CN101830924B - 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 - Google Patents

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 Download PDF

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CN101830924B
CN101830924B CN201010139386A CN201010139386A CN101830924B CN 101830924 B CN101830924 B CN 101830924B CN 201010139386 A CN201010139386 A CN 201010139386A CN 201010139386 A CN201010139386 A CN 201010139386A CN 101830924 B CN101830924 B CN 101830924B
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mbp
dbp
tbp
water
chcl
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CN101830924A (en
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邱湘莲
陶玉秋
刘云岗
陈慧
颜春林
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CNNC 272 URANIUM INDUSTRY Co Ltd
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Abstract

The invention relates a separation and detection method of an irradiation product DBP (Double-Base Propellant) 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 obtainan 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

TBP-kerosene-HNO 3Irradiation product DBP in the system or separation and the detection method of MBP
Technical field
The present invention relates to the TBP-kerosene-HNO in the extraction process (mainly being the extraction process in the nuclear industry) 3System specifically relates to TBP-kerosene-HNO 3The degradation rate of the tributyl phosphate in the system (being commonly called as TBP), particularly a kind of TBP-kerosene-HNO 3Irradiation product dibutyl phosphate in the system, the separation and the detection method of monobutyl phosphate.
Background technology
Since TBP (is tributyl phosphate C 12H 27O 4P) be used as since the extraction agent, because acidity, temperature and irradiation, can produce a certain amount of DBP (is dibutyl phosphate C 8H 19O 4P), MBP (is monobutyl phosphate C 4H 11O 4P) etc. irradiation product when the content of DBP, MBP reaches certain, in extraction process, is easy to generate emulsification, reduces decontamination effect improving, and the degraded product DBP behind the irradiation of TBP, MBP analyzing and testing is not found always the analytical procedure of a satisfaction at present.The domestic and international at present method to the degraded product DBP behind the irradiation of TBP, MBP assay determination mainly contains infrared light popularize law, vapor-phase chromatography and potentiometric titration etc.; These methods not only need expensive instrument; And reagent lacks; In various degree exist weak points such as the long or sensitivity of schedule of operation is lower, these methods especially are not suitable for the control analysis in the production process.
Summary of the invention
First purpose of the present invention is to overcome the above-mentioned deficiency of prior art and a kind of TBP-kerosene-HNO is provided 3Irradiation product DBP in the system and the separation method of MBP.
Second purpose of the present invention is to overcome the above-mentioned deficiency of prior art and a kind of TBP-kerosene-HNO is provided 3Irradiation product DBP in the system or the separation method of MBP.
The 3rd purpose of the present invention is to overcome the above-mentioned deficiency of prior art and a kind of TBP-kerosene-HNO is provided 3The detection method of irradiation product DBP in the system.
The 4th purpose of the present invention is to overcome the above-mentioned deficiency of prior art and a kind of TBP-kerosene-HNO is provided 3The detection method of irradiation product MBP in the system.
First technical scheme of the present invention is: a kind of TBP-kerosene-HNO 3Irradiation product DBP in the system and the separation method of MBP, it comprises following method steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing the organic phase and the Na that contains DBP, MBP and micro-TBP of TBP-kerosene-HNO3 system 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water, at this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation.
The present invention's first technical scheme further is: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8.
Second technical scheme of the present invention is: a kind of TBP-kerosene-HNO 3Irradiation product DBP in the system or the separation method of MBP, it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing the organic phase and the Na that contains DBP, MBP and micro-TBP of TBP-kerosene-HNO3 system 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water, at this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to PH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water has been realized DBP or MBP and TBP-kerosene-HNO like this 3The separation of system.
The present invention's second technical scheme further is: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to PH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L.
The 3rd technical scheme of the present invention is: a kind of TBP-kerosene-HNO 3The detection method of irradiation product DBP in the system, it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing the organic phase and the Na that contains DBP, MBP and micro-TBP of TBP-kerosene-HNO3 system 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water, at this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to PH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water has been realized DBP or MBP and TBP-kerosene-HNO like this 3The separation of system;
Four, get the CHCl that includes DBP that above-mentioned the 3rd step extraction obtains 3Organic phase is used distilled water diluting, adds ammonium superphosphate again, treat ammonium superphosphate dissolving after; Put into boiling water bath and be heated to after organic phase disappears, boil, after the cooling; Add S-WAT, treat the S-WAT dissolving after, be heated to and boil; This moment, the organophosphorus of DBP was converted into inorganic phosphorus, measured DBP content with phosphorus molybdenum blue colorimetric method.
The present invention's the 3rd technical scheme further is: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to PH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L; Described zero(ppm) water that is used to dilute of the 4th step and the CHCl that includes DBP that obtains by the 3rd step 3The ratio of the volume of two kinds of liquid of organic phase is 18～22: 4～6, and the weight that adds ammonium superphosphate is per 4～6 milliliters of CHCl that include DBP that obtained by the 3rd step 3Organic phase is 0.4～0.6 gram, and the weight that adds S-WAT is per 4～6 milliliters of CHCl that include DBP that obtained by the 3rd step 3Organic phase is 0.4～0.6 gram.
The 4th technical scheme of the present invention is: a kind of TBP-kerosene-HNO 3The detection method of irradiation product MBP in the system, it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing the organic phase and the Na that contains DBP, MBP and micro-TBP of TBP-kerosene-HNO3 system 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water, at this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to PH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water has been realized DBP or MBP and TBP-kerosene-HNO like this 3The separation of system;
Four, get the H that includes MBP that above-mentioned the 3rd step extraction obtains 2SO 4Water is used solid Na 2CO 3It is neutralized to neutrality, and pH value equals 6.5～7.5, adds ammonium superphosphate, boils, and cooling adds sodium phosphite, treat the sodium phosphite dissolving after, be heated to and boil, at this moment, the organophosphorus of MBP has been decomposed into inorganic phosphorus, with phosphorus molybdenum blue colorimetric method mensuration MBP content.
The 4th technical scheme further of the present invention is: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to PH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L; The weight that the 4th step added ammonium superphosphate is per 4～6 milliliters of H that include MBP that obtained by the 3rd step 2SO 4Water is 0.4～0.6 gram, and the weight that adds S-WAT is per 4～6 milliliters of H that include MBP that obtained by the 3rd step 2SO 4Water is 0.4～0.6 gram.
The main chemical name of using among the present invention and the parsing of symbol:
TBP-kerosene-HNO 3System: tributyl phosphate-kerosene-nitric acid system;
TBP: tributyl phosphate, molecular structural formula are
Figure GSA00000052341000061
DBP: dibutyl phosphate, molecular structural formula are
Figure GSA00000052341000062
MBP: monobutyl phosphate, molecular structural formula are
Figure GSA00000052341000063
Ml: milliliter;
Yellow soda ash: molecular formula is Na 2CO 3
Ammonium persulphate: molecular formula is (NH 4) 2S 2O 8
CHCl 3: trichloromethane is commonly called as chloroform.
The present invention compared with prior art has following characteristics:
The present invention is simple, convenient, does not need expensive instrument, and analytical cycle is short, and DBP and MBP can measure respectively, and the remolding sensitivity of measuring DBP, MBP is higher; Measuring the DBP variation coefficient is 0.023, and it is 98～103% that standard adds the recovery, and measuring the MBP variation coefficient is 0.052, and standard adds the recovery and is not less than 97%.、
In order to be illustrated more clearly in the present invention, enumerate following examples, but it there is not any restriction to scope of invention.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
A kind of TBP-kerosene-HNO 3Irradiation product DBP in the system and the separation method of MBP, it mainly comprises the steps (as shown in Figure 1):
One, gets TBP-kerosene-HNO 3Poor organic phase sample 9～11ml under the system in the uranium extraction technology is put in the 60ml separating funnel, adds 3～8%Na 2CO 3Solution 9～11ml extracted 2～10 minutes, standing demix, and the upper strata is the organic phase that comprises TBP-kerosene-HNO3 system, lower floor is the Na that includes DBP, MBP and micro-TBP 2CO 3Water;
Two, with the Na of the first step standing demix 2CO 3Water is put into the separating funnel of another 60ml, uses CHCl 3Washing once is in a ratio of 0.8～1: 0.8～1, i.e. and Na 2CO 3Water and CHCl 3Volume ratio be 0.8～1: 0.8～1, shook standing demix, the CHCl in the standing demix 2～10 minutes 3The TBP that includes trace in the organic phase, the clarification Na in the standing demix 2CO 3Water includes DBP and MBP; At this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation.
Embodiment 2
A kind of TBP-kerosene-HNO 3Irradiation product DBP in the system or the separation method of MBP through after above-mentioned two steps of embodiment 1, also comprise the steps: earlier
Three, get the clarification Na that embodiment 1 second goes on foot in the standing demix 2CO 3Water 4～6ml drops to nearly neutrality with 4～6mol/L sulfuric acid, and pH value equals 6.5～7.5, and promptly PH=6.5～7.5 add 4～6ml, 4.5～5.5mol/L sulphuric acid soln again, and this moment, solution acidity was 3～4mol/L, after shaking gently, added the CHCl of 9～11ml 3Extracted 1～3 minute, and left standstill more than 15 minutes; CHCl in the standing demix 3Include DBP in the organic phase; H in the standing demix 2SO 4Aqueous phase includes MBP.
Embodiment 3
A kind of TBP-kerosene-HNO 3The detection method of irradiation product DBP in the system through after above-mentioned three steps of embodiment 2, also comprises the steps: earlier
Four, adding distil water 18～22ml in the 100ml beaker gets the CHCl that the foregoing description 2 the 3rd step extraction obtains 3Organic phase 4～6ml is put in this beaker, adds ammonium superphosphate 0.4～0.6g, after waiting to dissolve, puts into boiling water bath and is heated to after organic phase disappears; Move to low-temperature furnace, continued to boil 3～6 minutes, with hot water purge wall of cup, cold slightly after; Add S-WAT 0.4～0.6g, after waiting to dissolve, be heated to and boil; Take off beaker, the organophosphorus of the DBP in the beaker is converted into inorganic phosphorus at this moment, measures DBP content with phosphorus molybdenum blue colorimetric method.
Experimental data 1
Get two kinds of TBP-kerosene-HNO 3Poor organic phase sample under the system in the uranium extraction technology promptly poorly has-1, poor-2 samples is arranged, and these two kinds of samples are done six experiments respectively with the method for embodiment 3, and the detected result that obtains DBP is shown in following table 1:
Table 1 sample analysis and precision are measured
Figure GSA00000052341000081
Embodiment 4
Irradiation product DBP in a kind of TBP-kerosene-HNO3 system and the separation method of MBP, it mainly comprises the steps (as shown in Figure 1):
One, gets TBP-kerosene-HNO in the zirconium hafnium extracting and separating 3Poor organic phase sample 9～11ml under the system is put in the 60ml separating funnel, adds 3～8%Na 2CO 3Solution 9～11ml extracted standing demix 2～10 minutes; The upper strata is the organic phase that comprises TBP-kerosene-HNO3 system, and lower floor is the Na that includes DBP, MBP and micro-TBP 2CO 3Water;
Two, with the Na of the first step standing demix 2CO 3Water is put into the separating funnel of another 60ml, uses CHCl 3Washing once is in a ratio of 0.8～1: 0.8～1, i.e. and water and CHCl 3Volume ratio be 0.8～1: 0.8～1, shook standing demix 2 minutes; CHCl in the standing demix 3The TBP that also includes trace in the organic phase; Clarification Na in the standing demix 2CO 3Water includes DBP and MBP; At this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation.
Embodiment 5
A kind of TBP-kerosene-HNO 3Irradiation product DBP in the system or the separation method of MBP through after above-mentioned two steps of embodiment 4, also comprise the steps: earlier
Three, get the clarification Na that embodiment 4 second goes on foot in the standing demix 2CO 3Water 4～6ml drops to nearly neutrality with 4～6mol/L sulfuric acid, and pH value equals 6.5～7.5, and promptly PH=6.5～7.5 add 4～6ml, 4.5～5.5mol/L sulphuric acid soln again, and this moment, solution acidity was 3～4mol/L, after shaking gently, added CHCl 39～11ml extraction 1～3 minute was left standstill more than 15 minutes; CHCl in the standing demix 3Include DBP in the organic phase; Clarification H in the standing demix 2SO 4Aqueous phase includes MBP.
Embodiment 6
A kind of TBP-kerosene-HNO 3The detection method of irradiation product MBP in the system through after above-mentioned three steps of embodiment 5, also comprises the steps: earlier
Four, get the H that the foregoing description 5 the 3rd step extraction obtains 2SO 4Water 4～6ml uses solid Na in beaker 2CO 3It is neutralized to neutrality, and pH value equals 6.5～7.5, adds ammonium superphosphate 0.4～0.6g, heated and boiled on low-temperature furnace; With hot water purge wall of cup, cold slightly after, add sodium phosphite 0.4～0.6g; After waiting to dissolve, be heated to and boil, take off beaker; At this moment, the organophosphorus of MBP has been decomposed into inorganic phosphorus, measures MBP content with phosphorus molybdenum blue colorimetric method.
Experimental data 2
Get two kinds of TBP-kerosene-HNO in the zirconium hafnium extracting and separating 3Poor organic phase sample under the system promptly poorly has-A, poorly has-the B sample, and these two kinds of samples are done six experiments respectively with the method for embodiment 6, and the detected result that obtains MBP is shown in following table 2:
Table 2 sample analysis and precision are measured
Figure GSA00000052341000101
The present invention is not limited to above-mentioned concrete grammar step, so long as pass through Na 2CO 3And CHCl 3Extract DBP and/or MBP from TBP-kerosene-HNO 3The method of separating in the system and/or detecting just drops within protection scope of the present invention.

Claims (6)

1. TBP-kerosene-HNO 3Irradiation product DBP in the system or the separation method of MBP, it is characterized in that: it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing TBP-kerosene-HNO 3The organic phase of system and the Na that contains DBP, MBP and micro-TBP 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to pH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water.
2. a kind of TBP-kerosene-HNO according to claim 1 3Irradiation product DBP in the system or the separation method of MBP is characterized in that: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to pH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L.
3. TBP-kerosene-HNO 3The detection method of irradiation product DBP in the system, it is characterized in that: it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing TBP-kerosene-HNO 3The organic phase of system and the Na that contains DBP, MBP and micro-TBP 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to pH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water;
Four, get the CHCl that includes DBP that above-mentioned the 3rd step extraction obtains 3Organic phase is used distilled water diluting, adds ammonium superphosphate again, treat ammonium superphosphate dissolving after; Put into boiling water bath and be heated to after organic phase disappears, boil, after the cooling; Add S-WAT, treat the S-WAT dissolving after, be heated to and boil; This moment, the organophosphorus of DBP was converted into inorganic phosphorus, measured DBP content with phosphorus molybdenum blue colorimetric method.
4. TBP-kerosene-HNO according to claim 3 3The detection method of irradiation product DBP in the system is characterized in that: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to pH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L; Described zero(ppm) water that is used to dilute of the 4th step and the CHCl that includes DBP that obtains by the 3rd step 3The ratio of the volume of two kinds of liquid of organic phase is 18～22: 4～6, and the weight that adds ammonium superphosphate is per 4～6 milliliters of CHCl that include DBP that obtained by the 3rd step 3Organic phase is 0.4～0.6 gram, and the weight that adds S-WAT is per 4～6 milliliters of CHCl that include DBP that obtained by the 3rd step 3Organic phase is 0.4～0.6 gram.
5. TBP-kerosene-HNO 3The detection method of irradiation product MBP in the system, it is characterized in that: it comprises the steps:
TBP-kerosene-the HNO that one, will contain irradiation product DBP and MBP 3System is used Na 2CO 3Solution extracts the back separatory, obtains containing TBP-kerosene-HNO 3The organic phase of system and the Na that contains DBP, MBP and micro-TBP 2CO 3Water;
Two, the Na that contains DBP, MBP and micro-TBP that the first step is obtained 2CO 3Water is used CHCl 3Extract the back separatory, obtain including the CHCl of micro-TBP 3Organic phase and the Na that includes DBP and MBP 2CO 3Water, at this moment DBP and MBP just with TBP-kerosene-HNO 3System has realized separation;
Three, get the Na that includes DBP and MBP that second step obtained 2CO 3Water is neutralized to pH=6.5～7.5 with sulfuric acid, adds sulfuric acid regulation solution acidity again, and making solution acidity is 3～4mol/L, uses CHCl then 3Extraction is separatory also, obtains including the CHCl of DBP 3Organic phase and the H that includes MBP 2SO 4Water has been realized DBP or MBP and TBP-kerosene-HNO like this 3The separation of system;
Four, get the H that includes MBP that above-mentioned the 3rd step extraction obtains 2SO 4Water is used solid Na 2CO 3It is neutralized to neutrality, and the pH value equals 6.5～7.5, adds ammonium superphosphate, boils, and cooling adds sodium phosphite, treat the sodium phosphite dissolving after, be heated to and boil, at this moment, the organophosphorus of MBP has been decomposed into inorganic phosphorus, with phosphorus molybdenum blue colorimetric method mensuration MBP content.
6. TBP-kerosene-HNO according to claim 5 3The detection method of irradiation product MBP in the system is characterized in that: the described TBP-kerosene-HNO that contains irradiation product DBP and MBP of the first step 3System and Na 2CO 3The ratio of the volume of solution is 3～8: 3～8, wherein Na 2CO 3The concentration of solution is every liter of Na 2CO 3Contain Na in the solution 2CO 330～80 grams; Use CHCl described in second step 3When extracting, contain the Na of DBP, MBP and micro-TBP 2CO 3Water and CHCl 3The ratio of volume be 3～8: 3～8; The Na that includes DBP and MBP described in the 3rd step 2CO 3Water, to be used for regulator solution acidity be the sulfuric acid of 3～4mol/L and the CHCl that is used to extract 3The ratio of the volume of three kinds of liquid is 4～6: 4～6: 9～11, be used for Na 2CO 3The sulfuric acid concentration that water is neutralized to pH=6.5～7.5 is 4～6mol/L, and the sulfuric acid concentration that is used for regulator solution acidity is 4.5～5.5mol/L; The weight that the 4th step added ammonium superphosphate is per 4～6 milliliters of H that include MBP that obtained by the 3rd step 2SO 4Water is 0.4～0.6 gram, and the weight that adds S-WAT is per 4～6 milliliters of H that include MBP that obtained by the 3rd step 2SO 4Water is 0.4～0.6 gram.
CN201010139386A 2010-04-02 2010-04-02 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 Expired - Fee Related CN101830924B (en)

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