CN102565180B - 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 PDF

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CN102565180B
CN102565180B CN201010602468.XA CN201010602468A CN102565180B CN 102565180 B CN102565180 B CN 102565180B CN 201010602468 A CN201010602468 A CN 201010602468A CN 102565180 B CN102565180 B CN 102565180B
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rhenium
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CN102565180A (en
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梁帮宏
张劲松
邓辉
杨彬
张舸
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Nuclear Power Institute of China
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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

A kind of method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance
Technical field
The invention belongs to molybdenum isotope abundance measurement field, be specifically related to a kind of method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance.
Background technology
The atomic number of molybdenum element (Mo) is 42, has 7 stable isotope 92Mo, 94Mo, 95Mo, 96Mo, 97Mo, 98Mo and 100Mo.Molybdenum is distributed widely in natural molybdenite and meteoritic abundance, and molybdenum is also the necessary micronutrient elements of animals and plants, and the measurement of molybdenum isotope abundance is significant in geology and biological research.Meanwhile, molybdenum isotope is positioned near mass distribution curve first peak value of 235U fission with thermal neutron product, and wherein 98Mo fission yield is that 5.75%, 98Mo can be used as desirable fuel element burnup measurement monitoring body.When measuring fuel element burnup, first measures destroy method the abundance of 98Mo in fuel element, with isotope dilution mass spectrometry, calculate the content of 98Mo in fuel element, then there is the amount of the 235U of fission in anti-release, thereby obtain the absolute burnup of fuel element, visible, the measurement of molybdenum isotope abundance also has important researching value in nuclear fuel element research field.
The thermal ionization mass spectrometry (tims) measuring method of molybdenum has the positive thermal ionization mass spectroscopy and negative thermal ionization mass spectrometry method, and traditional measuring method is all the positive thermal ionization mass spectroscopy, and the method is subject to the restriction of the high ionization current potential (7.1eV) of molybdenum, the very difficult Mo that ionizes out +, so Measuring Time is longer, is coated with sample amount larger.
In addition, choosing of cast charge is the key that thermal ionization mass spectrometry (tims) is measured, and existing negative thermal ionization mass spectrometry method adopts Sr (NO 3) 2and Ca (NO 3) 2as cast charge.Wherein, Sr (NO 3) 2in situation as cast charge, Measuring Time is longer; Ca (NO 3) 2in situation as cast charge, the relative standard deviation of measurement result is larger.
Summary of the invention
The technical matters that the present invention solves is to provide a kind of method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance that sample amount is little, Measuring Time is short and measurement result relative standard deviation is little that is coated with.
Technical scheme of the present invention is as described below:
The present invention includes step 1 rhenium band and be coated with sample, step 2 intensification measurement and three steps of step 3 correction data.
Wherein, step 1 specifically comprises the following steps:
Step 1.1 is dripped and is coated with 0.1～1 μ g molybdenum on the rhenium band silk of two rhenium band assemblies that comprises sample band and ionization band;
Step 1.2 is positioned over two rhenium band assemblies in vacuum environment, and to its access 5.5A electric current, continued power 10 minutes, adopts and burn belting removal surface impurity and water vapor;
Step 1.3 is taken out two rhenium band assemblies from burn belting, is placed in and is coated with on sampling device;
Step 1.4 is dripped and is coated with 1～2 μ L Na on the rhenium band silk of two rhenium band assemblies 2moO 4solution, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.5 pair two rhenium band assembly power-off;
Step 1.6 is dripped and is coated with 1 μ L SrCl on rhenium band silk 2solution, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.7 at the uniform velocity rises to 1.5A by electric current described in step 1.6 in 10～15s, and continued power 15s.
Step 2 specifically comprises the following steps:
Step 2.1 is positioned over sample rotating disk by two rhenium band assemblies, and sample rotating disk is positioned in mass spectrometer ion source;
Step 2.2 pair ion gun vacuumizes processing;
Step 2.3 rises to 2000mA by the ionization band in two rhenium band assemblies with the speed of 450～550mA/min, the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 230～270mA/min simultaneously;
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 voltage, ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 150～250mA/min by 2000mA, the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 130～170mA/min by 1000mA simultaneously;
Step 2.7 rises to 2800mA with the speed of 80～120mA/min by 2500mA by the ionization band in two rhenium band assemblies, the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 60～100mA/min by 1450mA simultaneously;
Step 2.8 micro-regulation 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 higher than 2800mA, lower than 2900mA; The sample belt current raising in two rhenium band assemblies, makes it higher than 1700mA, lower than 1770mA.
Step 3 is disturbed measurement data is revised by deduction oxygen isotope.
As preferred version of the present invention, the vacuum tightness of the vacuum environment described in step 1.2 is 1 * 10 -4pa.
As improvement of the present invention, in step 2.2 and step 2.4, vacuumize ion gun vacuum tightness after processing higher than 1 * 10 -6mbar, preferred value is 5 * 10 -7mbar.
As a further improvement on the present invention, in step 2.3, the ionization band in two rhenium band assemblies is risen to 2000mA with the speed of 500mA/min, the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 250mA/min simultaneously; In step 2.6, the ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 200mA/min, the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 150mA/min simultaneously; Step 2.7 rises to 2800mA by the ionization band in two rhenium band assemblies with the speed of 100mA/min, the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 80mA/min simultaneously; The ionization belt current raising in step 2.9 in two rhenium band assemblies is to 2850mA; The sample belt current simultaneously raising in two rhenium band assemblies is to 1720mA.
Beneficial effect of the present invention is:
(1) the positive thermal ionization mass spectroscopy needs the painting sample amount of tens microgram molybdenums, adopts Sr (NO 3) 2negative thermal ionization mass spectrometry method as cast charge needs 0.5～1 μ g to be coated with sample amount, and method of the present invention only needs 0.1～1 μ g to be coated with sample amount, and still can ionize out MoO more than 100mV when being coated with sample amount at 0.1 μ g 3 -ion current, the minimizing that is coated with sample amount not only can reduce operating personnel's radioactive dose, be beneficial to safety in production, and can be applied to the measurement of radioactive sample and the biological sample of low content;
(2) the needed Measuring Time of the positive thermal ionization mass spectroscopy is more than 90 minutes, adopts Sr (NO 3) 2the needed Measuring Time of negative thermal ionization mass spectrometry 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 method of cast charge, relative standard deviation, up to 0.1～0.3%, adopts Ca (NO 3) 2as the negative thermal ionization mass spectrometry method of cast charge, relative standard deviation is up to 0.582～1.348%, and method relative standard deviation of the present invention is only 0.046～0.171%, has reached higher measuring accuracy.
Embodiment
Below by embodiment, describe the present invention.
Embodiment 1
A kind of method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance of the present invention comprises the following steps: step 1 rhenium band is coated with sample, step 2 heats up and measures and step 3 correction data.
Step 1 specifically comprises the following steps:
Step 1.1 is dripped and is coated with molybdenum on the rhenium band silk of two rhenium band assemblies that comprises sample band and ionization band, and being coated with sample amount can be 0.1～1 μ g, is preferably 1 μ g;
Step 1.2 is positioned over two rhenium band assemblies in vacuum environment, and to its access 5.5A electric current, continued power 10 minutes, adopts and burn 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, is placed in and is coated with on sampling device;
Step 1.4 is dripped and is coated with 1～2 μ L Na on the rhenium band silk of two rhenium band assemblies 2moO 4solution, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.5 pair two rhenium band assembly power-off;
Step 1.6 is dripped and is coated with 1 μ L SrCl on rhenium band silk 2solution is as cast charge, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.7 at the uniform velocity rises to 1.5A by electric current described in step 1.6 in 10～15s, and continued power 15s, thoroughly to remove impurity and water vapor.
Step 2 specifically comprises the following steps:
Step 2.1 is positioned over sample rotating disk by two rhenium band assemblies, and sample rotating disk is positioned in mass spectrometer ion source, and wherein mass spectrometer can adopt Finnigan MAT262 thermal ionization mass spectrometer;
Step 2.2 pair ion gun vacuumizes processing, to vacuumize ion gun vacuum tightness after processing higher than 1 * 10 -6mbar is standard;
Step 2.3 is the speed with 450～550mA/min by the ionization band in two rhenium band assemblies, the speed that is preferably 500mA/min, rises to 2000mA, simultaneously the speed with 230～270mA/min by the sample band in two rhenium band assemblies, the speed that is preferably 250mA/min, rises to 1000mA;
Step 2.4 pair ion gun vacuumizes processing, to vacuumize ion gun vacuum tightness after processing higher than 1 * 10 -6mbar is 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 voltage, speed by the ionization band in two rhenium band assemblies with 150～250mA/min, be preferably the speed of 200mA/min, by 2000mA, rise to 2500mA, the speed with 130～170mA/min by the sample band in two rhenium band assemblies simultaneously, the speed that is preferably 150mA/min, rises to 1450mA by 1000mA;
Step 2.7 is the speed with 80～120mA/min by the ionization band in two rhenium band assemblies, be preferably the speed of 100mA/min, by 2500mA, rise to 2800mA, the speed with 60～100mA/min by the sample band in two rhenium band assemblies simultaneously, the speed that is preferably 80mA/min, rises to 1700mA by 1450mA;
Step 2.8 is so that ion current is standard by mass spectrometer slit as much as possible, micro-regulation 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 higher than 2800mA, lower than 2900mA, and preferred value is 2850mA; The sample belt current simultaneously raising in two rhenium band assemblies, makes it higher than 1700mA, lower than 1770mA, and preferred value is 1720mA.
Step 3 is disturbed measurement data is revised by deduction oxygen isotope, and makeover process is known to the skilled person general knowledge.
Data shown in table 1 are the molybdenum isotope abundance ratio measurement data of utilizing method of the present invention to obtain:
Table 1
Figure BDA0000040153160000061
Note: *r 140/146refer to tested MoO 3 -the ratio of the ion populations that in ionic group, mass number is 140 and the number of ions of mass number 146, the rest may be inferred for other ratio.
According to data shown in table 1, known relative standard deviation of the present invention is only 0.046～0.171%, has reached higher measuring accuracy.
By table 1 data, can obtain molybdenum isotope abundance measurement value.Data shown in table 2 are to utilize the comparison of molybdenum isotope abundance measurement value and the abundance reference value of method of the present invention:
Table 2
Figure BDA0000040153160000071
Shown in table 2 data, the 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 Contrast on effect of additive method in method of the present invention and prior art:
Table 3
Figure BDA0000040153160000072
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 -time, due to molybdenum under high temperature, be easily combined with oxygen and form negative ion, be therefore coated with sample amount and Measuring Time significantly reduces.The minimizing that is coated with sample amount not only can reduce operating personnel's radioactive dose, be beneficial to safety in production, and can be applied to the measurement of 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, painting sample amount 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 painting sample amount 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, is especially applicable to the radioactive sample of low content and the measurement requirement of biological sample.
Embodiment 2
The difference of the present embodiment and embodiment 1 is:
In step 2.2 and step 2.4, ion gun is vacuumized to processing, the ion gun vacuum tightness vacuumizing after processing of take is 5 * 10 -7mbar.

Claims (7)

1. a method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance, comprises the following steps:
Step 1 rhenium band is coated with sample;
Step 2 heats up and measures;
Step 3 is revised data;
It is characterized in that:
Step 1 specifically comprises the following steps:
Step 1.1 is dripped and is coated with 0.1～1 μ g molybdenum on the rhenium band silk of two rhenium band assemblies that comprises sample band and ionization band;
Step 1.2 is positioned over two rhenium band assemblies in vacuum environment, and to its access 5.5A electric current, continued power 10 minutes, adopts and burn belting removal surface impurity and water vapor;
Step 1.3 is taken out two rhenium band assemblies from burn belting, is placed in and is coated with on sampling device;
Step 1.4 is dripped and is coated with 1～2 μ L Na on the rhenium band silk of two rhenium band assemblies 2moO 4solution, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.5 pair two rhenium band assembly power-off;
Step 1.6 is dripped and is coated with 1 μ L SrCl on rhenium band silk 2solution, to two rhenium band assembly access 1.3A electric currents, continued power 60s;
Step 1.7 at the uniform velocity rises to 1.5A by electric current described in step 1.6 in 10～15s, and continued power 15s.
2. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 1, is characterized in that: the vacuum tightness of the vacuum environment described in step 1.2 is 1 * 10 -4pa.
3. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 1, is characterized in that: step 2 specifically comprises the following steps:
Step 2.1 is positioned over sample rotating disk by two rhenium band assemblies, and sample rotating disk is positioned in mass spectrometer ion source;
Step 2.2 pair ion gun vacuumizes processing;
Step 2.3 rises to 2000mA by the ionization band in two rhenium band assemblies with the speed of 450～550mA/min, the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 230～270mA/min simultaneously;
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 voltage, ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 150～250mA/min by 2000mA, the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 130～170mA/min by 1000mA simultaneously;
Step 2.7 rises to 2800mA with the speed of 80～120mA/min by 2500mA by the ionization band in two rhenium band assemblies, the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 60～100mA/min by 1450mA simultaneously;
Step 2.8 micro-regulation 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 higher than 2800mA, lower than 2900mA; The sample belt current raising in two rhenium band assemblies, makes it higher than 1700mA, lower than 1770mA.
4. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 3, is characterized in that: in step 2.2 and step 2.4, vacuumize ion gun vacuum tightness after processing higher than 1 * 10 -6mbar.
5. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 4, is characterized in that: the ion gun vacuum tightness vacuumizing in step 2.2 and step 2.4 after processing is 5 * 10 -7mbar.
6. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 3, it is characterized in that: in step 2.3, ionization band in two rhenium band assemblies is risen to 2000mA with the speed of 500mA/min, the sample band in two rhenium band assemblies is risen to 1000mA with the speed of 250mA/min simultaneously; In step 2.6, the ionization band in two rhenium band assemblies is risen to 2500mA with the speed of 200mA/min, the sample band in two rhenium band assemblies is risen to 1450mA with the speed of 150mA/min simultaneously; Step 2.7 rises to 2800mA by the ionization band in two rhenium band assemblies with the speed of 100mA/min, the sample band in two rhenium band assemblies is risen to 1700mA with the speed of 80mA/min simultaneously.
7. method for measuring negative thermal ionization mass spectrometry of molybdenum isotope abundance according to claim 3, is characterized in that: the ionization belt current raising in step 2.9 in two rhenium band assemblies is to 2850mA; The sample belt current raising in two rhenium band assemblies is to 1720mA.
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