#633_0825finalTS_2015_

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
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 III:
Date Received:
Date Forwarded to Linda:
Date Mailed:
cc: Chris Goforth
633
Pace Analytical Services, Inc. - Eden
Commercial Maintenance
Beth Swanson, Gary Francies, Nick Jones,
Todd Crawford and Tonia Springer
August 25, 2015
November 17, 2015
November 17, 2015
Nick Jones
November 25, 2015
❑ Insp. Initial ® Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
❑ Corrected ❑ Insp. Reg. Delay
Dana Satterwhite
December 3, 2015
December 11, 2015
December 14, 2015

Pat McCrory Donald R. van der Vaart
Governor Secretary
December 14, 2015
633
Mr. Barry Johnson
Pace Analytical Services, Inc. - Eden
205 East Meadow Road - Suite A
Eden, NC 27288
'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 August 25, 2015 by Tonja Springer, Gary
�Francies, Beth Swanson, Todd Crawford and Nick Jones. 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 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.
(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 (919)
1733-3908.
Sincerely,
Dana Satterwhite, Environmental Program Supervisor
Division of Water Resources
,Attachment
cc: Tonja Springer and Central Files
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] FAX: [phone]
Internet: www.cfi tab.org
An Equal Opportunity' Affirmative Action Employer

On -Site Inspection Report
LABORATORY NAME: Pace Analytical Services, Inc. - Eden
ADDRESS: 205 East Meadow Road - Suite A
Eden, NC 27288
CERTIFICATE #: 633
DATE OF INSPECTION: August 25, 2015
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Beth Swanson, Gary Francies, Nick Jones, Todd Crawford, and
Tonja Springer
LOCAL PERSON(S) CONTACTED: Barry Johnson
INTRODUCTION:
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 laboratory was very clean and well organized. Data was readily available and analysts were
knowledgeable and forthcoming. The organizational culture of this laboratory is one that focuses on
quality of data. Everyone we interacted with was interested and willing to adapt their processes to the
required and recommended changes. The system for traceability of standard and regent preparation is
effective, thorough and easy to follow. Laboratory personnel communicate well with sample collectors and
coordinate sample analyses effectively to manage workload and holding times.
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.
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.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General
Recommendation: It is recommended that the analytical balance be better stabilized to increase its
resistance to vibrations.

Page 2
#633 Pace Analytical Services, Inc. — Eden
Standard Operating Procedure (SOP)
Comment: BOD - Section 12.1.2.1 states that the sample temperature must be 20 ± 1°C. The method
allows 20 ± 3°C.
Comment: BOD - Section 13 states the duplicate acceptance criterion as "tighter than 10% RPD"
(Relative Percent Difference). The method allows <- 30% RPD.
Recommendation: BOD - It is recommended to rename the 5 ml seed control described in Section
12.1.10 as a seeded blank to distinguish it from the seed controls.
Recommendation: BOD - It is recommended to list the dechlorinating reagents (i.e., 2% H2SO4,
Potassium Iodide (KI) solution, 0.5% Starch Solution) in Section 10.
Comment: pH - Section 11.2.1.6 is a repeat of 11.2.1.2.
Comment: pH - Section 12.1.1.1.1 states, "unless a temperature compensated probe is used...".
Standard Methods 4500 H+ B-2000 (2) (a) requires the use of a pH meter with a temperature
compensating device.
Comment: pH - Section 12.1.1.2.2 states, "until they are within + 0.1 pH units..." instead of "± 0.1 pH
units", when referring to how close repeated measurements must be.
Recommendation: pH - It is recommended to consolidate the Quality Control (QC) Tables in Sections
11.1 and 13.1 since much of the information is repeated.
Comment: Residue, Suspended (TSS) - Section 13.2 indicates that a Method Blank (MB) with DI reagent
water is required. The same section also indicates that DI reagent water is used with the dry filter blank.
Method Blanks are not required and no water is to be put through the dry filter blank. If samples are being
weighed to constant weight, then a dry filter blank is not required.
Comment: TSS - Section 9.2 refers to Total Dissolved Solids (TDS) instead of TSS.
Comment: TSS - Section 12.2 does not mention that the maximum allowable residue weight gain is 200
Mg.
Comment: TSS - Sections 14.2 and 14.3 do not show recognizable depictions of the mathematical
symbols (e.g., _, +) in the formulas.
Comment: Nitrogen, Nitrate Hach 10206 - Table 10.2 states the final concentration of the MS as 0.25
mg/L. If the instructions are followed as stated, the final concentration would be 5 mg/L.
Comment: Nitrogen, Nitrate Hach 10206 - Section 13.1 states that the MS and MSD frequency
requirement is two for every 20 samples. The method frequency requirement is five percent of the
samples from each analytical batch as defined in Section 9.4.
Comment: Nitrogen, Nitrate Hach 10206 - Tables 11.1 and 13.1 state the Initial Calibration Blank (ICB),
Continuing Calibration Blank (CCB) and Method Blank (MB) acceptance criteria as < '/z PRL. NC
WW/GW LC Policy allows:5 % the reporting limit.
Comment: Nitrogen, Nitrate SM 4500 NO3- D-2000 - Section 13.1 indicates that an MSD is to be
analyzed once for every 10 samples. However, the MSD is not shown in the "order of readings" listed in
Section 12.2.4.

Page 3
#633 Pace Analytical Services, Inc. - Eden
Comment: Nitrogen, Nitrate SM 4500 NO3- D-2000 - Table 11.1 states the blank acceptance criteria as
<50% of the Reporting Limit. NC WW/GW LC Policy allows 5 1/2 the reporting limit.
Comment: Nitrogen, Nitrite SM 4500 NO2- B-2000 - Table 11.1 states the blank acceptance criteria as <
1/2 PRL and Section 13.1 states that the MB must be < PRL. NC WW/GW LC Policy allows 5 '/2 the
reporting limit.
Comment: Bacteria, Enterococci Enterolert® IDEXX - Section 13.6.2 states Waste Water requires 2
duplicates for every 20 samples (i.e., 10%). The method allows for a 5% frequency.
Comment: The Color, ADMI SM 2120 E-1993 and Color, PC SM 2120 B-2001 - Section 13.1 states the
Method Blank acceptance criterion as "< 1/2 PRL ", NC WW/GW LC Policy allows <- 1/ reporting limit.
A. Finding: An inconsistency and/or omission was noted between the SOP and laboratory
practice as follows:
General
o SOPs are intended to describe procedures exactly as they are to be performed.
Evaluate all SOPS for the proper use of the word "should".
BOD/CBOD -Standard Methods, 5210 B-2001
o Section 4.2 references the Hexavalent Chromium method SW-846 7196 A, which
is not applicable to this SOP.
o Section 6.2 states the sample pH acceptance criterion as 6.0-8.5. The method
requirement is 6.0 - 8.0.
o Section 9 references pipets but does not specify what kind.
o Section 10.4.3 and Section 12.2.3 state initial Dissolved Oxygen (DO) of all bottles
must be 7.0-9.0 mg/L. The initial DO of blanks must be 7.5-9.0 mg/L.
o Section 12.1.8 states for CBOD add Nitrification Inhibitor to all samples and QC.
This needs to be clarified and include language stating not to add inhibitor to
blanks.
o Section 12.1.13 states to add extra nutrients to sample volumes >200 ml. The
method requirement applies to sample volumes >201 ml.
o Section 13 states to flag data for a seed blank failure. Seeded blank failures do not
require associated data to be flagged.
o Section 13.3 needs to clarify if a duplicate is one dilution or all 3 dilutions.
o Section 13.5 does not state to only use acceptable dilutions for the final seed
correction factor (i.e., dilutions that meet the 2 and 1 rule for depletion).
o Section 13.7 states that the dilution water blank "should" be no more than 0.2
mg/L. The method requires that the dilution water blank must be equal to or less
than 0.20 mg/L.
Bacteria - E.coli - Standard Methods, 9223 B-2004 (Colilert 18) (MPN)
o The requirement for sample duplicates is not stated.
Color, ADMI - Standard Methods, 2120 E-1993 (ADMI)
o The title page does not reference the method approval year.
o Section 19.1 and Section 25.4 reference 18th Edition of Standard Methods for
2120E, rather than the Standard Methods Committee approval year (i.e., 1993).
Nitrogen, Nitrate - Standard Methods, 4500 NO3- D-2000
o The title page and Sections 1.1 and 25.4 reference the wrong Standard Methods
Committee approval year (i.e., 1992/2011) the correct approval year is 2000.

Page 4
#633 Pace Analytical Services, Inc. — Eden
o The requirement to perform a 5-standard calibration curve verification at least
every 12 months is not stated.
o Section 13.1 states that MS and MSD frequency requirement is once for every 10
samples. The method requirement is once daily or for every batch of 20 or fewer
samples.
o Instructions for making the LFM are not stated.
• Nitrogen, Nitrite — Standard Methods, 4500-NO2- B-2000
o The requirement to back -calculate each of the initial calibration standards is not
stated.
o The SOP, QC Section 13.1 states only an RPD requirement for the MSD. The
percent recovery must also be calculated.
• Nitrogen, Nitrate — Hach 10206
o Section 11.4.1.3 states to "let stand 5 to 10 minutes for full color development ..."
The method states in Section 11.3.3, "react for 15 minutes".
• pH — SW-846 9040C
o Section 13.3 states to dilute the sample if it is above the highest calibration
standard. Dilution of pH samples is not allowed. A higher pH buffer must be read to
bracket the sample.
• Turbidity — Standard Methods, 2130 B-2001
o Section 13.1 includes an LCS for hexavalent chromium. This appears to be a cut
and paste error and should be removed from this SOP.
• Residue, Suspended — Standard Methods, 2540 D-1997
o Section 13.2 lists the acceptance criterion for the dry filter blank as "within 50% of
PRL". The method requirement is within 4% of the initial weight or 0.5 mg,
whichever is less.
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 respond in writing stating that the SOPs will be revised to
address the items in this Finding within one year.
BOD — Standard Methods, 5210 B-2001
Comment: The form labelled "F-ASV-WC-015-Rev.17 4.08.2014" needs to be updated to match what is
being done in the laboratory. The following updates need to be made:
The requirement for seed control frequency is listed as a minimum of 3. This needs to be updated
to 2 seed controls and 1 seeded blank.
The requirement for Glucose Glutamic Acid (GGA) frequency is listed as a minimum of 2 GGAs.
The method requires analysis of 3 GGAs, and all 3 of the GGAs must be averaged regardless of
whether or not they are outside the acceptance limits.
The duplicate acceptance criterion is listed as <50% RPD for results which are <20 mg/L. The
laboratory is using an acceptance criterion of <10% RPD according to the checklist. The method
states a 30% RPD acceptance criteria for duplicates.
B. Finding: The dilution water blank value is not documented to two decimal places.
Requirement: Dilution water blanks serves as a check on quality of unseeded dilution waster and
cleanliness of incubation bottles. Determine initial and final DO as in 5210B. 5g and i. The DO
uptake in 5 d must not be more than 0.20 mg/L and preferably not more than 0.10 mg/L, before
making seed corrections. Ref: Standard Methods 5210 B-2001. (6) (c).

Page 5
#633 Pace Analytical Services, Inc. — Eden
Comment: Dilution water blanks are currently only documented to one decimal place. They must
be documented to two decimal places to show compliance with the method requirement.
C. Finding: Sample volumes <3 mLs are being measured without preliminary dilutions.
Requirement: For dilutions greater than 1:100 make a primary dilution before making final
dilution. This would be any measurements of less than 3 mLs sample volume if diluting directly
into BOD bottles. Ref: NC WW/GW LC Policy.
D. Finding: The laboratory is measuring samples volumes less than 20 mis using narrow -tip
Eppendorf pipets.
Requirement: Sample volumes less than 20 mis must be measured using a wide -tip pipet. For
dilutions greater than 1:100 make a primary dilution before making final dilution. This would be
any measurements of less than 3 mis sample volume if diluting directly into BOD bottles. Ref:
NC WW/GW LC Policy.
E. Finding: Samples are screened for Total Residual Chlorine (TRC) with test strips.
Requirement: It is acceptable to screen samples with DPD powder for the presence of Total
Residual Chlorine (use pillows appropriate for the volume of sample tested). Generally total
residual chlorine test strips are not adequate; however, these may be used for samples where
interference with DPD precludes their use. If DPD yields no pink color, chlorine is absent.
Document and proceed to set sample. If pink color is observed, chlorine is present. In those
cases, the titration procedure outlined below must be used to determine the proper amount of
Sodium Sulfite needed to neutralize chlorine in the sample. Ref: NC WW/GW LC Policy
F. Finding: Units are documented on the benchsheet for the Sodium Sulfite Solution as mL instead
of drops per 100 mLs.
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).
Color, PC — Standard Methods, 2120 B-2001 (PtCo)
G. Finding: The benchsheet and client reports have not been updated to include the approved
method reference year.
Requirement: Each laboratory shall develop and maintain a document outlining the analytical
quality control practices used for 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: This was observed on the client report for sample number 92256084.
Residue, Settleable — Standard Methods, 2540 F-1997
Comment: Duplicate analyses and blanks are not required for this method.

Page 6
#633 Pace Analytical Services, Inc. — Eden
Comment: The last column header on the benchsheet has the incorrect units of measure (i.e., mUUL).
The correct units are mUL.
Bacteria- Coliform Fecal — Standard Methods, 9222 D-1997
H. Finding: The unique identifier for the MFC broth was not updated on the benchsheet when a
new batch of broth was made.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory
must have the followinq information documented: Date received, Date Opened (in use), Vendor,
Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used. Documentation of solution preparation must include the analyst's initials,
date of preparation, the volume or weight of standard(s) used, the solvent and final volume of
the solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. Consumable materials such as pH buffers, lots of pre -made
standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
NC WW/GW LC Policy.
Comment: The unique identifier, IS-2999, was documented on the benchsheet for the months
of July and August.
Turbidi — Standard Methods, 2130 B-2001
Comment: The meter was not being calibrated according to the manufactures instructions. The meter
was not being placed in calibration mode when the standards were being read. Standards were simply
being read like a sample. All data reviewed showed that observed standard readings were within their
established acceptance ranges. Standard Methods, 1020 B (11) states: Perform both instrument
calibration and maintenance according to instrument manual instructions. Standard Methods, 2130 (4) (b)
states: Follow the manufacturer's operating instructions. Run at least one standard in each instrument
range to be used. Acceptable corrective action (i.e., the analyst was instructed as to how to properly
calibrate the meter as described in the instrument manual). The analyst stated that the meter would be
properly calibrated from that date forward. No further response is necessary for this Finding.
Finding: Samples with concentrations greater than 40 NTU are being diluted.
Requirement: Avoid dilutions whenever possible. Particles suspended in the original sample
may dissolve or otherwise change characteristics when the temperature changes or when the
sample is diluted. Ref: SM 2130 B-2001 (4) (a).
Comment: The quality control sheet for sample 92261587001 on 8/4/15 states a dilution factor
of 4 but incorrectly shows the initial and final sample volumes as 50 mLs. Although the SOP
currently states to dilute all samples over 40 NTU, the meter is capable of analyzing samples up
to 1000 NTU. Therefore, this sample should not have been diluted. A higher standard should
have been analyzed to calibrate the meter in the appropriate range for the sample.
J. Finding: Standard recoveries are not calculated on the benchsheets.
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).

Page 7
#633 Pace Analytical Services, Inc. — Eden
Comment: Standard recoveries must be documented on the benchsheet and evaluated against
established acceptance criteria to demonstrate that the analyst was aware of any Quality Control
failures.
pH — SW-846 Method 9040 C
Comment: Duplicates are being analyzed but are not required.
Comment: A calibration check is analyzed after every ten samples and/or at the end of the analysis. Only
one check standard is required immediately after calibration since the analysis is not performed off site.
Comment: It is not clear if the "20W in the benchsheet column heading "9040 C/20% solids (Y/N)"
means less than or greater than 20%. The SOP section 12.1.1.2.1 states if the sample is >20% solids,
remove the sample from the batch and have the project manager login the sample for 9045 D pH. If it is
determined that reporting by SW-846 9045 D is required then Certification must be obtained.
Recommendation: The note on the pH benchsheet says to circle the method used. There is not a
method being circled. Since the benchsheet has separate columns for each method, it is not necessary to
circle a method to determine which method is being followed. If a method is not going to be circled, it is
recommended that the lab remove the comment.
Chromium, Hexavalent —Standard Methods, 3500-Cr B-2009
Nitrogen, Nitrate — Hach 10206
Comment: The benchsheet (Page 4) states a 10% frequency requirement for MS and MSD. Both
methods and NC WW/GW LC only require a 5% frequency.
Nitrogen, Nitrite — Standard Methods, 4500-NO2- D-2000
Comment: All data reviewed showed initial and final sample volumes on page 1 of the benchsheet as
being 10 mi. The Quality Control Review page shows all initial and final volumes as 50 mi.
Comment: The benchsheet page 3 states the hold time as 24 hours from time of collection. Code of
Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II allows
48 hours.
K. Finding: The laboratory is using the wrong "True Value" concentration when calculating the MS
recovery.
Comment: SOP Section 14.3 shows the Matrix Spike Recovery calculation as:
% REC = (MS Conc. — Sample Conc.) * 100
True Value
The same standard and volume are used to spike samples as is used to make the
Initial Calibration Verification (ICV) standard. The observed concentration of the ICV
standard, instead of the True Value of the spike based on how it was made, is being
used as the True Value when calculating percent recovery of the MS.
L. Finding: The LFM and LFMD was not calculated correctly on 8/21/2015 and therefore the LFMD
concentration was entered in the LIMS system incorrectly.

Page 8
#633 Pace Analytical Services, Inc. — Eden
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 .085 (a) (7). Please send a copy of the corrected client report with the response to
this report.
Comment: The benchsheet on 8/21/2015 for the Cargil sample 92264305001 was used as the
LFM and LFMD. The benchsheet shows the initial and final volumes as 10 mL with a dilution
factor or 4. The LFMD concentration was incorrectly entered into LIMS. Therefore, the % recovery
for the LFMD and RPD between the LFM and LFMD were wrong. The correct % recovery for the
LFMD was 131 % and the RPD was 17% which was outside the acceptance criteria and should
have been qualified.
Comment: This report was a preliminary report and had not yet been sent out. The laboratory
indicated that the report would be corrected before it was mailed to the client.
M. Finding: The final result for sample 92253155001 was reported incorrectly to the client.
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 .085 (a) (7).
Comment: Sample 92253157001 was reported to the client as <0.01 mg/L. The value on the
benchsheet was 0.02 mg/L.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) to
the client reports. Settleable Residue data was reviewed for June 19, 2015. pH data sets were reviewed
for May 10 and June 16, 2015. Turbidity data sets were reviewed for July 29, August 4, August 5, August
6, August 13 and August 19, 2015. Hexavalent Chromium data was reviewed for April 17, 2015, Nitrogen,
Nitrite data sets were reviewed for June 5, August 11, August 12, August 18, August 19, August 20 and
August 21, 2015. Nitrogen, Nitrate data sets were reviewed for August 12, August 18, August 19, August
20 and August 21, 2015. TSS data was reviewed for June 1, 2015. Color ADMI data was reviewed for
June 3, 2015. Color PC data was reviewed for March 18, 2015. Enterococcus and E.coli data sets were
reviewed for June 17, 2015. Fecal Coliform data was reviewed for June 16, 2015. BOD data was
reviewed for May 29, 2015. The following errors were noted: The Nitrite sample result for sample
92253157001 from June 5, 2015 reported a result <0.01 mg/L (See Finding M).
In order to avoid questions of legality, it is recommended that you submit amended report(s) to your
client(s). A copy of this report will be made available to the Regional Office.
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
its assistance during the inspection. Please respond to all Findings and include an implementation
date for each corrective action.
Report prepared by: Tonja Springer Date: November 17, 2015
Report reviewed by: Nick Jones Date: November 25, 2015