HomeMy WebLinkAboutNC0081825_Laboratory Inspection_20121204VA
NC®ENR
DENR-FRO
DEC 10 2012
WQ
North Ca'rol,ina ,Depairtmerit of Environment and Natural Resources
- Division of -Water Quality
Beverly Eaves Perdue ''Charles Wakild; P: E. Dee Freeman
Governor Director Secretary
December.4, 2012
5242 _
Ms. Dianna McLaughlin
Town of Ansonville WWTP
PO Box 437
Ansonville, NC 28007-
Dear Ms. McLaughlin:
Your letter received November 14, 2012, concerning corrective actions taken in response to the
items cited in the July 11, 2012 inspection report has been received and reviewed. The actions taken
are acceptable with the exception of the following comments:
Proficiency Testing
B. Finding: The laboratory is not analyzing Proficiency Testing (PT) samples in the same manner
as environmental samples.
Requirement: All PT samples are to be analyzed and the results reported- in a. manner
consistent with the routine analysis and reporting requirements of compliance samples and any
other samples analyzed according to the requirements of 15A NCAC 2H .0800. Ref: Proficiency
Testing Requirernents, February' 20, -2012, Revision 1.2. r"
Comment: The laboratory's common practice was to analyze a known standard along with the
PT sample as additional quality control.
Laboratorvs 1st Response:
The proficiency testing samples are not run in conjunction with the field parameters on any
specific date. They are, however, run per the instructions included for each parameter limited to
pH and Ultra Low Residual Chlorine. The results speak for themselves. Our accuracy is
reflected in the acceptable results recognized by our vendor ERA. We routinely order a known
standard to assure field calibration of our instruments.
Auditors 1st Response:
Some proficiency testing providers offer matrix -matched quality control samples to
accompany their PT samples. Please be aware that the use of these for proficiency testing is
unacceptable. Routine samples are not accompanied by matrix -matched samples.
1617 Mail Service Center, Raleigh, North Carolina 27699.1617
Location: 512 N. Salisbury St. Raleigh, North Carolina 27604
Phone: 919-807-63001 FAX: 919-807-6492
Internet: www.ncwaterouality.orq
An Equal Opportunity l Affirmative Action Employer
No thCarolina
Naturally
Addressee #5242 Town of Ansonville WWTP
Date: December 4, 2012
Page 2 of 3
Normal qc samples are acceptable, i.e. known pH buffers but not vendor supplied matrix
matched samples usually supplied along with the PT sample.
Please respond indicating that you are not analyzing known value PT samples,
supplied by the PT vendor, alongside your blind Pt samples.
Laboratories 2"d Response:
We will review and seek to conform to the divisions guidance for Proficiency Testing, Dated
February 20, 2012. Please send us a hard copy by return mail for our files.
Auditors 2nd Response:
Cliff Notes" version of the Performance Testing is attached.
Dissolved Oxygen — Standard Methods, 18th Edition, 4500 0 G
F. Finding: The laboratory is not documenting the air calibration.
Requirement: The meter must be calibrated prior to analysis of samples. The meter must be
calibrated either by the air calibration method or according to the manufacturer's calibration
procedure. The laboratory must document each time that a calibration is performed. Ref:
Technical Assistance for the Field Analysis of Dissolved Oxygen (DO).
Laboratory Response:
Dissolved oxygen is not a NPDES permit requirement on our permit #NC0081825.
Therefore, we do not feel compelled to submit results for compliance. Historically, we have
recorded our process observations on our monthly DMR's for our record only.
Auditor Response:
We would like to clarify this issue. 15A NCAC 28 .0506 (b) (3) (J). states: The results of all
tests on the characteristics of the effluent, including but not limited to NPDES permit
monitoring requirements, shall be reported on the monthly report forms.
This means, if you continue to analyze for DO at the effluent you must report that data on the
DMR. If that is the case you also are required to document'the calibration of the meter and
the time the calibration is performed. If you choose to sample at another site other than the
final effluent, to monitor DO for plant operation purposes, than you would not be required to
report the data and also would not be required to document the calibration and calibration
time.
Laboratorvs 2"d Response:
Will cease to report process control data that might confuse the auditor. If so instructed, we
are prepared to decommission the Dissolved Oxygen Probe in question.
Auditors 2nd Response:
Addressee #5242 Town of Ansonville WWTP
Date: December 4, 2012
Rage 3 of 3
If you choose to sample at another site other than the final effluent, to monitor DO for plant
operation purposes, then you would not be required to report the data and also would not be
required to document the calibration and calibration time.
We recommend that if Dissolved Oxygen is not on your -permit, to remove it from your
certificate. An `Amendment to Certification Application is attached. We will remove Dissolved
Oxygen from the laboratorys certification upon the completion and submission to our
laboratory.
Total Residual Chlorine — Standard Methods, 18th Edition, 4500 CI G
We have received your five point calibration verification and it is acceptable. We would like to
make the following recommendation for the next time you verify the calibration curve.
Recommendation: It is recommended that the laboratory verify the internal calibration using
the concentrations: 20, 35, 50, 200 and 400 pg/L. (versus the 20, 50, 100, 250, and 400
pg/L concentrations you analyzed) This will verify the analytical range used to measure
Proficiency Testing (PT) and environmental samples, demonstrate accuracy at or below the
permit limit and allow the use of the 0.200 mg/L'(i.e., 200 pg/L) Gel Standard as the midrange
daily check standard. What we wantto see is three standards between 50 pg/L and the
reporting level -since 50 pg/L is the compliance limit and what we are really concerned with is
between the 50 and the reporting level standards.
Laboratorys Response:
Please send us a written dilution schedule that will result in the serial dilutions that you
suggest, i.e., m'illiters of solute/per.
Auditors Response:
Attached is directions on "how to" prepare the Total Residual Chlorine curve. -
Please complete the attached Amendment to Certification Application, if you wish to remove
Dissolved Oxygen from your certificate.
Thank you for your time and cooperation. If you have questions, we can be contacted at (919) 733-
3908, Ext. 249.
Sincerely,
Jeffrey R. Adams
Laboratory Section
Cc: Dana Satterwhite
Fayetteville Regional Office
NC WW/GW LC Proficiency Testing - The "Cliff Notes" Version
Non -field laboratories must have a documented plan (this is usually detailed in the laboratory's Quality
Assurance Manual) of how they intend to cover the applicable program requirements for proficiency
testing per their scope of accreditation.
o Laboratory Standard Operating Procedures (SOPs) must address how low and high level samples
will be analyzed, including concentration of the sample or adjustment of the normality of a
titrant or multiple dilutions.
The Proficiency Testing Calendar Year is January 1 to September 30. To renew certification each year,
laboratories must submit acceptable PT sample results to the NC WW/GW LC Program for each
parameter, analyte, technology and matrix (where a method is matrix -specific) by September 30.
NOTE: Even if a laboratory analyzes PT samples prior to September 30, it does not mean that those
samples will be graded and reported to the NC WW/GW LC Program by the September 30 deadline.
Laboratories must choose a study that meets all reporting and posting deadlines. Most PT studies are
open for 45 days from the day the PTs are shipped to the laboratories. After a study closes, PT providers
may take up to 30 days to issue reports to participating laboratories and their designated authorities.
This means, that in order to meet the September 30`h deadline, laboratories should participate in a PT
study that begins no later than mid -July, unless using "Rapid Response" type samples.
Each certified laboratory must have an EPA Lab Code. The EPA Lab Code is not the same as the NC
laboratory identification number assigned to each laboratory by this Office or NPDES permit number.
Do not report PT results using only the NC laboratory identification number or permit number.
The laboratory must obtain samples from a proficiency testing sample provider recognized by The
NELAC Institute (TNI) and approved by the NC WW/GW LC program. These samples may be part of an
official study, a supplemental study or quick turnaroundtype samples. Proficiency testing samples from
providers not approved by TNI and the NC WW/GW LC program cannot be accepted. Currently, there
are two Proficiency Testing Provider Accreditors that are recognized by TNI and approved by the NC
WW/GW LC program — American Association for Laboratory Accreditation (A2LA) and ACLASS.
Accredited vendors can be found at the following websites (check the list each time PT samples are
ordered as the list changes periodically):
A2LA - http://www.a2la.org/pt/ProficiencyTesting.cfm. Laboratories must choose a
vendor from the published list of "A2LA Accredited TNI Proficiency Testing Providers".
ACLASS - http://www.aclasscorp.com/search-accredited-companies.aspx. This link
takes you to a search page where you can find a list of approved PT providers by
selecting Proficiency Test Provider - TNI Vol. 3 in the dropdown list under the
Accreditation Standard field.
The NC WW/GW LC program has elected to follow the 2009'TNI Standard for PT reporting and grading.
The 2009 TNI standard evaluations of less than (<} values are listed below:
As "Acceptable" when the assigned value is greater than "0" and the value
reported with thelessthan (<) sign is greater than the lower acceptance limit.
As "Not Acceptable" . when the assigned value is greater than "0" and the value
reported with the less than (<) sign is less than the lower acceptance limit.
As "Acceptable" when the assigned value is equal to < PTRL '(Proficiency Testing
Reporting Limit),.
Before the close of a PT study, a laboratory must arrange with the PT provider for the study results to be
sent directly from the PT provider to the NC WW/GW LC office before or at the same time that results
are released to the laboratory. The NC WW/GW LC program will not accept PT results directly from the
participant laboratories.
A laboratory that fails a PT sample for a :parameter method technology must take steps to identify the
root cause of the failure, take corrective action, report the corrective action taken to this office and
participate in a second PT study meeting the criteria listed previously in this policy. Remedial PT results
and corrective action reports (CARs) are due in 90 days: While the NC WW/GW LC program only requires
matrix -specific PTs for parameter method technologies that are matrix -specific, if an unacceptable result
is obtained for a specific matrix, the remedial PT must be of same matrix.
For multi-analyte parameters (e.g., organic analyses), when greater than or equal to 80% of analytes are
acceptable, but one or more individual analytes are graded unacceptable, acceptable performance has
been demonstrated for the parameter method technology. The laboratory must, however, analyze a
remedial PT for the individual analytes that were graded unacceptable. When a remedial PT is graded
unacceptable for an individual analyte (constituting a second unacceptable result), the laboratory must
qualify data for those individual analytes as "estimated" (whether detected or not) until acceptable
results are obtained on twoconsecutive remedial PTs. Notification will be sent from this office of this
single analyte provisional certification outlining the effective date. Provisional Certification Forms,
identifying North Carolina clients .for which affected data may be reported, must be submitted within 30
days of receipt.
When a PT sample study for a parameter includes multiple ampules with each one containing a different
concentration level or different matrix, the results reported for each level are first, graded separately
using the 80% rule. Once the acceptability of each level has been determined, the >50% Rule is applied
to determine the overall acceptability of the study.
For multi-analyte groups containing four or less analytes, laboratories must report acceptable results for
100% of each of the individual analytes in the reference sample for the cumulative result to be
acceptable.
Each certified laboratory must have an EPA Lab Code. Please note that the EPA Lab Code is not the same
as the NC laboratory identification number assigned to each laboratory by the State Laboratory or
NPDES permit number. Do not report PT results using only the NC laboratory identification number or
permit number.
All PT samples are to be analyzed and the results reported in a manner consistent with the routine
analysis and reporting requirements of compliance samples and any other samples analyzed. PT samples
must be entered into the laboratory sample receipt log as samples and tracked through the laboratory
as routine environmental samples. Their preparation must also be documented.
The lab shall retain all records necessary to facilitate historical reconstruction of the analysis and
reporting of analytical results for PT samples.
o This means the laboratory must have available and retain for five years [pursuant to 15A NCAC
2H .0805 (a) (7) (G)] all of the raw data, including benchsheets, instrument printouts and
calibration data, for all PT analyses and the associated quality control analyses conducted by all
method technologies.
o These records shall include a copy of the reporting forms used by the laboratory to report the
analytical results to the PT provider. If the analytical results for the PT samples were entered or
uploaded electronically to a provider website, the laboratory shall retain a copy of the on-line
data entry summary or similar documentation of entry of the PT results from the PT provider
website.
For those laboratories that do not have adequate glassware for PT sample preparation, and have
another lab assist with making up the PT sample, it is the participant laboratory's responsibility to retain
the PT sample preparation documentation.
Some proficiency testing providers offer known quality control samples to accompany their PT samples.
Please be aware that the use of these for proficiency testing is unacceptable. Routine samples are not
accompanied by known quality control samples. These may; however, be used with remedial PT samples
as part of the troubleshooting process.
2/2012
'
TOTAL RESIDUAL CHLORINE CURVE PREPARATION
Prepare a stock solution (1000 ppm) by dissolving 891"mg K -ssium
permanganate) to a liter of di-H20.
Dilute 10 mL of stock solution (1000 ppm), to 100 ml with delonized water in a
volumetric flask. This is the Intermediate standard. (100 ppm).
Dilute 1.0 mL of the Intermediate standard (100 ppm), to 100 mL with deionized
water, a chlorine equivalent of 1.00 mg/L will be produced in the DPD reaction.
This is the Working standard.
From this Working standard you will make up your annual curve.
Since your permit limit is 28pg/L, I would recommend a lower reporting limit of 20
pg/L and the top of your curve at 400 pg/L.
Take 40 mL of working standard to 100 mL with deionized water in a volumetric
flask. This is your 400 pg/L standard.
Take 20 mL of working standard to 100 mL with deionized water in a volumetric
flask. This is your 200 pg/L standard.
Take 10 mL of working standard to 100 mL with deionized water in a volumetric
flask. This is your 100 pg/L standard.
Take 5 mL of working standard to 100 mL with deionized water in a volumetric flask.
This is your 50 pg/L standard.
Take 2 mL of working standard to 100 mL with deionized water in a volumetric flask.
This is your 20 pg/L standard.
Take 1 mL of working standard to 100 mL with deionized water in a volumetric flask.
This is your 10 pg/L standard.
The concentrations stated are just recommendations and you can choose the curve
points and the range you choose to cover. Just remember this, you have to have a
standard below your permitted limit of 28 ug/L and 2 standards below 50 ug/L. and
anything that is above your highest standard (400 ug/L) must be diluted into range.
STATE OF NORTH CAROLINA
DEPARTMENT OF ENVIRONMENT & NATURAL RESOURCES
DIVISION OF WATER QUALITY
WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION
Amendment to Environmental
Laboratory Certification Application
Form #101-Amendment October 2010
INSTRUCTIONS: This amendment application is only one part of the certification process; completing and submitting an
amendment form does not constitute certification. Upon review of the completed amendment request, additional clarifications and
information may be required. Clarifications received in a timely manner will expedite the amendment application process. Please
complete all applicable parts of this form using a typewriter, computer, or print legibly in ink.
To apply for an amendment to your current laboratory certification, return the original and one copy of this form to:
ENR/DWQ Laboratory Section
Certification Branch
1623 Mail Service Center
Raleigh, NC 27699-1623
For additional information, contact the Laboratory Certification program office:
Telephone: 919-733-3908
Fax: 919-733-6241
Program Homepage: http://portal.ncdenr.org/web/wq/lab/cert or www.dwglab.orq
AMENDMENT FEES: No fees are charged to file an amendment request.
ADDITIONAL/RECERTIFICATION PARAMETER FEES: Requests for additional parameters or recertification of a parameter
will be reviewed and invoices for all additions/recertifications will be calculated in accordance with 15A NCAC 2H .0800. For each
additional inorganic parameter (excluding metals), a fee of $50.00 will be assessed. For each additional organic parameter and
metals analyte, a fee of $100.00 will be assessed. For each recertification of a parameter, a fee of $200.00 will be assessed. Do
not submit payment until you receive an invoice.
Section A: Facility and Contact Information
Facility Name
Contact Person
E-Mail Address
NC Certification Number
Telephone #, ext.
Fax #:
Section B: Requested Amendment
Complete only applicable areas.
If facility information has changed, (i.e., name of facility, supervisor/manager change, phone numbers, email or other contact
information) - please indicate below. Complete the information regarding supervisor credentials or operator certification, when
applicable.
Laboratory Supervisor/Operator's Certificate Number: Grade/Type of Certificate(s):
Laboratory Supervisor Information. NOTE: An attached resume may be substituted for this section.
(1) Education:
List the College(s), University (ies), or Technical Institute(s) attended dates of attendance, and degree
received.
Page 2 of 3 N.C. Laboratory Certification Amendment
(2.) Experience: List work -related experience, indicating the employer, years of employment, and basic job description.
Deleting parameters:
If you are requesting to delete any parameter(s) from your certificate, please list the analytical parameter(s), including the specific
method number(s) and edition(s)/revision(s), below.
Adding parameters:
If you are requesting additional certified parameters, please list the information in the table below. All requested information must
be supplied. For all organic analytical categories, please attach a typed list of analyte specific lower reporting limits. DO NOT
provide us with the laboratory method detection limit, unless the lower reporting limit and method detection limit are the same
number. For "method reference", list all appropriate method number(s) and the approved reference(s), such as Standard Methods
for the Examination of Water and Wastewater, 18th, 19th or 20th Edition.
Analytical Parameter
Method Number(s) and Reference(s)
Lower Reporting Limit
Concentration
(include. units)
OFFICE
USE
ONLY
•
Page 3 of 3
N.C. Laboratory Certification Amendment
Parameter Tecertification:
If you are requesting recertification; list the parameter(t) with method number(s) and the approved reference(s) you wish to
recertify after the decertification period has expired.
It is required that an acceptable performance evaluation study (analyzed within the last six months) for each applicable
parameter to be added to the certificate attachment be supplied directly from the vendor to this office.
It is required that two (2) acceptable performance evaluation studies (analyzed after the decertification effective date and
within the last six months) be submitted directly from the vendor to this office for each applicable parameter prior to
recertification.
Are Performance Evaluation Studies (analyzed within the last six months) for each of the requested additional/recertified
analytical parameters being sent to the Laboratory Section?
Yes No
If not supplied, are they on order? Yes No
Anticipated Completion Date
Section C: Authorized Signature
This statement certifies that the information in this amendment is truthful and accurate, and that the applicant is aware
of all regulations regarding the Quality Assurance requirements of Laboratory Certification.
Signature of Laboratory Supervisor: Date:
Print Full Name:
First Name M.I. Last Name
Form101-amend 10/21/2010