Separation and detection method of irradiation product DBP (Double-Base Propellant) and/or MBP (Myelin Basic Protein) in TBP (Ttri-Butyl phosphate)-kerosene-HNO3 system

A technology for the separation of -HNO3, applied in the field of irradiated product dibutyl phosphate, which can solve the problems of low sensitivity, unsuitable for control analysis, long operating procedures, etc.

Inactive Publication Date: 2010-09-15
中核二七二铀业有限责任公司
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  • Abstract
  • Description
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Problems solved by technology

[0002]Since TBP (i.e. tributyl phosphate C12H27O4 P) Since it is used as an extractant, a certain amount of DBP (i.e. dibutyl phosphate C8H19O 4P), MBP (monobutyl phosphate C4H11O4P) and other irradiation Products, when the content of DBP and MBP reaches a certain level, it is easy to produce emulsification during the extraction process and reduce the purification effect. However, a satisfactory analysis method has not been found for the analysis and detection of DBP and MBP, the degradation products of TBP after irradiation.
At present, the methods for the analysis and determination of the degradation products DBP and MBP after TBP irradiation mainly include infrared spectroscopy, gas chromatography and potentiometric titration at home and abroad. These methods not only require expensive instruments, but also lack reagents. Inadequacies such as long operating procedures or low sensitivity make these methods especially unsuitable for control analysis in production processes

Method used

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  • Separation and detection method of irradiation product DBP (Double-Base Propellant) and/or MBP (Myelin Basic Protein) in TBP (Ttri-Butyl phosphate)-kerosene-HNO3 system
  • Separation and detection method of irradiation product DBP (Double-Base Propellant) and/or MBP (Myelin Basic Protein) in TBP (Ttri-Butyl phosphate)-kerosene-HNO3 system
  • Separation and detection method of irradiation product DBP (Double-Base Propellant) and/or MBP (Myelin Basic Protein) in TBP (Ttri-Butyl phosphate)-kerosene-HNO3 system

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Experimental program
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Effect test

Embodiment 1

[0042] A TBP-kerosene-HNO 3 The separation method of the radiation product DBP and MBP in the system mainly comprises the following steps (such as figure 1 shown):

[0043] 1. Take TBP-kerosene-HNO 3 Put 9-11ml of lean organic phase samples in the uranium extraction process under the system into a 60ml separatory funnel, add 3-8% Na 2 CO 3 The solution is 9-11ml, extracted for 2-10 minutes, standing for stratification, the upper layer is the organic phase containing TBP-kerosene-HNO3 system, and the lower layer is Na containing DBP, MBP and trace TBP 2 CO 3 water box;

[0044] Two, put the Na layered in the first step 2 CO 3 The aqueous phase was put into another 60ml separatory funnel, and the 3 Wash once, the ratio is 0.8~1:0.8~1, that is, Na 2 CO 3 Aqueous phase and CHCl 3 The volume ratio is 0.8~1:0.8~1, shaking for 2~10 minutes, standing for stratification, standing for the CHCl in the stratification 3 The organic phase contains a small amount of TBP, and the ...

Embodiment 2

[0046] A TBP-kerosene-HNO 3 The separation method of the radiation product DBP or MBP in the system, after the above-mentioned two steps of embodiment 1, also includes the following steps:

[0047] Three, get the clarification Na in the second step of embodiment 1 static stratification 2 CO 3 Water phase 4~6ml, add 4~6mol / L sulfuric acid dropwise to near neutrality, pH value is equal to 6.5~7.5, that is, PH=6.5~7.5, then add 4~6ml 4.5~5.5mol / L sulfuric acid solution, at this time the solution The acidity is 3~4mol / L, after shaking gently, add 9~11ml of CHCl 3 Extract for 1 to 3 minutes, stand still for more than 15 minutes; let the CHCl in the stratified 3 The organic phase contains DBP; the H in the standing stratification 2 SO 4 The aqueous phase contains MBP.

Embodiment 3

[0049] A TBP-kerosene-HNO 3 The detection method of the radiation product DBP in the system, after the above-mentioned three steps of embodiment 2, also includes the following steps:

[0050] 4. Add 18-22ml of distilled water to a 100ml beaker, and take the CHCl extracted in the third step of Example 2 above 3 Put 4-6ml of the organic phase in the beaker, add 0.4-0.6g of ammonium superphosphate, and after it dissolves, put it in a boiling water bath and heat until the organic phase disappears, then move to a low-temperature electric furnace, continue boiling for 3-6 minutes, and heat Rinse the wall of the cup with water. After cooling down slightly, add 0.4-0.6g of sodium sulfite. After dissolving, heat to boiling. Take off the beaker. At this time, the organic phosphorus of DBP in the beaker is converted into inorganic phosphorus. Use the phosphomolybdenum blue colorimetric method Determination of DBP content.

[0051] Experimental data 1

[0052] Take two TBP-kerosene-HNO...

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Abstract

The invention relates a separation and detection method of an irradiation product DBP (Double-Base Propellant) and/or MBP (Myelin Basic Protein) in a TBP (Tri-Butyl Phosphate)-kerosene-HNO3 system, which is characterized by comprising the following steps of: firstly, extracting the TBP-kerosene-HNO3 system containing the irradiation product DBP and MBP with a Na2CO3 solution and separating to obtain an organic phase containing a TBP-kerosene-HNO3 system and a Na2CO3 aqueous phase containing DBP, MBP and micro TBP; and secondly, extracting the obtained Na2CO3 aqueous phase containing DBP, MBP and micro TBP with CHCl3 and separating to obtain a CHCl3 organic phase containing micro TBP and a Na2CO3 aqueous phase containing DBP and MBP. The separation and detection method is simple and convenient, does not need expensive instruments and has a short analysis period.

Description

technical field [0001] The present invention relates to TBP-kerosene-HNO in extraction processes, mainly in the nuclear industry 3 systems, specifically involving TBP-kerosene-HNO 3 The degradation rate of tributyl phosphate (commonly known as TBP) in the system, especially a TBP-kerosene-HNO 3 The separation and detection method of the irradiation products dibutyl phosphate and monobutyl phosphate in the system. Background technique [0002] Since TBP (i.e. tributyl phosphate C 12 h 27 o 4 P) Since it was used as an extractant, a certain amount of DBP (i.e. dibutyl phosphate C 8 h 19 o 4 P), MBP (monobutyl phosphate C 4 h 11 o 4 P) and other irradiation products, when the content of DBP and MBP reaches a certain level, in the extraction process, it is easy to produce emulsification and reduce the purification effect. However, the analysis and detection of the degradation products DBP and MBP after the irradiation of TBP have not been found. A satisfactory analysi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11G01N21/78
Inventor 邱湘莲陶玉秋刘云岗陈慧颜春林
Owner 中核二七二铀业有限责任公司
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