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1. Scope
1.1 This test method covers the simultaneous determination
of 20 alloying and residual elements in carbon and low-alloy
steels in the concentration ranges shown (Note 1).
Element
Concentration Range, %
Quantitative Range, %B
Applicable Range, %A
Aluminum
Arsenic
Boron
Calcium
Carbon
Chromium
Cobalt
Copper
Manganese
Molybdenum
Nickel
Niobium
Nitrogen
Phosphorous
Silicon
Sulfur
Tin
Titanium
Vanadium
Zirconium
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
to
0.075
0.1
0.007
0.003
1.1
2.25
0.18
0.5
2.0
0.6
5.0
0.085
0.015
0.085
1.15
0.055
0.045
0.2
0.3
0.05
0.02 to 0.075
0.05 to 0.1
0.002 to 0.007
0.001 to 0.003
0.08 to 1.1
0.02 to 2.25
0.008 to 0.18
0.04 to 0.5
0.10 to 2.0
0.03 to 0.6
0.02 to 5.0
0.02 to 0.085
0.004 to 0.015
0.02 to 0.085
0.07 to 1.15
0.01 to 0.055
0.01 to 0.045
0.004 to 0.2
0.004 to 0.3
0.02 to 0.05
A
Applicable range in accordance with Guide E1763 for results reported in
accordance with Practice E1950.
B
Quantitative range in accordance with Practice E1601.
1
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved June 1, 2008. Published July 2008. Originally approved
in 1971. Last previous edition approved in 2005 as E415 99a (2005). DOI:
10.1520/E0415-08.
2
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: E2-1004.
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E415 08
Interlaboratory Testing of Chemical Analysis Methods
E1806 Practice for Sampling Steel and Iron for Determination of Chemical Composition
E1950 Practice for Reporting Results from Methods of
Chemical Analysis
3. Terminology
3.1 For definitions of terms used in this test method, refer to
Terminology E135.
4. Summary of Test Method
4.1 A capacitor discharge is produced between the flat,
ground surface of the disk specimen and a conically shaped
electrode. The discharge is terminated at a predetermined
intensity time integral of a selected iron line, or at a predetermined time, and the relative radiant energies of the analytical
lines are recorded. The most sensitive lines of arsenic, boron,
carbon, nitrogen, phosphorus, sulfur, and tin lie in the vacuum
ultraviolet region. The absorption of the radiation by air in this
region is overcome by evacuating the spectrometer and flushing the spark chamber with argon.
5. Significance and Use
5.1 This test method for the spectrometric analysis of metals
and alloys is primarily intended to test such materials for
compliance with compositional specifications. It is assumed
that all who use this test method will be analysts capable of
performing common laboratory procedures skillfully and
safely. It is expected that work will be performed in a properly
equipped laboratory.
6. Apparatus
6.1 Sampling Devices:
6.1.1 Refer to Practice E1806 for devices and practices to
sample liquid and solid iron and steel.
6.2 Excitation Source, capable of providing electrical parameters to spark a sample. See 11.1 for details.
6.3 Spark Chamber, automatically flushed with argon. The
spark chamber shall be mounted directly on the spectrometer
and shall be provided with a spark stand to hold a flat specimen
and a lower counter electrode of rod form.
NOTE 2Follow the manufacturers recommendations for cleaning the
excitation chamber (during continuous operation, this typically should be
done every 24 h). Follow the manufacturers recommendations for
cleaning the entrance lens or window (verifier data or other reference
sample intensity data can typically indicate when this is necessary).
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E415 08
TABLE 1 Internal Standard and Analytical Lines
Element
Aluminum
Arsenic
Boron
Calcium
Carbon
Chromium
Cobalt
Copper
Iron (IS)
Manganese
Molybdenum
Nickel
Niobium
Nitrogen
Phosphorus
Silicon
Sulfur
Tin
Titanium
Vanadium
Zirconium
Wavelength, nm
Line
ClassificationA
394.40
308.22
197.20
193.76
182.64
182.59
396.85
193.09
298.92
267.72
345.35
228.62
327.40
213.60
271.44
273.07
293.31
255.86
379.83
277.54
386.41
231.60
227.02
319.50
149.26
I
I
I
I
I
I
II
I
II
II
I
II
I
II
II
II
II
II
II
I
I
II
II
II
I
178.29
288.16
251.61
180.73
189.99
337.28
324.20
310.23
311.07
343.82
I
I
I
I
II
II
II
II
II
II
Possible InterferenceB
Element
Wavelength, nm
Line
ClassificationA
V, Mn, Mo, Ni
V, Mn
Mo, W
Mn
S, Mn, Mo
W, Mn, Cu
Nb
Al
Mn, V, Ni, Nb, Mo
Mn, Mo, W
Cr, Mo
Ni, Cr
Nb
Mo, Cr
Arsenic
189.04
Carbon
165.81
Copper
224.26
324.75
II
I
Ni
Mn, Nb
Molybdenum
202.03
281.62
II
II
Mn
212.415
II
Co
Cr, Mo, Ni
Zr
Mn
Cu, V, Co, Mn
V, Cr
Co, Ti
Nb, W
Mo, Al, V
Fe, Ti, Si, Mn, Cu, Ni
and nitride forming
elements such as Ti
Mo
Mo, Cr, W
Fe, V
Mn
Mn, Mo, Al
Nb
Nb
Fe, Mo, Nb, Ni
Mn, Ti, Fe
W
A
The numerals I or II in the line classification column indicate that the line has
been classified in a term array and definitely assigned to the normal atom (I) or to
the singly ionized atom (II).
B
Interferences are dependent upon instrument design, spectrum line choices,
and excitation conditions, and those listed require confirmation based upon
specimens selected especially to demonstrate suspected interferences.
Silicon
Possible InterferenceB
V, Cr
The numerals I or II in the line classification column indicate that the line has
been classified in a term array and definitely assigned to the normal atom (I) or to
the singly ionized atom (II).
B
Interferences are dependent upon instrument design, dispersion, spectrum
line choices, and excitation conditions, and those listed require confirmation based
upon specimens selected especially to demonstrate suspected interferences.
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E415 08
11. Excitation and Exposure
11.1 Electrical Parameters (Note 11):
11.1.1 Excitation parameters are normally established by
the spectrometer manufacturer. The following ranges are historical guidelines and newer instruments may vary from these.
Triggered Capacitor Discharge
Capacitance, F
10 to 15
Inductance, H
50 to 70
Resistance, V
3 to 5
Potential, V
940 to 1000
Current, A, r-f
0.3 to 0.8
Number of discharges
60
0.0025
residual
2.5
18 000
5 to 15
5 to 20
3 to 30
5 to 45
5 to 45
5 to 30
ft3/h
L/min
2.5 to 25
2.5 to 25
2.5 to 15
NOTE 12Select preburn and exposure periods after a study of volatization rates during specimen excitations. Once established, maintain the
parameters consistently.
NOTE 13A high-purity argon atmosphere is required at the analytical
gap. Molecular gas impurities, nitrogen, oxygen, hydrocarbons, or water
vapor, either in the gas system or from improperly prepared specimens
should be minimized.
11.3 Electrode SystemThe specimen, electrically negative, serves as one electrode. The opposite electrode is a
thoriated tungsten or silver rod, the tip of which has been
machined to a 90 or 120 angled cone. Use either a 3 mm, 4
mm, or 5-mm (60.1-mm) analytical gap. Condition a fresh
counter electrode with two to six excitations using the operating conditions described in 11.1 and 11.2.
11.4 Photomultiplier PotentialsThe sensitivity of the
photomultipliers is normally established and set by the spectrometer manufacturer based on the particular wavelengths
selected.
NOTE 14The range of anode to cathode potentials for a given tube
should be specified, that is 650 V dc to 1000 V dc. If within the potential
range the tube is either too sensitive or too insensitive for the element
concentration range, select another photomultiplier. The potentials on the
capacitors may be read directly, or a number of different readout systems
may be employed, which yield linear or logarithmic functions of the
potentials and which may be displayed as relative numbers or as numbers
5
MNL 7A Manual on Presentation of Data and Control Chart Analysis, ASTM
Manual Series, ASTM International, 7th ed., 2002.
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E415 08
14. Calculation
14.1 Using the average results obtained in 13.2, calculate
the concentration of the elements from the analytical curves
developed in 12.1.
15. Precision and Bias
15.1 PrecisionUp to eight laboratories cooperated in
performing this test method and obtained the statistical infor-
mation summarized in Table 3. Additional data for withinlaboratory variability of results, obtained by analyzing three
specimens of one material in seven laboratories in accordance
with source conditions specified in this method, are given in
Table 4. Other specimens may exhibit greater or less variability
using the same instrument and excitation conditions.
Number of
Laboratories
Repeatability, R1A
Relative
Repeatability, %
Reproducibility, R2A
Relative
Reproducibility, %
Aluminum
0.0669
0.0625
0.0212
7
5
7
0.004
0.003
0.005
5.98
4.80
23.6
0.025
0.023
0.011
34.7
36.8
51.9
Antimony
0.0038
0.0007
18.4
0.001
26.3
Arsenic
0.0415
0.0144
6
6
0.005
0.007
12.0
48.6
0.0272
0.0247
65.6
172.
Boron
0.0063
0.0038
0.0006
7
7
7
0.0007
0.0007
0.0003
11.1
18.4
50.0
0.0011
0.0042
0.0009
17.5
110.
150.
Carbon
1.054
0.507
0.033
7
7
7
0.053
0.025
0.025
5.03
4.93
75.8
0.108
0.061
0.042
10.2
12.0
127.
Chromium
1.574
1.307
2.128
0.118
0.093
7
6
7
7
7
0.043
0.123
0.057
0.003
0.003
3.38
9.41
2.68
2.54
3.23
0.176
0.124
0.232
0.011
0.008
13.8
9.49
10.9
9.32
8.60
Cobalt
0.157
0.114
0.0086
4
7
8
0.008
0.011
0.0007
5.10
9.65
8.14
0.057
0.023
0.004
36.3
20.2
46.5
Copper
0.435
0.150
0.054
7
7
7
0.025
0.009
0.008
5.75
6.00
14.8
0.039
0.026
0.022
8.97
17.3
40.7
Manganese
1.893
1.494
0.559
0.316
7
7
7
7
0.052
0.052
0.023
0.013
2.75
3.48
4.11
4.11
0.181
0.141
0.074
0.051
9.56
9.44
13.2
16.1
Molybdenum
0.561
0.325
0.147
7
7
7
0.012
0.008
0.005
2.14
2.46
3.40
0.168
0.037
0.016
29.9
11.4
10.9
Nickel
4.796
2.208
0.180
0.108
0.0578
6
7
6
7
7
0.275
0.112
0.012
0.006
0.003
5.73
5.07
6.67
5.56
5.19
0.691
0.164
0.022
0.010
0.015
14.1
7.43
12.2
9.26
26.0
Niobium
0.076
0.0084
0.0078
7
5
5
0.007
0.003
0.003
9.21
35.7
38.5
0.010
0.018
0.014
13.2
214.
179.
Phosphorus
0.0775
0.0379
0.0124
7
7
7
0.005
0.003
0.003
6.45
7.92
24.2
0.017
0.012
0.009
21.9
31.7
72.6
Silicon
1.063
0.391
0.176
7
7
7
0.031
0.015
0.006
2.92
3.84
3.41
0.107
0.099
0.035
10.1
25.3
19.9
Sulfur
0.0505
0.0209
7
7
0.006
0.005
0.015
0.007
29.7
33.5
Element
11.9
28.9
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E415 08
TABLE 3
Continued
Average
Concentration
Number of
Laboratories
Repeatability, R1A
Relative
Repeatability, %
Reproducibility, R2A
Relative
Reproducibility, %
0.0146
0.002
13.7
0.005
41.1
Tin
0.040
0.024
0.0056
7
7
7
0.002
0.002
0.001
5.00
8.33
17.9
0.024
0.011
0.007
60.0
45.8
125.
Titanium
0.190
0.029
0.0019
7
7
7
0.024
0.004
0.0007
12.6
13.8
36.8
0.045
0.017
0.002
23.7
58.6
105.
Vanadium
0.279
0.091
0.0026
7
7
7
0.007
0.002
0.0002
0.041
0.015
0.002
14.7
16.5
76.9
Zirconium
0.0439
0.0075
0.0025
5
5
5
0.006
0.002
0.001
0.009
0.012
0.008
20.5
160.
320.
Element
2.51
2.20
7.69
13.7
26.7
40.0
Average
Concentration, %
Laboratory
Standard
Relative Standard
Deviation, %A Deviation, RSD
%B
3.70
5.03
10.10
3.01
1.90
1.58
1.36
Element NBS
Value
Average Concentration, %
Laboratory
Standard
Deviation, %A
Relative Standard
Deviation, RSD %B
Molybdenum
0.068
0.068
0.0681
0.0663
0.069
0.068
0.069
0.0645
1
2
3
4
5
6
7
0.0012
0.0040
0.00173
0.00064
0.0011
0.00068
0.0005
1.46
5.91
2.60
0.92
1.60
0.98
0.73
Aluminum
0.095
0.087
0.0936
0.0823
0.0992
0.0999
0.095
0.0899
1
2
3
4
5
6
7
0.0032
0.0047
0.0083
0.0030
0.0019
0.0015
0.0012
Antimony
0.012
0.0125
no value
no value
no value
no value
0.0110
no value
1
2
3
4
5
6
7
0.0018
no value
no value
no value
no value
0.00031
no value
14.40
no value
no value
no value
no value
2.85
no value
Nickel
0.59
...
0.597
0.560
0.589
0.606
0.589
0.556
1
2
3
4
5
6
7
no value
0.0078
0.0069
0.0022
0.0097
0.00443
0.0027
no value
1.31
1.22
0.36
1.60
0.75
0.49
Arsenic
0.076
0.060
no value
0.1085
no value
0.0718
0.0871
0.0784
1
2
3
4
5
6
7
0.0024
no value
0.0045
no value
0.0029
0.00243
0.0021
4.00
no value
4.16
no value
4.00
2.79
2.64
Niobium
0.29
0.290
0.292
0.321
0.292
0.289
0.283
0.2636
1
2
3
4
5
6
7
0.0120
0.0108
0.0098
0.0037
0.0137
0.0059
0.0042
4.10
3.69
3.06
1.26
4.70
2.08
1.58
Boron
0.0025
0.0026
0.00174
0.0030
0.00257
0.00303
0.00242
0.0028
1
2
3
4
5
6
7
0.00040
0.00043
0.0003
0.00009
0.00014
0.00007
0.0001
15.40
24.68
10.13
3.50
4.60
2.89
2.23
Phosphorus
0.042
0.0414
0.0355
0.0414
0.0394
0.040
0.0369
0.0342
1
2
3
4
5
6
7
0.0022
0.00144
0.0012
0.00039
0.0014
0.00063
0.0004
5.30
4.04
2.85
1.00
3.50
1.72
1.30
Carbon
0.16
0.160
0.164
0.158
0.162
0.159
0.159
0.162
1
2
3
4
5
6
7
0.0080
0.0094
0.0046
0.0022
0.007
0.0037
0.0038
5.00
5.76
2.92
1.37
4.40
2.29
2.24
Silicon
0.39
0.403
0.392
0.393
0.398
0.389
0.437
1
2
3
4
5
6
0.0046
0.0058
0.0126
0.0030
0.0059
0.0032
1.14
1.49
3.21
0.75
1.50
0.73
Chromium
0.30
0.296
0.300
0.309
0.302
1
2
3
4
0.0048
0.0038
0.0039
0.0015
1.62
1.28
1.26
0.49
Sulfur
0.038
0.0376
0.0404
0.0363
0.0387
1
2
3
4
0.0020
0.00239
0.00118
0.00103
5.30
5.94
2.85
2.65
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E415 08
TABLE 4
Element NBS
Value
Average
Concentration, %
Laboratory
Standard
Relative Standard
Deviation, %A Deviation, RSD
%B
Continued
Element NBS
Value
Average Concentration, %
Laboratory
Standard
Deviation, %A
Relative Standard
Deviation, RSD %B
0.0392
0.0376
0.0375
5
6
7
0.0014
0.00132
0.0014
3.50
3.51
3.78
Tin
0.016
0.0164
0.0157
0.0207
0.0178
0.0158
0.016
0.0175
1
2
3
4
5
6
7
0.00067
0.00048
0.00046
0.00072
0.0026
0.00044
0.0004
3.75
3.08
2.21
4.04
2.90
2.77
2.27
0.300
0.304
0.298
5
6
7
0.0032
0.00220
0.0020
1.10
0.72
0.68
Cobalt
0.30
0.299
0.302
0.252
0.304
no value
0.299
0.3038
1
2
3
4
5
6
7
0.0054
0.0044
0.0137
0.0020
no value
0.00597
0.0029
1.80
1.45
5.45
0.66
no value
2.00
0.97
Copper
0.50
0.499
0.502
0.494
0.505
0.496
0.499
0.534
1
2
3
4
5
6
7
0.0116
0.0098
0.0212
0.00346
0.012
0.00852
0.0099
2.32
1.95
4.28
0.69
2.40
1.71
1.85
Titanium
0.084
0.079
0.089
0.0899
0.091
0.0882
0.085
0.1073
1
2
3
4
5
6
7
0.0043
0.0025
0.000324
0.0011
0.0005
0.00135
0.0017
5.44
2.81
3.60
1.17
1.30
1.59
1.55
Manganese
1.04
1.056
1.00
1.10
1.050
1.038
1.016
1.038
1
2
3
4
5
6
7
0.0092
0.0081
0.0143
0.0072
0.015
0.0117
0.0087
0.87
0.81
1.29
0.69
1.50
1.15
0.84
Vanadium
0.041
0.040
0.0402
0.0410
0.0413
0.0387
0.039
0.0458
1
2
3
4
5
6
7
0.00037
0.00054
0.0010
0.00022
0.0005
0.00036
0.0004
0.92
1.34
2.43
0.52
1.30
0.92
0.78
Zirconium
0.19
0.192
no value
0.305
0.187
1
2
3
4
0.0089
no value
0.0177
0.0048
4.70
no value
5.81
2.58
Zirconium
0.19
0.191
0.173
0.1941
5
6
7
0.0081
0.00495
0.0070
4.20
2.863
3.611
(d2
N21
where:
d = difference of determination from mean, and
N = number of determinations.
B
s
100!
x ~
where:
s = standard deviation, and
x = average concentration, %.
(1)
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: E01-1022.
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E415 08
TABLE 5 Statistical Information for Calcium and Nitrogen
Test Material
Number of
Laboratories
Found, %
Minimum SD (SM,
Practice E1601)
Calcium
C
G
6
7
0.00020
0.00036
0.000021
0.000025
0.000175
0.000181
0.00049
0.00051
H
F
8
8
0.00106
0.00118
0.000075
0.000134
0.000210
0.000249
0.00059
0.00070
55.7
59.0
D
J
8
8
0.00149
0.00186
0.000135
0.000129
0.000231
0.000298
0.00065
0.00083
43.3
45.0
A
I
8
8
0.00201
0.00207
0.000119
0.000064
0.000218
0.000181
0.00061
0.00051
30.3
24.4
B
E
8
8
0.00267
0.00288
0.000182
0.000258
0.000328
0.000436
0.00092
0.00122
34.4
42.5
Nitrogen
C
E
8
8
0.00125
0.00400
0.000143
0.000169
0.000781
0.000787
0.00218
0.00220
175
55.7
F
H
8
8
0.00478
0.00509
0.000175
0.000157
0.000779
0.000684
0.00218
0.00192
45.6
37.6
G
D
8
8
0.00751
0.00817
0.000247
0.000218
0.000715
0.000650
0.00200
0.00182
26.7
22.2
B
A
8
8
0.00977
0.01289
0.000264
0.000239
0.000587
0.000603
0.00164
0.00169
16.8
13.1
0.01364
0.000264
0.000813
0.00228
16.7
Test Material
Average Spectrometer
Value, %
Difference, %
Calcium
C
G
0.00027
0.0004
0.00020
0.00036
0.00007
0.00004
BS CA4A
BS CCS 1
0.00004
(0.00005)
chill-cast
wrought
H
F
0.0011
0.0014
0.00106
0.00118
0.00004
0.00022
ST 06
BS 58G
(0.00013)
(0.00019)
wrought
wrought
D
J
0.0016
0.0021
0.00149
0.00186
0.00011
0.00024
BS 54D
ST 08
(0.00015)
(0.00014)
wrought
wrought
A
I
0.0018
0.0022
0.00201
0.00207
0.00021
0.00003
BS CA1A
ST 07
(0.0003)
(0.0002)
chill-cast
wrought
B
E
0.0029
0.0033
0.00267
0.00288
0.00023
0.00042
BS CA2A
BS CSN 2D
(0.0003)
(0.0003)
chill-cast
wrought
Nitrogen
C
E
0.0011
0.0036
0.00125
0.00400
0.00015
0.00040
BS 54D
BS XAAS
(0.0003)
(0.00025)
wrought
wrought
F
H
0.0044
0.0056
0.00478
0.00509
0.00038
0.00051
BS XCCS
BS XCCV
(0.00025)
(0.00024)
wrought
wrought
G
D
0.0074
0.0087
0.00751
0.00817
0.00009
0.00053
BS XCCT
BS 56G
(0.0002)
(0.0004)
wrought
wrought
B
A
0.0106
0.0135
0.00977
0.01289
0.00083
0.00061
BS CA4A
BS CA1A
(0.0007)
(0.00075)
chill-cast
chill-cast
0.0136
0.01364
0.00004
BS 46A
(0.00038)
wrought
Rrel %
250
139
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E415 08
TABLE 7 Bias Data
Assumed
True
Value,
%
Average
Spectrometer
Value, %
Number of
Laboratories
Deviation from
Assumed True
Value, %
Aluminum
0.04
0.058
0.038
0.062
4
4
0.00
+0.004
Boron
0.007
0.006
0.001
Carbon
0.073
0.22
0.50
0.67
0.072
0.21
0.51
0.66
5
5
7
5
0.001
0.01
+0.01
0.01
0.05
0.08
0.37
0.85
1.51
0.05
0.09
0.35
0.85
1.57
5
7
5
3
7
0.00
+0.01
0.02
0.00
+0.06
Cobalt
0.12
0.17
0.11
0.16
7
4
0.01
0.01
Copper
0.016
0.056
0.070
0.101
0.017
0.054
0.065
0.098
3
7
3
3
+0.001
0.002
0.005
0.003
Manganese
0.44
0.57
0.98
1.43
0.43
0.58
0.94
1.49
5
5
5
7
0.01
+0.01
0.04
+0.06
Molybdenum
0.008
0.10
0.14
0.33
0.34
0.012
0.10
0.15
0.33
0.36
4
4
7
7
3
+0.004
0.00
+0.01
0.00
+0.02
0.034
0.10
0.038
0.11
5
7
+0.004
+0.01
Element
Chromium
Nickel
Element
Assumed
Average
True Value, Spectrometer Number of
%
Value, %
Laboratories
Deviation from
Assumed True
Value, %
0.35
0.56
0.34
0.54
5
3
0.01
0.02
Niobium
0.023
0.10
0.024
0.11
2
2
+0.001
+0.01
Phosphorus
0.005
0.009
0.036
0.046
0.089
0.005
0.009
0.038
0.042
0.078
5
5
7
5
7
0.000
0.000
+0.002
0.004
0.011
Silicon
0.024
0.18
0.19
0.35
0.40
0.029
0.18
0.18
0.36
0.39
3
7
5
5
7
+0.005
0.00
0.01
+0.01
0.01
Sulfur
0.008
0.032
0.034
0.053
0.006
0.028
0.038
0.051
4
5
3
7
0.002
0.004
+0.004
0.002
Tin
0.004
0.008
0.024
0.028
0.044
0.005
0.008
0.025
0.024
0.040
5
5
5
7
7
+0.001
0.000
+0.001
0.004
0.004
Titanium
0.002
0.027
0.002
0.029
7
7
0.000
+0.002
Vanadium
0.002
0.012
0.135
0.27
0.002
0.012
0.138
0.28
2
2
2
7
0.000
0.000
+0.003
+0.01
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