ISO 5189:2023
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) — Methods for chemical analysis of metal impurities in silicon dioxide powders using inductively coupled plasma-optical emission spectrometry
Fine ceramics (advanced ceramics, advanced technical ceramics) — Methods for chemical analysis of metal impurities in silicon dioxide powders using inductively coupled plasma-optical emission spectrometry
This document specifies methods for the chemical analysis of metal impurities present in silicon dioxide powders used as a raw material for fine ceramics. It stipulates the methods for the determination of metal impurity elements in silicon dioxide powders that are decomposed by acid decomposition. The aluminium, cadmium, calcium, copper, iron, lead, lithium, magnesium, manganese, nickel, potassium, sodium, titanium, zinc and zirconium contents in the test solution are determined by inductively coupled plasma-optical emission spectrometry (ICP-OES).
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INTERNATIONAL ISO
STANDARD 5189
First edition
2023-09
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of
metal impurities in silicon dioxide
powders using inductively coupled
plasma-optical emission spectrometry
Reference number
© ISO 2023
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Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Analytes and ranges . 1
5 Preparation of test sample . 2
5.1 General . 2
5.2 Sampling . 2
5.3 Drying . 2
5.4 Weighing . 2
6 Reporting analytical values . 2
6.1 Blank test . 2
6.2 Evaluation of analytical values . 2
6.3 Expression of analytical values . 3
7 Decomposition of test sample .3
7.1 Reagents . 3
7.2 Apparatus and instruments. 3
7.3 Sample decomposition . 3
7.4 Blank test . 4
8 Determination of impurity elements .4
8.1 Reagents . 4
8.2 Apparatus and instruments. 5
8.3 Measurement . 5
8.4 Drawing of the calibration curve . 5
8.5 Calculation . 5
9 Test report . 6
Annex A (informative) Analytical results obtained from the interlaboratory test .7
Bibliography .10
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Foreword
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INTERNATIONAL STANDARD ISO 5189:2023(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of metal
impurities in silicon dioxide powders using inductively
coupled plasma-optical emission spectrometry
1 Scope
This document specifies methods for the chemical analysis of metal impurities present in silicon dioxide
powders used as a raw material for fine ceramics.
It stipulates the methods for the determination of metal impurity elements in silicon dioxide powders
that are decomposed by acid decomposition. The aluminium, cadmium, calcium, copper, iron, lead,
lithium, magnesium, manganese, nickel, potassium, sodium, titanium, zinc and zirconium contents in
the test solution are determined by inductively coupled plasma-optical emission spectrometry (ICP-
OES).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Analytes and ranges
a) Aluminium (Al), range of 1,0 mg/kg to 100 mg/kg.
b) Cadmium (Cd), range of 1,0 mg/kg to 100 mg/kg.
c) Calcium (Ca), range of 1,0 mg/kg to 100 mg/kg.
d) Copper (Cu), range of 1,0 mg/kg to 100 mg/kg.
e) Iron (Fe), range of 1,0 mg/kg to 100 mg/kg.
f) Lead (Pb), range of 1,0 mg/kg to 100 mg/kg.
g) Lithium (Li), range of 1,0 mg/kg to 100 mg/kg.
h) Magnesium (Mg), range of 1,0 mg/kg to 100 mg/kg.
i) Manganese (Mn), range of 1,0 mg/kg to 100 mg/kg.
j) Nickel (Ni), range of 1,0 mg/kg to 100 mg/kg.
k) Potassium (K), range of 1,0 mg/kg to 100 mg/kg.
l) Sodium (Na), range of 1,0 mg/kg to 100 mg/kg.
m) Titanium (Ti), range of 1,0 mg/kg to 100 mg/kg.
n) Zinc (Zn), range of 1,0 mg/kg to 100 mg/kg.
o) Zirconium (Zr), range of 1,0 mg/kg to 100 mg/kg.
5 Preparation of test sample
5.1 General
Prepare the sample in accordance with ISO 8656-1, unless otherwise mutually agreed upon by the
analyser and customer.
5.2 Sampling
Collect the sample in accordance with ISO 8656-1.
5.3 Drying
Place 10 g of the sample into a flat-type weighing bottle (60 mm × 30 mm) and spread it uniformly at the
bottom of the bottle. Place the bottle in an air bath at 110 °C ± 5 °C for 2 h, then cover the mouth of the
bottle and cool in a desiccator for 1 h.
5.4 Weighing
Weigh the sample 1,0 g to the nearest 0,1 mg of the required quantity, using a balance.
6 Reporting analytical values
6.1 Blank test
Upon analysis, perform a blank test to correct the measured values.
6.2 Evaluation of analytical values
If the difference between the maximum and minimum analytical values does not exceed the tolerance
value (Table 1), report the average value. However, if the difference between the two values exceeds the
tolerance value, perform two additional analyses. If the difference between the values of these further
two analyses does not exceed the tolerance value, report the average value thereof. However, if the
difference again exceeds the tolerance value, report the median of the four analytical values.
The results of the interlaboratory test are given in Annex A.
Table 1 — Tolerances for analytical values
Unit: mg/kg
Item Value Criteria
5,0 Applicable to amounts of less than 50 mg/kg
Tolerance
25 Applicable to amounts of not less than 50 mg/kg
6.3 Expression of analytical values
Present the analytical values to two significant figures in mg/kg, in dryness.
7 Decomposition of test sample
Silicon dioxide powders are decomposed by acid decomposition.
7.1 Reagents
Use reagents of analytical grade.
7.1.1 Water, grade 1 or superior, as specified in ISO 3696.
7.1.2 Hydrofluoric acid (HF), (ISO 6353-3, R 67), 40,0 % to 42,0 % (mass fraction).
7.1.3 Nitric acid (HNO ), (ISO 6353-2, R19), 65 % (mass fraction).
7.1.4 Hydrochloric acid (HCl), (ISO 6353-2, R 13), 35 % (mass fraction).
7.1.5 Hydrochloric acid solution (1+3). Mix one part hydrochloric acid and three parts water (7.1.1).
7.1.6 Nitric acid solution (1+3). Mix one part nitric acid and three parts water (7.1.1).
7.2 Apparatus and instruments
Ordinary laboratory apparatus together with the following shall be used:
7.2.1 Hot plate, capable of heating at 400 °C.
7.2.2 PTFE (Polytetrafluoroethylene) beakers (25 ml) and covers.
7.2.3 Platinum dishes (20 ml or 30 ml) and covers.
7.2.4 PP (Polypropylene) volumetric flask (10 ml).
7.3 Sample decomposition
Weigh 1,0 g of the test sample and transfer it to a PTFE beaker (7.2.2) or platinum dishes (7.2.3). Add
15 ml of hydrofluoric acid (7.1.2) and 3 ml of nitric acid (7.1.3). Cover the beaker with a PTFE cover and
heat gently on a hot plate. After heating for 1 h, open the PTFE cover and continue to heat gently on a hot
pla
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