CN110308262A - It is a kind of based on TOA extraction soil in238Pu/239+240Pu analysis method - Google Patents

It is a kind of based on TOA extraction soil in238Pu/239+240Pu analysis method Download PDF

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CN110308262A
CN110308262A CN201910610895.3A CN201910610895A CN110308262A CN 110308262 A CN110308262 A CN 110308262A CN 201910610895 A CN201910610895 A CN 201910610895A CN 110308262 A CN110308262 A CN 110308262A
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张海玲
杨钰宁
武俊红
黄鹤翔
董文静
黄磊
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Abstract

The invention discloses in a kind of soil based on TOA extraction238Pu/239+240Pu analysis method belongs to plutonium isotope ratio analysis technical field in pedotheque, it is therefore intended that solves existing professional standard HJ 814-2016 and is directed to239+240The analysis of Pu, for238For Pu, this method cannot be removed228Th and241Am pairs238The problem of counting interference of Pu.For pedotheque238Pu/239+240Pu exists when analyzing228Th and241Am pairs238The counting of Pu is interfered, and210Po pairs239+240The problem of counting interference of Pu, on the basis of TOA extractive analysis Pu content, the application is effectively ensured by increasing co-precipitation and changing the measures such as hydrochloric acid washing amount238Pu/239+240The accuracy of Pu analysis.Blockage problem when subsequent upper prop can be effectively relieved in the present invention, improve nucleic spectral peak resolution ratio, utmostly reduce on α spectrogram228Th、241Am pairs238The interference of Pu and210Po pairs239+240The interference of Pu, it is final to obtain accurately238Pu/239+240Pu ratio.The Pu rate of recovery 75 ~ 95% may be implemented in this method,241Decontamination factor > 5 × 10 of Am3,228Decontamination factor > 10 of Th4,238The MDA(minimum of Pu detects activity) it is 0.15 ± 0.04 mBq,239+240The MDA of Pu is 0.16 ± 0.01 mBq.

Description

It is a kind of based on TOA extraction soil in238Pu/239+240Pu analysis method
Technical field
The present invention relates to plutonium isotope ratio analysis technical field in analysis field, especially pedotheque, specially one In the soil that kind is extracted based on TOA238Pu/239+240Pu analysis method.
Background technique
During nuclear activity, the radioactive elements such as micro plutonium can diffuse into surrounding enviroment by effluent, and through length Phase accumulation, forms specific distribution characteristics.Therefore, in nuclear facilities surrounding enviroment soil238Pu/239+240The information of Pu activity ratio is special Sign can be used for assessing nuclear activity.Wherein, key is to break through ultra trace in pedotheque238The High Sensitive Analysis of Pu, to obtain Accurate Assaying nuclide.
238Pu belongs to ultra trace nucleic, due to can not be with238U is distinguished, and leads to that analytical reagent composition cannot be used；And it adopts When with α spectrum analysis, soil sample amount needs to reach 25 ~ 50 g, wherein high impurity species are (mainly228Th and241Am) content Cause238Pu analysis may be interfered.For this purpose, sample pre-treatments become238Pu/239+240One necessary step when Pu is analyzed, To be eliminated as much as impurity species, isolate and purify238Pu and239+240Pu。
In soil238Pu/239+240The pre-treating method of Pu analysis, the current country has no correlative study；There are several phases in foreign countries The report of pass method, these methods include: commercial extracting resin (TEVA) method, anion-exchange resin method (Dowex 1*4, Dowex 1*8), two-stage anion-exchange resin method (Dowex 1*4+AG 1*4, Dowex 1*8+AG 1*8), anion exchange Resin-extraction combination (Dowex 1*4 and TTA extraction are combined).But in terms of means discussion, the existing main statement of report The Pu rate of recovery, does not discuss the decontamination degree of Th, Am, U etc., it is difficult to determine238Pu/239+240The accuracy of Pu analysis.
Currently, both at home and abroad about TOA(tri-n-octyl amine) extraction (liquid-phase extraction, Solid Phase Extraction) progress238Pu/239,240Pu In terms of the pre-treatment of analysis, not yet have been reported that.Existing report is that TOA liquid-phase extraction or solid phase extraction carry out plutonium in soil The pre-treatment of content analysis, and the domestic pre-treatment standard promulgated TOA solid phase extraction and carried out plutonium analysis in soil, The radiochemical analysis method of plutonium i.e. in professional standard HJ 814-2016(water and pedotheque, instead of national standard GB 11219.1- 89).
Therefore, nucleic spectral peak resolution ratio and impurity species decontamination degree can be improved in the one kind that is designed to provide of the application 's238Pu/239+240Pu analyzes pre-treating method, guarantees238Pu/239+240The accuracy of Pu analysis.
Summary of the invention
Existing professional standard HJ 814-2016 is directed to239+240The analysis of Pu, for238For Pu, this method cannot Remove228Th and241Am pairs238The counting of Pu is interfered.In addition, the high sample of individual humus contents, exists210The hangover of Po spectral peak It is right239+240The counting of Pu is interfered, and can not be obtained accurately238Pu/239+240Pu activity ratio.
Goal of the invention of the invention is, provides in a kind of soil based on TOA extraction238Pu/239+240Pu analysis method. For pedotheque238Pu/239+240Pu exists when analyzing228Th and241Am pairs238The counting of Pu is interfered, and210Po pairs239+240Pu Counting interference the problem of, on the basis of TOA extractive analysis Pu content, the application by increase co-precipitation and change salt acid elution The measures such as amount, providing a kind of can be improved nucleic spectral peak resolution ratio and impurity species decontamination degree based on TOA extraction238Pu /239+240Pu analyzes pre-treating method, guarantees238Pu/239+240The accuracy of Pu analysis.
To achieve the goals above, the present invention adopts the following technical scheme:
It is a kind of based on TOA extraction soil in238Pu/239+240Pu analysis method, includes the following steps:
(1) soil is weighed, and by 2 ~ 6h of calcination at 600 DEG C of weighed soil, and tracer is added into firing product242Pu, Obtain the first intermediate product；
(2) extraction for carrying out Pu to the first intermediate product of step 1 with nitrate leaching method, obtains soil pickle liquor；
(3) it is co-precipitated: concentrated ammonia liquor being added into the soil pickle liquor that step 2 obtains, adjusting pH value is 9 ~ 10, it is centrifuged after stirring, Supernatant is discarded, then dissolves the precipitating containing Pu with 6 ~ 8 mol/L nitric acid of 20 ~ 50 mL, obtains third solution；
(4) price adjustment of Pu: the third solution of step 3 is successively subjected to ferrous sulfamate reduction, sodium nitrite oxidation, Pu is turned Pu (IV) is turned to, nitric acid solution containing Pu is obtained；
(5) extraction and separation: Pu nitric acid solution will be contained and mix progress liquid-phase extraction with 10%TOA- xylene solution, take organic phase；
Or Pu nitric acid solution will be contained and separated by chromatograph column, the chromatograph powder of chromatograph column is TOA- dimethylbenzene, white monomer Mixture；
(6) purifying of Pu: when the step 5 is using liquid-phase extraction, with 10 mL, 10 mol/L salt acid elution organic phase 2 times, 10 3 mol/L nitric acid of mL washs 1 time, obtains organic phase and is denoted as the 6th solution；
Or the step 5 is using chromatograph column when being separated, with 50 ~ 60 mL, 10 mol/L hydrochloric acid, 30 mL, 3 mol/L nitre Acid successively washs chromatograph column；
(7) Pu in liquid-phase extraction is carried out to the 6th solution using -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid Back extraction, obtain the purification solution of Pu；
Or with -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid to the Pu on the chromatograph column after step 6 washing It is desorbed, obtains the purification solution of Pu；
(8) purification solution of the Pu obtained to step 7 carries out electro-deposition and plates source, then is measured with alpha spectrometer.
In the step (1), the additional amount of soil is 20 ~ 50 g, the soil first calcination 2 ~ 6 under 600 oC in Muffle furnace Then h adds tracer242Pu carries out nitration acid heat extraction.
In the step 2, the extraction of Pu is carried out according to nitrate leaching method specified in HJ 814-2016；The step 4 In, ferrous sulfamate reduction is carried out according to method specified in HJ 814-2016, sodium nitrite aoxidizes；In the step 8, Electro-deposition plating source is carried out according to purification solution of the method specified in HJ 814-2016 to the Pu that step 7 obtains, then uses alpha spectrometer Measurement.
It in the step 3, is centrifuged after stirring 30 min, discards supernatant, dissolved with 6 ~ 8 mol/L nitric acid of 20 ~ 50 mL Precipitating containing Pu.
In the step 3, concentrated ammonia liquor is added into the soil pickle liquor that step 2 obtains, adjusting pH value is 9 ~ 10, stirring 30 It is centrifuged after min, discards supernatant, precipitating successively washs one with 20 mL, 6 mol/L sodium hydroxide, 20 mL deionized waters respectively It is secondary, then dissolve the precipitating containing Pu with 20 ~ 50 mL, 6 ~ 8 mol/L nitric acid, and it is bright be heated to solution clarification to solution, obtains To third solution.
In the step 5, nitric acid solution containing Pu is mixed with the 10%TOA- xylene solution of 10 mL and carries out liquid-phase extraction.
It is first mixed with the organic phase that TOA liquid-phase extraction obtains in 10 mL, 10 mol/L hydrochloric acid and step 5 in the step 6 It closes, vibrates 2 min, stand and retain organic phase；Then, it is washed again with 10 mL, 10 mol/L hydrochloric acid, stands and retain organic phase； It is washed 1 time finally, vibrating 2 min with 10 mL, 3 mol/L nitric acid, stands and retain organic phase, and be denoted as the 6th solution；
Alternatively, first with the TOA- white carrier chromatograph column of 50 ~ 60 mL, 10 mol/L salt acid elution attachment Pu, then with 30 mL 3 Mol/L nitric acid washs chromatograph column, and finally with 2 mL water washing chromatograph columns, flow velocity is 1 mL/min.
For pedotheque238Pu/239+240Pu exists when analyzing228Th and241Am pairs238The counting of Pu is interfered, and210Po It is right239+240The problem of counting interference of Pu, the application, which provides, a kind of can be improved nucleic spectral peak resolution ratio and miscellaneous based on TOA extraction The pre-treating method of matter nucleic decontamination degree guarantees238Pu/239+240The accuracy of Pu analysis.
For this purpose, the application increases co-precipitation step on the basis of existing TOA extraction analyzes plutonium content, soil is realized Earth acid dip solution preconcentration and the resolution ratio for improving each nucleic peak on α spectrogram；Change hydrochloric acid washing amount, improves going for interference nucleic Dirty degree is established in the soil extracted based on TOA238Pu/239+240The pre-treating method of Pu analysis.
Here, detailed description are as follows for improvement of the inventor to the application.
(1) in the application, pedotheque, by pedotheque in the abundant calcination of Muffle furnace, can have before acid-hatching of young eggs extraction Effect removal organic matter, reduces blockage problem when subsequent upper prop.
(2) before acid extract carries out liquid phase or Solid Phase Extraction, concentrated ammonia liquor is added into soil pickle liquor to pH value The co-precipitation for carrying out Pu for 9 ~ 10.Using co-precipitation step, energy further Removal of dissolved organic matter, Ca, Mg ion etc., purification It is deposited on the substance of plating source on piece, nucleic is improved in the deposit uniformity of source on piece, improves the resolution of each nucleic spectral peak in α spectrum Rate；The effect for introducing co-precipitation front and back is shown in Fig. 1, with210Po with239+240For two spectral peaks of Pu, it can be seen that co-precipitation introduces Afterwards, hence it is evident that the resolution ratio for improving two spectral peaks reduces210Po pairs239+240The counting of Pu is interfered.In addition, based on co-precipitation step Suddenly, about 150 mL nitric acid liquid can be concentrated into 20 ~ 50 mL(is preferably 30 mL), it realizes preconcentration, sample can be shortened 1.5 ~ 2.1 h of product analysis time or so.
(3) when liquid-phase extraction, with when 10 mL, 10 mol/L salt acid elution 2 times or Solid Phase Extraction with 50 mL 10 Mol/L salt acid elution chromatograph column, can utmostly remove Th element,228An order of magnitude can be improved in the decontamination factor of Th, It greatly reduces on α spectrogram228Th pairs238The interference of Pu.Specific experiment data are as follows: when liquid-phase extraction, salt acid elution 1 time228Th Decontamination factor be < 3 × 103, salt acid elution 2 times228The decontamination factor of Th is > 4 × 104；When Solid Phase Extraction, 20 mL hydrochloric acid When washing228The decontamination factor of Th is < 2 × 103, when 50 mL salt acid elution228The decontamination factor of Th is > 104, it might even be possible to reach >105。
(4) the application couple is used in order to verify241The removal effect of Am, inventor are extracted using TOA, are used241Am standard liquid generation Entire pre-treatment flow operations are carried out for soil acid extract, confirmation > 95%241Am remains in TOA raffinate,241Am's goes The dirty factor > 5 × 103。
Based on above-mentioned improvement, blockage problem when subsequent upper prop can be effectively relieved in the application, improve nucleic spectral peak resolution ratio, Utmostly reduce on α spectrogram228Th、241Am pairs238The interference of Pu and210Po pairs239+240The interference of Pu, it is final to obtain accurately 's238Pu/239+240Pu ratio.The Pu rate of recovery 75 ~ 95% may be implemented in this method,241Decontamination factor > 5 × 10 of Am3,228Th's goes The dirty factor > 104,238The MDA(minimum of Pu detects activity) it is 0.15 ± 0.04 mBq,239+240The MDA of Pu is 0.16 ± 0.01 mBq。
Detailed description of the invention
Examples of the present invention will be described by way of reference to the accompanying drawings, in which:
The α spectrogram of the forward and backward liquid-phase extraction of co-precipitation step is added when Fig. 1 is 70000 s.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics ?.
In the present embodiment, the step of analysis method, is as follows.
(1) sample pretreatment
Soil after weighing 25 ~ 50 g drying screening, 2 h of calcination in Muffle furnace at 600 oC are added242Pu tracer, obtains First intermediate product.
(2) nitric acid Pu
30 min of extraction are heated to the first intermediate product with 100 mL, 8 mol/L nitric acid, the residue after centrifugation uses 50 again 8 mol/L nitric acid of mL, 10 min, residue uses 20 mL, 3 mol/L nitric acid and 20 mL deionized waters respectively after being centrifuged again It washed once, all supernatants mixing of above three step obtains soil pickle liquor.
(3) it is co-precipitated Pu
It is 9 ~ 10 that concentrated ammonia liquor to pH value is added into the soil pickle liquor after price adjustment, stirs 30 min, discards supernatant after centrifugation, Gained precipitating successively washed once with 20 mL, 6 mol/L sodium hydroxide and 20 mL deionized waters, and supernatant is discarded after centrifugation, It is eventually adding precipitating of 30 mL, the 8 mol/L nitric acid dissolution containing Pu, appropriate heating keeps solution clarification bright, obtains third solution.
(4) price adjustment of Pu
According to be added in every 100 mL third solution 0.5 mL ferrous sulfamate (mass fraction be 2% reduced iron powder and 24% Dithiocarbamic acid mixed solution, 0.1 mol/L nitric acid medium), react 5 ~ 10 min, restore Pu；0.5 mL is added thereto again 4 Mol/L sodium nitrites react 5 ~ 10 min, aoxidize Pu；Solution removal excessive nitrite sodium is boiled again, is cooled to room temperature, is obtained To nitric acid solution containing Pu.
(5) separation of Pu
The separation of Pu can extract two methods using liquid-phase extraction and solid phase chromatograph.
The process of liquid-phase extraction method is as follows: the 10%TOA- diformazan of nitric acid solution containing Pu and 10 mL that step (4) are obtained Benzole soln mixes, 2 min of oscillation extraction, after standing, retains organic phase.
The process of solid phase chromatograph extraction is: the nitric acid solution containing Pu that step (4) are obtained is logical with the flow velocity of 1 mL/min Cross chromatograph column (chromatograph powder is the mixture of TOA- dimethylbenzene, white monomer, with 20 mL, 8 mol/L nitric acid pre-acidified).
(6) purifying of Pu
Based on the liquid-phase extraction separation of Pu in step (5), the purifying of Pu is as follows using the process of liquid-phase extraction method: with 10 mL 10 Mol/L hydrochloric acid and step (5) obtain it is organic mix, vibrate 2 min, stand and retain organic phase；Again with 10 mL, 10 mol/ L hydrochloric acid washs again, stands and retains organic phase；It is washed 1 time finally, vibrating 2 min with 10 mL, 3 mol/L nitric acid, stands and protect Stay organic phase.
Based on the solid phase chromatograph extraction and separation of Pu in step (5), the purifying of Pu uses the process of solid phase chromatograph extraction such as Under: with 50 mL, 10 mol/L salt acid elution chromatograph column, chromatograph column then is washed with 30 mL, 3 mol/L nitric acid, finally with 2 ML water washing chromatograph column, flow velocity are 1 mL/min.
(7) back extraction or desorption of Pu
When liquid-phase extraction method, with what is obtained in -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid and step (6) Organic to mix, 2 min of oscillation are stripped Pu, retain water phase after standing, obtain Pu strip liquor.
When solid phase chromatograph extraction, with -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid with 0.5 mL/ The flow velocity of min desorbs Pu by chromatograph column, obtains Pu stripping liquid.
(8) Electrodeposition make source
Pu strip liquor or Pu stripping liquid are collected in galvanic deposition cell, it is 1.5~2.0 that ammonium hydroxide, which adjusts pH value,；Again by electro-deposition Slot is placed in the cold bath of flowing, 1 h of electro-deposition.Before electro-deposition terminates, 1 mL ammonium hydroxide is added and continues 1 min of electro-deposition, disconnects Power supply discards electrodeposit liquid, successively washs plating piece with water and dehydrated alcohol, then dries under infrared lamp, obtains plating piece.
(9) α spectrometry
Plating piece is placed in Low background α spectrum and is analyzed, according to Pu activity in sample, measures the s of 70000 s ~ 200000.
Embodiment 1
25 somewhere g soil-likes are taken, 0.128 Bq tracer is added after calcination242Pu, the extraction of 8 mol/L nitration acid heats, dense ammonia It is 9 ~ 10 realization co-precipitation that water, which is adjusted to pH value, and the dissolution of 30 mL, 8 mol/L nitric acid precipitates, 10%TOA- dimethylbenzene liquid-phase extraction, With 10 mL, 10 mol/L salt acid elution organic phase 2 times, 10 mL, 3 mol/L nitric acid is washed 2 times, 8 mL, 0.025 mol/L grass Sour -0.150 mol/L nitric acid solution is stripped Pu, and source is plated in electro-deposition and alpha spectrometer measures 200000 s.
Test result: the Pu rate of recovery=79.7%,241Decontamination factor=5.3 × 10 of Am3,228Decontamination factor=8 × 10 of Th4。
Embodiment 2
25 somewhere g soil-likes are taken, 0.128 Bq tracer is added after calcination242Pu, the extraction of 8 mol/L nitration acid heats, dense ammonia It is 9 ~ 10 realization co-precipitation that water, which is adjusted to pH value, and the dissolution of 30 mL, 8 mol/L nitric acid precipitates, TOA- white carrier Solid Phase Extraction, With 50 mL, 10 mol/L salt acid elution chromatograph column, 30 mL, 3 mol/L nitric acid washs chromatograph column, 8 mL, 0.025 mol/L grass Sour -0.150 mol/L nitric acid solution desorbs Pu, and source is plated in electro-deposition and alpha spectrometer measures 200000 s.
Test result: the Pu rate of recovery=91.4%,241Decontamination factor=5.1 × 10 of Am3,228Decontamination factor=4 × 10 of Th4。
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed New feature or any new combination, and disclose any new method or process the step of or any new combination.

Claims (7)

1. in a kind of soil based on TOA extraction238Pu/239+240Pu analysis method, which comprises the steps of:
(1) soil is weighed, and by 2 ~ 6 h of calcination at 600 DEG C of weighed soil, and tracer is added into firing product242Pu, Obtain the first intermediate product；
(2) extraction for carrying out Pu to the first intermediate product of step 1 with nitrate leaching method, obtains soil pickle liquor；
(3) it is co-precipitated: concentrated ammonia liquor being added into the soil pickle liquor that step 2 obtains, adjusting pH value is 9 ~ 10, it is centrifuged after stirring, Supernatant is discarded, then dissolves the precipitating containing Pu with 6 ~ 8 mol/L nitric acid of 20 ~ 50 mL, obtains third solution；
(4) price adjustment of Pu: the third solution of step 3 is successively subjected to ferrous sulfamate reduction, sodium nitrite oxidation, Pu is turned Pu (IV) is turned to, nitric acid solution containing Pu is obtained；
(5) extraction and separation: Pu nitric acid solution will be contained and mix progress liquid-phase extraction with 10%TOA- xylene solution, take organic phase；
Or Pu nitric acid solution will be contained and separated by chromatograph column, the chromatograph powder of chromatograph column is TOA- dimethylbenzene, white monomer Mixture；
(6) purifying of Pu: when the step 5 is using liquid-phase extraction, with 10 mL, 10 mol/L salt acid elution organic phase 2 times, 10 3 mol/L nitric acid of mL washs 1 time, obtains organic phase and is denoted as the 6th solution；
Or the step 5 is using chromatograph column when being separated, with 50 ~ 60 mL, 10 mol/L hydrochloric acid, 30 mL, 3 mol/L nitre Acid successively washs chromatograph column；
(7) Pu in liquid-phase extraction is carried out to the 6th solution using -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid Back extraction, obtain the purification solution of Pu；
Or with -0.150 mol/L nitric acid solution of 8 mL, 0.025 mol/L oxalic acid to the Pu on the chromatograph column after step 6 washing It is desorbed, obtains the purification solution of Pu；
(8) purification solution of the Pu obtained to step 7 carries out electro-deposition and plates source, then is measured with alpha spectrometer.
2. analysis method according to claim 1, which is characterized in that in the step (1), the additional amount of soil is 20 ~ 50 G, first 2 ~ 6 h of calcination under 600 oC in Muffle furnace of soil, then adds tracer242Pu carries out nitration acid heat extraction.
3. analysis method according to claim 1 or claim 2, which is characterized in that in the step 2, according to being advised in HJ 814-2016 Fixed nitrate leaching method carries out the extraction of Pu；In the step 4, amino sulphur is carried out according to method specified in HJ 814-2016 Sour ferrous reduction, sodium nitrite oxidation；In the step 8, step 7 is obtained according to method specified in HJ 814-2016 The purification solution of Pu carries out electro-deposition and plates source, then is measured with alpha spectrometer.
4. any one of according to claim 1 ~ 3 analysis method, which is characterized in that in the step 3, stir after 30 min from The heart discards supernatant, dissolves the precipitating containing Pu with the 8 mol/L nitric acid of 30 mL.
5. analysis method according to claim 4, which is characterized in that in the step 3, the soil acidleach that is obtained to step 2 Concentrated ammonia liquor is added in liquid, adjusting pH value is 9 ~ 10, is centrifuged after stirring 30 min, and supernatant is discarded, and is precipitated successively with 20 mL 6 Mol/L sodium hydroxide, 20 mL deionized waters washed once respectively, then dissolve the precipitating containing Pu with 30 mL, 8 mol/L nitric acid, And it is bright be heated to solution clarification to solution, obtains third solution.
6. any one analysis method according to claim 1 ~ 5, which is characterized in that in the step 5, Pu nitric acid solution will be contained It is mixed with the 10%TOA- xylene solution of 10 mL and carries out liquid-phase extraction.
7. any one analysis method according to claim 1 ~ 6, which is characterized in that in the step 6, first with 10 mL 10 Organic the mixing of mol/L hydrochloric acid and TOA liquid-phase extraction acquisition in step 5, vibrates 2 min, stands and retains organic phase；Then, It is washed again with 10 mL, 10 mol/L hydrochloric acid, stands and retain organic phase；Finally, vibrating 2 min with 10 mL, 3 mol/L nitric acid Washing 1 time stands and retains organic phase, and is denoted as the 6th solution；
Alternatively, first with the TOA- white carrier chromatograph column of 50 ~ 60 mL, 10 mol/L salt acid elution attachment Pu, then with 30 mL 3 Mol/L nitric acid washs chromatograph column, and finally with 2 mL water washing chromatograph columns, flow velocity is 1 mL/min.
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