Presentation on theme: "ISO Calibration Verification of Spark Emission Spectrometers"— Presentation transcript:
1ISO 17025 Calibration Verification of Spark Emission Spectrometers
2Presented 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:
3Canalytical 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.
5QS9000 Calibration work for QS 9000 companies to be performed by: the manufacturer’s direct representative.ORAccredited to ISO/IEC Guide 25 or ISO/IEC 17025
6TS16949ISO/TS will require that all suppliers comply with ISO and that all independent test and calibration lab sub-contractors be accredited to the standard.
7Challenges 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 SteelManufactures are not consistent with acceptance criteria.
15Sample Data Certified Measured Standard Number of Coverage 95% Content %UncertaintyDeviationMeasurementsDeltaFactorConfidenceYunKUY-UY+UBAS 4060.610.0100.004520.59200.6280BAS 4521.301.2640.0031.24801.2800BAS 4531.380.0201.3450.0021.32101.3690BAS 4540.800.0060.7550.0010.74700.7630CMSI 50640.340.3060.29800.3140BAS 4560.200.1670.15300.1810BAS 4580.490.4390.0080.41300.4650
16Customer receives a snapshot of each calibration curve’s integrity
17Standard Error of Estimate Summary SheetPrecision 1 SigmaStandard Error of EstimatePrecisionSEERange %Content %FactoryActualPass/FailAl0.01PASSC3.00.015Co0.20.0015Cr1.00.0035FAILCu0.5Mg0.050.022Mn0.009Mo0.005Ni0.004P0.0006S0.002Si2TiV0.0005
18Cover Letter Includes: Definitions Exceptions, trends with recommended plans of actionFormulas
19Definitions 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 1009Precision (Repeatability)The agreement among repeated measurements, usually expressed as repeatability or reproducibility. The precision is the Relative Standard Deviation (1 sigma).RangeThe analytical range of the calibration curve(s) of the particular element in the alloy tested. Represented in percent unless otherwise stated.ContentThe content of the sample, in percent, at which the comparison for precision was taken.AlphaThe slope of the comparison between the analysis mean of the element and the Certified Value.DeltaThe difference between the actual certified value and the measured content.Y-UThe measured content less the sum of the standard uncertainty and instrument confidence (U).Y+UThe measured content plus the sum of the standard uncertainty and instrument confidence (U).
20Certificate Requirements Name, Address, Instrument, SN.Elements, Exceptions, Standards.Environmental ConditionsUncertainty of MeasurementEvidence of Traceability
22Customer 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