CN105758964A - Method for analyzing tri-isoamyl phosphate in the presence of di-iso-amyl phosphate - Google Patents
Method for analyzing tri-isoamyl phosphate in the presence of di-iso-amyl phosphate Download PDFInfo
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- CN105758964A CN105758964A CN201610129358.3A CN201610129358A CN105758964A CN 105758964 A CN105758964 A CN 105758964A CN 201610129358 A CN201610129358 A CN 201610129358A CN 105758964 A CN105758964 A CN 105758964A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention provides a method for analyzing tri-isoamyl phosphate in the presence of di-iso-amyl phosphate.The method includes pre-treating samples to obtain to-be-detected samples; quickly analyzing the concentration of the TiAP (tri-isoamyl phosphate) by the aid of processes for jointly utilizing efficient liquid-phase chromatographic columns ZORBAX-Eclips XDB-C18 and ultraviolet detectors under the optimal conditions.The optimal conditions include that a proportion of liquid phases, namely acetonitrile and water, is 60:40 (v:v), the flow rate is 1 mL/min, the column temperatures are equal to the room temperature, the sample size is 20 micro-L, and the detection wavelengths are 200 nm.The method has the advantages of high speed and simplicity in operation.
Description
Technical field
The present invention relates to the analysis method of tri-isoamyl phosphate (TiAP) in the presence of di-iso-amyl phosphate.
Background technology
China is extensive builds large-scale nuclear power station, and business transports nuclear power station number will quickly be increased.The fast development of nuclear power
Substantial amounts of radioactivity spentnuclear fuel will be produced.PUREX flow process is mainly used in the post processing of spentnuclear fuel, in this flow process, first by extraction
Take agent and by uranium and be extracted into organic phase, the most again with reducing agent by uranium and separation.Tributyl phosphate (TBP) is as a kind of excellent
Extractant be widely used in the post processing of spentnuclear fuel.But, TBP solubility in water is relatively big, when TBP is for extracting relatively
During Pu and U of high concentration, easily reach saturated, three-phase occurs, thus affects the properly functioning of spentnuclear fuel post processing flow process.TiAP exists
Solubility in water is less, during with TiAP extraction high concentration Pu and U, will not produce three-phase, and therefore, TiAP is before one has application very much
The Novel Extractant of scape.Extractant uses under radiation environment, and therefore, extractant must have certain irradiation stability.
Research TiAP irradiation stability certainly will relate to the analysis of TiAP, may produce di-iso-amyl phosphate owing to TiAP decomposes, and di(2-ethylhexyl)phosphate is different
Pentyl ester may interfere with the analysis of TiAP, therefore must obtain the analysis method of the TiAP in the presence of di-iso-amyl phosphate.Up to the present,
There is not yet the analysis method of TiAP in the presence of document report di-iso-amyl phosphate.TiAP and di-iso-amyl phosphate are all that higher boiling has
Machine compound, can use liquid chromatography analysis in theory.We have studied multiple high pressure liquid and be separated post to TiAP and di(2-ethylhexyl)phosphate
The separating effect of isopentyl ester, also different flowing phases, different flow rate of mobile phase, temperature and the UV-detector of research in detail absorbs ripple
Long on TiAP and di-iso-amyl phosphate separating effect and response peak height with the impact of peak area, finally give analysis TiAP
Good condition.Under these conditions, TiAP and di-iso-amyl phosphate can separate well, i.e. di-iso-amyl phosphate does not interferes with TiAP
Analysis.It addition, the peak shape of TiAP is fine, the response peak area of TiAP is linear with its concentration, and its linear correlation degree is the highest.
Summary of the invention
It is an object of the invention to provide the analysis method of TiAP in the presence of a kind of di-iso-amyl phosphate.
In order to achieve the above object, the present invention is by the following technical solutions:
A. with the n-dodecane solution of the standard specimen TiAP compound concentration a series of TiAP in the range of 0～21.960mmol/L, warp
After efficient liquid phase chromatographic analysis, obtain the retention time of TiAP, and with peak area, sample concentration is mapped；
B. standard specimen di-iso-amyl phosphate is formulated as the n-dodecane solution of about 0.1 mol/L, through efficient liquid phase chromatographic analysis
After, obtain di-iso-amyl phosphate and obtain retention time；
C. testing sample is used high performance liquid chromatograph analysis, obtains the peak area of TiAP in this sample；Utilize the work of TiAP
Curve, i.e. can get the concentration of TiAP in sample；
Described high performance liquid chromatography condition is:
Chromatographic column: ZORBAX-Eclips XDB-C18
Flowing phase: acetonitrile: water=60:40(v:v)
Flow velocity: 1 mL/min
Column temperature: room temperature
Sample size: 20 μ L
Detection wavelength: 200nm.
Under this condition, the retention time of TiAP is about 4 min, and peak shape is fine.It addition, the radiolysis product that TiAP is possible
The retention time of thing di-iso-amyl phosphate is about 5.5 min, therefore di-iso-amyl phosphate is without interference with the analysis of TiAP.The method
Can quickly analyze TiAP, simple to operate.
Accompanying drawing explanation
Fig. 1 is under optimum analysis condition, the chromatogram of TiAP.
Fig. 2 is under optimum analysis condition, the chromatogram of di-iso-amyl phosphate.
Fig. 3 is the working curve diagram of TiAP.Wherein abscissa is the concentration of TiAP, unit: m M i.e.: m mol/L,
Ordinate is the peak area of TiAP chromatographic peak, unit: mAU*S
Fig. 4 is the HPLC figure of non-irradiated TiAP sample,
Fig. 5 is the HPLC figure of the TiAP sample after gamma-ray irradiation.
Fig. 6 is the radiolysis rate relation with pre-equilibration concentration of nitric acid of TiAP, and wherein abscissa is concentration of nitric acid (mol/L),
Ordinate is the radiolysis rate (%) of TiAP.
Detailed description of the invention
By example below, the present invention will be further described, but embodiment is not limiting as protection scope of the present invention.
Major experimental instrument: Agilent 1100 type high performance liquid chromatograph, including online degasser, quaternary pump, post
Incubator and UV-detector, chem workstation.
1) preparation of standard liquid:
(1) preparation of TiAP standard sample: accurately weigh 1.693g TiAP in 5mL volumetric flask, is diluted to carve with n-dodecane
Degree line, this is TiAP mother liquor, and concentration is 1.1mol/L.Pipette different amounts of TiAP mother liquor respectively in the volumetric flask of 10mL, use
Dilution in acetonitrile, to graduation mark, shakes up.Obtain 6 concentration point, respectively 1.098 mmol/L, 2.196 mmol/L, 4.392
mmol/L、8.784 mmol/L、10.980 mmol/L、21.960mmol/L。
(2) preparation of di-iso-amyl phosphate standard sample: accurately weigh 2.383g di-iso-amyl phosphate in 10mL volumetric flask
In, by dilution in acetonitrile to graduation mark, shaking up, this is di-iso-amyl phosphate mother liquor, and concentration is 1.0mol/L.Pipette a certain amount of phosphorus
Acid diisoamyl ester mother liquor, in 10mL volumetric flask, by dilution in acetonitrile to graduation mark, shakes up, and this sample concentration is 0.1mol/L.
2) drafting of TiAP working curve:
Under optimum analysis condition, analyze above-mentioned sample, obtain the peak area of TiAP under variable concentrations.With peak area to concentration
Mapping, TiAP concentration is in the range of 0 ~ 21.960mmol/L, and sample concentration is directly proportional to peak area, and working curve is: Y=
8.9233x-5.964 coefficient R2=0.9998
3) take testing sample to be analyzed, thus obtain the concentration of TiAP in sample
(1) the pre-equilibration acidity impact on TiAP irradiation stability
Take certain density TiAP/ n-dodecane solution, respectively with 1.0,2.0,3.0 and 5.0 mol/LHNO3Balance three times,
Then, take organic phase in bottle, sealing, irradiation.Take the sample after irradiation, by dilution in acetonitrile, then efficient by the present invention
Liquid chromatography analysis sample, result such as following table.
Claims (1)
1. the analysis method of the tri-isoamyl phosphate (TiAP) in the presence of a di-iso-amyl phosphate, it is characterised in that the method
Concretely comprise the following steps:
A. with the n-dodecane solution of the standard specimen TiAP compound concentration a series of TiAP in the range of 0～21.960 mmol/L,
After efficient liquid phase chromatographic analysis, obtain its retention time, then with peak area, sample concentration is mapped；
B. the n-dodecane solution of about 0.1 mol it is configured to standard specimen di-iso-amyl phosphate, through efficient liquid phase chromatographic analysis,
To determine under certain chromatographiccondition, the retention time of di-iso-amyl phosphate, so that it is determined that whether it affects dividing of TiAP
Analysis；
C. testing sample is used high performance liquid chromatograph analysis, obtains the peak area of TiAP in this sample；Utilize the work of TiAP
Curve, i.e. can get the concentration of TiAP in sample；
Described high performance liquid chromatography condition is:
Chromatographic column: ZORBAX-Eclips XDB-C18
Flowing phase: acetonitrile: water=60:40(v:v)
Flow velocity: 1mL/min
Column temperature: room temperature
Sample size: 20 μ L
Detection wavelength: 200nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610129358.3A CN105758964A (en) | 2016-03-08 | 2016-03-08 | Method for analyzing tri-isoamyl phosphate in the presence of di-iso-amyl phosphate |
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| CN201610129358.3A CN105758964A (en) | 2016-03-08 | 2016-03-08 | Method for analyzing tri-isoamyl phosphate in the presence of di-iso-amyl phosphate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064326A (en) * | 2016-12-19 | 2017-08-18 | 上海大学 | The analysis method of di-iso-amyl phosphate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01229972A (en) * | 1988-03-09 | 1989-09-13 | Fuso Yakuhin Kogyo Kk | Determining method of low carboxylic acid in body fluid material |
| CN104407062A (en) * | 2014-09-11 | 2015-03-11 | 上海大学 | Method for rapid analysis of tri-isoamyl phosphate (TiAP) |
| KR20150058996A (en) * | 2013-11-21 | 2015-05-29 | 롯데케미칼 주식회사 | Resin composition for manufacturing thermoplastic polyester resin having an outstanding rate of crystallization |
-
2016
- 2016-03-08 CN CN201610129358.3A patent/CN105758964A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01229972A (en) * | 1988-03-09 | 1989-09-13 | Fuso Yakuhin Kogyo Kk | Determining method of low carboxylic acid in body fluid material |
| KR20150058996A (en) * | 2013-11-21 | 2015-05-29 | 롯데케미칼 주식회사 | Resin composition for manufacturing thermoplastic polyester resin having an outstanding rate of crystallization |
| CN104407062A (en) * | 2014-09-11 | 2015-03-11 | 上海大学 | Method for rapid analysis of tri-isoamyl phosphate (TiAP) |
Non-Patent Citations (2)
| Title |
|---|
| MANI LAL SINGH 等: "Density, Viscosity, and Interfacial Tension of Binary Mixture of Tri-iso-amyl Phosphate (TiAP) and n‑Dodecane: Effect of Compositions and Gamma Absorbed Doses", 《JOURNAL OF CHEMICAL & ENGINEERING DATA》 * |
| 刘春霞 等: "磷酸三异戊酯、磷酸三仲丁酯对U(Ⅵ)、Th(Ⅳ)的萃取性能", 《核化学与放射化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064326A (en) * | 2016-12-19 | 2017-08-18 | 上海大学 | The analysis method of di-iso-amyl phosphate |
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