CN104007461A - Method for analyzing solution sample in hot cell - Google Patents
Method for analyzing solution sample in hot cell Download PDFInfo
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- CN104007461A CN104007461A CN201410232677.8A CN201410232677A CN104007461A CN 104007461 A CN104007461 A CN 104007461A CN 201410232677 A CN201410232677 A CN 201410232677A CN 104007461 A CN104007461 A CN 104007461A
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Abstract
The invention relates to a method for analyzing a radioactive substance. In order to solve the problems that analysis of the high-level solution samples cannot be fast completed due to the fact that the automation degree of the existing domestic hot cells is not high, a method for analyzing the solution sample in a hot cell is provided. The method comprises the following steps that upper prop adsorption is conducted on the high-level solution sample by adopting a solid phase extraction column, and then high-level impurity components are removed through eluent in an elution mode; inert gas is adopted to blow residue liquid in the solid phase extraction column away; the solid phase extraction column is transferred into a glove box, and the components to be tested are respectively eluted; the components to be tested are analyzed. By means of the method for analyzing the solution sample in the hot cell, analysis of the high-level solution sample can be fast completed, the operation process is greatly simplified, meanwhile conveying safety of the sample can be ensured, and stability and repeatability of an analysis result are improved.
Description
Technical field
The present invention relates to a kind of analytical approach of radiomaterial, particularly the analytical approach of solution example in a kind of hot cell.
Background technology
At core sciemtifec and technical sphere, conventionally in hot cell, carry out the analysis of highly radioactive solution sample, to avoid its radiation injury on people and the impact on environment.Operation in tradition hot cell mainly relies on mechanical arm, and the operation of mechanical arm is very complicated, and therefore the process of sample analysis is very difficult, wastes time and energy.
For the analysis of non-core field solution example, prior art adopts electronics and automation equipment to be improved the convenience of operation conventionally.But because the high radioactivity in hot cell and corrosive atmosphere all can cause radiation damage for many equipment such as electronics and automation equipment, parts, so that rapidly aging, damage, therefore affected the application in hot cell is analyzed of precision equipment that automaticity is higher.
Current, external state-of-the-art hot cell has reached higher automaticity, but its technical threshold is very high, and construction cost is high.By contrast, domestic existing hot cell automaticity is high not enough, therefore will realize the comparatively complicated analysis of highly radioactive solution sample, based on domestic reality, can consider analytical approach to be improved.
Traditional highly radioactive solution sample analysis method is mainly divided into two kinds.Be directly sample to be diluted to a safe scope by radiation protection requirement in hot cell, be then sent in glove box and analyze.The shortcoming of this method is: for the low sample of concentration of component to be measured, cannot both meet radiation protection requirement by enough extension rates, and carry out again quantitative test accurately, and also can produce a large amount of waste liquids because of dilution simultaneously.
Another kind is in hot cell, to adopt mechanical arm to carry out liquid-liquid extraction to sample, to component to be measured separate or enrichment after, then extract is sent in glove box and is analyzed.The shortcoming of this method is: the operation in hot cell is too complicated, shield because hot cell adopts nearly 1 meter of special lead glass of thick multilayer, make to divide a phase interface to be difficult to see clearly after extraction, require very high to Robot actions personnel, working strength is very big, and analytical effect is poor.
In recent years, solid phase extraction techniques realized gradually in some fields to traditional liquid-liquid extraction technology substitute, its maximum advantage is easy and simple to handle, time saving and energy saving, and extraction efficiency is very high.At present, there is on the market the multiple solid-phase extraction column for radioelement to select.But owing to being subject to the impact of the inner high radioactivity in hot cell and corrosive atmosphere, if use solid-phase extraction device in hot cell, cannot use electronics and automation equipment, cannot realize higher robotization.By Robot actions, step is very loaded down with trivial details, takes time and effort.
In conventional Solid-Phase Extraction operation, when component to be measured completes absorption on solid-phase extraction column, impurity composition has been leached after removal, according to the demand of analytical approach, need to pass through several times wash-out with different eluents, thereby each element to be measured is separated.
If solid-phase extraction device is operated in hot cell, in the time adding different eluent, will be very difficult by the operation of mechanical arm opening and closing solid-phase extraction device seal member so, and the stability of analysis result and repeated poor.Single wash-out operates just by 10-20 minute consuming time; And by polycomponent wash-out respectively, the time of processing single sample reaches 1-2 hour possibly.And due to operating conditions restriction, in hot cell, conventionally cannot adopt batch processing technology, make analysis efficiency low.
After extraction in hot cell completes, testing sample need to be sent to glove box by pneumatic sample conveying device conventionally.In pneumatic sample presentation process at a high speed, the inner pressurd vessel bottle cap of pneumatic sample presentation sample bottle easily gets loose, and causes leak of liquid; Outer container bottle need to be reused simultaneously, easily causes fluid sample to stain, and therefore causes the problem of sample delivery poor stability, and this has also limited the application of solid phase extraction techniques.
Therefore, on the basis of existence conditions, for realizing the express-analysis of highly radioactive solution sample in hot cell, simplify the operation course at home, guarantee sample delivery security, improve stability and the repeatability of analysis result, just need to develop a kind of new analytical approach.
Summary of the invention
Not high for solving domestic existing hot cell automaticity, cannot complete comparatively fast the analysis of highly radioactive solution sample, simplify the operation course simultaneously, guarantee sample delivery security, improve stability and the repeatability of analysis result, the invention provides the analytical approach of solution example in a kind of hot cell.The method comprises the following steps:
One, in hot cell, adopt solid-phase extraction column to carry out upper prop absorption to highly radioactive solution sample, then with leacheate, height is put to impurity composition drip washing and remove;
Two, adopt inert gas that the residual liquid in solid-phase extraction column is purged clean, obtain being loaded with the solid-phase extraction column of component to be measured;
Three, the solid-phase extraction column that is loaded with component to be measured is proceeded in glove box, then in glove box, component to be measured is distinguished to wash-out;
Four, component to be measured is analyzed, completed whole analytic process.
Described solid-phase extraction column is preferably the solid-phase extraction column of cartridge form.
Described inert gas is preferably nitrogen.
Described proceeding in glove box is preferably and adopts pneumatic sample conveying device to proceed in glove box.
In hot cell of the present invention, the analytical approach of solution example has changed the proper operation mode of classic method.According to classic method, height is put the drip washing of impurity composition, the wash-out of component to be measured all completes in hot cell, then contains the solution of component to be measured by sample bottle splendid attire, is sent to glove box analysis; And analytical approach of the present invention adopts inert gas is put impurity composition drip washing solid-phase extraction column to completing height to purge, then the solid-phase extraction column that does not contain liquid is directly proceeded to glove box, carry out wash-out and the analysis of component to be measured.
Compared to the proper operation mode of classic method, analytical approach of the present invention is mainly improved and be can be summarized as 2 points: one, the wash-out operation of component to be measured is undertaken by changing in hot cell in glove box, because the operation ease in glove box is far above hot cell, be convenient to carry out batch processing, therefore significantly improve analysis efficiency, simplified greatly operation; Simultaneously, because operating in glove box, the wash-out of component to be measured carries out, therefore also overcome classic method and adopted mechanical arm while component to be measured being carried out to wash-out in hot cell, operate miss mostly appears at the wash-out stage, easily occur wash-out not exclusively, stain, separate the problems such as not thorough.They are two years old, the object that shift to glove box in hot cell changes the not solid-phase extraction column containing liquid into by the sample bottle of carrying liquid, component to be measured can not be lost in transfer process, also can not stain, guaranteed the delivery safety of stability, repeatability and the sample of analysis result.
Embodiment
Below in conjunction with embodiment, embodiments of the present invention are described further.
Embodiment
Adopt the analytical approach of solution example in hot cell of the present invention to analyze simulated high-level radioactive waste, concrete steps are as follows:
One, the simulation solution example that preparation contains component uranium to be measured, neptunium, plutonium and other impurity elements, delivery is intended solution example 1mL, regulates the valence state of acidity and component to be measured, places stand-by;
Two, stand-by simulation solution example is passed through to cartridge type solid-phase extraction column, now uranium, neptunium, plutonium are adsorbed on solid-phase extraction column, and other impurity elements are leached removal;
Three, adopt nitrogen that the residual liquid in solid-phase extraction column is purged clean, obtain being loaded with the solid-phase extraction column of component to be measured;
Four, the solid-phase extraction column that is loaded with component to be measured is proceeded in glove box by pneumatic sample conveying device, then in glove box, with eluent, uranium, neptunium, plutonium are distinguished to wash-out;
Five, with the pre-diffraction-x-ray fluorescence analyzer of graphite crystal, uranium, neptunium, plutonium are carried out to quantitative test, complete whole analytic process.
Adopt above method to carry out parallel analysis 6 times, and the elution step that adopts batch processing mode, result to be presented in glove box need 1 hour altogether; And classic method carries out wash-out to single sample and approximately need 70 minutes in hot cell, 6 samples need to reach the time of 7 hours.
The recovery by calculating known uranium, neptunium, plutonium all between 90%-115%, proves the stability, repeatability of analysis result better.
Claims (4)
1. an analytical approach for solution example in hot cell, is characterized in that the method comprises the following steps:
One, in hot cell, adopt solid-phase extraction column to carry out upper prop absorption to highly radioactive solution sample, then with leacheate, height is put to impurity composition drip washing and remove;
Two, adopt inert gas that the residual liquid in solid-phase extraction column is purged clean, obtain being loaded with the solid-phase extraction column of component to be measured;
Three, the solid-phase extraction column that is loaded with component to be measured is proceeded in glove box, then in glove box, component to be measured is distinguished to wash-out;
Four, component to be measured is analyzed, completed whole analytic process.
2. the analytical approach of solution example in hot cell as claimed in claim 1, is characterized in that: described solid-phase extraction column is the solid-phase extraction column of cartridge form.
3. the analytical approach of solution example in hot cell as claimed in claim 1, is characterized in that: described inert gas is nitrogen.
4. the analytical approach of solution example in hot cell as claimed in claim 1, is characterized in that: described in proceed in glove box as adopting pneumatic sample conveying device to proceed in glove box.
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| CN201410232677.8A CN104007461A (en) | 2014-05-29 | 2014-05-29 | Method for analyzing solution sample in hot cell |
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| CN201410232677.8A CN104007461A (en) | 2014-05-29 | 2014-05-29 | Method for analyzing solution sample in hot cell |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093002A (en) * | 2016-06-02 | 2016-11-09 | 中国原子能科学研究院 | Sulfate radical and the device and method of phosphate radical in a kind of high activity liquid waste of mensuration simultaneously |
| CN106932423A (en) * | 2015-12-29 | 2017-07-07 | 中核四○四有限公司 | A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample |
| CN109557117A (en) * | 2018-12-29 | 2019-04-02 | 中国原子能科学研究院 | A kind of magnetic for hot cell helps sample preparation device |
| CN110780328A (en) * | 2019-11-05 | 2020-02-11 | 中国原子能科学研究院 | Automatic L-edge densimeter |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1892213A (en) * | 2006-03-16 | 2007-01-10 | 中国人民解放军63977部队 | Solid-phase micro-extracting device and method in gas-sampling tube |
-
2014
- 2014-05-29 CN CN201410232677.8A patent/CN104007461A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1892213A (en) * | 2006-03-16 | 2007-01-10 | 中国人民解放军63977部队 | Solid-phase micro-extracting device and method in gas-sampling tube |
Non-Patent Citations (5)
| Title |
|---|
| 张海霞等: "固相萃取", 《分析化学评述与进展》 * |
| 李梅等: "中子活化分析跑兔装置的建立", 《原子能科学技术》 * |
| 美延林等: "金属钚中微量杂质元素的化学光谱测定", 《原子能科学技术》 * |
| 邓惟勤等: "1 AW样品的预处理方法", 《核化学与放射化学》 * |
| 陶苗苗等: "1AF中镎的XRF分析前预处理方法研究", 《中国原子能科学研究院年报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106932423A (en) * | 2015-12-29 | 2017-07-07 | 中核四○四有限公司 | A kind of analysis method directly determined for slightly enriched uranium, neptunium, plutonium in sample |
| CN106093002A (en) * | 2016-06-02 | 2016-11-09 | 中国原子能科学研究院 | Sulfate radical and the device and method of phosphate radical in a kind of high activity liquid waste of mensuration simultaneously |
| CN106093002B (en) * | 2016-06-02 | 2019-06-18 | 中国原子能科学研究院 | Device and method that is a kind of while measuring sulfate radical and phosphate radical in high activity liquid waste |
| CN109557117A (en) * | 2018-12-29 | 2019-04-02 | 中国原子能科学研究院 | A kind of magnetic for hot cell helps sample preparation device |
| CN109557117B (en) * | 2018-12-29 | 2024-02-20 | 中国原子能科学研究院 | A magnetism helps system appearance device for hot laboratory cave |
| CN110780328A (en) * | 2019-11-05 | 2020-02-11 | 中国原子能科学研究院 | Automatic L-edge densimeter |
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Application publication date: 20140827 |