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NC Department of Environmental Quality | Division of Water Resources | Laboratory Certification Branch
4405 Reedy Creek Road | 1623 Mail Service Center | Raleigh, North Carolina 27699-1623
919-733-3908
December 7, 2023
5691
Mr. Mark Powers
Associated Asphalt Greensboro LLC
100 S. Chimney Rock Rd
Greensboro, NC 27409
Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC
WW/GW LCB) Maintenance Inspection
Dear Mr. Powers:
Enclosed is a report for the inspection performed on November 7, 2023 by Michael Cumbus.
Where Finding(s) are cited in this report, a response is required. Within thirty days, 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 02H .0800.
A copy of the laboratory’s Certified Parameter List at the time of the audit is attached. This list will
not 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 have questions or need additional information, please contact me at (919) 733-
3908 Ext. 259.
Sincerely,
Beth Swanson
Technical Assistance & Compliance Specialist
Division of Water Resources
Attachment
cc: Todd Crawford, Michael Cumbus, #5691
On-Site Inspection Report
LABORATORY NAME: Associated Asphalt Greensboro LLC
NPDES PERMIT #: NC0074241
ADDRESS: 100 S. Chimney Rock Rd.
Greensboro, NC 27409
CERTIFICATE #: 5691
DATE OF INSPECTION: November 7, 2023
TYPE OF INSPECTION: Field Industrial Initial
AUDITOR: Michael Cumbus
LOCAL PERSON CONTACTED:
Mark Powers
I. INTRODUCTION:
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater Laboratory
Certification Branch (NC WW/GW LCB) to verify its compliance with the requirements of 15A NCAC 02H
.0800 for the analysis of compliance monitoring samples.
II. GENERAL COMMENTS:
The facility is neat and well organized and has all the equipment necessary to perform the analyses. The
analyst was very forthcoming and responded well to suggestions from the auditor.
All required Proficiency Testing (PT) Samples have been analyzed for the 2023 PT Calendar Year and the
graded results were 100% acceptable.
Any time changes are made to laboratory procedures, Quality Assurance (QA) and/or Standard Operating
Procedure (SOP) document(s) must be updated and relevant staff retrained. Staff must acknowledge that
they have read and understand the changes as part of the documented training program. The same
requirements apply when changes are made in response to Findings, Recommendations or Comments
listed in this report, to ensure the methods are being performed as stated, references to methods are
accurate, and the QA and SOP documents are 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. Revisions to the SOPs, based on the Findings, Comments and Recommendations
within this report must be submitted to this office by February 29, 2024.
The laboratory is reminded that SOPs are required to be reviewed at least every two years and are intended
to describe procedures exactly as they are to be performed. Use of the word “should” is not appropriate when
describing requirements (e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs
for the proper use of the word “should”.
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Contracted analyses are performed by Meritech, Inc. (Certification #165).
Approved Procedure documents for the analysis of the facility’s currently certified Field Parameters were
provided at the time of the inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Recommendation: Current laboratory practice is to record the pH result on the chain of custody sent
to the contract laboratory first and then transfer the result to the benchsheet. It is recommended that
the laboratory record the analytical results solely on the laboratory benchsheet in order to facilitate
data retrieval and review. It would also reduce the possibility of transcription errors.
A. Finding: Error corrections are not properly performed.
Requirement: All documentation errors shall be corrected by drawing a single line through
the error so that the original entry remains legible. Entries shall not be obliterated by erasures
or markings. Wite-Out®, correction tape, or similar products designed to obliterate
documentation are not to be used; instead the correction shall be written adjacent to the error.
The correction shall be initialed by the responsible individual and the date of change
documented. Ref: 15A NCAC 02H .0805 (g) (1).
Comment: Several instances were noted where original entries were over-written and lacked
the date of change and the initials of the responsible party.
B. Finding: The laboratory lacks a documented training program.
Requirement: Each laboratory shall develop and implement a documented training program
that includes the following: that staff have the education, training, experience, or demonstrated
skills needed to generate quality control results within method-specified limits and that meet
the requirements of these Rules; that staff have read the laboratory quality assurance manual
or applicable Standard Operating Procedures; that staff have obtained acceptable results on
Proficiency Testing Samples pursuant to Rule .0803(1) of this Section or other demonstrations
of proficiency (e.g., side-by-side comparison with a trained analyst, acceptable results on a
single-blind performance evaluation sample, an initial demonstration of capability study
prescribed by the reference method). Ref: 15A NCAC 02H .0805 (g) (5).
Comment: The laboratory’s training program may be outlined in each of the applicable
parameter SOPs. The NC WW/GW LCB SOP Templates include an Employee Training
section.
C. Finding: Chemical containers are not dated when received and when opened.
Requirement: Chemical containers shall be dated when received and when opened. Ref:
15A NCAC 02H .0805 (g) (7).
Comment: This Finding applies to the pH electrode storage solution and the pH buffers.
D. Finding: The laboratory benchsheet is lacking required documentation: the method or
Standard Operating Procedure reference; the laboratory identification; the instrument
identification; the signature or initials of the analyst; the time of sample analyses; sample
identification and the proper units of measure.
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Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the method or Standard
Operating Procedure; the laboratory identification; the instrument identification; the signature
or initials of the analyst; the time of sample analyses (when required to document a required
holding time or when time-critical steps are imposed by the method, a federal regulation, or
this Rule); sample identification; the proper units of measure. Each item shall be recorded
each time samples are analyzed. Analyses shall conform to methodologies found in
Subparagraph (a)(1) of this Rule. Ref: 15A NCAC 02H .0805 (g) (2) (A), (B), (C), (E), (H), (I)
and (L).
Comment: Since the sample collector and the analyst are the same person, the laboratory
may include a blanket statement to this effect on the benchsheet.
E. Finding: QC results for pH are not being documented to demonstrate the analytical process
is in control and the established acceptance criteria are met.
Requirement: All laboratories shall use printable laboratory benchsheets. Certified Data shall
be traceable to the associated sample analyses and shall consist of: the quality control
assessments. Ref: 15A NCAC 02H .0805 (g) (2) (O).
Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).
Requirement: All check standard buffers must read within ±0.1 S.U. to be acceptable. If the
meter verification does not read within ±0.1 S.U., corrective actions must be taken before any
samples are analyzed. Ref: NC WW/GW LCB Approved Procedure for the Analysis of pH.
Comment: The laboratory is analyzing the 4.0 S.U. and 10.0 S.U. buffers as calibration
checks but is neither documenting the results nor evaluating them against the acceptance
criteria. An example benchsheet was provided to the analyst after the audit.
F. Finding: The laboratory benchsheet is lacking required documentation: meter calibration
time.
Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).
Requirement: The following must be documented in indelible ink whenever sample analysis
is performed: Meter calibration and meter calibration time. Ref: NC WW/GW LCB Approved
Procedure for the Analysis of pH.
Proficiency Testing
G. Finding: The laboratory is lacking a documented plan for PT procedures.
Requirement: Each laboratory shall develop documentation outlining the analytical quality
control practices used for the Parameter Methods included in its Certification, including
Standard Operating Procedures for each certified Parameter Method. Quality assurance,
quality control, and Standard Operating Procedure documentation shall indicate the effective
date of the document and be reviewed every two years and updated if changes in procedures
are made. Each laboratory shall have a formal process to track and document review dates
and any revisions made in all quality assurance, quality control, and Standard Operating
Procedure documents. Supporting Records shall be maintained as evidence that these
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practices are implemented. The quality assurance, quality control, and Standard Operating
Procedure documents shall be available for inspection by the State Laboratory. Ref: 15A
NCAC 02H .0805 (a) (7).
Requirement: Laboratories must have a documented plan [this is usually detailed in the
laboratory’s Quality Assurance Manual or may be a separate Standard Operating Procedure
(SOP)] of how they intend to cover the applicable program requirements for Proficiency
Testing per their scope of accreditation. This plan shall cover any commercially available PT
Samples and any inter-laboratory organized studies, as applicable. The plan must also
address the laboratory’s process for submission of PT Sample results and related Corrective
Action Reports (CARs). Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6,
Section 3.0.
Comment: The laboratory’s PT procedure may be outlined in each of the applicable
parameter SOPs. The NC WW/GW LCB SOP Templates include a section for the PT
procedure.
H. Finding: The laboratory is not documenting PT Sample analyses in the same manner as
routine Compliance Samples.
Requirement: All PT Sample analyses must be recorded in the same daily analysis records
(e.g., benchsheets) as for any Compliance Sample. This serves as the permanent laboratory
record. Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6, Section 3.6.
Requirement: The laboratory shall retain all records necessary to facilitate historical
reconstruction of the analysis and reporting of analytical results for PT Samples. This means
the laboratory must have available and retain for five years [pursuant to 15A NCAC 02H .0805
(a) (7) (E) and (g) (1)] all of the raw data, including benchsheets, instrument printouts and
calibration data, for all PT Sample analyses and the associated QC analyses conducted by
all Parameter Methods. Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6,
Section 4.0.
Comment: The laboratory currently documents the results of the PT analyses on the
instruction sheet that accompanies the PT Samples, rather than on the regular benchsheet.
I. Finding: Additional QC beyond what is routine for Compliance Samples is being analyzed
with PT Samples.
Requirement: Laboratories are required to analyze an appropriate PT Sample by each
Parameter Method and in each associated matrix on the laboratory’s CPL. The same PT
Sample may be analyzed by one or more methods. Laboratories shall conduct the analyses
in accordance with their routine testing, calibration and reporting procedures, unless otherwise
specified in the instructions supplied by the Accredited PT Sample 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, preparatory techniques (e.g., digestions, distillations and extractions) and
the same quality control acceptance criteria. PT Samples shall not be analyzed with additional
quality control. They are not to be replicated beyond what is routine for Compliance Sample
analysis. Although, it may be routine to spike Compliance Samples, it is neither required, nor
recommended, for PT Samples. PT sample results from multiple analyses (when this is the
routine procedure) must be calculated in the same manner as routine Compliance Samples.
Ref: Proficiency Testing Requirements, January 1, 2023, Revision 6, Section 3.6.
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Comment: The laboratory receives multiple bottles of the pH PT Sample and analyzes each
bottle. Results from the multiple analyses are then averaged. The analyst was informed that
since pH results are logarithmic, results cannot be averaged. The analyst was also informed
that since compliance samples are not analyzed multiple times, the PT Sample must be
analyzed only a single time.
Recommendation: It is recommended that the laboratory review their PT ordering policy and
order only one bottle of the PT Sample.
Quality Assurance/ Quality Control
J. Finding: The laboratory is not monitoring the temperature of the refrigerator where samples
are stored until relinquished to the contract laboratory.
Requirement: All analytical data and records pertinent to each certified analysis shall be
available for inspection upon request. Ref: 15A NCAC 02H .0805 (g) (1).
Requirement: Cool, ≤6 °C. Ref: Code of Federal Regulations, Title 40, Part 136; Federal
Register Vol. 86, No. 95, May 19, 2021; Table II.
Comment: The contract laboratory provides empty coolers for sample transportation and
storage. Samples are stored in the proper containers, and the sample bottles placed in the
cooler, which is then placed in the breakroom refrigerator until the courier arrives with ice. This
refrigerator is not monitored for temperature. Staff noted that the break room refrigerator
where the cooler is stored has an ice maker and suggested that they could supply the ice for
thermal preservation rather than waiting for the courier to provide the ice prior to sample
transportation.
Recommendation: Since the insulated cooler will prevent the refrigerator from cooling the
samples and meeting the thermal preservation requirements, it is recommended that the
laboratory add ice to the cooler rather than store the sample cooler in the break room
refrigerator.
pH – Standard Methods, 4500 H+ B-2011 (Aqueous)
Comment: Prior to August 2023, the laboratory was not calibrating the pH meter prior to compliance
sample analyses each day that sample analysis was performed. With the purchase of a new pH meter
in August 2023, calibration is now being performed at the required frequency.
K. Finding: Samples are not being stirred during analysis.
Requirement: Establish equilibrium between electrodes and sample by stirring sample to
ensure homogeneity; stir gently to minimize carbon dioxide entrainment. Ref: Standard
Methods, 4500 H+ B-2011. (4) (b).
L. Finding: The pH meter is not being calibrated with at least two buffers.
Requirement: Laboratory procedures shall comply with Subparagraph (a)(1) of this Rule. Ref:
15A NCAC 02H .0805 (g) (4).
Requirement: Instruments are to be calibrated according to the manufacturer’s calibration
procedure prior to analysis of samples each day compliance monitoring is performed.
Calibration must include at least two buffers. The meter calibration must be verified with a third
standard buffer solution (i.e., check buffer) prior to sample analysis. The calibration and check
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standard buffers must bracket the range of the samples being analyzed. Ref: NC WW/GW
LCB Approved Procedure for the Analysis of pH.
Comment: The laboratory’s current procedure is to perform a single point calibration using
the 7.0 S.U. buffer, per the manufacturer’s instructions. The manufacturer noted upon inquiry
that the pH meter, Fristaden Lab PHS-3C, has the capability for multi-point calibration. In an
email dated November 13, 2023, the auditor informed the lab of this capability and the
requirement to calibrate with a minimum of two buffers.
M. Finding: Values were reported that exceed the method specified accuracy of 0.1 units.
Requirement: By careful use of a laboratory pH meter with good electrodes, a precision of
±0.02 unit and an accuracy of ±0.05 unit can be achieved. However, ± 0.1 pH unit represents
the limit of accuracy under normal conditions, especially for measurement of water and poorly
buffered solutions. For this reason, report pH values to the nearest 0.1 pH unit. Ref: Standard
Methods, 4500 H+ B-2011. (6).
Comment: Per PT Vendor instructions, the PT Sample results should be reported to two
decimal places, which is an exception to the requirement for Compliance Samples.
Recommendation: The laboratory currently reports pH sample results to two decimal places.
It is recommended that the laboratory continue to measure and document sample results on
the benchsheet to two decimal places, and to round to the nearest 0.1 S.U. when reporting
results on the DMR.
IV. 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, implementation dates and steps taken to prevent recurrence
for each corrective action.
Report prepared by: Michael Cumbus Date: November 16, 2023
Report reviewed by: Tom Halvosa Date: November 28, 2023
Certificate Number:5691
Effective Date:1/1/2023
Expiration Date:12/31/2023
Lab Name:Associated Asphalt Greensboro LLC
Address:100 S. Chimney Rock Rd
Greensboro, NC 27409
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:
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.
CERTIFIED PARAMETERS
INORGANIC
pH
SM 4500 H+B-2011 (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.