HomeMy WebLinkAbout#253 - 2012 Insp - Final
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 253
Laboratory Name: Brunswick County Public Utilities - Wastewater
Inspection Type: Municipal Maintenance
Inspector Name(s): Todd Crawford
Inspection Date: June 6, 2012
Date Report Completed: June 19, 2012
Date Forwarded to Reviewer: June 19, 2102
Reviewed by: Chet Whiting
Date Review Completed: June 29, 2012
Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding __ Insp. CP___ Corrected
Unit Supervisor: Dana Satterwhite
Date Received: June 29, 2012
Date Forwarded to Linda: July 17, 2012
Date Mailed: July 18, 2012
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Brunswick County Public Utilities - Wastewater
NPDES PERMIT # NC0044873, NC0086819, WQ0000798, WQ0023693,
WQ0011614, WQ0012748
ADDRESS: PO Box 249
Bolivia, NC 28422
CERTIFICATE #: 253
DATE OF INSPECTION: June 6, 2012
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Todd Crawford
LOCAL PERSON(S) CONTACTED: Anna LeRoux
I. INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for the
analysis of environmental samples.
II. GENERAL COMMENTS:
The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses. A system of traceability for purchased reagents and consumable supplies was in place,
however, a system of traceability for prepared reagents and standards needs to be initiated.
The requirements associated with Findings A, B, C, D and H are new policies that have been implemented
by our program since the last inspection.
The laboratory is reminded that any time changes are made to laboratory operations; the laboratory
must update the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any
changes made in response to the Findings, Recommendations or Comments listed in this report must
be incorporated to insure the method is being performed as stated, references to methods are
accurate, and the QA and/or SOP document(s) is in agreement with approved practice and regulatory
requirements. In some instances, the laboratory may need to create a SOP to document how new
functions or policy will be implemented.
On May 18, 2012, EPA promulgated changes to the list of Clean Water Act (CWA) methods at 40 CFR
Part 136.3. This action, referred to as the Methods Update Rule (MUR) approves new methods, or
changes to existing methods, that affects over 100 EPA methods, Standard Methods, ASTM methods,
and other test procedures in Part 136 of Title 40 of the Code of Federal Regulations (CFR). The rule
also contains a number of clarifications relating to approved methods, sample preservation and holding
times, and method modifications. The final rule may be found at:
http://water.epa.gov/scitech/methods/cwa/update_index.cfm. The North Carolina Wastewater/
Groundwater Laboratory Certification (NC WW/GW LC) program will be asking certified laboratories to
move toward implementation of the new rule with changes fully implemented by the end of 2012. Each
laboratory will need to review the MUR and evaluate its effect on current laboratory practices. These
changes must be made in the laboratory’s Standard Operating Procedures and in Quality Manuals,
as well as any other place where the method is cited, e.g., reports, benchsheets, logs, etc. During
Page 2
#253 Brunswick County Public Utilities - Wastewater
this transition period, inspection reports will refer to the methods employed at the laboratory at the time
of the inspection, but will reference the requirements in the most recently approved version of the
method. Any difficulties encountered with meeting the requirements of these references by the date due
may be addressed in the written corrective action response.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Proficiency Testing
A. Finding: Proficiency Testing (PT) samples are analyzed with additional Quality Control standards
purchased from the PT provider.
Requirement: Laboratories shall conduct proficiency tests in accordance with their routine testing,
calibration and reporting procedures, unless otherwise specified in the instructions supplied by the
PT provider. This means that they are to be logged in and analyzed using the same staff, sample
tracking systems, standard operating procedures including the same equipment, reagents,
calibration techniques, analytical methods and preparatory techniques such as digestions,
distillations and extractions. They shall not be analyzed with additional quality control or replicated
beyond what is routine for environmental sample analysis. Results from multiple analyses (when
this is the routine procedure) must be calculated in the same manner as routine environmental
samples. The same quality control acceptance criteria must also be used. Ref: “North Carolina
Wastewater/Groundwater Laboratory Certification Program Proficiency Testing Requirements”,
February 14, 2011, Rev. 1.1, Section 3.6.
Documentation
B. Finding: The preparation of standards and reagents are not documented in such a way as to
provide traceability from preparation to analysis.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory must
have the following information documented: Date received, Date Opened (in use), Vendor, Lot
Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must be in
place that links standard/reagent preparation information to analytical batches in which the
solutions are used. Documentation of solution preparation must include the analyst’s initials, date
of preparation, the volume or weight of standard(s) used, the solvent and final volume of the
solution. This information as well as the vendor and/or manufacturer, lot number, and expiration
date must be retained for primary standards, chemicals, reagents, and materials used for a period
of five years. Consumable materials such as pH buffers, lots of pre-made standards and/or media,
solids and bacteria filters, etc. are included in this requirement. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
C. Finding: The preparation of Proficiency Testing (PT) samples is not documented.
Requirement: PT samples received as ampules must be diluted according to the PT provider’s
instructions. The preparation of PT samples must be documented in a traceable log or other
traceable format. The diluted PT sample becomes a routine environmental sample and is added
to a routine sample batch for analysis. Ref: Proficiency Testing Requirements, February 20,
2012, Revision 1.2.
Page 3
#253 Brunswick County Public Utilities - Wastewater
BOD - Standard Methods, 18th Edition, 5210 B
Comment: The pre-printed calculation formula on the laboratory benchsheet is incorrect. Final results,
however, were correctly calculated.
D. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen
Demand (BOD) bottles containing more than 67% (i.e., > 201 mL) sample.
Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients
may be limited in the diluted sample and, subsequently, reduce biological activity. In such
samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual BOD
bottles at a rate of 1 mL/L (0.33 mL/300-mL bottle) or use commercially-prepared solutions
designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B-2001. (5) (c) (2).
Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would
still be used in the BOD bottles. For the bottles containing more than 67% sample, extra
nutrient, mineral, and buffer solutions would be added in addition to the dilution water.
Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is
recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used.
Conductivity - Standard Methods, 18th Edition, 2510 B
E. Finding: The Automatic Temperature Compensator (ATC) has not been verified in the last 12
months.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the process
documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature
ranges of the samples to be analyzed. This may require the analysis of a third temperature
reading that is > 25 °C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
Comment: The ATC check was last performed on 03/17/11.
COD – HACH Method 8000
Recommendation: It is recommended that the laboratory rotate the position of samples, blanks and
quality control samples in the block digester during COD digestions. Random placement will help to
identify when optimal performance is not achieved in an individual sample well. It is also recommended
that the laboratory implement a temperature grid check of the block digester by alternating the well location
of the thermometer each time samples are digested. This will document heating uniformity and
consistency of all sample wells in the block.
Total Suspended Solids - Standard Methods, 18th Edition, 2540 D
Recommendation: A dry filter blank is being analyzed. However, the benchsheet indicates that 1000
ml is being put through the filter. It was stated that it was done that way to make the calculation work
out right. It is recommended that the blank acceptance criteria be based on the difference between the
initial and final filter weight and not of the weight per volume calculation.
Page 4
#253 Brunswick County Public Utilities - Wastewater
F. Finding: A quarterly check standard is not being analyzed.
Requirement: Excluding Oil and Grease, all residue parameters, leachate extractions, residual
chlorine, and coliform, analyze one known standard in addition to calibration standards each
day samples are analyzed to document accuracy. Analyze one suspended residue, one
dissolved residue, one residual chlorine and one oil and grease standard quarterly. For residual
chlorine, all calibration standards required by the approved procedure in use and by EPA must
be analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (B).
Ammonia Nitrogen – EPA Method 350.1
G. Finding: Samples are not being distilled prior to analysis and no distillation study is on file.
Requirement: Municipal and Industrial Laboratories shall analyze initially four samples distilled
and undistilled from each discharge and; thereafter, analyze two samples a year from each
effluent. Submit analytical results for four samples, distilled and undistilled, from each
discharge within 60 days of receipt of this report.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Code
of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007;
Table IB Footnote 6.
Comment: The titration method requires all samples to be distilled. For all other methods,
manual distillation is not required if comparability data on representative effluent samples are on
file to show that this preliminary distillation step is not necessary; however, manual distillation
will be required to resolve any controversies. In the case of low concentration effluents, the
samples must be spiked to allow for a meaningful statistical comparison. It is recommended that
samples with a concentration < 1.0 mg/L be spiked to yield a value in the 1 – 5 mg/L range.
Comparisons performed in this concentration range should check within 20% RPD. Additional
samples must be analyzed comparatively if the results do not indicate approximately the same
values for distilled and undistilled samples.
Recommendation: It is recommended that the distilled and undistilled sample portions be
analyzed by the same lab, using the same instrument, technology and methodology to minimize
uncertainty introduced by the analysis, yielding a truer representation of the effect of matrix and
the distillation process on sample results.
H. Finding: Laboratory reagent blanks routinely exceed 50% of the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Recommendation: Refer to EPA Method 350.1 section 7.1 and Standard Methods, 4500-NH3
B-1997 (3) (a) for preparing ammonia-free reagent water.
Ammonia Nitrogen – EPA Method 350.1
Total Phosphorus – EPA Method 365.4
I. Finding: Calibration standards in the middle of the curve are routinely dropped in order to make
the curve pass.
Page 5
#253 Brunswick County Public Utilities - Wastewater
Requirement: The verification of linearity must use a minimum of a blank and three standards. If
any verification data exceeds the initial values by ± 10%, linearity must be reestablished. If any
portion of the range is shown to be nonlinear, sufficient standards must be used to clearly define
the nonlinear portion. Ref: EPA Method 350.1, Rev.2.0 (1993) Section 9.2.2.
Comment: Nine calibration curve standards were typically analyzed and up to four may have been
dropped. An outlier calibration point (other than a high point or a low point) may be eliminated
only after an investigation has been performed and the reasons for the problem have been
documented (e.g., statistical test, or review of standard preparation logs). At no time may
calibration point/s be eliminated solely to meet or improve performance relative to calibration
curve acceptance criteria. In the latter case, the analyst has generated data that demonstrates
that the linear model does not apply to all of the data and re-analysis of the calibration must be
performed.
Coliform, Fecal - Standard Methods, 18th Edition, 9222D (MF)
J. Finding: Consumable materials used for the Fecal Coliform MF method are not properly tested.
Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a
comparison of the current lot in use (reference lot) against the new lot (test lot), must be made. As
a minimum, make single analyses on five positive samples. Ref: Policy based on Procedure for
Testing Consumable Materials Biological Testing.
Comment: Consumable testing was being conducted using only one positive sample.
IV. PAPER TRAIL INVESTIGATION:
No paper trail performed. Results are sent via email to the permit holders. Copies of Discharge
Monitoring Reports (DMRs) are not kept at the lab.
V. CONCLUSIONS:
Correcting the above-cited findings and implementing the recommendation will help this lab to produce
quality data and meet certification requirements. The inspector would like to thank the staff for its
assistance during the inspection and data review process. Please respond to all findings.
Report prepared by: Todd Crawford Date: June 19, 2012
Report reviewed by: Chet Whiting Date: June 29, 2012