GB/T 14353.19-2019 in English
VALIDMethods for chemical analysis of copper ores, lead ores and zinc ores—Part 19:Determination of tin content—Hydride generation atomic fluorescence spectrometry
- Issued on:2019-10-18
- Implemented on:2020-05-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$156.00
《GB/T 14353.19-2019铜矿石、铅矿石和锌矿石化学分析方法 第19部分：锡量测定 氢化物发生原子荧光光谱法》由TC93（全国自然资源与国土空间规划标准化技术委员会）归口，主管部门为自然资源部(国土)。
Introduction
1. Background of standard formulation and analysis of technological evolution
GB/T 14353 "Chemical analysis methods for copper, lead and zinc ores" is one of the important industry standards in China, which aims to standardize the determination methods of trace elements in metal ores. This part (Part 19) first introduced hydride generation atomic fluorescence spectrometry (HG-AFS) for the determination of tin content, replacing the traditional flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry.
The core advantages of this method are:
- High sensitivity: The detection limit is as low as 0.001%
- Good selectivity: Through hydride generation and atomic fluorescence technology, matrix interference is effectively eliminated
- Easy to operate: Suitable for large-scale sample analysis in the laboratory
2. Principle and steps of the method
The workflow of hydride generation atomic fluorescence spectrometry is as follows:
- Sample dissolution and pretreatment: The ore sample is dissolved with hydrochloric acid and nitric acid, and the pH is adjusted to 4.5 with ammonia water to form iron hydroxide precipitation as a carrier to separate interfering elements such as copper, lead, and zinc.
- Enrichment and secondary separation: The tin-containing precipitate is melted with sodium oxide and extracted with hot water to further remove interfering components.
- Chemometric analysis: Add masking agents (tartaric acid, thiourea, ascorbic acid) to an acidic medium to generate stannic hydrogen, which is then loaded into an atomizer through argon gas and decomposed into atomic tin.
- Fluorescence intensity detection: Use a high-intensity hollow cathode lamp to excite and measure the characteristic fluorescence intensity of tin atoms, establish a calibration curve, and calculate the tin content in the sample.
3. Comparative analysis of standard frameworks
| Standard dimensions | GB/T 14353.19—2019 | Traditional flame atomic absorption spectrometry | ICP-MS method |
|---|---|---|---|
| Sensitivity (detection limit) | 0.001% | 0.01%~0.1% | 0.005%~0.01% |
| Interference elimination | High-efficiency separation and masking technology | Complex matrix effect | Requires complex removal of non-metallic matrix |
| Operation cost | Low | High (requires high-frequency generator) | High (expensive equipment and complex maintenance) |
4. Implementation suggestions and precautions
Key points for sample preparation:
- Ensure that the sample particle size is less than 74μm
- The dried sample needs to be stored in a sealed container to prevent oxidation
- Choose the appropriate sample amount according to the tin content range (refer to Table 1)
Content range% Sample amount (mg) <0.005 0.5 0.005~<0.02 0.2
Instrument calibration recommendations:
- Regularly calibrate the working parameters of the atomic fluorescence spectrometer (refer to Table A.1)
- Perform blank tests and standard substance verification before each batch of analysis
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