George E. Detsis Manager, Analytical Services Program United States Department of Energy Office of Health, Safety and Security Office of Sustainability Support TNI Semi-Annual Meeting -- Forum on Laboratory Accreditation Louisville, Kentucky January , 2014

 Department of Energy Consolidated Audit Program Overview  DOE Findings and Causal Analysis Examples

Department of Energy Consolidated Audit Program (DOECAP) Improves Data Quality Confidence Reduction Costs and Liability. The DOECAP Program eliminates the potential for more than 90 additional field audits with a cost savings to DOE in excess of $3.6M per year. Department of Energy Consolidated Audit Program (DOECAP) U.S. Department of Energy P.O. Box 2001, 1916-T2 Oak Ridge, Tennessee Phone: Fax:

 FindingThe laboratory analyst uses an acceptance criterion for metals reagent water quality that does not meet the analytical SOPs. (Priority II) (Laboratory 7751, Rev. 6; Laboratory 7768, Rev. 2.2)  Discussion The SOP Laboratory 7751, Inductively Coupled Plasma Atomic Emission Spectrometry Metals Analysis, and Laboratory 7768, Inductively Coupled Plasma – Mass Spectrometry Element/Metals Sample Preparation and Analysis, Section 9.2, both specify reagent water with electrical resistivity of 18 or greater mega ohm-cm (Mohm-cm). The audit team’s interviews with the laboratory analyst indicate that the electrical resistivity of the reagent water used for trace metals analysis is at least 10 Mohm-cm, which does not meet the SOP requirements. The purified water system in Laboratory C-106 is equipped with an inline resistivity meter, and the meter is marked at 10 Mohm-cm to indicate the acceptability criterion. It should be noted that Laboratory is meeting the ASTM Type II water quality criterion of at least 1 Mohmcm and the EPA SW-846 reagent water definition.

 FindingThe laboratory analyst uses an acceptance criterion for metals reagent water quality that does not meet the analytical SOPs. (Priority II) (Laboratory 7751, Rev. 6; Laboratory 7768, Rev. 2.2)  Discussion The SOP Laboratory 7751, Inductively Coupled Plasma Atomic Emission Spectrometry Metals Analysis, and 7768, Inductively Coupled Plasma – Mass Spectrometry Element/Metals Sample Preparation and Analysis, Section 9.2, both specify reagent water with electrical resistivity of 18 or greater mega ohm-cm (Mohm-cm). The audit team’s interviews with the laboratory analyst indicate that the electrical resistivity of the reagent water used for trace metals analysis is at least 10 Mohmcm, which does not meet the SOP requirements. The purified water system in Laboratory C-106 is equipped with an inline resistivity meter, and the meter is marked at 10 Mohm-cm to indicate the acceptability criterion. It should be noted that is meeting the ASTM Type II water quality criterion of at least 1 Mohmcm and the EPA SW-846 reagent water definition.  Causal  Analysis The cause of the finding was an error of omission in the annual reviews of SOPs Laboratory 7751 and 7768 to change the water specifications. The reagent sections were being overlooked. The responsibility for this error falls upon the Quality Assurance Manager. The two SOP reagent sections had not been revised since the time that ASTM Type 1 water requirement (electrical resistivity ≥ 18 Mohm-cm [M Ω -cm]) was specified. The laboratory had adopted ASTM Type 2 water for metals which had changed from a minimum electrical resistivity of 10 to 1 M Ω -cm minimum. No issues appeared in method blanks analyzed using ASTM Type 2 water.  Detailed  Corrective  Action Plan The Laboratory SOPs 7751 and 7768 were immediately revised to reflect the ASTM Type 2 water requirement and usage. Also, the Operator Aid posted with the deionized water (DI) system was changed and the analyst responsible for monitoring the system was notified of the changes. The QAM has reviewed ALL SOPs that specify the use of DI water and made sure ALL were up to date.  Actions to  Prevent  Recurrence Fortunately the older requirements were stricter than the current ones, but this does not excuse the omission. All laboratory personnel involved in the use of the DI water have received the revised documentation. In the future, more care will be taken by the QAM and/or the recently hired QA Specialist to review all sections of the SOP with the same thoroughness.

 Finding Laboratory’s ICP/MS interference check solutions are not analyzed at the required frequency. (Priority II) (Laboratory 7768, Rev. 2.2; EPA SW-846, Method 6020A)  Discussion The SOP Laboratory 7768, Inductively Coupled Plasma – Mass Spectrometry Element/Metals Sample Preparation and Analysis, Section 11.9, and EPA SW-846, Method 6020A, Section 10.5, both require an ICP/MS interference check solution analysis to be performed at the beginning of an analytical run or once every 12 hours, whichever is more frequent.  The Laboratory performs its interference check solution analyses on an annual basis. Laboratory’s ICP/MS instrument software corrects for isobaric interferences as described in the Laboratory 7768, Sections 6 and 11.4, and the Laboratory verifies the adequacy of these corrections by performing the annual interference check solution analysis.

 Finding Laboratory’s ICP/MS interference check solutions are not analyzed at the required frequency. (Priority II) (Laboratory 7768, Rev. 2.2; EPA SW-846, Method 6020A)  Discussion The SOP Laboratory 7768, Inductively Coupled Plasma – Mass Spectrometry Element/Metals Sample Preparation and Analysis, Section 11.9, and EPA SW-846, Method 6020A, Section 10.5, both require an ICP/MS interference check solution analysis to be performed at the beginning of an analytical run or once every 12 hours, whichever is more frequent.  The Laboratory performs its interference check solution analyses on an annual basis. Laboratory’s ICP/MS instrument software corrects for isobaric interferences as described in the Laboratory 7768, Sections 6 and 11.4, and the Laboratory verifies the adequacy of these corrections by performing the annual interference check solution analysis.  Causal  Analysis The SOP Laboratory 7768 contains the SW-846 Method 6020A requirement to run the ICP/MS Interference Check Solution (ICS) at least every 12 hours when analyzing metals that may have Isobaric Interferences (IBI). Laboratory Perkin Elmer ELAN 9000 ICP/MS has within its software automatic corrections for the wide range of elemental IBI. Laboratory should have shown that the software alleviates the need for the 12 hour check and then reflected that in the SOP. The Laboratory checks of the ICS on an annual basis have shown that no issues have occurred.  Detailed  Corrective  Action Plan To assure DOECAP and our clients that the Isobaric Interferences are being handled properly, the laboratory will initiate the use of the ICS when analyzing any of the elements subject to IBI. This requirement will be ed to the analysts and a reminder of the requirement placed at the instrument. The laboratory manger will make sure the proper procedure is being followed with checks by the Quality Assurance Manager.  Actions to  Prevent  Recurrence Laboratory had assumed that capability of the instrument software with the annual checks met the Method 6020A requirements. Once the laboratory has sufficient data over multiple months to show that the routine use of the ICS is not necessary and thus the software is working properly, Laboratory will modify the SOP to include current practice.  Scheduled  Closing Date 12/31/13 to assure sufficient data has been collected per the CAP, since many of the metal analytes Laboratory performs by ICP/MS are not affected by IBI.

 Finding The laboratory does not have a system in place to record incidents involving the spillage of reagents and breakage of client samples. (Priority II) (QSAS, Rev. 2.8, Section 5.2, DOE-2)  Discussion The QSAS Manual requires the laboratory have a system in place to record spillage of reagents and samples. Each laboratory must protect the integrity of the client samples that are submitted for analysis. Spillage of reagents or solvents may impact the integrity of client samples by introducing contamination; thereby, invalidating the analytical results. No evidence was found of a system for the timely notification of clients in the event of the spillage of reagents and breakage of samples.

 Finding The laboratory does not have a system in place to record incidents involving the spillage of reagents and breakage of client samples. (Priority II) (QSAS, Rev. 2.8, Section 5.2, DOE-2)  Discussion The QSAS requires the laboratory have a system in place to record spillage of reagents and samples. Each laboratory must protect the integrity of the client samples that are submitted for analysis. Spillage of reagents or solvents may impact the integrity of client samples by introducing contamination thereby invalidating the analytical results. No evidence was found of a system for the timely notification of clients in the event of the spillage of reagents and breakage of samples.  Causal  Analysis The laboratory was unaware of a requirement to document sample and reagent spills.  Detailed  Corrective  Action Plan A protocol for recording such spills as well as a system for notifying clients will be developed.  Actions to  Prevent  Recurrence No actions should be required to prevent recurrence, once procedure and forms have been instituted.  Scheduled  Closing Date May 30, 2013