COMMITTEEDRAFT
ISO/CD 15151 | IDF 229
© ISO2010
–
All rights reserved
7
Add 0,5ml of H
2
O
2
(5.7) to all tubes except the blanks toneutralise thenitric vapour.
Transfer the content of the tube quantitatively in a 25 ml one-mark volumetric flask (6.3). Dilute to the 25 ml
markwithwater. Mix thoroughly. If necessary continuewith the dilution procedure in9.3.1.4.
9.3.1.3 Wet digestionwith internal standard
Cool the digested solution (9.2.2.2) to room temperaturewhile reducing toatmospheric pressure.
Add 0,5ml of H
2
O
2
(5.7) to all tubes except the blanks, to neutralise the nitric vapour. Transfer the content of
the tube quantitatively in a sampler tube. Dilute to 25ml withwater. Mix thoroughly. If necessary continuewith
thedilution procedure in 9.3.1.4.
9.3.1.4 Dilution
According to the type of test sample and element measured, dilute (dilution factor
f
1
) the test solution (either
9.3.1.1 or 9.3.1.2) by using the micropipette (6.5) in the required one-mark volumetric flasks (6.3). For the
dilution of test solutions made by 9.3.1.3, make the appropriate dilution taking into account the internal
standard.
9.3.2 ICP-AESmeasurement
Analytical lines, selectivity, limits of determination and quantification, precision, linear working area, and
interferences have to be established beforeoperating the ICP-AES system.
Set the spectrometer at the required wavelength depending on the element (analyte) of the
determination (see Annex B). Each value is the average from at least three individual measurements of the
test sample and standard solutions. Average the values if fallingwithin an accepted range.
9.3.2.1 Calibration
The volumes and corresponding concentrations are only given for guidance. Select both within the linear
range of the particular instrument used (at least 5 concentrations including zeromember).
Transfer the volumes of the solutions mentioned in table 2, by using the (micro) pipette (6.4 or 6.5), in
six 100 ml one-mark volumetric flasks (6.3) respectively. Dilute with water to the 100 ml mark and mix.
The obtained calibration solutions are tabled in table 2.
Table2—Pipette scheme for calibration solutions and concentrationof each element
Pipette (ml)
Element solution
Concentration (mg/l)
Flask number
Flask number
1
2
3
4
5
6
1
2
3
4
5
6
0
1
2
3
4
5
Ca (5.3)
0
100
200
300
400
500
0
1
2
3
4
5
K (5.3)
0
100
200
300
400
500
0
1
2
3
4
5
P (5.3)
0
100
200
300
400
500
0
3
6
9
12
15
Na (5.3)
0
30
60
90
120
150
0
2
4
6
8
10
Mg (5.3)
0
20
40
60
80
100
0
1
2
3
4
5
Fe (5.4.2)
0
4
8
12
16
20
0
1
2
3
4
5
Cu
0
0,5
1
1,56
2
2,5
MTE-03
FORWORKINGGROUP/ERPUSEONLY
DONOTDISTRIBUTE
