Is Your Analytical Result Accurate? Presented By: James S. Smith, Ph.D. Trillium, Inc. GSA North-Central Section 39 th Annual Meeting Minneapolis, Minnesota.

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Presentation transcript:

Is Your Analytical Result Accurate? Presented By: James S. Smith, Ph.D. Trillium, Inc. GSA North-Central Section 39 th Annual Meeting Minneapolis, Minnesota May 20, 2005

Analytical Chemistry 1. Qualitative – Identity of the analyte 2. Quantitative – How much is in the sample

Problem Beginning Mr./Ms. Name Plant Manager CompanyAddress Re: Notice of Violation and Assessment of Civil Penalties Dear Mr./Ms. Name:

Violation Plant Effluent into the POTW Sewer Maximum amount of mercury (Hg) in the effluent for the plant’s use permit is 150 ng/L (parts per trillion)

Results MonthHg Concentration (ng/L) December180 January210 February120 March130 April 10:30 AM810 11:15 AM210

Questions 1. Is there an analytical chemistry problem? 2. If there is an analytical chemistry problem then is the problem a. Qualitative? b. Quantitative? c. Both?

Analytical Method U.S. EPA Method 1531 Revision E Mercury in Water by Oxidation, Purge and Trap, Cold Vapor Atomic Fluorescence Spectrometry

Sampling must be accomplished using U.S. EPA Method 1669: Sampling Ambient Water for Determination of Trace Metals at EPA Water Quality Criteria Levels. MDL is 0.2 ng/L.

Laboratory/Samplers 1. Certified by the State for Methods 1669 and Laboratory has a clean room for the low level mercury analysis. 3. Calibration from 0.5 to 100 ng/L is excellent.

Calibration Curve

Regression Data ConcentrationArea (ng/L) R 2 =

Quality Control Precision Original analysis210 ng/L 1 st replicate210 ng/L 2 nd replicate200 ng/L Each sample was diluted by a factor of 10.

Blanks Instrument Blank16,748 16,28917,442 Method Blank21,459 = 0.1 ng/L 23,866

Check Standards5.0 ng/L found5.0 ng/L found5.2 ng/L

Method of Standard Additions (MSA) U.S. EPA SW-846, Method 7000A, Section 8.7 The standard addition technique involves adding known amounts of standard to one or more aliquots of the processed sample solution. This technique compensates for a sample constituent that enhances or depresses the analyte signal, thus producing a different slope from that of the calibration standards.

Standard Addition Plot

Mercury Analysis by the Method of Standard Additions Spike Concentration Original Concentration Expected Concentration Measured Concentration 10 ng/L 20 ng/L 30 ng/L 40 ng/L 21 ng/L 21 ng/L 21 ng/L 21 ng/L 31 ng/L 41 ng/L 51 ng/L 61 ng/L 23 ng/L 31 ng/L 33 ng/L 34 ng/L

MSA Results

Regression Data Spike ConcentrationArea (ng/L) R 2 =

Conclusion Accuracy of the Hg analysis is wrong. There may not be any Hg in the sample. The MSA can be used for any analysis as a check on its accuracy.