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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 6, 2023
267
Ms. Stefania Marroquin
Town of Apex Middle Creek WWTP Laboratory
P.O. Box 250
Apex, NC 27539
Subject: North Carolina Wastewater/Groundwater Laboratory Certification Branch (NC
WW/GW LCB) Maintenance Inspection
Dear Ms. Marroquin:
Enclosed is a report for the inspection performed on November 2, 2023 by Tom Halvosa and Jill
Puff. 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, Tom Halvosa, #267
On-Site Inspection Report
LABORATORY NAME: Town of Apex Middle Creek WWTP Laboratory
NPDES PERMIT #: NC0064050
ADDRESS: 300 Pristine Waters Dr.
Apex, NC 27502
CERTIFICATE #: 267
DATE OF INSPECTION: November 2, 2023
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Tom Halvosa and Jill Puff
LOCAL PERSON(S) CONTACTED:
Stefania Marroquin and Tony Giles
I. INTRODUCTION:
This laboratory was inspected by representatives 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. Staff
were 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/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. Revisions to the SOPs, based on the Findings, Comments and Recommendations
within this report must be submitted to this office by March 31, 2024.
The laboratory is 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 (e.g., Quality Control
(QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper use of the word “should”.
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#267 Town of Apex Middle Creek WWTP Laboratory
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.
Contracted analyses are performed by Waypoint Analytical - Greenville (Certification #10).
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: It is recommended that the laboratory add their name to the sample receipt log
and standards and reagents prep log.
A. Finding: The laboratory is not documenting the salinity value used to calibrate the Dissolved
Oxygen (DO) meter.
Requirement: All analytical records, including original observations and information
necessary to facilitate historical reconstruction of the calculated results, shall be maintained
for five years. Ref: 15A NCAC 02H .0805 (a) (7) (E).
Requirement: Determination of Initial DO: Use the Azide modification of the iodometric
method (Section 4500-O.C), membrane-electrode method (Section 4500-O.G), or optical-
probe method (Section 4500-O.H) to determine initial DO on all sample dilutions, dilution water
blanks, and, where appropriate, seed controls. Ref: Standard Methods, 5210 B-2016. (5) (g).
Requirement: Calibrate probe in accordance with manufacturer's instructions to obtain the
guaranteed precision and accuracy. Ref: Standard Methods, 4500 O H-2016. (4).
Requirement: The State Laboratory may develop Approved Procedures for Field Parameters
based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this
Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F).
Requirement: The following must be documented in indelible ink whenever sample analysis
is performed: Calibration variables (temperature, elevation or barometric pressure [in mmHg],
and salinity). Ref: NC WW/GW LCB Approved Procedure for the Analysis of Dissolved
Oxygen (DO).
Comment: This finding applies to both the DO and BOD parameter methods. A revision to
your SOP indicating that the salinity of the samples is ≤ 9 ppt and so the default concentration
of 0 ppt is used along with a blanket statement on the benchsheet that salinity is programmed
as 0 ppt would be sufficient.
Quality Assurance/Quality Control
B. Finding: Thermometers in the BOD and fecal coliform incubators are not verified against a
Reference Temperature-Measuring Device (TMD) at least every three months.
Requirement: Digital temperature-measuring devices and temperature-measuring devices
used in incubators shall be verified at the temperature of use every three months against a
Reference Temperature-Measuring Device and their accuracy shall be corrected. Ref: 15A
NCAC 02H .0805 (a) (7) (N) (iii).
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#267 Town of Apex Middle Creek WWTP Laboratory
Comment: The temperatures were verified once each quarter, but some were more than
three months apart.
C. Finding: For chemicals/reagents/consumables that do not have an expiration date, the
laboratory has not established a policy for assigning expiration dates.
Requirement: When commercially prepared chemicals, reagents, standards and
consumables have expiration dates listed as a month and year (with no specific day of the
month), the last day of the month will be considered the actual date of expiration. If no
expiration date is given by the manufacturer, the laboratory must use their policy for assigning
one. If the laboratory is unable to determine an expiration date for a chemical, reagent or
standard a one-year time period from the date of receipt shall be the expiration date unless
degradation is observed prior to this date. If neither a date received nor an expiration date can
be determined, the item must not be used. If the method does not specify an expiration date,
chemicals, reagents and standards prepared in the laboratory for use with that method must
be assigned an expiration date according to the laboratory’s policy for doing so. Monitor
materials for changes in appearance or consistency. Any changes may indicate potential
contamination or degradation, and therefore, the item must not be used, even if the
manufacturer’s or laboratory’s expiration date has not been exceeded. Laboratory-assigned
expiration dates may be re-evaluated based on performance and recovery data and new
expiration dates assigned at that time. Manufacturer-assigned expiration dates may not be
extended. Ref: NC WW/GW LCB Chemical, Reagent, Standard and Consumables Expiration
Date Policy (04/21/2022).
Comment: The sulfuric acid bottle did not have an expiration date.
BOD – Standard Methods, 5210 B-2016 (Aqueous)
Recommendation: The laboratory’s SOP states, “Samples not analyzed within 2 hours of collection
are stored at ≤ 6°C”. It is recommended that the laboratory change this language to “If samples are
not thermally preserved at ≤ 6°C within 15 minutes after collection, they must be analyzed within two
hours”.
Dissolved Oxygen – Hach 10360-2011, Rev. 1.2 (Aqueous)
Comment: The laboratory is calculating the theoretical DO immediately after calibration. This step is
not required.
Nitrogen, Ammonia – Standard Methods, 4500 NH3 D-2011 (Aqueous)
Recommendation: The laboratory analyzes a mid-point 50 mg/L laboratory-fortified blank (LFB) with
every run but does not vary the concentration over time. It is recommended that the laboratory vary
LFB concentrations to cover the range from the midpoint to the lower part of calibration curve,
including the reporting limit.
Recommendation: The laboratory is not rotating the range of the LFM spike concentrations. It is
recommended that the laboratory rotate the range of spike concentrations to verify performance at
various levels. Also, the concentration of the LFM spike should be the same as that of the LFB when
rotating spike concentrations.
D. Finding: The laboratory is not randomly selecting samples to fortify.
Requirement: As a minimum, include one duplicate sample or one LFM duplicate with each
sample set (batch) or on a 5% basis, whichever is more frequent, and process it independently
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#267 Town of Apex Middle Creek WWTP Laboratory
through the entire sample preparation and analysis. Ref: Standard Methods, 4020 B-2014. (8)
and Table 4020:I.
Requirement: Duplicate samples are analyzed randomly to assess precision on an ongoing
basis. If an analyte is rarely detected in a matrix type, use an LFM duplicate. An LFM duplicate
is a second portion of the sample described in 1020B.7 to which a known amount of the
analyte(s) of interest is added before sample preparation. If sufficient sample volume is
collected, this second portion of sample is added and processed in the same way as the LFM.
If there is not enough sample for an LFM duplicate, then use a portion of an alternate sample
(duplicate) to gather data on precision. As a minimum, include one duplicate sample or one
LFM duplicate with each sample set (batch) or on a 5% basis, whichever is more frequent,
and process it independently through the entire sample preparation and analysis. Evaluate
LFM duplicate results for precision and accuracy (precision alone for duplicate samples). Ref:
Standard Methods, 1020 B-2014. (8).
Comment: The laboratory routinely spikes the Influent sample, because the values of the
plant effluent are less than 1 mg/L.
Nitrogen, Total Kjeldahl - SM 4500 Norg B-2011 (SM 4500 NH3 C-2011) (Aqueous)
Comment: Standards and spikes are being analyzed at different volumes than the blank and
samples. This has a minimal effect on the recovery calculations.
pH – Standard Methods, 4500 H+ B-2011 (Aqueous)
Comment: The laboratory analyzes a second-source pH check buffer in addition to the required
check buffer. This is not required.
Recommendation: The laboratory includes a sentence on their benchsheet that describes the
process for calibration. It is recommended that the lab include a check box to signify that the
calibration was performed according to their requirements.
Temperature – Standard Methods, 2550 B-2010 (Aqueous)
E. Finding: The compliance temperature-measuring device is not checked at two temperatures
that bracket the range of observed sample temperatures.
Requirement: The State Laboratory may develop Approved Procedures for Field Parameters
based upon the methods in any of the sources referenced in Parts(a)(1)(A) through (F) of this
Rule. Ref: 15A NCAC 02H .0805 (a) (1) (F).
Requirement: To check a compliance temperature-measuring device, compare readings at
two temperatures that bracket the range of compliance samples routinely analyzed against a
Reference Temperature-Measuring Device and record all four readings. The readings from
both devices must agree within 0.5ºC. If they do not, the device may not be used for
temperature compliance monitoring. Ref: NC WW/GW LCB Approved Procedure for the
Analysis of Temperature.
Comment: The laboratory only checks the DO meter, which is used as the TMD, at one
temperature.
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#267 Town of Apex Middle Creek WWTP Laboratory
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: Tom Halvosa Date: November 16, 2023
Report reviewed by: Michael Cumbus Date: November 17, 2023
Certificate Number:267
Effective Date:1/1/2023
Expiration Date:12/31/2023
Lab Name:Town of Apex Middle Creek WWTP Laboratory
Address:300 Pristine Waters Dr.
Apex, NC 27502
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
Date of Last Amendment:1/19/2023
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
BACTERIA - COLIFORM FECAL
IDEXX Colilert ®18 (MPN) (Aqueous)
BOD
SM 5210 B-2016 (Aqueous)
COD
Hach 8000 (Aqueous)
DISSOLVED OXYGEN
Hach 10360-2011, Rev. 1.2 (Aqueous)
SM 4500 O G-2016 (Aqueous)
NITROGEN, AMMONIA
SM 4500 NH3 D-2011 (Aqueous)
NITROGEN, NO3 + NO2
SM 4500 NO3ˉ E-2016 (Aqueous)
NITROGEN, TOTAL KJELDAHL
SM 4500 Norg B-2011 (SM 4500 NH3 C-2011) (Aqueous)
pH
SM 4500 H+B-2011 (Aqueous)
PHOSPHORUS, TOTAL
Hach 10210 TNT (Aqueous)
RESIDUE, SUSPENDED
SM 2540 D-2015 (Aqueous)
RESIDUE, TOTAL
SM 2540 B-2015 (Aqueous)
TEMPERATURE
SM 2550 B-2010 (Aqueous)
TURBIDITY
SM 2130 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.