EPA 811-Z-94-006 Monday December 5, 1994 s E ^ Part II Environmental Protection Agency 40 CFR Parts 141 and 143 Analytical Methods for Regulated Drinking Water Contaminants; Final Rule ------- ------- 62456 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations ENVIRONMENTAL PROTECTION AGENCY 40 CFR Parts 141 and 143 [WH-FRL-5116-4] RIN 2040-AC12 National Primary and Secondary Drinking Water Regulations: Analytical Methods for Regulated Drinking Water Contaminants. AGENCY: Environmental Protection Agency (EPA). ACTION: Final rule. SUMMARY: EPA is promulgating the use of several new analytical methods and updated versions of previously approved methods for a number of regulated contaminants in drinking water. At the same time, the Agency is withdrawing approval of outdated methods or outdated versions of the same methods. The purpose of the rule is to approve new methods, withdraw outdated methods, and update older methods for analysis of regulated contaminants in drinking water. The rule is expected to eliminate unnecessary duplication by withdrawing older versions of the same method, and satisfy public requests for approval of new technologies in drinking water analyses. DATES: This final rule is effective on January 4,1995. The incorporation of the publications listed in this document are approved by the Director of the Federal Register as of January 4,1995. ADDRESSES: Copies of the public comments received on the proposal, EPA's responses, and all other supporting documents are available for review at the U.S. Environmental Protection Agency (EPA), Drinking Water Docket, 401 M Street, S.W., Washington, D.C. 20460. For access to the docket material, call (202) 260-3027 on Monday through Friday, excluding Federal holidays, between 9:00 am and 3:30 pm Eastern Time for an appointment. FOR FURTHER INFORMATION CONTACT: Dr. Jitendra Saxena, Drinking Water Standards Division, Office of Ground Water and Drinking Water (4603), U.S. Environmental Protection Agency, 401 M Street, S.W., Washington, D.C. 20460, (202) 260-9579. General information may also be obtained from the EPA Safe Drinking Water Hotline. Callers within the United States may reach the Hotline at (800) 426^1791. The Hotline is open Monday through Friday, excluding Federal holidays, from 9:00 am to 5:30 pm Eastern Time. For technical information regarding chemistry methods, contact Richard Reding, Ph.D., Office of Ground Water and Drinking Water (TSD), U.S. Environmental Protection Agency, Cincinnati, Ohio 45268, telephone (513) 569-7946, or Baldev Bathija, Ph.D., Office of Ground Water and Drinking Water (MC-4603), U.S. Environmental Protection Agency, Washington, D.C. 20460, telephone (202) 260-3040. For technical questions regarding microbiology methods, contact Paul S. Berger, Ph.D., Office of Ground Water and Drinking Water (MC-4603), U.S. Environmental Protection Agency, Washington, D.C. 20460, telephone, (202) 260-3039. SUPPLEMENTARY INFORMATION: EPA Regional Offices: I JFK Federal Bldg., One Congress Street, llth floor, Boston, MA 02203, Phone: (617)565-3610, Jerry Healey II 26 Federal Plaza, Room 824, New York, NY 10278, Phone: (212) 264-1800, Walter Andrews III 841 Chestnut Building, Philadelphia, PA 19107, Phone: (215) 597-9873, Stuart Kerzner IV 345 Courtland Street, N.E., Atlanta, GA 30365, Phone: (404) 347-3633, Wayne Aronson V 77 West Jackson Boulevard, Chicago, IL 60604, Phone: (312) 353-2151, Ed Walters VI1445 Ross Avenue, Dallas, TX 75202, Phone: (214) 655-7150, Thomas Love VII 726 Minnesota Avenue.Kansas City, KS 66101,Phone: (913) 276-7032, Ralph Langemeir VIII One Denver Place, 999 18th Street, Suite 500, Denver, CO 80202-2466, Phone: (303) 293-1652, Patrick Crotty IX 75 Hawthorne Street, San Francisco, CA 94105, Phone: (415) 744-1817, William Thurston X1200 Sixth Avenue, Seattle, WA 98101, Phone: (206) 553-4092, Kenneth Feigner Table of Contents I. Statutory Authority II. Regulatory Background III. Explanation of Today's Action IV. Response to Comments Received on the Proposed Rule and Notice of Availability V. Availability and Sources for Methods Information VI. Regulation Assessment Requirements VII. References I. Statutory Authority The Safe Drinking Water Act (SDWA), as amended hi 1986, requires EPA to promulgate national primary drinking water regulations (NPDWRs) which specify maximum contaminant levels (MCLs) or treatment techniques for drinking water contaminants (42 U.S.C. 300g-l). NPDWRs apply to public water systems (42 U.S.C. 300f(l)(A)). According to section 1401(1)03) of the Act, NPDWRs include "criteria and procedures to assure a supply of drinking water which dependably complies with such maximum contaminant levels; including quality control and testing procedures. * * *" In addition, Section 1445 (a) of the Act authorizes the Administrator to establish regulations for monitoring to assist in determining whether persons are acting in compliance with the requirements of the SDWA. EPA's promulgation of analytical methods is authorized under these sections of the SDWA as well as the general rulemaking authority in SDWA Section 1450(a) (42 U.S.C. 300j-9(a)). II. Regulatory Background EPA has promulgated analytical methods for all currently regulated drinking water contaminants for which MCLs or monitoring requirements have been promulgated. In most cases, the Agency has promulgated regulations specifying (i.e., approving) use of more than one analytical method for a contaminant, and laboratories may use any one of them for determining compliance with an MCL or monitoring requirement. After any regulation is published, EPA may amend the regulations to approve additional methods, or modifications to approved methods, or withdraw methods that become obsolete. On December 15,1993, EPA proposed to approve the use of several new methods and modifications of existing methods that EPA believed were as good as, or better than, current methods and procedures (58 FR 65622). The Agency also proposed to withdraw approval for outdated methods or outdated versions of the same methods. In addition, EPA published a Notice of Availability (NOA) (59 FR 35891) on July 14,1994, to make available data from EPA's evaluation of several new analytical methods, and to propose withdrawal of approval for several outdated EPA methods. EPA requested public 'comments on the proposal and on the NOA. Today's notice takes final action on the methods covered by the proposal and the NOA. III. Explanation of Today's Action With a few minor exceptions, which are described below, the actions described in the 1993 proposed rule and the 1994 NOA are approved in today's rule. The coliform transit time will remain at 30 hours, and the Agency will not require systems to hold samples at 10 °C during transit. EPA will approve the Colisure test for simultaneously determining the presence of total coliforms and E. coli. ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62457 In the July 1994 NOA, EPA described the new versions of EPA Methods 200.7, 200.8, 200.9, 245.1 (EPA, 1994a) and 504.1 (EPA, 1993d) that are approved in today's rule. Mercury and sodium have been added to the analytical scope of Methods 200.8 and 200.7, respectively. EPA is approving EPA Method 508.1 (EPA, 1994c), \vhich allows liquid-solid extraction (LSE) procedures to be used under Method 508 conditions for analysis of many analytes contained in EPA Methods 507 and 508. A minor revision to dioxin method 1613 that allows use of LSE is approved. Hexachlorocyclo-pentadiene has been added to the analytical scope of EPA Method 508. Trimethylsilyldiazomethane may be used as an alternative derivatizing reagent in Methods 515.1 and 515.2. EPA Methods 150.1,150.2 and 515.1 are not withdrawn. Turbidity measurements of samples need not be made immediately before beginning an analysis for metals; it is only necessary that the sample be acidified and held for sixteen hours. For EPA Method 531.1 (carbamales), samples no longer need to be frozen, thereby eliminating the possibility of frozen samples breaking the sample vial. Standard Method 6610 is approved as an alternative to Method 531.1. Analysis for 2,3,7,8-TCDD (dioxin) with Method 1613, or for asbestos with Method 100.1 or 100.2 can be simplified by using the guidance contained in the EPA document, Technical Notes on Drinking Water Methods (EPA, 1994d). Technical Notes contains mandatory and optional procedures that will be died in the drinking water regulations. EPA is also correcting minor errors in the 1993 proposal. An erroneous listing of USGS methods 1-2822-85 and I- 2823-85 for sulfate, and ASTM D2036- 91A for cyanide are removed in today's rule. The ASTM method had been listed twice in the table of approved methods. A typographical error occurred in listing the USGS method for silver and the ASTM method for chloride. The correct listings are USGS 1-3720-85 (silver) and ASTM D4327-91 (chloride). The effective date for all actions in this rule, except withdrawal of obsolete methods, is January 4,1995. The withdrawal date for obsolete methods is July 1,1996 (or 18 months from publication, whichever is later), which is a year later than proposed. After this date, EPA's manual "Methods for Chemical Analysis of Water and Wastes" (EPA, 1983a) will contain only three approved drinking water methods—Methods 150.1,150.2, and 245.2. To spare new laboratories the expense of purchasing this manual, EPA will provide single copies of these methods to users who do not have a copy of the 1983 manual. For the convenience of readers and for clarity of the rules, methods that are withdrawn will be specified only by tabulating them in the document, Technical Notes on Drinking Water Methods (EPA, 1994d), and in the next revision of the Manual for the Certification of Laboratories Analyzing Drinking Water (EPA, 1990b). IV. Response to Comments Received on the Proposed Rule and Notice of Availability EPA received 136 comments on the December 15,1993, proposal; 92 comments were related to chemical- analytical methods and 79 comments were related to the methods associated with the coliform and surface water treatment rules. The Agency received twenty comments on the July 14,1994, Notice of Availability. The commenters included analytical laboratories, water utilities, analytical instrument manufacturers, State and local regulators, and trade associations. A summary of major comments and the Agency's response to the issues raised are presented in this section. The Agency's detailed response to the comments received on the 1993 proposed rule and the 1994 NOA is available in the public docket for this rule (EPA, 1994e). A. New Methods Comment on the ten new methods was favorable. These methods, EPA methods 100.2, 551, 552.1, 555, Standard Methods 4500-C1-E, 4500-C1- H, 4500-C1-I, 4500-Os-B, 4500-C1O2-E and Great Lakes Instruments Method 2 were described in the 1993 proposal. Specific public comments on some of the methods are answered below. EPA Method 100.2 (asbestos) Four comments contained several suggestions and criticisms. Method 100.2 has been editorially revised to reflect the comments. These changes, however, do not affect the performance, cost or applicability of the method. One commenter asked EPA to approve SM 2570 for asbestos, which was published in a 1994 supplement to the eighteenth edition of Standard Methods (APHA, 1994). EPA does not approve SM 2570 for asbestos in today's rule, because this method differs in significant ways from Method 100.2. For example, SM 2570 uses a larger pore filter (0.45 micron) to trap asbestos fibers, while EPA method 100.2 uses a 0.22 micron filter. The commenter did not provide any data comparing asbestos trapping efficiency of these two filters, whereas EPA has data (EPA, 1994e) to show that larger pore-size filters trap fewer asbestos fibers in drinking water samples. Method 552.1 A commenter asked that the sodium hydroxide rinse in Method 552il be optional, because the rinse is not compatible with their LSE product. Method 552.1 was developed and validated with ion exchange cartridges to take advantage of the special chemical properties of dalapon and the other acids covered by the method. To efficiently extract the acids the ion exchange resin must be activated with a sodium hydroxide rinse. Sorbent conditioning and elution steps, which are specified in Method 552.1 or any LSE method, cannot be modified or eliminated to accommodate the support material. Thus, EPA will not allow the sodium hydroxide rinse in Method 552.1 to be optional, because EPA has received no data to support the commenter's request to make the rinse optional. The same commenter asked for a more generic definition of LSE media in Method 552.1 and in other LSE methods. The commenter believes EPA is unnecessarily narrowing the choice of LSE disks and cartridges. EPA does not believe LSE methods are overly restrictive in allowing use of alternative LSE disks or cartridges. However, EPA believes that additional guidance to help users correctly choose alternative LSE media without compromising the reliability of the analysis would be useful. The guidance is summarized below and will be published in Technical Notes on Drinking Water Methods (EPA, 1994d). The guidance is applicable to all LSE methods and supersedes the phrase "or equivalent" that is used in some methods to describe selection of alternative LSE cartridges or disks. Liquid-solid extraction is performed using various sorbents that are either packed into a cartridge or enmeshed in a disk of inert support material. EPA methods describe the cartridge or disk that was used to develop the LSE procedure, and to produce the data which is published in the method. If a product is mentioned in the methods, it is for information purposes only. EPA believes various LSE cartridges and disks may be used, provided they meet all quality control requirements of the method, and provided they contain a sorbent that uses the same physicochemical principles as the cartridge or disk that is described in the approved LSE method. To demonstrate that alternative LSE cartridges and disks meet all quality control criteria, the analyst must be aware of the chemistry of the method. For example, in ------- 62458 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations evaluating Method 552.1 the recovery of the free acid (not a chemical derivative) from the water sample must be tested with the alternative LSE cartridge or disk. In judging LSE disk media, both the sorbent and the support must be evaluated. In the case of sorbents, similarities in polarity are not sufficient. For example, a Gig-Silica sorbent may not perform the same as a styrene divinylbenzene copolymer sorbent. Thus, these sorbents would not be considered to be equivalent. In judging supports, any physical support used to hold the sorbent is acceptable provided the support is inert and compatible with the solutions or solvents required in the conditioning and elution steps of the method. However, any sorbent conditioning or elution steps, which are specified in the method must not be modified or eliminated to accommodate the support material. EPA Method 555 Several commenters noted that the method detection limits (MDLs) for some analytes were greater than MDLs in the alternative method (EPA Method 515.1), or were too high to meet monitoring triggers, which are specified at 40 CFR 141.24(h)(18). Thus, they questioned whether Method 555 was a suitable alternative to Method 515.2. EPA believes commenters mistakenly looked at MDLs in Table 2 of Method 555, which shows the results of spikes at 10 ppb. However, spikes at 0.5 ppb (Table 5 in the method) resulted in MDLs that are equivalent to Method 515.1 MDLs, and these MDLs have been validated in a second laboratory (EPA, 1992a). EPA also notes that monitoring triggers for several organic contaminants, including Method 555 analytes, may be amended in a future rulemaking (EPA, 1993b, 1994f). Great Lakes Instruments (GLI) Method 2 (turbidity) Some commenters objected to the method because it is vendor and instrument-specific. EPA generally develops and approves methods that are not vendor-specific. Users are not limited to the GLI method; generic methods SM 2130B and EPA 180.1 are approved for turbidity. However, under the Alternative Test Procedures (ATP) program EPA has approved vendor-specific methods or products as alternatives to approved methods (53 FR 5142, February 19, 1988). GLI Method 2 was evaluated under EPA's ATP program and recommended for approval as an alternative method. EPA realizes GLI is the source of copies of GLI Method 2, which is a factor a laboratory choosing to adopt this method must consider. Some commenters believed the GLI method should be approved as a version of an international procedure, ISO 7027. The ISO procedure measures turbidity via either 90° scattered or transmitted light depending on concentration. Although instruments conforming to ISO 7027 specifications are similar to the GLI instrument, only the GLI instrument uses pulsed, multiple detectors to simultaneously read both 90° scattered and transmitted light. EPA has received no data on the ISO 7027 use of separate 90° scattered or transmitted light measurements to judge equivalency to other approved turbidity methods. SM 4500-C1-E, Low Level Amperometric Titration A commenter noted a typographical error in a calculation in SM 4500-C1-E, which the Standard Methods Committee has agreed to correct. In approving SM 4500-C1-E, EPA will print the correct formula for SM 4500-C1-E in Technical Notes on Drinking Water Methods (EPA, 1994d). The Standard Methods Committee will publish a correction to this method in the next (19th) edition of Standard Methods (Eaton, 1993a). SM 6610 (APHA, 1994) A commenter asked to approve this method as an alternative to EPA Method 531.1. EPA aided the development of this method, which was published in 1994 in a supplement to the eighteenth edition of Standard Methods. EPA agrees •with the commenter, and will approve SM6610 for analysis of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbaryl, carbofuran, 3- hydroxycarbofuran, methomyl, and oxamyl. EPA Method 1613, Revision B, dioxin (EPA, 19941) EPA was asked to replace the approved Revision A of Method 1613 with Revision B. EPA agrees with the suggestion. As with Revision A, users can greatly simplify use of Revision B of Method 1613 when only 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) is to be determined in drinking water samples by using procedures described in Technical Notes on Drinking Water Methods (EPA, 1994d). EPA proposed Revision A of Method 1613 for the monitoring of several chlorinated dioxins and furans under the Clean Water Act on February 7,1991 (56 FR 5090), and approved it only'for measurement of 2,3,7,8-TCDD under the Safe Drinking Water Act on July 17, 1992 (57 FR 31803). In response to comments on the 1991 proposal, EPA developed Revision B. The only technical changes made in Revision B that affect determination of 2,3,7,8- TCDD in drinking water matrices are (1) slight changes in performance specifications based on the compilation of data from interlaboratory and other studies, (2) additional language intended to provide analysts with increased flexibility to use liquid solid extraction procedures, and (3) further clarification of the documentation required when analysts employ the flexibility provided in the method to use alternate techniques not explicitly described in the method. B. Expanded Scope for Already Approved Methods Comments on expanding the analytical scope of these five methods were favorable. These methods, EPA Methods 200.8, 200.9, 300.0, SM 4110B, and American Society for Testing and Materials (ASTM) method D4327-91, were discussed in the 1993 proposal or the 1994 NOA. Specific comments requesting that approved methods cover additional analytes are described and answered below. A commenter asked EPA to expand the scope of Method 200.8 to include additional metals that are not currently regulated by EPA. While EPA encourages laboratories to use any approved method for all contaminants that are within the analytical scope of the method, EPA can only approve a method for contaminants that are regulated. One commenter asked why Method 200.9 did not include the secondary drinking water contaminant, zinc. EPA believes analysis of zinc with Method 200.9 is impractical, because the instrument and procedure used are very sensitive to small amounts of lead. The analysis is subject to random contamination, and the concentration range of zinc that can be reliably measured is too narrow to be of use with typical drinking water samples. EPA recommends more suitable methods (EPA 200.7, 200.9, SM 3120B and SM 3111B) for measurement of zinc in drinking water samples. Commenters were concerned about expanding the scope of the ion chromatography methods to include fluoride. They believed that EPA did not have data to show that interference problems would not preclude use of ion chromatography for the analysis of fluoride in drinking water samples. EPA's 1990 study (Bionetics) which involved participation of seventeen laboratories demonstrated that fluoride can be reliably measured in drinking water samples with ion chromatography. Thus, EPA has no hesitation in approving the three proposed ion chromatography methods for the analysis of fluoride in drinking water. ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62459 C. Updated Methods Comment on updating earlier versions of six methods to the current versions was favorable. These methods, EPA Methods 504.1, 515.2, 524.2, 525.2, 548.1 and 549.1, were discussed in the 1993 proposal or the 1994 NOA. Problems were reported by a commenter with the use of trimethylsilyldiazomethane (TMSD) for derivatization of the analytes in Methods 515.1 and 515.2. The commenter suggested that EPA also allow the use of diazomethane for this purpose. EPA agrees with the commenter and, as discussed in the 1993 proposal, EPA allows use of either derivatizing reagent. However, because dalapon is not adequately derivatized by TMSD, the use of TMSD in Method 515.1 is not approved for analysis of dalapon. Procedures for using TMSD with Methods 515.1 and 515.2 are described in the document Technical Notes on Drinking Water Methods (EPA, 1994d). D. Updates to Methods by Reference to Most Recent Manual Comments were favorable on approving versions of previously approved methods that are now contained in the eighteenth edition of Standard Methods (APHA, 1992) and in five new EPA manuals (EPA, 1994a, 1991,1990a, 1992b and 1993a). These publications were described and discussed in the 1993 proposal or the 1994 NOA. Questions or requests from commenters about some of the methods contained in these publications are described and answered below. 1994 EPA Metals Manual (EPA, 1994a) Three commenters asked to add other regulated metals to the scope of Method 200.7, because use of a new axial configured inductively coupled plasma (ICP) atomic emission spcctroscopy (AES) instrument improves the sensitivity of the method to the required regulatory limits. EPA will not approve this request in today's rule, because Method 200.7 as written allows use of other types of ICP/AES instruments that cannot meet the regulatory limits for the additional metals. To extend the scope of Method 200.7 as suggested by the commenters would require either a formal ATP approval (EPA, 1993c), or publication of a new AES method that allowed only instruments with an axial configuration. 1991 Organic Methods Manual (EPA, 1991) One commenter requested a change in the scope of EPA Method 505 because of the detection limits for some method analytes. These changes included withdrawal of alachlor, atrazine and simazine, and addition of toxaphene. EPA is evaluating the detection limits in several methods. When this evaluation is complete, EPA may propose to withdraw approval of methods or modify the scope of methods, such as Method 505. In the interim, EPA does not agree that the scope of Method 505 should be changed to withdraw alachlor, atrazine and simazine. However, EPA agrees that analysis for these nitrogen-containing compounds may require use of a nitrogen-phosphorous detector (NPD) rather than the electron capture detector (ECD). Today's rule specifies that an NPD should be substituted for the ECD in Method 505 (or another approved method should be used) to determine alachlor, atrazine and simazine, if lower detection limits are required. EPA agrees with the comment about toxaphene. In today's rule EPA is correcting an omission in the 1993 proposal by continuing to approve Method 505 for toxaphene. However, EPA notes that the Method 505 MDL for toxaphene is very close to the MCL. To improve the sensitivity of the analysis analysts may wish to use Method 508 for toxaphene and other Method 505 analytes for which use of an NPD will not improve the sensitivity. Method 508 is very similar to Method 505 except that the MDLs are lower, because a larger sample volume is extracted. MCL compliance determination for PCBs requires that EPA method 505 or 508 be used as a screen for PCBs as Aroclors prior to quantitation as decachlorobiphenyl by EPA Method 508A. Three commenters requested that EPA switch the sequence of compliance methods for PCBs, i.e., use Method 508A to screen and Method 505 or 508 to quantify PCBs. The suggested change in the sequence of compliance methods is beyond the scope of this rule since it would require amending the MCL compliance determination sequence in 40 CFR 141.24(h)(13)(i)-(iii). Only Method 508A can measure decachlorobiphenyl, and § 141.24(h)(13)(ii) specifically requires "using Method 508A to quantify PCBs as decachlorobiphenyl". It was suggested by a commenter that EPA include hexachloro- cyclopentadiene (HCP) in the scope of EPA Method 508. EPA agrees with the commenter, and will allow measurement of HCP with EPA Method 508. However, the analyst must show that the analyte recoveries and other criteria, which are specified for HCP in Section 9 of Method 508.1 are achieved using Method 508 procedures. This option will be described in the document, Technical Notes on Drinking Water Methods (EPA, 1994d). 1993 EPA Inorganic Methods Manual (EPA, 1993a) A commenter asked what the differences were between Method 335.3 and the updated version, Method 335.4, since both versions require manual distillation of the sample to prepare it for measurement of cyanide. The technical differences between these methods are minor. EPA improved the automation of procedures in Method 335.4, and added the option to use a labor-saving distillation procedure. The distillation option is described in Method 335.4, and it is approved and described for other spectrophotometric methods in Technical Notes on Drinking Water Methods (EPA, 1994d). Two commenters objected to replacement of Method 335.3 with 335.4. The objection appeared to be based on the mistaken belief that Method 335.4 requires a manual distillation of the sample to prepare it for measurement of cyanide and that the earlier version, Method 335.3, did not. EPA has never allowed spectrophotometric measurements of cyanide in water samples without manual distillation of the sample using SM 4500-CN-C (cf. 40 CFR 136.3, Table IB; 59 FR 4507, January 31, 1994; and 57 FR 31839, July 17, 1992). Commenters may have been misled by a discussion in Method 335.3 of an alternate ultraviolet (UV) digestion procedure that does not require manual distillation. EPA has never approved this optional UV procedure for compliance measurements of cyanide, because EPA has no data to show that UV digestion would not provide inaccurate results that underestimate the level of contamination. To avoid manual distillation of the sample, laboratories may use a selective electrode method for cyanide. EPA notes that the "amenable" spectrophotometric methods, ASTM D2036-91B and SM 4500-CN-G, also require distillation prior to either free or total cyanide measurements. To further clarify EPA's intent to require manual distillation for all spectrophotometric determinations of cyanide, these methods will be listed at 40 CFR 141.23(k) in today's rule under the phrase "Manual distillation followed by". Immediately following this phrase, the rules specify use of SM 4500-CN- C to conduct this distillation. Microbiological Methods The vast majority of comments on the eighteenth edition version of microbiology methods concerned the maximum time between sample collection and analysis (transit time) of ------- 62460 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations drinking water samples. Commenters opposed reducing this time from 30 hours (16th edition of Standard Methods) to 24 hours (18th edition of Standard Methods). The Standard Methods committee reduced the transit time because of its concern about coliform die-off in the sample over time. Commenters opposed reducing the time because it would (1) be logistically impractical if not impossible to do, (2) increase costs for sample transport and resampling, (3) cause hardships in sample collection, and (4) complicate and decrease laboratory flexibility. A few commenters claimed that the reduced transit time is not supported by data. Coliforms usually die off over time, especially when water temperatures are warm, but EPA recognizes that there is debate among investigators over the rate of that decline. EPA is currently conducting additional studies on this question, using fecal coliforms and E. coli, and results are anticipated by the end of 1994. Given the logistical and other problems that might result by decreasing the transit time to 24 hours, EPA is deferring a decision on whether to reduce the transit time until more data become available. For the time being, the Agency has added a footnote to the Table in § 141.21(f)(3), allowing a maximum transit time of 30 hours. If EPA decides that a reduction from 30 hours is warranted, the Agency will work with the States to minimize the hardships identified in the public comments. Meanwhile, EPA strongly encourages States and systems to review their procedures and identify practical alternatives for providing samples to laboratories more quickly. Other commenters objected to the requirement in the 18th edition of Standard Methods to hold samples at less than 10 °C during transit. The Standard Methods committee specified this value because of its concern about coliform die-off in the sample at higher temperatures, where the bacterial metabolism of coliforms and non- coliforms alike is normally greater. Commenters objected to any EPA requirement that would require them to keep samples cool during sample transit. They asserted that this requirement would (1) be unnecessary and would complicate sample transport logistics, (2) increase sampling costs and shipping costs for both systems and laboratories, because coolers and ice Eacks cost money and samples are eavier and thus more expensive to ship, and (3) lead to problems with frozen samples or a significantly increased number of invalid samples. Commenters also stated that under the presence-absence concept, sample cooling was less important than under the earlier rule based on coliform density. EPA is deferring a decision on sample transit temperature until the Agency initiates a review, and possible revision, of the Total Coliform Rule. For the time being, the Agency has added a footnote to the Table in § 141.21(f)(3) encouraging, but not requiring, systems to hold samples at less than 10 °C during transit. Nevertheless, the Agency strongly encourages systems to cool their samples during transit, especially during warm summer months, to minimize coliform die-off. The Agency is currently conducting additional studies on this question, using fecal coliforms and E. coli, and results are anticipated by the end of 1994. If EPA decides that a reduction is warranted, the Agency will work with the States to minimize the hardships identified in the public comments. EPA is also approving a new method, the Colisure test, for simultaneously determining the presence of total coliforms and E. coli, both of which must be monitored under the Total Coliform Rule (40 CFR 141.21). Data supporting the use of this method was presented in the notice of July 14,1994 (NOA). Most commenters supported approval of the Colisure test, but several raised questions about the test, primarily concerning the incubation time. They cited the Broadway et al. (1992) data that indicated that only 64% and 69% of the bottles were total coliform- positive and E. co./j-positive, respectively, after 24 hours compared to the 48-hour results. According to the Broadway et al. data, 85% and 88% of the bottles were total coliform-positive and E. co/i-positive, respectively, after 28 hours compared to the 48-hour results. EPA agrees with the commenters who contended that 24 hours of incubation was insufficient for the Colisure test. The Agency, however, believes that the recovery rate after 28 hours is reasonable, and will approve the Colisure test as a 28-hour test. Moreover, based on additional data from the product manufacturer showing that the false-positive rate after 48 hours is small, EPA will allow laboratories to hold the test up to 48 hours before observing results. Chemical Methods There were only minor comments on the proposal to update chemistry methods to the versions contained in the 18th edition of Standard Methods. The 18th edition versions contain no or minor changes to earlier versions, and EPA received no comments to document specific hardships in converting to 18th edition chemical methods. Several commenters noted that, although thallium is not in the scope of SM 3113B, EPA erroneously approved SM 3113B for thallium (57 FR 31840, July 17,1992). EPA agrees and will delete this approval in today's rule. A commenter noted that the 18th edition version of SM 4500-C1-G omits instructions that would allow measurement of total residual chlorine in drinking water samples using a colorimetric method. The Standard Methods Committee has written (Eaton, 1993b) that an editorial omission, not a technical change, occurred in recent versions of SM 4500-C1-G. The error will be corrected in the next (19th) edition of Standard Methods. EPA corrects the error today by describing the omitted instructions in Technical Notes on Drinking Water Methods (EPA, 1994d). E. Methods To Be Withdrawn and Replaced General Comments Received on Withdrawal of Methods One commenter suggested that all methods carry a "draft" status for three years after publication; other commenters asked EPA to approve new methods more quickly. It would defeat EPA's intent to provide modern technology quickly, if a method had to be published, proposed, and then kept in draft status for three years. EPA balances this problem by allowing optional use of old or new methods during a transitional period, which in the case of this rule extends to July 1, 1996 (or 18 months after publication, whichever is later). Several commenters believed EPA was eliminating, or intended to eliminate, all autoanalyzer or colorimetric methods. This is incorrect; EPA is replacing only obsolete methods with equivalent ASTM, EPA and Standard Methods. EPA is not eliminating colorimetric or autoanalyzer technology for any regulated contaminant, except arsenic. Evidence of EPA's intent is in the 1993 methods manual (EPA, 1993a), which updated colorimetric methods for cyanide (335.4), nitrite and nitrate (353.2), and sulfate (375.2). EPA has and continues to approve autoanalyzer and colorimetric ASTM and Standard Methods for cyanide, fluoride, nitrite, nitrate and sulfate. Some commenters stated that changing from EPA methods to equivalent Standard Methods and ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62461 ASTM methods would be very time- consuming and expensive, but provided no specific information to support this statement. EPA is withdrawing methods that aro incomplete and often require users to rely on the equivalent ASTM or Standard Methods. Thus the change, in many cases, has already taken place. In other cases, there are very minor differences between the withdrawn and tho replacement methods. EPA notes that laboratories may continue to use a withdrawn method for other than compliance monitoring samples. EPA's actions in today's rule save laboratories money, because they need only support one version of an ASTM, EPA, or Standard Method. Prior to this rule, laboratories were required to use methods in the 14th, 16th, 17th, and 18lh editions of Standard Methods, and at least two different versions of EPA Methods 200.7 and 524.2. EPA received numerous comments requesting an extension of the withdrawal date for analytical methods. The suggested dates ranged from July 1, 1995, to July 1,2000. Based on these comments, EPA will extend the methods withdrawal date from July 1, 1995, to July 1,1996 (or 18 months from publication, whichever is later), which is beyond the withdrawal date suggested by most commenters. New methods or new versions of current methods will be approved within 30 days of publication Of the rule. This overlap in approval dates for new methods and withdrawal of obsolete methods will give laboratories sufficient time to become certified with the new methods. Comments on Withdrawal of Specific Methods Packed-Column EPA Methods Commenters generally favored withdrawal of packed column methods for volatile organic compounds (VOCs) and trihalomethanes (THMs), and replacing them with technologically advanced capillary column methods. Additional costs incurred in supporting older, obsolete methods until EPA withdraws these methods, and the suitability of capillary columns to handle the increasing number of regulated contaminants were cited as reasons for supporting withdrawal. The July 1,1995, withdrawal date may be too early, as pointed out by some commenters. EPA will extend the date to July 1,1996 (or 18 months from publication, whichever is later), to give laboratories more time to plan an orderly transition to capillary column methods. Some commenters asked EPA for continuation of the use of packed- column methods, if they meet current regulatory requirements. EPA feels that packed-column methods have many drawbacks. For example, the cis and trans dichloroethene isomers cannot be separated with the packed-columns specified for VOC analysis (Lyter, 1994). Such separation problems with packed- column methods have limited EPA's ability to prepare samples for EPA's laboratory performance evaluation (PE) program. To accommodate packed- column methods, separate PE samples are prepared for THMs and VOCs to minimize THM and VOC interferences that users of packed column EPA methods will experience. If only capillary columns are approved, EPA will have more latitude to mix VOCs and THMs in PE samples to better test laboratories with concentrations and mixtures of THMs and VOCs, as might realistically occur in drinking waters. EPA notes that laboratories may continue to use packed column methods for other than compliance monitoring analyses, such as routine plant operation or source evaluation samples. A commenter asked why EPA proposed to withdraw THM Methods 501.1 and 501.2 in the 1993 proposal, but subsequently proposed to continue approval of these packed column methods in the Information Collection Rule (ICR) (59 FR 6354 and 6413-6414, February 10,1994). In today's rule, EPA is clarifying why and how Methods 501.1 and 501.2 can and should be withdrawn without affecting analytical needs that were described in the ICR proposal. In the ICR, EPA proposed Methods 501.1 and 501.2 only because ICR data must be gathered quickly to support pending disinfectant byproduct control regulations. To support these regulations, EPA proposed to conduct THM monitoring at a limited number of PWS for eighteen months beginning in 1995. Since this data must be collected by laboratories certified to conduct THM analyses, it could be a hardship to revoke the certification of laboratories now using Methods 501.1 and 501.2. EPA notes that EPA also proposed and encouraged laboratories to use one of the capillary column methods (EPA Methods 502.2, 524.2 and 551) to conduct THM monitoring for the ICR. And in a subsequent disinfection byproduct rule (59 FR 38668, July 29, 1994) EPA proposed only capillary methods for THM compliance monitoring (59 FR 38821). As explained in the 1993 proposal and in the 1992 THM methods rule (58 FR 41344, August 3,1993), EPA intends to and will withdraw packed column methods for THM and VOC compliance analysis. To accommodate the special and immediate information collection needs of the ICR, EPA is deferring withdrawal of packed column Methods 501.1 and 501.2 until July 1,1996 (or 18 months after publication, whichever is later). This date is expected to be after the beginning of the proposed ICR monitoring period. When the ICR rule is promulgated, certification under Methods 501.1 and 501.2 will be granted such that the withdrawal date will not impede collection of THM data for the ICR. Colorimetric Methods for Arsenic—A commenter requested that EPA not withdraw colorimetric methods for arsenic. Because the detection limits of these methods are very near the MCL for arsenic, colorimetric measurements do not provide a reliable indication of variability of, or trends in, ambient concentrations of arsenic in the water supply when these concentrations are less than the MCL. EPA believes the detection limit deficiency warrants withdrawal of colorimetric methods for arsenic. In addition, since EPA approves other methods that measure all twelve regulated metals, including arsenic, it is not cost-effective to measure arsenic separately with a colorimetric method. The cost of a complete, broad-spectrum metals analysis by atomic absorption or ICP is not reduced if arsenic is not included. And EPA knows of no situation where arsenic is the only metal to be determined in a compliance sample. EPA believes that there is no scientific reason or economic need for a colorimetric method that only measures arsenic. However, EPA notes that withdrawal of these methods does not preclude their use for other than compliance monitoring samples. EPA Methods 208.2 and 354.1—A commenter asked EPA to replace EPA Methods 208.2 (barium) and 354.1 (nitrite) with the equivalent methods SM 3113B and SM 4500-NO2-B, which are published in the 18th edition of Standard Methods (APHA, 1992). EPA agrees and will withdraw Methods 208.2 and 354.1, since equivalent methods using the same equipment and procedures are approved. EPA Method 340.2 (fluoride)— Commenters expressed concern that withdrawal of this ion-selective electrode method will require use of EPA Method 300.0, which requires purchase of an ion chromatograph. This is incorrect; only the EPA ion-selective electrode method will be withdrawn. The ASTM and SM methods, which use the same equipment as the EPA method, are approved for fluoride compliance determinations. Hydrazine Methods for Nitrate and Nitrite—A commenter agreed with ------- 62462 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations EPA's withdrawal of hydrazine method 353.1, stating that the method is obsolete. The commenter, however, wanted EPA to make available at least one hydrazine method for nitrite and nitrate by approving SM 4500-NO3—H. EPA is withdrawing Method 353.1 because hydrazine is carcinogenic and toxic, and creates a significant hazardous waste disposal problem. SM 4500—NOs-H has the same problems and, therefore, cannot be approved. EPA believes users of hydrazine methods will be able to convert easily to the approved cadmium reduction methods for nitrate and nitrite by changing their reagent from hydrazine to cadmium when their supply of hydrazine is depleted. The cadmium methods, which have been approved for nitrate and nitrite since 1991, use the same equipment as the hydrazine methods. Flame AA for metals—Three commenters requested that flame atomic absorption (AA) and graphite furnace methods not be withdrawn. EPA has not withdrawn flame AA and graphite furnace methods published by ASTM or Standard Methods; only the obsolete EPA versions of these methods are withdrawn. Direct Aspiration Flame AA Methods—Some commenters wanted EPA to expand the scope of these methods to include metals other than barium and nickel. EPA cannot expand the scope, because the methods are not sensitive enough to measure metals other than barium and nickel. Method 515.1—EPA received many comments requesting that this method not be withdrawn, primarily for two reasons. First, neither proposed replacement method, 552.1 or 515.2, covers all of the regulated chemicals that are in Method 515.1. Secondly, the new dalapon method (552.1) requires significantly different equipment, procedures and skills than Method 515.1. Four commenters agreed with EPA's proposal to withdraw Method 515.1, because a combination of Methods 515.2 and 552.1 meets their regulatory needs. EPA agrees with the majority of commenters and will not withdraw Method 515.1. Methods for Secondary Contaminants—Some commenters believed that delisting a secondary contaminant method precludes its use for other than compliance monitoring samples. This is not correct; EPA does not certify laboratories for secondary monitoring, and EPA only recommends methods for secondary contaminants. Unless State requirements provide otherwise, laboratories may use methods other than those cited at 40 CFR143.4(b) for measurement of secondary contaminants. EPA Method 245.2 (mercury)—EPA was asked to withdraw this method, which is an automated, cold vapor method for mercury. EPA cannot withdraw this method because there is no other equivalent version of the method. Because EPA does not have enough information to assess the effect that withdrawal of Method 245.2 would have, it is deferring a decision on withdrawal. EPA Methods 150.1,150.2 (pH)—In the 1994 NOA, EPA proposed to replace these methods with equivalent ASTM and Standard Methods for pH. A commenter noted that the EPA methods are easier to use under field conditions. The commenter indicated that since many pH measurements are made in the field at the point of sample collection, withdrawal of the EPA methods would pose a significant hardship. EPA agrees with the commenter, and will not withdraw these methods until ASTM or Standard Methods pH methods are simplified for field use. F. Miscellaneous Reformat Listing of Methods in 40 CFR Parts 141 and 143—Commenters have asked EPA to improve the organization and clarity of the drinking water regulations. Commenters have criticized the organization of the rules, and noted difficulty in obtaining copies of drinking water regulations. They need the regulations, because they contain tables and lists of approved methods, and because mandatory method instructions are included in the text of the rules and in footnotes to the tables of methods. These instructions are not contained in the approved methods, because they were developed after the method was published. In today's rule, EPA is minimizing the use of footnotes and lengthy technical instructions in drinking water rules. EPA is accomplishing this by including these instructions in the document Technical Notes on Drinking Water Methods (EPA, 1994d). This EPA publication contains mandatory procedures, clarifications and helpful options, such as guidance on more efficient ways to conduct asbestos and dioxin compliance measurements. EPA will place these instructions in the affected method when the method is revised and published. EPA intends to use this document to publish future method corrections or modifications (after notice and comment in the Federal Register as necessary). EPA believes Technical Notes will be easier for users to obtain, read and photocopy than the tables of approved methods in the drinking water rules. Incorporating Technical Notes on Drinking Water Methods by reference in the rule has the effect of making its provisions as mandatory as those in the approved drinking water methods. EPA is improving the clarity of the rules by consolidating listings of analytical methods. Analytical methods for THMs have been moved from § 141.30 to § 141.24(e). Appendix C of § 141.30, which contained THM Methods 501.1 and 501.2, is withdrawn immediately, but the methods may be used for compliance monitoring under § 141.30 until July 1,1996 (or 18 months from publication, whichever is later). And analytical methods formerly specified for lead, copper, and corrosivity at 40 CFR 141.89(a) and sodium at § 141.41(d) are now listed with other inorganic methods at § 141.23(k)(l). EPA notes that although sodium was removed from the list of 83 contaminants included in the 1986 amendments to the SDWA (53 FR 26487), the provisions at § 141.41 still obtain. Specifications for Continuous Chlorine Monitoring Methods— Commenters favored the proposed specification for continuous chlorine monitoring measurements to be based on calibration with an approved grab sample method. Two commenters asked EPA to extend the calibration period to seven days. EPA has no data to support such an extension. However, the EPA protocol for continuous chlorine monitoring allows a laboratory to use an alternative protocol, if it is approved by the State. EPA believes it is prudent for States to monitor and approve changes to the EPA protocol, such as those suggested by commenters. The protocol approved in today's rule is specified at 40 CFR 141.74(a)(2), and allows States to grant variations, including certain changes in the chemistry of the method. Allow Interchange of Detectors in EPA Methods 505, 507, 508— Commenters favored this proposal. Two commenters noted that data with alternative detectors must be verified, and were concerned about poor BCD response of some nitrogen-containing compounds. EPA agrees that data must be verified when changing detectors, and that the results for all chemicals in Methods 505, 507 or 508 may not meet quality control requirements when an alternative detector is used. This is why Section 6.8.3 of Methods 507 and 508, and Section 10.4 of Methods 505, 507 and 508 allow alternative detectors only if the initial demonstration of capability criteria in Section 10 of each method is met by the alternative detector. ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62463 Ono commenter wanted to allow use of other detectors with EPA Method 504. EPA cannot approve this request, because EPA has no data to justify use of alternative detectors in Methods 504 or 504.1, which use an electron capture detector (ECD). The ECD has been the only detector capable of routinely measuring EDB and DBCP at the required parts-per-trillion concentrations (56 FR 3550, January 30, 1991). Guidance on Preserving Samples—A commenter asked that biocide procedures be dropped from the VOC methods, because EPA has dropped mercuric chloride as a biocide in synthetic organic chemical (SOC) methods. EPA dropped mercuric chloride from SOC methods, because EPA has no data to show that blodegradation of a regulated SOC occurs in a typical drinking water sample, and because mercuric chloride is toxic and a hazardous waste. However, EPA has data to show degradation (EPA, 1994e) in samples collected for measurement of VOCs. The biocide procedures required in the VOC methods require some combination of chilling, rapid transit and analysis, or acidification. None of these procedures pose health or waste disposal problems that compare with the problems associated \vith preservation using mercuric chloride. Therefore, EPA continues to require use of a biocide in VOC methods. Liquid-Solid Extraction (LSE) in EPA Methods 507 and 508—Some commenters believed more data were needed before EPA allowed use of LSE in Methods 507 and 508; EPA agrees. EPA stated in the December proposal that "the Agency regards this proposed modification as tentative and will base a final decision on whether to approve on public comment and additional EPA performance data." After studying this option and developing additional data (EPA, 1994e), EPA has decided not to add LSE as an option in Methods 507 and 508, because EPA does not have data to support use of this technique for all of the chemicals in the methods. As an alternative, EPA has developed and is approving Method 508.1 (EPA, 1994c). Method 508.1 uses the procedures and the electron capture detector that are used in Method 508, and it allows use of LSE. The scope of Method 508.1 covers many of the Method 507 and 508 analytes that are subject to regulated or unregulated contaminant monitoring requirements, but it does not include butachlor, PCBs or toxaphcne. In today's rule EPA will approve Method 508.1 for measurement of alachlor, atrazine, chlordane, endrin, heptachlor, heptachlor epoxide, hexachloro-benzene, hexachlorocyclopentadiene, lindane, methoxychlor, and simazine, which are regulated SOCs. It is also approved for aldrin, dieldrin, metolachlor, metribuzin, and propachlor, which are unregulated SOCs. Methods for Other Contaminants—In the 1993 proposal EPA provided guidance to systems that wish to measure chemicals that are not regulated, and need advice on what method to use. The guidance stated that "although EPA approves methods only for contaminants regulated under the Safe Drinking Water Act, the Agency encourages laboratories to use these methods for other contaminants if the method description specifically includes these contaminants." One commenter mistakenly believed that this eliminates the use of other methods or techniques, such as test kits. Although EPA encourages laboratories to save money by using a compliance method to measure all chemicals of interest that are in the analytical scope of the method, this does not preclude systems from using other methods, including test kits, for samples other than compliance monitoring samples. EPA cautions users to carefully evaluate the performance of a method when using it for samples other than compliance monitoring samples or for contaminants not regulated under the SDWA. For example, EDB and DBCP appear in the scope of EPA Methods 504.1, 502.2, 524.2 and 551. However, Methods 502.2 and 524.2 are not approved for compliance analyses, because they do not have the sensitivity to measure compliance with the EDB and DBCP MCLs. Methods Approval Process—Several commenters believe that the process of proposing and approving methods or method modifications will always be too slow to accommodate the technical and certification needs of the laboratory community. To solve this problem, commenters asked EPA to specify performance criteria in drinking water rules, or in the approved methods. The purpose of this would be to allow laboratories to use any analytical method, provided it met the mandatory criteria. EPA agrees that the present methods approval system is slow. To solve this problem, EPA and other organizations are seeking to consolidate methods across regulatory programs and media, and to write generic method performance criteria (EPA, 1994g). A performance-based method system, as suggested by commenters, might be part of the final solution. There are two groups working on this problem. The groups are the Intergovernmental Task Force on Monitoring, and EPA's Environmental Monitoring Management Council. A recommendation of these groups may be for EPA to propose a new method approval and method-writing protocol. The protocol would be designed to expedite approval of drinking water method modifications while maintaining the degree of control needed to ensure effective enforcement of drinking water regulations. Field and Test Kits—Two commenters noted an omission in the rule text in the 1993 proposal that appears to eliminate an important option. This option allows States to approve use of DPD colorimetric test kits for measurement of chlorine residuals. EPA did not intend to eliminate this option, and agrees the wording in the 1993 proposal (58 FR 65631) may be misleading. Today's rule clearly allows use of the DPD kits, provided the State also approves use of the kits. This option is specified at 40 CFR 141.74(a)(2). A commenter asked EPA to approve field kits for pH, and methods for continuous monitoring of pH and residual chlorine. EPA does not need to approve field methods for pH because currently, analysis with an approved pH method may be conducted in the field or in the laboratory. Regarding continuous monitoring methods, in today's rule, EPA provides criteria for continuous monitoring of chlorine residuals (40 CFR 141.74(a)(2)). Since EPA does not require continuous pH monitoring, EPA does not approve or disapprove methods for continuous measurement of pH. Turbidity—A commenter asked that turbidity measurements, which are specified in the drinking water regulations, be waived if no particulate or cloudiness is visible to the analyst. The present requirement is that turbidity be measured in all samples, and that digestion be performed if the turbidity is one NTU or greater. EPA cannot waive turbidity measurements on samples that appear to be clear, because samples with turbidity of up to three NTU can appear clear to the unaided eye. Corrosivity—One commenter noted the proposed rule made no reference to updating the methods for corrosivity in 40 CFR 141.42(c). These methods were published in 1980 and 1982 (45 FR 57346, August 27,1980 and 47 FR 10999, March 12,1982). In the Lead and Copper Rule (56 FR 26460, June 7, 1991), EPA agreed that corrosion control strategies could be developed or evaluated by measuring alkalinity and other parameters (56 FR 26489 and 26496). However, the Lead and Copper ------- 62464 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations Rule did not update or specify use of the methods in 40 CFR 141.42(c). Instead, more current methods were specified in 40 CFR 141.89(a) (56 FR 26509-26510). In today's rule, EPA eliminates possible confusion between the requirements in 40 CFR 141.89 and 141.42 by removing subparagraphs 40 CFR 141.42(a)-(c). New Technologies—Comments were received asking the Agency to evaluate and develop methods based on new technologies, such as bioassay, ELISA, and capillary electrophoresis. The Agency continues to incorporate new technologies in methods, and appreciates the many articles that were sent to draw attention to new technologies. In the last twenty years, the Agency has aided the development of the mass spectrometer into a powerful and routine analytical instrument. With suggestions from the laboratory community (56 FR 3550, January 30,1991), the Agency moved from packed to capillary column gas chromatographic technology, and expects to adopt innovative procedures and instruments in future methods. In the 1993 proposal, EPA invited public suggestions that EPA might consider approving in this rule or in a later rulemaking. This invitation was not meant to imply that new methods or method modifications submitted as suggestions would or could bypass requirements that are specified at 40 CFR 141.27. Some commenters __.,, expressed interest in having their method or instrumentation included in EPA-approved methods. EPA suggests that these commenters submit their data to EPA's Alternative Test Procedures (ATP) program for evaluation. A method or instrument can be considered for approval by EPA after it has received a favorable evaluation under the ATP program. A protocol for submitting ATP data is available from EPA (EPA, 1993c). V. Availability and Sources for Methods Information Commenters requested help in obtaining copies of analytical methods cited in drinking water rules. Sources of all approved methods are contained in the References section of this rule. These methods are available for review but not distribution at the EPA Drinking Water Docket (MC 4101), 401 M Street SW., Washington, DC 20460. For access to the docket material, please call (202) 260-3027 between 9 am and 3:30 pm, EST, Monday through Friday, excluding federal holidays. EPA only stocks or distributes copies of methods published by EPA. All other methods must be obtained from the publisher. Sources (with addresses) for all approved methods are cited at 40 CFR Parts 141 and 143, and in the References section of today's rule. Most EPA methods and the document, Technical Notes on Drinking Water Methods, may be purchased from the National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA 22161. The toll-free number is: (800) 553-6847, local: (703) 487-4650. Refer to the drinking water rules or the References section of this rule to obtain the NTIS order number and purchase information, or contact the Safe Drinking Water hotline. The hotline operates from 9 a.m. and 5:30 p.m. EST, Monday through Friday, excluding federal holidays. The toll-free number is (800) 426^1791. EPA Methods 504.1, 508.1 and 525.2 are not published in an NTIS manual. These methods may be obtained directly from EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268; the phone number is (513) 569-7586. Since Methods 150.1 (pH), 150.2 (pH) and 245.2 (mercury) are published in "Methods for Chemical Analysis of Water and Wastes" (EPA, 1983a), owners of this EPA manual do not need to reorder these methods. EPA believes most laboratories will need only the more recently published or approved methods that are listed in today's rule. These methods (or manuals) are as follows. Technical Notes on Drinking Water Methods, October 1994, NTIS PB95-104766; EPA Method 508.1, "Determination of Chlorinated Pesticides, Herbicides, and Organohalides in Water Using Liquid- Solid Extraction and Electron Capture Gas Chromatography", October 1994; EPA Method 100.2, "Determination of Asbestos Structures over lOum in Length in Drinking Water", June 1994, NTIS PB94- 201902; "Methods for the Determination of Metals in Environmental Samples—Supplement I", May 1994, NTIS PB94-184942; EPA Method 525.2, "Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction in Capillary Column Gas Chromatography/Mass Spectrometry", March 1994; EPA Method 504.1, "1,2-Dibromoethane (EDB), l,2-Dibromo-3-chloropropane (DBCP), and 1,2,3-Trichloropropane (123TCP) in Water by Microextraction and Gas Chromatography", 1993; "Methods for the Determination of Inorganic Substances in Environmental Samples", August 1993, NTIS PB91- 231498; "Methods for the Determination of Organic Compounds in Drinking Water—Supplement H," August 1992, NTIS PB92- 207703; Standard Methods for the Examination of Water and Wastewater 18th Edition Supplement, 1994; Colisure, Millipore Corp., 1994; and GLI Method 2, "Turbidity", Great Lakes Instruments, Inc., November 2, 1992. The American Society for Testing and Materials (ASTM) annually reprints all of the methods contained in the Annual Book of ASTM Methods, even methods that have not been editorially or technically revised. Thus, it is permissible to use any edition that contains the EPA-approved version of the compliance method. EPA notes that Orion Method 601 "Standard Method of Test for Nitrate in Drinking Water", which is equivalent to SM 4500-NO3-D (APHA, 1992), is identical to Orion Method WeWWG/5880. Method WeWWG/5880 is approved for nitrate analysis. ATI Orion republished the method in 1994 and renumbered it as 601, because the 1985 manual "Orion Guide to Water and Wastewater Analysis", which contained WeWWG/ 5880, is no longer available. In today's rule EPA cites WeWWG/5880 as 601 at 40CFR141.23(k)(l). VI. Regulation Assessment Requirements A. Executive Order 12866 Under Executive Order 12866 (58 FR 51735, October 4,1993), the Agency must determine whether the regulatory action is "significant" and therefore subject to OMB review and the requirements of the Executive Order. The Order defines "significant regulatory action" as one that is likely to result in a rule that may: (1) Have an annual effect on the economy of $100 million or more, or adversely affect in a material way the economy, a sector of the economy, productivity, competition, jobs, the environment, public health or safety, or State, local, or tribal governments or communities; (2) Create a serious inconsistency or otherwise interfere with an action taken or planned by another agency; (3) Materially alter the budgetary impact of entitlements, grants, user fees, or loan programs or the rights and obligations of recipients thereof; or (4) Raise novel legal or policy issues arising out of legal mandates, the President's priorities, or the principles set forth in the Executive Order. It has been determined that this rule is not a "significant regulatory action" under the terms of Executive Order 12866 and is therefore not subject to OMB review. B. Regulatory Flexibility Act The Regulatory Flexibility Act requires EPA to explicitly consider the ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62465 effect of these regulations on small entities. By policy, EPA has decided to consider regulatory alternatives if there is any economic impact on any number of small entities. This rule is consistent with the objectives of the Regulatory Flexibility Act because it will not have any economic impact on any small entities. This rule specifies analytical methods that laboratories must use for testing regulated drinking water contaminants. Monitoring requirements were promulgated in earlier notices. The rule would require laboratories to use the most recent version of a method and imposes no additional requirements. It is actually expected to reduce cost of analysis by eliminating current requirements to use different versions of the same method, and by allowing more contaminants to be analyzed simultaneously by using a single method. Therefore, the Agency believes that this notice would have no adverse effect on any number of small entities. C. Papenvork Reduction Act The rule contains no requests for information and consequently is not subject to the Paperwork Reduction Act, 44U.S.C. 350letseq. D. Science Advisory Board, National Drinking Water Advisory Council, and Secretary of Health and Human Services In accordance with section 1412(d) and (e) of the SDWA, the Agency consulted with the Science Advisory Board, the National Drinking Water Advisory Council, and the Secretary of Health and Human Services on this action and took their comments into account. VII. References APHA. 1992. Eighteenth edition of Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005. APHA. 1904. Method 6610 "Carbamate Pesticides" in Standard Methods for the Examination of Water and Wastewater, 18th Edition Supplement, 1994, American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C 20005. APHA. ASTM. 1994. Annual Book ofASTM Methods, 1994, Vol. 11.01 and 11.02, American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Bionclics. Report from Kenneth W. Edgell, et ol., "Determination of Inorganic Anions in Water by Ion Chromatography: Collaborative Study", Bionetics Corp., 16 Triangle Park Drive, Cincinnati, Ohio 45246,1991. Broadway, S., B. Pyle, G. McFeters. 1992. Final report of equivalency testing for Colisure. Montana State University, Bozeman, MT. Eaton. 1993a. Letter from Andrew D. Eaton, Standard Methods Committee, "Error in 4500-C1 E", American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005, June 4,1993. Eaton. 1993b. Letter from Andrew D. Eaton, Standard Methods Committee, "Inquiry on Chlorine Residual 4500-C1 (18th Edition)", American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005, October 26, 1993. EPA. 1974. Method 245.2, "Mercury, Automated Cold Vapor Technique", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268,1974. Also contained in reference EPA, 1983a. EPA. 1978. Method 150.1, "pH, Electrometric", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268,1978. Also contained in reference EPA, 1983a. EPA. 1982. Method 150.2, "pH Continuous Monitoring, Electro-metric", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268, December 1982. Also contained in reference EPA, 1983a. EPA. 1983a. "Methods for Chemical Analysis of Water and Wastes", EPA, March 1983, NTIS PB84-128677. EPA. 1983b. Method 100.1, "Analytical Method for the Determination of Asbestos Fibers in Water", September 1983, NTIS PB83-260471. EPA. 1990a. "Methods for the Determination of Organic Compounds in Drinking Water—Supplement I", July 1990, NTIS PB91-146027. EPA. 1990b. Manual for the Certification of Laboratories Analyzing Drinking Water, Third Edition, Office of Water Resource Center (RC-4100), 401 M. Street S.W., Washington, D.C. 20460, EPA 570-9-90- 008, April 1990. EPA. 1991. "Methods for the Determination of Organic Compounds in Drinking Water", December 1988, revised July 1991, NTIS PB91-231480. EPA. 1992a. Memorandum from Richard L. Carr, "Second Laboratory Validation of Method 555", December 10,1992, U.S. Environmental Protection Agency. EPA. 1992b. "Methods for the Determination of Organic Compounds in Drinking Water—Supplement II," August 1992, NTIS PB92-207703. EPA. 1993a. "Methods for the Determination of Inorganic Substances in Environmental Samples", August 1993, NTIS PB94-121811. EPA. 1993b. Memorandum from James R. Elder, "Detection Limits in Compliance Monitoring", December 16,1993, U.S. Environmental Protection Agency. EPA. 1993c. "Protocol for Nationwide Approval of New or Revised Methods", Rev. 1.4, EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268, July 14,1993. EPA. 1993d. Method 504.1, "1,2- Dibromoethane (EDB),'l,2-Dibromo-3- chloropropane (DBCP), and 1,2,3- Trichloropropane (123TCP) in Water by Microextraction and Gas Chromatography", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268,1993. EPA. 1994a. "Methods for the Determination of Metals in Environmental Samples— Supplement I", May 1994, NTIS PB94- 184942. EPA. 1994b. Method 525.2, Rev. 1.0, "Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction in Capillary Column Gas Chromatography/Mass Spectrometry", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268, March 1994. EPA. 1994c. Method 508.1, Rev. 1.0, "Determination of Chlorinated Pesticides, Herbicides, and Organohalides by Liquid-Solid Extraction and Electron Capture Gas Chromatography", EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268,1994. EPA. 1994d. Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994, NTIS PB95-104766. EPA. 1994e. "Response to Comments on December 15,1993, Analytical Methods Proposal, 58 FR 65622", Office of Water Docket (MC 4601), 401 M. St. S.W., Washington, D.C. 20460, October 1994. EPA. 1994f. Memorandum from Mary Ann Feige, et al., "Detection Limits in the Regulations", March 11,1994, U.S. Environmental Protection Agency. EPA. 1994g. Memorandum from Robert M. Sussman, "EMMC Activities", May 13, 1994, U.S. Environmental Protection Agency. EPA. 1994h. Method 100.2, "Determination of Asbestos Structures over lOjun in Length in Drinking Water", June 1994, NTIS PB94-201902. EPA. 1994i. Method 1613: "Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope-Dilution HRGC/HRMS", October 1994, NTIS PB95-104774. Great Lakes. GLI Method 2, "Turbidity", Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, WI53223, November 2, 1992. Lyter. Letter from P. Ted Lyter, Dept. of Environmental Resources, Commonwealth of Pennsylvania, P.O. Box 1467, Harrisburg, PA 17105-1467, January 12,1994. Millipore. "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography", Method B-1011, Millipore Corporation, Waters Chromatography Division, 34 Maple Street, Milford, MA 01757. Millipore. 1994. Colisure Presence/Absence Test for Detection and Identification of Coliform Bacteria and Escherichia coli in Drinking Water. February 28,1994. Millipore Corp., Technical Services Department, 80 Ashby Road, Bedford, MA 01730. ------- 62466 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations Orion. Technical Bulletin 601, "Standard Method of Test for Nitrate in Drinking Water", PN 221890-001, ATI Orion, 529 Main Street, Boston, MA 02129, July 1994. Technicon. 1972. Industrial Method No. 129- 71W, "Fluoride in Water and Wastewater", Technicon Industrial Systems, Tarrytown, NY 10591, December 1972. Technicon. 1989. Method No. 380-75WE, "Fluoride in Water and Wastewater", Technicon Industrial Systems, Tarrytown, NY 10591, February 1976. USGS. 1989. Methods 1-3720-85,1-3300-85, 1-1030-85,1-1601-85,1-2598-85,1- 1700-85 and 1-2700-85 in Techniques of Water Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A—1, 3rd ed., U.S. Geological Survey, Books and Open File Reports Section, Box 25425, Federal Center, Denver, CO 80225-0425, 1989. USGS. 1993. Method 1-2601-90 in Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory— Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, Open File Report 93-125, U.S. Geological Survey, Books and Open File Reports Section, Box 25425, Federal Center, Denver, CO 80225-0425,1993. List of Subjects 40 CFR Part 141 Environmental Protection, Chemicals, Incorporation by reference, Intergovernmental relations, Water supply. 40 CFR Part 143 Chemicals, Incorporation by reference, Intergovernmental relations, Water supply. Dated: November 25,1994. Carol M. Browner, Administrator. For the reasons set out in the preamble, parts 141 and 143 of title 40, Code of Federal Regulations, are amended as follows: PART 141—NATIONAL PRIMARY DRINKING WATER REGULATIONS 1. The authority citation for part 141 continues to read as follows: Authority: 42 U.S.C. 300f, 300g-l, 300g-2 300g-3, 300g-4, 300g-5, 300g-6, SOOj^i, 300J-9. 2. Section 141.21 is amended by revising paragraph (f)(3), removing and reserving (f)(4), revising the next to last sentence of (f)(5), revising the second sentence of (f](6)(i), revising the second sentence of (f)(6)(ii), Adding (F)(6)(iv), and adding a new sentence as the next to last sentence in (f)(8) to read as follows: § 141.21 Coliform sampling. ***** (fj*** (3) Public water systems must conduct total coliform analyses in accordance with one of the analytical methods in the following table. These methods are contained in the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20005. A description of the Colisure Test may be obtained from the Millipore Corporation, Technical Services Department, 80 Ashby Road, Bedford, MA 01730. The toll-free phone number is (800) 645-5476. Orga- nism Total Coli- forms1. Methodology Total Coliform Fermentation Technique 2-3-*. Total Coliform Membrane Fil- ter Technique. Presence-Ab- sence (P-A) Coliform Test4-5. ONPG-MUG Test6. Colisure Test7. Citation 9221 A, B. 9222A, B, C. 9221 D. 9223. 1The time from sample collection to initi- ation of analysis may not exceed 30 hours. 2 Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system conducts at least 25 parallel tests between this medium and lauryl tryptose broth using the water normally tested, and this com- parison demonstrates that the false-positive rate for total coliforms, using lactose broth, is less than 10 percent. 3 If inverted tubes are used to detect gas production, the media should cover these tubes at least one-half to two-thirds after the sample is added. 4 No requirement exists to run the com- pleted phase on 10 percent of all total coli- form-positive confirmed tubes. 5 Six-times formulation strength may be used if the medium is filter-sterilized rather than autoclaved. 6 The ONPG-MUG Test is also known as the Autoanalysis Colilert System. 7 The Colisure Test must be incubated for 28 hours before examining the results. If an examination of the results at 28 hours is not convenient, then results may be examined at any time between 28 hours and 48 hours. (4) [Reserved] (5)* * * The preparation of EC medium is described in the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, Method 9221E—p. 9-52, paragraph la. * * * (6)* * * (i) * * * EC medium is described in the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, Method 9221E—p. 9- 52, paragraph la. * * * (ii) * * * Nutrient Agar is described in the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, p. 9-47 to 9-48. (iii)* * * (iv) The Colisure Test. A description of the Colisure Test may be obtained from the Millipore Corporation, Technical Services Department, 80 Ashby Road, Bedford, MA 01730. ***** (8) * * * A description of the Colisure Test may be obtained from the Millipore Corp., Technical Services Department, 80 Ashby Road, Bedford, MA 01730. * * * ***** 3. Section 141.22(a) is amended by removing the next to last sentence and revising the last sentence to read as follows: § 141.22 Turbidity sampling and analytical .requirements. ***** (a) * * * Turbidity measurements shall be made as directed in § 141.74(a)(l). ***** 4. Section 141.23 is amended by removing paragraph (k)(2) and redesignating paragraph (k)(4) as (k)(2), by removing paragraph (k)(3) and redesignating paragraph (k)(5) as (k)(3), by removing and reserving paragraph (q), and revising paragraph (k)(l) to read as follows: § 141.23 Inorganic chemical sampling and analytical requirements. ***** (k) * * * (1) Analysis for the following contaminants shall be conducted in accordance with the methods in the following Table, or their equivalent as determined by EPA. Criteria for analyzing arsenic, barium, beryllium, cadmium, calcium, chromium, copper, lead, nickel, selenium, sodium, and thallium with digestion or directly without digestion, and other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994. This document also contains approved analytical test methods which remain available for compliance monitoring until July 1,1996. These methods will not be available for use after July 1,1996. This document is available from the National Technical Information Service, NTIS PB95- 104766, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll-free number is 800-553-6847. ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62467 Contaminant Antimony Arsento Asbestos Barium Beryllium Cadmium Chromium Cyanide Fluoride Mercury Nickel Nitrate Nitrite Selenium ThaMum Lead Cooper pH „ Conductivity Calcium Alkalinity Methodology ICP-Mass Spectrometry Hydride-Atomic Absorption Atomic Absorption; Platform Atomic Absorption; Furnace Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Hydride Atomic Absorption Transmission Electron Microscopy Transmission Electron Microscopy Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Direct Atomic Absorption; Furnace Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace Manual Distillation followed by Spectrophotometric, Amenable Spectrophotometric Manual Semi-automated Selective Electrode Ion Chromatography Manual Distill.; Color. SPADNS Manual Electrode Automated Electrode Automated Alizarin Manual, Cold Vapor Automated, Cold Vapor ICP-Mass Spectrometry Inductively Coupled Plasma ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Direct Atomic Absorption; Furnace Ion Chromatography Automated Cadmium Reduction Ion Selective Electrode Manual Cadmium Reduction Ion Chromatography Automated Cadmium Reduction Manual Cadmium Reduction Spectrophotometric Hydride-Atomic Absorption ICP-Mass Spectrometry Atomic Absorption; Platform Atomic Absorption; Furnace ICP-Mass Spectrometry Atomic Absorption; Platform Atomic absorption; furnace CP-Mass Spectrometry Atomic absorption; platform Atomic absorption; furnace Atomic absorption; direct aspiration CP CP-Mass Spectrometry Atomic absorption; platform Electrometric Conductance EDTA titrimetric Atomic absorption; direct aspiration nductively-coupled plasma Titrimetric EPA 22008 2 200 9 2 200 7 22008 2 200 9 9-]00 1 10 100 2 22007 2 200 8 22007 22008 22009 22007 22008 22009 2200 7 2 200 8 2 200 9 6 335 4 6 3000 2 245 1 12452 2 200 8 22007 22008 22009 6 3000 6 353 2 6 300 0 6 353 2 22008 22009 22008 22009 2 200 8 22009 2200 7 22008 22009 1 -(50 1 1 1502 22007 ASTM3 D-3697-92 D-2972-93C D 2972 93B D— 3645— 93B D2036-91 B D2036— 91 A 04327 91 D1179 93B D3223-91 D4327 91 D3867 90A D3867-90B D4327 91 D3867 90A D3867 90B D3859 93A D3859 93B D3559 90D D1688— 90C D1688-90A nioq'WM D1 125-91 A D51 1-93A D511-93B D1067-92B SM" 3113B OHODR 3113B ^114R •51OCIR 311 1D 3113B Q-ionR ^H^R 3113B O-tOflR 3113B 4500— CN C 4500CN G 4^nO— PM F 4500CN F 411 OR 4500F B D 4500F— C 4500F E 3112B 3120B 311 1B 3113B 411 OB 4500— NOs F 4^00— wn^ n 4500— NOs E 411 OR 4^nri— wo F 4Rnn— wn, F 4500— NO2 B •3114R 3113B 3113B 3113B 3111B O-JOflR A cnn_u + R OKIflR 3500-Ca D 3111B ii?nR 2320B. Other 5 1 QQr»n_ft£ 1 1 ^ftfl_7f>WP 11 1OQ 71 \A/ s Ft— inn 7fifl1 8R_1 n-i H ------- 62468 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations Contaminant phate12. Silica Tsmperature Methodology Colorimetric automated ascorbic acid Colorimetric ascorbic acid single reagent automated discrete - - Ion Chromatography Colorimetric molybdate blue* Colorimetric Molybdosilicate Heteropoly blu6 Automated method for molybdate-reactive silica Inductively-coupled plasma Thermometric Inductively-coupled plasma Atomic Absorotion: direct asoiration EPA 6 365.1 6 300.0 2200.7 2 200.7 ASTM3 D515-88A D4327-91 D859-88 SM4 4500-P-F. 4500-P-E. 4110. 4500-Si-D. 4500-Si-E. 4500-Si-F. 3120B. 2550B. 3111B. Other 5 1-1 030-85 5 1-1 601 -85 5 1-2601-90 si-2598-85 5l-1700-85 sl-2700-85 FOOTNOTES: 1 Methods 150 1 150.2 and 245.2 are available from US EPA, EMSL, Cincinnati, OH 45268. The identical methods were formerly in "Methods for Chemical Analysis of Water and Wastes", EPA-600/4-79-020, March 1983, which is available at NTIS, PB84-128677. 2 "Methods for the Determination of Metals in Environmental Samples—Supplement I", EPA-600/R-94-111, May 1994. Available at NTIS, PB 94-184942. 3 The procedures shall be done in accordance with the Annual Book of ASTM Standards, 1994, Vols. 11.01 and 11.02, American Society for Testing and Materials. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC. 4 The procedures shall be done in accordance with the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 DSC 552(a) and 1 CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC. 5 Available from Books and Open-File Reports Section, U.S. Geological Survey, Federal Center, Box 25425, Denver, CO 80225-^0425. 6 "Methods for the Determination of Inorganic Substances in Environmental Samples", EPA-600/R-93-100, August 1993. Available at NTIS, PB94-121811. 7 The procedure shall be done in accordance with the Technical Bulletin 601 "Standard Method of Test for Nitrate in Drinking Water", July 1994 PN 221890-001, Analytical Technology, Inc. This incorporation by reference was approved by the Director of the Federal Register in ac- cordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal Register, 800 North Cap- itol Street, NW., Suite 700, Washington, DC. 8 Method B-1011, "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography", Millipore Cor- poration, Waters Chromatography Division, 34 Maple Street, Milford, MA 01757. 9 Method 100.1, "Analytical Method For Determination of Asbestos Fibers in Water", EPA-600/4-83-043, EPA, September 1983. Available at NTIS, PB83-260471. 10Method 100.2, "Determination Of Asbestos Structure Over 10-nm In Length In Drinking Water", EPA-600/R-94-134, June 1994. Available at NTIS, PB94-201902. 11 The procedures shall be done in accordance with the Industrial Method No. 129-71W, "Fluoride in Water and Wastewater", December 1972 and Method No. 380-75WE, "Fluoride in Water and Wastewater", February 1976, Technicon Industrial Systems. This incorporation by ref- erence was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from the Technicon Industrial Systems, Tarrytown, NY 10591. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of Federal Register, 800 Capitol Street, NW., Suite 700, Washington, DC. 12Unfiltered, no digestion or hydrolysis. (q) [Reserved] 5. Section 141.24 is amended by removing and reserving paragraphs (f)(16), and (h)(12), adding paragraphs (e), reviewing paragraph (h)(13), introductory text, and paragraph (h)(13)(i) to read as follows: § 141.24 Organic chemicals other than total trihalomethanes, sampling and analytical requirements. ***** (e) Analyses for the contaminants in this section shall he conducted using the following EPA methods or their equivalent as approved by EPA. Methods 502.2, 505, 507, 508, 508A, 515.1 and 531.1 are in Methods for the Determination of Organic Compounds in Drinking Water, EPA-600/4-88-039, December 1988, Revised, July 1991. Methods 506, 547, 550, 550.1 and 551 are in Methods for the Determination of Organic Compounds in Drinking Water—Supplement I, EPA-600-4-90- 020, July 1990. Methods 515.2, 524.2, 548.1, 549.1, 552.1 and 555 are in Methods for the Determination of Organic Compounds in Drinking Water—Supplement II, EPA-600/R-92- 129, August 1992. Method 1613 is titled "Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope-Dilution HRGC/HRMS", EPA-821-B-94-005, October 1994. These documents are available from the National Technical Information Service, NTIS PB91- 231480, PB91-146027, PB92-207703 and PB95-104774, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll- free number is 800-553-6847. Method 6651 shall be followed in accordance with the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20005. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62469 Register, 800 North Capitol Street, NW., Suite 700, Washington, DC. Method 6610 shall be followed in accordance with the Supplement to the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1994, American Public Health Association. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20005. Copies may be inspected at EPA's Drinking Water Docket, 401M Street, SW., Washington, DC 20460; or at the Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, - Washington, DC. Other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA- GOO/R-94-173, October 1994, NTIS PB95-104766. This document also contains approved analytical methods which remain available for compliance monitoring until July 1,1996. These methods will not be available for use after July 1,1996. EPA Methods 504.1, 508.1 and 525.2 are available from US EPA EMSL, Cincinnati, OH 45268. The phone number is 513-569-7586. Contaminant Benzene Carbon tetrachloride Chtorobenzene 1 ,2-Dichlojobenzene 1,4-DtohlOfobenzene 1,2-DtcWoroothane .... cis-Dichlofoethylene .. trans- DicWoroethylene. Dfchtoromethane 1,2-Dichloropropane . Ethytoonzena Styrena Tetrachtoroethylene .. 1,1,1 -Trichtoroethane Trichtoroethylene Toluene 1.2,4- Trfchtorobenzene. 1,1-DfcWofoethylene . 1 ,1 ^-Trichtoroethane VlnyJ chtorida Xyfeoes (total) 2,3,7.8-TCOO (dioxin) 2,4-D 2.4.5-TP (Silvex) Atachtor AtrazJna Beitto(a)pyrene Carbofuran Chtordane Dalapon , Dt(2-elhylhexyl) adi- pate. Method 502.2, 524.2. 502.2,524.2,551. 502.2. 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2,524.2,551. 502.2, 524.2, 551. 502.2,524.2,551. 5022 5242 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 502.2, 524.2. 1613. 5152 555 515 1 515.2,555,515.1. 505' ,507, 525.2, 508.1. 505 ' 507 5252 508.1. 525.2,550,550.1. 531.1,6610. 505, 508, 525.2, 508.1. 552 1 515 1 506, 525.2. Contaminant Di(2-ethylhexyl) phthalate. Dibromochloro- propane (DBCP). Dinoseb , Diquat , Endothall Endrin , Ethylene dibromide (EDB). Glyphosate Heptachlor Heptachlor Epoxide .. Hexachlorobenzene .. Hexachlorocyclopent- adiene. Lindane Methoxychlor. Oxamyl PCBs2 (as decachlc- robiphenyl). (asAroclors) Pentachlorophenol .... Picloram . Simazine Toxaphene Total Trihalomethanes. Method 506, 525.2. 504.1,551. 515.2,555,515.1. 549.1. 548.1. 505, 508, 525.2, 508.1. 504.1,551. 547,6651. 505, 508, 525.2, 508.1. 505, 508, 525.2, 508.1. 505, 508, 525.2, 508.1. 505, 525.2, 508, 508.1. 505, 508, 525.2, 508.1. 505, 508, 525.2, 508.1. 531.1,6610. 508A. 505, 508. 515.2, 525.2, 555, 515.1. 515.2,555,515.1. 5051, 507, 525.2, 508.1. 505, 508, 525.2. 502.2,524.2,551. 1A nitrogen-phosphorous detector should be substituted for the electron capture detector in Method 505 (or another approved method should be used) to determine alachlor, atrazine and simazine, if lower detection limits are required. 2 PCBs are qualitatively identified as Aroclors and measured for compliance pur- poses as decachlorobiphenyl. (h)* * * (12) (Reserved) (13) Analysis for PCBs shall be conducted as follows using the methods in paragraph (e) of this section: (i) Each system which monitors for PCBs shall analyze each sample using either Method 505 or Method 508. ***** 6. Section 141.30 is amended by revising paragraph (e) and by removing removing Appendix A, Appendix B, and Appendix C to read as follows: §141.30 Total trihalomethane sampling, analytical and other requirements. ***** (e) Sampling and analyses made pursuant to this section shall be conducted by the total trihalomethane methods as directed in § 141.24(e), and in Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994, which is available at NTIS, PB95- 104766. ***** 7. Section 141.40 is amended by revising paragraphs (g), (n)(ll), and (n)(12) to read as follows: § 141.40 Special monitoring for inorganic and organic chemicals. ***** (g) Analysis for the unregulated contaminants listed under paragraphs (e) and (j) of this section shall be conducted using EPA Methods 502.2 or 524.2, or their equivalent as determined by EPA, except analysis for bromodichloromethane, bromoform, chlorodibromomethane and chloroform under paragraph (e) of this section also may be conducted by EPA Method 551, and analysis for 1,2,3-trichloropropane also may be conducted by EPA Method 504.1. A source for the EPA methods is referenced at § 141.24(e). ***** (n) * * * (11) Systems shall monitor for the unregulated organic contaminants listed below, using the method(s) identified below and using the analytical test procedures contained in Technical Notes on Drinking Water Methods, EPA- 600/R-94-173, October 1994, which is available at NTIS, PB95-104766. Method 6610 shall be followed in accordance with the Standard Methods for the Examination of Water and Wastewater 18th Edition Supplement, 1994, American Public Health Association. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies may be obtained from the American Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC. A source for EPA methods 505, 507, 508, 508.1, 515.2, 525.2 and 531.1 is referenced at § 141.24(e). Contaminants aldicarb aldicarb sulfone ... aldicarb sulfoxide aldrin butachlor carbaryl .. dicamba . dieldrin ... 3-hydroxycarbofuran methomyl Method 531.1, 6610. 531.1,6610. 531.1,6610. 505, 508, 525.2, 508.1. 507, 525.2. 531.1,6610. 515.2,555,515.1. 505, 508, 525.2, 508.1. 531.1,6610. 531.1,6610. ------- 62470 Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations Contaminants metolachlor metribuzin orooachlor Method 507, 525.2, 508.1. 507,525.2,508.1. 508.525.2,508.1. (12) Systems shall monitor for sulfate, an unregulated inorganic contaminant, by using the methods listed at §143.4[b). ***** 8. Section 141.41 is amended by revising paragraph (d) to read as follows: § 141.41 Special monitoring for sodium. ***** (d) Analyses for sodium shall be conducted as directed in § 141.23(k)(l). 9. Section 141.42 is amended by removing and reserving paragraphs (a) through (c). 10. Section 141.74 is amended by revising paragraphs (a)(l) and (a)(2), and removing paragraphs (a)(3) through (a)(7) to read as follows: § 141.74 Analytical and monitoring requirements. (a) * * * (1) Public water systems must conduct analysis of pH in accordance with one of the methods listed at § 141.23(k)(l). Public water systems must conduct analyses of total coliforms, fecal coliforms, heterotrophic bacteria, turbidity, and temperature in accordance with one of the following analytical methods and by using analytical test procedures contained in Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994, which is available at NTIS PB95- 104766. Orga- nism Total Coli- forms. Fecal Coli- forms. Heterot- rophic bac- teria2. Turbid- ity. Methodology Total Coliform Fermentation Technique/ 3,4,5/. Total Coliform Membrane Filter Tech- nique. ONPG-MUG Test6. Fecal Coliform MPN Proce- dure7. Fecal Coliforms Membrane Filter Proce- dure. Pour Plate Method. Nephelometric Method. Citation 1 9221 A, 9222A, 9223 9221 E 9222D 921 5B 21 SOB B, C B, C Orga- nism Tem- pera- ture. Methodology Nephelometric Method. Great Lakes In- struments. Citation 1 180.18 Method 29 2550 measurement at least every five days, or with a protocol approved by the State. FOOTNOTES: 1 Except where noted, all methods refer to the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992, American Public Health Association, 1015 Fif- teenth Street NW, Washington, D.C. 20005. 2 The time from sample collection to initi- ation of analysis may not exceed 8 hours. 3 Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system conducts at least 25 parallel tests between this medium and lauryl tryptose broth using the water normally tested, and this com- parison demonstrates that the false-positive rate for total coliforms, using lactose broth, is less than 10 percent. 4 Media should cover inverted tubes at least one-half to two-thirds after the sample is added. 5 No requirement exists to run the com- pleted phase on 10 percent of all total coli- form-positive confirmed tubes. 6 The ONPG-MUG Test is also known as the Autoanalysis Colilert System. 7A-1 Broth may be held up to three months in a tightly closed screwcap tube at 4°C. 8 "Methods for the Determination of Inor- ganic Substances in Environmental Samples", EPA-600/R-93-100, August 1993. Available atNTIS, PB94-121811. 9GLI Method 2, "Turbidity", November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, Wisconsin 53223. (2) Public water systems must measure residual disinfectant concentrations with one of the analytical methods in the following table. The methods are contained in the 18th edition of Standard Methods for the Examination of Water and Wastewater, 1992. Other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA- 600/R-94-173, October 1994, which is available at NTIS PB95-104766. If approved by the State, residual disinfectant concentrations for free chlorine and combined chlorine also may be measured by using DPD colorimetric test kits. Free and total chlorine residuals may be measured continuously by adapting a specified chlorine residual method for use with a continuous monitoring instrument provided the chemistry, accuracy, and precision remain same. Instruments used for continuous monitoring must be calibrated with a grab sample Resid- ual Free Chlo- rine. Total Chlo- rine. Chlorine Diox- ide. Ozone . Methodology Amperometric Titration. DPD Ferrous Titrimetric. DPD Colori- metric. Syringaldazine (FACTS). Amperometric Titration. Amperometric Titration (low level meas- urement). DPD Ferrous Titrimetric. DPD Colori- metric. lodometric Elec- trode. Amperometric Titration. DPD Method .... Amperometric Titration. Indigo Method .. Methods 4500-CI D 4500-CI F 4500-CI G 4500-CI H 4500-CI D 4500-CI E 4500-CI F 4500-CI G 4500-CI I 4500-CIO2 C 4500-CIO2 D 4500-CIO2 E 4500-O3 B 11. Section 141.89 is amended by revising paragraph (a) introductory text; removing the table in paragraph (a); and by removing and reserving paragraph (b) to read as follows: § 141.89 Analytical methods. (a) Analyses for lead, copper, pH, conductivity, calcium, alkalinity, orthophosphate, silica, and temperature shall be conducted with the methods in §141.23(k)(l). PART 143—NATIONAL SECONDARY DRINKING WATER REGULATIONS 1. The authority citation for part 143 continues to read as follows: Authority: 42 U.S.C. 300f, 300g-l, 300g-2 300g-3, 300g-4, 300g-5, 300g-6, 300J-4, 300J-9. 2. Section 143.4 is amended by revising paragraph (b) to read as follows: §143.4 Monitoring. ***** (b) Measurement of pH, copper and fluoride to determine compliance under § 143.3 may be conducted with one of the methods in § 141.23(k)(l). Analyses of aluminum, chloride, foaming agents, iron, manganese, odor, silver, sulfate, total dissolved solids (TDS) and zinc to determine compliance under § 143.3 may be conducted with the methods in ------- Federal Register / Vol. 59, No. 232 / Monday, December 5, 1994 / Rules and Regulations 62471 the following Table. Criteria for analyzing aluminum, copper, iron, manganese, silver and zinc samples with digestion or directly without digestion, and other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA- 600/R-94-173, October 1994, which is available at NTIS PB95-104766. Contaminant Aluminum CWoride Color Foaming Agents Iron Manganese Odor .... Silver Sutfate TDS Zinc .„ EPA aonn 7 2 200.8 2 200.9 1 3000 2 200 7 2 200.9 2200 7 2 200.8 2 200.9 2 200 7 2 200.8 2 200.9 1 -jnn n 1 375.2 2onn 7 2 200.8 ASTM3 rMQ07_Q1 PMooy Q1 SM4 311 3B 3111D 4500-CI— D KRAftC* 3111B 3113B 3111B 3113B 3111B 3113B 4500-SO4-F 4500-SO4-C,D .... 3111B. Other I— 6f 20-85° and > Determination of Inorganic Substances in Environmental Samples", EPA-600/R-93-100, August 1993. Available at NTIS, J Determination of Metals in Environmental Samples—Supplement I", EPA-600/R-94-111, May 1994. Available at NTIS, shall be done in accordance with the Annual Book of ASTM Standards, 1994, Vols. 11.01 and 11.02 American Society for incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U S C 552(a) i""i mX. n°- P1" i.i ?m J?18 ,American Society for Testing and Materials, 1916 Race Street, Philadelphia PA 19103 -,JMad/E cA? W78 W^Doc^tl 401 M Street- SW- Washington, DC 20460; or at the Office of the Federal Register' it, NW., Suite 700, Washington, DC. '" ""' don.? in accordance with the 18th edition of Standard Methods for the Examination of Water and Wastewater 1992 rrr^'TncS^I-J?"^ • '"corporation by reference was approved by the Director of the Federal Register in accordance'with 5 r—ivi-SSKfe81)? 1:CFR Pa£ 5-1' c°P'es mav be obtained from the American Public Health Association, 1015 Fifteenth Street NW Washina- ipn, DC 20005. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street, SW Washinaton DC 20460- or at thp riffirp nf th» Federal Register. 800 North Capitol Street, NW.. Suite 700, Washington, DC. «>"«iaiuN, uo ^u^ou, or at ine unice or me °Availabte from Books and Open-File Reports Section, U.S. Geological Survey, Federal Center, Box 25425, Denver, CO 80225-0425. [FR Doc. 94-29692 Filed 12-2-94; 8:45 ami QllUNO CODE 6J60-50-P ------- ------- ------- |