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Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride

A Raman spectroscopy, titanium tetrachloride technology, applied in the metallurgical field, can solve the problems of few quantitative analysis, low analysis stability, weak Raman signal intensity, etc., to achieve easy online analysis, low detection cost, non-destructive The effect of online analysis

Active Publication Date: 2019-05-17
CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because Raman spectroscopy is a scattering spectrum, the Raman signal is weak, and the signal intensity is affected by factors such as excitation light source power, instrument status, sample concentration and temperature, resulting in low analysis stability. Therefore, Raman spectroscopy has been used for a long time. Qualitative analysis, rarely used for quantitative analysis

Method used

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  • Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride
  • Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride
  • Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Get 5 parts of 25ml analysis pure titanium tetrachloride and add 1ml, 2ml, 3ml, 4ml and 5ml carbon disulfide respectively, be mixed with the standard solution that carbon disulfide mass concentration is respectively 2.84%, 5.52%, 8.05%, 10.46% and 12.74%, take 5 Insert glass capillary tubes with an inner diameter of 1 mm into 5 parts of the standard solution, use capillary action to draw a small amount of standard solution, and then immediately melt the two ends of the capillary with an alcohol lamp and seal it to obtain the standard sample of the capillary to be tested; the 5 standard samples of the capillary to be tested Subtract the baseline data from the standard sample Raman spectral data obtained after Raman spectral scanning to obtain 5 corrected spectral data, and extract 654.5 cm from the corrected spectral data -1 The peak height at (carbon disulfide characteristic peak) and 395cm -1 The peak height (titanium tetrachloride characteristic peak) at place, and ca...

Embodiment 2

[0032] Take 5 parts of 25ml of analytically pure titanium tetrachloride and add 1, 2, 3, 4 and 5ml of dichloromethane respectively to prepare the standards with dichloromethane molar concentrations of 6.42%, 12.06%, 17.06%, 21.53% and 25.53% respectively. solution, take 5 glass capillary tubes with an inner diameter of 2 mm and insert them into 5 parts of standard solution respectively, use capillary action to draw a small amount of standard solution, and then immediately melt the two ends of the capillary tube with a kerosene lamp and seal it to obtain the standard sample of the capillary tube to be tested; The standard sample Raman spectrum data obtained after the standard sample of the capillary was scanned by Raman spectrum was subtracted from the baseline data to obtain 5 corrected spectral data, and 705cm -1 The peak height at (dichloromethane characteristic peak) and 395cm -1 The peak height (titanium tetrachloride characteristic peak) at place, and calculate the ratio ...

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Abstract

The invention discloses a Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride. The method comprises the following steps of S1, preparing a standard sample, wherein volume content of each organic matter in the standard sample is known; S2, measuring Raman spectrum of the obtained standard sample, thereby obtaining standard sample Raman spectrum data and baseline data; S3, obtaining standard sample corrected spectrum data according to the standard sample Raman spectrum data and baseline data, and computing a spectrum intensity ratio of the organic matters inthe standard sample according to the standard sample corrected spectrum data; S4, drawing a standard curve; and S5, detecting and analyzing a to-be-detected sample. According to the method, glass capillaries which are very cheap and are easy to get are taken as Raman detection carriers, so detection cost is low; after two ends of the glass capillaries are melted and sealed, the titanium tetrachloride is isolated from external air, so the sample can be stored for a long time; and a detection error resulting from hydrolysis of the titanium tetrachloride can be avoided, so detection accuracy isimproved.

Description

technical field [0001] The invention relates to detection technical means in the field of metallurgy, in particular to a Raman spectrum rapid detection method for organic matter in titanium tetrachloride. Background technique [0002] Titanium tetrachloride occupies the core position of the titanium industry and is an important intermediate product for the preparation of titanium sponge and titanium dioxide. The quality of titanium tetrachloride directly affects the quality of titanium sponge and titanium dioxide. The impurities in titanium tetrachloride will be multiplied in the process of producing sponge titanium and titanium dioxide. Therefore, the analysis and control of impurities in titanium tetrachloride is the key to the quality control of sponge titanium and titanium dioxide. In order to remove impurities in titanium tetrachloride during production, it is necessary to perform rapid quantitative determination of the impurity content in order to control its quality. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
Inventor 向小艳夏文堂段渊尹建国袁晓丽安娟
Owner CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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