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Certificate of Analysis: (Batch AD) Certified Reference Material Information

The document is a Certificate of Analysis for a certified reference material, 11X C3 (batch AD), which is a cast iron disc produced by Maybrey Reliance Ltd and certified by MBH Analytical Ltd. It provides detailed assigned values for various elements by weight, along with their uncertainties, and outlines the methods of preparation, sampling, homogeneity, and chemical analysis. The intended use of this reference material is for calibration and sample preparation in optical emission and X-ray fluorescence spectrometry.

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0% found this document useful (0 votes)
48 views4 pages

Certificate of Analysis: (Batch AD) Certified Reference Material Information

The document is a Certificate of Analysis for a certified reference material, 11X C3 (batch AD), which is a cast iron disc produced by Maybrey Reliance Ltd and certified by MBH Analytical Ltd. It provides detailed assigned values for various elements by weight, along with their uncertainties, and outlines the methods of preparation, sampling, homogeneity, and chemical analysis. The intended use of this reference material is for calibration and sample preparation in optical emission and X-ray fluorescence spectrometry.

Uploaded by

Rohan Narang
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 4

11X C3 AD

Page 1 of 4
January 2019

CERTIFICATE OF ANALYSIS
11X C3 (batch AD)

Certified Reference Material Information


Type: CAST IRON (CHILL CAST)

Form and Size: Disc ~40mm diameter

Produced by: Maybrey Reliance Ltd

Certified and supplied by: MBH Analytical Ltd

Assigned Values
Percentage element by weight

Element C Si S P Mn Ni Cr Mo
Value 1 3.45 1.06 0.180 0.539 0.896 4.34 1.669 0.235
Uncertainty 2 0.02 0.02 0.006 0.005 0.008 0.03 0.018 0.005

Element Cu Al Ti V Co Nb W Sn
Value 1 0.351 0.0104 0.127 0.605 0.240 0.021 0.040 0.166
Uncertainty 2 0.004 0.0013 0.002 0.009 0.005 0.002 0.003 0.003

Element As Sb Pb Bi Zn Se B N
Value 1 0.086 0.243 0.0170 0.0124 0.007 0.028 0.0253 0.0075
Uncertainty 2 0.003 0.004 0.0012 0.0013 0.001 0.002 0.0008 0.0010

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 10th January 2019
MBH ANALYTICAL LIMITED ____________
C Eveleigh
11X C3 AD
Page 2 of 4
January 2019

Method of Preparation
This reference material was produced from commercial pig iron, with the minor and trace elements added as pure
elements or master alloys. The discs are the product of one melt poured into multiple chill moulds with feeding
systems designed to ensure sound discs. Approximately 2mm has been removed from the cast faces of the discs to
minimise surface effects.

Sampling
Milled samples for chemical analysis were taken from random positions within the casting sequence. In addition,
approximately 10% of all discs were selected for non-destructive homogeneity checking.

Homogeneity
Samples representative of the batch were checked for uniformity using an optical emission spectrometer.

For all accepted material, through-batch variation values were derived for each element as an indicator of any minor
compositional variation (as determined for the specific sample size and other limitations of 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 mostly operating within the terms of EN ISO/IEC 17025, using documented standard reference
methods and validated by appropriate reference materials.

The individual values listed overpage are the average of each analyst's results.

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 accreditation 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.

Of the individual results herein, some have traceability (to the mole) via primary analytical methods. Some are
traceable to substances of known stoichiometry. Most have traceability via commercial solutions. Furthermore,
some results have additional traceability to NIST standards, as part of the analytical calibration or process control.

Estimation of Uncertainties
The uncertainty values are generated from the 95% half-width confidence interval C(95%), which is derived from the
wet analysis results, in accordance with the following 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.

As a separate exercise, the degree of compositional variation of the batch for each element has been quantified by a
programme of non-destructive application testing, described above. These values have been combined, using the
square-root of the summed squares, to derive the final uncertainty values.

Usage
Intended use: With optical emission and X-ray fluorescence spectrometers.

Recommended Cast irons are generally prepared by grinding. However, users are recommended to follow the
method :of use: calibration and sample preparation procedures specified by the relevant instrument manufacturer.
Preparation should be the same for reference materials and the samples for test.

For optical emission spectroscopy, a minimum of five consistent replicate analyses is


recommended to provide the necessary sample size. 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-elemental effects.
11X C3 AD
Page 3 of 4
January 2019

Analytical Data
Percentage element by weight

Sample C Si S P Mn Ni Cr Mo
1 3.404 1.011 0.1650 0.5255 0.8782 4.260 1.624 0.2251
2 3.405 1.024 0.1692 0.5281 0.8805 4.300 1.624 0.2275
3 3.410 1.027 0.1701 0.5300 0.8835 4.311 1.629 0.2280
4 3.421 1.028 0.1742 0.5350 0.8864 4.326 1.631 0.2300
5 3.428 1.033 0.1743 0.5350 0.8945 4.330 1.639 0.2306
6 3.434 1.045 0.1770 0.5353 0.8968 4.330 1.665 0.2320
7 3.449 1.057 0.1810 0.5360 0.9000 4.333 1.669 0.2323
8 3.451 1.059 0.1827 0.5380 0.9017 4.340 1.669 0.2333
9 3.452 1.066 0.1856 0.5382 0.9040 4.353 1.674 0.2346
10 3.477 1.068 0.1860 0.5440 0.9060 4.377 1.685 0.2350
11 3.480 1.102 0.1865 0.5465 0.9080 4.416 1.698 0.2380
12 3.490 1.110 0.1890 0.5500 0.9092 4.437 1.700 0.2416
13 3.504 1.123 0.1910 0.5515 1.700 0.2420
14 3.511 0.1920 0.5535 1.710 0.2474
15 1.713 0.2480
Mean 3.451 1.058 0.1803 0.5390 0.8957 4.343 1.669 0.2350
Std Dev 0.036 0.035 0.0087 0.0088 0.0110 0.049 0.032 0.0070
C (95%) 0.021 0.021 0.0050 0.0051 0.0070 0.031 0.018 0.0039

Sample Cu Al Ti V Co Nb W Sn
1 0.3422 0.0088 0.1220 0.5845 0.2281 0.0172 0.0368 0.1600
2 0.3435 0.0090 0.1221 0.5900 0.2309 0.0173 0.0373 0.1605
3 0.3450 0.0093 0.1260 0.5929 0.2315 0.0195 0.0378 0.1605
4 0.3451 0.0094 0.1263 0.5938 0.2360 0.0204 0.0387 0.1612
5 0.3453 0.0098 0.1268 0.6033 0.2360 0.0205 0.0392 0.1620
6 0.3480 0.0102 0.1268 0.6080 0.2380 0.0210 0.0395 0.1635
7 0.3493 0.0108 0.1270 0.6103 0.2380 0.0222 0.0395 0.1668
8 0.3500 0.0130 0.1290 0.6120 0.2410 0.0224 0.0413 0.1674
9 0.3524 0.0132 0.1298 0.6140 0.2440 0.0230 0.0423 0.1680
10 0.3554 0.1310 0.6190 0.2450 0.0231 0.0433 0.1690
11 0.3580 0.6236 0.2450 0.0237 0.1701
12 0.3588 0.2480 0.0239 0.1706
13 0.3590 0.2510 0.1710
14 0.3610 0.2520 0.1720
Mean 0.3509 0.0104 0.1267 0.6047 0.2403 0.0212 0.0396 0.1659
Std Dev 0.0065 0.0017 0.0029 0.0128 0.0075 0.0023 0.0021 0.0044
C (95%) 0.0037 0.0013 0.0021 0.0086 0.0043 0.0015 0.0015 0.0026

Sample As Sb Pb Bi Zn Se B N
1 0.0817 0.2351 0.0144 0.0098 0.0048 0.0223 0.0224 0.0058
2 0.0827 0.2377 0.0145 0.0098 0.0051 0.0247 0.0240 0.0063
3 0.0834 0.2404 0.0153 0.0099 0.0055 0.0249 0.0245 0.0068
4 0.0842 0.2420 0.0158 0.0106 0.0060 0.0268 0.0248 0.0073
5 0.0852 0.2430 0.0163 0.0117 0.0066 0.0271 0.0250 0.0077
6 0.0856 0.2439 0.0168 0.0123 0.0071 0.0277 0.0253 0.0078
7 0.0870 0.2440 0.0171 0.0123 0.0074 0.0282 0.0256 0.0084
8 0.0873 0.2451 0.0172 0.0131 0.0082 0.0297 0.0256 0.0097
9 0.0890 0.2505 0.0181 0.0141 0.0093 0.0300 0.0261
10 0.0907 0.2513 0.0181 0.0145 0.0309 0.0264
11 0.0912 0.0196 0.0150 0.0313 0.0267
12 0.0209 0.0153 0.0273
Mean 0.0862 0.2433 0.0170 0.0124 0.0067 0.0276 0.0253 0.0075
Std Dev 0.0032 0.0050 0.0020 0.0021 0.0015 0.0028 0.0013 0.0012
C (95%) 0.0021 0.0036 0.0012 0.0013 0.0011 0.0019 0.0008 0.0010

For the derivation of the 95% confidence interval, C(95%), see page 2
11X C3 AD
Page 4 of 4
January 2019

Participating Laboratories
ElementLtd Middlesbrough, England UKAS accreditation 0239
Sheffield Assay Office Sheffield, England UKAS accreditation 0012
Anchorcert Analytical Birmingham, England UKAS accreditation 0667
Metals Technology (Testing) Ltd Sheffield, England UKAS accreditation 0963
Universal Scientific Laboratory Pty Ltd Sydney, Australia NATA accreditation 492
Shanghai Jinyi Test Tech Co Shanghai, China CNAS accreditation L0041
Luo Yang Copper Co Luo Yang, He Nan, China CNAL accreditation 0173
Raghavendra SpectroMet Laboratory Bangalore, India NABL accreditation T371
Gesra Labs India Pvt Chennai, India NABL accreditation 6238
Genitest Inc Montreal, Canada PJ accreditation L17-153
Tec-Eurolab Campogalliano, Italy ACCREDIA accreditation 52
Instytut Metalurgii Zelaza Gliwice, Poland PCA accreditation AB554
TUV Nord Czech Brno, Czech Republic CAI accreditation L-1060
Mineral & Metallurgical Laboratories Bangalore, India
Analyticka Laborator Lithea sro Brno, Czech Republic
INCDMNR-IMNR Pantelimon, Romania
AMG Superalloys UK Ltd Rotherham, England

Note: to achieve the above accreditation (UKAS, etc), test houses are required to
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 (infra-red detection)
Silicon 1, 3, 5, 7, 13 - 2, 4, 8, 9, 11, 12 gravimetric (perchloric acid)
6, 10 photometric (molybdenum blue)
Sulfur 5, 6, 9 - 1-4, 7, 8, 10-14 combustion (infra-red detection)
Phosphorus 1-3, 6, 7, 9, 12-14 - 4, 5, 8 photometric (molybdenum blue)
10, 11 volumetric (alkalimetric)
Manganese 1, 3-8, 10, 12 2, 9 11 volumetric (arsenite)
Nickel 1-4, 9, 11 12 5, 7, 8 gravimetric (dimethyl glyoxime)
6, 10 photometric (dimethyl glyoxime)
Chromium 1-3, 5, 6, 8, 9, 11, 13 10, 12, 14 4, 7, 15 volumetric (ferrous ammonium sulfate)
Molybdenum 1-5, 7-11, 14 6 12, 13, 15 photometric (thiocyanate)
Copper 1, 2, 4-6, 8-12 7, 14 3 photometric (BCO)
13 volumetric (thiosulfate)
Aluminium 2, 3, 5, 6, 8 4, 9 1 volumetric (EDTA)
7 photometric (chrome azurol S)
Titanium 1, 2, 4-7, 9 3 8, 10 photometric (diantipyryl methane)
Vanadium 1-5, 7, 9, 11 8, 10 6 volumetric (ferrous ammonium sulfate)
Cobalt 1-5, 7, 8, 11, 14 6, 10, 12 9 photometric (5-Cl-PADAP)
13 gravimetric
Niobium 1-6, 9-11 8, 12 7 photometric (chlorosulfophenol)
Tungsten 1-3, 5, 7-9 4, 6 10 photometric (thiocyanate)
Tin 2-9, 11, 14 1, 12, 13 10 gravimetric (oxide)
Arsenic 1-5, 7, 8, 10, 11 6, 9
Antimony 1, 3, 4, 6, 8, 10 2, 5, 7, 9
Lead 2-6, 10-12 7-9 1 gravimetric (sulfate)
Bismuth 1-6, 9, 10, 12 7, 8, 11
Zinc 1, 3-6, 8 2, 7, 9
Selenium 1, 2, 5-11 3, 4
Boron 2-12 1
Nitrogen - - 1-5, 8 inert gas fusion (thermal conductivity)
6, 7 photometric (Nessler reagent)

Notes
This Certified Reference Material has been produced and certified, wherever possible, in accordance with the requirements
of ISO 17034 and the associated Guides, taking into account the requirements of the ISO Guide to the Expression of
Uncertainty in Measurement (GUM).
The unidirectional solidification effects associated with this method of chill casting have led to the formation of
inhomogeneous segregates in the rear portion of the disc. The above certification is therefore only applicable from the front
face of the disc to a depth of 12mm. Material to the rear of the disc, to a depth of ~3 mm, is not certified.
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. Technical support for this certification will therefore expire in January 2039, although we reserve the
right to make changes as issue revisions, in the intervening period.
The manufacture, analysis and certification of this product were supervised by C Eveleigh, PhD, Technical Director, MBH
Analytical Ltd.
The material to which this certificate of analysis refers is supplied subject to our general conditions of sale.

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