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PMI Just In CasePositive Material IdentificationFerritscope TestingQUALITY DOCUMENTCALIBRATION OF NITON XRF ALLOY ANALYSERDOCUMENT NoQD-CAL-PMI-01REVISION02DATE10th June 2012PMI JUST IN CASE, Fern House, 32 Fern Valley, Crook, Co. Durham, DL15 9PZTel: 01388 763527 Mob: 07846 185234 e-mail: enquiries@pmijustincase.co.uk web: www.pmijustincase.co.uk
PMI-Just In CaseCalibration ProcedureContentsRevision 02th10 June ion9.0ReportingAppendix ICertificate of Self CalibrationAppendix IIAnnual Calibration CertificateAppendix IIICertified Reference Material (CRM) CertificateUncontrolled when printedQD-CAL-PMI-01Page 1 of 7
PMI-Just In CaseCalibration Procedure1.0PurposeTo define the scope and method of carrying out calibration of a Niton XRF Alloy Analyser.2.0ScopeThis procedure is a standard procedure that describes the methods for carrying outcalibration using the in-built self-calibrating function of the Niton XRF Alloy Analyser and alsoan annual comparison check against a Certified Reference Material (CRM) of knownchemical analysis.3.0ReferencesNiton XL3T 800 Alloy Analyser Operating Manual.API RP578 – Material Verification Program for New and Existing Alloy Piping SystemsPositive Material Identification Procedure QD-PMI-014.0DefinitionsPMI(Positive Material Identification)Physical testing of materials to determine the chemical composition and positively verifymaterial composition by determining the alloy content of a component or a weld without theneed to remove samples for analysis.XRF(X-ray Fluorescence Spectroscopy)A method of PMI using a portable X-ray fluorescence analyser to verify the chemicalelements that establish the positive identification for a particular material.When activated on a test item, an XRF analyser produces short wavelength electromagneticrays. These emitted rays interact with (excite) certain elements. As a result, the excitedelements then re-emit a new wavelength within a discrete energy band that is identifiable bythe analyser.When used along with material standards, the portable analyser can determine approximatechemical quantities for the target elements.CRM (Certified Reference Material)A reference material with one or more properties whose values are certified by a technicallyvalid procedure accompanied by or traceable to a certificate or other documentation, which isissued by a Certifying Body.5.0ResponsibilitiesPersonnel applying this procedure shall be familiar with this procedure and be competent inthe use of a Niton XL3T 800 Alloy Analyser6.0Safety All equipment shall be inspected for obvious defects prior to calibration.Revision 02th10 June 2012Uncontrolled when printedQD-CAL-PMI-01Page 2 of 7
PMI-Just In CaseCalibration Procedure7.0EquipmentPMI test equipment and its calibration shall meet the following criteria: Be suitable for the range of material compositions to be verifiedBe suitable for the range of surface curvatures and orientations to be encountered suchas welds and small bore fittings.Be sufficiently portable to gain access to each checkpoint under evaluation.Be capable of providing ‘direct read-out’ quantative results (% composition) of therequired chemical elements.8.0Calibration8.1For standard inspection the Niton XL3T 800 Alloy Analyser detector shall be used as acomparator check analysis during set-up.Activation of the analyser self calibration mechanism must only be done by authorised PMIJust In Case personnel.i.ii.iii.iv.v.Once the machine is switched on select ‘Utilities’ on the screen menuSelect ‘Calibrate’Select ‘Calibrate Detector’ – the analyser will automatically begin thecalibration cycle which takes approximately 1 minute.RES will appear once calibration is complete – ensure RES is under 220eV.If RES is greater than 220eV quarantine analyser and consult with Niton UK.These set-up checks shall be carried out as a minimum: Each time the analyser is switched onand re-confirmed at least at the following times: 8.2At intervals not exceeding each 50 determinations carried outEach time a different Standard or material range is requiredIf there is a significant change in equipment or material temperatureWhenever the equipment has been accidently knocked or adjustedWhenever any error is suspectedImmediately at the end of a work sessionA comparison check against a Certified Reference Material (CRM) must be done annually asa minimum. The CRM grade 1¼ Chromium and ½ Molybdenum is certified by AnalyticalReference Materials International and bears the Part Number (Q.A.No): IARM 35HN.i.ii.iii.iv.Revision 02th10 June 2012Obtain 5 readings (minimum of 20 seconds per reading) of the CRMRecord all readings on Calibration Certificate – see appendix IICalculate mean readings for Molybdenum (Mo), Iron (Fe), Manganese (Mn)and Chromium (Cr) and compare against CRM Certificate No 35HN01112007-IARM-P.In the event of sporadic, inconsistent readings quarantine the analyser andconsult with Niton UK.Uncontrolled when printedQD-CAL-PMI-01Page 3 of 7
PMI-Just In CaseCalibration Procedure9.0ReportingOn completion of self calibration, in accordance with section 8.1 above, the operator mustdate and sign the Certificate of Calibration – refer to Appendix I.Reporting of the comparison check against the CRM must be done annually as a minimum –refer to Appendix II.Certified Reference Material (CRM) – refer to Appendix III.All records to be kept for a minimum of 3 years.Revision 02th10 June 2012Uncontrolled when printedQD-CAL-PMI-01Page 4 of 7
PMI-Just In CaseCalibration ProcedureAPPENDIX IRevision 02th10 June 2012Uncontrolled when printedQD-CAL-PMI-01Page 5 of 7
PMI-Just In CaseCalibration ProcedureAPPENDIX IINITON XL3T 800 ALLOY ANALYSER - CALIBRATION CERTIFICATESERIAL No:47632Certified Reference Material (CRM): Grade 1¼Cr ½Mo / UNS K11572 Part No (Q.A.No): IARM 35HNReading12345MeanTime08/06/2012 20:2208/06/2012 20:2308/06/2012 20:2308/06/2012 20:2408/06/2012 20:25Alloy11 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.00SbSb Error SnSn Error PdPd Error AgAg Error AlAl Error LOD0.024 LOD0.035 LOD0.025 LOD0.177 LOD80 LOD0.024 LOD0.035 LOD0.026 LOD0.214 LOD80 LOD0.026 LOD0.036 LOD0.025 LOD0.209 LOD80 LOD0.024 LOD0.034 LOD0.024 LOD0.187 LOD80 LOD0.023 LOD0.036 LOD0.025 LOD0.188 LOD80 LOD LOD LOD LOD LODMoMo Error NbNb Error0.5000.015 LOD0.0040.4910.015 LOD0.0040.4820.015 LOD0.0040.4990.014 LOD0.0040.5010.015 LOD0.0040.495 LODReading12345MeanTime08/06/2012 20:2208/06/2012 20:2308/06/2012 20:2308/06/2012 20:2408/06/2012 20:25Alloy11 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.00ZrZr Error BiBi Error PbPb Error SeSe Error WW Error ZnZn Error CuCu Error LOD0.003 LOD0.008 LOD0.023 LOD0.007 LOD0.063 LOD0.024 0.1550.034 LOD0.003 LOD0.002 LOD0.015 LOD0.007 LOD0.066 LOD0.025 0.1470.034 LOD0.003 LOD0.007 LOD0.002 LOD0.006 LOD0.064 LOD0.022 0.1950.037 LOD0.003 LOD0.007 LOD0.004 LOD0.006 LOD0.065 LOD0.021 0.1660.034 LOD0.003 LOD0.002 LOD0.014 LOD0.006 LOD0.061 LOD0.025 0.1820.036 LOD LOD LOD LOD LOD LOD LODReading12345MeanTime08/06/2012 20:2208/06/2012 20:2308/06/2012 20:2308/06/2012 20:2408/06/2012 20:25Alloy11 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.001 1/4 Cr : 0.00NiNi Error CoCo Error FeFe Error MnMn Error0.0930.045 LOD0.289 97.510.185 0.6140.0650.1330.047 LOD0.286 97.530.185 0.5290.0660.1160.046 LOD0.287 97.490.184 0.5690.0650.0980.043 LOD0.279 97.490.181 0.6120.0640.1310.047 LOD0.287 97.520.184 0.5890.063 LOD LOD97.510.583CrCr Error VV Error1.1120.05 LOD0.0491.0930.05 LOD0.0551.1140.05 LOD0.0541.1060.049 LOD0.051.1310.05 LOD0.0551.111 LODTiTi Error LOD0.083 LOD0.08 LOD0.074 LOD0.084 LOD0.076 LODLOD Lack of DetectionDATE OF NEXT CALIBRATION – 8th JUNE 2013Revision 02th10 June 2012Uncontrolled when printedQD-CAL-PMI-01Page 6 of 7
PMI-Just In CaseCalibration ProcedureAPPENDIX IIIRevision 02th10 June 2012Uncontrolled when printedQD-CAL-PMI-01Page 7 of 7
CALIBRATION OF NITON XRF ALLOY ANALYSER DOCUMENT No QD-CAL-PMI-01 REVISION 02 DATE 10th June 2012 PMI JUST IN CASE, Fern House, 32 Fern Valley, Crook, Co. Durham, DL15 9PZ Tel: 01388 763527 Mob: 07846 185234 e-mail: enquiries@pmijustincase.co.uk web: www.pmijustincase.co.uk PMI Just In Case Positive Material Identification
