CN103728327A - Method for measuring uranium isotope ratio in single particles - Google Patents
Method for measuring uranium isotope ratio in single particles Download PDFInfo
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- CN103728327A CN103728327A CN201310700322.2A CN201310700322A CN103728327A CN 103728327 A CN103728327 A CN 103728327A CN 201310700322 A CN201310700322 A CN 201310700322A CN 103728327 A CN103728327 A CN 103728327A
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Abstract
The invention provides a method for measuring a uranium isotope ratio in single particles. The method comprises the following steps: S1, preparing a uranium-containing particle sample; S2, searching and identifying uranium-containing particles in the uranium-containing particle sample by utilizing a scanning electron microscope and an X-ray energy dispersive spectrometer; S3, after finding out the uranium-containing particles, transferring the uranium-containing particles onto a sample belt by utilizing a microoperation system; S4, carrying out isotope analysis on the sample belt by utilizing a thermal ionisation mass spectrometer and obtaining the uranium isotope ratio in the uranium-containing particles. Compared with the prior art, the method for measuring the uranium isotope ratio in the single particles, provided by the invention, does not need to carry out irradiation, cooling and etching, can greatly shorten the measurement period of particle analysis and improves analysis efficiency.
Description
Technical field
The present invention relates to nuclear safeguards technical field, particularly a kind of method of measuring uranium isotope ratio in single particulate.
Background technology
Particulate isotope analysis is one of important technology method of nuclear safeguards, for determining that undeclared nuclear material or nuclear activity provide a kind of effective way.Any core is produced and nuclear tests activity, no matter its safeguard measure how, all can be left a trace in corresponding environment; By or its peripheral gauge environmental sample inner at nuclear facilities, carry out particulate isotope analysis, can obtain near the important nuclear activity information of sampled point.This technology has strengthened finds out the ability of not declaring nuclear activity, has strengthened the validity of security system.
Particulate analysis flow process comprises that particulate reclaims, differentiates, locates the steps such as (transfer) and isotope analysis.In all multiparticulates isotope analysis technology, the most ripe is fission track-thermal ionization mass spectrometry (tims) (FT-TIMS) and these two kinds of modes of secondary ion mass spectrum (SIMS).Wherein, due to the high precision that TIMS measures, FT-TIMS has been widely recognized.FT-TIMS completes uranium particulate by fission track (FT) and finds and locate, then carries out isotope measure by thermal ionization mass spectrometry (tims) (TIMS), and FT detects to contain
235u etc. can be brought out by thermal neutron the effective ways of fission nuclide, sample particulate are coated on carrier, and surface coverage solid state track detector, then it is put into reactor and carries out By Thermal Neutron Irradiation, in uranium-bearing particulate
235u is heated and produces and bring out fission after neutron bombardment, and fission fragment is beaten on track detector, forms track.After cooling, solid state track detector is carried out to etch processes, obtain track group, track Tuan center is exactly the position of uranium-bearing particulate in sample.Need to, under optical microscope, by instruments such as glass fibre pin, metal fine needle or optics micro-clamps, pick up micron-sized particulate subsequently, be chosen to the sample band of TIMS, apply the reductive agents such as graphite, by TIMS, complete isotope measure.
The pattern of FT-TIMS associated working has made up the deficiency of method separately mutually.But manual particulate picking, transfer, waste time and energy, and particulate is easily lost, and efficiency is lower.And owing to will passing through all multi-steps such as reactor irradiation, detector etching, particulate transfer and TIMS measurement, cause measuring period relatively long.
Summary of the invention
The object of the invention is to overcome the defect of above prior art, a kind of method of measuring uranium isotope ratio in single particulate is provided, the method, without irradiation, cooling and etching, can significantly be reduced the measuring period of particulate analysis, improves analysis efficiency.
For achieving the above object, the invention provides a kind of side of measuring uranium isotope ratio in single particulate
Method, the method comprises: step S1, prepares uranium-bearing particulate samples;
Step S2, utilizes scanning electron microscope and X ray energy dispersive spectrometry to find in described uranium-bearing particulate samples and differentiates uranium-bearing particulate;
Step S3, finds after described uranium-bearing particulate, utilizes micro OS that described uranium-bearing particulate is transferred on sample band;
Step S4, recycling thermal ionization mass spectrometer carries out isotope analysis and draws uranium isotope ratio in described uranium-bearing particulate described sample band.
Further, described step S1 comprises that by sonic oscillation or the negative pressure mode of clashing into, uranium-bearing particulate being recycled to carbon plate forms sample.
Further; described by sonic oscillation mode by uranium-bearing particulate be recycled to carbon plate form sample be specially; there is the nucleopore membranes of uranium-bearing particulate to immerse in organic solvent absorption; by the ultrasound wave of Ultrasound Instrument, producing vibration departs from uranium-bearing particulate and nucleopore membranes; be suspended in the suspending liquid that forms particulate in organic solution; again by this hanging drop to carbon plate, after organic solvent volatilization, obtain the sample of uranium-bearing particulate.
Further; described by negative pressure clash into mode by uranium-bearing particulate be recycled to carbon plate form sample be specially; by the mode of bleeding, the uranium-bearing particulate in nucleopore membranes is smoked and struck on carbon plate, particulate is just adsorbed on carbon plate, completes the preparation of uranium-bearing particulate samples.
Further, described step S2 comprises will have the carbon plate of uranium-bearing particulate and sample band to put into the Electronic Speculum chamber of scanning electron microscope, after adjusting enlargement factor, find particulate, the particulate that utilizes the backward scattering pattern difference weight element of scanning electron microscope to form, complete the particulate in uranium-bearing particulate samples is carried out to preliminary screening, and then the particulate after preliminary screening is carried out energy spectrum analysis and confirms the uranium-bearing particulate in particulate by X ray energy dispersive spectrometry.
Further, described step S3 comprises after confirmation uranium-bearing particulate, by the superfine tungsten pin of micro OS control, relies on Electrostatic Absorption uranium-bearing particulate, is provoked, and is transferred to subsequently on sample band.
Further, between described step S3 and step S4, be also included in described sample belt surface one deck collodion film is set.
Further, describedly at described sample belt surface, one deck collodion film is set and is specially, to being placed with the mixed liquor that drips collodion and acetic acid isoamyl fat on the sample band of uranium-bearing particulate, after the evaporation of acetic acid isoamyl fat, can form one deck collodion film at sample belt surface.
The invention has the beneficial effects as follows: the present invention utilizes scanning electron microscope (SEM), X ray energy dispersive spectrometry (EDX) and micro OS (μ M) searching, picking, transfer uranium-bearing particulate, without irradiation, cooling and etching, can significantly reduce the measuring period of particulate analysis, improve analysis efficiency.
Accompanying drawing explanation
Fig. 1 is the measuring method process flow diagram of uranium isotope ratio in the single particulate of measurement of the present invention;
Fig. 2 is the uranium-bearing particulate picking process schematic diagram in measuring method of the present invention.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention and advantage are described in more detail.
As shown in Figure 1, be a kind of measuring method process flow diagram of measuring uranium isotope ratio in single particulate provided by the invention.The method comprises the steps:
Step S1, prepares uranium-bearing particulate samples.
The preparation of uranium-bearing particulate samples mainly contains two kinds of modes, by sonic oscillation or the negative pressure mode of clashing into, uranium-bearing particulate is recycled to carbon plate and forms sample.First kind of way is to have the nucleopore membranes of uranium-bearing particulate to immerse in organic solvent absorption, by the ultrasound wave of Ultrasound Instrument, producing vibration departs from uranium-bearing particulate and nucleopore membranes, be suspended in the suspending liquid that forms particulate in organic solution, again by this hanging drop to carbon plate, after organic solvent volatilization, can obtain the sample of uranium-bearing particulate.The second way is that the mode by bleeding is smoked the uranium-bearing particulate in nucleopore membranes strike on carbon plate, and particulate is just adsorbed on carbon plate, thereby completes the preparation of uranium-bearing particulate samples.
Step S2, utilizes in scanning electron microscope (SEM) and X ray energy dispersive spectrometry (EDX) uranium-bearing particulate samples and finds and differentiate uranium-bearing particulate.
The sample of uranium-bearing particulate is reclaimed to the carbon plate of uranium-bearing particulate and sample band and puts into the Electronic Speculum chamber of scanning electron microscope, after adjusting enlargement factor, find particulate, the particulate that utilizes the backward scattering pattern difference weight element of scanning electron microscope to form, complete the particulate in uranium-bearing particulate samples is carried out to preliminary screening, and then the particulate after preliminary screening is carried out energy spectrum analysis and confirms the uranium-bearing particulate in particulate by X ray energy dispersive spectrometry.Wherein sample band is rhenium band.Be uranium-bearing particulate picking process schematic diagram as shown in Figure 2, wherein, Fig. 2 (a) is the Electronic Speculum figure that finds uranium-bearing particulate, and Fig. 2 (b) is the particle diameter statistical graph that Electronic Speculum provides automatically, and Fig. 2 (c) is the energy spectrogram of uranium particulate.
Step S3, finds after uranium-bearing particulate, utilizes micro OS (μ M) that uranium-bearing particulate is transferred on sample band.
Confirm after uranium-bearing particulate, by the superfine tungsten pin of micro OS control, rely on Electrostatic Absorption uranium-bearing particulate, provoked, be transferred to subsequently on sample band.Fig. 2 (d) is the Electronic Speculum figure that provokes uranium-bearing particulate with tungsten pin, and Fig. 2 (e) is the Electronic Speculum figure that shifts uranium-bearing particulate with tungsten pin, and Fig. 2 (f) is the Electronic Speculum figure on sample band by uranium-bearing Micro-placing.
Step S4, recycling thermal ionization mass spectrometer carries out isotope analysis and draws uranium isotope ratio in uranium-bearing particulate sample band.
In order to strengthen sample ionization efficiency, sample is carried out before isotope analysis, to being placed with the mixed liquor that drips collodion and acetic acid isoamyl fat on the sample band of uranium-bearing particulate, after the evaporation of acetic acid isoamyl fat, at sample belt surface, form one deck collodion film, take out afterwards sample band and pack thermal ionization mass spectrometer into and carry out isotope analysis and draw uranium isotope ratio in uranium-bearing particulate.
Utilize said method and device to a natural uranium particulate samples (GBW04205) (particle diameter is about 6 μ and m) has carried out isotope analysis, and wherein, the heating-up temperature of sample band is set as 1650 ℃, and measurement result is:
235u/
238u is 7.29 × 10
-3, relative standard deviation is 0.88%, better with sample nominal value consistance.Said method and device to an enriched uranium uranium particulate samples (CRMU350) (particle diameter is about 2 μ and m) has carried out isotope analysis, and wherein, the heating-up temperature of sample band is set as 1650 ℃, and measurement result is:
234u/
238u is 4.20 × 10
-3, relative standard deviation is 7.73%,
236u/
238u is 3.09 × 10
-3, relative standard deviation is 11.70%, better with sample nominal value consistance.Here it should be noted that, under normal circumstances, in particulate, contain the isotope of four kinds of uranium
234u,
235u,
236u and
238u, in sample
235u and
238the content of U is higher, so
235u/
238u measures relatively easy, and precision of measurement is high, and relative standard deviation is less; And
234u and
236u is very low, measures difficulty higher, so the relative standard deviation of measuring is larger.
In sum, the present invention utilizes scanning electron microscope (SEM), X ray energy dispersive spectrometry (EDX) and micro OS (μ M) searching, picking, transfer uranium-bearing particulate, without irradiation, cooling and etching, can significantly reduce the measuring period of particulate analysis, improve analysis efficiency.
The foregoing is only the preferred embodiment of this practicality invention, is only illustrative for invention, and nonrestrictive.Those skilled in the art is understood, and in the spirit and scope that limit, can carry out many changes to it in claim, revise, and even equivalence, but all will fall in the protection domain of this practicality invention.
Claims (8)
1. a method of measuring uranium isotope ratio in single particulate, is characterized in that, the method comprises:
Step S1, prepares uranium-bearing particulate samples;
Step S2, utilizes scanning electron microscope and X ray energy dispersive spectrometry to find in described uranium-bearing particulate samples and differentiates uranium-bearing particulate;
Step S3, finds after described uranium-bearing particulate, utilizes micro OS that described uranium-bearing particulate is transferred on sample band;
Step S4, recycling thermal ionization mass spectrometer carries out isotope analysis and draws uranium isotope ratio in described uranium-bearing particulate described sample band.
2. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 1, is characterized in that, described step S1 comprises that by sonic oscillation or the negative pressure mode of clashing into, uranium-bearing particulate being recycled to carbon plate forms sample.
3. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 2; it is characterized in that; described by sonic oscillation mode by uranium-bearing particulate be recycled to carbon plate form sample be specially; there is the nucleopore membranes of uranium-bearing particulate to immerse in organic solvent absorption; ultrasound wave by Ultrasound Instrument produces vibration and makes uranium-bearing particulate and nucleopore membranes disengaging, is suspended in the suspending liquid that forms particulate in organic solution, then by this hanging drop to carbon plate; after organic solvent volatilization, obtain the sample of uranium-bearing particulate.
4. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 2; it is characterized in that; described by negative pressure clash into mode by uranium-bearing particulate be recycled to carbon plate form sample be specially; by the mode of bleeding, the uranium-bearing particulate in nucleopore membranes is smoked and struck on carbon plate; particulate is just adsorbed on carbon plate, completes the preparation of uranium-bearing particulate samples.
5. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 1, it is characterized in that, described step S2 comprises will have the carbon plate of uranium-bearing particulate and sample band to put into the Electronic Speculum chamber of scanning electron microscope, after adjusting enlargement factor, find particulate, the particulate that utilizes the backward scattering pattern difference weight element of scanning electron microscope to form, complete the particulate in uranium-bearing particulate samples is carried out to preliminary screening, and then the particulate after preliminary screening is carried out energy spectrum analysis and confirms the uranium-bearing particulate in particulate by X ray energy dispersive spectrometry.
6. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 1, is characterized in that, described step S3 comprises after confirmation uranium-bearing particulate, by the superfine tungsten pin of micro OS control, rely on Electrostatic Absorption uranium-bearing particulate, provoked, be transferred to subsequently on sample band.
7. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 1, is characterized in that, is also included in described sample belt surface one deck collodion film is set between described step S3 and step S4.
8. the method for uranium isotope ratio in the single particulate of measurement as claimed in claim 7, it is characterized in that, describedly at described sample belt surface, one deck collodion film is set and is specially, to being placed with the mixed liquor that drips collodion and acetic acid isoamyl fat on the sample band of uranium-bearing particulate, after the evaporation of acetic acid isoamyl fat, can form one deck collodion film at sample belt surface.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105486663A (en) * | 2016-02-29 | 2016-04-13 | 上海交通大学 | Method for detecting stable carbon isotopic ratio of soil through near infrared spectrum |
| CN105699322A (en) * | 2016-02-29 | 2016-06-22 | 上海交通大学 | Method for quickly detecting stable carbon isotope ratio of soil with near-infrared spectra |
| CN105699314A (en) * | 2016-02-29 | 2016-06-22 | 上海交通大学 | Method for detecting soil stable carbon isotope ratio through intermediate infrared spectrum |
| CN109164162A (en) * | 2018-10-25 | 2019-01-08 | 中国工程物理研究院材料研究所 | It is a kind of with graphene oxide be ionize reinforcing agent uranium isotope abundance measurement method |
| CN109342481A (en) * | 2018-12-04 | 2019-02-15 | 中国工程物理研究院材料研究所 | A kind of method of FIB-TIMS measurement uranium-bearing particle isotope ratio |
| CN109331665A (en) * | 2018-11-01 | 2019-02-15 | 中国原子能科学研究院 | Preparation method containing particle film |
| CN109900771A (en) * | 2017-12-08 | 2019-06-18 | 核工业北京地质研究院 | A kind of measuring method of uranium isotope ratio |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486663A (en) * | 2016-02-29 | 2016-04-13 | 上海交通大学 | Method for detecting stable carbon isotopic ratio of soil through near infrared spectrum |
| CN105699322A (en) * | 2016-02-29 | 2016-06-22 | 上海交通大学 | Method for quickly detecting stable carbon isotope ratio of soil with near-infrared spectra |
| CN105699314A (en) * | 2016-02-29 | 2016-06-22 | 上海交通大学 | Method for detecting soil stable carbon isotope ratio through intermediate infrared spectrum |
| CN105486663B (en) * | 2016-02-29 | 2018-10-19 | 上海交通大学 | A method of detecting the stable carbon isotope ratio of soil using near infrared spectrum |
| CN105699314B (en) * | 2016-02-29 | 2018-10-19 | 上海交通大学 | A method of detecting soil stabilization carbon isotope ratio using middle infrared spectrum |
| CN105699322B (en) * | 2016-02-29 | 2018-10-19 | 上海交通大学 | The method that the stable carbon isotope ratio of soil is quickly detected using near infrared spectrum |
| CN109900771A (en) * | 2017-12-08 | 2019-06-18 | 核工业北京地质研究院 | A kind of measuring method of uranium isotope ratio |
| CN109900771B (en) * | 2017-12-08 | 2021-10-19 | 核工业北京地质研究院 | Method for determining uranium isotope ratio |
| CN109164162A (en) * | 2018-10-25 | 2019-01-08 | 中国工程物理研究院材料研究所 | It is a kind of with graphene oxide be ionize reinforcing agent uranium isotope abundance measurement method |
| CN109164162B (en) * | 2018-10-25 | 2021-02-26 | 中国工程物理研究院材料研究所 | Uranium isotope abundance measurement method using graphene oxide as ionization enhancer |
| CN109331665A (en) * | 2018-11-01 | 2019-02-15 | 中国原子能科学研究院 | Preparation method containing particle film |
| CN109331665B (en) * | 2018-11-01 | 2021-01-05 | 中国原子能科学研究院 | Method for producing film containing fine particles |
| CN109342481A (en) * | 2018-12-04 | 2019-02-15 | 中国工程物理研究院材料研究所 | A kind of method of FIB-TIMS measurement uranium-bearing particle isotope ratio |
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Application publication date: 20140416 |