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ISO Calibration Verification of Spark Emission Spectrometers

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Presentation on theme: "ISO Calibration Verification of Spark Emission Spectrometers"— Presentation transcript:

1 ISO 17025 Calibration Verification of Spark Emission Spectrometers

2 Presented by Ken Suddaby Canalytical Instrumentation Services Inc
Presented by Ken Suddaby Canalytical Instrumentation Services Inc Heritage Road, Unit 7 Burlington, Ontario Canada L7L 4X9 Tel: Fax:

3 Canalytical Incorporated in 1997.
Sales and service representative for several manufacturers whose products include Spark Emission, ICP and Mercury Analyzers. Provider of 3rd party service on various spectrometer brands.

4 Why ISO 17025

5 QS9000 Calibration work for QS 9000 companies to be performed by:
the manufacturer’s direct representative. OR Accredited to ISO/IEC Guide 25 or ISO/IEC 17025

6 TS16949 ISO/TS will require that all suppliers comply with ISO and that all independent test and calibration lab sub-contractors be accredited to the standard.

7 Challenges to Accreditation
No Defined Standard to Certify compliance of Spark Emission performance. ASTM only have recommended methods and practices. ie ASTM- E Standard practice for Evaluating an Optical Emission Vacuum Spectrometer to Analyze Carbon and Low-Alloy Steel Manufactures are not consistent with acceptance criteria.

8 Process to Accreditation

9 Requirements for ISO17025 Development of Quality Manual
Acceptance criteria of Spark emission spectrometers?

10 Criteria of Acceptance
Precision Accuracy Test Uncertainty Ratio of 4:1 as Compared to Factory Specifications

11 Measurement Uncertainty
Type B Evaluation of Standard Uncertainty As per NIST Technical Note 1297

12 Precision CRM is Analyzed for 5 consecutive burns to obtain the Standard Deviation Compared to the Instrument Manufacturers’ published precision data at the various levels of concentration.

13 Determination of Accuracy
Calculate the Standard Error (SE) from the Delta of the CRMs. Compare this data to The Calculated Standard Error (SE) of the CRMs from their Confidence level.

14 The Report Includes

15 Sample Data Certified Measured Standard Number of Coverage 95%
Content % Uncertainty Deviation Measurements Delta Factor Confidence Y u n K U Y-U Y+U BAS 406 0.61 0.010 0.004 5 2 0.5920 0.6280 BAS 452 1.30 1.264 0.003 1.2480 1.2800 BAS 453 1.38 0.020 1.345 0.002 1.3210 1.3690 BAS 454 0.80 0.006 0.755 0.001 0.7470 0.7630 CMSI 5064 0.34 0.306 0.2980 0.3140 BAS 456 0.20 0.167 0.1530 0.1810 BAS 458 0.49 0.439 0.008 0.4130 0.4650

16 Customer receives a snapshot of each calibration curve’s integrity

17 Standard Error of Estimate
Summary Sheet Precision 1 Sigma Standard Error of Estimate Precision SEE Range % Content % Factory Actual Pass/Fail Al 0.01 PASS C 3.0 0.015 Co 0.2 0.0015 Cr 1.0 0.0035 FAIL Cu 0.5 Mg 0.05 0.022 Mn 0.009 Mo 0.005 Ni 0.004 P 0.0006 S 0.002 Si 2 Ti V 0.0005

18 Cover Letter Includes: Definitions
Exceptions, trends with recommended plans of action Formulas

19 Definitions Standard Error (SE) or Standard Error of Estimate (SEE)
This is a measure of how well a calibration has been defined; Standard Error (SE) is used in this practice as an indicator of accuracy. It is CRM (Certified Reference Material) dependant and instrument operator dependant. ATSM E 1009 Precision (Repeatability) The agreement among repeated measurements, usually expressed as repeatability or reproducibility. The precision is the Relative Standard Deviation (1 sigma). Range The analytical range of the calibration curve(s) of the particular element in the alloy tested. Represented in percent unless otherwise stated. Content The content of the sample, in percent, at which the comparison for precision was taken. Alpha The slope of the comparison between the analysis mean of the element and the Certified Value. Delta The difference between the actual certified value and the measured content. Y-U The measured content less the sum of the standard uncertainty and instrument confidence (U). Y+U The measured content plus the sum of the standard uncertainty and instrument confidence (U).

20 Certificate Requirements
Name, Address, Instrument, SN. Elements, Exceptions, Standards. Environmental Conditions Uncertainty of Measurement Evidence of Traceability

21 In Conclusion

22 Customer Summary A quick visual of each analytical line.
Provides the statistical data for each analytical line. Includes: Standard Deviation of each CRM, Variance, 95% Confidence level, Measurement Uncertainty, Standard Error of the range tested. Also provide the R2 Value and alpha. ISO Certification

23 Identify Trends

24 Identified trends Improved customers accuracy Identified hardware issues through precision

25 The End


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