#40_2017_0516_JS_FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 40
Laboratory Name: Pace Analytical Services LLC -Asheville NC
Inspection Type: Commercial Maintenance
Inspector Name(s): Jason Smith, Todd Crawford, Gary Francies, Tom Halvosa, Anna Ostendorff,
Dana Satterwhite, Tonja Springer and Beth Swanson
Inspection Date: May 16 and 17, 2017
Date Forwarded for Initial June 16, 2017 Review:
Initial Review by: Anna Ostendorff
Date Initial Review June 27, 2017 Completed:
D lnsp. Initial D lnsp. Reg
Cover Letter to use: Dlnsp. No Finding Olnsp. CP
Ocorrected cgjlnsp. Reg. Delay
Unit Supervisor/Chemist Ill: Todd Crawford
Date Received: June 29, 2017
Date Forwarded to Admin.: July 25, 2017
Date Mailed: August 1, 2017
Special Mailing Instructions:
40
Mr. Barry Johnson
Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive
Asheville, NC 28804
ROY COOPER
MICHEAL S. REGAN
S.JAY ZIMMERMAN
August 1, 2017
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Johnson:
Enclosed is a report for the inspection performed on May 16 and 17, 2017 by Jason Smith. I apologize
for the delay in getting this report to you. Where Finding(s) are cited in this report, a response is
required. Within thirty days of receipt, please supply this office with a written item for item description of
how these Finding(s) were corrected. Please describe the steps taken to prevent recurrence and include
an implementation date for each corrective action. If the Finding(s) cited in the enclosed report are not
corrected, enforcement actions may be recommended. For Certification maintenance, your laboratory
must continue to carry out the requirements set forth in 15A NCAC 2H .0800.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect
any changes made during the audit. Copies of the checklists completed during the inspection may be
requested from this office. Thank you for your cooperation during the inspection. If you wish to obtain an
electronic copy of this report by email or if you have questions or need additional information, please
contact me at [phone] ext. 251.
Attachment
Sincerely,
��
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
cc: Dana Satterwhite, Jason Smith, Master File #40
Water Sciences Section
NC Wastewater/Groundwater Certification
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Lab Name:
Address:
Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive
Asheville, NC 28804-
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
INORGANIC
ALKALINITY
SM 2320 B-1997, Rev. 2011 (Aqueous)
BACTERIA -COLIFORM FECAL
SM 9222 D-1997 (MF) (Aqueous)
IDEXX Colilert ®18 (MPN) (Aqueous)
BOD
SM 521 O B-2001, Rev. 2011 (Aqueous)
CERTIFIED PARAMETERS
IGNITABILITY
SW-846 1010 A (Pensky-Martens) (Aqueous)
INORGANIC PHENOLS
EPA 420.4, Rev. 1.0, 1993 (Aqueous)
SW-846 9065 (Aqueous)
NITROGEN, AMMONIA
EPA 350.1, Rev. 2.0, 1993 (Aqueous)
NITROGEN, NITRATE
Certificate Number:
Effective Date:
Expiration Date:
Date of Last Amendment:
40
1/1/2017
12/31/2017
5/26/2017
SM 5210 B-2001 (ASTM D 888-09 C) (LOO) (Aqueous)
BROMIDE
(N03 + N02 EPA 353.2, Rev. 2.0, 1993) -(N02 EPA 353.2, Rev. 2.0, 1993) (Aqueous)
(N03 + N02 SW-846 9056 A) -(N02 SW-846 9056 A) (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
CBOD
SM 521 O B-2001, Rev. 2011 (Aqueous)
SM 5210 B-2001 (ASTM D 888-09 C) (LOO) (Aqueous)
CHLORIDE
SM 4500 er E-1997, Rev. 2011 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
CHLORINE, TOTAL RESIDUAL
SM 4500 Cl G-2000, Rev. 2011 (Aqueous)
COD
SM 5220 D-1997. Rev. 2011 (Aqueous)
CYANIDE
SM 4500 cN-E-1999, Rev. 2011 (Total) (Aqueous)
Lachat 10-204-00-1-X, Rev. 2.2, 2005 (SW-846 9012B) (Total) (Aqueous)
Lachat 10-204-00-1-X, Rev. 2.2, 2005 (SW-846 9012B) (Total) (Non-Aqueous)
Lachat 10-204-00-1-X, Rev. 2.2, 2005 (Total) (Aqueous)
DISSOLVED OXYGEN
SM 4500 0 G-2001, Rev 2011 (Aqueous)
FLUORIDE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
HARDNESS TOTAL
SM 2340 B-1997, Rev.2011 (Ca EPA 200.7, Rev. 4.4,1994+Mg EPA 200.7, Rev. 4.4,1994) (Aqueoui
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
NITROGEN, NITRITE
EPA 353.2, Rev. 2.0, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
NITROGEN, N03 + N02
EPA 353.2, Rev. 2.0, 1993 (Aqueous)
NITROGEN, TOTAL KJELDAHL
EPA 351.2, Rev. 2.0, 1993 (Aqueous)
ORGANIC CARBON, TOTAL
SM 531 O B-2000, Rev. 2011 (Combustion) (Aqueous)
SW-846 9060 A (Combustion) (Aqueous)
PAINT FILTER LIQUIDS
SW-846 9095B
pH
SM 4500 H+B-2000, Rev. 2011 (Aqueous)
SW-846 9040 C (Aqueous)
SW-846 9045 D (Non-Aqueous)
PHOSPHATE, ORTHO
SM 4500 P E-1999, Rev. 2011 (Aqueous)
EPA 365.1, Rev. 2.0, 1993 (Aqueous)
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
PHOSPHORUS, TOTAL
EPA 365.1, Rev. 2.0, 1993 (Aqueous)
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Lab Name:
Address:
Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive
Asheville, NC 28804-
The above named laboratory, having duly met the requirements of 1 SA NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
RESIDUE, DISSOLVED 180 C
SM 2540 C-1997, Rev. 2011 (Aqueous)
RESIDUE, SETTLEABLE
SM 2540 F-1997, Rev. 2011 (Aqueous)
RESIDUE, SUSPENDED
SM 2540 D-1997, Rev. 2011 (Aqueous)
RESIDUE, TOTAL
SM 2540 B-1997, Rev. 2011 (Aqueous)
SILICA
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 601 O D (Aqueous)
SW-846 6010 D (Non-Aqueous)
SULFATE
EPA 300.0, Rev. 2.1, 1993 (Aqueous)
SW-846 9056 A (Aqueous)
SULFIDE
SM 4500 s:2-D-2000, Rev. 2011 (Aqueous)
TURBIDITY
EPA 180.1, Rev. 2.0, 1993 (Aqueous)
VECTOR ATTRACTION REDUCTION
Option 1: Reduction in Volatile Solids
Option 2: Anaerobic Batch Digestion
Option 3: Additional Digestion of Sludge
METAL
SPLP METALS
SW-846 1312 (Aqueous)
SW-846 1312 (Non-Aqueous)
TCLP METALS
SW-846 1311 (Aqueous)
SW-846 1311 (Non-Aqueous)
ALUMINUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
CERTIFIED PARAMETERS
SW-846 6020 B (Aqueous)
ANTIMONY
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
ARSENIC
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
BARIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
BERYLLIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
BORON
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
CADMIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
Certificate Number:
Effective Date:
Expiration Date:
Date of Last Amendment:
40
1/1/2017
12/31/2017
5/26/2017
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Lab Name:
Address:
Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive
Asheville, NC 28804-
The above named laboratory, having duly met the requirements of 1 SA NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
CALCIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
CHROMIUM HEXAVALENT
SM 3500-Cr-B-2009, Rev. 2011 (Aqueous)
SW-846 7196 A (Aqueous)
SW-846 7196 A (Non-Aqueous)
EPA 218. 7, Rev. 1.0, 2011 [NCAC .02L Variance] (Aqueous)
CHROMIUM TOTAL
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
COBALT
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
COPPER
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
IRON
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
CERTIFIED PARAMETERS
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
LEAD
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
LITHIUM
SW-846 6020 B (Aqueous)
MAGNESIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
MANGANESE
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
MERCURY
EPA 245.1, Rev. 3.0, 1994 (Aqueous)
SW-846 7470 A (Aqueous)
SW-846 7471 B (Non-Aqueous)
EPA 1631 E (Aqueous)
MOLYBDENUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 601 O D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
NICKEL
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
Certificate Number:
Effective Date:
Expiration Date:
Date of Last Amendment:
40
1/1/2017
12/31/2017
5/26/2017
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Lab Name:
Address:
Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive
Asheville, NC 28804-
The above named laboratory, having duly met the requirements of 15A NCAC 2H.0800, is hereby certified for the measurement of the parameters listed below.
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
POTASSIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SELENIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SILVER
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 601 O D (Aqueous)
SW-846 601 O D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
SODIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
STRONTIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
THALLIUM
CERTIFIED PARAMETERS
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
TIN
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
TITANIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
VANADIUM
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
ZINC
EPA 200.7, Rev. 4.4, 1994 (Aqueous)
SW-846 6010 D (Aqueous)
SW-846 6010 D (Non-Aqueous)
EPA 200.8, Rev. 5.4, 1994 (Aqueous)
SW-846 6020 B (Aqueous)
Certificate Number:
Effective Date:
Expiration Date:
Date of Last Amendment:
40
1/1/2017
12/31/2017
5/26/2017
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples. Laboratories are subject to civil penalties and/or decertification for infractions
as set forth in 15A NCAC 2H.0807.
On-Site Inspection Report
LABORATORY NAME: Pace Analytical Services LLC -Asheville NC
2225 Riverside Drive ADDRESS:
Asheville, NC 28804
CERTIFICATE#: 40
DATE OF INSPECTION: May 16 and 17, 2017
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Jason Smith, Todd Crawford, Gary Francies, Tom
Halvosa, Anna Ostendorff, Dana Satterwhite, Tonja
Springer and Beth Swanson
LOCAL PERSON(S) CONTACTED: Barry Johnson and Craig Tronzo
I.INTRODUCTION:
This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements
of 15A NCAC 2H .0800 for the analysis of environmental samples.
II.GENERAL COMMENTS:
The facility is well organized and has all the equipment necessary to perform the analyses.
Benchsheets are well designed, easy to follow and concise. Records are well organized and easy
to retrieve. The laboratory has a detailed and effective system of traceability. Staff were
forthcoming and seemed eager to adopt necessary changes. Laboratory management
encourages a culture of continuous process improvement, including implementing Lean
management principles within the past year. These principles are intended to achieve incremental
changes in the laboratory to improve the efficiency and data quality.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program
outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by June 30, 2018.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre-audit review or to 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 each
approved practice, test, analysis, measurement, monitoring procedure or regulatory
requirement being used in the laboratory. In some instances, the laboratory may need to create
an SOP to document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
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Ill.
(e.g. Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "All analytical data pertinent
to each certified analysis must be filed in an orderly manner so as to be readily available for
inspection upon request", are intended to be a requirement to document information pertinent to
reconstructing final results and demonstrating method compliance. Use of this requirement is not
intended to imply that existing records are not adequately maintained unless the Finding speaks
directly to that.
All required Proficiency Testing (PT) samples for the 2017 PT calendar year have not yet been
analyzed. The laboratory is reminded that results must be received by this office directly from the
vendor by September 30, 2017.
FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Recommendation: The percent recovery of MS/MSD results and/or Relative Percent Difference
(RPO) of duplicate results are calculated by the Laboratory Information Management System
(LIMS) and results are reviewed by the analyst on the computer. It is recommended that the
results of these calculations be documented on the benchsheet to more clearly show that the QC
was evaluated while filling out the QC Summary Sheet, which is used to ensure data qualifiers are
reported when needed.
A.Finding: The units of measure are incorrectly or not consistently documented on
laboratory worksheets.
Requirement: All laboratories must use printed laboratory bench worksheets that
include a space to enter the signature or initials of the analyst, date of analyses, sample
identification, volume of sample analyzed, value from the measurement system, factor
and final value to be reported and each item must be recorded each time samples are
analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).
Comment: Units of measure were missing on the Inorganic Phenols and Cyanide
standard and reagent preparation worksheets and the Total Organic Carbon QC
Summary Sheet.
Comment: The sample preparation sheet for Conductivity listed the units of measure as
mg/L instead of µmhos/cm or µSiem.
B.Finding: Some benchsheet references do not accurately reflect the laboratory's certified
methods.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
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Comment: The benchsheet for documenting pH values for Hexavalent Chromium
samples by Standard Methods, 3500 Cr B-2009 references Standard Methods, 3500 Cr D-
2009.
Comment: The QC Summary Sheet for Turbidity references EPA Method 180.2 instead
of EPA Method 180.1.
Comment: The Metals Batch Summary Form references SW-846 6010 C instead of SW-
846 6010 D.
Proficiency Testing
C.Finding: The laboratory is not consistently analyzing PT samples in the same manner as
compliance samples.
Requirement: As specified in 15 NCAC 2H .0800, in order to meet the minimum
standards for Certification, laboratories must use acceptable analytical methods. The
acceptable methods are those defined or referenced in the current State and federal
regulations for the environmental matrix being tested. All samples, (including PT
Samples) that are, or that may, be used for Certification purposes, must be analyzed using
approved methods only. 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. Laboratories must document any exceptions. All PT Sample analyses must be
recorded in the daily analysis records as for any Compliance Sample. This serves as the
permanent laboratory record. Ref: Proficiency Testing Requirements, May 31, 2017,
Revision 2.0.
Comment: The Mercury by EPA Method 1631 E PT sample was analyzed at multiple
dilutions, some of which were within the calibration range and reportable. It was then
reanalyzed the next day and the results were reported from the second day analysis.
Reporting
D.Finding: The results of all tests on the characteristics of the effluent are not being
consistently reported to clients.
Requirement: 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. Ref: 15A NCAC 28 .0506 (b) (3) (J).
Comment: This was noted for Fecal Coliform duplicate analyses. When samples are
duplicated, only the first result is reported. In order to meet this requirement, the results
must be averaged or both results must be reported.
Recommendation: It is recommended that the laboratory review all parameters to ensure
clients are provided with adequate information to comply with this requirement.
E.Finding: QC failures are not consistently reported with the results.
Requirement: When quality control (QC) failures occur, the laboratory must attempt to
determine the source of the problem and must apply corrective action. Part of the
corrective action is notification to the end user. If data qualifiers are used to qualify
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samples not meeting QC requirements, the data may not be useable for the intended
purposes. It is the responsibility of the laboratory to provide the client or end-user of the
data with sufficient information to determine the usability of the qualified data. Ref: NC
WW/GW LC Policy.
Comment: This was noted for Nitrite Nitrogen by EPA Method 353.2 on May 2, 2017. The
recovery of the 0.04 mg/L standard was 79%. The laboratory established acceptance
criterion is ± 20% for standards at this concentration (i.e., equal to or less than double the
reporting limit).
Comment: This was noted for Total Solids by Standard Methods, 2540 B-1997 on March
26, 2017. The recovery of the standard was 81 % and the acceptance criterion is± 10%.
Quality Control
F.Finding: MS results are not properly calculated on a consistent basis.
Requirement: If the spike solution volume constitutes >1 % of the total sample volume,
the sample concentration or spike concentration must be adjusted by calculation. Ref: NC
WW/GW LC Policy.
Comment: See the attached NC WW/GW LC Technical Assistance document for further
information.
Comment: The MS samples for COD and Mercury are prepared with a spiking solution
that is >1 % of the total volume and the results are not adjusted by calculation.
Comment: Current NC WW/GW LC Policy allows the MS to dilute the sample up to 10%,
but this policy is in the process of being updated to meet the Standard Methods
requirement of a maximum dilution of 5%.
Recommendation: It is recommended that the MS volume be reduced to :51 % of the total
volume. This would allow the laboratory's current recovery formula to be used.
General Laboratory
G.Finding: The laboratory does not consistently notify the client and the State Laboratory
when receiving samples that do not meet sample collection, holding time, or preservation
requirements.
Requirement: Chromium VI ....... Cool, :56 °C18 , pH = 9.3-9.720 . Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II.
Requirement: At any time a laboratory receives samples which do not meet sample
collection, holding time, or preservation requirements, the laboratory must notify the
sample collector or client and secure another sample if possible. If another sample cannot
be secured, the original sample may be analyzed but the results reported must be
qualified with the nature of the infraction(s) and the laboratory must notify the State
Laboratory about the infraction(s). The notification must include a statement indicating
corrective actions taken to prevent the problem for future samples. Ref: 15 NCAC 2H
.0805 (a) (7) (N).
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Comment: A sample analyzed for Hexavalent Chromium on March 31, 2017 was
improperly preserved at pH 9.86 S.U. The laboratory did not notify the client or NC
WW/GW LC staff and sample results were not qualified.
Alkalinity -Standard Methods, 2320 B-1997, Rev. 2011 (Aqueous)
Recommendation: It is recommended that the sample volume and calculated normality of the
acid be added to the instrument printout.
H.Finding: Results are not calculated properly.
Requirement: Potentiometric titration to end-point pH:
Alkalinity, mg CaCQ3/L = (A x N x 50,000) / ml sample
where:
A = ml standard acid used and
N = normality of standard acid
Ref: Standard Methods, 2320 B-1997. (5) (a).
Comment: All sample results were calculated using the following low-level (< 20 mg/L)
alkalinity procedure and formula:
Alkalinity, mg CaC03/L = [(28 -C) x N x 50,000] / ml sample
where:
B = ml titrant to first recorded pH,
C = total ml titrant to reach pH 0.3 unit lower, and
N = normality of acid
Comment: For the data reviewed, sample results reported were 2-4 mg/L less than the
results when calculated properly.
I.Finding: The laboratory uses 50 ml of sample for all analyses.
Requirement: Potentiometric titration of low alkalinity: For alkalinities less than 20 mg/L
titrate 100 to 200 ml according to the procedure of ,I c above, using a 1 O ml microburet
and 0.02N standard acid solution. Ref: Standard Methods, 2320 B-1997. (4) (d).
Comment: Alkalinity is considered a method-defined parameter per the definition in the
Code of Federal Regulations, Part 136.6, Section (a) (5). This means that the method may
not be modified to reduce the sample volume per Section (b) (3).
Bacteria -Coliform Fecal -Standard Methods, 9222 D-1997 (MF) (Aqueous)
Recommendation: The laboratory only calculates the result per 100 ml of sample for dilutions
that result in plates that meet the 20-60 colony requirement. It is recommended that the laboratory
calculate the result per 100 ml for all plates to verify that the results are consistent between
dilutions.
J.Finding: The laboratory is not checking the pH of prepared media properly.
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Requirement: Rehydrate product in 1 l water containing 10 ml 1 % rosolic acid in 0.2 N
NaOH. Heat to near boiling, promptly remove from heat, and cool below 50 °C. If agar is
used, dispense 5-to 7-ml quantities to 50 x 12-mm petri plates and let solidify. Final pH
should be 7.4 ± 0.2. Ref: Standard Methods, 9222 D-1997. (1) (a).
Comment: The laboratory adds a small amount of DI water to the hot agar in order to
allow pH analysis with a standard pH electrode. The addition of DI water is not included in
the method and may have an effect on the pH of the solution.
Recommendation: It is recommended that the laboratory use a pH electrode for surface
measurements, which is made to be used for solid and semi-solid samples, and analyze
the agar after it solidifies without the addition of DI water.
K.Finding: The laboratory is not sterilizing the phosphate buffer and magnesium chloride
solutions.
Requirement: Stock phosphate buffer solution -Sterilize by filtration or autoclave. Store
stock solution under refrigerated conditions and discard if turbidity develops. Ref: Standard
Methods, 9050 C-2005. (1) (a) (1).
Requirement: Magnesium chloride stock solution -Sterilize and store stock solution
under refrigerated conditions, discarding if solution becomes turbid. Ref: Standard
Methods, 9050 C-2005. (1) (a) (2).
L.Finding: The pH of the phosphate buffer solution is not being documented. This is
considered pertinent data.
Requirement: Stock phosphate buffer solution -Dissolve 34.0 g potassium dihydrogen
phosphate (KH2P04) in 500 ml reagent-grade water, adjust to pH 7.2 ± 0.5 with 1 N
sodium hydroxide (NaOH), and dilute to 1 l with reagent-grade water. Ref: Standard
Methods, 9050 C-2005. (1) (a) (1 ).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
M.Finding: The laboratory was not documenting the use of heat-indicating tape.
Requirement: Use heat-indicating tape to identify supplies and materials that have been
sterilized. Ref: Standard Methods, 9020 B-2005. (4) (h).
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
N.Finding: The laboratory does not evaluate duplicates with countable plates with greater
than 60 colonies.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
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Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
0.Finding: Positive control plates are not countable.
Requirement: A culture positive must be analyzed with each batch of prepared media and
once per week for purchased ready-to-use media. A sample volume that yields a
countable plate must be analyzed so that individual colonies may be verified to have
proper morphology (e.g., color, shape, size, surface appearance). Ref: NC WW/GW LC
Policy.
Comment: The laboratory currently uses a purchased positive control. They are working
on using a new source (Wastewater Treatment Plant influent) to improve their ability to
control the coliform concentration of positive controls.
Bacteria -Coliform Fecal -IDEXX Colilert ®18 (MPN) (Aqueous)
P.Finding: One instance of this method being used for stream samples was noted.
Requirement: The Environmental Protection Agency (EPA) Region 4 Science and
Ecosystem Support Division approves the use of IDEXX Colilert-18 for the detection and
enumeration of fecal coliforms in wastewater samples as an Alternate Test Procedure
(ATP) until it has been formally promulgated nationally as part of 40 CFR Part 136 under
the Clean Water Act. Ref: EPA Region 4 (Science and Ecosystem Support Division)
Approval of Colilert-18 for the Detection and Enumeration of Fecal Coliforms in
Wastewater Samples, Rev. 0, October 2010, (1 ).
Comment: Colilert-18® may not be used for fecal coliform analysis of storm water
samples, stream monitoring tied to NPDES permits (e.g., upstream, downstream),
groundwater monitoring wells or for biosolids monitoring under 503 regulations. It may;
however, be used for any wastewater analysis including when wastewater is used in an
application such as spray irrigation or used for beneficial reuse as reclaimed water.
Q.Finding: The laboratory has not established procedures for calculating a final result from
the sample dilutions.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Bacteria -Coliform Fecal -Standard Methods, 9222 D-1997 (MF) (Aqueous)
Bacteria -Coliform Fecal -IDEXX Colilert ®18 (MPN) (Aqueous)
Recommendation: Since the LIMS is not able to include greater-than signs with numerical
results, it is recommended that results that are greater than the reported value be qualified to
ensure clients are given the most accurate representation of the data.
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BOD -SM 5210 B-2001, Rev. 2011 (Aqueous)
CBOD -SM 5210 B-2001, Rev. 2011 (Aqueous)
Comment: The QC Summary Sheet states that results must be flagged if the Dissolved Oxygen
(DO) uptake is < 2 mg/L. This is not required if an undiluted (300 ml) sample is analyzed.
Recommendation: The first page of data packs states that 5, 20 and 30 ml of seed are used for
the seed controls. In the data reviewed, the laboratory used 4, 16 and 24 ml of seed. It is
recommended that the laboratory update the values on the first page of the data pack or add
"unless otherwise noted".
Recommendation: It is recommended that the laboratory reduce the lowest volume set for
effluent samples to 25 ml. The laboratory currently uses 50 ml, which may not always
demonstrate compliance with permit limits. No instances of this were noted in the data reviewed.
R.Finding: The laboratory uses only the lowest blank result to determine blank acceptance.
Requirement: It has been determined that multiple Dilution Water Blanks in the same
batch using the same dilution water are to be treated as replicates and averaged. The
average of the dilution water blanks in a batch must not be more than 0.20 mg/l. Ref:
"BOD Multiple Dilution Water Blanks", Standard Methods Joint Editorial Board
memorandum dated August 1, 2014.
S.Finding: Documentation does not demonstrate that the initial DO is measured within 30
minutes of sample preparation. This is considered pertinent data.
Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard
Methods, 521 O B-2001. (5) (g).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: If sample racks are put into the incubator at intervals not exceeding 30
minutes and those times are documented, adherence to this requirement would be
demonstrated.
T.Finding: Hydrogen peroxide is often present in one sample site and is not treated.
Requirement: Samples containing hydrogen peroxide -Hydrogen peroxide remaining in
samples from some industrial bleaching processes such as those used at paper mills and
textile plants can cause supersaturated oxygen levels in samples collected for BOD
testing. Mix such samples vigorously in open containers for sufficient time to allow the
hydrogen peroxide to dissipate before setting up BOD tests. Check adequacy of peroxide
removal by observing dissolved oxygen concentrations over time during mixing or by using
peroxide-specific test strips. Mixing times can vary from 1 to 2 h depending on the amount
of hydrogen peroxide present. The peroxide reaction can be considered complete when
the DO no longer increases during a 30-min period without mixing. Ref: Standard
Methods, 5210 B-2001. (4) (b) (5).
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Chromium Hexavalent-SW-846 Method 7196 A (Aqueous & Non-aqueous)
U.Finding: The laboratory is not analyzing the second source standard after every 15
samples.
Requirement: Verify calibration with an independently prepared check standard every 15
samples. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 7196 A, Rev. 1, July 1992, Section 8.4.
COD-Standard Methods, 5220 D-1997. Rev. 2011 (Aqueous)
Comment: The QC Summary Sheet states that the Method Blank must be less than the Method
Detection Limit (MDL). The laboratory may expand this acceptance criterion to less than or equal
to one half the reporting limit.
Recommendation: It is recommended that questions and information regarding low level
analyses (e.g., true value of standards) be added to the QC Summary Sheet.
Recommendation: The benchsheet documents the starting time of digestion and states that the
hot block turns off automatically after two hours. It is recommended that the laboratory verify the
timer at least annually.
Conductivity-EPA Method 120.1, Rev. 1982 (Aqueous)
Conductivity -SW-846 Method 9050 A (Aqueous)
V.Finding: The Automatic Temperature Compensator (ATC) check is not being properly
performed.
Requirement: The ATC must be verified prior to initial use and annually (i.e., 12 months)
thereafter at two temperatures by analyzing a standard or sample at 25 °C (i.e., the
temperature to which conductivity values are reported) and a temperature(s) that brackets
the temperature ranges of the environmental samples routinely analyzed. This may require
the analysis of a third temperature reading that is > 25 °C (see #3 below). The manner in
which the ATC is verified may depend upon the meter's capabilities and the
manufacturer's instructions. The following is one option.
1.Pour an adequate amount of conductivity standard or sample into a beaker or other
container and analyze at 25 °C. Document the temperature and conductivity value.
2.Lower the temperature of the standard or sample (e.g., by placing the container in a
refrigerator or ice chest) to less than the lowest anticipated sample temperature and
analyze. Document the temperature and conductivity value.
3.If samples greater than 25 °C are to be analyzed, perform the following additional step:
Raise the temperature above 25 °C to greater than the highest anticipated sample
temperature (e.g., by placing the container in a hot water bath) and analyze. Document
the temperature and conductivity value.
As the temperature increases or decreases, the value of the conductivity standard or
sample must be within ±10% of the true value of the standard or ±10% of the value of the
sample at 25 °C. If not, corrective action must be taken. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Specific Conductance (Conductivity).
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Comment: The laboratory only checks the temperature sensor at three temperatures.
The value of a standard or sample are not documented to demonstrate that the ATC is
functioning correctly.
W.Finding: The 10 µmhos/cm standard is not being properly prepared.
Requirement: Potassium Chloride (KCI) Conductivity standards may be purchased in
the ranges desired, or they may be prepared according to Table 251 O: I of Standard
Methods, 2510 A -1997. A portion of the standard should not be used for more than
one calibration. Discard any used standard portions. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Specific Conductance (Conductivity).
Requirement: Standard potassium chloride solution, KCI, 0.0100M: Dissolve 745.6 mg
anhydrous KCI in conductivity water and dilute to 1000 ml in a class A volumetric flask
at 25°C and store in a COrfree atmosphere. This is the standard reference solution,
which at 25 °C has a conductivity of 1412 µmhos/cm. Ref: Standard Methods, 2510 B-
1997. (3) (b) and Table 2510:1.
Comment: The laboratory prepares an intermediate standard by diluting 500 mg of
anhydrous KCI to 1 L that it considers 1000 µmhos/cm. 2.0 ml of the intermediate
solution is diluted to 200 ml to prepare the 10 µmhos/cm. However, since Conductivity
is not linear to the KCI concentration, the true value is not able to be determined by
applying a dilution factor equation.
Comment: Based on the SOP, it appears that other standards were also improperly
prepared in the past. However, the laboratory now purchases these standards (except
10 µmhos/cm) at the required concentrations.
Comment: The laboratory currently analyzes more standards than required. The
laboratory may discontinue analysis of the 10 µmhos/cm standard as acceptable
corrective action. If the laboratory chooses to continue analysis of a standard in this
range, it must be prepared per Table 2510:1 or purchased at the desired concentration.
Inorganic Phenols -SW-846 Method 9065 (Aqueous)
X.Finding: The laboratory is not analyzing the second source standard after every 15
samples.
Requirement: Verify calibration with an independently prepared check standard every 15
samples. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods; 3rd Edition, Method 9065, Rev. 0, September 1986, Section
8.5.
Cyanide-Standard Methods, 4500 CN-E-1999, Rev. 2011 (Total) (Aqueous)
Y.. Finding: The titer of the stock standard is not checked weekly.
Requirement: Check titer weekly because the solution gradually loses strength. Ref:
Standard Methods, 4500 CN-E-1999. (3) (b).
Comment: The laboratory checks the titer monthly.
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Mercury-EPA Method 245.1, Rev. 3.0, 1994 (Aqueous)
Z.Finding: The laboratory digests the calibration standards.
Requirement: Prepare calibration standards by transferring 0.5, 1.0, 2.0, 5.0, and 10 ml
aliquots of the 0.1 µg/ml CAL (Section 7.6) to a series of sample containers (Section
6.5.2). Dilute the standard aliquots to 100 ml with reagent water (Section 7.2) and process
as described in Sections 11.1.2, 11.1.3 (without heating), and 11.1.5. Ref: EPA Method
245.1, Rev. 3.0 (1994), Section 11.2.2.
Metals -EPA Method 200.7, Rev. 4.4, 1994 (Aqueous)
AA. Finding: Hydrochloric acid is being added to dissolved metals samples.
Requirement: For the determination of dissolved analytes in ground and surface waters,
pi pet an aliquot (.::20 ml) of the filtered, acid preserved sample into a 50 ml polypropylene
centrifuge tube. Add an appropriate volume of (1 +1) nitric acid to adjust the acid
concentration of the aliquot to approximate a 1 % (v/v) nitric acid solution (e.g., add 0.4 ml
(1+1) HN03 to a 20 ml aliquot of sample). Cap the tube and mix. The sample is now
ready for analysis (Section 1.3). Ref: EPA Method 200.7, Rev. 4.4 (1994), Section 11.1.1.
Metals -EPA Method 200.7, Rev. 4.4, 1994 (Aqueous)
Metals -EPA Method 200.8, Rev. 5.4, 1994 (Aqueous)
BB. Finding: The laboratory is not maintaining the proportionality of reagents when using a
reduced sample volume.
Requirement: For the determination of total recoverable analytes in aqueous samples
(other than drinking water with <1 NTU turbidity), transfer a 100 ml (±1 ml) aliquot from a
well mixed, acid preserved sample to a 250 ml Griffin beaker (Sections 1.2, 1.3, 1.6, 1.7,
1.8, and 1.9). (When necessary, smaller sample aliquot volumes may be used.) Ref: EPA
Method 200.7, Rev. 4.4 (1994), Section 11.2.2.
Requirement: Add 2 ml (1+1) nitric acid and 1.0 ml of (1+1) hydrochloric acid to the
beaker containing the measured volume of sample. Ref: EPA Method 200.7, Rev. 4.4
(1994), Section 11.2.3.
Requirement: For the determination of total recoverable analytes in aqueous samples
(other than drinking water with <1 NTU turbidity), transfer a 100 ml (±1 ml) aliquot from a
well mixed, acid preserved sample to a 250 ml Griffin beaker (Sections 1.2, 1.3, 1.7, and
1.8). (When necessary, smaller sample aliquot volumes may be used.) Ref: EPA Method
200.8, Rev. 5.4 (1994), Section 11.2.2.
Requirement: Add 2 ml (1 +1) nitric acid and 1.0 ml of (1 +1) hydrochloric acid to the
beaker containing the measured volume of sample. Ref: EPA Method 200.8, Rev. 5.4
(1994), Section 11.2.3.
Comment: The laboratory uses 0.3 ml of concentrated nitric acid for 15 ml of sample.
Since this is concentrated, rather than 1: 1, the laboratory must use 0.15 ml. Or the
laboratory could use 0.3 ml of (1:1) nitric acid.
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Metals -SW-846 Method 6010 D (Aqueous)
CC.Finding: The laboratory is not using the proper volume of nitric acid for digestion.
Requirement: Transfer a 100-ml representative aliquot of the well-mixed sample to a
150-ml Griffin beaker and add 3 ml of concentrated HN03. Cover the beaker with a
ribbed watch glass or equivalent. Place the beaker on a hot plate or equivalent heating
source and cautiously evaporate to a low volume (5 ml), making certain that the sample
does not boil and that no portion of the bottom of the beaker is allowed to go dry. Cool the
beaker and add another 3-ml portion of concentrated HN03. Cover the beaker with a
nonribbed watch glass and return to the hot plate. Increase the temperature of the hot
plate so that a gentle reflux action occurs. Ref: EPA SW-846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3010 A. Rev. 1, July 1992,
Section 7 .1 .
Comment: The laboratory adds 0.3 ml of concentrated nitric acid to 15 ml of sample for
digestion. In order to meet the method requirements, the laboratory must add two 0.45 ml
volumes of nitric acid at the specified steps of the digestion for a total of 0.9 ml.
Metals -SW-846 Method 6010 D (Non-aqueous)
DD. Finding: The laboratory is not digesting samples properly.
Requirement: For the digestion of samples for analysis by GFAA or ICP-MS, add 10 ml
of 1: 1 HN03, mix the slurry, and cover with a watch glass or vapor recovery device. Heat
the sample to 95 °C ± 5°C and reflux for 10 to 15 minutes without boiling. Allow the sample
to cool, add 5 ml of concentrated HN03, replace the cover, and reflux for 30 minutes. If
brown fumes are generated, indicating oxidation of the sample by HN03, repeat this step
(addition of 5 ml of cone. HN03) over and over until no brown fumes are given off by the
sample indicating the complete reaction with HN03. Using a ribbed watch glass or vapor
recovery system, either allow the solution to evaporate to approximately 5 ml without
boiling or heat at 95 °C ± 5 °C without boiling for two hours. Maintain a covering of solution
over the bottom of the vessel at all times. Ref: EPA SW-846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3050 B. Rev. 2, December
1996, Section 7 .2.
Requirement: After the step in Section 7.2 has been completed and the sample has
cooled, add 2 ml of water and 3 ml of 30% H202. Cover the vessel with a watch glass or
vapor recovery device and return the covered vessel to the heat source for warming and to
start the peroxide reaction. Care must be taken to ensure that losses do not occur due to
excessively vigorous effervescence. Heat until effervescence subsides and cool the
vessel. Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3 rd Edition, Method 3050 B. Rev. 2, December 1996, Section 7.2.1.
Requirement: Continue to add 30% H202 in 1-ml aliquots with warming until the
effervescence is minimal or until the general sample appearance is unchanged. NOTE: Do
not add more than a total of 10 ml 30% H202. Ref: EPA SW-846 Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 3050 B. Rev.
2, December 1996, Section 7.2.2.
Requirement: Cover the sample with a ribbed watch glass or vapor recovery device and
continue heating the acid-peroxide digestate until the volume has been reduced to
approximately 5 ml or heat at 95°C ± 5°C without boiling for two hours. Maintain a
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covering of solution over the bottom of the vessel at all times. Ref: EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method
3050 B. Rev. 2, December 1996, Section 7.2.3.
Requirement: For the analysis of samples for FLAA or ICP-AES, add 10 ml cone. HCI to
the sample digest from 7.2.3 and cover with a watch glass or vapor recovery device. Place
the sample on/in the heating source and reflux at 95 °C ± 5°C for 15 minutes. Ref: EPA
SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd
Edition, Method 3050 B. Rev. 2, December 1996, Section 7.3.
Comment: The laboratory uses 0.5-1.0 g of sample (half of the amount in the method, so
all other reagents must be halved as well). 5.0 ml of deionized water, 1.0 ml of
concentrated HNQ3 and 2.5 ml of concentrated HCI are added and the sample is digested
at 90-95 °C for 30 minutes. After cooling, 3.0 ml of 30% H202 is added and the sample is
digested for another 30 minutes.
Nitrogen, Total Kjeldahl -EPA 351.2, Rev. 2.0, 1993 (Aqueous)
Comment: The table on the benchsheet lists the low-level curve verification standard as 20 mg/l.
This needs to be corrected to 5 mg/l to accurately reflect the laboratory's current practice.
Recommendation: Per EPA Method 351.2, Section 10.7, it is recommended that the laboratory
reanalyze the second source standard as a continuing calibration check.
Phosphate, Ortho -Standard Methods, 4500 P E-1999, Rev. 2011 (Aqueous)
Comment: The benchsheet column used to record the percent recovery of the Initial Calibration
Verification (ICV) and Continuing Calibration Verification (CCV) standards does not have a
column heading identifying what the results represent.
EE. Finding: The laboratory does not use six standards for calibration.
Requirement: Prepare individual calibration curves from a series of six standards within
the phosphate ranges indicated in 4500 P C.1 c. Ref: Standard Methods, 4500 P E-1999.
(4)(c).
Comment: The laboratory uses five standards for calibration.
Phosphorus, Total -EPA Method 365.1, Rev. 2.0, 1993 (Aqueous)
Recommendation: The digestion log lists the Continuing Calibration Blank (CCB) and CCV
standard after every ten samples and at the end of the sample set, indicating that each one is
digested separately. However, the laboratory only digests one of each per sample set. It is
recommended that the CCB and CCV only be listed once on the digestion log to more accurately
reflect current practices.
FF. Finding: The calibration standards are not digested properly.
Requirement: Prepare a series of at least three standards, covering the desired range,
and a blank by pipetting and diluting suitable volumes of working standard solutions
(Section 7.12 or 7.13) into 100 ml volumetric flasks. Ref: EPA Method 365.1, Rev. 2.0
(1993), Section 10.1.
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Requirement: Process standards and blanks as described in Section 11.0. Ref: EPA
Method 365.1, Rev. 2.0 (1993), Section 10.2.
Comment: The laboratory digests the working standard and then makes dilutions of
that for the calibration standards.
Residue, Total -Standard Methods, 2540 B-1997, Rev. 2011 (Aqueous)
Residue, Dissolved -Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous)
Residue, Suspended -Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous)
GG. Finding: The laboratory is not consistently drying samples for at least one hour for the
second drying time to verify constant weight.
Requirement: Dry evaporated sample for at least 1 h in an oven at 103 to 105 °C, cool
dish in desiccator to balance temperature, and weigh. Repeat cycle of drying, cooling,
desiccating, and weighing until a constant weight is obtained, or until weight change is less
than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 B-
1997. (3) (b).
Requirement: Dry evaporated sample for at least 1 h in an oven at 180 ± 2 °C, cool in a
desiccator to balance temperature, and weigh. Repeat cycle of drying, cooling,
desiccating, and weighing until a constant weight is obtained, or until weight change is less
than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 C-
1997. (3) (d).
Requirement: Dry for at least 1 h in an oven at 103 to 105 °C, cool dish in desiccator to
balance temperature, and weigh. Repeat cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained, or until weight change is less than 4% of
previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 D-1997. (3)
(c).
HH. Finding: The laboratory uses automatic pipets that are not wide-bore for small sample
volumes.
Requirement: Apparatus: Wide-bore pipets. Ref: Standard Methods, 2540 B-1997. (2)
(h).
Requirement: Apparatus listed in 2540B.2a-h is required. Ref: Standard Methods, 2540
C-1997. (2).
Requirement: Apparatus listed in 2540B.2 and C.2 is required. Ref: Standard Methods,
2540 D-1997. (2).
Residue, Settleable -Standard Methods, 2540 F-1997, Rev. 2011 (Aqueous)
II.Finding: There was no result documented on the benchsheet for the sample analyzed on
March 15, 2017.
Requirement: All laboratories must use printed laboratory bench worksheets that
include a space to enter the signature or initials of the analyst, date of analyses, sample
identification, volume of sample analyzed, value from the measurement system, factor
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IV.
and final value to be reported and each item must be recorded each time $amples are
analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).
JJ. Finding: The sample volumes for all samples were not documented on March 29, 2017.
Requirement: All laboratories must use printed laboratory bench worksheets that include
a space to enter the signature or initials of the analyst, date of analyses, sample
identification, volume of sample analyzed, value from the measurement system, factor and
final value to be reported and each item must be recorded each time samples are
analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).
KK. Finding: The laboratory does not always analyze one liter of sample.
Requirement: Collect a minimum of 1 liter of sample. Pour exactly 1 liter of well mixed
sample into the Imhoff Cone. Ref: NC WW/GW LC Approved Procedure for the Analysis
of Settleable Solids.
Comment: The laboratory often receives less than one liter and also performs duplicate
analyses without collecting two liters. The sample result and reporting limit are adjusted
based on the volume analyzed.
Comment: Duplicate analyses are not required.
Comment: Settleable Residue is considered a method-defined parameter per the
definition in the Code of Federal Regulations, Part 136.6, Section (a) (5). This means that
the method may not be modified to reduce the sample volume per Section (b) (3).
TCLP Metals -SW-846 1311 (Non-Aqueous)
LL.Finding: An inconsistency was noted between the SOP and laboratory practice as follows:
the laboratory occasionally uses less than 100 g of sample, but Section 12.5.1 of the SOP
requires 100 g. This was noted for samples 92337724001 and 92337724002.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Comment: TCLP is considered a method-defined parameter per the definition in the Code
of Federal Regulations, Part 136.6, Section (a) (5). This means that the method may not
be modified to reduce the sample volume per Section (b) (3).
Turbidity-EPA Method 180.1, Rev. 2.0, 1993 (Aqueous)
Comment: The laboratory is reminded that NC WW/GW LC policy is to avoid dilutions whenever
possible in order to insure consistency among laboratories. Samples need only be diluted if their
concentration falls outside the allowable calibration range of the meter.
PAPER TRAIL INVESTIGATION:
No paper trail performed.
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V.CONCLUSIONS:
Correcting the above-cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like
to thank the staff for their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation and implementation
dates for each corrective action.
Report prepared by: Jason Smith
Report reviewed by: Anna Ostendorff
Date: June 16, 2017
Date: June 27, 2017
North Carolina Wastewater/Groundwater Laboratory Certification
Matrix Spiking Policy and Technical Assistance (05/11/2012)
Policy Statement
Unless the referenced method states a greater frequency, spike 5% of samples on a monthly basis.
Laboratories analyzing less than 20 samples per month must analyze at least one matrix spike (MS) each
month samples are analyzed. If MS results are out of control, the results must be qualified or the
laboratory must take corrective action to rectify the effect, use another method, or employ the method of
standard additions. When the method of choice specifies MS performance acceptance criteria for
accuracy, and the laboratory chooses to develop statistically valid, laboratory-specific limits, the
laboratory-generated limits cannot be less stringent than the criteria stated in the approved method.
When spiking with multi-component standards, if the method does not specify the spiking components,
the Laboratory Control Spike (LCS) and MS must contain all analytes that are reported.
If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and
the MS prepared using the diluted sample. The recovery of the MS samples must be bracketed by the
calibration range.
The volume of spike solution used in MS preparation must in all cases be :,; 10% of the total MS volume. It
is preferable that the spike solution constitutes :,; 1 % of the total MS volume so that the MS can be
considered a whole volume sample with no adjustmen.t (i.e., volume correction) by calculation necessary.
If the spike solution volume constitutes >1 % of the total sample volume, the sample concentration or spike
concentration must be adjusted by calculation.
Technical Assistance
Spike Preparation
The spike concentration may be set at either 5 to 50 times the Method Detection Limit (as determined by
the Method Detection Limit or MDL study) for the analyte, or at 1 to 10 times the ambient level (average
concentration) of the analyte in samples. There are several options for preparing spikes, for example:
Option 1 (Recommended -easiest) -If the spike solution volume is equal to 1 % or less of the
total sample volume, direct subtraction of the unspiked sample is allowed. When the volume of
the standard solution spiked into a sample or a sample extract is less than 1 % of the total volume
then the final concentration need not be adjusted (e.g., 10 µL of spike solution added to a 1 ml
final extract results in only a negligible 1 % change in the final extract volume).
Option 2 -Adjust spike solution to a known volume with sample. In this case the sample
concentration must be adjusted. When the volume of spike solution exceeds 1 % of the total MS
volume the sample concentration must be adjusted prior to determining spike recovery.
The general equation for spike recovery is as follows:
% R = amt. of target in spiked sample -amt. of target in unspiked sample
(cone. or mass) (cone. or mass) x 100
amt. of target spiked into the sample
( cone. or mass)
To apply this to the sample preparation schemes described above, refer to the following exa.mples.
Spike Preparation Examples
Option 1 -If the spike solution volume is equal to 1 % or less of the total sample volume, direct subtraction
of the unspiked sample is allowed.
Option 1 Example:
0.5 mis of a 1000 mg/L standard spike added to 100 mis of sample has a theoretical value of 5
mg/L.
(A)The spiked sample recovery is 5.1 mg/L
(B)If the unspiked sample result is 0.5 mg/L
(C)Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) -unspiked sample result (B) divided by
theoretical value (C) X 100 or
5.1 -0.5 X 100 = 92% recovery
5.0
A - B X 100 = Percent recovery
C
Option 2 -Adjust spike solution to a known volume with sample. In this case the sample concentration
must be adjusted.
Option 2 Example 1:
10 mis of spike (concentration 50 mg/L) brought to 100 mis with sample the theoretical MS value is
5 mg/L.
(A)The spiked sample recovery is 5.1
(B)If the unspiked sample result is 0.5 mg/L
(C)% sample is 0.90 (sample volume used (90) divided by final volume (100))
(D)Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) -(unspiked sample result (B) x % sample
(C)) divided by theoretical value (D) X 100 or
5.1 -(0.5 x 0.9) X 100 = 93% recovery
5.0
Option 2 Example 2: Larger spike volume
A - (B x C) X 100 = Percent recovery
D
25 mis of spike (concentration 50 mg/L) brought to 250 mis with sample the theoretical MS value
is 5 mg/L.
(A)The spiked sample recovery is 5.6
(B)If the unspiked sample result is 0.5 mg/L
(C)% sample is 0.90 (sample volume used (225) divided by final volume (250))
(D)Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) -(unspiked sample result (B) x % sample
(C)) divided by theoretical value (D) X 100 or
5.6 -(0.5 x 0.9) X 100 = 103% recovery
5.0
Corrective Action/Qualifications for MS
A -(B x C) X 100 = Percent recovery
D
Spike accuracy is usually based on a range of percent recovery (e.g., 80-120%). Refer to the method of
choice for specific acceptance criteria for the matrix spikes until the laboratory develops or adopts
statistically valid, laboratory-specific performance criteria for accuracy. If a MS fails, and the LCS is
acceptable, qualify the data for the MS sample. Repeated failures for a specific matrix may require use of
an alternate method or method of standard addition. Base the sample batch acceptance on the results of
the LCS analyses (and other quality control results) rather than the MS alone, because the matrix of the
spiked sample may interfere with the method performance. If a MS and the associated LCS fail, re­
prepare and reanalyze affected samples.
Post Digestion Spikes (PDS)
Post Digestion Spikes (PDS) are used for some analyses (e.g., metals) to assess the ability of a method
to successfully recover target analytes from an actual sample matrix after the digestion process has been
performed. The PDS results are used with MS results to evaluate matrix interferences. The MS and PDS
should be prepared from the same environmental sample. A PDS is not to be analyzed in place of a MS.
Post Digestion Spikes must be reported as post-digested and must not be misrepresented as pre­
digested spikes. (Exception: TCLP and SPLP samples are always spiked post digestion.)
Corrective Action/Qualifications for Post Digestion Spikes
In general, if the MS recovery for an analyte does not fall within the quality control acceptance range but
the PDS recovery is acceptable, then a matrix affect (associated with the preparatory process) should be
suspected and the unspiked sample results must be qualified on the basis of the matrix spike recovery.
However, when historical data for the effect does not exist, the laboratory would normally be expected to
perform a second digestion and reanalysis of the MS to confirm the result. The result would be confirmed
if the MS recoveries and PDS recoveries for both sets of analyses were similar in magnitude and bias.
When both the MS recovery and PDS recovery for a particular analyte falls outside of quality control
acceptance range in the same manner (i.e., the PDS and MS failures are of similar magnitude and the
direction of bias is the same), confirmatory analyses are unnecessary but the data must be qualified.
Parameters Excluded from MS Requirements
Acidity
BOD/CBOD
Chlorophyll
Color-ADMI
Conductivity
lgnitability
Paint Filter Test
pH
Salinity
Total Residual Chlorine
Alkalinity
Aquatic Humic Substances
All Bacteriological Parameters
Color -PtCo
Dissolved Oxygen
All Residues
Turbidity
Temperature
Sulfite
Vector Attraction Reduction (All Options)
(Field Laboratories and Field Setting analyses are exempt.)