Rapid exact stable reliable silicon iron sample digestion method

An accurate and stable technology, used in chemical analysis by titration, preparation of samples for testing, etc., can solve problems such as unfavorable quantitative detection of large-scale samples, volatile silicon tetrafluoride, and low measurement results, and achieve good promotion. Application value, reducing the solubility of precipitates, and the effect of simple and quick operation

Inactive Publication Date: 2014-04-23
WUKUN STEEL
View PDF3 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the gravimetric method is used to determine the silicon content with high accuracy, but the operation time is long, which is not conducive to the quantitative detection of large batches of samples
Potassium fluorosilicate titration method has the advantages of simple operation and rapid determination of large quantities of samples. However, in conventional detection operations, due to the violent digestion reaction, the silicon tetrafluoride produced by the reaction of silicon and hydrofluoric acid is very volatile. lead to low test results

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A. Dissolution: Put 0.1000g of the ferrosilicon sample to be digested into a polytetrafluoroethylene digestion bottle, add 10ml of concentrated nitric acid and 5ml of hydrofluoric acid in turn, then seal the digestion bottle and shake it gently; Place the digestion bottle in a water bath, heat at 60°C for 5 minutes, and then cool the sample solution to 23°C with running water.

[0027] B. Precipitation: After the sample solution in step A is cooled, add 5ml of 5% urea solution, 10ml of 15% potassium fluoride solution and 2.5g of potassium nitrate in sequence, seal and shake well, then cool in running water for 15min.

[0028] C. Filtration: filter the cooled sample solution in step B with a quantitative filter paper in a polytetrafluoroethylene sample bottle, and wash the digestion bottle and the precipitation with 10ml of 15% potassium chloride solution three times, and move the precipitation and the filter paper into a polytetrafluoroethylene sample bottle. Add 15ml o...

Embodiment 2

[0031] A. Dissolution: Put 0.1200g of the ferrosilicon sample to be digested into a polyethylene digestion bottle, add 11ml of concentrated nitric acid and 6ml of hydrofluoric acid in turn, then seal the digestion bottle and shake it gently; after the sample is dissolved, put the digestion bottle Place in a heating mantle, heat at 55°C for 6min, and then cool the sample solution to 20°C with a cold water bath.

[0032] B. Precipitation: After the sample solution in step A is cooled, add 6ml of 5% urea solution, 11ml of 15% potassium fluoride solution and 3g of potassium nitrate in sequence, seal and shake well, then cool in a cold water bath for 18min.

[0033] C. Filtration: Filter the cooled sample solution in step B into a polytetrafluoroethylene sample bottle with quantitative filter paper, and wash the digestion bottle and the precipitate with 11ml of 15% potassium chloride solution four times each, and move the precipitate and filter paper into Add 18ml of 5% potassium c...

Embodiment 3

[0036] A. Dissolution: Put 0.0800g of the ferrosilicon sample to be digested into a polytetrafluoroethylene digestion bottle, add 9ml of concentrated nitric acid and 4ml of hydrofluoric acid in sequence, then seal the digestion bottle and shake it gently; Place the digestion bottle in a microwave digestion apparatus, heat at 65°C for 4min, and then cool the sample solution to 25°C with running water.

[0037] B. Precipitation: After the sample solution in step A is cooled, add 4ml of 5% urea solution, 9ml of 15% potassium fluoride solution and 2g of potassium nitrate in sequence, seal and shake well, then cool in running water for 12min.

[0038] C. Filtration: Filter the cooled sample solution in step B into a polytetrafluoroethylene beaker with quantitative filter paper, and wash the digestion bottle and the precipitation twice with 9ml of 15% potassium chloride solution, and move the precipitation and filter paper into a polytetrafluoroethylene beaker. Add 12ml of 5% potass...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a rapid exact stable reliable silicon iron sample digestion method, and belongs to the technical field of test analysis sample pretreatment. The method comprises the steps of firstly placing 0.0800-0.1200g of silicon iron sample into a plastic digestion bottle, successively adding 9-11ml of nitric acid and 4-6ml of hydrofluoric acid, and sealing the digestion bottle; placing the digestion bottle into a heater to heat for 4-6 min under the temperature of 55-65 DEG C after the sample is dissolved, and then cooling the sample to 20-25 DEG C; successively adding 4-6ml of urea solution, 9-11ml of potassium fluoride solution and 2-3g of potassium nitrate, sealing and shaking up, and cooling for 12-18min; filtering a sample solution in a sample bottle, washing the digestion bottle and sedimentation by using the 9-11ml of potassium fluoride solution; shifting the sedimentation and a filter material into a plastic sample bottle, and adding 12-18ml of potassium chloride-ethanol solution. The digestion method provided by the invention has the advantages that various losses in the sample treatment are effectively prevented, the stability, reproducibility and veracity of a testing result are improved, the dissolution is rapid, the sample manufacturing time is shortened, a sample solution is directly used for measuring silicon content, the method is simple and rapid, and the popularization and application value is good.

Description

technical field [0001] The invention belongs to the technical field of test and analysis sample pretreatment, and in particular relates to a fast, accurate, stable and reliable ferrosilicon sample digestion method. Background technique [0002] The commonly used chemical analysis methods for determining the silicon content in ferrosilicon alloys mainly include gravimetric method and potassium fluorosilicate titration method. Among them, the determination of silicon content by gravimetric method has high accuracy, but the operation time is long, which is not conducive to the quantitative detection of large batches of samples. The potassium fluorosilicate titration method has the advantages of simple operation and rapid determination of large quantities of samples. However, in conventional detection operations, due to the excessive digestion reaction, the silicon tetrafluoride produced by the reaction of silicon and hydrofluoric acid is very volatile. resulting in low measure...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N31/16
Inventor 朵勇陈彬彬段璇苏莉周字勇张炬
Owner WUKUN STEEL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap