United States
        Environmental Protection
                                        Labcert  Bulletin
  In This Issue...

       This issue of the Labcert Bulletin addresses
       issues which have been brought to our
       attention by laboratories, and Regional and
  State Certification Officers. You will find articles
  on the National Environmental Methods Index
  (NEMI), recent legislation, Stagel Disinfectants
  and Disinfection  Byproducts  Rule,  chlorite,
  cyanide, and other drinking water issues.

  If there are certification topics you would like to
  see discussed, please call,,write, fax or e-mail the
  editors. There is a form on page 6  for you to use
  to add your name to our mailing list or to update
  your information.
           EdGlick 513-569-7939
         Patricia Hurr 513-569-7678
       Caroline Madding 513-569-7402

       USEPA  MS 140
       Technical Support Center          ;
       26 W. Martin Luther King Dr.
       Cincinnati, OH 45268             .

       FAXNumben 513-569-7191
            Contact for

    USEPA Laboratory ID


 Every laboratory  wishing to be certified to
 analyze compliance monitoring drinking water
 samples  must have a unique laboratory ID
 Number. Laboratories must include this number
 when reporting proficiency testing (PT) results.

 Charles Feldmann, Office of Ground Water and
 Drinking Water, Technical Support Center,  is
 the primary contact for  assignment of new
 laboratory IDs. He may be reached at 513-569-
 7671 or FAX: 513-569-7191.

 If the  laboratory has ever participated in a
 USEPA-run PT study, the laboratory will already
 have a unique ID number.  Please review any
 previous "study results" report to locate the ID
 number.  If a laboratory cannot locate this
 information, the laboratory should contact
 Mr. Feldmann for assistance.


Drinking water regulations require laboratories to
demonstrate proficiency by successful analysis of
aPT sample each year for contaminants using the
same analytical method  that is used to report
compliance monitoring results.
      An electronic version of this publication and much more can be found on the Office of Ground Water
      and Drinking Water web page at http://www.epa.gov/OGWDW/standards.html.  This site has
      information about drinking water regulations and laboratory certification.  The "Manual for the
Certification of Laboratories Analyzing Drinking Water," and past issues of the Labcert Bulletin can also
be found at this address.

       National Environmental Methods Index (NEMI)
                                  Herb Brass
       Office of Ground Water and Drinking Water, Technical Support Center

I EMI is an Oracle database of environmental method summaries for use in regulatory and non-
regulatory water quality analyses. The database may be searched from anywhere in the world, free
of charge, using the Internet at www.nemi.gov.
                                          provided to the appropriate website, so that the
                                          method can be purchased or otherwise obtained.
With NEMI, you  can compare methods at a
glance and find the method that best meets your
needs. NEMI also supports sharing of monitoring
data among different agencies and projects, which
may use different methods at different times. The
Advisory  Committee  on Water  Information
(ACWI), the senior advisory committee in the
federal government  that  deals  with  water
information,  has  "endorsed   the  continued
development and timely delivery of NEMI as a
vital tool to enhance the generation of comparable
data of known quality,  across all entities that
conduct water  quality monitoring."   A letter
announcing  the public  release of NEMI was
recently co-signed  by Diane Regas, then EPA
Deputy Assistant Administrator for Water, and
Bob Hirsch, US Geological Survey Associate
Director for Water.  The letter can be accessed at:

NEMI has been developed under the guidance of
the Methods and  Data Comparability Board
(MDCB).  EPA and USGS co-chair the MDCB,
which includes representatives from the federal,
state/tribal, and private sectors.  The MDCB and
its parent organization, the National Water Quality
Monitoring Council are committees under ACWI.
Currently, NEMI contains information on more
than  600   chemical,   microbiological,  and
radiological  water  methods that are used for
compliance  and other purposes.   Regulatory
information,  that includes citations in the Federal
Register, are available for drinking water and
wastewater methods.   For  each method, NEMI
provides  a  summary of  the  procedure and
performance data. Quick method comparisons are
arranged in tables, with supporting details in text.
Links are provided  to full methods available on
line or, when the methods are proprietary, a link is
                                          The NEMI database was constructed using a state-
                                          of-the-art  Oracle platform  so that it could
                                          accommodate a broad range of method types that
                                          require different data fields and search parameters.
                                          The following classes of methods are currently
                                          being  or  will soon  be  added   additional
                                          chemical,   microbiological,  and  radiological
                                          methods; biological and field methods; methods
                                          related to  water security; and methods used in
                                          matrices other than water.  A  strategic  plan is
                                          being developed to accommodate the addition of
                                          these  methods   consistent  with  expressed
                                          priorities, anticipated resources, and time.
                                               Rule to Update Drinking Water and
                                                     Wastewater Methods

                                          On October 23, 2002, a final "methods update"
                                          rule was published in the Federal Register (Vol.
                                          67, No. 205, pp 65220-65253). This rule approves
                                          updated versions of chemical, microbiological,
                                          and radiological analytical methods developed by
                                          ASTM, Standard Methods,  the US Geological
                                          Survey, and the Department  of Energy. No EPA
                                          methods were approved.  The methods apply to
                                          the Safe Drinking Water Act and the Clean Water
                                          Act compliance monitoring programs.

                                          A Fact Sheet and the Final Rule are available at
                                          http://www.epa.gov/ogwdw/regs.html  and

  Additional Methods Approval

  On October 29,2002, a final rule was published in
  the  Federal Register (Vol.  67,  No. 209, pgs
  65888-65902) that approves EPA Method 515.4
  to   support   previously  required  NPDWR
  compliance monitoring  for  2,4-D,  2,4,5-TP,
  dinoseb,  pentachlorophenol,  picloram   and
  dalapon.  In  addition, EPA  Method 531.2 is
  approved for carbofuran and oxamyl. Additional
  methods approved in this Federal Register include
  a method for the determination of atrazine,  two
  methods for the determination of cyanide,  two
  methods for the determination of total coliforms
  and E. coli, a  method for the determination of
  heterotrophic bacteria, and a  method for  the
  determination of turbidity. More information can
  be found at http://www.epa.gov/ogwdw/regs.html.

         Chlorite  Monitoring
      Requirements under the
             Stage 1 DBPR

      The Stage   1   Disinfectants/Disinfection
      Byproducts  Rule requires two types  of
      chlorite monitoring for systems that! use
 chlorine dioxide in their treatment process: daily
 monitoring at the entry point to the distribution
 system and monthly monitoring at three points in
 the distribution system.

 Daily chlorite monitoring:
 The water entering the distribution system must be
 analyzed daily  for chlorite using  one of  three
 approved analytical methods.  Standard Method
 4500-C1O2 E is an amperometric method; for
 determining  both chlorite and chlorine dioxide.
 EPA Method 300.0 and  EPA Method 300.1 are
 both  ion chromatographic  methods.    It  is
 anticipated that most of the daily analyses will
 be performed by treatment plant personnel using
 SM 4500-C1O2 E. The rule states that the analyses
 must be performed by a party approved by the
 State. This is the same type of approval that is
required to measure disinfectant residuals such as
chlorine dioxide or chlorine.
  Distribution system chlorite monitoring:
  In order to demonstrate compliance with  the
  chlorite maximum contaminant level  (MCL),
  water systems using chlorine dioxide must collect
  a set of three samples in the distribution system on
  a monthly basis. One sample is collected near the
  first customer, one at a location representative of
  average residence time, and the third at a location
  reflecting  maximum residence time  in   the
  distribution system.    The  samples  must  be
  analyzed using either EPA Method 300.0  or EPA
  Method 300.1 and the laboratory must be certified
  to perform the analysis.

  Compliance with the chlorite MCL of 1.0 mg/L is
  based on the arithmetic average of each 3-sample
  set from the distribution system.  If any daily
  sample  at the entry  point indicates a chlorite
  concentration greater  than the  MCL, then  the
  water system must collect a set of distribution
  system samples on the following day. If none of
  the daily samples have chlorite concentrations
  greater than the MCL, then the distribution  system
  sampling is only required once each month.  A
 chlorite  compliance determination is made  for
 each 3-sample set.
          Stage 1 DBF Rule

 The Stage 1 Disinfection By-Product (DBF) Rule
 which was promulgated  in  December  1998
 became effective for large surface water systems
 in January 2002. These utilities were required to
 begin monitoring for additional DBFs at that time.
 All large surface water systems must monitor for
 five haloacetic acids with the summation of their
 concentrations to be reported as HAAS (similar to
 the  concept  used for total trihalomethanes).
 Utilities that use chlorine dioxide must monitor
 for chlorite and systems using ozone must monitor
 for bromate. This means that laboratories need
 to be certified to analyze for HAAS, chlorite
 and bromate.

The DBF Rule also requires that water systems
monitor for TOC.  The regulation requires the

 TOC analyses be performed by a party approved
 by the State.   Please contact your states to
 ascertain they are approving laboratories for TOC.
  Methods 300.0 and 300.1

          Differences and

               Dan Hautman
  Office of Ground Water and Drinking Water,
          Technical Support Center

 In response to  compliance inquiries about the
 appropriate use of EPA Method 300.0 and EPA
 Method 300.1,  this article has been prepared to
 clarify the differences and similarities, as well as
 to relate the significance of these differences to
 both laboratory certification and the classification
 of these methods as approved for  compliance
 monitoring.  Both of these methods employ ion
 chromatography   (1C)  with   suppressed
 conductivity detection, hence, when considering
 the determinative step, they are identical.  The
 only  real  differences  between  these  two
 procedures are the specified analytical columns, 
 with their  respective eluents, and for Part B, the
 "on column" injection volume.

 Method 300.1 was written primarily to identify
 specific parameters (column, eluent and injection
 volume) which could be employed to allow the
 quantitation of lower concentrations of bromate in
 drinking water.  While doing this primarily for
 bromate, it was decided that it would be best to
 include  all  the 300.0  analytes  into  300.1.
 Additionally, we could simplify the method by
 specifying a single analytical column for  both
 Parts A and B, and include some additional QC
 such as a surrogate analyte.

 EPA Method 300.0 is the general purpose 1C
method approved for compliance monitoring of
 fluoride, nitrate, nitrite, chloride, sulfate, and o-
phosphate  as well as chlorite at water systems
 employing chlorine dioxide disinfection.
By closely examining Method 300.0, Section 2.4,
regarding method  modifications and Sections and  regarding optional analytical
columns, it becomes clear that Method 300.1
completely overlaps  into Method 300.0.   A
laboratory can adopt the parameters, columns and
specifications identified in 300.1, apply and pass
all the required QC that is shown in Section 9 of
300.0, and legitimately claim for certification or
approved method classification that they are using
Method 300.0, modified as permitted in the above
referenced sections. The reverse can not be said
about applying the operating conditions found in
Method 300.0 to Method 300.1. Comparable low
level measurements of bromate are not possible
using the  Method 300.0  standard operating

If you have additional questions do not hesitate to
contact Dan Hautman at 513-569-7274 or E-mail
at Hautman.Dan@epa.gov.

         Another Website

They make it easier all the time. At
http://www.epa.gov/fedreg/subscribe.htm you can
subscribe  to have  the  daily  Federal Register
delivered to your email box. You may suscribe to
any or all  of the 12 categories, one of which is
"Water." And if your mailbox gets too full, you
can unsubscribe at any time.

                 Cyanide Clarification
e were recently asked for clarification about the cyanide methods, specifically, what methods are
approved for analysis of cyanide in drinking water and whether or not distillation is required.
 The 1994 Technical Notes (EPA600/R-94/173, October 1994) emphasizes that spectrophotometric
 measurements for cyanide in water always require a manual distillation of the sample to prepare the sample
 for measurement.  EPA felt the Technical Note was needed because some laboratories seemed to be
 unaware of the requirement to distill samples.  Although free cyanide is regulated, the  approved
 spectrophotometric methods are for total and amenable cyanide; therefore, distillation is required. The
 "total" cyanide methods are used to screen samples for cyanide. If the "total" cyanide level is greater than
 the MCL (0.2 mg/L), then analysis for "free" (amenable) cyanide must be performed to see if the MCL has
 been exceeded.  The "total" cyanide analysis is still recommended because it is cheaper than the amenable

 All approved methods for cyanide are listed at 40 CFR 141.23(k)(l). The mandatory manual distillation
 procedure is described in Standard Method SM-4500-CN-C and ASTM D2036-91.  The approved
 amenable, manual and automated spectrophotometric methods are shown in the table below.
Technology (use only after distillation)
Manual Spectrophotometric, Amenable
Manual Spectrophotometric, Total
Semi-automated Spectrophotometric, Total





Free cyanide can also be determined by one method approved for drinking water compliance monitoring
analysis that does not require distillation, the specific ion electrode method, SM-4500-CN-F.  When using
this method, it is mandatory to maintain a constant ionic strength background for the electrode measurement,
that is, samples and standards must contain the same concentration of sodium hydroxide. More information
concerning methods can be found in FRN Vol 57, No 138, Friday, July 1992, p 31800.
    IT! tiinmntTfltt TVfYYl/tft^c frfrr\ ^-/Joxr t/^r*-"'>5/v*Te*^r* <4Qrt-;^M-^rt^4 +*,.X^4^.'?^. ^	a r*!> j.^f**.,_ *	TT--*IV ~*"- ^<>r^-

 Sparging Chlorite  Samples
       The ion chromatographic methods for chlorite recommend that the sample be sparged in order to
       remove any residual chlorine dioxide that may be present in the sample.  This is because chlorite is
       formed from chlorine dioxide. Thus, chlorine dioxide will cause a positive bias in the analytical result
 if it isn't removed at the time of sample collection.
 Most water systems do not use chlorine dioxide as
 a residual disinfectant, so usually the water
 leaving the treatment plant does not contain a
 significant chlorine dioxide residual. If this is the
 case, the water system does not need to worry
 about the sparging step. In fact, sparging chlorite
 compliance samples is only recommended when
 chlorine dioxide is present at  a high enough
 concentration that  if it  completely converted to
 chlorite, it would result in a chlorite concentration
 near the maximum contaminant  level (MCL) of
 1.0  mg/L.     Since  the  chlorine  dioxide
 concentration is monitored daily at the entry point
 to the distribution system, water systems should
 know whether there is a potential for significant
 chlorine dioxide residuals at the chlorite sampling

 If it is determined that chlorine dioxide poses a
 potential  problem  in  chlorite   compliance
 monitoring samples,  then the  sampler  should
 sparge the samples at the time of collection. Since
 chlorine dioxide is volatile, it  is  not hard to
 remove  it.  The sample  should be collected in a
 clean, wide-mouth container (such as a beaker or
 Erlenmeyer flask).   The  sparging gas can be
 obtained by using a lecture bottle of nitrogen or
helium fitted with a regulator and connected to a
disposable glass Pasteur pipette with P VC tubing.
The gas flow should be adjusted to produce  a
steady flow of bubbles.  After .10-15 minutes of
sparging, all traces of chlorine dioxide should be
removed from the sample. It can then be poured
from the container into the sample bottle that
contains the ethylenediamine (EDA) preservative.
 In   order  to  eliminate  potential  cross-
 contamination problems, it is recommended that
 a clean container and a new disposable pipette be
 used at each sampling point.

 A blank should be prepared and  analyzed for
 chlorite prior to the first field use of the sparging
 apparatus.  Reagent water should be sparged for
 15 minutes and then poured into a sample bottle
 that contains the EDA preservative. This blank
 sample should be analyzed for chlorite in order to
 ensure that contaminants are not introduced into
 the sample from the sparging gas or the  PVC
 tubing which would interfere with the chlorite
 analysis.  Periodic preparation  and analysis of
 sparged blanks  is recommended to demonstrate
 that the sparging procedure does not introduce

            Fax It To Us
 Please add/change (circle one) my name to the
 Labcert Bulletin mailing list.
   Fax#:  "
Fax to:
Susan Hagedorn
26 W. M.L. King Drive
Cincinnati,. OH 45268

        MICRO PT Q & A

 The following are  some  questions we  have
 received concerning evaluation of Micro PTs.
 In the discussion:
    Positive = Present    Negative = Absent

 1. False Positives: Is it permissible to report a
 false  positive result on both a total coliform.
 analyte and a fecal coliform/E. coli analyte in the
 same or separate samples within the PT set and be
 considered "acceptable" for the study?
 Yes.  One sample (vial) may be missed per
 analyte.   However,  a  lab cannot  report an
 "Absent" for a Total Coliform and a "Present"
 for Fecal/E. Coli for the same sample (vial) and
 have  that  false  positive  be  considered
 "acceptable."  If a  lab reports  "absent" for
 Total Coliform, the test ends.

 2.  False Negatives:  Does  one false negative
 reported value result in a "not acceptable" for the
 PT study, even though a lab could still pass nine
 out often samples within the set for one analyte
 but not the other?
 Yes.   This means the  lab missed a positive
 sample which is a public health concern.

 3. Analyte Definition: It is my understanding that
 Total  Coliform is considered one analyte and
 Fecal Coliform/fi'. Coli. is considered one analyte.
 That is correct.

 4. "Acceptable " analysis of a sample: Each PT
 study consists often samples. If a lab misses one
 analyte  within the  sample,  is  the  sample
 considered "not acceptable"?
Any false  negative or  more  than  one false
positive per analyte would be considered "not
 acceptable". Otherwise same as answer No. 1.
 And......More Websites
 Other websights that you may find useful are:
 www.epa.gov/ogwdw/regs.html lists drinking water

 www.epa.gov/ogwdw/methods/methods.html lists all
 promulgated methods and contains copies of some

 www.epa.gov/safewater/faq/sco.htm  lists  state
 certification contacts for every state and also gives
 links to lists of state laboratories certified for drinking
 water analyses.   There are  links for those states,
 which  have  electronic  lists  of  their  certified

 www.epa.gov/ttn/nelac/  contains   the   NELAC
 Standards, lists NELAC Accrediting Authorities and
 accredited laboratories, and has information about past
 and future NELAC meetings;

 html lists NIST-accredited PT providers;

www.epa. gov/qualitv/   contains  all  EPA  Quality
Documents and requirements, as well as available QA
training and information about the annual EPA  QA

    United States
    Environmental Protection
  OfSce of Ground Water and Drinking Water
  Cincinnati, OH 45268
  March 2003
                           In This Issue..!

                           S NEMI      -       t ft      , . ,   ,
                           / Recent promulgation of drinking   /
                              water methods  " <- <  ';  - " - * '*--_,
                           S Chlorite sampling and, monitoring ;
                           ;   requirements outlined  ^  '-^  '^''-> f/
                           V Cyanide methods clarified \.,(> ~  rj, ~-
                           S EPA Method 30