the spectrometer; s
2
rt is the stability of target preparation, including the effect of
introducing an internal standard; and s
2
rs is the quality of the solution preparations
from the sclerotium sample. Each solution was prepared twice to isolate these error
components. For each solution, two aliquots were taken, an internal standard was
introduced, and finally, a target was prepared from each aliquot. Each target was
measured twice, with the sample positioned independently in the spectrometer.
The ICP-OES and ICP-MS results are compiled in Table 5.3. The elements
detected by particle induced X-ray emission spectrometer, PIXE, using the same
standard sample (MYK3A) were: Na, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu,
Zn, Br, Pb, Sr, although concentration values of Cl, Ni, and Sr were not significant
enough to determine reliably (Watanabe et al. 2007). The PIXE methods showed
good correspondence with ICP-OES analysis such as: the contents of Al, Fe, and Si
Table 5.3 The element concentrations in Myoko 3A sclerotia grains as determined by inductively
coupled plasma optical emission spectrometry (*) and inductively coupled plasma mass spectrometry analyses
No.
Element
Concentration, μg g
À1 (n ¼ 4)
Variance, %
Average
S
2
rr
S
2
rt
S
2
rs
S
2
r
P
ICP-OES
*
1
Al
21,684
0.22
5.87
5.89
8.32
2
Ca
1457
0.11
5.86
5.88
8.30
3
Cu
38.5
3.81
1.57
5.36
6.76
4
Cr
0.49
0.00
5.89
5.89
8.33
5
Fe
3421
0.04
5.89
5.89
8.33
6
K
534
3.24
3.10
5.57
7.15
7
Mn
13.4
0.89
5.71
5.86
8.23
8
Mg
105
0.12
5.85
5.88
8.30
9
Na
896
2.12
9.31
1.94
9.74
10
Ni
1.62
4.07
10.3
2.22
11.3
11
Pb
167
0.88
5.55
5.81
8.08
12
Sr
24.5
0.20
5.88
5.89
8.32
13
Si
455
0.71
5.52
5.79
8.03
14
Ti
137
0.54
5.85
5.89
8.32
15
V
11.7
9.73
19.8
8.08
23.5
16
Zn
67.7
0.17
5.75
5.85
8.20
ICP-MS
17
As
2.98
0.65
5.80
5.88
8.28
18
Ba
177
0.04
5.79
5.86
8.24
19
Be
5.45
0.23
5.88
5.89
8.33
20
Co
4.05
0.04
5.89
5.89
8.33
21
Cd
0.55
0.37
5.86
5.89
8.32
22
Li
0.79
0.49
4.40
5.45
7.02
23
Se
3.44
1.15
5.74
5.89
8.30
24
Sn
0.64
0.78
5.30
5.72
7.84
5 Chemical Characterization of Sclerotia Grains Collected from a Volcanic Ash. . .
87
2
rt is the stability of target preparation, including the effect of
introducing an internal standard; and s
2
rs is the quality of the solution preparations
from the sclerotium sample. Each solution was prepared twice to isolate these error
components. For each solution, two aliquots were taken, an internal standard was
introduced, and finally, a target was prepared from each aliquot. Each target was
measured twice, with the sample positioned independently in the spectrometer.
The ICP-OES and ICP-MS results are compiled in Table 5.3. The elements
detected by particle induced X-ray emission spectrometer, PIXE, using the same
standard sample (MYK3A) were: Na, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu,
Zn, Br, Pb, Sr, although concentration values of Cl, Ni, and Sr were not significant
enough to determine reliably (Watanabe et al. 2007). The PIXE methods showed
good correspondence with ICP-OES analysis such as: the contents of Al, Fe, and Si
Table 5.3 The element concentrations in Myoko 3A sclerotia grains as determined by inductively
coupled plasma optical emission spectrometry (*) and inductively coupled plasma mass spectrometry analyses
No.
Element
Concentration, μg g
À1 (n ¼ 4)
Variance, %
Average
S
2
rr
S
2
rt
S
2
rs
S
2
r
P
ICP-OES
*
1
Al
21,684
0.22
5.87
5.89
8.32
2
Ca
1457
0.11
5.86
5.88
8.30
3
Cu
38.5
3.81
1.57
5.36
6.76
4
Cr
0.49
0.00
5.89
5.89
8.33
5
Fe
3421
0.04
5.89
5.89
8.33
6
K
534
3.24
3.10
5.57
7.15
7
Mn
13.4
0.89
5.71
5.86
8.23
8
Mg
105
0.12
5.85
5.88
8.30
9
Na
896
2.12
9.31
1.94
9.74
10
Ni
1.62
4.07
10.3
2.22
11.3
11
Pb
167
0.88
5.55
5.81
8.08
12
Sr
24.5
0.20
5.88
5.89
8.32
13
Si
455
0.71
5.52
5.79
8.03
14
Ti
137
0.54
5.85
5.89
8.32
15
V
11.7
9.73
19.8
8.08
23.5
16
Zn
67.7
0.17
5.75
5.85
8.20
ICP-MS
17
As
2.98
0.65
5.80
5.88
8.28
18
Ba
177
0.04
5.79
5.86
8.24
19
Be
5.45
0.23
5.88
5.89
8.33
20
Co
4.05
0.04
5.89
5.89
8.33
21
Cd
0.55
0.37
5.86
5.89
8.32
22
Li
0.79
0.49
4.40
5.45
7.02
23
Se
3.44
1.15
5.74
5.89
8.30
24
Sn
0.64
0.78
5.30
5.72
7.84
5 Chemical Characterization of Sclerotia Grains Collected from a Volcanic Ash. . .
87