12X 352 E

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June 2019

CERTIFICATE OF ANALYSIS
12X 352 (batch E)

Certified Reference Material Information

Type: LOW-ALLOY STEEL (WROUGHT)

Form and Size: Disc ~40mm diameter

Manufactured by: Instytut Metalurgii Zelaza, Poland

Certified and Supplied by: MBH Analytical Ltd

Assigned Values
Percentage element by weight

Element C Si S P Mn Ni Cr Mo Cu
Value 1 0.356 0.413 0.101 0.067 0.817 0.344 0.248 0.230 0.125
Uncertainty 2 0.005 0.007 0.005 0.003 0.007 0.005 0.003 0.005 0.003

Element Co V W Al Ti Nb Ta Sn As
Value 1 0.0253 0.0251 0.275 0.263 0.240 0.063 (0.018) 0.109 0.0293
2 0.0012 0.0008 0.006 0.005 0.003 0.002 - 0.004 0.0015
Uncertainty

Note: Values 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 14th June 2019
MBH ANALYTICAL LIMITED ______________
C Eveleigh
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Method of Preparation
This material was produced by vacuum induction melting and ingot casting, followed by hot forging.

Sampling
Samples for wet chemical analysis were taken from several positions within the batch. In addition, approximately
10% of all
discs were selected for 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
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 as 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 uncertainty for each element has been derived by combining these two factors, using the square-root of the
summed squares.

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

Recommended Steels are generally prepared by linishing, grinding, turning or milling. However, users are
method of use: 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.

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-element effects.
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Analytical Data
Percentage element by weight

Sample C Si S P Mn Ni Cr Mo Cu
1 0.3457 0.3916 0.0951 0.0623 0.7976 0.3270 0.2384 0.2145 0.1166
2 0.3479 0.3973 0.0953 0.0624 0.8069 0.3302 0.2407 0.2172 0.1176
3 0.3480 0.3983 0.0975 0.0656 0.8090 0.3312 0.2408 0.2185 0.1190
4 0.3520 0.4030 0.0981 0.0661 0.8092 0.3363 0.2420 0.2213 0.1203
5 0.3520 0.4080 0.0993 0.0667 0.8093 0.3400 0.2437 0.2255 0.1209
6 0.3543 0.4110 0.1030 0.0671 0.8101 0.3443 0.2454 0.2257 0.1218
7 0.3556 0.4125 0.1030 0.0699 0.8128 0.3450 0.2455 0.2262 0.1243
8 0.3580 0.4140 0.1033 0.0701 0.8138 0.3460 0.2463 0.2265 0.1250
9 0.3602 0.4150 0.1060 0.0711 0.8180 0.3472 0.2468 0.2310 0.1250
10 0.3630 0.4186 0.1065 0.8210 0.3474 0.2480 0.2323 0.1250
11 0.3630 0.4210 0.1067 0.8218 0.3490 0.2500 0.2325 0.1267
12 0.3640 0.4290 0.8273 0.3513 0.2524 0.2380 0.1277
13 0.3690 0.4295 0.8280 0.3520 0.2540 0.2400 0.1301
14 0.4303 0.8290 0.3520 0.2550 0.2403 0.1310
15 0.8360 0.3600 0.2568 0.2450 0.1330
16 0.2580 0.2480 0.1333

Mean 0.3564 0.4128 0.1013 0.0668 0.8167 0.3439 0.2477 0.2302 0.1248

Std Dev 0.0072 0.0123 0.0044 0.0032 0.0104 0.0093 0.0061 0.0100 0.0053

C (95%) 0.0043 0.0071 0.0029 0.0024 0.0058 0.0051 0.0032 0.0053 0.0028

Sample Co V W Al Ti Nb Ta Sn As
1 0.0231 0.0233 0.2640 0.2491 0.2307 0.0590 0.0147 0.1010 0.0258
2 0.0233 0.0237 0.2648 0.2500 0.2327 0.0592 0.0160 0.1028 0.0273
3 0.0241 0.0238 0.2665 0.2510 0.2365 0.0603 0.0172 0.1050 0.0278
4 0.0242 0.0240 0.2680 0.2540 0.2377 0.0610 0.0190 0.1050 0.0279
5 0.0250 0.0244 0.2690 0.2574 0.2400 0.0610 0.0205 0.1051 0.0288
6 0.0250 0.0245 0.2707 0.2586 0.2415 0.0614 0.0207 0.1053 0.0290
7 0.0251 0.0246 0.2785 0.2618 0.2420 0.0621 0.0212 0.1057 0.0293
8 0.0257 0.0247 0.2800 0.2641 0.2420 0.0633 0.1073 0.0294
9 0.0258 0.0249 0.2827 0.2647 0.2430 0.0637 0.1080 0.0296
10 0.0258 0.0259 0.2850 0.2667 0.2436 0.0644 0.1082 0.0302
11 0.0263 0.0259 0.2910 0.2670 0.2439 0.0663 0.1120 0.0309
12 0.0266 0.0261 0.2705 0.2440 0.0666 0.1125 0.0311
13 0.0267 0.0264 0.2705 0.0669 0.1180 0.0312
14 0.0274 0.0267 0.2710 0.1180 0.0317
15 0.0270 0.2714 0.1195
16 0.2740

Mean 0.0253 0.0251 0.2746 0.2626 0.2398 0.0627 0.0184 0.1089 0.0293

Std Dev 0.0013 0.0012 0.0092 0.0083 0.0045 0.0027 0.0025 0.0058 0.0017

C (95%) 0.0007 0.0007 0.0061 0.0044 0.0028 0.0017 0.0024 0.0032 0.0010

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.
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Participating Laboratories
Element Ltd Middlesbrough, England UKAS accreditation 0239
Anchorcert Ltd Birmingham, England UKAS accreditation 0667
Sheffield Analytical Services Sheffield, England UKAS accreditation 0012
Metals Technology (Testing) ltd Sheffield, England UKAS accreditation 0963
Universal Scientific Laboratory Pty Ltd Milperra, NSW, Australia NATA accreditation 0492
Genitest, Inc Montreal, Canada PJ accreditation L17-153
Shanghai Jinyi Test Tech Co Shanghai, China CNAS accreditation 0041
Luo Yang Copper Co Luo yang, He Nan, China CNAS accreditation 0173
Raghavendra SpectroMet Laboratory Bangalore, India NABL accreditation 0371
TCR Engineering Services Ltd Mumbai, India NABL accreditation 0367
Instytut Metalurgii Zelaza Gliwice, Poland PCA accreditation AB554
Tec-Eurolab Campogalliano, Italy ACCREDIA accreditation 52
TUV Nord Czech Brno, Czech Republic CAI accreditation L1060
INCDMNR-IMNR Pantelimon, Romania
Scrooby’s Laboratory Service CC Benoni, South Africa
Mineral & Metallurgical Laboratories Bangalore, India
AMG Superalloys UK Ltd Rotherham, England
Analyticka Laborator Lithea sro Brno, Czech Republic

Note: to achieve the above accreditation (UKAS, 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 (infra-red detection)
Silicon 1-3, 9-12, 14 - 4, 6, 8 photometric (molybdenum blue)
5, 7, 13 gravimetric (perchloric acid)
Sulfur 4 - 1-3, 5-11 combustion (infra-red detection)
Phosphorus 1-4, 6-8 - 5 photometric (molybdenum blue)
9 volumetric (alkalimetric)
Manganese 2-8, 11-13 1, 14 9 photometric (periodate)
10, 15 volumetric (arsenite)
Nickel 2-11 12, 15 1, 13 photometric (dimethyl glyoxime)
14 gravimetric (dimethyl glyoxime)
Chromium 1-8, 10-12, 15 9, 13 14, 16 volumetric (ferrous ammonium
Molybdenum 1-11, 14 12 13, 15, 16 photometric (thiocyanate)
Copper 1, 2, 4-7, 9-13 3, 8, 16 14 photometric (BCO)
15 volumetrioc (thiosulfate)
Cobalt 1-4, 6, 7, 9-12 5, 8, 14 13 photometric (5-chloro PADAB)
Vanadium 1-6, 9, 11, 14, 15 7, 10, 13 8, 12 volumetric (ferrous ammonium sulfate)
Tungsten 1-3, 5-7, 9, 10 4, 11 8 photometric (thiocyanate)
Aluminium 1-3, 5, 7-13, 15 4, 6 14, 16 photometric (chrome azurol S)
Titanium 1-4, 6, 8-11 7 5, 12 photometric (di-antipyryl methane)
Niobium 1-9, 12 11 10 photometric (chlorosulfophenol)
13 gravimetric
Tantalum 1-7 -
Tin 1-3, 5-8, 10, 12, 14, 15 4, 11, 13 9 gravimetric (oxide)
Arsenic 1, 2, 4-10, 12-14 3, 11

Notes
This Certified Reference Material has been produced and certified 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).

This certification is applicable to the whole of the disc. However, in accordance with normal practice for emission spectrometry, it is
appropriate to avoid usage of the centre of the disc, ~8 mm 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.
Technical support for this certification will therefore expire in June 2039, although we reserve the right to make changes as issue revisions,
in the intervening period.

This sample is also available in the form of chippings, for the assessment of ‘wet’ analytical techniques.

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.