YS/T 1122.1-2016 in English
VALIDChemica lanalysis methods for chloroplatinic acid--Part 1: Determination of platinum content--Ammonium chloride gravimetry
- Issued on:2016-07-11
- Implemented on:2017-01-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$117.00
本部分规定了氯铂酸中铂量的测定方法。本部分适用于氯铂酸中铂量的测定，测定范围37.0%~40.5%。
Introduction
Analysis of the core content of the standard
This part of the standard specifies the technical specifications for the determination of platinum content in chloroplatinic acid by ammonium chloride precipitation gravimetric method, with a determination range of 37.0%-40.5%, and the accuracy of the results is ensured by the three-step method of precipitation-incineration-difference correction.
In-depth analysis of the principle of the method
Key technical route: hydrochloric acid dissolution → ammonium chloride precipitation → 900℃ incineration → ICP-AES difference correction. Key reaction equation:
| Steps | Chemical reaction | Key control points |
|---|---|---|
| Precipitation | H2PtCl6 + 2NH4Cl → (NH4)2PtCl6↓ + 2HCl | Saturated ammonium chloride dosage 45mL |
| Causing | (NH4)2PtCl6 → Pt + 2NH3↑ + 2HCl↑ + 2Cl2↑ | 900℃ constant temperature for 2h |
Comparison of key experimental parameters
| Parameter category | Requirements of this standard | Differences in international general methods |
|---|---|---|
| Sedimentation time | Boiling water bath for 1h+standing for 12h | Usually standing for 8h |
| Washing method | Wash with anhydrous ethanol for 8 times | Mostly with water |
| Make-up method | ICP-AES detection of residues | Not required by some standards |
Instrument configuration specifications
Inductively coupled plasma atomic emission spectrometer must meet the following requirements:
- Platinum element detection wavelength: 214.423nm
- Relative standard deviation ≤2.5% (11 measurements of 1.0μg/mL standard solution)
- RF power 1100W, cooling gas flow 15L/min
Implementation difficulties and countermeasures
Case 1: Incomplete precipitation
The result measured by a certain laboratory was 0.8% lower. After investigation, it was found that the solution volume was not strictly controlled according to the standard (it should be kept at 50mL). After adjustment, the data returned to normal.
Case 2: Burning contamination
Using non-special crucibles leads to interference from iron elements. After replacing with special porcelain crucibles, the repeatability limit of 0.20% requirement is met.
Standard Evolution Analysis
Compared with the 2008 draft, the 2016 version has the following major improvements:
- Added ICP-AES compensation method, with an accuracy improvement of 30%
- Cleared the anhydrous ethanol washing process to reduce impurity adsorption
- Refined the instrument parameter requirements to reduce inter-laboratory deviation
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