CN104236972A - Preparation method and analysis method of aqueous samples - Google Patents
Preparation method and analysis method of aqueous samples Download PDFInfo
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- CN104236972A CN104236972A CN201410428528.9A CN201410428528A CN104236972A CN 104236972 A CN104236972 A CN 104236972A CN 201410428528 A CN201410428528 A CN 201410428528A CN 104236972 A CN104236972 A CN 104236972A
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Abstract
The invention discloses a preparation method and an analysis method of aqueous samples. The preparation method is used for analyzing the content of hydrogen and oxygen isotopes in water under the high vacuum environment. The preparation method of the aqueous samples comprises the following steps: providing a plurality of glass slides with determined sizes; putting carriers on the glass slides under the dry experimental environment; dropwise adding water with different content of hydrogen and oxygen isotopes to the carriers on the glass slides to form hydrates; transferring the glass slides to a primary vacuum chamber, volatilizing excess water to form the required aqueous samples. The analysis method of the aqueous samples comprises the steps of forming the sample by adopting the preparation method and transferring the sample to the vacuum chamber for analysis. By virtue of the preparation method, water is well retained; the problem that the water is easy to volatilize in the high vacuum can be avoided; a relatively good analysis effect can be achieved.
Description
Technical field
The present invention relates to isotope analysis field, particularly relate to a kind of preparation method of aqueous specimen.
Background technology
Along with the fast development of science and technology, interpenetrating of each door subject technology is more remarkable.Vacuum has highlighted its superiority and importance as an independent subject, such as, under high vacuum environment, effectively can avoid the interference of extraneous factor to the analysis of physical and chemical property detecting sample.
Hydrogen, oxygen are the widest element that distributes, Oxygen and Hydrogen isotope research relates to universe, the moon, each layer circle of the earth, comprise lithosphere, hydrosphere, air ring, particularly various water Oxygen and Hydrogen isotope research, it to multiple Petrogenesis And Metallogenesis process and Material Source significant.
Consider the unique advantage under high vacuum environment, imperative to Oxygen and Hydrogen isotope research under vacuum conditions.But as the common water containing Oxygen and Hydrogen isotope, be then be easy to volatilization under high vacuum environment, cause cannot realizing directly analyzing moisture under high vacuum environment.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of aqueous specimen and analytic approach to send out, to realize measuring hydrogen atom isotope and the isotopic object of oxygen atom under high vacuum environment.
Based on this, the invention provides a kind of preparation method of aqueous specimen, for carrying out under high vacuum environment in water, Oxygen and Hydrogen isotope is containing quantitative analysis, and the method comprises:
The slide glass of multiple setting size is provided;
Under the experimental situation of drying, carrier is placed on each slide glass;
The carrier of each slide glass instills the water that Oxygen and Hydrogen isotope content is different, forms hydrate;
Slide glass is transferred to primary vacuum chamber, unnecessary moisture evaporation is fallen, form required aqueous specimen.
Optionally, for the preparation method of described aqueous specimen, described slide glass is rectangle, and setting size is length of side 0.5cm-8cm.
Optionally, for the preparation method of described aqueous specimen, described carrier is the anhydrous compound of not hydrogeneous oxygen element.
Optionally, for the preparation method of described aqueous specimen, the anhydrous compound of described not hydrogeneous oxygen element adopts 1mg-20mg.
Optionally, for the preparation method of described aqueous specimen, the water that the Oxygen and Hydrogen isotope content of described instillation is different is 0.01mL-0.1mL.
Optionally, for the preparation method of described aqueous specimen, described slide glass is for being formed carrying out cutting through prewashed wafer.
Optionally, for the preparation method of described aqueous specimen, before slide glass is transferred to primary vacuum chamber, first slide glass is fixed on the sample stage of high vacuum analytical equipment.
The invention provides a kind of analytical approach of aqueous specimen, comprising: the aqueous specimen of preparation method's acquisition of the aqueous specimen described in utilization, is transferred to high vacuum chamber analysis by described aqueous specimen.
Optionally, for the analytical approach of described aqueous specimen, before described aqueous specimen is transferred to high vacuum chamber, the vacuum tightness of described primary vacuum chamber is made to reach more than 1E-6mbar.
Compared with prior art, in the preparation method of aqueous specimen provided by the invention and analytical approach, carrier placed by slide glass, and on carrier, instill the different water of Oxygen and Hydrogen isotope content, form hydrate, then unnecessary moisture evaporation is fallen, thus obtain aqueous specimen.Compared to existing technology, adopt this preparation method simple, with low cost, containing water in the sample of acquisition, define required aqueous specimen, solve water due to volatile in high vacuum and make the problem of sample fails.Further, do not contain hydrogen-oxygen element in slide glass and carrier, avoid the interference to sample.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the preparation method of embodiment of the present invention aqueous specimen;
Fig. 2 is the process flow diagram of the analytical approach of embodiment of the present invention aqueous specimen.
Embodiment
Below in conjunction with schematic diagram, the preparation method of aqueous specimen of the present invention and analytical approach are described in more detail, which show the preferred embodiments of the present invention, should be appreciated that those skilled in the art can revise the present invention described here, and still realize advantageous effects of the present invention.Therefore, following description is appreciated that extensively knowing for those skilled in the art, and not as limitation of the present invention.
In order to clear, whole features of practical embodiments are not described.They in the following description, are not described in detail known function and structure, because can make the present invention chaotic due to unnecessary details.Will be understood that in the exploitation of any practical embodiments, a large amount of implementation detail must be made to realize the specific objective of developer, such as, according to regarding system or the restriction about business, change into another embodiment by an embodiment.In addition, will be understood that this development may be complicated and time-consuming, but be only routine work to those skilled in the art.
In the following passage, more specifically the present invention is described by way of example with reference to accompanying drawing.According to the following describes and claims, advantages and features of the invention will be clearer.It should be noted that, accompanying drawing all adopts the form that simplifies very much and all uses non-ratio accurately, only in order to object that is convenient, the aid illustration embodiment of the present invention lucidly.
Central idea of the present invention is, provides a kind of preparation method of aqueous specimen, comprises the steps:
Step S101: the slide glass that multiple setting size is provided;
Step S102: under the experimental situation of drying, is placed on each slide glass by carrier;
Step S103: instill the water that Oxygen and Hydrogen isotope content is different on the carrier of each slide glass, forms hydrate;
Step S104: slide glass is transferred to primary vacuum chamber, falls unnecessary moisture evaporation, forms required aqueous specimen.
Based on this thought, please refer to Fig. 1, Fig. 1 is the process flow diagram of the preparation method of embodiment of the present invention aqueous specimen.This method comprises:
Step S101, provides the slide glass of multiple setting size.Preferably, in order to avoid the interference of slide glass itself, the slide glass that the embodiment of the present invention adopts is obtained by wafer.Described wafer is clean and tidy to ensure through prerinse, and moisture is removed in drying further.Described wafer cuts after cleaning up, and preferably, this cutting makes wafer form multiple rectangular tiles, and its size can be that the length of side is at 0.5cm-8cm.Usually can be chosen as square, the such as length of side is the square of 0.5cm.Described slide glass size decides by needing the amount of carrying out the aqueous specimen analyzed, therefore, and the square etc. of can also to be such as the length of side be 1cm, the square of maximum usual length of side 8cm.Certainly, described slide glass can also be other arbitrary shapes.In the present embodiment, the slide glass that multiple size is identical is adopted.
Step S102, under the experimental situation of drying, is placed on carrier on each slide glass.The present invention is the water in order to prepare containing Oxygen and Hydrogen isotope, in order to avoid the interference of carrier, need in carrier also not containing these two kinds of elements, and need the volatilization under vacuum conditions of anti-sealing simultaneously, therefore inventor thinks that after research utilizing some anhydrous compounds to meet after water can form hydrate, this makes it possible to water to retain, prevent volatilization.Such as described carrier can be anhydrous calcium chloride, and usually adopting the anhydrous calcium chloride of 1mg-20mg, such as, is the anhydrous calcium chloride placing 10mg on each slide glass in the present embodiment.Certainly, the anhydrous compound of this not hydrogeneous oxygen element can also be other materials, such as, be anhydrous magnesium chloride etc.
Step S103, the carrier of each slide glass instills the water that Oxygen and Hydrogen isotope content is different, forms hydrate.Isotope protium, deuterium, tritium at least containing hydrogen in the water that each slide glass instills, and the isotope of oxygen
16o,
18the one of O.After instillation, for anhydrous calcium chloride, six calcium chloride hydrate can be combined into water, which forms the aqueous specimen in the present invention.The water that described each slide glass instills for 0.01mL-0.1mL, in the present embodiment, adopt 0.05mL.In order to ensure the better combination of water and anhydrous calcium chloride, can rock slide glass.
Step S104, is transferred to primary vacuum chamber by slide glass, is fallen by unnecessary moisture evaporation, forms required aqueous specimen.Usually, before slide glass is transferred to primary vacuum chamber, first slide glass is fixed on the sample stage of high vacuum analytical equipment.Described primary vacuum chamber can adopt of the prior art any one, such as gas lock (Air-lock).After being transferred to primary vacuum chamber, start to vacuumize, unnecessary moisture evaporation is fallen, preferably, ensure that the vacuum tightness of primary vacuum chamber is at least that 1E-6mbar can realize.
So far, prepared by the aqueous specimen in the present invention.
Next be introduced the analytical approach of aqueous specimen of the present invention, as shown in Figure 2, the method comprises: step S201: provide the aqueous specimen obtained by the preparation method of described aqueous specimen.Step S202: after guaranteeing that the vacuum tightness of described primary vacuum chamber is at least 1E-6mbar, described aqueous specimen is transferred to high vacuum chamber analysis, just can obtains kind and the content of Oxygen and Hydrogen isotope in water.
The vacuum tightness of described high vacuum chamber is due to the vacuum tightness of primary vacuum chamber.In the present embodiment, described high vacuum chamber is analyzes chamber (Analysis chamber), also can for having the equipment of similar effect.
In the preparation method and analytical approach of aqueous specimen of the present invention, water is existed in the form of hydrates, retained the water that will carry out analyzing.The moisture evaporation not forming hydrate is fallen simultaneously, avoid the interference to analysis result due to the volatilization gradually of moisture.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (9)
1. a preparation method for aqueous specimen, for carrying out under high vacuum environment in water, Oxygen and Hydrogen isotope is containing quantitative analysis, and the method comprises:
The slide glass of multiple setting size is provided;
Under the experimental situation of drying, carrier is placed on each slide glass;
The carrier of each slide glass instills the water that Oxygen and Hydrogen isotope content is different, forms hydrate;
Slide glass is transferred to primary vacuum chamber, unnecessary moisture evaporation is fallen, form required aqueous specimen.
2. the preparation method of aqueous specimen as claimed in claim 1, it is characterized in that, described slide glass is rectangle, and setting size is length of side 0.5cm-8cm.
3. the preparation method of aqueous specimen as claimed in claim 1, it is characterized in that, described carrier is the anhydrous compound of not hydrogeneous oxygen element.
4. the preparation method of aqueous specimen as claimed in claim 3, is characterized in that, the anhydrous compound of described not hydrogeneous oxygen element adopts 1mg-20mg.
5. the preparation method of aqueous specimen as claimed in claim 1, it is characterized in that, the water that the Oxygen and Hydrogen isotope content of described instillation is different is 0.01mL-0.1mL.
6. the preparation method of aqueous specimen as claimed in claim 1, is characterized in that, described slide glass is for being formed carrying out cutting through prewashed wafer.
7. the preparation method of aqueous specimen as claimed in claim 1, is characterized in that, before slide glass is transferred to primary vacuum chamber, be first fixed on by slide glass on the sample stage of high vacuum analytical equipment.
8. an analytical approach for aqueous specimen, comprising: the aqueous specimen utilizing the preparation method as the aqueous specimen in claim 1-7 as described in any one to obtain, is transferred to high vacuum chamber analysis by described aqueous specimen.
9. the analytical approach of aqueous specimen as claimed in claim 8, is characterized in that, before described aqueous specimen is transferred to high vacuum chamber, make the vacuum tightness of described primary vacuum chamber be at least 1E-6mbar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410428528.9A CN104236972B (en) | 2014-08-27 | The preparation method of aqueous specimen and the method for analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410428528.9A CN104236972B (en) | 2014-08-27 | The preparation method of aqueous specimen and the method for analysis |
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| Publication Number | Publication Date |
|---|---|
| CN104236972A true CN104236972A (en) | 2014-12-24 |
| CN104236972B CN104236972B (en) | 2017-01-04 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2059242U (en) * | 1990-01-04 | 1990-07-11 | 河北煤炭科学研究所 | Deuterium sampling system in water |
| JPH0371035A (en) * | 1989-08-10 | 1991-03-26 | Fuji Electric Co Ltd | Method for preparing hydrophobic sample |
| GB2309782B (en) * | 1996-02-03 | 1999-05-19 | Univ Open | Isotopic analysis of water |
| CN102621276A (en) * | 2012-03-09 | 2012-08-01 | 中国科学院寒区旱区环境与工程研究所 | Device capable of controllably correcting ratio, gradient and vertical fractional distillation process measurement of oxyhydrogen stable isotope in atmospheric water |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0371035A (en) * | 1989-08-10 | 1991-03-26 | Fuji Electric Co Ltd | Method for preparing hydrophobic sample |
| CN2059242U (en) * | 1990-01-04 | 1990-07-11 | 河北煤炭科学研究所 | Deuterium sampling system in water |
| GB2309782B (en) * | 1996-02-03 | 1999-05-19 | Univ Open | Isotopic analysis of water |
| CN102621276A (en) * | 2012-03-09 | 2012-08-01 | 中国科学院寒区旱区环境与工程研究所 | Device capable of controllably correcting ratio, gradient and vertical fractional distillation process measurement of oxyhydrogen stable isotope in atmospheric water |
Non-Patent Citations (3)
| Title |
|---|
| BAO-LONG XU ET AL.: "Experimental studies of oxygen and hydrogen isotope fractionations between precipitated brucite and water at low temperatures", 《GEOCHIMICA ET COSMOCHIMICA ACTA》 * |
| JUSKE HORITA ET AL.: "PROCEDURE FOR THE HYDROGEN ISOTOPE ANALYSIS OF WATER FROM CONCENTRATED BRINES", 《CHEMICAL GEOLOGY (ISOTOPE GEOSCIENCE SECTION)》 * |
| 谢狄霖 等: "含水物质红外光谱测试的样品制备", 《分析仪器》 * |
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Address after: Room 507, building 09, Northwest District, Suzhou nano City, No. 99, Jinjihu Avenue, Suzhou Industrial Park, China (Jiangsu) pilot Free Trade Zone, Suzhou, Jiangsu 215000 Patentee after: Shengke nano (Suzhou) Co.,Ltd. Address before: Room 507, building 09, northwest Suzhou nano City, 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province, 215123 Patentee before: SHENGKE NANO (SUZHOU) Co.,Ltd. |