GB/T 4702.18-2020 in English
VALIDChromiun metal—Determination of vanadium content—Tantalum reagent trichloromethane extraction spectrophtometry method
- Issued on:2020-03-06
- Implemented on:2020-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$156.00
《GB/T 4702.18-2020金属铬 钒含量的测定 钽试剂三氯甲烷萃取分光光度法》由TC318(全国生铁及铁合金标准化技术委员会)归口,TC318SC1(全国生铁及铁合金标准化技术委员会化学分析分会)执行,主管部门为中国钢铁工业协会。
Introduction
Technical background and evolution of standards
As the 18th part of the GB/T 4702 series, this standard improves the analysis system of metallic chromium. Compared with the traditional chemical analysis method, the detection limit of the method is reduced to 0.010% by using spectrophotometer combined with organic solvent extraction technology, which significantly improves the detection accuracy of trace vanadium.
Detailed explanation of the principle of the method
In the sulfuric acid-perchloric acid medium, after the chromium is volatilized and removed by chromyl chloride, pentavalent vanadium and tantalum reagent form a purple-red complex. After extraction with chloroform, the absorbance is measured at a wavelength of 530nm. Key reaction equation:
| Reaction stage | Chemical process | Key control points |
|---|---|---|
| Pretreatment | Cr + 3HClO4→H2CrO4 + Cl2↑ | Yellow smoke completely disappeared |
| Color development | VO3- + Tantalum reagent→[V-Tantalum reagent] complex | pH<1 |
Key operating specifications
Practical application cases
When a steel plant tested ferrochrome (Cr content 92.3%), 0.400g of sample was weighed and 10mL of test solution was taken. The calibration curve showed that 3.50μg of vanadium standard solution corresponded to an absorbance of 0.217, and the sample measured value was 0.203. The vanadium content was calculated to be 0.042%, and RSD = 1.8%.
| Parameters | Requirements | Allowance Deviation |
|---|---|---|
| Sample Weight | 0.200g/0.400g | ±0.0001g |
| Oscillating Time | 60s | ±5s |
| Standing Stratification | 10min | ±0.5min |
Quality Control Requirements
The laboratory allows strict classification of tolerance: when the vanadium content is 0.010%~0.050%, the tolerance is 0.004%; when it is 0.10%~0.50%, it is relaxed to 0.025%. The instrument performance needs to be verified regularly with standard substances to ensure the wavelength accuracy of the spectrophotometer is ±2nm.
Implementation suggestions
- The perchloric acid fume phase must be completed in a fume hood to avoid the escape of chromyl chloride
- After color development, the determination should be completed within 30 minutes to prevent the decomposition of the complex
- When the chloroform extract is emulsified, a small amount of ethanol can be added to break the emulsion

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