Fasteners & Metals Testing Program
Research Summary Report # 101 – 1st Q 2013
Analysis: 147 – Preliminary Test
Analysis Name: Grain Size
Materials: 316 Stainless Steel, Titanium (CP Ti Gr4)
Overview
Determination of the Average Grain Size of Stainless Steel and Titanium was conducted by CTS in the 1st
quarter of 2013. For this test, all participants received two samples, Y09 (Stainless Steel) and Y10 (Titanium).
Labs were required to perform mounting and surface preparation using polishing and etching techniques
as described in ASTM E3 and ASTM E407. 28 participants submitted results to CTS for at least one sample.
ASTM E112 and/or ASTM E1382 were the referenced standards for determining the average grain size.
Below is a breakdown of the different methods used:
Breakdown of Methods Used
1.
2.
3.
4.
5.
6.
7.
Comparison (21)
Automatic Image Analysis (3)
General Intercept (2)
Heyn Linear Intercept (1)
Abrams Three-Circle (0)
Planimetric (Jeffries) (0)
Not Specified (1)
Comparison
25
Automatic Image Analysis
20
General Intercept
15
Heyn Linear Intercept
10
5
0
Figure 1: This chart shows the different methods
used to determine the average grain size.
Analysis
The results were analyzed using a two sample statistical model. The following tables and graphs represent
the results of this preliminary test. The Data Flags assigned do not warrant corrective actions. This report is
for study only and should not be used as proof of participation in a proficiency testing program for Grain
Size Measurement. Due to the success of this test we have decided to offer two new grain size tests in
2014. We will be offering:
147-2014-1 Grain Size: Stainless Steel
148-2014-1 Grain Size: Inconel
You may click on the links to visit our website for more information. Sign up today!
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Key for Fasteners & Metals Program Web Summary Report
-
Lab Mean
-
The average of the test results obtained by the participant.
Grand Mean
-
The average of the LAB MEANS for all included participants. Laboratories flagged
with an X or an M (see DATA FLAG column) are excluded from the GRAND MEAN.
Between-Lab
Standard Deviation -
An indication of the precision of measurement between the laboratories.
The greater the spread of the LAB MEANS about the GRAND MEAN, the larger the
BETWEEN-LAB STANDARD DEVIATION (and vice versa).
Comparative
Performance Value (CPV)
An indication of how well a laboratory's results agree with the other participants.
The CPV is a ratio indicating the number of standard deviations from the GRAND MEAN.
CPV = (LAB MEAN - GRAND MEAN)/ BETWEEN-LAB STANDARD DEVIATION.
The closer a laboratory's COMPARATIVE PERFORMANCE VALUE is to zero, the more
consistent its results are with the other participants' data (and vice versa).
Instr Code
-
A code indicating the manufacturer of the instrument used to perform the test (see
separate INSTRUMENT CODE LIST for each test section).
Data Flag
-
DATA FLAGS are assigned based on the simultaneous analysis of both samples
tested. Refer to the following chart for an explanation of each symbol:
Data
Flag
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WebCode
Statistically
Included/Excluded
ACTION REQUIRED
*
INCLUDED
CAUTION - review testing procedure and monitor future
results. Results fall outside the drawn 95% ellipse but within a
99% ellipse that is calculated but not drawn. Labs flagged with
an * do not typically receive a specific note regarding the flag.
If this error is repeated in future rounds, however, a lab may
need to stop and review its testing procedures. The initial data
flag is not cause for alarm.
X
EXCLUDED
STOP - immediate review of data and/or testing procedure is
required (all tests exept Chemical Analyses). Results fall outside
the 99% ellipse. See the specific note following the data for more
information on why the data are excluded. For Chemical Analyses
see an additional Memo.
M
EXCLUDED
PROCEED - lab was unable to report data for at least one
sample. However, a lab receiving two or more M flags for a test
may need to stop and review its testing procedures.
Graph
-
For each laboratory, the Lab Mean for the second sample (y-axis) is plotted against the
Lab Mean for the first sample (x-axis) with each point representing a laboratory. The
horizontal and vertical cross-hairs are the Grand Means for each sample. When 20 or
more laboratories are included in the statistics, an ellipse is also drawn so that 95% of
the time a randomly selected laboratory will be included inside the ellipse. Plotted data
flags are explained above. Labs not receiving a data flag appear as points on the plot.
Interlaboratory Testing Program for Metals
Analysis 147 - Preliminary Test Results
Conducted in 2013
Average Grain Size - ASTM Grain Size Number (G)
ASTM E112, ASTM E1382
Sample Y09 - Stainless Steel
Sample Y10 - Titanium
Data
Flag
Lab Mean
Diff. from
Grand Mean
CPV
072MLD
M
7.20
0.25
0.40
No Data Reported
Comparison
072MLD
M
7.46
0.51
0.83
No Data Reported
General Intercept
7.50
0.55
0.89
WebCode
0U5MXA
Lab Mean
Diff. from
Grand Mean
6.40
-0.34
CPV
Analysis Method
Comparison
-0.60
36GPW5
M
6.20
-0.75
-1.22
No Data Reported
Comparison
4FDZPD
X
4.90
-2.05
-3.34
5.70
-1.04
-1.86
Comparison
5TBE74
8.10
1.15
1.87
8.00
1.26
2.26
Comparison
6LCTD8
7.00
0.05
0.08
6.20
-0.54
-0.96
Comparison
6U5UO1
M
7.19
0.24
0.39
No Data Reported
Heyn Linear Intercept
6U5UO1
M
7.21
0.26
0.42
No Data Reported
Automatic Image Analysis
6ZX4H4
M
7.20
0.25
0.40
No Data Reported
Comparison
7D92UM
X
5.40
-1.55
-2.52
5.80
-0.94
-1.68
7.20
0.25
0.40
6.80
0.06
0.11
Comparison
-1.50
Automatic Image Analysis
8C6U4B
BYEY8W
5.90
-0.84
Comparison
5.97
-0.98
-1.60
CCDGZP
M
7.80
0.85
1.38
No Data Reported
Comparison
CCXZ96
M
8.48
1.53
2.48
No Data Reported
Automatic Image Analysis
E6226X
7.40
0.45
0.73
6.70
-0.04
-0.07
Comparison
F82621
7.30
0.35
0.57
6.70
-0.04
-0.07
Comparison
H8D8DX
6.40
-0.55
-0.90
6.00
-0.74
-1.32
Not Specified
HRCF22
7.00
0.05
0.08
7.20
0.46
0.83
Comparison
HTQ63P
6.00
-0.95
-1.55
6.90
0.16
0.29
Comparison
IBJ6P0
7.00
0.05
0.08
6.70
-0.04
-0.07
Comparison
PVYBEW
7.30
0.35
0.57
6.30
-0.44
-0.78
Comparison
QWY8EW
M
7.00
0.05
0.08
No Data Reported
Comparison
R3U1WJ
M
6.40
-0.55
-0.90
No Data Reported
Comparison
SCGMKX
7.56
0.61
0.99
7.60
0.86
1.54
General Intercept
SN7SQY
6.70
-0.25
-0.41
7.00
0.26
0.47
Comparison
UEYF1X
6.80
-0.15
-0.25
6.40
-0.34
-0.60
Comparison
ZOG38A
6.00
-0.95
-1.55
7.00
0.26
0.47
Comparison
Summary Statistics
Sample Y09 - Stainless Steel
Sample Y10 - Titanium
Grand Means
6.95
ASTM G
6.74
ASTM G
Btwn Labs Stan Dev
0.61
ASTM G
0.56
ASTM G
Avg Within Lab Stan Dev
0.50
ASTM G
0.35
ASTM G
Statistics based on
16 of 28 reporting participants
Interlaboratory Testing Program for Metals
Analysis 147 - Preliminary Test Results
Conducted in 2013
Average Grain Size - ASTM Grain Size Number (G)
ASTM E112, ASTM E1382
Sample Y09 - Stainless Steel
Sample Y10 - Titanium
6.95 ASTM G
6.74 ASTM G
Analyst Comment: An ellipse wasn't drawn because an insufficient number of labs reported the Average Grain Size for both
speciemens.
+2σ 8.0
ZOG38A
8.5
UEYF1X
ZOG38A
UEYF1X
SN7SQY
SCGMKX
R3U1WJ
QWY8EW
PVYBEW
IBJ6P0
HTQ63P
HRCF22
H8D8DX
F82621
E6226X
CCXZ96
CCDGZP
BYEY8W
8C6U4B
7D92UM
6ZX4H4
6U5UO1
6U5UO1
6LCTD8
5TBE74
4FDZPD
36GPW5
0U5MXA
072MLD
3.0
SN7SQY
SCGMKX
R3U1WJ
QWY8EW
PVYBEW
IBJ6P0
HTQ63P
HRCF22
H8D8DX
F82621
E6226X
CCXZ96
CCDGZP
BYEY8W
8C6U4B
7D92UM
6ZX4H4
6U5UO1
6U5UO1
6LCTD8
5TBE74
4FDZPD
36GPW5
0U5MXA
072MLD
‐1.0
072MLD
GM 072MLD
CPVs
Stainless
2.0
Titanium
1.0
0.0
‐2.0
‐3.0
‐4.0
Figure 2: This chart shows the CPVs for each lab. Average Grain Size
Stainless
Titanium
7.5
7.0
6.5
‐2σ 5.5
6.0
5.0
4.5
Figure 3: This chart shows the Average Grain Size values for each lab. The Grand Means and G at 2σ away from the Grand Means are shown for reference. WebCode: PVYBEW
Sample Y09: 316 Stainless Steel
Etchant:
60% Nitric Acid
Mag: N/A Method:
G=
CPV =
Comparison
7.3
0.57
Mag: N/A WebCode:
PVYBEW
Sample Y10: Titanium (CP Ti Gr4)
Etchant:
Krolls
Method:
G=
CPV =
Comparison
6.3
-0.78
Mag: 100x Mag: 100x WebCode: UEYF1X
Sample Y09: 316 Stainless Steel
Etchant:
10% Oxalic
Method:
G=
CPV =
Comparison
6.8
-0.25
WebCode:
UEYF1X
Sample Y10: Titanium (CP Ti Gr4)
Etchant:
Krolls
Method:
G=
CPV =
Comparison
6.4
-0.60
Mag: 100x WebCode: F82621
Sample Y09: 316 Stainless Steel
Etchant:
PWA - 17
Method:
G=
CPV =
Comparison
7.3
0.57
Mag: 100x WebCode:
F82621
Sample Y10: Titanium (CP Ti Gr4)
Etchant:
Krolls
Method:
G=
CPV =
Comparison
6.7
-0.07
Mag: 100x WebCode: HTQ63P
Sample Y09: 316 Stainless Steel
Etchant:
10% Oxalic
Method:
G=
CPV =
Comparison
6.0
-1.55
WebCode:
HTQ63P
Sample Y10: Titanium (CP Ti Gr4)
Etchant:
186 - 10% HF 5% Nitric Acid
Mag: 100x WebCode: SCGMKX
Sample Y09: 316 Stainless Steel
Etchant:
40% Nitric Acid
Method:
G=
CPV =
Comparison
7.56
0.99
Mag: 500x WebCode: 6U5UO1
Sample Y09: 316 Stainless Steel
Etchant:
10% Oxalic
Methods:
G=
CPV =
Mag: 100x Heyn Linear Intercept, Automatic Image Analysis
7.19, 7.21
0.39, 0.42 Method:
G=
CPV =
Comparison
6.9
0.29
Mag: 100x Mag: 100x WebCode: H8D8DX
Sample Y09: 316 Stainless Steel
Etchant:
#149 HCL, H20, H202
Method:
G=
CPV =
Not Specified
6.4
-0.90
WebCode:
H8D8DX
Sample Y10: Titanium (CP Ti Gr4)
Etchant:
2% HF
Mag: N/A WebCode: CCDGZP
Sample Y09: 316 Stainless Steel
Etchant:
Not Specified
Method:
G=
CPV =
Comparison
7.8
1.38
Mag: 100x WebCode: 072MLD
Sample Y09: 316 Stainless Steel
Etchant:
9% Oxalic
Method:
G=
CPV =
Comparison, General Intercept
7.2, 7.46
0.4, 0.83
Method:
G=
CPV =
Not Specified
6.0
-1.32