y

AMENDED REPORT NO. 756B

(Issued March 2012)


Hardness Testing of Metals
Proficiency Testing Program
Round 3


March 2012





ACKNOWLEDGMENTS

PTA wishes to gratefully acknowledge the technical assistance provided for this
program by Mr I Harrison, Amdel Limited, Whyalla Laboratory, OneSteel Site, a
Division of Bureau Veritas Australia Pty Ltd. This assistance included providing
input into the design of the program, technical advice and discussion of the final
report, as well as supplying the samples.


COPYRIGHT PROFICIENCY TESTING AUSTRALIA 2012

PO Box 7507 Silverwater NSW 2128 AUSTRALIA





CONTENTS

1. FOREWORD 1
2. FEATURES OF THE PROGRAM 1
3. FORMAT OF THE APPENDICES 2
4. STATISTICAL DESIGN OF THE PROGRAM 2
5. OUTLIER RESULTS 3
Table A: Summary Statistics for All Tests 3
Table B: Summary of Statistical Outliers 4
6. PTA AND TECHNICAL ADVISER'S COMMENTS 4
7. REFERENCES 6

APPENDICES
APPENDIX A
Summary of Results
Brinell Hardness A1.1 - A1.2
Rockwell B Hardness A2.1 - A2.2
Methods Used and Surface Preparation A3.1 - A3.2
APPENDIX B
Homogeneity Testing B1.1
Stability Testing B1.1
APPENDIX C
Instructions to Participants C1.1
Results Sheet C2.1

-1-

1. FOREWORD

This report summarises the results of a proficiency testing program on the
hardness properties of metals. It constitutes the third round of an ongoing series
of programs.

Proficiency Testing Australia conducted the testing program in November /
December 2011. The aim of the program was to assess laboratories' ability to
competently perform the nominated tests.

The Program Coordinator was Dr M Bunt. The Technical Adviser was Mr I
Harrison, Amdel Limited, Whyalla Laboratory, OneSteel Site, a Division of
Bureau Veritas Australia Pty Ltd. This report was authorised by Mr P Briggs,
PTA General Manager.


2. FEATURES OF THE PROGRAM

(a) A total of 25 laboratories participated in the program. Two of these laboratories
did not return results for inclusion in the final report. Laboratories from the
following states and countries received samples:

8 NSW
6 VIC
4 SA
3 QLD
1 WA
1 TAS
1 BRAZIL
1 CHINA

To ensure confidential treatment of results, each laboratory was allocated a
unique code number. All reference to participants in this report is by allocated
code numbers.

(b) The results reported by participants are presented in Appendix A.

(c) Laboratories were provided with a 14 mm thick hot rolled structural sample,
conforming to AS/NZS 3679.1, for this program. The sample was tested for both
Rockwell B and Brinell hardness. The sample was supplied in the as rolled
condition, with scale remaining on both rolled surfaces. The test surface(s)
required preparation to meet the requirements for testing to AS 1816.1 / ISO
6506.1 Brinell (preferably HBW 10/3000) and AS 1815.1 / ISO 6508.1 - Rockwell
HRB hardness testing.

-2-

(d) Laboratories were requested to perform the tests according to the Instructions to
Participants provided and to record the results, along with an estimate of their
measurement uncertainty (MU) for each result, on the accompanying Results
Sheet, which was distributed with the samples. Copies of these documents
appear in Appendix C.

(e) Prior to distribution, the samples were tested for homogeneity by Amdel Limited,
Whyalla Laboratory, OneSteel Site. Based on the results of this testing, the
homogeneity of the samples was established (see Appendix B).

(f) The samples were also tested for stability by Amdel Limited, Whyalla Laboratory,
OneSteel Site. The analysis of the stability testing results showed that the
samples were sufficiently stable for testing for the duration of the program (see
Appendix B).


3. FORMAT OF THE APPENDICES

(a) Appendix A is divided into three sections (A1-A3).

Sections A1-A2 contain the analysis of results reported by laboratories for Brinell
and Rockwell B hardness. These sections contain:

i) a table of results reported by laboratories for each test, with estimates of
their MUs and calculated z-scores;
ii) a listing of the summary statistics; and
iii) ordered z-score charts.

Section A3 contains information on the methods used by the participants and the
surface preparations they performed.

(b) Appendix B contains details of the homogeneity and stability testing.

(c) Appendix C contains copies of the Instructions to Participants and Results Sheet.



4. STATISTICAL DESIGN OF THE PROGRAM

For each statistically analysed test, robust statistical procedures were used to
generate the z-scores and summary statistics for each hardness determination -
number of results, median, normalised interquartile range (IQR), minimum,
maximum and range.

For each participant, the robust z-score calculated for each hardness result was
based on the average hardness value reported for each test.



-3-

5. OUTLIER RESULTS

Robust z-scores have been used to assess each laboratorys testing
performance. When calculated from single results, z-scores are used to detect
excessively high or excessively low results in comparison to the consensus value
(the median). Any result with an absolute z-score greater than or equal to 3.0
(i.e. -3.0 or 3.0) is classified as an outlier.

For further details on the calculation and interpretation of robust z-scores, please
see the Guide to Proficiency Testing Australia (2011).

The following table summarises the results submitted by participants for the
program.

Table A: Summary Statistics for All Tests

Test Summary Statistics Average Result
Number of Results 20
Median 164.0
Normalised IQR 5.4
Brinell
(HBW)
Uncertainty (Median) 1.5
Number of Results 22
Median 84.25
Normalised IQR 1.82
Rockwell B
(HRB)
Uncertainty (Median) 0.49


Notes:

1. For each test, the results for all test methods were pooled for analysis.
2. Summary statistics were calculated for the average hardness value reported
for each test.
3. The uncertainty of the median was calculated as:
n
normIQR

.


-4-

Table B: Summary of Statistical Outliers
(by laboratory code number)

Test Outliers
Brinell (HBW) 3
Rockwell B (HRB) 2, 19


6. PTA AND TECHNICAL ADVISERS COMMENTS

Consensus values (medians), derived from participants results, are used as the
assigned values in this program. These values are not metrologically traceable
to an external reference. The summary statistics, uncertainties of the assigned
values and outliers, for each of the tests, are reported in Tables A and B above.
Complete details of the statistical analyses appear in Appendix A.


6.1 Return rate

Twenty-three of the 25 (92%) laboratories that participated in the program
returned results. Of these 23 laboratories, nineteen (83%) submitted results for
both tests.

The return rate for all tests is as follows:

Brinell (HBW) 20 out of 23 87%
Rockwell B (HRB) 22 out of 23 96%


6.2 Performance summary

One or more statistical outliers were reported by three of the 23 laboratories
(13%) that returned results in this round of the program. For comparison, 9% of
the participants reported outlier results in Round 2 of this program (see Report
No. 703 for more details).

A total of 42 results were analysed in this program. Of these results, three (7%)
were outlier results. For comparison, 8% of the results analysed in Round 2 of
this program were outlier results (see Report No. 703 for more details).

-5-

6.3 Brinell Hardness

A total of 20 laboratories tested the sample for Brinell hardness. Of these
laboratories, 18 tested using the AS 1816.1 method, while two laboratories tested
using the ISO 6506-1 method (see Appendix A3 for more details).

For the laboratories that used the AS 1816.1 method, the median and standard
error of the Brinell hardness results was 164.0 1.4 BHN. For all methods
pooled, the median and standard error of the Brinell hardness results was 164.0
1.5 BHN.

The methods were pooled when analysing the results.

The coefficient of variation (CV) for the Brinell hardness results was 3.29%. This
is higher than the CVs of 2.54% and 1.53% obtained for the two samples tested
for Brinell hardness in Round 2 of this program (see Report No. 703).

One laboratory (code 3) reported an outlier result. One other laboratory (code 1)
obtained an |z-score| > 2.0.

Fifteen laboratories reported measurement uncertainties associated with their
Brinell hardness test results in this round.



6.4 Rockwell B Hardness

A total of 22 laboratories tested the sample for Rockwell B hardness. Of these
laboratories, 19 tested using the AS 1815.1 method, two laboratories tested
using the ISO 6508-1 method and one laboratory reported using both AS 1815.1
and ISO 6508-1 (see Appendix A3 for more details).

For the laboratories that used only the AS 1815.1 method, the median and
standard error of the Rockwell B hardness results was 84.50 0.61 HRB. For all
methods pooled, the median and standard error of the Rockwell B hardness
results was 84.25 0.49 HRB.

The methods were pooled when analysing the results.

The CV for the Rockwell B hardness results was 2.16%. This is higher than the
CV of 1.18% obtained for the sample tested for Rockwell B hardness in Round 2
of this program (see Report No. 703).

For Rockwell B hardness, two laboratories (codes 2 and 19) reported outlier
results.




-6-

Laboratory 19 reported that they were concerned about the large variation in their
Rockwell B hardness results, so they conducted an investigation. They
performed another two tests on the sample, as it was provided. These results
were consistent with their initial results. They then stripped the sample with HCl
and these results had less variation. The results of the follow-up testing
performed by laboratory 19 were not reported. However, using HCl is not an
appropriate sample preparation. The sample needed some form of physical
preparation to provide a flat, parallel and clean surface for testing.

Fifteen laboratories reported measurement uncertainties associated with their
Rockwell B hardness test results in this round.



6.5 General Comments

The intent behind supplying samples for this round in the as rolled condition, with
roll scale still adhered, was to test the participants in preparing the test piece
prior to testing. As is evident from some of the comments made by participants
in Appendix A3, and the fact that some participants did not perform any surface
preparation, this might have introduced an unintended variability in the results.
This might have been detrimental to the success of the program, given that many
participants did not recognise the need to prepare the samples for testing. In
future rounds, supplying the participants with samples fully prepared for testing
will be something to seriously consider.



7. REFERENCES

1. Guide to Proficiency Testing Australia (2011). (This document is located on
the PTA website at www.pta.asn.au under Programs / Documents).

2. AS 1815.1-2007 Metallic materials Rockwell hardness test Test method
(scales A, B, C, D, E, F, G, H, K, N, T).

3. AS 1816.1-2007 Metallic materials Brinell hardness test Test method
(ISO 6506-1: 2005, MOD).

4. ISO 6506-1: 2005 Metallic materials Brinell hardness test Part 1: Test
method.

5. ISO 6508-1: 2005 Metallic materials Rockwell hardness test Part 1: Test
method (scales A, B, C, D, E, F, G, H, K, N, T).

6. AS/NZS 3679.1-2010 Metallic materials Structural steel - Hot-rolled bars
and sections.

APPENDIX A


Summary of Results

Section A1

Brinell Hardness
A1.1

Brinell Hardness (HBW) Results and Z-Scores
Lab
Code
Temp.
(
o
C)
Test 1 Test 2 Test 3 Average MU () Z-Score
1 15 177 178 176 177 5 2.41
2 - 159 161 161 160 - -0.74
3 24 187 187 197 190 3.33 4.82
5 21.5 167 168, 166 166, 162 166 5 0.37
6 22 167 169 168 168 2 0.74
7 23 167 170 167 168 - 0.74
8 23.0 163 169 165 166 8 0.37
10 22.7 163 166 166 165 4.2% 0.19
11 23 166 166 165 166 4 0.37
13 20 163 163 163 163 - -0.19
14 21.1 161 159 158 159 - -0.93
16 21 170 170 170 170 3 1.11
17 23 163 160 161 161 4.0 -0.56
18 27 166 167 167 166.7 2.2 0.50
20 21 157 158 159 158 3.5 (2.2%) -1.11
21 21 164 163 163 163 - -0.19
22 23 156 156 156 156 2.6 -1.48
23 25 156 156 156 156 4 -1.48
24 22.4 159 159 159 159 * -0.93
25 20.6 163 159 164 162 6.9 -0.37


Summary Statistics

Statistic Average Result
Number of Results 20
Median 164.0
Normalised IQR 5.4
Uncertainty (Median) 1.5
Robust CV 3.29%
Minimum 156
Maximum 190
Range 34




A1.2

Notes:

1. denotes an outlier (i.e. |z-score| 3.0).
2. Summary statistics and z-scores have been calculated for the average results
reported.
3. * Laboratory 24 reported their MU as 95% 2% at 382 HBW.







































Brinell Hardness (HBW)
2
01
4
2
4
21
72
5
1
3
2
1
1
0
581
11
8
67
1
6
1
3
2
3
2
2
-3
-2
-1
0
1
2
3
Laboratory Code
R
o
b
u
s
t

Z
-
S
c
o
r
e

Section A2

Rockwell B Hardness
A2.1

Rockwell B Hardness (HRB) Results and Z-Scores
Lab
Code
Temp.
(
o
C)
Test 1 Test 2 Test 3 Average MU () Z-Score
1 15 83.9 83.9 84.4 84.1 1.5 -0.08
2 - 64 64 64 64 - -11.15
3 25 85.6 86.1 87.0 86.2 0.41 1.07
5 23 84.3 84.6, 84.5 84.4, 84.6 84.4 3.1 0.08
6 22 87 87 87 87 1 1.51
7 20 82.8 83.0 82.8 82.9 - -0.74
10 19.9 86.7 86.5 86.2 86.5 2.26% 1.24
11 23 84.8 84.5 85.4 84.9 1.0 0.36
12 20 85.1 85.7 86.0 85.6 0.2 0.74
13 20 84 84 83 84 - -0.14
14 21.1 83.1 83.2 83.2 83.2 - -0.58
15 22 83.5 83.7 83.7 83.6 - -0.36
16 21 87.1 87.0 87.2 87.1 1 1.57
17 23 84.7 85.5 84.5 84.9 1.0 0.36
18 27 81.4 81.0 81.1 81.2 0.64 -1.68
19 22 78.7 72.8 82.1 77.9 - -3.50
20 21 84.7 83.7 85.2 84.5 0.8 (0.9%) 0.14
21 21 84.2 84.8 85.0 84.7 - 0.25
22 23 82 82 82 82 0.60 -1.24
23 25 83.7 83.8 83.8 83.8 1.8 -0.25
24 22.4 81.2 82.1 81.6 81.6 * -1.46
25 20.6 86 87 89 87.3 2.0 1.68


Summary Statistics

Statistic Average Result
Number of Results 22
Median 84.25
Normalised IQR 1.82
Uncertainty (Median) 0.49
Robust CV 2.16%
Minimum 64.0
Maximum 87.3
Range 23.3



A2.2

Notes:

1. denotes an outlier (i.e. |z-score| 3.0).
2. Summary statistics and z-scores have been calculated for the average results
reported.
3. Since their Rockwell B results showed large variation, laboratory 19 conducted an
investigation. They performed another two tests on the sample, as it was
provided (scale). These results were consistent with their initial results. They
then stripped the sample with HCl and these results had less variation. The
results of their follow-up testing were not reported. The results displayed in the
table above are from their initial testing.
4. * Laboratory 24 reported their MU as 95% .82 at 76.2 & .57 at 93.6.






























Rockwell B Hardness (HRB)
1
9
1
8
2
4
71
4
1
5
1
3
1
5
2
02
1
1
1
1
7
1
2
3
1
0
6
1
62
5
2
2
2
2
3
-3
-2
-1
0
1
2
3
Laboratory Code
R
o
b
u
s
t

Z
-
S
c
o
r
e

Section A3

Methods Used and
Surface Preparation
A3.1

Methods Used
Lab Code Brinell Rockwell B
1 ISO 6506-1:2005 ISO 6508-1:2005
2 AS 1816.4, AS 1816.1 AS 1815.1
3 AS 1816 AS 1815.1
5 AS 1816.1 - 2007 AS 1815.1 - 2007
6 AS 1816.1 (2007) AS 1815.1 (2007)
7 AS 1816.1 - 2007 AS 1815.1 - 2007
8 AS 1816.1 - 2007 -
10 AS 1816 HBW 10/3000 AS 1815
11 AS 1816.1 AS 1815.1
12 - AS 1815.1
13 AS 1816.1 (ISO 6506.1) AS 1815.1
14 AS 1816.1 - 2007 AS 1815.1 - 2007
15 - AS 1815.1 - 2007
16 AS 1816.1 - 2007 AS 1815.1 - 2007
17 AS 1816 AS 1815
18 AS 1816 AS 1815
19 - AS 1815.1, ISO 6508.1
20 AS 1816.1 - 2007 AS 1815.1 - 2007
21 AS 1816.1 AS 1815
22 AS 1816.1 AS 1815.1
23 ISO 6506-1 ISO 6508-1
24 AS 1816.1 - 2007 AS 1815.1 - 2007
25 AS 1816.1 - 2007 AS 1815.1 - 2007
A3.2

Surface Preparation
Lab
Code
Preparation Details
1 The rough surface oxide skin was removed about 0.3 mm in depth in the
grinder.
2 Removed 0.5 mm from each surface by milling.
3 No surface preparation.
5 Test surface polished using sandpaper 400 grid.
6 Linished flat by removing the scale back to a bare metal finish of 80-grit.
Note: Preparation of surface to 120-grit bare metal finish. Tested the
unstamped face.
7 Top and bottom surfaces were ground to approximately 0.8 Ra and to be
parallel.
8 Grind.
10 Surface ground to remove rust and scale followed by linishing to 320 grit finish
for both tests. Also coarse linish on reverse side to ensure sample sat evenly.
11 Precision surface grinder machine used to clean up ~80% of face (stamped
face), finish essentially the same as test surface (~0.18 m RA).
12 Linished to remove scale and ensure surface was flat.
13 Surface scale present on surfaces was removed by linishing. The surface for
testing was machined by approximately 0.5 mm and subsequently ground
using 180 grit abrasive paper.
14 No surface preparation.
15 Removal of minimum 0.5 mm by belt linisher and kept cool. Wet polished 120,
320, 600 grit paper. Surface ground underneath of sample to ensure opposite
test face is parallel. All scale and lubricant free. Total force duration 6
seconds.
16 0.5 mm machined off from both surfaces then surface ground and polished to
P600 finish on testing surface.
17 Light surface grind on both sides.
18 Both surfaces were milled to remove surface corrosion and mill scale,
approximately 0.50 to 0.75 mm was removed from both surfaces. The surface
that was hardness tested (opposite side to the hard stamped number) was wet
polished to P1200 grit.
19 No surface preparation.
20 Both surfaces were linished smooth. One side was then metallographically
prepared to P400 grit.
21 Milled parallel, ground - P240, cleaned with meth. spirits.
22 The surface was ground to remove the scale on the surface.
23 Surface grinding and polishing was done on both sides.
24 Surfaces ground and polished to 1200 grit.
25 Surface ground on both sides.








APPENDIX B

Homogeneity and
Stability Testing

B1.1

HOMOGENEITY TESTING

Before the samples were distributed to participants, ten randomly selected samples were
tested for homogeneity by Amdel Limited, Whyalla Laboratory, OneSteel Site. The CV of
the results for the Brinell homogeneity testing was 1.48%, while the CV of the results for
the Rockwell B homogeneity testing was 2.90%. Analysis of the homogeneity testing
data indicated that the samples were sufficiently homogeneous for the program and,
therefore, any participant results identified as extreme cannot be attributed to sample
variability.


STABILITY TESTING

Three randomly selected samples were also tested for stability by Amdel Limited,
Whyalla Laboratory, OneSteel Site. This testing took place at the same time as the
participants tested the samples. Analysis of the stability testing results showed that the
samples were sufficiently stable for testing for the duration of the program.


APPENDIX C


Instructions to Participants

and

Results Sheet
C1.1
Hardness Testing of Metals, Round 3 November 2011 Page 1 of 2
PROFICIENCY TESTING AUSTRALIA

Hardness Testing Of Metals Proficiency Testing Program
Round 3, November 2011

Instructions to Participants

To ensure that the results of this program can be analysed correctly, participants are asked to adhere
carefully to these instructions.

1) The sample for this hardness testing program consists of a 14 mm thick hot rolled structural
sample, conforming to AS/NZS 3679.1. It is to be used for both Rockwell B and Brinell testing
and has been supplied in the as rolled condition, with scale remaining on both rolled surfaces.
The test surface(s) will then require preparation to the required surface finish to meet the
requirements for testing to AS 1816.1 / ISO 6506.1 Brinell (preferably HBW 10/3000) and AS
1815.1 / ISO 6508.1 - Rockwell HRB hardness testing. Testing may be performed on either of
the scale surfaces following suitable preparation. If it is felt that the obverse surface needs to
be prepared to ensure accuracy of the test, then please do so. The sample is identified with a
number stamped on one of the rolled surfaces and an adjacent vertical cut face.

2) All testing is to be performed in accordance with the relevant Standard. Please use the
attached result sheet to record and report your results to Proficiency Testing Australia.

3) Do not discard the hardness test samples until you have received the final report. You may be
asked to carry out a retest or to return the samples to Proficiency Testing Australia for retesting
at the laboratory that performed the homogeneity tests.

4) For this program, your laboratory has been allocated the code number on the attached Results
Sheet. All reference to your laboratory in reports associated with this program will be via this
code number, thus ensuring the confidentiality of your results.

5) Laboratories are also requested to calculate and report an estimate of uncertainty of
measurement for each reported measurement result. All estimates of uncertainty of
measurement must be given as a 95% confidence interval (coverage factor k 2).

6) Return the Results Sheet, either by mail, email or facsimile, to:












All results should arrive at the above address by no later than Monday 19 December 2011.
Results reported later than this date may not be analysed in the final report.


Mark Bunt
Proficiency Testing Australia
PO Box 7507
Silverwater NSW 2128
AUSTRALIA

Telephone: + 61 2 9736 8397 (1300 782 867)
Fax: +61 2 9743 6664
Email: mbunt@pta.asn.au
C2.1
Hardness Testing of Metals, Round 3 November 2011 Page 2 of 2
PROFICIENCY TESTING AUSTRALIA

Hardness Testing Of Metals Proficiency Testing Program
Round 3, November 2011

RESULTS SHEET

Laboratory Code:


Results
Sample
I.D.
Scale
Report
to
nearest
Test
Temp.
C
Test 1 Test 2 Test 3 Average MU ()
Standard

(AS, ISO,
etc.)
Brinell 1 BHN
HRB
0.1
HRB



Did you carry out surface preparation on the obverse surfaces of the samples for the hardness tests?
Yes / No

If Yes, please give details of preparation.
.
.
.
.
.
.

Print Name: __________________________
Signature: ___________________________
Date: _______________________________



-----End of Report-----