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A method for detecting free hydrochloric acid content in titanium tetrachloride aqueous solution

An aqueous solution and content technology, applied in the field of analytical chemistry, can solve the problems of less aqueous solution and unsuitable detection and analysis of extremely acidic system of aqueous solution, and achieve the effect of mild process, simple and practical method, and strong operability

Inactive Publication Date: 2016-05-11
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Currently, for TiCl 4 The research on the detection and analysis methods of aqueous solution is still relatively small, and the analysis methods of advanced precision instruments are not suitable for TiCl 4 Detection and Analysis of Aqueous Extreme Acid System

Method used

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  • A method for detecting free hydrochloric acid content in titanium tetrachloride aqueous solution
  • A method for detecting free hydrochloric acid content in titanium tetrachloride aqueous solution
  • A method for detecting free hydrochloric acid content in titanium tetrachloride aqueous solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 5 mL of TiCl with a concentration of 1.99 mol / L 4 Put the aqueous solution in a beaker; slowly add 0.5mol / L NaOH standard solution drop by drop, and use a pH meter to measure the pH value of the solution while dropping, and control the pH value of the end point of the solution to be less than 0.1, according to the amount of NaOH standard solution added and the end point of the solution pH value, calculated to get the original TiCl 4 The content of free HCl in the aqueous solution; three groups were measured repeatedly under the same conditions for comparison. The calculation results are shown in Table 1.

[0036] Table 1

[0037]

[0038] As can be seen from Table 1, the free hydrochloric acid content that the 3 repeated tests of embodiment 1 detects is respectively 0.0304mol / L, 0.0323mol / L, 0.0315mol / L, after calculation, the relative deviation of its sample measurement result is 3.04 %.

Embodiment 2

[0040] Take 5 mL of TiCl with a concentration of 2.55 mol / L 4 Put the aqueous solution in a beaker; slowly add 0.5mol / L NaOH standard solution drop by drop, and use a pH meter to measure the pH value of the solution while dropping, and control the pH value of the end point of the solution to be less than 0.1, according to the amount of NaOH standard solution added and the end point of the solution pH value, calculated to get the original TiCl 4 The content of free HCl in the solution; three groups were measured repeatedly under the same conditions for comparison. The calculation results are shown in Table 2.

[0041] Table 2

[0042]

[0043]

[0044] As can be seen from Table 2, the free hydrochloric acid content that the 3 repeated tests of embodiment 2 detects is respectively 0.0409mol / L, 0.0433mol / L, 0.0417mol / L, after calculation, the relative deviation of its sample measurement result is 2.91 %.

Embodiment 3

[0046] Take 5 mL of TiCl with a concentration of 2.90 mol / L 4 Put the aqueous solution in a beaker; slowly add 0.5mol / L NaOH standard solution drop by drop, and use a pH meter to measure the pH value of the solution while dropping, and control the pH value of the end point of the solution to be less than 0.1, according to the amount of NaOH standard solution added and the end point of the solution pH value, calculated to get the original TiCl 4 The content of free HCl in the aqueous solution; three groups were measured repeatedly under the same conditions for comparison. The calculation results are shown in Table 3.

[0047] table 3

[0048]

[0049] As can be seen from Table 3, the free hydrochloric acid content that the 3 repeated tests of embodiment 3 detects is respectively 0.0478mol / L, 0.0493mol / L, 0.0500mol / L, after calculation, the relative deviation of its sample measurement result is 2.29 %.

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Abstract

The invention relates to a method for detecting content of free hydrochloric acid in a titanium tetrachloride water solution. The method comprises the following steps: 1) pumping different volumes of TiCl4 into a certain amount of ultrapure water under protection of a cold water bath by virtue of a peristaltic pump, so as to obtain different concentration of TiCl4 water solutions; 2) neutralizing TiCl4 water solutions with a standard NaOH solution, so that the pH value of the titration end point is smaller than or equal to 0.1; and 3) calculating the content of free HCl in an original TiCl4 water solution according to the gross of the standard NaOH solutions and the final pH value of the solution. The detection method provided by the invention is high in maneuverability, rapid and accurate; meanwhile, the pH value of the titration end point is controlled to be smaller than or equal to 0.1; the detection interference generated by hydrolysis is avoided; the accuracy of the detection result is improved; and the relative deviation of the detection result is smaller than 4%.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for detecting and analyzing an aqueous solution of titanium tetrachloride, in particular to a method for detecting the content of free hydrochloric acid in an aqueous solution of titanium tetrachloride. Background technique [0002] Titanium tetrachloride, the chemical formula is TiCl 4 It is an important intermediate for the production of titanium metal and its compounds. At room temperature, TiCl 4 It is a colorless or light yellow liquid, one of the few transition metal chlorides that are liquid at room temperature, highly corrosive, and has a pungent sour smell. [0003] TiCl 4 Chemically unstable, it is a strong Lewis acid, and it will react exothermicly with Lewis bases (even weak Lewis bases) to form adducts, so TiCl 4 Very volatile and hydrolyzed, TiCl 4 When the liquid is exposed to the air, it will quickly react with the moisture in the air to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16G01N31/22
Inventor 朴玲钰马佩军杜剑桥路瑞芳吴志娇张晓
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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