Observations & Trends From Inorganic & Organic MAPEP Data

1. Observations & Trends From Inorganic & Organic MAPEP Data Loren R Jose, Mary Verwolf Radiological and Environmental Sciences Laboratory September 22, 2010 DOECAP ASP 2010 Workshop Seattle, Washington

2. Topics False Positive/Negative Tests Random Reporting Errors Letters of Concern Examples of Historical Trending using the MAPEP Database

3. False Positive/Negative Testing False Positive: The analyte is reported as being present in a sample, when in fact it is not detectable in the sample. False Negative: The analyte is reported as not being present in a sample, when in fact it is detectable in the sample.

4. Example of Organic False Positive/Negative Results • Footnotes on MAPEP Report: • = False Positive • = False Negative

5. Examples of Inorganic False Positive/Negative Results Footnotes on MAPEP Report: (1) = False Positive (2) = False Negative

6. Random Reporting Errors Calculation errors resulting in: Reporting results in the wrong units i.e. µg/L instead of mg/L Dilution errors Concentration of original sample versus serial dilutions Reporting the wrong isomers for organic analytes

7. Criteria for Letters of Concern • Not acceptable performance for a targeted analyte in same matrix for the two consecutive test sessions (DOECAP Priority 1 Finding) Pu-238 +N (MaS13) -N (MaS14) • Not acceptable performance for a targeted analyte in two or more sample matrices for the current test session Cs-137 +N (MaW14) +N (MaS14)

8. Criteria for Letters of Concern (cont.) • Consistent bias, either positive or negative, at the “Warning” level for a targeted analyte in the same matrix for the two most recent test sessions Sr-90 +W (RdF13) +W (RdF14) • Quality issues (flags other than “Acceptable”) that weren’t identified by the above criteria for a targeted analyte in a given sample matrix over the last three test sessions Am-241 -N (MaS12) +W (MaS13) -N (MaS14)

9. Criteria for Letters of Concern (cont.) • Any other performance indicator and/or historical trend that demonstrates an obvious quality concern Pu-238 F+ (MaS12) F+ (RdV13) F+ (RdF14)

10. Class 4 Concern • Internal trending • Laboratories that stop reporting data because of a quality problem Pu-238 +N (MaS13) -N (MaS14) NR (MaS15) Sr-90 F+ (MaW13) F+ (MaW14) NR (MaW15)

11. Other Benefits The MAPEP program helps identify and solve analytical problems by: • Direct technical assistance • Studying the data collected • The MAPEP database is unique because the analytical methodology used for each reported result is captured • Many interesting questions can be examined because of this unique feature • Examples

18. Inorganic Trending Examples Are you using the appropriate sample preparation technique for inorganic analytes? Antimony in Soil Selenium in Soil Total Uranium in Soil by Mass Spec

19. Inorganic Sample Preparation Methods Sample preparation method choice dependent on: Analyte – not all analytes can be reported from one sample prep method Matrix – not all matrices require the same sample prep method

20. Conclusions • Letters of Concern convey important potential quality problems that can be corrected before a non conformance occurs • It is difficult, for many laboratories, to maintain acceptable performance for all analytes • MAPEP plays a crucial role in identifying analytical problems that are otherwise difficult to recognize

21. Conclusions (cont) • DOE oversight and contracting personal need to follow up, examine, and ensure the quality issues are corrected before analytical services are procured • MAPEP will provide technical assistance whenever possible