GB/T 12690.18-2017 in English
VALIDChemical analysis methods for non-rare earth impurity of rare earth metals and their oxides-Part 18:Determination of zirconium content
- Issued on:2017-10-14
- Implemented on:2018-05-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$127.00
《GB/T 12690.18-2017稀土金属及其氧化物中非稀土杂质化学分析方法 第18部分：锆量的测定》由TC229（全国稀土标准化技术委员会）归口，主管部门为国家标准化管理委员会。
Introduction
GB/T 12690.18—2017 Standard Overview
This standard is Part 18 of the Chemical Analysis Methods for Non-rare Earth Impurities in Rare Earth Metals and Their Oxides, which is specifically for the determination of zirconium content. The standard specifies two methods: inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS), which are suitable for the quantitative analysis of zirconium content in rare earth metals and their oxides.
Scope of application
This standard applies to the following two methods:
1. ICP-OES: the measurement range is $>0.010\% \sim 0.20\%$
2. ICP-MS: the measurement range is $0.0005\% \sim 0.010\%
Principle of the method
Inductively coupled plasma optical emission spectrometry (ICP-OES)
The sample is dissolved in nitric acid and sulfuric acid, and the sample is measured in a dilute acid medium using an inductively coupled plasma optical emission spectrometer. The influence of the matrix on the measured elements is corrected by the matrix matching method.
Inductively coupled plasma mass spectrometry (ICP-MS)
The sample is dissolved in nitric acid and sulfuric acid, and the sample is measured in a dilute acid medium using an inductively coupled plasma mass spectrometer. The influence of the matrix on the measured elements is corrected by the internal standard method.
| Method | Measurement range | Applicable scenarios | Sensitivity |
|---|---|---|---|
| ICP-OES | $>0.010\% \sim 0.20\% | Determination of high content zirconium | Medium sensitivity |
| ICP-MS | $0.0005\% \sim 0.010\% | Determination of low content zirconium | High sensitivity |
Analysis steps and result calculation
ICP-OES:
The mass fraction of zirconium in the sample is calculated according to formula (1):
$$ w = \frac{(\rho - \rho_{0})V \times 10^{-6}}{m} \times 100\% $$ICP-MS:
The mass fraction of zirconium in the sample is calculated according to formula (2):
$$ w = \frac{(\rho - \rho_{0})V \times 10^{-9}}{m} \times 100\% $$Case Study
Application Example: Determination of zirconium content in a rare earth oxide sample.
- Sample preparation: Rare earth oxides were dried at $105^\circ C$ for 1 hour and placed in a desiccator to cool to room temperature.
- Analysis steps: Dissolve, adjust volume, and measure on the machine according to the standard process.
- Results: The zirconium content was measured to be $0.05\% \pm 0.002\%
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