United States Office of Ground Water
Environmental Protection and Drinking Water
Agency
Technical
Support Division
EPA-814-N-94-001
August 1994
vvEPA Labcert Bulletin
We're Back!!!
And just in time to update you on the
proposed Information Collection Rule (ICR).
This edition contains a summary of the rule,
proposed February 10, 1994.
Other articles in this issue provide news on
the Methods Update Federal Register Notice
(MUFRN), a revised list of resources and a
regulations update. If you have ideas about
other certification topics you would like to see
discussed, please call, write or FAX the editors.
We have included a FAX sheet to update or
add your name to our mailing list or to send us
your comments.
Ed Glick 513 569-7939
Mary Ann Feige 513 569-7944
Carol Madding 513 569-7402
26 W. Martin Luther King Dr.
Cincinnati, OH 45268
In This Issue —
ICR Proposal - Here's the Scoop ..... 1
Availability of Granular Cadmium ... 3
Method Update Federal Register Notice 3
Fax Sheet . 3
Regulations Update 4
Holding Times 5
Letters to the Editors 5
Info World .... 5
Resources 6
The Perils of Positives 8
ICR Proposal
Here's the Scoop
The proposed Information Collection Rule
(ICR) was published in the Federal Register on
February 10, 1994 (59 FR 6332). This FR
notice proposes requirements for monitoring
microbial contaminants, disinfection byproducts
(DBPs), and general water quality parameters.
It also proposes reporting requirements for
treatment plant design and operating data and
requirements for conducting bench and pilot
scale DBP precursor removal studies for public
water systems. The purpose of the ICR is to
provide EPA with monitoring data and water
treatment process information for developing the
Enhanced Surface Water Treatment Rule and
Disinfection/Disinfection By-Products
Regulation. Promulgation is expected in
September with monitoring to begin in early
1995.
Microbial Monitoring
If the rule is promulgated as proposed, surface
water systems or groundwater systems under the
influence of surface water (Subpart H systems)
serving 10,000 people or more would be
required to conduct microbial monitoring.
Systems serving 100,000 people or more would
be required to conduct 18 consecutive months of
monitoring for Giardia, Cryptosporidium,
viruses, fecal coliforms or E. coli, and total
coliforms, while systems serving at least
10,000, but fewer than 100,000 people would
be required to conduct one year of bimonthly
monitoring for all the above, except viruses.
Printed on Recycled Paper
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Disinfection Byproduct (DBP) Monitoring
If the rule is promulgated as proposed, all
systems serving 100,000 or more persons would
be required to conduct DBP and general water
quality monitoring concurrently with microbial
monitoring. The general water quality
monitoring would include measurements of pH,
alkalinity, turbidity, temperature, calcium and
total hardness, total organic carbon
(TOC),absorbance of ultraviolet light at 254 nm
(UV254), bromide, ammonia, and disinfectant
residuals. The DBPs would include
trihalomethanes, haloacetic acids,
haloacetonitriles, chloral hydrate, chloropicrin,
haloketones, and total organic halide (TOX).
Additional monitoring would be required for
specific DBPs generated by the use of
alternative disinfectants or hypochlorite
solutions: 1) cyanogen chloride for systems
using chloramines, 2) chlorate for systems using
hypochlorite solutions, 3) chlorite, chlorate,
bromate and aldehydes for systems using
chlorine dioxide and 4) bromate and aldehydes
for systems using ozone. Ground water systems
serving > 50,000 persons would be required to
conduct TOC monitoring of their source water.
I^ahnratorv Approval for Chemistry
ICR analyses must be performed by
laboratories that have been evaluated for their
capability to produce accurate and precise data.
As part of the process to ensure that only
qualified laboratories conduct these analyses,
laboratories that plan to analyze ICR samples
would be required to register with EPA. For
ICR analyses that are already covered by a state
certification or approval process, laboratories
intending to perform these analyses would be
required to document their state
certification/approval to perform those same
analyses for the ICR.
Laboratories that would be performing
analyses that are not part of current drinking
water regulations (and, therefore, not part of
state certification or approval processes) would
be required to pass an EPA evaluation process
prior to receiving approval to perform the
analyses for the ICR. Approval would be made
on a method by method basis. A laboratory
applying for approval would furnish EPA with
specific information concerning personnel,
equipment, and sample handling protocols
involved with each ICR analysis. Method
detection limit (MDL), initial demonstration of
capability (IDC), and EPA performance
evaluation (PE) study data would also be
submitted to EPA. The laboratory would be
expected to have a Quality Assurance Manual
specific to the ICR and to meet specific criteria
for each method, which includes passing at least
one PE study prior to receiving EPA approval
to perform analyses for the ICR.
During the ICR monitoring period,
laboratories would be required to report specific
quality control data with the monitoring data
and to participate in quarterly PE studies.
These QC data would be used to verify that the
monitoring data are of sufficient quality to
achieve the objectives of the ICR. They would
also be used to evaluate laboratory performance.
Laboratories would be expected to demonstrate
continuing successful performance during the
monitoring period in order to maintain approval
to perform ICR analyses.
Laboratory Approval for Microbiology
Laboratories already certified by their State or
EPA Region for total and fecal coliforms and
for E. coli will receive approval to analyze ICR
samples. A laboratory would have to be
approved by EPA to perform Giardia,
Cryptosporidium and viruses analyses for the
ICR. To receive this approval, a laboratory
would be required to review the Guidance
Manual and training modules (which include
videos and manuals for protozoa and viruses),
satisfactorily analyze QC and PE samples, and
may be required to pass on-site evaluation. For
protozoa, the principal analyst in the laboratory
would be approved. For viruses, each
individual analyst in the laboratory would need
to be approved.
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Laboratory Approval Requests
Laboratories that plan to analyze samples for
the ICR should write to the following address:
ICR Laboratory Coordinator
Technical Support Division
Office of Ground Water and
Drinking Water, USEPA
26 West Martin Luther King Drive
Cincinnati, OH 45268
See the Federal Register for details of the
proposed rule. Copies of the guidance manuals
will be available by the promulgation date.
For information on how to receive a copy of
the guidance manuals or other information,
contact the Safe Drinking Water Hotline:
1-800-426-4791
Availability of Granular
Cadmium
Some concern has been expressed by analysts
involved in the determination of nitrite and
nitrate, in both drinking water and wastewater
analysis, about the availability of the proper
mesh size of cadmium used in the cadmium
reduction method. The 40-60 mesh granular
cadmium specified in U.S. EPA 353.2
(automated) and 353.3 (manual) cadmium
reduction methods is currently unavailable.
EMSL-Ci has determined there are several
other mesh sizes that have been successfully
used and can produce accurate results. The
following mesh sizes are acceptable for the
above mentioned methods: 12-50 mesh sold by
EM Scientific (catalogue # 2001) and the 12 -
20 mesh sold by Fisher Scientific (catalogue #
C 3-500).
This article was submitted by Jim O'Dell
of the EMSL-Ci and he can be reached for
comment on 513 569-7307.
Method Update Federal
Register Notice
Proposed Rule- 58 FR 65622 (Dec. 15,1993).
In this rule, EPA proposed to update 89
chemical or microbiological methods to versions
that are in the most current manuals published
by ASTM, EPA, USGS, and Standard Methods.
The rule proposed to expand the analytical
scope of five methods, add ten new methods,
and replace or withdraw several older methods.
One hundred thirty public comments were
received and are being evaluated by EPA. EPA
expects to publish a final rule by January 1995.
Fax It To Us
(Please print legibly in black pen)
Please add/change (circle one) my name to
the Labcert Bulletin mailing list.
Name
Company
Address
Telephone
Fax#
Fax to: Grace Zile
USEPA - TSD
26 W. M.L. King Drive
Cincinnati, OH 45268
FAX 513-569-7191
COMMENTS:
3
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REGULATIONS UPDATE
RULE
PROMULGA-
TION DATE
EFFECTIVE
DATE
COMMENTS
NIPDWRs
12/24/75
6/24/77
THMs
11/29/79
11/29/81 (83)
VOCs - Phase I
7/8/87
1/9/89
Monitoring revised 7/1/91
Fluoride
Revised
4/2/86
10/2/87
MCL will not be changed
SWTR - Surface Water Treatment Rule
6/29/89
12/31/90
TCR - Total Coliform Rule
6/29/89
12/31/90
Methods for E. coli
1/8/91
1/8/91
MMO-MUG approved 6/10/92
Phase II SOCs and IOCs
1/30/91
7/30/92
Standardized Monitoring
Reproposed Phase IIB (PCP & Ba)
Aldicarbs postponed 5/27/92
7/1/91
1/1/93
Aldicarbs Proposal Expected
Fall '94
DWPL - Drinking Water Priority List
1/14/91
New list will not be published
until SDWA is reauthorized
Lead & Copper
6/7/91
12/7/92
Tech. Corr. Expected 6/94
Phase V SOCs, IOCs & VOCs
7/17/92
1/17/94
(MCLs)
Monitor, eff. 1/93
Sulfate deferred
Methods Update Federal Register Notice
Proposed 12/15/93
Radionuclides
7/9/76
6/24/77
New Proposal 7/18/91
Final Expected 4/95
THM Methods
8/3/93
9/2/93
502.2 & 524.2 (8/3/93)
ICR - Information Collection Rule
Proposed 2/10/94
Final expected 9/94
Disinfection/Disinfection Byproducts &
Enhanced Surface Water Treatment Rule
Proposal Expected
July '94
Phase VIB SOCs, IOCs & VOCs
Proposal Expected
February '95
Arsenic
Proposal Expected
November '95
Sulfate
Proposal Expected
November '94
Groundwater Disinfection
Proposal Expected
August '95
July 1994
4
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Extract Holding Times For
Methods 504 and 505
In Chapter 4 of "The Manual For The Certifi-
cation Of Laboratories Analyzing Drinking
Water" the holding times listed for extracts in
Methods 504 and 505 are identified as "analyze
immediately". This is an error and will be
corrected this year with the revision of the
manual.
Method 504 states that an extract may be held
by inverting the extracted sample until analysis.
No extract holding time is listed. There is no
discussion of extract holding times listed in 505
either.
Using either method the Editors suggest
analyzing as soon as possible. Typically, an
analyst extracts a batch of samples and sets
them up in an autosampler which runs
overnight. This would result in extract holding
times of up to 24 hours. Until holding time
data can be acquired, the Editors suggest that a
holding time of 24 hours is not unreasonable.
For longer holding times, QC needs to be
increased to verify recoveries. We would
welcome any information you would like to
share on this subject.
^ "Letters, We Get
Letters, We Get Lots And
Lots Of Letters."
Wen , we got one letter anyway.
Dear Editors:
In our laboratory, we have found that recovery
and precision for dinoseb in method 515.1 is
greatly improved by using a stream of nitrogen
gas to concentrate the extract rather than
concentrating it on a water bath at 60-70° as
recommended in the method. Recovery for
other analytes is also improved. Our recoveries
for dinoseb ranged from 15-45% using the
water bath and from 55-84% using nitrogen.
Precision of the recoveries for 2,4-D and Silvex
were also greatly improved. This procedure
takes a little longer but improves precision,
recovery, and makes cleanup of the KD vial
easier. Since many of the 515.1 analytes
decompose at their boiling point, we believe that
blowing the extracts down with nitrogen at room
temperature is a good way to improve precision
and recovery. If you have any questions, please
feel free to call me at 801-584-8400.
Dr. Sanwat Chaudhuri
Utah Dept. of Health
Info World
W e've given you our address, we've given
you our phone numbers, we've given you our
FAX number. Now we've added yet another
means of communication.
U.S. EPA regional personnel can send us files
through the WAN (wide area network) by
accessing our mail names: MFEIGE,
EGLICK, and CM ADDING. When sending
a file on the WAN, you have to notify us that
it has been sent.
Outside the Agency, you can communicate
with us through Internet by accessing our E-
Mail addresses. Our addresses are:
FEIGE.MARYANN, GLICK.EDWARD, and
MADDING. CAROLINE followed by
@EP AM AIL. EPA. GOV@IN
Give it a try. We can start to send files back
and forth. If you have a topic you would like to
see us discuss or if you have a contributing
article, you now have another way to contact
us.
5
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RESOURCES
Methods for the Determination of Organic Compounds in Drinking Water
(Includes EPA Methods 502.1, 502.2, 503.1, 504, 505, 507, 508, 508A, 515.1, 524.1, 524.2,
525.1, and 531.1)
EPA/600/4-88/039, July 1991 NTIS #PB-91-231480 Cost $44.50
Methods for the Determination of Organic Compounds in Drinking Water-Supplement I
(Includes EPA Methods 506, 513, 547, 548, 549, 550, 550.1, 551, and 552)
EPA/600/4-90/020, July 1990 NTIS #PB-91-146027 Cost $36.50
Methods for the Determination of Organic Compounds in Drinking Water-Supplement II
(Includes EPA Methods 515.2, 524.2, 548.1, 549.1, 552.1, 553, 554, and 555)
EPA/600/R-92/129, August 1992 NTIS #PB-92-207703 Cost $36.50
Methods for the Determination of Metals in Environmental Samples
(Includes EPA Methods 200.1, 200.2, 200.3, 200.7, 200.8, 200.9, 218 6 245 1 and 245 3)
EPA/600/4-91/010, June 1991 NTIS #PB-91-231498 Cost $44.50
Methods for the Determination of Inorganic Substances in Environmental Samples
(Includes EPA Methods 180.1, 300.0, 335.4, 350.1, 351.2, 353.2, 365.1, 375 2 410 4 420 4)
EPA/600/R-93/100, August 1993 NTIS #PB-94-121811 Cost $27.00
Methods for Chemical Analysis of Water and Wastes
(Includes methods for metals and inorganics.)
EPA/600/4-79/020, March 1993 NTIS #PB-84-128677 Cost $52.00
Lead and Copper Rule Guidance Manuals
Vol I: Monitoring Requirements NTIS #PB92-112101 Cost $36.50
Vol II: Corrosion Control Treatment NTIS #PB-101533 Cost $36.50
The above manuals are available from: NTIS, US Dept of Commerce 5285 Port Roval Road
Springfield, VA 22161, 800-553-6847.
The Lead and Copper Rule Guidance Manuals (Volume I #20282, Volume II #20299, or the set
#20301) are also available from AWWA. Member prices are $25.50 each or $40 for the set.
Non-member prices are $32 each or $52/set.
Method 1613: Tetra- through Octa- Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS (Revision A) is available from: USEPA Office of Water Resource Center RC-
4100, 401 M Street, SW, Washington, DC 20460 (202-260-7786), Document #44011-90-024, or
from: USEPA, CERI, 26 W. Martin Luther King Drive, Cincinnati, OH 45268 (513-569-7562)
Document #EPA/600/R/93/018.
6
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Method 525.2 Determination of Organic Compounds in Drinking Water by Liquid-Solid
Extraction and Capillary Column Gas Chromatography/Mass Spectrometry, Revision 1
available from EMSL, 26 W. M.L.King Drive, Cincinnati, OH 45268 (513-569-7586).
Unregulated Contaminant Monitoring Implementation Guidance EPA 810-B-92-026, December
1992. This document will be available shortly. Contact the Drinking Water Hotline at
800-426-4791 for more information.
Safe Drinking Water Act Reauthorization Overview, EPA 810-S-94-001, February 1994. This
document discusses the major issues surrounding reauthorization of the Safe Drinking Water Act.
Contact EPA's Office of Water Resource Center (202-260-7786).
Drinking Water Laboratory Certification Workshop will be offered August 30-31 in Chicago,
Illinois. This two day workshop provides information on the Drinking Water Regulations, analytical
methodologies, and State certification programs. For more information contact Nasim Ansari at
616/337-8696 or write to Technical Education Services, P.O. Box 642, Portage, MI 49081-0642
The Certification Officers Training Courses will be offered in Cincinnati the week of July 11 for
chemistry and July 18 for microbiology. The courses will also be offered in San Francisco the week
of October 31 for chemistry and November 14 for microbiology. These courses are only open to
regional and state certification personnel. To register, contact your Regional certification officer.
The courses in San Francisco bracket the AWWA/WQTC Conference.
The Water Environment Federation's Conference, "Environmental Laboratories: Testing The
Waters" is slated for August 13-16, 1995 in Cincinnati, Ohio. Deadline for abstract submittal is
August 1, 1994. For more information call WEF's Conference Department at 703-684-2462.
The 1994 International Hazardous Materials Spills Conference will be held in Buffalo, N.Y.
from October 31 to November 3, 1994 at the Hyatt Regency Hotel and Convention Center. To
receive registration materials contact Angela Moody 703 442-9824. If you have questions regarding
the conference contact Sarah Bauer (202-260-8247).
The Perils Of Positives
To illustrate the perils of not being skeptical
of anomalies, and not carefully following
confirmation procedures, we describe a case
where a contaminant in a sample was
misidentified. Using EPA Method 504, two
laboratories misidentified dibromochloro-
methane (DBCM) as 0.29 and 29 ppb of
ethylene dibromide (EDB). The error was not
discovered until much effort, money, and
anxiety were expended conducting additional
sampling and analyses.
Method 504 uses an electron capture detector
(ECD), which is very sensitive but will detect
any electrophilic contaminant. This means that
while an ECD is excellent at detecting and
measuring trace contaminants, it is subject to
many interferences. It is stated twice in Method
504 that DBCM, a common disinfection by-
product in chlorinated water supplies, can elute
close to EDB. Rigorous confirmation
procedures must be followed before taking
action on a result.
In this case, data reviewers knew the
presumed EDB positive result occurred in
~ u.S. GOVERNMENT PRINTING OFFICE: 1994 - 550-
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samples from a chlorinated surface water
supply. Occurrence of EDB at many times the
MCL in such a supply is unlikely. However,
they and the laboratories neglected to thoroughly
confirm the result before talcing irreversible and
expensive action. In any method, even one
that uses a selective detector, an analyst must
know where interferences may occur and, if a
positive that requires action is found, it must be
confirmed. In this incident, a THM standard
could have been analyzed immediately to
determine if adequate separation was being
achieved between EDB and DBCM. If not, the
temperature program could have been adjusted
to achieve this separation and a duplicate sample
analyzed. Method 504 has other confirmation
procedures that include analysis on a second
column with dissimilar retention times and a
GC-MS analysis using Method 524.2 conditions
if adequate sensitivity can be attained.
Knowledge of probable contaminants in a
sample, and of method interferences are key
parts of quality assurance. Laboratories
reporting data must realize that users of
occurrence data are often unfamiliar with
analytical methods. Thus, program personnel
may assume that data provided is just what it
appears to be, nothing more, nothing less. Data
reviewers should ask whether a result is logical,
and not assume that the laboratory has
thoroughly eliminated analytical error from the
results. When resampling, the laboratory and
program personnel need to work closely
together to insure that the information is
accurate.
Starting in our next edition, we will highlight
one or more methods in each issue, beginning
with Method 504. We will discuss how to
avoid typical problems and suggest alternate
columns and other helpful information. We
invite our readers to submit ideas and tfyeir
experiences with drinking water methods.
METHOD NOTE
EMSL has advised us that the amber sample
bottle for Methods 549 and 549.1 can be any
type of plastic. It does not have to be PVC as
stated in the method.
United States Environmental Protection Agency Bulk Rate
OGWDW-TSD Postage & Fees Paid
Cincinnati, OH 45268 EPA
Postage No. G-35
Official Business, Penalty for Private Use $300
U.S. EPA Region ill
Eo^ional Center for Environments
Information
1650 Arch Street (3PM52)
Philadelphia, PA 19103
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