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ISO 17025 Calibration Verification of Spark Emission Spectrometers - PowerPoint PPT Presentation


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ISO 17025 Calibration Verification of Spark Emission Spectrometers. Presented by Ken Suddaby Canalytical Instrumentation Services Inc. 1110 Heritage Road, Unit 7 Burlington, Ontario Canada L7L 4X9 Tel: 905 331 3386 Fax: 905 331 3388. Canalytical. Incorporated in 1997.

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Presented byKen SuddabyCanalytical Instrumentation Services Inc.1110 Heritage Road, Unit 7Burlington, OntarioCanadaL7L 4X9 Tel: 905 331 3386Fax: 905 331 3388

canalytical
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.
qs9000
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
ts16949
TS16949

ISO/TS 16949 will require that all suppliers comply with ISO 17025 and that all independent test and calibration lab sub-contractors be accredited to the standard.

challenges to accreditation
Challenges to Accreditation
  • No Defined Standard to Certify compliance of Spark Emission performance.
  • ASTM only have recommended methods and practices. ie ASTM- E1009-95 Standard practice for Evaluating an Optical Emission Vacuum Spectrometer to Analyze Carbon and Low-Alloy Steel
  • Manufactures are not consistent with acceptance criteria.
requirements for iso17025
Requirements for ISO17025
  • Development of Quality Manual
  • Acceptance criteria of Spark emission spectrometers?
criteria of acceptance
Criteria of Acceptance

Precision

Accuracy

Test Uncertainty Ratio of 4:1 as Compared to Factory Specifications

measurement uncertainty
Measurement Uncertainty
  • Type B Evaluation of Standard Uncertainty
    • As per NIST Technical Note 1297
precision
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.
determination of accuracy
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.
the report

The Report

Includes

cover letter
Cover Letter
  • Includes:
    • Definitions
    • Exceptions, trends with recommended plans of action
    • Formulas
definitions
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).
certificate requirements
Certificate Requirements
  • Name, Address, Instrument, SN.
  • Elements, Exceptions, Standards.
  • Environmental Conditions
  • Uncertainty of Measurement
  • Evidence of Traceability
customer summary
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 17025 Certification
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Identified trends

Improved customers accuracy

Identified hardware issues through precision