#530_2015_1120_final

INSPECTION REPORT ROUTING SHEET

To be attached to all inspection reports in-house only.

Laboratory Cert. #: 530

Laboratory Name: Pace Analytical Services, Inc. – Minneapolis, MN

Inspection Type: Maintenance/Abbreviated/Desk Audit

Inspector Name(s): Dana Satterwhite, Gary Francies, Roy Byrd

Inspection Date: 11/20/2015 – 12/18/2015

Date Report Completed: 12/1/2015

Date Forwarded to Reviewer: 12/1/2015

Reviewed by: Gary Francies

Date Review Completed: 1/22/2016

Cover Letter to use: Insp. Initial Insp. Reg.
Insp. No Finding Insp. CP
Corrected Insp. Reg. Delay

Unit Supervisor/Chemist III: Dana Satterwhite

Date Received: 1/22/2016

Date Forwarded to Linda: 1/22/2016

Date Mailed: 1/26/2016

_____________________________________________________________________

EPA Methods 200.8 and 245.1

On-Site Inspection Report

LABORATORY NAME: Pace Analytical Services, Inc.

ADDRESS: 1700 Elm St SE Suite 200
Minneapolis, MN 55414

CERTIFICATE #: 530

DATE OF INSPECTION: November 20, 2015

TYPE OF INSPECTION: Maintenance/Abbreviated/Desk Audit

AUDITOR(S): Dana Satterwhite, Gary Francies, Roy Byrd

LOCAL PERSON(S) CONTACTED: Ms. Melanie Ollila and Mr. Nathan Boberg

I. 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.

II. GENERAL COMMENTS:

This was an abbreviated audit performed at the request of the Division of Water Resources and was
limited to data for the following Pace Project Numbers: 92261557, 92265303, 92260963 and 92265356.
The laboratory sent complete data packages which included raw data [i.e., instrument printouts and/or
benchsheets] including associated calibration curves, associated digestion logs, chain of custody records,
method detection limit study summaries and standard operating procedures.

Proficiency Testing (PT) samples have been analyzed for all certified parameters. The laboratory has
fulfilled its PT requirements for the 2015 proficiency testing calendar year.

Contracted analyses were performed by Pace Analytical Services, Inc. – Ormond Beach, FL (Certification
#667) and Pace Analytical Services, Inc. – Asheville, NC (Certification #40).

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.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Standard Operating Procedures (SOPs)

Recommendation: It is recommended that all SOPs be reviewed and evaluated for use of the word
“should”. 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 Finding A, not all have been listed in this report.
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Recommendation: It is recommended that the ICP-MS Method 6020/6020A/200.8 SOP #S-MN-I492-
rev. 23 refer to the use of Kinetic Energy Discrimination (KED) as an acceptable interference reduction
technology under 40 CFR Part 136.6 (b) (4) (iv), Method Modifications and Analytical Requirements,
Allowable Changes, which reads:

In general, IC-MS is a sensitive and selective detector for metal analysis; however isobaric interference
can cause problems for quantitative determination, as well as identification based on the isotope pattern.
Interference reduction technologies, such as collision cells or reaction cells, are designed to reduce the
effect of spectroscopic interferences that may bias results for the element of interest. The use of
interference reduction technologies is allowed, provided the method performance specifications relevant
to ICP-MS measurements are met.

Comment: In the Mercury EPA Method 245.1 SOP# S-MN-I-359 Rev.23 – Section 9, Table 9.1 – The
description for the analytical balance states “accurate to at least 10 mg”. Please verify that based upon
its intended use in this method, this statement of accuracy is adequate for the data quality objectives of
the method.

A. Finding: An inconsistency and/or omission was noted between the Standard Operating
Procedure (SOP) and laboratory practice as follows:

 The SOP does not describe in detail how the method is performed.

Preparation of Aqueous Samples for ICPMS Analysis SOP
SOP# S-MN-I-523-rev.10 – Section 7, Table 7.1 – The SOP does not state that when
samples are received unpreserved, 1+1 nitric acid must be added at least 24 hours prior to
digestion for Clean Water Act (CWA) monitoring. [Ref: 40 CFR Part 136, Table II, footnote
19.] NOTE: This is appropriately noted in the analytical SOP# S-MN-I-492-Rev. 22.

SOP# S-MN-I-523-rev.10 – Section 10, Table 10.1 – It appears that the Standard Stock
solution concentration (i.e., 20 mg/ml) is incorrect. The concentration appears to calculate
to be 20 µg/ml.

SOP# S-MN-I-523-rev.10 – Section 12.1 – The SOP does not state that for compliance
monitoring under the Clean Water Act, samples must be digested regardless of turbidity.
[Ref: 40 CFR Part 136, Table I, footnote 4.]

SOP# S-MN-I-523-rev.10 – Section 12.2 – The SOP does not state that the pH must be
verified (i.e., pH <2) immediately before digestion. [Ref: EPA Method 200.8, Section 8.3]

SOP# S-MN-I-523-rev.10 – Sections 12.2.5 and 12.2.6 – The SOP needs additional
instruction regarding sample digestion. For example, Samples should be gently refluxed
and not allowed to boil vigorously or allowed to go to dryness, etc.

SOP# S-MN-I-523-rev.10 – Section 12.2.8 – The SOP does not state the volume
samples are brought up to (i.e., 50 ml - according to the data reviewed – there is no
indication of concentration in the calculation). Also, this should be quantitatively measured
unless the digestion cups are marked at 50 ml. Accurate measurement is critical.

SOP# S-MN-I-523-rev.10 – Section 13, Table 13.1 – The SOP does not clearly state that
although EPA SW -846 Method 3020 A allows a matrix spike frequency of 5%, EPA
Method 200.8 requires 10% of routine samples be spiked. [Ref: EPA Method 200.8,
Section 9.4.2]
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ICP-MS Method 6020/6020A/200.8 SOP
SOP# S-MN-I-492-Rev. 22 – Section 10, Table 10.1 - It appears that the references to
Attachment II in the table for Calibration Stock Standard solutions and Initial Calibration
Verification solutions are incorrect. It appears they should reference Table 10.2.

SOP# S-MN-I-492-Rev. 22 – Section 10, Table 10.1 - The concentrations of the Stock
solutions are not noted. Consequently, proper Working Standard preparations in Table
10.2 cannot be verified.

SOP# S-MN-I-492-Rev. 22 – Section 10, Table 10.2 – The SOP does not list units in the
column header for Final Concentration.

SOP# S-MN-I-492-Rev. 22 – Section 10, Table 10.2 - It appears the solvent volume for
ICS-AB is incorrect. It appears it should be 9.75 mL.

SOP# S-MN-I-492-Rev. 22 – Section 11, Table 11.1 - The SOP does not describe
demonstrating instrument stability by analyzing the tuning solution a minimum of 5 times
with resulting RSD of absolute signals <5%. [Ref: EPA Method 200.8, Revision 5.4,
Section 10.2.2]

SOP# S-MN-I-492-Rev. 22 – Section 11, Table 11.1 - For North Carolina
W astewater/Groundwater clients, blanks (including ICB, CCB and MB) must be evaluated
to ≤½PQL or as otherwise specified by the reference method (in this case - <10% of
analyte level for a sample or 2.2 times analyte MDL). It is noted that ≤½RL may be used
per client; however, it did not appear that the data packages reviewed were assessed to
that level – although all the data met this requirement. This assessment may be performed
on the project management level. The lab appears to be monitoring and meeting the %
RSD requirement. [Ref: NC WW/GW LC Policy and EPA Method 200.8, Revision 5.4,
Section 9.3.1]

Mercury EPA Method 245.1
SOP# S-MN-I-359 Rev.23 – Section 10, Table 10.2 – It appears the solvent volume for
the Low Level Mercury Calibration Intermediate Standard is incorrect. It appears it should
be 984.9 ml.

SOP# S-MN-I-359 Rev.23 – Section 10, Table 10.2 – It appears the solvent volumes for
Standard 1 and the CRDL standard are incorrect. It appears they should each be 29.7 ml.

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 April 30, 2016.

B. Finding: The laboratory is not analyzing a filtered Laboratory Reagent Blank (LRB) or filtered
Laboratory Fortified Blank (LFB) when samples must be filtered.

Requirement: The LFB is analyzed exactly like a sample, and its purpose is to determine
whether the methodology is in control and whether the laboratory is capable of making accurate
and precise measurements. Ref: EPA Method 200.8, Revision 5.4, Section 3.8.
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Requirement: An aliquot of reagent water or other blank matrices that are treated exactly as a
sample including exposure to all glassware, equipment, solvents, reagents, and internal
standards that are used with other samples. The LRB is used to determine if the method analytes
or other interferences are present in the laboratory environment, reagents, or apparatus. Ref:
EPA Method 200.8, Revision 5.4, Section 3.10.

Comment: This finding was not observed in the data sets reviewed; however, the SOP does not
indicate filtered LFBs and LRBs are analyzed when samples must be filtered for undissolved
material that does not settle out of the sample digestate prior to analysis on the instrument .

IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, chain-
of-custody forms, etc.) and client reports. Data were reviewed for the following Pace Project Numbers:
92261557, 92265303, 92260963 and 92265356. No transcription errors were detected. The facility
appears to be doing a good job of accurately transcribing data.

V. CONCLUSIONS:

Correcting the above-cited Findings and implementing the recommendations will help this lab 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: Dana Satterwhite Date: 12/1/2015
Report reviewed by: Gary Francies Date: 1/22/2016