Ref. No. [UMCES] CBL 2013-020
ACT VS12-03
Audits
Three types of audits were performed during the verification test: a PE audit of the
reference method measurements (GC-MS analyses), a technical systems audit (TSA) of the
verification test performance, and a data quality audit.
Performance Evaluation Audit
A PE audit was conducted to assess the quality of the reference method measurements
(GC-FID analyses) made in this verification test. The reference method PE audit was performed
by supplying “blind” PE samples to TestAmerica, in Sacramento, CA as part of the laboratory
tests.
A quantitative hydrocarbon standard for TPH analysis was formulated from freshly
opened vial of #2 Diesel Fuel Oil (5000 ppm in methanol; Spex Certiprep S-WDF-25;
Lot#T1101213004) using a 1:10000 dilution in MilliQ water for a final concentration of 500 ppb
directly in the sampling jars provided by Test America. These spiked samples were shipped to
and analyzed by Test America along with lab test samples for the same challenge compound.
One of the spiked replicate samples was lost during transport. For the remaining blind sample
the Test America analysis report indicated a TPH content of 410 ppb compared to the calculated
original concentration of 500 ppb, or an underestimate of TPH of 18% by Test America.
Comparison of paired samples from the laboratory tests with the same lot of #2 Diesel Fuel CRM
indicated an average underestimate of predicted TPH of 9.5%.
Technical Systems Audit
Two TSAs were performed during this verification. The ACT Quality Manager
performed a TSA on May 24-25, 2011 at Moss Landing Marine Laboratory during the initial
laboratory tests; and the ACT Chief Scientist performed a TSA on October 31-November 2,
2011 during the tank tests at the Bedford Institute of Oceanography. The purpose of the TSAs
was to assess and document the conformance of on- site testing procedures with the requirements
of the Test Protocols and associated SOPs. The TSAs consisted of observations of instrument
deployments, reference sample collections and analysis, and data acquisition and handling
procedures. The TSAs also included an inspection of test records and documents, e.g., chain of
custody (COC) documentation, record books, and instrument calibration logs. The audits
confirmed that:
Test instrument set-up and deployment was performed according to the Test Protocols and
vendor instructions.
Reference sample preparation procedures were performed according to the Test Protocols
requirement.
Test documentation provided a complete and traceable record of reference sample collection
and analysis.
Equipment used in the test was calibrated and monitored according to Test Protocols
requirements and standard laboratory procedures.
There were no adverse findings. However, there were a number of deviations in the test
procedures specified in the Test Protocols. These deviations are documented in this report and
had no negative effects on the test data quality and objectives.
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