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1. Scope
1.1 This guide describes the essential activities that are
required to produce samples for interlaboratory studies.
1.2 The suitability of a particular interlaboratory sample
developed using this guide will depend on the tests being
made.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
3. Terminology
3.1 DefinitionsFor definitions of terms used in this practice, refer to Terminology D 121.
4. Summary of Practice
4.1 Test samples of adequately defined composition and
homogeneity are required for interlaboratory studies. These
samples should be typical in all respects to the samples for
which the test method is applicable.
4.1.1 The sample should be of sufficient quantity to perform
all necessary tests and replicates. Guidelines specifying minimum quantities are given in Practice D 2013.
4.1.2 The top size must be consistent for the test being run.
4.2 Differences in results due to the homogeneity or oxidation, or both, of the test sample should be minimal with respect
to other errors.
2. Referenced Documents
2.1 ASTM Standards:
D 121 Terminology of Coal and Coke2
D 346 Practice for Collection and Preparation of Coke
Samples for Laboratory Analysis2
D 2013 Practice for Preparing Coal Samples for Analysis2
D 2234 Practice for Collection of a Gross Sample of Coal2
D 2492 Test Methods for Forms of Sulfur in Coal
D 2961 Test Method for Single Stage Total Moisture Less
than 15 % in Coal Reduced to 2.36-mm (No. 8 Sieve)
Topsize2
D 3172 Practice for Proximate Analysis of Coal and Coke2
D 3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke3
D 3302 Test Method for Total Moisture in Coal2
D 4596 Practice for Collection of Channel Samples of Coal
in the Mine2
D 5142 Test Methods for the Proximate Analysis of Coal
and Coke by Instrumental Procedures2
D 5263 Test Method for Determining the Relative Degree
of Oxidation in Bituminous Coal by Alkali Extraction2
E 178 Practice for Dealing with Outlying Observations3
E 691 Practice for Conductiing an Interlaboratory Study to
Determine the Precision of a Test Method3
E 826 Practice for Testing Homogeneity of Materials for
1
This practice is under the jurisdiction of ASTM Committee D05 on Coal and
Coke and is the direct responsibility of Subcommittee D05.30 on Quality Assurance.
Current edition approved April 10, 2002. Published July 2002.
2
Annual Book of ASTM Standards, Vol 05.06
3
Annual Book of ASTM Standards, Vol 14.02.
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6796
evaluate the test method. The degree of homogeneity is related
to the size of the sample analyzed. Hence the minimum size of
a sample meeting a specified homogeneity must be stated, and
this must be equal to or smaller than the size of the sample
specified in the test method. Also, different tests may require
different sample sizes to achieve homogeneity. Tests for
homogeneity should be made. An acceptable method for
measuring homogeneity is given in Appendix X1.
7.3 The uncertainties in homogeneity, moisture, or sample
composition, or a combination thereof, should not exceed one
third of the measurement uncertainties they are expected to
evaluate. When this specification is met, sample uncertainties
make a negligible contribution to the variance of the test
results. While replicate samples may be used in practical
analysis to average out sample variations, this is not feasible in
the case of samples for Interlaboratory Studies; hence, homogeneity should be attained as far as possible.
7.4 Samples not meeting the homogeneity requirements
above for a given test should not be used in interlaboratory
studies unless they are re-mixed (all samples must be recombined and the entire sample rehomogenized, see 6.2) and
retested. In some cases, samples that are inhomogeneous for
one test may be homogeneous for other tests.
7.5 Top size of the sample must be consistent with required
top size or reduced to the appropriate size.
7.6 Sample stability may be determined. See Note 4.
7.6.1 MoistureFor most tests moisture should be determined and compared to other results and calculated to a
common basis.
7.6.2 OxidationCoals (particularly those of low rank)
stored for a long period of time may become oxidized. If pyrite
becomes oxidized it may affect forms of sulfur determinations
(see Test Methods D 2492). Bituminous coals are generally
stable for long periods of time but the degree of oxidation of
bituminous coals can be determined using Test Method
D 5263.
D 6796
minimum the rank, percent ash, top size, approximate moisture
content, special handling comments, amount of sample available and original purpose for which the standard was collected
shall be recorded. Sample location, sample type (run of mine;
D 121, channel sample; D 4596, etc). Maintain all results with
the samples until they are published, at which time only the
reference need be maintained.
9.2 Record when the sample was collected, record when the
sample was prepared, and record how the sample has been
maintained.
9.3 A list of samples currently available with the information listed in 8.1 and 8.2 should be accessible to interested
parties who may wish to use them for interlaboratory studies.
10. Keywords
10.1 ash; coal; coke; combustion residue; homogeneity;
laboratory; moisture; oxidation; quality control
9. Record Keeping
9.1 Characteristics of the sample should be recorded. At a
APPENDIXES
(Nonmandatory Information)
X1. TEST FOR HOMOGENEITY
Use the more complete table in when actually using this test
procedure.
X1.1.5 Whenever possible at least 4 separate sub-samples
taken from each container and labeled with the container
number and sub- sample number (that is, 02-1 for container 02
sub-sample 1). All sub-samples with the same extension (for
example, XX-1) shall be determined together as a sample set
with appropriate standards and reference materials.
X1.1.6 Examine the data and discard any values that have
been determined to be outliers according to Practice E 178.
(See warning note below.) If outliers occur, repeat the complete
test, as provisions are not made for missing data in the
mathematical treatment.
WarningThe use of Practice E 178 dealing with outliers
should be done with extreme care to ensure that values are not
discarded that may be valid for the analysis.
X1.1.7 When a test is complete, data should be tabulated
according to Table X1.2. Data may be used in its raw form or
normalized to a reference material.
X1.1.8 Compute C, B, c, and G, (see Table X1.2), where: C
= sum of each column; B = sum of each row; c = mean of each
column; and G = sum of B1 ...Bn; b = number of replicate
measurements (that is, runs); and c = number of containers.
X1.1.9 Choose a significance level (;) for the test (See Note
X1.1).
NOTE X1.1A 95 % significance level is recommended for this procedure. See (2) for more extensive tables containing values at other
significance levels.
D 6796
TABLE X1.1 Short Table of Random NumbersA
96
19
39
97
14
03
33
59
02
33
59
50
43
91
62
03
57
36
70
08
85
54
18
43
75
10
23
55
13
89
94
93
71
05
30
45
85
20
50
92
56
86
57
20
98
74
54
33
85
22
85
15
80
80
61
96
76
20
55
79
28
75
23
63
19
35
66
63
96
88
97
13
32
31
37
91
71
48
11
97
85
10
43
39
60
35
17
32
78
65
73
85
40
03
55
82
73
72
01
46
77
32
62
30
60
40
44
40
57
26
25
20
72
18
67
60
76
06
70
53
74
09
69
09
19
11
58
82
71
47
82
59
68
14
10
40
74
80
02
41
44
64
80
30
98
81
81
90
43
41
27
63
24
65
86
03
56
93
48
34
47
09
80
38
54
81
72
15
89
52
47
13
33
12
56
00
09
63
17
03
89
75
97
35
41
54
66
98
73
45
26
94
44
79
22
14
91
10
65
84
92
55
33
07
38
47
15
17
84
54
89
18
64
27
18
16
91
03
80
13
53
80
46
60
90
63
78
89
23
13
07
12
18
48
31
03
27
00
39
36
04
11
94
25
45
02
07
20
02
74
86
87
81
71
33
24
47
82
74
71
11
54
34
10
28
61
03
72
87
04
90
42
58
19
75
19
08
92
29
20
17
98
85
68
00
98
85
40
66
77
62
58
60
74
12
01
81
65
85
27
26
77
67
30
71
60
75
24
36
33
65
34
27
78
92
97
63
38
14
82
05
29
19
57
39
63
03
59
25
86
30
84
17
18
69
96
19
92
82
96
81
78
82
17
49
05
26
28
69
02
45
33
28
01
13
09
78
19
22
89
65
68
23
88
33
25
48
01
25
23
90
63
34
63
03
74
07
14
13
22
29
60
13
36
63
76
55
57
01
46
15
45
94
78
82
77
25
44
56
57
21
29
11
84
33
21
73
90
67
74
20
02
46
84
69
14
46
58
49
00
84
03
03
78
56
58
71
72
85
45
89
93
08
57
77
27
56
51
28
21
35
36
93
34
71
94
45
63
88
77
89
45
34
47
72
21
78
80
19
68
42
54
15
42
98
78
44
25
25
26
87
24
59
11
49
69
79
19
33
59
89
68
00
09
01
77
51
52
67
14
79
34
98
54
57
65
49
95
34
47
91
00
79
45
08
18
19
87
20
48
23
87
36
32
96
21
01
37
94
36
48
64
28
80
92
03
32
17
35
98
80
16
50
62
89
84
36
83
51
39
26
45
01
45
33
57
61
86
29
93
71
31
26
89
16
00
87
32
15
23
96
23
10
00
74
22
33
66
62
47
25
12
97
10
72
51
25
22
07
64
98
87
77
40
94
80
48
14
75
56
99
91
48
04
28
70
22
75
64
72
42
34
35
70
13
05
06
74
92
17
41
05
63
97
35
05
53
48
78
44
01
43
31
97
95
38
19
51
69
53
36
60
50
28
60
08
92
55
66
36
57
38
50
77
69
39
88
78
35
02
64
84
34
74
50
86
98
59
53
49
64
43
21
92
72
25
62
56
26
04
11
28
02
15
27
60
61
90
25
89
25
11
46
87
19
64
32
31
33
70
28
51
57
42
50
42
41
69
48
95
64
05
23
13
56
52
47
84
37
18
20
36
59
00
11
47
28
19
15
08
05
10
65
70
52
36
04
20
68
64
36
50
92
08
02
60
44
99
97
15
22
10
69
59
59
48
20
24
15
63
58
72
09
04
48
85
48
24
13
81
30
98
69
04
68
26
80
56
41
84
45
01
47
04
87
53
40
03
57
94
53
46
45
74
70
44
40
73
47
74
25
68
60
75
15
56
00
41
70
75
22
90
94
90
51
40
02
49
75
05
89
29
76
94
25
37
59
41
39
80
11
65
47
89
47
56
33
64
92
81
02
56
26
79
88
34
47
23
58
43
94
36
77
78
09
84
15
65
11
74
75
44
00
51
29
73
62
79
54
52
87
97
02
50
08
80
55
29
48
07
43
62
70
81
12
77
12
96
57
55
49
58
97
91
72
54
10
40
42
62
80
87
69
64
25
31
59
86
77
69
81
27
80
27
48
73
03
17
89
85
64
93
62
05
95
39
05
28
75
44
15
07
39
78
52
06
06
60
11
87
14
45
21
08
33
24
38
07
44
69
62
81
60
99
79
59
93
10
83
69
74
78
55
61
30
57
42
23
56
70
37
87
31
75
31
19
02
76
64
76
60
79
74
54
54
69
78
48
84
73
34
88
48
27
38
85
22
64
88
82
95
16
74
37
39
18
51
34
01
61
91
22
31
34
93
68
05
75
73
05
93
08
62
82
79
06
16
49
69
51
40
83
17
84
62
03
91
01
44
81
03
72
22
12
88
20
52
54
09
30
48
77
22
03
42
70
60
10
34
34
48
07
63
63
45
36
32
83
23
73
36
30
47
70
11
41
13
74
61
52
31
05
30
87
43
89
97
95
01
58
52
50
23
43
20
85
42
44
28
77
98
30
05
18
84
41
65
32
82
31
46
62
27
87
66
33
55
42
39
11
96
92
60
80
79
02
17
39
06
41
84
59
22
83
23
91
88
44
33
46
09
46
08
32
60
77
29
99
58
28
23
19
77
03
18
74
65
00
91
92
18
17
91
44
29
91
02
00
07
17
35
98
34
35
54
00
54
50
38
59
59
61
65
42
13
24
95
84
66
42
20
11
32
03
86
32
96
21
06
77
86
36
17
36
70
60
63
93
04
13
Reprinted with permission from A Million Digits, by The Rand Corporation, Copyright, The Free Press, 1955.
C1=
c1=
C2=
c2=
Specimen Number
4
C3=
c3=
C4=
c4=
C5=
c5=
...
...
...
cA
Cn=
cn=
Total
B1=
B2=
B3=
B4=
B5=
Bn=
G = (B1 . . . Bn)
A
B
X1.1.10 From Table X1.3, obtain the q value that corresponds to c and <, where: < = the number of degrees of
freedom:
, 5 ~b 2 1! 3 ~c 2 1!
(X1.1)
(X1.2)
D 6796
TABLE X1.3 Values of q for Various Combinations for c and v at 95 % Significance Level
v
10
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
24
30
40
60
120
`
17.97
6.08
4.5
3.93
3.64
3.46
3.34
3.26
3.2
3.15
3.11
3.08
3.06
3.03
3.01
3
2.98
2.97
2.96
2.95
2.92
2.89
2.86
2.83
2.8
2.77
26.98
8.33
5.91
5.04
4.6
4.34
4.16
4.04
3.95
3.88
3.82
3.77
3.73
3.7
3.67
3.65
3.63
3.61
3.59
3.58
3.53
3.49
3.44
3.4
3.36
3.31
32.82
9.8
6.82
5.76
5.22
4.9
4.68
4.53
4.41
4.33
4.26
4.2
4.15
4.11
4.08
4.05
4.02
4
3.98
3.96
3.9
3.85
3.79
3.74
3.68
3.63
37.08
10.88
7.5
6.29
5.67
5.3
5.06
4.89
4.76
4.65
4.57
4.51
4.45
4.41
4.37
4.33
4.3
4.28
4.25
4.23
4.17
4.1
4.04
3.98
3.92
3.86
40.41
11.74
8.04
6.71
6.03
5.63
5.36
5.17
5.02
4.91
4.82
4.75
4.69
4.64
4.59
4.56
4.52
4.49
4.47
4.45
4.37
4.3
4.23
4.16
4.1
4.03
43.12
12.44
8.48
7.05
6.33
5.9
5.61
5.4
5.24
5.12
5.03
4.95
4.88
4.83
4.78
4.74
4.7
4.67
4.65
4.62
4.54
4.46
4.39
4.31
4.24
4.17
45.4
13.03
8.85
7.35
6.58
6.12
5.82
5.6
5.43
5.3
5.2
5.12
5.05
4.99
4.94
4.9
4.86
4.82
4.79
4.77
4.68
4.6
4.52
4.44
4.36
4.29
47.36
13.54
9.18
7.6
6.8
6.32
6
5.77
5.59
5.46
5.35
5.27
5.19
5.13
5.08
5.03
4.99
4.96
4.92
4.9
4.81
4.72
4.63
4.55
4.47
4.39
49.07
13.99
9.46
7.83
6.99
6.49
6.16
5.92
5.74
5.6
5.49
5.39
5.32
5.25
5.2
5.15
5.11
5.07
5.04
5.01
4.92
4.82
4.73
4.65
4.56
4.47
(X1.3)
where:
s = [(S S S )/(b 1)(c 1)]1/2
b
c
X1.1.15 If the absolute difference between any two mean
values (that is c1cn) exceeds W, then there is strong
evidence, at the 95 % confidence level, that the samples are not
homogeneous. If the absolute difference between any two
mean values does not exceed W, then the samples shall be
considered to be homogeneous.
X1.1.13 Compute S = sum of the squares of all the measurements in the tables and subtract G2/cb:
c
b
S 5 ~Gi51
! ~Gj51
! Y2ij 2 ~G2/cb!
(X1.4)
where:
Yij = individual values in the table.
X1.1.14 Compute the homogeneity factor W:
W 5 qs/b1/2
(X1.5)
D 6796
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