CN102095620A - Method for recovering particles of wiping sample by using conductive adhesive as carrier - Google Patents

Method for recovering particles of wiping sample by using conductive adhesive as carrier Download PDF

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Publication number
CN102095620A
CN102095620A CN 201010620695 CN201010620695A CN102095620A CN 102095620 A CN102095620 A CN 102095620A CN 201010620695 CN201010620695 CN 201010620695 CN 201010620695 A CN201010620695 A CN 201010620695A CN 102095620 A CN102095620 A CN 102095620A
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China
Prior art keywords
carrier
graphite carbon
carbon plate
conducting resinl
particulate
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CN 201010620695
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Chinese (zh)
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CN102095620B (en
Inventor
王同兴
张燕
赵永刚
李少伟
李井怀
沈彦
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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Publication of CN102095620A publication Critical patent/CN102095620A/en
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Abstract

The invention discloses a method for recovering particles of a wiping sample by taking conductive adhesive as a carrier, which comprises the steps of firstly, putting a graphite carbon sheet into absolute ethyl alcohol to be cleaned for 1-2 minutes, taking out the graphite carbon sheet to be dried, and then covering the graphite carbon sheet with the conductive adhesive; and then, loading the recovered carrier into a recovery device for particle recovery, wherein the recovery process is carried out for 4-10 minutes in a vacuum state. The invention provides the method for recovering the particles of the wiping sample by taking the conductive adhesive as the carrier, which has the advantages of simple operation, quick recovery, high recovery rate and good dispersibility of the recovered particles.

Description

A kind of is the particle recovering method of the wipe samples of carrier with the conducting resinl
Technical field
The present invention relates to the particulate analysis technical field in the nuclear safeguards environmental monitoring, particularly a kind of is the particle recovering method of the wipe samples of carrier with the conducting resinl.
Background technology
IAEA in 1993 proposed one " 93+2 " plan and mainly strengthened the nuclear safeguards system on 2 o'clock, and one of them is environmental sampling (comprising wipe samples) and environmental monitoring.Particulate analysis is a high-sensitivity analysis technology in the environmental monitoring, has become the routine techniques in the nuclear safeguards environmental monitoring, and the effect that can not replace is arranged.The micron or the sub-micron particulate that have responsive nucleic can form gasoloid and suspend for a long time in atmosphere, thereby can be spread in the environment far away.Collect these particulates, specific species is wherein carried out analysis to measure, can provide valuable information for strengthening the nuclear safeguards system.Generally adopt cleaning wiping cloth that the wiping sampling is carried out in around the nuclear facilities and inside, come acquired information by single uranium particulate on secondary ion mass spectrum (SIMS) the analysis wipe samples.
SIMS is ripe to the measuring technique of the isotope ratio of particulate, to the transfer of particulate on the cleaning wiping cloth be recycled into to accurately analyzing the committed step of uranium isotope ratio.It is at present main in the world that what adopt is that the supersonic oscillations method reclaims particulate, earlier the particulate sonic oscillation on the cleaning wiping cloth in heptane, again the heptane hanging drop that contains particulate to carbon plate, consolidate evaporate to dryness for 300 ℃ and be used for sims analysis.But there are two problems in this method: the one, and the recovery lower (being about 25%); The 2nd, a plurality of particulates that reclaim are easily assembled together, are unfavorable for the analysis of single particulate.
Once described a kind of device of recovering particles by using vacuum collision method in another part of applicant Chinese patent application prospectus CN101655422A (open day is on February 24th, 2010), this patent only is described the structure of device.And yet there are no play-by-play in the pertinent literature at home and abroad for the method that reclaims particulate at present.
Summary of the invention
The present invention has overcome deficiency of the prior art, provide a kind of simple to operate, gain quick return, recovery height, reclaim microparticulate good be the particle recovering method of the wipe samples of carrier with the conducting resinl.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of is the particle recovering method of the wipe samples of carrier with the conducting resinl, and key is that this method at first is placed on the graphite carbon plate and cleans 1~2 minute in the absolute ethyl alcohol, takes out and treats conducting resinl to be covered on the graphite carbon plate its drying then; The recovery carrier that the graphite carbon plate is made is packed into and is carried out particulate in the retracting device and reclaim then, and removal process was carried out under vacuum state 4~10 minutes.
Described graphite carbon plate cleans to the graphite carbon plate is positioned in the container that absolute ethyl alcohol is housed in absolute ethyl alcohol, cleans in ultrasonic oscillator.Described drying is treated its drying for the graphite carbon plate being placed on volatilize on the filter paper.Described removal process is meant that under vacuum state reclaiming particulate carried out 5 minutes in the vacuum bag glove, and vacuum bag glove air intake opening charges into oxygen continuously, and it is certain that the aeration quantity in the vacuum bag glove keeps.
Compared with prior art, the invention has the beneficial effects as follows:
Complicated operation, the recovery that the present invention has changed traditional particle recovering method is low, the shortcoming of recovery microparticulate difference.And adopt the graphite carbon plate in absolute ethyl alcohol, to clean in the method, and guaranteed the cleaning on carbon plate surface, utilize ultrasonic oscillator to clean and can better remove the carbon dust on carbon plate surface.The carbon plate scavenging period is controlled at the fastness of the carbon plate that can guarantee that carbon plate cleaned up like this in 1~2 minute and can guarantee.The removal process of particulate is carried out under vacuum state, has guaranteed that recovery particulate process avoids polluting.
Embodiment
Below by embodiment the present invention is described in further detail:
A kind of is the particle recovering method of the wipe samples of carrier with the conducting resinl, and this method may further comprise the steps:
At first get the graphite carbon plate and be positioned in the beaker that absolute ethyl alcohol is housed, in ultrasonic oscillator, cleaned 1~2 minute, to remove the carbon dust on graphite carbon plate surface.After the graphite carbon plate cleans and to finish, be placed on treat the ethanol volatilization on the filter paper after, cut-off directly is about the conducting resinl of 20mm, covers on the graphite carbon plate, makes the recovery carrier.
Then, pack on the carrier platform of particulate retracting device, connect particulate retracting device, spinner-type flowmeter and vacuum pump with vacuum hose with reclaiming carrier; The escape pipe of vacuum pump is put into waste gas and is reclaimed solution.Open new vacuum bag glove, its air intake opening connects welding bottle, charges into oxygen, instruments such as the polybag that wipe samples is housed, tweezers, scissors are put into from the gas outlet of vacuum bag glove, the sealing gas outlet, treat the bag glove inflation after, stop to inflate.The wipe samples of clip 1/3~1/2 is used for reclaiming in the vacuum bag glove, with tweezers remaining sample is put back in the polybag.
At last, open the gas outlet of vacuum bag glove, send into the particulate retracting device, open the gas switch of welding bottle simultaneously, charge into oxygen, make the aeration quantity in the vacuum bag glove keep certain, help the reclaimer operation in the vacuum bag glove like this.With the fixing wipe samples of tweezers, open vacuum pump simultaneously, control the speed of exhaust by regulating spinner-type flowmeter; The front port of particulate retracting device is placed on the wipe samples, and the retracting device that moves around reclaims particulate.Recovery time is relevant with the sample size on the cleaning wiping cloth, and present embodiment carries out 4~10 minutes recovery, preferably adopts 5 minutes, and it is fastest to guarantee that like this recovery maximum can reclaim again.
This method can effectively be recovered to the particulate on the cleaning wiping cloth and reclaim on the carrier, can improve the particulate recovery on the cleaning wiping cloth and the dispersiveness of particulate again, for SIMS has created condition to the isotope ratio measurement of elements such as the uranium of single particulate, plutonium.

Claims (5)

1. one kind is the particle recovering method of the wipe samples of carrier with the conducting resinl, it is characterized in that, this method at first is placed on the graphite carbon plate and cleans 1~2 minute in the absolute ethyl alcohol, takes out and treats conducting resinl to be covered on the graphite carbon plate its drying then; Then the graphitic carbon sheet is packed into and carry out particulate in the retracting device and reclaim, removal process was carried out under vacuum state 4~10 minutes.
2. according to claim 1 a kind of be the particle recovering method of the wipe samples of carrier with the conducting resinl; it is characterized in that; described graphite carbon plate cleans to the graphite carbon plate is positioned in the container that absolute ethyl alcohol is housed in absolute ethyl alcohol, cleans in ultrasonic oscillator.
3. according to claim 1 a kind of be the particle recovering method of the wipe samples of carrier with the conducting resinl, it is characterized in that described drying is volatilized for the graphite carbon plate is placed on the filter paper.
4. according to claim 1 a kind of be the particle recovering method of the wipe samples of carrier with the conducting resinl, it is characterized in that described removal process reclaimed 5 minutes under vacuum state.
5. according to claim 1 a kind of be the particle recovering method of the wipe samples of carrier with the conducting resinl; it is characterized in that; described removal process is meant that under vacuum state reclaiming particulate carries out in the vacuum bag glove; and vacuum bag glove air intake opening charges into oxygen continuously, and it is certain that the aeration quantity in the vacuum bag glove keeps.
CN2010106206955A 2010-12-23 2010-12-23 Method for recovering particles of wiping sample by using conductive adhesive as carrier Active CN102095620B (en)

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CN102095620B CN102095620B (en) 2012-11-28

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768221A (en) * 2012-08-10 2012-11-07 中国原子能科学研究院 Method for measuring particle recovery rate
CN103901095A (en) * 2014-03-25 2014-07-02 中国原子能科学研究院 Method for measuring uranium isotope ratio of single particle
CN111257071A (en) * 2020-01-17 2020-06-09 胜科纳米(苏州)有限公司 Preparation method of sample for dynamic secondary ion mass spectrometer and prepared sample

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007333456A (en) * 2006-06-13 2007-12-27 Japan Atomic Energy Agency Method for detecting particle-containing fissionable material using fission track method
JP2008026056A (en) * 2006-07-19 2008-02-07 Japan Atomic Energy Agency Detection method according to enrichment of particles containing fission materials
CN101655422A (en) * 2009-09-02 2010-02-24 中国原子能科学研究院 Device for recovering particles by vacuum collision method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007333456A (en) * 2006-06-13 2007-12-27 Japan Atomic Energy Agency Method for detecting particle-containing fissionable material using fission track method
JP2008026056A (en) * 2006-07-19 2008-02-07 Japan Atomic Energy Agency Detection method according to enrichment of particles containing fission materials
CN101655422A (en) * 2009-09-02 2010-02-24 中国原子能科学研究院 Device for recovering particles by vacuum collision method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《Journal of Nuclear Science and Technology》 20041130 Fumitaka ESAKA et al. Efficient isotope ratio analysis of uranium particles in swipe samples by total-reflection X-ray fluorescence spectrometry and secondary ion mass spectrometry 1027-1032 1-5 第41卷, 第11期 *
《中国原子能科学研究院年报 2009》 20100731 王同兴等 抽气碰撞法回收擦拭样品上铀微粒的方法研究 388 1-5 , *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768221A (en) * 2012-08-10 2012-11-07 中国原子能科学研究院 Method for measuring particle recovery rate
CN102768221B (en) * 2012-08-10 2016-01-20 中国原子能科学研究院 The measuring method of particle recovery rate
CN103901095A (en) * 2014-03-25 2014-07-02 中国原子能科学研究院 Method for measuring uranium isotope ratio of single particle
CN103901095B (en) * 2014-03-25 2017-01-04 中国原子能科学研究院 A kind of assay method of individual particle Measurement of Uranium Isotope Ratio
CN111257071A (en) * 2020-01-17 2020-06-09 胜科纳米(苏州)有限公司 Preparation method of sample for dynamic secondary ion mass spectrometer and prepared sample

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