CN103487497A - Boron isotope abundance measuring method using carbon nanotube as ion emitting agent - Google Patents
Boron isotope abundance measuring method using carbon nanotube as ion emitting agent Download PDFInfo
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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
The present invention relates to the fields of measurement of boron isotope abundance, specifically refer to a kind of boron isotope abundance measuring method of carbon nano-tube as the emission of ions agent of usining.
Background technology
The thermoelectricity ionography is to measure the most popular method of boron isotope abundance, comprises the positive thermal ionization mass spectroscopy and negative thermal ionization mass spectrometry method.The negative thermal ionization mass spectrometry method is surveyed boron, precision and highly sensitive, but due to tested ion BO
2 -mass number little (42 and 43), thus shunt effect and mass discrimination comparatively serious, accuracy of measurement is not high, and under the existence as residual ion exchange resin, sweet mellow wine and nitrate radical, is easy to produce CNO at organic impurities
-ion (m/z=42), cause isobaric interference.The positive ion method, M
2bO
2 +(M alkali metal: Na, K, Cs etc.) mass of ion obviously increases, although can reduce shunting and mass discrimination, the positive ion ionizing efficiency is not high, generally is coated with the sample amount in the microgram magnitude, and nanogram magnitude sample high-acruracy survey is difficulty comparatively.
Therefore, also there is no a kind of method of measuring this precision boron istope at present.
Summary of the invention
The object of the present invention is to provide a kind of boron isotope abundance measuring method, the emission of ions agent that the method adopts carbon nano-tube to measure as boron isotope abundance, to improve the emission of ions performance of thermal ionization mass spectrometry (tims) measurement Determination of Trace Boron sample; And the method for making sample while by optimization, using carbon nano-tube as the emission of ions agent, be coated with sample technology, measuring condition, set up a kind of method of measuring the high precision boron isotope abundance.
Purpose of the present invention is achieved through the following technical solutions: a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent, comprise the following steps:
(1) sample preparation: comprise the carbon nanotube suspension preparation, generate agent solution preparation, the pre-service of rhenium band, wherein:
carbon nanotube suspension preparation: take carbon nano-tube and be placed in sample bottle, add deionized water, form uniform suspension stand-by after disperseing;
Generation agent solution preparation: by alkali metal salt M
2cO
3after dissolving with distilled water, the dilution constant volume;
The pre-service of rhenium band: the biobelt plug-in unit of rhenium band is placed in and burns degasification in belting, with remove with on moisture content and impurity, after burning and be with, be cooled to room temperature in vacuum system, taking-up is positioned in exsiccator stand-by;
(2) be coated with sample: a wherein rhenium band of pretreated biobelt plug-in unit is made to the sample band, process is as follows: wherein a rhenium band is placed in and is coated with on the sample device, get the boron sample drop in band central authorities, after large water gaging is removed in baking, get the generation agent solution, cover on the boron sample, after large water gaging is removed in baking, get again the CNTs suspension and be coated on sample, dry, make the sample band; An other rhenium band in the biobelt plug-in unit, as the ionization band, takes off it after the sample band is down to room temperature, by the sample band, together with the ionization band, installs on the sample rotating disk to be measured; :
(3) sample measurement: the rotating disk that will install band is sent in ion gun, opens mass spectrometer, and sample band and ionization band are carried out to hyperthermic treatment, when ion current occurring, starts data acquisition.
The temperature of above-mentioned sample rhenium band and ionization rhenium band rises all by its turn-on current, by self-heating, realizes, the amplitude that its temperature raises and speed all realize by controlling the size of current of passing through.
In described step (1):
the ultrasonic dispersion used in the carbon nanotube suspension preparation, and ultrasonic jitter time is at least 15 minutes; In used time not for a long time, need to carry out again ultrasonic dispersion as the CNTs suspension of preparation before use.
The deionization resistivity of water > 18M Ω .cm.
The carbon nano-tube specification is the composite carbon nano-tube, and diameter is less than 10nm.
In rhenium band preprocessing process, adopt the energising heating while burning band, the electric current rising, the vacuum tightness of burning belting is not less than 5 * 10
-3pa, be warming up to 2050 ℃-2100 ℃, and burning the band time is half an hour.
While generating the agent preparation, the M/B mol ratio is 0.5-1.0.
In described step (2):
Dry and adopt the energising heating, getting the boron sample drop carries out in 160 ℃ of-180 ℃ of temperature in the Postcentral oven dry of sample band, turn-off current, oven dry after covering on the boron sample by the generation agent solution is carried out in 190 ℃ of-210 ℃ of temperature, oven dry after being coated on sample by the CNTs suspension is first dried and is gone most of moisture in 190 ℃ of-210 ℃ of temperature, then be down to 160 ℃ of-180 ℃ of oven dry, after drying, keep 30s.
When getting the CNTs suspension and being coated on sample, must apply fully.
In described step (3):
Use the electric current automatic heating during to sample band and the hyperthermic treatment of ionization band, 240 ℃-260 ℃, default sample band, ionization is with 1150 ℃-1250 ℃, and heating rate is: 80-100 ℃/min of sample band, 350-400 ℃/min of ionization band.
When ion current occurring, regulate disk position, ion lens system and band temperature, make ion current signal intensity maximum, signal is the most steady, after stablizing 3～5min, starts data acquisition.
In sum, advantage of the present invention is as follows:
(1) improve boron sample ions emitting performance: after having adopted carbon nano-tube as the emission of ions agent, boron emission of ions intensity obviously improves, and ionizing efficiency improves nearly 3 times, and ion current stability also makes moderate progress.
(2) improve measuring accuracy:
10b/
11the relative standard is in 0.1% for the B isotopic abundance ratio.
(3) reduce and be coated with the sample amount: the painting sample amount of this method only needs the nanogram level, can realize high precision, measure the boron isotope abundance value exactly, has effectively reduced painting sample amount.
(4) reduce probe temperature: the carbon nano-tube of usining can significantly reduce the probe temperature of boron sample as cast charge, can reduce the be heated too fast volatilization and suppress shunt effect of boron sample, makes the sample measurement result more accurate.
The accompanying drawing explanation
Fig. 1 using carbon nano-tube during as cast charge on the schematic diagram that affects of boron sample ions intensity of flow and stability;
The carbon nano-tube of Fig. 2 different size is as cast charge pair
89(M
2bO
2 +) ion current intensity effect schematic diagram.
Wherein: the specification of carbon nano-tube described in figure is:
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited only to this.
Measuring method disclosed by the invention mainly consists of sample preparation, painting sample and the large step of sample measurement three, now for three steps, is described in detail respectively.
(1) sample preparation: comprise the carbon nanotube suspension preparation, generate agent solution preparation, the pre-service of rhenium band, wherein:
The carbon nanotube suspension preparation: the carbon nano-tube (CNTs) that takes 0.02g is placed in the 25ml sample bottle, add the 10ml deionized water, it is stand-by that ultrasonic dispersion forms uniform suspension in 15 minutes, if the carbon nanotube suspension of preparation use not for a long time needs to carry out ultrasonic dispersion before use again.
The carbon nano-tube of using is the composite carbon nano-tube, and its diameter is 1nm, and length is 5-15 μ m.
Through research and comparison multi-solvents, as ethanol, sucrose solution, acetone etc., and consider the dropping situations of carbon nano-tube, on after the impact of vacuum system and the impact on test result, the present invention selects resistivity > deionized water of 18M Ω .cm is as the dispersion solvent of carbon nano-tube.
Generation agent solution preparation: by alkali metal salt M
2cO
3, as Na
2cO
3, K
2cO
3, Cs
2cO
3deng, after dissolving with distilled water, the dilution constant volume, its concentration is according to the preparation of boron sample concentration, M/B mol ratio 0.5.
The pre-service of rhenium band: rhenium-rhenium biobelt plug-in unit size is selected 0.04 * 0.7 * 18mm; By the degasification in burning belting of biobelt plug-in unit, with remove with on moisture content and impurity, burn belting and can use at present common on the market burning belting get final product, turn-on current, electric current rising in burning band process, and make the vacuum tightness of burning belting be not less than 5 * 10
-3pa, make temperature rise to 2050 ℃, and burning the band time is half an hour, and burning is cooled to room temperature after being with in vacuum system, and taking-up is positioned in exsiccator stand-by;
(2) be coated with sample:
A wherein rhenium band of pretreated biobelt plug-in unit is made to the sample band, sample rhenium band is for the evaporitic environment of sampling, process is as follows: wherein a rhenium band is placed in and is coated with on the sample device, getting boron sample (B solution) 1 μ L (250ng) drips in band central authorities, after in 160 ℃ of temperature, most water (drying to the visible drop of nothing) is removed in baking, turn-off current, get the generation agent M of 1 μ L
2cO
3solution, cover on the boron sample, galvanization, in 190 ℃ of temperature, dry remove most water after to without visible drop, turn-off current, get again 1 μ L CNTs suspension and be coated on sample, cover fully, first in 190 ℃ of temperature, dry and go most of moisture, then be down to 160 ℃ of oven dry, keep 30s after drying, turn-off current, make the sample band;
An other rhenium band in the biobelt plug-in unit, as the ionization band, takes off it after the sample band is down to room temperature, by the sample band, together with the ionization band, installs on the sample rotating disk to be measured;
(3) sample measurement:
The rotating disk that installs band is sent in ion gun, is opened mass spectrometer, until system vacuum reach laboratory to the instrumentation requirement after, carry out baseline correction and Faraday cup adjustment.Afterwards, the sample band and the ionization belt current that the carbon nano-tube obtained through above-mentioned steps are coated with to sample boron sample carry out hyperthermic treatment, and automatic heating is preset as 240 ℃, sample band, and ionization is with 1150 ℃, and heating rate is: 80 ℃/min of sample band, and 350 ℃/min is with in ionization;
When ion current occurring, regulate disk position, ion lens system and band temperature, make ion current signal intensity maximum, signal is the most steady, after stablizing 3min, can start data acquisition.
The temperature of above-mentioned sample rhenium band and ionization rhenium band rises all by its turn-on current, by self-heating, realizes, the amplitude that its temperature raises and speed all realize by controlling the size of current of passing through.
embodiment 2:
The difference of the present embodiment and embodiment 1 only is:
In the step of the present embodiment (1), the carbon nano-tube of using is the composite carbon nano-tube, and its diameter is 9nm, and length is 5-15 μ m; Generating M/B mol ratio in the agent solution preparation is 1.0; During the pre-service of rhenium band: in burning belting, during degasification, make temperature rise to 2100 ℃ the biobelt plug-in unit, burning the band time is half an hour, after burning and be with, is cooled to room temperature in vacuum system, and taking-up is positioned in exsiccator stand-by;
In the step of the present embodiment (2): by pretreated biobelt plug-in unit wherein a rhenium band is made the sample band time, process is as follows: wherein a rhenium band is placed in and is coated with on the sample device, getting boron sample (B solution) 1 μ L (250ng) drips in band central authorities, after in 180 ℃ of temperature, most water (drying to the visible drop of nothing) is removed in baking, turn-off current, get the generation agent M of 1 μ L
2cO
3solution, cover on the boron sample, galvanization, in 210 ℃ of temperature, dry remove most water after to without visible drop, turn-off current, get again 1 μ L CNTs suspension and be coated on sample, cover fully, first in 210 ℃ of temperature, dry and go most of moisture, then be down to 180 ℃ of oven dry, keep 30s after drying, turn-off current, make the sample band;
In the step of the present embodiment (3):
The rotating disk that installs band is sent in ion gun, is opened mass spectrometer, until system vacuum reach laboratory to the instrumentation requirement after, carry out baseline correction and Faraday cup adjustment.Afterwards, the sample band and the ionization belt current that the carbon nano-tube obtained through above-mentioned steps are coated with to sample boron sample carry out hyperthermic treatment, and automatic heating is preset as 260 ℃, sample band, and ionization is with 1250 ℃, heating rate is: 100 ℃/min of sample band, and 400 ℃/min is with in ionization;
When ion current occurring, regulate disk position, ion lens system and band temperature, make ion current signal intensity maximum, signal is the most steady, after stablizing 5min, can start data acquisition.
Other parts of the present embodiment are identical with embodiment 1, repeat no more.
embodiment 3:
The difference of the present embodiment and embodiment 1 only is:
In the step of the present embodiment (1), the carbon nano-tube of using is the composite carbon nano-tube, and its diameter is 4nm, and length is 5-15 μ m; Generating M/B mol ratio in the agent solution preparation is 0.75; During the pre-service of rhenium band, by the degasification in burning belting of biobelt plug-in unit, make temperature rise to 2075 ℃, burning the band time is half an hour, after burning and be with, is cooled to room temperature in vacuum system, and taking-up is positioned in exsiccator stand-by;
In the step of the present embodiment (2): by pretreated biobelt plug-in unit wherein a rhenium band is made the sample band time, process is as follows: wherein a rhenium band is placed in and is coated with on the sample device, get boron sample (B solution) 1 μ L (250ng), accurately drip in band central authorities, after in 170 ℃ of temperature, most water (drying to the visible drop of nothing) is removed in baking, turn-off current, get the generation agent M of 1 μ L
2cO
3solution, cover on the boron sample, galvanization, in 200 ℃ of temperature, dry remove most water after to without visible drop, turn-off current, get again 1 μ L CNTs suspension and be coated on sample, cover fully, first in 200 ℃ of temperature, dry and go most of moisture, then be down to 170 ℃ of oven dry, keep 30s after drying, turn-off current, make the sample band;
In the step of the present embodiment (3):
The rotating disk that installs band is sent in ion gun, is opened mass spectrometer, until system vacuum reach laboratory to the instrumentation requirement after, carry out baseline correction and Faraday cup adjustment.Afterwards, the sample band and the ionization belt current that the carbon nano-tube obtained through above-mentioned steps are coated with to sample boron sample carry out hyperthermic treatment, and automatic heating is preset as 250 ℃, sample band, and ionization is with 1200 ℃, and heating rate is: 90 ℃/min of sample band, and 375 ℃/min is with in ionization;
When ion current occurring, regulate disk position, ion lens system and band temperature, make ion current signal intensity maximum, signal is the most steady, after stablizing 4min, can start data acquisition.
Other parts of the present embodiment are identical with embodiment 1, repeat no more.
Useful technique effect of the present invention is embodied in the following aspects:
(1) the present invention adopts carbon nano-tube as the emission of ions agent first in the positive thermal ionization mass spectroscopy of boron is measured, and has greatly improved boron sample ions emitting performance, has reduced probe temperature.
Strong and stable ion current is that thermal ionization mass spectrometry (tims) is accurate, the assurance of high-acruracy survey, boron sample positive ion ionizing efficiency is not high separately, and very responsive to measuring temperature, the slightly high sample volatilization of temperature is very fast, nanogram magnitude sample is easy to exhaust, and affected by shunt effect, be difficult for Measurement accuracy.
M in the present invention
2bO
2 +on the rhenium band, production process is shown below:
H
3BO
3+M
2CO
3→M
2B
4O
7→M
2BO
2 ++B
3O
5 -
In the use carbon nano-tube is carried out the boron isotope abundance testing process of the positive thermal ionization mass spectroscopy as the emission of ions agent, carbon nano-tube is different from uranium for the mechanism of action of boron sample, the reducing metals such as neodymium: carbon nano-tube (Carbon nanotubes, CNTs) be a kind of carbon materials with special crystalline structure, be different from traditional crystal formation carbon materials graphite and adamantine two-dimensional structure and three-dimensional structure, carbon nano-tube has unique 1-dimention nano tubulose micromechanism, large specific surface area, abundant gap structure and good many characteristics such as electric conductivity, in using the method for carbon nano-tube as the emission of ions agent, the volatilization of being heated of boron sample molecule, through carbon nanotube layer the time, intercepted, played the effect of slowly-releasing, make the ion current emission more steady.In addition, carbon nano-tube covers sample surfaces, when slowing down the sample volatilization, sample molecule thermal motion path is restricted, and volatility range is more concentrated, has improved the utilization ratio of sample, thereby ion current intensity is obviously improved.
The existence of carbon nano-tube has improved M
2bO
2 +ion yield, reduce probe temperature, suppresses shunt effect, improves the utilization factor of boron sample, thereby can reduce the requirement that sample is coated with to the sample amount, and the sample of nanogram magnitude can Measurement accuracy.As seen from Figure 1, use the method for carbon nano-tube as the emission of ions agent in the present invention, boron emission of ions intensity obviously improves, and ionizing efficiency improves nearly 3 times, and ion current stability also makes moderate progress.
In addition, the specification of carbon nano-tube is to M
2bO
2 +emission of ions effect and the impact of measurement result be there are differences, as shown in Figure 2, in method provided by the invention, used CNTs-3 type carbon nano-tube can obtain effect preferably.
(2) improve measuring accuracy:
Adopt the boron sample of traditional positive ion method measurement nanogram magnitude as stated in the Background Art comparatively difficult, enable to measure data,
10b/
11b isotopic abundance ratio relative standard deviation is generally in 0.5% left and right, and uses measuring method provided by the present invention,
10b/
11the relative standard is in 0.1% the B isotopic abundance ratio, following table listed the classic method used as stated in the Background Art and this method the boron sample measurement result relatively.
The boron sample of classic method and this method
10b and
11b abundance ratio measurement result (n=30)
N means the number of times of one group of sample measurement image data, calculates the data amount check of relative standard deviation.
(3) reduce the sample amount that is coated with:
Traditional the positive thermal ionization method is measured boron sample isotopic abundance, is coated with the sample amount and need to reaches microgram magnitude (several microgram), and for radioactive sample, reducing painting sample amount is also the key of minimizing personnel radioactive dose; In addition, if in testing sample, boron concentration is very low, as environmental sample, need concentrated sample preparation before mass-spectrometer measurement, process is loaded down with trivial details, in operating process, also easily introduces and disturbs, and affects measurement result accuracy.
This method, by the selection of emission of ions agent, the optimization of painting quadrat method (comprise and be coated with sample program, bake out temperature, heat time heating time etc.), is coated with the sample amount and only needs the nanogram level, can realize high precision, measure the boron isotope abundance value accurately, has effectively reduced painting sample amount.
(4) reduce volatilization and the loss of boron sample, further improve measuring accuracy:
The boron sample is very responsive to temperature, volatile loss, therefore be coated with sample bake out temperature and time control, and intensification measuring process (comprising the choosing of preset temperature, heating rate, finishing temperature, stand-by period etc.) is very important, method provided by the invention can be in the situation that dry moisture in sample, reduce B volatilization loss, also just further improved measuring accuracy.
Claims (10)
1. using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent for one kind, it is characterized in that: comprise the following steps:
(1) sample preparation: comprise the carbon nanotube suspension preparation, generate agent solution preparation, the pre-service of rhenium band, wherein:
Carbon nanotube suspension preparation: take carbon nano-tube CNTs and be placed in sample bottle, add deionized water, form uniform CNTs suspension stand-by after disperseing;
Generation agent solution preparation: by alkali metal salt M
2cO
3after dissolving with distilled water, the dilution constant volume;
The pre-service of rhenium band: rhenium band biobelt plug-in unit is placed in and burns degasification in belting, with remove with on moisture content and impurity, after burning and be with, be cooled to room temperature in vacuum system, taking-up is positioned in exsiccator stand-by;
(2) be coated with sample: a wherein rhenium band of pretreated biobelt plug-in unit is placed in and is coated with on the sample device, get the boron sample drop in band central authorities, after large water gaging is removed in baking, get the generation agent solution, cover on the boron sample, after large water gaging is removed in baking, get again the CNTs suspension and be coated on sample, dry, make the sample band, then take off after the sample band is down to room temperature, install on the sample rotating disk to be measured together with another rhenium band of being with as ionization in pretreated biobelt plug-in unit; :
(3) sample measurement: the rotating disk that will install band is sent in ion gun, opens mass spectrometer, and sample band and ionization band are carried out to hyperthermic treatment, when ion current occurring, starts data acquisition.
2. a kind of boron isotope abundance measuring method of carbon nano-tube as the emission of ions agent of usining according to claim 1, it is characterized in that: in described step (1), the ultrasonic dispersion used in the carbon nanotube suspension preparation, and ultrasonic jitter time is at least 15 minutes; In used time not for a long time, need to carry out again ultrasonic dispersion as the CNTs suspension of preparation before use.
3. according to claim 1ly a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent, it is characterized in that: in described step (1), the deionization resistivity of water > 18M Ω .cm.
4. a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent according to claim 1 or 3 is described, it is characterized in that: in described step (1), carbon nano-tube is the composite carbon nano-tube, and diameter is less than 10nm.
5. a kind of boron isotope abundance measuring method of carbon nano-tube as the emission of ions agent of usining according to claim 1, it is characterized in that: in described step (1), in rhenium band preprocessing process, adopt the energising heating while burning band, the electric current rising, the vacuum tightness of burning belting is not less than 5 * 10
-3pa, be warming up to 2050 ℃-2100 ℃, and burning the band time is half an hour.
6. according to claim 1ly a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent, it is characterized in that: in described step (1), while generating the agent preparation, the M/B mol ratio is 0.5-1.0.
7. a kind of boron isotope abundance measuring method of carbon nano-tube as the emission of ions agent of usining according to claim 1, it is characterized in that: in described step (2), dry and adopt the energising heating, getting the boron sample drop carries out in 160 ℃ of-180 ℃ of temperature in the Postcentral oven dry of sample band, turn-off current, oven dry after covering on the boron sample by the generation agent solution is carried out in 190 ℃ of-210 ℃ of temperature, oven dry after being coated on sample by the CNTs suspension is first dried and is gone most of moisture in 190 ℃ of-210 ℃ of temperature, then be down to 160 ℃ of-180 ℃ of oven dry, keep 30s after drying.
8. according to claim 1ly a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent, it is characterized in that: in described step (2), must apply fully when getting the CNTs suspension and being coated on sample.
9. a kind of boron isotope abundance measuring method of carbon nano-tube as the emission of ions agent of usining according to claim 1, it is characterized in that: in described step (3), use the electric current automatic heating during to sample band and the hyperthermic treatment of ionization band, 240 ℃-260 ℃, default sample band, ionization is with 1150 ℃-1250 ℃, heating rate is: 80-100 ℃/min of sample band, 350-400 ℃/min of ionization band.
10. according to claim 1ly a kind ofly using carbon nano-tube as the boron isotope abundance measuring method of emission of ions agent, it is characterized in that: in described step (3), when ion current occurring, make ion current signal intensity maximum, signal is the most steady, after stablizing 3～5min, starts data acquisition.
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