Infrared spectrum quantitative analysis method of gas fluoride
An infrared spectroscopy and quantitative analysis technology, which is applied in the field of infrared spectroscopy quantitative analysis of gas fluoride, can solve the problems of errors and inability to quantitative analysis, and achieve the effects of avoiding errors, direct and simple analysis methods, and improving analysis efficiency.
Pending Publication Date: 2020-07-14
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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Problems solved by technology
[0005] The technical problem actually solved by the present invention is to overcome the existing infrared spectroscopy technology for the highly corrosive gas fluoride, which cannot be quantitatively analyzed through the absorption coefficient, and the unnecessary error usually caused by the quantitative analysis of gas based on the ideal gas state equation. defects, providing a method for quantitative analysis of gas fluoride by infrared spectroscopy
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Embodiment 1
[0060] In Example 1, MoF 6 Quantitative analysis of infrared spectroscopy as an example to illustrate, MoF 6 Produced by the reaction of fluorine gas and metal Mo foil.
[0061] Example 1
[0062] 1. Accurately weigh 1g of Mo foil and place it in the reactor part. After connecting the pipeline, vacuumize to confirm the airtightness of the overall system, including the gas preheating part, the reactor part, the gas sample pool of the infrared detection part, and the condensation collection part.
[0063] 2. The pipeline and cold trap of the reactor part and the condensate collection part are heated to 100 ° C, and 10 mL / min of fluorine and argon mixed gas (fluorine gas volume percentage 20%) and 10 mL / min of argon pretreatment (mentioned above The gas also needs to be preheated to 100°C), and flows through the infrared spectrum to quantitatively analyze the entire device and pipeline to remove trace moisture and avoid MoF 6 loss of response;
[0064] 3. After the pretreatme...
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The invention discloses an infrared spectrum quantitative analysis method of gas fluoride. The method comprises the following steps: (1) in fluoride preparation, carrying out infrared spectrum detection on gases obtained at different reaction times; (2) obtaining a unit pressure absorbance change curve by taking t as an abscissa and the unit pressure absorbance as an ordinate; (3) integrating theabsorbance per unit pressure relative to t to obtain an integral area; (4) repeating the steps (1)-(3), preparing fluorides with different masses to obtain at least three groups of integral areas, andcollecting the mass of each group of fluorides; 5, fitting to obtain a standard linear regression equation by taking the integral area as an abscissa and the fluoride mass as an ordinate; (6) substituting the integral area of any reaction curve into the equation. On the basis of the infrared spectrum technology, the relation between the unit pressure absorbance change curve integral area and thecondensation collection amount is established in combination with the condensation collection operation, the mass of fluoride can be directly calculated after the related standard curve is obtained, the operation process is simplified, and the analysis efficiency is improved.
Description
technical field [0001] The invention belongs to the technical fields of nuclear energy industry technology and dry metallurgy, and in particular relates to an infrared spectrum quantitative analysis method of gas fluoride. Background technique [0002] The fluorination and volatilization method is the key technology for the separation and recovery of uranium in the dry post-processing, because the fluorination volatile products except F 2 In addition, it also contains UF 6 、MoF 6 , TcF 6 Fluoride gases with strong oxidizing and corrosive properties, they are especially sensitive to moisture in the air, and are prone to hydrolysis reaction to produce metal oxyfluoride and toxic HF, and can also react with most metal substances, so conventional Advanced instruments (such as gas chromatography, gas chromatography mass spectrometry, etc.) are difficult to achieve effective and accurate analysis. Infrared spectrometer has the characteristics of high sensitivity, rapid detecti...
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Login to View More IPC IPC(8): G01N21/3504G01N1/28G01N1/42
CPCG01N21/3504G01N1/28G01N1/42
Inventor 程治强崔荣荣窦强李晴暖
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI