Transcript Canalytical Instrumentation Services Inc. 1110 Heritage

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
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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.
Why ISO 17025
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
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
• 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.
Process to Accreditation
Requirements for ISO17025
• Development of Quality Manual
• Acceptance criteria of Spark emission
spectrometers?
Criteria of Acceptance
Precision
Accuracy
Test Uncertainty Ratio of 4:1 as Compared
to Factory Specifications
Measurement Uncertainty
• Type B Evaluation of Standard Uncertainty
– As per NIST Technical Note 1297
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
• 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
Includes
Sample Data
Standard
Certified
Certified
Measured
Standard
Number of
Content %
Uncertainty
Content %
Deviation
Measurements
Y
u
n
Delta
Coverage
95%
Factor
Confidence
K
U
Y-U
Y+U
BAS 406
0.61
0.010
0.61
0.004
5
0.00000
2
0.00800
0.5920
0.6280
BAS 452
1.30
0.010
1.264
0.003
5
0.03600
2
0.00600
1.2480
1.2800
BAS 453
1.38
0.020
1.345
0.002
5
0.03500
2
0.00400
1.3210
1.3690
BAS 454
0.80
0.006
0.755
0.001
5
0.04500
2
0.00200
0.7470
0.7630
50
64
0.34
0.004
0.306
0.002
5
0.03600
2
0.00400
0.2980
0.3140
BAS 456
0.20
0.010
0.167
0.002
5
0.03300
2
0.00400
0.1530
0.1810
BAS 458
0.49
0.010
0.439
0.008
5
0.05100
2
0.01600
0.4130
0.4650
CMSI
Customer receives a snapshot of
each calibration curve’s integrity
Measured vs Certified
1.2
1
Ce rtifie d
0.8
0.6
0.4
0.2
0
0
0.2
Measured
0.4
0.6
0.8
1
1.2
y = 1.0004x - 0.0095
R2 = 0.9976
Summary Sheet
Standard Error of
Estimate
Precision 1 Sigma
Precision
SEE
Range %
Content %
Factory
Actual
Factory
Actual
Pass/Fail
Pass/Fail
Al
0.005 - 0.1
0.01
0.00025
0.000122
0.002786
0.005084
PASS
PASS
C
1.5 - 4.0
3.0
0.015
0.021945
0.048572
0.096287
PASS
PASS
Co
0.001 - 0.3
0.2
0.0015
0.005423
0.004626
0.017967
PASS
PASS
Cr
0.1 - 2.0
1.0
0.0035
0.004934
0.015657
0.135717
PASS
FAIL
Cu
0.1 - 1.0
0.5
0.0035
0.000999
0.009469
0.031859
PASS
PASS
Mg
0.02 - 0.1
0.05
0.022
0.003598
0.002309
0.008276
PASS
PASS
Mn
0.05 - 2.0
1.0
0.009
0.004587
0.013280
0.019135
PASS
PASS
Mo
0.3 - 0.5
0.5
0.005
0.003161
0.010447
0.023419
PASS
PASS
Ni
0.2 - 2.0
1.0
0.004
0.003264
0.025343
0.046243
PASS
PASS
P
0.001 - 0.1
0.05
0.0006
0.002159
0.002474
0.002928
PASS
PASS
S
0.001 - 0.1
0.05
0.002
0.006611
0.002077
0.006793
PASS
PASS
Si
1.0 - 3.0
2
0.01
0.013916
0.045782
0.059672
PASS
PASS
Ti
0.01 - 0.1
0.01
0.00022
0.000222
0.002985
0.009629
PASS
PASS
V
0.001 - 0.1
0.05
0.0005
0.000253
0.004599
0.003665
PASS
PASS
Cover Letter
• Includes:
– Definitions
– Exceptions, trends with recommended plans
of action
– Formulas
Definitions
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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
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Name, Address, Instrument, SN.
Elements, Exceptions, Standards.
Environmental Conditions
Uncertainty of Measurement
Evidence of Traceability
In Conclusion
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
Identify Trends
Measured vs Certified
0.2000
0.1800
0.1600
Ce r tifie d
0.1400
0.1200
0.1000
0.0800
0.0600
0.0400
0.0200
0.0000
0
0.02
Measured
0.04
0.06
0.08
0.1
0.12
y = 1.1035x + 0.0046
R2 = 0.997
Identified trends
Improved customers accuracy
Identified hardware issues through precision
The End