CN110514508A - It is a kind of it is easy, quickly, the device and method that efficiently separate enrichment boron - Google Patents

It is a kind of it is easy, quickly, the device and method that efficiently separate enrichment boron Download PDF

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Publication number
CN110514508A
CN110514508A CN201910887796.XA CN201910887796A CN110514508A CN 110514508 A CN110514508 A CN 110514508A CN 201910887796 A CN201910887796 A CN 201910887796A CN 110514508 A CN110514508 A CN 110514508A
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China
Prior art keywords
cover
shaped body
goblet
hole
hot plate
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CN201910887796.XA
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CN110514508B (en
Inventor
肖军
贺茂勇
邓丽
张飞
金章东
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Institute of Earth Environment of CAS
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Institute of Earth Environment of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/0011Heating features
    • B01D1/0017Use of electrical or wave energy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample

Abstract

The present invention provide it is a kind of it is easy, quickly, the device and method that efficiently separate enrichment boron, including goblet and cover-shaped body, and electric hot plate and temperature controller, there is cylindrical cavity in the middle part of the cover-shaped body, acidic liquid sample is placed in cylindrical cavity, goblet and cover-shaped body have the screw thread of cooperation, can screw up sealing completely.Goblet tips upside down on cylindrical cavity, is put into togerther in the hole of electric hot plate, and temperature controller is electrically connected with the realization of electric hot plate several holes, for accurately controlling the heating temperature in each hole.When solution evaporation completely, cover-shaped body cylindrical cavity condensation after, extracted, it is to be measured.The present invention expands the application range of nature sample, and the solid sample after most of fluid sample and resolution can be used the present apparatus, can in high volume carry out sample treatment, expand the scope of application of sample, has bigger market and application space.

Description

It is a kind of it is easy, quickly, the device and method that efficiently separate enrichment boron
Technical field
The invention belongs to chemical element purification technique field more particularly to it is a kind of it is easy, quickly, efficiently separate enrichment The device and method of boron.
Background technique
As shown in Figure 1, be the device of existing separating boron, boron there are two stable isotope,10B and11B.The two are stablized Between isotope it is big it is of poor quality cause Fractionation of boron isotope difference in nature huge (+145 ‰), and then make boron istope from It is widely used in right boundary.Multi-purpose MC-ICP-MS (mostly reception inductivity coupled plasma mass spectrometry) carries out boron istope test at present. Before carrying out the test of sample boron istope, needs to separate the boron in sample with other elements, then be enriched with again.Majority The method of effects of boron resin or the method separation and concentration boron of effects of boron resin and zwitterion resin-bonded were used, it is continuous to grasp Make the time at 9 hours or so.
In solution, boron is mainly with H3BO3With B (OH)4 -Two kinds of forms exist.Boron in acid condition, solution mainly with H3BO3Form exists, volatile, especially under high temperature environment.Using this feature, design within Gaillardet et al. 2001 Device as shown in Figure 1 carries out the separation and enrichment of boron in liquid.About 50-100 μ L acidic sample is placed in the PFA lid of 5mL Among son 101, it is placed on plane electric hot plate 103 and heats after then wrapping cup 102 with aluminium-foil paper.Utilize acidity Under the conditions of boron boiling characteristics, be evaporated to boron element at the tip of top, and other elements continue to stay on lid.Equal samples After being evaporated, cup is cooled down under natural conditions.Then the liquid after evaporative condenser at the tip of top is taken out, it is to be measured.
Although the device of figure 1 above can carry out the separation and enrichment of fluid sample boron, also suffer from certain drawbacks.1. should Device can only evaporate 50-100 μ L acidic sample.It is more again, it can be more than the capacity at the tip of top, sample is made to will continue to reflux to lid In son, the effect of separation is not achieved.Due to generally requiring the concentration of final sample boron in 100 μ g/L when test, need 3mL, it is therefore desirable to which the boron concentration of primary sample is higher than 3 μ g/mL.But nature fluid sample, mainly river water, well water, rain The boron concentration of water is mostly ppb grades, therefore upper figure equipment will not be widely used, and be only suitable for high boron concentration samples.
Device in Fig. 1 needs to open lid and then takes out the sample at the tip of top after sample evaporative condenser, The technical difficulty of operation is larger, is not careful, and the drop of top will be fallen down.
The heating of plane electric hot plate is uneven, and only cover-shaped body can be heated, and cooling effect of the goblet vulnerable to air, So that the temperature of cup body easily changes, especially intermediate and edge sample is difficult to make the evaporating temperatures of all samples all, warm Degree is maximum up to 5 degrees Celsius.Therefore the time of each sample evaporative condenser gap, unification difficult to realize can be not easy to grasp Make.
Summary of the invention
It is an object of the invention to solve the problems of the above-mentioned prior art, provide it is a kind of it is easy, quickly, efficiently separate The device and method for being enriched with boron, and sample treatment can be in high volume carried out, the scope of application of sample has been expanded, there is bigger city Field and application space.
The present invention adopts the following technical scheme:
A kind of device that is easy, quick, efficiently separating enrichment boron, including goblet and cover-shaped body and electric hot plate and temperature Device is controlled, there is cylindrical cavity in the middle part of the cover-shaped body, be placed in cylindrical cavity to enrichment solution, goblet back-off is screwed in On cover-shaped body with cylindrical cavity, goblet oral area is inserted into the cavity between cover-shaped body cylindrical cavity and outer rim, composition Container is heated, is put into togerther in the hole of electric hot plate, temperature controller is electrically connected with the realization of electric hot plate several holes, each for accurately controlling The heating temperature of aperture.
The further technical solution of the present invention is that the most outside diameter of hypanthial most outside diameter and/or cover-shaped body is equal The internal diameter in the hole < guarantees that cover-shaped body and/or cup-shaped physical efficiency are put into the hole of electric hot plate.
The further technical solution of the present invention is that goblet is buckled on cover-shaped body, and goblet and cover-shaped body have matched spiral shell Line can screw up completely together, achieve the purpose that sealing sample to be evaporated.
Further technical solution is that composition heating container when being put into togerther in the hole of electric hot plate, retains goblet bottom There are 0.5cm outside hole.
Further technical solution is that temperature controller accurately controls heating temperature, makes temperature in each hole of electric hot plate not 0.5 degree Celsius can be differed.
Preparation process of the invention is:
The container for the acid solution that step 1. production is collected
Using the goblet of suitable size, corresponding cover-shaped body is then processed, middle part has in cylinder in cover-shaped body Chamber can be put into solution to be enriched with.
Step 2. production heating container
Goblet is tipped upside down on cover-shaped body, is connected through a screw thread and tightens, is put into electric heating plate hole, only stays 0.5cm outside Portion facilitates the condensation of evaporation solution and last cup lid body to take out.
Step 3. heating preparation plasticity solution
Heating temperature is accurately controlled with temperature controller.Electric hot plate is put into after there is hole, goblet and cover-shaped body can combine Kong Zhong ensure that cover-shaped body and cup-shaped body side surface can be heated simultaneously, and can achieve the temperature in each hole not using protractor 0.5 degree Celsius can be differed, heating temperature consistency has been reached, when evaporating in cylindrical cavity to enrichment solution reaches a certain amount of When, flowing back into the cover-shaped body outside cylindrical cavity along cup wall to enrichment solution for evaporation is evaporated when to enrichment solution Completely, after condensing, goblet can be opened, is not in the phenomenon that B solution to be enriched with is missed.
Beneficial effects of the present invention:
Apparatus of the present invention expand the application range that boron istope is produced, and sample after most of fluid sample and solid resolution The device can be used in the Separation of Boron Isotopes enrichment of product.This method only need to be put into sample, cover lid goblet convenient for operation, It is placed on electric hot plate and heats, then condensation is taken out.Sample pre-treatments are carried out without staying in laboratory all day.
Currently, the electric hot plate that the present invention designs can once be put into multiple samples.It later can be according to laboratory estrade Size designs bigger electric hot plate, goblet and cover-shaped body, is put into more samples in batches.
It is time saving, laborsaving, convenient for operation in short, apparatus of the present invention, sample treatment can be in high volume carried out, sample has been expanded The scope of application, have bigger market and application space.
Detailed description of the invention
Fig. 1 is the device of existing separating boron in background technique;
Fig. 2 is hypanthial structural schematic diagram of the invention;
Fig. 3 is the structural schematic diagram of cover-shaped body of the invention;
Fig. 4 is schematic structural view of the invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 2,3, 4, a kind of device that is easy, quick, efficiently separating enrichment boron of the invention, including goblet 1 With cover-shaped body 2 and electric hot plate 3 and temperature controller 4, there is in the middle part of the cover-shaped body 2 cylindrical cavity 201, set to enrichment solution In in cylindrical cavity 201, goblet is tipped upside down on cylindrical cavity 201, and 1 oral area of goblet is inserted into cover-shaped body cylindrical cavity In cavity 202 between 201 and outer rim 203, composition heating container is put into togerther in the hole 30 of electric hot plate 3, temperature controller 4 and electricity 3 several holes 30 of hot plate realize electrical connection, for accurately controlling the heating temperature in each hole 30.
The further technical solution of the present invention is the most outside diameter of goblet 1 and/or the most outside diameter of cover-shaped body 2 The internal diameter in the equal hole < guarantees that cover-shaped body 2 and/or goblet 1 can be put into the hole 30 of electric hot plate 3.
The further technical solution of the present invention is that goblet 1 and cover-shaped body 2 have matched screw thread, can be screwed up together, Reach sealing effect.
Further technical solution is that composition heating container when being put into togerther in the hole 30 of electric hot plate 3, retains goblet 1 There are 0.5cm outside hole 30 for bottom.
Further technical solution is that temperature controller 4 accurately controls heating temperature, makes the temperature in each hole 30 of electric hot plate 3 Degree will not differ 0.5 degree Celsius.
Preparation process of the invention is:
The container for the acid solution that step 1. production is collected
In order to promote the evaporation capacity of sample, the goblet 1 of suitable size is used, naturally it is also possible to continue as needed with more The goblet 1 of large volume.Then corresponding cover-shaped body 2 is processed, middle part has cylindrical cavity 201, Ke Yifang in cover-shaped body 2 Enter solution to be enriched with.
Step 2. production heating container
Cover-shaped body 2 is put into the hole 30 that electric hot plate 3 has, and be buckled to goblet 1,1 port of goblet insertion lid In cavity 202 between shape body cylindrical cavity 201 and outer rim 203, goblet 1 and cover-shaped body 2 all have screw thread, cover-shaped body 2 Outer rim (non-cylindrical inner cavity 201) and 1 port outer rim 203 of goblet can screw up completely together, play the role of sealing, or 1 oral area outer rim 203 of person's goblet has external screw thread, and 2 outer rim of cover-shaped body, 203 inner wall has internal screw thread, and 1/ cover-shaped body 2 of goblet can Be put into each hole 30 of electric hot plate 3 completely, 1 bottom of goblet only stays 0.5cm outside hole 30, facilitates the cold of evaporation solution Solidifying and final unit taking-up.
Step 3. heating preparation plasticity solution
Accurately control heating temperature with temperature controller 4, electric hot plate 3 there is hole, goblet 1 and cover-shaped body 2 to combine after simultaneously It is put into hole 30, it is ensured that cover-shaped body 2 and goblet 1 are heated simultaneously, and it is Celsius that the temperature in each hole 30 will not differ 0.5 Degree, has reached heating temperature consistency, when evaporating in the cylindrical cavity 201 of cover-shaped body 2 to enrichment solution reaches a certain amount of When, evaporation can flow back into the cover-shaped body 2 outside cylindrical cavity 201 to enrichment solution along cup wall, when to enrichment solution After evaporating complete, condensation, goblet 1 can be opened, be not in the phenomenon that being missed to enrichment solution.
Embodiment
Experiment display, the acidic sample of 3mL use the PFA cup of 15mL, naturally it is also possible to which it is bigger to continue use as needed The cup of volume.Then corresponding cover-shaped body 2 is processed, middle part has cylindrical cavity 201 in cover-shaped body 2, is put into the liquid of 3mL Body acidic sample.
As shown in figure 3, cover-shaped body 2 is put into the hole 30 that electric hot plate 3 has, and it is buckled to cup, cup can be complete It is put into each hole 30 of electric hot plate 3 entirely, only stays 0.5cm in outside.
Heating temperature is accurately controlled with temperature controller 4, electric hot plate 3 is put into after there is hole, goblet 1 and cover-shaped body 2 to combine In hole 30, ensure that cover-shaped body 2 and goblet 1 can be heated simultaneously, the temperature in each hole 30 will not differ 0.5 degree Celsius, Reach heating temperature consistency, when the liquid acidic solution evaporation in cylindrical cavity 201 reaches a certain amount of, the liquid of evaporation Body acid solution can flow back into lid (cavity 202 between outer rim 203 of cylindrical cavity 201) along cup wall, when After acid solution evaporates complete, condensation, cup can be opened, be not in the phenomenon that acid solution is missed.
At 90 DEG C, 18 hours can evaporating completely it is complete.Acidic liquid sample is put into of the invention by general that afternoon Device can take out for excessively complete night second day.Without continuously staying in laboratory as crossing effects of boron resin column.In order to save 3 temperature of electric hot plate can also be increased to 110 DEG C, can be evaporated 3mL sample within 4 hours at this time by the time.It is time saving and energy saving, And convenient for operation.
Compared with the background technology, the present invention, it machined biggish cylindrical cavity 201, can be put into a greater amount of wait be enriched with Sample.After enriched sample evaporation, does not hang over instead of at upper tips as shown in Figure 1, flow back into cover shape as shown in Figure 2 In body 2, worry is completely dispensed with because misoperation falls down sample.
And the hole that can be put into goblet 1 as shown in Figure 2 is opened on electric hot plate 3, cover-shaped body 2 and goblet 1 can be same (when using pervious plane electric hot plate 103, only cover-shaped body 2 can be heated Shi Shoure, and goblet 1 is vulnerable to the cold of air But act on, so that the temperature of cup body easily changes), heating can be made more uniform, every place's sample temperature will not differ 0.5 and take the photograph Family name's degree.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features; And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and Range.

Claims (6)

1. a kind of device that is easy, quick, efficiently separating enrichment boron, which is characterized in that including goblet and cover-shaped body, Yi Ji electricity Hot plate and temperature controller, the cover-shaped body middle part have cylindrical cavity, are placed in cylindrical cavity to enrichment solution, goblet falls It being buckled on cover-shaped body, goblet oral area is inserted into the cavity between cover-shaped body cylindrical cavity and outer rim, composition heating container, and one It rises and is put into the hole of electric hot plate, temperature controller is electrically connected with electric hot plate several holes, for accurately controlling the heating temperature in each hole.
2. a kind of device that is easy, quick, efficiently separating enrichment boron according to claim 1, which is characterized in that goblet Most outside diameter and/or cover-shaped body the equal hole < of most outside diameter internal diameter, guarantee that cover-shaped body and/or cup-shaped physical efficiency are put into electricity In the hole of hot plate.
3. a kind of device that is easy, quick, efficiently separating enrichment boron according to claim 1, which is characterized in that goblet Screw thread is all had with cover-shaped body, goblet is buckled on cover-shaped body, is that sealing is screwed up by screw thread.
4. a kind of device that is easy, quick, efficiently separating enrichment boron according to claim 1, which is characterized in that heating is held When device is put into togerther in the hole of electric hot plate, retaining goblet bottom, there are 0.5cm outside hole.
5. a kind of device that is easy, quick, efficiently separating enrichment boron according to claim 1, which is characterized in that temperature controller Heating temperature is accurately controlled, the temperature in each hole of electric hot plate is made not differ 0.5 degree Celsius.
6. a kind of device that is easy, quick, efficiently separating enrichment boron according to claim 1, which is characterized in that it is prepared Technique includes the following steps:
The container for the acid solution that step 1. production is collected
Using the goblet of suitable size, corresponding cover-shaped body is then processed, middle part has cylindrical cavity in cover-shaped body, puts Enter B solution to be enriched with;
Step 2. preparation heating container
Goblet is tipped upside down on cover-shaped body, is tightened by screw thread, is put into the hole of electric hot plate, goblet or/and cover-shaped body are equal It can be put into any one hole of electric hot plate, and there are 0.5cm outside hole for reservation goblet bottom;
Step 3. heating preparation plasticity solution
Heating temperature is accurately controlled with temperature controller, the temperature in each hole is made not differ 0.5 degree Celsius, has reached heating temperature Degree is consistent, when in cylindrical cavity when enrichment solution evaporation reaches a certain amount of, evaporation can be along cup-shaped to enrichment solution Internal wall flows back into the cavity between cover-shaped body cylindrical cavity and outer rim, when after enrichment solution evaporation completely, condensation after, can Goblet is opened, B solution to be enriched with is obtained.
CN201910887796.XA 2019-09-19 2019-09-19 Device and method for simply, conveniently, quickly and efficiently separating and enriching boron Active CN110514508B (en)

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CN110514508B CN110514508B (en) 2023-12-29

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB890925A (en) * 1959-11-20 1962-03-07 Tack Air Conditioning Ltd Improvements relating to vaporising devices
CN102378641A (en) * 2009-03-31 2012-03-14 吉纳瓦克有限公司 Method and sample holding assembly for use in sample preparation
US20140106397A1 (en) * 2011-06-30 2014-04-17 3M Innovative Properties Company Systems and methods for detecting an analyte of interest in a sample using filters and microstructured surfaces
CN104729906A (en) * 2015-04-14 2015-06-24 中国科学院地球环境研究所 Efficient and pollution-free boron isotope pressurization separating device for low-boron environmental samples
CN104964941A (en) * 2015-06-29 2015-10-07 浙江大学 Method and separating and collecting device for detecting elemental selenium quickly and quantitatively
CN206074339U (en) * 2016-07-18 2017-04-05 宁波出入境检验检疫局检验检疫技术中心 One kind is universal to catch up with sour heating instrument
CN207816690U (en) * 2018-03-01 2018-09-04 广西壮族自治区水产科学研究院 A kind of ICP-MS detects the simple system of total mercury content in natural mineral water
CN210571663U (en) * 2019-09-19 2020-05-19 中国科学院地球环境研究所 Simple, convenient, quick, high-efficient separation enrichment boron's device

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB890925A (en) * 1959-11-20 1962-03-07 Tack Air Conditioning Ltd Improvements relating to vaporising devices
CN102378641A (en) * 2009-03-31 2012-03-14 吉纳瓦克有限公司 Method and sample holding assembly for use in sample preparation
US20140106397A1 (en) * 2011-06-30 2014-04-17 3M Innovative Properties Company Systems and methods for detecting an analyte of interest in a sample using filters and microstructured surfaces
CN104729906A (en) * 2015-04-14 2015-06-24 中国科学院地球环境研究所 Efficient and pollution-free boron isotope pressurization separating device for low-boron environmental samples
CN104964941A (en) * 2015-06-29 2015-10-07 浙江大学 Method and separating and collecting device for detecting elemental selenium quickly and quantitatively
CN206074339U (en) * 2016-07-18 2017-04-05 宁波出入境检验检疫局检验检疫技术中心 One kind is universal to catch up with sour heating instrument
CN207816690U (en) * 2018-03-01 2018-09-04 广西壮族自治区水产科学研究院 A kind of ICP-MS detects the simple system of total mercury content in natural mineral water
CN210571663U (en) * 2019-09-19 2020-05-19 中国科学院地球环境研究所 Simple, convenient, quick, high-efficient separation enrichment boron's device

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