§ 16.102. Approved EPA and DEP analytical methods and detection limits.

 Appendix A, Table 2A contains approved Department analytical methods and detection limits. The following data elements are to be used as follows:

   (1)  The Chemical Abstracts Service (CAS) number, a unique chemical identifier, is to be used for completeness of identification. The CAS number should always be verified to ensure proper identification, particularly with chemicals with ambiguous or unfamiliar names, or both.

   (2)  If the EPA has an approved test method for analysis of a specific pollutant, the NPDES permittee shall use the approved test method (or an approved alternate test method) for the specific pollutant under 40 CFR Part 136 (relating to guidelines establishing test procedures for the analysis of pollutants). Methods are detailed in one or more of the following sources:

     (i)   EPA-approved analytical methods and guidelines in 40 CFR Parts 122, 136, 141, 143, 430, 455 and 465. EPA-approved analytical methods must be sufficiently sensitive and capable of detecting and measuring the pollutants at or below the applicable water quality criteria or permit limits consistent with the EPA’s regulations in 40 CFR Part 122 (relating to EPA administered permit programs: the National Pollutant Discharge Elimination System) and 40 CFR Part 136.

     (ii)   If an EPA-approved analytical method is not available for a pollutant, an analytical method may be used that is capable of detecting and measuring the pollutant at or below the applicable water quality criterion or permit limit. The analytical method should be consistent with guidelines for developing analytical methods, as described in this Chapter.

     (iii)   Standard Methods for the Examination of Water and Wastewater, 20th Edition, APHA-AWWA-WEF, 1998.

     (iv)   Hach Handbook of Wastewater Analysis, Hach Chemical Company, 1979.

     (v)   Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029. Applied Research Laboratories, Inc., 1986-Revised 1991, Fison Instruments, Inc.

     (vi)   ASTM Annual Book of Standards, Section 11, Water. American Society for Testing and Materials, 1999.

   (3)  MDL is the method detection limit for each chemical for each method. The MDL is defined as the minimum concentration that can be measured and reported with 99% confidence that the value is above zero—that is, something is really there. The MDL achieved in a given analysis will vary depending on instrument sensitivity and matrix effects.

     (i)   When MDLs are not available, detection limits based on other criteria approved by the Department may be used.

     (ii)   For any pollutant with an effluent limitation below the method detection limit, the permittee is expected to generally achieve the detection limit of the most sensitive method that is below detection available.

     (iii)   If two approved analytical methods for the same parameter have detection limits that differ by less than 1 µg/l or a factor of 2 (whichever is greater), the permit may be written designating either method as acceptable. The permittee also has the option of using an alternate method approved by the Department and the EPA that the permittee selects as long as the level of detection of the cited method or the numerical water quality-based limit are achieved.

     (iv)   When the EPA has not performed an MDL study or reported the detection limit, other sources—particularly, Standard Methods—are consulted. When there is no literature on detection limit, the Department’s Bureau of Laboratories may develop a detection limit or review and approve a Department-accredited lab’s development of a detection limit using an MDL study.

   (4)  Permittees will be required to meet the detection limits listed in Appendix A, Table 2A.

   (5)  When permittees cannot meet a listed detection limit, they may be granted case-specific MDLs if they submit complete documentation demonstrating a matrix effect in their particular effluent. The permittees shall follow the procedure for determining MDLs published in Appendix B of 40 CFR Part 136. The Bureau of Laboratories will evaluate the data and advise the regional office of their decision.

Source

   The provisions of this §  16.102 adopted March 10, 1989, effective March 11, 1989, 19 Pa.B. 1059; amended April 9, 1993, effective April 10, 1993, 23 Pa.B. 1727; amended November 17, 1995, effective November 18, 1995, 25 Pa.B. 5067; amended November 17, 2000, effective November 18, 2000, 30 Pa.B. 6111; amended February 11, 2005, effective February 12, 2005, 35 Pa.B 1223; corrected March 18, 2005, effective February 12, 2005, 35 Pa.B. 1761 and 1890; amended July 10, 2020, effective July 11, 2020, 50 Pa.B. 3485. Immediately preceding text appears at serial pages (343902) and (367479).

Cross References

   This section cited in 25 Pa. Code §  250.10 (relating to measurement of regulated substances in media).

APPENDIX A

TABLE 1
[Reserved]

TABLE 1A
[Reserved]

TABLE 2A

APPROVED DEP ANALYTICAL METHODS AND
DETECTION LIMITS

Parameter (CAS)		Method Number (Description) Source	Detection Limit (µg/l)
* 14M	CYANIDE, FREE (00057125)	—(DEP Free CN method, Auto) Not EPA approved	1
—	BENZENE METADISULFONIC ACID (00098486)	OR 357A Test America, HPLC/UV or LC/MS/MS	50
—	BENZENE MONOSULFONIC ACID (00098113)	OR 357A Test America, HPLC/UV or LC/MS/MS	50
—	P-PHENOL SULFONIC ACID (00098679)	OR 357A Test America, HPLC/UV or LC/MS/MS	50

 * EPA currently measures ‘‘total cyanide’’ to satisfy cyanide limits and has not yet approved analytical methods for ‘‘free cyanide.’’ Free cyanide is a DEP required analysis, and either of the three listed methods are acceptable for its determination.

TABLE 2B
[Reserved]

TABLE 3
[Reserved]

Source

   The provisions of this Appendix A adopted March 10, 1989, effective March 11, 1989, 19 Pa.B. 1059; corrected April 7, 1989, effective March 11, 1989, 19 Pa.B. 1575; amended August 31, 1990, effective September 1, 1990, 20 Pa.B. 4628; amended December 21, 1990, effective December 22, 1990, 20 Pa.B. 6299; amended January 18, 1991, effective January 19, 1991, 21 Pa.B. 234; amended April 9, 1993, effective April 10, 1993, 23 Pa.B. 1727; amended October 15, 1993, effective October 16, 1993, 23 Pa.B. 4906; amended November 17, 1995, effective November 18, 1995, 25 Pa.B. 5067; amended November 17, 2000, effective November 18, 2000, 30 Pa.B. 6111; amended May 15, 2009, effective May 16, 2009, 39 Pa.B. 2543; amended July 19, 2013, effective July 20, 2013, 43 Pa.B. 4103; amended July 10, 2020, effective July 11, 2010, 50 Pa.B. 3485. Immediately preceding text appears at serial pages (367480) to (367500).

Cross References

   This appendix cited in 25 Pa. Code §  16.41 (relating to changes and additions); 25 Pa. Code §  16.51 (relating to human health and aquatic life criteria); 25 Pa. Code §  16.102 (relating to approved EPA and DEP analytical methods and detection limits); and 25 Pa. Code §  93.1 (relating to definitions).

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