Boron isotope abundance measuring method using carbon nanotube as ion emitting agent

A technology of isotopic abundance and carbon nanotubes, which is used in measurement devices, preparation of test samples, material analysis by electromagnetic means, etc., can solve the problem of low positive ion ionization efficiency, difficulty in high-precision measurement, and isobaric It can improve the ion emission performance, the sample measurement results are accurate, and the emission intensity can be improved.

Active Publication Date: 2014-01-01
NUCLEAR POWER INSTITUTE OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Negative thermal ionization mass spectrometry is used to measure boron, which has high precision and sensitivity, but due to the detected ion BO 2 - The mass number is small (42 and 43), so the shunt effect and mass discrimination effect are serious, the measurement accuracy is not high, and in the presence of organic impurities such as residual ion exchange resin, mannitol and nitrate, it is easy to produce CNO - Ion (m / z= 42), causing isobaric interference
Positive ion method, M 2 BO 2 + (M alkali metal elements: Na, K, Cs, etc.) The mass of ions is significantly increased. Although the shunt and mass discrimination effects can be reduced, the ionization efficiency of positive ions is not high. Generally, the sample amount is in the order of micrograms and nanograms. It is difficult to measure with high precision
[0003] Therefore, there is currently no method for measuring boron isotopes to that precision

Method used

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  • Boron isotope abundance measuring method using carbon nanotube as ion emitting agent
  • Boron isotope abundance measuring method using carbon nanotube as ion emitting agent
  • Boron isotope abundance measuring method using carbon nanotube as ion emitting agent

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Embodiment 1

[0036] The measurement method disclosed in the present invention is mainly composed of three major steps of sample preparation, sample coating and sample measurement, and the three steps are now described in detail.

[0037] (1) Sample preparation: including carbon nanotube suspension preparation, generator solution preparation, and rhenium tape pretreatment, of which:

[0038] Preparation of carbon nanotube suspension: Weigh 0.02g of carbon nanotubes (CNTs) into a 25ml sample bottle, add 10ml of deionized water, and disperse ultrasonically for 15 minutes to form a uniform suspension for use. The tube suspension has not been used for a long time and needs to be ultrasonically dispersed before use.

[0039] The carbon nanotubes used are compound-walled carbon nanotubes with a diameter of 1 nm and a length of 5-15 μm.

[0040] After studying and comparing various solvents, such as ethanol, sucrose solution, acetone, etc., and considering the shedding of carbon nanotubes, the im...

Embodiment 2

[0051] The difference between this embodiment and embodiment 1 is only:

[0052] In step (1) of this embodiment, the carbon nanotubes used are composite-walled carbon nanotubes with a diameter of 9 nm and a length of 5-15 μm; the M / B molar ratio in the preparation of the generator solution is 1.0; During pretreatment: When degassing the double-tape inserts in the burning device, raise the temperature to 2100°C, and the burning time is half an hour. After the burning is completed, cool it to room temperature in a vacuum system, take it out and place it in a desiccator stand-by;

[0053] In step (2) of this embodiment: when one of the rhenium strips of the pretreated double-band insert is made into a sample strip, the process is as follows: one of the rhenium strips is placed on the sample applicator, and the boron sample (boron solution ) 1μL (250ng) was dropped on the center of the strip, and most of the water was dried at 180°C (dried until no visible droplets), then the cur...

Embodiment 3

[0059] The difference between this embodiment and embodiment 1 is only:

[0060] In step (1) of this embodiment, the carbon nanotubes used are composite-walled carbon nanotubes with a diameter of 4 nm and a length of 5-15 μm; the M / B molar ratio in the preparation of the generator solution is 0.75; During pretreatment, the double-tape insert is degassed in the burning device, and the temperature is raised to 2075°C. The burning time is half an hour. After the burning is completed, it is cooled to room temperature in a vacuum system, taken out and placed in a desiccator to wait. use;

[0061] In step (2) of this embodiment: when one of the rhenium strips of the pretreated double-band insert is made into a sample strip, the process is as follows: one of the rhenium strips is placed on the sample applicator, and the boron sample (boron solution ) 1μL (250ng), drop accurately on the center of the belt, dry most of the water at 170°C (dry to no visible droplets), disconnect the cu...

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Abstract

The invention discloses a boron isotope abundance measuring method using a carbon nanotube as an ion emitting agent. The boron isotope abundance measuring method comprises the following steps: (1) preparing a sample: preparing a carbon nanotube suspension, preparing a generating agent solution, and preprocessing rhenium strips; (2) loading the sample: manufacturing one of the rhenium strips of a preprocessed double-strip insert into a sample strip, and loading the sample strip together with an ionization strip onto a sample turnplate for following measurement; and (3) measuring the sample: sending the strip-loaded turnplate into an ion source, starting a spectrometer, heating the sample strip and the ionization strip, and when ion current occurs, starting data collection. By using the carbon nanotube as the ion emitting agent and by optimizing a sample preparing method, a sample loading technology and measuring conditions during use of the carbon nanotube as the ion emitting agent, the boron ion emitting intensity and the ionization efficiency are significantly improved and the stability of an ion flow is also improved to some extent, the measuring accuracy is improved, and the sample loading amount and the measuring temperature are reduced.

Description

technical field [0001] The invention relates to the field of measuring boron isotope abundance, in particular to a method for measuring boron isotope abundance using carbon nanotubes as ion emitters. Background technique [0002] Thermionic ion spectrometry is the most common method for measuring boron isotopic abundance, including positive thermal ionization mass spectrometry and negative thermal ionization mass spectrometry. Negative thermal ionization mass spectrometry is used to measure boron, which has high precision and sensitivity, but due to the detected ion BO 2 - The mass number is small (42 and 43), so the shunt effect and mass discrimination effect are serious, the measurement accuracy is not high, and in the presence of organic impurities such as residual ion exchange resin, mannitol and nitrate, it is easy to produce CNO - Ions (m / z= 42), causing isobaric interference. Positive ion method, M 2 BO 2 + (M alkali metal elements: Na, K, Cs, etc.) The mass o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64G01N1/28
Inventor 李已才梁帮宏张劲松陈云明张舸杜文鹤孙鹏
Owner NUCLEAR POWER INSTITUTE OF CHINA
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