CN101571460B - Sampling device for small-volume samples - Google Patents

Sampling device for small-volume samples Download PDF

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CN101571460B
CN101571460B CN200910147720XA CN200910147720A CN101571460B CN 101571460 B CN101571460 B CN 101571460B CN 200910147720X A CN200910147720X A CN 200910147720XA CN 200910147720 A CN200910147720 A CN 200910147720A CN 101571460 B CN101571460 B CN 101571460B
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way valve
sample
pipe
hot cell
quantitative ring
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CN101571460A (en
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吴继宗
张丽华
刘焕良
牟凌
钱红娟
范德军
汪南杰
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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Abstract

The invention discloses a sampling device for a small-volume sample, which comprises a six-way valve (1), a quantitative ring (2), a dilution pump (6) and a circulating pipe, wherein the six-way valve (1) is respectively connected with the quantitative ring (2) and the dilution pump (6) through the circulating pipe, the six-way valve (1) is connected with an isolated air pumping system (3) through the circulating pipe, and the isolated air pumping system (3) is formed by connecting a U-shaped water seal pipe (5) and an injector (4). The invention has simple structure and operation, high sampling accuracy, good precision and high sampling speed, and reduces the labor intensity of operators.

Description

The sampler of small samples
Technical field
The present invention relates to the field, hot cell, be specifically related to the sampler of radioactivity small samples in a kind of hot cell.
Background technology
Assay laboratory in aftertreatment factory, operations such as the quantitative sampling of hot sample, dilution, separation all need be carried out in the hot cell, all belong to the hot sample as the lysate of spentnuclear fuel, the 1 round-robin charging of main technology and some process samples.The hot sample not only radioactivity strong (>100Ci/L), and chemical toxicity big (belonging to extremely malicious class) also easily produces gasoloid, therefore must promptly in the hot cell, operate at the shielding of strictness and the protection condition work of finishing drilling.The hot cell is the cast iron case or the steel case (but wall thickness is relevant with the maximum operational ton) of a heavy wall, the outside coats with the thick loaded concrete of 0.5m-1m, the hot cell antetheca is provided with hagioscope, flint glass thickness on the hagioscope is in 30cm~50cm scope, the hot cell antetheca also is equipped with mechanical arm, operating personnel can just can make the slave arm in the hot cell carry out some simple actions by the master arm of mechanical arm outside the operation hot cell.Because the lead glass of hot cell hagioscope is thicker, its light transmission is relatively poor, scale mark on operator's sight glass vessel is brought certain difficulty, in addition, mechanical arm can only carry out some shirtsleeve operations, and its dirigibility, accuracy of action and operator are nothing like the staff direct control to the perceptibility of action.Therefore operation hot sample is the work both careful, that labour intensity is big again in the hot cell.
At present, the reprocessing analysis laboratory of countries in the world still adopts transfer pipet to take a sample in the hot cell, generally transfer pipet is fixed on the special support, the hoistable platform that can control outside the hot cell is arranged below, so that the transfer pipet head is stretched in the glass container; The transfer pipet upper port links to each other with a tracheae, is used to draw sample, and this tracheae passes the hot cell wall and links to each other with air strainer, and the air strainer other end is connected with a minipump and surge tank, and air-breathing and venting can be by a push-button switch control.The sampling process of this device is as follows: the sample presentation bottle that will send the hot cell earlier to is opened with mechanical arm, sample bottle is placed hoistable platform central authorities, outside the hot cell, start the rising switch of hoistable platform, make the transfer pipet head stretch into certain depth among the sample solution, open air-breathing switch then, sample is just slowly sucked transfer pipet, operating personnel observe liquid level by fixing telescope and whether reach scale mark, after liquid level reaches scale mark, stop suction, open the decline switch of hoistable platform, the sample presentation bottle is removed, with mechanical arm volumetric flask is placed hoistable platform central authorities again with mechanical arm, once more hoistable platform is risen, the transfer pipet head will stretch in the volumetric flask, open air escape cock, and the sample in the transfer pipet just flows in the volumetric flask, reduce hoistable platform, with mechanical arm volumetric flask is taken off, and then carry out whole sampling process as sample, reach the purpose of cleaning transfer pipet with diluted acid.Here it is present more advanced sampler and sampling mode, this kind sampler have intuitively, advantage reliably, but have following shortcoming: (1) complicated operating process requires height to staff's eyesight and operating experience.Accuracy and precision are difficult to guarantee when (2) getting small samples, the sample sampling of particularly micro-volume (micro updating).Therefore the sampling method in the hot cell is improved or reforms analytical approach, the reduction labor intensity of operating personnel for the strong setting-out product of expansion, the very necessity of increasing work efficiency all.
Summary of the invention
The present invention has overcome shortcoming of the prior art, and a kind of structure, simple to operate is provided, sampling accuracy height, and precision is good, and sample rate is fast, reduces the sampler of the small samples of labor intensity of operating staff.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of sampler of small samples, comprise six-way valve, quantitative ring, dilution pumps, runner pipe, six-way valve is connected by runner pipe with quantitative ring, dilution pumps respectively, described six-way valve connects isolated extract system by runner pipe, and isolated extract system is connected to form by U-shaped dip pipe and syringe.
In order better to make device be applicable to the hot environment in hot cell, described six-way valve, quantitative ring, runner pipe all adopt stainless steel.
Compared with prior art, the invention has the beneficial effects as follows:
This device cooperates with isolated extract system by six-way valve, quantitative ring, realized only need carrying out two shirtsleeve operations in the hot cell, be that mechanical arm inserts the sample introduction pipe in the sample to be got, to go out the sample pipe inserts in the volumetric flask that receives sample, all the other actions are all at hot cell external application hand direct control, and simple to operate in the hot cell realized remote-controlled operation, solve the problem that mechanical arm can't be operated, reduced labor intensity of operating personnel simultaneously; Sample rate is fast, and this device can be finished the primary sample process at 3 minutes.By adopting quantitative ring, improved the accuracy and the precision of sampling greatly, precision is better than 1.0%, and makes the sampling minimum volume can reach micro updating.
Description of drawings
The structural representation of Fig. 1 device
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
A kind of sampler of small samples, comprise six-way valve 1, quantitatively encircle 2, dilution pumps 6, runner pipe, six-way valve 1 is connected by runner pipe with quantitative ring 2, dilution pumps 6 respectively, six-way valve 1 connects isolated extract system 3 by runner pipe, and isolated extract system 3 is connected to form by U-shaped dip pipe 5 and syringe 4.As shown in Figure 1, six-way valve 1, quantitatively encircle 2 and the part runner pipe that connects usefulness place the hot cell; The change-over switch 9 and the part runner pipe of isolated extract system 3, dilution pumps 6, six-way valve place the personnel operation district.Operating personnel are by the state of six-way valve change-over switch 9 control six-way valves 1, by isolated extract system 3 and runner pipe control sampling.Six-way valve 1 in the hot cell, quantitatively encircle 2, parts such as runner pipe adopt stainless steel material, make it more appropriate to the hot environment in hot cell.
Wherein six-way valve 1 is used for device sample introduction and the switching that goes out the sample state, and operating personnel control the switching of six-way valve change-over switch 9 by cable control six-way valve 1.Quantitatively ring 2 is used for accurately pipetting sample, and its volume adopts titrimetry accurately to demarcate, and quantitatively the variable range of ring is 10 μ L~1000 μ L, can be according to the experiment demand decision volume of self.Isolated extract system 3 connects to form the effect of U-shaped dip pipe 5 by U-shaped dip pipe 5 and syringe 4 by runner pipe: the one, with high setting-out product and personnel operation separate from, prevent that radioaerosol from leaking; The 2nd, the leakproofness of the whole device of observation.
The sampling process of this device is as follows:
During sample introduction, operating personnel place the sample introduction state by six-way valve change-over switch 9 with six-way valve 1, i.e. the logical state of the solid line of six-way valve 1 as shown in Figure 1, and syringe 4 is bled, and sample is filled with quantitative ring 2 from sample bottle 7, finishes accurately pipetting of sample.When going out sample, operating personnel place out the sample state by six-way valve change-over switch 9 with six-way valve 1, the i.e. logical state of six-way valve 1 dotted line as shown in Figure 1, open dilution pumps 6, quantitatively the sample in the ring 2 is pushed in the diluted sample bottle 8 by deionized water, utilize dilution pumps 6 to carry the deionized water of deciding volume, finish the automatic dilution of sample.
Embodiment 1
When present embodiment adopted syringe 4 to bleed 1.8mL, this moment, sample was filled with the quantitative ring 2 of 1.0034mL, to the HNO of 0.905mol/L, 2.923mol/L 3Parallel sampling.
Sampling process is as follows:
During sample introduction, operating personnel place the sample introduction state by six-way valve change-over switch 9 with six-way valve 1, the state that six-way valve 1 solid line promptly shown in Figure 1 is logical, mechanical arm inserts the sample introduction pipe in the sample bottle 7, syringe 4 1.8mL that bleeds, sample is filled with quantitative ring 2, finishes accurately pipetting of sample.When going out sample, operating personnel place out the sample state by six-way valve change-over switch 9 with six-way valve 1, it is the logical state of six-way valve 1 dotted line shown in Figure 1, mechanical arm will go out the sample pipe and insert in the diluted sample bottle 8, open dilution pumps 6, quantitatively the sample in the ring 2 is pushed in the diluted sample bottle 8 by deionized water, utilizes dilution pumps 6 to carry the deionized water of deciding volume, finishes the automatic dilution of sample.
After sampling is finished, adopt the NaCO of 0.05mol/L 3The precision and the accuracy of this device are investigated in (benchmark) titration.As shown in table 1.
Table 1 is the ring sampling volume quantitatively
Figure G200910147720XD00041
Test findings shows, the sampling accuracy of this sampler and precision height, favorable reproducibility.

Claims (2)

1. the sampler of a small samples, comprise six-way valve (1), quantitative ring (2), dilution pumps (6), runner pipe, six-way valve (1) is connected by runner pipe with quantitative ring (2), dilution pumps (6) respectively, it is characterized in that, described six-way valve (1) connects isolated extract system (3) by runner pipe, isolated extract system (3) is connected to form by U-shaped dip pipe (5) and syringe (4), and six-way valve (1) is connected with the six-way valve change-over switch (9) that is positioned at the personnel operation district.
2. the sampler of a kind of small samples according to claim 1 is characterized in that, described six-way valve (1), quantitative ring (2), runner pipe all adopt stainless steel.
CN200910147720XA 2009-06-18 2009-06-18 Sampling device for small-volume samples Active CN101571460B (en)

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Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102410942A (en) * 2011-07-25 2012-04-11 迈瑞尔实验设备(上海)有限公司 Online sampling system
CN102607932B (en) * 2012-03-12 2014-04-02 同济大学 Underwater in-situ sample introduction diluter
CN104020487B (en) * 2014-05-29 2016-06-22 中国原子能科学研究院 The sampling method of fluid sample in hot cell
CN104062170B (en) * 2014-06-23 2016-09-14 青岛普仁仪器有限公司 Automatic on-line micro-example dilution mixture system and mixed method
CN104048855A (en) * 2014-06-24 2014-09-17 山西大学 Rainfall isotope sample collection measurer
CN105004572A (en) * 2015-07-27 2015-10-28 中国原子能科学研究院 Automatic quantitative sampling device
CN107300485A (en) * 2017-08-28 2017-10-27 杭州春来科技有限公司 Sample liquid definite value sampling apparatus and method
CN107970458A (en) * 2018-01-03 2018-05-01 山东省肿瘤防治研究院(山东省肿瘤医院) A kind of positron emitting tracer Fully automated synthesis module based on 18F-BF3 marks
CN109323912A (en) * 2018-11-21 2019-02-12 中国核电工程有限公司 Dilution divides sample system and application
CN113189026A (en) * 2021-03-30 2021-07-30 中国原子能科学研究院 Method and system for jointly detecting content of tetravalent uranium and hydrazine

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CN101236139A (en) * 2007-01-30 2008-08-06 力晶半导体股份有限公司 Supermicro-analysis sampling bottle and its sampling method

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CN1955712A (en) * 2005-10-25 2007-05-02 中国农业大学 Automatic separation flow circuit device
CN101236139A (en) * 2007-01-30 2008-08-06 力晶半导体股份有限公司 Supermicro-analysis sampling bottle and its sampling method

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