 8
6 . 8

5.6
10.. 3

3.6
2.7
1.5
2.3
1.6

1.0

98.5

Relative.
Std. Dev.b
35.7
4.2
3.0
5.0

4.7
5.7
6.2
4.3
2.9

3.3
2.8

4.2
9 .7
9.4
16.4
20.4

19 .9




Number of
Chlorines0
1
2
2
21
3J
3
3
3
4
31
4J
4
41
5j
4
5
5
5
51
6J
5
ej



25%
75%




33%
67%

SOI
10%




85%
15%
75%
25%

     aRetention time relative to p,p'-DDE=100.   Measured from
first appearance of solvent.
     bStancard deviation of six results as a cercentaae of
the mean of the results.
     C7rom GC-MS data.   Peaks containing mixtures of iseiners
of different chlorine numbers are bracketed.

-------
                          3-25
                            Table 4

                  Composition of Aroclor 1248


RRTa
21
28
32
47
40

47
54

58
70
78
84
98
104

112
125

146

Total
Mean
Weight
Percent
1.2
5.2
3.2
8.3
8.3

15.6
9.7

9.3
19.0
6-6
4.9
3.2
3.3

1.2
2.6

1.5

103.1

Relative
Std. Dev.b
23.9
3.3
.3.8
3.6
3.9

1.1
6 .0

5.8
1.4
2-7
2.6
3.2
3.6

6.6
5.9

10. 0



Number of
Chi or
2
3
3
3
31
4j
4
31
4J
4
11
4
5
5
41
5J
5
51
ej
5
6j
ines"




85%
15%

10%
90%

80%
20%



10%
90%

90%
10%
85%
15%

     aRetention time relative to p,p'-DDE=100.  Measured from
first appearance of solvent.
     ^Standard deviation of six results as a percentage of
the mean of the results.
     cFrom GC-MS data.  Peaks containing mixtures of isorrvers
of different chlorine numbers are bracketed.

-------
                           3-26
                            Table  S

                  Composition of Aroclor 1254
Mean

RRT£
47
54
58
70

84
98
104
125

146

160
174
203
232
Total
Weight
Percent
6.2
2.9
1.4
13.2

17.3
7.5
13.6
15.0

10. 4

1.3
8.4
1. 8
1.0
100.0
:=::=:::— ^^—— —————— ^-— —
Relative
Std. Dev.b
3.7
2.6
2.8
2.7

1.9
5.3
3.8
2.4

2.7

8.4
5.5
18.6
26.1



Number of
Chi or
4
4
4
41
5J
5
5
5
51
6J
5
6j
6
6
6
7
ines



25%
75%



70%
30%
30%
70%





     aRetention time relative to p,p'-DDE=100.   Measured  frora
first appearance.of solvent.
     ^Standard deviation of six results  as  a  percentage of  the
mean of thfe results.
     GFrom GC-MS data.  Peaks containing mixtures  of  iscners
are bracketed.

-------
                           3-27
                            Table 6

                 Composition of Arocior 1260


RRT*
70
84
[~ 98
Li 04

117
125

146
160

174
203

T232
L244

280
332
372
448
523
Total
Mean
Weight
Percent
2.7
4.7
3.8

3.3
12.3

14.1
4.9

12.4
9. 3

9-8

11.0
4.2
4.0
.6
1.5
98.6

Re la
Std.
6.
1.
3.

6 .
3.

3.
2.

2.
4-

3.

2.
5.
8.
25.
10.

tive.
Dev.°
3
6
5

7
3

6
2

7
0

4

4
0
6
3
2



Number of
Chlorines0
5
5
5
6
6
5'
6.
6
6'
7
6


d
60%
40%

1 15%
1 85%

1 50%
J 50%

61 10*
7j 90%
6
7
7
7
8
8
8
e
10%
90%






     aRetention time relative to p/p'-DDE=100.   Measured from
first appearance of solvent.  Overlapping peaks that are
quantitatsd as one peak are bracketed.
     ^Standard deviation of six results as a mean of the
results.
     GFrom GC-MS data.  Peaks containing mixtures of isomers
of different chlorine numbers are bracketed.
     ^Composition determined at the center of peak 104.
     Composition determined at the center of peak 232.

-------
COMPRESSED_

AIR 	
                                        ^PRESSURE
                                           ^GAUGE
SUPPLY
JXZ
0-5

PSIG
              SHUT-OFF
                VALVE
             REGULATOR
                                           NEEDLE
                                            VALVE
                              I cm
                      FLEXIBLE
                       TUBING
              SILICA GEL

                  5 cm  3
                     cm
                              /GLASS
                           /"WOOL
                           &
                                  £  10/30
                                  15 ml
                               RESERVOIR
                          1
                           ?
                                  §  10/30
                       \2-
                                 23 cm  x 4.2 mm 1.0.
                                 2 cm  x 2 mm I.D.
         FIGURE  I.   MICROCOLUMN  SYSTEM

-------
     I  SULFUR |
_J
<
h-
o
U-
o
u  20
     0
                   HEPTACHLOR
                                DDE
              M I R E X
                                    ALDRIN
              TECHNICAL   CHLORODANE
                    OP'  a  PP'    DDT
                                                                        X-CHLORDANE
6        8        10

VOLUME  n-HEXANE   ml

-------
                                      3-30


                                    REFERENCES

 (1)  "Method  for  Organochlorine  Pesticides  in  Industrial  Effluents," U.S.
     Environmental Protection Agency, National  Environmental  Research Center,
     Analytical Quality  Control  Laboratory,  Cincinnati, Ohio  45263,  19"3.

 (2)  Leoni, V., "The  Separation  of Fifty Pesticides  and Related Compounds
     and  Polychlorinated Biphenyls into Four Groups  by Silica Gel Micro-
     column Chromatography,"  Journal  of Chromatographv, 62_,  65 (1971).

 (3}  McClure,  V.  E.,  "Precisely  Deactivated Adsorbents Applied to the
     Separation of Chlorinated Hydrocarbons  "  Journal  of  Chronatographv,  70,
     168  (1972).                 '              	'	" —

 (4)  "Methods  for Organic Pesticides  in Water  and Wastewater," U.S.  Environ-
     mental Protection Agency, National Environmental  Research Center,
     Analytical Quality  Control  Laboratory,  Cincinnati, Ohio  45263,  1971.

 (3)  "Handbook for Analytical Quality Control  in Water and Wastewater
     Laboratories,"  Chapter 6, Section 6.4,  U.S.  Environmental Protection
     Agency,  National Environmental Research Center,  .Analytical Quality
     Control  Laboratory, Cincinnati,  Ohio 4526S,  1972.

 (6)  "Pesticide Analytical Manual," U.S. Dept.  of Health,  Education, and
     Welfare,  Food and Drug Administration,  Washington, D.C.

 (7)  Bellar,  T. A. and  Lichtenberg, J. J.,  "Method for the Determination of
     Polychlorinated  Biphenyls in Water and Sediment," U.S.  Environmental
     Protection Agency,  National Environmental  Research Center, .Analytical
     Quality  Control  Laboratory, Cincinnati, Ohio 4526S,  1975.

 (8)  Webb,  R.  G.  and  McCall,  A.  C. , "Quantitative PCB  'Standards for  Electron
     Capture  Gas  Chromatography."  Presented at the  164th  National  ACS
     Meeting,  New York,  August 29, 1972.  (Submitted to the  Journal  of
     Chromatographic  Science  for publication).

 (9)  Goerlitz, D. F.  and Law, L. M.,  "Note  on  Removal  of  Sulfur Interferences
     from Sediment- Extracts for Pesticide Analysis," Bulletin of Environmental
     Contamination and Toxicology, 6_, 9 (1971).

(10)  Mills, P. A., "Variation of Florisil Activity:   Sample  Method for  Measuring
     Adsorbent Capacity  and its  Use in Standardizing Florisil Columns,"
     Journal  of the  Association of Official .Analytical Chemists, 51_, 29 (1963).

(11)  Steere,  N. V.,  editor, "Handbook of Laboratory  Safety,"  Chemical Rubber
     Company,  18901  Cranwood  Parkway, Cleveland,  Ohio  4412S,  1971,  pp.  230-254.

-------
                                    3-1






                                   APPENDIX I





15.   Standardization of Florisil Column by Weight Adjustment Based on Adsorption




     of Laurie  Acid.




     15.1   A rapid method for determining adsorptive capacity of Flcrisii is




           based on adsorption of lauric acid from hexane solution (6]  (S).




           An excess of lauric acid is used and amount not adsorbed is  measured




           by alkali titration.  Weight of lauric acid adsorbed is used to




           calculate, by simple proportion, equivalent quantities of Florisil




           for batches having different adsorptive capacities.




     15.2  Apparatus




           15.2.1  Buret. -- 25 ml with 1/10 ml graduations.




           15.2.2  Erlenmeyer flasks.  — 125 ml narrow mouth and 25 ml, glass




                   stoppered.




           13.2.5  Pipet. -- 10 and 20 ml transfer.




           13.2.4  Volumetric flasks.  -- 500 ml.




     13.3  Reagents and Solvents




           15.3.1  Alcohol,  ethyl. -- USP or absolute, neutralized to




                   phenolphthalein.




           13.3.2  Hexane. — Distilled from all glass apparatus.




           15.3.3   Lauric acid. --Purified, CP.




           13.3.4   Lauric acid  solution. -- Transfer  10.000 g  lauric acid to




                   500 ml volumetric  flask, dissolve  in hexane, and dilute  to




                   500 ml (1 ml * 20  mg).




           13.3.5  Phenolphthalein Indicator.  -- Dissolve 1 g  in alcohol and




                   dilute to 100 ml.

-------
                               5*2
      15.5.6  Sodium hydroxide.  -- Dissolve 20 g NaOH (pellets, reagent




              gxadej in water and dilute to 500 ml  (IN).   Dilute 25 ml




              IN NaOH to 500 ml  with water (0.05NJ.   Standardise as follows:




              Weigh 100-200 mg lauric acid into 125  ml Erlenmeyer flask.




              Add 50 ml neutralized ethyl  alcohol and 5 drops phenol-




              phthalein indicator;  titrate to  permanent end point.   Calculate




              mg lauric acid/ml  0.05 N_ NaOH (about  10 mg/al) .




15.4   Procedure




      15.4.1  Transfer 2.000 g Florisil  to 25  ml glass stoppered Erienneyer




              flasks.   Cover loosely with  aluminum  foil and heat overnight




              at 130°C.   Stopper,  cool  to  room temperature, add 20.0 ml




              lauric acid solution (400  mg),  stopper, and shake occasionally




              for 15 min.   Let adsorbent settle and  pipet 10.0 ml of




              supernatant into 125 ml Erlenmeyer flask.   Avoid inclusion




              of any Florisil.




      15.4.2  Add 50 ml neutral  alcohol  and 5  drops  indicator solution;




              titrate with 0.05N_ to a permanent end  point.




15.5   Calculation of Lauric Acid Value  and Adjustment of Column Weight




      15.5.1  Calculate amount of lauric acid  adsorbed on Florisil  as




              follows:




              Lauric Acid value * mg lauric acid/g  Florisil = 200 - (ml




              required for titration X  mg  lauric acid/ml 0.05N_NaOH).




      15.5.2  To obtain an equivalent quantity of any batch of Florisil,




              divide 110 by lauric acid value  for that batch and multiply




              by 20 g.   Verify proper elution  of pesticides by 15.6.

-------
                                0-0
13.6  Test for Proper Elution Pattern and Recovery o£ Pesticides:




      Prepare a test mixture containing aidrin, heptachlor epo.xide




      p,p'-DDE, dieldrin, Parathion and malathion.  Dieldrin and




      Parathion should elute in the 15% eluate; all but a trace of




      malathion in the 309i eluate and the others  in the 6% eluate.

-------
               37
                  AROCLOR 1242
Figure 3. Column: 3% OY-1,  Carrier Gas: Nitrogen at 60 ml/min,
         Column  Temperature: 170 C, Detector:  Electron Capture

-------
                              AROCLOR 1254
                         I04
                             125
                                  48
                                        174
                                                       232
Figure 4. Column:  3%  OY-1, Carrier Gas: Nitrogen  at  50  ml/min,
         Column Temperature: 170 C, Detector:  Electron  Capture

-------
                               AROCLOR 1280
                               280
                                                        528
Figure  5. Column: 3% OY-1, Carrier Gas: Nitrogen  at  60  ml/min,
         Column  Temperature: 170  C,  Detector:  Electron Capture

-------
/I
                               AROCLOR 1242
               I
                      I
                      I
I
0
3
6
       21
24
                       9       12      15      18
                       RETENTION TIME IN MINUTES
Figure  6. Column: 1.5%  OY-17  + 1.95%  QF-1, Carrier Gas: Nitrogen
at 60 ml/min,  Column  Temperature: 200 C, Detector:  Electron Capture

-------
                                                        AROCLOR 1254
Figuie 7. Column: 1.5% 0V 17 <  1.95%
         Detector: Electron Capture.
 RETENTION TIME  IN MINUTES
OF I, Carrier Gas: Nitrogen at 60 ml/min,  Column  Temperature:   200  C,

-------
       I
       I
J_
I
I
I
I
I
                                                               I
I
I
I
I
I
I
I
J
54
0
3
        12
      15
       ie
                                          36
                                          39
                                                                                                                 48
                                                               51
                                                21      24      27      30      33

                                                  RETENTION TIME IN MINUTES
Figure  8. Column: 1.5%  0V 17  t  1.957. QF-1,  Carrier  Gas: Nitrogen  at 60  ml/min,  Column Temperature:  200C, Detector:  Election Capture

-------
                RRT of first peak < 47?
              YES
     Is  there a distm ct
     peak with RRT  78?
RRT
47
58?
      YES
  NO
YES
   Use 1242 for
 peaks -  RRT  84
 Use  1242 for
peaks -  RRT 70
    Use  1254
    for p eaks
   -  RRT 104
           Is there  a  distinct
           peak  with RRT 117?
         YES
     NO
                    Use  1254 for  all
                    peaksl RRT 174
     Use 1260 for
     all other peaks
                      Use 1260  for
                        all p eaks
Figure  9. Chromatogram Division Flowchart  (8)

-------
           Attachment B
 Tentative Method of Testing for
Polychlorinated Biphenyls in Watei

-------
  - o
              ENVIRONMENTAL PROTECTION  AGENCY
                                REGIUN II
                     EDISON. NEW JERSEY O8817

2-SA-T5J                                                OAIL. January 22, 1'J76
••r-CT  Tentative  Method  of  Test For
     Poiychlcrinntcc] Biphcnyls in Water.
                                       ^. -•
     Chief,- Technical  Support Branch
                             Tentative Method of Test

                     For  PolychlorinatocI biphcnyls in Water

     1.  Scope £ Application

         1.1  This method covers  the determination of certain  polychlorinatcd
         biphenyls  (PCB's)  including Aroclors 1016, 1221,  1232,  1242, 1248,
         1254 and 1260.

         1.2  The method  covers the analysis of water samples.

         1.3  This method used a  Finnigan Mass Spectrometer and  Systems Industries
         Data System.  Other GC/MS  systems could be employed for the sair.e
         analysis.

     2.  Applicable References

         2.1  0.  Hutzinger,  S. Safe,  V.  Zitko, "The Chemistry  of PCB's" CRC  Press,
         Cleveland, Ohio  44128  (1974).

         2.2  S.  Safe £ 0.  Hutnir.ger,  "Mass Spectrrraetry of Pesticides and
         Pollutants", CRC Press,  Cleveland, Ohio,  1973.

         2.3  Methods for Organic Pesticides in Water and Wastewntcr, EPA, NERC,
         Cincinnati, Ohio 45263,  (1971).

         2.4  Current Practice in GC-MS  Analysis of Orgjiiics in  Watur, iil'A
         Protection Technoloyy Service,  EPA -R2-73-277, August 1973.

         2.5  E.  J.  BonclJ.i,  M.S. Sr.ory  and J. H.  Kjiio'.iL, Dynamic M.i:-. s ^pcc! vm-.v 'try
         Vol.  2,  177-202, iieyden  &  Son Ltd.,  1971,  U.K.

         2.6  E.  J.  Bonclli,  Aii.il .  Chc-n. ,  -\-\,  ^03-o^u (1072).

         ...7  T  A.  Dellai:  S  J. J.  Licht OIUVM\; ,  ASTM,  ST!% f'7J, "IV-:: 1 '.^ (I')?',).

         .--0  J.  \v .  EichelL.i.'Uu'i." , L.  \'..  li.nrj:' .i;u!  W.  I,. !UuK!e,  A:ij_iJ . i.'i  r:i.   .;.•,
                                                                  "

-------
                                  -2-
    2.9  F. W. McLat'fcrty, "Interpretation c£ Mass Spectra", 2nd Ed., i-.'A
    Benjamin, Inc., Reading, Mass., 1973.

3.   Summary

    PCB's are liquid-liquid extracted and the extract concentrated.
    Identification and quantitation is made by computerized gas chromatogra:
    mass spectrometry.   Either electron impact (70 cv) or chemical ionizatic
    (methane reagent gas) mass spectrometry is employed.  The detection
    limit is approximately 20 ng/1 for the PC3 mixtures listed in Section 1.
    when analyzing a 100 ul extract from a one liter water sample and
    operating the C.I.  mass spectrometer at 1.0 amp filament current, -2200
    V continuous dynode, 10~& A/V, 750 microns reagent gas pressure.  In
    the E.I. mode at 5004" ma, -2200 V., 10~7 A/V,  the detection limit is
    200 ng/1.  At 10~8 A/V, the detection limit is 20 ng/1.

4.   Interferences

    No interferences are encountered using molecular ion cluster scanning
    for biphenyl, mono-, di-, etc. chlorobiphenyls and checking isotope
    intensity ratios.

5.   Apparatus R Reagents

    5.1  Computerized GC/MS.

    5.2  Separatory funnel, 2000 ml, with Teflon  stopcock.

    5.3  100 ml and 2000 ml graduated cylinders.

    5.4  Pesticide grade hexane.

    5.5  Pesticide grade methylene chloride.

    5.6  Pesticide grade acetone-

    5.7  Anhydrous sodium sulfatc, granular,  reagent grade.

    5.8  Sodium chloride, reagent grade.

    5.9  Pyrex glass wool.

    5.10  Pyrex chromatographic column, approx.  20 mm. o.d., 200 mm lon<;,
    with Pyrex glass wool plug at bottom.

    5.11  Kuderna-Daniuh (K-U)  glassware.

-------
                                  -3-


     5.11.1  Synder columns, three-bail  (macro).

     5.11.2  Evaporative flasks, 500 ml.

     5.11.3  Receiver ampuls, 4.0 ml, graduated.

     5.11.4  Receiver ampuls, 2.0 ml, graduated to 0.01 ml from 0.30  to
     0.00 ml.

     5.11.5  Ampul stoppers.

     5.11.6  Beaker,  250 ml.

     5.12  Microsyringe,  10 ul.

     5.13  PC3 mixtures (Aroclor) standards as mentioned in 1.1 above.

6.  Extraction of Sample

    6.1  Add about 20 gms sodium chloride to a separatory funnel  (5.2) .
    Transfer about 1  liter of water sample  (measured exactly) .  Extract
    the sample twice  with 60 ml  of methylcne chloride-hexane  (15r- v/v)
    and once with 60  ml hexane.

    6.2  Dry the combined extracts by passing through a 10 era chromatographic
    column (5.8)  of anhydrous sodium sulfate (previously rinsed with  hexane).
    Collect in K-D flask.

    6.3  For trace quantities,  concentrate to 1.0 ml in 4.0 ml receiver ampul
    on steam bath, using dry N2  stream to reach a volume of about 1 ml.

    6.4  Transfer extract (rinsing ampul with 1 ml of hexane) to 2.0  ml
    ampul and  concentrate to 0.10 ml (100 ul)  using dry N2 stream.  For
    larger concentrations of PCD's use a larger volume of extract and/or
    operate the M.S.  at lower sensitivity to avoid signal saturation.

7.  Analysis of Extract by Computerised GC/MS

    7.1  Gas chromatocjraphic conditions.
    Use 6 ft.  X 2 mm  i.d.  glass  column, packed with 3"- Dexsil 300 GC,  OV-1
    or OV-101  on GO/SO mesh acid-washed Chromosorb G.  Helium carrier gas
    flow rate  of 20 ml/min.  inlet, (resulting in about 1.5 ml/min. outlet)
    is used.   The coJ umn Lcmj>eraturo is proqra::',niL'd fc) 10°C/min. from 150-2tiO°C
    (OV-1 coiled coli:i-.ui)  on from 175-JSO°C  (IVxsil 300 GC U-tubc) .  Charge  3 ul

-------
                                     -4-
    extract.  Allow 75  sec.  for  solvent  to elute.  Turn on  RF  &  ionizer  i.
    start collecting data.   Methane  (750 u) is  the carrier  gas  for  CI  MS.

    7.2 E.I. Mass Spectrometer Operating Conditions
    70 ev. electron energy
    -2200 V continuous  dynodc
    10~7 A/V sensitivity  (10~8 A/V if available)
    500"1" ua  (max) filament current

    7.3 E.I. Mass Spectrometer Scan Conditions
    Mass Range:  153-157; 188-193; 222-227; 256-261; 290-295;  324-331;
    358-364; 392-398.
    Integration Time:   50; 50; 50; 50; 50; 50;  50; 50
    Samples/AMU:  1; 1; 1; 1; 1; 1; 1; 1

    7.4 C.I. MS Operating Conditions
    750 microns methane reagent  gas  (optimize signal on MS by using  652
    amu of FC-43 on oscilloscope)
    -2200 V continuous  dynode
    1.0 ma filament current

    7.5 C.I. Mass Spectrometer Scan Conditions
    Sams as for E.I. (7.3).

8.  Qualitative Identification of ?CB's

    The presence of PCS mixtures is qualitatively assured from their ma=;s
    spectra and GC retention data, using the-molecular ion region for
    biphenyl (present in Aroclor 1221 and 1232)  and the molecular ion  isotr;.
    clusters for mono- through heptachloiobiphenyls.
    153-157 biphenyl 154M+ (El), 155 (C.I.)
    188-193 monochlorobiphenyls
    222-227 dichlorobiphenyls
    256-261 trichlorobiphenyls
    290-296 tetrachlorobiphenyls
    324-331 pentachlorobiphenyls
    35S-361 hexachlorobiphenyl
    392-398 heptachlorobiphenyl
    The theoretical peak intensities in these  molecular ion regions  are
    given in Table' A-2, p. 260 of reference 2.9  above.   If C.I.  (methane)
    is used,  the masses arc one greater then for E.I,.  Identification  of
    the particular Aroclor mixture or even several mixtures can be
    determined  by comparison with standards.

-------
                                  -5-
9 .   Quantitative Determination o£ PCI3' 3

    Once the Aroclor mixture present has been identified (e.g., as Aroclor
    1016),  a known standard is run and  a GC peak present in both  (such  as
    th a:-, largest 013 biphenyl in the case of 101G)  is used for quantitation
    fro;* total ion intensities in the 256-261 amu region.  In the case  of
    a mixture, such as 1016 and 1254, 1254 is first determined from a Cl^
    biphenyl peak not present in 1016.   The trichlorobiphenyl peak,
    mentioned above,  is used to determine the 1016,  correcting for the
    1254 contribution for that peak.  Similar approaches are used for other
    mixtures.
    A standard is run before and after  each daily batch of samples.  It has
    been found that the total ion intensity over the course of 8 hrs.
    varies  by about i 5 to 7% from the  mean.   (2 runs).

10.   Minimun Detectable Levels

     These  are given  in the Summary (3).

11.   Quality Control  Data

     In  order  to assure the validity  of  the analytical  results,  samples
     of  laboratory  potable water v/ere measured  into  1 liter borosilicatc
     bottles closed with  aluminum foil-lined  screw caps.   The water was
     then spiked with 1016 Aroclor.   The  PCB  mixture was  added as  an
     acetone solution.

     Results
                              PCB-1016,  ug/1
     Sample No.     Date     Added          Found

       B           8/21       0             <1

       L           8/21       5.4           6.4

       I           8/21       51.4           53

       H           8/21     446            447

       H-2         0/26       5.0           6.6

       1-2         8/2G       yi.2           83 . 5

       L-2         8/26       12.M           11.4
  Recovery
Per Cent of
Added Amount
    119

    103

    100

    112

     97

-------
     Triplicate samples collected at GIL '.-.'atcr Intake I on 8/26/75
     gave the following results:
                                                     PCB
            Station          Date Collected          ug/1

            Intake I              8/25/75             16
                                                      15
                                                      15

12.  Glassware Preparation

     1.  All glassware is v/ashed 3 times in an automatic washer,
     first with a detergent water solution, then twice with distilled
     water and dried.

     2.  All glassware is then carefully rinsed once with acetone
     and once with hcxane.

     3.  The drying agent, reagent grade granular anhydrous Na-,50^
     is dried for a minimum of 24 hours at 105°C.  It is kept at this
     temperature prior to usage.  Only materials used for pesticide and
     PCB analyses are kept in this oven.

     4.  The glass wool and the Na->SO^ are rinsed with hcxane and stored
     at 105°C.

                                              Si.
/•  ^ Si.     -   -. (•
    - ''^'^^
B.  F.  Dudenbostel
    Chemist

-------
           Attachment C
Determination of CO Emissions from
        Stationarv Sources

-------
S-i^i5&^i^v»^^J:*c^»^^'^'T*™'^'
vWi»V'",'tf£5*i°i'-? .Vr*#**4p*i~±> »p£5
•iZrSSSiSSSMi-caJ^SefeswtSS
   App. A
                          Title  40—Protection  of  Environment
   METHOD 10—DErmMETATiOfr OF CAJIBON MON-
    OXIDE EMISSIONS FROM STATION'AP.T SOUECE3

     1. Principle and ApTilica.bilT.ty.
     1.1   Pnnc-.pla. An intfrgratad or continuous
   gas sample la extra,cvecl from a sampling point
   and analyzed for carbon monoxide (CO) con-
   tent using a  Lull-type noadlsperslva Infra-
   red analyser (ND131)  or uquivalont.
     1J2  Applicability.  TbJs  method  Is  appli-
   cable  lor  the  determination, of carbon mon-
   oxide  emissions from  stationary sources only
   when  specmecl by  tha test  procedures  for
   determining  complla.nce  with  new  source
   performance  standards. Trie  test  procedure
   will  Indicate  whether  a.  continuous or  an
   Integrated sample  U to be used.
     2. Range and sensitivity.
     2.1   Sengs. 0 to l.OtC1 ppm.
     12  Sensitivity.  ;'.[[niznu.-n detectable con-
   centration la  20  ppm for  j, 0 to l.COO ppm
   span.
     3. InterjererLr.&s. Any substance having a
   ntrong  absorption  of liii'rored  energy  will
    it'-rfere  to somo  extent. For example,  dls-
   : Irnlnatlon ratios for water (H_O) and  car-
   Don dloxlda  (CO,)  aro  3.5  percent H.O  per
   7 \ pm  CO and 10 pi*_rc;ur.  CO. per  10 ppm
   CO, respectively, for devices  measuring La the
   ? 500  to 3.000 ppm  range. For devices meas-
   uring In the 0 to 100 ppin  raaco. Interference
   ratios  can be  aa high 3J 3.5 percent H_O  per
   25 ppm CO and  10 pen:enf CO,  per  50 pprn
   CO. The use of slllcv. gel  anc! ascarlte traps
   will  ajlevlato  the  rnsjo"  iDterfertrico prob-
   lems.   The  .tncB.-jij-Vi'd gaa  I'olumo niuat  b«  .
   corrected  u" the3« ti'apa a.re used.
     4. Precisian and accT/'ac-:/.
     4.1  Precision. The precision of most NDIK
   analyzers  la  approjil'raately ±-,2  percent of
   epan.
     4.2  .\ccv.racy. The .iccuracy of moot NDER
   analyzers  Is  upproxln.'a.t'-lT i;S  percent of
   span  af:er callbmtlon.
     S. Apparatus.
     S.I  Continuous sample  (Figure 10—1).
     5.1.1 Probe. Sca.lnjes.3  steel  or sheathed
    Pyrex ' glass, equipped with ?.  CJter to remova
   partlculata matter.
     5.1.2 Atr-c&oled  condenser  01'  equivalent.
    To remove any excels molitvtre.
      SJ2  Inte'jrc.ted sa.-m.pla. ("Fttf-jro 10-2).
      5^2.1 Probe. Stainless  stefl  or  sheathed
    Pyrei glass, equipped \vtth  »  filter to remove
    partlculate matter.
      5.2.2 Air-cooled  t.'ondt'-n.Ter  or  equivalent.
    To remove any excels molsci.iro.
      6.2.3 Va/rff.  Needle va.lv:. or equivalent, to
    to adjust now rate.
      3J2.-t Pump. Leak-free diaphragm  typ«. or
    equivalent, to transport  gous.
      5.2.5 Rate muter. P.otameter. or equivalent,
    to measure a flow  rungo  from 0 to  1.0 liter
    per mm.  (0.035 cfm).
      S.2.6 flexible  bay. Tjdlar,  or  equivalent,
    with  a capacity of 60 to 90 liters  (2 to 3 f t').
 LeaJt-t«3t the  baj In the laboratory  before
 using by evacuating b&g  with a pump fol-
 lowed by a  dry gas meter. When evacuation
 Is complete, there should be no flow through,
 the meter.
   5J2.7 Pitot tube.  Type S, cr equivalent, at-
 tached  to the probe so that the  sampling
 rate can be regulated  prcpcrtlonal to  the
 stack gas velocity when velocity Is varying.
 with the time or a  sample  traverse 13 con-
 ducted.
   5.3 Analysis (Flg-ure 10-0) .
   5 J.I Carbon  mononde andy-trr. Nondlsper-
 «l7e Infrared  spectrometer,  or  equivalent.
 This  Instrument  should  be  demonstrated,
 preferably by  the  manufacturer, to meet or
 exceed   manufacturer's  specifications  and.
 those described In this methcd.
   5.3.2  Drying tube.  To contain   approxi-
 mately 200 g of silica gel.
   5.3.3  Calibrction  gaj. Hefel'  to par^Ljrapb.
"6.:.
   5.3.4  Filter. As  recommended  by  N
 manufacturer.
              "Alfl-COOUD CCKSIKStff
     'Mention  of trade nnme? or specific prod-
   ucts cio«s not constitute endorsement by tlau
   Environmental  Protection Agency.
    53.5 CO. removal tube. To contain approxi-
  mately 500" g of oscarlte.
    63.6 Ice  water bath.. For ascarlte and slllcra
  gel tubes.
    5.3.7 Value.  Needle valve, or equivalent, to
  adjust flow rate
    5.3.8 Rate meter. Rotameter or equivalent
  to measure gas flow rate of 0 to 1.0 lltar per
  mln. (0.035 cfm) through NTJIR.
    5.3.9 Recorder (optional}. To provide per-
  manent record of NTJIP. readings.
    6. Reagents.
                   a

  8.1 Calibration gas?
of CO  In nltrozen  (K
prepurt3«i grade of N
tlonai  concintritlonj
mately to 80 percent a
span concentration si
the applicable source
The calibration g^se'
the Ennufactnrer to
of the specified concer
                                                               6.2 Silica gel. Indict
                                                             djrled at 173- C (347' :
                                                               63 Ascar-.te. Commg
                                                               7. Procedure.  -  ~
                                                               7.1 Siimpliny.
                                                               7.1.1  Ccm£tnuo-uj
                                                             equipment  as siown
                                                             sure ail  connections
                                                             probe  In the 3tacS a"
                                                             purge  the saxnpliig
                                                             lyier  and  be^Ln  dra
                                                             anaJyzer. .\llow 5 —
                                                             to  stabUlrc. thea  -K
                                                             In; as required by  '.:
                                                             \ ~,3. and 8). CO,  con
                                                             deterrr-ined  by  uslns
                                                             grated sample  prooec
                                                              Location	
                                                              Test	
                                                              Data	_	
                                                              Op«rator	
                                                                            '   Ctoc'
     9. Calculatio-n—Ccr
   monoxide In the stock
   where:

-------
jr.p fol-
..-ua'.icu
•.'.irougb,

eat, at-
i.-r.?ltng
 to tie
T~7!r.;
^ con-
--.rated.
-e»t or
pprcxl-

 i— apb.
                               -environmental Protection  Agency
                                                                                                      App. A
  6.1 CzU&ration fa.-;es. E^own concentration
c' CO In nltrogaa (K,) ;or Lasmimenc spaa,
prepuriaed ;jr&as of N, for sero, aad two eddl-
tioaal concentrations corresponding approxi-
mately to 60 percent and 20 percent spa-a_ The
apan concentration s£all not erci?od U times
tne applicable source  performance standard.
The  calibration  gtaes shall bs cerslflod by
tha manufacturer to  be  within ^2  percent
of the specified coacenrraUoo,
                        6.2 SiJles gel. Indicating 'type. 6 to 16 mesh,
                      dried at 175° C (347= P) for 2 hours.
                        6.3 .-\scctr.te. Coromerciaily available.
                        7. Procedure.

                        7.1.1  Continuous sampling.  Set  up  the
                      equipment is shown In Figure 10-1 mailing
                      sure all connections are leik "ree. Flacs the
                      probe lr. the staclt at s sarapllng point imd
                      purge  tto  scjapllng lino. Connect  the  ojia-
                      lyzer  and  begin  clra?rlng sample  Into  thet
                      ar.alyzer.  .Vllow  5 minutes  lor  tns ay3tem
                      to sr.abUl^a. then record the onalf^er  read-
                      ing as required by the  tost  procedure.  (Sea
                      t 7.2 and 8). CO]  content of ths gas may be
                      determined by using  th8  Method  3  Inta-
                      gTn.t?d ssunple procedure (38 FR 124883), or

                                                             10-1.—Field
by  weighing the aacarlto  CO, remoTaJ tnb«
aild computing CO, concentration  from tha
gaa  volvms  wunpusd  and  the weight gain
or the tube.
  7.1^2  integrated  sampling.  Eracruats  the
fleilbls bag. Set up the equlpmant  aj ihowrx
In  Hgvjre  10-2 vrlth  the  bag disconnect^.
Place tb.8 probe In the stack aad purge the
sampling lino.  Connect the bag, making JUT«
that Ell coD-cectloos ara leaJs Iree. Sample att
e,  r&ts  proporHonsl  to the Etaci  velodty.
COf coatees ol the ja^ may be  determined
by  xislng this  Method 3  Integrated  samplo
proccdurtss  (38 KR  248381, or by  weighing-
i^he ajicajlte  CO. removal  tuba  and comput-
ing CO3 coaccntratlon ircd the  gas voluxna
samplad tuaci tha weight gain ot the tuh«.  _
  7.2 CO -inaiusl?. Itsscdble tha apparatus aj
shown la Flijuro 10—3, calibrate  the  Loacru-
mant, s^d perTortn other required
aa  descrtlMd In paragraph 8. Purso
with ND prior to introduction ot each
DLreer, tie sample stream through the Instru-
ment for Che teat period, recording the read-
ings. Check; the zero a.nd span again EJ.'ter the
tesc to assure  chat any drllt or mail unction
Is detected. Record tha sample data on Table
1O-1.
   8.  Calibration. Assembls tha apparatus ac-
cording to Figure 10-3. Generally an Instru-
 monr requires s warm-up period before sta-
 bility Is obtalnad. FolloTu  tte manufacturer's
 Instructions for spoculc  proceilur^i. Ailo-cr  a
 minimum time  of one  hour for  warm-up.
. During  tills  tlma  check  th®  sampla  condl- _
 tlonlng apparatus. I B.. alter, condenser. dry-
 Ing tube, and CO, removal tube,  to  ausure
 that ciicci  component Is In good  opermnlngr
 condition. Zero and calibrate tno laatrumont
 acoordlricf to tho mucuiacturer'3 procedures
 using, respectively, nitrogen and the callbra.

Test - -,-~™.- - .«



Clock tim@

„ 	 , „„ 	 ,„_„_...„ „ Commep.t5:




Rotamctgr setting, liters per minute
(cubic feet per minute)

                                                                                                    I
                                                                                                    -a'
 il'.lca

 •t. to

 •I'etJt
 • per


  per-
   9.  Caicnilat-ion—Concentration of cartxtn monoxide. CaJculat® tha concentration of carbon
 moncxlc'o ta tha stacS usLag equation 10—1.

                               Ccootooh = C'coKDja(l~Fcoj)                equatioD 10-1
 where:
      C
-------
App. A

10. Bibliography.
10.1  McElroy. Fran*. The Intertech NDtB-CO
     Analyzer. Presented  at  lltii  Methods
     Conference oa Air Pollution, University
     of California, Berkeley. Calif, April  1,
     1970.
H0.2  Jacobs, M, B., et al.. Continuous Deter-
     mination ot  Carbon Monoxide-  and Hy-
     drocarbons In Air by a Modifled Infra-
     red  Analyzer, J. Air  Pollution Control
     Association, 3(3): 110-114. August 1959.
Title  40—Protection  of Environment
                      10.3 MSA  LIRA Infrared Gas  and  liquid
                          Analyzer Instruction Boot, Mine Safety
                          Appliances Co., Technical Products Di-
                          vision, Pittsburgh, P».
                      10.4 Models 21SA, 31SA, and 41SA Infrared
                          Analyzers,  Beckcua Instruments, lac..
                          Sec&man Instructions  1635-B, Fullsr-
                          ton, Calif.. October 1367.
                      10.S Continuous  CO   Monitoring  System.
                          Model A5511, Interteca Corp.. Princeton,
                          NJ.
                      10.8 UNOK Infrared Gas Analyzers, Bendir
                          Corp., Ronceverte, Weat Virginia.
                                       ADDSNDA

  A., ferjorma.net Sptciflcziiona lor ffDIR Carbon Monazide Analyzers.

Rang?  (minimum)	.	  O-lOOOppm.
Output  (minimum)	  0-10mV.
MlaUsiiin datectab'.B sensitivity	  20 ppm.
PJsa time, 90 percent (maximum)	  30 seconds.
*:I1 time, 90 percent (maximum)	  30 seconds. -
2; ro drift (maximum)	._	  10«J in 8 hours.
Sp?,n drift (maximum)	  10% in 8 hours.
Precision  (minimum)	  :£ 2% of full scale.
No)-a (maximum)	'.	  :£ 1% of full scale.
Ll.aea.risy (maximum deviation)	  2% of fxUl scale.
Interference rejection ratio—	',—':	  COr—1000 to 1, H:O—500 to 1.
  B. Definitions of Performance Speeiftea-
t>'>rw,
    • .n'jc—Tie  minimum  and  maximum
BI :i..:arerucnt limits.
  Output—Electrical signal which 13 propor-
tional to the measurement; Intended for coa-
incCon to readout or data processing devices.
dually expressed as millivolts or mllllamps
full scale at a given impedance.
  Tull scale—The maximum measuring limit
tor a given range.
  Minimum   detectable   itnaiiivity—Tha
smallest amount of input concentration that
can be detected  aa tie- concentration ap-
proaches zero.
  Accuracy—The  degree of  agreement .be-
tween  a measured value and  th» true value;
usually expressed as ± percent of full scale.
  Time to 90 percent response—The time in-
terval from  a step change In the Input con-
centration at the instrument Inlet to a read-
Ing of 80  percent of  the ultimate  recorded
concentration.
  Rise Time (30 -percent)—Tho Interval be-
tween  initial response time &ad time to 90
percent response after a step Increase in the
inlet concentration.
  fall  Time (SO percent)—The Interval be-
tween  Initial response tlrae and time to 90
percent response after a step decrease In the
Inlet concentration.
  Zero Drift—The change In Instrument out-
put over a  stated  time period, utually 24
hours,  of  unadjusted continuous operation
whoa th» input concentration Is zero; usually
•ipremd u percent full »cal«.
                      •  Span Drift — The change in Iristrument out-
                      put over a  stated  time period, usually 24
                      hours,  of unadjusted continuous operailon
                      when the Input, concentration  Is a  stated
                      upscale value; usually expressed as percent
                      fall scale.
                        Precision— The degres of agreement be-
                      tween  repeated  measurements of the sane
                      concentration, expressed as the  average de-
                      viation of the single results Iron the ms&n.
                        A'oiis — Spontaneous   deviations   from  a
                      mean output not caused  by Input concen-
                      tration changes.
                        Linearity — The  maximum -deviation be-
                      tween an actual Instrument reading and the
                      reading predicted  by » straight line  drawn
                      between upper and lower calibration points.
                      MTTHOO 11 — DrrsjujDiATiojf or srnsoGsif strv-
                        ITDt EMISSIONS FROM STATIONAaT SOU3CT3
                        1. Principle and. o
                        1.1  Principle.  Hydrogen  su!2de  (HJS)  Is
                      collected from the source In a series of midget
                      Iznplngers and  reacted with  alXallne cad-
                      mium  hydroxide  (Cd(OH),]  to  form cad-
                      mium  sulflde  (CdS). The  precipitated CdS
                      is  then dissolved  in hydrochloric acid and
                      absorbed- In  a Jcnown volume of Iodine solu-
                      tion. The  Iodine consumed Is a measure  of
                      th» H,S content of the gas. Aa implager con-
                      taining hydrogen peroxide is Included to re-
                      move  SOj  as an  Interfering species.
                        U Applicability. This method  Is applica-
                      ble for the  determination  of  hydrogen rul-
                      flde emissions from stationary sources coly
                      wh«n  specified  by the test procedure* for
                                          96
                  Chapter  I-
            compliance .
pertortaance standards,'.  C'",T.
  2. ApparatiiS.        '.
  2.1 Sampling train. :.•;.-**• ""
  2.1.1 Sampling line — 6- to 7-r
Teflon l tubing to connect sara;
sampling valve, with, provision
to prevent condensation; A pr
lag valve  prior to ts* Tefloa :
may  be required  depending'
stream, pressure.
  2.12  Impingen — Five  rnldgs
each wttix 30-rrU capacity, or eq-
  2.1J Ice bath, container — To
sorbiag solution at a constant tt
  2.1.4  Silica  eel  drying  tube-
pump and dry gas m»c«r.
  2.1 J Needle raise, or equizaie
steel or other  corrosion reslstaa
adjust gas flow ri:c.
  2.1.8 Pump — Leai fre«, dlapb-
equlvalent, to transport  gas, (
If sampling stream under posit:
  2.1.7  Dry gas -rr.eter — Su£c!e:
to measure samp:*  volume to •
cent.
  2.1JS Sate meter — P.otaniater, ;
to  measure a Cow  rats of 0 tt
minute (0.1 ft'/min).
   2.13 Graduated  cylinder — 35
   2.1.10 Bcrometer — 7o m«»»ure
pressure  v/ltMn s^J ^-" (0.1
   2.2 Sample P.ecovery.
   2^.1 Sample container — SCO-::
 pered Iodine  Cask.
   2.2.2 Pipeite — 50-ml  volume t:
   2.2.3 Beofcers— 250 tal.
   2^.4 Wash  hottlf — Class.
   2JJ Anctyra.
   2.3.1 Flask— iOO-=i glaw-sto:
   2.3.2 Burette — O=.s 50 ml.
  "2.3.2 Flask — 125-mi coriical.
   3. Ssayents.     .   •- ••- ......
   3.1 Sampling.
-  3.1.1 Abiorg-ing  solution — Cc
 droxloe (Cd(OH>.)— Mis 4J g c
 fato hydrate  (3 "cdSO,.SH,O)  :
 sodlura hydroxide (NaOH)  1= 1
 tilled water (E.O) . Mis well.  .
   Note: The cadmium hydrozl;
 this mlrtur* will precipitate as
- pension. Therefore,  this solut'.
 thoroughly mixed before using
 even distribution of the cadmiu
   3.1— Bydrogen peroxide, 3 per
 30  percent hydrogen  p*roslde
 as needed. Prepare fresh, dallr;
   3.2 Ssmple recovery.
   3^2.1 Hydrochloric acid soluti
  percent  by weight — mix 230 =
    'Meatiou of trade nimes or s
  ucts does uot constitute eudors'
  Environmental Protection AgeBw

-------
               Attachment
Gas Analysis for C02/  02/ Excess Air, and
           Dry Molecular Weight

-------
4.17BS
-RULES AND REGULATIONS
                           3.  Shirrharv R. T.. W.  F.  Todd. and  W. S.  Smith.
                         Sl^ruliconcfl ot Errors in Stack Sajnplioi Mwmjurameau.
                         U.i.  EaviroixmeiiLa* ProuKUua  Araacy,  i>*»&rca
                         Tn*n*la Part, N.C-^PreMQtwl at tb« Annual Mmumot
                         tn«  ALT PoUutioa Coocrol  Association, SL  Loon, Mo..
                         Jui» 14-iu. lorn.;
                         - 4. $ciaf
                         Vert  Joha tVileyuid Sona, lac. UM7.
                           ft.  fluid  iUtera — Their  Theory  und  Application,
                         Amancan 300*17 °f M***fa*-""^J Eocine«o  N«w Yon
                         N.Y. 1WO.
                           T. A3HRAE Hindboot of Fur*iamtauli  1077, p. 2S.
                           ft  AAnnai 3oa* o/ AiTM Standards, Part 2L  ly'-L p,
                         W V.
                           •).  VoUaro. R, F. Oojd*Un« for Tyr» 3  Pilot Tub*
                         CoDorouon.  C.S. EnnronmftntaJ Protection Agency.
                         Kee*A.-cb  TiAn*tficaenL C 3.  Envtrorunaatol rroiectloa \««TICT.
                         ZrnJsioa  Measure mem   Brincti,  R*>wj-cn  Tnan^U
                         Parr,  N.C. October  lOTti.
                            11 VoUaro. P.. F.  EstAhlrstunwt oJ * Sueliru Co«ffl-
                         citnt  Vslua (r>r  properly  Conjtruct*d Typ* ^  HI tot
                         Tuoea. U.S. Enrirorunsntal ProtcruoQ Air 1976,
                           11 VoUaro,  R. F  Ao Er&luAtlon of Siaglfl-V*locily
                         CabTpraoon Techniqaes aj a Mania of Det&nmnlug Typo
                         8 Phot Tut* Co«ffic:enti.  C.3. EnTirooroftauil  Protrt>
                         M"" A^dncy. Eaission Men5ur^tD«Qt Branch, R«Aafcii
                         Tnar.el«  Part. N.C. Amrujt 1975.
                           It Vollaro. R. F.  The L"» of Typ« S PItot Tub« toe
                         the Measurrment of Low Velocities, O'.S. EnviroameotaJ
                         Protect! OQ  Agency,  EmissioD Mw^suremftot  Bnuica,
                              «Jch Tnanji^'Parfe. N.C. Nov«mb«r 19 T6.
                               SmiLh, Marvin L. Velocity CaJibranon of EPA
                                Sourc*  SompUnz  Prot>e.   Coited  Technologies
                         Corporauon,  Pratt  and   Whicooy  Aircraft
                         East Hanlord COOTL 1371. -
                            16. Vollaro. R. F. Rtcarm: ended Procwia
                         TT^versea LD DTICLS sanller than  12 Inches in Diametw.
                          U.S.  E D TITD OIE e n tiU  Protect too  Agency,  Eoussroti
                         N'ea^ojBmeni Branch. P.esoArcii Tnangia P*ft, N.C.
                         NoTBtnb«  197TI.
                            17. Over. z. and R, C. PaakbnrK- The
                         of AiJ Flow. ^Lh  Ed_, London. Penramon Press.  1
                            13. VoUart>, B-  F. A survey oi CornrnerclaUy Av
Prob**,  PrepfLred by c
MIOULTT o.'  Ui«  EQTir
                                    ni"s. U.S. Es'Tr?cn2eQLaJ Prorectlon Aeencv,
                                    it«iscj-?aa*tic  Branch.   Res^arcfi   TrlangL*
                                                   .
                                       ^ "*'- C- C. S\.  Pierre,  D. S. StnjLh. D.
                                       .  &MUMT. Ai Ejp*nm«aL4J
                                              UoIvenitT o^ Wtndjw for tit
                                             msnt, Toroaw,
                               3 - OjJ  X**AJ.T3»  rOB
                       l.l   Prlnrlpla. A cu y
                     by  on«» of ii>* following
                                                  U ul
                                                             Crora »
                                r OercBUt carbon dloEd« (COu, p»irceJit ciy-
                     Cea  iO:>. and. i/  necRtsary.  rrotnt  o»rcM>n c3oaoi_!d«
                     (CO).  U B dry mowcuiw weig.it ddUfnircaUoa Li to b*
                     cxftda,  p4Lh«ir in ur»t or ft FTTHO ' aaaJ> ter 01*7 b« awd
                     far tb« anjJysLJ: (or imress *ir or cnxuAioo nc* correcuoa
                     factor drUrnunuLioa. *n Orso-i wiaivter tnujt N* ir«t*d.
                        IJ2   App.icabuKj-.  Ttuj  mecaod is  ayplic^bl* lor d*-
                     tcrmioJns  COi ind Oi coacejatnLioas, »ic«» MT, ami
                     dry mouictiJjLr "Mffbt of ft wmipl« Lmm a s&j scrnaon o^ a
                     loull-ioeJ corobuJUoQ procwa,
                     topUcuiDU looi-ntr -TTXAUM vh<
                     inat compountlj och«r U^MI COi. Oi.  CO, and -
                     (Nt) ire  uot  prasent la  coact ntnuioTn  jmaa«uU  u>
                       (jcnfr meiiio«l3. 04 wall xi niodiflcucionj Uy Lh*  prtx»-
                     dur» described  hartin, ar* a no appbcauu for irrcJ? or \J
                     of cb« »oov9 - J « c< rnLLoa d o nj . EtamD'** of sp#-nXio  ouO-
                     odj and aiodliiisiuoaj mcluo«. 1 1) a  miua-rxwnt.  ^*cnp*
                     Un<  en i* i bod  asan  to  Oni»L  anjjJyier  io  »raUTTc tndl-
                     vidaaJ ^rxb samplrt ootaaawi at c_j*^i r
                     temj described  ber*ia. oubcr iimpboz  jy^Kerru (c.t-
                    , liquid displiictmeni) m^y b« ui«*d pro»id&d sucn 57*1*033
                     a/«  capabl* of obtainun?  a  rspreieQCiUvu 5ajno<« wid
                     nmintainmj a coruujiL sampunsf rate, and are OLQtrwTa*
                     capaiils ^of  yieJdia?  iccspt-ibla rasulLi.  L's* of  sucn
                     Tysiemsla yublwt LO ttio approrii of tbe Ad-miTLUUTiLor.
                       i.1  Grai) SajnoLuiij r Fiyxira 3-1).
                       2-1.1  ProtM. The prob« sooold  b*  rasda of yta-olesm
                     nael or boronit\cn.Le pLa^s lubuix and sbotud b-» «gmpp*d
                     wnb an m-itaci or om -a Lac It fuuer LO rBmor^ pan.cui*u>
                     raaLLar (i piu^ of glass wool is saujfuctory lor LQU our-
                     ' po»). Aoy other ciflLeriAi iaen LO Oi,  COi, CO. and  Ni
                     and re^utant to tomFwracuj-B at iArnpiuut condiuoru may
                     b«  used  for  the  probe; ammpios  o/ ruch
                     aJurojnuia. copper, qaaru gbiiJ and Tflilon.
                       J.I.- Pump^ A  orse-way 5Cjue«i9  oulb,  &f eq
                     b used io imcLspon -.ha £us  saxapis  io  the
                       2.2  lnte
-------
                               RULES AND  REGULATIONS
                         PROBE
                                                 FLEXIBLE TUBING

                 FILTER (GLASS WOOL)
                                     SQUEEZEBULS
                                                                        •TO ANALYSER
                                  Figure 3-1. Grab-sampling train.
                                                 RATE METER
          AIR-COOLED
          CONDENSER
PROBE
    \
        FILTER
     (GLASS WOOL)
                                            VALVE
                                                 QUICK DISCONNECT	*-Tj

                                                              :	W.
                                       RIGID CONTAINER'
                                                                            BAG
                           Figure 3-2. Integrated gas-sampling train.
                   KOERAJ. JtWISTU, VOL. 42, NO. 160—THURSDAY, AUGUST 18, 1977

-------
 41770
                                                           RULES  AND  REGULATIONS
  2.2.2  Condenser. An air-cooled or water-cooled eoo-
 donser.  or  other condenser  tnai will aoc rrmOTa Ow
 COi, CO. and Ni. may be used to retno»« eiees matenn
 which would tatafcn with UM operacua ol tae pump
 tad flow meur.         — ••-.•
  2.2.3  Valre. A aexila T«in Is eod to adjust 3»tnpt»
 pu flaw ra(«.   '          •  —
  2.2.4  PTIIBB. A  v»*-« pump. «
 tquiTalwu. Is us*d  to transport sample «»u u> in« flexible
 bat. IruLAU a small snnte unk b*r»een tn» pump and
 ran :net*r  to «iirainate CM  oul»Uon eJltnl ol to* di*-
 phrmrni pump on the rotarneur.
  :.2J  Kau Meter. TH« rotaaeur. or eqolretant rate
 neter. nwd ihould be raoaoie  ol measuring Jo" nit*
 u> within 3:2 o«e«ni of ire j»l««t«d iH» rat*. A low
 raw ran»» or JOO to HHMan'/min is jiii^rsi«i.
  2.2.8  FlttibU Da*. .Ml? lea*-lr«» pi»J"c " z.. Tfdiar.
 Mylar. Teflon) or piasuc-coaKd  aluminum '•?•!.. alumi-
 num Mylar)  bat:. or •wiuirnient.  ha^iru  >  capacity
 p>-,;:junt with, the selected  flow rate and time Icnjtn
 ol t.ie lot ran.  may be osKl. A capacity in <°« ""»!• °<
 U w •» uten Is surctsud.
  To leak-cheek the oac. connect It to i water manometer
 ind prwnmif the o« 10 J to 10 eta K:O ''.• to 4 la. ErO).
 AJUrw to st»n* dry molKular
                                                    tadjcaud ui o«ctloo A i.
                                                      3.2A  R*p"«i UM anaiytiA and calculadQn procadtina
                                                    cnUJ tb* uidinduai dry molecular wwc&u for &ny t^r««
                                                    analyau diller (roui loetr  tnaan  by oo caor* Uiaa  OJ
                                                    Z.'1-moie (OJ IbAb-moUl. Ann<« theae UXTM coUcubw
                                                    weittbu. and rapon Uio ranilU to Ux ncanm 0.1 ti-ox»«
                                                    (0.1 IbiltxaoU).
                                                      3.3  Multi-Point. IntefraUd SampUof aod Aoalytxal
                                                    Prwudun.
                                                      3J.1  Oolwi  othanrtM  rwciUed  by tb«  Adalnl>
                                                    traxor, a DUnimam of «ltbt tr«v«r9* pointi isiu >t uvd
                                                    for clroular slack* bannf diamcun leo tb«o 0.61 in
                                                    (14 tn.). a mmrmum o( nine sbaU be 03*^1 for rectACjralar
                                                    nacka  harms, tqamltat  dlaaeun  \a*  U:an O.S1 a
                                                    (24 in.), and a nmitaum of twelve cravtne poinu 3ball
                                                    be cuvd (or all otbtr c«Ma..Tbe tnvarM poinu snail &•
                                                    located acoordinc to Method 1. .Thr tue of fewer POLCLI
                                                    U mb)eet to approval ol tbe AdaunlJBUtor.
                                                      3.3.2  Follow th« priccdnrae cxiuined In  Sec do as 3J12
                                                    through 3JJ, ticrpt >'nr the loUovnnc tranne all mat-
                                                    pUog poinu and saiapU at *acn point (or an equal lea^tJl
                                                    o( tiiaa. Record umpUn| data ai jnown la Fijian 3-i.
                                                                                                                     Ran CarrniJM fnOtr or Ezcttt .\tr
                                                      NOTC.— A 7yriu-trP* oomborooo m analyiar la not
                                                    arrnririi-U* lor urm u or eoiuaoa rau corr*cuon bcior
                                                    ^^JT^jp^^i^miliae aopravtd by tba  Administrator.
                                                    II t>ot&  percent COi anti p«rr«ot Oi are aaeaatirad. tbe
                                                    aoaiyueal remlu of any oi the tbrm prtrmlorm
                                                    beio-w nsay auo b* osed i
                                                      £»ch of the three pnxadara b«low ^ball b« aand only
                                                    whfn vp^tiijifd in an applicable wbpart u/ th* standard!.
                                                    Tbe OM of tbwe procetrunw for otner purp«M>« tnuil b**e
                                                    rpeeuta pnor aoproTul of toe Adniiaiatnior.
                                                      4.1  ai04le>i'ouu.   Grab  SampUAf ami   AnalyUcal
                                                      4.1.1  The mmpllnt point tn the dact ihaJl tfthir CM
                                                    at the eanrrotd of tne cruen^fcuon or at a point DO eloaer
                                                    utnewaiUtt-.^r. 100m uufu.onleaiauierwuxpeculeil
                                                    by the Adau:iutr%uur.
                                                      4.1^  3«t up tbe equipment M ihovrn In Fliun 3-1,
                                                    ^•'^irt sure  all ooonectionj abaail o< tne anjuyier are
                                                    l^bt aod KMl-trr*.  L>*eJ«nKK tne Orau aoalrur *a-
                                                    oorrluK to Ue proetdur*  de»enb«l la 3*oioa  V. Ttuj
            tr»yi ^i-c.
            u.  For Oral mi Fyrita ir JT"» rnaln-
         u opuration proc«du;-t». taUo» t j« instnicQooj
«comm«nd«l by  th»  cifloulJctnrw, Uilaa  olbertnai
srv«'iflet». ia» meajunm burttt* o«
' tin O.tot muK t»«\ »: i^ast 0,1 paroent
   Asy <•' *.t» tnr« sampta« »n« b»
 H tb< fcntroiU o/ -Jw CTWJ section or i: » point no eJo**
 to tilt "nUa ^s»a 1.00 m J 5.3 ft ). unUaa otbenru* ip»di*l
    t>   aun.                      _
    1.2 6*t up tt* »qalr=<«B M lixnrn in r*tnr»
    lojif sure ill coimcj-303 »h««d by
followinj tbe procedure ia Section 4: hoireYW. Uu> leak-
check Is optional.
  3 1J  Place t--.e probe in the stack, wittt tbe Sp al tha
probe poji'.iooed al Ue sampling point; purge the sasipt-
ins  UneT Draw a sample into :b«  anAlyter and Imme-
diately analyr« l« <°r P«reect COi and percent Oa, Deur-
mine Uw percentage oi the gas Out u Ni and CO by
subtract!:,* the sum of tbe percent COi and  p*rcan: O»
torn 100 percent. Calculate Use dry molecular wej*ht aa
Indicated in Section  8.3.
  3.1.4   R«p«: tbe  samplias, analysis, and calculation
procedures, ur.til the dry moiecular i-eijats of any three
crab samples  difltr  frora tlwr mean by no  more than
0 3 iVs-tnoie (0.3 Ui/lu-mc4*). Average these three molec-
ular weijh'j.  an-;  r-port  tha  results  to  the nearest
01 t/z-mole (Ih/lb-r-.ole).                 .    .  ,   ,
  3.2  Sinfle-Point.lnietrated Sampling and Analytical

  S.l; "rhe sampling poll' ta the duct shall be located
  "IsS^tcakihuck  (op'tTonal)  the  fleiible ba?  as In
  Section 2i«. Set up ihu equipment as shown in '-jure
  3-2. Just  prior to  sampling. leak-check (.optional)  the
  trtla by pLtcins a Yar.uu.-J cauee at the condensw ir.let,
  pullinit »  Yuc'jum  ol at least JM mm Hz (10 La. Hg),
  plugging tbe outlet at the  quick iiscor.nect, and then
  turnins ol the pan?. Tbe taciturn, should romam stable
  for alienator nunuu. Eracua'.c tbe£e.tibU: bag. Conn«t
  the prnb- and place it in the stiC*. with tbe tip ol the
  probe poj'.uoncd at tfte sampling pntnr purie the samp>-
  irj Ui.e. X*it. cof.r.-ct the bi? and calM sure that all
  connections are ti!'i: und l<^lc te«-
    323  Sample »•. 4 constant rale. Tbe samBUrjt  run
  soould be simiUianteus  with,  and for  the same total
  >r,etb of ti:n° u. the pollutant emission rate determina-
  tion. Coilo. '.-..-.n of at l<-ast 30 Uten (1.00 ft') of sample cas
  is rtcorv.n: -v.JjU:  hownYer, smaller Yolume*  may be
  coll'-.'Ud. ;f desired.
    3.2.4 Obtain one Integrated  Rue gas sample anrlnc
  eacb pullutant  e;ni5-ion rite dciermitiation.  Within 3
  h'nin afur tae simple is inktn. aiialyte it lor percent
  Cf)i ind  rwrcfnt 0; uSitiB citm-r an Orsat anilytcr  or a
   Fyrite-type comtristiun  gas analyzer. If an Orsat  ana-
   lyser 15 used,  it is recommenced that  th* Orsat U-ik-
   i-~-t rt»!u-ribed In  Section i be fwrfi-rmi-d l>»!'»re  this
   Oftcrmuuuon:  howeYer. th? rhiv k i;  optional.  Deter-
   t£iDeth» r^rcrnxjp of the zas that \- N':ar-l CL>by  suS
   U*.iing tlie sum of the percent CO  »:.u percent Oi
TIME




TRAVERSE
FT.




AVERAGE
% 0 E V "* " 1 •a^aw^.nwaw^ne. ) 1 HQ /
\ n awn / *
Q
1pm





MUST BE < 1*0%
%DEV.a





                                                                        Figure 3-3.   Sampling rate data.
  4.1 J  P'.oc* the probe In tbe i tack, with the tip of th»
probe poallloned at tbe sampling point: ptme toe sao-
ruin^ Uoe. Draw a sample Into tbe analyzer, for emission
rate correction factor determination,  immediately ana>.
lyre tbe sample, as outlined m Sections 4.1.4 acd 4.U.
for percent COt or percent Ox, If eicess clr Is desired,
proceed as follows: (1) immediately acajyte  the sample.
as la Sections 4.1.4 and 4-l.i. for percent  CO;, Oi. ar.d
CO: (2) determine the percentage of  the ms that Is  Ni
by subtracting tbe sum. of the percent COi,  percent Ot.
and percent  CO from 100  percent:  and  (.:> calculate
percent eicen air as outlined in Section i.2.
  4.1.4  To ensure complete abaorprJon ol tbe CO-. O-.
or IX applicable. CO, make repealed passes through each
absorbing solution ontil  two consecutive  msdio^s are
the same. SeYcral passes (three or (oorl should b» =ade
between  readings.  (If  constant readings  cannot  be
obtained  after tuc.e cocoecuttYe r»iJ2{3,  replies the
absorbing solutlim.)
  4J.S  After  tbe analysis   Is  completea,  leak-cheer
(mandatory) the Orsat analyzer once ajain. as ducribtd
In Section 3. For the results of tbe analysis  to be ralid.
the Orut acalyter must pass this leak test  before and
after tbe analysis. NOTE.—Since thU sinil*-poisl. ?rab
sampling and analytical procedure is normally conduct**!
In conjunction  with  a single-point, grub sampiiag »ad
analytical procedure (or a pollutant, only one anaiyrts
is ordinarily conducted. Therefore, yreat cart nsust w
taken to obtain  a Yalid sample and analysis. Although
In  most cases only COi or Oi is requind.  it is recom-
mended that both COi and  O: be measured, and teat
Citation  J in tbe Bibliography be used to Yalidau the
analytical data.
   4.S  Sinslo-hoint, Intejrated Samplinj and Aaslr:I»l
Trocedurp.
   4.2.1  The sampling point ia the duct shall oe loca:^4
as specified in Section 4.1.1.
   4.J/J  Lenk-chrck (mandatory) the fi»t:b!» ba»_as 13
Seciion 2.'J.«. S'"t up llie e'iui|im*nt as sho'*^. .^  7;?ir*
                          '  U
                                 the coa-1-rti^r ir.lr'..
                                 im Hg (10 J. Uti.
 filugj;ng  tte cutlet it the quick disco&aect, isi ^«a
                                                      beciion :...». S'"t up me e'luipmem u
                                                      3-2. Just prior to s^inplinc. le:vii-chec«
                                                      tnin by pLacinc a Y^'imn: cau?K at t!n
                                                      pullinj a YKuun of n'. least i*> rim
' tcrclag oC the pomp. The. ncrona shaQ remain (table
 for at '.east O.S minnu. E-ramta toe UailbU be*.  Coo-
 nect tbe probe and place i: in t.Vstsck, mthlhe Upof the
 probe positioned al the sampuru point: puro the  sam-
 pling Una. Next, connect the bag aod  make sera  thai
 all connections are tijrht  and leak free,
    4.2.3  Sample at a constant rate, or u spectCed by tbe
 Administrator. Tbe sampling run must be simultaneous
 imh. and lor the same total length of time as. the pollut-
 ant rmialon  rate determination. Collect  at  laait 30
 liters il.OO ft') of sample gas. Smaller Yolumes  may be
 collected, subject to approval of the Adminisinuor.
    4.2.4  Obtain one intrgrated iue gas sample during
 each pollutant emission rate determination. For emission
 r*-* crrr*cuon tsc'-or determination, analyze the sample
 Tl-.hia 4 hours ahrr U is taken for percent COtor percent
 Oi (u  outlined ia Sections 4.2J  throuj* 4.1.7).  The
 Orsat-analyzer mnst be  leak-checked (?re Section o)
 br'ivre the analysis. U excess air is d6*ir>?d. proceed as
 follows:  (1) »-ithin 4  hours alter the sejnple Is taken.
 aaalyie it (as in Sections 4.2-S through 4.2,7) tor percent
 COi Ot and CO: (2) dttensiine ;he peroatage of tbe
 fasttatisNibysubtractru thesumotths percent COt
 p^wtt O-. asd p»rwut CO fr?m 100  percent; (3) c»l-
 cu!»:e prcent ?i:ess air. as outlined ia oevtion 6.2.
    4.2.J  To ensu-'» complete absorption of tbe COt. Oi.
 er if appucable. CO, make repeated passes  through eacn
 a^.-fj: ticg solution unril two sonsvcntiYe r-*djcjs are tbe
 Sims, i-r-ral passes itliree cr four) sbouiu  be made be-
 •.•"-n readings. (If cocstant roadlnfs canaot be obtiinsd


    iT:.*  Repeat the analysis tmtll the foUowlng criteria
 ar- met:
    4.2.-LI  For percent COi, rep«»t the a.^aljtlcal pro-
 c»T— *• ur.ttl the results of any three analyses diiler by no
 n;:r» '~.IQ :aj 0.3 percent by volume »b*n COi o grantee
 u.3-' 4.  • r^rrer.t or ''b) 0.2 ^TH0 ci^cr by oo more
                                          H-D5RAI REC1STEX, VOl.  42, NO.  16*—THURSDAY, AUGUST 13,  1777

-------
                                                              RULES  AND   REGULATIONS
                      7nlum» \shen C^ is less th%o l.! 0
                     iic 5v Tolujoe 'I'beQ Or is srwiLtr
                     ui- Ltia  Uirw seccpUb/*
                       ih.d resuJu  LO  tO«
pwiTfi.i. ^r  -, i 0._' ^'
Ulan ! i.O f-T- out. A^
~rcent  O;  aad ropori,  ih.
portent.
  <_2.6.3  For pcrwnt CO,
cTart imtil LQ« IT5U1L3 oi dny tfinre a.ix»l 73 ITS  i3  corr.plft
i-n-tndiiorv! tb« Orssc aoaJ y-r«r one- araiQ. as dftsribM
        n o. Forihe rcsuiu cf the n;aJ \-sis to oe vajict. : !-.e
        ai^ier must na^a tbis le4t l«ii  o*»(or« aad al^r
         jj. Note  AKhuunb 01 moal L'^iar.Cf^ onJ v COj
or O] 13 requ^rxi, i: 13 reco nun ended, iiiat both CO? ind
Oi be rrun-iircd.  ind that Clcauon i m ;b# DiDUo^rmpay
bt u:«l 10 TiucL»t* ihe anjJyxjoU daii.
  •1 3  .Maiu-tPomt,  I.iic^raLeU 3*icpun? and Analytical
procouir?.
  4.0,1  IjcLh tbe minimam nambier
U:
  3.1.1  3nni the liquid levpt m e^cb pip*ct« up to th«
re/i-reccB LQATI on Ui« eapdiary njbia^ and. then clos« tti«
pipene uiopcocfc.
  0.1.2  Kaii* the l*T<>liQg bulb Tufflaentl> fo bnnz the
cor-laiDa ligojJ m^p-^coa onco tne rrwJusied portiou o(
Uj« bureue and t.Vn da-ie ibe maoaioJd jiopcoc
  5.1.3  Ri^c-Trd tbfl meaisciLJ posiuoa.
  5.1.4  Obser79
liquid l«v«J la tb
nuontes.
  5.U  For the Or?At analyirr to  pa^s tbe leak-ch*dE,
two conc!i;(on3auyi b* met.
  .S.i.5,1  Th«t Uqold >T«1  in *acb pip«tte must not  fall
belov t&o  bociom  o/ Uw capillary uaDing  danoj tois
+-aunut*lm«rTai.
  5.1.5.2 Tba meaisoia in  tbe bur^n* aiust cot change
by  more than 0.2 cu dimun ttu3+-^jQculnierrai.
  5.1.3  If the aoaJvier taJJj  thrt leai«k proceilur*. aJJ
rubber  ct3nu«roaf  wad stopcorts sbordd  b« cbecied
anUl tb« causa of tn* ieai is tdf-ntmed. L«a£iii« slopcocts
must b« dis^sa«;mbk til.
        Peirrujt COi or Toluxn* (drr b«lj).
   .i-Perr«al Oiftr Tolum« (drr b«ju>.
 "~oC9—Pereanc CO by Tolam? id-T ouu).
  ^'^Vi^ Hereenc Ni br »olum«  (dry b*xu).
  (J.2V*— ELiUo of Oi lo  Ni In (ur, v.-v.
  0.2H)- Maiccu!^/ wri-rrii o( Ni or CO. Jindp<; by 100.
fl.2  P.r«nc  Eicvaa  ia/.  CalouLaL*  the p*rc*at tic^ss
   (if  applieaill*), t?7  •rob^tilultnt   Ui<«  approtmai*
 luoa of cxrantO:. CO.ar.d N: (obuucfilrom ifv-uoii
1.0 or 1.2.4) uiio  El4QiUon J-l.
                                                                                                       I 100
                                     Equation 3-1

  Norr.—The  *naoMou afeovt iDiiro« that  «—bU-nt
air ;s HM'" cu*)i * ntii spprrci^bl*
amoonts oi  N(  anr present  icoaJ, oil. AaJ natoral  tiu
do ooc  coniAia appr^ciaoU axoouatj of N it or wh^n

to JopriTal of th« Adnuoucrator, i/t r»^uire'i.
  6-j  Dry   Mol*cuiar  ^"i?ht,  Cj»  EquMion  i-J  to
CiiJculjiw ins  dry  'aoJwr^Jjw  w^ijnt o(   tn« 3iark  T^-t
  NOTK.—Thf an-ivf c«l.upou ifi* nnhiJlLS
                                                      metDoJ, unlcjtt Chtt appn'timaaoa
                                                      lh« jaiijfj*'uoa of ih* .^(JjnLaiitnuor. U.i. KnviroruiiNH
                                                      tnl  h*roi»*cnoa A«fn«*T. "> t* miMDl* o4 Vi-Mmj r-uiiu
                                                      v-nliin I r*n:»nt. 11 jO u( '.lif t«icn*iu:« nw-thoj,
                                                        Sort. — Th* r«f»r»t»'r ftifUiiKl fn»j" yt*W ^u«Uon*bli
                                                      mulLS  whwi aoouwl  ;t> ?3kiir3U'il gn jUeLca  w (o
                                                      -,trcamj ihat i-oamm vati-r tiro p. ^n  Thftriuf,  vh-'n
                                                      tbn*ii t
                                                                                                                                         mrt-bod, ai l
                                                                                                                                           to «1° C '^
                                                        r^s leoiCHtr&tiirc. N»st,
                                                         ie, «itbtf  by:  (1)
                                                                                 tuuiff LUA noucur* F»rn(ii«
                                                                                  payctxrojnttrj: caart ud
                                                      making approonat«  (xxrwruoos  J  lUrJc  pressiui :i'
                                                      
-------
                      Attachment E
 Determination of Total Polychlorinated Biphenyl  (PCS)
Emissions from Industrial, Sewage Sludge, and Municipal
           Refuse Incinerators  (Draft Method)

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                PART A.   INDUSTRIAL,  SEWAGE  SLUDGE. AND
                     MUNICIPAL REFUSE INCINERATORS
1.   Principle and Applicability

     1.1  Principle.   Gaseous  and particulate PCBs  are withdrawn isokinet-
ically from the source using a sampling train.   The PCBs  are collected in
the Florisil adsorbent tube and in the impingers in front of the adsorbent.
The total PCBs in the train are determined by perchlorination to decachloro-
biphenyl (DCB) and gas chromatographic determination of  the  DC3.

     1.2  Applicability.   This method is applicable for  the  determination
of PCB emissions (both vaporous and particulate) from industrial, sewage
sludge, and municipal refuse incinerators.

2 .  Ran%e and Sensitivity

          The range of the analytical method nay be expanded considerably
through concentration and/or dilution.  The total method  sensitivity is also
highly dependent on the volume of gases sampled.  However, the sensitivity of
the total method as described here is about 10 ng DCB for each analytical
replicate*

3.  Interferences

          Excessive quantities of acid-resistant organics may cause signifi-
cant  interferences obscuring  the analysis of DCB in the perchlorinated  ex-
tracts.  Biphenyl, although unlikely  to be present in-samples from combus-
tion  sources,  can form DCB in the perchlorination processes.

          Throughout  all stages  of sample handling and analysis, care  should
be  taken to  avoid contact of  samples  and  extracts with synthetic organic
materials other  than  TFE®  (polytetrafluoroethylene).  Adhesives must not be
used  to hold TFE® liners on lids, and  lubricating and sealing greases must
not be used  on any sample exposed portions of the sampling train.

4.  Precision and Accuracy

          From sampling with  identical and paired sampling trains, the  pre-
cision of the method  has been determined  to be  10 to 15Z of the PCB concentra
tion measured.   Recovery efficiencies  on  source samples spiked with PCB com-
pounds ranged  from 85 to 95%.
                                     52

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5.   Apparatus

     5.1  Sampling Train.   See Figure A-l;  a series  of four impingers with a
solid adsorbent trap between the third and  fourth impingers.   The train may
be constructed by adaptation from a Method  5 train.   Descriptions of the
train components are contained in the following subsections .

          5.1.1  Probe nozzle—Stainless steel (316)  with sharp,  tapered
leading edge.  The angle of taper shall be  £ 30 degrees and the  taper shall
be on the outside to preserve a constant internal diameter.  The probe noz-
zle shall be of the button-hook or elbow design, unless otherwise specified
by the Administrator.  The wall thickness of the nozzle shall be less than
or equal to that of 20 gauge tubing, i.e.,  0.165 cm (0.065 in.)  and the dis-
 tance from the tip of the nozzle to the first bend or point of disturbance
shall be at least two times the outside nozzle diameter.  The nozzle shall
be constructed from seamless stainless steel tubing.  Other configurations
and construction material may be used with  approval from the  Administrator.

          5.1.2  Probe liner--3orosilicate  or quartz  glass  equipped with a
connecting fitting that is capable of forming a leak-free, vacuum tight con-
nection without sealing greases; such as Kontes Glass Company "0" ring spher-
ical ground ball joints (model K-671300) or University Research  Glassware SVL
teflon screw fittings.

          A stainless steel (316) or water-cooled probe nay be used for sam-
pling high temperature gases with approval  from the  Administrator.  A probe
heating system may be used to prevent moisture condensation in the probe.

          5.1.3  Pitot tube — Type S, or equivalent,  attached  to  probe to
allow constant monitoring of the stack gas  velocity.  The face openings of
the pitot tube and the probe nozzle shall be adjacent and parallel to each
other but not necessarily on the same plane, during sampling.  The free
space between the nozzle and pitot tube shall be at least 1.9 cm (0.75 in.).
The free space shall be set based on a 1.3  cm (0.5 in.) ID nozzle, which is
the largest size nozzle used.

          The pitot tube must also meet the criteria specified in Method 2
and be calibrated according to the procedure in the calibration section of
that method.

          5.1.4  Differential pressure gauge—Inclined nanometer capable of
measuring velocity head to within 10% of the minimum measured value.  Below
a differential pressure of 1.3 mm (0.05 in.) water gauge, micromanoneters
with sensitivities of 0.013 mm (0.0005 in.) should be used.  However,
                                    53

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                       Stack
                       Wall
                                                     Thermometer"

                                           Florisil  Tube
Check
Valve
Reverse-Type
Pitot Tube
                                         Control Box
                    Figure A-l._  PCB Sampling Train  for Incinerators
                                              54

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micromanometers are not easily adaptable to field conditions and are not
easy to use with pulsating flow.  Thus, other methods or devices acceptable
to the Administrator may be used when conditions warrant.

          5.1.5  Impingers—Four impingers with connecting fittings able to
form leak-free, vacuum tight seals without sealant greases when connected to-
gether as shown in Figure A-l.  The first and second impingers are of the
Greenburg-Smith design.  The final two impingers are of the Greenburg-Sraith
design modified by replacing the tip with a 1.3 cm (1/2 in.) ID glass tube
extending to 1.3 cm (1/2 in.) from the bottom of the flask.

          5.1.6  Solid adsorbent tube—Glass with connecting fittings able to
form leak-free, vacuum tight seals without sealant greases (Figure A-2).  Ex-
clusive of connectors, the tube has a 2.2 cm inner diameter, is at least 10 cm
long, and has four deep indentations on the inlet end to aid in retaining the
adsorbent.   Ground glass caps  (or equivalent) must be provided to seal the
adsorbent-filled tube both prior to and following sampling.

          5.1.7  Metering system—Vacuum gauge, leak-free pump, thermometers
capable of measuring  temperature to within 3°C (*- 5°F), dry gas meter with
27, accuracy at the required sampling rate, and related equipment, or equiv-
alent, as required to maintain  an isokinetic sampling rate and to determine
sample volume.  When  the metering system is used in conjunction with a pitot
tube, the system shall enable checks of isokinetic rates.

          5.1.8  Barometer--Mercury, aneroid, or other barometers capable
of measuring atmospheric pressure to within 2.5 cm Hg (0.1 in. Hg).  In many
cases, the barometric reading may be obtained from a nearby weather bureau
station, in which case the station value shall be requested and an adjust-
ment for elevation differences  shall be applied at a rate of -2.5 mm Hg
(0.1 in. Hg) per 30 m  (100 ft)  elevation increase.

     5.2  Sample Recovery

          5.2.1  Ground glass caps--To cap off adsorbent tube and the other
sample exposed portions of the  train.

          5.2.2  Teflon FEF® wash bottle—Two, 500 ml, Nalgene No. 0023A59
or equivalent.

          5.2.3  Sample storage containers—Glass bottles, 1 liter, with
TFE®-lined screw caps.

          5.2.4  Balance—Triple beam, Ohaus Model 7505 or equivalent.

          5.2.5  Aluminum foil--Heavy duty.
                                     55

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                              . j 28/12
    10cm
rr \
\
\
\
\ f v
\
\ j*~*
\
\
\
\
/
\ ^~s





                            2.5cm O.D.




                            2.2cm I.D.
                             j 28/12
Figure  A-2.  Floristl Adsorbent Tube
                  56

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          5.2.6  Metal can—To recover used silica gel.

     5.3  Analysis

          5.3.1  Glass Soxhlet extractors—40 inn ID complete with 45/50 
-------
          5.3.19  Porcelain casserole--Capable  of withstanding  temperatures
as high as 650°C.

6.  Reagents

     6.1  Sampling

          6.1.1  Florisil--Floridin  Co.,  30/60  mesh, Grade A.   The Florisil
is  cleaned  by 8 hr Soxhlet extraction with  hexane  and  then  by  drying for
8 hr in an oven at 110°C and is  activated by heating to 650°C  for 2 hr (not
to exceed 3 hr) in a muffle furnace.   After  allowing to cool to near 110°C
transfer the clean, active Florisil  to a  clean, hexane-washed glass jar and
seal with a TFE^-lined lid.  The Florisil should be stored at  110°C until
taken to the field for use.  Florisil  that has  been stored more than 1 month
must be reactivated before use.

          6.1.2  Glass wool—Cleaned by  thorough rinsing with hexane, dried
in a 110° C oven, and stored in a hexane-washed  glass jar with TFE®-lined
screw cap.

          6.1.3  Water--Deionized,  then  glass-distilled, and stored in hexane-
rinsed glass containers with TFE®-lined  screw caps.

          6.1.4  Silica gel--Indicating  type, 6-16  mesh.  If previously used,
dry at 175°C for 2 hr.  New silica  gel may be used  as  received.

          6.1.5  Crushed ice.

     6.2  Sample Recovery

          6.2.1  Acetone—Pesticide  quality, Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in  original  containers  and used as received.

          6.2.2  Hexane—Pesticide  quality,  Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in  original  containers  and used as received.

     6.3  Analysis

          6.3.1  Hexane--Pesticide  quality,  Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in  original  containers  and used as received.

          6.3.2  Acetone — Pesticide  quality, Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in  original  containers  and used as received.

          6.3.3  Water—Deionized and  then glass-distilled,  stored in hexane-
rinsed glass containers with TFE@-lined  screw caps.
                                   58

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          6.3.4  Sodium sulfate (Na2SO^)--Anhydrous,  granular.   Clean by
overnight Soxhlet extraction with hexane,  drying in a 110°C oven,  and then
heating to 650°C for 2 hr.  Store in 110°C oven or in glass jar  closed with
TFE®-lined screw cap.

          6.3.5  Sulfuric acid (H2S04)--Concentrated, ACS  reagent  grade or
equivalent.

          6.3.6  Antimony pentachloride (SbCl^)--Baker Analyzed  Reagent or
equivalent.

          6.3.7  Hydrochloric acid (HC1)  solution—ACS reagent grade  or
equivalent, 50% in water.

          6.3.8  Glass wool—Cleaned by thorough rinsing with hexane,  dried
in a 110°C oven, and stored in a hexane-rinsed glass  jar with TFE®-lined cap.

          6.3.9  Decachlorobiphenyl--RPP  Corp., No.  RPC-60, or equivalent.

          6.3.10  Compressed nitrogen—Prepurified.

          6.3.11  Carborundum boiling stones--Hengar Co. No.  133-B or equiv-
alent, rinsed with hexane.

7.  Procedure

     Caution:  Section 7.1.1 should be done in the laboratory.

     7.1  Sampling.  The sampling shall be conducted  by competent  personnel
experienced with this test procedure and  cognizant of the  constraints  of the
analytical techniques for PCBs, particularly contamination problems.

          7.1.1  Pretest preparation.  All train components shall  be  main-
tained and calibrated according to the procedure described  in APTD-0576,
unless otherwise specified herein.

               7.1.1.1  Cleaning glassware.  All glass parts of  the train
upstream of and including the adsorbent tube, should  be cleaned  as described
in Section 3A of the 1974 issue of "Manual of Analytical Methods for  Analysis
of Pesticide Residues in Human and Environmental Samples."   Special care
should be devoted to the removal of residual  silicone grease sealants  on
ground glass connections of used glassware.  These grease  residues should be
removed by soaking several hours in a chromic acid cleaning solution  prior
to routine cleaning as described above.
                                    59

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               7.1.1.2  Solid adsorbent tube.   Weigh 7.5  g of Florisil, ac-
tivated within the last 30 days and still warm from storage in a. 110°C oven,
into the adsorbent tube (pre-rinsed with hexane)  with a glass wool plug in
the downstream end.  Place a second glass wool plug in the tube to hold the
sorbent in the tube.   Cap both ends of the tube with ground glass caps.  These
caps should not be removed until the tube is fitted to the train immediately
prior to sampling.

          7.1.2  Preliminary determinations.  Select the  sampling site and
the minimum number of sampling points according to Method 1 or as specified
by the Administrator.  Determine the stack pressure, temperature, and the
range of velocity heads using Method 2 and moisture content using Approxi-
mation Method 4 or its alternatives for the purpose of making isokinetic
sampling rate calculations.  Estimates may be used.  However, final results
will be based on actual measurements made during  the test.

          Determine the molecular weight of the stack gases using Method 3.

          Select a nozzle size based on the maximum velocity head so that
isokinetic sampling can be maintained at a rate less than 0.75 cfm.  It is
not necessary to change the nozzle size in order  to maintain isokinetic
sampling rates.  During the run, do not change the nozzle size.

          Select a suitable probe length such that all traverse points can
be sampled.  Consider sampling from opposite sides for large stacks to re-
duce the length of probes.

          Select a sampling time appropriate for  total method sensitivity
and the PCB concentration anticipated.  Sampling  times, should generally fall
within a range of 2 to 4 hr.

          It is recommended that a buzzer-timer be incorporated in the con-
trol box (see Figure  1) to alarm the operator to  move the probe to the next
sampling point.

          In some circumstances, e.g., short batch processes, it may be
necessary to sample through two or more batches to obtain sufficient sample
volume.   In these cases,  sampling should cease during loading/unloading of
the furnace.

          7.1.3  Preparation of collection train.   During preparation and
assembly of the sampling  train, keep all train openings where contamination
can enter covered until just prior to assembly or until sampling is about to
begin.   Irnr.ediateiy prior to assembly, rinse all  parts of the train upstream
ot the  adsorbent tube  with hexane.
                                     60

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Mark the probe with heat resistant tape or by some other method at points
indicating the proper distance into the stack or duct for each sampling
point.

          Place 200 ml of water in each of the first two icrpingers, and
leave the third impinger empty.  CAUTION:  do not use sealant greases in
assembling the train.  If the preliminary moisture determination shows that
the stack gases are saturated or supersaturated, one or two additional empty
impingers should be added to the train between the third inrpinger and the
Florisil tube.  See Section 10.1.  Place approximately 200 to 300 g or more,
if necessary, of silica gel in the last impinger.  Weigh each irnnin^er (stem
included) and record the weights on the icroingers and on the data sheet.

          Unless otherwise specified by the Administrator, attach a tempera-
ture probe to the metal sheath of the sampling probe so that the sensor is
at least 2.5 cm behind the nozzle and pitot tube and does not touch any
metal.

          Assemble the train as shown in Figure A-l.  Thrcnjgh all parts of
this method use of sealant greases such as stopcock grease to seal ground
glass joints must be avoided.

          Place crushed ice around the impingers.

          7.1.4  Leak check procedure--After the sampling train has been as-
sembled, turn on and set (if applicable) the probe heating system(s) to reach
a temperature sufficient to avoid condensation in the probe.  Allow time for
the temperature to stabilize.  Leak check the train at the sampling site by
plugging the nozzle and pulling a 380 mm Hg (15 in. Hg) vacuum.  A leakage
rate in excess of 47=, of the average sampling rate of 0.0057 m-Vmin (0.02 cfm)
whichever is less, is unacceptable.

          The following leak check instruction for the sampling train de-
scribed in APTD-0576 and APTD-0581 may be helpful'.  Start the pump with by-
pass valve fully open and coarse adjust valve completely closed.  Partially
open the coarse adjust valve and slowly close the bypass valve until 380 mm
Hg (15 in. Hg) vacuum is reached.  Do not reverse direction of bypass valve.
This will cause water to back up into the probe.  If 380 mm Hg (15 in. Hg)
is exceeded, either leak check at this higher vacuum or end the leak check
as described below and start over.

          When the leak check is completed, first slowly remove the plug
from the inlet to the probe and immediately turn off the vacuum pump.  This
prevents the water in the impingers from being forced backward into the
probe .
                                     61

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          Leak checks shall be conducted as  described  above prior to each
test run and at the completion of each test  run.   If leaks  are found to be
in excess of the acceptable rate, the test will  be considered invalid.  To
reduce lost tine due to leakage occurrences, it  is recommended that leak
checks be conducted between port changes.

          7.1.5  Train operation--During the sampling  run,  an isokinetic
sampling rate within 107.,  or as specified by the Administrator, of true iso-
kinetic shall be maintained.  During the run,  do not change the nozzle or
any other part of the train in front of and  including  the Florisil tube.

          For each run, record the data required  on the  data sheets.  An
example is shown in Figure A-3.  Be sure to  record the initial dry gas meter
reading.  Record the dry gas meter readings  at the beginning and end of each
sampling time increment, when changes in flow  rates are  made, and when sam-
pling is halted.  Take other data point readings  at least once at each sam-
ple point during each time increment and additional readings when significant
changes (207, variation in velocity head readings) necessitate additional ad-
justments in flow rate.  Be sure to level and  zero the manometer.

          Clean the portholes prior to the test  run to minimize chance of
sampling deposited material.  To begin sampling,  remove  the nozzle cap,
verify (if applicable) that the probe heater is  working  and up to tempera-
ture, and that the pitot tube and probe are  properly positioned.  Position
the nozzle, at the first traverse point with  the  tip pointing directly into
the gas stream.  Immediately start the pump  and  adjust the  flow to isokinetic
conditions.  Nomographs are available for sampling trains using type S pitot
tubes with 0.85 + 0.02 coefficients (C ),  and  when sampling in air or a stack
gas with equivalent density (molecular weight, M^j, equal to 29 + 4), which
aid in the rapid adjustment of the isokinetic  sampling rate without excessive
computations.  APTD-0576 details the procedure for using these nomographs.
If C  and M^ are outside the above stated ranges, do not use the nomograph
unless appropriate steps are taken to compensate for the deviations.

          When the stack is under significant  negative pressure (height of
impinger stem), take care to close the coarse  adjust valve  before inserting
the probe into the stack to avoid water backing  into the probe.  If neces-
sary, the pump may be turned on with the coarse  adjust valve closed.

          When the probe is in position, block off the openings around the
probe and porthole to prevent unrepresentative dilution  of  the gas stream.

          Traverse the stack cross section,  as required  by  Method 1 or as
specified by the Administrator.  To minimize chance of extracting deposited
material, be careful not to bump the probe nozzle into the  stack walls when
sampling near the walls or when removing or  inserting  the  probe through the
portholes.
                                   62

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                                                                    FIELD DATA
                     PLANT,
                     DATE _
                     SAMPLING LOCATION.
                     SAMPLE TYPE .	
                     RUN NUMBER	
                     OPERATOR 	
                    AMBIENT TEMPERATURE
                    BAROMETRIC PRESSURE .
                    STATIC PRESSURE. (P,)_
                    FILTER NUHBER(j)	
                                               PHODE LENGTH AND TYPE .
                                               NOZZLE 1.0 ______ .
                                               ASSUMED MOISTURE.'. _
                                               SAMPLE BOX NUMBER __
                                               HCTER BOX NUMBER __
                                               METER Al^ _
                                               C FACTOR. _
                                               PROBE HEATER SETTIKG
                                               HEATER BOX SETTING
                                               REFERENCE 4p__
                                                            SCHEMATIC OF TRAVERSE POINT LAYOUT
                                                      READ AND RECORD ALL DATA EVERY.
                                                                                          MINUTES
TRAVERSE
POINT
NUMBER























N, CLOCK TIME.
sSLl"c\^!c«
TIME. Kin N^
— — — ^^^























CAS METER READING
(Vml. II3
























VELOCITY
HEAD
tip,), m. H20























ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. II20|
DESIRED























ACTUAL























STACK
TEMPERATURE
(T,l.-F























DRYGM METER
TEMPERATURE
INLET

-------
          During the test run,  make  periodic  adjustments  to keep the probe
temperature at the proper value.   Add  more  ice  and,  if  necessary, salt to
the ice bath, to maintain a temperature  of  less  than 20°C (68°F) at the
impinger/silica gel outlet, to  avoid excessive  moisture losses.   Also, peri-
odically check the level and zero of the manometer.

          If the pressure drop  across  the train becomes high enough to make
isokinetic sampling difficult to  maintain,  the  test  run should be terminated.
Under no circumstances should the train  be  disassembled during a test run to
determine and correct causes of excessive pressure drops.

          At the end of the sample run,  turn  off the punp,  remove the probe
and nozzle from the stack, and  record  the final  dry  gas meter reading.  Per-
form a leak check.*  Calculate  percent isokinetic (see  calculation section)
to determine whether another test run  should  be  made.   If there  is difficulty
in maintaining isokinetic rates due  to source conditions, consult with the
Administrator for possible variance  on the  isokinetic rates.

          7.1.6  Blank train--For each series of test runs, set  up a blank
train in a manner identical to that described above, but  with the nozzle
capped with aluminum foil and the exit end of the last  impinger  capped with
a ground glass cap.  Allow the train to  remain assembled  for a period equiv-
alent to one test run.  Recover the blank sample as  described in Section 7.2.

     7.2  Sample recovery-  Proper cleanup procedure begins as soon as the
probe is removed from the stack at the end of the samp'ling period.

          When the probe can be safely handled, wipe off all external par-
ticulate matter near the tip of the probe nozzle.  Remove the probe from the
train and close off both ends with aluminum foil.  Cap off the inlet  to the
train with a ground glass cap.

          Transfer the probe and impinger assembly to the cleanup area.  This
area should be clean and protected from the wind so that the chances  of con-
taminating or losing the sample will be  minimized.

          Inspect the train prior to and during disassembly and note  any ab-
normal conditions.  Treat the samples as follows:

          7.2.1  Adsorbent tube—Remove  the Florisil tube from the train and
cap it off with ground glass caps.
   With acceptability of the test run to be based on the same criterion as
     in 7 . 1.4.

                                     64

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          7.2.2  Sample container No.  I — Remove the  first  three impingers.
Wipe off the outside of each impinger  to remove excessive  water and  other
debris,  weigh (stem included),  and record  the  weight on  data  sheet.   Pour
the contents directly into container No. 1 and seal.

          7.2.3  Sample container No.  2--Rinse each  of the first three im-
pingers  sequentially first with 30 ml  acetone  and then with 30 ml hexane,
and put  the rinses into container No.  2.  Quantitatively recover material
deposited in the probe using 100 ml acetone and then 100 ml hexane and add
these rinses to container No. 2 and seal.

          7.2.4  Silica gel container--Remove  the last impinger, wipe the
outside  to remove excessive water and  other debris,  weigh  (stem included),
and record weight on data sheet.  Transfer the contents  to the used  silica
gel can.

     7.3  Analysis.  The analysis of the PCB samples should be conducted by
chemical personnel experienced in determinations of  trace  organics utilizing
sophisticated, instrumental techniques.  All extract transfers should be
made quantitatively by rinsing the apparatus at least three times with hex-
ane and  adding the rinses to the receiving container. A boiling stona should
:>a used  in all evaporative steps to control "bumping."

          7.3.1  Extraction

               7.3.1.1  Adsorbent tube.  Expel the entire  contents of the
adsorbent tube directly onto a glass wool plug in the sample holder of a
Soxhlet  extractor.  Although no extraction thimble is required, a glass
thinble  with a coarse-fritted bottom may be used.

               Rinse the tube with 5 ml acetone and  then with 15 ml hexane
and put  these rinses into the extractor.  Assemble the extraction apparatus
and extract the adsorbent with 170 ml  hexane for at least  4 hr.  The ex-
tractor should cycle 10 to 14 times per hour.   After allowing the extrac-
tion apparatus to cool to ambient temperature, transfer the extract into a
Kuderna-Danish evaporator.

               Evaporate the extract to about 5 ml on a steam bath and
allow the evaporator to cool to ambient temperature  before disassembly.
Transfer the extract to a 50-ml separatory funnel and set  the funnel aside.

               7.3.1.2  Sample container No. 1.  Transfer  the aqueous sam-
ple to a 1,000-ml separatory funnel.  Rinse the container  with 20 ml acetone
and then with two 20-ml portions of hexane, adding the rinses to the sep-
aratory  funnel.
                                     65

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               Extract the sample with three  100 nil portions of hexane,
transferring the sequential extracts  to a Kuderna-Danish evaporator.

               Evaporate the extract  to about 5 ml and allow the evaporator
to cool to ambient temperature before disassembly-  Filter the extract through
a micro column of anhydrous sodium sulfate into the 50 ml separatory funnel
containing the corresponding Florisil extract.   The micro column is prepared
by placing a small plug of glass  wool in the  bottom of the large portion of
a disposable pipette and then adding  anhydrous  sodium sulfate until the tube
is about half full.

               7.3.1.3  Sample container No.  2.  Transfer the organic solu-
tion into a 1,000 ml separatory funnel.  Rinse  the container with two 20 ml
portions of hexane and add the rinses to the  separatory funnel.  Wash the
sample with three 100 ml portions of  water.   Discard the aqueous layer and
transfer the organic layer to a Kuderna-Danish  evaporator.

               Evaporate the extract  to about 5 ml and allow the evaporator
to cool to ambient temperature before disassembly.  Filter the extract through
a micro column of anhydrous sodium sulfate into the 50 ml separatory funnel
containing the corresponding Florisil and impinger extracts.

          7.3.2  Extract cleanup—Clean the combined extracts (in 50 ml
separatory funnel) by shaking with 5  ml concentrated sulfuric acid.  Allow
the acid layer to separate and drain  it off.

          Transfer the hexane layer to a Kuderna-Danish evaporator and evap-
orate to about 5 ml.  Allow the evaporator to cool to ambient temperature
before disassembly.

          The extract should be essentially colorless.  If it still shows
significant color, additional cleanup may be  required before assaying for
PCBs.  In this event, further clean the extract by liquid chromatography on
Florisil according to procedures  described in Section 5A of the 1974 issue
of "Manual of Analytical Methods  for  Analysis of Pesticide Residues in Human
and Environmental Samples"  Reduce the Florisil eluant to about 10 ml by
Kuderna-Danish evaporation techniques described above.

          Transfer the cleaned extract to a 25  ml volumetric flask and di-
lute to volume with hexane.  Pipette  three 5.0  ml aliquots into culture
tubes for perchlorination.  Retain the remaining 10 ml for later verifica-
tion, if required (see Section 10.2).

          7.3.3  Extract perchlorination--Evaporate the aliquots in the cul-
ture tubes just to dryness with a gentle stream of dry nitrogen. If the ali-
quots will not evaporate to dryness,  refer to Section 10.3 concerning special
cases. Add 0.2 ml antL-no-ny pentachloride with a 1 ml glass-TFE® syringe and

                                    66

-------
seal  the  tube  with a TFcf^-lined screw cap.  Heat the reaction mixture to 160°C
for 2 hr  by  placing the tube in a hole in an aluminum block on a hot plate.

         Allow  the tube to  cool to  ambient room temperature before adding
about 2 ml of  507,  HC1 in water to destroy residual  antimony pentachloride.
This  is a convenient "stopping point" in the perchlorination procedure.

         Extract  the reaction mixture by adding about 1  ml. hexane to the
tube, shake, and allow layers  to separate.   Remove  the upper hexane layer
with  a disposable  pipette and  filter through a micro column of anhydrous
sodium sulfate directly into a 5 ml  volumetric flask.   Repeat the extraction
three tines  for  a  total of four extractions.  Dilute the  extract to volume
with hexane.

          7.3.4  PCS determination—Assay the perchlorinated extracts for
decachlorobiphenyl (DCB) by gas chromatographic comparison with DCS stan-
dard solutions and correct this result for  the DCB  concentration determined
for the  blank  train.  (Column temperature and carrier gas flow parameters
if 240°C  and 30  ml/min, are typically appropriate.   The concentrations of the
standard  solutions should allow fairly close comparison with DCB in the sam-
ple extracts.   Standards near 25 to 50 picograms/microliter may be appropriate.)

8.  Calibration

          Maintain a laboratory log of all calibrations.

     8.1   Sampling Train

          8.1.1   Probe nozzle--Using a micrometer,  measure the inside dia-
nater of  the nozzle to the nearest 0.025 mm (0.001 in.).   Make three separate
measurements using different diameters each time and obtain the average of
the measurements.   The difference between the high and low numbers shall not
exceed 0.1 mm (0.004 in.).

          When nozzles become nicked, dented, or corroded, they shall be re-
shaped,  sharpened, and recalibrated before use.

          Each nozzle shall be permanently and uniquely identified.

          8.1.2   Pitot tube—The pitot tube shall be calibrated according
to the procedure outlined in Method 2.

          S.I.3  Dry gas meter and orifice meter—Both meters shall be  cali-
brated  according to the procedure outlined in APTD-0576.  When diaphragm
                                     67

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pumps with bypass valves are used,  check for proper metering system design
by calibrating the dry gas  meter at an additional flow rate of 0.0057 m3/min
(0.2 cfm) with the bypass valve fully opened and then with it fully closed.
If there is more than + 27,  difference in flow rates when compared to the fully
closed position of the bypass valve, the system is  not designed properly and
must be corrected.

          8.1.4  Probe heater calibration—The probe heating system shall be
calibrated according tc the procedure contained in APTD-0576.  Probes con-
structed according to APTD-0581 need not be calibrated if the calibration
curves in APTD-0576 are used.

          8.1.5  Temperature gauges—Calibrate dial and liquid filled bulb
thermometers against mercury-in-glass thermometers.  Thermocouples should
be calibrated in constant temperature baths.

     8 .2  Analytical Apparatus

          8.2.1  Gas chromatograph--Prepare a working curve from at least
five standard injections of different volumes of the DCS standard.

9.  Calculations

          Carry out calculations, retaining at least one extra decimal fig-
ure beyond that of the acquired data.  Round off figures after final calcu-
lations .

     9.1  Nomenclature

     GQ = Corrected weight  of DCB in nth perchlorinated aliquot (n = 1,  2, 3),  pg.

     G  = Total weight of PCBs (as  DCB)  in  sample,  ng.

     GS = Concentration of  PCBs in  stack gas, ug/nr', corrected to standard
            conditions of 20°C, 760 mm Hg (68°F,  29.92 in.  Hg) on dry basis.

     AQ = Cross-sectional area of nozzle, n? (ft,2).

    Bws = Water vaP°r in the gas stream,  proportion by volume.

      I = Percent of isokinetic sampling.

     My - Molecular weight  of water,  18  g/g-mole (18 Ib/lb-mole) .

   Pbar = Barocnetric pressure at  the sampling site, nm Hg (in. Hg) .
                                    68

-------
    PS = Absolute stack gas pressure, mm Hg (in. Hg).

  Pstd = Standard absolute pressure, 760 cm Hg (29.92 in Hg).

     R = Ideal gas constant, 0.06236 mm Hg-ra3/0K-g-mole (21.83 in.
           Hg-ft3/°R-lb-mole).

    Tm = Absolute average dry gas meter temperature CK (°R) .

    Ts = Absolute average stack gas temperature °K (°R).

  Tstd = standard absolute temperature, 293°K (528°R).

    V]_c =• Total volume of liquid collected in impingers and silica gel, ml.
           volume of water collected equals the weight increase in grams
           times 1 ml/gram

    V = Volume  of gas  sample  as measured by dry gas  meter,  dcm  (dcf).

\Wstd) = Volume  of  gas  sample measured  by  the dry gas meter  corrected to
            standard conditions,  dscm (dscf).

V / C(js = Volume of  water vapor in the gas  sample corrected to standard
            conditions,  scm (scf).

     Vt = Total volume of sample, ml.

     V  = Stack gas  velocity,  calculated by EPA Method' 2, n/sec  (ft/sec).
      s

     AH  = Average pressure differential  across the orifice  meter, mm
            (in.  H20).

     pw  = Density of water, 1  g/ml (0.00220 Ib/ml).

      9  = Total Sampling time,  min.

   13.6  = Specific gravity of  mercury.

     60  *• Sec/min.

    100  = Conversion to percent.
                                      69

-------
     9.2  Average dry gas meter temperature  and  average orifice pressure
drop. See data sheet (Figure A-3).

     9.3  Dry gas volume.  Correct  the  sample volume measured by  the  dry
gas meter to standard conditions [20°C,  760  mm Hg  (68CF, 29.92 in. Hg)] by
using Equation A-l).
          Vm(std)
= V
   m
                        Lstd
                         Lm
AH "
Pbar 13.6
Pstd
•*• ^H
= r w bar 13.6
T
m •
                                                   Equation A-l
where     K = 0.3855  °K/mm  Hg  for metric units

            = 17.65 °R/in.  Hg  for English units

     9.4  Volume  of water vapor
Vw(std) = Vic  -T
                             RT
                               std
                              pstd
                                      K Vic
                                  Equation A-2
where     K = 0.00134 m /ml  for metric units

            = 0.0472 ft3/ml  for English units

     9.5  Moisture content
                      w(std)
                   m(std) + Vw(std)
                                                   Equation  A-3
     If the liquid droplets  are  present  in the gas stream assume the  stream
to be saturated and use  a  psychrometric  chart to obtain an approximation
of the moisture percentage.
                                   70

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    9.6  Concentration
         9.6.1  Calculate the total PCB residue (as DCS) in the sample from
the weights of DCS in the perchlorinated aliquots according to Equation A-A.

         Gs  = 5(G1  + G2 + G3)                               Equation A-A
         9.6.2  Concentration of PCBs (as DCB) in stack gas.  Determine the
concentration of PCBs in the stack gas according to Equation A-5.
                  G
         Cg = K 	                                      Equation A-5
                Vm(std)

where      K = 35.31 ft3/m3
     9 .7  Isokinetic variation

         9.7.1  Calculations from raw data.
                    100  T   CK  V.   +  (V  /T  )   (P.   ) + AH/13. 6)]
                    _ s      Ic      in m     oar
                                   60  9 vs   Ps  An
                                                            Equation A- 6
    where     K = 0.003A6 mm Hg-m3/ml-°K for metric units

                = 0.00267 in. Hg-ft3/ml-°R for English units

         9.7.2  Calculations from  intermediate values.
                      Ts  Vm(std)   Pstd
                  Tstd  vs  9  An   Ps   60  (1

                  K     Ts  Vm(std)	
                    ps  vs  An  ®   (1-B^)                  Equation A-7
    where     K = A.323 for metric units

                = 0.094A for English units


                                    71

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     9.8  Acceptable results. The  following range  sets the  limit  on accept-
able isokinetic  sampling results:

          If 907. < I < 1107., the results are acceptable. If the results, are
low in comparison to the standards and I is beyond the acceptable range,  the
Administrator may option to accept the results,

10.  Special Cases

     10.1  Sampling moisture saturated or supersaturated stack gases. One
or two additional modified Greenburg-Smith impingers may be added to the
train between the third impinger and the Florisil tube to accommodate addi-
tional water collection when sampling high moisture gases. Throughout the
preparation, operation, and sample recovery from the train, these  additional
impingers should be treated exactly like the third impinger.

     10.2  PCS verification. It is recommended that an unperchlorinated
aliquot from at  least one sample be subjected to GC/MS examination to verify
that PCB isomers are present.

          To accomplish this, the unperchlorinated portion of each  extract
is first screened by GC with the same chromatographic system used  for DCB
determination except for a cooler column temperature, typically 165 to 200°C.
The elution patterns are compared with those of commercial PCB mixtures (in
hexane solution) to determine the most similar mixture.

          After determining what PCB isomers are possible present,  the sam-
ple is examined by GC/MS using multiple ion selection techniques  for ions
characteristic of the molecular clusters of the PCBs possibly present.

     10.3  Evaporation of extracts for perchlorination» For cases where the
extract will not evaporate to dryness or excessive PCB loss by volatiliza-
tion is suspected, the hexane may be removed by azeotrophic evaporation from
the hexane/chloroform mixture.

          Add 3 ml of chloroform to the aliquot in the culture tube. Add
a boiling chip and concentrate by slow boiling in a water bath to  1 ml.
Repeat the chloroform addition and evaporation three times in order to remove
all residual hexane.  Then further concentrate (slowly) to a volume of ap-
proximately 0.1 ml.  Under no circumstances should the water bath  tempera-
ture be permitted to  exceed 76 C or the solvent be evaporated to  dryness.
The final volume (0.1 ml) may be determined with sufficient accuracy by
comparison of solvent level with another reaction vial containing  0.1 ml
of chloroform.  When a volume of 0.1 ml is achieved, cap the reaction vial
immediately and allow to  cool.  Proceed with the perchlorination as described
in Section 7.3.3.
                                  72

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11.   References

         Martin,  Robert M., "Construction Details of Isokinetic Source
Sampling Equipment," Environmental  Protection Agency, Air Pollution Control
Office Publication No. APTD-0581.

          1973 Annual Book of ASTM  Standards, Part 23, Designation:  D 1179-72,

         Thompson, J. F.,  Ed.,  "Analysis of Pesticide Residues in Human and
Environmental Samples," Environmental Protection Agency, Research Triangle
Park, N.C.,  1974.
                                    73

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               Attachment F
Determination of Nitrogen Oxide Emissions
         from Stationary Sources

-------
  11TS4
                                                         RULES  AND   REGULATIONS
     Edteric Add Standard. 0 0100 N  Prrthaie or
        to -O.CDC V amrutt 0.0100 N NeOH wtjjch
 1 1        .
 ,'l i reparation of collection train. Nfeejure 15 ml of
  nrnnt ixpropanol Into U» njdiet bubbler and li
 I ail errant hydrce^n peroxide into e»rh o( lie am
 TO=Ji;'iUiipiEj«n. Leare the flr.il mid?«t UEpinr,er
 ~ jHyjable tie train u ibo-am in F!:rure f/-l- Adlujt
 flb« ceaur to a tezaperanir* mfflcimt to pr*Tent «-*t*r
          Pl»ce cruioed ice uid irmier around u*
 igtBim.
 4 1 J Uti-cberk jrccerfnre,. A le*± crwk prior to tbe
 cpltot nm 14 optional; bo-w^rer. a lealc rhecr ajter the
 DDLS* rm U mand*iory. The ieaJt-cceci proeedur* u
 i ;ollff»i:
 ffl'.o tM probe duconnecUd, piace a Tucurun (iug» at
 y luiit to tbe babbler and pud * Tvruum of 230 nira
 10 to.) HI; pl'-H o< nlnrh of! Ui« outlet of the flo-w aeter,
 sd then. ram off *.i» pxorp. Tee Tacmim &hsil remain
 uhk lor at  I*ejt  30  vcondv  Carefully  raleue-  tie
 innni giun beton n'ftacx the tow nwter end to
 rwut tick io» of ti' uounrrr Svud.
 Otlw '••** cierk pro.Tda.-to nay be used. lubHrt 10
 It iOBroTil of tie Admr Jt.-ator. U.3. EnTironinentmJ
 •pcijcuon Ai»acy  Tie xocedun used In  Method  i J
 £i wiuble (or dUo»ir»rs) pucps.
 6g* F) or los. At th»
 condaslon of each rjn, turn off Cw porno, remoTe prnb<
 (rorn th« *tact ind  record tb« ftna] readlruo- Conduct &
 Ink cbeci uj.n Section 4.1 J>. (Taj» l»AJt cberk b nar.i»-
 urr.) Ii'i '«i^c b found. 10(4 th« u«x ran. Drain too lc«
titb. «nd fjrre tb« reicaJnint pan ol th« tnun by draw-
ijj d«an vntient nr tflrou jii  tin ryitan (or 15 irlnuta
 Itlhi sampUtK  rau
 CUan ambient ilr csn b*  pnrrid*d by p&sstcz  air
 Uuno^b a cbarcoaJ fljtax or  tKrough an e£ira midget
 taplnger with 15 mJ of 3 percent HjOt. The tester OAY
 cpi Ui staply ox imbltnt air, witbont punaculon.
 U  Simple Recorery. D'jconnect tb« LTapLacors allit
 parrinji. Ducard theccntantscH tne nudget babbler. Povir
 Ibi congou of tbe dW«rt Izpmxen Into s  l«ai-(TM
 polyfihylflneboltUfor ihjpQAnL RULM trrt thr«« mjdt«t-
Lmpiajen and tbe amn«ca3(  cabea with deioruud,
d^Ill«t to tht drrin*
                                                 rao4 %cd pull a ractrora of 220 ™™ (10 UL) Be: plu< or
                                                 pineb oa Ui« outlet or UM flow rc«tcr. and tb«n Cora oil
                                                 itn ptnuQ. Tb» racoca shall nmain rabie for it i«*n
                                                 X aecoodi. Cverally r*leaae t^a Tvcnua sauxt  belora
                                                 nleajuu tb< flow meter end.
                                                   Nan, callbrau LM mauttnt xyiUa (at tb« mmpoaf
                                                 floir rale nwdfitd try  Lb< nutted) u follow!: crracwce
                                                 aa apprepnately o«d mt un  mel«- («^..  1 Ut« per
                                                 nrolauoa) to tb> inlet of ti» dfTtex mba. Maxa larra
                                                 lndeo*ndant e*Ubnuju rona, r**^* u '*^<* £T« rtToffi-
                                                 boiu o/ the dry ;u meur per ran. CaieaUu tn« dhora-
                                                 aoo (actor, X vwet ten mettr caiibraaoo Torooa dj-ndsd
                                                 bv Ibe dry ivi meur voiuac. bott 'olcmej adloiud to
                                                 t39 aus« reJereoc* tamperaum  and cnsura). Cor oocA
                                                 ran, ind ar«rage tie resuin. U any Y TUU* deriaMi by
                                                 morv than 2 peront from tte  aTerave. t^« a«unc{
                                                 57>rum u tuucnr/taal* (or UK. Ot&em». CM lie ir-r-
                                                 ace u Lb.a c&libnuon factor for snbaeqaeat UA ra&A.
                                                   i-U Past-Tun Callbrauon Cieci. Xlur acn &*Jd
                                                 tolMrle, condoeiacalibrauoncbccc  u In S«e'Jon S.1.1
                                                 ilxr»«, atcept for tie foUovxnz Tur.iuoaj: (a) me leal
                                                 thtet U not us b« ooodocttd, (b) tarw. or mum reroiu-
                                                 uocu of tb« dry gu maur may be tued. ind (c) ooly tm
                                                 independent runs need b* nude. If tt* aOibraDon lartor
                                                 dou not dtriau by son Uan i pereat from Lbe Lnjiti
                                                 calibration factor (deterailntd In Seeoon 5.1.1), tbtn tie
                                                 dry I" iceur i>lam« obuued dnr^( vb« ten una
                                                 &n accepubla. If til dii tuition ficur deruia by aw*
                                                 tivn i puctnt, raakllbrmu lh«  meurUK trynem u La
                                                 StcUooJ.1.1. &ad lor tb« e*Jcnlauo
                                                 glxu thenaomalarv
                                                   5.3   Kourctur. Th«ntaoieu>r c«*d not t» calibrated
                                                 bml  Tolmnetnc ^*<^* and dUnta to exactly ICO ml
TlUi dekjolied. dijtllled w»Ler. Pipe tie a 2>ml allqooc of
lili Mloaon Into a li'>mJ Erlenmeyer flux, add 80 ml
or ICO percent iaopropenot and ciro to [oar drope of tbortn
bdlcaur, and titrau to a pinz andpoint ucng 0.0100 N
birtoni percotante. Repeu aad  arerx* the Utratloa
tolioo. Runat'jkn^c TiLheach »nn ol samples. Repe-
al*  tluuioiu nun *£TM wltain 1 percent or 0- ml.
i.

 3.1  Metering Eyitan.
 1.1.1 laiaal Calibration. Before !U Initial o» In tbe
Held, Urn 1-eJr chsct tie metenot ryrttem (dryic* tube,
         t, pump, rtrtAzaeter, aad dry gu meter) aj
                                                       ~ •Concentration   TorcmM Deucnd by tbe dry (a*
                                                           meur.  axncud  to naadard1  conditions,
                                                       V,»-
SiC3-
  Dry
                                                            djon (a.
                                                            Total yotonve of aohitlon bi wblcb Ox roKor
                                                            dlodde rvnp^ i3 contained. 100 mL
                                                            Voluma of barium percbJorau Utrant caea
                                                            for  lb« sunpU, ml (a»er»<« of rtplicau
                                                            UtraUona).
                                                            Volum« o< barlom percnlorau Utraot nied
                                                            (or tb« blank, ml.
                                                            Dry cu meter-call bnibm lactor.
                                                            Eqol Talent wtl*ht of mlfw dioxide.
                                                             sampU lit  tolome, ccmcted U>
                                               wberr:

                                                 /Ci—0.3i» 'Kfasa Hg (or metric onlu.
                                                   -17.44 *R/in. Hg lor Entljah """•»
                                                 6J  tHUfar dioxide cocowLrauoo. -
                                                 here:
                                                 i"»— EJ3mt/meq. lor metric nnlu.
                                                   — 7.0G1X10-* Ib/TtK). lor Entlisi nnn«-
                                                                                     Kqnattooe-J
                                                7.

                                                 U Auxmbefie Enrrrinra from  Snlruric Add Ujno-
                                                t*cronr« rrmujem. L'^. DHrw. PH3. Dinaioo o< AH
                                                Pollntion.  Pnoltt Health  Serrioa PnMjotlm  No.
                                                W9-AP-U. Clrmnrtail. Otuo. 196i.
                                                 2. Corbert. P.  7. The DtUrnunHion o( 8O> acd  8Oi
                                                In  F!a« Owes. JoonuJ o/ llx Lnautauoi FuaLtf 3^
                                                5*3, 15*1.
                                                 3. Maccr. B. E. andZ. K. Dlecl.Ue«uchnx 7hie-Oa»
                                                SOi and 3Ov rci»u. ;or: 9*-97. NoTonber 1867.
                                                 •4. Paooo. W. F. and J. A. BrinX Jr. New Equipment
                                                and Tfduueroea  for Sampling Chemical PTIXJJ« G*jea.
                                                J. Air PoDnuoo Contre4 Ajecciajloo. ;3: 182. 1983.
                                                 S. Rom,J.J. 
                                                ErrTiioru  trora  3t»iion»ry Sounzi (FaBij-Foal jir«l
                                                8Leam Crtstra^on). EoTironmenuJ Protpcilon Ajtencrt
                                                Research   Tr_a=ti«   Part.  N.C.  BrA-oiiOii*-,--t-024.
                                                Doounber  1S7X
                                                 7. Anrmil Book o< ASTM St&ndarda. Pvt lU Waur.
                                                Atmoapbenc Analyni. Amenc&n cocuty for Teadnf
                                                and Miitrlili. P^tUdelpcoa, Fi. 197-4. pp. 40-12.
                                                 8. Knoll. J. S.  and M. R. MidjeU. Tie ApoUcatioa o4
                                                EPA Meibod 6 to Hufi SnUar Dioude Coocancrauaoa.
                                                Enriroiucental  ProcectioQ A^eocy. &ae
                                                Park. N.C. E PA-eOOrt-7o-Ba. July 1»7J.

                                                Mrrnoo  7— DrrriKE
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                                                       RULES  AND  REGULATIONS
                                                                                             417S5
                                                                                                                       SQUEEZE BULB
        PROBE
                                                      FLASK VAL'
      FILTER



 GROUND-GLASS SOCKET.

      § NO. 12/5
5.WAT STWCCCK.'

T-60K-. 5 PT'SU
2-mrn BORE. 8-*nm OO
           FLASK
                                                FLASX SHiaO^*
                                                                           THERMOMETER
            GROUND-GLASS- CONE,

             STANDARD TAPER.

              SLEEVE NO. 24/40
                                                                      210mm
GROUND-GLASS
SOCKET. § NO, 12/S
FfRBC
                                                                                                            	FOAM ENCASEMENT
                                                                                                        BOILING FLASK •
                                                                                                        2-LITER. ROUND-eOTTOM. SHORT NECK.
                                                                                                        WITH J SLEEVE NO. 24/40
                                     Figure 7-1.  Sampling train,  flask valve, and flask.
  2.1,2 Collwtlon TSask, TwvUter bcrosttleata, round
 bottom fluk, with short Deck aod 24/40 naadard Ui*r
 opining, protected agaicat iaploaioo or breakage,
  2.1.3 Flask Valre. T-bor»  stopcock conceded to a
 2V40 standard tsper Joint.
  2.1.4 Temperature Gacge, Dial-type, thermometer, or
 other temperature gauge, capabla of m<«5unng 1* C
 (2* F) Intervals from -6 to xf C (2S to 12S* F).
  2.1.S Vacnura.Line, Tubin* capable ol withstanding
 avicunasol75 mm H« (3 in. Eg) absolute pressure, with
 "T" connection and T-bore stoprock.
  3.1.5 Vacuus  Game.  G-rooe manometer. 1 meter
 (3ft in.), with 1-ran i.O-l-i—)  divisions, or other,  gsutn
 ^p»b'.« of measuring pi mure to wiihin  -*-^-> f m Hg
 (0.10 in. Hg).
  2.1.7 Pump. Capabla  ot evacuating the collection
 flosk to a preaare equal to or less than 75 ma Hg (3 In.
 Hit) absolute.       •   •
  2.1.S Squeete 3ulb. Oae-way.
•  2.1.4 Voluoetrta Pip«tt«, 2S ml.
  2.1.10  Etapi'ock and Groc&d Joint Grease, A high-
 vacuum. htch-ump*racur* cbioroBuorocarbon grease la
 required. Halocj.-bon 1>-S3 ha< b«en found to be eflectlve.
  2.1.11  Barometer. Mercury, aneroid, or other barom-
 eUr capable ot B««junag atmoaphenc pnssun u> within
 2J ma Hg (0.110. Hg). la many case*, the baronucrt*
 ratxliog may be obtuned from a nearby national weather
 tcrvlce nation, la vMch case the nation value (which Is
 tbe at*jlul« barometric prueure) shall b« requested and
 an adjustment tor elevation  dtBerence* between tba
 wwta*/ nation lid u=pUog point shall be appUed at a
 rale of miaus 2J torn Hg (0,1 In. Hg) per 30 m (100 ft)
elevaiiou increase, or vice viraa lor elevation dfrease.
  2J  Simple  Recovery. Tbe loUowlag  equipment Is
requlnd for sacpl< recovery:
  2.2.1 Graduated Cylindrr. SO ml wltb 1-ml divisions.
  2A2 Storage  Containers.  Leak-free  polyethylene

  2^.3 Wash Bottle. ?olyettylen« or glass.   •
  2-M Class Stirring Rod.
  S.2JJ Ttat Paper lor Indicating pH. To cover the pH
 range ot 7 to 14.
  2.3_ Analysis. For the analysis,  the following1 eqalp- -

  2..1.1 Volumetrle Pipettes. Two 1 ml. two 2 ml, on»
 3 in, «ne 4 ml, two 10 al. and one V> ml lor cub sample
 acd su'i'Urd.
                                                   2JL2  PQreeUln Bnpontinii DfehM. ITS- to 2M-cU
                                                 capacity with Us (or pouring,  on* lor each sample and
                                                 each nandard. The Coon No. 4500* (shaUow-lorm. l<4
                                                 ml) has b*eo found to be satisfactory, Altertuuimy,
                                                 polysethyl pentene b4aken (Na4« No. 1203. 150 ml), or
                                                 Itau beaktn (liO ml) may be used, f^Mn |\ass bmken
                                                 are used, ctchlnn o( the beakera may OUM »Ud matter
                                                 to b* pm*nt In the analytical sue. the solids should b*
                                                 removed by nitration lx» Section 4 J) .
                                                   2-1..1  Stram Bath. Low-temp*r*ton orpn^ or therrao-
                                                 tuucally controlled hot plaus kept txiiow 70* C (ISO* ? )
                                                 arc accepublo aittmatlTa.
                                                 •  2J.4  Dropping Pipette or Dropper. Thrre rKmlrrt.
                                                   1-2.5  Polytthyleo* Policcraan.  Oae (or each sample
                                                 and each standard.
                                                   J.3.8  Gndoutd Cylinder. 100ml wtLhl^nldlrUonv
                                                   2.J.7  Volumetric Flasks. 60  ml (one for each satnpl*),
                                                 100 ml (one for each samnle and earh standard, and oot
                                                 tor th* working standard KNOi solution), and 10CO ml
                                                 (one).
                                                   2..1J  Spectrephotometcf. To measure absorbaac* at
                                                 410 run.
                                                   2.3.8  Graduated Ptpetti. 10 ml with 0.1-nl divisions.
                                                   2.3.10  ten Paper for Indicating pH. To COTS tb»
                                                 pK note of 7 to 14.
                                                   2J.11  Analytical Balance-To measure to within 0.1
                                                   Unlro otbervls* Indlcattd. 11 Is Intended lh»i all
                                                 reagenu conlorm to the s?»-:.Bc»tlons established by the
                                                 Committee on Analytical Reagents of  the  American
                                                 Chemical Society, wtj'r* such spwiBcaUoos  an avail-
                                                 ablevothenrise, use the best available grade.
                                                   3.1  SarapUng.  To prepare the absorbing solction.
                                                 cautiously add 2.S ml concentrated HioO, to 1 Uter of
                                                 deiontied, distilled water. MlJ well and add e  ml of 3
                                                 percent  hydrogen peroxide, freshly prep*«d from 30
                                                 percent  hydnxen peroxide  solution. The   absorbing
                                                 solution should be osed within 1 week of its preparation.
                                                 Do not expose to extreme htat or direct surijbt.
                                                   3^  Sample Recovery. Two reajecu «-•• required for
                                                 sample recovery'
                                                   3.2.1 Sodium Hydrotide (IN). Dissolr» 40 s NaOH
                                                 In d»ionii«d. distilled water and dilau to 1 liter.
                                                   3.2 J \Vai*r.  Deiontzed. distilled to conform to ASTM
                                                 sp*c.3c»Uc3 D 1103-74, Type X  At the opuoa ot ;h«
                                                      analyst, the K1CSO. test fat coidiubU orgaalg Batyc
                                                      may b* omitted when high eoooatrauoos U org-anjc
                                                      matter an not expected to Bo present.
                                                       . U Acaiysu. Vor lie aoalyiis, vtn loUawtcg rwgenU
                                                      annqtund:
                                                        3-3.1  FuminjSuUurleAeid. lStoHp«rcentbyw»i«al
                                                      tne nUur tnoilde,  ULs-NOLZ WITH  CAUTION.
                                                        J-3JJ  r'henoL Whlta solid.
                                                        3.3.3  SuUnne Acid. Conecncrated. « pancat mini-
                                                      naunanay. HANDLE WITH CAUTION.
                                                        3J.4  Potassium Nitrate. Dried at 105 la 110* C (733
                                                      u>230°F) foramini-n«mot2boufs)UgpnotMpJip«fa-
                                                      tioa o( standard sotuuoo.
                                                        3.3^  Standard  KNOi Soludoo.  Dls»»T»  exactly
                                                      2.1S8 g of dned potusium nitrau (K>'0t) la dtiomied,
                                                       cUnillrd water  and diluu to 1 Uur with dclaniud,
                                                       distilled w&ur In a l.OCOt&l volumetric Bask.
                                                        3J.8  Working Staad&rd EMOi Soluiioo, Dilate  10
                                                       id of the standard solution to 100 ral  with daiaruud
                                                       distilled water.  One sililliur of th* worcuut 3uu>^ud
                                                       aolution Is equivalent to 100 u* nicroten  dioude  (NOi).
                                                        SJ.7  Water. Oeioniud, dlsdUed as la S«cUoa 3.2J2.
                                                        3JJ  PhenoldisuUoaic Acid Solution. Dissolve 2S g
                                                       of p'ire white phenol la ISO ml coocentraud tulfuric
                                                       acid on a steam hath. Cool, add "5 cal  Ivuiing tuUurle
                                                       •eld, tad heat at 100* C (212* F) foe 2  haura. Sun 13
                                                       a dirk, stoppered bocUa.

                                                       4. Procure*                  .  '

                                                        4.1 Sampling.
                                                        4.1.1  Pipetu 25 ml ol absorbing solution lota a atmpl*
                                                       fMf, reuirdng a suAclfnt quantity for ow In prvnarvng
                                                       the calibration s'JJUiirds. lrj<>rt the f.iik T«IT« supper
                                                       Into the floii with the valve in the  "sarje" position.
                                                       Aswmhie the sampling  train  as shown in Fiiun 7-1
                                                       ar.d place the probe at the sampling potot. Mik» svi"
                                                       that all &ttingi an tight  and leak-Tree, and that all
                                                       ground ilsss  Joints have b*«n properly  grwjed  with a
                                                       high-vacuum,  higb-wcr-erature   cdoronuorecarbon-
                                                       b*i«d jtopcoci: grsa*e. Turn th» Railt  valve ar.d tha
                                                       PUSIB valve  to tbeir "evicusta" positlora. Eracuatu
                                                       the ."ji'i to 75 nun Hg (3 in. Us) absolute pressure, or
                                                       leas. Evacuation to a pr-ssure apprachuat th» v»tf
                                                       pnsssurs of wat«r it the et^urjr t«iapena:ra vs desirsiil*.
                                                       Turn Ui« pump v»i»e to its "vent" poiir.on and turn
                                                       cfT t^.e puzp. Check for leaii?! by ot««rvins the
                                                       no=eu>r (or aoy prssurt fluitusuoo.
                                     RDIRAL UCISTW, VOL  42, NO.  160—THURS3AT,  AUGUST 13, 1977

-------
 41786
        RULES  AND  REGULATIONS
grater Una SO mm H< '0.4 la. Hr.) OT*T a period ol
1 sils'-ru is not unpubl«.  and ta* fte/lc is not to b*
ur«* until UM leakage  prooi*m is corrected. rrtssun
la ib* ±uk la not to ejceed 75 am H« (3 In. Bt)*b*oluu
ai tb* am* sampuax U eomm*nctd. ) Record the volum*
cj th* flj«k and raiv* (V,), to* Bask umptratun (Til,
cod  the  barotxuale  preaun.  Turn ta* OuJE v»)v*
counterctockwue to lu "purgV poaltlon tod da th*
am* with tbe pump vaiv*. Pnr?« tbe  prob* and ta*
vacir.ua mo* osinf UK squao* bulb. li condensation
ocean In tb*  proo* and th* iVuk »al»« ww, heat th*
Croo* utd pum until UK eonduueUoo. disappears.
Jiean. turn tb* pump valre to its "vent"  paaaoa. Turn
tbe flask T»|»* cloekVa* to its "evacuate paaKion and
rtxrd the dllennoB In to* mercury l»veis >o tb* maoom-
«ur. Tb* absotau internal craaun La  to* ttaik (A)
fc a)as* to tb* barometric precsar* lea taa Tnanomeur
rwding. ba-r+dtauiy turn tbe oatk. valve to th* "sam-
ple" poxttlon and permit tb* gas -jo «nt«r to* flask tindl
y«a»uiB« In tb* Bask and sampl* Un* (I.*., duct, stack)
are equal. This will usually requir* about 15 seconds:
a tanner period Indicate* a "pluif ' in tb* prob*, which-
nan a* ecmcUd b-Jcre samplui* U continued, After
eell!eU2j tie aampi*. com ta* datk v*l»« to iu "porje"
pnrtC0B u\d disconnect la* Sask from  tb* sampuof
trii.n. 8na^» tb* uatk (or at least 5 minutes.
  V.J2  It ta* gas beiss; aaiap'wd contains Insufficient
«r7Y«a lor the converaan of NO u> NOi («-g.. in an-
Wicabi* lubpart ai th* suadard may pxjuir* ^^"t »
nnp» o4 a calibration JM minnn o< NO Ui Ni). Ow
or7.t;ii 3o*U b< loarx^cni into U» tuJc to perajt dlj
navMsan. Oxrt«n =uy t» lutrodtmd Into u>* f"*
bT C:B o< thm  neUxxlj;  a) B«lon opii2j{  flMir, stub vlUi port crUndx. oirjtn. U>ea
tvacouc Ruk u> 75 «nin  a? (3 in. H?) *b*otat« prosun
or ken; or C) tnj*et cxnm Into th« ftuX »Iur stapling;
Of (3) t*f%l£ft(4 BAQPUflJf Tttb.  fc Tnl^);T\lTTT« ol 60 mm
Eg  C In. H|) TKuum  remimlM LA tb« C.uk,  record
this ftaal prtoon, and  tiati Tint tb« Qjuk to th« u-
cxopbcra until •-&• £a*k premn  U aiaont «ou»l to
soaoopbwle prwturs.
  42  Sampl* R«oTWT.!«tth«fl*ik»tiar»m!i>usuai
o( 16 boun tod tb«a ahaka tb* camnu lor t minuu*.
wawr, to tb* itopoock. Meaiur* in* voltun* ol water to
=rJO ml. Rnord tbia voltcne on Ui* ftaik.
  1.J  Sp«Bropbo«om«t*t CaUbratioo.
  6.2J  OpUmam Wartlenxin D*ierminaiian. For both
fixed  and  -rartabl*  wartlenftn  iptccropnotomeun.
calibraU acatnM uaodard oerOAvd warnenirtb o< <10
am. «»«ry ft moalha. AlttnuUlTsiy, tar nnabt* taw
loojtb 3p»eam»>ocan th* ipectnun b«rw«ea
•400 and 416 on oso* a 300 we N Oi acaodard aolaUoa (M
S»etion S.i2). II a peak do«s uot oerer, tb* speewopho
tom«ter Is probably tnaUaneUoninc. and should c* r*-
paired. Wh«n a nttk h obtained wttbin the 400 to 415 am
range, th* waTden»tn *t wnicn tbis peak occurs shall b*
the optimum wankn«tb (or the measurement ol ab-
sorbano* (or both tn* (Undardi and nmpte*.
  4.2.2  Determination o( 8p»etrophoUim*ter CaJjbra.
^lon Factor E. Add 0.0. 1.0. 10. 3.0.  and 4.0 mi of UM
KNd working standard solotton (1 ml -100 w NOrt to
a serial o( fir* porwlain «»«oor»Un» dlshw. To each, add
25 nU o( absorbinf notation. 10 ml deionlted. dtstUled
•nitr. and sodium hydroxide (IN), dropwise, until in*
pH il between 9 and 12 (about 2J to 3S drops each).
Bfldnmmt with tbe tTmporatlon step, follow tb* analy-
st] procedure ol SeeUoa 4.2. anUl th*  solution bai be«n
avatmvt to tbe 100 ml Tatumioric flask and diraud (o
th* mark. Meamn Uw abaorbanc* o< Mch »loUon. at th*
optimom wavelength, as determined In  Section &.2.I.
This ealibraUon procrdnn must be mp*ated on each day
that samples ar* aaalyied. CalcuUU the speetropboiom*
rter calibration factor M loUowa:
  (.4  Sampl* concentration,' dry basis, corrected ta
standard conditions.
 Open Un valve tram tl» Bask to tb* maaom*ur and
 record  ta*  flask temperature (T/),  th* b*rom*ol«
 prwsure, and the diAtrmc* between tb* marrory levets
 ti tt» maaam»t*». The  tbaoluto inuroal prMsur* In
 ts* nw'c (Pr) Is tb* barometric pretaon less ta* man-
 cmewx rndiag. Traosler th* cocunu  ol th* flask to a

 vltri vml portions ol dtkmlud. dUUUM water and add
 tb* rinse watar to th* bom*. Adjust tb* pB to between
 « tad 12 by addia* socliuai byaraod* U N), drop-n**
 (about  25 to U drops).  Cheek th* pH or d3ppln« a
 rUrriax rod into th* Mlcaon aad then  touching tb* rod
 to tb« pB test paper. Remove M llctl* material as possfal*
  • tizg this sup.  Mark ib* beupxt of tb* liquid Uv«4 »
      tb* container can  bo cb-jcod for Wka/te  after
          Label  tb* ora:xnw u> claarty identity  it*


 and confirm wbetber «jr not aoy ample wu lost dunnt
 shiptcrai; now this oo th* anatyticai data sheet. If a
 aotinsble amouat of leakao bu oeeorred, either void
 UM umple or us* mMbods, subject to th* approval of
 tbe AdalaiscMcsr, to comet tb* naal  results, Unmedi-
 auiy prior  to analysis, transfer the  coatenu of tb*
 thippiar, coatauaer to a 50*ctl volumetric &askr aad
 ruvM tbe coatalaor twice with 5-ml portions of deioaiied.
' ditlll*d **Ur; Blur tb«*«
  ihrM rlOM*. Wuh th* ruur with at  l*art ;hr«.  15-ml
  por.ions  ol doonlud. dlrull*d water.  Add th* filter
  wejhiao tn tht  onnunta of  in* 'volumttno ^Mt aad
  dllut*  to tti* main with dtlonii*d, duuUed water. If
  inllili an abxni, ib« Mlutloa can b* rrarjicrred directly
  t.i tb*  100-ml volumitnc Auk and dlluUJ to th* mark
  with diiooltod. dlstUM wuur. Mix th* coateau  ol th*
  fact t^orouitbiv, and raaasur* Ih* abserbanc* at  tb*
  optimum w«7tuen(th us*d lor th* nandards (S«ctioa
  i J.I), uiim tb« blaiix somlion as a uro relerance. OiluU
  the sunpld anil tbe blank with equal  roluaas ol delOD-
  tud. dlsiUrd water il tbi abaorhaac* exceeds At, tb*
  ab«orbanc«olthi400w«NUisUadard  (aniiKUoniJL:).
                                 Equation 7-1
 where:
  .Ef.-CaUbntiea (actor
  A, - Absorbent* o( th* 1(XV»« NOt standard
  AI- Abeof banoe ol tb« 200^4 NOi standard
  Xi-Abwrbaooe at tb* 3O>»g NOi staadam
  At- Abaorbanc* o( tba 40t>w« NO> (tandard
  V4  BaronuUr. Calibrau a«alnst a mercury barom-
 •ter.
  5.4  Temperature Oaoit*. Calibrau dial tbermonMltrs
 against mercory-tn-fiajs tbermometen.
  5^  Vacnom Oam*. CaUbrat* nwcbaalcal note*. U
 osed, analnst a mareury maoomtter socb a» thai speci-
 fied In 2.1A
  5.8  Analytical Balance. Callbrau  acainst standard
 •weights.
                                                     Carry oat tb* ealcalaUans, retalnlnx at leait one extra
                                                   dedmaj nfor«-a*yond that ol tb* acqolred data. Round
                                                   off atmta af-er anal calculation*.
                                                     C.I  Nomcnclacore.
                                                       A - Abwrbance ot am pi*.
                                                       C-CooeenmUon ol NOt aa NOi. dry  basis, cor-
                                                          rwud   to  standard   cooditlooa,
                                                                 .
                                                                  bctor (le,, 25/5, aiO.  eU.. required
                                                          only i( sample dllntlon was aexled to redoe*
                                                          the abnrbanc* Into th* rang* o( calibration).
                                                      K t— 8p«ctrophotom«t*r catibratton lactor.
                                                       m— HassoINOtuNOiln (as sample, of.
                                                      P/- Flnaiabsohit* pressure ol (I ask, mm H( (In. Eg).
                                                      ^i-lnitlal abwJut* pnason ot Oask. mm Hi UQ-
                                                          BK).
                                                     P.^- 8 tandard abaotate pressure, 7W) mm U( O.Kin.
                                                          B<).
                                                      T/-Finalab»ohjUt«np«ratnreo( flask ,'K (*R).
                                                      T/- Initial absolute temperature ol flask. *X (*R).
                                                     T«<- Standard abaalnU umprratur*. 293° K (228* R)
                                                      V.,-e*mpl* Tolnm*  at  tundard  condiOoni  (dry
                                                          basis), ml.
                                                      Vr»Volom« at flask and ralr*. ml.
                                                      V.- Volume of abwrbirjt sohillon. 25 ml.
                                                        2-MV25, tb* alinoot lactor. (K other than a IS-ml
                                                          allqoot wa* avd  (or analyji*. the comapood-
                                                          ina (actor must b* sabstltut*d).
                                                     a.2  Earnplt yoreme, dry barts, correct*! ta standard
                                                   condltioni.
                                                    cher*:
                                                                                     Equation 7-2
                                                                      °K
                                                      A',-0.3858 —^rj- for metric units
   SI  Vlaali Volnrct. Tbe volume ol tb* collection f.iik-
 C.v.p. 7^ive combination must b* known prior tn san-
 plicf. Ajwmblc Uj« r.iit and nuk valvp and till wiLti
                                                          -17.64  f-ft" for English unite

                                                          Total nt NOi p*r sampl*.
                                  Equation 7-3

   Notz.—K other than »2.Vjnl aliquot I) used for analy-
 sis, tb* (actor 2 mtut be replaced by
 Itf.lot.
                                 Equation 7-4
where:
    ,- 10"
            jig/ml
     -6.243X 10-» ^^ for English unit*.
7.

  \. Standard lietbods of Cbemical Analysia. «th td.
New York, D. Vaa Nonrand Co» Inc. U42. VoL U
p. 329-SO.
  2. Standard Method ot Teat (ar Oxides of Nhrortn la
Oweoto Combustion Product* (PhtnotdisuUonx Add
ProredDre). In : l«iS Book o( A3TM Standards. Part 2&.
PoilaUelpoia, Pa. 1968. ASTM Dcmsnaaon, D-UOO-60,
p. 725-729.
  3. Jacob. M. B. To* Cnamlcal Analysis of Air PoUnW
anta. Sow  York.  latencieoc* PniiliiSers, lac. I9o0.
Vol. 10. p. isi-aai.
  4. B«aRy,  R. I_, U B. Bcrftr, and H. H. ScisrtnlE.
Determination o< Orid« of Nttroaen by tbe PiMDOtdfeaJ-
tonic Acid M«thn«l Banaa  ol iiinca, CJ. O*pt. ot
Inurtor. FL I. XS7. February 1MX.
  4. Hamil. H. f.  acd D.  E, Camann. CoUabonttni
Study  o( Metbod lor the Determination of Nltro^a
Ocd« Emissions from Stadonary Source* (FooiU Fliei-
rtrrt Steam Oecentors). Southwest Reoearei Ic5dtst»
report (or £nTiraameatal Protactloa Ajtccy. 'Himareh.
Triaosl* Park. N.C. October 5, 1773.
  6. Hamil. H. f.  and B. 2. Tnomas. CoDaboratiTV
Study  ol Method tor th* DrtarmlnaUon of Nraroc*a
Oxide Emissions mm Stationary Source* CNide Acid
Plants). Soatirwest Baorth, lojtitvn* report (or Erv-
Tironmiotai Protection Agtncy. Pmosrrti TrUorb
Park. N.C. May 8, 1974.
MCTSOD S— DzmuczxxTtoM o»  Struwc  Ar™
  AMD  SdJTja Diozmi Eicaaio^a now
                                                   1. Proofl* and ApfUalOlH  ' ' ,
                                                     1.1  Princlpl*. A ras sampte Is extracted bokii>*t!ea2y •
                                                   from th* tuck.  Th* soUorie acid mist (Indndins JoiTur
                                                   trioxide) aad th* raltar dioxide an separaud. aod botti
                                                   tractions ar* measured separately by the banma-Ujona
                                                   tiaKtloo metbod.
                                                     \2  Applicability. This nutbod Is appUeabU (or tb*
                                                   determination  of  solraric acid mist  (including soUor
                                                   trioiida, and In tbe absence of other parUcoUt* matter)
                                                   aad sultar djoiid* enusitona (rom sudoa&ry aooroaa.
                                                   CoUaboraQT* testa  have shown that tb* minimr.™ •
                                                   deuetabl* ILaJo ot tha method are 0.05 milllcnu&si'cnbM
                                                   meter  (O.COXICr'  poubds/cublo foot)  for suUnr moiid*
                                                   and 1 J m&(m> (0.74   ia-> IWltl (or raUur dioxide. No
                                                   opper limits hare  been established. Based on theoretical
                                                   calculations (or 200 mlllUiien  of 3 prronot  hydrogen
                                                   perotlde solntioo, tb*  upper  concentration- limit  tor
                                                   goiter dioxide in a 1.0 m> (15J It1) |u sample Is aboct
                                                   12,500 mt/m> {7.7X10-1  IbAt')-  The upper Umlt can b* -4-5
                                                   extended by Increasins UM quantity o/ptraxid* soluttoa
                                                   in th* impingtn.
                                                     Possible Interferinf agents of this method an fnorideo.
                                                   tree ammonia,  and  dimethyl aniline. If any of  tbes*
                                                   Intertving ateats an preaont  (this can be deuraliwd by
                                                   knowledp ol the  process), alternative methods, subject
                                                   to  tb*  approval  o( tha  Administrator,  an reqniiwl
                                                     FUurable particolau matter msy b* deurtclntd alon«
                                                   wltb SOi and SOt (sab)ect to  tbe approval of the Ad-
                                                    mlnistmor); how«rer, tb* proeedon Died fsr parrlcaUu
                                                   matter must b* cocsiAant with th*  speclncadoo* aad
                                                    procedore jlTto in Method 5.
   2.1  SampUnii.  A 9cbem»tie o* th* sampUas tn
 used la this method Is shown In ?l«ur* fr-k; ft is srmlUr  .-::•)
 to the Method 5 train except that the. alur pMldoo Is
 dl(fer«nt and the Blur holder does not hav* lo M h*aud.
 Commercial model* o* this train an available. Tar tboa -r
 who desire to build their own, however, compete on»-  •'
 strucrlon details are described la APTU-0581. Chan«*s
 trom th* APTDXU81 document and allowabl* mcdV
 fteations to Flfure ft-1 ar* t>':
 SKT. pllnj train sre described In A PT D/S74. £inc» correet
 uta(« u Unponant In obtalninx vaud rnolu, aU tts«* •
 should read  the APTD-C676 document and adopt tb* ~
 operatinf and malnunanoe procedures out!ln?«l la v,-i
 unless otherwise speciAed herein. Further  details and «^
 iruldellnea on operation and ctaintenanee are (Sveo in •"
 ,M-ihc4 5 and should b* read and tollowed whenever •
 they are applicable.
   1U1 Ptob»Nottl*.8am«asMelhod5,9«ctJonJJJ-  ^.y,.
   2.1.2 Probe Uner. BoroeiUcataor quarts glfc*, «1'JLJ"?^,
 beaiirt jyr.'m to prevent viable eondewatioa dune* Aff -
 «a.-Bp;mj. Do not UK ra«a! probe llwrs.              ~\
   2JJ  I'ltot Tub*, aamtss Method 5, SeeO*>oS-L3.  -
                                                 MGISTSI. VO4. «S, NO. 160—THUISDAY,  AUGUST U,  1977

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                                                  RULES AND  REGULATIONS


                          TEMPERATURE SENSOR
                                                                                                                                  417S7
                                         PROBE
  OB£
                     PITOTTU8E

                     TEMPERATURE SENSOR
                                                                                                           THERMOMETER
                                                                    FILTER HOLDER
                  /
                                                                                                                       .CHECK
                                                                                                                      /VALVE
  EVEF5E TYPE
  tITOT TXJSE
                                                                                                                               VACUUM
                                                                                                                                 LINE
                                                                                                                          VACUUM
                                                                                                                           GAUGE
                                                                                                             MAIN VALVE
                                 DRY TEST METER
                                         Figure 8-1: Sulfuric acid mist sampling train.
 1. DtSutnlUl Titaan G»uj». Sun* ai Method i,
 Ita 2.1.4.
 US FQtcr Holder. BorariUe&te (!aa, with a gh»«
 UUf ivippon »-d a silicon* rubber (nittt. OttMr
 jlzaatenaU. e.j., T«flon or Viton, may b* oaednib-
 ff tba approval ol the Administrator. Tbe holder
 p'shall provide a poaiUf* MM uaiaa lr*Xa» (.-on
 luidn or around lb« liter. Tb* ftltar boldtr shall
 iiiod betwMo tbe ftr« ud Mcoad Implnjin. Nou:
 col beat tbe filter hoidtr.
 16 IsipUif!.-*— Four. aj ihown In Tlnre H. Tb«
 ind thirl  il^ili i* o( tb« Orenburg -Smith datra
 i"rj3d*rd  up*. TtK wood »nd (onrth iluil be of
 Orwobun-Salth dwljc, mcdifirt by rtplaclne th«
 n;»1ih »a »pproiiffi«ulT 13 icJJianut (UJ In.)  ID
 i lub«, tl»rlnj tn uucoastn.-uil Up lockUd 13 mm
 S'.l (ram tt« bottem o( \ta lUwlf. SunUtr coU*ctloo
IBI, which &*•• tr«a ippro'td by ih« Ad=ii£u>-
or,' CUT boawd.
  - M«t»n.-vj  Snum. S*m«  M  Method 5, Section
                                              12.4 Trlp'B&Unea. S0&frmme»p«dt7, tommranto
                                             ±OJ ( (owaurf only U i moinun content &nal• iix- 1« u*rt.)
          OnUu. L»»».fr». p«i!yelhyleni hotUie,
        -o»L'rtoJ
  X7nleai oibendM Indicated. eJl r**«enu «J> to conform
to the spwinauon* e3l»hlish«d by the Cnamutr* on
Analytical T.t-wrntt ot tbe Amehc&n Chemical Society,
where rocfa ipctfleattoni an irailabU. OUienrtM, lu*
the b*st armllabl* (nde.
  SJ  BampUnf.
  3.1.1  Fllun- 8am* ai Method J, Sectloo 3.1.1.
  3.1 J  RlUea Oel. 6»mf ai M-'.hod S. Swtloa 3.1i
  3.1 J  W«». Delonu»d, dw-.lied to conform to ASTM
sp«M3caUon DtlM-7«, Trpe 3 At tne or' ion  o< th*
analyn. Ibn KMnOi test for ortdiiable orfitnic matter
may be omitted when  hlih conanxnulonj a( orgaalc
matter are not eipccud to be preMm.
  3.1. i  bopropaool. 10  Ptrcrnt.  Mix !00 ml of bopro-
panol witt 300 ml. of daloolxed. dljuUed waur.
  NOTX.— Cxperienn hu thswn that only A.C.S. trade
lsop;oc*not 1)  m:\ititelarf.  TCJLS c»»« ihown  taat
lioprapanol oM*m»d Ircn  ccc^cxrcial gourcu occa-
caunntlly Bai ptrotide  Unpunue* uat will cam* u-
roeeorair bifb raltarle add mist Beasomn«nl. TJj»
the followiag Vast for det«etlQ( p«nxide3 in each tot of
l»prapaaol: SSate 10 mi of tbe iKpropeaol witb. 10 tal
of fmaly prepared 10 permit potasiitua loviide aolatioa.
Pnp&n a blaok by lusUarly tmUnt 10 ml ol disuil«4
wtt«r. Alter 1 raiaate, read the abaor be>aee on a •pectro»
piotonettr at Ii3 oaoomeren. II tbo aSs« bane* exccecU
0.1. tbe iMpropanol gbaU not be UMd. Peroxides may bo
r&tnoted from i»prop«Aol by rcdlstUilol. or by pevna^
through a column oJ acCvKd alamioa. Hcrwrrrr. rv-
a^eav-fradelsopropanol wita sniubly low peroxide lert Is
Is readily a*«iiaol« from commercial  KOTOS: therefore,
refection of contaminated  lota may  b« more eQciant
than following th* peroxide removal procedure-
  3.1.5  Hydrotea  Peroxide. 3 Permit. Dilau 100 nl
of 30 D*rm.".t bydror» n peroxide to 1 liter WIL3 deioalMd,
diftiUed vmur. Prepare (ntti daily.
  3.1.8  C.-tuhrdloe.
  3.3  Eaavle rucorerr.
  3J.1  Wbtcr. Suoe u 3.1 J.
                                                                                              3.1 Anaiysix
                                                                                              3 3.1  W&ur. Same u J.1.3.
                                                                                              3.3.2  l!«propKn«l. 100 Perrtnt             .  .  .
                                                                                              3.3.3  Ti-5-io lodlcator. l-(o-arsooopheoyUio)-2-ciapbr
                                                                                             tbnl-3 6-i;>i:Jonlc acid, diwdium so4t. or «ol»e O.M c In 100 ml ol delonlied. dlstll>d w»uir.
                                                                                              3.3.4  B&rlum PerchloraU (0.0100 Normal).
                                                                                             In "JXi tr.l deionlted, diiaUod w»nr >ind dilau to 1 liur
                                                                                             with lanprotMnol; 1.3 g of barium chloride dihydrst*
                                                                                             OaCli '-HiO) may be u»d irutewl ol tbe b«--3Jn por-
                                                                                             chtomte, S'.and»rciii« with jul.'ur.c acid ai in ration J.Z.
                                                                                             This voluuon m^r. b* proucud a«&lni\ eraporauxt at
                                                                                             alltimao.
                                 FZDERAl RKSISTH, VOL  43, NO. UO—THUWOAY.  AUGUST  18. 1977

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417S8
       RULES  AND  REGULATIONS
       SoUnm Add Starxtod (0.0100 N). Piur'iam at
             =UODOJ N trtla« OOIOO N N«OH t&M
h« previously  t— ^0 sttadardiud kgBlm  primary
standard pouaviu&i acid prrrhtUtt

4.
      : rttain » portion of each m«nt far OM u > •
bUok Mbulao. PUo* kboutaxi t o( ubc* t«l in UM CounA
             .      -
  4.1.1  PT»I««I Preparation. FoBow th« praednn oat.
lined la Method i, Beetlan 4.1.1; filun sbould b» ia-
cctcted, but need oot b* dtaiceattd. wmdwd, or ld«na-
lied. If tbt eUa«ai iru cau b* cocaidtnd dry , L*. , mau-
lers Ine. Ul« alica g«l need oot b* w«i«b*d.
  4.1.2  Preliminary Determinations.  Follow tb* pro-
eKture outlined 10 Metnod i, Samoa 4.L2.
  4.1.3  Prepartuio oi CoU*eeoa Train. FoUow it* p«o-
efdurs  ootlinad ia Mttbod i, 6*cttoa 4.1.J- (tietpt toe
the second pamrspb tni otatr obviously luappucabU
pans) ted os»'?ljrar* 8-1 instead cJ Fljnrt b-i. R»Dlao*
tie vrond parazrapa *1Ux: Plan 100 ml at 80 penult
tsoprcpaool la tfl* ant lmpiMi.tr, 100 ml ot 3 pwetot
byilrcf *a pwoxld* ia bota tb* second aad Curd ua>
  Non.— U motjmrt oootcct li to b* deUoainid Vr
liaplni«r Mulyns, wajb e*cb oX tb» first Um* Unpir-ftn
(pliMfctnorOUK aolddoa) to U>« M*raa 0-b t *od nraxd
tarn wii«liu. Tt» i»«iKbt of to* «iUo nd (or siUc» ttl
ploj ooouin«r) mod »l» bo dMamuua to Ui» HMnat
0-4 » mod recorded.
  4.M  Fntcst  L««k-Ctn)dt Praosdar*. ToUo*  tb«
bane pnndun ouUiowt la Hetbod 5, SKOOD 4.1. ti,
Doting tax tit prate bwxr io«U b* «d]usud to Uw
T^ntt^mi}  td&ponton  n^olnd to pnTWt ooade&a**
ttoa. tad tin tbM Yecbtz* 9uct> «.*•••• plwgiog UM
Inirt to  Ui« Uier bolder • • V" so*U b< noticed br.
..... plcniix U» iaM to to. But lapui«ir • • '."
Tb* pnucTUu-cntek 1> optloo»L
  4JL5  Tnln Opentloo. Follow th« bade  pnecdom
omllo«d la Melbod 5, Section «.U. In coaloaeooo -vita
on tibMtamOtf toth«on« la Tijrart ft-2. Tb4 nmptint
nu 3^*11 not «c«nl 0.030 JB*/OUI (1.0 ctn) danac UM
ran. PenodiokQr du-it>t in* i*n, obw-ri to* ooaixctUMi
            Uir prab« tad Ant Impinjcer (or ncxui o(
            U It dog* orror. *4]us Ui» prab* bamur
            d to to* Tr>tr.>fWMt« tAmp4ra£Qz% nqatxwi
to pnTvnl coodwuttioo. II aa)
tooted tb* xpKliad nU, UM U*t*T >b*U clUMT roid til*
ran or 30*11 pUa to *orract to* «apl* Tolaia* *• oat-
Ua*d la 0*eflott4-3ot Mctbod &. Tmrn-Hii'tiT ttttf oonw
pootot  chaotu,  w«t&iid»tory) leak-
 ehwJc M la S«:uun 4. 1.4.3 or Metaod 5 (wilti tpprophau
 moc2>1, vitb tbt prabidiMonaiYbM),
 po—t tte rrt of tbt train, by drm»Tax clr*a
 « .'M.-j-.t ill -.hrai;;.', th* «m«a lor 15 ciinuus *t tS«
 a • •:.-%* flT» rut Ox-d lor «uapUs(.
   Nqn.— C'la«n tir.tl-nt all coa bi prorldtd by p«ula(
 all ti;ou7h & ch.vcukl iUur. A*, thr option ol tit tnUr,
 c.Tihi«at &;r \wi Jiouc d^*i"JnK) ^^7 t*« U3*d.
   4.1.4  CtkttUtioa ol Purnnt L«akinctie. Fallow tbt
  '
   •i.li  Coaulnv No. i. u t nol^an ceouat uuiru*
             Flgur*<-2. Field dau.

 li to be doo*. w«i|b th* tint Impinfv pln«ue5tOJ|Uidrecord tbi» wjjght.
           tn« contents o( tht firs lapin«r to t JA>cJ
           cylinder. Rirvs« the probe, ttrrr impingi-, ill
          ! iltssw»r« brfore tbt filter, tod tb« Innt Sai.'
 of tbt ftlUr bolder u-tth SO p«rce=t t3opror>tr."(. Add tb*
 rtoM tolutlon to tbt cylioder. D'.luw to liO nil with 80
 percent isuproptaol. Add tb« filter to tht Klutton.  =ux,
 tnd Uvultr to tbt jtorut eoauiaer. Protect th* wluzor.
 t(«lr.n tTaporaticn. .v*vk tbt level  ol liquid oa btt
 conulntr an-', identify th: »mpl»coat*aner.
   4 J-3 Cont«lc;r No. 2. If a rcsuture conten; iriimi
 Is to be don*.  w«uh  tbt second ind t^iid ins'j-.j-rj
 (plui conunu) to thu o»--est OJ>  |  ted  record  [hn«
 •vrti^au. Also, wtivh. tht sp«nt silica (el  (ot aiTca ;•!
 plus tmpi.-.:r-r) to the a««nst 0 J j.
   Tniuler the solutions trora  tht ncond  tnd  tbird
 taplfueu to t lOOCvinl undiuud  cylinder. Rics* til
 cotmectlnx tltsr^an ita^ludintbtckbtlt ol (Uitr holder)
 b«tw«*a Uie tlur uxl Uiic* etl Us plater wkUi -Wnr,.;i«<1,
 dlstiu*d wtur, sad edd this rins* inror to tb*
 Dilate to t volume of 1000 rrj vrttb dtioau«d.
 wst<7. Transfer t^e sotouoa to t stor&se coQt*latr. Mark
 tb* lerel of liquid on tb« coauioc. S<&1 tiid ideatirjr U*
 umpl* coattiner.
   4J  Analysis.
   Sou tac icvel ot liquid ia cont*ia«mtad2. tad no-
 tea winter or  not my sample vu lost durvcg ihlp-
 — er.t; nou this oa tht aaaiytical dtu sh«i. II t aottc*-
 tole &ziou=t of  Ib&^u^t bu  occurred, either void dt
 SB.— p> or UM rjettjdj. sublet u th« tpproTtl of tie
      ii-.c'-ei.
   4J.1  CoQtiiatr No.  1. itatt tti container boldly
     teoprop&nol solatioo and tb« filter.  If tb*
                    -
 drops of thorin Indicator, and ::fM ta* tttruiou
 Tim t Mcocd tUquat of nunpl* ted iT«r»i« th* UtriUoo
                                      FEOIZAi REO1STU,  VOL  
-------
                                  RULES  AND  REGULATIONS
                                                                                41789
T*!DM. lUpUcaU y trailon* meat tpw wtthin 1 peraoi
or 0.: ml winch* w LJ greater.
  4JL2  Coauuwr  No. 2. Tbcrtwjiily *"'« tb« «"i"*""
In th« container balding tbe content) of UM wcooxl and
tuird Lsslnicen. P1p»tte * lo-ml iliqaot of jampi* Into •
230-ml  ErUameye/ (Luk. Add ml o< bopropanol. 2  to
4 drops of taonn IniUcttor. and tltnU to a pink end point
nolnc 0.0100 N b«rlQm p*cr^Lbv«£«. Bepeat th« tftratiAa
wttb. a oeooad aliquot o«jampU aad armr* tn« tt&atida
rainae. Replicate dttatlooj man agrv wimia, 1 p*rmt
or 0-3 mi. wblefMnr li cnacer.
  4.3J  Blanka. Prepew» blanks try adding 2to4drep«
o( tnorln Indicator to 100 ml at 80 percent bopnpual.
        h. hl«Jlk7l In th« ..TTI. nr .nr...
  M  Gallant* etroipmaiit tains t&4 pnradnm imei.
fled In Uu foUowtn* section* o( JUtnod 5: B— -H™ JJ
(suuilaf lyjum); Section  i-S (umpcratzm gaogM);
Section S.7  rbaromeur).  Nou toat tb« recommended
lau-choci: of tb« mturiox rjTWm. d«cr.bed la S«cOea
&4 of Mjtbod 5, aljo appUM u tHi_< miUxod.
  U  BUadjkrdlM the Danraa pcrchknu nlotlao vith
23 ml of n«ndant  saUurld acid, to wtUcn 100 ml ol 100
ptrant ijopropaaol bu brna »dd*d.

8. CslnlaOau

  Note.— Carry cnt csicnlAUotu nUlnlct at U>ut oo«
ertra decimal imr» txytiad tbat of UM acquind ti'*
Hoond off Oinrr« att«r n^mj <»*i/-nUttOT^
  (a  Nnm«ncl»tcj».
       /4.-Cro«»-v«nloD»l ana of ooiila, EI> (ft1).
                 vapor  In tS« zu ICMHI, proportioa
                       flncladlnt SOi) cooowtntioa.
             t/dvm Ob/dacT).
     CBOi-SaJm- dJonde coacanlndoti,  i/dxm Ob/
             cbc/).
        7—Perwnt o(l»lcin pnaan, mm Hf (In.
TOO
        Hi
                .
     ?"l*d-8Undird
             03.92 In. Eg).
       I". - ATertio ibaolnui dry ru
             (>M Flra» S-2), • K r B).
       T.— AV«JTUJ» abwluU jtack jilUmpaniom (M*
             Fl)itir»S-2).' EC H).
     Tttd-SUndxrt  abwlut* Umpcraton,  293*  Z
             (53« B).
       V.-Volun« of sampU lUqoot UtraUd. ICO ml
             for H>SO« and 10 ml lor SO >.
       Vj.-Total Tolomiof liquid oo CUcUd In l2pln««n
             and tlk» tti, oL
       V.-Voltcnu o< rai mmpl« u mc*Jond by dry
           ru = m«t«r camaM to ninrtird coadiUaai,
        ».— ATETSO T*at>  ?*» nlodtr,  calcalat«d by
           Mnbodi. Eqoanon2-«. crcji* data obUincd
           from Metiod 8, m/Tne Itttxx).
    V»ln- Total Tonxc*  of  wltruoo In wblch  the
           mitortc  ixld or lallnr  dloilde sunpl* Lj
           contaiaod, 2.V ml or 1,000 ml. rnpKUTtly.
       Vi-Volcan*  of bariara porcnlonu tiuut tuvd
           for tb* saxnpiA. ™*-  .
      Vit»Volam«  of b&daa perchJonU tltrmnt tatd
           for tb« blank, ml
        y- Dry s«J  met« odibrttion factor.
      ^W— ATSITU» pressure d--T>p tcroa orLOc* met«r,
           mm (In.) HpO.
        9 — Toul sampUnf ttm«, min.
      13.8-8 p«clJlls trSTlty of UMreury.
          » Cooraniorj to p«mnt.
          no dry »« m«*r t«mp«r»tur» and
      prunin drop. €•• data 3be«t (Tlf ur* ft- 2).
  8-3  Dry GUJ Volume.  Comet tb> lamplt Tolcun*
mtasurvd  bf tbt dry xaJ mrl«r to standard  conditionj
Car C and 780 mm Hj orM* f and 29.32 tn. Hj) by nsifl|
Equtloo i-1.
                                 13.6/
                             . P^-KAtf/13.6)
                                 Equation 8-1
              ,     Hj for mitrlcanJU.
    -17.44 'R/ln. HI lur EajlUJi unite.

  NOT!.—If the Ua* rmte c^^er^f dncrlt-d la P«ction eJ of Metbod i), or ihall
      at* tte u»nip»F

                  1. Atmo3t&Gri£ ^misilooa CTOTH Solfnric Add MACD»
                Jactnriiii  ProcsOM. OJ. DHEW.  PH3, Dirlilan of
                Air PolTotioo- Public Healtb Serrice Pnbliollnn No.
                9W-AP-13- CLnclncsti, Ohio, 196J.
                  2. Corbttt. P. F. Tbe D-temunilkiQ of SOi and SOi
                In Floe Q&M- Joom&l of tbe Iiun raw of Fuel.
                1901.
                  X Martin. Robert M.Constrocttoo Deta3a of
                Soorca Samp ling Equipment. ED TITO am en Lai Protection
                Agency. Researcb TnanjU Pali:. N.C. Air PoUntion
                ConDTil OCcs Pablteslion No. AJTD-OM1. April, 1971.
                  4. Pirtoa, w. F.and J. A. Brtai. Jr. Ne» Eqolptnaot
                and TecboiqaM for SitEplinjs Chemical Pmcxa Gasea,
                Journal of Air Pollution Control AJaocUtLon. /3.-183. 1»«3.
                  S. Bom, J. J. Maintenance, Calibntloo. and O wralaoa
                of  Ijotuetio Source-SaapUn«  Equipment.  OQc* of
                All Protrami,  Earlronmental  Pro^ction A««ney.
                rUatarcb. Triaafle Part. N.C. APTD-Ci7S- March. 1972.
                  j. H.mii  £L  y. »ad  D. E. CamAnn. Collabontir»
                Stadr of Metbod  for Deteraiinadon of Bolfar Dioiid*
                Emlislonj from Stationary Sourow  (Tond  Faal-Flred
                Btecm Generator)). Enrtroam»cuJ Prot«ilOQ AisncT.
                R«»arcli  TrLinjl* Park,  N.C.   EPA '140/4-74-001.
                D«««mb«r, 19T3.
                  7. >nnn»l Book of A9TM SUndarda. Part 31; Water,
                Atmoapherlc Analrilj.  pp. *0-(2.  Amfrlcan eoci*tr
                for  Tanln< aad lUurlalx Pbiladalpbia, Pa. 1»74.
                         •       •       •       •       •

                <~ra. Ill, 114. 301 (a). Clean Air Act.  »c. 4(a) of Pub. L.
                Sl-604, >4 But. 16&3; »c- 4'a) of Pnb. L. 91-604. W Stat.
                1SS7;  MC. 1 Of Pub. L. 90-144, 81  Stat. 504  [42  OJ.C.
                Ui7c-«, l§STc-», l*S7g(»)).)

                    (rBDoc.T7-13S08 Piled 3-17-77; 8: 43 am]
               FJD£«AL  RECISTf*, VOL.  42, NO.  160—THUXSOAY, AUGUST 18,  1977

-------
             Attachment G
Determination of Particulate Emissions
       from Stationary Sources

-------
                                  RULES AND  REGULATIONS
                      M,  wrt It lnu> '.b«iuck, ud
lample at a camum rue  ine
ourut OJ ml
  3.3  ral(mi*fum« TK^a^l—rcfrtJ^ nfrtth'HI p***^"t.»c-
carau mautur* dxUEmtaadm.  arr  rvM coll«cud. Tti«
lollowtnf oqtmiiam xUqtcu«i7  •«jnui>  tn* moutar*
amtcnt. for tb« porpaM a( d«^iiunic« Ivluneuc sam-
pling r»ia saciinct ^ .--" •-t»I— \i«
  SJ.l  Noromci«Ou»-r-  --
                     >; profnnleo.  br  ^oliimr.   ot
                      tn li»-CM tuxam IOTUI; th«
                        . """»
                                           ion by
                                                        3 J.4  AppraiiauU
             .
      P.- Abootote
          barametrio.
                               Ow> dry K" oner.
                                      T60  mm H{
          l in.  Ht)
                 .    i—
                ru anbun, aoern (mm HE)
                        (or Tn«ir*e  omu wid  21.45
                                 Til)  lor
                              »t mciT. "K (*R)
                  -          tunprraran,  iO*  E
          (528" B)
                                r eontmu, mi,
                                    n(»nu, ml.
                                  br drr r" ffimr,
          dem (dd)
   V.l.m-Drr ru-nteo* mM«iml b? dry m tn»t«r.
          comcud  t»- ntadard  ooodluou,  dxm
          (djcfl.
  Vr.<(ur>m«ur). Tb« rtcommecdeJ leak
check o< th« mntanm Jysu™ ( Section i.8 o< Meuvxl i)
&ljo ftppi]«a u> tb« re/er»fKv ^ipLDod. For tbe apprann»
tlon method. UM tbo procedurw onillned in Secdon 5.1 J
o/ Metbod fl ui caliDrau Ui« metering 5T5teiru and- Ui«
prondon  ci  Metood i, Sectxm  i-7 u calibnu ti«
baj omet«r. '         ^
  1. Air Pollution Engineering MAUO»I (Second Edition).
Danlelacn, I. A. (ed.). U.S. Znvirarunenm Prot«3on
Ag§n ayallible. For chaMes from  APTD-06S1
 and for aliomble modiAcaLlona oif the train ohovn tn
 Figun £-1, M< tbe following sabwcnoro.
  Tne  operutlnc and  maintenance  pr«r*dur»3 for the
 sampling train are described In APTD-0578 (Cltacion 3
 In Section 7). Slnee correct uaaje ia Important in obtain-
 In It ralid rwalo, all users sbodld read APTD-iSTJ and
 adopt  tbe operating and  rnaintenanc* procedures oat-
 lined tn it, nnJesi othenrlse specified herein. The tan>
     train consists of the following components:
                FIOIRAL IECISTH, VOC 41.  N
-------
                                                       RULES ANO  REGULATIONS
                                                                                                    4177;
                          TEMPERATURE SENSOR
                  REVERSE-TYPE
                    P1TOTTUBE
                                                                                 IMP1NGER TRAIN OPTIONAL, MAY BE REPLACED
                                                                                         BY AN  EQUIVALENT CONDENSER
                                                                                                                                    CHECK
                                                                                                                                    VALVE
                                                                                                                                    VACUUM
                                                                                                                                       LINE
                                            THERMOMETER


                                            FILTER HOLDER
                                                           HEATED AREA
                                      TEMPERATURE
           THERMOMETER

                 /
PtTOTTUBE

        PROBE
                                                  STACK
                                             —•WALL
                                                                        IMPINGERS                       ICE BATH

                                                                                      BY-PASS VALVE
PITOT MANOMETER

              ORIFICE
                                                                                                               VACUUM
                                                                                                                GAUGE
                                                                                                    MAIN VALVE
                                  THERMOMETERS   a
                                                     DRY GAS METER
                                             AIR-TIGHT
                                                 PUMP
                                                    Fjgure 5 1.  Particulate-sampling train.
  2.1.1  Probi XOCL.
                        ea si**l CIA or fl*m with
limrp. tapered Waging *dg*. Tb> acgl* o( tapur
bo <3P and Lb« txxr laall b*oa t&toutaide to preserve
a constant Uiiora»J *;.—.-.. Tb« probl* anal* s&all b»
ol  lh« buttoa-noak or elb»w dMitn. ucLaa oUxnriM
ipeelned  by  UM  Adnuumur. U  ""^* ai sainiea
ttteel, Ib-e  ooule. thall !M coaxCTJctad from •*«™i-tt cufc-
let: OUuraauruui «' coartrucdoo m»y b* used, subject
Co  the apprwnl ol tbe. Artminrtinmir.
 A ra&ge o< aoul* ute* suitable lor i»lda«as ««"'t'""t
Ihould b» avallAbl*, » t.i B-32 to L27 era (H to }4 la.)—
or  larger  U higher volume. sampling  vaiai an  r«d during
nmpUm. prob«5 coiuu-Jcl*d oceordic* to A.PTD-OSM
tnd uuiiztot it>e  calibreuoo CU.-TM o( APTD-G57B (or
C*iibr3le>l nxcrd-nt  to  Cie practdurt  outlined In
          ) »TU  &• eoruidtrid «ff piablt.
          j aboui 4SO* C .900* ?)•
quaru liiun sluOi M im. Imoloy *:.\." or oilier
rurroilon  rMisiucu m«uuit madt ol»«aojleu uibmK may
b« iu* Admlniaintor.
  •.' l.J  r'ltol Tub*. Typ« a. 1U ^Mcrb»d in 6liall W auu'n«d to th« prcU tu
                          orutant monitunnr of th»
             plao> ol (tit pltot tube siiaU b« «im Ttth or abtm tb«
               cu*  ouurn«d in S«cooa 4 at
             U*tbod 2.
               2-1.4  DUIaranUa. Prusur* Gtuga. IncJlatd  E3*nnn-
             •ur or equinum den- 1 krvo), u  sacribwl is Section
             2Jof Mttflod2. Oo*manam*ur stall b« iu«4.arT«k>city.
   Mtniloo o  lrad« ni3«i or irwrlP/.- product do*« ooi"
r Mtiuiitt  tndorMmtni by Ibe Enriroaaitiilal 1'ruioc-
:.ia A^eocy.
             pzanux
               2.1J  FUter Hoider. BorofiUau (lao, with s rtaas
             bit flltw soppon and a sliraoc rubber fuktt. Otbcr
             matnialj of construction* (ex., nles> Rm, Teflon.
             Viton) may be used, subject ui  ippnnl oi ibt Ad-
             mloiaruor. Tbc bolder das en stall pnride a pcoiUTi
             Mai agsinst lnkM» L.-OOT tb<- oot*ide or aroond '-ir (Uurr.
             Tbe bolder, «h*U b< atucbed immediately u UM outlet
             ol tb« probe (or cyclone, U used).
               2.1.9  Filter n»dn« Synem. Any beulng 975t«9a
             espabl« ol maintaining a letnperamrr arouod tb« filter
             hoMer durinf sampung o. 13>±14* C (l&±y.' F), or
             sucb  otber tcapi-rature as  specified  by an applicable
             sobpart ot tb« staadards or approred by tbe Adminis-
             trator for a particular application.  Alternatively. l£e
             UBtfr ciiy opt to operate tbe equipment at a temperature
             lover than thai specified. A temperature gauie npabte
             ol measuring tftnpmiure to wiitiin rr* C (.V** F) shall
             be lonalled so thai  tbe lemprrauire around tbe filter
             bolder con be regulated and tnooilo.-ed dunng sooiplin;.
             He»ung 'njer)  may b<- usr>l. j'-'.':«t
             to tb.' i-iprovil o:  the  AJniuiUirator.  Thr rtrsi »n 1
             jcconj liupincrrs  shill  conuun Vaoim (iui:iti'.iff o;
             w^tir (Six'ilon «.1.3). tV ihint ?hali ty emi>:v  an-J the
             fourth :;-ht o( siUt-a M. or
             •qulralcat  d««iccanL A thrniioroLtcr,  capable o<' ir.rH^ur-
 tng temperature to irithln 1* C (2* H itaO. b« placed
 at tbt  outlet  of iba fourth  Implnger for  mauumog
 purvonea.
   AltenxadTely, ao7 VT^tera that cools the  saMnpi« g»a
 stream aod a&rvi mematmoavnt o^ tbe war oo«den5ed
 and molAurt  leanng  tat  condenser,  a*ca  to  vtthia
 1 ml or I g may b» used, subject u ib* spproral ol tbe
 Admlolstrauir. Acceptable  mewia are  to mauure ino
 coadenMd »»i«- e:tb*  F) ao4 determining
 the vdghi gain.                   •
   U aeana other than  silica gel an used to determine
 the amount of aoUtore leannj Ittf coadeasrr. ii  J
 recommended  IhAt siUca scj  (or  equivalent)  sxill  b«
 used between tbecondeaser srsuc aad pump to pre-rmt
 moisture condensation In the puropoad mtenrnc derice9
 and to avoid tbe nerd to mafrf correctior.a for  mocsuxre la
 the aetercd voiujae.
   NotJt.—If a detemlaatlon of the portfculate  csaner
 collected In the impingm is drsiml in additloo to mois-
 ture content, the impinger l\-utm described  at-ove shall
 be usod. without modification.  Indirlctua. iuia or
. control  agencies  ren/Jtnn*  thii  mformMion thill  b«
 cont^cxed as 10 the saaple iixutery and aaairsis of the
 lopnissr contents.
   ilJ  Metrnnf  System.  Vacuum  Baojr. \rak-'r»
 pujnp. thermoccters capablr oi measunn? tempi-return
 to»ituin T*C (5.4* F).dry gas metercapable of mewunaj
 volume to within  '- p*rcvnt. and rv-laitrd ^luiprnejtt. as
 •bo'jrn in Fijur? i-l. Otber meteriag syslcros rapaWe of
 maintaining sampling  rates wiibin  10 IHTCTOI  ol ao-
 tiiietic and 01 determinin*, sample votiunr>  to within i
 perwni  aay \>»  used, subjrct to the  apprpv*! o the
 Ail:: .^s-.rator. \Vhrn tbr meienni: smcro  is u»rd :n
 cnn;jnctioii ^ii!i a pilot lube, ihe system staii eaabl*
 cbrt:'i' oi iMSii—tic rain.
   #.:i-!>l;i'Str^u;ii'.ilizinjmrtrrtnjsystenisdwirntrt for
 h.--^ T flow nt-3 troji thai dt- met.
   •J.:.'.»  B^rom-'t-r. .Merrury. aneroid, or nther Ijaromeier
 eiir^iU- o'  rv.eosurini atmosphcnc prw^ure Lo  with.n
 1;.^ :nm Us (C.I in. He). In many ca>?!>. Ihe barometric
 f.i-i:!i; may b» 9fx.oir.rt from n owirby natior.ul «-miuer
 s-.-rr.cf siution, in v,h-ch cu» Hie suuoo v^lue (wtiicli U
                                     FeOiRAl RECISTSU,  VOL 42,  NO.  160—THURSDAY,  AUGUST  13,  J977

-------
4*773
                                                            RULES  AND  REGULATIONS
th« absolute benraieCrte prmsun) shall b* miuaited tad
an xliustment. tot  el^vadoo ditferencea tMiwem  U>«
wnuner station and sampUa point saatl b« applied at *
nie of minus ii mm Hj iO_l In. Hg) per 30 m (100 ry
i'l»vaaoo Intireaw or vio* versa lor elevation deensa*.
 •2.1.10  Q«J  DOUICT   Determination  Equipment.
Temperature s*aaor and preasun ffftuf*, as described
in Sections 2.3 and 2.4 of Method 2, and gas analyur,
I (necessary. as described in Method 3. Tha tempvratun
*»nsor shall,  preferably.  b«  permanently attached  to
» n* pitot tub* or samptine orub« in a rtced configuration.
such that th* tipof thes*Mi3or?rt*nd3 beyond the leading
edze ol tb* prob* sheath sad dan not touch in 7 metai.
Alternatively. th* senior ir.»T  t>«  attached lost prior
to us* in th* n-id. Note. however, chat if ta* temperature
wasor i] auarlied In the fluid, tb* sensor must b* placed
in an  imfrfensiiro.fr** arrangement with respect to  th*
T?r*»  5 pitnt t'ibf  openings lire Method 2. i'irur* 2-T).
Ai & second aiierttaave. if a difference of not more than
1 percent ui tbe average velocity measurement is to b*
Introduced. the tamperature ;rauiie need not be attached
to tna probe or pilot cub*. (This alurnatiT* b subject -
to too approval of tn« Administrator.)
  2,2   Saispl*  Recovery.  Tb*  loUowinij  lUms-  ar»
needed.
  2.2.1  Probe-Liner and Probe-N'otil* Brasbei.  Xylon
crutl* hnisbe* with stainless 5tml wira handles. Tb*
prohe  V>r.^b shall  have extensions  lat least as long as
the probet of stainless si*rl. Nylon, Teflon, Of slmilirly
Inert maunal. The crushes shall b* properly sued and •
sbioml to brush out the probe liner and nouJe.
  2-2.2 Wash  Bottles— Two.  Glaa waah  bonlea  are
re*ommended. p»ly«thyl»na wash  bottles may be used
at the option of the tester. It 12 recommended that acetone
net b« stored In pcly«tl:yi«n« bottles tat lonccr  than a
month.
  2 .2.3  Glass Simple Storage, Containers. Chemically
resistant, borotiiicaia giau bocti*s. lor acetona wasbea.
£00 ml or 1000 ml. Screw cap Imen shall either be robber*
barked Ttaon or shall b* coruLnu.-t#d so as to b* ieak-(re*
and resistant to chemical aft art1 hy acetone.  (S'amrw
mouth glass bottles baT« b~n found to. be lea proa* to
         AlUmaUTcJy, poiyethylnM boctlea  may b*
    .
  2.2.4  Petri Dtsha. For alter samples, fjan or poU-
etbyiece,  uixleas otbenru* speei^ad by . the j^doun-
Isuator.
  2J2.i  Graduated Cylinder and/or Balance. To meas-
ure condensed crater to within 1 mJ or 1 g. Cradnated .
ryunden ihail baire lubdlTisions no crrater than 2 ml.
Moat Ubomtory balancu are capable ol weighine. to the
nearest O.o t or-lm. JS-ny ol theM balsncea is suitabl* (or
cs* acre u>d in Section 2.3.4.
  2.2.6  Flanic Storaf o ConUista. Air-Uiht tOBtainerj
to store silica gel.               ,
  22.7  Funnel and Bubber  PoUmnan.  To aid  In
transfer of silica |el to container: not neeeEary U liUea
{el Is veiihed in the field.
  2.2.S  ? utmel. Clast or polyvthleea. to aid in iampV*
recovery.
  2.3  AnViyils..?or analysis. tb*!ol2owiaf equipmentls
needed.
  2.3.1  Glass WeigblnK DWwt
  2.3J2  Deaiccator.
  2.3.3  Analytical Balance. To nwawr* to within 0.1
  rrj.-
  2.3.4  Balaoca. To mmiore to wltUn OJ f.
  2.3.3  D«Jctrj. 2jO =1.
  S. 3.S  Hydrometer. To m**oura the reUtlrt humidity
of the laboratory earlromneoc.
  2.3.7  Tcmp«rinir» Cauice. To measure the tem
tnro of the laboratory env;rootneai.
  3.1  SaaplSnt. The rc&;;nts used iu sampUuf ore *s
 (nllowi:
  3.1.1  niters.  OUra Cb-r  flltwj, without  onraala
 binder, exnibltiax at luut 9u.9i percent ejtciency ( <0.0i
 percent p'ne'.rMmn)  on  OJ-nucxon dioctyl phthalate
 snjot* partldM. Tbt  Uter «fl\civncy tnt shall be con-
 tfuct"! in &c-71. Tcit dMa from the sappU«r'i  nullity control
 prosrusi are fulncieat for this purpose.
  3.1.2.  Silk*  Oel. Indicattnc 'vpe, 8 to 16 mnh, I/
 pmvitiusly uvd. fry at 17S* C (IXr1 F) for 2 boars. New
 silica Rel m&y be used at receired.  Alternatirply, othrr
 tyix4 uf ds '.e^uiraltot or b«itfr^  may be oded.
 5UO]*1**: to thr ^ppruT^J of the Admtnisxrator.
  3.1.3  Waur.  Vt'hen analysts o(  the. material cuojht In
 thr Lmpmufr* ii rmuir-d. daulled  wil»r  shall be used.
 Ryu blanks pnor to luM ua« to «iiminan a high blank
 on t<\>i '* ot nopcock eruie oar be uied, tub-
 Jtct :o f.* spprorrvl o( thr \djniiuttraior.
  .1.2  rj:!inl«.K«corer>-. \ceton«— roionnl gnje. 4  b<>ttlfs  from meial contiiincrs; thus.
 .-\cewre r-!"\n.'.s slia.'.  h« run  prior to field us* and only
 ucetone w;v,i  low blank vr.iuas (<0.001 percentl .ihAll be
 ui'-'l. In tio C4*< shall a blrvuk value of creator than ij.OOl
 > :-"*nt of the »eii;iit rl fr>'loni! UifJ he subinuttd from
 i. .••««..;.. * filtcn ta  thes*
 eoatainen at all  times ewepi  donog sampling  and
 weighiot.
  Desiccau  tht alters it M±5.r C (M±IO* F)  and
 ambient pmsnr* for at  least 2t hours and weigh at in-
 tervals  of at ieut 6 hours to a constant weight. I.e.,
  th« length of probes.
  Select a total sampling time greater than or equal to
 the. miniaium total sampling time specified in the ten
 procedures for  the rpociiitc industry such that (1) th*
 aiunpuag time per point is not less than 2 min (or  some
 greater lima interval as spudded by tha Administrator I.
 and (2) th* sample volume taken (corrected to standard
 conditional will'iicnd th* required minimum total gas
 aaapl' volume. The latter is based oa aa approximate
 average sampling rate.
  It is recommended that the number of minutes sam-
 pled at each point be aa integer or aa integer plus one
 h»ll minute, in order to  avoid timekeeping errors.
  In torn* circumstances, e.r., batch cycles. It may b<
 n<*«asary to sample for shorter times at  the traverse
 points and to  obtain smaller ;as sample  volumes. In
 these cases,  the  Administrator' i approval must  first
 tx  obtained.
  4 1.3  Preparation of Collection Train. During  pnp-
 aration and assembly of the  sampling train, keep till
 opvoings where contamination can occur covered until
 Just prior to assembly or until sampling Is about to bofin.
  Place 100 ml of water In each o! ihe rest two uupinjen.
 leave the third Unplnger eznpty, and transfer approii-
 ciateiy C'JC to  3u) g of preveighed  silica  gol from Its
 container to the fourth Ixnpinger. More silica gel may b*
 us*d. but tart should b* takfcn to ensure that it is not
 eutrathe sampling train has be«n assembled, tnro on
 and set th* dlur and probo heating systems at thtdeaind
 operating temperatura. Allow dm* for th* temperature*
 to stabiiitt. If a V iton A 0-iing or other leak-tree connec-
 tion is used in assembling tb* prob* nocti* to the prob*
 liner, leak-check tbe train at tb* sampling sit* by ptug-
 guag th* notzl* and pullicg a 380 mm Hg ui in- H*J
 vacuum.
   NOT*.—A lower vacuum may b* used.. ?raTid»d that
 It is not exceeded during th* test.
   If an asbesto* string is used, do cot connect th* prob*
 to th* train during th* lemkakag*
 rates in excess of 4 percent of the arerag* sampling  rat*
 or O.CTXU7  m',min  (0.02 cto), whichever is  less, ar*
 uxtaixeptabl*.
   The lo(lowing leak-check Instructions for tb* sampling;
 train described in APTD-M76 and APTD-05B1 may b*.
 helpful. Start  the pump with bypass vale* fully open
 and coarse  ad)ust valve completely  closed. Partially
 open tbe coarse adjust valve and slowly clos* tb* by?*>a
 valve until tbe desired vacuum is reached. Do not revers*
 direction of bypass  valve,; this will cause water to back
 up into tfaa filter holder. If th* desired vacuum is ex-
 ceeded, either leak-check at this higher vacuum or end
 the leak check as shown below and start over.
   When tbe leak-check is completed, first slowly remove
 the  plug from the inlet to toe prob*. filter holder,  or
 cyclone (if  applicable) and immediately turn oil th*
 vaccum pump. This prevents th* water in the impingers
 from being  forced backward  into the niter holder  and
 silica gel from .being entrained backward luto the third
 impinger.
   4.1.4.2  Leak-Checks During Sample Run. Tf. during
 tt* sampling  run,  a compon«nt  (a.g.. filter a&aejcbly
 or Impinger)  change becomes necessary, a leak-check
 shall be conducted immediately  before  the change  is
 mad*. Tbe leak-check shall b* dom  according to the
 procedure outlined  in Section 4.1.4.1 abov*. except that
 It shall b* done at a vacuum equal to or greater than th*
 muuniizj value recorded np to that point in  tbe test.
  If the leakage rate is found to be no greater than O.OXrS?
 m'/min (0.02 cfm) or 4 percent of th* average sampling
 rate (whichever is less), th* results are acceptable, aad
 no correction will need to be applied to th* total volume
 of dry gas metered: if, however,  a higher leakage  rat*,
 is obtained, the tester shall  either record the iwkag*
 rate and plan ro  correct tb* sample volurc* as suown  in
 Section 0.3  of this method, or shall void th* sampling
 run.
   Immediately after  component  changes, leak-checks
 are optional: if such leak-checks an done, the procedure
 outlined in Section 4.1.4.1 above shall be used.
   4.1.4.3 Tost-int Leak-Check. A leik-checL Is nanda-
 tory at thf conclusion of each sampling run. The Irak-
 chock shall h» don* in accordance «"ith  Uie procedures
 outlined In Section 4.1.4.1. eicept that It ;haU be con-
 ducted at a vacuum «tual to or ^renter  than th* ntail-
 mum value rcorhrd durinn tlie  sampling ntn. If th*
 leakage rate is found to t» no gieater thinO.000.i7 rnVmin
  (O.ff-' cfm) or  4  prrcent ot the arena* sampuue  rat*
  (whichever Is le&j,', the results are  acceptable, and no
 correction need b» applied to th« total vulum» of dry IKS
 metered. If, however, a higher leuk»for*
 and s.'ur i ,u:h leii check, nud vh«n sumplu>£ 13 tuviusL
                                        FEDtXAl
                                                         iS, VOl. 43, NO.  160 — 7HUS5DAY,  AUGUST  18, 1977

-------
                                                        RUlsS AND  REGULATIONS
 •ui 3li*r mdlnn rtotititd by Tlfon &-2 at \aat aan
   ^.•b mnpl* point auriiu «cli am* menntBi u>d
  Vina*! mdlao *h»a 3iiaifi-
  •ul >U)iuan«au  in  flo« nte.  Le»«l sad ure UM
 auo:ii«ur. Bteniu* lh* maaoauur l»»el and tero raty
 tli du< WT\br»uoa< autl umpcraau* ouo(<*, ra»i«
 .-•ciUc "j*--Jtj dunot Uia tnvcn*.
  Clean th* porthoUi ortor ta UM tart ran M minimi**
UM ch*Do» of aoicHiat daootlud maunalL Tn  bap*
sampling, runat* UM nouM cap, T*nty Uuu a>« filur
and yrob* Oman* ryiuau an ut> ta tampwaair*. acd
that UM pitoi tutM and prob* an prepmy pcniuoiMd.
PojiUoo tb* ooule at ta* arr. invent pouu v.vb in* op
poinuag du*cUy u»o UM cat nream. T*n~,»itimiiy surt
UM pomp tad adlon to* flow ta tsotln«ac ooodiaocu.
NomotTtfiat ar* arauabk, vbien aid la UM rapid adlow
                                                                                  w
                                                 eoxapaaaom. Tfi»* noauwtu *r» iWunmi lor »•
                                                 W*MU UM Trp» 9 piy tnb» oxffieitai U IU&±KU&. and
                                                 •JM tucx nJ xrolrvtuu density (dr» mowotar wvtat)
                                                 I* aqaal ta •:»=*. i.PTD-0678 dauui* UM oroo*"tar« lor
                                                 T-«!3j th* noiaocrapra.  II Ci tad i/j an maid* Uv*
                                                 v-«J»« stated raa**> da nat ost UM cnmotnoO oaioo
                                                 appropnwa reap* (*•• Citation 7 tn S*e;ua 7) an u*aa
                                                 u eoiop«n«»i« lor UM d4HMlaov
  LOCATION	

  n?E«ATOR

  BATE	

  RUN NO..	

  SAMPLE BOX HO..

  METES BOX N0._

  MSTEBAH9	

  C FACTOR	
                                          AMSIEST TEMPERATURE.

                                          BAROMETRIC PRESSURE.

                                          ASSUMED MOISTURE. X _

                                          FROtElENCTH.adl)	.
                                         •NOI21E lp£«TIPlCAT10n "n

                                          AVERAGE CALI1RATEO NOZZLE DIAMETER, i
  PITOTTU3E COEFFICIENT, t,.
                                                SCHEMATIC Of STACK CKOSS SECTION
                                          LEAK RATE. »3/«-.(rfa)	

                                          PROBE UNER MATERIAL	

                                          STATIC PRESSURE, aa HIG*. H|j.

                                          FILTER 1"
TRAVERSc POI^^T
. N1JMS£H












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       th« jtaclc b under sutrofi-.-i
     t o! ncpuntr :v«3j'i, UJu c&:« ta close tb< coan*
      r«rtini iSo prab« into tt» TUct v>
PUT*IT. vaut  Iron bxrtiU i^ta tbo  Slur holdw. U
ni^— ss»ry. tho pump aiy b* tumed oa irtUi th« cc«n*
u-Ijrjt T»IT» doe«d.
  Whoa tb« pmb« is la posittaa. block aS th« o'xninti
^rcur.d til* prob«  5nd  portholv Xo prtveai unrtpr*-
s«nt*tiT* dllntlun of the zu str^acn. •
  Tntr«tilul not
to b'lmp  ttt  prub* until* Into th» suck  wtlli  vtita
vtmplin; np»r th« ralb or trbrn rtaonni  or u-j«mri
tiit [>rob*  iLrr:i'n tt«  rrr.tnu ta
k-ip t*i» '*mp«mtur* troimd tlw IUt«r boidtc »t tti*
prni>«r  ItreU »dd mor* 1ft  and. U  nfC«tui>t uotbtr conpUl* Oltw UMtcblr
\-< "<"d rather thin iltempunj to chxnzt lot Uter itMll.
             .                     ,
»wt (*» Section 4.1 4.2). Th« tottl p«rUcuj3t» wjgj
itiMl . Mi-ludc tb> siiramitiOQ of ill alter kwmbly »uh->.
  .v «'.ngl« train 'RiUl b« und for the eatire umpl* rue.
tn »pt In CUM »-h*r» sL-ialUowu laopUr j a rmulred
in two or u»-" ii r;»r»w du"ts ir at two or rr''f< di;.'erent
 n wo or u»-" ii r;»r»   u"s ir a  wo or rr''f<  ;.eren
!.•>• \> rtnj w:l!\iH the saoi* duct, or, in coses where cquip-
it.fci.C'f'».l:ir« oocwi'Jitu a c^in{9 of tr«irs. In all otbcr
sitnnnoiv tn« TI..< o( tvro or more truni will b< aubj^t to
.h- •ippctiv*. j; ;U» .vlaiiijtnto:.
      -  Figure  5-2.  Part'.culata field data.


  Xote that irfa«n two or mor* tralnj an owd, Mpant*
analyiM of tb* Iraac-ball  and (U sppUdbU) Imptniw
catcbeg trotn acb train sball b« porlorcicd. unltu ideca-
csl aoide slu> vere OMd oa ail tnlni. in voicb CAM. va«
front-ball cattbtt (ram th*  Lndindml truna may b»
cambuicd (\s icay tha taptnger eatcbas 1 aod pot ia»iriJ
o( Iront-hAl! catcb aad on* acalysti o( Lapingu catcb
m»7 b* pcrforatd.  Coosnlt wHb tb* Adsuninratot tor
detalU conwnung tb* calculsUoa o( rwulu vb*a tiro or
moro traini an us*d.
  At tb* end o( tb* wmpl* nin, ton off tht eoane adl'ut
T«lr*. riooT* tb* prob* and nottl* Lisra tbt suet, cum
oil th* pump, nrord th* final dry ju zi*t«r r>a>ling, and
coaduct a po«-u»t Iwik-cbtct. u outlined  In SKI: on
4.1.4.1. AIM.  leak-check th« pilot Usu u Otvrtb«d in
MeUiod 2. Section 3  I: th* Unu tctut ru> tali l**Jc-:b^.t,
In order ta ralldat*  tb* v«locuy bead dsu.
  4.1.8 Calculation of  Percent  Uotar.'tic. C»lail»u
p«rr*at bokuuttc (w« C»lcula:lou, Section ») ta diui-
nune  whether tb*  nin v&s ralid or another ten nin
ibould b* mad*. II tbtr* vu djnrolty in m&intairurf
iMldn-clc ratu due to jource coacUtmns.  coniult »".-.b
tb* f JJm]niy-r*tnf for pOUiblv TarikOC* CO tb* iSO^UltClC
ntu.
  4.2  Si*mp\e Hecofery.  Proper  cleanup  proce*1ure
br?iru u soon u the prob* Is remotj'd (rasa the succ »t
ih» end Of the sampling period. Allow the prab« to cool.
  When th* probe  can be ulely h^dltd. wip« o2 ill
etumol partlcolate matter near tbt tip of toe prob*
notilc and place u cap ov»r it to preveot Icnin* or ga;^r,j
particulate matter.  t>o not cap o3 tbe probe  tip Uglily
whilt'the sampllai train D cooiia? clo^- u  thu woull
create a Tacuiiin In  the filler hoU»r. thus dravnnt va-^r
torn ti» imrur.f en  imo th« fU:«r  holi?r.
  •Uetore movma ihe sampla train -,o l!.e  c!-»nup «'/»,
rcmoTt ih< prnL>« from itie sa:iii-l> ;r»ir.. »nj>? o- ''.*
                                                           ere&». and cap the open oaU*t at tbe pnb*. B»
                                                          not to low &ny eoadenjate that ml9h: D* preaecib
                                                          d the rdiccno ftta» from tie (Uur inlet vber* tb*
                                                    probe wu !i3MDeton* bllut."
                                                      Iasp«:t ine train prior to and dutlnr dUaswiablT and
                                                    -ote ar.f aicoraji  coudluoos. T.-v«i th* vunpld ill
                                                          .
                                                      Cw.'i — -V». /. Caretully remove tn» Mtir from th»
                                                    liter ho'.'^r »nd plac* It In itj Mcntiaid pstri disa con-
                                                    tainer. V-* i pair of twwzers and or clean dispojibl*
                                                    «u."pc»l I'.ores to handle th*  Alter. U It b necessary to
                                                    fold •..** i:'??. do so 5u:b that the  paracuiite cite la
                                                    laslde tat fold. CareJ'illy trans!er to the r*:rt diib, any
                                                    part-;a~i:e mistier andjor liter fih«—  »-'jicn  adaere to
                                                    the ."J'.v bolder  «isl;e:,  by ados a  dry nyloK briAU
                                                    bnu1! ir.>l ;r a s'jitp-ed?sd bUde. Seal thecont»ia«r.
                                                      Cii'J.^.-— ,Vo. t. Tatinit e»re to M«  this  dust oa ui«
                                                    outs'..!* ol :'yt probe or other citertot surtK** dan* not
                                                    ;-:t ir.to t=«  N»--=i>;-\ cUACtltatiTely  roroT«r p«rUcui»«
                                                    =.\::»r o: .>:  y cond»iuute Irotn tU* pro'j* a*ti«, prol»
                                       FEDESAl. RECIZTES, VOL.  43,  NO.  160—THURSDAY,  AUSL'ST 13,  1977

-------
417SO
                                                            RULES ANt> REGULATIONS
fitcna. prob* lintt, and frmn
          j«* oomcra'B*iiby tbg
         b* o»d. wtun. »5beifl«i fcy tho
                               oi Uta Uliaf boiiitr by
                              ceUbrmaart placing O«
                                         y b«* Q4*d
  Rant.
         dlxactiooj oo.
               .
  Cart-folly rtrmovo the proas
rurfaro uy ncmng witii  icrio
tjrujo:r.(t witfl a nrloo bru'
rxr--nn« rtiuo shows  r.o r-^
        u^-rtnw of U» Baffl*
         anti rtcaa the  iosi
luL-ur viUL acauw* In  a
                               Pdarm u

                            c^k Md cJraa Ui« load*
                            e fmr.i a wtub boute and
                             urubli.  Bruao until tb*
                            le paru^Iai, aitai  wtmifc
                            s-ortaer with acrtone.
                             parts  of  Uia.
                               way mrtQ  no-
    .          .
  fnia* the pr>H-> brv-^  wuh  &«WHW by
rounnz the pro'w wlule ^mlnln* ac^rma into its upp«
pud so thai all tnsxl-r "urracrs will f» -wetted  vlTft a*
wunpt^ rrtntpJnfr.  A frrmi^i (^ara or pol7>?thTl|'fl*) may
Ui Oicd 10 a*d In traaiitmas aqoiti %u*ii«o to LO« con-
MJii-»r. FtHlcrw iho bcf^trtw  nrrap? wltFi ft pn>L>« bmah.
IJoid  th» prob« in an mclin^  p<>iiineu aqiurt acewo*
intn ti« trppT end aa tV pmri* braan u twic^ pasii«l
>t Uh Q r viiiui^ icooa tiiTjUtin tliu prol***:  hoed. & •MJBpi*
cooLAjO'-r andern»aLii  Uie io*-sr ••Mfl  o( iA6 prob*. and
men  &ny  a*
  iui ict^fj*i^, aud f|iuiorti
   ihfl  flHEDpI* cooiaintT.  A/Ti-r *J)« orc?hrrdt.  mate  a
 uul iv-«iood nose of iho prot_*j> aa [i It Is sblpp*d to tiio  laborato-rr. Wwfc  U»
h**iffht  of tbe Ould IBTCJ to deterniLna •wbethcf or  ixH
Iftiicags octurrwl during transput Lalwl Lb« ctjnt&m«r
to clearly Identify its ronttriu.
  Contcinfr l\'o. 3. Note ibe color oftbc indJcatJnjt sQTc1*
5«i to fletaisrujia Jit hM beta rcmpwtely sp^ncand rafc^A
a notation of lu condiQTn, TntQi^f Uit- slLtca gnl tram
ti« fourth Lmpmiir to ILS ontuwU cont&ixurr ajid »e«J.
A funnel may ma^a 1 1 eamer to potir Lbesilira JTB! without
sudlinz. J. rubber polu-auiw* iray  tm LLt*sd EJ an &ija nnalysu of LQe Lmpjngtr catcJS
LI r«aiu'»-J is«9  Note, Src^on i.1.7).
  U" a diiTtfirnt  typo of cociJ^Ti^'' la a."*f For  purpows of
t-'ii« Secu&n. 4 3, Ule  t«m "coortaui; wptght" meaca a
0 jitTpnc* or nu tnoro thin 0 i og  or 1 p*irc*nt of u>LaJ
>*8ifbt leu  uu-f »riEht, wbjch^Ter ts 8TP4t*r. txtwwn
tvo cin?js:uU»« •»1nJihLT.Sa, w;tb  no l*ifl tbJU) C  tour? o/
  Run Na._

  Filter No..
. Amount liquid lost during transport

  Acstone blank volume, ml	

  Acetone wash volume, mi	
                                                       Acetone blank concsntration, mg/mg (equation 5-4).

                                                       Acetone wash blank, rng  (equation 5-5)	
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED,
mg
RNAL WEIGHT


I^^^^CL
TARE WEIGHT


I^xC^
Less acetone blank
Weight of paniculate matter
WEIGHT GAIN
-
.- -
-



FINAL
INITIAL
LIQUID COLLECTED
TOTAL VOLUME COLLECTED
VOLUME OF LIQUID
WATER COLLECTED
IMPINGER
VOLUME,
ml.




SILICA GEL
WEIGHT,
&



g* ml
                                                              * CONVERT WEIGHT OF WATER TO VOLUME BY DIVIDING TOTAL WEIGHT
                                                                INCREASE BY DENSITY Of WATER (1g/ml);

                                                                                                                        3   - VOLUME WATER, ml
                                                                                                               1 g/ml


                                                                                            Figure  5-3.  Analytical  data.
                                        FLD:FLAI  UGISTJ*.  vcu  «,  NO. 140—-THURSDAY,  AUGUST  is,  1977

-------
            r. the sarcpl* nuy b*.OT«i dri«3 at 105" C
     K) for 1 to S hours, cooli-il in th* diMiccftior. and
     wi to A COILS taut w*>tKhc. u/vi^ a otb«rwu« sp»9cLfi<*l
by tna \dmmLStraxor. The KAC*K m&y aiio opt  to ovta
rtl-y thoflampleat 106 * C (.20* F) lor 2 to 3 boon, weisn
*h> itunpM, n-nd UM thii w«iio  or
        , subject  co tfle approvftl of  tha Admuusx
10 cumc- ta« final r caul Li. Me*Auro tho liquid in
contain w fitb^r  TolumBOlcaUy  to ^1 ml  ox jt
metrKaltT  to iO-i g. Tranaier the cont«au to  t
,150-ml txalcer  and ev»porai* to  drrneja at anibt«at
t«nip€r»cu.™  and  presiurB. 0(*atccsi« for ?l boors aad
weijti ta a con*t,uit wet^bL  Beport the renlu to tb«
QMrest 0.1  mi.
  Ciinfam.rr Ao. J. Weigh the 3p»at siliefl R«l Cor silica RO!
plus Lmpmcw)  to tb« aev»xA 0^ e tuuig & btUnca. Tbu
nap may be coodLictKl 10 c&« fctd.
  "Aaton* £i&nk"  Con/aiTur. Measuro acetone la tbij
          eitber  YoLumaciiaiUy
 Tnru/M the acctoae Co A tar«d 2.VWnU be*ka.r BJQC!
 onte to drynM* at ambient Lamp*f»turc and pr«»ssar»,
 PealccttA tor 24  boon and we*.^ to a coau&at wetjttjt,
 Report tha rsauiu to tbe ortn-st 0.1 mj.
  NOTIL— At tha  option o( the uatAr, tho coaUaU of
 CaaUinw No. 2 as w«Q tu tna ac*tc>Ge bLaafc
'may b* »raporat**d, ax unip«r*tur«9 higher
 eot- II er&pontn>n 'a doa« at an ei«tVB>d tJ
 the ump«r^cun* Li oat b« b«lo*r tbe boiiin^ point o( tbe
 »l»ent' also, to praroat "bumping," tbe evaporation
 procasa miiat b*« closely iupcrTL3*d. and the COQU^QU of
 the b«itw muat bf» T^i/t-a occajionaJly to ouantAui an
     temperature, tJsn tfrtrecid Ci*re, as acetona u highly
              jas ^ low g*-?>i petal.
     Atan ft kooratorr loff oi oil ealibratioai.
  i.l  Piob* Nosile. Prob-e ao«il»rj sti&U  b« calibrated
 be/ora their iiutial UM in tii* ftcld. Uainc a micrometar,
         he irmde diameter of the nozzle to the near«di
                                                           RULES  AND  REGULATIONS
                                                  0.02! nun id. 001 la. ). Make three separate
                                                  using dUerent diameters each Urue, and obtain in* a»er-
                                                  a«e o< the meefur&annu. Til* dulereace between th« h.^n
                                                  and loir numbers iball not  exceed 0.1 mm  (O.IXM in.).
                                                  Wbea noiil«t become nicked. dtoced. c« temperaturt
tcnjJXea. Dial trlennometen. suca u &r» ua«Ki Cor tae dry
£01 oitur  tod  condeoj«r oullrt. itaU  be  cm!K>r»(*d
airaitsc ourmry-irr-glaji ib»rmnm«i«n.
  ^A  LxKji Cbto^ o4 ^Ittrrinti drnem Saovn In r*1cnrt
i-l. Tow porQoo o( th« «mplin« train Iram the pump
u>ib«ortUee mtur ihould twl«k cnecimci nnor loinidal
uvundUHreacb jfupment- Ui»X»«» altrr lb» pomo \«1U
nsuii in !•«  Tolucit  h«n«  m-orrlfd LUan Is  aoniAlly
sampled. Tbe. [otlo«rtnn  proonlurr  U  m »A *• •" I  *>*•
F^rur* A— I): Close the  main T^l»t on ifi* ci«l«r boi.
Invrt  » oa*-oolt  mbb^r  not>p*r with  rub&er tub»n«
afljchnd Into  the ortdc* txbaujt pipe. OLKoaoeca and
Tern tb* low ttdt OJ lae orlGoa rn*aom« L4 am
(5 to 7 Ln.)  vmur  oolnmn by blowing luto the rubber
tnbinx. Pinch ofl tht tuOtag and nhtem ( tie ouaaoaituer
Cor oat minuta. A lota  of presort on the omaomtttr
Indlc^xn » Inil: In  tbt cn««^r boL: k»ri. Lf pramL. muA
be oorr>-ct*d.
  5.7  Baroomer.  Calltxrue K»UL«. a mercury berom-
8. Caieaiatioru

  Carry ocrt rajcalalioal. retalniiat at le«5t ooe em
decimal a^ura btyocul toai oV tb« aoqulr^i dafa  Bound
on nirura after tbt ftnul oiJ»"
         component  changt  (^Ml,   X  3 .... n)(
         m'/min  (cfm).
        -Leakaeo rate obserrwl during thi post -test
         leak check, nj,'mln (ctm).
        ""TotiXi amount of  paniculAte ms'tercoutxitfra,

        -Molecular weight  of water,  15.0  fnj-tnoU
         (13.0 lb/lb-mol«).
        —Maw of residue of acetone aft»r araporatioo,
            .
        -Boron«trle  prw>ur9 at t'
         nun Hn (In. Eg).                 .   _
        -Abiolute stable iMprtasuro. mm H? (in. Hir>.
        -3ur.-L--d  absoluio  prn<5ure,  760  am  Hj
         (•-•<.« in. Eg).
                                                    T.
       -Ideal gas constant, 0.062M mm Hg-mVE-g-
        mole (21.M in. Hg-«V°R-lb-mole).
       -Absolut* average, dry ras meter umperatnre
        (see Figure S-J), "K ("ft).
T,     -Absolute areng^stack gas temperature (see

T,u   -Standard   ab»tat»  temperature,  233*  E
        (52S' E).
V«     —Volume of acetone blank, mL
V,,   -Volume o( acetone used In wa»h. mL
    Vu —Total volume of liquid collected in impingers
        »nd silica gel (j*e Figure 4-3). ml.
    Ym" Volume o( ;u sample as measured by dry ga*
        met«r, dcm (dd).
V.(.«i-Voluin« of  gas sample measured by the dry
        gas meter, corrected to standard conckdou,
        dscm (dsc/).
V.(..4)-Volunie of  irster vapor In the gu jampla,
        corrected to standard condition*, scm isc/].
    V.-Stack gas Telocity, calculated by Method t.
        Equation  2-9,  using data,  obtained  from
        Method 4,  m.'ste (ts/sec).
    I^.-Weigbt of resldut in acetone w»ah. mj.
     y-Dry gas meter  caiibracioe factor.
    AH-A«ra?» pressure- differential across tbe orinr«
        meter ue* F'urur* 4-2), oa HjO (in. HrO).
    • ,-Deusity  o(  acetone, mg/ml  (see  label on
        bottle).
    /.-Detuny  o.' waier.  O.WS2  t'ml   (0.0,^201
        Ib/ml).
     1 = Total sarcpling  tisie. min.
      ' I: " Samplin< tim« interral, from   e  ttnnnt
          at a run until tht OTA component cnacga,
          Tnln
         w          time Laurrmi, b«rw*cn rw« suc-
          cefclive component ci*-an$eA, t>e?Lru3inc with
          th« interral between  the  tm and second
          changea. nuxu
       1,-SampUnt tLma tnterrj, turn th« final (n^t
          component caarijrs until  the  tnd  oi  tbe
          sampling run,  min.
     115»3p»ciac gravity at mercury.
       G0"»3ec/min-
      100— ConTenion to percent.
  6J  ATlraia dry gai Eeter temperature and
or!2c« preaaure drop. See daiA sheet (Figure 5-2).
  6J  Dry Gas Vo'.umt.  Correct the sajnple roliicit
measured by tb» dry f«  meiw to standard  conditions
CO* C, 760 Tnm Hg or W f , 29.92 in. Hj) by
Equation
                                  13.6
                              P..
                                                                                                                                                      i-i
                                       FEDERAL  RECISTE»,  VOL.  42,  NO.  160—THURSDAY,  AUGUST  13, 1977

-------
                                 RULES  AND  REGULATIONS
mi— 0 JSAfl •
  - 17.M '
                  H« .'or m^rtc  L  Ko  mrapooeot cnann* maj«
a*mplinc ran. In tnu c**«, repUc« ^ « In Equation
vita tbe expression;
                                                    NOT*.— ti
                                                   itnama. two
                                                               Maraud
                      or  walar  dreplet4»d«n  t»»
                      of lb» mautun <-nouat a< UK
              « nra*i*w one Lmn t
               &rt4 * Mcor.d Crom to*
         mmtioooi.  Tr» io»-«- ca to*
       i t>* rrmjiderpd carrot. Tb% pracedar* (w d*t«i.
        tii t7 oixtun ooatdat httd««l uoon cmnmpuoa oi
                  U n««c tn  Cu Nnu o( »>moa U
olM* purpowa oC Uiu aKtbod. U)«ir«rM>
          rapwmcure trom Firm V?
                     . prondMj tfr«c
lh« ui-ftac* umpvmcun Haior LI ± i* C U" FV
  6.6  Ac«lon« BUJix Coacuttnuoc.
  fb) Cat* U. Cm« or man eompaaut rn«nn>»
dnnmr tb« «rnplmr nm. la Uu* ca». replace
and 5UbnhUt« only lor thoae
vnica nosed L.

  6.i  Talma* a/ vatrtr -raoor.
                                  rat« (I, or L,)
     —0.001333 nj*/rni Jor in«tr!e urttt
     -O.CM7D7 rt«rnJ lor Enilnh uiutl.
      MoLjtnn Conunt.
             B,.=
                        V    St
                                                                           • P.

                                                   (.7  Actuxw Wa«h DUnl

                                                                 IF.-C.V../,.

                                                   «J  Total  Particniate TTeltht. Detarmin* Ou

                                                 torn oonuiaan 1 »nd 2 \em the ar«mn« bbuik IM« 1
                                                 S-JL Nor».—R»iar to 8*cGon <_] J u again la calculation
                                                 of mula LnTorniu  two or mon Hur aaembliM of two
                                                 or mom sampling cr&uu.
                                                ^  6^  ParocuMu CooomtratlaB.
                                                     6.10
                                                                    To
                                                                                         UalUpl7 by
                                                 t:lij

                                                 sift'
                                                                   !b/n»
                                                               «0a V»rl»don.
                                                     &.11J  Calculi rtno From R»w
  A',-O.COMS< mm ns-mVml-'K tor oelrlc onJta.
     -O.OO^aa in. H»-(t'ttnJ-'R lor Eojjlish onlu.
  8-1LJ  Calculation
                      T.V.
 8.13
   n i— 1 Vft tor m«tru onit3
     -CLli-tiO lor Entliib muU.
    13 Ao«pUbl« RtMitta.  LI 50 p«re«nt  
 abl« raog«, or, U I iJ le^s tb&a 90 percent,  tb« AHTnmi*.
 trator may opt to accept ta« rr^uiix CM  Citation i to
 matajcdgaiAnLs. Otafnri», reject tb« reaultj and r*p«at
 Mitten.
   1. Addendum to Sp Tnad(J*
                                                 Park, N.C. .N'oFtovtxr. 1076 (unpubliined p«par>.
                                                   9.  tr.nn.i Boot of AjTM St&ndvdj. Part 24. Ouoona
                                                 Fii^li; Coai and Cokt; Atmovpharid Aoalysia, Aja«rtcui
                                                 Sociicy  tor TuOni aod  '"-'IT'I  FhiUddlptua,  Pa.
                                                 l»7t pp. «17-522.
                                                   METHOD
                                                                          Tiox   or  Sinrcx
                                                                    FEOM STATIONABT
                                                                                            DIOTTPE
 L Prtntiflt and .-tppleaiSUf

  1.1 PrlnripU. A r»J  »apU li eitrsctod Irom li»
 nmpllnf  point IB tn« stack.  To* suUucc  acid mm
 Cincludint suirof  crioxldf) and tb« soirar dioijd* ar*
 i«pa.-«t4KL To* mltor dioiidt Inc^oO  J measured by
 tb« bantua-taorta Utr&^on meUuxk
  U AppUcabiilty.  Tnii method la applicable for Uu
 determination of stiUur dlnilde emiuioos trom stationary
 K.UTCM. The tnintT-inm datecublt limit ol tb« icetnod
 nu b««n drtermined lo b4 3.4 milligr&cu IIEZ' of SOt'm1
 (112X10-' Ib'ft '). AJtboosh no upper limit baj bMn
 utabliibtd. tedU  DST«  sbow-n tbat eoncmtnuoci  u
 bigb u 80,000 mtin' ol  60i can be coVlecwd efficiently
 In two nudset Lmpin^tn, escb concainlng 15 miiii!it*r?
 o( 3 ptrwnt" aydroien p«roi;de, at a r»i» of 1.0 1pm lor
 20 minoto. Baaed on ibeorettcaJ calcoiaUou, tb« uppnr
 conc*atruion limit In a 2>htei £unpl« li about 93.3CQ
                                                       .
                                                    Poasibl* !irUr>r«ots are fr*» aimxotia. w«ter-«X)hjbU
                                                  eatlotu,  and naoridd. Tb«  cauotu and fioortdM  ar»
                                                  remoTed by jlaaj wool tilers and an uopror»ool bobbin-.
                                                  and hetc.e doom aSect tb« 3Oi analyst*, vfbeo nmpka
                                                  art beiot taLen trom a tu su<«m vitb M{b cooc« (fuci as  tn Inleta to
                                                  eonrrcl d«Ti«s), e hi?n-«aiclencT glasa tb*r ftlt«r man
                                                  be ued  in pitt«-o( tbe !ii;-5  wool plug (I.e., tnt oo* in
                                                  tb* prot1*' to remoTt the cation inwrferentj.
                                                    Fre« srmonia interlero by re««!j:| »1th SOi to form
                                                  purticuiau solflte and by reacting  wttn tbe indicator:
                                                  If Im ammonia H pr«Mnt (tnia can b* deterrr.inwl br
                                                  tnowledfe of tn« proo=» and noicku; whiu panlcui*t4
                                                  matiB rn tn« prob* and  ljoprop»nol babbler), aluroo-
                                                  CT« methods. rab)«ct to tbe approi&l of tbc Aflm'Tintrm-
                                                  tor,  XJ.B.  Enrlronmtr.tal  ProttK.tioi>  AjencT,  art
                                                  nqolrod.
               FEDERAL 8EGISTH,  VOL  42, NO.  160—THUBSDAY,  AUGUST  18,  1977

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                      Attachment E
 Determination of Total Polychlorinated Biphenyl  (PCS)
Emissions from Industrial, Sewage Sludge, and Municipal
           Refuse Incinerators  (Draft Method)

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                PART A.   INDUSTRIAL.  SEWAGE  SLUDGE. AND
                    MUNICIPAL REFUSE INCINERATORS
1.  Principle  and Applicability

     1.1  Principle.   Gaseous  and particulate PCBs  are withdrawn isokiaet-
ically  from the  source using a sampling train.  The PCBs  are collected in
the Florisil adsorbent tube and in the impingers in front of the adsorbent.
The total PCBs in  the train are determined by perchlorination to decachloro-
biphenyl  (DC3) and  gas chromatographic determination of  the DCS.

     1.2  Applicability.   This method is applicable for  the determination
of PCB  emissions (both vaporous and particulate) from industrial, sewage
sludge, and municipal refuse incinerators.

2. Range and  Sensitivity

         The  range of the analytical method may be expanded considerably
through concentration and/or dilution.  The total method  sensitivity is also
highly dependent on the volume of gases sampled.  However, the sensitivity of
the total method as described here is about 10 ng DCS for each analytical
replicate.

3.  Interferences

          Excessive quantities of acid-resistant organics may cause signifi-
cant interferences obscuring  the analysis  of DCS in the perchlorinated ex-
tracts.  Biphenyl, although unlikely  to be present in-samples from combus-
tion sources, can form DCS in the perchlorination processes.

          Throughout  all stages  of sample handling and analysis,  care  should
be taken to avoid contact  of  samples  and  extracts with synthetic organic
materials other than TFE®  (polytetrafluoroethylene).  Adhesives must not be
used to hold TFE® liners on lids, and  lubricating and sealing greases must
not be used on any sample  exposed portions of the sampling  train.

4.  Precision and Accuracy

          From sampling with  identical and paired sampling  trains, the pre-
cision of  the method  has been determined  to be  10 to 15Z  of the  PCB concentra
tion measured.  Recovery efficiencies  on  source  samples spiked  with PCB com-
pounds ranged from 85  to 95Ti.
                                     52

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 5. Apparatus

    5.1  Sampling Train.   See Figure A-l;  a  series  of  four impingers  with a
 solid adsorbent trap between  the  third  and  fourth impingers.   The train may
 be constructed by adaptation  from a  Method  5  train.   Descriptions of the
 train components are contained in the  following subsections.

         5.1.1  Probe nozzle—Stainless  steel (316)  with sharp,  tapered
 leading edge.  The angle  of taper shall be  £  30 degrees and the  taper shall
 be on the outside to preserve a  constant internal diameter.  The probe noz-
 zle shall be of the button-hook  or elbow design,  unless otherwise specified
 by the Administrator.   The  wall  thickness of  the nozzle shall be less  than
 or equal to  that of 20 gauge  tubing, i.e.,  0.165 cm  (0.065 in.)  and the dis-
 tance from the tip of  the nozzle  to  the first bend or point of disturbance
 shall be at  least two  times the  outside nozzle diameter.  The nozzle shall
 be constructed from seamless  stainless  steel  tubing.  Other configurations
 and construction material may be  used  with  approval  from the  Administrator.

         5.1.2  Probe liner--Borosilicate or quartz  glass  equipped with a
 connecting fitting that is  capable of  forming a leak-free,  vacuum tight con-
 nection without sealing greases;  such  as Kontes Glass Company "0" ring spher-
 ical ground  ball joints (model K-671300) or University  Research  Glassware SVL
 teflon screw fittings.

         A  stainless  steel (316) or water-cooled probe nay be used for sam-
 pling high temperature gases  with approval  from the Administrator.  A  probe
 heating system may be  used  to prevent  moisture condensation in the probe.

         5.1.3  Pitot tube--Type S, or equivalent,  attached  to  probe to
 allow constant monitoring of  the  stack gas  velocity.  The face openings of
 the pitot tube and the probe  nozzle  shall be  adjacent and parallel to each
 other but not necessarily on  the  same  plane,  during  sampling. The free
 space between the nozzle  and  pitot tube shall be at  least 1.9 cm (0.75 in.).
 The free space shall be set based on a 1.3  cm (0.5 in.) ID nozzle, which is
 the largest  size nozzle used.

         The pitot tube  must also meet the criteria specified in Method 2
 and be calibrated according to  the procedure  in the  calibration  section of
 that method.

         5.1.4  Differential pressure  gauge—Inclined  manometer capable of
measuring velocity head to  within 10%  of the  minimum measured value.  Below
a differential pressure of  1.3 mm (0.05 in.)  water gauge, micromanoneters
with sensitivities of  0.013 mm  (0.0005 in.) should be used.  However,
                                    53

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                       Stack
                       Wall
                                                    Thermometer

                                           Florlsil Tube
        Probe

Reverie-Type"
Pitot Tube
      Manometer
                                         Control Box
                   Figure  A-l._  PCS Sampling Train  for Incinerators
                                              54

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micromanometers are not easily adaptable to field conditions and are not
easy to use with pulsating flow.  Thus, other methods or devices acceptable
to the Administrator may be used when conditions warrant.

          5.1.5  Impingers—Four impingers with connecting fittings able to
form leak-free, vacuum tight seals without sealant greases when connected to-
gether as shown in Figure A-l.  The first and second impingers are of the
Greenburg-Smith design.  The final two impingers are of the Greenburg-Sraith
design modified by replacing the tip with a 1.3 cm (1/2 in.) ID glass tube
extending to 1.3 cm (1/2 in.) from the bottom of the flask.

          5.1.6  Solid adsorbent tube — Glass with connecting fittings able to
form leak-free, vacuum tight seals without sealant greases (Figure A-2).  Ex-
clusive of connectors, the tube has a 2.2 cm inner diameter, is at least 10 cm
long, and has four deep indentations on the inlet end to aid in retaining the
adsorbent.   Ground glass caps  (or equivalent) must be provided to seal the
adsorbent-filled tube both prior to and following sampling.

          5.1.7  Metering system--Vacuum gauge, leak-free pump, thermometers
 capable of measuring  temperature to within 3CC  (~ 5°F) , dry gas meter with
27» accuracy at the required sampling rate, and  related equipment, or equiv-
alent, as required to maintain  an isokinetic sampling rate and to determine
sample volume.  When  the metering system is used in conjunction with a pitot
tube, the system shall enable checks of isokinetic rates.

          5.1.8  Barometer--Mercury, aneroid, or other barometers capable
of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).  In many
cases, the barometric reading may be obtained from a nearby weather bureau
station, in which case the station value shall  be requested and an adjust-
ment for elevation differences  shall be applied at a rate of -2.5 mm Hg
 (0.1 in. Hg) per 30 m (100 ft)  elevation increase.

     5.2  Sample Recovery

          5.2.1  Ground glass caps—To cap off adsorbent tube and the other
sample exposed portions of the  train.

          5.2.2  Teflon FEF® wash bottle—Two,  500 ml, Nalgene No. 0023A59
or equivalent.

          5.2.3  Sample storage containers—Glass bottles, 1 liter, with
TFE®-lined screw caps.

          5.2.4  Balance—Triple beam, Ohaus Model 7505 or equivalent.

          5.2.5  Aluminum foil—Heavy duty.
                                     55

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    10cm
if A
\
\
\
\_, ^
\
\ .*-
A
\
\
\
r
\ ^~s
r
i






                           2.5cm O.D




                           2.2cm l.D.
                             j 28/12
Figure  A-2.  Florisil Adsorbent Tube
                  56

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          5.2.6  Metal can—To recover used silica  gel.

     5.3   Analysis

          5.3.1  Glass Soxhlet extractors—40 nm ID complete  with  45/50  
-------
          5.3.19  Porcelain  casserole—Capable  of withstanding  temperatures
as high as 650°C.

6.  Reagents

     6.1  Sampling

          6.1.1  Florisil—Floridin  Co.,  30/60  mesh, Grade A.   The Florisil
is  cleaned  by 8 hr Soxhlet  extraction with  hexane  and  then  by  drying for
8 hr in an oven at 110°C and is  activated by heating to 650°C for 2 hr (not
to exceed 3 hr) in a muffle  furnace.  After  allowing to cool to near 110°C
transfer the clean, active Florisil  to a  clean,  hexane-washed glass jar and
seal with a TFE^-lined  lid.   The Florisil should be stored at 110°C until
taken to the field for  use.   Florisil that has  been stored more than 1 month
must be reactivated before use.

          6.1.2  Glass  wool—Cleaned by  thorough rinsing with hexane, dried
in a 110° C oven, and stored  in a hexane-washed  glass jar with TFE@-lined
screw cap.

          6.1.3  Water--Deionized, then  glass-distilled,  and stored in hexane-
rinsed glass containers with TFE®-lined  screw caps.

          6.1.4  Silica gel--Indicating  type, 6-16  mesh.  If previously used,
dry at 175°C for 2 hr.   New  silica gel may be used  as  received.

          6.1.5  Crushed ice.

     6.2  Sample Recovery

          6.2.1  Acetone—Pesticide  quality, Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in original  containers  and used as received.

          6.2.2  Hexane—Pesticide quality,  Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in original  containers  and used as received.

     6.3  Analysis

          6.3.1  Hexane—Pesticide quality,  Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in original  containers  and used as received.

          6.3.2 Acetone--Pesticide  quality. Burdick and Jackson "Distilled
in Glass" or equivalent, stored  in original  containers  and used as received.

          6.3.3  Water--Deionized and then glass-distilled,  stored in hexane-
rinsed glass containers with TFE@-lined  screw caps.
                                   58

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          6.3.4  Sodium sulfate (Na2S04)--Anhydrous,  granular.   Clean by
overnight Soxhlet extraction with hexane, drying in a 110°C oven,  and then
heating to 650°C for 2 hr.  Store in 110°C oven or in glass jar closed with
TFE®-lined screvj cap.

          6.3.5  Sulfuric acid (I^SO^)--Concentrated, ACS reagent  grade or
equivalent.

          6.3.6  Antimony pentach-loride (SbCl5)--Baker Analyzed Reagent or
equivalent.

          6.3.7  Hydrochloric acid (HC1) solution--ACS reagent  grade or
equivalent, 507= in water.

          6.3.8  Glass wool—Cleaned by thorough rinsing with hexane, dried
U a 110°C oven, and stored in a hexane-rinsed glass  jar with TFE©-lined cap.

          6.3.9  Decachlorobiphenyl--RFP Corp., No. RPC-60, or  equivalent.

          6.3.10  Compressed nitrogen—Prepurified.

          6.3.11  Carborundum boiling stones--Hengar Co. No. 133-B or equiv-
alent, rinsed with hexane.

7.  Procedure

     Caution:  Section 7.1.1 should be done in the laboratory.

     7.1  Sampling.  The sampling shall be conducted by competent  personnel
experienced with this test procedure and cognizant of 'the constraints of the
analytical techniques for PCBs, particularly contamination problems.

          7.1.1  Pretest preparation.  All train components shall  be main-
tained and calibrated aqcording to the procedure described in APTD-0576,
unless otherwise specified herein.

               7.1.1.1  Cleaning glassware.  All glass parts of the train
upstream of and including the adsorbent tube, should be cleaned as described
in Section 3A of the 1974 issue of "Manual of Analytical Methods for Analysis
of Pesticide Residues in Human and Environmental Samples."  Special care
should be devoted to the removal of residual silicone grease sealants on
ground glass connections of used glassware.  These grease residues should be
removed by soaking several hours in a chromic acid cleaning solution prior
to routine cleaning as described above.
                                    59

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               7.1.1.2  Solid adsorbent  tuba.   Weigh 7.5  g  of Florisil, ac-
tivated within the last 30 days  and  still warm from storage in a 110°C oven,
into the adsorbent tube (pre-rinsed  with hexane)  with a glass wool plug in
the downstream end.   Place a second  glass wool plug in the  tube to hold the
sorbent in the tube.   Cap both ends  of the tube with ground glass caps.  These
caps should not be removed until the tube is  fitted to the  train immediately
prior to sampling.

          7.1.2  Preliminary determinations.   Select the  sampling site and
the minimum number of sampling points according to Method 1 or as specified
by the Administrator.  Determine the stack pressure, temperature, and the
range of velocity heads using Method 2 and moisture content using Approxi-
mation Method 4 or its alternatives  for the purpose of making isokinetic
sampling rate calculations.  Estimates may be  used.  However, final results
will be based on actual measurements made during  the test.

          Determine  the molecular weight of the stack gases using Method 3.

          Select a nozzle size based on the maximum velocity head so that
isokinetic sampling  can be maintained at a rate less than 0.75 cfm.  It is
not necessary to change the nozzle size  in order  to maintain isokinetic
sampling rates.  During the run, do  not  change the nozzle size.

          Select a suitable probe length such  that all traverse points can
be sampled.  Consider sampling from opposite sides for large stacks to re-
duce the length of probes.

          Select a sampling time appropriate for  total method sensitivity
and the PCB concentration anticipated.  Sampling  times, should generally fall
within a range of 2  to 4 hr.

          It is recommended that a buzzer-timer be incorporated in the con-
trol box (see Figure  1) to alarm the operator  to  move the probe to the next
sampling point.

          In some circumstances, e.g., short batch processes, it may be
necessary to sample  through two  or more  batches to obtain sufficient sample
volume.  In these cases, sampling should cease during loading/unloading of
the furnace.

          7.1.3  Preparation of  collection train.   During preparation and
assembly of the sampling train,  keep all train openings where contamination
can enter covered until just prior to assembly or until sampling is about to
begin.   Immediately prior to assembly, rinse all  parts of the train upstream
of the  adsorbent tube with hexane.
                                    60

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     the probe with heat  resistant  tape  or by some  other method at points
indicating  the proper  distance  into the  stack or duct for each sampling
point.

         Place  2'00 ml of water in  each  of the first two impingers, and
 .£ave the third  irnpinger  empty.  CAUTION:   do not use sealant greases in
assembling  the train.   If the preliminary moisture  determination shows that
the stack gases  are saturated or supersaturated, one or two additional empty
impingers should be added to the train between the  third impinger and the
Florisil  tube.   See Section 10.1.  Place approximately 200 to 300 g or more,
if necessary,  of silica gel in the  last  impinger.  Weigh each inroinger (stem
included) and  record  the  weights on the  imningers and on the data sheet.

         Unless otherwise specified by  the Administrator, attach a tempera-
ture probe  to  the metal sheath of the sampling probe so that the sensor is
at Least  2.5  cm  behind the nozzle and pitot tube and does not touch any
metal.

         Assemble the train as shown in Figure A-l.  Through all parts of
th:..j method use  of sealant greases  such  as stopcock grease to seal ground
glass joints must be  avoided.

         Place  crushed ice around  the impingers.

         7.1.4   Leak check procedure--After the sampling train has been as-
sembled,  turn  on and  set  (if applicable) the probe heating system(s) to reach
a temperature  sufficient  to avoid condensation in the probe.  Allow time for
the temperature  to stabilize.  Leak check the train at 'the sampling site by
plugging  the  nozzle and pulling a 380 mm Hg (15 in. Eg) vacuum.  A leakage
rate in excess of 47,  of the average sampling rate of 0.0057 nP/min (0.02 cfm)
whichever is  less, is unacceptable.

         The  following leak check instruction for the sampling  train de-
scribed in  APTD-0576  and  APTD-0581 nay be helpful'.  Start the pump with by-
pass valve  fully open and coarse adjust  valve completely closed.  Partially
open the  coarse  adjust valve and slowly close the bypass valve until 380 mm
Hg (15 in.  Hg) vacuum is  reached.  Do not reverse direction of bypass valve.
This will cause  water to  back up into the probe.  If 380 mm Hg (15 in. Hg)
is exceeded,  either  leak  check at this higher vacuum or end the  leak check
as described below and start over.

         When the leak check is completed, first slowly remove  the plug
from the  inlet to the probe and immediately turn off the vacuum  pump.  This
prevents  the water in the impingers from being forced backward into  the
probe.
                                     61

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          Leak checks  shall  be  conducted  as  described  above  prior to each
test run and at the completion  of  each  test  run.   If  leaks are  found to be
in excess of the acceptable  rate,  the test will be considered  invalid.   To
reduce lost tine due to leakage occurrences,  it is recommended  that leak
checks be conducted between  port changes.

          7.1.5  Train operation—During  the  sampling  run, an  isokinetic
sampling rate within 107.,  or as specified by  the Administrator,  of true iso-
kinetic shall be maintained. During the  run,  do not  change  the  nozzle  or
any other part of the  train  in  front of and  including  the Florisil tube.

          For each run, record  the  data required on the data sheets. An
example is shown in Figure A-3. Be sure  to  record the initial dry gas  meter
reading.  Record the dry gas meter  readings  at the beginning and end of each
sampling time increment, when changes in  flow  rates are made, and when  sam-
pling is halted.  Take other data  point readings at least once  at each  sam-
ple point during each  time increment and  additional readings when significant
changes (20% variation in velocity  head readings)  necessitate  additional ad-
justments in flow rate.  Be  sure to level and  zero the manometer.

          Clean the portholes prior to  the test run to minimize  chance  of
sampling deposited material. To begin  sampling, remove the  nozzle cap,
verify (if applicable) that  the probe heater  is working and  up  to tempera-
ture, and that the pitot tube and  probe are  properly positioned.  Position
the nozzle at the first traverse point  with  the tip pointing directly into
the gas stream.  Immediately start  the  pump  and adjust the flow to isokinetic
conditions.  Nomographs are  available for sampling trains using  type S  pitot
tubes with 0.85 + 0.02 coefficients (C  ), and  when sampling  in air or a stack
gas with equivalent density  (molecular  weight, M^, equal  to  29+4), which
aid in the rapid adjustment  of  the  isokinetic  sampling rate  without excessive
computations.  APTD-0576 details the procedure for using  these  nomographs.
If C  and M^ are outside the above  stated ranges,  do not  use the nomograph
unless appropriate steps are taken to compensate for  the  deviations.

          When the stack is  under  significant  negative pressure (height of
impinger stem), take care to close  the  coarse  adjust  valve before inserting
the probe into the stack to  avoid water backing into  the  probe.   If neces-
sary, the pump may be  turned on with the  coarse adjust valve closed.

          When the probe is  in  position,  block off the openings  around  the
probe and porthole to  prevent unrepresentative dilution of  the gas stream.

          Traverse the stack cross  section,  as required by Method 1 or  as
specified by the Administrator. To minimize  chance of extracting deposited
material, be careful not to  bump the probe nozzle  into the stack walls  when
sampling near the walls or when removing  or  inserting  the probe  through the
portholas.
                                   62

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                                                                            FIELD DATA
                            PLANT.
                            DAT£_
                           SAMPLING LOCATION.
                           SAMPLE TYPE _____
                           RUN NUMBER .	
                           OPERATOR 	
                           AMBIENT TEMPERATURE
                           BAROMETRIC PRESSURE .
                           STATIC PRESSURE. (Pjl_
                           FILTER NUMBER Is)	
                                                PliOBE LENGTH AND TYPE.
                                                NOZZLE I D _____ _ .
                                                ASSUMED MOISTURE.'. _
                                                SAMPLE OOX NUMBER _
                                                METER BOX NUMBER __
                                                METER 4He _
                                                C FACTOR. _
                                                PROBE HEATER SETTING
                                                HEATER BOX SETTING
                                                REFERENCE AP
                                                                    SCHEMATIC OF TRAVERSE POINT LAYOUT
                                                             READ AND RECORD ALL DATA EVERY.
                                           MINUTES
TRAVERSE
POINT
NUMBER
1























^v CLOCK TIME
>7FLINC \CLOCK,
TIME. mm N^
	 	 _























GAS METER READING
(VBI. IIJ
























VELOCITY
HEAD
Upjl. in. H20























ORIFICE PRESSURE
DIFFERENTIAL
(AH), in. tl^Ol
DESIRED













	 . 	








ACTUAL























STACK
TEMPERATURE
(TSI."F























DRYGAS METER
TEMPERATURE
INLET

to
       COMML H r S

       fl'A iDuil ?3'j
         i  n
Figure A-3.    Field Data  Sheet

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          During the test run,  make  periodic adjustments  to keep the probe
temperature at the proper value.   Add  more ice and,'if necessary, salt to
the ice bath, to maintain a temperature of less than 20°C (68°F) at the
impinger/silica gel outlet, to  avoid excessive moisture losses.  Also, peri-
odically check the level and zero of the manometer.

          If the pressure drop  across  the train becomes high enough to cake
isokinetic sampling difficult to  maintain, the test  run should be terminated.
Under no circumstances should the train be disassembled during a test run to
determine and correct causes of excessive pressure drops.

          At the end of the sample run, turn off the pump,  remove the probe
and nozzle from the stack,  and  record  the final dry  gas meter reading.  Per-
form a leak check.*  Calculate  percent isokinetic (see calculation section)
to determine whether another test run  should be made.   If there is difficulty
in maintaining isokinetic rates due  to source conditions, consult with the
Administrator for possible  variance  on the isokinetic  rates.

          7.1.6  Blank train—For each series of test runs, set up a blank
train in a manner identical to that  described above, but  with the nozzle
capped with aluminum foil and the exit end of the last impinger capped with
a ground glass cap.  Allow the train to remain assembled  for a period equiv-
alent to one test run.  Recover the  blank sample as  described in Section 7.2.

     7.2  Sample recovery.  Proper cleanup procedure begins as soon as the
probe is removed from the stack at the end of the samp'ling period.

          When the probe can be safely handled, wipe off  all external par-
ticulate matter near the tip of the  probe nozzle.  Remove the probe from the
train and close off both ends with aluminum foil.  Cap off the inlet to the
train with a ground glass cap.

          Transfer the probe and  impinger assembly to the cleanup area.  ThLs
area should be clean and protected from the wind so that  the chances of con-
taminating or losing the sample will be minimized.

          Inspect the train prior to and during disassembly and note any ab-
normal conditions.  Treat the samples as follows:

          7.2.1  Adsorbent tube—Remove the Florisil tube from, the train and
cap it off with ground glass caps.
   '•<.'ith acceptability of the test run to be based on the sane criterion as
     in 7 1.4
                                     64

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          7.2.2  Sample container No. I — Remove the first three impingers.
Wipe off the outside of each impinger to remove excessive water and other
debris,  weigh (stem included), and record the weight on data sheet.  Pour
the contents directly into container No. 1 and seal.

          7.2.3  Sample container No. 2--Rinse each of the first three im-
pingers  sequentially first with 30 ml acetone and then with 30 ml hexane,
and put  the rinses into container No. 2.  Quantitatively recover material
deposited in the probe using 100 ml acetone and then 100 ml hexane and add
these rinses to container No. 2 and seal.

          7.2.4  Silica gel container—Remove the last impinger, wipe the
outside  to remove excessive water and other debris, weigh (stem included),
and record weight on data sheet.  Transfer the contents to the used silica
b'el can.

     7.3  Analysis.  The analysis of the PCS samples should be conducted by
chemical personnel experienced in determinations of trace organics utilizing
sophisticated, instrumental techniques.  All extract transfers should be
made quantitatively by rinsing the apparatus at least three times with hex-
ane and adding the rinses to the receiving container.  A boiling stone should
be used  in all evaporative steps to control "bumping."

          7.3.1  Extraction

               7.3.1.1  Adsorbent tube.  Expel the entire contents of the
adsorbent tube directly onto a glass wool plug in the sample holder of a
Soxhlet extractor.  Although no extraction thimble is required, a glass
thimble with a coarse-fritted bottom may be used.

               Rinse the tube with 5 ml acetone and then with 15 ml hexane
and put these rinses into the extractor.  Assemble the extraction apparatus
and extract the adsorbent with  170 ml hexane for at least 4 hr.  The ex-
tractor should cycle 10 to  14 times per hour.  After allowing the extrac-
tion apparatus to cool to ambient temperature, transfer the extract into a
Kuderna-Danish evaporator.

               Evaporate the  extract to about 5 ml on  a  steam bath and
allow the evaporator to cool  to ambient temperature before disassembly.
Transfer the extract to a 50-ml separately funnel and  set the funnel aside.

               7.3.1.2  Sample container No. 1.  Transfer the aqueous sam-
ple to a 1,000-ml separatory  funnel.  Rinse  the container with  20 ml acetone
and then with two 20-ml portions of hexane, adding the rinses to the sep-
aratory funnel.
                                     65

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               Extract the sample with  three  100 ml  portions  of hexane,
transferring the sequential extracts  to a Kuderna-Danish  evaporator.

               Evaporate the extract  to about 5 ml and  allow  the evaporator
to cool to ambient temperature  before disassembly.   Filter the extract through
a micro column of anhydrous sodium  sulfate  into the  50  ml separatory  funnel
containing the corresponding Florisil extract.  The  micro column is prepared
by placing a small plug of glass wool in the  bottom  of  the large portion of
a disposable pipette and then adding  anhydrous sodium sulfate until  the tube
is about half full.

               7.3.1.3  Sample  container No.  2.  Transfer the organic solu-
tion into a 1,000 ml separatory funnel.  Rinse the container  with two 20 ml
portions of hexane and add the  rinses to the  separatory funnel.   Wash the
sample with three 100 ml portions of  water.   Discard the  aqueous layer and
transfer the organic layer to a Kuderna-Danish evaporator.

               Evaporate the extract  to about 5 ml and  allow  the evaporator
to cool to ambient temperature  before disassembly.   Filter the extract through
a micro column of anhydrous sodium  sulfate  into the  50  ml separatory  funnel
containing the corresponding Florisil and impinger extracts.

          7.3.2  Extract cleanup--Clean the combined extracts (in 50  ml
separatory funnel) by shaking with  5  ml concentrated sulfuric acid.   Allow
the acid layer to separate and  drain  it off.

          Transfer the hexane layer to  a Kuderna-Danish evaporator and evap-
orate to about 5 ml.  Allow the evaporator  to cool to ambient temperature
before disassembly.

          The extract should be essentially colorless.  If it still shows
significant color, additional cleanup may be  required before  assaying for
PCBs.  In this event, further clean the extract by liquid chromatography on
Florisil according to procedures described  in Section 5A  of the 1974  issue
of "Manual of Analytical Methods for  Analysis of Pesticide Residues  in Human
and Environmental Samples"  Reduce  the  Florisil eluant  to about 10 ml by
Kuderna-Danish evaporation techniques described above.

          Transfer the cleaned  extract  to a 25 ml volumetric  flask and di-
lute to volume with hexane.  Pipette  three  5.0 ml aliquots into culture
tubes for perchlorination.  Retain  the  remaining  10  ml  for later verifica-
tion, if required (see Section  10.2).

          7.3.3  Extract perchlorination--Evaporate  the aliquots in the cul-
ture tubes just to dryness with a  gentle stream of dry  nitrogen. If the ali-
quots will not evaporate to dryness,  refer  to Section 10.3 concerning special
cases. Add 0.2 ml antimo-ny pentachloride with a 1 ml glass-TFE® syringe and

                                    66

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seal  the  tube  with a TFEf®-lined screw cap. Heat the reaction mixture to 160°C
for 2 hr  by  placing the tube in a hole in an aluminum, block on a hot plate.

         Allow  the tube to cool to ambient room temperature before adding
about 2 ml of  507, HC1 in water to destroy residual antimony pentachloride.
This  is a convenient "stopping point" in the perchlorination procedure.

         Extract the reaction mixture by adding about 1 ml hexane to the
tube, shake, and allow layers to separate.  Remove the upper hexane layer
with  a  disposable pipette and filter through a micro column of anhydrous
sodium  sulfate directly into a 5 ml volumetric flask.   Repeat the extraction
three tines  for  a total of four extractions.  Dilute the extract to volume
with  hexane.

          7.3.4   PCS determination—Assay the perchlorinated extracts for
decachlorobiphenyl (DCS) by gas chromatographic comparison with DCB stan-
dard  solutions and correct this result for the DCB concentration determined
for the blank  train.   (Column temperature and carrier gas flow parameters
of 240 = C  and 30  ml/min, are typically appropriate.  The concentrations of the
standard  solutions should allow fairly close comparison with DCB in the sam-
ple extracts.   Standards near 25 to 50 picograms/microliter may be appropriate.)

8.  Calibration

          Maintain a laboratory log of all calibrations.

     8.1  Sampling Train

          8.1.1  Probe nozzle—Using a micrometer, measure  the inside dia-
neter of the nozzle  to  the nearest 0.025 mm  (0.001 in.).  Make three separate
measurements using different diameters each  time and obtain  the average of
the  measurements.  The difference between  the high and  low  numbers shall  not
exceed 0.1 mm (0.004 in.).

          When nozzles become nicked, dented, or corroded,  they shall be  re-
shaped,  sharpened, and recalibrated before use.

          Each nozzle  shall be  permanently  and  uniquely identified.

          8.1.2  Pitot  tube—The  pitot  tube  shall  be  calibrated  according
to the procedure outlined  in Method 2.

          8.1.3  Dry gas meter  and orifice  meter—Both  meters  shall  be cali-
brated according  to  the procedure  outlined  in APTD-0576.   When diaphragm
                                     67

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pumps with bypass valves are used,  check for proper metering system design
by calibrating the dry gas meter at an additional flow rate of 0.0057 m3/min
(0.2 cfm) with the bypass valve fully opened and then with it fully closed.
If there is more than + 27. difference in flow rates when compared to the fully
closed position of the bypass valve, the system is not designed properly and
must be corrected.

          8.1.4  Probe heater calibration--The probe heating system shall be
calibrated according to the procedure contained in APTD-0576.  Probes con-
structed according to APTD-0581 need not be calibrated if the calibration
curves in APTD-0576 are used.

          8.1.5  Temperature gauges—Calibrate dial and liquid filled bulb
thermometers against mercury-in-glass thermometers.  Thermocouples should
be calibrated in constant temperature baths.

     8.2  Analytical Apparatus

          8.2.1  Gas chromatograph--Prepare a working curve from at least
five standard injections of different volumes of the DCS standard.

9.  Calculations

          Carry out calculations, retaining at least one extra decimal fig-
ure beyond that of the acquired data.  Round off figures after final calcu-
lations .

     9.1  Nomenclature

     Gn  = Corrected weight of DCS in nth perchlorinated aliquot (n = 1,  2, 3),  pg.

     Gg  = Total weight of PCBs  (as  DCS)  in  sample, ug.

     Cs  = Concentration of PCBs in  stack gas, ug/m3, corrected to standard
            conditions  of 20°C,  760 mm Hg (68°F,  29.92  in. Hg) on dry basis.

     An  ° Cross~sect:I-onal area  of nozzle, m? (ft2).

    Bws  * Water vapor in the  gas stream,  proportion by volume.

      I  - Percent  of  isokinetic sampling.

     ^  = Molecular weight of water,  18  g/g-mole (18 Ib/lb-mole) .

   Pbar  " Barometric  pressure at the  sampling site,  mm Hg (in. Hg).
                                    68

-------
    PS — Absolute stack gas pressure, inm Hg  (in. Hg).

  Pstd = Standard absolute pressure, 760 mm  Hg (29.92 in Hg).

     R = Ideal gas constant, 0.06236 nm Hg-ra3/°K-g-niole (21.83  in.
           Hg-ft3/°R-lb-mole).

    Tm = Absolute average dry gas meter temperature °K (*R).

    Ts = Absolute average stack gas temperature °K (°R).

  Tstd = Standard absolute temperature, 293°K (528°R).

    V]_c = Total volume  of  liquid collected in impingers and silica gel, ml.
           volume of water collected equals  the weight increase in grams
           times 1 ml/gram

    V  = Volume  of gas sample  as measured by dry gas  meter,  dcm. (dcf).

^m(std) ~ Volume  of gas sample  measured by the dry  gas meter corrected to
            standard  conditions,  dscm  (dscf).

V /   ,\ = Volume of  water vapor in the gas sample corrected to standard
 w(std)         ...          f   f\
            conditions, scrn (scr;.

     Vt = Total volume of sample, ml.

     V  =  Stack gas  velocity,  calculated by  EPA Method 2,  m/sec  (ft/sec).

     AH = Average pressure differential across the  orifice meter,  Em
            (in.  H20).

     pw =  Density of water,  1  g/ml (0.00220  Ib/ml).

      9  =  Total Sampling time,  min.

    13.6 "  Specific gravity of mercury.

     60 =  Sec/min.

    100 •  Conversion to percent.
                                      69

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      9.2   Average  dry gas meter temperature and average orifice pressure
 drop.  See  data  sheet (Figure A-3).

      9.3   Drv gas  volume.  Correct the sample volume measured by the dry
 gas  meter  to standard conditions [20°C, 760 mm Hg (68°F, 29.92 in. Hg)] by
 using  Equation  A-l)-
V /  ..  = v
 m(std)    yra
                         std
•bar    13.6
   Pstd
                                              K V,
                                                 n
                                          bar    13.6
where     K = 0.3855 °K/mm Hg for metric  units

            = 17.65 °R/in.  Hg for English units

     9.4  Volume of water vaoor
          VwCstd) « Vlc
                            K Vlc
                                                         m
                                                   Equation  A-l
                    Equation A-2
where     K = 0.00134 m /ml  for metric  units

            = 0.0472 ft3/ml  for English units

     9.5  Moisture content


          R    -     Vstd)
                  Vm(std)  + Vw(std)
                                                   Equation  A-3
     If the  liquid  droplets are present in the gas stream assume the  stream
to be saturated  and use a psychrometric chart to obtain an approximation
of Che moisture  percentage.
                                   70

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     9-6   Concentration

          9.6.1  Calculate  the  total PCB residue (as DCB) in the sample fron
the  weights  of DCB  in  the perchlorinated aliquots according to Equation A-4-

          GS . 5(G1 + G2 + G3)                               Equation A-4
          9.6.2   Concentration  of PCBs  (as DCB) in stack gas.  Determine the
concentration of  PCBs  in  the  stack  gas  according to Equation A-5.
                   G
          cs  * K	                                      Equation A-5
                  m(std)

where      K  = 35.31 ft3/m3
     9.7   Isokinetic  variation

          9.7.1   Calculations from  raw data.


                   100   Ts  CK  Vlc  +  (Vm/Tm)   (Pfaar) + AH/13.6)]
                                   60  9 vs   Ps  An
                                                            Equation A-6
    where     K = 0.00346 mm Hg-m3/ml-°K  for metric units

                = 0.00267 in. Hg-ft3/ml-°R  for English units

         9.7.2  Calculations from  intermediate values.


              x „     Ts  Vm(std)   Fstd
                " Tstd  vs  8  An   Ps  60

                        Ts  Vm(std)	
                  K
                    ps  vs  An      (1-Bws^                  Equation A-7
    where     K = 4.323  for metric  units

                = 0.0944 for English units
                                     71

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      9.8   Acceptable results. The  following range sets the  Limit on  accept-
 able  isokinetic  sampling results:

           If 90% < I < 110%, the results are acceptable. If the results  are
 low  in  comparison to the standards and I is beyond the acceptable  range,  the
 Administrator may option to accept the results.

 10.   Special Cases

      10.1  Sampling moisture saturated or supersaturated stack gases. One
 or two  additional modified Greenburg-Smith impingers may be added  to the
 train between the third impinger and the Florisil tube to accommodate addi-
 tional  water collection when sampling high moisture gases. Throughout the
 preparation, operation, and sample recovery from the train, these  additional
 impingers  should be treated exactly like the third impinger.

      10.2  PCS verification. It is recommended that an unperchlorinated
 aliquot from at  least one sample be subjected to GC/MS examination to verify
 that  PCB isomers are present.

          To accomplish this, the unperchlorinated portion of each extract
 is first screened by GC with the same chromatographic system used  for DCS
 determination except for a cooler column temperature, typically 165 to 200°C.
 The elution patterns are compared with those of commercial PCB mixtures (in
 hexane  solution) to determine the most similar mixture.

          After determining what PCB isomers are possible present, the sam-
 ple is examined by GC/MS using multiple ion selection techniques for ions
 characteristic of the molecular clusters of the PCBs possibly present.

     10.3  Evaporation of extracts for perchlorinatioru For cases where the
 extract will not evaporate to dryness or excessive PCB loss by volatiliza-
 tion is suspected, the hexane may be removed by azeotrophic evaporation from
 the hexane/chloroform mixture*

          Add 3 ml of chloroform to the aliquot in the culture tube. Add
 a boiling chip and concentrate  by slow boiling in a water bath to  1 ml.
 Repeat the  chloroform addition and evaporation three times in order to remove
 all residual  hexane.  Then further concentrate  (slowly) to a volume of ap-
 proximately 0.1 ml.  Under no circumstances should the water bath tempera-
 ture  be  permitted to  exceed 16°C or the solvent be evaporated to dryness.
The final  volume (0,1 ml)  may be determined with sufficient accuracy by
 comparison  of solvent level with another reaction vial containing 0.1 ml
of chloroform.  When a volume of 0.1 ml is achieved,  cap the reaction vial
 L-mediately and allow to  cool.  Proceed with the perchlorination as described
 in Section  7.3.3.
                                  72

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11.  References

          Martin, Robert M.,  "Construction Details of Isokinetic Source
Sampling Equipment," Environmental Protection Agency, Air Pollution Control
Office Publication No.  APTD-0581.

          1973 Annual Book of ASTM Standards. Part 23, Designation:  D 1179-72,

          Thompson, J.  F., Ed.,  "Analysis of Pesticide Residues in Human and
Environmental Samples," Environmental Protection Agency, Research Triangle
Park, N.C., 1974.
                                    73

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               Attachment F
Determination of Nitrogen Oxide Emissions
         from Stationary Sources

-------
 417S4
                                                           RULES  AND  REGULATIONS
 US  Sdtee Acid  SUnojrt. O.OtOO V.    rriM or
,uiiiUrd:ie to -O.oae N ajrurua 0.01W N NaOH wbjch
   pr-nouJly  been  stjind~"^"
 4.1 Saapflcj.
 4.1.1  Preparation of rollBrUon train. Me»jur« li nl of
» percent uopropunoi Into ti» mid*«t bubbxr and 15
ol ol 3 «rant hydroren peroxide Inso each ol ti« irn
twocldii't LapiciOT. Leare the aril Budget licpinrer
in jUisimbL* ti» train u iooam In Fi:rur» >>l. Adjust
prabe c»t«r to a temperature jumc:nu to pr»Tent »^t»r
ositiensauan. Place cruaned loo and srai*r around tn«
       .
 4.U  Leai-ebork •pr&xdart. A J«ai chicle prior to tin
•splint ran u opoonal: iow«Ter. » Irak rtwci af ur the
U3PU3K ran ii rrnnflainor- Tfc^laai-ccecJt procedure J
ti follows:
 Wl:o u» prob» disconnected. plac» » fi«rtram frsAure at
tb* lni«t f th» babbler and puil i noiiim  of 2s) cira
(10 In.) Ha; pi'JS or nlncti or th* outlet of tb« flow meur,
ud then ram ofl '.t» pmr.p. Tt« vacuum shall remain
lUhlt lor tt lout  30  vcondi. Carefully r»le»j» tie
ncjcn r»u*t t«Jor« rj'/«3icj the four 3Mt«r tad uj
prt7eat bart tiow of thi- unpLriirer ^Tild.
 OtStr U*i-eier)c pro.-edc.-ts may b* med. tub^rt to
tbaioproral of tie AdmirutraLor. Q.3. EnrtronjrientaJ
?n>t«tioa .Anncy. Ti* xocrdi^i cued in Method 3 11
not witablo  (or di*Dfrirm/-si padpa.
 41."i  oAmple cfU'-cr .m. Record  the IrdtiAl dry rafl
rv^r rsadinj and i~i'jmetr.c  proj«ui«. To i-Tin s»ra-
plirjl, pcmr.oft uh« -o o( Ua« prob* »t Lhcaimphnj poult,
«inc*ct Ci«»  proiv U'» U« bubbler,  and start  th« pi-j^p.
Adliat  ti«  ?an:'jl': Ho«r  to  &  conrtint rmu of up-
nroonASaiy  1.0 Lt'jr'nun a- '^iicat«63° F) or Vos. At to*
concioalon ot e*ch rjn, tarn ot? t!v» pump, remoTe prob«
(rem th« rt«fc ind record th« ftn»J  readings. Conduct &
Wtchxku'.n Section 4.1.2. (Ttu> l«4X check Ij n»nii»-
lorjr.) Ii a nMi^: Is found, 7014 ^b* t«cx mn. Drain ib.« lc«
t»lb. tnd pursre UM ramilram put o/ tbo cnin by dr»w-
Ins cle&a inibient Mr inrou£j3 UM 7y5t&a for 15 izinuCea
ltth« 5»mpUru rnu.
 Claan ambient  lir can b« pnjrid»d by p&sstni air
Ummfb a chnrcoil flJur  or  uirough an  tr_r» midg;l
topln^sr with 13 ml of 3 psrcant HjOi. The t««r nay
opt to simply DJ* idblftut air, witbo^it punflc*iloo-
 4.2  SaiopU RecoTrary- D'jconnect tbo l-Tipuiion afL«t
purjinj. Ducvd theccntanuof Lb«nudget babbier. Pour
tbi con^au of tba tsJdjst tnpinxtn Into a leak-trw
wlT«thylan« bottl* for ihiprDAot. Rinaath* Lore«mjio''Jd abe4t. U a
amount of k-xjumo t-Lj occurred, dtier TO id UM sampk*
or me m>tbod>, snbWci to UM appnrral of Lba Admini>-
truer, U) correct tic imJ ncolu.
 Traailw Ui« nmtenu o< tiw stora«« container to a
ICXVnl Tolnmetnc fliik and  ciltnci to *i»«Jy 100 nl
vlth dskiaiiod, diitliUd irua. Plpetis a a>mJ aliquot of
tijj somaoQ into a ISO-mi Etimmeyar flaik, add SO ml
ol 100 percent bo propane 1 and nro to [our drops ot tbonn
h&caur, and titrau to o pink endpaint linrn! 0 0100 N
banam percWorat*. R*p«ai aad arerufe tb« titration
7oluzi*i. Run »b'juiiwTJj each seri«ol samples. JUptt-
cal4 tltrations tsun &$ra« irlthin  1 p-arcent  OT 0^ mi,
»hjcio?«r li itrf ar.

 (Non.— Prot*«  tho 0.0100 N  Imrinjn  perchlorau
soJuCon from eraponaon at ail time*.) •

i.
      j: pl»c« a racoon j»u«« at Us« IrJet to tie drylrn
mb« and pull a Tacaora ol liO ™m tio in.)  Hi: piuc or
pmcn otf tn« outlet ar th« flow m«trr. and tb«n tnrn off
th« parop.  Tha racnua ihail ranjun ^abl*: for at >**n
30 xcoodju CareluUy nle&H tho rac&unz gau(t  beioro
rt\rt.fmt Lto Dow m at leu: fly* rerotc-
Lioiu o/ tie dry ja» mtier per ran. CaicnLit* tie alion-
aoQ (actor,  X vwet ten mettr v»--3a.-ometrK  prensure at tb« e3lt orlflci o( ti*
           dry fM meur. mm Hj (In. H().
                    ab«luu>  prewrm, 760  mm  H»

                           eLtr abaohit* Umperatara,
                                           ,_  _
                     abaoint*  Umperarore,  3r  K
           (S3* H).
       V.-Volom« of sampte ali m^k5um
 rmng tie pbftooldi2uUoaio*cid (PD3) prooBdare.
   U  AppUcuburcy. Till metnod U applicable to tins
 meuuraiaant of oicrornn, oj^ded ejnittMi Crom
 source*. Tie range oX to« metiod  bJU boen
 to Ni 2 to 4OO mfllirrajns N 0 , (ai NOO per dry s
 cubic m*ter, wrUxxrc barin( to dilate La» mmpto.
   2.1  SAID pilot (a» Tlcun 7-1). Other grab
 rjntemj or equipment,  capaMa  of  EDcejumna ounpie
 yolome to wltnin -^-in p«rc«Gt acd ^*n^^rjnn a someiACtt
 sample Totom* to aUow anAlrtl£&l  n prod del b»ltT7 to
 wltbla ±j permt, wOl  bo conjiderol accepxabke tit/at-
 niUre* iub|«rt to appro-rai ot ti« Administrator. O -3,
 EoruTjomenial  PnrucdOQ  Armey. T6»
 «qulpmeot U oaed In nunpllngt
   2-LJ Probe.  Barceflie&U  Slav tnWtui,
 heated to parent -water coodinaiaoQ acxl
 with an ln-ctack or ocd-ctack filter to mmoTe p
 matter (a plo« ot fl*J« -wooi i3 swiatoolary loe  tiia
 tmrpote).  Suinleoa ttoel  or TefVm ' tnMnv muy aim bo
 used for UM pro&a. Haafiiat Ll not naoeaaanr U IJM pro
 remain] dry damn UM {XirpUn period,
                                                       i Mention ot trad* Maw* or jporifla predncta 6ea at*
                                                      eotutturte  ejxloneioent  by UM  SnTtrcsuacotkt P»»
                                                      to: don A^caey.
                                        FEDE»AL »EOISn», VOU 42, NO. 160—THURSDAY,  AUGUST II,  1977

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                                                           RULES  AND  REGULATIONS
                                                                                                                                                417S5
                                                                                                                            SQUEEZE BULB
           PROSE
                                                         . FLASK VALV
        FILTER
  GROUND-GLASS SOCXfT,
          NO. 12/5
                  110
  >WAY STCPCOCK--
  T-flOfS. I  prssx,
  2-mm BORE, 8-nvn QO
                                                   FLASX
                                                                                                               PURGE
                                                                               THERMOMETER
                                 CCN£,
GRCUrVO-GL&SS

 STANDATO TAPEH,

  SL££VH Ma 2
                                                                          210 mm
                                               GROUND-GLASS
                                               SOCKET. § NO.  12/5
                                               PYR£X
                                                                                                                — -fO&M ENCASEMENT
                                                                                                            BOILING RASX -
                                                                                                            2-UTOCROUND-907TOM. SHCOT NECX,
                                                                                                            WITH J SLEWS NO. 24/40
                                       Figure 7-1.  Sampling  train, flask valve, and flask.
  Z.tS  Collection JiasX Two-liter boraule&te, round
 bot:om fM'I, with short seek and  24/40 standard t&ptr
 opening, protected asaffiss impkrwon or bresta^-a,
  2.L3  Flsji Valra. T-bor» stopcock connected to &
 2ViO sundard tipw Joint.
  2.1.4  TempersCOT Gacg«. Dial-type thermoowter. or
 other Umperacurs glut*, capablo  of measuring I* C
 (2* F) Intervals from -i to SO* C (24 to 125- F).
  2.1.J  Vacuum Line, Tcbina capable ol wlibstandlOf
 »vacumo(7JmmHi[ (3m. HS) absoloM pressure, wllh
  T" connection and T-bora rtopewk.
  2.1.8  Vacuum G»tw». G-tube mocotooter. 1 metw
 (36 la.), vtth 1-na (0.1-iaJ diTtsiocs. or  other esairo
 eapah'.e o( aieasurinz pressure to wiOiin i2J ma  Hz
 (0.10 in. Hj).
  2.1.7  Pump.  C»p«ta» ol  eTBCTifttlBS  tSs  coU«ctioa
 flssi to » pre«a.-» sqaal to or laa than 75 me* HLg U in.
 H?) ntuoluM.       •   •
  2.1.8  SqueeieBulb. Oc»-w»y.
  2.1.9 Voluo«trt: Pipette. 23 ml.
  2.1.10 ECop:ock »ml Gro-ccd Joint Qreaaa, A high-
 Tuuuja, hiph-i«=ip«ftrar» chlorofluorocftrbon gros* Li
 requlrwl. Halocarbon 05-53 iiu tw«n  (ound to b« eflsty TO.
  2.1.11  B&rom«lar. M«rtnr?, uieroid, or other b&rom-
 et«r c»pabls ol naasurva^ »tmosph«nc pressure to Tithun
 2J C51 Kg (0.1 10. Hi). In CADT csMa. tne b&fomacrb
 f»4l;a4ic»7b«obt£jned(rom & ctaroy nAliontl Tefitbcr
 Mrrict nation, la which cfc» tb* station valu« (whicn Is
 th« ib*jiun bammetrie pressure) shall be re quisled uid
 •n  »dJU3ttnent  lor' elzTaiiou dlSsrenws b»lw«n tb«
 »»t6er iduon ajd sa=pUng point shali be appLeJ it a
«»t« o( minus 2J mm Eg (0.1 la. Hg) per 30  m (1W ft)
devjuou incms«, or vice rena (or elevation der.Tas*.
  t2  Jimpl» RaxTerr. Th«  loUowlng tqulpment Is
rtqulrM for stepl* reeovery:
  •>•} 1   Cndtis'.ed CyUndtr. SO ml ^tii  1-m! dl-»tslon».
  2i2  Etarije  Containers.  L«»k-tr» polyethylen«

  iij  wMh Bottle. Polyethylene  or glass.   •
  2.2.1   Glass Stlrrinl Rod.
  2.2J  Twt Psper (or Indicating pH. To COTST th« pH
nag* o(7 to 14.                      ,
  7^  Analysis. Tor lh« analrus.  the followinj Kjait>- .
                                                                  Dtab«, ITi- to 2SO-mi
                                      capacity vlth Up for pounny. oo« lor each jamcle and
                                      each standard. Th« COOTS No. liOO» (shaiiow-form. )W
                                      ml) has be«o found to b« satisiactorf. Altfraativet^.
                                      polynietbyl p«nten« beakers (Naije No. 12O3, 150 ml), or
                                      glass beaiirs (liO ml) may b« ussd.  Wtwi glou b«t?r3
                                      are Lu«d. etchind of the beakers may cause »Ud m&Uer
                                      to b« pnomt In the analytical nao, the iolidj sbouJd t»
                                      removed by filtration (s*» 3*ctlon 4J).
                                       2-1. .1  Seram Bath. Low-tempenUonsov-mor thermiv
                                      staUcalJy controUM hot plate kept betow 70° C UW 7)
                                      arc accepublo alternatives.
                                       2-H   Dropping Pipette or  Dropper. Thrw  reqmrsd.
                                       SJJ.4  Polyethylen* Policeman. One for each lampi®
                                      and each standard.
                                       2J.S  GraduatBd Cylinder. 100ml with 1-tol dl-rtiionj.
                                       2.a.7  Volumetric Flastj. M ml (one for  me ft saaplf),
                                      100 ml (one for each sample and ear h ^taAdard. and ooa
                                      for tho vorklox studied O'Oi souiuoa), and 1000 ml
                                      (one).
                                       2JJ  Spectrophotomite. To measore sbaorb&nca at
                                      410 run.
                                       2.3.9  Oraduatcd PIp-rte. 10ml with 0.1-tnl dlTtsloos.
                                       2.S.10  Te
-------
  4178S
         SULSS  AND  REGULATIONS
        *bftj 10 mm H
 1 ~'~'Tt-ft Ls net
 ur-ci^ un^il tQ« l
 La *b« •*-•"*• a not to
 0.1 Lfcfl fljDC STJCT p Lin IT J^ DJ
 cJ Lbo Sjifii: irxl raJ^a  O'
 tcxl  Lb«  barcraiflcnc
                 to its
           Uje pizmp  v
 vacuum tacs an/is UJQ
 occurs in the proof* tod
 JTOOC aod punro  until
    x turn Ui« pujE3 THJ
 ("0.4 La. BO o^ UJB atopaoefc. M«ajuro Uw ^lama o'
     ml. Recoftl t&u voluaic on Ui« ftuk.
  8 4 SarnpU  'Mncan
         coodJUoaa.
                                                                                                                                        'dry
                                                                                                                                                   camsct«J
   .
  5 2-1  Opamum W»»l«MLh Doumsunaiioa. For
fised  and  vwiJJUfl  wuTOJ«rteth  8p^3Crophotom
caljbfBA*  fc£aiQ3t aiaodATd oardJ^d  ^rav»»onfrt& o
am, eTttT a mcMiUij. AiUmmUvaiy, tor
Uo«th n»£Q^p(>o'^ni(it(^-a, scan
                                                                                                   ol
       *_i» a~£r=nc& in ^ mercury ^3'eJi in the m&ooai-
*&«•. T5« aissoia^a intoned  pr^ssare to  tile tiaafe  (Pi)
IB  pasnrut dis
eo37«J3:an- OTyjen nay t>a inJr-^diacad  into lii« flAtt
by era oi  Lireo  meUxxls;  Q) B-oforo aT^omuns tio
g^cpiin^ flMX, nxLLh ^rlLb p^ii"D crliiKl&i  oay^an, then
C7ucra0« Sadk to 75 3Lm E^ (3 in. Hrj) Eubcotmo praeisur®
cf tesa; 07 (2) LaJ'jrt cry^im Lnto Lbo flaai: aJiar mnpiin^:
or (3) tansizAts Eamouns "»nth & mirLLmtjrn a/ 50  mm
Hg (2 )n_  Hg) ¥Tbaiu^a rtmaLolDfl LH Uio fte»sJr,  nsoord
Uua rtn^l p/esjanra, and cboD Ysni th-a £L&>ii: to the su*
          until tba Cj^ii prtssoro u alnaaji aquaJ. lo
Section 4.2.2). H a p«a^ docs not occur.  tlM
Lometef 15 probably m&lfoncUoalna, aod ahould b« r»-
paired When a paa£ h obtain^ w^Uiin th« 4CO to 415 nm
ranye, the -eTTei^Ui at wolcfc Una p**Jt oonira 3&aU bo
ih* opOEicrm warei«f>BCb (or  tfw  m«airemar
aorbanofi for beta tft« iuadAfda and  ssropl^.
  A.2.2  D*t*najaaCion  o( 8 p*-ctjo photometer
^lon Factor E*. Add 0.0. 1.0, 2-0, 3A and 4-0 ml £ ti»
£NO» worirlns stirwianl aoiacion (1 mJ-100 wZ NOi) u>
a sari« of GT» porraUun flvaporatijyr dbh«. To ^;h  &dd
23 mJ of ibsofbtng i*ohiClofl. 10 ml dflionJwdl. duCUUsl
tniai, sad sodinm  bydraaado (IN), dropwua, onUl to*
pH }B bersseffl 9 and  12 C&boae 25  to 13 drapa each).
B^rlniunf  with the «v^poraiion step, follow tb« an&Jf-
aia proredors of SecUoo 4 .a. antli the soroGon tms txwn
tranaMn-H u> the 100 ml ^Dajraacric flask and dJhatfd to
tbamarte. Meascro Uw abs&rbano* o( »^d5 solation, at t^«
oDUmoin  "s^Bv^iaaffUa.  as determined In SecUon 4.2.1.
Thl3caiitjrauoA pn?c«iaraiiiiist b* rBp»at*d on aschdi?
UiAt sample an> analyr«d. CAlcajlat* ttie spec crop CtoUTm-
PMT cajjbrs-ciofi factor &fl t
                                   Equation 7-1
                 of tho
                 o« Use
                             NOi standard
  4.2  Sampl-a Rftcover7  Lot tiio flmk sat (of a minimum
of 16 hours tmd Lhac. ic^ks  H£HJ oim^nu (of 2 nunuias.
Gconect tiw fliy^ ;o u EDardiT/ flUert U-tufc»® maoooataf-
Opsri tb*  1?aJvci tram tlw SjniL to tb-s maaaaiatAr aind
record  too nijfc   tGrapara^apj  (T^}>  Lh© burois«a1c
       ,                             manrary l«^9b
      maaaraaL*-r. Tbe  abeolute  Lnlaroal prtaeajn Ln
t^o  dflds (Pr) Ls Uaa baracaetilc pTBaooro lesa tho siars»
omoWJ n^LfjLng- Tran^&f tho c0ntanU! o^ Uia flAfcS to 6
tew^-fr?*  potyef-byleno bottle.  Rlnsa Ct>s fl^^k t^rtaj
•arid .'j-jul ponionj o^ doronjisfd, '±L:-uljwl waiif and &cid
too  rinsn W^LAT ui Uio boru*. AcUosi UM pH
0 dnd 12 by wiciin^ sodtirs Ja>Tarajada 0. N)f
(abrrat 25  Eo &5 drops),  Cb^ik UK pH "br  dlp
fftimry? rod Luto Lbe tolcj^oa c^id than toucning  ttw nxl
to tba pH t«st paper. RcniovQ,B^ LJ riis niatarisj aj poaELbla
  irj[ Lais swp. iUrt i^n ^sj~^i of CM Uqoid Uvei 3*
     the coDLiLiiej' can  tv? c&^t±Bd  fo*- katc^s  aH-a-
                tho Di^^Lisi&r to ciaarly id*ali^ its
      Baromeujf. CaiJbraia
                                                                                  NOi
                                             barem-
   .
  5.4  Tompsirfttare Q&a^v. C&librmU dial thenaonwtei-B
                                   -
  5J.  Vacno^n Oauga. CiiibraU m«d?enJcftl  emusea, If
Q3«d. a^&In5i & marcury maDom«Uf socb as thai speci-
fied LQ2.1JS.
  i.fl  An&Jytieal Baiaoca.  Caiibrat*  against
                         s, petaiolnt at l«Mt one
                         o( th* fccqalred d*(
oS figures &ftw liraaJ caJcuIaUoJMk
  6.1  Nomenclature.
    X™ Ahaorbajic* of sampJa.
    C«Cotkt.xnCraUcMi of NO. u NOr, dry basda, cop-
                ofc^ ti>& k^j^i of tha Llo.oid in c
    confirm T7l>«U>ir -or not DJIJ suspia T-Tt
        E.; now Una oss UD-J-  oatLbrQckl daU flh&at» Lf a
  iiT^ab^ 8J30HQ15 oi itt'-icA^- has cecGT'ed, either vnid
    ;.uT.plo or usy ni'i^KxL^, 3B,t*->ee£ to t^e  approT&l ol
    AdmLn.LscrtiJii', *»o corrvcrt tJ>c lioal nssultA Iima-sdiF-
  i7  pnof to anaiyaii, u-aaaiaf tho coac^fiU of tb*
       g coaLfiuaer  to  a SO-tnJ  YoiomQ&li  najkr and
       » coQLsJnar r^ea rrttii 6- mi porUoo^ of d&ionifed.
        w-ttar. Add C^o rinse •wais' w  th« fi^afe ana
  lijt* to the mo-fe  vnth ddonissd, dirtiUed wst^r; fTLfat
           P'.pet^a i 25- nt  aiiqoae Into Uio pnxxiila
            diSJ3. Kettiro.  E^iy nrLca^d  portion of the
     -lo  to the paly-L'thjykjQo  .U-orags bcEUa.  E^aporiLa
tba 26-di Miqiiot to  drrness cm a s&a&m bath &ad allow
to oooL Add * ml.ohfeaotdi3Tili?aSi axJd solation to tbe
dr;td rssidas and inturax* tboroojii^' -aith a po^lfit-byl-
tD1? policernaD. M^o sura iho-ioidtioTi conUicts &!] th*
r*iicj«. Add  1 ml d^oaic^a, distilled ^•ruiar and fois1
drups of coa[^ntr3^i s-vj/cnc ackl, H&sE. U3e soluttoa
era D p^ea'n bbth far 3 nunLitAS wit£i crc&sioa&i ffUrrlny.
.UJo^ t.*io toladon to CDO', add SO mJ dfefanJu^l, distQl« the range of calibration).
       aHaas ofNO« &a NOjin ga        .
        Flofti &b«)hit< pressure &f flast, mm Hg (In.
       -IfuUal ab*olutj? prcssora
                                     ask ,*K (*R).
                volom« ai
                                                 .
                                          Z (62S* R)
                                     eoodietans  (dry
                                , ml.
   V.,,
                                ,
    V« n Volume of ftbeorbln^ flotation.
     2«-60/^S,  the obqaot factor. (If oUier than a
        aUqoot ww  o.'wd  for &naJy3l«, th?
        inff factor muat ba sabatitutwi).
  C.2 EAmpJe Tohi23«, dry tmyls, oorrcct3 e^tsiTBadT^,
fubj^rx to tJie aopro^nii of th-o ^.dsinistrato?) . ajj iollows:
fJttr CinDU^ei "^aatman No- 41 frfter pap*rinU) & ICO-ml
volutnatnc rtwt; rtnje the evEporu^ng dJsh wliji thrw
5-mJ portions ol duoniiE-i, distilled s'aUr; fjttr theaa
      rias*^. W&sh the nliar -s-ltb  aX 1-east thrfca 15-cU
         of  d»ionU*d,  dlraHed ^ratar.  Add tbs  filur
         to the coatsnLi  of Lha ToJo^ialric fiii^  aod
diijx^ to th« rr'jirij  witi dciooiMd, distilled "«^Laf. I/
soLJda fcra it5?nt. ihe SilcrJoQ CLQ be Trarjiamjd dirKUy
t.5 Ue IQO-ml volam*tnc fjai: aad  diluted to the r
                                                      v...
                                                                                      Ti.
                            .
 tvi  tiwroujibiy, and mea.surs Ibs e^jK3rbs^c« U tb«
 cptunum  T-iTt-firistb aa&d iof  Ita  standA.nl 3  (S«Uon
 i.2.1), rj:::^ tiw blruj ic',c.uoa as a ^ero reference. DiluU
 U;a sirr.plcj and '.he  oUni: -zr.ih e known  p^ior Ln
    ?. As&j»nble ULJ-J .^LII; a^a Aa&scy
Triangle Pwi. N.C. Octobor S, 1973.
  8. Hamil, H.  F. tnd  B. E. Thomas, Co
Sti3d7 oi Mrtiiod tor  tiso  Dr&ornunaUOTi oi N
Ond« Emisnona from Stationary Soorrm CN Icrlc Acid
PlanU).  Soatirwess ReM&rdJ laitttute  report (or Eiv-
•viroomacrtai  Prow^rdon A^ftncy.
Past. N.C. May 8, 1874.
METHOD 3-D BITS EMTWATIOK 01? amJTTSJC  ASD
  AWB Smroa DIOUDS  EicaaioMffl Faoa
  Sotmoa

1. J^rindpbanf/lppUaiMUtf
  1.1  Prindpla. A JM mmpki b ertractsd
trom  the rtscte. The suifnne acid mist, (irn-lnding soi-'ur
trioiid«) &od the raLftu dJood* are SQpsjxDad, eod
tractions a« meaamid ssparawlj by tba
  U  ApplieabUlty. Thb moiiiod la sppUrabls to tha
6«i*nalnAUon ol mlfuno acid  mire  (Uidudii^ soltar
trionda, and In the ibMrroe ol oth« jxrUcnUt* mtttar)
and sultnr dJoudA e/nissioiu from sraMooaJT  fwmreaa.
              tasu  bavo sbown  Lhac tbe  TninJmnra
      abk llnua o4 lh& nwUiod BJIS 0.0i DuUiipTMUV'cabki
       (O.OJy.10-' poiuxlVcublo  foot)  (or sulfur oloiidt
ojid U mgjrn' (aT<   1O-1 Ib/ft1)  tor sulfur dloslda. No
upper Umiu bjnr« b«Q ertabLhh^d. Baaed on th«oretldad
calcuiftUonA for  200 milillitar3 of 3 p«r«Qt bydrogoni
p«rodd« Kjlotioo,  tbe uppar coooantrBaon- limit tor
3aUnr dioxide in » 1.0 W (3iJ It>) s»s sampls  U abool
12,400 nsrtn'  (7.7X10-" lb/f.'). Tha uppsr limit can b»  ,
iitAoded b-y Incnairia U» quantity oJptnnidjt toiuUaE
In Lb« imp^ngon.
  Possibl* kit«riertn5 a^nts of this raeUnxl ftftt &ncffic3«a,
free ammcmia, and  dimeLhyl aniitna, U aay  o( thaw
lnl«r(»ring agents am present  (UUs caa be diU/mkud b?
Jmowiidj? of  tht procaas), alUnmtiTe  metaodl, 3ub|*cC
to  tli«  appfOTeJ of Lh«  Administrator,  flj^i nta! probe HrLprs-
   2-lJ  PltotTub*. Same u  Jietbod 5, 8
                                                   EK5ISTT1, VOL 42, NO.  UC—THUSSOAY,  AUGUST  18, 1977

-------
                                                        RULES  AND  REGULATIONS


                                T£M?ERATUHE SSHSOR
                                                                                                                                       417S7
      g—^--—^ •••-••• "  -        _ _  <
                                            PR08I
 F8QSE
             7
 REVERSE TYPE
   PITOT TTJSE
                       PITOT TUBE

                       TZM?EBATURI SEKS3R
                                                                          FILTER HOLDER
                                                                                                              THERMOMETER
                                                                                                                              .CHECK

                                                                                                                             /VALVE
                                                                                                                            |H '
                                                                  ICE BATH             IMP1NGERS


                                                                         BY-PASS VALVE
                                                                                                                                  VACUUM
                                                                                                                                     LINE
                                                                                                                             VACUUM
                                                                                                                               GAUGE

                                                                                                                MAIN VALVE
                                   DRY TEST METER
                                           Figure 8-1".  Sulfuric acid mist sampling train.
   U.< DtCtnntUl Presraro Gnus*. S*ia«M Method J,

   1U Ftiter Holder. Boimillcato glass, irtth « gtaai
  mt fUter juppon aad a lilieon* robber faibet. Oibsr
  ruut materials, e.g., Tanon of Vtton. may b» ossd STID-
  82to lb" »Pf>roTiJ "1 the Administrator. The holder
  wjn jhmll proTld* a poaiUTa WA! against InJuz* torn
  lu outaide or around tb» filter. The fllur bolder shall
  w placed b*tw«n the first and wcood taplnjsra. Ncu:
  Do cot beat tb* al«r hoidtr.
   S.l.8 taplmnrs—Four, as shorn la Tliron 8-1. Tb«
  Wt and third liiili b» o/ tb« Onwabanf-Staith deslsn
  J™ «t«>tainfd  Irtm cccuEnrcial sourcu  occa-
rmnnilly hat perailda Unpuntiw that will causa w-
          iyh ralftirie add  mist  neajnnmMnt.  TT»
tba foUowing t.ASt for detecting p«rar!de3 In e«cb lot of
Isopropiuiol: Sh&ks 10 ml of the uo pro paool wlUi 10 ni
o( /rwaly prepared 10 percent potostiom IcKlid* solatioa.
Prepare a ilao-t by ti^ularly  cmUof 10 ml of <1iitll.led
wnier. Alter 1 mlaata, mad the abjor banca on % spectro-
pbotoraeUr at 1S2 nanometirj. 1J tno absocbacoi eicoedj
0.1. tbe Ljoprop*nol sbaU not b« as«-
a^ent^radalsopifopanol wun sujtably lonrp«aTaddoleTBli
Ij rnadily nrwiobk from commercial soorcea; thtrttore.
ntaction of conuminat*d lou cay  bt man jEkiant
tb&n foUovIng lh« p«roucU removal pnx^dun.
  3.1J  Hydrosan  Peroild«,  3  Perwnt- Dllot* ICO Tnl
o(30p»reej\tnydro«tn parotids to lUtinrtth
dinilled vrsur. Preparo frMh daily.
  3.1.8  Crushed loa.
  3,2  Sample llacoTery.
  3^.1  Water. Sn"n as 3.1.1
                                                                                                  3.3
                                                                                                  3.3.1  Wiur. Same
                                                                                                  3.3.2  Isocropwjol, 100 Peir«at.
                                                                                                  3-3.3  T'-ma Indjcitor. l-(o-*r5onoph»nylaio>-2^i»pb-
                                                                                                tbol-3,  6-dl5i:Uonlc acid, disodium salt, or CTnlrsJ«n^
                                                                                                D'.asclve O.M g In 100 ml ol deionlieil, disUU»d watar.
                                                                                                  3.1*  Barium Parchlor&u (0.0100 Nonaal). Dts=l-n>
 In 3O1 c-J deionlwcS. disulled sniler^ nd dilats to 1 IIUT
 with [sr>proi7*nol; 1.22 g of b&ntnn chiorld* dthyiirv*
 {BaC^^:Hr•j) may be used losteftd of th* ba.-.n2s p«>-
 chlora:e. StandardiiB with jul.'ur.c acirt « In ?-rUon ;• 2.
 This soluuon iciis be prot««d agalaat «npor»Coo 51
 ail timea.
                                   FIDERAL S£GI5TE«, VOL 42, NO.  UO—THUU3AY.  AUGUST  18, 1977

-------
 41TS8
                                                           RULES  AND  REGULATIONS
  3.3-5 SoUnrtt Acid Standard (0.0300 N). Pnjthao* or
EtimiajTiiLe to ^raoCCB N ajnun« OJ31CO -N' N»OH ti»*
him  oroTtoaaiy  i*— °  jtandiroiml  againsi  frnna/T
rtandird potasaum i£
       : rttAin  & portloa ol saah r^uant  for oaa u  »
                   flbous 200 g oi ulicb sal In Lb« lounji
   _           .
  4 1_1  PTBIOCI Preparukm. Follow tba procedure oat-
lined la Method  i, B«tJan 4.1J; fllun jtoajd b» IB-
fpwr.nl, but nwd noi bo drareested. wmsiwd, or Idami-
iied I/ the efjnftni iras caji b* cocsiderBd dry , La. , mois-
ture lrw». tb» slica eel nwd no* b« weighed.
  4 1.2  preliminary DeierrcunjiLionj- Follow the pro-
eodure  outlined in Motnod 5, Section -1.1-i
  41.3  f^parsJ^a of ColiairEiC'a Train. Follow tb« pjo»
txlura  oatkned In  MottKXt i, &wooo i.1-3' (inapt tor
the 5*oMirut
0-5 g snd reaord«L
  4.L*   Prrtcrj L»i-Cls«ck  Prooednra. Follow tin
basic procectun outUn«d In Hemod  5, 3«coon i.l.i-1,
coons vhx Uit protM beaur  &O&11 t» &cUualed  to U»
minlr^rrm  t€fflpar*tUTB  reqQiTwl to pfBI^BOt  OOQd*nJ>^
tloo. aa4 iiso ULU T«t»» such us. "• •  • plugging UM
Lnkt to  th« flJLn-  nokltf •  •  '." ibaU b« replaoBCl by.
               the tnl«* to Ina flias
  4-L-i  Train OpertUoo,  Follow tb« baste procedures
ootliziad La irfaibod i, Section 4.1-5, In cooJoDenoa ~vr\i
                                                                                                    erf
 oa a Ab«t «*"P*» to th» cx>« In
 raw uail nu* nc*~\i 0.030 nj'itun a.O c&n) dunas
 rtm. Panoilieul>r du. ictt tb« U^K,
 hn« b«t^«^Mi Ui4> protM UK! am LnrpinAai lor
 coad«OAUca. II it doui« occar, wllust t^o pfoJD
 »tanff apw^rd to  UM minimnm tAmpara&3r» raqulnxi
 to prQT^ai cr>cKi4n3a£lotL. II oompoa&ot duugios  NK>OTXI«
 B«cBS3Br7 dorwc a run. & kMiA-cn«dc fthfcH b« doo« Uo»
 ZDodUul; Man each duuu*. i»x>ardini! to U» prccodnni
 aariinsd In Ssedon -U.U of iletiiod 5 (irtta uppfwcw-LMo
 BuxHf)n»rtnn«. u mcotknMd  In  Scctloo tl.4  a/  Uxla
 mtttiod):  record all  LtaJt  ritaa, U t&o Icnttxn ratois)
 uuxed ti« ippdifsl rsna, UM unu-r xb&U &!U>or mid Uj»
 run or «ft*^  pl&n to «Drr«ct ta« aunpio "raloma AA oo%-
lin«d tn S«edoo U  of Metbod i. LoinusdiAUlsr oXUr COD>
poo tat  change*,  l«sA<±>«j3  im  optioa&l. U
WJj-i!i«ii3 «™ dooa, UM procKlnn oaUiowi is
      01  Muthod  i  (Tttb
  PLANT.
  OPE3ATOH _ .

  DATE _

  RUN NO __

  SAMPLE BOX NO. _

  METEHBOXNO._
  C FACTO H
  P1TOTTU8S COEFFICIENT. Cp.
                                      STATIC PRJSWJRE, SHE H( G& MgJ

                                      AMBIINT TEM?f aATURE _
                                      ASSUMIB MOISTURE,%

                                      PROSE LENGTH, m (W _
                                               SCHEMATIC Of STACX CSOSS SECTICW
                                      NOZZLE IDENTIFICATION N0.___	

                                      AVERAGE CALIBRATED NOZZU DIAMETEfl, em(iaj.

                                      PROBE HEATER SFTTI MS	_.

                                      LEAK RATE, m^/min,lEfm)__	

                                      PROBE LINER MATERIAL	

                                      FltTBRHO.   	    '    	:	
TRAVERSE ?OIHT
tl UMBER •'


,









TOTAl
SAMF11M6
TWE
15 (, B™.
VAeuuu
sm H3
r«.H>r
, 1












AVHRAGS













STACK
TEH?£aATURE
as).
»Cl»F)














VELoerry
HEAD
,, the
  i^t.- s^iil eiiher conrct ths eainpls volojn*, ej o
   3e uwd.
  <-1.8 Ciknli;ioa  ol ft/cent isotiaetic.  Follow tea
f^^'^TB ou^aed in M g acd record tau weight.
  Transfer t»« conienu of ths orst iioplnjer to i 1'fl-cJ
gridoated cylinder.  Rins« the probe, nrst impingtr, &11
ooantcuoj gljS5w»r« before ta« nlu>r, and the Iront half
of tae ftlUr oolder with SO percect Isopronar.^!. Add tb»
linie solution to the cylinder. Dilute to 250 Tril with 50
percent tsupropanol. Add th« filter to tha solution. -MIT,
and tranter to tbeytora^e coatainer. Prottct the soliiuor.
against eTaporitlcr.. .'•.irk  the laTel  of liquid oa Let
container and id^nufy thasamplfe-coatainer.
  4iJ  Conlair.:r No. 5. II a m^iJturB conwnt i^iiysia
la to be don*,  w^uh tbe second ind tiird impinsen
(plus contents) to tho nearest 0-i  g  icd record  thfw
•weights. Also, w«i«h the spent jilica jel (or  silica ;;1
pluj Lmpu^cprl to the n«*nst 0.5 £.
   Trao^zr  the aolat'.oru from th» woond  »ad  tiird
taplnge/s to a 1000-nJ gradiiited  cylinder. Rinse «U
conaectir.^ jliir^AT* (including back balf of filter bolder)
between tie rjter iod uiics gal Lmplnjer
 distilled w»ter, and add thii rin« wst«r to the
 Dilute to a volume of 1COO ml with dtioau>&d. di?riUf*A
 wster. Transfer the notation to & storasa cootainer. Mitt
 the lerel o! liquid on the coatalner. Sea! and identify the
 sample container.
   •1J  AruUyii
   Not* tae level of liquid In eontilneralaodS, and con-
 firm whether or not any sample was lost dorlrn ainp-
 I=e3t; note fh[< on the analytical data sheet. Lf a DoCce-
 ttsla taioont of ltaii?» n«  occurred, eltber Toid  tie
   mple or uw methi>lj.  subject to the approril of tae
                                     .
        Contiiner N'o.  1. ShaKe thi container fcolditff
 the bopropanol aolatioo ami  tan  filter.  If tiw  tila
 S?«at a up, allow the fra?r.exi--s to settle for a lew nlnoto
 b*',irr r«=ioTics: a acple. P'.;-^te a 100-nl oUiiuot of
 thj solution into a 2^O-izLl Erltnzn»yer Iwi, add 2 to 4
 d.-tjp3 of thorin Indicator. a-Td t:crat» to a pini taclpi^i
 ttsln« 0-01 CO S ban am per chlorate. Rep-sn to» tltrn:ou
 Trtin a iscond aliquot afwjnpl* and lytraja
                                       FcDElAJ. EEOISTH,  VOL.  <2,  NO.  160—THU2SOAY,  AUGUST  IB. 1977

-------
                                  RULES  AND  REGULATIONS
      .  eplicate tltniioiu meat t^rw within 1 pwtMit
or 0.2 ml. which* TU is greater.
  4-3J  Couuuiar No. 2. Thoromtily ™'T tb» «nlnti>««
In the conUioar holding the eonUnu o( ta« aecood aod
ttlrd uaalngen. Piped* * lO-ml ikqool of «»mpu Lnio m
2JO.nl irlanmeyM tut- Add ml o< Uopropmol. 1  to
4 drops of thortn mdlrXtr. and How* to a pint endpalns
Tyring 0.0100 N barium parchlorata. Rapo^l to« trtratioa
wtth m second aUqoo* of aajjipU and anrare tQf t
                                    e   f    ^cn
     . R»piicate dtrallooj mnzt a£m within 1 penoit
or OJ ml, wblciWTw Li (nat«r.
  4.3J  Blanks. Prepare blanks by »ddin»; 2 to 4 drop*
of thortn Lcdlcaior to 100 ml o/ 80 p*raai l»aropanoi.
Tlcritt the blanri In UM
  3.1  Calibret* eerainmaot miny t&* procedure* *p»ci-
fl«d in tti* foUowinj eectiooj o( Method 5: Section JJ
(meterinj lyman); 3«cUoa  SJ (tmnperamro gaaiw):
8«doa S.7  rbarorn»L«r).  Not* that  tB« reoomme3>d*d
I«ai-cb<>ct of the mtwrtnjt jrn«m. «
                               CBlU. EV> (ff).
                                icwuu, proportiao
                      ,
  CH>3O(-9aI/uric icid fincladlng SOi) ooooantr»aoc,
            t/dicm Gb/dacO.
     C30i-Sui!cr dioxide coacantndoa,  g/dxm (lb/
            dscn.
        7— Psrwnt of LsotLutk sunpUn^.
         "           of barium.
                          .
        r— Biroceuio presmra U ti«
            mm Hf (In. Eg).
       P, -Abaolata suci gu pi MI are,
            EgJ.
     P(td-8tAnd&rd
            C3.92U1. E?).
      T. - AT>TU> ib«ola
            (JM Flr^ra 8-2), • K r B).
     Trtd

       V.
                                       pllag slto,

                                       -m Hj (In.
                                     790
            Fl?ar«»-2).' E (• H).
           Sticdirf  tixoluta  tuapen&m, 2X1* K
            (S3- S).
           Volm« of EMnpU illqaot ttt»Ud, 100 n»J
            far E^Oi »oa 10 nil lor 9O>.
           Toul Tolaci* of Uauld ooC*rted In Inplnjtn
            &cd silica gal, Tni.
           Volcm. o/ nj HasnU u mcuand by dry
           e^j ^»ur, dc^ (dcf)- .
           VolacM! at tu  s*aipU DMjarsd by th« dry
           gu m«t£r cnmcua u> ntnfltrd coadlUoai,
           rivm (dxf).
       », — Artrso "">• ru ralodty. ci^nlited by
           Mrthod I, £q o»noa 2-«. otr* diU obukiad
           from Method 8, nv»e (fL'see)-
    V»ki-Tocil  Tonnzj oi Mlotloa  la  vbJcb the
           •aittTic iu:id or  ralrar dlozJda  s&zapU Is
           ooatained, 1V3 nl or 1,000 ml, rwp, mJa.
      13.8- Specific grarlty at BMreury.
       Vi

      Vu
       100"CoOT«rsloo to perCTnt.
  8J  Arer«9 dry gaj m«« t«mp*ralur» and i
oriioe preasurj d.-op. S« d»u ab«t C?ljur» g-2).
  SJ  Dry Gsa Volume.  Corrtrt tb« sample Tolomt
mnsurrd  by th« dry KM mewr to standtrd conditions
(W C &nd T60 mm Hf or 48° 1 »nd 29.32 la. Hg) by nsLng
EqoitionS-1.
                              P.*
                                 Equation S-l

where:
  tf,«.-O.MS3*K/inni Hg for metric units.
     - 17.M • R/ln. Hg tar English unit*.

  NOT*.—If the leai rate ct^wrexl d'lrtag any manda-
tory Itii-cbtcts ti=wdj the «p«ited accepiabU rate,
tte t«;«T shall either correct the value of V. in Equation
8-1 las  deicnb*i  in Section «J of Method 5), or shell
LiTalldat* Ite lost run.
                                                       8.4 Volnm» of Vfsttr Vapor sod MoltTim Cotrtent.
                                                     "ilrnlaTo the Tnlome of v^tar ^aoor n.i^^ Kquailoa
                                                     W of Methul 5; ti> veJlcht o< vuer coU«^e>i in UM
                                                     impii^in iod «il!o> gti cxa b« dlrtctry con-nrud u
                                                     miillilun IL&« »p«iae granry at nut u 1  I'm!). Cii-
                                                     cuiALe th« moiscurB contact oi th* exact {u. r^«^T Equa-
                                                     tion 6-a of Metaod i. Tbe "T^oi*" tn 8*cnoo d-iolketLod
                                                     S abo appllea to Um m*U»d. Not* ">" U th« t3o«n gmi
                                                     stn*m can b« coojid«mi dry, Lh« T^lom
                                                     and rrrurmre cotocnt n««l CM be calcuiaiad.
                                                                                      Equation 8-2
                                                     where:
                                                       A'i-0.04904 cAnffliecialTaUat for ineCrle anita.
                                                         — 1.081XK1-1 lb/n«q tor Eotliai unlta.
                                                       && Sullor "Ilin^ t nrift^Tntrfcr'Tn
                                                                               y^T.
                                                                                      Equation 8-3
                                                       A'i-O.CO3B|t/ra«j fornjetric anlti.
                                                         -T.OaiXlO-1 lbnn«I tot EajUiJi aura.
                                                       9.7  Lao^daeQc Varutian.
                                                       6,74.  Cilcnlnf'oa Iram rs^> <1nr»
                                                         100 T.^ V.,
                                 Eqxiation 8-4

where:
  i"i-0.0034«* mm Hi-m'/mi-*E (or metric anlu.
    -O.OOW78 tn. Hj^t'rtnl-'R for Ecgkia aniu.
  fl.7 J C&lcai&tioa from Int
                                 Equation 8-5
Then:
  iTt-trn for metric units.
    -O.CB450 for Ennliih ooitt.
  4J  Auxpubl*  Rtsul^. IJ 90 p«rc«nt non o( SoUor Dlotid*
ZmliSloAs trom Stadonary Sourceo  fFoail  ?o«i-Flr»
-------
             Attachment G
Determination of Particulate Emissions
       from Stationary Sources

-------
41775
                            RULES  AND  REGULATIONS
                                                      It Into '.be jtaci, and
                        sample at i mnm«nl rax* vw/ mosi«n  *boiu  30
                        liters (1.1 ft1) or nnal TTrib*« ttqiud dreplem lire earned
                        orer from th* fJrst.-impm«w  ta  Un  ••mgvrf   R/-CDHJ
                        temperature. t* >!JMUB« atoul dry pd  mner rniiillnci  **
                        required by Flrcre 4-i.  '--i.
                          3.£-3  After  ooU«ct}jj$--t&«r3aHip^ omnbtr* the «m-
                        tenu of tbe t w« unpjngors aad jozzuure tba voicst to Lbe
                         3.3  Calep-ALJarta-Th..^^^^ tpj!tjylfj pj^wtfufd Li
                        desiimed  to  efitmasn . th» mm^rnm La  UM suuit cu^
                        UierrJom, other  rtim, vmca wo oaiy IMU^UT (or to-
                        cent. moi«ur» d.maraln*aara. »r» noi coU«cu»J. Tii«
                        lolloping  8qa»tioMad«jiBU«tj «UHULP [ho mouta™
                                   tho  txu^nm g^  CL-T *»r contents, mJ.
  — Dry &U ToUoai jaauurcd by dry PJ m»t«r,
   dcm (dd)..
  —Drf gajureterae nMBKirad br dry ru meUr.
            '  «- auradani  coodiLiooa,  dscm
                              V/
                              V<
                             V.
                                  to stUKUrd rnixilrVmt. u-n (sen.
                            •  «.,». Denary of wMar. afflWSirtni (0.00201 lb/m!).
                          3.3.3  Voiamo a^ w^sr ~
                                                         Equation 4-5
                        vhera:
                          K,-0.fXH333 tnVrnl far SMirte units
                            -aw;07 ft*/ml tar .EnsHJO anns.
                                           • I,
                                               V.P.
                               -
                            —17.6* *
                                                          Equation 4-6


                                   •S/mm HU for metric 0-iiU
                                                                                    -4- (0.025)
                                                                                                              Equatiou
                                                 4.1
      Tor th« rtltftaca metiiod, cahbraw »qii]tra)iint u
«p«i«J li tha tollawuii Mcaooa o( M»Lhod i. oectloo.4 J
(moinrmg  rynua); &rctlim  5-i (iempr
and  S«cuon A." \7xinTznaL«f). Tb« reco
ebeck of tba uiauniBi nmun I Section 6.6 o( MoOxxl i)
also *ppU«a to tbo re^c? inetbod. Tor tli« approxuB*-
tlon mecbod. UM tho proc* cahbrAU tbo metering 5T3X«m. tno> tb«
procedure  o< Meibod i, &*cuon  6.7 u>  cxllbreu tbe
barameur.
  1. Air Pollution InjiawrlB!|MAaa«J(S*
-------
                                                       BULES AND  REGULATIONS
                                                                                                                                         41777
                          TEMPERATURE SENSOR
                   -  PROBE

                   TEMPERATURE

P.TOTTUBE         f*SOR
                     /n
        PROBE   /
                _/     h-WALL
              k    •».   *—'	
                  REVERSE-TYPE
                    P1TOTTUBE
                                                                                 IMPINGER TRAIN OPTIONAL, MAY BE REPLACED
                                                                                          BY AN EQUIVALENT CONDENSER
                                                            HEATED AREA    THERMOMETER
            THERMOMETER

                  /
                                                      IMPINGERS                      ICE BATH

                                                                    BY-PASS VALVE
                                     PITOT MANOMETER

                                                   ORIFICE
                                                                                                                                     CHECK
                                                                                                                                     VALVE
                                                                                                                                      VACUUM
                                                                                                                                        LINE
                                                                                                                VACUUM
                                                                                                                 GAUGE
                                  THERMOMETERS
                                                     DRY GAS METER
                                                               AIR-TIGHT
                                                                  PUMP
                                                     rjgure 5  1. Paniculate-sampling, train.
  2.1.1  Probe Xocxla. SrthiViM s£*«l (31R or gbs* with
abarp, tapered leading  evica. Tbe. ac*U  o( tapir shaQ
be- SCO* and- the- .taper inea'l b* oo t&e outside to preserve
ft conscuit ttti^roai ftiimmr Tbe proble i ****** f H»r^ ^^
of UM buttoo-hooJt or elbe*" de*i«rc. unless otherwise
specified  by UM  ArrminitrraMr. u made ai scaiaiem
ite«l. toe- DOuM ihall b* eansarueted tram mmlm .Tii>
1cg:c>ib*raaunai*oiconjtructioa may be used, subject
to the appro**! of tb» Artminrtira.vir.
  A nags of aottl*. SUM sui cattle. tot isoldaetta ~™piint
»hould 1>« araila&a, t£_ ) Mining » 8" tern-
penaire at  tbe »it end danng xunpliof o< 120-±H* C
(SloiiS* F), or each other uaperatun «J lp«Ui«d  by
an appUcftble subpart o^ Ui« sCAadArda or approved  by
Che Adcuois&ator lor t  p&rtlcuXv nppUcAtioo.  (T&9
te^urizuy opt Ujopcnxe th« e^uipcien£«tai«c2perimrt
lowv in»a mat specified.) Sinn ;Sf icuad tunperuurt
at u>*outl«to(ib« probe ii not tuu&Ux monitored duhnx
si^pUnl. probu conjlrjcwd occordLu to APTD-OiSI
and utiiuioi the calibrauoo CUTTM of APT!>-Oi76  (or
e^ttbrat^l accordihc to  l^e  procedure  outlined  in
APTlXii'O) »ill b« considered aerrpuble.
  Ei:a«r borj«iii between 490
and MO* C (>"« and l.£JO* F). Boib trpt! ol Unen may
be tu«d  at hither teoperatitfts ibin spoci&ed lor siort
periodi of time, subject to tbe approTal of tbi Adminis-
c»:or. Tbe  solwnmt luDperuurt (or boroiillrwe li
SJJ" C (1.JCS* F), and tor rjuaru li Is !,» • C C.nj* F).
  Wbenever practical, crery eL'orv tbouid be made to UM
IxxuiiUnM  or quaru iili= probe iLT.»n.  AlteJT.atively,
oeutl Unen (e.j.. 316 stauiiu* $tKi, J ncoloy K!i.' tit oilier
nim»ion ruistuat meuui aiad« of warn If is tubme may
be U5ed,  subjrc. lo tbe  approval of ihf Administrator.
  :.!.3   Puol Tube. Type i. a.- descrbed m Sn-iion C.I
of Method 3, or other devin approved by tbe Adirjnis-
t.TM/jr The  pitot nibe ;ball be aiiu-hed to the prcU  (as
^io»*n in Ki'jur? VI > to al'ov constant moniuinnv of the
s'_*cJ( iu v>K>:it7  The Levant (ii;s procure)
                              pljtae of rt« pilot tube snail be ev*n Ttth or abort the
                              noczi* «nc-T plane (see Method 2. Figuri -.Mb) durmg
                              samplioc. Tbe Type 6 pilot tnb« assembly shall nave a
                              kaova coaficient, detarcaicad as ouuiaad la Secooa 4 at
                              Method 2.
                                2U.4  Ciffartntla. Prenura  Gauga. TnfUned Baooov
                              etar or equjvmiant der i-1 ttwo), u  jcrib»d  in Section
                              2Jof Method:. One manomtxe/stall be os*d or velocity.
                              faead (ip) readion, aad UM other, tor onflc* diZanofla.
  • Meniioo o. trade na=w or srvwiftc product- do« not"
  Mstltiite endorsement by tic EnTirorcaental Proicc-
                                2.U  FUter Holder. BonalUeaU nUo, with a irtaa
                              trtt •Alter joppon and a allcooe rubber puket. Oibcr
                              matmaLs  of construction' (e^..  nainlen  fieri. TeDon.
                              Viton)  may be ued.  subject u appronl 01' ibe Ad-
                              nioinruor. Tbe bolder design shall proride  > ponUrt
                              .«Bal aolnst Irakace Jvm tbr oot fl'.-iible
                              cotinocLoru between  the  Lmp.necrs.  csne  nutrnals
                              other than :te;, or tuln: fleiible vacuum line*:: connect
                              the filter toidi-r 10 tho conU>-iuer) may be uir»I. >u!i:m
                              to IS'-  a-.provil o:  the Admiuiitrstor. Thf nm  airj
                              second  Itupinccrs shall contain kuoivn  t(u^::t;:ip? o'.
                              wuli-r (Set-lion 1.1.3). t.V thirrt shall ly rmp:>-. an'J the
                              fourth  shjll eonuun a Known  weight  or siLo fr\. or
                              equivalent d>«iccanL A taprn:om<.tc:. earuljic o, :i:e»jur-
 Inf teraperetun to within 1* C (5* 7) shaU bo placed
 at the outlet of the fourth Impinger  for mocturiat
 punxxea.
   Alternatively, any frnera that  cools tbe auap*« ?u
 stream aod allovj meuurement tt the  coodtao l>r:
 (I)  monitonnc the  temperature  and  pressure at rba
 exit a( the condenser and  using Dalian t Uw  ol partkl
 pruaura; or (2) peeing tni sample gas lUmm (hrouiti
 a ured slUcs ft\ (or equlralent  dctiocnnt) trap »'Ub
 exit gases kept below 20* C (i*ol mruunut
 volorae to within 2 percvnt. and  rrtairt "iui|irre;n. u
 •ho'jrn in Figurr i-1.  Other mrtcriag syst'roi rspaUe o!
 maintaining sarnnlirg rates vltbin 10  (utrmt ol  L»>
 kinetic and 01  d»terminine:  sample volume-, to within .'
 percent may V used,  subject to  the  approval  o ihi
 Ai!:::i:Jnram".-r, llifrr-jry. anerolil. or other l»ronei«T
 ettrt''!*1 o! rr.easurinz atmoaphcnc preKnire w wuh.n
 '^ mm Us (C.I :ii. Etc). In many case*, the baromiMnc
 r*vi::r; may be cMoir.M from * nmrby natior.ui WMUDPT
 s:rT.c>- il-t.ou, in u hich cj£e the station value (wtucb a
                                     FEDERAL  REGISTER,  VOL  42, NO. 160—THURS3AY, AUGUST 13,  1977

-------
 4x773
 tiv» absolute baf,yrn«£nc Dre»ur«) sh^ b* rw)uerted and
 an a* li us tm eat  (or  aUvmion  cUlZorences. twtweea the
 v^fcidtr nation arxi sampiicj point snaU tm applied at a
 rue of ounui 2.3 imn Hj «U Uu H«) per iO m UOO MJ
 i-lrroaoo loiivtta* or TIO« fersm £br elevation decrau*.
  •2.1.10  Qua  Dinner   Determination   Equipmoct.
 Ttmperttluja wttior  and proaara irauae, aa described
 in Soeuonj 1.2 and  2.4 o( Method 2, and ccai ajutlymr.
 Ifn^ccbiAT?. aa d*^*cnb-«d in Method 3. Tha iomp*raiuji6
 **naor shall,  preferably. b<* pemiAowntJy attached to
 in» pilot cub* or sampling oruthi in a ibc?d conJigiirauon.
 iiich liiai tr« tip at tha «<*n«r*ruindj fyyoaU tne lauim^
 edz* oi  the prob« ihffeUi anti dcwa not touch any mauu.
 AU*iriaxi7*iy. tb«  vn*or may b« attached  jost  pnof
 lo us* in tb*> n=Jd. Now, bpw»v*r, fflAt t/ ino Lemparaoiro
 sensor is aiiarlied In Lh«  /i»ld, the stnsor muse t» pLssoed
 in an intrrfiTiMH-^frea ammffp.njenc witb rwpect to Lha
 Typ11 S fMtot tub* operunes is« Method 2, i'ignrv 2-7).
 A^ a second aiuriuiDTe.  if a duferencs ol not more Lh&n
 1 percent ui  the average velocity measurement 13 10 b«
 Introduced, the tirn p«r»nirt jrautte ntr&i noc b* otcjijieti
 to ine prot-9 or pitgc cub«.  (This alurnauve la aub
 to tho approval nl vo« Administrator.)
  2.2 SarcpU
     .
2.3.1  Glass Weighing Di5b«.
2,3.2  D^-Dccauw.
2,3.3  AnaiTUcaJ BaUnco. Ta
     .
  2.3.4  Baianc*. To mfasart to within O^S g.
  2.3.S  Bnken.UOsl.
  2.3.6  Hysrom#t«r. To ranftsure tbe relative
 of the laboratory eaTirotmieDt.
  2.3.7  Tcmp^nj-tUrt Gauica, To. m**sur« the
 turo of th« laboratory eovirorunmt,
  3.1   SampllnB- The reagents osed LQ sampliu? are w
 follows;
  3.1.1  Filters.   Olara  fib*r  OJtcrt,  u^.thoat  orraaic
 binder, eihibiaaj at kajt 9y.93 p^rceot eiEciecey (<0.d5
 pcrcoQt p^ncLmtion) on Q.3-micrt3n  dioctyl  phtnalate
 saiote parriclw. Ths filter efflc.-vncy test shall be con-
 cluctwi m accordance with A3T?»I standard  method D
 ?jSG-71. Test  dnta  Irom the supplier's) quality control
 progrusi are 5ufRci?nt for this purpo-w.
  3.1.2. Silica G«l.  Indicating type. (S to 16  rawh, If
 previoiLily uvd, dry at 175" C (350" P) (or 2 boara. Now
 silica  Kel may be used aj receircd.  AlteraatiTcly, ether
 typys uf dftiiccan'S t*»auirQieat or b*i>rl  may b* as*d,
 5uoj*r: to thr  ippruTil of the Administrator.
  3.1.3  Water. V/hen analysis of the material «.a;ht In
 tht* Imuin«er3 is rwiuir-d, dLsuUed  water  shail b« -osed.
 ftau h!ar,fcs pnor ;o ueM us*  to eliminate a high bJaa*
 on i HO; ^niples.
  3.1.4  Crushed I«.
  3.1.5  Stopcock Grca«. Actton*-lMoluble,  hcat-sUbls
 iiti-;,f.i of stopcock gre^e may bo us«i, sub-
jtct to t'.* approral of the .Vd-curustracor.       ,  .
  .1.2   i-aninM KecoTery. Acetone— rea^enl grada,  stored in pciyetiiyiitna  bottled -kjc longer U3an a
 month.
  2.2.3  Glads Fimpla Slor*^e Cootaiaws, Cb«nika!iDy
 rediatant,  borosiJJcata glaaii bodies, (or acytone  w*4b«i,
 500 ..T I or 1000ml. Screw cap I mew shaU father be mbfc>«r-
 btt'LLiA Tadon or sbaU twcoriotr!u.-t«3.iJiAnt to chemical attaci by acatono. CN'ojrtnB'
 raouch t;laa3 bottler hav« b**n  found to. bo le*s protw to
     .
  2.2.4  Petri  Dlsbes. For CLlti  b->tiles  from rn*ial  containers; tnus,
acetone rlin^s bha-1 b* run prior to field usa and only
acotone wi.i iow blank vr.luas (r.
  4.U  PrcUnunary  Determ.initiocj. Select: the  MLtn-
plinj 3it« and the minimum noinbcr of samplirjfr points
according to Method 1 or aa specified by tne Adroj.nLitn»-
tor. Det«rrun« the stact presjar?,  temporatura, and the
raoge o( vetocicy heads using Method 2; U U nvcoanaeaded,
chtat a Ifak-chect of tha pitot lines is** M«thod 2, Sec-
tion  3.1) be ptfrformftd. Deterrrun*)  tha moiirmro cocuaot
usuig AnprotunatioQ .Method  4 or  its alcem&ilves £OJT
thvi purpos* of tnalclnff isoiinauc sampling  rate MtrUn?3.
Dfternun* the stacfc ECU dry molecular weipht, aa d«3-
cnb*d in iiethod 2, Section 3.6: If inte^rat&d Method. 3
sarcplioff Lsos*-
naif minute, ;n order to avoid tlm*t«pLn? errora.
  In some corcuaulaac«,  e.g., batch cycles,  it may  b*
necessary to  sample for  shorter times at  in a traTers*
points and to obtain smaller  pas sample  volornea.  In
tbrae esses,  :hc  Admioistrator's  appro7al  auat  first
be obtained.
  4 1.3  Prep-.arB.tion of Collection  Train. During prep-
aration and  assembly of  the sampling trajn. ke«p  ail
opvoi-nzs where contajninfltion can occur co^trad until
Just prior to assembly or until 5«=:pLjic 's about to L«a;:n.
  Place 100 ml of wattr in e*:h o' the first rwo Lffipingtirs,
leave tbe tflLrd iinpingef  ejnpty, tnd transfer approxi-
mately 200  to  3tA)  g ot preweiyhed  silica pel from  its
comamcr to the fourth impinj»r. MOTS silica  pel  Ey*r  b<
us**d. but raj* shouJd  b*  taktn to eruure  tbar it 12 noc
eutraitiKt and  ferried out f/om  th* impinge? during
sampling. Place the con^Jner  In a clean pl&ce for later
uie in the sample rocov-ry Alt^matiTejy,  the w»i?bc of
lh« silica gel plus Iznpmter may be dtftemiined w rh*>
cearest 0 5 g and recorded.
  U-iina a tweezer or rle^n  d.iposable stirplcal gior«,
place a  lai*!ed (IdentiA^l1  ard  »-*!«h*d  niter in toe
lU;v- hui-Jer.  Be sitre thac fhrr futrr j properly centered
and  the pasi:#t prop*rlj-  puK-wl  so &3 to prevent the
sample pas srrrtm from circurr.r.«itmj th« tiller. Cb-Mfc
the nltpr for teiirn a/f*r assembly .5 completed.
  \> ni*;i iziiLSi Itrers are u^d.  jr^tiJl tbe sJMi'fied DOII.J
using a  Viwn  A  0-nn;  a-o#n r.act temperatures  are
l*"«,thari 2'*j° C <."U/° t')  and in aiteatoa  string £^<^
wU-*n t<*mwr\iUirt>» wiU
b^tit rwujrtftnc CAtJfl or  by x^nti oUicr  met-bod to d^jioL
£Ji« prop-iy tiiffiauce mU> L&e euicJc or dace, tar t
plms point,
  fia? up tho Cruln &a in Flenr* 5-1, aains (If t
ft T«ry Light ctmc of siiicona cpsajw on  ail (rrc-cuid ;
joints, KreaAina only tbe oin^r r>on:oa (*«3.
to Q9yjct th* prob*
f) fJio craan durinc tiio lenii inlet TO the tUtar bolder
(cyclon-s, if apputTtblaJ and puUIng a CiJy abov»). Then COD-
neCG  tho prob« to the train ind l*ak-cbe^li  oi about 23
mm Hg (1 in. HIT.) vftcuam- aJternaUvtly. tho p«b« oiajr
D« leoA -c becked ^iiij the  rt-at of  Lbe saaipUng tnun, Ln.
one s't^p, at ioO mm Hff (15 in. Ho  Tacuum,  U>Aiaff»
rates in ezcess ot -t percent of tho arerine saJUpLuij rau>
or 0.00057 03 J,nnn iQ-C^J  ctm),  wbjctwvpr  LS leas, are
D^aixep table.
  Tho toUoirLnfr. Itatc -check Injtracdoru .'ortbw sa=ipunz
tram  described m APTD~"^76 and APTD-uial  may b«.
help/uJ. Start iba pujnp with bypass voJive lully op-?n
Qjid  coarse idjujt  vatr«  completaJy  closed.  Partullr
opon the aiai-3* adjust vaJvo and slowly clc-w tb« bypiijj
%alvn until t bed «ired va-cuum u reached,. X>o notmversj*
direcDon o( bypjtss ^al%o, this wdl caoM water Co o»»clc
up Into too niter bolder.  I/ tha desired Ttwiuiun  Li «-
cwifrd, either Isat-cb^k ac this bi*hur ^acuun or and
th& leftk cbttic 05 shown b-ciow n.nd stjj-t o^tr.
  Wb«D the lea!rg enLrained biurtwirtl into the Laird
LmpLDger.
  •i.L-4-2  L&ifc-ChocJu During Siraplo Run. Tf. daiiD^
tbe sampling run, a component (e.g., filter niiarcbiy
or Impunger) chdj'.se becomea nec cocclu.5ioa of each Enmplmj* FUJI.  Tb*  itralc-
ch^ck shall rw dona in  accordance  •snth iJie procrdorti
outlined In Srtfion 4.1.4.1, «c*pt that U ?t*aU  b« COQ-
ducte *,iinpl? voluxue aei shown in S<-ct.kmti.:Jo( ibu cm?Lho
-------
i r^quLred by Fljnrs 5-« ot least onr«
           -^i tuna incite eat aod
Tsie olh«r rsadl
iC -v:b « oomoicr&pcis
                                                                                         appropriate fiBOa (M« Clt&Uoa 7 In 5«c'J>aa T) ara
                                                                                                             dtruulacu.
   PLANT
   LOCATION _

   OPERATOR

   DATE _

   P.LIN NO __

   SAMPLE BOX ;jo._

   METEH BOX NO. _
   C FACTOR
                                             AMBIENT TEWPERATURI.

                                             3ABOM£TaiCPR£S5UHE_
                                             PROSE ItNCTH.a(lt)      	

                                            ;NOZZL£ IOUTIFICAT10» WO..	

                                             AVERAGE CALIBRATED N01ZLI OIAJMETER.

                                             PROBE HtArERSETTlNS	

                                             LEAK RATS. a^/mUda)	

                                             PROSE LINER MATERIAL	
   PITOTTU3£COEFFIC!ENT,C,.
                                                   SCHEUAT1C Of 5TACH CTOSS SECTION
                                             STATIC f RESSURE, SUi lt| (Ifc H»(.

                                             FILTER NO	
TRAVESSc POINT
.NUMEtJl
1










-
TOTAL
SAMPLING
TIM£
(SI. min.













AVERAGE
VACUUM"
mm Hg
[iruHgi














STACK
TEWPEfUOfflE
(Ts>
•ci°n










•



\,-aocin
H€AO
(A?s).
im^In.JHjO













pressure
OIFFEKNTIA1.
ACROSS
ORIflCE
tl£TER
mmH2O
(!n. H^OI













1
GASSAkff'U
VOCU.«£
"J (It3)










•
*


GAS 3A»»a TElfitJUTUIS
AT CW GAS «TEB
IMXt
*C (V)



OUTUT
•C («F1



1








A»».








A«9.
A»», • .
FILTEfl HOLDEfl
TEWtAATUSZ.
•ci*n














Ta8>tRATUft£
OP GAS '
LLA\/IW3
CONCOS5B CO
LAST IMPIMCfca,
"CO)














                                                               Figure 5-2. Partlculate Held data.
  When the ata^k b under 3i£^i£:int ne?sti7p
Chft;?bc of unpmaier s^eoil, tazs ca_-e to C'.QSG tiia co*rw
Bd)u5i. v<7* before inj«rti3g tts prob« mto tt^  stack to
prjv*r: watw trotn bactiris uico  th*  2iUr hoLdar. U
         . the pump ^137 b* turr-^1 on •wtUa ths
                 .
  '.Vhon th* pmbfl ts in poalrtoa, bloct oC tho op*nic?3
arour.d  tns prob«  and  [Hinhols  to  pr?veaE unrtpre-
Kr.cariTd dil;iLion of the :as 5Cro.3a. -
  Trava.Tri ;b» Jtackcrosj-jecnoa, u r?q'dirwl by MeUiod
I or as specified by the Admuiiitrswr, being careful not
to b-irnp  tts prob« imiile Lnto the  s'-sct waila irbeti
^mpl^nc ne*r tb« walla or n-ben reconnz or L~oenrg
I'li probs  through  tba  ponha:«i3; this  i^.runuifca th»
Lhan!.*- of ercrstiin?  de^siied ds^enrU..
  Diinog  th* leat run,  mate  periodic  adjii5tTr.er;*-s to
k-cp the '-fimpenuuTB around Uw fllwr hoidec &t th«
pru^er lerel; add mor« Ire  and,  if  nece^sarr,  salt to
maintain a Cinp«ra:ure of l&is ifcan ^0* C '''.•?*" fi at cbc
conderuflr.'3:hc3  fd  outlet.   Also, periodicfclly  ch*ct
t::* levei and rero of the manometer.
  If the pressure drop across to* ,rUti»r  btoomes too b-lzh,
makip.z:  iso^aetic iimpLn?  dutcid;  to oia^arjun. the
tilur r~»y be replaced in :ba rcids', of a  sainpls ran, U
is rp<:nmmeadtt.j> c&u,h*s.
  A ?'.r.(;Jfl iraja sdoJi be iJ5?d  for the eatue .^acip1.* run,
tirept in casej wh?r« slniuJUiQwu sadpUrg u r^oiiLreil
iri two or n»*'" i< rirace d'l^ts or at C-WQ or r~'.r^ dii'ercnt
1"- -.' '»"o \* ,'. VD ihs S3 a a d.ict. or, m  ca^tj Mrncrt ?<|iup-
FI.- .;-f t.l ir- ccTfis:'-a^> i ci^n j« oftrairs In all other
i:MMr,&-i^. t -"»!,. e Q.' LVTQ o.- more tmnj w ii; L'< aubj-'t to
             '
  Nota that wtxen two or mora trains ITS a»4,
anilywa of tb* tront-hail aad  (U appiicftbU)
catcbM iT3n eacb train shali b* per formed, unless idena-
cal noitl« iirw wars as««i OQ ail traina, in vtucb caaa. tls«
tront-baU  catcbea from  tt»  LndiTidoai traina may b«
combined  (aj may the impLnger catcbmland oD»ftnfliy3i3
of Zront-half catch aad one analysis of Lrapinjc/ catch
may be performed. Conjnlt with. tb« Adjrjnisir»tof tor
details concerning the calcuLatioa of results -wtea tro or
nor* trams an xued.
  At th« end of tbe sample niiu turn ofl th? coar« adj^irt
7^1 s-5, remove the probe and nottla L-ora tbe suet,  cum
otl the pomp, record The final (try &u z:«t*r reading, ar.d
conduct a  post-test ItaJc-cbect, aj  ouUined in Se*-fon
4.1.4.3. Also, leak  ;nur., wip* u^  i j*
                                                                                          sC!eoo* creaje, and cap the op«a outlet of tba prob*. Be
                                                                                          careful not to LOM any coodensat* that mlah; b« prea«ic.
                                                                                          Wipeofl the suicoDegreia* trom tie tlur inlet wberf tb»
                                                                                          preb« was fajwned and  cap tt. P.emoTe  the arcbiitc*!
                                                                                          cord  fron ft« last ImpLnger and can ttre Lnipuiger. Lf a
                                                                                          flertbU Llns is  a*?d b a ptur of  iwe^en and'or clesa diaposibl*
                                                                                          furpc*! e'.or« to handle the  nltor. II it is necesaarr to
                                                                                          fold :r.? ^••>r, do so su:b that the panJccuate cate Is
                                                                                          Inside ;ae fold. Carefully tranter to the p*trl  dbh any
                                                                                          pard?u_i:e  matter andior filter Qte~ •winch tda^re 10
                                                                                          the  .flJ:-^r holder  p«Lske:,  by asia^ & dry nylon brUtla
                                                                                          bru*1! ir.d or a_sbarp-ed?sd, blade. Seal the coataiaer.
                                                                                            C^"*-:--- .Vj. f. Takinst cars to ?*e tha;  doit oa the
                                                                                          ouistde o; *.2-»  probe or other ciicrior surtKtas  d>« cot
                                                                                          ?•»! ir.:o :_* ^.ii[.;\  quintlcaurely rtcoT
                                                                                          d.\'.:*.'  o: .- .7  condeij^ite trom tbe pro'krt aaztl«,
                                         FEOSAAL  REGICTER,  VOL. 47,  NO.  160	THUS^AY,  AUOUST  13,  1977

-------
                                               by
417SO
flmna. proh* Uner, and trnn*. h_-yj/ Q£ L^A Ci\i*r bo
washing dee* uocaooncntB wrtfl acet^wi* w?rt
wash ;a  * t^aj» cnntunen. Dlsnliwl w*i*r :nay b«i <
Li3tawt of aactaaa whaa approve*! by tiur
and Jhall" be osod icti^n. s^*cif*wl bjr th«
la thoa cajd. save a WVLU tlant nu£ toilov Ui« Aduun-
tja^tor*! cLLiaetloa* oa loilys*. Parlnnn  Ui«  acatAm
iicafts M follow.
  Carefully irmov« ths prob* ooiil^ aod dean th* indds
•urfaco  by nosing with action*.1  ,'rnni a wa^b bouto and
bru5b;r.(f wiih a  nyloa bru'J- brush.  Brush andl tb«
rvr«-onft  rliiM  shows r.o  vj-iol* p&ruci*i,  s-'tai isba«A»
y.^.j ^ Fr-'-r**Tr- of UM »»<>• *ortaer with acetone.
  linisii ftnti  nosa  the lo^de  parts  of ih&
ftictur with. acaum*  In A sxuila/ way until my
parriclea rrtnain.
  Puii« th# pr4Ht*  Bn*
rnuiiDi the prob* wtiili?
fud » thtu all insid-
luiif. L:
                                             V. rr h
                        fc_^i \>f orm^  cnj\_
                         ritK-U majincr  at  l«wi
                        av« small cre>nf.«,  lUnia each mrtect
 thTM times or more if needed to ramose visiblfl  pardcrt-
 laU.  Mxte d iir:ij r:it3s of tha bnj&a and lilwir holder.
 Corcfnily nns* out til?  ?Iaia C7ciono. siao (J appUf*bi«).
 Aiuj oil ccfltocrt wa^hiiijts And p^raculaca maoer have
 b«n co'lecu'i  in the sampk conuLiccr, tlgbttn th« lid
 on tho iample cofltAJj^f 30  thAt a^econ* wiH not l«Jt
 craf wb^n U la shlppiy jp^ocand maJ^o
 a aotatton o^ iu condiQ*7n. Traniitrf th* siLica gnl trom
 tt« fourth. Impineer to ITJ ori^mai contajjiirr and «*L.
 A funnelnuiy maiM it*asief to peopth»silirft pel without  .
 spdiuig. A rubb«r pouoeciMi rc»y tw used lu an aid in
 rcmo-nng the  silic* ?ei from  tiia  unpinger. It U no*
 nbcou&ry to remove the smivll fl^jruint of dust parUcl«a
 thai may adhere Co the impmrv ^fai*
 a notation of any color or Ciniin the Liquid catch. MfAsure
 th? Urjuid whtrn is Ln th« first thr^ Lmpingpra to v.thia
 •*! ml by using a praduat  REGULATIONS


Rant	
                                                       Date.
                                                       Run Na._
                                                       Filter No..
Amount liquid lost during transport

Acetone  blank volume, mi	

Acetone  wash volume, ml	
Acetone blank concentration, mg/mg (equation 5-4).

Acetone wash blank, mg (equation 5-5)	
CONTAINER
NUMBER
1
2
TOTAL
WEIGHT OF PARTICULATE COLLECTED,
mg
JHNAL WEIGHT


j^>-
-------
                                                           RULES  AND  REGULATIONS
                                                                                                                                                41781
   A!t*rn»tir»l r. ih* 50.— pl« 0147 IW.OTMI dried st 105* C
 riS? >') .'or 2 to ". hunrs. coolrtl to tn« dcxiccalor. aod
 w«t;beil u> A coiuLAUt w^tcbt. luii^ja otbwwiM specified
 by tii« Adaiuistrator. The tester CUT alio opt to ov«o
 rt.-7 t.-i« sample at 105 * C (») • F) for 2 to 3 hoars, vreijb
 th» sara PM. and UM tbi* wwi^ht QJ a fir\*i wet^btk
   Cmtamtr Xo.t. Not* tbeUftlolliq aid uitbtcoaUlamr
 and corinnn on tb> aoalria >n*eC «b«to>r or not ke*fca«a
 occurred durm« transport. U a  noucoable amouat ol
 leakage hu  occurred. uUier Toid the s&mpU or  UM
 raetboiU. subrect Co tb* &pp'mvel of the AdmtaJ5trmtor.
 to correct the ftnal rcsultx Meaeure the liquid in this
 cotitninpr either Tolumetncally  to  ±1 nil or eravi*
 IDftrwallT  to ±0-i I. Transfer the eonteou to a tared
 250-ml  twaktr  nnd ermporau  to  dryneu at ambuot
 Ucpencun  &od pruxure. Dniccau  for C»  hoon and
 weigb to a constant weight. Eeport the resulta to  ttu
 nearest O.I mz.
   Con/nnxr A'o. J. Weigh the ipeot liUca (el (or 3 1 lira (el
 plus Ucpiacer)  to the oew tst U^ K uiin^ a balaoca. This
 stjp OUT be  conducted m  the (Vld.
   "Acttone Skint"  Contn:ntr. Maasun acetone la this
 container  either  Toluznetricallr  or (rrariinetr.caUr-
 Transfer the  aoetco« Co a tared i'JVmJ beakar and erap-
 onu to dryctii at ambient  temperature and preoora.
 DMiecatx for :4 houn and »*cfl to a conuant »eitat-
 Rcport the ruuiu to the narnt O.I mi.
   NOTE.— A.t the option of the tetter, the conUotl of
 Container No. "2, oa well as tb* acetone blank container
'HXST be er«porat4d at Unpenturea nixrier than ambi-
 ent. I/ evaporation \i don* at an eUra>d tempera&w,
 tb* t*rap  the procedure outlined  in
                                                 Sfcnon 4 of lletOod X
                                                   S.3  MeCertng Srsvm. Before Its Initial OM in the field.
                                                 the Betennt synem mail be calibrated  accoroinf to tne
                                                 procedure outuned in J.PT0-OA78. Instead *t the  leak rat*. The leak rate should not aurcd
                                                 0.0ui57 m '/tain lO.CUcta).
                                                   Alter each  field ose. the calibration  of the metering
                                                 rystam shall b* ctwckad by p*rloraunf tore* calibration
                                                 runs  at a singla, Interaitdiau orllice wniiK (based on
                                                 tbe previous Attd ten),  with  the racuum set  at tb*
                                                 maomum  value nacheil dunng tbe  ten teriea. To
                                                 adjust the vacuum, insert a valve betwem tb* wet test
                                                 meter and  the inlet of tae metering system. Calculate
                                                 tbe average value ol tbe calibration factor. Lf tbe calibra-
                                                 tion has changed by more  than 5 percent, recall brat*
                                                 the metar over the fall range of orifice  settings,  as out-
                                                 lined  in APT0-Q57S.
                                                   Alternadre  proeedum. e.^..  oslnr the orifice meter
                                                 coefficients, may  be used, subject to lae  approval of the
                                                 Administrator.
                                                    N'nTE.— lrth»drr m mtUrraiBdini nlaa obtained
                                                  b- shall other b* vmUed, or aucuUiloni 'or
                                                  tb» tnl j*nes shall b* perforated nan* whicnmr m*ur
                                                  coefficient  value (I.e.. before or Unit  pov  u» lower
                                                  valu* o( total Sam pi* voiuma.
                                                    i.« Profe* Heater Calibration. TtM prob*. b*atlni(
                                                  system shall b* calibrated betor*  It* Uuaal  u*» ID tb*
                                                  6»ld according to th* procedure outlined m APTD-OSTa.
                                                  Probes conscrucwd acconiinir to APTD-OMI nod not
                                                  b* calibrated If th* calibrauoa eame la
                                                         .
                                                        Temperature  Gau**a.  CM th*  prae*dun  la
                                                  Soettoo 4-; of Melboti 2 to cmlibnu In-suick t*mp*ra:un
                                                  gauges. Dial thermometers, sucn as ar* U9*d lor ta* dry
                                                  tvu  m-nl- L««*a«« alter tb» pomp <»1U
                                                  rwult la  1««  votum* btinx rrronlrd lhaa b actually
                                                  sacpUd.  Tn» follovtm  iiracAlurr  U lusx**ud  !»••
                                                  Frpn-e 5— t): CloM «\r main run on U» ci«t*r bai.
                                                  In*rt » on*-tool*  ruobrr  *topo*r with rubber tubtiut
                                                  attached Into  th* oriae* maauit pip*. Dl«eo 11 u> Li cm
                                                  (5 to 7 In.) nur  ooltuiu br bk>"ln< tola lb* rnbb*
                                                  tnbUK. Placb.  ad ID* aitxnf ud oonrn to* m«aaai«Mr
                                                  for oa« minutA. A Iocs of pnsson on Ui« raftaomtur
                                                            leak In  tb» mvor bou t««n. L( prorac. mua

                                                                                  a mweorr baroor
                                                    5.7  Bkromtttr. Calibnu
                                                  cur.

                                                  «. Caleaialiant

                                                    Ctiry oat rmlealktiooi. nUktaiai  »t laut   aa&l ralnibtaoc. Otb«r forcxi ot uw
                                                  rqiutioaa may b« u»d M
                                                  raulta.
                       RUSSER
                       TUBING
                                       RUBBER
                                       STOPPER
                                                       ORIFICE
                               BY-PASS VALVE
                                                                                                               VACUUM
                                                                                                                GAUGE
«ha** ^J
CLOSED x 	 XY*
Oi nil* IMTfi TTiafM* rrV_ -*-
UHTJLMANOMETEfl 1^
READS S TO 7 INCHES L-" '^-
WATER COLUMN - ORIFICE
MANOMETER
^

•;
'.


^VENT
M *

} — ,
[DRY TEST METER]
\
a A
-

•— M
((
/ JS
                                                                                                                        MAIN VALVE
                                                                                                                           CLOSED

                                                                                                                   •AIR-TIGHT
                                                                                                                      PUMP
                                                       Figure 5-4.  Leak check of meter box.
a, t
A,
/
L,
Lt



L,
P.
       Noffitnclatur*
         -CroiVMCtior.si we»of noiiK m1 (til.
         ~Waur npor in ih« cu s:ream, pruportioa
          by 7olaau.
         MAc*u>n* blaalc ratdue concentrstioas, mz/f.
         *>Codcentratioa of purticulau .mitter in itacjc
          gss.  dry basis, corrected to 3taada;d condi-
          tions. i/dsom (x,'dscf).
         »Perc>nt of Lsokjflttic samplln;.
          pret«st leak check of (or a leak chtek loUow-
          ln(t a component ch&nze;  equal  to C.0005T
          jn'/siin (0.02 eta) or 4 percent at ;h* average
          sxnplinj rate, whichever is less,
         -Indlndoul leataj- rate observed during the
          leak check conducted  prior  to  the r'i»"
          component  change  (1-1,  2,  3 ....»),
          mVmia (cfm),
         »Leakue rate observed during ths post-test
          leak check, m'/min (c(m).
         —Total amount of paniculate ms".»r collected,
          m?.
         —Mo'.eculir  weieht  of water,  13.0 (r/s-mol*
          (13.0 lt>,1D-mol«>.
         "Miss of residue of acetone after enpontioo,
          m».
         •* Barometric prNkurt  at  tin sampling jj'.e.
          mm lig (in. Eg).
         <• Absolute staciceasprasure, mm Hg (In. H»>:
         «3unIl^.-ti  abso;uta pr« meter, corrected to standard  conditions,
        dscm (dscf).
"•(•«)— Volume of water Taper In tb* gas nmpla,
        corrected to standard conditions, scm (scf).
    V. -Stack ras velocity, calculated by .\Utbod  S,
        Equation  2-9,  using data  obtained  trom
        Method i, m.'sae (ft/sec).
    Jf".- Weight of residue In acetone wash. EC.
     y-Dry ru meter calibratioe factor.
   aH- Average pressure differential across the ortflc*
        meter (see Furunfr-l), am HiO  (in. UrO).
    «.«De'Jsity of acetoaa,  mtvml  (see  label oa
        bottle).
    ,. -Density  ot  n'M,  O.XV1 1'ml  (O.OC2XH
        Ib/mi).
     »=» Total sampling tim», min.
      ' >>—SarapUnic tin* Interval, from th* beginning
          of a run until tbe first component eoacje,
          mifi
       »,-SvmpUng time  Interral. b«tw««a two suc-
          cessive component changea, be^Lrxinc  with
          th» interval between  th*  Crn aad Mumd
          change*, min.
      •,-Samplint time Interval, from tb* final  (i")
          component  eb^nire until  the  er.d  of  the
          saoiplinc run. min.
     13.6 • Sp*ciic gravity of marcury.
      60—Sec/min.
      100—Conrcnion to percent.
      Average dry gas Deter temperature and irenji
  _   pressure drop. Se* dat* sheet (Fifure >:i.
  6J  Dry Ga» Volume.  Correct the sample roltun*
me«LSure
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                               ,  RULES  AND  REGULATIONS
  nil — OJ&ifl *Tr/mm H* 'or io«*rtfl tmftj
    — 17.64 * KyLn. Hf Id g'r'ClfT-^ OXLltJ
               ob««rr«(i durng UT a/ U>« mAa
Wk. --M^""t (La., Ci* posl-i*^ i«*)c cb*ci or U&k.
*">TM1 rk"Tftfl PTMX to CQEQpOO£Jlt Ci*CLje*) IIT**"! ^ Z-«_ LI
.L, o* IM Axcvwij. X*a, EqufcOcn VI must t>» medial*! u
fallows;
  (»)  Ca«* L No component  chJunuM tnmJ« dnrtntf
tfcmplinj ran. In thu caws, repLaca V » m Equation i-i
vita tbo «iprtssion;

                V-- (£,-£,.)»]

  fb) C&»* IT. On* or mcr» aomparuml rhansc* m&Je
dnrim? the snnplmy ran- In taia caw, rfpiaca V. m
                                                          .— la
                                                          * CTTO cumaulafioria of U» mouuire -t>ni*Dt o/
                                                        3-40 3-aall CM rn*4a, ooe Lrom Ui« unuuaeKf fcasj
                                                       iaccra v-3t, and a aooor.d tram tJ3» monoaDQoo
                                                                         w IOW-T 
                                                           De r: outxij^ cont*ai bts*Kl UDKJO uamDpuo
                                                            rcrv*l)tx7n,3 LB Kisan tn d* Not* n^ ^*i 4. For U3« pfirpava of U3ii miUioO, Ui*
                                                                        troai F^nirw
the
  b.6
                                                              tmnp^racuni WOJOT u * 1* C
                                                                       Coaouierwioa.
jid subtfiHate ouly for tiioae
rnicb. aictted X«.

 8.1 Talma* o/ v&Ur taoor.
                                    rat« [I* or
                                                      6.7  J.c«ton« ^'
                                                                     rr.-c.v.,.,.
                                                                                          Equitlao
                                                      8J  Total  Pirtcmljit* Wfi^it. D«urnuc<  ui»  K
                                                     p&rclniiata cMds from Ui« jiua of Li« wtfi^a
                                                     (rom coniaijifin 1 and ^ l«a tao acnuaiw biAni ^AI
                                                     fr-3 V. NOTE. — H*^ar to fl«ct;on 4-1-5 La aasux LB
                                                     oi rajuJcs Ln^olTinfi: t-wo cr more dJu/ tswsiti
                                                     or mare sarDpil-^c crwnj.
                                                    ,  AS  P»mcnJ*u COTKeutnttan.
                                                                 (0.001 g/my)
                                                       6.10  CcmTeruoo jf
 irher«:
  Jii—0.001333 roVmi Sa/ metric tmtts
     —0.04TOT rtVmJ lor Snthai nmti.
               CoDt-ent-,
                                                                                           Ua]tlpi7 by
                                                     K,'tt»
                                                                                           li-U
                                                                                            i20
                                                                                           Oi 31
                      i« (aulj ~T ' w (»u
                                       Equation 5-

                              ioor.fg,V|.4-rrjr..) (pb.,4
                                                       i.U  ImtLneHo Vnrl»aon.
                                                       S.1LJ  CsJcolailoo F.-Mm Ban Bttta.
   A',-0.«SM54 mm Ha-m1,'ml-*K tor nstric anJts.
     -O.OKSiB in. Hs—(t'ftnl-'H.for Eogliail aalu.
                                       '
                       T.V. ^
                                                      8. YoQafD, H. F. A Sorcer o/ ComnwrcIiCy A
                                                              tjvnrifi yof tb« ilnaJUT^m^Ot 0( Lx)W.
                                                              nM. U.S. Eavu-oomeauJ Prousctiofl A
                                                              Mqaaar^nieat  Bruich.
                                                    Park, N.C. Nofaaw**1,  1378 (oapubliihed
                                                      U. Aunoal Book of A5TM aticiarti. Pan2i-
                                                    y\if\i; Coai Md Coie; Atzc»rpli4no Aoolyat
                                                    Societ7  lor
                                                    l»7i. pp. 617-52Z

                                                    METHOD  6—DZTnuris.iriov  or  Srxrcx  DI
                                                           Zaiaaio.vs  FROM Stir.o.\ABT
                                       Equation 5-8  1- Prmciplt c&l Appli
   JTj — t Vf> tor in«tri« units
     — 
 miteladgswou. Otienrixr, reject tti< result! ind rep*»i
 Ui« test.
   1  Addendum to Spccilralions (or IncicenUor Testing
    Federal Faciliuu. PH3, NCAPC. Dtc. 4. 1967.
   2. M«r;ia.  RutMrt il  CouiroctioTi  Detalh oV I»-
                ,
    7. Shigthan, R. T. Adjmtejsnu In th» EPA JJ
  rn'pb for  Dlflertnt Pitot  Tnb« Co«ffici«na  ud
  Molecalor   Weights.  Buck  BampUnf  N«w
  Ocu)b«r, 1J7-1.
 Protection Aseacy.  P^seft/ih  Triangle Park,  N.C.
 APTD-OM1.  April, 1071.
   3. Rcon, Jeroa:*  J.  Mais Unine*.  Calibration, and
 Operation o( Lsoiinetic Source Sampling Equipment.
 EnTironnwDtal Protection  Agency. Eaaearch Tn&ogU
 Park. N.C.APTD-OJ7?. Marcli. 19T2.
   •t  Smith, '»'. 8..  R.  T. Snifehira,  and V. 7. Todd.
 A Method of Inwrprctiast Stack Sampling Dau.  Pap«r
 Pwaented at th»  43d  xnVin»i Me*urrg of the An Pailu.
 tlon Control Ajsouiition,  St. Louii, Mo. Jon«  14-19,

   4.'3miUi. VF. 8., « al. Stack Oaa Sampling InprOTed
 and SLmplirtrri Witii  Neir Ecraipmant. APCA  "

   «. S oeciJlcaacci  for laeineraijr Testint  at
   .. ^.rrToaa KCAPC. 19o:.
                                                      1.1  Prlncipl*. A pu s»mpU b  eitTictnl  Irom  t±m
                                                    sampling  point Ln  co« nact.  Tha suUunc »cld mut
                                                    Uncludxcg  sulfT2J  sioilde) &nd the suirar dioijdo  in
                                                    Mparai«'
                                                    12.13X10"'  lb/(t'). Althoogb  no upper Ucit ttaj b«*n
                                                    established, tests  baTO sboirn that coo»acr»uoca BJ
                                                    higb aj SO.000 r"t/7"' of 60> can be collected  efflclenUT
                                                    In rwi nudee: 'jofiontn, ea^h concaining li  milliiittn
                                                    o( 3 p*rcent" hydrogen p^rotde, at  a r»> of 1.0 Ipn for
                                                    30 minowa- Baaed on iboorcdcil calculaiioaa,  th« upp^r
                                                    enoc'ocmlon linut in i 20-Uui Simple U about B,3'er-5ombu
                                                    eiuoos,  and  6narid«.  The cauou and  3aond«e a/»
                                                    removed by ;la«i wool Sit ITS aod an i«opror«Jol bnbb.w,
                                                     und hro-e'do not idect the 5Oi anair3>»- ^ben aajapl«
                                                     sue bong Uien doc: a Bis strrtra with high  concentr*-
                                                     tionj erf very fcna meiallie  himea liuci as tn inlets  to
                                                     eomrcl d.Tlcra!. a hi?h--£lclfac7 glaa £t«r filter mujt
                                                     be ts-d ia  pia«*-o( tb« slia wool plug (I.e.,  tn» ocu la
                                                     theprob-i to renm»e the cation iswriennts.
                                                       Prw iP-^nocia iawrtena by reacting  witb SOi to .orm
                                                     particulau mliu and by iracti^g *tti tbe tna,-cator;
                                                     it (re* aiimoaU b present (tbis can in ileumin*a t>r
                                                     tcwwlwlse o( th« proocn ind nuttcin?  »hiu parJcul»«
                                                     matter ta tSa prob« and Ljopropajiol babbte), aAtero*-
                                                     Cre methoclJ. rab)e« to tbe approval o( tSa Adm-nittr»-
                                                     Va-,  U.S.  EoriroE7r.tr.ial  Protection  A£eiic7,  art
                                                     nqolred.
                FHDEIIA1  BEOISTEK,  VOL.  42, NO.  160—7HU8SDAY,  AUGUST  I!,  1977

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