CN102565180A - Method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance - Google Patents
Method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance Download PDFInfo
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- CN102565180A CN102565180A CN201010602468XA CN201010602468A CN102565180A CN 102565180 A CN102565180 A CN 102565180A CN 201010602468X A CN201010602468X A CN 201010602468XA CN 201010602468 A CN201010602468 A CN 201010602468A CN 102565180 A CN102565180 A CN 102565180A
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Abstract
The invention belongs to the field of measurement of molybdenum isotope abundance, and more particularly relates to a method for measuring the negative thermal ionization mass spectrometry of molybdenum isotope abundance. The method comprises the three steps of rhenium strip sample coating, temperature raise measurement and data correction. According to the method disclosed by the invention, a negative thermal ionization mass spectrometry measuring method is adopted, a double-rhenium-strip assembly is used, and a SrCl2 solution is used as a cast charge. The method disclosed by the invention solves the technical problems of large sample coating amount, long measuring time and larger relative standard deviation of a measuring result in the prior art. According to the method disclosed by the invention, all index parameters are relatively balanced, thus the technical effects of smaller sample coating amount, short measuring time and smaller relative standard deviation of the measuring result are achieved; and the method is particularly suitable for measuring requirements of a radioactive sample and a biological sample with low cost.
Description
Technical field
The invention belongs to molybdenum isotope abundance measurement field, be specifically related to the negative thermal ionization mass spectrometry (tims) measuring method of a kind of molybdenum isotope abundance.
Background technology
The atomic number of molybdenum element (Mo) is 42, and 7 stable isotope 92Mo, 94Mo, 95Mo, 96Mo, 97Mo, 98Mo and 100Mo are arranged.Molybdenum is distributed widely in natural molybdenite and meteoritic abundance, and molybdenum also is the necessary micronutrient elements of animals and plants, and the measurement of molybdenum isotope abundance is significant in geology and biological research.Simultaneously, molybdenum isotope is positioned near mass distribution curve first peak value of 235U fission with thermal neutron product, and wherein the 98Mo fission yield is 5.75%, and 98Mo can be used as desirable fuel element burnup measurement monitoring body.When measuring the fuel element burnup, at first measures destroy method the abundance of 98Mo in the fuel element; Calculate the content of 98Mo in the fuel element with isotope dilution mass spectrometry; The anti-then amount of releasing the 235U that fission takes place; Thereby obtain the absolute burnup of fuel element, visible, the measurement of molybdenum isotope abundance also has important researching value in the nuclear fuel element research field.
The thermal ionization mass spectrometry (tims) measuring method of molybdenum has positive thermal ionization mass spectrometry (tims) method and negative thermal ionization mass spectrometry (tims) method, and conventional measurement all is positive thermal ionization mass spectrometry (tims) method, and this method receives the restriction of the high ionization current potential (7.1eV) of molybdenum, and very difficult ionization goes out Mo
+, so Measuring Time is longer, it is bigger to be coated with the appearance amount.
In addition, choosing of cast charge is the key that thermal ionization mass spectrometry (tims) is measured, and existing negative thermal ionization mass spectrometry (tims) method adopts Sr (NO
3)
2And Ca (NO
3)
2As cast charge.Wherein, Sr (NO
3)
2Under the situation as cast charge, Measuring Time is longer; Ca (NO
3)
2Under the situation as cast charge, the relative standard deviation of measurement result is bigger.
Summary of the invention
The technical matters that the present invention solves provides a kind of negative thermal ionization mass spectrometry (tims) measuring method of molybdenum isotope abundance that the appearance amount is little, Measuring Time short and the measurement result relative standard deviation is little that is coated with.
Technical scheme of the present invention is described below:
The present invention includes step 1 rhenium band and be coated with appearance, step 2 intensification measurement and three steps of step 3 correction data.
Wherein, step 1 specifically may further comprise the steps:
Step 1.1 is dripped on the rhenium band silk of the two rhenium band assemblies that comprise sample band and ionization band and is coated with 0.1～1 μ g molybdenum;
Step 1.2 is positioned over two rhenium band assemblies in the vacuum environment, and it is inserted the 5.5A electric current, and continued power 10 minutes adopts and burns belting removal surface impurity and water vapor;
Step 1.3 is taken out two rhenium band assemblies from burn belting, place to be coated with on the sampling device;
Step 1.4 is dripped on the rhenium band silk of two rhenium band assemblies and is coated with 1～2 μ L Na
2MoO
4Solution inserts 1.3A electric current, continued power 60s to two rhenium band assemblies;
Step 1.5 pair two rhenium band assembly outages;
Step 1.6 is dripped on rhenium band silk and is coated with 1 μ L SrCl
2Solution inserts 1.3A electric current, continued power 60s to two rhenium band assemblies;
Step 1.7 at the uniform velocity rises to 1.5A with the said electric current of step 1.6 in 10～15s, and continued power 15s.
Step 2 specifically may further comprise the steps:
Step 2.1 is positioned over the sample rotating disk with two rhenium band assemblies, and the sample rotating disk is positioned in the mass spectrometer ion source;
Step 2.2 pair ion gun vacuumizes processing;
Step 2.3 rises to 2000mA with the ionization band in two rhenium band assemblies with the speed of 450～550mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 230～270mA/min;
Step 2.4 pair ion gun vacuumizes processing;
Step 2.5 keeps the ionization band 2000mA electric current in two rhenium band assemblies, and sample band 1000mA electric current adds 10KV voltage to two rhenium band assemblies;
Step 2.6 keeps two rhenium band assembly 10KV voltages; Ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 150～250mA/min by 2000mA, simultaneously the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 130～170mA/min by 1000mA;
Step 2.7 rises to 2800mA with the speed of 80～120mA/min by 2500mA with the ionization band in two rhenium band assemblies, simultaneously the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 60～100mA/min by 1450mA;
Step 2.8 fine setting sample disk position, the line focusing of going forward side by side;
Ionization belt current in the two rhenium band assemblies of step 2.9 rising makes it be higher than 2800mA, is lower than 2900mA; Sample belt current in the two rhenium band assemblies of rising makes it be higher than 1700mA, is lower than 1770mA.
Step 3 is disturbed through the deduction oxygen isotope measurement data is revised.
As preferred version of the present invention, the vacuum tightness of the vacuum environment described in the step 1.2 is 1 * 10
-4Pa.
As improvement of the present invention, the ion gun vacuum tightness that vacuumizes in step 2.2 and the step 2.4 after the processing is higher than 1 * 10
-6Mbar, preferred value is 5 * 10
-7Mbar.
As further improvement of the present invention, in the step 2.3, the ionization band in two rhenium band assemblies is risen to 2000mA with the speed of 500mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 250mA/min; In the step 2.6, the ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 200mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 150mA/min; Step 2.7 rises to 2800mA with the ionization band in two rhenium band assemblies with the speed of 100mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 80mA/min; Ionization belt current in the step 2.9 in the two rhenium band assemblies of rising is to 2850mA; Sample belt current in the two rhenium band assemblies of rising simultaneously is to 1720mA.
Beneficial effect of the present invention is:
(1) positive thermal ionization mass spectrometry (tims) method needs the appearance amount that is coated with of tens microgram molybdenums, adopts Sr (NO
3)
2Negative thermal ionization mass spectrometry (tims) method as cast charge needs 0.5～1 μ g to be coated with the appearance amount, and method of the present invention only needs 0.1～1 μ g to be coated with the appearance amount, and when being coated with the appearance amount at 0.1 μ g, still can ionization go out the MoO more than the 100mV
3 -Ion flow, the minimizing that is coated with the appearance amount not only can reduce operating personnel's radioactive dose, be beneficial to safety in production, and makes it can be applied to the measurement of the radioactive sample and the biological sample of low content;
(2) the positive needed Measuring Time of thermal ionization mass spectrometry (tims) method is more than 90 minutes, adopts Sr (NO
3)
2The needed Measuring Time of negative thermal ionization mass spectrometry (tims) method as cast charge is 30 minutes, and method Measuring Time of the present invention only needs 20 minutes, has significantly improved work efficiency;
(3) adopt Sr (NO
3)
2As the negative thermal ionization mass spectrometry (tims) method of cast charge, relative standard deviation adopts Ca (NO up to 0.1～0.3%
3)
2As the negative thermal ionization mass spectrometry (tims) method of cast charge, relative standard deviation is up to 0.582～1.348%, and method relative standard deviation of the present invention is merely 0.046～0.171%, has reached higher measuring accuracy.
Embodiment
Describe the present invention through embodiment below.
Embodiment 1
The negative thermal ionization mass spectrometry (tims) measuring method of a kind of molybdenum isotope abundance of the present invention may further comprise the steps: step 1 rhenium band is coated with appearance, step 2 heats up and measures and step 3 correction data.
Step 1 specifically may further comprise the steps:
Step 1.1 is dripped on the rhenium band silk of the two rhenium band assemblies that comprise sample band and ionization band and is coated with molybdenum, is coated with the appearance amount and can be 0.1～1 μ g, is preferably 1 μ g;
Step 1.2 is positioned over two rhenium band assemblies in the vacuum environment, and it is inserted the 5.5A electric current, and continued power 10 minutes adopts and burns belting removal surface impurity and water vapor; The vacuum tightness of above-mentioned vacuum environment is preferably 1 * 10
-6MbarPa;
Step 1.3 is taken out two rhenium band assemblies from burn belting, place to be coated with on the sampling device;
Step 1.4 is dripped on the rhenium band silk of two rhenium band assemblies and is coated with 1～2 μ L Na
2MoO
4Solution inserts 1.3A electric current, continued power 60s to two rhenium band assemblies;
Step 1.5 pair two rhenium band assembly outages;
Step 1.6 is dripped on rhenium band silk and is coated with 1 μ L SrCl
2Solution inserts 1.3A electric current, continued power 60s as cast charge to two rhenium band assemblies;
Step 1.7 at the uniform velocity rises to 1.5A with the said electric current of step 1.6 in 10～15s, and continued power 15s, thoroughly to remove impurity and water vapor.
Step 2 specifically may further comprise the steps:
Step 2.1 is positioned over the sample rotating disk with two rhenium band assemblies, and the sample rotating disk is positioned in the mass spectrometer ion source, and wherein mass spectrometer can adopt Finnigan MAT262 thermal ionization mass spectrometer;
Step 2.2 pair ion gun vacuumizes processing, is higher than 1 * 10 with the ion gun vacuum tightness that vacuumizes after the processing
-6Mbar is a standard;
Step 2.3 is with the speed of the ionization band in two rhenium band assemblies with 450～550mA/min; Be preferably the speed of 500mA/min, rise to 2000mA, simultaneously with the speed of the sample band in two rhenium band assemblies with 230～270mA/min; Be preferably the speed of 250mA/min, rise to 1000mA;
Step 2.4 pair ion gun vacuumizes processing, is higher than 1 * 10 with the ion gun vacuum tightness that vacuumizes after the processing
-6Mbar is a standard;
Step 2.5 keeps the ionization band 2000mA electric current in two rhenium band assemblies, and sample band 1000mA electric current adds 10KV voltage to two rhenium band assemblies;
Step 2.6 keeps two rhenium band assembly 10KV voltages; With the speed of the ionization band in two rhenium band assemblies with 150～250mA/min; Be preferably the speed of 200mA/min, rise to 2500mA, simultaneously with the speed of the sample band in two rhenium band assemblies with 130～170mA/min by 2000mA; Be preferably the speed of 150mA/min, rise to 1450mA by 1000mA;
Step 2.7 is with the speed of the ionization band in two rhenium band assemblies with 80～120mA/min; Be preferably the speed of 100mA/min; Rise to 2800mA by 2500mA; With the speed of the sample band in two rhenium band assemblies, be preferably the speed of 80mA/min simultaneously, rise to 1700mA by 1450mA with 60～100mA/min;
Step 2.8 is finely tuned the sample disk position, the line focusing of going forward side by side so that ion flow is a standard through the mass spectrometer slit as much as possible;
Ionization belt current in the two rhenium band assemblies of step 2.9 rising makes it be higher than 2800mA, is lower than 2900mA, and preferred value is 2850mA; Sample belt current in the two rhenium band assemblies of rising simultaneously makes it be higher than 1700mA, is lower than 1770mA, and preferred value is 1720mA.
Step 3 is disturbed through the deduction oxygen isotope measurement data is revised, and makeover process is a general knowledge as well known to those skilled in the art.
Data shown in the table 1 are the molybdenum isotope abundance ratio measurement data of utilizing method of the present invention to obtain:
Table 1
Annotate:
*R
140/146Refer to tested MoO
3 -Mass number is 140 ion populations and the ratio of the number of ions of mass number 146 in the ionic group, and the rest may be inferred for other ratio.
According to data shown in the table 1, but the relative standard deviation of knowledge capital invention is merely 0.046～0.171%, has reached higher measuring accuracy.
Can obtain molybdenum isotope abundance measurement value by table 1 data.Data shown in the table 2 are to utilize the comparison of the molybdenum isotope abundance measurement value and the abundance reference value of method of the present invention:
Table 2
Shown in table 2 data, molybdenum isotope abundance that method of the present invention is measured and international reference value are coincide, and show that data that the present invention records accurately and reliably.
Table 3 is depicted as the effect comparison of additive method in method of the present invention and the prior art:
Table 3
With respect to the 1st kind of method, the relative standard deviation of the inventive method is bigger, but utilizes negative thermal ionization method to measure MoO
3 -The time, because molybdenum combines to form negative ion easily under the high temperature with oxygen, therefore be coated with appearance amount and Measuring Time and significantly reduce.The minimizing that is coated with the appearance amount not only can reduce operating personnel's radioactive dose, be beneficial to safety in production, and makes it can be applied to the measurement of the radioactive sample and the biological sample of low content; Shorten Measuring Time and greatly improved work efficiency.
With respect to the 2nd kind and the 3rd kind of method, the appearance amount of being coated with and the Measuring Time of the inventive method significantly reduce, and have reached higher measuring accuracy.
With respect to the 4th kind of method, the appearance amount of being coated with of the inventive method is bigger, but relative standard deviation obviously reduces, and measuring accuracy significantly improves.
In sum, each index parameter of method of the present invention is comparatively balanced, especially is fit to the radioactive sample of low content and the measurement requirement of biological sample.
Embodiment 2
The difference of present embodiment and embodiment 1 is:
In step 2.2 and the step 2.4 ion gun being vacuumized processing, is 5 * 10 with the ion gun vacuum tightness that vacuumizes after the processing
-7Mbar.
Claims (9)
1. a molybdenum isotope abundance is born the thermal ionization mass spectrometry (tims) measuring method, may further comprise the steps:
Step 1 rhenium band is coated with appearance;
Step 2 heats up and measures;
Step 3 is revised data.
2. molybdenum isotope abundance according to claim 1 is born the thermal ionization mass spectrometry (tims) measuring method, and it is characterized in that: step 1 specifically may further comprise the steps:
Step 1.1 is dripped on the rhenium band silk of the two rhenium band assemblies that comprise sample band and ionization band and is coated with 0.1～1 μ g molybdenum;
Step 1.2 is positioned over two rhenium band assemblies in the vacuum environment, and it is inserted the 5.5A electric current, and continued power 10 minutes adopts and burns belting removal surface impurity and water vapor;
Step 1.3 is taken out two rhenium band assemblies from burn belting, place to be coated with on the sampling device;
Step 1.4 is dripped on the rhenium band silk of two rhenium band assemblies and is coated with 1～2 μ L Na
2MoO
4Solution inserts 1.3A electric current, continued power 60s to two rhenium band assemblies;
Step 1.5 pair two rhenium band assembly outages;
Step 1.6 is dripped on rhenium band silk and is coated with 1 μ L SrCl
2Solution inserts 1.3A electric current, continued power 60s to two rhenium band assemblies;
Step 1.7 at the uniform velocity rises to 1.5A with the said electric current of step 1.6 in 10～15s, and continued power 15s.
3. molybdenum isotope abundance according to claim 2 is born the thermal ionization mass spectrometry (tims) measuring method, it is characterized in that: the vacuum tightness of the vacuum environment described in the step 1.2 is 1 * 10
-4Pa.
4. molybdenum isotope abundance according to claim 1 and 2 is born the thermal ionization mass spectrometry (tims) measuring method, and it is characterized in that: step 2 specifically may further comprise the steps:
Step 2.1 is positioned over the sample rotating disk with two rhenium band assemblies, and the sample rotating disk is positioned in the mass spectrometer ion source;
Step 2.2 pair ion gun vacuumizes processing;
Step 2.3 rises to 2000mA with the ionization band in two rhenium band assemblies with the speed of 450～550mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 230～270mA/min;
Step 2.4 pair ion gun vacuumizes processing;
Step 2.5 keeps the ionization band 2000mA electric current in two rhenium band assemblies, and sample band 1000mA electric current adds 10KV voltage to two rhenium band assemblies;
Step 2.6 keeps two rhenium band assembly 10KV voltages; Ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 150～250mA/min by 2000mA, simultaneously the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 130～170mA/min by 1000mA;
Step 2.7 rises to 2800mA with the speed of 80～120mA/min by 2500mA with the ionization band in two rhenium band assemblies, simultaneously the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 60～100mA/min by 1450mA;
Step 2.8 fine setting sample disk position, the line focusing of going forward side by side;
Ionization belt current in the two rhenium band assemblies of step 2.9 rising makes it be higher than 2800mA, is lower than 2900mA; Sample belt current in the two rhenium band assemblies of rising makes it be higher than 1700mA, is lower than 1770mA.
5. molybdenum isotope abundance according to claim 4 is born the thermal ionization mass spectrometry (tims) measuring method, it is characterized in that: the ion gun vacuum tightness that vacuumizes in step 2.2 and the step 2.4 after the processing is higher than 1 * 10
-6Mbar.
6. molybdenum isotope abundance according to claim 5 is born the thermal ionization mass spectrometry (tims) measuring method, it is characterized in that: the ion gun vacuum tightness that vacuumizes in step 2.2 and the step 2.4 after the processing is 5 * 10
-7Mbar.
7. molybdenum isotope abundance according to claim 4 is born the thermal ionization mass spectrometry (tims) measuring method; It is characterized in that: in the step 2.3; Ionization band in two rhenium band assemblies is risen to 2000mA with the speed of 500mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 250mA/min; In the step 2.6, the ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 200mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 150mA/min; Step 2.7 rises to 2800mA with the ionization band in two rhenium band assemblies with the speed of 100mA/min, simultaneously the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 80mA/min.
8. molybdenum isotope abundance according to claim 4 is born the thermal ionization mass spectrometry (tims) measuring method, it is characterized in that: the ionization belt current in two rhenium band assemblies that raise in the step 2.9 is to 2850mA; Sample belt current in the two rhenium band assemblies of rising is to 1720mA.
9. molybdenum isotope abundance according to claim 1 is born the thermal ionization mass spectrometry (tims) measuring method, it is characterized in that: step 3 is disturbed through the deduction oxygen isotope measurement data is revised.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983685A (en) * | 2014-05-30 | 2014-08-13 | 中国地质科学院水文地质环境地质研究所 | Low-temperature conversion and determination method of chlorine isotopes in chloro herbicide |
| CN106198705A (en) * | 2016-06-27 | 2016-12-07 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as high sensitivity cast charge |
| CN110940721A (en) * | 2019-12-20 | 2020-03-31 | 内蒙古通威高纯晶硅有限公司 | Method for measuring metal impurities on surface of crushing tool |
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| US4075312A (en) * | 1977-06-06 | 1978-02-21 | The United States Of America As Represented By The United States Department Of Energy | Process for recovering evolved hydrogen enriched with at least one heavy hydrogen isotope |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983685A (en) * | 2014-05-30 | 2014-08-13 | 中国地质科学院水文地质环境地质研究所 | Low-temperature conversion and determination method of chlorine isotopes in chloro herbicide |
| CN103983685B (en) * | 2014-05-30 | 2016-04-27 | 中国地质科学院水文地质环境地质研究所 | The low temperature conversion of chlorine isotope and assay method in a kind of chloro herbicide |
| CN106198705A (en) * | 2016-06-27 | 2016-12-07 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as high sensitivity cast charge |
| CN106198705B (en) * | 2016-06-27 | 2018-12-21 | 中国科学院地质与地球物理研究所 | Niobium pentaoxide is used for micro-example chromium isotope measuring technology as highly sensitive cast charge |
| CN110940721A (en) * | 2019-12-20 | 2020-03-31 | 内蒙古通威高纯晶硅有限公司 | Method for measuring metal impurities on surface of crushing tool |
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| CN102565180B (en) | 2014-04-30 |
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