Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof

A spectral measurement and volatility technology, applied in the field of instrument analysis, can solve problems affecting the accuracy of research, and achieve the effects of good quality, improved measurement accuracy, and high signal-to-noise ratio

Inactive Publication Date: 2010-01-20
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The biggest disadvantage of the above sample pool is that: since the research molten salt inevitably volatilizes to the outside world, if the composition of the v

Method used

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  • Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof
  • Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof
  • Sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and use method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The Raman spectrum measurement method of high-temperature volatile molten salt using the above-mentioned sample cell is as follows.

[0037] The cryolite (Na) of the sample to be analyzed 3 AlF 6 ) After being loaded into the platinum crucible, the gap between the crucible cover and the opening of the platinum crucible is sealed with high-temperature quick-drying cement, so that the molten salt volatiles will not escape and reduce the composition change caused by the uneven volatilization of the sample. For Raman The effect of spectrometry.

[0038] During the measurement, current was supplied to the heating platinum wire, the sample to be analyzed was heated to a measurement temperature of 1015°C, and the temperature of the platinum crucible was measured with a thermocouple, that is, the temperature of the molten salt sample in the platinum crucible was measured. The temperature gradient inside the platinum crucible is very small. The crucible cover and the molten sa...

Embodiment 2

[0046] The method for measuring the Raman spectrum of a high-temperature volatile molten salt using the sample cell of the present invention is as follows.

[0047] The samples to be analyzed (NaF and AlF 3 NaF-AlF with a molar ratio of 1:1 3 mixture) into the platinum crucible, the gap between the crucible cover and the platinum crucible mouth is sealed with high-temperature quick-drying cement.

[0048] During the measurement process, a current is supplied to the heating platinum wire, and the sample to be analyzed is heated to the measurement temperature of 941°C, 981°C, and 1024°C in sequence, and the temperature of the platinum crucible is measured with a thermocouple, that is, the temperature of the molten salt sample in the platinum crucible is measured.

[0049] The sample cell is used with the HR800 microlaser Raman spectrometer of Horiba Jobin Y'von Company. During the measurement, the microscope lens of the Raman spectrometer is aligned with the hole in the center...

Embodiment 3

[0054] The method for measuring the Raman spectrum of a high-temperature volatile molten salt using the sample cell of the present invention is as follows.

[0055] The samples to be analyzed (NaF and AlF 3 NaF-AlF with a molar ratio of 1.5:1 3 mixture) into the platinum crucible, the gap between the crucible cover and the platinum crucible mouth is sealed with high-temperature quick-drying cement.

[0056] During the measurement process, a current is supplied to the heating platinum wire, and the sample to be analyzed is heated to the measurement temperature of 942°C, 981°C, and 1024°C in sequence, and the temperature of the platinum crucible is measured with a thermocouple, that is, the temperature of the molten salt sample in the platinum crucible is measured.

[0057] The sample cell is used with the HR800 microlaser Raman spectrometer of Horiba Jobin Y'von Company. During the measurement, the microscope lens of the Raman spectrometer is aligned with the hole in the cent...

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Abstract

The invention provides a sealed sample cell for Raman spectrum measurement of high-temperature volatile molten salt and a use method thereof. The sample cell comprises a platinum crucible, a crucible cover, a hearth, a hearth cover and heating platinum wires. The use method is characterized by adopting high-temperature alumina cement to seal the gap between the crucible cover and the mouth of the platinum crucible after feeding samples to be analyzed into the platinum crucible; during measurement, providing current for the heating platinum wires to heat the samples to be analyzed to the measurement temperature, adopting a thermocouple to measure the temperature of the platinum crucible; using the sample cell by matching an upper laser inlet type micros laser Raman spectrometer. The sealed sample cell of the invention can be used for Raman spectrum analysis of the high-temperature volatile molten salt such as cryolite and NaF-AlF3 molten salt with different mol ratios. The use method of the invention can avoid the ingredients of the molten salt to be measured from being affected by escape of the volatile substances, thus improving the measurement precision of the Raman spectrum.

Description

technical field [0001] The invention belongs to the technical field of instrument analysis, and in particular relates to the Raman spectrum measurement technology of high-temperature volatile molten salt. Background technique [0002] High-temperature fluoride or chloride molten salt has the characteristics of high temperature, corrosiveness, volatility, etc. Therefore, special materials and techniques are required to realize the Raman spectroscopy measurement of its molten salt structure. Several types of sample cells have been developed for Raman spectrometry of volatile molten salts at home and abroad, but they all have shortcomings. [0003] like Figure 4 Shown is a windowless sample cell for high-temperature corrosive molten salt Raman spectroscopy, which uses the surface tension effect of the liquid to prevent the molten salt from flowing out of the sample cell; the windowless sample cell was later improved, Two smaller diameter holes were added in the same plane of ...

Claims

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Application Information

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IPC IPC(8): G01N21/01G01N21/65C04B9/06
Inventor 胡宪伟王兆文高炳亮石忠宁于亚鑫
Owner NORTHEASTERN UNIV
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