Approved Methods
„
SDWA and CWA
Official approved methods for Drinking
Water and Clean Water are listed in the 40
Code of Federal Regulations (CFR) 141
and 136
… Microbial
methods: listed in each rule for
which they are to be used (i.e. TCR, SWTR,
GWR)
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
2
Safe Drinking Water Act
„
Safe Drinking Water Act
For compliance samples, laboratories
must use only the analytical methodology
specified in the
„
… Total
Coliform Rule (40 CFR 141.21(f))
… Surface Water Treatment Rule
(40 CFR 141.74(a))
… Groundwater Rule (40 CFR 141.402 (c)(2))
A laboratory must be certified for all
analytical methods that it uses for
compliance purposes. At a minimum, the
laboratory must be certified for one total
coliform method and one fecal coliform or
E. coli method
3
Total Coliform Rule (40 CFR
141.21 (f))
„
„
„
„
„
4
Surface Water Treatment Rule (40
CFR 141.21 (f))
Total Coliform Fermentation (SM 9221 A, B)
Total Coliform Membrane Filtration (SM 9222 A,
B, C)
Presense-Absence (P-A) Coliform Test (SM 9221
D)
ONPG-MUG Test (SM 9223)
Colisure, E*Colite Test, m-ColiBlue 24,
Readycult, Chromocult, and Colitag
„
Total Coliform
… Fermentation
Technique (SM 9221 A, B)
Coliform Membrane Filter Technique (SM
9222 A, B, C)
… ONPG-MUG Test (SM 9223)
… Total
„
Fecal Coliform
„
Heterotrophic bacteria
… Fecal
… Pour
5
Coliform Procedure (SM 9221 E, D)
plate, SimPlate (SM 9215 B)
6
1
Clean Water Act- Approved Methods for
Wastewater and Sewage Sludge (CFR 136.3
Table IA)
Ground Water Rules (40 CFR
141.402 (c)(2))
„
…
…
…
…
„
Colilert, Colisure (SM 9223 B)
Membrane Filter (EPA 1604, M-ColiBlue)
24, E*Colite,
EC MUG, NA MUG (SM 9221 F, 9222 G)
…
…
„
„
„
„
…
„
7
MPN ( EPA 600/8-78-017 p. 132, EPA 1680, 1681, SM 9221
CE
Membrane Filtration (EPA 600/8-78-017 p. 124, SM 9222 D,
USGS B-0050-85
E. coli
„
PA (EPA 1602)
Single Agar Layer (EPA 1602)
MPN (SM 9221 B, EPA 600/8-78-017 p. 114)
Membrane Filtration (EPA 600/8-78-017 p.108, SM 9222 B,
USGS B-0025-85)
Fecal Coliform
„
Multiple Tube (SM9230 B)
Membrane Filter (SM 9230 C, EPA 1600)
Enterolert
Coliphage
…
Total Coliform
„
Enterococci
…
„
„
E.coli
MPN (9223 B, USGS 991.15, Colilert, Colilert 18)
Membrane Filtration (EPA 1603, mColiBlue 24)
8
References
„
40 CFR Chapters part 136 – 149 can be
found at:
http://www.access.gpo.gov/nara/cfr/waisid
x_08/40cfrv22_08.html
9
2
SDWA Coliform Positive
„ Each
SDWA Actions for
Positive Cultures
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
total coliform-positive (TC+)
routine sample must be tested for the
presence of fecal coliforms or E.coli.
„ If any routine sample is TC+, repeat
samples are required
2
Repeat Sampling Requirements
Repeat Sampling Requirements
„ Within
„ One
24 hours of learning of a TC+
routine sample result, at least 4
repeat samples must be collected and
analyzed for total coliforms.
repeat sample must be collected
from the original site; one within five
service connections upstream; one
within five service connections
downstream and one random sample.
3
4
Additional Routine Sample
Requirements
Repeat Sampling Requirements
„
If any repeat sample is TC+, the water supply
must analzye that TC+ culture for fecal coliforms
or E.Coli.
„
The water supply must also collect another set
of repeat samples, unless the maximum
contaminant level (MCL) has been violated and
the system/lab has notified the state, in which
case a district engineer will collect the repeat
samples.
5
„A
positive ROUTINE or REPEAT total
coliform result requires a minimum of
five ROUTINE samples be collected
the following month the water supply
provides water to the public unless
waived by the state.
6
1
SDWA Actions for Positive Cultures
For more information contact:
Drinking Water Message Center
651.201.4650
800.818.9318
[email protected]
7
2
Standard Operating Procedure
Manual Common Findings
„
Common Microbiology
Findings
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
„
Table of Contents
Manual must be uniquely identified
„
„
„
Serial number
Page numbers and total number of pages
Clearly defined end of the manual
„
Effective Dates
„
Copy to the commissioner
… Must
maintain a record of the effective dates
… Submit
a copy of revised SOPs within 30 days after
the effective date of the revision
2
Quality Assurance Manual
Common Findings
Common Micro Findings
Internal auditing
Tracking purity of reagents, standards,
media and reagent grade water
„ Failed PTs
„ Training and education of personnel
„ Subcontracting samples
„ Handling client complaints
„
„
„
„
„
Samples not stored separate
Chlorinated water sample checks
Sterility checks and blanks
… Blank
on each lot or batch of media (includes
chromofluorogenic reagent)
… Filtration techniques
… Sample containers
… Dilution water
… Membrane filters
3
Common Micro Findings, Cont.
„
4
Common Micro Findings, Cont.
Test variability
„
… Reproducibility
„
„
… None
Test Performance
… Verification
Documentation of media
„
of positives
or incomplete
Autoclaves
… Demonstration
of sterilization temperature
records
… Timing device
… Incomplete
Water monitoring
… Water
used in the prep of media, solutions or
buffers
5
6
1
Common Micro Findings, Cont.
„
Incubators and water baths
…
„
…
„
Temp checked 4 hours apart
Labware
Washed and reused
Volumetric equipment
…
Verified for accuracy
7
2
Sample Handling and Receipt
Sample Handling,
Receipt and
Acceptance
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
„
Transportation, receipt, handling
protection, storage, retention and
disposal of samples
„
Maintain system of
identifying/tracking samples to
ensure samples cannot be
confused physically or within the
laboratory’s documentation
„
„
„
„
food
Store standards and samples in separate locations
standards
„
samples
Condition of sample recorded upon receipt
Sample Handling and Receipt, Cont.
„Chlorine
Residual Checks
Laboratory shall check chemical preservation prior
to or during sample preparation or analysis
„ Microbiological samples from chlorinated water
systems do not require an additional chlorine
residual check in the lab if the following conditions
are met:
Identify number and types of
containers for each field of testing
Verify and record thermal
and chemical preservation
Maintain a chronological list
of samples, including the
container number and type,
received
Retain correspondence with
client on samples not
meeting the sample
acceptance criteria
EF-6.17.09
1 of 2
EF-6.17.09
2 of 2
Sample Handling and Collection
„
Requirements in the Code of
Federal Regulations (CFR). 40
CFR 136, Table II.-Required
Containers, Preservation
Techniques and Holding Times
„
Information in table takes
precedence over specific
information in methods
„
State agency methods (i.e.
performanced based methods
such as perfluorinated organic
compounds)
„
• Sufficient sodium thiosulfate is added to each container
and
• One container per lot is checked to ensure efficacy of
sodium thiosulfate, or
• Chlorine residual is verified by the collector and is <= 0.1
mg/L
EF-6.17.09
2 of 2
Sample Handling and Receipt, Cont.
Sample Handling and Receipt, Cont.
„
EF-6.17.09
1 of 2
1
Sample Acceptance and Rejection Policy
Sample Acceptance Policy
„
„
Written sample acceptance policy
… Made
available to sample collection personnel
outline circumstances that samples will be
accepted or rejected
… Must
„
Retain correspondence and records of
conversation concerning decision to dispose of
rejected sample or to proceed with analysis
Sample Acceptance Policy, Cont.
… Specified
holding times
… Adequate
sample volume
to be used when samples show
signs of damage, contamination, inadequate
preservation, or loss of integrity.
The sample acceptance policy at a
minimum must include the following items:
… Documentation,
including sample
identification
… Sample
… Use
labeling
of appropriate sample containers
Chain- of-Custody
„
… Procedures
„
„
The procedures and
records that
document the
possession and
handling of samples
from collection
through disposal
Chain-of-custody
form (legal)
Sample submission
form (non-legal)
Reference
„
Electronic Code of Federal Regulations Weblink:
http://ecfr.gpoaccess.gov/cgi/t/text/textidx?c=ecfr&tpl=%2Findex.tpl
2
Proficiency Testing (PT)
definition
„
Proficiency Testing
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
Is a means to evaluating a laboratory’s
performance under controlled conditions
relative to a given set of criteria through
analysis of unknown samples provided by
an external source.
2
Proficiency Testing Sample
Fields of Proficiency Testing
definition
„
Is a sample, the composition which is
unknown to the analyst and is provided to
test whether the analyst/laboratory can
produce analytical results within specified
acceptance criteria
„
PT program organized by fields of
proficiency testing. The following
collectively define fields of proficiency
testing
… Matrix
… Technology/method
… Analyte/analyte
and
group
3
Fields of Proficiency Testing
4
Proficiency Testing Requirements
Laboratories are permitted to analyze one
PT sample by multiple methods for a given
analyte within a technology.
„ If a laboratory reports more than one
method per technology per study, an
unacceptable result for any method would
be considered a failed study for that
technology for that analyte.
„
5
„
Initial accreditation
… Must
successfully complete two PT studies for each
requested field of proficiency testing within the most
three recent rounds attempted
… The three recent rounds must have occurred within
18 months of the laboratory’s application date
… The successful PT studies must be at least 15
calendar days apart from the closing date of one
study to the shipment date of another study
6
1
Proficiency Testing Requirements
„
Proficiency Testing Requirements
Continuing accreditation
„
… Must
complete two PT studies for each field of
proficiency testing out of the most recent
three
… Completion dates of successive proficiency
rounds for a given field of proficiency testing
must be approximately six months apart
7
Supplemental PT studies
… Laboratory
want to add fields of testing to
their scope
… Corrective Action
8
Proficiency Testing Requirements
Samples must be analyzed and the results
returned to PT Provider no later than 45
calendar days from the opening of the
study.
„ PT sample must be analyzed the same as
routine samples
„
9
2
Quality Assurance Manual
defined
SOP vs. QAM
What’s the
difference???
„
Commonly referred to as
the “QA manual”
„
A written record of the
laboratory’s plan to
ensure that sample
integrity is maintained;
sample testing is
appropriately conducted;
and reporting of data is
accurate.
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
2
QA Manual Requirements
Standard Operating Procedure Manual
defined
„
REVIEW
REVISE
„
SUBMIT
„
APPROVE
and IMPLEMENT
Commonly referred to as
“SOPs” or “SOP
manual”
A written record of
procedures used by the
laboratory for the
analysis of samples.
SOPs are the
operational backbone of
an analytical laboratory.
3
Standard Operating Procedure
Manual
4
SOP Manual Requirements
Key points to consider include:
„ Is there enough information so that the results are
repeatable?
„ Is cross-referencing clear enough that analysts can
easily obtain all the instructions that they need?
„ SOPs describe in detail all laboratory operations such as
preparation of reagents, reagent water, standards,
culture media, proper use of balances, sterilization
practices, and dishwashing procedures, and corrective
actions
„ SOPs are unique to the laboratory
5
REVIEW
REVISE
SUBMIT
APPROVE
and IMPLEMENT
6
1
QAM vs. SOP
QAM vs. SOP
Requirement
QAM
SOP
Requirement
QAM
SOP
Written plan / Table of
Contents
Yes
Yes
Record of effective dates for
all procedures
No
Yes
May include separate
procedure or documents
by reference
Yes
Yes
Reviewed periodically and
updated when necessary
Yes
Reviewed annually
Identification on each
page/Laboratory Name
Yes
Yes
Documentation of the review
process must include scope
of review, id of the reviewer,
date review complete
yes
Yes
Clear indication of end of
document
Yes
Yes
Must submit with application
Yes
Yes
Revision Number/Date
revision effective
Yes
Yes
7
QAM vs. SOP
8
QAM vs. SOP
Requirement
QAM
SOP
Requirement
QAM
SOP
Revisions must be submitted
in its entirety within 30 days
of revision
Yes
Yes
equipment maintenance &
scheduling
Yes
No
collection and transportation
of samples
Yes
No
data accuracy & precision for
each certified method
/analyte/test category
Yes
Yes
tracking samples (e.g. chain
of custody; reporting &
records retention)
Yes
No
validation of data conversion,
transcription, & reporting
Yes
No
Sample acceptance and
rejection criteria
Yes
No
tracking of standards,
reagents, and media
Yes
No
Determine continual
compliance (internal auditing)
Yes
No
correction of unacceptable PT
results & performance of
quality control checks
Yes
No
9
QAM vs. SOP
10
Key Points
Requirement
QAM
SOP
training & education
requirements
Yes
No
subcontract testing
Yes
No
addressing client complaints
Yes
No
Procedure
No
Yes
Regulations require well-documented
plans and activities
„ Lack of documentation leads to
inconsistent training and implementation
„ Personalize your instructions to ensure
understanding and use
„
11
12
2
Client Communications
What documents must a lab provide to a
client?
„ When does a client need to notified?
„ How does a client need to notified?
„
Client
Communications
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
2
Client Communications
„
Client Communications
A laboratory must make available its
current certificate and corresponding
scope of certification upon the request of a
client.
„
Suspension or revocation of laboratory’s
certification
… Upon
receiving the notice of suspension or
revocation, the laboratory must notify all
clients
… Notification must be in writing and a copy of
the notification must be sent to MDH
3
4
Client Communications
„
Client Communications
Voluntary withdrawal of certification
„
… By
the effective date of the withdrawal of
certification, the laboratory must notify current
clients and regulatory agencies of its intent to
withdraw its certification and must indicate the
effective date of the withdrawal
… Notification must be in writing and a copy of
the notification must be sent to MDH
5
Suitability of a sample for environmental
testing
… Must
consult the client for further instructions
maintain a written record of the
discussion
… Must
6
1
Client Communications
„
Client Communications
Samples analyzed by procedure other
than as written
… Must
„
Test Report
… Must
include deviations from the standard
operating procedure, such as failed QC,
additions to, or exclusions from the test
method
… Unacceptable instrument calibration
… Conditions that may have affected the quality
of results
have a record that includes
Sample identification traceable to client
Modification to the procedure
„ Reason for modification
„ Client’s authorization or acknowledgment of the
modification
„
„
7
8
Client Communications, Cont.
„
Test Report
… Definition
of data qualifiers
for which the lab is not certified
… Signify data reported that was done by a
subcontracted laboratory
… Results
9
2
Corrective Action
definition
What happens when it
fails!?!?!?
An action taken by the laboratory to
eliminate or correct the causes of an
existing nonconformance and prevent the
recurrence of the nonconformance
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
2
Corrective Action Plan
Corrective Action Steps
definition
A report which addresses specific items and
sets a specific date of completion,
generated by the laboratory in response to
deficiencies.
Establish policy and procedure
Designate appropriate personnel
„ Root cause
„ Select and implement corrective action
„ Monitor
„
„
3
4
Corrective Action
„
Corrective Action
Equipment/Instrument
„ Calibration
not within established
acceptance criteria
„ Not
working properly (problem)
„ Instrument is dirty (root cause)
„ Cleaning is necessary due to malfunction
(corrective action)
„ Cleaning will be set up on a regular
schedule (implement)
„ Continued proper operation (monitor)
Corrective action performed and all
associated samples reanalyzed
… If samples can not be reanalyzed data
associated with the unacceptable calibration
must be qualified on the final report
…
5
6
1
Corrective Actions
„
Corrective Actions
Quality Control Fails
„
… Not
within
acceptance criteria
… Sterility
checks/blanks show
growth
… Positive and
negative controls
Unacceptable Proficiency Test Results
… Within
30 days of notification submit
corrective action plan
… Within 30 days of notification submit the
laboratory’s request to purchase a PT sample
… Within 30 days of receiving the results of the
PT sample, submit a copy of the results
7
8
Corrective Action
Corrective Actions
„
„
Internal audit finding
External audit finding
… Within
30 days of
notification submit
corrective action planned
and taken
… If not received within 30
days regulatory action
maybe taken upon your
lab’s certification
… Conduct
at least annually to determine
compliance with the quality system and
testing requirements
9
10
2
Documentation of Laboratory Personnel
Training
Demonstration of
Laboratory Personnel
(Training and Documentation)
Minnesota Department of
Health Environmental
Accreditation Program
„
„
„
„
Documentation of Laboratory Personnel
Training, Cont.
1.
Documentation of Laboratory Personnel
Training, Cont.
Evidence that
each employee
has read,
understood and
is using the
approved
revision of the
laboratory’s QA
and SOP manual
2.
Documentation of Laboratory Personnel
Training, Cont.
3.
Maintain
documentation
of continued
proficiency
annually
Current job descriptions and table of organization
Laboratory personnel must have demonstrated capability
in the activities for which they are responsible. This must
be documented.
Initials and signatures of anyone analyzing or reviewing
data must be on file
Management must ensure and document that laboratory
staff maintain capability to perform job functions by the
following items:
Attendance at
training or
workshops
Reference
„
Environmental Laboratory Certification Program
http://www.health.state.mn.us/divs/phl/cert/index.html
1
Reporting
Reporting, Records and
Data Handling
Minnesota Department of Health
Environmental Laboratory
Accreditation Program
Test Reports
„
Title, such as “Test Report”, “Laboratory Results”
or “Certificate of Results”
„
Name, address and telephone number and name
of the contact person
„
Name and address of subcontract laboratory (if
applicable)
Test Report, continued
„
Reporting must be accurate,
legible, objective and
unambiguous
„
Modification in the procedure
must be documented
„
If your lab issues a DMR
Report, a formal test is not
required
„
Test report information should
include at a minimum the
following items:
Test Report, continued
Unique identification of the test report and
page numbers (i.e. 1 of 1)
„ The name of the client and the project
name (if applicable)
„ Identification of the approved method used
„ A description, the condition of, and
unambiguous identification of the sample
„
Test Report, continued
„
Date and time of sample collection
„
Date of analysis of the environmental test
„
The date of receipt of the sample (if
critical)
„
The test results and units of measurement
(when appropriate)
„
Time of sample preparation and time of
sample analysis (critical)
„
Identification of the person authorizing the
test report
2
Test Report, continued
Results relate only to the samples
„ Report reproduction
„ Deviations from standard operating
procedures
„ Document test results that do not meet the
requirement, or for which the laboratory is
not certified
„
Records, continued
Records
„
Records must allow for historical reconstruction
„
Records must be kept for five years
„
Electronic records are acceptable as long as you
maintain software and hardware to support the
records.
„
Records of signatures and initials of analysts
Data Handling
„
All observations used to calculate the final
result must be recorded immediately
„
Maintain work areas
for data handling and
storage areas
„
No erasures, overwritten files, or markings
„
Confidential business
information/trade
secret
„
Protect/maintain integrity and security of
the data
„
Retain sufficient raw
data for results
reconstruction
Data Handling within Lab Procedures
Contacts and more information
„
„
Conversion, transcription, and validation of
data
„
Handling out-of-control or unacceptable
data
„
Qualifying data on final reports
Environmental Laboratory Accreditation Program
Minnesota Department of Health
601 Robert Street North
Saint Paul, MN 55155
651-201-5200
http://www.health.state.mn.us/divs/phl/cert/index.html
[email protected]
„
Laboratory Accreditation Program Staff:
Lynn Boysen, [email protected]
Stephanie Drier, [email protected]
Denise Schumacher, [email protected]
Susan Wyatt, [email protected]
3
Contacts and more information
„ Environmental
Health’s Drinking
Water Message Center
(651)-201-4650 or
toll-free at 1-800-818-9318
[email protected]
4