13X 30403 A
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December 2011
CERTIFICATE OF ANALYSIS
13X 30403 (batch A)
Certified Reference Material Information
Type: STAINLESS STEEL (WROUGHT)
Form and Size: Disc, 40mm diameter
Manufactured by: Stock Bar
Certified and Supplied by: MBH Analytical Ltd
Assigned Values
Percentage element by weight
Element C Si S P Mn Ni Cr
Value 1 0.0201 0.284 0.0248 0.0297 1.488 7.92 18.25
Uncertainty 2 0.0014 0.007 0.0012 0.0012 0.012 0.04 0.06
Element Mo Cu Co V Nb W N
Value 1 0.192 0.217 0.101 0.113 (0.019) 0.018 0.081
Uncertainty 2 0.003 0.004 0.003 0.003 - 0.002 0.003
Note: values given in parentheses are not certified - they are provided for information only.
Definitions
1
The certified values are the present best estimates of the true content for each element. Each value
is a panel consensus, based on the averaged results of an interlaboratory testing programme, detailed
on page 3.
2 The uncertainty values are generated from the 95% confidence interval derived from the wet analysis
results, in combination with a statistical assessment of the homogeneity data, as described on page 2.
Certified by:
on 24th December 2011
MBH ANALYTICAL LIMITED ______________
C Eveleigh
13X 30403 A
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December 2011
Method of Preparation
This reference material was produced from commercial barstock to UNS S30403. The metallurgical history is
unknown.
Sampling
Samples for chemical analysis were taken from various positions throughout the batch. At least 10% of all discs were
selected for non-destructive homogeneity testing.
Homogeneity
The discs were checked for lateral segregation, and for local and batch homogeneity using an optical emission
spectrometer.
Using the combined data from each surface, standard deviation values were derived for each element as a n indicator
of any non-homogeneity (as determined for the specific sample size taken by the spectrometer).
Chemical Analysis
Analysis was carried out on millings taken from samples representative of the product. It was performed by a panel of
laboratories operating within the terms of EN ISO/IEC 17025 - 2005, using documented standard reference methods
and validated by appropriate reference materials.
The individual values listed overpage are the average of each analyst's results.
Estimation of Uncertainties
Each element certified has been analysed by several laboratories, and 95% half-width confidence intervals (C(95%)) for
the resultant mean values have been derived by the method shown on page 3.
As a separate exercise, the degree of non-homogeneity of the batch for each element has been quantified by a
programme of non-destructive application testing, discussed above.
The final certified uncertainty for each element has been derived by combining these two factors, using the square -
root of the summed squares.
Traceability
Much of the analytical work performed to assess this material has been carried out by laboratories with proven
competence, as indicated by their accreditation to ISO 17025. It is an implicit requirement for this accreditatio n that
analytical work should be performed with due traceability, via an unbroken chain of comparisons, each with stated
uncertainty, to primary standards such as the mole, or to nationally- or internationally-recognised reference materials.
In addition, some of the results derived as part of this testing programme have traceability to NIST standards, as part
of the analytical calibration or process control.
Usage
Intended use: With optical emission and X-ray fluorescence spectrometers.
Recommended Steels are generally prepared by linishing, grinding, turning or milling. However, users
method of use: are recommended to follow the calibration and sample preparation procedures specified by
the relevant instrument manufacturer.
Preparation should be the same for reference materials and the samples for test.
The recommended sample size is at least five replicate analyses. Users are advised to
check against possible bias between reference materials and production samples due to
differences in metallurgical history, and be aware of possible inter-element effects.
13X 30403 A
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December 2011
Analytical Data
Percentage element by weight
Sample C Si S P Mn Ni Cr
1 0.0162 0.273 0.0220 0.0283 1.458 7.858 18.16
2 0.0177 0.275 0.0226 0.0284 1.472 7.867 18.16
3 0.0178 0.276 0.0240 0.0286 1.473 7.889 18.16
4 0.0186 0.278 0.0243 0.0286 1.475 7.890 18.21
5 0.0195 0.283 0.0244 0.0289 1.484 7.920 18.25
6 0.0200 0.285 0.0247 0.0295 1.491 7.923 18.28
7 0.0210 0.288 0.0248 0.0304 1.492 7.930 18.30
8 0.0215 0.289 0.0256 0.0306 1.496 7.985 18.31
9 0.0218 0.289 0.0258 0.0307 1.499 8.000 18.32
10 0.0220 0.291 0.0260 0.0310 1.500 18.33
11 0.0220 0.295 0.0262 0.0317 1.504
12 0.0232 0.0267 1.513
Mean 0.0201 0.284 0.0248 0.0297 1.488 7.918 18.25
Std Dev 0.0022 0.007 0.0014 0.0012 0.016 0.049 0.07
C (95%) 0.0014 0.005 0.0009 0.0008 0.010 0.038 0.05
Sample Mo Cu Co V Nb W N
1 0.186 0.208 0.0951 0.105 0.0171 0.0145 0.0750
2 0.187 0.208 0.0958 0.106 0.0184 0.0155 0.0765
3 0.187 0.209 0.0973 0.110 0.0185 0.0159 0.0777
4 0.189 0.210 0.0976 0.111 0.0188 0.0174 0.0793
5 0.189 0.216 0.0982 0.112 0.0190 0.0174 0.0810
6 0.192 0.217 0.0986 0.112 0.0191 0.0176 0.0818
7 0.193 0.218 0.1029 0.116 0.0192 0.0192 0.0833
8 0.194 0.221 0.1030 0.117 0.0201 0.0204 0.0836
9 0.195 0.222 0.1033 0.118 0.0205 0.0840
10 0.196 0.224 0.1042 0.119 0.0221 0.0880
11 0.198 0.224 0.1058
12 0.199 0.225 0.1073
13 0.1077
Mean 0.192 0.217 0.1013 0.113 0.0188 0.0181 0.0810
Std Dev 0.004 0.007 0.0044 0.005 0.0009 0.0025 0.0040
C (95%) 0.003 0.004 0.0026 0.003 0.0007 0.0018 0.0028
Note: C(95%) is the 95% half-width confidence interval derived from the equation:
C(95%) = (t x SD)/n
where n is the number of available values, t is the Student's t value for n-1 degrees
of freedom, and SD is the standard deviation of the test results.
13X 30403 A
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December 2011
Participating Laboratories
Exova Materials Testing Middlesbrough, England UKAS accreditation 0239
Metals Technology (Testing) Ltd Sheffield, England UKAS accreditation 0963
Sheffield Assay Office Sheffield, England UKAS accreditation 0012
Universal Scientific Laboratory Milperra, NSW, Australia NATA accreditation 0492
Laboratory Testing, Inc Hatfield, PA, USA A2LA accreditation
0117
Genitest, Inc Montreal, Canada PRI accreditation
123077
Institute of Iron and Steel Technology Shanghai, China CNAL accreditation 0783
Luo Yang Copper Co Luo Yang, He Nan, China CNAL accreditation 0173
Sargam Metals Pvt Ltd Chennai, India NABL accreditation 0025
TCR Engineering Services Ltd Mumbai, India NABL accreditation 0367
Raghavendra Spectrometallurgical Lab. Bangalore, India NABL accreditation 0371
De Bruyn Spectroscopic Solutions Ltd Johannesburg, South Africa
Coleshill Laboratories Ltd Birmingham, England
London & Scandinavian Met. Co Ltd Rotherham, England
Note: to achieve the above-noted accreditation (eg UKAS, NATA, etc), test houses must
demonstrate conformity to the general requirements of EN ISO/IEC 17025.
Analytical Methods Used
ELEMENT RESULT No. & METHOD
ICP-AES FAAS OTHER
Carbon - - all combustion (IR or volumetric
detection)
Silicon 1-3, 7, 10 - 5, 9, 11 gravimetric (perchloric acid)
4, 6, 8 photometric (molybdenum blue)
Sulfur 6, 9 - 1-5, 7, 8, 10-12 combustion (IR or volumetric
detection)
Phosphorus 1-3, 5, 7, 11 - 4, 8 volumetric (alkalimetric)
6, 9, 10 photometric (molybdenum blue)
Manganese 3-5, 8, 10-12 6 1, 9 volumetric (ferrous ammonium sulfate)
2, 7 photometric (periodate)
Nickel 1-4 9 5-7 gravimetric (dimethyl glyoxime)
8 volumetric (dimethyl glyoxime/EDTA)
Chromium 2, 3, 5, 9 - 1, 4, 6-8, 10 volumetric (ferrous ammonium sulfate)
Molybdenum 1-3, 5, 7, 8, 11, 12 4 6, 10 photometric (thiocyanate)
9 ICP-MS
Copper 1, 2, 4, 6, 9-12 7, 8 3 volumetric (thiosulfate)
5 photometric (BCO)
Cobalt 1, 3, 5-8, 10-12 2, 4, 9
Vanadium 1, 2, 4-6, 10 3, 8 7, 9 volumetric (ferrous ammonium sulfate)
Niobium 1, 2, 4-6 - 3 ICP-MS
7, 8 photometric (thiocyanate)
Tungsten 1-6, 8 - 7 ICP-MS
Nitrogen - 2, 9 photometric (Nessler reagent)
1, 10 volumetric (hydrochloric acid)
3-8 inert gas fusion (thermal conductivity)
Notes
This Certified Reference Material has been produced and certified in accordance with the requirements of ISO Guide 34-2009,
ISO Guide 31-2000 and ISO Guide 35-2006, taking into account the requirements of the ISO Guide to the Expression of
Uncertainty in Measurement (GUM).
This certification is applicable to the whole of the disc. However, in accordance with normal practice for OES, it is appropriate
to avoid usage of the central portion of approx 6mm diameter.
This material will remain stable indefinitely, provided adequate precautions are taken to protect it from cross-contamination,
extremes of temperature and atmospheric moisture. All production records will be retained for a period of 20 years from the
date of this certificate. This certification will therefore expire in December 2031, although we reserve the right to make changes
as issue revisions, in the intervening period.
