Parsons ES Evaluator: Tammy Chang

AFCEE Observer: Ed Brown

CSSA Observer: Brian Murphy

DataChem Representatives: Bob Di Rienzo, Kevin Griffiths, Richard Wade, Mitchell Peterson

The following findings were identified during the on-site evaluation by Parsons ES evaluator. The final evaluation report will be sent upon completion by October 22, 1999.

  1. SW 846 Method 8330

  1. Not all refrigerators or walk-in coolers being used for explosive samples, extracts and standards had a Min/Max thermometer to monitor the temperature over weekends and holidays or possible indoor power outage.

  2. The repipetor for acetonitrile was being shared between two laboratories with two different organic solvents.

  3. Analyst did not write down the traceablity of the sodium chloride being used in the sample preparation.

  4. Analyst did not use balance to check the weight of soil samples during the drying process to ensure that constant weight has been achieved as instructed in the SW 846 method 8330.

  5. Analyst did not know the acceptance criteria for the daily calibration of the top-load balance.

  6. Analyst could not locate the Certificate of Analysis for 3,4-Dinitrotoluene (20CS5958) which was being used as the surrogate.

  7. There was not a Retention Time Window Study conducted as required in the section 8.5 of the SOP. QA Manager stated that retention window is set at the wider range of ±0.05 min of the CCV and ± three times standard deviation of the three replicate injections.

  8. Analyst did not give a satisfactory answer when asked what is the reason for using ortho-cresol as the internal standard during the analysis.

  9. Analyst gave conflicting answers during the interview when asked what are the acceptance criteria of the retention time for the internal standard.

  10. Some run logs did not contain unique identification numbers for CCVI, CCV2, etc.

  11. Analyst assigned one week expiration date for each CCV prepared. Section 5.5 of the SW 846 method 8330 requires all calibration standards must be prepared fresh on the day of calibration.

  12. Section 8.2 of the SOP states that the concentration of ICV and CCS is the same as the calibration standard SW8330/#5 in Table 3 which is 1000 ppb. However, the analyst used 200 ppb as the concentration of ICV and CCS.

  13. The analyst was not familiar with manual calculation for CCS check.

  14. There was not an SOP and a training program for manual integration.

  15. Analyst did not calibrate secondary column for every AFCEE project.

  16. Analyst was calibrating the primary column with standards concentration ranging from 2 ppb to 1000 ppb. However, section 8.1 of the SOP states that the calibration ranges for water samples are generally ranging from 0.2 ppb to 200 ppb depending on the analyte.

  17. Analyst did not follow section 9.6.1 of the SOP to include a standard at the low end of the calibration range before and after the field sample.

  18. In an analyst reviewed data package, analyst misidentified and misreported a target analyte from the secondary column chromatogram of one sample.

  1. Sample Receipt, Storage, Preservation, Custody and Disposal

  1. The sample custodian checks the accuracy of the laser thermometer by reading it in 4°C walk in cooler. However, the analyst did not know the acceptance criteria for the laser thermometer.

  2. The sample custodian did not keep a record of the daily laser thermometer check.

  1. Safety and Instrumentation Maintenance

  1. Gloves and lab coats were not consistently be worn when working with samples.

  2. Boxes were stored in hallways.

  3. After out of control events with the instrument (LC8), there was no documentation in the instrument maintenance logbook to show system was brought back in control.

  1. QC Function

  1. Section 2.2.2 of DataChem’s QAPP states that QA Manager is responsible to conduct and document an annual internal audit of laboratory procedures. QA Manager has not conducted any internal audits and is not planning to perform one.

  2. There was no data review system in writing (such as a checklist) to be followed by the analysts, peer reviewers and project managers.

Tammy Chang

October 12, 1999

Tammy Chang, Parsons ES