Rapid exact stable reliable silicon iron sample digestion method

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...

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