United States          Office of Water (4303)          EPA-821-R-97-018
             Environmental Protection     Off ice of Air and Radiation   .     October 1997
             Agency             Office of Air Quality Planning and
                              Standards (RTF)



vxERA,    The Pulp, Paper, and Paperboard


             Point Source Category
                           Part 430; Final Rule

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This copy of the Pulp and Paper Industry "Cluster Rules" is
being provided as a service to the public before Federal
Register Publication.  It is subject to editing and
reformatting to conform to Federal Register requirements.
The only official version of this document will be that
published in the Federal Register.

For the reasons set out in the preamble, title 40, chapter I

of the Code of Federal Regulations is amended as follows:


     1.  Part 430 is revised to read as follows:

PART 430-THE PULP, PAPER, AND PAPERBOARD POINT SOURCE
CATEGORY

General Provisions

Sec.
430.00    Applicability.
430.01    General definitions.
430.02    Monitoring requirements.
430.03    Best management practices (BMPs)plans for spent
pulping liquor, soap, and turpentine management, spill
prevention, and control.

Subpart A-Dissolving Kraft Subcategory

Sec.
430.10    Applicability; description of the dissolving kraft
          subcategory.
430.11    Specialized definitions.
430.12    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          'of best practicable control technology currently
          available (BPT).
430.13.   Effluent limitations guidelines representing the
          degree of effluent reduction attainable by the
          best conventional pollutant control technology
          (BCT) .
430.14    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable (BAT).
430.15    New source performance standards (NSPS).
430.16    Pretreatment standards for existing sources
          (PSES).
430.17    Pretreatment standards for new sources (PSNS).


                             785

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Subpart B-Bleached Papergrade Kraft and Soda Subcategory

Sec.
430.20    Applicability; description of the bleached
          papergrade kraft and soda subcategory.
430.21    Specialized definitions.
430.22    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).
430.23    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology (BCT).
430.24    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable (BAT).
430.25    New source performance standards (NSPS).
430.26    Pretreatment standards for existing sources
          (PSES).
430.27    Pretreatment standards for new sources (PSNS).
430.28    Best management practices (BMPs).

Subpart: C-Unbleached Kraft Subcategory

Sec.
430.30    Applicability; description of the unbleached kraft
          subcategory.
430.31    Specialized definitions.
430.32    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).
430.33    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology (BCT).
430.34    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable (BAT).
430.35    New source performance standards (NSPS).
430.36    Pretreatment standards for existing (PSES).
430.37    Pretreatment standards for new sources (PSNS).
Subpart D-Dissolving Sulfite Subcategory
Sec.
430.40
Applicability; description of the dissolving
sulfite subcategory.
                             786

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 430.41     Specialized  definitions.
 430.42     Effluent  limitations  representing  the  degree  of
           effluent  reduction attainable by the application
           of best practicable control technology currently
           available (BPT).
 430.43     Effluent  limitations  representing  the  degree  of
           effluent  reduction attainable by the best
           conventional pollutant control technology  (BCT).
 430.44     Effluent  limitations  representing  the  degree  of
           effluent  reduction attainable by the application
           of best available technology economically
           achievable  (BAT).
 430.45     New source performance standards  (NSPS).
 430.46     Pretreatment standards for existing sources
           (PSES).
 430.47     Pretreatment standards for new sources  (PSNS).


 Subpart E-Papergrade Sulfite Subcategory

 Sec.
 430.50    Applicability; description of the papergrade
           sulfite subcategory.
 430.51     Specialized definitions.
 430.52    Effluent  limitations  representing the degree  of
          effluent  reduction attainable by the application
          of best practicable control technology currently
          available  (BPT).
 430.53    Effluent  limitations  representing the degree  of
          effluent  reduction attainable by the best
          conventional pollutant control technology  (BCT).
 430'. 54    Effluent  limitations  representing the degree  of
          effluent reduction attainable by the application
          of best available technology economically
          achievable (BAT).
 430.55    New source performance standards (NSPS).
 430.56    Pretreatment standards for existing sources
           (PSES).
 430.57    Pretreatment standards for new sources  (PSNS).
 430'. 58    Best management practices (BMPs) .

 Subpart P-Semi-Chemical Subcategory

 Sec.
430.60    Applicability;  description of the semi-chemical
          subcategory.
430.61    Specialized definitions.
430.62    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).


                             787

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430.63    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology (BCT).
430.64    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable  (BAT) .
430.65    New source performance standards (NSPS).
430.66    Pretreatment standards for existing sources
          (PSES).
430.67    Pretreatment standards for new sources (PSNS).
Subpart G-Mechanical Pulp Subcategory

Sec.
430.70    Applicability; description of the mechanical pulp
          subcategory.
430.71    Specialized definitions.
430.72    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available  (BPT).
430.73    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology  (BCT).
430.74    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable  (BAT).
430.75    New source performance standards  (NSPS).
430.76    Pretreatment standards for existing sources
           (PSES).
430.77    Pretreatment standards for new sources  (PSNS).
Subpart H-Non-Wood Chemical Pulp Subcategory

Sec.
430.80    Applicability; description of the non-wood
          chemical pulp subcategory.
430.81    Specialized definitions.
430.82    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available  (BPT).
430.83    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology  (BCT).
430.84    Effluent limitations representing the degree of
          effluent reduction attainable by the application


                             788

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          of best available technology economically
          achievable  (BAT) .
430.85    New source performance standards  (NSPS).
430.86    Pretreatment  standards for existing sources
           (PSES).
430.87    Pretreatment  standards for new sources  (PSNS).
Subpart I-Secondary Fiber Deink Subcategory

Sec.
430.90    Applicability; description of the secondary fiber
          deink subcategory.
430.91    Specialized definitions.
430.92    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available  (BPT).
430.93    Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology  (BCT).
430.94    Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable  (BAT).
430.95  '  New source performance standards (NSPS).
430.96    Pretreatment standards for existing sources
          (PSES).
430.97    Pretreatment standards for new sources  (PSNS).


Subpart J-Secondary Fiber Non-Deink Subcategory

Sec.
430.100   Applicability; description of the secondary fiber
          non-deink subcategory.
430.101   Specialized definitions.
430.102   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).
430.103   Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology  (BCT).
430.104   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically  -
          achievable  (BAT) .
430.105   New source performance standards (NSPS).
430.106   Pretreatment standards for existing sources
          (PSES).


                             789

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430.107   Pretreatment standard's for new sources  (PSNS).


Subpart K-Fine and Lightweight Papers from Purchased Pulp
Subcategory

Sec.
430.110   Applicability; description of the fine and
          lightweight papers from purchased pulp
          subcategory.
430.111   Specialized definitions.
430.112   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).
430.113   Effluent limitations representing the degree of
          e'ffluent reduction attainable by the best
          conventional pollutant control technology (BCT).
430.114   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable  (BAT).
430.115   New source performance standards (NSPS).
430.116   Pretreatment standards for existing sources
          (PSES).
430.117   Pretreatment standards for new sources  (PSNS).
Subpart L-Tissue, Filter, Non-Woven, and Paperboard from
Purchased Pulp Subcategory

Sec.
430.120   Applicability; description of the tissue, filter,
          non-woven, and paperboard from purchased pulp
          subcategory.
430.121   Specialized definitions.
430.122   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best practicable control technology currently
          available (BPT).
430.123   Effluent limitations representing the degree of
          effluent reduction attainable by the best
          conventional pollutant control technology (BCT).
430.124   Effluent limitations representing the degree of
          effluent reduction attainable by the application
          of best available technology economically
          achievable (BAT).
430.125   New source performance standards (NSPS).
430.126   Pretreatment standards for existing sources
          (PSES).
430.127   Pretreatment standards for new sources  (PSNS).

                             790

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APPENDIX A to  Part 430— Methods  1650  and Method 1653



Authority:  Sections 301,  304,  306,  307,  308,  402,  and 501



of the Clean Water Act, as amended,  (33 U.S.C.  1311, 1314,



1316, 1317, 1318,  1342, and  1361),  and Section 112 of the



Clean Air Act, as amended  (42 U.S.C. 7412).



General Provisions




§430.00   Applicability.




      (a)  This part applies to  any pulp, paper,  or



paperboard mill that discharges or may discharge process



wastewater .pollutants to the waters  of the United States, or



that introduces or may introduce process wastewater



pollutants into a publicly owned treatment works.




      (b)  The following table presents the subcategorization



scheme codified in this Part,  with references to former



subpart designations contained in the 1997 edition of  40 CFR



parts 425 through 699:
                             791

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§430.01  General definitions.
     In addition to the definitions set forth in 40 CFR part
401 and 40 CFR 403.3, the following definitions apply to
this part:
     (a)  Adsorbable organic halides (AOX).   A bulk
parameter that measures the total mass of chlorinated
organic matter in water and wastewater.
     (b)  Annual average.  The mean concentration, mass
loading or production-normalized mass loading of a pollutant
over a period of 365 consecutive days  (or such other period
of time determined by the permitting authority to be
sufficiently long to encompass expected variability of the
concentration, mass loading, or production-normalized mass
loading at the relevant point of measurement).
     (c)  Bleach,plant.  All process equipment used for
bleaching beginning with the first application of bleaching
agents  (e.g., chlorine, chlorine dioxide, ozone, sodium or
calcium hypochlorite, or peroxide), each subsequent
extraction stage, and each subsequent  stage where bleaching
agents are applied to the pulp.  For mills in Subpart E of
this part producing specialty grades of pulp, the bleach
plant includes process equipment used  for the hydrolysis or
extraction stages prior to the first application of   (
bleaching agents.  Process equipment used for oxygen
delignification  prior  to the application of bleaching agents
is not part of the bleach plant.

                             794

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      (d)  Bleach plant effluent.  The total discharge of



process wastewaters from the bleach plant from each physical



bleach line operated at the mill, comprising separate acid



and alkaline filtrates or the combination thereof.



      (e)  Chemical oxygen demand  (COD).  A bulk parameter



that measures the oxygen-consuming capacity of organic and



inorganic matter present in water or wastewater.  It is



expressed as the amount of oxygen consumed from a chemical



oxidant in a specific test.



      (f)  Elemental chlorine-free (ECF).   Any process for



bleaching pulps in the absence of elemental chlorine and



hypochlorite that uses exclusively chlorine dioxide as the



only chlorine-containing bleaching agent.



      (g)  End of the pipe.  The point at which final mill



effluent is discharged to waters of the United States or



introduced to a POTW.



      (h)  Fiber line.   A series of operations employed to



convert wood or other fibrous raw material into pulp.  If



the final product is bleached pulp,  the fiber line



encompasses pulping, de-knotting, brownstock washing, pulp



screening, centrifugal cleaning, and multiple bleaching and



washing stages.



      (i)  Minimum level(ML).   The level at which the



analytical system gives recognizable signals and an



acceptable calibration point.   The following minimum levels



apply to pollutants in this  part.





                            795

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Pollutant
2,3,7,8 -TCDD
2,3,7,8-TCDF
Trichlorosyringol
3,4,5 -Trichlorocatechol
3,4, 6 -Trichlorocatechol
3,4,5 -Trichloroguaiacol
3,4, 6 -Trichloroguaiacol
4,5, 6-Trichloroguaiacol
2,4,5 -Trichlorophenol
2,4, 6 -Trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4, 6-Tetrachlorophenol
Pentachlorophenol
AOX
Method
1613
1613
1653
1653
1653
1653
1653
1653
1653
1653
1653
1653
1653
1653
1650
Minimum level
10 pg/La
10 pg/La
2.5 ug/Lb
5.0 ug/Lb
5.0 ug/Lb
2.5 ug/Lb
2.5 ug/Lb
2.5 ug/Lb
2.5 ug/Lb
2.5 ug/Lb
5.0 ug/Lb
5 . 0 ug/Lb
2.5 ug/Lb
5.0 ug/Lb
20 ug/Lb
" picograms per liter.
micrograms per liter.
      (j)  New source.  (1)  Notwithstanding the criteria



codified at 40 CFR 122.29(b)(1), a source subject to subpart



B or E of this part is a  "new source" if it meets the



definition of "new source" at 40 CFR 122.2 and



          (i)  It is constructed at a site at which no other



source is located; or



          (ii)  It totally replaces the process or



production equipment that causes the discharge of pollutants



at an existing source, including the total replacement of a
                             796

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fiber line that causes the discharge of pollutants at an



existing source, except as provided in paragraph  (j)(2) of



this section; or



           (iii)  Its processes are substantially independent



of an existing source at the same site.  In determining



whether these processes are substantially independent, the



Director shall consider such factors as the extent to which



the new facility is integrated with the existing plant; and



the extent to which the new facility is engaged in the same



general type of activity as the existing source.



           (2)  The following are examples of changes made by



mills' subject to Subparts B or E of this part that alone do



not cause an existing mill to become a "new source":



           (i) Upgrades of existing pulping operations;



           (ii) Upgrades or replacement of pulp screening and



washing operations;



           (iii) Installation of extended cooking and/or



oxygen delignification systems or other post-digester, pre-



bleaching delignification systems;



           (iv) Bleach plant modifications including changes



in methods or amounts of chemical applications, new chemical



applications, installation of new bleaching towers to



facilitate replacement of sodium or calcium hypochlorite,



and installation of new pulp washing systems; or



           (v)  Total replacement of process or production



equipment that causes the discharge of pollutants at an





                             797

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existing source .(including a replacement fiber line) , but



only if such replacement is performed for the purpose of



achieving limitations that have been included in the



discharger's NPDES permit pursuant to § 430.24(b).



      (k)  Non-continuous discharger.  (1)  Except as



provided in paragraph (k)(2) of this section, a



non-continuous discharger is a mill which is prohibited by



the NPDES authority from discharging  pollutants during



specific periods of time for reasons other than treatment



plant upset control, such periods being at least 24 hours in



duration.  A mill shall not be deemed a non-continuous



discharger unless its permit, in addition to setting forth



the prohibition described above, requires compliance with



the effluent limitations established for non-continuous



dischargers and also requires compliance with maximum day



and average of 30 consecutive days effluent limitations.



Such maximum day and average of 30 consecutive days effluent



limitations for non-continuous dischargers shall be



established by the NPDES authority in the form of



concentrations which reflect wastewater treatment levels



that are representative of the application of the best



practicable control technology currently available, the best



conventional pollutant control technology,  or new source



performance standards in lieu of the maximum day and average



of 30 consecutive days effluent limitations for conventional



pollutants set forth in each subpart.





                             798

-------
           (2)  A mill  is  a non-continuous discharger  for the



purposes  of  determining applicable effluent  limitations



under Subparts B or E  of  this part  (other than conventional



limits for existing sources) if, for reasons other  than



treatment plant  upset  control  (e.g., protecting receiving



water quality),  the mill  is prohibited by the NPDES



authority from discharging pollutants during specific



periods of time  or if  it  is required to release its



discharge on a variable flow or pollutant loading rate



basis.



      (1)   POTW.   Publicly owned treatment works as defined



at 40  CFR 403.3(o).



      (m)   Process wastewater.  For Subparts B and E only, '



process wastewater is  any water that, during manufacturing



or processing, comes into direct contact with or results



from the  production or use of any raw material, intermediate



product,  finished product, byproduct, or waste product.   For



purposes  of  Subparts B and E of this part,  process



wastewater includes boiler blowdown; wastewaters from water



treatment  and other utility operations; blowdowns from high



rate  (e.g.,  greater than  98 percent)  recycled non-contact



cooling water systems to the extent they are mixed and co-



treated with other process wastewaters; wastewater,



including  leachates,  from landfills owned by pulp and paper



mills subject to Subparts B or E of this part if the



wastewater is commingled with wastewater from the mill's





                             799

-------
manufacturing or processing facility; and storm waters from



the immediate process areas to the extent they are mixed and



co-treated with other process wastewaters.   For purposes of



this part, contaminated groundwaters from on-site or off-



site groundwater remediation projects are not process



wastewater.



     (n)  Production.   (1)  For all limitations and



standards specified in this part except those pertaining to



AOX and chloroform:  Production shall be defined as the



annual off-the-machine production  (including off-the-machine



coating where applicable) divided by the number of operating



days during that year.  Paper and paperboard production



shall be measured at the off-the-machine moisture content,



except for Subpart C of this part  (as it pertains to pulp



and paperboard production at unbleached kraft mills



including linerboard or bag paper and other mixed products,



and to pulp and paperboard production using the unbleached



kraft neutral sulfite semi-chemical  (cross recovery)



process), and Subparts F and J of this part (as they pertain



to paperboard production from wastepaper from noncorrugating



medium furnish or from corrugating medium furnish) where



paper and paperboard production shall be measured in air-



dry-tons  (10% moisture content).  Market pulp shall be



measured in air-dry tons  (10% moisture).  Production shall



be determined for each mill based upon past production



practices, present trends, or committed growth.





                             800

-------
           (2)  For AOX and chloroform limitations and



standards specified in Subparts B and E of this part:



Production shall be defined as the annual unbleached pulp



production entering the first stage of the bleach plant



divided by the number of operating days during that year.



Unbleached pulp production shall be measured in air-dried-



metric-tons  (10% moisture) of brownstock pulp entering the



bleach plant at the stage during which chlorine or chlorine-



containing compounds are first applied to the pulp.  In the



case of bleach plants that use totally chlorine free



bleaching processes, unbleached pulp production shall be



measured in air-dried-metric tons (10% moisture)  of



brownstock pulp entering the first stage of the bleach plant



from which wastewater is discharged.  Production shall be



determined for each mill based upon past production



practices, present trends, or committed growth.



     (o)  TCDD.  2,3,7,8-tetrachlorodibenzo-p-dioxin.



     (p)  TCDF.  2,3,7,8-tetrachlorodibenzo-p-furan.



     (q)  Totally chlorine-free (TCP)  bleaching.   Pulp



bleaching operations that are performed without the use of



chlorine, sodium hypochlorite, calcium hypochlorite,



chlorine dioxide,  chlorine monoxide, or any other



chlorine-containing compound.



     (r)  Wet Bar-king.  Wet barking operations shall be



defined to include hydraulic barking operations and wet drum



barking operations which are those drum barking operations





                             801

-------
that use substantial quantities of water in either water



sprays in the barking drums or in a partial submersion of



the drums in a "tub" of water.



§ 430.02  Monitoring requirements.




     This section establishes minimum monitoring frequencies



for certain pollutants.  Where no monitoring frequency is



specified in this section or where the duration of the



minimum monitoring frequency has expired under paragraphs



(b)- (e) of this section, the permit writer or pretreatment



control authority shall determine the appropriate monitoring



frequency in accordance with 40 CFR 122.44 (i) or 40 CFR Part



403, as applicable.



     (a)  BAT, NSPS, PSES, and PSNS-monitoring frequency for



chlorinated organic pollutants.  The following monitoring



frequencies apply to discharges subject to Subpart B or



Subpart E of this part:
                             802

-------
CAS
number
1198556
2539175
2539266
2668248
32139723
56961207
57057837
58902
60712449
87865
88062
95954
1746016
51207319
67663
59473040
Pollutant
Tetrachlorocatechol
Tetrachloroguaiacol
Trichlorosyringol
4 , 5 , 6-trichloroguaiacol
3 , 4 , 6-trichlorocatechol
3 , 4 , 5 - tri chlorocatechol
3 , 4 , 5 - trichloroguaiacol
2,3,4,6 - tetrachlorophenol
3 ,4, 6-trichloroguaiacol
Pentachlorophenol a
2,4, 6-trichlorophenol <*
2,4; 5 - trichlorophenol
2,3,7,8-TCDD
2,3,7,8-TCDF
chloroform e
AOX f
Minimum Monitoring
Frequency
non-TCF a
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
weekly
daily
TCP b
C
c
C
c
c
c
c
c
c
c
c
c
c
c
c
none
specified
non-TCF: Pertains to any fiber line that does not use exclusively
TCF bleaching processes.
TCF: Pertains to any fiber line that uses exclusively TCF
bleaching processes, as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3) and certified under 40 CFR
122.22 or, for indirect dischargers, as reported to the
pretreatment control authority under 40 CFR 403.12(b),(d), or (e).
This regulation does not specify a limit for this pollutant for
TCF bleaching processes.
Monitoring frequency does not apply to this compound when used as
a biocide.  The permitting or pretreatment control authority must
determine the appropriate monitoring frequency for this compound,
when used as a biocide, under 40 CFR 122.44(i) or 40 CFR Part 403,
as applicable.
                             803

-------
CAS number
1198556
2539175
2539266
2668248
32139723
56961207
57057837
58902
60712449
87865
88062
95954
1746016
51207319
67663
Pollutant
Tetrachlorocatechol
Tetrachloroguiacol
Trichlorosyringol
4,5, 6-trichloroguaiacol
3,4, 6-trichlorocatechol
3,4, 5-trichlorocatechol
3,4,5 - trichloroguaiacol
2,3,4, 6 - tetrachlorophenol
3,4, 6-trichloroguaiacol
Pentachlorophenol e
2,4, 6 - trichlorophenol e
2,4, 5 -trichlorophenol e
2,3,7,8-TCDD
2,3,7,8-TCDF
Chloroform
Minimum Monitoring
Frequency
non-ECFa
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
weekly
Advanced
ECF b'f
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
monthly
TCF c
d
d
d
d
d
d
d
d
d
d
d
d
d
d
d
non-ECF: Pertains to any fiber line that does not use exclusively
ECF or TCF bleaching processes.
Advanced ECF: Pertains to any fiber line that uses exclusively
Advanced ECF bleaching processes, or exclusively ECF and TCF
bleaching processes as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3)  and certified under 40 CFR
122.22.  Advanced ECF consists of the use of extended
delignification or other technologies that achieve at least the
Tier I performance levels specified in § 430.24(b) (4) (i) .
TCF: Pertains to any fiber line that uses exclusively TCF
bleaching processes, as disclosed by the discharger in its permit
application under 40 CFR 122.21(g)(3)  and certified under 40 CFR
122.22.
This regulation does not specify a limit for this pollutant for
TCF bleaching processes.
Monitoring frequency does not apply to this compound when used as
a biocide.  The permitting authority must determine the
appropriate monitoring frequency for this compound,  when used as a
biocide, under 40 CFR 122.44(i).
                             805

-------
f     Monitoring requirements for these pollutants by mills certifying
      as Advanced ECF in their NPDES permit application or other
      communication to the permitting authority will be suspended after
      one year of monitoring.  The permitting authority must determine
      the appropriate monitoring frequency for these pollutants beyond
      that time under 40 CFR 122.44 (i).

      (d)   Reduced monitoring frequencies  for AOX  under the

Voluntary Advanced Technology Incentives  Program  (year one).

The  following monitoring frequencies apply to direct

dischargers enrolled in the Voluntary Advanced Technology

Incentives Program established under Subpart B of this part

for  a duration of one year after  achievement of the

applicable BAT limitations specified in §  430.24(b) (4) (i)  or

NSPS specified in § 430.25(c)  (2) :
CAS
Number
59473040
Pollutant
AOX
Non-ECF, any
Tier a
daily
Advanced
ECF, any
Tier b
weekly
TCP, any
Tier c
none
specified
a     non-ECF: Pertains to any fiber line that does not use  exclusively
      ECF or TCF bleaching processes.
b     Advanced ECF:  Pertains to any fiber line that uses exclusively
      Advanced ECF bleaching processes or exclusively ECF and TCF
      bleaching processes, as disclosed by the discharger in its permit
      application under 40 CFR 122.21(g)(3)  and certified under 40 CFR
      122.22.  Advanced ECF consists of the use of extended
      delignification or other technologies that achieve at  least the
      Tier I performance levels specified in § 430.24(b) (4) (i) .
0     TCF: Pertains  to any fiber line that uses exclusively  TCF
      bleaching processes, as disclosed by the discharger in its permit
      application under 40 CFR 122.21(g)(3)  and certified under 40 CFR
      122:22.

      (e)   Reduced monitoring frequencies for AOX under the

Voluntary Advanced Technology Incentives Program  (years two

through five).   The following monitoring frequencies apply
                                806

-------
to mills enrolled in the Voluntary Advanced Technology



Incentives Program established under Subpart B of this part



for a duration of four years starting one year after



achievement of the applicable BAT limitations specified in §



430.24(b) (4) (i) or NSPS specified in § 430.25 (c) (2) :
                             807

-------



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      (3)  Immediate Process Area: The location at the mill




where pulping, screening, knotting, pulp washing, pulping



liquor concentration, pulping liquor processing, and



chemical recovery facilities are located, generally the



battery limits of the aforementioned processes.  "Immediate



process area" includes spent pulping liquor storage and



spill control tanks located at the mill, whether or not they



are located in the immediate process area.



      (4)  Intentional Diversion: The planned removal of




spent pulping liquor, soap, or turpentine from equipment



items in spent pulping liquor, soap, or turpentine service



by the mill for any purpose including, but not limited to,



maintenance, grade changes, or process shutdowns.



      (5)  Mill: The owner or operator of a direct or




indirect discharging pulp, paper, or paperboard



manufacturing facility subject to this section.



      (6)  Senior Technical Manager: The person designated by




the mill manager to review the BMP Plan.  The senior



technical manager shall be the chief engineer at the mill,



the manager of pulping and chemical recovery operations, or



other such responsible person designated by the mill manager



who has knowledge of and responsibility for pulping and



chemical recovery operations.



      (7)  Soap: The product of reaction between the alkali




in kraft pulping liquor and fatty acid portions of the wood,





                             809

-------
turpentine that do occur.  BMPs must be developed according



to best engineering practices and must be implemented  in  a



manner that takes into account the specific circumstances at



each mill.  The BMPs are as follows:



      (1)  The mill must return spilled or diverted spent



pulping liquors, soap, and turpentine to the process to the



maximum extent practicable as determined by the mill,



recover such materials outside the process, or discharge



spilled or diverted material at a rate that does not disrupt



the receiving wastewater treatment system.



      (2)  The mill must establish a program to identify and



repair leaking equipment items.  This program must include:



          (i)  Regular visual inspections (e.g., once per



day) of process areas with equipment items in spent pulping



liquor, soap, and turpentine service;



          (ii)  Immediate repairs of leaking equipment



items, when possible.  Leaking equipment items that cannot



be repaired during normal operations must be identified,



temporary means for mitigating the leaks must be provided,



and the leaking equipment items repaired during the next



maintenance outage;



          (iii)   Identification of conditions under which



production will be curtailed or halted to repair leaking



equipment items or to prevent pulping liquor,  soap,  and



turpentine leaks and spills;  and



          (iv)  A means for tracking repairs over time to





                             811

-------
identify those equipment items where upgrade or replacement



may be warranted based on frequency and severity of leaks,



spills, or failures.



      (3)  The mill must operate continuous, automatic



monitoring systems that the mill determines are necessary to



detect and control leaks, spills, and intentional diversions



of spent pulping liquor, soap, and turpentine.  These



monitoring systems should be integrated with the mill



process control system and may include, e.g., high level



monitors and alarms on storage tanks; process area



conductivity  (or pH) monitors and alarms; and process area



sewer, process wastewater, and wastewater treatment plant



conductivity  (or pH) monitors and alarms.



      (4)  The mill must establish a program of initial and



refresher training of operators, maintenance personnel, and



other technical and supervisory personnel who have



responsibility for operating, maintaining, or supervising



the operation and maintenance of equipment items in spent



pulping liquor, soap, and turpentine service.  The refresher



training must be conducted at least annually and the



training program must be documented.



      (5)  The mill must prepare  a brief report that



evaluates each spill of  spent pulping  liquor, soap, or



turpentine that is not  contained at the immediate process



area  and any  intentional diversion of  spent pulping liquor,



soap,  or turpentine that is  not  contained  at the immediate





                             812

-------
containment for spent pulping liquor bulk storage tanks.



      (8)  The mill must install and maintain secondary



containment for turpentine bulk storage tanks.



      (9)  The mill must install and maintain curbing, diking



or other means of isolating soap and turpentine processing



and loading areas from the wastewater treatment facilities.



      (10)  The mill must conduct wastewater monitoring to



detect leaks and spills, to track the effectiveness of the



BMPs, and to detect trends in spent pulping liquor losses.



Such monitoring must be performed in accordance with



paragraph (i) of this section.



      (d)  Requirement to develop a BMP Plan. (1)  Each mill



subject to this section must prepare and implement a BMP



Plan.  The BMP Plan must be based on a detailed engineering



review as described in paragraphs (d)(2) and (3) of this



section.  The BMP Plan must specify the procedures and the



practices required for each mill to meet the requirements of



paragraph (c) of this section, the construction the mill



determines is necessary to meet those requirements including



a schedule for such construction, and the monitoring program



(including the statistically derived action levels)  that



will be used to meet the requirements of paragraph (i) of



this section.  The BMP Plan also must specify the period of



time that the mill determines the action .levels established



under paragraph (h) of this section may be exceeded without



triggering the responses specified .in paragraph (i)  of this





                             814

-------
section.



      (2)  Each mill subject to this section must conduct a



detailed engineering review of the pulping and chemical



recovery operations -- including but not limited to process



equipment, storage tanks, pipelines and pumping systems,



loading and unloading facilities, and other appurtenant



pulping and chemical recovery equipment items in spent



pulping liquor, soap, and turpentine service -- for the



purpose of determining the magnitude and routing of



potential leaks, spills, and intentional diversions of spent



pulping liquors, soap, and turpentine during the following



periods of operation:



      (i) Process start-ups and shut downs;



      (ii) Maintenance;



      (iii) Production grade changes;



      (iv)  Storm or other weather events;



      (v) Power failures; and



      (vi) Normal operations.



      (3)  As part of the engineering review,  the mill must



determine whether existing spent pulping liquor containment



facilities are of adequate capacity for collection and



storage of anticipated intentional liquor diversions with



sufficient contingency for collection and containment of



spills.  The engineering review must also consider:



      (i)  The need for continuous, automatic monitoring



systems to detect and control leaks and spills of spent





                             815

-------
pulping liquor, soap, and turpentine;



     (ii)  The need .for process wastewater diversion



facilities to protect end-of-pipe wastewater treatment



facilities from adverse effects of spills and diversions of



spent pulping liquors, soap, and turpentine;



     (iii)  The potential for .contamination of storm water




from the immediate process areas; and



     (iv)  The extent to which segregation and/or collection



and treatment of contaminated storm water from the immediate



process areas is appropriate.



     (e)  Amendment of BMP Plan.  (1)  Each mill subject to



this section must amend its BMP Plan whenever there is a



change in mill design, construction, operation, or



maintenance that materially affects the potential for leaks



or spills of spent pulping liquor, turpentine, or soap from



the immediate process areas.



     (2)  Each mill subject to this section must complete a



review and evaluation of the BMP Plan five years after the



first BMP Plan is prepared and, except as provided in



paragraph  (e)(1) of this section, once every five years



thereafter.  As a result of this review and evaluation, the



mill must amend the BMP Plan within three months of the



review if'the mill determines that any new or modified



management practices and engineered controls are necessary



to reduce significantly the likelihood of spent pulping



liquor,  soap, and turpentine leaks, spills, or intentional




                             816

-------
           (ii)  Records of initial and refresher training



conducted in accordance with paragraph  (c)(4) of this



section;



           (iii)  Reports prepared in accordance with



paragraph  (c)(5) of this section; and



           (iv)  Records of monitoring required by paragraphs



(c)(10) and  (i) of this section.



      (h)  Establishment of wastewater treatment system



influent action levels.  (1)  Each mill subject to this



section must conduct a monitoring program, described in



paragraph  (2) of this section, for the purpose of defining



wastewater treatment system influent characteristics  (or



action levels), described in paragraph  (3) of this section,



that will trigger requirements to initiate investigations on



BMP effectiveness and to take corrective action.



      (2)  Each mill subject to this section must employ the



following procedures in order to develop the action levels



required by paragraph  (h) of this section:



           (i)  Monitoring parameters.  The mill must collect



24-hour composite samples and analyze the samples for a



measure of organic content  (e.g., Chemical Oxygen Demand



(COD) or Total Organic Carbon (TOC)).  Alternatively, the



mill may use a measure related to spent pulping liquor



losses measured continuously and averaged over 24 hours




(e.g., specific conductivity or color).



           (ii)  Monitoring locations.  For direct





                             818

-------
dischargers, monitoring must be conducted at the point



influent enters the wastewater treatment system.  For



indirect dischargers monitoring must be conducted at the



point of discharge to the POTW.  For the purposes of this



requirement, the mill may select alternate monitoring



point(s) in order to isolate possible sources of spent



pulping liquor, soap, or turpentine from other possible



sources of organic wastewaters.that are tributary to the



wastewater treatment facilities (e.g., bleach plants, paper



machines and secondary fiber operations).



      (3)  By the date prescribed in paragraph (j)(1)(iii) of



this section, each existing discharger subject to this



section must complete an initial six-month monitoring



program using the procedures specified in paragraph  (h)(2)



of this section and must establish initial action levels




based on the results of that program.  A wastewater



treatment influent action level is a statistically



determined pollutant loading determined by a statistical



analysis of six months of daily measurements.  The action



levels must consist of a lower action level, which if




exceeded will trigger the investigation requirements



described in paragraph (i)  of this section,  and an upper




action level, which if exceeded will trigger the corrective




action requirements described in paragraph  (i)  of this



section.
                             819

-------
      (4)  By the date prescribed in paragraph  (j)(1)(vi) of



this section, each existing discharger must complete a



second six-month monitoring program using the procedures



specified in paragraph  (h) (2) of this section and must



establish revised action  levels based on the results of that




program.  The initial action levels shall remain in effect



until replaced by revised action levels.



      (5)  By the date prescribed in paragraph  (j)(2) of this



section, each new source  subject to this section must



complete a six-month monitoring program using the procedures



specified in paragraph  (h) (2) of this section and must



develop a lowe±- action  level and an upper action level based




on the results of that  program.



      (6)  Action levels developed under this paragraph must



be revised using six months of monitoring data after any



change in mill design,  construction, operation, or



maintenance that materially affects the potential for leaks



or spills of spent pulping liquor, soap, or turpentine from



the immediate process areas.



      (i)  Monitoring, corrective action, and reporting



requirements.  (1)  Each  mill subject to this section must



conduct daily monitoring  of the influent to the wastewater



treatment system in accordance with the procedures described



in paragraph (h)(2) of  this section for the purpose of



detecting leaks and spills, tracking the effectiveness of



the BMPs, and detecting trends in spent pulping liquor




                             820

-------
once per year.



      (j)  Compliance deadlines.   (1)  Existing direct and



indirect dischargers.  Except as provided in paragraph



(j)(2) of this section for new sources,  indirect discharging



mills subject to this section must meet  the deadlines set



forth below.  Except as provided in paragraph  (j)(2) of this



section for new sources, NPDES permits must require direct



discharging mills subject to this section to meet the



deadlines set forth below.  If a deadline set forth below



has passed at the time the NPDES permit  containing the BMP



requirement is issued, the NPDES permit  must require



•immediate compliance with such BMP requirement(s).



           (i)  Prepare BMP Plans and  certify to the



permitting or pretreatment authority  that the BMP Plan has



been prepared in accordance with this regulation not later



than  [insert date 12 months after date of publication] ;




           (ii)  Implement all BMPs specified in paragraph



(c)  of this section that do not require  the construction of



containment or diversion structures or the installation of



monitoring and alarm systems not later than  [insert date 12




months after date of publication].




           (iii)  Establish initial action levels required by



paragraph  (h)(3) of this section not  later than  [insert date




12 months after date of publication].




           (iv)  Commence .operation of any new or upgraded





                             822

-------
after commencement of discharge, based on six months of



monitoring data obtained prior to that date in accordance



with the procedures specified in paragraph  (h)(2) of this



section.



Subpart A-Dissolving Kraft Subcategory




§ 430.10  Applicability; description of the dissolving kraft




subcategory.




     The provisions of this subpart apply to discharges



resulting from the production of dissolving pulp at kraft



mills.



§ 430.11  Specialized definitions.




     For the purpose of this subpart, the general



definitions, abbreviations, and methods of analysis set



forth in 40 CFR part 401 and § 430.01 of this part shall



apply to this subpart.



§ 430.12  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




     (a)  Except as provided in 40 CFR 125.30 through



125.32, any existing point source subject to this subpart



must achieve the following effluent limitations representing



the degree of effluent reduction attainable by the



application of the best practicable control technology



currently available (BPT), except that non-continuous



dischargers shall not be subject to the maximum day and




                             824

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average of 30 consecutive days limitations but shall be



subject to annual average effluent limitations:



                          Subpart A
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
23.6
37.3
(J)
Average of daily
values for 30
consecutive days
12.25
20.05
0)
Non-continuous
dischargers
6.88
11.02
H
       the range of 5.0 to 9.0 at all times.






      (b)  The following limitations establish the quantity



or quality of pollutants or pollutant properties, controlled



by this section, resulting from the use of wet barking



operations, which may be discharged by a. point source



subject to the provisions of this subpart.  These



limitations are in addition to the limitations set forth in



paragraph  (a) of this section and shall be calculated using



the proportion- of the mill's total production due to use of



logs which are subject to such operations.  Non-continuous



dischargers shall not be subject to the maximum day and



average of 30 consecutive days limitations, but shall be



subject to annual average effluent limitations:
                             825

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                          Subpart A
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
3.2
6.9
C1)
Average of daily
values for 30
consecutive days
1.7
3.75
(l)
Non-continuous
dischargers
(Annual Average)
0.95
2.0
t1)
Within the range of 5.0 to 9.0 at all times.



      (c)  The following limitations establish the quantity



or quality of pollutants or pollutant parameters, controlled



by this section, resulting from the use of log washing or



chip washing operations, which may be discharged by a point



source subject to the provisions of this subpart.  These



limitations are in addition to the limitations set forth in



paragraph (a) of this section and shall be calculated using



the proportion of the mill's total production due to use of



logs and/or chips which are subject to such operations. Non-



continuous dischargers shall not be subject to the maximum



day and average of 30 consecutive days limitations, but



shall be subject to the annual average effluent limitations:
                             826

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                          Subpart A
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
0.70
(x)
Average of daily
values for 30
consecutive days
0.2
0.4
C1)
Non- continuous
dischargers
(Annual Average)
0.1
0.2
(l)
xWithin the range of 5.0 to 9.0 at all times.

      (d)  The following limitations establish the quantity

or quality of pollutants  or pollutant properties, controlled
                                             sr
by this section, resulting from the use of log  flumes or  log

ponds, which may be discharged  by a point source subject  to

the provisions of this subpart.  These limitations are  in

addition to the limitations set forth in paragraph  (a)  of

this section and shall be calculated using the  proportion of

the mill's total production due to use of logs  which are

subject to such operations.  Non-continuous  dischargers

shall not be subject to the maximum day and  average of  30

consecutive days limitations but shall be subject to the

annual average effluent limitations:
                             827

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                          Subpart A
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.6
1.45
(x)
Average of daily
values for 30
consecutive days
0.35
0.8
(l)
Non-continuous
dischargers
(Annual Average)
0.2
0.4
H
xWithin the range of 5.0 to 9.0 at all times.




§ 430.13  Effluent limitations  guidelines representing  the




degree of effluent reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




     Except as provided in 40 CFR 125.30 through 125.32,  any



existing point source  subject to this subpart shall achieve



the following effluent limitations representing the degree



of effluent reduction  attainable by the application of  the



best conventional pollutant control technology  (BCT): The



limitations shall be the same as those specified for



conventional pollutants (which  are defined in 40 CFR 401.16)



in § 430.12 of this subpart for the best practicable control



technology currently available  (BPT) .



§ 430.14  Effluent limitations  representing the degree  of




effluent reduction attainable by the application of the best




available technology economically achievable  (BAT).




     Except as provided in 40 CFR 125.30 through 125.32,  any
                             828

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existing point  source  subject to this subpart where



chlorophenolic-containing biocides are used must achieve  the



following effluent  limitations representing the degree of



effluent reduction  attainable by the application of the best



available technology economically achievable  (BAT).  Non-



continuous dischargers shall not be subject to the maximum



,day mass limitations in kg/kkg  (lb/1000 Ib) but shall be



subject to concentration limitations.  Concentration



limitations are only applicable to non-continuous



dischargers.  Permittees not using chlorophenolic-containing



biocides must certify  to the permit-issuing authority that



they are not using  these biocides:



                          Subpart A
Pollutant or
pollutant property
Pentachlorophenpl
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0025
0.016
Milligrams/liter
(0.011) (55.1)/y
(0.068) (55.1)/y
y = wastewater discharged in kgal per ton of product
§ 430.15  New source performance standards  (NSPS).




     Any new source subject to this subpart must  achieve the



following new source performance standards  (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BOD5 and TSS, but shall be subject to annual
                             829

-------
average effluent limitations.  Also,  for non-continuous



dischargers, concentration limitations  (mg/1)  shall  apply,



where provided.  Concentration limitations will only apply



to non-continuous dischargers.  Only  facilities where



chlorophenolic-containing biocides are used  shall be subject



to pentachlorophenol and trichlorophenol limitations.



Permittees not using chlorophenolic-containing biocides must



certify to the permit-issuing authority that they are not



using these biocides:



                          Subpart  A
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Tr i chlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
15.6
27.3
(l )
Average of
daily
values for
30
consecutive
days
8.4
14.3
t1 )
Non - cont inuous
Dischargers
(Annual Average)
4.4
7.5
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0025
0.016
Milligrams/liter
(0.012) (50.7)/y
(0.074) (50.7)/y
y = wastewater discharged in kgal per ton at all times
      the range of 5.0 to 9.0 at all times.
                             830

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§ 430.16  Pretreatment standards for existing sources

(PSES).

     Except as provided in 40 CFR 403.7 and 403.13, any

existing source  subject to this subpart that introduces

pollutants, into  a publicly owned treatment works must:

comply with 40 CFR part 403;  and achieve the following

pretreatment standards for existing sources (PSES) if it

uses chlorophenolic-containing biocides.  Permittees not

using chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides.  PSES  must  be attained on or before July 1, 1984:

                          Subpart A
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
•PSES
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (55.1)/y
(0.082) (55. l)/y
Kg/kkg (or pounds per
1,000 Ib) of product8
0.0025
0.019
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to impose mass effluent limitations.
§ 430.17  Pretreatment  standards for new sources (PSNS).

     Except as provided in 40  CFR 403.7,  any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must:  comply with 40 CFR part

403; and achieve the  following pretreatment standards for

new sources  (PSNS)  if it uses  chlorophenolic-containing
                             831

-------
biocides.   Permittees not using chlorophenolic-containing

biocid.es must  certify to the permit-issuing authority that

they are not using these biocides:

                          Subpart A
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.012) (50. 7) /y
(0.089) (50.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0025
0.019
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
Subpart B-Bleached Papergrade Kraft and Soda Subcategory

§ 430.20  Applicability;  description of the bleached

papergrade kraft  and soda subcategory.

     The provisions of this subpart apply to discharges

resulting from: the production of market pulp at bleached

kraft mills;  the  integrated production of paperboard, coarse

paper, and tissue paper at bleached kraft mills; the

integrated production of pulp and fine papers at bleached

kraft mills;  and  the integrated production of pulp and paper

at soda mills.

§ 430.21  Specialized definitions.

      (a)  The general definitions, abbreviations, and

methods of analysis set forth in 40 CFR part 401 and §

430.01 of this part apply to this subpart.
                              832

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      (b)   Baseline BAT limitations  or NSPS means  the  BAT
limitations  specified in §430.24(a)(1) or  (2),  as
applicable,  and the NSPS specified  in § 430.25(b)(1)  or (2),
as applicable,  that apply to any direct discharger  that is
not  "enrolled"  in  the "Voluntary Advanced Technology
Incentive's Program. "
      (c)   Enroll means to notify the permitting authority
that a mill  intends to participate  in the "Voluntary
Advanced Technology Incentives Program."  A mill  can  enroll
by indicating its  intention to participate in the program
either as  part  of  its application for a National  Pollutant
Discharge  Elimination System  (NPDES) permit, or through
separate correspondence to the permitting authority as  long
as the mill  signs  the correspondence in accordance with 40
CPR 122.22.
     (d)   Existing effluent quality means the level at  which
the pollutants  identified in § 430.24(a)(1)  are present  in
the. effluent of a  mill  "enrolled" in the "Voluntary Advanced
Technology Incentives  Program."
     (e)   Kappa number  is  a measure of the lignin content in
unbleached pulp, determined after pulping and prior to
bleaching.
     (f)  Voluntary Advanced Technology Incentives Program
is the program established under § 430.24(b)  (for existing
direct dischargers) and  § 430.25 (c)  (for new direct
dischargers)  whereby participating mills agree to accept

                             833

-------
enforceable effluent limitations and conditions in their



NPDES permits that are more stringent than the "baseline BAT



limitations or NSPS" that would otherwise apply, in exchange



for regulatory- and enforcement-related rewards and



incentives.



§ 430.22  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available  (BPT).




      (a)  Except as provided in 40 CFR 125.30 through



125.32, any existing point source subject to this subpart



must achieve the following effluent limitations representing



the degree of effluent reduction attainable by the



application of the best practicable control technology



currently available (BPT):



                          Subpart  B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
15.45
30.4
(*)
Average of daily
values for 30
consecutive days
8.05
16.4
t1)
Non- continuous
dischargers
(Annual Average)
4.52
9.01
(l)
^Within the range of 5.0 to 9.0 at all times.
                             834

-------
                              Subpart  B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
13.65
24.0
(l)
Average of daily
values for 30
consecutive days
7.1
12 . 9
(*) '
Non-continuous
di s chargers
(Annual Average)
3.99
7.09
t1)
       the range of 5.0  to  9.0 at all times.




                             Subpart  B
Pollutant
or
pollutant
parameter
BOD5
TSS
pH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
'Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
10.6
22.15
t1)
Average of daily
values for 30
consecutive days
5.5
11.9
(x)
Non-continuous
dischargers
(Annual Average)
3.09
6.54
(x)
Within the range of 5.0  to  9.0 at all times.
                                 835

-------
                          Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
soda facilities where pulp and paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any
1 day
13.7
24.5
(*)
Average of daily
values for 30
consecutive days
7.1
13.2
(x)
Non-continuous
dischargers
(Annual Average)
3.99
7.25
t1)
       the range of 5.0 to 9.0 at all times.




      (b)  The following limitations  establish the  quantity



or quality of pollutants or pollutant  properties,  controlled



by this section,  resulting from the  use  of  wet barking



operations, which may  be discharged  by a point source



subject to the provisions of. this  subpart.   These



limitations are  in addition to  the limitations set forth in



paragraph  (a) of  this  section and  shall  be  calculated  using



the proportion of the  mill's total production due  to use of



logs which are subject to such  operations:
                             836

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                             Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1 day
2.3
5.3
(x)
Average of daily
values for 30
consecutive days
1.2
2.85
H
Non - cont inuous
dischargers
(Annual Average)
0.70
1 . 55
(a)
Within the range of 5.0 to 9.0 at all times.




                             Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.25
5.75
t1)
Average of daily
values for 30
consecutive days
1.2
3.1
t1)
Non-continuous
dischargers
(Annual Average)
0.65
1.70
(*)
xWithin the
                                 837

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                          Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraf t facilities where pulp and fine papers ' are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1.95
5.3
t1)
Average of daily
values for 30
consecutive days
1.0
2.85
C1)
Non-conti nuou s
dischargers
(Annual Average)
0.55
1.55
(l)
Within the range of 5.0 to 9.0 at all times.




                          Subpart B
Pollutant
or
pollutant
parameter
BOD5
TSS
pH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.05
5.25
(l)
Average of daily
values for 30
consecutive days
1.1
2.8
(l)
Non- continuous
dischargers
(Annual Average)
0.60
1.55
H
aWithin the range of 5.0 to 9.0 at  all times.




      (c)  The following limitations establish the quantity



or quality of pollutants or pollutant  parameters, controlled



by this section,  resulting from the use of log washing or



chip washing operations,  which may be  discharged by a point



source subject to the  provisions of this subpart.  These



limitations are  in addition to the limitations set forth in



paragraph  (a) of this  section and shall be calculated using
                             838

-------
the proportion of the mill's total production due to  use of



logs  and/or chips which are subject  to  such operations:



                           Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.2
0.6
H
Average of daily
values for 30
consecutive days
0.1
0.3
H
Non - cont inuous
dischargers
(Annual Average)
0.1
0.15
H
^•Within the range of 5.0 to 9.0 at all times.




                           Subpart  B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.25
0.65
H
Average of daily
values for 30
consecutive days
0.15
0.35- -
n
Non-continuous
dischargers
(Annual Average)
0.05
0.20
(x)
•"•Within the range, of 5.0 to 9.0 at all times.
                               839

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                          Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.2
0.55
t1)
Average of daily
values for 30
consecutive days
0.1
0.3
(:) '.
Non - c ont i nuou s
dischargers
(Annual Average)
0.05
0.15
C1)
Within the range of 5.0 to 9.0 at all times.




                          Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
pH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.5
(a)
Average of daily
values for 30
consecutive days
0.1
0.25
(*)
Non- continuous
dischargers
(Annual Average)
0.05
0.15
H
xWithin the range of 5.0 to 9.0 at all times.




      (d)  The following limitations establish the quantity



or quality of pollutants or pollutant  properties, controlled



by this section,  resulting from the use of log flumes or  log



ponds, which may be  discharged by a point source subject  to



the provisions of this subpart.   These limitations are  in



addition to the  limitations set forth in paragraph  (a)  of
                              840

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this section and-shall be calculated using the proportion of



the mill's  total production due  to use of logs which are



subject to  such operations:



                           Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where market pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.4
1.15
H
Average of daily
values for 30
consecutive days
0.2
0.6
(x)
Non- continuous
dischargers
(Annual Average)
0.15
0.35
(*)
 Within the range of 5.0 to 9.0 at all times.




                           Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.45
1.25
(l)
Average of daily
values for 30
consecutive days
0.25
0.7
C1)
Non- continuous
di s chargers
(Annual Average)
0.10
0.35
t1')
1Wxthin the range of 5.0 to 9.0  at all times.
                              841

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                           Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
bleached kraft facilities where pulp and fine papers are
produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
1.15
n
Average of daily
values for 30
consecutive days
0.2
0.6
(l)
Non-continuous
dischargers
(Annual Average)
0.10
0.30
(a)
Within the range of 5.0 to 9.0 at all times.
                           Subpart B
Pollutant
or
pollutant
parameter
BODS
TSS
PH
BPT effluent limitations for
soda facilities where pulp and papers are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.3
1.1
H
Average of daily
values for 30
consecutive days
0.2
0.55
(J)
Non- continuous
dischargers
(Annual Average)
0.10
0.35
H
xWithin the range of 5.0 to 9.0 at all times.




§ 430.23  Effluent limitations representing the degree  of




effluent reduction attainable by the application of  the best




conventional pollutant control technology  (BCT).




     Except as provided in 40 CFR 125.30 through 125.32,  any



existing point source  subject to this subpart must achieve
                              842

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the following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best conventional pollutant control technology -(BCT) .  The



limitations shall be the same as those specified in § 430.22



of this subpart for the best practicable control technology



currently available  (BPT).



§ 430.24  Effluent limitations representing the degree of




effluent reduction attainable by the application of best




available technology economically achievable  (BAT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart must achieve



the following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best available technology economically achievable (BAT).



     (a)  Except as provided in paragraph  (b)  of this



section--(1)  the following effluent limitations apply with



respect to each fiber line that does not use an exclusively



TCP bleaching process, as disclosed by the discharger in its



NPDES permit application under 40 CFR 122.21(g)(3) and



certified under 40 CFR 122.22:
                             843

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                        Subpart  B
Pollutant-
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol

AOX
COD
BAT effluent limitations
Maximum for any
1 day

-------
      This regulation does not specify this type of limitation for this
      pollutant; however, permitting authorities may do  so as
      appropriate.
      picograms per liter.
      grams per 1,000 kilograms (g/kkg).
      [Reserved].
           (2) The  following effluent limitations apply with

respect  to each fiber line that  uses exclusively TCF

bleaching processes,  as disclosed by the discharger in its

NPDES  permit application under 40 CFR 122.21(g)(3)  and

certified under 40  CFR 122.22:

                            Subpart B
Pollutant or
pollutant
property
AOX
COD
BAT effluent limitations (TCF)
Continuous dischargers
Maximum for
any 1 day
Monthly
average
Non-continuous
dischargers
Maximum for
any 1 day
Annual
Average
kg/kkg(or pounds per 1,000 Ib) of product

-------
quality  or  the  discharger's  current  effluent limitations



established under  CWA  section  301(b)(2), whichever are more



stringent,  for  the pollutants  identified in paragraph  (a)(1)



of this  section (with  the  exception  of COD).  For AOX, the



permitting  authority must  determine  existing effluent



quality  for each fiber line  enrolled in the Voluntary



Advanced Technology Incentives Program at the end of the



pipe based  on loadings attributable  to that fiber line.  For



the remaining pollutants,  with the exception of COD, the



permitting  authority must  determine  existing effluent



quality  for each fiber line  enrolled in the Voluntary



Advanced Technology Incentives Program at the point where



the wastewater  containing  those pollutants leaves the bleach



plant.   These limitations  must be recalculated each time the



NPDES permit of a  discharger enrolled in the Voluntary



Advanced Technology Incentives Program is reissued, up to:



                (i)   [insert  date 6 years from date of




publication] for all pollutants in paragraph (a)(1) of this




section  except  AOX; and



                (ii) The date specified in paragraph



(b) (4) (ii)  of this section for achieving the applicable AOX



limitation  specified in paragraph  (b) (4) (i) .



          (2)   Best Professional Judgment Milestones:




Narrative or numeric limitations and/or special permit



conditions, as  appropriate,  established by the permitting
                             846

-------
authority on the basis of his or her best professional



judgment that reflect reasonable interim milestones toward



achievement of the effluent limitations specified in



paragraphs  (b)(3) and  (b)(4) of this section, as applicable.



           (3)  Six-year Milestones:  By  [insert date six




years from  the date of publication], all dischargers




enrolled in the Voluntary Advanced  Technology Incentives



Program must achieve the following:



               (i) The effluent limitations specified in



paragraph  (a)(1)  of this section, except that, with respect



to AOX, dischargers subject to Tier I effluent limitations



specified in paragraph (b)(4)(i) of this section must



achieve the AOX limitation specified in that paragraph; or



               (ii) For dischargers that use exclusively TCF



bleaching processes as of  [insert date six years from the




date of publication], the effluent  limitations specified in




paragraph  (a)(2)  of this section.
                             847

-------
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                (ii)  Deadlines.  (A)  A discharger  enrolled



in Tier  I of the Voluntary Advanced Technology  Incentives



Program  must achieve the Tier I  limitations  in  paragraph



 (b) (4) (i) of this section by  [insert date  six years  from the




date of publication].




                    (B)  A discharger enrolled  in  Tier  II  of



the Voluntary Advanced Technology Incentives Program must



achieve  the Tier II limitations  in paragraph (b)(4)(i)  of



this section by  [insert date eleven years  from  the date of




publication].




                    (C)  A discharger enrolled  in  Tier  III



of the Voluntary Advanced Technology Incentives Program must



achieve  the Tier III limitations in paragraph (b) (4) (i)  of



this section by  [insert date sixteen years from the  date of




publication].




     (c)  [RESERVED].




     (d)   The following additional effluent limitations



apply to all dischargers subject to this section in



accordance with the previous subcategorization scheme unless



the discharger certifies to the permitting authority that it



is not using these compounds as biocides.   Also, for non-



continuous dischargers, concentration limitations  (mg/1)



shall apply.  Concentration limitations will only  apply  to



non-continuous dischargers:






                             849

-------
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0019
0.012
Milligrams /liter
(0.011) (41. 6) /y
(0.068) (41. 6) /y
y = wastewater discharged in kgal per ton of product
Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
0.010
Milligrams /liter
(0.011) (35.4)/y
(0.068) (35.4)/y
y = wastewater discharged in kgal per ton of product
    850

-------
                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014 .
0.0088
Milligrams/liter
(0.011) (30.9)/y
(0.068) (30.9)/y
y = wastewater discharged in kgal per ton of product
      (e)  Pursuant to 40 CFR 122.44(1) and 122.45(h), a



discharger must demonstrate compliance with the effluent



limitations in paragraph  (a)(1) or  (b)(3) of this section,



as applicable, by monitoring for all pollutants  (except for



AOX and COD) at the point where the wastewater containing



those pollutants leaves the bleach plant.  The permitting



authority may impose effluent limitations and/or monitoring



requirements on internal wastestreams for any other



pollutants covered in this section as appropriate under 40



CFR 122.44 (i) and 122.45.(h). In addition, a discharger



subject to a limitation on total pulping area condensate,



evaporator condensate, and bleach plant wastewater flow



under paragraph (b)(4)(i) of this section, for Tier II and



Tier III, must demonstrate compliance with that limitation



by establishing and maintaining flow measurement equipment



to monitor these flows at the point or points where they



leave the pulping area,  evaporator area, and bleach plant.
                             851

-------
§ 430.25  New  source performance  standards (NSPS).




     New sources  subject to  this  subpart  must  achieve the



following new  source performance  standards (NSPS),  as



applicable.



      (a)  The  following standards apply to each new source



that commenced discharge after  [insert date 10 years before




the date 60 days  from  the date  of publication}  and  before




[insert date 60 days from the date of publication} ,  provided




that the new source was constructed to meet these standards:



                          Subpart  B
Pollutant
or
pollutant
property
BODS
TSS
PH
1982 New Source Performance Standards for
bleached kraft facilities where market pulp is produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non- continuous
dischargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
10.3
18.2
(x)
5.5
9.5
t1)
2.88
5.00
t1)
(*) Within the range of 5.0 to 9.0 at all times.
                             852

-------
                           Subpart  B
Pollutant
or
pollutant
property
BODS
TSS
pH
1982 New Source Performance Standards for
bleached kraft facilities where paperboard, coarse paper,
and tissue paper are produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non - c ont inuous
di s chargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
8.5
14.6
(*)
4.6
7.6
H
2.41
4.00
(l)
   Within the range of 5.0 to 9.0 at all times.
                           Subpart  B
Pollutant
or
pollutant
property
BOD5
TSS
pH
1982 Hew Source Performance Standards for
bleached kraft facilities where pulp and fine papers are
produced and soda facilities where pulp and paper are
produced
Continuous dischargers
Maximum for any 1
day
Average of daily
values for 30
consecutive days
Non- continuous
dischargers
Annual average
kg/kkg (or pounds per 1,000 Ib)
of product
5.7
9.1
(x)
3 .1
4.8
f1)
1.62
2.53
H
   Within the range of 5.0 to 9.0 at all times.






      (b)   Except as provided in paragraph (c)  of this



section--(1)  The following  standards apply with respect  to
                               853

-------
each new source fiber line that does not use an exclusively



TCP bleaching process, as disclosed by the discharger in its



NPDES permit application under 40 CFR 122.21(g)(3) and



certified under 40 CFR 122.22, and that commences discharge



after [insert date 60 days from publication] :
                             854

-------
Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5- ,
trichloroguaiacbl
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2 , 4 , 5-trichlorophenol
2,4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol
i
AOX
BODS
TSS
pH
NSPS
Maximum for any
1 day

-------
  COD
C1)
"
-------
      pollutant; however, permitting authorities may do so as
      appropriate.
c     [Reserved].
d     Kilograms per 1,000 kilograms (kg/kkg).
 C1)    Within the range of 5.0 to 9.0 at all times.



      (c)   With'respect  to each new source fiber line that is

enrolled in the Voluntary Advanced Technology Incentives

Program,  dischargers subject to this section must achieve:

           (1)   The  standards specified  in paragraph  (b)(1)

of this  section  (except for AOX)  or paragraph (b)(2) of this

section,  as applicable;  and
                              857

-------
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      (d)  These additional standards apply to all new



sources, regardless of when they commenced discharge, in



accordance with the previous subcategorization scheme unless



the discharger certifies to the permitting authority that it



is not using -these compounds as biocides.  Also, for non-



continuous dischargers, concentration limitations  (mg/1)



shall apply.  Concentration limitations will only apply to



non-continuous dischargers:





                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0019
0.012
Milligrams /liter
(0.013) (36. 6) /y
(0.077) (36.6)/y
y = wastewater discharged in kgal' per ton of product
                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
lb)of product
0.0016
0.010
Milligrams /liter
(0.012) (31.7)/y
(0.076) (31.7)/y
y = wastewater discharged in kgal per ton of product
                             859

-------
                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental NSPS for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.0088
Milligrams/liter '
(0.014) (25.1)/y
(0.084) (25.1)/y
y = wastewater discharged in kgal per ton of product
      (e)  Pursuant to 40 CFR 122.44(1) and 122.45(h), a



discharger must demonstrate compliance with the limitations



in paragraph  (b)(1) or  (c)(1) of this section, as



applicable, by monitoring  for all pollutants  (except for



AOX, COD, BOD5,  TSS,  and pH)  at the point where the



wastewater containing those pollutants leaves the bleach



plant.  The permitting authority may impose effluent



limitations and/or monitoring requirements on internal



wastestreams for any other pollutants covered in this



section as appropriate under 40 CFR 122.44 (i) and 122.45(h).



In addition, a discharger  subject to a limitation on total



pulping area condensate, evaporator condensate, and bleach



plant wastewater flow under paragraph  (c)(2) of this section



must demonstrate compliance with that limitation by



establishing and maintaining flow measurement equipment



monitoring these flows at  the point or points where they



leave the pulping area, evaporator area, and the bleach
                             860

-------
plant.               •



§ 430.26 Pretreatment standards for existing sources  (PSES)




     Except as provided in 40 CFR 403.7 and 403.13, any



existing source subject to this subpart that introduces



pollutants into a publicly owned treatment works must:



comply with 40 CFR part 403; and achieve the following



pretreatment standards for existing sources (PSES).



     (a)   (1)  The following pretreatment standards apply



with respect to each fiber line operated by an indirect



discharger subject to this section, unless the indirect



discharger discloses to the pretreatment control authority



in a report submitted under 40 CFR 403.12(b)  that it uses



exclusively TCF bleaching processes at that fiber line.



These pretreatment standards must be attained on or before



[insert date 3 years from publication date] :
                             861

-------
                        Subpart B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2, 4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol
AOX
PSES
Maximum for any
1 day

-------
with respect to each fiber line operated by an indirect

discharger subject to this section if the  indirect

discharger discloses to the pretreatment control authority

in a report submitted under 40 CFR 403.12(b)  that it uses

exclusively TCP bleaching processes at that fiber line.

These pretreatment standards must be attained on or before

[insert  date 3 years from publication date] :

                           Subpart  B
Pollutant or
pollutant
parameter
AOX
PSES (TCP)
Maximum for any 1 day

-------
                    Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
lb)of product
0.0019
0.014
Milligrams /liter
(0.011) (41.6)/y
(0.082) (41.6)/y
y = wastewater discharged in kgal per ton of product
                    Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
0.012
Milligrams /liter
(0.011) (35.4)/y
(0.082) (35.4)/y
y = wastewater discharged in kgal per ton of product
                    Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.011
Milligrams /liter
(0.011) (30.9)/y
(0.082) (30.9)/y
y = wastewater discharged in kgal per ton of product
(c)  An indirect discharger must demonstrate compliance
                        864

-------
with the pretreatment standards in paragraph  (a)(1) of this

section by monitoring at the point where the wastewater

containing those pollutants leaves the bleach plant.

§ 430.27 Pretreatment standards for new sources  (PSNS).


     Except as provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources (PSNS).

     (a)  (1)   The following pretreatment standards apply
              !
with respect to each fiber line that is a new source, unless

the indirect discharger discloses to the pretreatment

control authority in a report submitted under 40 CFR 403.12

that it uses exclusively TCF bleaching processes at that

fiber line:
                             865

-------
                              Subpart  B
Pollutant
or
pollutant property
TCDD
TCDF
Chloroform
Trichlorosyringol
3,4,5-
trichlorocatechol
3,4,6-
trichlorocatechol
3,4,5-
trichloroguaiacol
3,4,6-
trichloroguaiacol
4,5,6-
trichloroguaiacol
2,4, 5-trichlorophenol
2, 4, 6-trichlorophenol
Tetrachlorocatechol
Tetrachloroguaiacol
2,3,4,6-
tetrachlorophenol
Pentachlorophenol
AOX
PSNS
Maximum for any
1 day

-------
indirect  discharger subject to this  section if the indirect

discharger discloses to the pretreatment  control authority

in a  report submitted under 40 CFR 403.12(b)  that it uses

exclusively TCP bleaching processes  at that fiber line:

                          Subpart B
Pollutant or
pollutant
parameter
AOX
PSNS (TCP)
Maximum for any 1 day

-------
                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where market pulp is
produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
lb)of product
0.0019
0.014
Milligrams /liter
(0.013) (36. 6) /y
(0.093) (36.6) /y
y = wastewater discharged in kgal per ton of product
                          Subpart B
Pollutant or pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where paperboard,
coarse paper, and tissue paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0016
0.012
Milligrams /liter
(0.012) (31.7)/y
(0.092) (31.7)/y
y = wastewater discharged in kgal per ton of product
                          Subpart B
Pollutant or pollutant
parameter
Pentachlorophenol
Trichlorophenol
Supplemental PSNS for
bleached kraft facilities where pulp and fine
papers are produced and soda facilities where
pulp and paper are produced
Maximum for any 1 day
kg/kkg
(or pounds per 1,000
Ib) of product
0.0014
0.011
Milligrams /liter
(0.014) (25.1)/y
(0.101) (25. I) /y
y = wastewater discharged in kgal per ton of product
      (c)  An indirect discharger must demonstrate  compliance



with the pretreatment standards in paragraph  (a)(1)  and of
                             868

-------
 this  section by monitoring  at  the point where  the wastewater



 containing  those pollutants leaves  the bleach  plant.



 §430.28 Best management practices  (BMPs).




      The definitions  and  requirements set  forth  in  40  CFR



 430.03 apply to facilities  in  this  subpart.



 Subpart C--Unbleached Kraft Subcategory




 §430.30  Applicability;  description of the unbleached kraft




 subcategory.




      The provisions of this subpart are applicable  to



 discharges  resulting  from:  the production  of pulp and  paper



 at unbleached kraft mills;  the production  of pulp and  paper




 at unbleached kraft-neutral sulfite semi-chemical  (cross



 recovery) mills; and  the  production of pulp and  paper  at



 combined unbleached kraft and  semi-chemical mills,  wherein



 the spent semi-chemical cooking  liquor is  burned within the



 unbleached  kraft chemical recovery  system.



 § 430.31  Specialized definitions.




      For the purpose  of this subpart, the  general



 definitions, abbreviations,  and  methods of analysis set



 forth in 40 CFR part  401  and § 430.01 of this  part  shall



.apply to this subpart.



 § 430.32  Effluent limitations representing the  degree of




 effluent reduction attainable  by the application of the best




 practicable control technology currently available  (BPT).
                             869

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      Except as provided in 40 CFR 125.30 through 125.32, any




existing point source subject to this subpart must achieve



the  following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best  practicable control technology currently available



 (BPT) :




                          Subpart C
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
unbleached kraft facilities
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1
day
5.6
12.0
(l)
Average of daily values for 30
consecutive days
2.8
6.0
(x)
                          Subpart C
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
unbleached kraft facilities producing pulp and paper using
the unbleached kraft-neutral sulfite semi-chemical (cross
recovery) process
Kg/kkg (or pounds per 1,000 lb) of product
Maximum for any 1
day
8.0
12.5
C1)
Average of daily values for
consecutive days
30
4.0
6.25
(x)
lWithin the range of 6.0 to 9.0 at all times.
                             870

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                          Subpart C
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
unbleached kraft facilities where pulp and paper are
produced using a combined unbleached kraft and semi-
chemical, process, wherein the spent semi-chemical cooking
liquor is burned within the unbleached kraft chemical
recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1
day
a
a
a
Average of daily values for 30
consecutive days
a
a
a
a[Reserved].




§ 430.33  Effluent limitations guidelines representing the




degree of effluent reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart shall achieve



the following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best conventional pollutant control technology (BCT), except



that ndn-continuous dischargers shall not be subject to the



maximum day and average-of-30-consecutive-days limitations,



but shall be subject to annual average effluent limitations:
                             871

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                          Subpart C
Pollutant
or
pollutant
property
BODS
TSS
PH
BCT effluent limitations for
unbleached kraft facilities
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
5.6
12.0
H
Average of daily
values for 30
consecutive days
2.8
6.0
C1)
Non- continuous
dischargers
(Annual Average)
1.9
3.6
(l)
^Within the range of 6.0 to 9.0 at all times .
Subpart C
Pollutant
or
pollutant
property
BODS
TSS
pH
BCT effluent limitations for unbleached kraft-neutral
sulfite semi-chemical (cross recovery) process and/or a
combined unbleached kraft and semi-chemical process,
wherein the spent semi -chemical cooking liquor is burned
within the unbleached kraft chemical recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
8.0
12.5
t1)
Average of daily
values for 3 0
consecutive days
4.0
6.25
'(*)
Non-continuous
dischargers
(Annual Average)
2.9
3.57
t1)
^Within the range of 6.0 to 9.0 at all times.




§ 430.34  Effluent  limitations  representing the degree of




effluent reduction  attainable by the application of the best




available technology economically achievable (BAT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart where
                             872

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chlorophenolic-containing biocides are used must achieve the



following effluent limitations representing the degree of



effluent reduction attainable by the application of the best



available technology economically achievable (BAT).  Non-



continuous dischargers shall not be subject to the maximum



day mass limitations in kg/kkg (lb/1000 Ib), but shall be



subject to concentration limitations.  Concentration



limitations are only applicable to non-continuous



dischargers.  Permittees not using chlorophenolic-containing



biocides must certify to the .permit-issuing authority that



they are not using these biocides:



                         Subpart C
Pollutant or
pollutant, property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
unbleached kraft facilities
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Milligrams/ liter
(0.011) (12. 6) /y
(0.010) (12.6)/y
y = wastewater discharged in kgal per ton of product
                             873

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                          Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
• BAT effluent limitations for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft-neutral
sulfite semi-chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00064
0.00059
Milligrams/ liter
(0.011) (14.0)/y
(0.010) (14.0)/y
y - wastewater discharged in kgal per ton of product
§ 430.35  New source performance standards (NSPS).




     Any new source subject to this subpart must achieve the



following new source performance standards (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BOD5 and TSS, but shall be subject to annual



average effluent limitations.  Also, for non-continuous



dischargers, concentration limitations  (mg/1) shall apply,



where provided.  Concentration limitations will only apply



to non-continuous dischargers.  Only facilities where



chlorophenolic-containing biocides are used shall be subject



to pentachlorophenol and trichlorophenol limitations.



Permittees not using chlorophenolic-containing biocides must



certify to the permit-issuing authority that they are not



using these biocides:
                             874

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Subpart C
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where
linerboard is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.4
5.8
C1 )
Average of
daily
values for
30
consecutive
days
1.8
3.0
(x )
Maximum for any 1
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Non-continuous
Dischargers
(Annual Average)
0.94
1.6
(M
day
Milligrams/
liter
(0.015) (9.4)/y
(0.013) (9.4)/y
y = wastewater discharged in kgal per ton at all times
   875

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                      Subpart C
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where
bag paper and other mixed products are produced)
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
5.0
9.1
(x )
Average of daily
values for 30
consecutive days
2.7
4.8
(1 )
Non-
continuous
Dischargers
(Annual
Average)
1.4
2.5
t1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00058
0.00053
Milligrams/
liter
(0.012) (11.4)/y
(0.011) (11.4)/y
y = wastewater discharged in kgal per ton at all times
the range of 5.0 to 9.0 at all  times.
                          876

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                           Subpart  C
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft-neutral
sulfite semi -chemical (cross recovery) process
and/ or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.9
7.3
t1 )
Average of
daily
values for
,30
consecutive
days
2.1
3.8
(1 )
Non- continuous
Dischargers
(Annual Average)
1.1
1.9
t1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00064
0.00059
Milligrams/
liter
(0.013) (11.5)/y
(0.012) (11.5)/y
y = wastewater discharged in kgal per ton at all times
xWithin the range of 5.0 to 9.0 at all times.




§ 430.36  Pretreatment standards for existing sources




(PSES).




     Except as provided in 40  CFR 403.7  and 403.13,  any



existing source  subject to this subpart  that introduces



pollutants into  a publicly owned treatment works must:



comply with 40 CFR part 403; and achieve the following
                             877

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pretreatment standards for existing sources  (PSES)  if it

uses  chlorophenolic-containing biocides.  Permittees not

using chlorophenolic-containing  biocides must  certify to  the

permit-issuing authority-that they are not using those

biocides.   PSES must  be attained on or before  July 1, 1984:

                            Subpart C
Pollutant or'
pollutant property
Pentachlorophenol
Tri chlorophenol
PSES for
unbleached kraft facilities
Maximum for any 1 day
Milligrams/ liter
(0.011) (12. 6) /y
(0.010) (12.6)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
"The following equivalent mass  limitations are provided as guidance in
cases where POTWs find it necessary to impose mass effluent limitations.

                            Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft -neutral
sulfite semi-chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
Maximum for any 1 day
Milligrams/liter
(0.011) (14.0)/y
(0.010) (14.0)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00064
0.00059
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases where POTWs find it necessary to impose mass effluent limitations.
                               878

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§ 430.37   Pretreatment standards for new sources (PSNS).

      (a)  Except as provided in 40 CFR  403.7,  any new source

subject to this subpart that introduces  pollutants into a

publicly  owned treatment works must: comply with 40 CFR part

403; and  achieve the following pretreatment standards for

new sources (PSNS)  if it uses chlorophenolic-containing

biocides.   Permittees not using chlorophenolic-containing

biocides  must  certify to the permit-issuing authority that

they are  not using these biocides:

                           Subpart C
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
unbleached kraft facilities where linerboard
produced
is
Maximum for any 1 day
. Milligrams/liter
(0.015) (9.4)/y
(0.013) (9.4) /Y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases where POTWs  find it necessary to impose mass effluent  limitations.
                              879

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                            Subpart C
Pollutant or
pollutant property
Pent achl oropheno 1
Trichlorophenol
PSNS for
unbleached kraft facilities where bag paper
other mixed products are produced
and
Maximum for any 1 day
Milligrams/liter
(0.012) (11.4)/y
(0.011) (11. 4) /y
Kg/kkg (or pounds per 1,
Ib) of product3
000
0.00058
0.00053
y = wastewater discharged in kgal per ton of product
 "The following equivalent mass limitations are provided as guidance in
cases where POTWs find it  necessary to impose mass effluent limitations.

                            Subpart  C
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
PSNS for
unbleached kraft facilities where pulp and paper
are produced using the unbleached kraft-neutral
sulfite semi-chemical (cross recovery) process
and/or a combined unbleached kraft and semi-
chemical process, wherein the spent semi-chemical
cooking liquor is burned within the unbleached
kraft chemical recovery system
. Maximum for any 1 day
Milligrams /liter
(0.013) (11.5)/y
(0.012) (11.5)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00064
0.00059
y = wastewater discharged in kgal per ton of product
 "The following equivalent mass limitations are provided as guidance in
cases where POTWs find it  necessary to impose mass effluent limitations.

Subpart D--Dissolving Sulfite Pulp Subcategory

§ 430.40  Applicability; description of the dissolving

sulfite pulp  subcategory.

     The provisions of this  subpart are applicable  to

discharges resulting  from  the production of pulp at
                                880

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dissolving sulfite mills.



§ 430.41  Specialized definitions.




     For the purpose of this subpart, the general



definitions, abbreviations, and methods of analysis set



forth in 40 CFR part 401 and § 430.01 of this part shall



apply to this subpart.



§ 430.42  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




     (a)  Except as provided in 40 CFR 125.30 through



125.32, any existing point source subject to this subpart



must achieve the following effluent limitations representing



the degree of effluent reduction attainable by the



application of the best practicable control technology



currently available (BPT), except that non-continuous



dischargers shall not be subject to the maximum day and



average of 30 consecutive days limitations but shall be



subject to annual average effluent limitations:
                             881

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                              Subpart D,
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where nitration grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
41.4
70.65

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                            S.ubpart D
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
dissolving sulfite pulp facilities where cellophane grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
48.05
70.65
(^
Average of daily
values for 30
consecutive days
24.95
38.05
(l)
Non - cont inuous
dischargers
(Annual Average)
14.0
20.9
(l)
^within the range of  5.0 to 9.0 at all times.
                           Subpart D
Pollutant
or
pollutant
property
BODS
TS'S
pH
BPT effluent limitations for
dissolving sulfite pulp facilities where acetate grade
pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
50.80 0)
70.65
(2)
Average of daily
values for 30
consecutive days
26.40 C1}
38.05
(2)
Non-continuous
dischargers
(Annual Average)
14.83 (x)
20.9
(2)
 BODS effluent limitations were remanded  (Weyerhaeuser Company,  et al v.
Costle, 590 F. 2nd 1011; D.C.  Circuit 1978).
2Within the range of 5.0 to 9.0 at all times

      (b)   The following limitations  establish the quantity

or quality of pollutants  or pollutant properties, controlled

by this  section, resulting  from the  use  of wet barking
                                                  \
operations,  which may  be  discharged  by a point source

subject  to the provisions of this subpart.   These
                               883

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limitations  are  in addition to  the limitations  set  forth in



paragraph  (a)  of this  section and shall  be  calculated using



the proportion of the  mill's total production due to  use of



logs which are subject to  such  operations.   Non-continuous



dischargers  shall not  be subject  to' the  maximum day and



average of 30  consecutive  days  limitations,  but shall be



subject to annual average  effluent limitations:



                          Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day,
0.7
0.15
(x)
Average of daily
values for 30
consecutive days
0.35
0.1
C1)
Non - cont inuous
dischargers
(Annual Average)
0.2
0.05
H
xWithin the range of 5.0 to 9.0 at all times.






      (c)  The following  limitations  establish the quantity



or quality of pollutants or pollutant parameters, controlled



by this section,  resulting from the  use of log washing or



chip washing operations,  which  may be discharged by a point



source subject to the provisions of  this subpart.  These



limitations are  in addition to  the limitations set forth in



paragraph  (a) of  this section and shall be calculated using



the proportion of the mill's total production due to use of



logs and/or chips which  are subject  to such operations. Non-



continuous dischargers shall not be  subject to the maximum




                             884

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 day and average of 30 consecutive days limitations, but



 shall be subject to the annual average effluent limitations



                          Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.15
(x)
Average of daily
values for 30
consecutive days
0.1
0.1
-(l)
Non-continuous
dischargers
(Annual Average)
0.05
0.05
H
•'Within the range of 5.0 to 9.0 at all times.






      (d)  The  following limitations establish the quantity



or quality  of  pollutants or pollutant  properties,  controlled



by this  section,  resulting from the use of log flumes or log



ponds, which may be  discharged by a point source subject to



the provisions of this subpart.   These limitations are in



addition to the  limitations set forth  in paragraph (a)  of



this section and shall be calculated using the proportion of



'the mill's  total  production due to use of logs which are



subject  to  such  operations.   Non-continuous dischargers



shall not be subject to the maximum day and average of 30



consecutive days  limitations but shall be subject  to the



annual average effluent limitations:
                             885

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                          Subpart D
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.15
C1)
Average of daily
values for 30
consecutive days
0.1
0.1
t1)
Non-continuous
dischargers
(Annual Average)
0.05
0.05
(x)
aWithin the range of 5.0 to 9.0 at all times.




§ 430.43  Effluent limitations guidelines representing  the




degree of effluent reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart shall achieve



the following effluent limitations representing the degree



of effluent reduction attainable by the application of  the



best conventional pollutant control technology  (BCT): The



limitations shall be the same as those specified for



conventional pollutants (which are defined in 40 CFR 401.16)



in § 430.42 of this subpart for the best practicable control



technology currently available (BPT).



§ 430.44  Effluent limitations representing the degree  of




effluent reduction attainable by the application of the best




available technology economically achievable  (BAT).




     Except as provided in 40 CFR 125.30 through 125.32, any
                             886

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existing point source subject to this subpart where

chlorqphenolic-containing biocides are used must achieve the

following effluent limitations representing the degree of

effluent reduction attainable by the application of the best

available technology economically achievable (BAT).   Non-

continuous dischargers shall not be subject to the maximum

day mass limitations in kg/kkg.(lb/1000 Ib) but shall be
                                             ;
subject to concentration limitations.  Concentration

limitations are only applicable to non-continuous

dischargers.  Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:

                          Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
BAT effluent limitations for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane pulps are
produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams/liter
(0.011) (66.0)/y
(0.058) (66.0)/y
y = wastewater discharged in kgal per ton of product
                             887

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                          Subpart  D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0033
0.021
Milligrams/liter
(0.011) (72.7)/y
(0. 068) (72 .7) /y
y = wastewater discharged in kgal per ton of product
§ 430.15  New source performance standards (NSPS).




     Any new source subject to this subpart must achieve the



following new source performance standards (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BODS and TSS, but shall be subject to annual



average effluent limitations.  Also, for non-continuous



dischargers, concentration limitations (mg/1) shall apply,



where provided.  Concentration limitations will only apply



to non-continuous dischargers.  Only facilities where



chlorophenolic-containing biocides are used shall be subject



to pentachlorophenol and trichlorophenol limitations.



Permittees not using chlorophenolic-containing bfocides must



certify to the permit-issuing authority that they are not



using these biocides:
                             888

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                              Subpart D
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlprophenol
NSPS for
dissolving sulfite pulp facilities where
nitration grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
.Maximum for any 1
day
26.9
40.8
C1 )
Average of
daily
values for
30
consecutive
days
14.5
21.3
(l )
Non - cont inuous
Dischargers
(Annual Average) •
7.59
11.2
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams /liter
(0.012) (59.0)/y
(0.012) (59.0)/y
y = wastewater discharged in kgal per ton at all times
'•Within the range of 5.0 to 9.0 at all  times.
                                  889

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                              Subpart  D
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where viscose
grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
28.7
40.8
t1 )
Average of
daily
values for
30
consecutive
days
15.5
21.3
(x )
Non- continuous
Dischargers
(Annual Average )
8.12
11.2
(M
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams/liter
(0.012) (59.0) /y
(0.012) (59.0)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
                                 890

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                              Subpart D
Pollutant or
pollutant property
BOD 5
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where
cellophane grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
31.2
40.8
f1 )
Average of
daily
values for
30
consecutive
days
• 16.8
21.3
(l )
Non-continuous
Dischargers
(Annual Average)
8.80
11.2
' ' (* )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.019
Milligrams /liter
(0.012) (59.0) /y
(0.076) (59.0)/y
y = wastewater discharged in kgal per ton at all times
'•Within the range of 5.0 to 9.0 at all  times.
                                  891

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                          Subpart D
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
39.6
41.1
(l )
Average of
daily
values for
30
consecutive
days
21.4
21.5
t1 )
Non- continuous
Dischargers
(Annual Average)
11.2
11.3
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0033
0.021
Milligrams /liter
(0.012) (65.7) /y
(0.075) (65.7)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all  times.




§ 430.46  Pretreatment standards for existing  sources




(PSES)..




     Except as provided in 40 CFR 403.7  and  403.13,  any



existing source  subject to this  subpart  that introduces



pollutants into  a publicly owned treatment works  must:



comply with 40 CFR part 403; and achieve the following



pretreatment standards for existing sources  (PSES)  if it



uses chlorophenolic-containing biocides.  Permittees not
                             892

-------
using  chlorophenolic-containing biocides must certify to the

permit-issuing, authority that they are not using  these

biocides.   PSES must be  attained on  or before July 1,  1984:


                           Subpart  D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane grade pulps are
produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (66.0) /y
(0.082) (66. 0) /y
Kg/kkg (or pounds per
1,000 Ib) of product a
0.0030
0.023
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass  effluent  limitations.

                           Subpart  D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.011) (.72 .7) /y
(0.082) (72.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0033
0.025
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent  limitations.

§ 430.47   Pretreatment  standards for new sources  (PSNS).

     Except as provided in  40 CFR 403.7,  any new  source

subject to this subpart that introduces  pollutants  into  a

publicly  owned treatment works must: comply with  40  CFR  part
                               893

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403;  and achieve the following pretreatment standards  for

new  sources  (PSNS)  if it uses chlorophenolic-containing

biocides.  Permittees not using chlorophenolic-containing

biocides must  certify to the  permit-issuing authority  that

they are not using these biocides:

                            Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
dissolving sulfite pulp facilities where
nitration, viscose, or cellophane grade pulps are
produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.012) (59.0) /y
(0.092) (S9.0)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0030
0.023
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases  when POTWs find it necessary to  impose mass effluent limitations.
                            Subpart D
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
dissolving sulfite pulp facilities where acetate
grade pulp is produced
Maximum for any 1 day
Milligrams /liter (mg/1)
(0.012) (65.7) /y
(0.091) (65.7) /y
Kg/kkg (or pounds per
1,000' Ib) of product3
0.0033
0.025
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations  are provided as guidance in
cases when POTWs  find it necessary to  impose mass effluent limitations.
                               894

-------
 Subpart  E-Papergrade  Sulfite  Subcategory




 § 430.50 Applicability;  description  of the papergrade




 sulfite  subcategory.




     The provisions of  this subpart apply to discharges •



 resulting from the: integrated production of pulp and paper



 at papergrade sulfite mills,  where blow pit pulp washing



 techniques are used;  and  the  integrated production of pulp



 and paper at papergrade sulfite mills where vacuum or



 pressure drums are used to wash pulp.



 § 430.51 Specialized definitions




     (a)  Except as provided  in paragraphs (b) and (c) of



 this section, the general definitions, abbreviations, and



 methods  of analysis set forth in 40 CFR part 401 and



 § 430.01 of this part apply to this subpart.




     (b)  Sulfite cooking liquor is defined as bisulfite



 cooking  liquor when the pH of the liquor is between 3.0 and



 6.0 and  as acid sulfite cooking liquor when the pH is less



 than 3.0.




     (c)  For this subpart, the segments for the papergrade



 sulfite  subcategory are defined as follows:




          (1)  The calcium-, magnesium-,  or sodium-based



 sulfite pulp segment consists of papergrade sulfite mills



where pulp and paper are produced using an acidic cooking



liquor of calcium,  magnesium,  or sodium sulfite,  unless



those mills are specialty grade sulfite mills;




                             895

-------
           (2)  The ammonium-based sulfite pulp segment



consists of papergrade sulfite mills where pulp and paper



are produced using an acidic cooking liquor of ammonium



sulfite, unless those mills are specialty grade sulfite



mills;                                               .



           (3)  The specialty grade sulfite pulp segment



consists of those papergrade sulfite mills where a



significant portion of production is characterized by pulp



with a high percentage of alpha cellulose and high



brightness sufficent to produce end products such as plastic



molding compounds, saturating and laminating products, and



photographic papers.  The specialty grade segment also



includes those mills where a major portion of production is



91 ISO brightness and above.



§ 430.52  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




      (a)  Except as provided in 40 CFR 125.30 through



125.32, any existing point source subject to this subpart



must achieve the following effluent limitations representing



the degree of effluent reduction attainable by the



application of the best practicable control technology



currently available (BPT):
                             896

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                           Subpart E
             [Bisulfite  liquor/surface condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH.
BPT effluent limitations for
papergrade sulf ite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
31.8
43.95
(x)
Average of daily
values for 30
consecutive days
16.55
23.65
H
Non- continuous
dischargers
(Annual Average)
9.30
12.99
(l.)
Within the .range of 5 . 0 to 9.0 at all times.
                           Subpart E
           [bisulfite liquor/barometric  condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent .limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
. 34.7
52.2
H
Average of daily
values for 30
consecutive days
18.05
28.1
(J)
Non - cont inuous
dischargers
(Annual Average)
10.14
15.44
(l)
•"•Within the range of 5 . 0 • to 9.0 at all  times .
                              897

-------
                            Subpart E
           [Acid  sulfite liquor/surface condensers]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
32.3
43.95
(l)
Average of daily
values for 30
consecutive days
16.8
23.65
t1)
Non- continuous
dischargers
(Annual Average)
9.44
12.99
(a)
*Within the range of 5.0 to 9.0 at all  times.

                           Subpart E
         [Acid sulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
. 35.55
52.2
(')
Average of daily
values for 30
consecutive days
18.5
28.1
H
Non-continuous
dischargers
(Annual Average)
10.39
15.44
(l)
lWithin the range of 5.0 to 9.0 at all times.
                               898

-------
                             Subpart E
              [Bisulfite  liquor/surface  condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1, 000 Ib) of product
Continuous dischargers
Maximum for any 1
day
26.7
43.95
(x)
Average of daily
values for 30
consecutive days
13.9
23.65
C1)
Non-continuous
dischargers
(Annual Average)
7.81
12.99
(x)
^Within the range of 5.0 to 9.0 at all times.
Note:   Limitations above do not apply to mills using continuous
digesters.

                             Subpart  E
            [bisulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
.TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.4
52.2
H
Average of daily
values for 30
consecutive days
15.3
28.1
t1)
Non- continuous
dischargers
(Annual Average)
8.60
15.44
t1)
       the range  of 5.0 to 9.0 at all times.
Note:   Limitations above do not apply to mills using continuous
digesters.
                                899

-------
                             Subpart  E
            [Acid sulfite liquor/surface  condensers]
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash, pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.75
43.95
(l)
Average of daily
values for 30
consecutive days
15.5
23.65
(l)
Non- continuous
dischargers
(Annual Average)
8.71
12.99
P)
Within the range of  5.0 to 9.0 at all times.
Note:   Limitations above do not apply to mills using continuous
digesters.

                             Subpart E
          [Acid sulfite liquor/barometric condensers]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where vacuum, or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
32.5
52.2
(l)
Average of daily
values for 30
consecutive days
16.9
28.1
(l)
Non- continuous
dischargers
(Annual Average)
9.49
15 .44
P)
Within the range of  5.0 to 9.0 at all times.
Note:   Limitations above do not apply to mills using continuous
digesters.
                                900

-------
                          Subpart E
                    [Continuous digesters]
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for papergrade sulfite facilities
where vacuum, or pressure drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
38.15
53.75
(x)
Average of daily
values for 30
consecutive days
19.85
28.95
t1)
Non- continuous
dischargers
(Annual Average)
11.15
15.91
(*)
Within,the range of 5.0 to 9.0 at all times.

      (b)  The following limitations establish  the  quantity

or quality of pollutants  or pollutant properties,  controlled

by this section, resulting from the use of wet barking

operations, which may be  discharged by a point source

subject to the provisions of this subpart.  These

limitations are in addition to  the limitations set forth in

paragraph  (a) of this section and shall be calculated  using

the proportion of the mill's total production  due  to use of

logs which are subject to such  operations:
                             901

-------
                           Subpart  E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulf ite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
2.7
7.5
(l)
Average of daily
values for 30
consecutive days
1.45
3.95
n
Non - cont inuous
dischargers
(Annual Average)
0.80
2.19
(i)
JWithin the range of 5.0 to 9.0 at all times.




                          Subpart  E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
3.05
7.5
(l)
Average of daily
values for 30
consecutive days
1.6
3.95
H
Non -cont inuous
dischargers
(Annual Average)
0.90
2.19
(x)
Within the range of 5.0 to 9.0 at all times.




      (c)  The following limitations establish the quantity



or quality of pollutants or pollutant parameters, controlled



by this section,  resulting from the use of log washing or



chip washing operations,  which may be discharged by a point



source subject to the  provisions of this subpart. These



limitations are  in addition to the limitations set forth in
                              902

-------
paragraph (a)  of this section and shall be calculated using



the proportion of the mill's total production, due to use of



logs  and/or  chips which are  subject to such operations:



                          Subpart E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
2.55
C1)
Average of daily
values for 30
consecutive days
0.1
1.35
(a)
Non- continuous
dischargers
(Annual Average)
0.05
0.75
, (x)
^Within the range of 5.0 to  9.0 at all times.
                          Subpart E
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 >lb) of product
Continuous dischargers
Maximum for any 1
day
0.35
2.55
t1)
Average of daily
values for 30
consecutive days
0.2
' 1.35
(a)
xwithin the range of 5.0 to 9.0 at all times .
Non- continuous
dischargers
(Annual Average)
O.l
0 .75
(l)'

      (d)  The following limitations  establish the quantity



or quality of pollutants or pollutant properties,  controlled



by this section, resulting from the  use  of  log'flumes or log
                             903

-------
ponds, which may be discharged by a point source  subject  to



the provisions  of this subpart.  These limitations  are  in



addition to  the limitations set forth in paragraph  (a)  of



this section and shall be calculated using the proportion of



the mill's total production due to use of logs which  are



subject to such operations:



                          Subpart  E
Pollutant
• or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where blow pit washing
techniques are used
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.35
1.7
(x)
Average of daily
values for 30
consecutive days
0.2
0.9
(l)
Non- continuous
dischargers
(Annual Average)
0.1
0.5
t1)
lWithin the range of 5.0 to 9.0 at all times.
                          Subpart  E
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
papergrade sulfite facilities where vacuum or pressure
drums are used to wash pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.7
1.70

-------
 §  430.53   Effluent  limitations  representing the  degree  of




 effluent  reduction  attainable by the  application of  the best




 conventional pollutant  control  technology  (BCT).




     Except as provided in  40 CFR 125.30 through 125.32, any



 existing  point source subject to this subpart must achieve




 the following effluent  limitations representing  the  degree



 of effluent reduction attainable by the application  of  the



 best conventional pollutant control technology  (BCT).   The



 limitations shall be the  same as those specified for



 conventional pollutants in  § 430.52 of this  subpart  for the



 best practicable control  technology currently available



 (BPT).




 § 430.54  Effluent limitations representing  the degree of




 effluent  reduction  attainable by the  application  of  best




 available  technology economically achievable (BAT).




     Except as provided in 40 CFR 125.30 through  125.32, any



 existing point source subject to  this  subpart must achieve



 the following effluent  limitations representing the  degree



 of effluent reduction attainable  by the application  of  the



best available technology economically achievable (BAT).



     (a)   (1)   The  following effluent  limitations apply to



all dischargers in  the  calcium-,  magnesium-, or sodium-based



 sulfite pulp segment:
                             905

-------
                            Subpart E
 Production of Calcium-,  Magnesium-,  or Sodium-based  Sulfite
                              Pulps
Pollutant
or
pollutant
property
AOX
COD
BAT effluent limitations
Continuous dischargers
Maximum for
any 1 day
Monthly
Average
Non- continuous dischargers
Maximum for
any 1 day
Annual
average
kg/kkg (or pounds per 1,000 Ib) of product

-------
Subpart E- -Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa •
TCDFa
Chloroform8
Trichlorosyringol3
3 , 4 , 5 - trichlorocatechol3
3,4, 6-trichlorocatechola
3,4, 5-trichloroguaiacola
3,4,6- trichloroguaiacol3
4,5, 6- trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenola

AOX
COD
BAT effluent limitations
Maximum for any
1 day

-------
      the particular "pollutant.
      This regulation does not specify this type of limitation for this
      pollutant;'however, permitting authorities may do so as
      appropriate.
      [Reserved].
                 (ii)   The following effluent  limitations

apply  to all dischargers in the  ammonium-based sulfite pulp

segment  with respect  to each fiber line that uses

exclusively TCP bleaching processes,  as disclosed by the

discharger in its NPDES permit application under 40 CFR

122.21(g)(3) and certified under 40 CFR 122.22:

   Subpart E - Production of Ammonium-based  Sulfite Pulps
Pollutant or
pollutant
property
AOX
COD
BAT effluent limitations (TCP)
Continuous dischargers
Maximum for
any 1 day
Monthly
average
Non-continuous
dischargers
Maximum for
any 1 day
Annual
Average
kg/kkg (or pounds per 1000 Ib) of product

-------
Subpart E--Production of  Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Chloroform3
Trichlorosyringol3
3,4,5 -,trichlorocatechola
3,4, 6-trichlorocatechola
3,4,5 - trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2 , 4 , 5 - trichlorophenol3
2,4, 6 - trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6 - tetrachlorophenola
Pent achl or opheno la
f
AOX
COD
BAT effluent limitations
Maximum for any
1 day

-------
b     "
-------
using these  compounds as biocides.  Also, for non-continuous



dischargers,  concentration limitations  (mg/1) shall  apply.



Concentration limitations will only apply to non-continuous



dischargers::



                          Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental BAT effluent limitations
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 Ib) of
product
0.00058exp(0. 017x)
0.0036exp(0.017x)
Milligrams /liter
( (0.011) (12.67)exp(0.017x) ) /y
( (0.068) (12.67)exp(.0.017x) ) /y
x = percent sulfite pulp in final product
y = wastewater discharged in kgal per ton of product
      (c)  Pursuant to 40 GFR 122.44(i) and 122.45(h), a



discharger must demonstrate compliance with the limitations



in paragraphs  (a)(2) or  (a)(3) of this section, as



applicable, by monitoring for all pollutants  (except for AOX



and COD) at the point where the wastewater containing those



pollutants leaves the bleach plant.  The permitting



authority may impose effluent limitations and/or monitoring



requirements on internal wastestreams for any other



pollutants covered in this section as appropriate under 40



CFR 122.44 (i) and 122.45(h).




§ 430.55  New source performance standards (NSPS).




     New sources subject'to this subpart must achieve the



following new source performance standards (NSPS), as
                             911

-------
applicable.



      (a)  The following  standards apply to each new source



regardless of when it  commenced discharge:



                          Subpart E
Pollutant
or
pollutant
property
BODS
TSS
PH
1982 NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
4.38exp(0.017x)
5.81exp(0.017x)
(l) .
Average of daily
values for 30
consecutive days
2.36exp(0.017x)
1 3.03exp(0.017x)
(l)
Non- continuous
dischargers
(Annual Average )
Average of daily
values for 30
consecutive days
divided by 1.91
Average of daily
values for 30
consecutive days
divided by 1.90
f1)
x = percent sulfite pulp in final product
Within the range of 5.0 to 9.0 at all times.






      (b)  The following  standards  apply with respect to each



new source fiber line that  commences discharge after [insert




date  60 days from publication] .




           (1)  The following standards apply to all new



sources in the calcium-,  magnesium-, or sodium-based sulfite



pulp  segment:
                             912

-------
                            Subpart E
 Production of Calcium-,  Magnesium-, or  Sodium-based Sulfite
                              Pulps
Pollutant
or
pollutant
property
AOX
COD
NSPS
Continuous dischargers
Maximum for
any 1 day
Monthly
Average
Non-continuous dischargers
Maximum for
any 1 day
Annual
average
kg/kkg (or pounds per 1,000 Ib) of product

-------
Subpart E--Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDF"
Chloroform*
Trichlorosyringol"
3,4, 5-trichlorocatechola
3,4, 6-trichlorocatechola
3,4,5 -trichloroguaiacol3
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol*
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3

AOX
COD
NSPS
Maximum for any
1 day

-------
      40 CFR 122.22.
b     "
-------
Subpart E--Production of Specialty Grade  Sulfite  Pulps
Pollutant
.or
pollutant property
TCDDa
TCDF"
Chloroform3
Trichlorosyringol3
3,4, 5 - trichlorocatechol3
3,4, 6-trichlorocatechola
3,4,5 - trichloroguaiacola
3,4, 6- trichloroguaiacol3
4,5, 6 -trichloroguaiacol1
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol
2,3,4, 6- tetrachlorophenol3
Pentachlorophenol3

AOX
COD
NSPS
Maximum for any
1 day

-------
 b     "
-------
dischargers, concentration limitations  (mg/1) shall apply.



Concentration limitations will only apply to non-continuous



dischargers:



                          Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Tr i chlorophenol
Supplemental NSPS
Maximum for any 1 day
kg/kkg =
(or pounds per
1,000 Ib) of
product
0.00058exp(0.017x)
0.0036exp(0.017x)
Milligrams/liter
( (0.015) (9.12)exp
( (0.094) (9.12)exp
(0.017x) )/y
(0.017x) )/y
x = percent sulfite pulp in final product
y =s wastewater discharged in kgal per ton of product
      (d)  Pursuant to 40 CFR 122.44(i) and 122.45(h), a



discharger must demonstrate compliance with the standards in



paragraphs  (b)(2) or  (b)(3) of this section, as applicable,



by monitoring  for all pollutants  (except for AOX, COD, BOD5/



TSS, and pH) at the point where the wastewater containing



those pollutants leaves the bleach plant.  The permitting



authority may  impose effluent limitations and/or monitoring



requirements on internal wastestreams for any other



pollutants covered in this section as appropriate under 40



CFR 122.44 (i)  and 122.45(h).



§ 430.56 Pretreatment standards for existing sources  (PSES)„




     Except as provided in 40 CFR 403.7 and 403.13, any



existing source subject to this subpart that introduces



pollutants into a publicly owned  treatment works must:




                             918

-------
comply with 40 CFR part 403; and achieve the following



pretreatment standards for existing sources  (PSES).



     (a)  The following pretreatment standards must be



attained on or before  [insert date 3 years from publication




date] .




          (1)   The following pretreatment standards apply to



all indirect dischargers in the calcium-,, magnesium-, or



sodium-based sulfite pulp segment:
                             919

-------
                            Subpart  E
 Production of Calcium-,  Magnesium-,  or Sodium-based Sulfite
                              Pulps
Pollutant
or
pollutant
property
AOX
PSES
Maximum for any 1 day
Monthly Average
kg/kkg (or pounds per 1,000 Ib) of product

-------
    Subpart E--Production of Ammonium-based Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringola
3,4, 5 -trichlorocatechola
3,4, 6-trichlorocatechola
3,4, 5 - trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechola
Tetrachloroguaiacola
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
PSES
Maximum for any
1 day

-------
40 CFR 403.12 (b)  that  it  uses exclusively TCP bleaching

processes at that fiber line:

   Subpart  E  -  Production of  Ammonium-based Sulfite Pulps
Pollutant or
pollutant
parameter
AOX'
PSNS (TCP)
Maximum for any 1 day

-------
            (3)(i)   The following pretreatment  standards apply

to all indirect dischargers  in the specialty  grade  sulfite

pulp  segment:

   Subpart E--Production of  Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringol3
3,4, 5 - trichlorocatechol3
3 , 4 , 6-trichlorocatechola
3,4, 5-trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5, 6-trichloroguaiacola
2,4, 5-trichlorophenola
2, 4, 6-trichlorophenola •
Tetrachlorocatechola
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pent achl oropheno la
PSES
Maximum for any
1 day

-------
apply with respect to each fiber line  operated by an

indirect  discharger producing specialty grade sulfite pulps

if the  indirect discharger discloses to the pretreatment

control authority in a report submitted under 40 CFR

403.12(b)  that it uses exclusively TCP bleaching processes

at that fiber line.  These pretreatment standards must be

attained  on or before [insert date 3 years  from publication

date]:

                           Subpart E
Pollutant or
pollutant
parameter
AOX
PSES (TCP)
Maximum for any 1 day

-------
                          Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSES
Maximum for any . 1 day
kg/kkg
(or pounds per
1,000 -Ib) of
product
0.00058exp(0.017x)
0.0043exp(0.017x)
Milligrams /liter
( (0.011) (12.67)
( (0.082) (12.67)
exp (0. 017x) ) /y
exp(0.017x) ) /y
x = percent sulfite pulp in final product
y = wastewater discharged in kgal per ton of product
      (c)  An indirect discharger must demonstrate compliance



with the pretreatment standards in paragraphs  (a)(2) or



(a)(3) of this section, as applicable, by monitoring for  all



pollutants at the point where the wastewater containing



those pollutants leaves the bleach plant.
                             925

-------
§ 430.57 Pretreatment standards for new sources (PSNS).

     Except  as  provided in 40 CFR 403.7,  any new source

subject to this subpart that introduces pollutants into a

publicly owned  treatment works must:  comply with 40 CFR part

403; and achieve the following pretreatment standards  for

new sources  (PSNS).

      (a)   (1)   The following pretreatment standards apply  to

each indirect discharger in the calcium-,  magnesium-,  or

sodium-based sulfite pulp segment that  is a new source:

                           Subpart  E
 Production of Calcium-, Magnesium-,  or Sodium-based Sulfite
                             Pulps
Pollutant
or
pollutant
property
AOX
PSNS
Maximum for any 1 day
Monthly Average
kg/kkg (or pounds per 1,000 Ib) of product

-------
      Subpart E--Production of  Ammonium-based  Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringol3
3,4, 5-trichlorocatechola
3 , 4 , 6 - trichlorocatechol3
3 , 4 , 5 - trichloroguaiacola
3,4, 6-trichloroguaiacola
4,5,6 - trichloroguaiacol3
2,4, 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechol3
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
PSNS
Maximum for any
1 day

-------
pretreatment control  authority in  a report submitted under

40 CFR 403.12(b) that it uses exclusively TCP bleaching

processes at that  fiber line:

   Subpart  E  - Production of Ammonium-based Sulfite Pulps
Pollutant or
pollutant
parameter
AOX
PSNS (TCP)
Maximum for any 1 day

-------
    Subpart  E--Production  of Specialty Grade Sulfite Pulps
Pollutant
or
pollutant property
TCDDa
TCDFa
Trichlorosyringol3
3,4,5- trichlorocatechol3
3,4,6 -trichlorocatechola
3,4, 5-trichloroguaiacola
3,4, 6-trichloroguaiacola
4, 5, 6-trichloroguaiacola
2 , 4 , 5-trichlorophenola
2,4, 6-trichlorophenola
Tetrachlorocatechola
Tetrachloroguaiacol3
2,3,4, 6-tetrachlorophenola
Pentachlorophenol3
PSNS
Maximum for any
.1 day

-------
pulps  if  the indirect discharger  discloses to the

pretreatment control authority  in a report submitted under

40 CFR 403.12(b)  that it uses exclusively TCP bleaching

processes at that fiber line:

  Subpart E - Production of Specialty Grade Sulfite Pulps
Pollutant or
pollutant
parameter
AOX
PSNS • (TCF)
Maximum for any 1 day

-------
                          Subpart E
Pollutant or
pollutant
property
Pentachlorophenol
Trichlorophenol
Supplemental PSNS
Maximum for any 1 day
kg/kkg
(or pounds per
1,000 lb) of
product
0.00058exp(0.017x)
0.0043exp(0.017x)
Milligrams /liter
( (0.015) (9.12)exp
( (0.114) (9.12)exp
(0.017x) )/y
(0.017x) )/y
x = percent sulf ite pulp in final product
y = wastewater discharged in kgal per ton of product
      (c)  An indirect discharger must demonstrate compliance



with the pretreatment standards in paragraphs  (a)(2) or



 (a)(3) of this section, as applicable, by monitoring for all



pollutants at the point where the wastewater containing



those pollutants leaves the bleach plant.



§ 430.58 Best management practices (BMPs).




     The definitions and requirements set forth in 40 CFR



430.03 apply to facilities in this subpart.



Subpart F--Semi-Chemical Subcategory




§ 430.60  Applicability; description of the semi-chemical




subcategory.




     The provisions of this subpart are applicable to



discharges resulting from the integrated production of pulp



and paper at semi-chemical mills.
                            931

-------
§ 430.61  Specialized definitions.




     For the purpose of this subpart, the general



definitions, abbreviations, and methods of  analysis  set



forth in 40 CFR part 401 and § 430.01 of this part shall



apply to this subpart.



§ 430.62  Effluent limitations representing the degree of




effluent reduction attainable by the application of  the best




practicable control technology currently available  (BPT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart must achieve



the following effluent limitations representing the  degree



of effluent reduction attainable by the application  of the



best practicable control technology currently available




(BPT) :



                          Subpart F
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations
ammonia base mills
Kg/kkg (or pounds per 1,000 Ib)
Maximum for any 1 day
8.0
10.0
H
for
of product
Average of daily values for
30 consecutive days
4.0
5.0
(*)
aWithin the range of 6.0 to 9.0 at all times.
                             932

-------
                           Subpart F
Pollutant
or
pollutant
property
BODS
TSS
PH .
BPT effluent limitations
sodium base mills
Kg/kkg (or pounds per 1,000 Ib)
Maximum for any 1 day
8.7
11.0
n
for
of product
Average of daily values for
30 consecutive days
4.35
5.5
(l)
       tne range or 6.0 to 9.0 at all times.

 § 430.63  Effluent limitations guidelines representing the

 degree of effluent reduction attainable by the application
k
 of the best conventional pollutant control technology (BCT).

     Except as provided in 40 CFR 125.30 through 125.32,  any

 existing point source subject to this subpart shall achieve

 the following effluent limitations representing the degree

 of effluent reduction attainable by the application of the

 best conventional pollutant control technology (BCT):  The

 limitations shall be the same as those specified for

 conventional pollutants (which are defined in 40 CFR 401.16)

 in § 430.62 of this subpart for the best practicable control

 technology currently available (BPT),  except that non-

 continuous dischargers shall not be subject to the maximum

 day and average-of-30-consecutive-days limitations,  but

 shall be subject to annual  average effluent limitations

 determined by dividing the-average-of-30-consecutive-days

 limitations for BODS by 1.36 and TSS by 1.36.
                             933

-------
§ 430.64  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




available technology economically achievable (BAT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart where



chlorophenolic-containing biocides are used must achieve the



following effluent limitations representing the degree of



effluent reduction attainable by the application of the best



available technology economically achievable (BAT). Non-



continuous dischargers shall not be subject to the maximum



day mass limitations in kg/kkg  (lb/1000 Ib),  but shall be



subject to concentration limitations.  Concentration



limitations are only applicable to non-continuous



dischargers.  Permittees not using chlorophenolic-contairiing



biocides must certify to the permit-issuing authority that



they are not using these biocides:



                          Subpart  F
Pollutant or
pollutant property
Pentachlorophenol
Tr i chl orophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0012
0.00043
Milligrams /liter
(0.029) (10.3) /y
(0.010) (10.3) /y
y = wastewater discharged, in kgal per ton of product
§ 430.65  New source performance standards  (NSPS) .




     Any new source subject to this subpart must achieve the
                             934

-------
following new:source performance standards  (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BODS and TSS, but shall be subject to annual



average effluent limitations.  Also, for non-continuous



dischargers, concentration limitations  (mg/1)  shall apply,



where provided.  Concentration limitations will only



apply to non-continuous dischargers.  Only facilities where



chlorophenolic-containing biocides are used shall be subject



to pentachlorophenol and trichlorophenol limitations.



Permittees not using chlorophenolic-containing biocides must



certify to the permit-issuing authority that they are not



using these biocides:
                             935

-------
                          Subpart F
Pollutant or
pollutant property
BOD5
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for • any 1
day
3.0
5.8
(i )
Average of
daily
values for
30
consecutive
days
1.6
3.0
(1 )
Non- continuous
Dischargers
(Annual Average)
0.84
1.6
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0012
0.00043
Milligrams/liter
(0.041) (7.3)/y
(0.014) (7.3)/y
y = wastewater discharged in kgal per ton at all times
lWithin the range of 5.0 to 9.0 at all times.




§ 430.66  Pretreatment standards for existing  sources




(PSES).




     Except as provided in 40 CFR 403.7 and 403.13,  any



existing source  subject to this  subpart that introduces



pollutants into  a publicly owned treatment works  must:



comply with 40 CFR part 403; and achieve the following



pretreatment standards for existing  sources  (PSES)  if it



uses chlorophenolic-containing biocides.  Permittees not



using chlorophenolic-containing biocides must  certify to  the
                             936

-------
permit-issuing authority that they are not using these

biocides.   PSES must be attained on or before  July 1,  1984:

                          Subpart  F
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligrams/ liter
(0.032) (10.3)/y
(0.010) (10.3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0 . 0014
0.00043
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance-in
cases when POTWs find it necessary to impose mass equivalent
limitations.

§430.67  Pretreatment  standards for new sources  (PSNS).

      (a)  Except  as provided in 40 CFR 403.7,  any new source

subject to  this subpart that introduces pollutants  into a

publicly  owned treatment works must: comply with 40  CFR part

403; and  achieve  the following pretreatment standards for

new sources  (PSNS) if it uses chlorophenolic-containing

biocides.   Permittees not using chlorophenolic-containing

biocides  must  certify to the permit-issuing authority that

they are  not using these biocides:
                             937

-------
                          Subpart F
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/ liter
(0.045) (7. 3)/y
(0.014) (7.3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0014
0.00043 .
y = wastewater discharged in kgal per ton of product
• The following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to impose mass equivalent   |
limitations.

Subpart  G-Mechanical Pulp Subcategory

§ 430.70  Applicability;  description of the mechanical pulp


subcategory.

     The  provisions  of this  subpart are applicable to

discharges resulting from:  the production of pulp and paper

at groundwood  chemi-mechanical mills;  the production of pulp

and paper at groundwood mills through the application of the

thermo-mechanical process;  the integrated production of pulp

and coarse paper, molded  pulp products, and newsprint at

groundwood mills; and the integrated production of pulp and

fine paper at  groundwood  mills.

§ 430.71  Specialized definitions.

     For  the purpose of this subpart,  the general

definitions, abbreviations,  and methods of analysis set

forth in  40  CFR part 401  and §430.01 of this part shall
                             938

-------
apply  to  this  subpart.




§ 430.72   Effluent limitations representing the degree of




effluent  reduction attainable by the application of the best




practicable  control technology currently available (BPT).




      (a)   Except  as provided in 40  CFR 125.30  through



125.32, any  existing point  source subject to this subpart



must achieve the  following  effluent limitations representing



the degree of  effluent  reduction attainable by,the



application  of the best practicable control technology



currently available (BPT),  except that non-continuous



dischargers  shall  not be  subject to the maximum day and



average of 30  consecutive days limitations  but  shall  be



subject to annual  average effluent  limitations:



                          Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
13.5
19.75
C1)
Average of daily
values for 30
consecutive days
7.05
10.65
H
Non-continuous
dischargers
(Annual Average)
3.96
5.85
(x)
•'Withxn the range of 5.0 to 9.0 at all times.
                             939

-------
                             Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
10.6
15.55
P)
Average of daily
values for 30
consecutive days
5.55
8.35
(M
Non- continuous
dischargers
(Annual Average)
3.12
4.59
(*)
Within the range of 5.0  to  9.0 at all times.




                             Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
7.45
12.75
t1)
Average of daily
values for 30
consecutive days
3.9
6.85
(l)
Non- continuous
dischargers
(Annual Average)
2.19
3.76
(*)
Within the range of 5.0 to 9.0 at all times.
                                 940

-------
                          Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
6.85
11.75
t1) .
Average of daily
values for 30
consecutive days
3.6
S.3
(M
Non- continuous
dischargers
(Annual Average)
2.0
3.5
t1)
      (b)  The following limitations establish the quantity

or quality of pollutants or pollutant properties, controlled

by this section, resulting from the use of wet barking

operations, which may be discharged by a point source

subject to the provisions of this subpart.   These
                                              i
limitations are in addition to the limitations set forth in

paragraph  (a)  of this section and shall be calculated using

the proportion of the mill's total production due to use of

logs which are subject to such operations.   Non-continuous

dischargers shall not be subject to. the maximum day and

average of 30 consecutive days limitations,  but shall be

subject to annual average effluent limitations:
                            941

-------
                              Subpart  G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.9
2'. 6
(l)
Average of daily
values for 30
consecutive days
0.45
1.45
(l)
Non-continuo\is
dischargers
(Annual Average)
0.25
0 .80
H
xWithin the range of 5.0 to 9.0  at all times.




                             Subpart  G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo -mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.9
2.7
(a)
Average of daily
values for 30
consecutive days
0.45
1.45
(*)
Non- continuous
dischargers
(Annual Average)
0.3
0 .75
H
xWithin the range of 5.0 to 9.0  at all times.
                                 942

-------
                           Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1.15
2.0
C1)
Average of daily
values for 30
consecutive days
0.55
1.1
H
Non- continuous
dischargers
(Annual Average)
0.30
0.60
C1)
'•Within the range of 5.0 to 9.0 at all times,
                           Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for '
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1.1
1.95
H
Average of daily
values for 30
consecutive days
0.55
1.1
n
Non - cont inuous
dischargers
(Annual Average)
0.35
0. 60
t1)
^•Within the range of 5.0  to 9.0  at all times.






      (c)  The following limitations  establish the quantity




or quality  of pollutants or pollutant  parameters, controlled




by this  section,  resulting from the  use  of log washing or




chip washing operations, which  may be  discharged by a point
                              943

-------
source subject to the provisions of  this  subpart.   These



limitations are in addition to  the limitations  set  forth in



paragraph  (a) of this section and shall be  calculated using



the proportion of the mill's total production due to  use of



logs and/or chips which are subject  to such operations.  Non-



continuous dischargers shall not be  subject to  the  maximum



day and average of 30 consecutive days limitations, but



shall be subject to the annual  average effluent limitations:



                          Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.05
0.25
(*)
Average of daily
values for 30
consecutive days
0.05
0.15
H
Non- continuous
dischargers
(Annual Average)
0.05
0.10
(l>
^•Within the range of 5.0 to 9.0 at all times.
                             944

-------
                      Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo -mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.05
0.30
H
Average of daily
values for 30
consecutive days
. 0.05
- 0 . 15
P)
Non-continuous
dischargers
(Annual Average)
0.05
0.05
t1)
the range of  5.0 to 9.0 at all times.




                      Subpart  G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded' pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.20
t1)
Average of daily
values for 30
consecutive days
0.05
0 .15
C1)
Non- continuous
dischargers
(Annual Average)
0.05
0.10
H
the range of 5.0 to 9.0 at  all times.
                         945

-------
                          Subpart G
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.2
C1)
Average of daily
values for 30
consecutive days
0.05
0.15
H
Non- continuous
dischargers
(Annual Average )
0.05
0.10
(l)
JWithin the range of 5.0 to 9.0 at all times.






      (d)  The following limitations establish the quantity



or quality of pollutants or pollutant properties, controlled



by this section, resulting from the use of log flumes or  log



ponds, which may be discharged by a point source subject  to



the provisions of this subpart.  These limitations are  in



addition to the limitations set forth in paragraph  (a)  of



this section and shall be calculated using the proportion of



the mill's total production due to use of logs which are



subject to such operations.  Non-continuous dischargers



shall not be subject to the maximum day and average of  30



consecutive days limitations but shall be subject to the



annual average effluent limitations:
                             946

-------
                              Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0.55
C1)
Average of daily
values for 30
consecutive days
0.05
0.3
(*)
Non- continuous
dischargers
(Annual Average)
0. 05
0.15
t1)
^Within the range of 5.0 to 9.0  at  all times.




                             Subpart  G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.15
0 .60
H
Average of daily
values for 30
consecutive days
0.15
0.35
P)
Non- continuous
dischargers
(Annual Average)
0.05
0.15
P)
^within the range of 5.0 to  9.0 at all times.
                                 947

-------
                           Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp' products, and
newsprint at groundwood mills occurs ',
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.25
0.45
(l)
Average of daily
values for 30
consecutive days
0.1
0.25
t1)
Non- continuous
dischargers
(Annual Average)
0 .05
0.15
(*)
xWithin the range of 5.0 to 9.0 at all times.
                           Subpart G
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0 .2
0.4
(l)
Average of daily
values for 30
consecutive days
0.05 '
0.25
(l)
Non- continuous
dischargers
(Annual Average)
0.05
0.15
(l)
xWithin the range of 5.0 to 9.0  at all times.






      (e)    For  those mills using zinc hydrosulfite as a



bleaching agent in the manufacturing process,  the following



effluent limitations are to be added to  the  base limitations



set forth in paragraph  (a)  of this section.   Permittees not
                              948

-------
using zinc hydrosulfite as a bleaching agent must certify to



the permit issuing authority that they are not using this



bleaching compound.  Non-continuous dischargers shall not be



subject to the maximum day and average of 30 consecutive



days effluent limitations, but shall be subject to annual



average effluent limitations:



                          Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood chemi -mechanical mills -are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.34
Average of daily
values for 30
consecutive days
0.17
Non- continuous
dischargers
(Annual Average)
0.11
                         Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where pulp and paper at
groundwood mills are produced through the application of
the thermo -mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.26
Average of daily
values for 30
consecutive days
0.13
Non- continuous
dischargers
(Annual Average)
0.09
                            949

-------
Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and coarse paper, molded pulp products, and
newsprint at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.30
Average of daily
values for 30
consecutive days
0.15
Non- continuous
dischargers
(Annual Average)
0.10
Subpart G
Pollutant
or
pollutant
property
Zinc
BPT effluent limitations for
mechanical pulp facilities where the integrated production
of pulp and fine paper at groundwood mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
0.275
Average of daily
values for 3 0
consecutive days
0.135
Non- continuous
dischargers
(Annual Average)
0.090
   950

-------
§ 430.73  Effluent limitations guidelines representing the




degree of effluent reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




      (a) (1)  The following applies to:  mechanical pulp



facilities where the integrated production of pulp and



coarse paper, molded pulp products, and newsprint at



groundwood mills occurs; and mechanical pulp facilities



where the integrated production of pulp and fine paper at



groundwood mills occurs:



      (2)  Except as provided in.40 CFR 125.30 through .




125.32, any existing point source subject to this subpart



shall achieve the following effluent limitations



representing the degree of effluent reduction attainable by



the application of the best conventional pollutant control



technology (BCT) :. The limitations shall be the same as those



specified for conventional pollutants (which are defined in



40 CFR 401.16)  in § 430.72 of this subpart for the best



practicable control technology currently available (BPT).



      (b)  The following applies to mechanical pulp



facilities where pulp and paper at groundwood chemi-



mechanical mills are produced'and mechanical pulp facilities




where pulp and paper at groundwood mills are produced




through the application of the thermo-mechanical process:



[Reserved]




§ 430.74  Effluent limitations representing the degree of






                             951

-------
effluent reduction attainable by the application of the best     j^t

                                                                 9
available technology economically achievable  (BAT).



      (a)  The following applies to mechanical pulp


facilities where pulp and paper at groundwood mills are


produced through the application of the thermo-mechanical


process; mechanical pulp facilities where the integrated


production of pulp and coarse paper, molded pulp products.,


and newsprint at groundwood mills occurs; and mechanical


pulp facilities where the integrated production of pulp and


fine paper, at groundwood mills occurs:  (1)  Except as


provided in 40 CFR 125.30 through 125.32, any existing point


source subject to this subpart must achieve the following


effluent limitations representing the degree of effluent         Jttfe,

                                                                 V
reduction attainable by the application of the best              :


available technology economically achievable  (BAT), except


that non-continuous dischargers shall not be subject to the


maximum day mass limitations in kg/kkg  (lb/1000 Ib), but         ;


shall be subject to concentration limitations.


Concentration limitations are only applicable to non-


continuous dischargers.  Pentachlorophenol and •


trichlorophenol limitations are only applicable at               '


facilities where chlorophenolic-containing biocides are


used.  Permittees not using chlorophenolic-containing


biocides must certify to the permit-issuing authority that
                             952

-------
they are not using these biocides.  Zinc limitations are




only applicable at facilities where zinc hydrosulfite is




used as a bleaching agent.  Permittees1 not using zinc




hydrosulfite as „a bleaching agent must certify to the permit




issuing authority that they are not using this bleaching



compound:



                          Subpart  G
Pollutant or
pollutant property
Pentachlorophenol
Tri chl or opheno 1
Zinc
BAT effluent limitations for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo -mechanical process
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00097
0. 00088
0 .26
Milligrams /liter
(0.011) (21.1)/y
(0.010) (21.1)/y
(3.0) (21.1)/y
y = wastewater discharged in kgal per ton of product
                             953

-------
                          Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
BAT effluent limitations for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood mills
occurs
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0011
0.00099
0.30
Milligrams /liter
(0.011) (23.8) /y
(0.010) (23 . 8) /y
(3.0) .(23. 8) /y
y ~ wastewater discharged in kgal per ton of product
                          Subpart G
Pollutant or
pollutant property
Pent achl oropheno 1
Trichlorophenol
Zinc
BAT effluent limitations for
mechanical pulp facilities where the integrated
production of pulp and fine paper at groundwood
mills occurs
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0010
0.00092
0.27
Milligrams /liter
(0.011) (21.9)/y
(0.010) (21.9)/y
(3.0) (21.9)/y :
y = wastewater discharged in kgal per ton of product
      (b)  The following applies to mechanical pulp



facilities where pulp and paper at groundwood chemi-



mechanical mills are produced:




[Reserved]




§ 430.75  New source performance standards  (NSPS).





                             954

-------
      (a)   The following applies to mechanical  pulp




 facilities where pulp and paper at groundwood  mills are




 produced through the application of the  thermo-mechanical



 process;  mechanical  pulp facilities where  the  integrated



 production of pulp and coarse  paper, molded pulp products,



 and newsprint at groundwood mills occurs;  and  mechanical



 pulp facilities  where the integrated production of pulp  and



 fine paper at groundwood mills occurs:  (1)  Any new source



 subject  to this  subpart  must achieve the following new



 source performance standards  (NSPS), except that non-



 continuous dischargers  shall not  be  subject to the maximum



 day and  average  of 30  consecutive days effluent limitations



 for BOD5  and  TSS,  but  shall be subject to  annual average



 effluent  limitations.  Also, for  non-continuous dischargers,



 concentration limitations  (mg/1)  shall apply,  where



 provided.   Concentration limitations will  only apply to  non-



 continuous  dischargers.   Pentachlorophenol and



 trichlorophenol  limitations are only applicable at



 facilities  where chlorophenolic-containing biocides are



used.  Permittees  not using chlorophenolic-containing



biocides must  certify to the permit-issuing authority that



they are not using these biocides.  Zinc limitations are



only applicable at facilities where zinc hydrosulfite is



used as a bleaching agent.  Permittees not using zinc



hydrosulfite as a bleaching agent must certify to the permit



issuing authority that they are not using this  bleaching





                            955

-------
compound:
                             Subpart G
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
Zinc
NSPS for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo-mechanical process
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.6
8.7
0 )
Average of
daily
values for
30
consecutive
days
2 .5
4.6
t1 )
Non- continuous
Dischargers
(Annual Average)
1.3
2.4
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00097
0.00088
0.17
Milligrams/liter
(0.017) (13. 8) /y
(0.015) (13.8)/y
(3.0) (13. 8) /y
y = wastewater discharged in kgal per ton at all times
xWithin the range  of 5.0 to 9.0 at all times.
                                956

-------
                      Subpart G
Pollutant or
pollutant property
BODS
TSS
pH
'

Pentachlorophenol
Trichlorophenol
Zinc
NSPS for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood mills
occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
-. 4.6
7.3
(a )
Average of
daily
values for
30
consecutive
days
2.5
3.8
(* )
Non-continuous
Dischargers
(Annual Average)
1.3
2.0
(l ) '
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
• 0.0011
0.00099
0.21
Milligrams/liter
(0.016) (16.8)/y
(0. 014) (16.8) /y
(3.0) (16.8)/y
y = wastewater discharged in kgal per ton at all times
the range of 5.0 to 9.0 at  all times.
                         957

-------
                          Subpart
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
Zinc
NSPS for
mechanical pulp facilities where the integrated
production of pulp and fine paper at groundwood
mills occurs
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.5
5.8
(l )
Average of
daily
values for
30
consecutive
days
1.9
3.0
r )
Non- continuous
Dischargers
(Annual Average)
0.99
1.58
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0010
0.00092
0.19
Milligrams/ liter
(0.016) (15.4)/y
(0.014) (15.4)/y
(3.0) (15.4)/y
y = wastewater discharged in kgal per ton at all times
*Within the range of 5.0 to 9.0 at all times.




      (b)  The  following applies to mechanical pulp




facilities where pulp and paper at groundwood chemi-




mechanical mills are  produced:                        ;




[Reserved]




§ 430.76  Pretreatment standards for existing sources
(PSES).
      (a)  The  following applies to mechanical pulp
                              958

-------
facilities where pulp and paper at groundwood mills are




produced through the application of the thermo-mechanical



process; mechanical pulp facilities where the integrated



production of pulp and coarse paper, molded pulp products,



and newsprint at groundwood mills occurs; and mechanical



pulp facilities where the integrated production of pulp and



fine paper at groundwood mills occurs: (1)  Except as



provided in 40 CFR 403.7 and 403.13, any existing source



subject to this subpart that introduces pollutants into a



publicly owned treatment works must comply with 40 CFR part



403 and achieve the following pretreatment standards for



existing sources (PSES).  Pentachlorophenol and



trichlorophenol limitations are only applicable at



facilities where chlorophenolic-containing biocides are



used.  Permittees not using chlorophenolic-containing



biocides must certify to the permit-issuing authority that



they are not using these biocides.   Zinc limitations are



only applicable at facilities where zinc hydrosulfite is



used as a bleaching agent.   Permittees not using zinc



hydrosulfite as a bleaching agent must certify to the



permit-issuing authority that they are not using this



bleaching compound.  PSES must be attained on or before July



1, 1984:
                             959

-------
                              Subpart  G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSES for
mechanical pulp facilities where pulp and paper
at groundwood mills are produced through the
application of the thermo -mechanical process
Maximum for any 1 day
Milligrams/ liter
(mg/1)
(0.011) (21.1)/y
(0.010) (21.1)/y
(3.0) (21.1)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00097
0.00088
0.26
y = wastewater discharged in kgal per ton of product
'The  following equivalent mass limitations are provided as guidance in
cases when POTWs find it  necessary  to  impose mass effluent limitations.
                              Subpart  G
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
Zinc
PSES for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded piilp
products, and newsprint at groundwood mills
occurs
Maximum for any 1 day
Milligrams/liter
(mg/1)
(0.011) (23. 8) /y
(0.010) (23.8)/y
(3.0) (23. 8) /y
Kg/kkg (or pounds per 1,000
Ib) of product"
0.0011
0.00099
0.30
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to  impose mass effluent limitations.
                                  960

-------
                           Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSES for
mechanical pulp facilities where the
production of pulp and fine paper at
mills occurs
integrated
groundwood
Maximum for any 1 day
Milligrams/liter
(mg/1)
(0.011) (21.9)/y
(0.010) (21.9)/y
(3.0) (21. 9) /y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.0010
0.00092
0.27
y = wastewater discharged in kgal per ton of product
    roiiowing equivalent mass limitations are provided as guidance in
cases  when POTWs find it necessary to impose mass effluent limitations.


      (b)   The following applies to mechanical  pulp

facilities where pulp and paper at groundwood  chemi-

mechanical mills are produced:

[Reserved]


§ 430.77   Pretreatment standards for new sources (PSNS).

      (a)   The following applies to mechanical  pulp

facilities where pulp and paper at groundwood  mills are

produced  through the application of the thermo-mechanical

process;  mechanical  pulp facilities where the  integrated

production of pulp and coarse paper, molded pulp products,

and newsprint at groundwood mills occurs; and  mechanical

pulp  facilities  where  the integrated production  of pulp and

fine  paper at groundwood mills  occurs: (1)   Except as

provided  in 40 CFR 403.7,  any new sourcessubject to this
                             961

-------
subpart that introduces  pollutants into a publicly owned

treatment works must  comply with 40 CFR part 403 and achieve

the following pretreatment standards for new sources  (PSNS).

Pentachlorophenol  and trichlorophenol limitations are only

applicable at facilities where chlorophenolic-containing

biocides are used.  Permittees not using

chlorophenolic-containing biocides must certify to the

permit-issuing authority that they are not using these

biocides.  Zinc limitations are only applicable at

facilities where  zinc hydrosulfite is used as a bleaching

agent. Permittees  not using zinc hydrosulfite as a bleaching

agent must certify to the permit issuing authority that they

are not using this bleaching compound:

                           Subpart  G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where pulp and papesr
at groundwood mills are produced through the
application of the thermo-mechanical process
Maximum for any 1 day
Milligrams/liter
(mg/1)
(0.017) (13. 8) /y
(0.015) (13.8)/y
(3.0) (13. 8) /y
Kg/kkg (or pounds per 1,000
Ib) of product3
0.00097
0.00088
0.17
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                              962

-------
                             Subpart G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where the integrated
production of pulp and coarse paper, molded pulp
products, and newsprint at groundwood mills
occurs
Maximum for any 1 day
Milligrams/liter
(mg/1)
(0.016) (16.8)/y
(0.014) (16. 8) /y
(3.0) (16.8)/y
Kg/kkg (or pounds per 1,000
Ib) of product3
, 0.0011
0.00099
0.21
y = wastewater discharged in kgal per ton of product
aThe  following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                             Subpart  G
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
Zinc
PSNS for
mechanical pulp facilities where the
production of pulp and fine paper at
mills occurs
integrated
groundwood
Maximum for any 1 day
Milligrams /liter
(mg/1)
(0.016) (15.4)/y
(0.014) (15.4) /y
(3.0) (15.4)/y
Kg/kkg. (or pounds per 1,000
Ib) of product3
0.0010
0.00092
0 . 19
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as  guidance in
cases  when POTWs find it necessary to  impose mass  effluent limitations.
      (b)  The following applies to mechanical pulp

facilities where pulp  and paper at groundwood chemi-

mechanical mills are produced:
                                963

-------
 [Reserved]




Subpart H-Non-Wood Chemical Pulp




§ 430.80  Applicability; description of the non-wood




chemical pulp subcategory.




     The provisions of this subpart are applicable to



discharges resulting from the production of pulp and paper



at non-wood chemical pulp mills.  This subcategory includes,



but is not limited to, mills producing non-wood pulps from



chemical pulping processes such as kraft, sulfite, or socla.



§ 430.81  Specialized definitions.




     The general definitions, abbreviations, and methods of



analysis set forth in 40 CFR 401 and § 430.01 of this part



shall apply to this subpart.



§ 430.82  Effluent limitations representing the degree of




effluent reduction attainable by the application of best




practicable control technology currently available (BPT).




 [Reserved]




§ 430.83  Effluent limitations representing the degree of




effluent reduction attainable by the application of best




conventional pollutant control technology (BCT).     ;




 [Reserved]




§ 430.84  Effluent limitations representing the degree of




effluent reduction attainable by the application of best






                             964

-------
 available technology economically achievable (BAT).




 [Reserved]





 §  430.85  New source performance standards (NSPS)




 [Reserved]





 §  430.86   Pretreatment  standards for existing sources (PSES)




 [Reserved]





 §  430.8-7   Pretreatment  Standards for new  sources  (PSNS) .




 [Reserved]




 Subpart I-Secondary Fiber Deink





 §  430.90  Applicability; description of the





 deink-subcategory.




     The provisions  of  this subpart  are applicable to




 discharges resulting  from the integrated  production  of pulp




 and paper at  deink mills.




 §  430.91  Specialized definitions.





     For the  purpose  of this subpart, the general




 definitions,  abbreviations, and methods of analysis  set




 forth in 40 CFR part  401 and §  430.01 of  this part shall




 apply to this subpart.




 §  430.92  Effluent limitations representing the degree of





 effluent reduction attainable by the application of  the best




practicable control technology currently available (BPT).
                             965

-------
     Except as provided in 40 CFR 125.30 through 125.32, any

existing point source subject to this  subpart must achieve

the following effluent limitations representing the degree

of effluent reduction attainable by the application of the

best practicable control technology currently available

(BPT), except that non-continuous dischargers shall not be

subject to the maximum day and average of 30 consecutive

days limitations but shall be subject  to annual average

effluent limitations:

                          Subpart I
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations -
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
18.1
24.05
(l)
Average of daily
values for 30
consecutive days
9.4
12.95
(l)
Non-continuous
dischargers
(Annual Average)
5.3
7 .12
n
Within the range of 5.0 to 9.0 at all times.

§ 430.93  Effluent  limitations  guidelines representing the


degree of effluent  reduction attainable by  the  application


of the best conventional  pollutant  control  technology  (BCT).


     Except as provided in 40 CFR 125.30 through  125.32,  any
                                                \
existing point source subject to this  subpart shall achieve

the following effluent limitations  representing the-degree

of effluent reduction attainable by the application of the

best conventional pollutant control technology  (BCT) : The:

                             966

-------
 limitations shall be the  same as  those specified  for

 conventional pollutants  (which are defined in 40  CFR  401.16)

 in  § 430.92 of this subpart for the best practicable  control

 technology currently available  (BPT).

 § 430.94  Effluent limitations representing the degree of
                                                            f
 effluent reduction attainable by  the application  of the best

 available technology economically achievable  (BAT).

     Except as provided in 40 CFR 125.30 through  125.32, any

 existing point source subject to  this subpart where

 chlorophenolic-containing biocides are used must  achieve the

 following effluent limitations representing the degree of

 effluent reduction attainable by  the application  of the best

 available technology economically achievable (BAT).  Non-

 continuous dischargers shall not  be subject to the maximum

 day mass limitations in kg/kkg (lb/1000 Ib)  but shall be

 subject to concentration limitations.  Concentration

 limitations are only applicable to non-continuous

dischargers.   Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using these biocides:
                             967

-------
                          Subpart  I
     (Facilities  where  fine  or tissue paper  is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0069
Milligrams/liter
(0.029) (24.4)/y
(0.068) (24.4)/y
y = wastewater discharged in kgal per ton of product
                          Subpart  I
          (Facilities where newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0010
Milligrams/liter
(0.029) (24.4)/y
(0. 010) (24.4) /y
y = wastewater discharged in kgal per ton of product
§ 430.95  New source performance standards  (NSPS).

     Any new source subject to this subpart must achieve the

following new source performance standards  (NSPS), except

that non-continuous dischargers shall not be subject to the

maximum day and average of 30 consecutive days effluent

limitations for BOD5 and TSS, but shall be  subject to annual

average effluent limitations.  Also, for non-continuous

dischargers, concentration limitations  (mg/1) shall apply,
                             968

-------
where provided.  Concentration  limitations will  only apply

to non-continuous dischargers.  Only  facilities  where

chlorophenolic-containing biocides are used  shall  be subject

to pentachlorophenol and trichlorophenol  limitations.

Permittees not using chlorophenolic-containing biocides must

certify to the permit-issuing authority that they  are not

using these biocides:

                          Subpart I
          (Facilities where fine paper is  produced)
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum . for any 1
day
5.7
8.7
(* )
Average of
daily
values for
30
consecutive
days
3.1
4.6
P )
Non -continuous
Dischargers
(Annual Average)
1.6
2.4
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0069
Milligrams /liter
(0.045) (15. 9) /y
(0.104) (15. 9) /y
y = wastewater discharged in kgal per ton at all times
1Wj.thin the range of  5.0 to 9.0 at all times.
                             969

-------
                           Subpart  I
          (Facilities where tissue  paper is produced)
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
9.6
13.1
(x )
Average of
daily
values for
30
consecutive
days
5.2
6.8
0 )
Non- continuous
Dischargers
(Annual Average)
2.72
3.58
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0069
Milligrams /liter
(0.036) (19.5)/y
(0. 085) (19.5) /y
y « wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times.
                              970

-------
                          Subpart I
           (Facilities  where  newsprint  is produced)
Pollutant or,
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
. NSPS
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
' 6.0
12 .0
C1 )
Average of
daily
values for
30
consecutive
days
3.2
6.3
(: )
Non- continuous
Dischargers
(Annual Average)
1.7
3.3
C1 •).
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0010
Milligrams/ liter
(0.044) (16.2)/y
(0.015) (16.2)/y
y = wastewater discharged in kgal per ton at all times
       the range of 5.0 to 9.0 at all times.
§ 430.96  Pretreatment standards for existing sources

(PSES).


      (a)  Except as provided in 40 CFR 403.7 and 403.13,  any

existing source subject to this subpart that introduces

pollutants into a publicly owned treatment works must:

comply with 40 CFR part 403; and achieve the following

pretreatment standards for existing sources  (PSES) if it

uses chlorophenolic-containing biocides.  Permittees not

using chlorophenolic-containing biocides must certify to  the

                             971

-------
permit-issuing authority that they are not  using these

biocides.   PSES must be  attained on or before July 1,' 1984:

                           Subpart  I
     (Facilities  where fine or  tissue paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligrams/liter
mg/1)
(0.032) (24.4)/y
(0.082) (24.4)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0084
y = wastewater discharged in kgal per ton of product
* The following equivalent mass limitations are provided as guidance  in
cases when POTWs find it necessary to impose mass equivalent
limitations.
                           Subpart  I
           (Facilities where newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES
Maximum for any 1 day
Milligrams /liter
mg/1)
(0.032) (24.4)/y
(0.010) (24.4) /y
, Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0010
y = wastewater discharged in kgal per ton of product
• The following equivalent mas limitations are provided as guidance in
cases when POTWs find it necessary to impose mass equivalent.
limitations.
§ 430.97   Pretreatment  standards for new  sources (PSNS).


      (a)   Except as provided in 40 CFR 403.7,  any new source

subject to this subpart that introduces pollutants into a

publicly  owned treatment works must: comply with 40 CFR part

403;  and  achieve the  following pretreatment standards for
                               972

-------
new sources  (PSNS)  if it  uses chlorophenolic-containing

biocides.  Permittees not using chlorophenolic-containing

biocides must  certify to  the permit-issuing authority that

they are not using these  biocides:

                            Subpart I
           (Facilities  where fine paper is produced)
Pollutant or
pollutant property
Pent achloropheno 1
Trichlorophenol
PSNS
, Maximum for any 1 day
Milligrams /liter
rag/1)
(0.049) (15.9)/y
(0.126) {15. 9) /y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0084
y = wastewater discharged in kgal per ton of product
  The following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to 'impose  mass equivalent
limitations.

                            Subpart I
          (Facilities where tissue paper is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/ liter
mg/1)
(0.040) (19.5)/y
(0.103) (19.5)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0.
0.
0033
0084
y = wastewater discharged in kgal per ton of product
 Tne following equivalent mass  limitations are provided as  guidance in
cases when POTWs find it necessary to impose mass equivalent
limitations.
                               973

-------
                          Subpart I
           (Facilities where  newsprint is produced)
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS
Maximum for any 1 day
Milligrams/liter
mg/1)
(0.048) (16.2)/y
(0.015) (16.2)/y
Kg/kkg ( or pounds per
1,000 Ib) of product3
0 .
0.
0033
0010
y = wastewater discharged in kgal; per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to impose mass equivalent
limitations.

Subpart J-Secondary Fiber Non-Deink

§ 430.100  Applicability;  description of the secondary fiber

non-deink sttbcategory.

     The provisions of this  subpart are applicable to

discharges resulting  from the production of: paperboard from

wastepaper; tissue paper from wastepaper without deinking at

secondary fiber mills;  molded products from wastepaper

without deinking  at secondary fiber mills; and builders'

paper and roofing felt from  wastepaper.

§ 430.101  Specialized definitions.

     For the purpose  of this subpart:

      (a)  Except  as provided below, the general definitions,

abbreviations, and methods of analysis set forth in 40 CFR

part 401 and § 430.01 of this part shall apply to this

subpart.

      (b)  Noncorrugating medium furnish subdivision mills
                             974

-------
are mills where recycled corrugating medium is not used in



the production of paperboard.




      (c)  Corrugating medium furnish subdivision mills are



mills where only recycled corrugating medium is used in the



production of paperboard.




§ 430.102  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




      (a)  Except as provided in 40 CFR 125.30 through




125.32, any existing point source subject to this subpart



must achieve the following effluent limitations representing



the degree of effluent reduction attainable by the



application of the best practicable control technology



currently available (BPT):




                         Subpart J
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
secondary fiber non-deink facilities where paperboard from
wastepaper is produced- -noncorrugating medium finish
subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Maximum for any 1 day
3.0
5.0
H
Average of daily values for
30 consecutive days
1.5
2.5
(l)
                            975

-------
                           Subpart J
Pollutant
or
pollutant
property
BODS
TSS
PH
BPT effluent limitations for
secondary fiber non-deink facilities where paperboard from
wastepaper is produced- -corrugating medium finish
subdivision
Kg/kkg (or pounds per 1,000 Ib) of product .
Maximum for any 1 day
5.7
9.2
(x) ;
Average of daily values for
30 consecutive days
2.8
4.6

Within the range of 6.0 to 9.0 at all times.

                          Subpart  J
Pollutant
or
pollutant
property
BODS
TSS
pH
Setteable
Solids
BPT effluent limitations for
secondary fiber non-deink facilities where builders ' paper
and roofing felt from wastepaper are produced
Kg/kkg (or pounds per 1,000 Ib)
Maximum for any 1 day
5.0
5.0
t1)
(2)
of product
Average of daily values
30 consecutive days

for
3.0
3.0
t1)
(2)
Within the range of 6.0 to 9.0 at all times.
2Not to exceed 0.2 ml/1.

      (b)  Except as provided in 40 CFR  125.30  through:

125.32,  any existing point source subject  to this  subpart

must achieve the following effluent limitations  representing

the degree  of effluent reduction attainable by the

application of the best practicable control technology

currently available (BPT), except that  non-continuous

                              976

-------
dischargers  shall not be subject to the maximum day and



average  of 30  consecutive days limitations but shall be



subject  to annual average effluent limitations:



                          Subpart  J
Pollutant
or
pollutant
property
BOD5
TSS
pH
BPT effluent limitations for
secondary fiber non-deink facilities where tissue from
wastepaper is produced without deinking
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
1 13.7
17.05
n
Average of daily
values for 30
consecutive days
7.1
9.2

-------
   [   (a)   Except,as provided in 40  CFR 125.30  through



 125.32,  any existing point  source subject  to this  subpart



 shall achieve the  following effluent  limitations



'representing the degree of  effluent reduction  attainable by



 the  application of the best conventional pollutant control



 technology (BCT):  The limitations shall be the same as those



 specified for conventional  pollutants (which are defined in



 40 CFR 401.16)  in  §430.102  of this  subpart for the best



 practicable control technology currently available (BPT).



   ;   (b)   For secondary fiber non-deink facilities where



 paperboard from wastepaper  is produced, non-continuous



 dischargers shall  not be subject to the maximum day and



 average-of-30-consecutive-days limitations,  but shall be



 subject to annual  average effluent  limitations determined by



 dividing the average-of-30-consecutive-days limitations for



 BODS and TSS by 1.77 and 2.18.




      (c)   For secondary fiber non-deink facilities where



 builders'' .paper and roofing felt from wastepaper are



 produced,  non-continuous dischargers  shall not be  subject to



 the  maximum day and average-of-30-consecutive-days



 limitations,  but shall be subject to  annual average effluent



 limitations determined by dividing  the average-of-30-



 consecutive-days limitations for BODS and  TSS  by 1.90 and




 1.90.



 § 430.104  Effluent limitations representing the degree of
                             978

-------
.Subpart J
Pollutant or
pollutant property
Pent achl orophenol
Trichlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00087
0.00030
Milligrams/liter
(0.029) (7.2)/y
(0.010) (7.2)/y
y = wastewater discharged in kgal per ton of product
Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0017
0.00060
Milligrams/liter
(0.029) (14.4) /y
(0.010) (14.4) /y
y = wastewater discharged in kgal per ton of product
   980

-------
                          Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Tr i chlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0011
Milligrams/liter
(0.029) (25.2)/y
(0.010) (25.2)/y
y = wastewater discharged in kgal per ton of product
                          Subpart  J
\ Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
deinking
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product •
0.0026
0.00088
Milligrams /liter
(0.029) (21.1) /y
(0 . 010) (21.1) /y
y = wastewater discharged in kgal per ton of product
§ 430.105  New source performance standards (NSPS).




     Any new source subject to this subpart must achieve the



following new source performance standards  (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BOD5 and TSS, but shall be  subject to annual



average effluent limitations.  Also, for non-continuous



dischargers, concentration limitations  (mg/1)  shall apply,




                             981

-------
 where provided.  Concentration limitations will only apply
 to non-continuous dischargers.  Only facilities where
 chlorophenolic-containing biocides are used shall be subject
 to pentachlorophenol and trichlorophenol limitations.
 Permittees not using chlorophenolic-containing biocides must
 certify  to the permit-issuing authority that they are not
 using these biocides:
                          Subpart J
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced- -
noncorrugating medium furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
2.6
3.5
(l )
Average of
daily
values for
30
consecutive
days
1-4
1.8
(x )
Maximum for any 1
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00087
0.00030
Non -continuous
Dischargers
(Annual Average)
0.73
0.95
C1 )
day
Milligrams/liter
(0.065) (3.2)/y
(0.023) (3.2)/y
y = wastewater discharged in legal per ton at all times
"•Within the range of  5.0 to 9.0 at all times.
                             982

-------
                             Subpart J
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced- -
corrugating medium finish subdivision)
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.9
4.4
(l )
Average of
daily
values for
30
consecutive
days
2.1
2.3
t1 )
Non- continuous
Dischargers
(Annual Average)
1.1
1.2
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.00087
0.00030
Milligrams/ liter
(0.065) (3.2/y
(0.023) (3.2)/y
y = wastewater discharged in kgal per ton at all times
xWithin the range of 5.0  to 9.0 at all times.
                                 983

-------
                              Subpart J
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
1.7
2.7
C1 )
Average of
daily
values for
30
conse.cutive
days
0.94
1.40
P )
Maximum for any 1
Kg/kkg (or pounds
per 1,.000 Ib) of
- product
0.0017
0. OOOSO
Non-continuous
Dischargers
(Annual Average)
0.49
0.74
: c1 )
day
Milligrams/ liter
(0.155) (2.7)/y
(0.053) (2.7) /y
y = wastewater discharged in kgal per ton at all times
•'witnin tne range of 5.0 to 9.0  at all times.
                                 984

-------
                             Subpart J
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Tr i chlorophenol
NSPS for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.6
10.2
(l )
Average of
daily
values for
30
consecutive
days
2.5
5.3
(x )
Non - cont inuous
Dischargers
(Annual Average)
1.3
2.8
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0030
0.0011
Milligrams/liter
(0.045) (16.3)/y
(0.015) (16.3)/y
y = wastewater discharged in kgal per ton at all times
xWithin the range of 5.0 to 9.0 at all times.
                                 985

-------
                          Subpart J
Pollutant or
pollutant property
BODS
TSS
PH


Pentach.loroph.enol
Tr i chlorophenol
NSPS for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
de inking
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
2.1
4.4
(l )
Average of
daily
values for
30
consecutive
days
1.1
2.3
(1 )
Non-continuous
Dischargers
(Annual Average)
0.58
1.21
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0 .0025
0.00088
• Milligrams /liter
(0.107) (5.7)/y
(0.037) (5.7)/y
y = wastewater discharged in kgal per ton at all times
       the range of 5.0 to 9.0 at all  times.




§ 430.106  Pretreatment standards for existing  sources




(PSES).




     Except as provided in 40 CFR 403.7 and 403.13,  any



existing source subject to this  subpart that  introduces



pollutants into a publicly owned treatment works must:



comply with 40 CFR part 403; and achieve the  following



pretreatment standards for existing sources  (PSES)  if it



uses chlorophenolic-containing biocides.  Permittees not
                             986

-------
using chlorophenolic-containing biocides must certify  to the

permit-issuing authority that they are not  using these

biocides.  PSES must be  attained  on or before July 1,  1984:

                            Subpart  J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day :
Milligrams/liter (mg/1)
(0.032) (7.2)/y
(0.010) (7.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product.3
0.00096
0.00030
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to impose mass effluent limitations.
                            Subpart  J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (14.4)y
(0.010) (14.4)y
Kg/kkg (or pounds per
1,000 Ib) of product*
0.0019
0. 00060
y - wastewater discharged in kgal per ton of product
• The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                                987

-------
                           Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (25.2)y
(0.010) (25.2/y
Kg/kkg (or pounds per
1,000 Ib) of product a
0.0034
0.0011
y = wastewater discharged in kgal per ton of product
  The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                           Subpart  J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
secondary fiber non-deink facilities where molded
products from wastepaper are produced without
deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (21.1)y
(0.010) (21.1)y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0028
0.00088
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when'POTWs find it necessary to impose mass  effluent  limitations.

§ 430.107  Pretreatment standards for  new sources  (PSNS).

     Except as, provided in 40 CFR 403.7,  any new source

subject  to this subpart that introduces  pollutants into  a

publicly owned treatment works must: comply with 40 CFR  part

403; and achieve the  following pretreatment standards  for

new sources (PSNS)  if  it uses chlorophenolic-containing

biocides.   Permittees  not using chlorophenolic-containing
                               988

-------
biocides must certify to the permit-issuing  authority that

they are not using  these biocides:

                             Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for :
secondary fiber non-deink facilities where
paperboard from wastepaper is produced
Maximum for any 1 day
Milligrams /liter (mg/1)
(0.072) (3. 2)/y
(0.023) (3. 2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.00095
0.00030
y = wastewater discharged in kgal; per ton of product
a The following equivalent mass limitations are provided as guidance  in
cases when POTWs find it necessary to impose mass effluent  limitations.
                             Subpart  J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where
builders ' paper and roofing felt from wastepaper
are produced
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.171) (2.7)/y
(0.053) (2. 7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0019
0.00060
y = wastewater discharged in kgal per ton of product
 The following equivalent mass limitations are provided as guidance in
cases when POTWs find it  necessary to impose mass effluent  limitations.
                                989

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                            Subpart  J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where tissue
from wastepaper is produced without deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.049) (16.3)/y
(0.015) (16. 3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0034
0.0011
y = wastewater discharged in kgal per ton of product
  The following equivalent mass limitations  are provided'as guidance in
 cases when POTWs find it necessary to impose mass effluent limitations.
                            Subpart J
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for
secondary fiber non-deink facilities where molded
prodiicts from wastepaper are produced without
deinking
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.118) (5.7)/y
(0.037) (5.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0028 •
0.00088
y = wastewater discharged in kgal per ton of product
  The following equivalent mass limitations are provided as guidance in
 cases when POTWs find it necessary to impose  mass effluent limitations.

 Subpart K-Pine and Lightweight Papers from  Purchased Pulp

 § 430,110  Applicability; description of the fine and


.lightweight  papers from purchased pulp subcategory.

      The provisions of this  subpart are applicable to

 discharges resulting from the  production of:   fine paper at

 nonintegrated mills; and lightweight paper  at nonintegrated
                               990

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mills.



§ 430.111  Specialized definitions.




     For the purpose of this subpart:



      (a)  Except as provided in paragraphs  (b) and (c) of



this section, the general definitions, abbreviations, and



methods of analysis set forth in 40 CFR part 401 and



§ 430.01 of this part shall apply to this subpart.



      (b)  Cotton fiber furnish subdivision mills are those



mills where significant quantities of cotton fibers  (equal



to or greater than 4 percent of the total product) are used



in the production of fine papers.



      (c)  Wood fiber furnish subdivision mills are those



mills where cotton fibers are not used in the production of



fine papers.                                      .    :



§ 430.112  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source 'subject to this subpart must achieve



the following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best practicable control technology currently available *



(BPT), except that non-continuous dischargers shall not be



subject to the maximum day and average of 30 consecutive



days limitations but shall be subject to annual average






                             991                       :

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effluent limitations:
                             Subpart K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills
where fine paper is produced from purchased pulp- -wood
fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
'Maximum for any 1
day
8.2
11.0
H
Average of daily
values for 30
consecutive days
4.25
5.9
(-1)
Non- continuous
dischargers
(Annual Average)
2.4
3.2
(x)
lWitnin the range of 5.0 to  9.0 at all  times.
                            Subpart K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills
where fine paper is produced from purchased pulp- -cotton
fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
17.4
24.3
H
Average of daily
values for 30
consecutive days
9.1
13 .1
t1)
Non- continuous
dischargers
(Annual Average)
5.1
7.2
P)
       the range of 5.0  to 9.0 at all times.
                               992

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                          Subpart  K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills
where lightweight papers are produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
24.1
21.6
C1)
Average of daily
values for 30
consecutive days
13.2
10.6
(l)
Non - cont inuous
dischargers
(Annual Average)
7.37
6.6
(l)
xWithin the range of 5.0 to 9.0 at all times.
                          Subpart  K
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills where
lightweight papers are produced from purchased pulp--
electrical grade papers subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
38.0
34.2
(l)
Average of daily
values for 30
consecutive days
20.9
16.7
(x)
Non -cont inuous
dischargers
(Annual Averacfe)
11.7
9.5
(x) •
xWithin the range of 5.0 to 9.0 at all times.






§ 430.113  Effluent limitations guidelines representing  the




degree of effluent  reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




     Except as provided in 40 CFR 125.30 through 125.32,  any




existing point source  subject to this  subpart shall achieve
                             993

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 the following effluent  limitations  representing  the degree



 of  effluent reduction attainable  by the  application of  the



 best conventional  pollutant  control technology (BCT): The



 limitations shall  be  the  same  as  those specified for




 conventional pollutants (which are  defined  in  40 CFR 401.16)



 in  § 430.102 of  this  subpart for  the best practicable



 control  technology currently available  (BPT).




 § 430.114   Effluent limitations representing the degree of




 effluent reduction attainable  by  the application of the best




 available technology  economically achievable (BAT).




      Except  as provided in 40  CFR 125.30 through 125.32,  any



 existing point source subject  to  this subpart where




 chlorophenolic-containing biocides  are used must  achieve  the



 following effluent  limitations representing the  degree  of



 effluent reduction  attainable  by  the application of the best



 available technology economically achievable (BAT).  Non-



 continuous dischargers  shall .not  be subject to the  maximum



 day mass limitations in.kg/kkg  (lb/1000 Ib)  but  shall be



 subject  to concentration limitations.  Concentration



 limitations  are only applicable to non-continuous



 dischargers.  Permittees not using chlorophenolic-containing



biocides must certify to the permit-issuing authority that



they are not using these biocides:
                             994

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Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
BAT effluent limitations for non- integrated mills
where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
D.001'8
0.00064
Milligrams/liter
(0.029) (15.2)/y
(0.010) (15.2)/y
y « wastewater discharged in kgal per ton of product
Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for non- integrated mills
where fine paper is produced from purchased
pulp- -cotton fiber furnish subdivision
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0051
0.0018
Milligrams/liter
(0.029) (42.3)/y
(0.010) (42.3)/y
y « wastewater discharged in kgal per ton of product
    995

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                          Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for non- integrated mills
where lightweight papers are produced from
purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0059
0.0020
Milligrams/ liter
(0.029) (48.7)/y
(0,010). (48. 7) /y
y = wastewater discharged in kgal per ton of product
                          Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for non -integrated mills
where lightweight papers are produced from
purchased pulp- -electrical grade papers
subdivision
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0093
0.0032
Milligrams /liter
(0.029) (76.9)/y
(0.010) (76.9)/y
y = wastewater discharged in kgal per ton of product
§ 430.115  New source performance standards  (NSPS).




     Any new source subject to this subpart must achieve the



following new source performance standards  (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BOD5 and TSS, but shall be subject to annual



average effluent limitations.  Also, for non-continuous



dischargers, concentration limitations  (mg/1) shall apply,
                             996

-------
where provided.  Concentration limitations will only apply



to non-continuous dischargers.  Only facilities where



chlorophenolic-containing biocides are used shall be subject



to pentachlorophenol and trichlorophenol limitations.



Permittees not using chlorophenolic-containing biocides must



certify to the permit-issuing authority that they are not



using these biocides:
                             997

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Subpart K
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Tri chlorophenol
NSPS for non- integrated mills
. where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
3.5
4.4
t1 )
Average of
daily
values for
30
consecutive
days
1.9
2.3
(1 )
Non-continuous
Dischargers
(Annual Average)
1.0
1.2
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0018
0.00064
Milligrams /liter
(0.047) (9.4)/y
(0.016) (9.4)/y
y = wastewater discharged in kgal per ton at all times
Within the range of 5.0 to 9.0 at all times .
  998

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                             Subpart  K
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills
where fine paper is produced from purchased
pulp — cotton fiber furnish subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
7.8
9.5
(x )
Average of
daily
values for
30
consecutive
days
4.2
4.9
t1 )
Non- continuous
Dischargers
(Annual Average)
2 ,. 2
2.6
(z )
Maximum for any 1 day
Kg/kkg (or pounds
per 1, 000 Ib) of
product
0.0051
0.0018
Milligrams/liter
(0.039) (31.1)/y
(0.014) (31.1)/y
y - wastewater discharged in kgal per ton at all times [
*Within the range of 5.0  to  9.0 at all times.
                                 999

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                      Subpart K
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills
where lightweight papers are produced from
purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
13.7
12 .0
(1 )
Average of
daily
values for
30
consecutive
days
6.7
5.2
c1 )
Maximum for any 1
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0059
0.0020
Non-continuous
Dischargers
(Annual Average)
4.5
3.2
(M
day
Milligrams/liter
(0.037) (38.2) /y
(0. 013) (38.2) /y
y = wastewater discharged in kgal per ton at all times
tne range  or 5.0 to 9.0 at  all times.
                         1000

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                          Subpart K
Pollutant or
pollutant property
BODS
TSS
PH


Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
24.1
21.1
(x ).
Average of
daily
values for
30
consecutive
days
11.7
9.2
0 )
Non- continuous
Dischargers
(Annual Average)
7.9
5.. 6
(1 )
Maximum for any 1 day
Kg/kkg (or pounds
per 1, 000 Ib) of
product
0.0093
0.0032.
Milligrams/ liter
(0.033) (66.8) /y
(0.012) (66.8) /y
y = wastewater discharged in kgal per ton at all times
Htfithin the range of 5.0 to 9.0 at all times.




§ 430.116  Pretreatment standards for existing  sources




(PSES).




     Except as provided in 40 CFR 403.7 and 403.13,  any



existing source subject to this subpart that  introduces



pollutants into a publicly owned treatment works must:



comply with 40 CFR part 403; and achieve the  following



pretreatment standards for existing  sources  (PSES)  if it



uses chlorophenolic-containing biocides.  Permittees not



using chlorophenolic-containing biocides must certify to  the




                            1001

-------
permit-issuing authority  that they are not  using these

biocides.   PSES must be attained on or before July  1,  1984:

                             Subpart K
Pollutant or
pollutant property
Pent achl oropheno 1
Tri chl orophenol
PSES for non- integrated mills
where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (15.2)/y
(0.010) (15.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0020
0.00064
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                             Subpart  K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills
where fine paper is produced -from purchased
pulp- -cotton fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (42.3)/y
(0.010) (42.3)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0056
0.0018
y = wastewater discharged in kgal per ton of product
 The following equivalent mass  limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                                1002

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                            Subpart  K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills
where lightweight papers are produced from
purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (48.7)/y
(0.010) (48.7)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0065
0.0032
y ~ wastewater discharged in kgal per ton of product
* The following equivalent mass limitations  are provided as guidance in
cases when POTWs  find it necessary to impose mass effluent limitations.
                            Subpart K
Pollutant or
pollutant property
t
Pentachlorophenol
Trichlorophenol
PSES for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (76. 9) /y
(0.010) (76.9)/y
Kg/kkg (or pounds per
1,000 Ib) of product2
0.010
0.0032
y = wastewater discharged in kgal per ton of product
"The following equivalent mass limitations are provided as guidance in
cases  when POTWs find it necessary to impose mass effluent limitations.
§ 430.117  Pretreatment standards for new  sources (PSNS).

      Except as provided in 40  CFR 403.7, any new source

subject to this  subpart that introduces pollutants into  a

publicly owned treatment works must: comply  with 40 CFR  part

403;  and achieve the following pretreatment  standards  for
                               1003

-------
new sources  (PSNS) if it  uses chlorophenolic-containing

biocides.  Permittees not using chlorophenolic-containing

biocides must  certify to  the permit-issuing authority that

they are not using these  biocides:

                            Subpart  K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where fine paper is produced from purchased
pulp- -wood fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.052) (9.4)/y
(0.016) (9. 4)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0020
0.00064
y = wastewater discharged in kgal per ton of product
aThe following  equivalent mass limitations are provided as guidance in
cases  when POTWs find it necessary to impose mass  effluent limitations.
                            Subpart  K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where fine paper is produced from purchased
pulp- -cotton fiber furnish subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0:044) (31.1)/y
(0.014) (31.1)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0056
0.0018
y = wastewater discharged in kgal per ton of product
aThe following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to impose mass effluent limitations.
                               1004

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                               Subpart K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills
where lightweight papers are produced ' from
purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.041) (38.2) /y
(0.013) (38.2)/y
Kg/kkg (or pounds per
1,000 Ib) of prpduct3
0.0065 .
0.0020
y = wastewater discharged in kgal per ton of product
* The following  equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                              Subpart  K
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non- integrated mills where lightweight
papers are produced from purchased pulp--
electrical grade papers subdivision
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.037) (66.8) /y
(0.012) (66. 8) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.010 ;
0.0032 ;
y = wastewater discharged in kgal per ton of product
• The  following equivalent mass limitations are provided as guidance in
cases when POTWs  find it necessary to  impose mass effluent limitations.
                                 1005

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 Subpart L-Tissue,  Filter, Non-woven,  and Paperboard  from




 Purchased Pulp




 § 430.120  Applicability; description of the  tissue,  filter,




 non-woven, and paperboard from purchased pulp subcategory.




    The provisions of this subpart are applicable to



 discharges resulting from the production of:  tissue papers



 at nonintegrated mills; filter and non-woven  papers at




 nonintegrated mills; and paperboard at nonintegrated  mills.



 The production of electrical grades of board  and matrix



 board is not included in this subpart.




 § 430.121  Specialized definitions.




    For the purpose of this subpart,  the general



 definitions, abbreviations,  and methods of analysis set



 forth in 40 CFR part 401 and § 430.01 of this part shall



 apply to this subpart.




 § 430.122  Effluent limitations representing  the degree of




 effluent reduction attainable by the application of the best




practicable control technology currently available (BPT).




     Except as provided in 40 CFR 125.30 through 125.32,  any



existing point source subject to this subpart must achieve



the following effluent limitations representing the degree



of effluent reduction attainable by the application of the



best practicable control technology currently available



 (BPT),  except that non-continuous dischargers shall not be  -
                            1006

-------
subject  to the maximum day  and average of 30 consecutive



days limitations but shall  be subject to annual average



effluent limitations:



                           Subpart L
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for
non- integrated mills where tissue papers are produced from
purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
11.4
10.25
C1)
Average of daily
values for 30
consecutive days
6.25
5.0
(l)
Non -continuous
dischargers
(Annual Average)
3 .49
2.84
C1)
^Within the range of 5.0 to 9.0 at all times.
                              i
                              i

                           Subpart L
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non- integrated mills where
filter and non-woven papers are produced from purchased
pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
29.6
26.6
(*)
Average of daily
values for 30
consecutive days
16.3
13.0
(^
Non- continuous
dischargers
(Annual Average)
9.1
7.4
t1)
Within the range of 5.0 to 9.0 at all times.
                              1007

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                          Subpart L
Pollutant
or
pollutant
property
BODS
TSS
pH
BPT effluent limitations for non-integrated mills where
paperboard is produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous dischargers
Maximum for any 1
day
6.5
,5.8
•C1)
Average of daily
values for 30
consecutive days
3.6
2.8
H
Non-continuous
dischargers
(Annual Average)
2.0
1.6
C1)
       cne range or 5.0 to 9.0 at all times.






§ 430.123  Effluent  limitations guidelines representing the




degree of effluent reduction attainable by the application




of the best conventional pollutant control technology  (BCT).




     Except as, provided in 40 CFR 125.30 through 125.32,  any



existing point source  subject to this subpart shall achieve



the following effluent  limitations representing the degree



of effluent reduction  attainable by the application of  the



best conventional pollutant control technology (BCT): The



limitations shall be the same as those specified for



conventional pollutants (which  are defined in 40 CFR 401.16)



in §430.122 of this subpart for the best practicable control



technology currently available  (BPT).




§ 430.124  Effluent limitations representing the degree of




effluent reduction attainable by the application of the best




available technology economically achievable (BAT).
                            1008

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     Except as provided in 40 CFR 125.30 through 125.32, any



existing point source subject to this subpart where  :



chlorophenolic-containing biocides are used must achieve the



following effluent limitations representing the degree of



effluent reduction attainable by the application of the best



available technology economically achievable  (BAT).   Non-



continuous dischargers shall not be subject to the maximum



day mass limitations in kg/kkg (lb/1000 Ib) but shall' be



subject to concentration limitations.  Concentration



limitations are only applicable to non-continuous



dischargers.  Permittees not iUsing chlorophenolic-containing



biocides must certify to the permit-issuing authority that



they are not using these biocides:



                         Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
non- integrated mills where tissue papers are
produced, from purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product ;
0.0028
0.00096
Milligrams/liter
(0.029) (22. 9) /y.
(0.010) (22 .9) /y
y * wastewater discharged in kgal per ton of product
                            1009

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                          Subpart  L
Pollutant or
pollutant property
Pentachlorophenol
Tri chlorophenol
BAT effluent limitations for
non- integrated mills where filter and non-woven
papers are produced from purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1;000 Ib) of
product
0.0072
0.0025
Milligrams /liter
(0.029) (59. 9) /y
(0.010) (59.9)/y
y = wastewater discharged in kgal per ton of product
                          Subpart  L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
BAT effluent limitations for
non- integrated mills where paperboard is produced
from purchased pulp
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.001S
0.00054
Milligrams/ liter
(0.029) (12.9)/y
(0.010) (12. 9) /y
y = wastewater discharged in kgal per ton of product
§ 430.125  New source performance standards (NSPS).




     Any new source subject to this subpart must achieve the



following new source performance standards  (NSPS), except



that non-continuous dischargers shall not be subject to the



maximum day and average of 30 consecutive days effluent



limitations for BOD5 and TSS, but shall be subject to annual



average effluent limitations.  Also, for non-continuous
                            1010

-------
dischargers, concentration limitations  (mg/1) shall apply,



where provided.  Concentration limitations will only apply



to non-continuous dischargers.  Only facilities where



chlorophenolic-containing biocides are used shall be subject



to pentachlorophenol and trichlorophenol limitations.;



Permittees not using chlorophenolic-containing biocides must



certify to the permit-issuing authority that they are,not



using these biocides:
                            UOll

-------
                      Subpart L
Pollutant or
pollutant property
BODS
TSS
pH


Pentach.loroph.enol
Trichlorophenol
NSPS for non- integrated mills where tissue papers
are produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
7.0
6.0
•(* )
Average of
daily
values for
30
consecutive
days
3.4
2.6
(l )
Non- continuous
Dischargers
(Annual Average)
2.3
1.6
(l )
Maximum for any 1 day.
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0028
0.00096
Milligrams/ liter
(0,035). (19. l)/y
(0.012) (19.1) /y
y = wastewater discharged in kgal per ton at all times
tne range  of 5.0 to 9.0 at all times.
                         1012

-------
                             Subpart L
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
,. NSPS for
non- integrated mills where filter and non-woven
papers are produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
17.1
15.0
C1 )
Average of
daily
values for
30
consecutive
days
8.3
6.6
(l )
Non- continuous
Dischargers
(Annual Average)
5.6
4.0.
(l )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.0072 .
0.0025
Milligrams /liter
(0.037) (47. 5) /y
(0.013) (47.5)/y
y = wastewater discharged in kgal - per ton at all times
Within the range of 5.0 to 9.0 at all times.
                                1013

-------
                          Subpart L
Pollutant or
pollutant property
BODS
TSS
pH


Pentachlorophenol
Trichlorophenol
NSPS for non- integrated mills where paperboard is,
produced from purchased pulp
Kg/kkg (or pounds per 1,000 Ib) of product
Continuous Dischargers
Maximum for any 1
day
4.0
3.5
P )
Average of
daily
values for
30
consecutive
days
1.9
1.5
(l )
Non-continuous
Dischargers
(Annual Average)
1.3
0.9
(x )
Maximum for any 1 day
Kg/kkg (or pounds
per 1,000 Ib) of
product
0.001S
0.00054
Milligrams/ liter
(0.033) (11.2)/y
(0.012) (ll.2)/y
y = wastewater discharged in kgal per ton at all times
xWithin the range of 5.0 to 9.0 at all times.




§ 430.126  Pretreatment standards for existing  sources




(PSES).




     Except as provided in 40 CFR 403.7 and  403.13,  any



existing source subject to this  subpart that introduces



pollutants into a publicly owned treatment works must:



comply with 40 CFR part 403; and achieve the following



pretreatment standards for existing sources  (PSES)  if  it



uses chlorophenolic-containing biocides.  Permittees not



using chlorophenolic-containing  biocides must certify  to  the
                            1014

-------
permit-issuing authority that they  are not using these

biocides.   PSES must be.attained on or before July 1,  1984:

                             Subpart  L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for
non- integrated mills where tissue papers are
produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (22.9) /y
(0.010) (22. 9) /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0031
0.00096
y =» wastewater discharged in kgal per ton of product
0 The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                             Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for '
non- integrated mills where filter and non-woven
papers are produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (59. 9) /y
(0.010) (59. 9} /y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0080
0.0025 •
y = wastewater discharged in kgal per ton of product
*  The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations
                                1015

-------
                           Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSES for non-integrated mills where paperboard is
produced from purchased pulp
Maximum for any 1 day
Milligrams/liter (mg/1)
(0.032) (12. 9) /y
(0.010) (12. 9) /y -
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0017
0.00054
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
§ 430.127  Pretreatment standards for new  sources (PSNS).

     Except  as  provided in 40 CFR 403.7, any new source

subject to this subpart that introduces pollutants into a

publicly owned  treatment works must: comply with 40 CFR part

403; and achieve the following pretreatment standards for

new sources  (PSNS)  if it uses chlorophenolic-containing

biocides.  Permittees not using chlorophenolic-containing

biocides must certify to the permit-issuing authority that

they are not using  these biocides:
                             1016

-------
                               Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Tr i chl oropheno 1
PSNS for non- integrated mills where tissue papers
are produced from purchased pulp
Maximum for any 1 day
Milligrams/ liter (mg/1)
(0.038) (19.1)/y
(0.012) (19.1)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0031
0 .00096
y = wastewater discharged in kgal per ton of product
a The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                               Subpart L
Pollutant or
pollutant property
Pentachlorophenol
Trichlorophenol
PSNS for non -integrated mills where filter and
non-woven papers are produced from purchased pulp
Maximum for any 1 day >
Milligrams/liter (mg/1)
(0.040) (47.5) /y
(0.013) (47.5)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0080
0.0025
y = wastewater discharged in kgal per ton of product
• The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose mass effluent limitations.
                                 1017

-------
                           Subpart  L
Pollutant or
pollutant property
Pent achloropheno 1
Trichlorophenol
PSNS for
non- integrated mills where paperboard is produced
from purchased pulp
Maximum for any 1 day
"Milligrams/liter (mg/1)
(0.037) (11.2)/y
(0.012) (11.2)/y
Kg/kkg (or pounds per
1,000 Ib) of product3
0.0017
0.00054
y = wastewater discharged in kgal per ton of product
a  The following equivalent mass limitations are provided as guidance in
cases when POTWs find it necessary to impose  mass effluent  limitations.
Appendix A  to  Part 430--Methods 1650 and 1653

                         Method 1650

                  Adsorbable Organic Halides

           by Adsorption and Coulometric  Titration

1.0  Scope  and Application

1.1  This method is for determination of adsorbable organic

halides  (AOX)  associated with the Clean Water Act; the

Resource Conservation and Recovery Act; the Comprehensive

Environmental  Response,  Compensation, and Liability Act; and

other organic  halides amenable to combustion and coulometric

titration.  The method is designed to meet the survey and

monitoring  requirements of the Environmental Protection

Agency  (EPA) .

1.2  The method is applicable to the determination of AOX  in

water and wastewater.  This method is a combination of
                             1018

-------
several existing methods for;organic halide measurements



(References 1 through 7).



1.3  The method can be used to measure organically-bound



halides (chlorine, bromine, iodine) present in dissolved or



suspended'form.  Results are:reported as organic chloride



(Cl~) .   The detection limit of  the method is usually



dependent on interferences rather than instrumental



limitations.  A method detection limit (MDL; Reference 8) of



6.6 /ig/L,  and a minimum level  (ML; Section 18) of 20 /zg/L,



can be achieved with no interferences present.



1.4  This method is for use by or under the supervision-of



analysts experienced in the use of a combustion/micro-



coulometer.  Each laboratory that uses this method must



demonstrate the ability to generate acceptable results using



the procedures described in Section 9.2.



1.5  Any modification of the method beyond those expressly



permitted  (Section 9.1.2)  is subject to application and



approval of an alternate test procedure under 40 CFR 136.4




and 136.5.                 '  '•                        \



2.0  Summary of Method




2.1  Sample preservation:  Residual chlorine that may be



present is removed by the addition of sodium thiosulfate.



Samples are adjusted to a pH < 2 and maintained at 0 to 4°C



unt i1 analys i s.



2.2 Sample analysis: Organic halide in water is determined



by adsorption onto granular activated carbon  (GAG), washing




                            1019

-------
the adsorbed sample and GAG to remove inorganic halide,



combustion of the sample and GAG to form the hydrogen



halide, and titration of the hydrogen halide with a micro-



coulometer, as shown in Figure 1.



2.3  Micro-coulometer.




2.3.1  This detector operates by maintaining a constant



silver-ion concentration in a titration cell.  An electric



potential is applied to a solid silver electrode to produce



silver ions in the cell.   As hydrogen halide produced from



the combustion of organic halide enters the cell, it is



partitioned into an acetic acid electrolyte where it



precipitates as silver halide.  The current produced is




integrated over the combustion period.  The electric charge



is proportional to the number of moles of halogen captured



in the cell. (Reference 6) .




2.3.2  The mass concentration of organic halides is reported



as an equivalent concentration of organically bound chloride



(cr) .



3.0  Definitions




3.1  Adsorbable organic halides is defined as the analyte



measured by this method.   The nature of the organo-halides



and the presence of semi-extractable material will influence



the amount measured and interpretation of results.



3.2  Definitions for terms  used in this method are given in



the glossary at the end of  the method (Section 18).



4.0  Interferences





                            1020

-------
4.1  Solvents, reagents, glassware, and other sample



processing hardware may yield elevated readings from the



tnicro-coulometer.  All materials used in the analysis shall



be demonstrated to be free from interferences under, the



conditions of analysis by running method blanks initially



and with each sample batch (samples' started through the



adsorption process in a -given eight-hour shift, to a maximum



of 20 samples).  Specific selection of reagents and



purification of solvents may be required.            ;



4.2  Glassware is cleaned by detergent washing in hot water,



rinsing with tap water and distilled water, capping with



aluminum foil, and baking at 450°C for at least one hour.



For some glassware, immersion in a chromate cleaning



solution prior to detergent washing may be required.  If



blanks from glassware without cleaning or with fewer:



cleaning steps show no detectable organic halide, the



cleaning steps that do not eliminate organic halide may be




omitted.



4.3  Most often, contamination results from methylene



chloride vapors in laboratories that perform organic



extractions.  Heating, ventilating, and air conditioning



systems that are shared between the extraction laboratory



and the laboratory in which 'organic halide measurements are



performed transfer the methylene chloride vapors to  the air



in the organic halide laboratory.  Exposure of the activated



carbon used in the analysis results in contamination.






                            1021            •         :

-------
Separate air handling systems, charcoal filters, and glove



boxes can be used to minimize this exposure.



4.4  Activated carbon.




4.4.1  The purity of each lot of activated carbon must be



verified before each use by measuring the adsorption



capacity and the background level of halogen  (Section 9.5).



The stock of activated carbon should be stored in its



granular form in a glass container that is capped tightly.



Protect carbon at all times from sources of halogen vapors.



4.4.2  Inorganic substances such as chloride, chlorite,



bromide, and iodide will adsorb on activated carbon to an



extent dependent on their original concentration -in the



aqueous solution and the volume of sample adsorbed.



Treating the activated carbon with a solution of nitrate



causes competitive desorption of inorganic halide species.



However, if the inorganic halide concentration is greater



than 2,000 times the organic halide concentration,



artificially high results may be obtained.



4.4.3 Halogenated organic compounds that are weakly adsorbed



on activated carbon are only partially recovered from the



sample.  These include certain alcohols and acids such as



chloroethanol and chloroacetic acid that can be removed from



activated carbon by the nitrate wash.




4.5  Polyethylene gloves should be worn when handling



equipment surfaces in contact with the sample to prevent



transfer of contaminants that may be present on the hands.





                            1022

-------
5.0  Safety




5.1  The toxicity or carcinogenicity of each reagent used in



this method has not been precisely determined; however, each



chemical substance should be 'treated as a potential health



hazard.  Exposure to these substances should be reduced to



the lowest possible level.  The laboratory is responsible



for maintaining a current awareness file of OSHA regulations



regarding the safe handling of the chemicals specified in



this method.  A reference file of material safety data



sheets  (MSDSs) should be made available-to all personnel



involved in the chemical analysis.  Additional information



on laboratory safety can be found in References 9 through



11.



5.2  This method employs strong acids.  Appropriate



clothing, gloves, and eye protection should be worn when



handling these substances.



5.3  Field samples may contain high concentrations of toxic



volatile compounds.  Sample containers should be opened in a



hood and handled with gloves that will prevent exposure.



6 . 0  Equipment and Supplies




Note:  Brand names, suppliers, and part numbers are for




illustrative purposes only.  No endorsement is implied.




Equivalent performance may be achieved using apparatus and




materials other than those specified here, but demonstration




of equivalent performance that meets the requirements of





                            1023

-------
 this method is  the responsibility of  the laboratory.




 6.1  Sampling equipment.




 6.1.1  Bottles: 100- to 4000-mL, amber glass, sufficient  for



 all testing (Section 8.2).  Detergent water wash, chromic



 acid rinse,  rinse with tap and distilled water, cover with



 aluminum foil,  and heat to 450°C for at least one hour



 before use.




 6.1.2  PTFE liner: Cleaned as above and baked at 100 to



 200°C for at least one hour.




 6.1.3  Bottles  and liners must be lot certified to be free



 of organic  halide by running blanks according to this



 method.




 6.2  Scoop  for  granular activated carbon (GAG): Capable of



 precisely measuring 40 mg (±5 mg) GAC (Dohrmann Measuring



 Cup 521-021, or equivalent).



 6.3  Batch  adsorption and filtration system.



 6.3.1  Adsorption system:  Rotary shaker,  wrist action



 shaker, ultrasonic system, or other system for assuring



 thorough contact of sample with activated carbon.   Systems



 different from  the one described below must be demonstrated



 to meet the performance requirements in Section 9 of this



method.




 6.3.1.1  Erlenmeyer flasks:  250- to 1500-mL with ground-



glass stopper,   for use with rotary shaker.



 6.3.1.2  Shake table:  Sybron Thermolyne Model LE "Big Bill"



rotator/shaker,  or equivalent.





                            1024

-------
6.3.1.3  Rack attached to shake table to permit agitation of



16 to 25 samples simultaneously.



6.3.2  Filtration system  (Figure 2).



6.3.2.1  Vacuum filter holder: Glass,'with fritted-glass



support  (Fisher Model 09-753E, or equivalent).



6.3.2.2  Polycarbonate filter: 0.40 to 0.45 micron, 25-mm



diameter (Micro Separations Inc, Model K04CP02500, or



equivalent).               • ,   .



6.3.2.3  Filter forceps: Fisher Model 09-753-50, or



equivalent, for handling filters.  Two forceps may better



aid in handling filters.  Clean by washing with detergent



and water,  rinsing with tap and deionized water, and air



drying on aluminum foil.



6.3.2.4  Vacuum flask: 500- to 1500-mL (Fisher 10-1800, or



equivalent).                :



6.3.2.5  Vacuum Source: A pressure/vacuum pump, rotary



vacuum pump, or other vacuum,source capable of providing at



least 610 mm (24 in.) Hg vacuum at 30 L/min free air



displacement.



6.3.2.6 Stopper and tubing to mate the filter holder to the



flask and the flask to the pump.



6.3.2.7  Polyethylene gloves:  (Fisher 11-394-110-B, or



equivalent).



6.4  Column adsorption system.



6.4.1  Adsorption module: Dohrmann AD-2,  Mitsubishi TXA-2,



or equivalent with pressurized sample and nitrate-wash






                            1025

-------
reservoirs, adsorption columns, column housings, gas and gas



pressure regulators, and receiving vessels.  For each sample




reservoir, there'are two adsorption columns connected in




series.  A small steel funnel for filling the columns and a



rod for pushing out the carbon are also required.  A  •



schematic of the column adsorption system is shown in Figure




3-



6.4.2  Adsorption columns: Pyrex, 5 ±0.2 cm long x 2 mm ID,



to hold 40 mg of granular activated carbon  (GAG).



6.4.3  Cerafelt: Johns-Manville, or equivalent, formed into



plugs using stainless steel borer (2 mm ID) with ejection



rod (available from Dohrmann or Mitsubishi) to hold 40 mg of



granular activated carbon (GAG).  Caution: Handle Cerafelt



with gloves.



6.4.4  Column holders: To support adsorption columns.



6.5  Combustion/micro-coulometer system: Commercially



available as a single unit or assembled from parts.  At the



time of the writing'of this method,  organic halide units



were commercially available from the Dohrmann Division of



Rosemount Analytical, Santa Clara, California; Euroglas BV,



Delft, the Netherlands; and Mitsubishi Chemical Industries,



Ltd.,  Tokyo, Japan.



6.5.1  Combustion system: Older systems may not have all of



the features shown in Figure 4.  These older systems may be



used provided the performance requirements  (Section 9)  of



this method are met.






                            1026

-------
6.5.1.1  Combustion tube: Quartz, capable of being heated to



800 to 1000°C and accommodating a boat sampler.   The tube



must contain an air lock for introduction of a combustion



boat, connections for purge and combustion gas,  and



connection to the micro-coulometer cell.



6.5.1.2  Tube furnace capable of controlling combustion tube



in the range of 800 to 1000°C.



6.5.1.3  Boat sampler: Capable of holding 35 to 45 mg of



activated carbon and a polycarbonate filter, and fitting



into the combustion tube (Section 6.5.1.1).   Some



manufacturers offer an enlarged boat and combustion tube for



this purpose.  Under a time-control led sequence, the boat, is



first moved into an evaporation zone where water and other



volatiles are evaporated, and then into the combustion zone



where the carbon and all other organic material in the boat



are burned in a flowing oxygen stream.  The evolved gases



are transported by a non-reactive carrier gas. to the micro-



coulometer cell.



6.5.1.4  Motor driven boat sampler: Capable of advancing the



combustion boat into the furnace in a reproducible time



sequence.  A suggested time sequence is as follows:



     A.  Establish initial gas flow rates:  160 mL/min CO2;



     4 0 mL/min O2.



     B.  Sequence start.



     C.  Hold boat in hatch for five seconds to allow



     integration for baseline subtraction.





                            1027

-------
     D.  Advance boat  into vaporization  zone.




     E.  Hold boat  in  vaporization  zone  for 110  seconds.




     F.  Establish  gas flow rates for  combustion:  200  tnL/min



     O2; 0 mL/min CO2;  advance  boat  into  pyrolysis' zone



      (800°C).




     G.  Hold bpat  in  pyrolysis zone for six minutes.



     H.  Return gas flow rates to initial values;  retract



     boat  into hatch to cool and to allow remaining HX to  be



     swept  into detector  (approximately  two minutes).



     I.  Stop integration at 10 minutes  after sequence



     start.




Note:  If  the signal from the detector does not  return to




baseline,  it may be necessary to extend  the pyrolysis




time.The sequence above may need to be optimized for each




instrument.



6.5.1.5  Absorber: Containing sulfuric acid to dry the gas



stream'after combustion to prevent backflush of  electrolyte



is highly recommended.



6.5.2  Micro-coulometer system: Capable  of  detecting the



equivalent of 0.2 j*g of Cl"  at  a  signal-to-noise  ratio of 2;



capable of detecting the equivalent of 1 /zg of Cl" with a



relative standard deviation less than 10%,  and capable of



accumulating a minimum of the equivalent of  500  (j.g of  Cl"



before a change of electrolyte is required.



6.5.2.1  Micro-coulometer cell: The three cell designs
                            1028

-------
presently in use are shown in Figure 1.  Cell operation is

described in Section 2.

6.5.2.2  Cell controller: Electronics capable of measuring

the small currents generated'in the cell and accumulating

and displaying the charge produced by hydrogen halides

entering the cell.  A strip-chart recorder is desirable for

display of accumulated charge.

6.6  Miscellaneous glassware:  nominal sizes are specified

below; other sizes may be used, as necessary.
                             t
6.6.1  Volumetric flasks: 5-, 10-, 25-, 50-, 100-, and 1000-

mL.

6.6.2  Beakers: 100-, 500-, and 1000-mL.

6.6.3  Volumetric pipets: 1- 'and 10-mL with pipet bulbs.

6.6.4  Volumetric micro-pipets: 10-, 20-, 50-, 100-, 200-,

and 500-/iL with pipet control (Hamilton 0010, or
                             \
equivalent).                                         ,     .

6.6.5  Graduated cylinders: 10-, 100-, and 1000-mL.

6.7  Micro-syringes: 10-, 50-, and 100-/zL.

6.8  Balances.                                       i

6.8.1  Top-loading, capable of weighing 0.1 g.
                             <*
6.8.2  Analytical, capable of weighing 0.1 mg.

6.9  pH meter.

6.10  Wash bottles: 500- to 1000-mL, PTFE or polyethylene.

6.11  Strip-chart recorder: suggested but not required--

useful for determining end of integration  (Section 11.4.2).

7.0  Reagents and Standards

                            1029

-------
7.1  Granular  activated carbon (GAG) :  75 to 150 /j.m (100 to



200 mesh);  (Dohrmann,  Mitsubishi,  Carbon Plus,  or
                                 •*


equivalent) , with chlorine  content less than 1  /ig Cl" per



scoop  (<  25 /zg Cl" per gram) , adsorption capacity greater



than 1000 /zg Cl"  (as 2,4,6-trichlorophenol) per scoop



(>25,000  /zg/g) ,  inorganic halide retention of less  than 1  izg



Cl" per scoop in the presence of 10 mg of  inorganic halide



(< 20 /ig  Cl" per gram in the presence of 2500 mg of



inorganic halide), and that meets  the  other test  criteria  in



this method.



7.2  Reagent water: Water in which organic halide is  not



detected by this  method.



7.2.1  Preparation: Reagent water  may  be generated  by:



7.2.1.1  Activated carbon:  Pass tap water  through a carbon



bed (Calgon Filtrasorb-300, or equivalent).



7.2.1.2  Water purifier: Pass tap  water through a purifier



(Millipore Super  Q, or equivalent).



7.2.2  pH adjustment: Adjust the pH of  the reagent  water to



< 2 with nitric acid for all reagent water used in  this



method, except for the  acetic acid solution (Section  7.13).



7.3  Nitric acid  (HNO3) : Concentrated,  analytical grade.



7.4  Sodium chloride  (NaCl) solution  (100  /zg/mL of  Cl")  :



Dissolve 0.165 g  NaCl  in 1000 mL reagent water.   This



solution is used  for cell testing  and  for  the inorganic



halide rejection  test.



7.5  Ammonium chloride  (NH4C1)  solution  (100 /zg/mL of Cl") :





                            1030

-------
Dissolve 0.1509 g NH4C1 in 1000 mL reagent water.



7.6  Sulfuric acid: Reagent grade  (specific gravity  1.84).



7.7  Oxygen: 99.9% purity.



7.8  Carbon Dioxide: 99.9% purity.



7.9  Nitrate stock solution: In a  1000-mL volumetric flask,



dissolve 17 g of NaNO3 in approximately 100 mL of reagent



water, add 1.4 mL nitric acid  (Section 7.3) and  dilute to



the mark with reagent water.



7.10  Nitrate wash solution: Dilute 50 mL of nitrate stock



solution (Section 7.9) to 1000 mL  with reagent water.



7.11  Sodium thiosulfate  (Na2S2O3)   solution (1 N)  : Weigh 79



grams of Na2S2O3 in a 1-L volumetric flask and dilute to the



mark with reagent water.



7.12  Trichlorophenol solutions



Note:  The calibration solutions in this section employ 100-




mL volumes.  For determinations requiring a larger or




smaller volume, increase or decrease the size of the




volumetric flasks commensurately.  For example,  if a 1-L




sample is to be analyzed, use 1000-mL 'flasks  (Sections




7.12.3.1 and 7.12.4) and 10 times  the volume of  reagent




water (Sections 7.12.3.1 and 7.12.4).  The volume of stock




solution added to the calibration  solutions and  precision




and recovery (PAR) test solution remain as specified




(Sections 7.12.3.2 and 7.12.4) so  that the same  amount of
                            1031

-------
 chloride is delivered to the coulometric cell regardless of




 the volume of the calibration and PAR solutions.




 7.12.1   Methanol:  HPLG grade.




 7.12.2   Trichlorophenol stock solution (1.0 mg/mL of Cl") :



 Dissolve 0.186 g of 2,4,6-trichlorophenol in 100 mL of



 halide-free methanol.




 7.12.3   Trichlorophenol calibration solutions.



 7.12.3.1  Place approximately 90 mL of reagent  water in each



 of  five  100-mL volumetric flasks.




 7.12.3.2 Using a calibrated micro-syringe or micro-pipets,



 add 2, 5,  10,  30,  and 80  //L of the trichlorophenol stock



 solution (Section  7.12.2)  to the volumetric flasks and



 dilute each to the mark with reagent water to produce



 calibration solutions of  2,  5,  10,  30,  and 80 ./zg Cl" per 100



 mL  of solution (20,  50, 100,  300,  and 800 /zg/L) .




 7.12.3.3   Some instruments  may have a calibration range that



 does not  extend to 800  /zg/L (80 ,tzg of Cl") .  For those



 instruments, a narrower dynamic range may be  used.   However,



 if  the concentration of halide in  a sample exceeds that .



 range, the  sample  must  be diluted  to bring the  concentration



within the  range calibrated.




 7.12.4  •Trichlorophenol precision  and recovery  (PAR)  test



 solution  (10 /zg/L  of  Cl") : Partially fill a 100-mL



volumetric  flask,,  add 10 itL of  the  stock  solution  (Section



 7.12.2),  and dilute  to  the  mark with reagent  water.



 7.13  Acetic acid  solution:  Containing  30  to  70% acetic acid




                             1032

-------
in deionized water, per the instrument manufacturer's



instructions.



8.0  Sample Collection, Preservation, and Storage




8.1  Sample preservation.



8.1.1  Residual chlorine: If the sample is known or



suspected to contain free chlorine, the chlorine must be



reduced to eliminate positive; interference that may result



from continued chlorination reactions.  A knowledge of the



process from which the sample is collected may be of value



in determining whether dechlorination is necessary.



Immediately after sampling, test for residual chlorine using



the following method or an alternative EPA method  (Reference




12) :



8.1.1.1  Dissolve a few crystals of potassium iodide in the



sample and add three to five drops of a 1% starch solution.



A blue color indicates the presence of residual chlorine.



8.1.1.2  If residual chlorine is found, add 1 mL of sodium



thiosulfate solution (Section 7.11) for each 2.5 ppm of free



chlorine or until the blue color disappears.  Do not add an



excess of sodium thiosulfate.1  Excess sodium thiosulfate may



cause decomposition of a small fraction of the OX.



8.1.2  Acidification: Adjust the pH of aqueous samples to <



2 with nitric acid.  Acidification inhibits biological



activity and stabilizes chemical degradation, including



possible dehalogenation reactions that may occur at high pH.



Acidification is necessary to facilitate thorough





                            1033

-------
adsorption.




8.1.3  Refrigeration: Maintain samples at a temperature of 0



to 4°C from time of collection until analysis.



8.2  Collect the amount of sample necessary for analysis



(Section 11) and all QC tests  (Section 9) in an amber glass



bottle of the appropriate size '(Section 6.1.1).



8.3  Analyze samples no less than three days nor more than



six months after collection.



9.0  Quality Control




9.1  Each laboratory that uses this method is required to



operate a formal quality assurance program.  The minimum



requirements of this program consist of an initial



demonstration of laboratory'capability, an ongoing analysis



of standards and blanks as tests of continued performance,



and analysis of matrix spike and matrix spike duplicate



(MS/MSD)  samples to assess accuracy and precision.



Laboratory performance is compared to established



performance criteria to determine if the results of analyses



meet the performance characteristics of the method.



9.1.1  The laboratory shall make an initial demonstration of



the ability to produce acceptable results with this method.



This ability is demonstrated as described in Section 9.2.



9.1.2  The laboratory is permitted to modify this method to



improve separations or lower the costs of measurements,



provided that all performance specifications are met.  Each



time a modification is made to the method, the laboratory is





                            1034

-------
required to repeat the procedures in Sections 9.-2.2 and 10



to demonstrate continued method performance.  If the



detection limit of the method will be affected by the



modification, the laboratory should demonstrate that the MDL



(40 CFR 136, Appendix B) is less than or equal to the MDL in



this method or one-third the; regulatory compliance level,



whichever is higher.



9.1.3  The laboratory shall spike 10% of the samples with



known concentrations of 2,4,6-trichlorophenol to monitor



method performance and matrix interferences  (interferences



caused by the sample matrix).  This test is described in



Section 9.3.  When results of these spikes indicate atypical



method performance for samples, the samples are diluted to



bring method performance within acceptable limits.   '



9.1.4  Analyses of blanks are required to demonstrate



freedom from contamination. ;The procedures and criteria for



analysis of blanks are described in Section 9.4.



9.1.5  The laboratory shall,!on an ongoing basis,



demonstrate through the analysis of the precision and



recovery (PAR) standard that'the analysis system is in



control.  These procedures are described in Section 9.10.



9.1.6  The laboratory shall perform quality control tests on



the granular activated carbon.  These procedures are



described in Section 9.5.



9.1.7  Samples are analyzed in duplicate to demonstrate



precision.   These procedures:are described in Section 9.6.





                            1035

-------
 9.2   Initial  demonstration of  laboratory capability.



 9.2.1 Method Detection Limit  (MDL):   To establish  the




 ability  to  detect AOX,  the laboratory should determine the



 MDL per  the procedure  in 40 CFR  136,  Appendix B using the



 apparatus,  reagents, and standards  that  will be used in the



 practice of this method.   An MDL.less than of equal to the



 MDL in Section 1.3  should be achieved prior to the practice



 of this  method.




 9.2.2  Initial precision and recovery (IPR): To establish



 the ability to generate acceptable  precision and recovery,



 the laboratory shall perform the following operations:



 9.2.2.1  Analyze four  aliquots of the PAR standard  .(Section



 7.12.4)  and a  method blank according  to  the procedures in



 Sections 9.4 and 11.




 9.2.2.2  Using the  blank-subtracted results of the set of



 four analyses,  compute  the  average  percent recovery (X)  and



 the standard deviation  of  the percent  recovery (s)  for the



 results.




 9.2.2.3  The average percent recovery shall be in the range



 of 81 to 114 /zg/L and the  standard  deviation shall be less



 than 8 //g/L.   If X  and  s meet these acceptance criteria,



 system performance  is acceptable and  analysis of blanks and



 samples may begin.  If, however, s  exceeds the precision



 limit or X  falls outside the range  for recovery,  system



performance is unacceptable.  In this  case, correct the



problem and repeat  the  test.           -






                             1036

-------
them to determine the concentration after  spiking.



9.3.2.1  Compute the percent recovery of each  analyte  in



each aliquot:



                , „        100 (Found - Background}
               % Recovery =	-
                                   T

               •where:

                    T is the  true value of the spike



9.3.2.2  Compute the relative percent difference  (RPD)



between the two results (not between the two recoveries)  as



described in Section 12.4.



9.3.2.3  If the RPD is less than 20%, and  the  recoveries for



the MS and MSB are  within the range of 78  to 116%,  the



results are acceptable.


9.3.2.4  If the RPD is greater than 20%, analyze  two



aliquots of the precision and recovery standard  (PAR).



9.3.2.4.1  If the RPD for the two aliguots of  the PAR  is



greater than 20%, the analytical system is out of control.



In this case, repair the  problem and repeat the analysis of



the sample batch, including the MS/MSD.


9.3.2.4.2  If, however, the RPD for the two aliquots of the



PAR is less than 20%, dilute !the sample chosen for the



MS/MSD by a factor  of 2 - 10 : (to remain within the working



range of the analytical system) and repeat the MS/MSD  test.



If the RPD is still greater than 20%, the  result  may not be



reported for regulatory compliance purposes.   In  this  case,



choose another sample for the MS/MSD and repeat analysis of



the sample batch.




                            1038

-------
preparation (Section  11.1).   If using the micro-column

procedure,  adsorb  the method  blank using two columns, as

described  in  Section  11.   Combust the GAG from each  column

separately, as  described  in Section 11.

9.4.1.3  If the result from the blank from the batch method

or the sum of the  results  from two columns is more than 20

/^g/L, analysis  of  samples  is  halted until the source of

contamination is eliminated and a blank shows no evidence of

contamination at this level.

9.4.2  Nitrate-washed GAG blanks: Analyzed daily to

demonstrate that the GAG is free from contamination.

9.4.2.1  Nitrate-washed GAG blank for the batch procedure:

Analyze a batch nitrate-washed GAG blank by adding a scoop
                                  *
of dry GAG  to the  assembled filter apparatus containing the

polycarbonate membrane and washing the GAG with the nitrate

wash solution (Section 7.10)  using the procedure in Section

11.2.6.

9.4.2.2  Nitrate-washed GAG blank for the column procedure:

Analyze a column nitrate-washed GAG blank .by assembling two

carbon columns  in  series and washing the columns with the

nitrate wash solution (Section 7.10)  using the procedure in

Section 11.3.4.2.  Analyze the GAG in each column

separately.  The results of the second analysis must be

within ±0.2 /zg  Cl"  of  the  first.  A difference greater than

0 .2 /zg Cl"  indicates a lack of homogeneity in the GAG that

could introduce unacceptable variability.   If the difference


                            1040

-------
exceeds this amount, the GAC\should be replaced.     '

9.4.3  The result for the reagent water blank  (Section

9.4.1) shall not exceed the result for the nitrate wash
                             I
blank  (Section 9.4.2.1 or 9.4.2.2) by more than 0.5 //g Cl".

9.5  Granular activated carbon  (GAC) .batch testing: Each lot

number or batch of activated carbon received from a supplier

is tested once before use to ensure adequate quality.  Use

only GAC that meets the test criteria below.

9.5.1  Contamination test: Analyze a scoop of GAC.  Reject

carbon if the amount of OX exceeds 1 /zg  (25 /zg Cl"/g) .

9.5.2  Inorganic chloride adsorption test: Attempt to adsorb

NaCl from 100 mL of a solution containing 100 mg/L in

reagent water.  Wash with nitrate solution and analyze.  The
                     •s
amount of halide should be less than 1 /^g Cl" larger than

the blank.  A larger amount indicates significant uptake of

inorganic chloride by the carbon.  Reject carbon if the 1 /-tg

level is exceeded.           '

9.6  Samples that are being used for regulatory compliance

purposes shall be analyzed in duplicate.

9.6.1  The procedure for preparing duplicate sample aliquots

is described in .Section 11.5.

9.6.2  Calculate the RPD by following the same procedure

described in Section 12.4.

9.6.3  If the RPD is greater than 20%, the analyses must be

repeated.

9.6.4  If the RPD remains greater than 20%, the result may


                            1041

-------
not be reported for regulatory compliance purposes.



9.7  The specifications in this method can be met if the



apparatus used is calibrated properly and maintained in a



calibrated state.  The standards used for calibration



(Section 10), calibration verification  (Section 9.9), and



for initial  (Section 9.2.2) and ongoing  (Section 9.10)



precision and recovery should be identical, so that the most



precise results will be obtained.



9.8  Depending1 on specific program requirements, field



duplicates may be collected to determine the precision of



the sampling technique.




9.9  At the beginning and end of each eight-hour shift




during which analyses are performed, system performance and



calibration are verified.  Verification of system



performance and calibration may be performed more



frequently, if desired.



9.9.1  If performance and calibration are verified at the



beginning and end of each shift (or more frequently),



samples analyzed during that period are considered valid.



9.9.2  If performance and calibration are not verified at



both the beginning and end of a shift (or more frequently),



samples analyzed during that period must be reanalyzed.



9.9.3  If calibration is verified at the beginning of a



shift,  recalibration using the five standards described in



Section 10.6 is not necessary; otherwise, the instrument



must be recalibrated prior to analyzing samples (Section






                            1042

-------
10) .



9.9.4  Cell maintenance and other changes to the analytical



system that can affect system performance may not be



performed during the eight-hour  (or shorter) shift.  :



9.10  Calibration verification and ongoing precision and



recovery: Calibration and system performance are verified by



the analysis of the 100 /ig/L PAR standard.



9.10.1  Analyze a blank  (Section 9.4) and analyze the PAR



standard (Section 7.12.4) immediately thereafter at the



beginning and end of each shift.  Compute the concentration



of organic halide in the blank and in the PAR standard using



the procedures in Section 12.  The blank shall be less than



2 fig Cl"  (20 />ig/L equivalent).



9.10.2  Subtract the result for the blank from the result of



the PAR standard using the procedures in Section 12, and



compute the percent recovery' of the blank-subtracted PAR



standard.  The percent recovery shall be in the range of 78



to 116%.



9.10.3  If the recovery is within this range, the analytical



process is in control and analysis of blanks and samples may



proceed.   If, however, the recovery is not within the



acceptable range, the analytical process is not in control.



In this event, correct the problem and repeat the ongoing



precision and recovery test ;(Section 9.10), or recalibrate



(Sections 10.5 through '10.6) .



9.10.4  If the recovery is nbt within the acceptable range






                            1043

-------
for the  PAR  standard analyzed at the end of the eight-hour




shift, correct  the problem, repeat the ongoing precision  and



recovery test  (Section  9.10), or recalibrate  (Sections  10.5



through  10.6),  and reanalyze the sample batch that was



analyzed during the eight-hour shift.




9.10.5   If the  recovery is within the acceptable range  at



the end  of the  shift, and samples are to be analyzed during



the next eight-hour shift, the end of shift verification may



be used  as the  beginning of shift verification for the



subsequent shift, provided the next eight-hour shift begins



as the first shift ends.




9.11  It is suggested but not required that the laboratory



develop  a statement of  data quality for AOX and develop QC



charts to form  a graphic demonstration of method



performance.  Add results that pass the specification in



Section  9.10.2  to initial and previous ongoing data.



Develop a statement of  data quality by calculating the



average percent recovery  (R)  and the standard deviation of



percent recovery  (sr) .   Express  the  accuracy as  a:recovery



interval from R - 2sr to R +  2sr.  For example, if R = 95%



and sr =  5%,  the accuracy  is  85  to 105%.



10.0  Calibration and Standardization




10.1 Assemble the OX system and establish the operating



conditions necessary for analysis.   Differences between



various makes and models of instruments will  require



different operating procedures.  'Laboratories should follow





                            1044

-------
the operating instructions provided by the manufacturer of

their particular instrument. ; Sensitivity, instrument

detection limit, precision, linear range, and interference

effects must be investigated ;and established for each

particular instrument.  Calibration is performed when the

instrument is first set up and when calibration cannot be

verified (Section.9.9).

10.2  Cell performance test: 'inject 100 /iL of the sodium

chloride solution (10 /xg Cl~;  Section 7.4)  directly into the

titration cell electrolyte.  Adjust the instrument to

produce a reading of 10 /ig Clr.     .                  ".

10.3  Combustion system test:; This test can be used to

assure that the combustion/micro-coulometer systems are

performing properly without introduction of carbon.  This

test should be used during initial instrument setup and when
                             -;
instrument performance indicates a problem with the

combustion system.


10.3.1  Designate a quartz boat for use with the ammonium

chloride (NH4C1)  solution only.

10.3.2  Inject 100 juL of the NH4C1  solution (Section 7.5)

into this boat and proceed with the analysis.

10.3.3  The result shall be between 9.5 and 10.5 /zg Cl".   If

the recovery is not between these limits, the combustion or

micro-coulometer systems are 'not performing properly.  Check

the temperature of the combustion system, verify that there

are no leaks in the combustion system, confirm that the cell



                            1045                     !

-------
is performing properly  (Section  10.2), and then repeat the



test.




10.4  Trichlorophenol combustion test: This test can be used



to assure that the combustion/micro-coulometer systems are



performing properly when carbon  is introduced.  It  should be



used during instrument  setup and when it is necessary to



isolate the adsorption  and combustion steps.



10.4.1  Inject 10 //L of the 1 mg/mL trichlorophenol stock



solution  (Section 7.12.2) onto one level scoop of GAC in a



quartz boat.




10.4.2 Immediately proceed with  the analysis to prevent loss



of trichlorophenol and to prevent contamination of the



carbon.




10.4.3  The result shall be between 9.0 and 11.0 /zg Cl".   If



the recovery is not between these limits, the



combustion/micro-coulometer system shall be adjusted and the



test repeated until the result falls within these limits.



10.5  Background level of Cl":  Determine  the  average



background level of Cl"  for the.entire  analytical  system as



follows:



10.5.1  Using the procedure in Section 11 (batch or column)



that will be used for the analysis of samples, determine the



background level of Cl"  in  each of  three  portions  of reagent



water.  The volume of reagent water used shall be the same



as the volume used for analysis of samples.



10.5.2  Calculate the average  (mean)  concentration of Cl"






                            1046

-------
and the standard deviation of the concentration.


10.5.3  The sum of the average concentration plus two times


the standard deviation of the concentration shall be less


than 20 /zg/L.  If not, the water or carbon shall be
                            i

replaced, or the adsorption system moved to an area free of


organic halide vapors, and the test (Section 10.5) shall be


repeated.  Only after this test is passed may calibration


proceed.


10.6  Calibration by external standard: A calibration line


encompassing the calibration range is developed using


solutions of 2,4,6-trichlorophenol.


10.6.1  Analyze each of the five calibration solutions


(Section 7.12.3) using the procedure in Section 11 (batch or


column) that will be used for the analysis of samples, and


the same procedure that was used for determination of the


system background  (Section 10-5) .  Analyze these solutions


beginning with the lowest concentration and proceeding to


the highest.  Record the response of the micro-coulometer to


each calibration solution.  :                         :


10.6.2  Prepare a method blank as described in Section 9.4.


Subtract the value of the blank from each of the five


calibration results, as described in Section 12.


10.6.3  Calibration factor  (ratio of response to


concentration) Using the blank subtracted results, compute


the calibration factor at each calibration point, and


compute the average calibration factor and the relative



                            1047

-------
standard  deviation  (coefficient of variation; Cv) of the



calibration  factor  over the calibration range.



10.6.4  Linearity:  The Cv of the calibration factor shall be



less than 20%; otherwise, the calibration shall be repeated



after adjustment of the combustion/micro-coulometer system



and/or preparation  of fresh calibration standards,




10.6.5  Using the average calibration factor, compute the



percent recovery at each calibration point.   The recovery at



each calibration point "shall be within the range of 80 to



111%.  If any point is not within this range, a fresh



calibration  standard shall be prepared for that point, this




standard  shall be analyzed, and the calibration factor




(Section  10.6.3) and calibration linearity (Section 10.6.4)



shall be  computed using the new calibration point.  All



points used  in the  calibration must meet the 80 to 111%



recovery  specification.



11.0 Procedure




11.1  Sample dilution: Many samples will contain high



concentrations of halide.  If analyzed without dilution, the



micro-coulometer can be overloaded,  resulting, in frequent



cell cleaning and downtime.  The following guidance is



provided to  assist  in estimating dilution levels.



11.1.1  Paper and pulp mills that employ chlorine bleaching:



Samples from pulp mills that use a chlorine  bleaching



process may  overload the micro-coulometer.   To prevent



system overload, the maximum volume suggested for paper





                            1048

-------
industry samples that employ halide in the bleaching process



is 100 mL.  An adsorption volume as small as 25 mL may be



used, provided the concentration of AOX in the sample can be



measured reliably, as defined by the requirements in Section



9.11.  To minimize volumetric: error, an adsorption volume



less than 25 mL may not be used.  If AOX cannot be measured



reliably in a 100-mL sample volume, a sample volume to a



maximum of 1000 mL must be used.  The sample and adsorption



volumes are suggested for paper industry samples employing



chlorine compounds in the bleaching process:

1
Paper or pulp mill stream
i
Evaporator condensate
Process water
Pulp mill effluent
Paper mill effluent
-ombined mill effluent
Combined bleach effluent ;
2- stage filtrate ;
E-stage filtrate

Sample
volume
(mL) *
100
100
30
10
5
1
0.5
0.5
Adsorp-
tion
volume
(mL)
100
100
50
25
25
25
25
25
* Assumes dilution to final volume of 100 mL.
All sample aliquots (replicates, diluted
samples) must be analyzed using the same fixed
final volume (sample volume plus reagent water,
as needed) .
11.1.2  Sample dilution procedure.




11.1.2.1  Partially fill a precleaned volumetric flask with



pH < 2 reagent water, allowing for the volume of sample to



be added.



                            1049

-------
 11.1.2.2   Mix sample  thoroughly by tumbling or shaking



 vigorously.




 11.1.2.3   Immediately withdraw the required sample aliquot



 using a pipet or micro-syringe.




 Note: Because it will be necessary to rinse the pipet or




 micro-syringe (Section  11.1.2.5) , it may be necessary to




 pre- calibrate the pipet or micro-syringe to assure that the




 exact volume  desired  will be delivered.




 11.1.2.4   Dispense or inject the aliquot into the volumetric



 flask.




 11.1.2.5   Rinse the pipet or syringe with small portions of



 reagent water and add to the flask.




 11.1.2.6   Dilute to the mark with pH < 2 reagent water.



 11.1.3  All samples to be reported for regulatory compliance



 monitoring purposes must be analyzed in duplicate, as



 described  in  Section  11.5.




 11.1.4  Pulp  and Paper in-process samples:  The concentration



 of organic halide in  in-process samples has been .shown to be



 20 to 30%  greater using the micro-column adsorption



 technique  than using  the.batch adsorption technique.   For



 this reason,  the micro-column technique shall  be used for



monitoring in-process samples.   Examples of in-process



 samples include": combined bleach plant effluent,  C-stage



 filtrate,   and E-stage filtrate.



 11.2  Batch adsorption and filtration.
                            1050

-------
11.2.1  Place the appropriate volume of sample (diluted if



necessary), preserved as described in Section 8,  into an



Erlenmeyer flask.



11J2.2  Add 5 mL of nitrate stock solution to the sample




aliquot.



11.2.3  Add one level scoop of activated carbon that has



passed the quality control tests in Section 9.



11.2.4  Shake the suspension I for at least one hour in a




mechanical shaker.



11.2.5  Filter the suspension through a polycarbonate



membrane filter.  Filter by suction until the liquid level



reaches the top of the carbon.



11.2.6  Wash the inside surface of the filter funnel with 25



mL  (±5 mL) of nitrate wash splution in several portions.



After the level of the final;wash reaches the top of the



GAG, filter by suction until,the cake is barely dry. i The



time required for drying should be minimized to prevent



exposure of the GAG to halogen vapors in the air, but should



be sufficient to permit drying of the cake so that excess



water is not introduced into the combustion apparatus.  A



drying time of approximately:10 seconds under vacuum has



been shown to be effective for this operation.



11.2.7  Carefully remove the;top of the filter holder,



making sure that no carbon is lost.  This operation is most



successfully performed by removing the clamp, tilting the



top of the filter holder  (the funnel portion) to one side,





                            1051

-------
and lifting upward.




11.2/8  Using a squeeze bottle or micro-syringe, rapidly



rinse the carbon from the inside of the filter holder onto



the filter cake using small portions of wash solution.



Allow the cake to dry under vacuum for no more than 10




seconds after the final rinse.  Immediately turn the vacuum



off.




11.2.9  Using tweezers, carefully fold the polycarbonate



filter in half, then in fourths, making sure that no carbon



is lost.



11.3  Column adsorption.




11.3.1  Column.preparation: Prepare a sufficient number of



columns for one day's operation as follows:



11.3.1.1  In a glove box or area free from halide vapors,



place a plug of Cerafelt into the end of a clean glass



column.



11.3..1.2  Fill the glass column with one level scoop



(approximately 40 mg)  of granular activated carbon that has



passed the quality control tests in Section 9.



11.3.1.3  Insert a Cerafelt plug into the open end of the



column to hold the carbon in place.



11.3.1.4  Store the columns in a glass jar with PTFE lined



screw-cap to prevent infiltration of halide vapors from the



air.



11.3.2  Column setup.




11.3.2.1  Install two columns in series in the adsorption






                            1052

-------
module.



11.3.2.2  If the sample is known or expected to contain



particulates that could prevent free flow of sample through



the micro-columns, a Cerafelt plug is placed in the tubing



ahead of the columns.  If a Measurement of the OX content of



the particulates, is desired, the Cerafelt plug can be washed



with nitrate solution, placed in a combustion boat, and



processed as a separate sample.                 .     •



11.3.3  Adjusting sample flow rate: Because the flow'rate



used to load the sample onto the columns can affect the



ability of the GAG to adsorb: organic halides, the flow rate



of the method blank is measured, and the gas pressure used



to process samples is adjusted accordingly.  The flow rate



of the blank, which is composed of acidified reagent water



and contains no particulate matter, should be greater than



the flow rate of any sample 'containing even small amounts of



particulate matter.         \



11.3.3.1  Fill the sample reservoir with the volume of



reagent water chosen for the analysis (Section 9.4.1.2)  that



has been preserved and acidified as described in Section 8.



Cap the reservoir.



11.3.3.2  Adjust the gas pressure per the manufacturer's



instructions.  Record the time required for the entire   • •



volume of reagent water to pass through both columns.  The



flow rate must not exceed 3 piL/min over the duration of the



time required to adsorb the volume.  If this flow rate is





                            1053

-------
 exceeded,  adjust gas pressure,  prepare  another blank,  and



 repeat  the adsorption.



 11.3.3.3   Once the flow rate for  the blank has been



 established,  the same adsorption  conditions must be applied



 to  all  subsequent samples  during  that eight-hour shift,  or



 until another method blank is processed, whichever  comes



 first.  To aid in overcoming breakthrough problems,  a  lower



 gas pressure  (and,  therefore, flow rate) may be used for



 processing of samples,  if  desired.  If  the sample adsorption



 unit is disassembled or cleaned,  the flow rate must  be



 checked before processing  additional samples. '••



 11.3.3.4   Elute the  pair of  columns with 2 mL  of nitrate



 wash solution.   The  flow rate of  nitrate wash  solution must



 not exceed 3  mL/min.



 11.3.3.5   Separate the  columns and mark for subsequent



 analysis.
                                  &


 11.3.4  The adsorption  of  sample volumes is performed in a



 similar fashion.  Fill  the sample reservoir with the sample



volume chosen for the analysis  (Section 11.1), that has  been



preserved  as  described  in  Section 8.   All analyses must  be



performed with  this volume  (sample volume plus reagent



water,  as needed) in order to maintain a flow rate no



greater than  that determined for the blank (see Section



11.3.3) .



11.3.4.1  Use the same gas pressure for sample adsorption as



is used for the blank.
                            1054

-------
11.3.4.2  Elute the columns with 2 mL of the nitrate wash


solution.                    '

11.3.4.3  Separate the columns and mark for subsequent


analysis.

11.3.5  If it is desirable to make measurements at levels


lower than can be achieved with the sample volume chosen, or  ,


if the instrument response of an undiluted sample is less


than three times the instrument response of the blank


(Section 12.6.3), a larger sample volume must be used.


11.4  Combustion and titration.

11.4.1  Polycarbonate filter Jand GAG from batch adsorption.


11.4.1.1  Place the folded polycarbonate filter containing


the GAG in a quartz combustion boat, close the airlock, and


proceed with the automated sequence.                             dttk


11.4.1.2  Record the signal from the micro-coulometer for a


minimum integration time of 10 minutes and determine the


concentration of Cl" from calibration data,  per Section 12.
                                                                 t

11.4.2  Columns from column adsorption.

11.4.2.1  Using the push rod, push the carbon and the

Cerafelt plug(s) from the first column into a combustion


boat.  Proceed with the automated sequence.


11.4.2.2  Record the signal from the micro-coulometer for a


minimum integration time of 10 minutes and determine the

concentration of Cl" for the first column from calibration


data, per Section 12.

11.4.2.3  Repeat the automated sequence with the second



                            1055

-------
 column.




 11.4.2.4  Determine  the  extent of breakthrough  of  organic



 halides from  the  first column to the  second  column,  as



 described in  Section 12.




 11.4.3  The two columns  that are used for the method blank



 must be combusted separately, as is done for samples.




 11.5   Duplicate sample analysis: All  samples to be reported



 for regulatory compliance purposes must be analyzed  in



 duplicate.  This  requirement applies  to both the batch and .



 column adsorption procedures.  In addition,  if it is



 necessary to  dilute  the  sample for the purposes of reducing



 breakthrough  or maintaining the concentration within the



 calibration range, a more or less dilute sample must be




 analyzed.   The adsorption volumes used for analysis of



 undiluted samples, diluted samples,  and all  replicates must



 be the same as the volume used for QC tests  and calibration



 (Sections 9 and 10).




 11.5.1  Using results from analysis of one sample volume



 (Section 11.4) and the procedure in Section  11.1.2,•



 determine if the dilution used was within the calibration



 range of the instrument and/or if breakthrough exceeded the



 specification in Section 12.3.1.   If the breakthrough



 criterion was exceeded or the sample was not within 'the



 calibration range, adjust the dilution volume as needed.   If



the breakthrough criterion was not exceeded.and the sample



dilution was within the calibration range,  a second volume






                            1056

-------
at the same dilution level may be used.

11.5.2  Adsorb  the  sample using the same technique  (batch or

column) used  for the first sample volume.  Combust the GAG

from the second volume as described in Section 11.4, :and

calculate the results as described in Section 12.  Compare

the results of  the  two analyses as described in  Section

12.4.                             .

11.5.3  Duplicate analyses are not required for  method

blanks, as different dilution levels are not possible.

11.5.4  Duplicate analyses of the PAR standard used for

calibration verification  (Section 9.10) are not  required.

12.0 Data Analysis  and Calculations

12.1  Batch Adsorption Method: Calculate the blank-

subtracted concentration of adsorbable organic halide

detected in each sample  (in micrograms of chloride per

liter) using  the following equation:                 '

                       AOX (jig/L) = (C ~vB}

  •where:
  C = \ig Cl' from  micro-coulometer for the sample
  B = [ig Cl' from  micro-coulometer for the reagent water blank (Section 9.4.1)
  V = volume of sample in liters    !
This  calculation is performed for each of the two dilution

levels analyzed for each  sample.

12/2  Column  Adsorption Method: Calculate the blank-

subtracted concentration  of 'adsorbable organic halide

detected in each sample  (in micrograms of chloride  per

liter) using  the following equation:

                             1057

-------
                                [(C.+C_) -(£+£,)]
                      AOX (jig/L) = —l-	2—-1	2—
   •where:
   C, = lig CI~ from micro-coulometer for first column from the sample
   C2 = p.g Cl' from micro-coulometer for second column from the sample
   #1 = V-g from micro-coulometer for first column from the reagent -water blank (Section 9.4.1)
   B2 - fig Cl' from micro-coulometer for second column from the reagent -water blank (Section 9.4.1)
   V = volume of sample in liters
12.3   Percent breakthrough:  For each sample analyzed  by the

column method,  calculate the percent breakthrough of  halide

from  the first  column to the second column,  using the
following equation:

                                   (C, - 5-H100)
                 % Breakthrough  -
12.3.1   For samples to be reported for regulatory compliance
purposes,  the percent breakthrough must be  less than  or

equal to 25% for  both of the  two analyses performed on each

sample  (see Section 11.5).

12,3.2   If the breakthrough exceeds 25%, dilute the affected
sample  further, maintaining the amount of halide at least

three times higher than the level of blank,  and reanalyze

the  sample.  Ensure that the  sample is also analyzed  at a
second  level of dilution that is at least a factor of 2

different   (and still higher than three times the blank).

12.4  Relative percent difference (RPD): Calculate the

relative percent  difference between the results'of the two

analyses of each  sample, using the following equation:

                              1058

-------
                    RPD =
                           \fAOX l + AOXJ]
12.5  High concentrations of AOX: If the amount of halide



from either analysis exceeds the calibration range, dilute



the sample and reanalyze, maintaining at least a factor of 2



difference in the dilution levels of the two portions of the .



sample used.



12.6  Low concentrations of AOX: The blank-subtracted final



result from the batch procedure or the sum of the blank-



subtracted results from the two carbon columns should be



significantly above the level of the blank.



12.6.1  If the instrument response for a sample exceeds the



instrument response for the blank by a factor of at least 3,



the result is acceptable.



12.6.2  If the instrument response for a sample is less than



three times the instrument response for the blank, and the



sample has been diluted, analyze a less dilute aliquot of



sample.



12.6.3  If the instrument response of an undiluted sample



containing AOX above the minimum level is less than three        .



times the instrument response for the blank,  the result is



suspect and may not be used for regulatory compliance



purposes.  In this case, find the cause of contamination,



correct the problem, and reanalyze the sample under the          ;



corrected conditions.                                             '






                            1059                                 ^^

-------
12.7  Report results that meet all of the specifications  in



this method as the mean of the blank-subtracted values  from



Section 12.1 or 12.2 for the two analyses at different



dilution levels, in /ug/L of Cl~ (not as 2,4,6-




trichlorophenol), to three significant figures.  Report the



RPD of the two analyses.  For samples analyzed by the column



procedure, also report the percent breakthrough.



13.0  Method Performance




The specifications contained in this method are based on



data from a single laboratory and from a large-scale study



of the pulp and paper industry.         -'



14.0 Pollution Prevention




14.1  The solvents used in this-.method pose little threat to



the environment when recycled and managed properly.



14.2  Standards should be prepared in volumes consistent



with laboratory use to minimize the volume of expired



standards to be disposed.



15.0 Waste Management




15.1  It is the laboratory's responsibility to comply with



all federal,  state,  and local regulations governing waste



management, particularly the hazardous waste identification



rules and land disposal restrictions, and to protect the



air,  water, and land by minimizing and controlling all



releases from fume hoods and bench operations.  Compliance



with all sewage discharge permits and regulations is also
                            1060

-------
required.                    '                        ;



15.2  Samples preserved with HC1 or H2SO4  to pH  <  2  are



hazardous and must be neutralized before  being  disposed, or



must be handled as hazardous waste.  Acetic acid  and silver



acetate solutions resulting from cell flushing  must be



disposed of in accordance with all applicable federal,,
                             !•


state, and local regulations.



15.3  For further information on waste management,  consult



"The Waste Management Manual .for Laboratory Personnel," and



"Less is Better: Laboratory Chemical Management for Waste



Reduction," both available from the American Chemical



Society's Department of Government Relations and  Science



Policy, 1155 16th Street N.W.-, Washington, B.C. 20036'.
                            1061

-------
16.0 References




16.1   "Total Organic Halide,  Methods  450.1--Interim,"




Prepared by Stephen Billets and James J.  Lichtenberg, USEPA,



Office of Research and Development, Physical and  Chemical



Methods Branch, EMSL-Cincinnati,  Cincinnati, OH 45268, EPA



600/4-81-056  (1981).




16.2  Method 9020, USEPA Office of Solid  Waste, "Test



Methods for Evaluating Solid  Waste, SW-846," Third Edition,



1987.




16.3   "Determination of Adsorbable Organic Halogens  (AOX),"



"German Standard Methods for  the Analysis of Water, Waste



Water and Sludge--General Parameters  of Effects and



Substances," Deutsche Industrie Norm  (DIN) Method 38 409,



Part 14, DIN German Standards Institute, Beuth Verlag,



Berlin, Germany (1987).




16.4   "Water Quality:  Determination  of Adsorbable Organic



Halogens (AOX)," International  Organization for



Standard/Draft International  Standardization (ISO/DIS)



Method 9562 (1988).




16.5  "Organically Bound Chlorine by  the AOX Method," SCAN-W



9:89, Secretariat,  Scandinavian Pulp,  Paper and Board



Testing Committee,  Box 5604, S-11486,  Stockholm,  Sweden



(1989)  .




16.6  Method 5320,  "Dissolved Organic Halogen," from



"Standard Methods for the Examination of Water and



Wastewater," 5320,  American Public Health Association, 1015





                            1062

-------
15th St. NW, Washington, DC 2|0005  (1989) .

16.7  "Canadian Standard Method for the Determination of

Adsorbable Organic Halides  (AOX) in Waters and Wastewaters,"
                                                     l
Environment Canada and The Canadian Pulp and Paper   >

Association  (1990).

16.8  40 CFR Part 136, Appendix B.

16.9  "Working with Carcinogens," DHEW, PHS, CDC, NIOSH,

Publication 77-206,  (Aug 1977).

16.10   "OSHA Safety and Health Standards, General Industry"

OSHA 2206, 29 CFR 1910  (Jan 1976) .

16.11   "Safety in Academic Chemistry Laboratories," ACS

Committee on Chemical Safety  (1979).

16.12   "Methods 330.4 and 330.5 for Total Residual

Chlorine," USEPA, EMSL-Cincinnati, Cincinnati, OH 45268,

EPA-4-79-020  (March 1979).

16.13   "Validation of Method  1650: Determination of Organic

Halide," Analytical Technologies Inc., ERCE Contract 87-

3410,'November 15, 1990.  Available from the EPA Sample

Control Center, DynCorp, 300 IN. Lee St., Alexandria, VA

22314  (703-519-1140) .

17.0 Figures
                            1063

-------
            a.
                       b.  Dohrmann
                                                                              c. Euroglas
Silver
Sensor
Electrode
  Silver/Silver
  Chloride
  Reference
  Electrode
                          Gases
                          In
Platinum
Electrode

Silver
Generator
Electrode
                   Gases
                   Out   '
Silver/Silver
Acetate
Reference
Electrode
              Stirrer
                                      Gases
      Silver
      Sensor
      Electrode
                                                          Gases
                                                          In
Silver
Generator
Electrode

Platinum
Electrode
            Silver
            Generator
            Electrode
           Gases Infcd
                                   Platinum
                                   Electrode
                                                No Stirrer
                                                                  Silver
                                                                  Sensor
                                                                  Electrode
Silver/Silver
Chloride
Reference
Electrode
                   Figure 1.  Microcoulometric Titration Cells (from Reference 7)


                                                     1064

-------
Funnel
Clamp
Stain tess-
S-feeI Support


PTFE Gasket


Base	
No. 5
Stopper.
          Figure 2. Filter Apparatus

                  1065

-------
     Sample
     Reservoir
     (1of4)
   GAG Column 1
   <3AC Column 2
              I
                                                  Nit rate Wash
                                                  Reservoir
Figures. Schematic of the Column Adsorption System

                       1066

-------
           1235
            11
 1.
 2.
 3.
 4.
 5.
 6.
 7.
10.
11.
1 2.
   Stripping Devfce
   Sample inlet for AOX
   AOX Sample
   Furnace
   Combustion Tube              :
   Absorber-fifed with HjSO^       |
   Tltratfoncell
S.  Working electrodes
9.  Measuring electrodes
   St'ner
   Tftraction mfc ro -processor
   Gas flow and tern pe ratu le contio I device
          Figure 4. Schematic of an AOX Apparatus

                              1067

-------
18. 0  Glossary of Definitions and Purposes




     These definitions and purposes are specific to this



     method but have been conformed to common usage as much



     as possible.




18.1  Units of weight and measure and their abbreviations.



18.1.1  Symbols.




           °C     degrees  Celsius



           /u<3     microgram



           //L     microliter



           <      less than



           >      greater  than




           %      percent



 18.1.2  Alphabetical characters.



           cm     centimeter



           g      gram



           h      hour




           ID     inside diameter



           in     inch



           L      liter



           m      meter



           mg     milligram



           min    minute



           mL     milliliter



           mm     millimeter



           N      normal;  gram molecular weight of solute



                  divided  by hydrogen equivalent of solute,





                            1068

-------
                 per  liter of  solution

           OD    outside diameter
                            i
           ppb   part-per-billion

           ppm   part-per-million

           ppt   part-per-trillion

           psig  pounds-per-square  inch gauge

           v/v   volume per iunit volume

           w/v   weight per 'unit volume

18.2  Definitions and acronyms  (in alphabetical order).

                 Analyte:  AOX tested for by this method.

                 Calibration standard  (CAL):  A  solution

           prepared from a secondary standard and/or  stock

           solution which is; used to calibrate the response

           of the instrument! with respect to analyte

           concentration.   ;

                 Calibration verification standard  (VER):

           The mid-point calibration standard  (CSS)  that is

           used to verify calibration.

                 Field blank:  An aliquot of reagent  water

           or other reference matrix that is placed in a

           sample container in the laboratory or the  field,

           and treated as a sample in all respects,

           including  exposure to sampling site conditions,

           storage, preservation, and all analytical

           procedures.  The purpose of the field blank is

           to determine if the field or sample transporting



                            1069

-------
procedures and environments have contaminated



the  sample.




       IPR:   Initial  precision and  recovery;  four



aliquots of  the diluted PAR standard analyzed  to



establish the ability to generate  acceptable



precision and accuracy. An IPR is  performed



prior  to the first time this method is used and



any  time the method  or instrumentation is



•modified.




       Laboratory blank:  See Method blank.



       Laboratory control sample  (LCS):   See



Ongoing precision and recovery sample  (OPR).



       Laboratory reagent blank:  See Method



blank..




       May:   This action, activity, or procedural



step is neither required nor prohibited.



       May not:  This action, activity, or



procedural step is prohibited.



       Method blank:  An aliquot of reagent water



that is treated exactly as a sample including



exposure to all glassware,  equipment,  solvents,



reagents, internal standards,  and surrogates



that are used with samples.  The method blank is



used to determine if analytes or interferences



are present in the laboratory environment,  the



reagents, or the apparatus.






                 1070

-------
      Minimum  level  (ML):  The level at which

the entire analytical system must give a

recognizable signal and acceptable calibration

point for the analyte. It is equivalent to the

concentration of the lowest calibration

standard, assuming that all method-specified

sample weights, volumes, and cleanup procedures

have been employed.

      Must:  This| action, activity, or

procedural step is required.

      OPR:  Ongoing precision and recovery

standard; a laboratory blank spiked with a known

quantity of analyte. The OPR is analyzed exactly

like a sample.  Its purpose is to assure that the

results produced by the laboratory remain within

the limits specified in this method for

precision and recovery.

      PAR:  Precision and recovery standard;

secondary standard that is diluted and spiked to

form the IPR and OPR.

      Preparation;blank:  See Method blank.

      Primary  dilution standard:  A solution
                  t
containing the specified analytes that is

purchased or prepared from stock solutions and

diluted as needed;to prepare calibration  '

solutions and other solutions.


                 1071

-------
       Quality control  check sample  (QCS):   A



sample containing all  or a  subset of the



analytes at known concentrations. The QCS is



obtained from a source external to the



laboratory or is prepared from a source of



standards different from the source of



calibration standards.  It  is used to check



laboratory performance with test materials



prepared external to the normal preparation



process.




       Reagent water:   Water demonstrated to  be



free from the  analyte  of interest and




potentially interfering substances at the method



detection limit for the analyte.



       Relative standard deviation  (RSD):  The



standard deviation multiplied by 100, divided by



the mean.




    .   RSD:  See Relative standard deviation.



       Should:  This action, activity, or



procedural step is suggested but not required.



       Stock solution:  A solution^ containing an



analyte that is prepared using a reference



material traceable to EPA,  the National



Institute of Science and Technology (NIST),  or a



source that will attest to the purity and



authenticity of the reference material.






                 1072

-------
      VER:  See Calibration verification



standard.
                 1073

-------
                         Method 1653




             Chlorinated Phenolics in Wastewater



               by In Situ Acetylation and GCMS



 1.0   Scope and Application




 1.1   This  method is  for determination of  chlorinated



 phenolics  (chlorinated  phenols, guaiacols,  catechols,



 vanillins,  syringaldehydes) and other compounds  associated



 with  the Clean Water Act;  the Resource Conservation and



 Recovery Act;  and the Comprehensive Envirpnmental Response,



 Compensation,  and Liability Act; and that are amenable  to  in




 situ  acetylation, extraction, and analysis by capillary




 column gas  chromatography/mass spectrometry  (GCMS).  This



 method is based  on existing methods for determination of



 chlorophenolics  in pulp and paper industry wastewaters



 (References 1  and 2) .




 1.2   The chemical compounds listed in Table 1 may be



 determined  in waters and,  specifically,  in in-process



 streams and wastewaters associated with the pulp and paper



 industry.  The method is designed to meet the survey and



monitoring requirements of the Environmental Protection



Agency (EPA) .  < •




 1.3  The detection limit of this method is usually dependent



on the level of interferences rather than instrumental



limitations. The method detection limits (MDLs)  in Table 2
                            1074

-------
typify the minimum quantity that can be detected with no


interferences present.           .


1.4  The GCMS portions of this method are for use only by-


persons experienced with GCMS or under the close supervision


of such qualified persons.  Laboratories unfamiliar with


analyses of environmental samples by GCMS should run the


performance tests in Reference 3 before beginning.


1.5  Any modification of the method beyond those expressly


permitted is subject to the application and approval of


alternative test procedures under 40 CFR Parts 136.4 and


136.5.


2.0  Summary of Method



2.1  A 1000-mL aliquot of water is spiked with stable


isotopically labeled analogs: of the compounds of interest


and an internal standard.  The solution is adjusted to


neutral pH, potassium carbonate buffer is added, and the pH


is raised to 9 - 11.5.   The chlorophenolics are converted in
                            I                         '


situ to acetates by the addition of acetic anhydride.  After



acetylation, the solution is, extracted with hexane.  The


hexane is concentrated to a final volume of 0.5 mL, an


instrument internal standard is added, and an aliquot of the


concentrated extract is injected into the gas chromatograph
                            I             -            -

 (GC).  The compounds are separated by GC and detected by a


mass spectrometer  (MS)  .  The' labeled compounds and internal


standard serve to correct this variability of the analytical
                             1075

-------
 technique.




 2.2   Identification of a pollutant  (qualitative  analysis)  is



 performed by comparing the relative  retention time  and mass



 spectrum to that  of an authentic  standard.  A compound is



 identified  when its relative  retention time and  mass



 spectrum agree.




 2.3   Quantitative analysis is performed in one of two ways



 by GCMS  using extracted ion-current  profile  (EICP)  areas:



 (1) For  those compounds listed  in Table 1 for which



 standards and labeled  analogs are available,  the GCMS system



 is calibrated and the  compound  concentration  is  determined



 using an isotope  dilution technique;  (2) for  those  compounds



 listed in Table 1 for  which authentic  standards  but no.



 labeled  compounds are  available,  the GCMS system is



 calibrated  and the compound concentration is  determined



 using an internal standard technique.




 2.4   Quality  is assured through reproducible  calibration and



 testing  of  the extraction and GCMS systems.



 3.0   Definitions




 3.1   Chlorinated  phenolics  are the chlorinated phenols,



guaiacols,  catechols, vanillins,  syringaldehydes and other



 compounds amenable  to  in situ acetylation,  extraction,  and




determination by  GCMS using this method.




3.2  Definitions  for other terms used-in this method are



given in  the glossary at  the end of the method (Section



20.0).




                            1076

-------
4.0  Interferences           ;
                             !                        "-

4.1  Solvents, reagents, glassware, and other sample

processing hardware may yield artifacts and/or elevated

baselines, causing misinterpretation of chromatograms and

spectra.  All materials used,in the analysis shall be
                             t
demonstrated to be free from interferences under the

conditions of analysis by running method blanks initially

and with each sample batch  (samples started through the

extraction process on a given eight-hour shift, to a maximum

of 20).  Specific selection of reagents and purification of
                             !
solvents by distillation in all-glass systems may be

required.  Glassware and, where possible, reagents are

cleaned by using solvent rinse and baking at 450°C for a

minimum of one hour.

4.2  Interferences co-extracted from samples will vary

considerably from source to source, depending on the

diversity of the site being sampled.  Industry experience

suggests that high levels of'non-chlorinated phenols may

cause poor recovery of the compounds of interest,

particularly in samples collected in the vicinity of a

source of creosote, such as a wood-preserving plant

 (Reference 1).               ,

4.3  The internal standard, 3,4,5-trichlorophenol, has been

reported to be an anaerobic degradation product of   '

2,3,4, 5-tetrachlorophenol and/or pentachlorophenol

 (Reference 1) '.  When an interference with this or another


                             1077

-------
 compound occurs,  labeled pentachlorophenol or another



 labeled  compound  may.be used as an alternative internal



 standard; otherwise, the internal standards and reference



 compounds must be used as specified in this method.




 4.4  Blank contamination by pentachlorophenol has been



 reported (Reference 1) to be traceable to potassium



 carbonate; it has also been reported that this contamination



 may be removed by baking overnight at 400 to 500°C.



 4.5  Catechols are susceptible to degradation by active



 sites on injection port liners and columns, and are subject




 to oxidation to the corresponding chloro-o-benzoquinones




 (Reference 2) .  A small amount of ascorbic acid may be added




 to samples to prevent auto-oxidation (Reference 2; also see



 Section  11.1.6).  For pulp and paper industry samples,



 ascorbic acid may be added to treated effluent samples only.



 5.0  Safety




 5.1  The toxicity or carcinogenicity of each compound or



 reagent used in this method has not been precisely



 determined; however,  each chemical compound should be



 treated as a potential health hazard.   Exposure to these



 compounds should be reduced to the lowest possible level.



The laboratory is responsible for maintaining a current



awareness file of OSHA regulations regarding the safe



handling of the chemicals specified in this method.  A



reference file of materials safety data sheets (MSDSs)



should be made available to all personnel involved in these




                            1078

-------
analyses.  Additional information on laboratory safety can



be found in References 4 through 6.



5.2  Samples may contain high concentrations of toxic



compounds, and should be handled with gloves and a hood



opened to prevent exposure.



6.0  Equipment and Supplies




Note:  Brand names, suppliers, and part numbers are for




illustrative purposes only. [NO endorsement is implied.




Equivalent performance may be achieved using apparatus and




materials other than those specified here, but demonstration    ;




of equivalent performance that meets the requirements of




this method is the responsibility of the laboratory.





                            l

6.1.1  Sample bottles and caps.



6.1.1.1  Sample bottle: Amber glass, 1000-mL minimum, with



screw-cap.  If amber bottles'are not available, samples



shall be protected from light.



6.1.1.2  Bottle caps: Threaded to fit sample bottles.  Caps



shall be lined with PTFE.
                            !                         ,


6.1.1.3  Cleaning bottles: Detergent water wash, cap with



aluminum foil, and bake at 450°C for a minimum of one hour



before use.



6.1.1.4  Cleaning liners: Detergent water wash, reagent


                            !                         '           •
water  (Section 7.4) and solvent rinse, and bake at



approximately 200°C for a minimum of 1 hour prior to use.



                            1079

-------
6.1.1.5  Bottles  and  liners must be  lot-certified to be  free



of chlorophenolics by running blanks according to this



method.  If blanks from bottles and/or liners without



cleaning or with  fewer cleaning steps show no detectable



chlorophenolics,  the  bottle and liner .cleaning steps that do



not eliminate chlorophenolics may be omitted.



6.1.2  Compositing equipment: Automatic or manual



compositing system incorporating glass containers cleaned



per bottle cleaning procedure above.  Sample containers are



kept at 0 to 4°C during sampling.   Glass or PTFE tubing only



shall be used.  If the sampler uses a peristaltic pump, a



minimum length of compressible silicone rubber tubing may be



used in the pump only.  Before use, the tubing shall be



thoroughly rinsed with methanol, followed by repeated



rinsing with reagent water (Section 7.4)  to minimize sample



contamination.  An integrating flow meter is used to collect



proportional composite samples.



6.2  Extraction apparatus.



6.2.1  Bottle or beaker: 1500- to 2000-mL capacity.



6.2.2  Separatory funnel: 500- to 2000-mL, glass, with PTFE



stopcock.




6.2.3  Magnetic stirrer: Corning Model 320,  or equivalent,



with stirring bar.                          -



6.3  Polyethylene gloves: For handling samples and



extraction equipment  (Fisher 11-394-110-B, or equivalent).



6.4  Graduated cylinders: 1000-mL,  100-mL, and 10-mL






                            1080

-------
nominal.

6.5  Centrifuge: Capable of accepting 50-mL centrifuge tubes

and achieving 3000 RPM.      \

6.5.1  Centrifuge tubes.     |

6.5.1.1  35-mL nominal, with PTFE-lined screw-cap.

6.5.1.2  15-mL nominal, conical graduated, with ground-glass

stopper.

6.6  Concentration apparatus 1

6.6.1  Kuderna-Danish  (K-D) concentrator tube: 10-mL,

graduated  (Kontes K-570050-1025, or equivalent) with

calibration verified.  Ground-glass stopper (size 19/22

joint) is used to prevent evaporation of extracts.
                             I
6.6.2  Kuderna-Danish  (K-D) evaporation flask: 1000-mL

(Kontes K-570001-1000, or equivalent), attached to

concentrator tube with springs  (Kontes K-662750-0012).

6.6.3  Snyder column: Three-ball macro  (Kontes

K-503000-0232, or equivalent).

6.6.4  Snyder column: Two-ball micro  (Kontes K-469002-0219,

or equivalent).

6.6.5  Boiling chips: Approximately 10/40 mesh, extracted

with methylene chloride and baked at 450°C for a minimum of

one hour.                    ;

6.6.6  Nitrogen evaporation apparatus: Equipped with a water

bath controlled at 35 to 40°C (N-Evap, Organomation

Associates, Inc., South Berlin, MA, or equivalent),
                         *    I
installed in a fume hood.  This device may be used in place


                             1081

-------
 of  the micro-Snyder column concentrator in Section 6.6.4



 above.




 6.7 Water bath:  Heated,  with concentric ring cover,  capable



 of  temperature control  (+ 2°C),  installed in  a  fume hood.



 6.8 Sample vials:  Amber  glass,  1-  to 3-mL, with PTFE-lined



 screw-cap.



 6.9 Balances.




 6.9.1   Analytical:  Capable of weighing 0.1 mg.



 6.9.2   Top loading:  Capable of weighing 10 mg.



 6.10  pH meter.




 6.11  Gas  chromatograph:  Shall have splitless or on-column




 injection  port  for  capillary column,  temperature program



 with 50°C hold, and  shall  meet all  of  the  performance



 specifications  in Section 9.




 6.12  Gas  chromatographic column: 30  m (±5 m) x  0.25 mm



 (±0.02  mm)  I.D. x 0.25 micron, 5% phenyl,  94% methyl, 1%



vinyl silicone bonded-phase  fused-silica  capillary column (J



 & W DB-5,  or equivalent).




 6.13  Mass  spectrometer:  70  eV electron impact ionization,



shall repetitively scan from 42  to  450 amu in 0.95 to 1.00



second, and shall produce  a  unit resolution (valleys between



m/z 441 - 442 less than 10%  of the  height  of  the  441 peak),



background-corrected mass  spectrum  from 50 ng



decafluorotriphenylphosphine  (DFTPP)  introduced through the



GC inlet.  The spectrum shall meet  the mass-intensity



criteria in Table 3  (Reference 7).   The mass  spectrometer






                             1082

-------
shall be interfaced to the GC such.that the end of the


capillary column terminates within I cm of the ion source,


but does not intercept the electron or ion beams.  All


portions of the column which: connect the GC to the ion


source shall remain at or above the column temperature


during analysis to preclude Condensation of less volatile


compounds.                  (


6.14  Data system: Shall collect and record MS data, store


mass-intensity data in spectral libraries, process GCMS


data, generate reports, and compute and record response

                            !
factors.


6.14.1  Data acquisition: Mass spectra shall be collected


continuously throughout the analysis and stored on a mass


storage device.
                            i

6.14.2  Mass spectral libraries: User-created libraries


containing mass spectra obtained from analysis of authentic


standards shall be employed to reverse search GCMS runs for


the compounds of interest  (Section 10.2).


6.14.3  Data processing: The! data system shall be used to
                           .
search, locate, identify, and quantify the compounds of


interest in each GCMS analysis.  Software routines shall be


employed to compute retention times, and to compute peak


areas at the m/z's specified  (Table 4).  Displays of


spectra, mass chromatograms, and library comparisons are


required to verify results.


6.14.4  Response factors and multi-point calibrations: The



                             1083

-------
data  system  shall be used to record and maintain  list's  of




response  factors  (response ratios for isotope dilution)  and



multi-point  calibration curves  (Section 10).  Computations



of relative  standard deviation  (coefficient of variation)



are used  for testing calibration linearity.  Statistics on



initial  (Section 9.3.2) and ongoing  (Section 9.6)



performance  shall be computed and maintained.



7.0   Reagents and Standards




7.1   Reagents for adjusting sample pH.




7.1.1  Sodium hydroxide: Reagent grade, 6 N in reagent



water.




7.1.2  Sulfuric acid: Reagent grade, 6 N in reagent water.



7.2   Reagents for sample preservation.



7.2.1  Sodium thiosulfate (Na2S2O3)  solution (1 N)  : Weigh 79



g Na2S2O3 in a 1-L volumetric flask and dilute to the mark



with  reagent water.



7.2.2  Ascorbic acid solution: Prepare a solution of



ascorbic acid in reagent water at a concentration of 0.1



g/mL.  This  solution must be prepared fresh on each day when



derivatizations will be performed.  Therefore, do not



prepare more than will be used that day.   (A 50-mL volume is



sufficient for ten analyses).



7.3   Solvents: Hexane, acetone,  and methanol.  Distilled in



glass  (Burdick and Jackson,  or equivalent).



7.4  Reagent water: Water in which the compounds of interest



and interfering compounds are not detected by this method.





                            1084

-------
7.5  Reagents for derivatization.                  '


7.5.1  Potassium carbonate  (K2CO3) .


7.5.1.1  Purification: Spread in a shallow baking dish, heat


overnight at 400 to 500°C.   ;


7.5.1.2  Solution: Dissolve 150 g purified K2CO3  in 250 mL


reagent water.


7.5.2  Acetic anhydride: Redistilled reagent grade.


7.6  Analytical standards.   '


7.6.1  Derivatization: Because the chlorinated phenolics are


determined as their acetate derivatives after in situ



acetylation, the method requires that the calibration


standards be prepared by spiking the underivatized materials


into reagent water and carrying the spiked reagent water


aliquot through the entire derivatization and extraction


procedure that is applied to ,the field samples.


7.6.2  Standard solutions: Purchased as solutions or
                             i

mixtures with certification to their purity, concentration,


and authenticity, or prepared from materials of known purity


and composition.  If chemical purity of a compound is 98% or


greater,  the weight may be used without correction to


compute the concentration of :the standard.  When not being


used, standards are stored in the dark at -20 to -10°C in


screw-capped vials with PTFE-lined lids.  A mark is placed


on the vial at the level of the solution so that solvent


evaporation loss can be detected.  The vials are brought to


room temperature prior to use.



                            1085

-------
 7.6.3   If  the  chemical  purity of  any standard does  not  meet



 the  98% requirement  above,  the laboratory must correct  all



 calculations,  calibrations,  etc.,  for the difference  in



 purity.




 7.7  Preparation  of  stock solutions:  Prepare  chlorovanillins



 and  chlorosyringaldehydes in acetone,  as  these compounds are



 subject  to degradation  in methanol.   Prepare  the remaining



 chlorophenolics in methanol.   Prepare all standards per the



 steps below.   Observe the safety precautions  in Section 5.



 7.7.1  Dissolve an appropriate  amount of  assayed reference



 material in a  suitable  solvent.  For  example,  weigh 50  mg



 (±0.1 mg) of pentachlorophenol  in a 10-mL ground-glass-



 stoppered volumetric flask and  fill to the mark with



 methanol.  After  the pentachlorophenol is completely



 dissolved, transfer the solution to a 15-mL vial with



 PTFE-lined cap.




 7.7.2  Stock solutions  should be checked  for  signs of



 degradation prior to the preparation  of calibration or



performance test standards and  shall  be replaced after  six



months, or sooner if comparison with  quality  control check



 standards indicates a change in concentration.



 7.8  Labeled compound spiking solution: From  stock solutions



prepared as above, or from mixtures,  prepare one spiking



solution to contain the labeled chlorovanillin  in acetone



and a second spiking solution to contain  the remaining



chlorophenolics,  including the 3,4,5-trichlorophenol sample






                             1086

-------
matrix internal standard  (SMIS) , in methanol .   The labeled



compounds and SMIS are each at a concentration of 12 . 5
7.9  Secondary standards for calibration: Using stock



solutions  (Section 7.7), prepare one secondary standard



containing the chlorovanillins and chlorsyringaldehydes



listed in Table 1 in acetone , and a second secondary standard



containing the remaining chlorophenolics in methanol.  The



monochlorinated phenol, guaiacol, and catechol are included



at a concentration of 25 /ig/mL; the tri chlorinated



catechols, tetrachlorinated guaiacol and catechol,



pent achl orophenol , 5 , 6 - di chl or ovani 1 1 in , and



2 , 6-dichlorosyringaldehyde are included at a. concentration.



of 100 /ig/mL; and the remaining compounds are included at a



concentration of 50 /zg/mL, each in their respective



solutions .                   !



7.10  Instrument internal standard  (IIS): Prepare a solution



of 2,2 ' -difluorobiphenyl  (DFB) at a concentration of 2 . 5




mg/mL in hexane .



7.11  DFTPP  solution: Prepare a solution of DFTPP at 50




jj.g/mL in acetone             \



7.12  Solutions for obtaining authentic mass spectra



 (Section 10.2) : Prepare mixtures of compounds at



concentrations which will assure authentic spectra are



obtained for storage in libraries.



7.13  Preparation of calibration solutions.






                             !l 087

-------
7.13.1  Into five 1000-mL aliquots of reagent water, spike



50, 100, 200, 500 and 1000 |UL of each of the two solutions



in Section 7.9.  Spike 1.00 mL of each of the two labeled




compound spiking solutions  (Section 7.8) into each of the



five aliquots.




7.13.2  Using the procedure in Section 11, derivatize and



extract each solution, and concentrate the extract to a



final volume of 0.50 mL.  This will produce calibration



solutions of nominal 5, 10, 20, 50, and 100 /zg/mL of the




native chlorophenolics and a constant, concentration of 25



/^g/mL of each labeled compound and the SMIS (assuming 100%



derivatization and recovery).  As noted in Section 11.1.6,



ascorbic acid is added to all samples of final effluents to



stabilize chlorocatechols, but is not added to samples of



pulp and paper in-process wastewaters.   Therefore,  it is



necessary to prepare separate sets of five initial



calibration standards with and without the addition of



ascorbic acid.  Also,'in the event that the laboratory is



extracting final effluent samples by both the stir-bar and



separatory funnel procedures (see Section 11.3),  initial



calibration standards should be prepared by both methods.



7.13.3  These solutions permit the relative response



(labeled to unlabeled) and the response factor to be



measured as a function of concentration (Sections 10.4 and



10.5) .



7.13.4  The nominal 50 /zg/mL standard may also be used as a






                            1088

-------
calibration verification standard  (see Section 9.6).
                             i
7.14  Ongoing precision and recovery  (OPR) standard: Used

for determination of initial ; (Section 9.3.2) and ongoing

(Section 9.6) precision and recovery.  This solution is

prepared by spiking 500 /iL of each the two solutions of the

secondary calibration standards  (Section 7.9) and 1 mL of

each of the two labeled compound spiking solutions  (Section

7.8) into 1000 mL of reagent [water.

7.15  Stability of solutions: All standard solutions

(Sections 7.7 through 7.14) shall be analyzed within 48

hours of preparation and on a monthly basis thereafter for

signs of degradation.  Standards will remain acceptable if

the peak area at the quantitation m/z relative to the DFB
                             i
internal standard remains within ±15% of the area obtained

in the initial analysis of the standard.

8.0  Sample Collection, Preservation, and Storage

8.1  Collect'samples in glass containers (Section 6.1)

following conventional sampling practices (Reference 9) .

Aqueous samples are collected in refrigerated bottles using
                             l
automatic sampling equipment.'

8.2  Sample preservation.

8.2.1  Residual chlorine: If the sample contains residual

chlorine, the chlorine must be reduced to eliminate positive

interference resulting from continued chlorination

reactions.   Immediately after sampling,  test for residual

chlorine using the following method or an alternative EPA

                           ' 1089

-------
method  (Reference 10).




8.2.1.1  Dissolve a few crystals of potassium iodide in the



sample and add three  to five drops of a 1% starch solution.



A blue color indicates the presence of residual chlorine.



8.2.1.2  If residual  chlorine is found, add 1 mL of sodium



thiosulfate solution  (Section 7.2.1) for each 2.5 ppm of



free chlorine or until the blue color disappears.



8.2.2  Acidification: Adjust pH of all aqueous samples to <2



with sulfuric acid  (Section 7.1.2).  Failure to acidify



samples may result in positive interferences from continued



chlorination reactions.




8.2.3  Refrigeration: Maintain sample temperature at 0 to



4°C from time of collection until extraction,  and maintain



extracts at a temperature of 0 to 4°C from time of



extraction until analysis.



8.3  Collect a minimum of 2000 mL of sample.  This will



provide a sufficient  amount for all testing.  Smaller



amounts may be collected if the stream is known to contain



high levels of chlorophenolics.



8.4  All samples must be acetylated and extracted within 30



days of collection,  and must be analyzed within 30 days of



acetylation.  If labeled compound recoveries for a sample do



not meet the acceptance criteria in Table 5 and the 30-day



holding time is not met, a new sample must be collected.



9.0  Quality Control
                             1090

-------
9.1  Each laboratory that uses this method is required to
                            i,


operate a formal quality assurance program (Reference 8).



The minimum requirements of this program consist of an



initial demonstration of laboratory capability, analysis of



samples spiked with labeled compounds to evaluate and



document data quality, and analysis of standards and blanks



as tests of continued performance.  Laboratory performance



is compared to established performance criteria to determine



if the results of analyses meet the performance



characteristics of the method.
                            i

9.1.1  DFTPP spectrum validity shall be checked at the



beginning of each eight-hour; shift during which analyses are



performed.  This test is described in Section 9.2.



9.1.2  The laboratory shall make an initial demonstration of



the ability to generate acceptable results with this method.



This ability is established as described in Section 9.3.



9.1.3  The laboratory is permitted to modify this method to



improve separations or lower! the costs of measurements,



provided all performance specifications are met.  Each time



a modification is made to the method, the laboratory is



required to repeat the procedures in Sections 10.3 and 9.3.2



to demonstrate method performance.  If the detection limits



for the analytes in this method will be affected by the



modification, the laboratory should demonstrate that each



MDL  (40 CFR 136, Appendix B) is less than or equal to the



MDL in this method or one-third the regulatory compliance




                            1091

-------
level, whichever is higher.
9.1.4  The laboratory shall spike all samples with labeled
compounds and the sample matrix internal standard (SMIS) to
monitor method performance.  This test is described in
Section 9.4.  When results of these spikes indicate atypical
method performance for samples, the samples are diluted to
bring method performance within acceptable limits (Section
13).
9.1.5  Analyses of blanks are required to demonstrate
freedom from contamination.  The procedures and criteria for
analysis of a blank are described in Section 9.5.
9.1.6  The laboratory shall, on an ongoing basis,
demonstrate through analysis of the ongoing precision and
recovery standard  (Section 7.14) that the analysis system is
in control.  These procedures are described in Section 9.6.
9.1.7  The laboratory shall maintain records to define the
quality of data that is generated.  Development of accuracy
statements is'described in Section 9.4.4 and 9.6.3.
9.2  DFTPP spectrum validity: Inject 1 /iL of the DFTPP
solution  (Section 7.11) either separately or within a few
seconds of injection of the OPR standard  (Section 9.6)
analyzed at the beginning of each shift.  The criteria in
Table 3 shall be met. .
9.3  Initial demonstration of laboratory capability.
9.3.1  Method Detection Limit(MDL): To establish the ability
to detect the analytes in this method, the laboratory should
               \
                             1092

-------
determine the MDL per the procedure in 40 CFR 136, Appendix      .^^
                                                                 w
B using the apparatus, reagents, and standards that will be      '^^
used in the practice of this 'method.  MDLs less than or
equal to the MDLs in Table 2 should be achieved prior to the
practice of this method.
                             i                        '
9.3.2  Initial precision and ;recovery (IPR) :  To establish
the ability to demonstrate control over the analysis system
and to generate acceptable precision and accuracy, the
laboratory shall perform the following operations:
9.3.2.1  Derivatize, extract, concentrate, and analyze four
1000-mL aliquots of the ongoing precision and recovery
standard (OPR; Section 7.14),i according to the procedure in
Section 11.  Separate sets of IPR aliquots must be prepared
with the addition of ascorbic acid and without.
9.3.2.2  Using results of the four analyses,  compute the
average percent recovery (X) 'and the relative standard
deviation of the recovery (s) for each compound, by isotope
dilution for pollutants with !a labeled analog, and by
internal standard for pollutants with no labeled analog and
for the labeled compounds and the SMIS.
9.3.2.3  For each compound,  compare s and X with the
corresponding limits for initial precision and recovery in-
Table 5.  If s and X for all icompounds meet the acceptance
criteria, system performance [is acceptable and analysis of
blanks and samples may begin.(  If, however,  any individual s
exceeds the precision limit or any individual X falls

                             1093                                 ^^

-------
outside the range  for  recovery,  system performance  is



unacceptable  for that  compound.   In  this  event,  correct  the



problem and repeat the test  (Section 9.3.2).




9.4  Labeled  compound  recovery:  The  laboratory  shall spike



all samples with labeled compounds and the  sample matrix



internal standard  (SMIS) to assess method performance on the



sample matrix.




9.4.1  Analyze each sample according to the method  beginning



in Section 11.           •       -




9.4.2  Compute the percent recovery  (P) of the  labeled




compounds and the SMIS using the  internal standard  method



(Section 14.3) with 2,2'-difluorobiphenyl as the reference



compound.




9.4.3  Compare the labeled compound  and SMIS recovery for



each compound with the corresponding  limits in  Table 5.  If



the recovery of any compound falls outside its  warning



limit,  method performance is unacceptable for that  compound



in that sample.  Therefore, the sample is complex.  The



sample is diluted and reanalyzed per  Section 13.



9.4.4  As part of the QA program for  the laboratory, it  is



suggested,  but not required,  that method accuracy for



samples be assessed and records maintained.   After the



analysis of five samples for which the labeled  compounds



pass the tests in Section 9.4.3, compute the average percent



recovery (P)  and the standard deviation of the percent



recovery (sp)  for the labeled compounds only.   Express the






                            1094

-------
accuracy assessment  as  a percent  recovery interval from P -

2sp to P + 2sp  for each matrix.   For example, if P = 90% and

sp = 10%, the accuracy  interval is expressed as 70 .to 110%.

Update the accuracy  assessment for each compound on a

regular basis  (e.g., after each 20 to 30 new accuracy

measurements).

9.5  Blanks: Reagent water blanks are analyzed to

demonstrate freedom  from contamination.

9.5.1  Extract  and concentrate a  1000-mL reagent water blank

with each sample batch  (samples started through the

extraction process on the same eight-hour shift, to a

maximum of 20 samples).  Blanks associated with samples to

which ascorbic  acid  is  added ;must be prepared with ascorbic

acid, and blanks associated with samples to which ascorbic

acid is not added must  be prepared without ascorbic acid.

Analyze the blank immediately after analysis of the OPR

(Section 7.14)  to demonstrate freedom from contamination.

9.5.2  If any of the compounds of interest (Table 1)  or any

potentially interfering compound is found in an aqueous

blank at greater than 5 //g/L , (assuming a response factor of

one relative to the sample matrix internal standard for

compounds not listed in Table 1),  analysis of samples is

halted until the source of contamination is eliminated and a

blank shows no  evidence of contamination at this level.

9.6  Calibration verification and ongoing precision and

recovery: At the beginning of each eight-hour shift during
                             !
                            1095

-------
  which analyses are performed,  analytical  system performance

  is  verified for all compounds.   Analysis  of  DFTPP  (Section

  9.2)  and the nominal 50 //g/mL  OPR (Section 11.1.5)  is  used

  to  verify all performance criteria.  Adjustment and/or

  recalibration,  per Section 10,  shall be performed until  all

  performance criteria are met.   Only after all performance

  criteria are met may samples and blanks be analyzed.

'  9.6.1 Analyze the extract of  the OPR  (Section  11.1.5) at


  the beginning of each eight-hour shift and prior to analysis

  of  samples  from the same batch.   Alternatively,  a separate
     /
  calibration verification may be  performed using an aliquot


  of  the midpoint  calibration standard from Section 7.13  (with


  a nominal concentration of 50 /Kj/mL) .  This alternative may

  be  used  to  check instrument performance on failure of  an

  OPR,  or  when samples  extracted with an OPR aliquot are not

  analyzed within  the same eight-hour analysis shift.

  9.6.1.1  Retention  times:  The absolute retention time of

  2,2'-difluorobiphenyl  shall be within the range of 765 to

  885 seconds,  and the  relative retention times of all

 pollutants  and labeled  compounds  shall fall within the

  limits given  in  Table 2.


  9.6.1.2  GC resolution:  The valley height between

 4,6-dichloroguaiacol and 3,4-dichloroguaiacol at m/z 192

 shall not exceed  10% of  the height of the taller of the two

 peaks..
                             1096

-------
9.6.1.3  Multiple peaks:  Each compound injected shall give a
                             I

single, distinct GC peak.


9.6.2  Compute the percent recovery of each pollutant (Table     .


1) by isotope dilution (Section 10.4)  for those compounds
                             f           ,             ,            H
that have labeled analogs.  Compute the percent recovery of


each pollutant that has no labeled analog by the internal


standard method  (Section 10.5), using the


3,4,5-trichlorophenol (SMIS)  as the internal standard.


Compute the percent recovery;of the labeled compounds and


the SMIS by the internal standard method,  using the


2,2'-difluorobiphenyl as the:internal standard.


9.6.2.1  For each compound, compare the recovery with the


limits for ongoing precision[and recovery in Table 5.  If


all compounds meet the acceptance criteria, system               dfe


performance is acceptable and analysis of blanks and samples


may proceed.  If, however, any individual recovery falls


outside of the range given, system performance is


unacceptable for that compound.  In this event, there may be
                             i,

a problem with the GCMS or with the


derivatization/extraction/concentration systems.


9.6.2.2  GCMS system: To determine if the failure of the OPR


test  (Section 9.6.2.1) is due to instrument drift, analyze


the current calibration verification extract  (Section


7.13.4), calculate the percent recoveries of all compounds,


and compare with the OPR recovery limits in Table 5.  If all
                             I                           *

compounds meet these criteria, GCMS performance/stability is



                             1097

-------
verified,  and  the  failure of the OPR analysis is attributed




to problems  in the derivatization/extraction/concentration



of the OPR.  In this case, analysis of the sample extracts



may proceed.   However, failure of any of the recovery



criteria in  the analysis of a sample extract requires



rederivatization of that sample  (Sections 13.3.1 and



13.3.2).   If,  however, the performance/stability of the GCMS



is not verified by analysis of the calibration verification



extract, the GCMS  requires recalibration and all extracts



associated with the failed OPR must be reanalyzed.



9.6.3  Add results that pass the specifications in Section



9.6.2.1 to initial and previous ongoing data for each  ,



compound.  Update  QC charts to form a graphic representation



of continued laboratory performance.  Develop a statement of



laboratory accuracy for each pollutant and labeled compound



in each matrix type (reagent water,  C-stage filtrate,



E-stage filtrate,  final effluent, etc.)  by calculating the



average percent  recovery (R)  and the standard deviation of



percent recovery (sr).   Express the accuracy as a recovery



interval from  R  - 2sr to R + 2sr.  For example,  if R = 95%



and sr = 5%,  the accuracy is 85 to 105%.



9.7  The specifications contained in this method can be met



if the apparatus used is calibrated properly,  then



maintained in  a  calibrated state.  The standards used for



calibration  (Section 10)  and for initial  .(Section 9.3.2)  and



ongoing (Section-9.6)  precision and recovery should be






                            1098

-------
identical, so that the most precise results will be

obtained.  The GCMS instrument in particular will provide

the most reproducible results if dedicated to the settings

and conditions required for the analyses of chloropheholics

by this method.              ;

9.8  Depending on specific program requirements, field

replicates may be collected to determine the precision of

the sampling technique,  and spiked samples may be required

to determine the accuracy of the analysis when the internal

standard method is used.

10.0 Calibration and Standardization

10.1  Assemble the GCMS and establish the operating

conditions in Section 12.   Analyze standards per the

procedure in Section 12 to demonstrate that the analytical

system meets the minimum levels in Table 2, and the

mass-intensity criteria in Table 3 for 50 ng. DFTPP.

10.2  Mass-spectral libraries: Detection and identification

of compounds of interest are dependent upon spectra stored

in user-created libraries.

10.2.1  Obtain a mass spectrum of the acetyl derivative of

each chlorophenolic compound  (pollutant, labeled compound,

and the sample matrix internal standard) by derivatizing and

analyzing an authentic standard either singly or as part of
                             i
a mixture in which there is no interference between closely

eluting components.  That only a single compound is present

is determined by examination of the spectrum.   Fragments not


                            1099

-------
attributable to;- the compound under study indicate the



presence of an interfering compound.




10.2.2  Adjust the analytical conditions and scan rate  (for



this test only) to produce an undistorted spectrum at the GC



peak maximum.  An undistorted spectrum will usually be



obtained if five complete spectra are collected across the



upper half of the GC peak.  Software algorithms designed to



"enhance" the spectrum may eliminate distortion, but may



also eliminate authentic m/z's or introduce other



distortion.




10.2.3  The authentic reference spectrum is obtained under



DFTPP tuning conditions  (Section 10.1 and Table 3) to



normalize it to spectra from other instruments.




10.2.4  The spectrum is edited by removing all peaks in the



m/z 42 to 45 range, and saving the five most intense mass



spectral peaks and all other mass spectral peaks greater



than 10% of the base peak (excluding the peaks in the m/z 42



to 45 range).  The spectrum may be further edited to remove



common interfering m/z's.  The spectrum obtained is stored



for reverse search and for compound confirmation.



10.3  Minimum level:  Demonstrate that the chlorophenolics



are detectable at the minimum level (per all criteria in



Section 14) .   The nominal 5 /ig/mL calibration standard



(Section 7.13)  can be used to demonstrate this performance.



10.4  Calibration with isotope dilution:  Isotope dilution is



used when (1)  labeled compounds are available,  (2)






                            1100

-------
interferences do not preclude its use, and (3)  the
guantitation m/z (Table 4) extracted  ion-current  profile

(EICP)  area for the compound ;is in the calibration range.
Alternative labeled compounds and quantitation  m/z's may be
used based on availability.  ;If any of the above  conditions

preclude  isotope dilution, trie internal standard  calibration
method  (Section 10.5)  is used.

10.4.1  A calibration curve encompassing the  concentration

range is  prepared for each compound to be  determined.   The
relative  response (pollutant to labeled) vs.  concentration
                              [
in standard solutions is plotted or computed  using a linear

regression.   The example in Figure 1  shows a  calibration
curve for phenol using phenol-d5 as the isotopic  diluent.
                              i
Also shown are the ±10% error limits  (dotted  lines) .
                              i
Relative  response (RR)  is determined  according  to the
procedures described below.  'A minimum of  five  data points
are employed for calibration.;
10.4.2  The relative response of a pollutant  to its labeled

analog  is determined from isotope ratio values  computed from
acquired  data.   Three isotope ratios  are used in  this

process:                      ;

          RX = the isotope ratio measured for the pure pollutant.
          R = the isotope ratio measured for the labeled compound.
          R'm = the isotope ratio of an analytical mixture of pollutant
              and labeled compounds.
                              1101

-------
 The m/z's are selected such that Rx > Ry.   if R^  is  not


 between 2Ry and 0.5RX,  the method does not  apply and the


 sample is analyzed by  the internal standard  method.


 10.4.3  Capillary columns sometimes separate the


 pollutant-labeled pair when deuterium labeled compounds are


 used,  with the labeled compound eluted first (Figure 2)


 For this case,


        area
               , at the  retention time of the pollutant  (RT.).
           1
           1


       L    7'2"
R  =	.	  at the retention time of the labeled compound (RT,).
    \area mjz\                                       1
       \area at mjz (at RTj]
     = -f	:	-4, as measured in the mixture of the pollutant and
       \area at m2/z (at RTJl

                           labeled compounds (Figure 2), and RR = R  .
10.4.4   When the pollutant-labeled pair is not separated (as


occurs with carbon-13-labeled compounds),  or when another


labeled  compound with interfering spectral masses overlaps


the pollutant (a case which  can occur with isomeric


compounds),  it is necessary  to determine the contributions


of the pollutant and labeled compound to the respective  EICP


areas.   If  the peaks are separated well enough to permit the


data system or operator to remove the contributions of the
                              1102

-------
compounds to each other, the equations  in Section 10.4.3

apply.  This usually occurs when  the  height of the valley
between the two GC peaks at the same  m/z  is less than 70 to
90% of the height of the shorter  of the two peaks.  If
significant GC and spectral overlap occur,  RR is computed

using the following equation:

                          (* r RJ(R + 1)
                     RR =
                                    +
                Where:        \
                Rx is measured as shown in figure 3A,
                R  is measured as shown in figure 3B,
                R  is measured as shown in figure 3C.
For example, Rx = 46100/4780 = 9.644; Ry = 2650/43600 =
0.0608; R,,, = 49200/48300 = 1.1019; thus, RR =  1.114.
10.4.5  To calibrate the analytical  system by isotope
dilution, analyze a  1-juL aliquot  of  each of the calibration
standards  (Section 7.13) using the procedure  in Section 12.

Compute the RR at each  concentration.
10.4.6  Linearity: If the ratio of relative response to
concentration for any compound is constant (less than 20%
coefficient of variation) over the five-point calibration
                            - \
range, an averaged relative response/concentration ratio may

be used for that compound; otherwise,  the complete
calibration curve for that compound  shall be used over the

five-point calibration  range.1
10.5  Calibration by internal  standard: The method contains
two types of internal standards,  the sample matrix internal

                             1103

-------
standard (SMIS)  and the instrument internal standard (IIS) ,

and  they are used for different quantitative purposes.   The

3,4, 5-trichlorophenol sample  matrix internal standard (SMIS)

is used for measurement of  all  pollutants with no  labeled

analog and when the criteria  for isotope dilution  (Section

10.4)  cannot be met.  The 2 , 2 ' -dif luorobiphenyl instrument

internal standard (IIS) is  used for determination  of the

labeled compounds and the SMIS.   The results are used for
             s
intralaboratory statistics  (Sections 9.4.4 and 9.6.3).

10.5.1  Response factors: Calibration requires the

determination of response factors (RF)  for both the

pollutants  with no labeled  analog and for the labeled

compounds  and the SMIS.  The  response factor is defined  by

the  following equation:
                          RF -   -
                               w,, *
  Where:
  As = the area of the chracteristic mass for the compound in the daily standard.
  Ajs = the area of the characteristic mass for the internal standard.
  Cjs '- the concentration of the internal standard (\iglmL).
  Cs = is the concentration of the compound in the calibration standard
When this  equation is used to determine the response  factors

for pollutant  compounds without labeled analogs, use  the

area  (Ais)  and concentration  (Cis)  of 3,4, 5-trichlorophenol

(SMIS) as  the  internal standard.  When this equation  is used

to determine the response factors for the labeled analogs
                              1104

-------
and the  SMIS,  use  the area (Ais)  and concentration (Cis) of
2,2'-difluorobiphenyl as the
                              internal  standard.
10.5.2  The  response factor is determined for at  least  five



concentrations  appropriate  to the response of each compound



(Section  7.13); nominally,  5,  10,  20,  50,  and 100 /zg/mL.



The amount of SMIS  added to each solution is  the  same  (25



£tg/mL) so that  Cis remains constant.   Likewise,  the



concentration of  IIS is  constant in  each  solution.   The area
                             i

ratio  (As/Ais) is plotted versus  the  concentration ratio



(Cs/Cis) for each compound in the standard  to  produce a



calibration  curve.



10.5.3  Linearity:  If the response factor  (RF)  for any



compound  is  constant (less  than 35%  coefficient of


variation) over the  five-point calibration range,  an



averaged  response factor may be  used for that compound;



otherwise, the complete  calibration  curve  for that compound



shall be  used over the five-point  range.



10.6  Combined calibration: By using calibration  solutions



(Section  7.13) containing the  pollutants,  labeled compounds,



and the internal standards, a  single set of analyses can be



used to produce calibration curves for the isotope dilution



and internal standard methods.   These curves  are  verified



each shift (Section  9) by analyzing  the OPR standard, or an



optional  calibration verification  (VER) standard.



Recalibration is required only if  OPR criteria  (Section 9,, 6


and Table 5)  cannot  be met.



                             '
                             1105

-------
 11.0   Sample  Derivatization,  Extraction, and Concentration


 The procedure described  in  this  section uses a stir-bar in a

 beaker for  the derivatization.   The extraction procedures

 applied to  samples depend on  the type of sample being

 analyzed.   Extraction of samples from in-process wastewaters

 is performed  using a separatory  funnel procedure.  All
                               K
 calibrations,  IPR, OPR,  and blank analyses associated with

 in-process  wastewater samples must be performed by the

 separatory  funnel procedure.

     Extraction of samples  of final effluents and raw water

 may be  performed using either the stir-bar procedure or the

 separatory  funnel procedure.  However, all calibrations,

 IPR, OPR, blank, and sample analyses must be performed using

 the same procedure.  Both procedures are described below.

 11.1  Preparation of all sample  types for stir-bar

 derivatization.

 11.1.1  Allow sample to warm to  room temperature.

 11.1.2  .Immediately prior to measuring,  shake sample

vigorously  to insure homogeneity.

 11.1.3  Measure 1000 mL  (±10 mL)  of sample into a clean

 2000-mL beaker.  Label the  beaker with the sample number.

 11.1.4  Dilute  aliquot(s).

 11.1.4.1  Complex samples:   For samples that are expected to

be difficult  to derivatize,  concentrate,  or are expected to

overload the  GC column or mass spectrometer,  measure an

additional  100 mL (±1 mL) into a clean 2000-mL beaker and


                            1106

-------
dilute to a final volume of 1000-mL (±50 mL) with reagent       jflb,

water.  Label with the sample number and as the dilute

aliquot.  However, to ensure'adequate sensitivity, a 1000-mL

aliquot must always be prepared and analyzed.
                            s
11.1.4.2  Pulp and paper industry samples: For in-process

streams such as E-stage and C-stage filtrates and other

in-process wastewaters," it may be necessary to prepare an

aliquot at an additional level of dilution.  In this case,
                                                     '
dilute 10 mL (±0.1 mL) of sample to 1000-mL  (±50 mL).

11.1.5  QC aliquots: For a batch of samples of the same type

to be extracted at the same time (to a maximum of 20),  place

two 1000-mL (±10 mL) aliquots of reagent water in clean

2000-mL beakers.  Label one beaker as the blank and the
                            I
other as the ongoing precision and recovery  (OPR) aliquot.
                            i
Because final effluent samples are treated with ascorbic

acid and in-process wastewater samples are not (see Section

11.1.6), prepare an OPR aliquot and a blank for the final

effluent and a separate pair 
-------
 are present.   Separate  calibration curves must be prepared



 with and without  the  addition of ascorbic acid (Section



 7.13.2).




"11.1.6.1.  Spike 5 to  6  mL  of  the ascorbic acid solution



 (Section 7.2.2) into  each  final  effluent  sample,  and the



 associated calibration  standards,  IPR and OPR aliquots,  and



 blank.




 11.1.6.2   For  pulp and  paper  industry C-stage filtrates,



 E-stage  filtrates,  and  untreated effluents,  omit  the




 ascorbic  acid  to  prevent the  conversion of chloro-o-quinones




 to  catechols.   Prepare  calibration standards,  IPR and OPR



 aliquots,  and  blanks  associated  with  these samples without



 ascorbic  acid  as  well.




 11.1.7   Spike  1000  /zL of the  labeled  compound spiking



 solution  (Section 7.8)  into the  sample and QC aliquots.



 11.1.8   Spike  500 /iL of the nominal 50 /ng/mL calibration



 solution  (Section 7.13.4)  into the OPR aliquot.



 11.1.9  Adjust  the  pH of the  sample aliquots to between  7.0



 and 7.1.   For  calibration  standards,  IPR  and OPR  aliquots,



 and blanks, pH  adjustment  is  not  required.



 11.1.10  Equilibrate all sample  and QC solutions  for



 approximately  15  minutes,  with occasional  stirring.



 11.2  Derivatization: Because derivatizatipn must  proceed



 rapidly, particularly upon the addition of the K2CO3 buffer,



 it  is necessary to  work with  one  sample at a time  until  the



 derivatization  step (Section  11.2.3)  is complete.





                            1108

-------
 11 .,2.1   Place  a  beaker containing  a  sample  or QC  aliquot on

 the magnetic stirrer in a fume  hood,  drop a clean stirring

 bar into the beaker,  and increase  the speed of the stirring

 bar until the  vortex is drawn to the  bottom of the beaker.

 11.2.2   Measure  25  to 26 mL of  K2CO3  buffer  into a graduated
                             j
 cylinder or other container and 25 to 26 mL of acetic acid

 into another.

 11.2.3   Add the  K2CO3 buffer to  the sample or QC aliquot,

 immediately  (within one to three seconds) add the  acetic

 anhydride, and stir for three to five minutes to  complete

 the derivatization.          >

 11.3  Extraction: Two procedures are  described below for the

 extraction of  derivatized samples.  The choice of  extraction

 procedure will depend on the sample type.   For final

 effluent samples, either of two procedures  may be  utilized

 for extraction of derivatized samples.  For samples of

 in-process wastewaters,  the separatory funnel extraction

procedure must be used.

Note:  Whichever procedure is employed, the same  extraction


procedure must be used for calibration standards,  I PR


 aliquots, OPR  aliquots,  blanks, and the associated field


 samples.             •        >


 11.3.1   Stir-bar extraction of  final  effluents.
                             1109

-------
 11.3.1.1  Add 200  mL  (±20 mL)  of  hexane  to  the beaker and



 stir  for  three to  five minutes, drawing  the vortex to the



 bottom of the beaker..




 11.3.1.2  Stop the stirring and drain the hexane and a



 portion of the water  into a 500-  to 1000-mL separatory



 funnel.   Allow the layers to separate.




 1113.1.3  Drain the aqueous layer back into the beaker.



 11.3.1.4  The formation of emulsions can be expected in any



 solvent extraction procedure.  If an emulsion forms, the



 laboratory must take  steps to break the emulsion before  '



 proceeding.   Mechanical means of  breaking the emulsion




 include the use of  a  glass stirring rod,  filtration through



 glass wool, and other techniques.  For emulsions that resist



 these techniques,  centrifugation  is nearly  100% effective.



     If centrifugation is employed to break the emulsion,



 drain the organic  layer into a centrifuge tube,  cap the



 tube,  and centrifuge  for two to three minutes or until the



phases separate.   If  the emulsion cannot be completely



broken, collect as much of the organic phase as possible,



and measure and record the volume of the organic phase



collected.




     If all efforts to break the emulsion fail,  including



centrifugation, and none of the organic phase can be



collected, proceed with the dilute aliquot  (Section



11.1.4.2).  However, use of the dilute aliquot will
                            1110

-------
sacrifice the sensitivity of the method, and may not be

appropriate in all cases.

11.3.1.5  Drain the organic layer into a Kuderna-Danish

(K-D) apparatus equipped with a 10-mL concentrator tube.

Label the K-D apparatus.   It,may be necessary to pour the

organic layer through a funnel containing anhydrous sodium

sulfate to remove any traces'of water from the extract.

11..3.1.6  Repeat the extraction (Section 11.3.1.1 through

11.3.1.5) two more times using another 200-mL of hexane for

each extraction, combining the extracts in the K-D
                            i
apparatus.                  ;

11.3.1.7  Proceed with concentration of the extract, as

described in Section 11.4.  •

11.3.2  Separatory funnel extraction of either final

effluents or in-process wastewaters.

11.3.2.1  Transfer the derivatized sample or QC aliquot to a

2-L separatory funnel.      |

11.3.2.2  Add 200 mL  (±20 mL)  of hexane to the separatory

funnel.  Cap the funnel and extract the sample by shaking
                            I

the funnel for two to three minutes with periodic venting.
                            i
11.3.2.3  Allow the organic layer to separate from the water

phase for a minimum of 10 minutes.

11.3.2.4  Drain the lower aqueous layer into the beaker used

for derivatization (Section 11.2), or into a second clean 2-

L separatory funnel.   Transfer the solvent to a 1000-mL K-D
                            i

flask.  It may be necessary to pour the organic layer



                            •1111

-------
through a funnel containing anhydrous sodium sulfate to



remove any traces of water from the extract.



11.3.2.5  The formation of emulsions can be expected in any



solvent extraction procedure.  If an emulsion forms, the



laboratory must take steps to break the emulsion before



proceeding.  Mechanical means of breaking the emulsion



include the use of a glass stirring rod, filtration through



glass wool, and other techniques.  For emulsions that resist



these techniques, centrifugation may be required.



     If centrifugation is employed to break the emulsion,



drain the organic layer into a centrifuge tube, cap the



tube, and centrifuge for two to three minutes or until the



phases separate.  If the emulsion cannot be completely



broken, collect as much of the organic phase as possible,



and measure and record the volume of the organic phase



collected.  If all efforts to break the emulsion, including



centrifugation,  fail and none of the organic phase can be



collected, proceed with the dilute aliquot (Section



11.1.4.2) .  However, use of the dilute aliquot will



sacrifice the sensitivity of the method, and may not be



appropriate in all cases.



11.3.2.6  ,If drained into a beaker,  transfer the aqueous



layer to the 2-L separatory funnel (Section 11.3.2.1).



Perform a second extraction using another 200 mL of fresh



solvent.
                            1112

-------
11.3.2.7  Transfer the extract to the 1000-mL K-D flask in
Section 11.3.2.4.            :
11.3.2.8  Perform a third extraction in the same fashion as
above.
11.3.2.9  Proceed with concentration of the extract, as
described in Section 11.4.   '
11.4  Macro concentration: Concentrate the extracts in
separate 1000-mL K-D flasks equipped with 10-mL concentrator
tubes.  Add one to two clean boiling chips to the flask and
attach a three-ball macro-Snyder column.  Prewet the column
by adding approximately 1 mL of hexane through the top.
                             i
Place the K-D apparatus in a hot water bath so that the
entire lower rounded surface of the flask is bathed with
steam.  Adjust the vertical position of the apparatus and
the water temperature as required to complete the
concentration in 15 to 20 minutes.  At the proper rate of
distillation, the balls of the column will actively chatter
but the chambers will not flood.  When the liquid has
reached an apparent volume of; 1 mL,  remove the K-D apparatus
from the bath and allow the solvent to drain and cool for at
                             I
least 10 minutes.  Remove the, Snyder column and rinse the
flask and its lower j oint into the concentrator tube with 1
to 2 mL of hexane.  A 5-mL syringe is recommended for this
operation.
                             1113

-------
 11.5   Micro-concentration:  Final  concentration of  the



 extracts may be accomplished using  either a micro-Snyder



 column or nitrogen evaporation.



 11.5.1 Micro-Snyder column: Add  a  clean boiling chip  and




 attach a two-ball micro-Snyder column to the concentrator



 tube.   Prewet the column by adding  approximately 0.5 mL



 hexane through the top.  Place the  apparatus in the hot



 water  bath.  Adjust the vertical  position and  the water



 temperature as required to  complete the concentration  in 5



 to 10  minutes.  At the proper rate  of distillation, the



 balls  of the column will actively chatter but  the chambers



 will not flood.  When the liquid  reaches an apparent volume



 of approximately 0.2 mL, remove the apparatus  from the water



 bath and allow to drain and cool  for at least  10 minutes.



 Remove  the micro-Snyder column and rinse its lower joint



 into the concentrator tube with approximately  0.2 mL of



 hexane.  Adjust to a final volume of 0.5 mL.



 11.5.2  Nitrogen evaporation:  Transfer the concentrator tube



 to a nitrogen evaporation device and direct a gentle stream



 of clean dry nitrogen into the concentrator.   Rinse the



 sides of the, concentrator tube with small volumes of hexane,



 and concentrate the extract to a final volume of 0.5 mL.



 11.6  Spike each extract with 10 /^L of the



2,2'-difluorobiphenyl IIS (Section 7.10)  and transfer the



concentrated extract to a clean screw-cap vial  using hexane



to rinse the concentrator tube.   Seal  the vial  with a






                            1114

-------
PTFE-lined lid, and mark the level on  the vial.  Label with      Jttfe

the sample number and  store in the dark at -20 to -10°C

until ready for analysis.    [

12.0  GCMS Analysis          ;


12.1  Establish the following operating conditions:

     Carrier gas flow:       , Helium at 30 cm/sec at 50°C

     Injector temperature:   | 300°C

     Initial temperature:    , 5DOC

     Temperature program:    \ 8°C/min to 270QC

     Final hold:              Until after 2,6-

                              dichlorosyringaldehyde elutes

Adjust the GC conditions to meet the requirements in Section

9.6.1.1 and Table 2 for analyte separation and sensitivity.

Once optimized, the same GC conditions must be used for the

analysis of all standards, blanks, IPR and OPR aliquots, and

samples.

12.2  Bring the concentrated'extract  (Section 11.6) or

standard  (Sections 7.13 and 7.14) to room temperature and

verify that any precipitate has redissolved.  Verify the

level on the extract  (Sections 7.13, 7.14, and 11.6) and

bring to the mark with solvent if required.

12.3  Inject a 1-yiL volume of the standard solution or

extract using on-column or splitless injection.  For 0.5 mL

extracts, this l-/iL injection volume will contain 50 ng of

the DFB internal standard.  If an injection volume other
                             I
than 1 {JJL is used, that volume must contain 50 ng of DFB.


                             1115

-------
 12.4   Start the GC column temperature ramp upon injection.


 Start  MS  data collection after the solvent peak elutes.


 Stop data collection after the 2,6-dichlorosyringaldehyde


 peak elutes.   Return the column to the initial  temperature


 for analysis  of the next sample.


 13.0   Analysis of Complex Samples


 Some samples  may contain high levels  (>1000 /zg/L)  of  the


 compounds of  interest,  interfering compounds, and/or  other


 phenolic  materials.   Some samples  will not concentrate to


 0.5 mL (Section 11.5);  others will overload the  GC column

    .      •                                  s
 and/or mass spectrometer;  others may  contain amounts  of


 phenols that  may exceed the  capacity  of the derivatizing


 agent.


 13.1   Analyze the dilute aliquot  (Section  11.1.4)  when the


 sample will not  concentrate  to'0.5 mL.  If  a dilute aliquot


 was not extracted,  and  the sample  holding  time  (Section 8.4)


 has not been  exceeded,  dilute an aliquot of  sample with


 reagent water,  and derivatize and  extract  it (Section


 11.1.4).  Otherwise,  dilute  the extract (Section 14.7.3)   and


 quantitate  it  by the  internal standard method (Section


 14.3) .


 13.2   Recovery of  the 2,2'-difluorobiphenyl  instrument


 internal  standard: The  EICP  area of the internal standard


 should be within a  factor of  two of the area in the OPR or


VER standard  (Section 9.6).   If the absolute areas of the


 labeled compounds  and the SMIS are within a factor of two of



                             1116

-------
the respective areas in the OPR or VER standard, and the DFB



internal standard area is less than one-half of its

                            I


respective area, then internal standard loss in the extract



has occurred.  In this case,• analyze the extract from the



dilute aliquot  (Section 11.1,4).



13.3  Recovery of labeled compounds and the sample matrix



internal standard (SMIS): SMIS and labeled compound recovery



specifications have been developed for samples with and

                            l

without the addition of ascorbic acid.  Compare the



recoveries to the appropriate limits in Table 5.



13.3.1  If SMIS or labeled compound recoveries are outside



the limits given in Table 5 and the associated OPR analysis
                            i


meets the recovery criteria, ; the extract from the dilute



aliquot (Section 11.1.4)  is analyzed as in Section 14.7.



13.3.2  If labeled compound or SMIS recovery is outside the



limits given in Table 5 and the associated OPR analysis did



not meet recovery criteria, a problem in the



derivatization/extraction/concentration of the sample is



indicated, and the sample must be rederivatized and

                 **v          •

reanalyzed.



14,0  Data Analysis and Calculations




14.1  Qualitative determination:  Identification is



accomplished by comparison of data from analysis of a sample



or blank with data stored in the mass spectral libraries.



Identification of a compoundjis confirmed when the following
                            l


criteria are met:





                            1117

-------
 14.1.1   The  signals  for m/z 43 .(to  indicate  the  presence of



 the  acetyl derivative) and all characteristic  m/z's  stored



 in the  spectral  library  (Section  10.2.4)  shall be present



 and  shall maximize within the same  two  consecutive scans.



 14.1.2   Either  (1) the background corrected  EICP areas,  or



 (2)  the  corrected relative intensities  of the  mass spectral



 peaks at the GC  peak maximum shall  agree within  a factor of



 two  (0.5 to 2 times) for all m/z's  stored in the library.



 14.1.3   The relative retention time shall be within  the



 window specified in Table 2.




 14.1.4   The m/z's present in the mass  spectrum  from the



 component in the sample that are not present in  the



 reference mass spectrum shall be accounted for by



 contaminant or background ions.   If the mass spectrum is



 contaminated, an experienced spectrometrist  (Section 1.4)



 shall determine the presence or absence of the compound.



 14.2  Quantitative determination by isotope  dilution: By



 adding a known amount of a labeled compound  to every sample



prior to derivatization and extraction,  correction for



 recovery of the pollutant can be made because  the pollutant



 and its labeled analog exhibit the same effects upon



derivatization,  extraction,  concentration, and gas



chromatography.   Relative response  (RR)  values for sample



mixtures are used in conjunction with calibration curves



described in Section 10.4 to determine concentrations



directly, so long as labeled compound spiking levels are






                            1118

-------
constant.   For the phenol example given  in Figure 1  (Section

10.4.1), RR would be equal to 1.114.  For  this RR value,  the

phenol  calibration curve  given in Figure 1 indicates a

concentration of 27 /ig/mL in the sample  extract (Cex) .

14.2.1   Compute the concentration in the extract using the

response ratio determined from calibration data (Section

10.4) and  the following equation:


                  Cex(iig/mL) = (An x C,) / (Al x  RR)
        Where:
        C  = concentration of the pollutant in the extract.
         An= area of the characteristic mlz for the
             pollutant.
         C{ = concentration of the labeled compound  in  the extract.
         A, = area of the characteristic mlz for the labeled compound.
        RR = response ratio from the [initial calibration.



14.2.2   For the IPR  (Section 9.3.2) and  OPR  (Section 9.6),

compute the percent recovery of each pollutant using the

equation in Section 14.6.  The percent recovery is used for

the evaluation of method  and laboratory  performance, in the

form of IPR (Section 9.3.2)  a;nd OPR  (Section 9.6).

14.3  Quantitative determination by internal standard:
                               ?
Compute the concentration using the response factor

determined from calibration data (Section  10.5) and the

following  equation:

-------
                  Cex(vglmL)  = (As x Cjs) I (Ais x RF)

         Where:
         C ex = concentration of the pollutant in the extract.
          AS= area of the characteristic mlz for the pollutant.
         Cjs = concentration of the internal standard in the extract
              (see note below).
         Ajs = area of the characteristic mlz for the internal standard.
         RF = response factor from the initial calibration.

Note:   When this equation is used  to compute the  extract

concentrations  of native compounds  without labeled analogs,

use  the area  (Als)  and concentration  (Cis) of

3,4,5-trichlorophenol (SMIS)  as the internal standard.

     For the IPR  (Section 9.3.2) and OPR (Section 9.6),

compute the percent  recovery using  the equation in Section
14.6.

Note:   Separate calibration curves  will be required for

samples with and without the addition of ascorbic acid,  and

also for both extraction procedures  (stir-bar and separatory

funnel)  where applicable.

14.4   Compute the concentration of  the labeled compounds and
the  SMIS using  the equation in  Section 14.3,  but  using  the
area and concentration  of the 2,2'-difluorobiphenyl as  the
internal standard, and  the area of  the labeled compound or
SMIS as As.

14.5   Compute the concentration of  each pollutant  compound
in the sample using  the  following equation:
                               1120

-------
                                    V
                                     o
         •where:
          Cs = Concentration of the pollutant in the sample.
         Cex = Concentration of the pollutant in the extract.
         Vex = Volume of the concentrated extract (typically 0.5 mL).
          Vo = Volume of the original sample in liters.

Pritnaryl4.6   Compute the  recovery of each labeled compound

and the  SMIS  as the ratio of:concentration  (or  amount)  found
to the concentration  (or  amount)  spiked, using  the following
equation:

              _              Concentration found   ,„„
              Percent recovery - —•	 x 100
                             Concentration spiked

These percent recoveries  are:used to assess method
performance according to  Sections 9 and 13.

14.7  If the  EICP area at the quantitation m/z  for any
compound exceeds the calibration range of the system,  three
approaches are used to obtain results within the  calibration
range.
»
14.7.1   If the recoveries of;all the labeled compounds in
the original  sample aliquot meet the limits in  Table 5, then

the extract of the sample may be diluted by a maximum of a
factor of  10,  and the diluted extract reanalyzed.
14.7.2   If the recovery of any labeled compound is outside
its limits in Table 5, or if;a tenfold dilution of the
extract  will  not bring the pollutant within the calibration
                    £
range, then extract and analyze a dilute aliquot  of the

                              1121

-------
sample  (Section 11).   Dilute 100 mL, 10 mL, or an



appropriate volume of sample to 1000 mL with reagent water



and extract per Section 11.         "



14.7.3  If the recoveries of all labeled compounds in the



original sample aliquot (Section 14.7.1) meet the limits in



Table 5, and if the sample holding time has been exceeded,



then the original sample extract is diluted by successive



factors of 10, the DFB internal standard is added to give a



concentration of 50 jug/mL in the diluted extract, and the



diluted extract is analyzed.  Quantitation of all analytes



is performed using the DFB internal standard.



14.7.4  If the recoveries of all labeled compounds in the



original sample aliquot (Section 14.7.1) or in the dilute



aliquot (Section 14.7.2)  (if a dilute aliquot was analyzed)



do not meet the limits in Table 5, and if the holding time



has been exceeded, re-sampling is required.



14.8  Results are reported for all pollutants, labeled



compounds, and the sample matrix internal standard in



standards, blanks, and samples, in units of /zg/L.



14.8.1  Results for samples which have been diluted are



reported at the least dilute level at which the area at the



quantitation m/z is within the calibration range (Section



14.7).



14.8.2  For compounds having a labeled analog, results are



reported at the least dilute level at which the area at the



quantitation m/z is within the calibration range (Section






                            1122

-------
 14.7) and the  labeled  compound  recovery  is within  the  normal

 range for the  method  (Section 13.3).

 15.0 Method Performance      i


 15.1  Single laboratory performance  for  this method  is

 detailed in References 1, 2, and  11.  Acceptance criteria

 were established  from multiple  laboratory use of the draft

 method.                      ;

 15.2  A chromatogram of the ongoing  precision and  recovery

 standard (Section 7.14) is shown  in  Figure 4.

 16.0 Pollution Prevention

                             f
 16.1  The solvents used in this method pose little threat to

 the environment when'recycled and managed properly.

 16.2  Standards should be prepared in volumes consistent
                             i
with laboratory use to minimize the volume of expired

 standards to be disposed.

 17.0 Waste Management


 17.1  It is the laboratory's responsibility to comply with

all federal,  state, and local regulations governing waste

management,  particularly the hazardous waste identification

rules and land disposal restrictions, and to protect the

air,  water,  and land by minimizing and controlling all

releases from  fume hoods and bench operations-.  Compliance

with all sewage discharge permits and regulations is also

required.                     \
                             1123

-------
17.2   Samples preserved with HCl  or H2SO4 to pH < 2 are



hazardous  and must be  neutralized before being disposed,  or



must be handled  as hazardous waste.



17.3   For  further information on  waste  management,  consult



"The Waste Management  Manual for  Laboratory Personnel", and



"Less  is Better: Laboratory  Chemical Management  for Waste



Reduction", both available from the American Chemical



Society's Department of  Government Relations and Science



Policy, 1155 16th Street N.W., Washington,  B.C.  20036.



18.0 References




18.1   "Chlorinated Phenolics in Water by In Situ




Acetylation/GC/MS Determination," Method CP-86.01,  National



Council of the Paper Industry for Air and Stream



Improvement, Inc., 260 Madison Avenue, New  York, NY 10016



(July  1986).




18.2   "6240-Chlorinated  Phenolics  (Interim'standard) ," Draft



Version, U. S. Environmental  Protection Agency,  Manchester



Laboratory, Manchester,  Washington.



18.3   "Performance Tests for the  Evaluation of Computerized



Gas Chromatography/Mass  Spectrometry Equipment and



Laboratories," USEPA, EMSL Cincinnati, OH 45268,



EPA-600/4-80-025 (April  1980).



18-.4   "Working with Carcinogens," DHEW, PHS, CDC, NIOSH,



Publication 77-206 (August 1977).



18.5   "OSHA Safety and Health  Standards,  General Industry,"



OSHA 2206,  29 CFR 1910  (January 1976).




                             1124

-------
18.6  "Safety in Academic Chemistry Laboratories," ACS


Committee on Chemical Safety  (1979).


18.7  "Interlaboratory Validation of U. S. Environmental


Protection Agency Method 1625A, Addendum Report," SRI


International, Prepared for Analysis and Evaluation Division


(WH-557), USEPA, 401 M St. SW, Washington, DC 20460  (January


1985).


18.8  "Handbook of Analytical Quality Control in Water and
                             !.

Wastewater Laboratories," USEPA, EMSL, Cincinnati, OH 45268,


EPA-600/4-79-019  (March 1979):.


18.9  "Standard Practice for ^Sampling Water," ASTM Annual


Book of Standards, ASTM, Philadelphia, PA, 76 (1980).


18.10  "Methods 330.4 and 330.5 for Total Residual


Chlorine," USEPA, EMSL, Cincinnati, OH 45268, EPA


600/4-70-020  (March 1979).   \


18.11  "Determination of Chlorophenolics, Special Analytical


Services Contract 1047, Episode 1886," Analytical


Technologies, Inc., Prepared :for W. A. Telliard, Industrial


Technology Division  (WH-552) ,' USEPA, 401 M St. SW,


Washington, DC 20460  (June 1990) .


18.12  "Determination of Chlorophenolics by GCMS,


Development of Method 1653," Analytical Technologies, Inc.,


Prepared for W. A. Telliard, Industrial Technology Division


(WH-552), USEPA, 401 M St. SW, Washington, DC 20460  (May


1991) .                       '
                             1125

-------
19.0  Tables and Figures
Table 1.  Chlorophenolic Compounds Determined by GCMS using



Isotope Dilution and Internal Standard Techniques
Compound
4-chlorophenol .
2 , 4 -dichlorophenol
2 , 6 -dichlorophenol
2,4, 5 - trichlorophenol
2,4, 6-trichlorophenol
2,3,4, 6-tetrachloroph-
2nol
pentachlorophenol
4-chloroguaiacol
3 , 4-dichloroguaiacol
4 , 5 -dichloroguaiacol
4 , 6 -dichloroguaiacol
3 , 4, 5-trichloroguaia-
30l
3,4, 6-trichloroguaia-
=01
4,5, 6-trichloroguaia-
30l
tetrachloroguaiacol
4 - chlorocatechol
3 , 4 -dichlorocatechol
3 , 6 -dichlorocatechol
4 , 5 -dichlorocatechol
3,4, 5-trichlorocatec-
iol
3,4, 6-trichlorocatec-
101
tetrachlorocatechol
5-chlorovanillin
5 - chl orovani 1 1 in
5, 6-dichlorovanillin
Pollutant
CAS Registry
106-48-9
120-83-2
87-65-0
95-95-4
88-06-2
58-90-2
87-86-5
16766-30-6
77102-94-4
2460-49-3
16766-31-7
57057-83-7
60712-44-9
2668-24-8
2539-17-5
2138-22-9
3978-67-4
3938-16-7
3428-24-8
56961-20-7
32139-72-3
1198-55-6
19463-48-0
18268-76-3
18268-69-4
EPA-EGD
1001
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
1015
1016
1017
1018
1019
1020
1021
1022
1023
1024
1025
Labeled Compound
Analog

d3




»C6
»c6





13C6
»C6



13c6


13c6
13c6


CAS Registry

93951-74-7




85380-74-1
136955-39-0





136955-40-3
136955-41-4



136955-42-5


136955-43-6
136955-44-7


EPA-
EGD

1102




1107
1108





1114
1115



1119


1122
1123


                            1126

-------
2-chlorosyringaldehyde 76341-69-0
2,6-
iichlorosyringaldehyde
trichlorosyringol
                       76330-06-8 r
                        2539-26-6
                                     1026
                                     1027
1028
Sample matrix internal standard (SMIS)
3,4,5-trichlorophenol
                         609-19-8
                                      184
Instrument internal standard (IIS)
2,2'-di£luorobipheny1
                         388-82-9
 164
                                  1127

-------

CO.
o
-H
rH
O
a
 M
_[_1 ^ ^_,
(U -H
Pi H

Compound



Q»
_
W|3
^•i



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rH
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in
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rH


H
CO
vo
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in
vo
o


n
00
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4-chlorophenol



rH
O
O
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in
CM


CTl
r-
r~
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in
c--
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co
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6 - di chl oropherio 1
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VD
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CO
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CO



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•*
CM

CM
O
rH
rH



m
H
o





in
CM


VD
o
o
rH
1
r-
CTl
CTl
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CM
O
rH
rH




CTl
H
CO



4 -dichlorophenol
CM


CM
0
CM
rH


















O
O
•
H




„
VD
T~H




in
CM
CO


i-i
-dif luorobipheny
(I.S.)
CM
CM

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VO
rH
















P)
O
rH
H
1
r-
f-
o
rH


„
VD
rH-




O
O
CTl



hloroguaiacol-13C(
0
•*

CO
0
rH
rH



CTl
O
O





in
rH


CM
O
O
rH
I
CO
CTl
CTl
O


CO
0
rH
rH




O
O
CTl



-chloroguaiacol
•*


co
0
CM
rH



rH
E-
O





m
CM


in
CTl
CO
o
i
CTl
c*.
CO
o



CO
rH




o
CM
CTl


rH
6-trichloropheno
«*
CM

in
o
0
rH



F-
m
o





in
CM


CM
tn
CTl
o
1
vo
PI
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CO





CTl
CTl


i-H
5-trichloropheno
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CM

••*.
O
0
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CTl
m
o





in
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rH


in
r-
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1
H
VD
CTl
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o
0



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vo
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rH



in
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in
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t*.
cn
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VD
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rH
rH
O
rH



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in
o





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O
rH















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r-
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rH
1
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^
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p-
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r-
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o
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CO
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rH
o
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CO
PI
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in
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CO
f-
0
rH
1
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in
o
rH



CO
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PI
0
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,3,4, 6-tetrach-
lorophenol
CM


VD
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r-
vo
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1
r-
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rH
rH
H
I 	 1


hlorovanillin-13C(
u
m

PI
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rH
rH



rH
O
rH





in
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rH
O
O
rH
1
00
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rH
rH




rH
rH
rH
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-chlorovanillin
m


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in
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O
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VJJ
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in
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rH
1
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r-
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rH



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CM
rH
rH


-chlorovanillin
VD


*
CM
0
rH



O
VO
o





in
CM


in
o
rH
rH
1
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O
rH



CO
rH




P)
rH
rH


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t
PI

r-
rH
0
rH















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H
1

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VO
rH




CO
in
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rH

c?
ichlorocatechol-1
7
in
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CTl
rH
rH
rH

oo

-------



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I~J ^"S^
Q cn

III
s


's
EH 0
D4 ^
p4 ^
•H
S

o

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o ra ..
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<•-*



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O
O
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1
00
o\
"I
o

o\
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rH
rH
CO
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in
•^

cn
rH
rH



cn
^j4
•
O
in
CN

o
vo
H
rH
1
O
CN
H
rH


CO
H
r-
D-
rH
rH


-trichloroguaiacol
in
"*1
M
CN
rH
O
rH









^
CO
•*
H
1
•cji
^*
^
rH


VO
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CO
0

H


-trichloroguaiacol-
"C6
VO
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M^"
^
rH
H
rH
in
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O




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CN
o
o
rH
1
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cn
cn
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rH
H
CO
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t
VD
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^
rH
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rH
^
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to

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rH
1
m
in
rH
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oo
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ro
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CN
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VD
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00
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in

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CN
CN
rH
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m

m
CN
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CN

o
n
CN
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cn
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in
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Lorosyringaldehyde
X!
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VO
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H
1
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rH
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d
ft

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0
rH
t-H
00
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in

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o
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1
00
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cn
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O
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rH
CO
VO
CN
rH


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0)
ft


r-
o
CN
rH
ro
in
O




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in

CO
ro
CN
rH
1
CO
O
CN
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CO
rH
CO
VO
CN
rH


-trichlorocatechol
in
•^
ro
o
CN
o
rH









r-
00
in
H
1

ro
in
rH

^
VO
rH
cn
co
CN
rH


chloroguaiacol -13C6
ns
SH
4J
4J
in
rH
rH
rH
ro
CN
O




O
m

CN
o
o
H
1
00
cn
cn
o

in
rH
rH
rH
O
cn
CN
rH


rachloroguaiacol
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4J

in
rH
CN
rH
<*
VD
p




in
CN

o
r-
CN
rH
1
O
^3*
CN
rH

^J1
CO
r-l
rH
O
ro
rH


ichlorosyringol |
SH
4J


co
CN
o
H









o
cn
vo
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1
O
ro
vo
H


vo
r-l
in
vo
ro
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chlorocatechol-13C6
n!
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CN
H
H



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H
O
in

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m
rH
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cn
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ro
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ed by the internal standard
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-------
                             f
Table 3.  DFTPP Mass  Intensity  Specifications1
     1 Reference 7
Mass
51
68
69
70
127
197
198
199
275
441
442
443
Intensity Required
8 to 82% of m/z 198
less than 2% of m/z 69
11 to 91% of m/z 198
less than 2% of m/z 69
32 to 59% of m/z 198
less than 1% of m/z 198
basfe peak, 100% abundance
4 to 9% of m/z 198
11 to 30% of m/z 198
44 to 110% of m/z 443
30 to 86% of m/z 198
14 to 24% of m/z 442
                            1131

-------
Table 4.  Characteristic m/z's of.Chlorophenolic Compounds
Compound
4 -chlorophenol
2 , 4 -dichlorophenol
2 , 4 - di chl orophenol - d3
2 , 6-dichloropheno'l
2,4, 5 - trichlorophenol
2,4, 6 -trichlorophenol
2,3,4, 6-tetrachlorophenol
pentacJU-oropftenol
pentachlorophenol"13C6
4 -chloroguaiacol
4-chloroguaiacol-13C6
3 , 4 -dichloroguaiacol
4 , 5 -dichloroguaiacol
4 , 6 -dichloroguaiacol
3,4, 5-trichloroguaiacol
3,4, 6-trichloroguaiacol
4 , 5 , 6-trichloroguaiacol
4,5, 6-trichloroguaiacol-13C6
tetrachloroguaiacol
tetrachloroguaiacol-13C6
4 -chlorocatechol
3 , 4-dichlorocatechol
3 , 6 -di chlorocatechol
4, 5 -di chlorocatechol
4 , 5-dichlorocatechol-13C6.
3,4, 5 - trichlorocatechol
3,4, 6 -trichlorocatechol
tetrachlorocatechol
tetrachlorocatechol -13C6
5-chlorovanillin
5-chlorovanillirr13C6
6-chlorovanillin
5, 6-dichlorovanillin
2 -chlorosyringaldehyde
2 , 6-dichlorosyringaldehyde
trichlorosyringol
Primary m/z
128
162
167
162
196
196
232
266
272
158
164
192
192
192
226
226
226
234
262
268
144
178
178
178
184
212
212
248
254
186
192
186
220
216
250
256
Sample Matrix Internal Standard (SMiS)
3,4, 5 -trichlorophenol
196
Instrument Internal Standard (IIS)
2,2' -dif luorobiphenyl
190
                            1132

-------











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-------
        10 -
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                                                        J	L
                 T
                  2
T	1	1	1	J—
 10    20      50      100   200
                                Concentration (ng/mL)
                        The dotted lines enclose a ±10% error window.
             Figure 1.  Relative Response Calibration Curve for Phenol
                                      1136
Figure 3.  Extracted Ion-Current Profiles for (3A) Unlabeled Compound, (3B) Labeled
          Compound, and (3C) Equal Mixture of Unlabeled and Labeled Compounds
                                     1138
                                     1140

-------
     Area at

VER:.  See Calibration verification .standard.
                         1145

-------
       Area at
Area at
M/Z
                                                     Area at
  Figure 2.  Extracted Ion-Current Profiles for Chromatographically
           Resolved Labeled (Mg/Z) and Unlabeld (M-,/Z) Pairs
                                 1137

-------
 10 -
1.0 -
0.1  -
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                             10
—r-
 20
—i—
 50
—i	r—
 100   200
                           Concentration (ng/mL)
                  The dotted lines enclose a ±10% enor window.
      Figure 1.  Relative Response Calibration Curve for Phenol
                                 1136

-------
                      Area= 46100
                                              Area= 47SO
            (3BJ
                    Area= 2650
                                              Area= 43600
            (3CJ
                     Area = 49200
                                             Aiea= 4S300
Figure 3.   Extracted Ion-Current Profiles for (3A) Unlabeled Compound, (3B) Labeled
          Compound, and (3C) Equal Mixture of Unlabeled and Labeled Compounds
                                   1138

-------
•J0:12
13:24            1648            20:00

           Retention lime (Minutes)
  I
23:12
                 Figure 4.   Chromatograim of Chlorophenolbs
                                   1139

-------
20.0 Glossary of Definitions and Purposes



These definitions and purposes are specific to this method



but have been conformed to common usage as much as possible,



20.1 Units of weight and measure and their abbreviations



20.1.1  Symbols.



           °C          degrees  Celsius



           AtL          microliter  '



           <           less  than



           >           greater  than



           %           percent






20.1.2  Alphabetical characters.



           cm   •       centimeter
                                  *


           g   ,        gram



           h           hour



           ID          inside diameter



           in.         inch



           L           liter



           M           Molecular ion



           m           meter



           mg          milligram



           min         minute



           mL          milliliter



           mm          millimeter



           m/z         mass-to-charge ratio
                            1140

-------
           N           normal;  gram molecular weight of


                       solute;divided by hydrogen equivalent


                       of  solute,  per liter of solution


           OD          outside  diameter


           pg          picogram


           ppb         part-per-billion


           ppm         part-per-million


           ppt         part-per-trillion


           psig        pounds-per-square inch gauge
                             ,            ,

           v/v         volume:per  unit volume


           w/v         weight,per  unit volume





20.2  Definitions and acronyms (in alphabetical order).
                     *        ''

     Analyte:  A chlorophenol'ic tested for by this method.


The analytes are listed in Table 1.


     Calibration standard (CAti) :   A solution prepared from a


secondary standard and/or stock solutions and used to


calibrate the response of the; instrument with respect to


analyte concentration.


     Calibration verification standard  (VER):  The mid-point


calibration standard (CSS) that is used to verify


calibration.   See Table 4.   '              .                      '    "
                             <                                    i

     Chlorophenolics:   collectively, the analytes listed in


Table 1.                     i


     CS1, CS2, CSS, CS4,, CS5:'  See Calibration standards and


Table 4.                     '



                             11141                                  ^^

-------
      Field blank:   An aliquot  of  reagent  water or other



 reference  matrix that is  placed in a  sample  container in the



 laboratory or  the  field,  and treated  as a sample  in all



 respects,  including exposure to sampling  site  conditions,



 storage, preservation, and  all  analytical procedures.   The



 purpose of the field blank  is  to  determine if.  the field or



 sample transporting procedures  and environments have



 contaminated the sample.




      GC:   Gas  chromatograph or  gas chromatography.



      HRGC:  High resolution GC.




      IPR:   Initial  precision and  recovery; four aliquots of



 the diluted PAR standard  analyzed to  establish the  ability



 to generate acceptable precision  and  accuracy.  An  IPR  is



 performed  prior to  the first time  this method-  is  used and



 any time the method  or instrumentation is modified.



      K-D:   Kuderna-Danish concentrator; a device  used to



 concentrate the analytes in a solvent.



      Laboratory blank:  See Method blank.




      Laboratory control sample  (LCS):   See Ongoing precision



 and recovery standard  (OPR).




      Laboratory reagent blank:   See Method blank.



     May:  This action, activity,  or procedural step is



neither required nor prohibited.




     May not:   This action,  activity,  or procedural step is



prohibited.
                            1142

-------
     Method blank:  An aliquot of reagent water that is



treated exactly as a sample including exposure to all



glassware, equipment, solvents, reagents, internal



standards, and surrogates that are used with samples.  The



method blank is used to determine if analytes or



interferences are present in•the laboratory environment,  the



reagents, or the apparatus. ;


     Minimum level  (ML):  The level at which the entire



analytical system must give a recognizable signal and
                            n


acceptable calibration pointjfor the analyte.  It is



equivalent to the concentration of the lowest calibration



standard, assuming that all method-specified sample weights,



volumes, and cleanup procedures have been employed.



     MS:  Mass spectrometer or mass spectrometry.



     Must:  This action, activity, or procedural step is



required.


     OPR:  Ongoing precision and recovery standard  (OPR); a



laboratory blank spiked with: known quantities of analytes.



The OPR is analyzed exactly like a sample.  Its purpose is



to assure that the results produced by the laboratory remain



within the limits specified in this method for precision and



recovery.                   :


     PAR:  Precision and recovery standard; secondary



standard that is diluted and spiked to form the IPR and OPR.



     Preparation blank:  See Method blank.
                             1143

-------
      Primary  dilution  standard:  A  solution containing the



specified  analytes  that  is  purchased  or prepared from stock



solutions  and diluted  as needed  to  prepare calibration



solutions  and other solutions.



      Quality  control check  sample  (QCS):  A sample



containing all or a subset  of- the analytes at known



concentrations.  The QCS is obtained  from a source external



to the laboratory or is  prepared from a source of standards



different  from the  source of calibration standards.  It is



used  to check laboratory performance  with test materials



prepared external to the normal  preparation process.



      Reagent  water:  Water  demonstrated to be free from the



analytes of interest and potentially  interfering substances



at the method detection  limit for the analyte.



      Relative standard deviation (RSD):  The standard



deviation  times 100 divided by the mean.



      RF:   Response  factor.  See  Section 10.5.1.



      RR:   Relative  response.  See Section 10.4.4.



      RSD:  See Relative  standard deviation.



      Should:  This  action,  activity, or procedural step is



suggested  but not required.




      Stock solution:  A  solution containing an analyte that



is prepared using a reference material traceable to EPA,  the



National Institute  of Science and Technology (NIST),  or a



source that will attest  to  the purity and authenticity of



the reference material.






                            1144

-------
VER:  See Calibration verification standard.
                        1145

-------

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-------