GB/T 4698.10-2020 in English
VALIDMethods for chemical analysis of titanium sponge, titanium and titanium alloys—Part 10:Determination of chromium content—Ammonium ferrous sulfate titration and inductively coupled plasma atomic emission spectrometry(with vanadium)
- Issued on:2020-03-06
- Implemented on:2021-02-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$156.00
《GB/T 4698.10-2020海绵钛、钛及钛合金化学分析方法 第10部分:铬量的测定 硫酸亚铁铵滴定法和电感耦合等离子体原子发射光谱法(含钒)》由TC243(全国有色金属标准化技术委员会)归口,TC243SC3(全国有色金属标准化技术委员会稀有金属分会)执行,主管部门为中国有色金属工业协会。
Introduction
Core changes in the standard revision
| Technical indicators | 1996 edition | 2020 edition | Improvement significance |
|---|---|---|---|
| Determination range | 0.30%-12.00% | Method 1: 0.30%-15.00% Method 2: 0.010%-15.00% | Extended detection limit, covering a wider content range |
| New methods | Ammonium ferrous sulfate titration method only | ICP-AES method added | Provide highly sensitive modern detection methods |
| Precision clause | Not specified | Add repeatability/reproducibility limit | Reliability index of quantitative method |
Method 1: Technical analysis of ammonium ferrous sulfate titration
Key reaction mechanism:Separation and determination of vanadium and chromium by selective oxidation:
①Selective oxidation of vanadium by KMnO4 at room temperature (V4+→V5+)
② Co-oxidation of vanadium chromium under heating conditions (NH4)2S2O8/AgNO3 (Cr3+→Cr6+)
Typical operating parameters:
• Dissolution system: H2SO4(1+1)+HNO3 digestion
• Indicator: N-phenylanthranilic acid (pink→yellow-green endpoint)
• Titrant concentration: 0.025mol/L (NH4)2Fe(SO4)2
Method 2: Key points of innovation in ICP-AES method
Instrument configuration requirements:
• Hydrofluoric acid resistant injection system
• Resolution <0.006nm@200nm
• Recommended analysis line: Cr 283.56nm
Sample pretreatment:
Dissolve in HCl-HF mixed acid, oxidize titanium with HNO3, and use plastic volumetric flask to set the volume to prevent fluorine corrosion
Calibration strategy:
Establish working curves in sections (0.01-8% and 8-15%), and use high purity titanium (wCr <0.001%) for matrix matching
Implementation suggestions and precautions
- Method selection principle:>0.3% preferably uses titration method (arbitration method), <0.3% must use ICP-AES method
- Interference control: The vanadium content in the titration method must be accurately deducted, and the ICP-AES method should pay attention to the spectral interference of the titanium matrix
- Quality control: Each batch of tests should be verified with a standard sample (such as YSBC18804-1 titanium alloy standard sample)
- Safety protection: Calcium gluconate gel should be provided for emergency use when treating with hydrofluoric acid
Technology evolution analysis
This standard reflects the transformation of titanium alloy detection technology from traditional wet chemical method to instrumental analysis:
• 1984 version: Volumetric method only
• 1996 version: Optimized titration conditions
• 2020 Edition: Introducing ICP-AES to achieve full coverage of high and low content, and reduce the detection limit by 30 times

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