CN115219302A - Tantalum pentafluoride emission agent and preparation method thereof - Google Patents
Tantalum pentafluoride emission agent and preparation method thereof Download PDFInfo
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- CN115219302A CN115219302A CN202210849647.6A CN202210849647A CN115219302A CN 115219302 A CN115219302 A CN 115219302A CN 202210849647 A CN202210849647 A CN 202210849647A CN 115219302 A CN115219302 A CN 115219302A
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- tantalum pentafluoride
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
Abstract
The invention discloses a tantalum pentafluoride propellant and a preparation method thereof, and the preparation method comprises the following steps: firstly, taCl is weighed 5 Dissolving the powder in HF solution, and adding HNO 3 Solution, H 3 PO 4 Finally, adding high-purity water and uniformly mixing to obtain an emitting agent solution; then, the transmitting agent solution passes through an ion exchange resin exchange column, and filtrate is collected; and finally, adding ion exchange resin into the filtrate, standing for 3-5d, and removing the ion exchange resin to obtain the purified tantalum pentafluoride propellant. The prepared tantalum pentafluoride propellant solution can effectively meet the strontium Sr isotope measurement requirements of samples with nanogram magnitude and even lower content, the strontium background value is extremely low, the sample demand is reduced by 2-3 magnitude orders, the sensitivity is improved, a new choice is provided for the analysis of samples which are difficult to obtain or reproduce, and the application of the strontium isotope measurement technology in wider fields is facilitated.
Description
Technical Field
The invention relates to the technical field of isotope measurement, in particular to a tantalum pentafluoride emitting agent and a preparation method thereof.
Background
Isotope test technology is widely used in various fields because the test precision is far beyond the conventional test. As the requirements for test samples become more stringent and the requirements for test results become more demanding, how to obtain stronger and more stable ion signals with limited samples is an important point in isotopic methods.
The strontium isotope is an important component in an isotope system, and is widely applied to the aspects of geology dating, earth evolution, environment monitoring, biological source tracing, ancient climate reconstruction, sea level reconstruction and the like. Isotope tests in the prior art require strontium contents of at least the microgram level (10) while meeting the test accuracy and precision requirements -6 ～10 -7 g) For nanogram scale (10) - 9 g) The precision of the test is sharply reduced, and the accuracy is not reliable any more. The fundamental reason is that at very low isotope contents it is difficult to ionize a single, stable, high intensity ion stream, making the test unsatisfactory. I.e. the prior art propellants are difficult to meet.
Therefore, how to provide an emitting agent which meets the strontium isotope measurement requirement of a sample with the nanogram level or even lower content is a problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In view of the above, the invention provides a preparation method of tantalum pentafluoride emission agent solution, so that the prepared product meets the strontium isotope measurement requirement of samples with nanogram magnitude or even lower content.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a tantalum pentafluoride emission agent comprises the following steps:
(1) Weighing TaCl 5 Dissolving the powder in HF solution, and adding HNO 3 Solution, H 3 PO 4 Finally, adding high-purity water and uniformly mixing to obtain an emitting agent solution;
(2) Passing the propellant solution through an ion exchange resin exchange column, and collecting filtrate;
(3) And adding ion exchange resin into the filtrate, standing for 3-5d, and removing the ion exchange resin to obtain the purified tantalum pentafluoride propellant.
Preferably, said TaCl is present in step (1) 5 HF solution, HNO 3 Solution, H 3 PO 4 The mass ratio of (A) to (B) is 6:3:9:7.
preferably, the HF solution concentration in step (1) is 22N 3 The solution concentration was 14N.
Preferably, the high purity water in step (1) has a conductivity of 18.2 megaohms.
Preferably, the amount of high purity water added in step (1) is TaCl 5 Powder basis, taCl 5 The concentration in the mixed solution reaches 0.02g/mL.
Preferably, the ion exchange resin is a Sr-Spec specific ion exchange resin.
In addition, the invention also provides the tantalum pentafluoride emission agent with the low strontium background value, which is prepared by adopting the scheme.
According to the technical scheme, compared with the prior art, the invention discloses the tantalum pentafluoride emission agent and the preparation method thereof, and the tantalum pentafluoride emission agent has the following beneficial effects:
the preparation method can effectively meet the strontium Sr isotope measurement requirements of nanogram-level or even lower-content samples, for nanogram-level trace strontium samples, no matter standard strontium solution or rock powder is adopted, under the condition of adding the tantalum pentafluoride propellant solution, the ionic signal intensity completely reaches the normal measurement range of an instrument, and the measurement result of the isotope ratio falls within the recommended value range of standard substances. The strontium background value of the prepared tantalum pentafluoride propellant solution is extremely low, the required quantity of samples is reduced by 2-3 orders of magnitude, the sensitivity is improved, a new choice is provided for the analysis of samples which are difficult to obtain or reproduce, and the application of a strontium isotope measuring technology in a wider field is facilitated.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a tantalum pentafluoride emission agent:
(1) Weighing 1.2g TaCl 5 The powder was dissolved in 0.6g of 22N HF solution, and 1.8g of 14N HNO was added 3 Solution, 1.4g H 3 PO 4 Finally, adding high-purity water (18.2 megaohms) to the volume of the solution of 60mL, and uniformly mixing to obtain an emitting agent solution;
(2) Passing the propellant solution through an exchange column filled with Sr-Spec specific ion exchange resin (TRISKEM, france), and collecting the filtrate;
(3) Adding Sr-Spec specific ion exchange resin (French TRISKEM company), standing for 3-5d, and removing the ion exchange resin to obtain the purified tantalum pentafluoride propellant.
Examples of the experiments
Tantalum pentafluoride emitter strontium background value measurement
Draw 100 microliters of purified TaF 5 Adding a proper amount of high-purity propellant solution with known concentration 84 Sr diluent, the mixed solution is stood for several days to reach strontium isotope balance between the diluent and the emitting agent.
Sucking 2 microliter of mixed solution of the emitting agent and the diluent, transferring the mixed solution onto a tungsten metal filament which is completely degassed, slowly heating the filament until the filament shows dark red, and then measuring the strontium isotope composition of the mixed solution by using a thermal ionization mass spectrometer. According to measured 84 Sr/ 86 The Sr ratio was calculated to give the base value of strontium per microliter of emitter solution.
The results are given in table 1 below.
TABLE 1 measurement of Sr background of secondary purified tantalum pentafluoride emitter solutions
| Numbering | Propellant solution | 84 Sr/ 86 Sr measurement value | Calculated Sr background (picogram/microliter) |
| 1 | Secondary purification | 50.50 | 0.022 |
| 2 | Secondary purification | 51.90 | 0.021 |
| 3 | Secondary purification | 52.77 | 0.021 |
| Mean value of | 0.02 |
From 3 replicate measurements, the Sr background average for the twice purified tantalum pentafluoride emitter solution was 0.02 picograms (pg) per microliter. When the thermal ionization mass spectrometer is used for measuring the strontium isotope ratio, the dosage of the propellant solution required by each sample is only 1 microliter, so the background from the propellant solution does not significantly influence the Sr background value of the whole process.
Isotope measurement experiments were specifically performed as follows:
measurement of strontium Standard solution of (I) micro sample
Using a strontium standard solution (NIST SRMNBS 987), nanogram-grade sample strontium isotope measurement was performed. When the thermal ionization mass spectrometer is used for measuring the strontium isotope, the dosage of the strontium sample is tested according to 2.5 nanograms, 1 nanogram and 0.1 nanogram. According to the sample amount, the NBS987 solution with the corresponding volume is sucked for measurement. When the thermal ionization mass spectrometer is used for measuring the strontium isotope ratio, a tungsten metal strip with a single-filament structure is used for heating and evaporating strontium elements, and the results are shown in the following table 2.
TABLE 2 measurement of Sr isotope in trace standard substance solution (NBS 987)
Remarking: measurements for each sample were taken 60-75 scans; each scanning acquisition time is 4 seconds, and the standing is 1 second; of standard substance NBS987 87 Sr/ 86 Reference value range of Sr: 0.710248 +/-30.
The result shows that in the measuring process, the strontium ion signal intensity is high and stable, and the measured isotope ratio precision and accuracy meet the measuring requirement.
When 2 parts of strontium are measured using 2.5 nanograms of sample, 88 the signal intensity of Sr ion can reach 8.4V and 3.5V, and the measured signal intensity is 87 Sr/ 86 The Sr ratio is 0.710265 + -1 and 0.710244 + -12, which is coincided with the recommended value range of standard substance.
Within the error range, the repeated measurement values of 4 parts of samples with the strontium content of 1 nanogram are coincident with the recommended value range of the standard substance 87 Sr/ 86 The Sr ratio ranges from 0.710237 + -9 to 0.710290 + -12.
Within the error range, the repeated measurement values of 6 parts of samples with the strontium content of 0.1 nanogram also fall within the recommended value range of the standard substanceEnclose, it 87 Sr/ 86 The Sr ratio ranges between 0.710204 + -19 and 0.710278 + -14.
(II) standard rock powder (BCR-2 basalt) nanogram strontium isotope measurement
The separation and purification of lead element in rock standard powder sample is completed in a purification laboratory, and the lead isotope ratio is measured by using a TRITON Plus thermal ionization mass spectrometer of Thermo Fisher Scientific company. An appropriate amount of rock powder sample was accurately weighed into a 7 ml Teflon-sealed jar, and 200. Mu.l of purified 14N HNO was added 3 And (3) shaking the acid solution uniformly, adding 2 ml of purified 22N HF acid solution, mixing uniformly, and then sealing and heating for about one week to fully dissolve the sample.
The results are shown in Table 3:
TABLE 3 measurement of trace standard rock powder (BCR-2 basalt) Sr isotope
Remarking: measurement of each sample 60-75 scans were taken; each scanning acquisition time is 4 seconds, and the standing is 1 second;
of standard rock powder BCR-2 87 Sr /86 Reference value range of Sr: 0.704097-0.705035;
sequence numbers 1-2:0.10g of a dissolved sample, taking 1/5 of separated and purified Sr, and diluting to 2ppm; sequence numbers 3 to 7:0.10g of a dissolved sample, separating and purifying Sr, and diluting to 2ppm;
sequence number 8-11: dissolving 0.09g of sample, taking 1/3 of separated and purified Sr, and diluting to 2ppm; sequence number 9-15: dissolving 0.02g of sample, separating and purifying Sr, and diluting to 2ppm;
serial number 16-17:0.10g of a dissolved sample, taking 1/5 of separated and purified Sr, and diluting to 2ppm; serial number 18-20:0.10g of dissolved sample, and Sr is separated and purified and diluted to 2ppm;
serial No. 21-25: dissolving 0.09g of sample, taking 1/3 of separated and purified Sr, and diluting to 2ppm; serial number 26-28:0.02g of a dissolved sample, and separated and purified Sr is diluted to 2ppm.
The test results show that the strontium solution samples of BCR-2 basalt obtained by different modes 88 The Sr ion signal intensity mostly exceeds 1V, and a stable ion signal intensity can be maintained during the test. The measurement results of the usage amount of the 2 nanogram and 1 nanogram strontium samples are basically consistent, and the measurement requirement of the Sr isotope ratio of a trace sample can be met.
The results of repeated measurements of 28 micro-samples all fell within the recommended value range for BCR-2 basalt standard substance (0.704097-0.705035), and the measured results were 87 Sr/ 86 The Sr ratio varies from 0.704923 + -25 to 0.705125 + -19, with an average of 0.705036.
Comparative example
A comparative experiment was carried out on a standard solution (NBS 987) without an emitter under the same configuration and measurement method, and the Sr samples were used in an amount of 200 ng and 10 ng, respectively.
In the experimental process, the current intensity of the tungsten metal filament is increased to about 3000mA, 88 the Sr ion signal intensity can reach about 1V, but the Sr ion signal intensity is extremely unstable, and rapidly decays to about 1mV within 2 minutes, the current intensity is continuously increased to 4500mA, the signal intensity is basically lower than 1mV, and data collection cannot be carried out.
And a test of strontium isotope measurement is carried out by adopting a tantalum metal filament and a rhenium metal filament. The result shows that the combination of the emitting agent solution and the tantalum metal filament with the single-band structure can also be applied to the measurement of the strontium isotope ratio, but the effect is obviously lower than that of the combination of the emitting agent solution and the tungsten filament with the single-band structure. The combination of the emitting agent solution and the rhenium filament band with a single-band structure can not meet the requirement of micro-sample measurement.
According to the technical scheme, the novel preparation method of the tantalum pentafluoride propellant solution is developed, and the prepared product meets the strontium isotope measurement requirement of a sample with nanogram magnitude or even lower content.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation method of the tantalum pentafluoride emission agent is characterized by comprising the following steps:
(1) Weighing TaCl 5 Dissolving the powder in HF solution, and adding HNO 3 Solution, H 3 PO 4 Finally, adding high-purity water and uniformly mixing to obtain an emitting agent solution;
(2) Passing the propellant solution through an ion exchange resin exchange column, and collecting filtrate;
(3) And adding ion exchange resin into the filtrate, standing for 3-5d, and removing the ion exchange resin to obtain the purified tantalum pentafluoride propellant.
2. The method of claim 1, wherein the TaCl in step (1) is added to the tantalum pentafluoride emitter 5 HF solution, HNO 3 Solution, H 3 PO 4 The mass ratio of (A) to (B) is 6:3:9:7.
3. the method according to claim 1, wherein the HF solution in the step (1) has a concentration of 22N, HNO 3 The solution concentration was 14N.
4. The method of producing a tantalum pentafluoride emitter according to claim 1, wherein the conductivity of the high-purity water in the step (1) is 18.2 megaohms.
5. The method of producing a tantalum pentafluoride emitter according to claim 1, wherein the amount of high purity water added in the step (1) is TaCl 5 Powder basis, taCl 5 The concentration of the mixed solution reaches 0.02g/mL.
6. The method of claim 1, wherein the ion exchange resin is a Sr-Spec specific ion exchange resin.
7. A tantalum pentafluoride emitter as claimed in any one of claims 1 to 6.
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| CN105301089A (en) * | 2015-10-23 | 2016-02-03 | 宁波出入境检验检疫局检验检疫技术中心 | Method for measuring strontium isotope ratios of samples at different positions of strawberry tree and authenticating producing areas of waxberries |
| CN109696466A (en) * | 2019-02-27 | 2019-04-30 | 中国科学院地质与地球物理研究所 | The highly sensitive cast charge and method of thermal ionization mass spectrometer for the test of submicrosample strontium isotope |
| CN110146584A (en) * | 2019-06-17 | 2019-08-20 | 中国科学院地质与地球物理研究所 | A kind of Nd and Sm separation method applied to thermal ionization mass spectrometry (tims) Nd isotope analysis |
| CN112456556A (en) * | 2020-11-30 | 2021-03-09 | 东北大学 | Method for preparing tantalum oxide nanospheres |
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- 2022-07-19 CN CN202210849647.6A patent/CN115219302A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105301089A (en) * | 2015-10-23 | 2016-02-03 | 宁波出入境检验检疫局检验检疫技术中心 | Method for measuring strontium isotope ratios of samples at different positions of strawberry tree and authenticating producing areas of waxberries |
| CN109696466A (en) * | 2019-02-27 | 2019-04-30 | 中国科学院地质与地球物理研究所 | The highly sensitive cast charge and method of thermal ionization mass spectrometer for the test of submicrosample strontium isotope |
| CN110146584A (en) * | 2019-06-17 | 2019-08-20 | 中国科学院地质与地球物理研究所 | A kind of Nd and Sm separation method applied to thermal ionization mass spectrometry (tims) Nd isotope analysis |
| CN112456556A (en) * | 2020-11-30 | 2021-03-09 | 东北大学 | Method for preparing tantalum oxide nanospheres |
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