Attachment_-_ADEQ_Audit_Report.docx

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Pace Analytical September 4, 2018

September 4, 2018

Eric Johnson Environmental Science dba Pace Analytical National 12065 Lebanon Road Mt. Juliet, TN 37122

Dear Mr. Johnson:

Any laboratory offering analyses of Arizona drinking water, wastewater, air, and any matter, pollutant, contaminant or hazardous substance for compliance with A.R.S. § 49-101 et seq., must be licensed and inspected by the Arizona Department of Health Services Office of Laboratory Licensure and Certification (Office) pursuant to A.R.S. § 36-495.01 et seq. and A.A.C. R9-14-601 et seq. These statutes and rules were promulgated to establish minimum standards of proficiency, methodology, quality assurance, operations and safety for laboratories licensed to perform environmental compliance testing.

An announced on-site inspection of your Arizona laboratory’s compliance testing of drinking water, wastewater, air and any matter, pollutant, contaminant or hazardous substance for adherence with Arizona’s statutes and regulations was conducted on July 24-26, 2018. During the on-site survey the office requested compliance samples performed within the past year. From the list that your laboratory provided, the Office randomly picked samples and their corresponding daily quality control checks for various methods licensed by the laboratory for review during the on-site inspection.

Below is our detailed written report of findings provided pursuant to A.R.S. § 41-1009 listing those areas in which Pace Analytical (AZ0612), was deficient as noted during our on-site inspection. As required by A.A.C. R9-14-605.G, please submit Pace Analytical’s written plan of correction and expected dates of completion within 30 days from the date of this letter. A plan of correction response is required for each of the following findings:

Report of Findings

1. The laboratory did not properly qualify sample L971597-14 which was received at 14°C (outside method preservation criteria) in noncompliance with A.A.C. R9-14-617.8.d. Multiple methods reported for this sample require maintaining a temperature of 4°C from the time of collection to analysis. The sample results must be qualified when temperature requirements are not met.

2. The laboratory did not comply with its quality assurance plan to obtain the correct documentation/information from the customer in the event sample shipments are not accompanied by the correct documentation (QAM Rev. 17, Sec. 2.4.2) in noncompliance with A.A.C. R9-14-615.B. The chain-of-custody for sample L972009-01 did not list the sample matrix or the method by which metals should be tested. A chain-of-custody should be checked for completion and accuracy. Any discrepancies must be documented.

3. The laboratory did not ensure that the compliance testing is performed using an approved wastewater method in noncompliance with A.A.C. R9-14-612.2.a. The laboratory reported the following final results that are currently not licensable methods under the AZ wastewater program. These results must be flagged with the appropriate ADEQ data qualifier (T6- the reported result cannot be used for compliance purposes).

A. SDG: L976058 received: 03/08/2018 Radiochemistry by Method 906 (Tritium) and Method DOE Ga-01-R/901.1 (21-day)

B. SDG: L972912 received: 02/23/2018 Ra-228 by Method 904

4. SDG: L972912 received: 02/23/2018 reported final result for Method SM7500 Ra B M that was not on the laboratory’s current Arizona List of Licensed Parameters in noncompliance with A.R.S. §36-495.01 et seq. Method modifications must be approved by EPA through the ATP process. This result must be flagged with the appropriate ADEQ data qualifier (T6- the reported result cannot be used for compliance purposes).

5. EPA Method 300.0 for the Determination of Anions by Ion Chromatography Revision 2.1

The laboratory did not comply with a complete and current standard operating procedure that meets the requirement of the method in noncompliance with A.A.C.R9-14-611.2, -612.2.A.1. and -615.C.3. Laboratory SOP Section 10.4.1 states in part that the linear calibration ranges are established for each instrument consisting of a method blank and at least 3 calibration points. EPA Method 300.0 Section 9.2.2 Linear Calibration Range (LCR) states in part that the LCR must be determined initially and verified every six months or whenever a significant change in instrument response is observed or expected. New instruments- IC19 and IC20 did not have an LCR study performed as part of the Initial Demonstration of Performance (IDP).

6. SW846 Method 6010C for the Determination of Inductively Coupled Plasma-Atomic Emission Spectrometry Revision 3 February 2007

The laboratory did not meet the requirement of the method that the post digestion spike addition should be recovered within 80-120% of the known value (Method 6010C Section 9.9.1) in noncompliance with A.A.C. R9-14-612.A.1. Laboratory SOP 340386 Section 10.9.1.2- Post digestion MS states in part that the recovery should fall within a ±25% acceptance range, relative to the known true value or otherwise within the laboratory derived acceptance limits. In addition, this method requirement must be set up in LIMS.

7. The laboratory did not comply with a complete and current standard operating procedure in noncompliance with A.A.C. R9-14-615.C.3. SOP 360402 Section 1.4 for Radiation survey meter check states in part that source check results are to be documented and include: date, initials and pass or fail result. Ludlum model 12 with 44-9 pancake probe did not have check results recorded.

8. EPA Method 8270C for Semivolatile Organic Compounds by Gas Chromatography/ Mass Spectrometry (GCMS)

A. The highest concentration calibration standard demonstrated detector saturation for multiple analytes, and was not scientifically valid or defensible, in noncompliance with A.A.C. R9-14-615.A. A review of the high calibration standard from 02/28/2018, file 0228_11.d, showed apparent saturation for phenanthrene, anthracene, and Di-n-butyl phthalate, among other analytes.

B. The laboratory did not require recovery criteria of ±20% for non-SPCC and non-CCC compounds in a calibration verification (EPA Method 8000C, Sec. 11.7) in noncompliance with A.A.C. R9-14-613.B.2. If an 8000 series method does not include specific quality control requirements, the laboratory must follow all requirements in EPA Method 8000C. Alternatively, the laboratory may statistically generate limits from historical data (AZDHS Information Update #80, Paragraph 10)

9. EPA Method 524.2, Revision 4.1 for the Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/ Mass Spectrometry

A. The laboratory did not determine that the absolute areas of the quantitation ions of the surrogates had not decreased by more than 30% from the areas measured in the most recent continuing calibration check (EPA Method 524.2, sec. 10.3.4) in noncompliance with A.A.C. R9-14-611.A.2.

B. The laboratory did not require the analyst to meet the current standard operating procedures MRL check acceptance criteria of ±50% (SOP #330364, Sec. 10.12) in noncompliance with A.A.C. R9-1-615.C.3. An MRL check analyzed 02/02/2018 recovered 177% and 180% for bromomethane and chloroethane, respectively. The laboratory must qualify the sample results.

10. The laboratory reported test results that were not on the laboratory’s current Arizona List of Licensed Parameters in noncompliance with A.R.S. §36-495.01 et seq. These compliance sample results must be flagged with the appropriate ADEQ data qualifier as cannot be used for compliance purposes.

Laboratory Sample L972424-01 reported wastewater test result by Standard Methods 22nd Ed, 2012, 9222D. In addition the sample was received past the holding time of 8 hours (Exhibit 1) 40 CFR, Revisions in Table II 136.3/e May 18, 2012.

THIS IS A REPEAT FINDING SIMILAR TO THE OFFICE’S MARCH 22-23, 2016 (FINDING #1) ON-SITE INSPECTION

Laboratory’s 2016 response: “Enclosed you will find ESC Lab Sciences add on application and supporting documentation for total phosphorus. This add on application is in response to finding 1.A. from our March 2016a assessment.”

11. The sample containers were not all tested for sterility (SM 9060.A.1, 9020B.5.d, and Table 9020:I) in noncompliance with A.A.C. R9-14-612.2.a. The QEC Microbiology sample container, lot #180317 was not traceable to the sterility check that is required by the laboratory’s SOP, QUALITY CONTROL AND QUALITY ASSURANCE OF MICROBIOLOGICAL EQUIPMENT, AND TESTING MATERIALS, section 8.1.2.

12. EPA Method 1622/1623; Cryptosporidium and Giardia in Water by Filtration/IMS/FA

A. The laboratory was not maintaining records for sampling capsules of a grade equal to or greater than that required by the approved method in noncompliance with A.A.C. R9-14-615.C.2 and 611.2.a. The laboratory did not obtain a certificate of analysis verifying that filters in use are acceptable for the methods approved (EPA Method 1622 and 1623 section 6.2.2.1 and Supplement 2 to EPA Manual for the Certification of Laboratories Analyzing Drinking Water, 5th ed., 2005 Section 3.12.1).

EPA Method 1622 and 1623 6.2 NOTE: Check at least one filter per batch to ensure that the filters have not been affected by improper storage or other factors that could result in brittleness or other problems. At a minimum confirm that the test filter expands properly in water before using the batch or shipping filters to the field.

B. The laboratory was not verifying that the tubing used for the filter inlet was conditioned to minimize sample contamination (EPA Method 1622 and 1623 section 6.3.1) in noncompliance with A.A.C. R9-14-611.2.a. Before use, the tubing must be autoclaved, thoroughly rinsed with detergent solution, followed by repeated rinsing with reagent water to minimize sample contamination. Alternately, decontaminate using hypochlorite solution, sodium thiosulfate, and multiple reagent water rinses. In addition verify that tubing to which oocysts and cysts will not easily adhere is in use.

C. The laboratory was not recording the actual results of quality control data validating the test results, including the calibration and calculations performed in noncompliance with A.A.C. R9-14-617.7.h. A record of calibration was not provided validating the graduation lines marked on the carboy used to determine the volume of samples filtered (EPA Method 1622 and 1623 section 6.4.1).

13. Standard Methods 2540D for the Determination of Non-filterable (TSS) Solids

The filter was not washed with three successive 10-mL volumes of reagent-grade water allowing complete drainage between washings after the sample was filtered (SM 2540C.3.d) in noncompliance with A.A.C. R9-14-612.2.a. The analyst washed the filter two times; a third rinse was done after questioning from the auditor.

Please note that the findings listed above as well as the recommendations listed below may be applicable to other Arizona licensed methods and should be corrected accordingly.

Please respond to the following recommendations:

1. Since the ADHS new rules were approved on October 1, 2016, we have adopted the Standard Methods for the Examination of Water and Wastewater 22nd edition 2012 for all Arizona compliance testing. Laboratory SOPs should reference this version, as well as all applicable method and QA/QC Sections (SM2020, SM4020 and SM5020).

2. The laboratory should update their software and instrument list to reflect current IC, ICP, ICP/MS and Radioactivity counters used to analyze AZ compliance samples.

3. The laboratory should clarify in SOP 360401how sample preservation is checked and recorded. In addition, to include this drinking water requirement from the DW Manual 5th Edition Chapter VI, Table VI-2: Sample Handling, Preservation, and Instrumentation- It is recommended that the preservative be added to the sample at the time of collection unless suspended solids activity is to be measured. If the sample has to be shipped to a laboratory or storage area unpreserved, acidification of the sample (in its original container) may be delayed for a period not to exceed 5 days. A minimum of 16 hours must elapse between acidification and analysis.

4. The laboratory should request to drop Mercury (Hg) by EPA Method 200.8 under their drinking water program.

5. Mercury section should include the ical information for Cal Stds 0.2- 10ppm on the prep bench sheet.

6. Laboratory SOP 340386 should be revised to reflect Method 6010C requirements:

A. Section 7.14 Lower limits of quantitation are verified when all analytes in the LCSL sample are detected within historical laboratory accuracy limits of their true value. The lower limit of quantitation check (LLQC) sample should be analyzed establishing the lower laboratory reporting limits and on an as needed basis to demonstrate the desired detection capability. Ideally, this check sample and the low-level calibration verification standard will be prepared at the same concentrations with the only difference being the LLQC sample is carried through the entire preparation and analytical procedure. Lower limits of quantitation are when all analytes in the LLQC sample are detected within ± 30% of their true value. (Method 6010C Inductively Coupled Plasma-Atomic Emission Spectrometry Revision 3, February 2007 Section 10.1.3.1- Lower limit of quantitation check sample)

B. Section 10.7.3 for SW-846 Method 6010C- The CCVLL recovery should be within historical laboratory accuracy limits. The LLCCV standard should be made from the same source as the initial calibration standards at the established lower limit of quantitation as reported by the laboratory. The acceptance criteria for the LLCCV standard should be ± 30% of its true value. (Method 6010C Inductively Coupled Plasma-Atomic Emission Spectrometry Revision 3, February 2007 Section 10.3.4)

7. The laboratory extraction benchsheet for EPA method 507 listed EPA 3510C as the preparation method. Though 3510C is similar to the 507 extraction, there are differences between the two extraction procedures. The office recommends clearly indicating on the benchsheet that the extraction procedure is performed according to EPA 507.

8. The sonicator log book for EPA 8330 extraction did not identify the thermometer used for monitoring temperature. The office recommends including the thermometer serial number or other internal identifier in the extraction log book.

9. The temperature logs for freezers “F8” (s/n m27937) and “F8” (s/n 6361170417080130) should include the thermometers’ serial number or other internal identifier.

10. The laboratory should maintain verification that all sampling ancillary materials such as cubitainers are conditioned to minimize sample contamination by maintain the certificate of analysis for methods 1622 and 1623.

11. The laboratory should document the internal diameter of the Pasteur pipette used to aspirate off the supernatant to 5 mL above the pellet as indicated in the SOP; ISOLATION AND IDENTIFICATION OF GIARDIA AND/OR CRYPTOSPORIDIUM IN WATER, section 10.4.8.

12. The laboratory should record the waterbath calibration-corrected temperature with a 0.1ºC NIST traceable thermometer (SM 9020B.4.a and 9030B.12). The laboratory was recording the temperature from the waterbath incubators internal digital thermometer. A data logger is acceptable.

13. Microbiology pipettes need to be decontaminated in disinfectant solution before discarding (SM 1090H.2). The analyst stated that the disposable pipettes were discarded without decontamination.

14. Microbiology records for media and reagents need to include the date received and opened in a logbook or computer file (SM 9020B.5.j and 5.j.7).

Pursuant to A.A.C. R9-14-605.G, Pace Analytical (AZ0612) is required to submit to the Department, within 30 days from the date of this letter, a written corrective action plan to correct each finding listed above with completion dates acceptable to the Department.

If you have any questions, please do not hesitate to contact me, Galan Larson, Imelda Guevara or Mary Cornell at (602) 364-0720.

Sincerely, Isaac Robert Program Manager Office of Laboratory Licensure and Certification Bureau of State Laboratory Services

IR: mc cc: File

Exhibit 1

Douglas A. Ducey | Governor Cara M. Christ, MD, MS | Director

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