GB/T 34499.1-2017 in English
VALIDMethod for chemical analysis of iridium compounds - Part 1: Determination of iridium content - Electricity titration using ferrous sulfate
- Issued on:2017-09-29
- Implemented on:2018-04-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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《GB/T 34499.1-2017铱化合物化学分析方法 第1部分：铱量的测定 硫酸亚铁电流滴定法》由TC243（全国有色金属标准化技术委员会）归口，TC243SC5（全国有色金属标准化技术委员会贵金属分会）执行，主管部门为中国有色金属工业协会。
Introduction
Interpretation of the National Standard of the People's Republic of China GB/T 34499.1-2017
Scope and Applicability of the Standard
This standard applies to the determination of iridium content in the following iridium compounds:
- Chloroiridic acid (H₂IrCl₆)
- Iridium trichloride (IrCl₃)
- Iridium tetrachloride (IrCl₄)
- Ammonium chloroiridate ((NH₄)₂IrCl₆·Γ)
- Iridium acetate (Ir(OAC)₃)
- Iridium acetylacetonate (Ir(OAC)₃) >IrC₁₅H₂₁O₆)
Measurement range: The mass fraction of iridium is $8\% \sim 60\%$.
| Compound Name | Chemical Formula | Applicable Scope |
|---|---|---|
| Chloroiridic Acid | H₂IrCl₆ | $8\% \sim 60\%$ |
| Iridium Trichloride | IrCl₃ | $8\% \sim 60\% |
| Iridium Tetrachloride | IrCl₄ | $8\% \sim 60\% |
Method principle and technical requirements
The sample is treated with nitric acid and hydrochloric acid-hydrogen peroxide to form a solution. In the medium of hydrochloric acid and sulfuric acid, iridium (IV) is titrated with ferrous sulfate standard titration solution. The potential is controlled at $+0.50~\mathrm{V}$, and the end point is indicated by the current method.
Case analysis: Preparation and calibration of ferrous sulfate standard titration solution
The preparation method of ferrous sulfate standard titration solution is as follows:
- Weigh $0.318~\mathrm{g}$ ferrous sulfate and dissolve it in $1000~\mathrm{mL}$ sulfuric acid solution (density $1+1$).
- The calibration process is carried out in parallel with the sample determination. Pipette $10.00~\mathrm{mL}$ iridium standard solution and titrate according to standard operating procedures.
Reagents and Equipment
Key reagents:
- Ferrous sulfate standard titration solution ($c \approx 0.0011~\mathrm{mol/L}$)
- Hydrochloric acid (density $1.19~\mathrm{g/mL}$)
- Nitric acid (density $1.42~\mathrm{g/mL}$)
- Hydrogen peroxide (30% volume fraction)
Key equipment:
- Potentiostat (given potential: $-3~\mathrm{V} \sim +3~\mathrm{V}$)
- Platinum indicator electrode and saturated calomel electrode
- High temperature and high pressure digestion apparatus
Analysis steps and result calculation
Calculate the mass fraction of iridium according to the following formula:
$$ \Delta w_{\mathrm{Ir}} = \frac{c \cdot (V_5 - V_0) \cdot V_3 \times 192.22 \times 10^{-3}}{m_0 \cdot V_4} \times 100\% $$Wherein: $c$ the actual concentration of ferrous sulfate standard titration solution, $V_5$ the volume consumed by the titration test solution, $V_0$ the volume consumed by the titration blank, $m_0$ the mass of the sample.
Precision and Tolerance
| Mass fraction of iridium/% | Repeatability limit $r$/% | Tolerance/% |
|---|---|---|
| $8.00 \sim 20.00$ | $0.07$ | $0.10$ |
| $20.00 \sim 30.00$ | $0.15$ | $0.15$ |
| $30.00 \sim 40.00$ | $0.20$ | $0.20$ |
Implementation suggestions
To ensure the accuracy of the analysis results, it is recommended that:
- Strictly follow the standard operating procedures for sample processing and titration.
- Regularly calibrate the concentration of the ferrous sulfate standard titration solution.
- Strengthen the professional training of operators, especially the operation of the current titration device.
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