#12_0203_FINAL

CDE
North Carolina Department of Environment and Natural Resources
Pat McCrory
Governor
12
Ms. Cheryl Johnson
March 17, 2015
Pace Analytical Services, Inc. -Huntersville
9800 Kincey Avenue, Suite 100
Huntersville, NC 28078
Donald R. van der Vaart
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Johnson:
Enclosed is a report for the inspection performed on February 3, 2015 by Beth Swanson, Gary
Francies, Dana Satterwhite, Jason Smith, Nick Jones, and Todd Crawford. 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. 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.
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 us at (828)
296-4677.
Attachment
cc: Master file
Beth Swanson
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone [phone] I FAX: [phone]
Internet: www,dwqlab.org
An Equal Opportunity\ Mirmative Action Employer
Laboratory Cert. #:
Laboratory Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist Ill:
Date Received:
Date Forwarded to Linda:
Date Mailed:
cc: Chris Goforth
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
12
Pace Analytical Services, Inc. -Huntersville
Commercial Maintenance, Requested
Beth Swanson, Gary Francies, Dana Satterwhite
Jason Smith, Nick Jones, Todd Crawford
February 3, 2015
February 18, 2015
February 24, 2015
Jason Smith
2/25/2015
D lnsp. Initial
D lnsp. No Finding
D Corrected
Gary Francies
2/25/2015
3/17/2015
3/17/15 \S.,-
[gj lnsp. Reg.
0 lnsp. CP
D lnsp. Reg. Delay
On-Site Inspection Report
LABORATORY NAME: Pace Analytical Services, Inc. -Huntersville
9800 Kincey Avenue, Suite 100
Huntersville, NC 28078
ADDRESS:
CERTIFICATE #: 12
DATE OF INSPECTION: February 3, 2015
TYPE OF INSPECTION: Commercial Maintenance and Requested
AUDITOR(S): Beth Swanson, Gary Francies, Dana Satterwhite,
Jason Smith, Nick Jones, and Todd Crawford
LOCAL PERSON(S) CONTACTED: Cheryl Johnson
I. INTRODUCTION:
II.
Ill.
This laboratory was inspected by a representative 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.
GENERAL COMMENTS:
The facility has all the equipment necessary to perform the laboratory's certified analyses. The system for traceability
of standard and reagent preparation is effective, thorough, and easy to follow.
This was a maintenance inspection which was performed at the request of the laboratory.
The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must update
the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any changes made in response
to the Findings, Recommendations or Comments listed in this report must be incorporated to insure the method is
being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is in
agreement with approved practice and regulatory requirements. In some instances, the laboratory may need to
create a SOP to document how new functions or policy will be implemented.
The requirements associated with Findings F and G have been implemented by our program since the last
inspection.
FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Comment: There were no units or acceptance criteria on the temperature log for refrigerator R-27. The North
Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Demonstration
of acceptable corrective action (i.e., an updated log which included proper units of measure for temperature and
acceptance criteria for the reading) was generated and posted at the time of the inspection. No further response is
necessary for this finding.
A. Finding: There is no record of the date put into use for consumables used in the analysis of fecal
coliform, i.e., media and filters.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory must have the
following information documented: Date received, Date Opened {in use), Vendor, Lot Number, and
Expiration Date (where specified). Consumable materials such as pH buffers, lots of pre-made standards
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and/or media, solids and bacteria filters, etc. are included in this requirement. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
Comment: The date opened and date the consumable testing was conducted is recorded, but there is no
record of the actual date put into use for analysis.
B. Finding: The TCLP benchsheet was lacking units of measure for pH (i.e., Standard Units or s.u.).
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: 15A NCAC 2H .0805 (a) (7) (A).
Standard Operating Procedures (SOPs)
Recommendation: It is recommended that all SOPs be reviewed for use of the word "should" and other instances
where a specific action is not identified with phrases such as "at least" and "a minimum". SOPs are intended to
describe procedures exactly as they are to be performed. While some uses of the word "should" versus "must" are
noted in the finding below, it is likely that not all instances were found during the audit.
C. Finding: Inconsistencies were noted between the Standard Operating Procedures (SOPs) and laboratory
practice as follows:
o The SOP is in direct conflict with the method and/or a regulatory requirement.
• Organochlorine Pesticides and PCBs (EPA 608, SW-846 8081 B, SW-846 8082 A) -
The SOPs indicate that the State of North Carolina is notified when samples are received
out of hold time. Per the NC Administrative Code 15A NCAC 2H .0805 (a) (7) (N), the State
must also be notified if samples do not meet sample collection or preservation requirements.
The proper notification procedure is conducted by the laboratory, but the SOP must be
updated to include preservation requirements in addition to the hold time requirements.
• TCLP (SW-846 1311) -Section 12.2.2.7 leaves out the word "not" in the instructions (i.e., "if
this point is not reached ... ").
o The SOP does not describe in detail how the method is performed.
• Purgeable Organics (EPA 624, SW-846 8260 B, SM 6200 B-1997) -The SOP does not
state the volume of sample purged.
• Purgeable Organics (EPA 624) -The SOP states "should" in section 11.2 and also says
that "a minimum of three concentration levels" are used. The SOP needs to state the actual
number used.
• Purgeable Organics (SM 6200 B-1997) -Section 11.2.1 states "at least" five calibration
standards are run to meet the requirement. State specific number and concentration of
standards analyzed. If the calibration scheme varies, then explain those circumstances in
the SOP.
• Purgeable Organics (SM 6200 B-1997) -The amount of bromofluorobenzene (BFB) tune
standard used is not stated in the SOP.
• Purgeable Organics (SM 6200 B-1997) -The frequency of blank analysis is not cited in
the SOP.
• Organochlorine Pesticides and PCBs (EPA 608, SW-846 8081 B) -The SOP does not
mention the EPA 608 method requirement to adjust pH to range of 5.0 -9.0 s.u. with NaOH
or H2 SO4 if the sample is not extracted within 72 hours.
• TCLP (SW-846 1311) -Section 12.5.1 of the SOP does not specify that particle reduction is
carried out if necessary.
• TCLP (SW-846 1311) -Section 12.6.1 does not specify that the filtered sample is the TCLP
extract.
• TCLP (SW-846 1311) -The following instances of the use of "should" were noted and need
to be addressed. The sections include 7.5, 7.6, 7.7, 9.7, 10.1.6, 10.1.6.1, 10.1.6.2, 10.1.6.3,
12.2.2.3, 12.2.2.4, and 12.5.4.
o Miscellaneous errors noted in the SOP
• TCLP (SW-8461311)-Section 12.3.2 is a carryover from 12.3.1 and can be removed.
• TCLP (SW-846 1311) -In section 12.4.4, a pH value from section 12.4.2 is referenced, but
the correct section is 12.4.3.
• TCLP (SW-846 1311) -In section 12.7.2, a worksheet attachment is referenced in section
16, which is not there.
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#12 Pace Analytical Services, Inc. -Huntersville
• TCLP (SW-846 1311) -Section 12.10.9 references section 11.2, but the correct reference
is 12.2.
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). Please
submit updated SOPs with the items listed above addressed by June 15, 2015.
Recommendation: It is recommended that references to the Minimum Detection Limit (MDL) SOP
and MDL section of the Quality Assurance Manual (QAM) be added to the SM 6200 B-1997 SOP.
Recommendation: It is recommended that all SOPs be reviewed for similar issues.
Fecal Coliform (MF) -Standard Methods, 9222 D-1997
Comment: The temperature correction for the thermometer in the incubator was not posted. NC WW/GW LC
Policy states: Also document any correction that applies (even if zero) on both the thermometer/meter and on a
separate sheet to be filed. Demonstration of acceptable corrective action (i.e., posting the temperature correction)
was completed at the time of the inspection. No further response is necessary for this finding.
Recommendation: It is recommended that when less than 100 ml of sample is to be filtered, the full volume of
sample is added at one time, or that smaller measured aliquots be added to the filter until the desired amount is
reached. Aliquots must not be removed from the funnel after the sample has been added due to settling and the
chance for filtering a non-homogenous sample. While we cannot find a direct reference to cite for this, (thus cited as a
recommendation and not a finding); we believe that this subsampling technique does not produce a representative
homogenous subsample. We request a response to this recommendation.
D. Finding: The fecal coliform benchsheet references the incorrect method code.
Requirement: Standard Methods 9222 D-1997. Ref: Code of Federal Regulations, Title 40, Part 136;
Federal RegisterVol. 77, No. 97, May 18, 2012; Table 1B.
Comment: Currently the benchsheet references the 18th Edition of Standard Methods.
E. Finding: The laboratory is not using the method-specified phosphate buffer.
Requirement: Stock phosphate buffer solution: Dissolve 34.0 g potassium dihydrogen phosphate (KH 2
PO 4 ) in 500 ml reagent-grade water, adjust to pH 7.2 ± 0.5 with 1N sodium hydroxide (NaOH), and dilute
to 1 L with reagent-grade water. Sterilize by filtration or autoclave. Store stock solution under refrigerated
conditions and discard if turbidity develops. Ref: Standard Methods, 9050 C-2006. (1) (a) (1).
F. Finding: The laboratory is not testing a culture positive with each batch of media prepared.
Requirement: Use certified reference cultures. For each lot of medium received, each laboratory
prepared batch of medium, and each lot of purchased prepared medium, verify appropriate response by
testing with known positive and negative control cultures for the organism(s) under test. Record results.
Ref: Standard Methods, 9020 B-2005. (9) (b).
Comment: Standard Methods for the Examination of Water and Wastewater, 9020 A-2005 states that the
quality control (QC) requirements in section 9020 are not mandatory. Each laboratory must develop its
own QC suitable for its needs and, in some cases, as required by regulatory agencies, standard setting
organizations, and laboratory certification or accreditation programs. 9020 A-2005 also states that the
program must be practical and require only a reasonable amount of time or it will be bypassed. Once a
Quality Assurance (QA) program is established, about 15% of overall laboratory time should be spent on
different aspects of the program. Based upon this language, and in conjunction with method specified
requirements, the NC WW/GW LC program has established minimum requirements for maintaining
certification with our program. At this time, negative control cultures are not required for coliform analyses.
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Comment: The laboratory prepares agar medium, which has a hold time of two weeks, approximately
every week.
G. Finding: Plate comparison counts are not being conducted.
Requirement: For routine performance evaluation, repeat counts on one or more positive samples at
least monthly, record results, and compare the counts with those of other analysts testing the same
samples. Replicate counts for the same analyst should agree within 5% (within analyst repeatability of
counting) and those between analysts should agree within 10% (between analysts reproducibility of
counting). If they do not agree, initiate investigation and any necessary corrective action. Ref: Standard
Methods, 9020 B-2005. (9) (a).
Purgeable Organics -EPA 624; SW-846 8260 B; Standard Methods, 6200 B-1997
Organochlorine Pesticides and PCBs -EPA 608; SW-846 8081 B; 8082 A
Diesel Range Organics -EPA SW-846 8015C
Gasoline Range Organics -EPA SW-846 8015C
Base/Neutral Acid Organics -EPA 625; EPA SW-846 8270 D
1, 2-Dibromoethane (EDB)-EPA 504.1; EPA SW-846 8011
H. Finding: The laboratory's blank acceptance criteria exceed 50% of the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of reagent, method and
calibration blanks must not exceed 50% of the reporting limit or as otherwise specified by the reference
method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Diesel Range Organics -EPA SW-846 8015C
Gasoline Range Organics -EPA SW-846 8015C
I. Finding: An inconsistency was noted between the Manual Integration SOP and laboratory practice as
follows: The laboratory was not documenting the rationale for manual integrations performed on samples
above the calibration range to obtain an estimated value for determining the dilution factor to use on
subsequent analyses.
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: The laboratory's manual integration SOP (#S-CAR-Q-016-rev.06) Section 12.6.2 states: The
analyst making the changes must sign and date each chromatogram and documentation must exist to
indicate the rationale for the manual integration. This may be performed in several different ways
depending on the department or laboratory. The reason for the integration can be noted on the analytical
data review checklist, captured by the chromatography data processing software in an audit train, written
by hand on a hardcopy printout of the raw data, or using a pre-made stamp requiring date and initial or by
using a letter code system.
Comment: The same requirement would apply to all other organics methods where applicable.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and client
reports. Data were reviewed for the following projects: Analyses dates 1/26/2015 through 1/29/2015 for Oil and
Grease EPA 1664 Rev. B; analyses dates 1/7/2015, 1/15/2015, and 1/21/2015 for Oil and Grease SW-846 9071B;
project number 92233310 for DRO/GRO SW-846 8015B; analyses dates 1/27/2015 and 1/28/2015 for PCBs SW-
846 8082A; project number 9223149 for EDB SW-846 8011; and lab ID 92234383001 for BNAs SW-846 8270D.
No transcription errors were detected. The facility appears to be doing a good job of accurately transcribing data.
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V. CONCLUSIONS:
Correcting the above-cited findings and implementing the recommendations will help this lab to produce quality
data and meet certification requirements. The inspectors would like to thank the staff for its assistance during the
inspection and data review process. Please respond to all findings and include an implementation date for
each corrective action.
Report prepared by:
Report reviewed by:
Beth Swanson
Jason Smith
Date: February 18, 2015
Date: February 24, 2015