Pretreatment method for detecting boron impurities of titanium dioxide

Abstract

The invention relates to a pretreatment method for detecting boron impurities of slagging constituent, in particular to a pretreatment method for detecting boron impurities of titanium dioxide, which comprises the following steps: adding nitric acid and hydrofluoric acid into titanium dioxide so as to enable titanium dioxide to be dissolved, adding propylene glycol to be subjected to complexation with boron after diluting acidity through adding water, performing oscillation and standing, extracting boron complex by adopting normal hexane, then performing standing stratification, heating the normal hexane phase of the upper layer till full volatilization, adding nitric acid into the residue, then adding water for dilution, and finally performing detection after constant volume. The method has the advantages as follows: the gathering function of boron is obvious, few titanium ions exist in the solution to be detected, the influence of the matrix effect is greatly reduced, and the extraction yield is greater than 90%; the recovery of the boron can be improved to more than 95% from 80-82%, and the method detection limit of the boron is reduced to 0.5 ppm from 2 ppm; in addition, the pollution to the sampling system of an apparatus is avoided, and the method is simple and easy to operate, and improves the detection accuracy.

Description

technical field

[0001] The invention relates to a pretreatment method for detecting boron impurities in a slagging agent, in particular to a pretreatment method for detecting boron impurities in titanium dioxide. Background technique

[0002] In a society where energy is scarce and low-carbon environmental protection is advocated, solar energy, as an environmentally friendly new energy, has great application value. Solar cells can convert solar energy into electrical energy, and solar-grade polysilicon materials are important raw materials for solar cells. Therefore, the preparation technology of solar-grade polysilicon materials is particularly important. At present, the main technical routes for preparing solar-grade polysilicon materials worldwide include: improved Siemens method, silane method, and metallurgical method. The principle of the improved Siemens method is to use high-purity hydrogen to reduce high-purity trichlorosilane on a high-purity silicon core at a tem...

Examples

Embodiment 1

[0023] A pretreatment method step for detecting boron impurities in titanium dioxide:

[0024] (1) Sampling: Weigh 0.5g sample of titanium dioxide into a PTFE beaker.

[0025] (2) Sample digestion: Add 2.0ml of nitric acid with a mass fraction of 70% and 1.0ml of hydrofluoric acid with a mass fraction of 49% into the beaker to completely digest the sample.

[0026] (3) Propylene glycol complexed boron: add 5.0ml of water to the digestion solution to dilute, measure 2.0ml of propylene glycol into the beaker, ultrasonically oscillate for 3 minutes and then let stand for 5 minutes.

[0027] (4) Transfer and liquid separation: Pour the solution in the beaker into the PP separating funnel, wash the beaker, and put the washing liquid into the PP separating funnel.

[0028] (5) Add n-hexane for stratification: Add 5.0ml of n-hexane into the PP separatory funnel, shake and let stand for stratification, ultrasonically oscillate for 3 minutes, and let stand for 5 minutes to take the up...

Embodiment 2

[0032] The steps of a pretreatment method for detecting boron impurities in titanium dioxide are as follows:

[0033] (1) Sampling: Weigh 1.0g sample of titanium dioxide into a PTFE beaker.

[0034] (2) Sample digestion: Add 2.5ml of nitric acid with a mass fraction of 70% and 2.0ml of hydrofluoric acid with a mass fraction of 49% to the beaker to completely digest the sample.

[0035] (3) Propylene glycol-complexed boron: add 10.0ml of water to the digestion solution to dilute, measure 2.0ml of propylene glycol into the beaker, ultrasonically oscillate for 5 minutes and then let stand for 10 minutes.

[0036] (4) Transfer and liquid separation: Pour the solution in the beaker into the PP separating funnel, wash the beaker, and put the washing liquid into the PP separating funnel.

[0037] (5) Add n-hexane for layering: Add 7.0ml of n-hexane into the PP separatory funnel, shake and let stand for stratification, ultrasonically oscillate for 5 minutes, and let stand for 10 minu...

technical field

[0001] The invention relates to a pretreatment method for detecting boron impurities in a slagging agent, in particular to a pretreatment method for detecting boron impurities in titanium dioxide. Background technique

[0002] In a society where energy is scarce and low-carbon environmental protection is advocated, solar energy, as an environmentally friendly new energy, has great application value. Solar cells can convert solar energy into electrical energy, and solar-grade polysilicon materials are important raw materials for solar cells. Therefore, the preparation technology of solar-grade polysilicon materials is particularly important. At present, the main technical routes for preparing solar-grade polysilicon materials worldwide include: improved Siemens method, silane method, and metallurgical method. The principle of the improved Siemens method is to use high-purity hydrogen to reduce high-purity trichlorosilane on a high-purity silicon core at a tem...

Examples

Embodiment 1

[0023] A pretreatment method step for detecting boron impurities in titanium dioxide:

[0024] (1) Sampling: Weigh 0.5g sample of titanium dioxide into a PTFE beaker.

[0025] (2) Sample digestion: Add 2.0ml of nitric acid with a mass fraction of 70% and 1.0ml of hydrofluoric acid with a mass fraction of 49% into the beaker to completely digest the sample.

[0026] (3) Propylene glycol complexed boron: add 5.0ml of water to the digestion solution to dilute, measure 2.0ml of propylene glycol into the beaker, ultrasonically oscillate for 3 minutes and then let stand for 5 minutes.

[0027] (4) Transfer and liquid separation: Pour the solution in the beaker into the PP separating funnel, wash the beaker, and put the washing liquid into the PP separating funnel.

[0028] (5) Add n-hexane for stratification: Add 5.0ml of n-hexane into the PP separatory funnel, shake and let stand for stratification, ultrasonically oscillate for 3 minutes, and let stand for 5 minutes to take the up...

Embodiment 2

[0032] The steps of a pretreatment method for detecting boron impurities in titanium dioxide are as follows:

[0033] (1) Sampling: Weigh 1.0g sample of titanium dioxide into a PTFE beaker.

[0034] (2) Sample digestion: Add 2.5ml of nitric acid with a mass fraction of 70% and 2.0ml of hydrofluoric acid with a mass fraction of 49% to the beaker to completely digest the sample.

[0035] (3) Propylene glycol-complexed boron: add 10.0ml of water to the digestion solution to dilute, measure 2.0ml of propylene glycol into the beaker, ultrasonically oscillate for 5 minutes and then let stand for 10 minutes.

[0036] (4) Transfer and liquid separation: Pour the solution in the beaker into the PP separating funnel, wash the beaker, and put the washing liquid into the PP separating funnel.

[0037] (5) Add n-hexane for layering: Add 7.0ml of n-hexane into the PP separatory funnel, shake and let stand for stratification, ultrasonically oscillate for 5 minutes, and let stand for 10 minu...