CN1786701A - Method for determining content of (18) 0 isotope in water - Google Patents
Method for determining content of (18) 0 isotope in water Download PDFInfo
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- CN1786701A CN1786701A CN 200410089362 CN200410089362A CN1786701A CN 1786701 A CN1786701 A CN 1786701A CN 200410089362 CN200410089362 CN 200410089362 CN 200410089362 A CN200410089362 A CN 200410089362A CN 1786701 A CN1786701 A CN 1786701A
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Abstract
The invention supplies a measuring method for 18O isotopic content in water that takes reaction of water sample and surfeit guanidine hydrochloride at vacuum state. It transmits to CO2< / SUB> molecule, then wipes off impurity gas by isotope low temperature refrigeration, uses gas phase isotope velocitron measuring 18O isotopic content in CO2, thus, the 18O isotopic content is determined in water sample. The invention is suited for measuring isotopic content of 18O in fully abundance range in water sample. It requires little water sample, is easy and simple to handle, has good repetitiveness, high measuring accuracy, etc.
Description
Technical Field
The invention relates to a splitting method, in particular to a method for splitting a water body in water18And (3) a method for measuring the content of the O isotope.
Background
The oxygen element in nature has three stable isotopes, the mass numbers of which are respectively 16, 17 and 18 and are respectively recorded as16O、17O and18and O. The abundances (atomic contents) of the compounds in natural water molecules are respectively,16o: 99.76 atomic%;17o: 0.04 atomic%;18o: 0.2 atomic%. By oxygen we mean in general that including16O、17O and18and O. Therein17O and18o is called heavy oxygen isotope because of their sum16The external properties of O are similar, and can be replaced mutually without influencing the physicochemical properties of the original substances, so that the O can be used as a tracer atom and widely applied to a plurality of fields of physicochemical, biological, medical science, environmental science and the like. Particularly, in recent years, with the improvement of science and technology and the living standard of people, the demand for heavy oxygen isotopes, which are essential elements of oxygen, has been increasing. In particular to the Positron Emission Tomography (PET) technology appearing in the nuclear medicine phase display field at present, and the application of heavier oxygen isotopes opens up a new and wider application prospect.
The heavy oxygen isotope is mainly in the form of heavy oxygen water, i.e. heavy oxygen isotope18Water with an O isotope content higher than its natural abundance.
At present, in water18The analysis of the O isotope abundance usually adopts an exchange method, and the method takes more than 24 hours for measuring once, and has the advantages of long time consumption, poor anti-interference performance, low repeatability and low accuracy. And the water sample consumed for one measurement is more, usually a few milliliters. And heavy oxygen water, especially18The heavy oxygen water with O abundance more than 95 atom percent is extremely expensive, and the exchange method is utilized to determine the oxygen content in the water sample18The O isotope abundance is inconvenient and expensive for heavy oxygen water production enterprises。
Disclosure of Invention
The invention aims to overcome the defect of the prior art for measuring water18The method for O isotope content has the defects of providing a simple, quick, convenient, practical, low-price, accurate and reliable water18And (3) a method for measuring the content of the O isotope.
The purpose of the invention is realized by packaging a water sample (1-15 microliter) to be measured in a capillary tube, then placing the capillary tube and guanidine hydrochloride in a reaction glass tube together, pumping air in the reaction glass tube by using an established vacuum packaging sample preparation device, and sealing the reaction glass tube when the vacuum degree in the reaction glass tube is reduced to 0.01-1.0 Pa (absolute pressure), thereby avoiding CO in the air2Has an influence on the reaction result. Then breaking the capillary tube filled with the water sample in the sealed reaction glass tube to ensure that the water sample is fully contacted with the guanidine hydrochloride, then placing the reaction glass tube in a muffle furnace, controlling the temperature to be between 120 and 350 ℃, and reacting for 1 to 6 hours to ensure that the water sample and the guanidine hydrochloride are fully and completely reacted to ensure that the water sample in the water sample18Complete transfer of O isotope atom to CO generated by reaction2And (4) removing in molecules. After the reaction is finished and the reaction glass tube is cooled to room temperature, the reaction glass tube is placed in a constant temperature liquid with the temperature of minus 50 to minus 100 ℃, and CO in the gas generated by the reaction is removed by a freezing method2And foreign impurity gases. Then the end of the reaction glass tube is broken off and the purified CO is removed2Injecting gas into a gas isotope mass spectrometer, and calculating CO according to the peak intensity of 44-49 measured by the gas isotope mass spectrometer2In18Content of O isotope to obtain water18The content of the O isotope.
The invention is suitable for the range of full abundance in water samples18The water sample amount required by each determination is only a few microliters, the determination is reduced by about 1000 times compared with the commonly used exchange method, the operation is simple and convenient, the repeatability is good, the test precision is high, and a method for determining the content of the O isotope is provided for the heavy oxygen water production enterprises in ChinaSimple, feasible, accurate and reliable18And (3) a method for measuring thecontent of the O isotope.
Drawings
FIG. 1 shows a water system of the present invention18A schematic view of a reaction glass tube used in the method for measuring the content of O isotope;
FIG. 2 shows the water of the present invention18A schematic diagram of a vacuum-packed sample preparation apparatus used in the method for measuring the content of an O isotope.
Detailed Description
Referring to fig. 1, fig. 1 is a schematic view of a reaction glass tube used in the present invention. One end of the reaction glass tube 1 is an open end 11, the other end is a tapered closed end 12, and a narrow neck 13 is preset at the open end. When the device is used, the capillary tube 2 and the guanidine hydrochloride 3 which are packaged with a water sample are put into the reaction glass tube from the open end 11, and the thin neck 13 is sealed off after the vacuum packaging sample preparation device is connected and vacuumized. Then the whole can be put into a muffle furnace for heating reaction and put into a low-temperature constant-temperature liquid tank for freezing. Before measurement, the end 12 of the thin seal is broken and injected.
Referring to fig. 2, see fig. 1 in combination. Fig. 2 is a schematic diagram of a vacuum packaging sample preparation device used in the present invention, which includes a reaction glass tube 1, a gas phase isotope mass spectrometer 4, a vacuum pump 5, a constant temperature liquid tank 6, a cryotrap 7, valves 81, 82, 83, 84, 85, 86, and corresponding connecting pipes. After the capillary tube 2 and guanidine hydrochloride 3 which are packagedwith a water sample are arranged in the reaction glass tube 1, the reaction glass tube 1 is connected to a vacuum packaging sample preparation device, the valves 81, 82, 83 and 86 are opened, the valves 84 and 85 are closed, the vacuum pump 5 is started, the pressure in the reaction glass tube 1 is reduced to 0.01-1.0 Pa (absolute pressure), the reaction glass tube 1 is sealed from the thin neck 13, the valves 81, 82 and 86 are closed, and the vacuum pump 5 is stopped. Taking down the reaction glass tube 1, breaking the sample sealing capillary tube 2 to fully mix the water sample and the guanidine hydrochloride, placing the reaction glass tube 1 in a muffle furnace, controlling the temperature between 120 and 350 ℃, and reacting for 1 to 6 hours to fully mix the water sample and the guanidine hydrochlorideComplete reaction, making the water sample in18Complete transfer of O isotope atom to CO generated by reaction2And (4) removing in molecules. Then the reaction glass tube 1 after full reaction is placed in a constant temperature liquid tank 6 with the temperature of-50 to-100 ℃, and CO generated by the reaction is removed by a freezing method2Impurity gases outside the gas. Then the valves 84 and 85 are opened, the drawn end 12 of the reaction glass tube 1 is broken off, and the purified CO is discharged2Injecting gas into the gas phase isotope mass spectrometer 4, and calculating CO according to the peak intensity of 44-49 measured by the gas phase isotope mass spectrometer2In18Content of O isotope to obtain water18The content of the O isotope.
The process of the present invention is further illustrated below with reference to several specific examples.
Example 1.
Mixing 8 microliters of natural water (18The abundance of O is 0.204 percent) is injected into the capillary tube, then the capillary tube is placed into a reaction glass tube filled with guanidine hydrochloride, the capillary tube is connected into a vacuum packaging sample preparation device, the vacuum degree is pumped till the vacuum degree is kept at about 0.01Pa, and the thin neck of the reaction glass tube is sealed off. And breaking the capillary tube, contacting the water sample with guanidine hydrochloride, and then placing the mixture into a muffle furnace to keep the mixture at 250 ℃ for 1 hour. After the reaction is finished, the reaction glass tube is put into a constant-temperature liquid tank at the temperature of-70 ℃, and CO generated in the reaction is removed by a freezing method2Impurity gases outside the gas. Then the frozen purified CO is2Measuring the peak intensity of 44-49 in an injected gas isotope mass spectrometer, and calculating CO2In the molecule18The content of O isotope atoms. The measured result shows that the water sample is in18The O isotope content was 0.203%, and the measurement error was 0.49%.
Example 2.
Mixing 15 microliter18Injecting a standard water sample with 10.6% of O abundance into a capillary tube, then putting the capillary tube into a reaction glass tube filled with guanidine hydrochloride, connecting the capillary tube into a vacuum packaging sample preparation device, vacuumizing until the vacuum degree is kept at about 0.1Pa, and sealing off the thin neck of the reaction glass tube. Breaking the capillary tube to make the water sample contact with guanidine hydrochloride, and thenPutting the mixture into a muffle furnace,the temperature is kept for 3 hours in the environment of 120 ℃. After the reaction is finished, the reaction glass tube is put into a constant-temperature liquid tank at the temperature of minus 50 ℃, and CO generated in the reaction is removed by a freezing method2Impurity gases outside the gas. Then the frozen purified COis2Measuring the peak intensity of 44-49 in an injected gas isotope mass spectrometer, and calculating CO2In the molecule18The content of O isotope atoms. The measured result shows that the water sample is in18The content of O isotope is 10.65%, and the measurement error is 0.47%.
Example 3.
Mixing 1 microliter18Injecting a standard water sample with 86.8% of O abundance into a capillary tube, then putting the capillary tube into a reaction glass tube filled with guanidine hydrochloride, connecting the capillary tube into a vacuum packaging sample preparation device, vacuumizing until the vacuum degree is kept at about 0.01Pa, and sealing off the thin neck of the reaction glass tube. And breaking the capillary tube, contacting the water sample with guanidine hydrochloride, putting the contact product into a muffle furnace, and keeping the contact product at the temperature of 300 ℃ for 6 hours. After the reaction is finished, the reaction glass tube is placed into a constant-temperature liquid tank at the temperature of 100 ℃ below zero, and CO generated in the reaction is removed by a freezing method2Impurity gases outside the gas. Then the frozen purified CO is2Measuring the peak intensity of 44-49 in an injected gas isotope mass spectrometer, and calculating CO2In the molecule18The content of O isotope atoms. The measured result shows that the water sample is in18The O isotope content was 86.64%, and the measurement error was 0.19%.
Example 4.
Mixing 6 microlitres18Injecting a standard water sample with 96.8% of O abundance into a capillary tube, then putting the capillary tube into a reaction glass tube filled with guanidine hydrochloride, connecting the capillary tube to a vacuum packaging sample preparation device, keeping the vacuum degree at about1.0Pa, and sealing off the thin neck of the reaction glass tube. And breaking the capillary tube, contacting the water sample with guanidine hydrochloride, and then placing the mixture into a muffle furnace to keep the mixture at 350 ℃ for 5 hours. After the reaction is finished, the reaction glass tube is put into a constant-temperature liquid tank at the temperature of minus 80 ℃, and CO generated in the reaction is removed by a freezing method2Impurity gases outside the gas. Then the frozen purified CO is2Measuring 44-49 peak intensity in an injected gas isotope mass spectrometer, and calculatingCO discharge2In the molecule18The content of O isotope atoms. The measured result being that of the water sample18The O isotope content was 96.3%, and the measurement error was 0.05%.
Claims (3)
1. In water18The method for measuring the content of the O isotope is characterized by comprising the following steps: the method comprises the following steps:
a、18transfer of O isotope
Heating a small amount of water sample and excessive guanidine hydrochloride to react in a vacuum state to ensure that the guanidine hydrochloride in the water sample18Complete transfer of O isotope atoms to CO2In the molecule, the chemical reaction equation is as follows:
b、CO2purification of gases
Removal of CO from gases formed by reactions by cryogenic freezing2Other impurity gases to obtain pure CO2A gas;
c、18determination of the O isotope content
Purified CO2Gas injection gas isotope mass spectrometer for measuring molecular18The content of O isotope atoms and calculating the content of O isotope atoms in the water sample18The content of O isotope atoms.
2. Water according to claim 118The method for measuring the content of the O isotope is characterized by comprising the following steps: the vacuum state in the step a is absolute pressure of 0.01-1.0 Pa, the reaction temperature is controlled to be 120-350 ℃, and the reaction time is controlled to be 1-6 hours.
3. Water according to claim 118The method for measuring the content of the O isotope is characterized by comprising the following steps: the low-temperature freezing temperature in the step b is controlled between-50 ℃ and-100 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102967678A (en) * | 2012-11-20 | 2013-03-13 | 中国食品发酵工业研究院 | Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water |
| CN102967661A (en) * | 2012-10-28 | 2013-03-13 | 中国食品发酵工业研究院 | Rapid determination method for oxygen stable isotope of ethanol in alcoholic beverage |
| CN105021732A (en) * | 2014-11-03 | 2015-11-04 | 中国食品发酵工业研究院 | Method for fast determination of oxygen isotope composition of water in beverage wine |
| CN106501048A (en) * | 2016-12-07 | 2017-03-15 | 黑龙江省科学院技术物理研究所 | A kind of preparation facilitiess of Diagnosis of Helicobacter pylori Infection detection sample and the preparation method of detection sample |
| CN106769346A (en) * | 2017-03-21 | 2017-05-31 | 中国科学院地质与地球物理研究所 | The method of hydrogen isotope in analysis water |
| CN109946407A (en) * | 2017-12-20 | 2019-06-28 | 核工业北京地质研究院 | A kind of mineral inclusion water sample extraction element for H isotope analysis |
| CN111268678A (en) * | 2020-03-12 | 2020-06-12 | 江苏华益科技有限公司 | Preparation method, device and application of high-abundance oxygen-18 carbon dioxide |
| CN113758991A (en) * | 2021-09-10 | 2021-12-07 | 北京善为正子医药技术有限公司 | Purity detection method of high-abundance oxygen-18 water |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1112260A1 (en) * | 1982-07-16 | 1984-09-07 | Институт Геохимии И Физики Минералов Ан Усср | Method of extracting oxygen from solid inorganic substances |
| CN2476014Y (en) * | 2001-04-25 | 2002-02-06 | 西南石油学院 | Carbon. oxygen isotope analysis laser micro sampler |
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2004
- 2004-12-10 CN CNB2004100893629A patent/CN100348976C/en active Active
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102967661A (en) * | 2012-10-28 | 2013-03-13 | 中国食品发酵工业研究院 | Rapid determination method for oxygen stable isotope of ethanol in alcoholic beverage |
| CN102967661B (en) * | 2012-10-28 | 2014-09-10 | 中国食品发酵工业研究院 | Rapid determination method for oxygen stable isotope of ethanol in alcoholic beverage |
| CN102967678A (en) * | 2012-11-20 | 2013-03-13 | 中国食品发酵工业研究院 | Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water |
| CN102967678B (en) * | 2012-11-20 | 2014-08-13 | 中国食品发酵工业研究院 | Offline pretreatment device and method for simply measuring oxygen stable isotope ratio in water |
| CN105021732A (en) * | 2014-11-03 | 2015-11-04 | 中国食品发酵工业研究院 | Method for fast determination of oxygen isotope composition of water in beverage wine |
| CN106501048A (en) * | 2016-12-07 | 2017-03-15 | 黑龙江省科学院技术物理研究所 | A kind of preparation facilitiess of Diagnosis of Helicobacter pylori Infection detection sample and the preparation method of detection sample |
| CN106501048B (en) * | 2016-12-07 | 2019-04-09 | 中国地质科学院水文地质环境地质研究所 | A kind of preparation facilities of Diagnosis of Helicobacter pylori Infection test sample and the preparation method of test sample |
| CN106769346A (en) * | 2017-03-21 | 2017-05-31 | 中国科学院地质与地球物理研究所 | The method of hydrogen isotope in analysis water |
| CN106769346B (en) * | 2017-03-21 | 2020-02-07 | 中国科学院地质与地球物理研究所 | Method for analyzing hydrogen isotopes in water |
| CN109946407A (en) * | 2017-12-20 | 2019-06-28 | 核工业北京地质研究院 | A kind of mineral inclusion water sample extraction element for H isotope analysis |
| CN111268678A (en) * | 2020-03-12 | 2020-06-12 | 江苏华益科技有限公司 | Preparation method, device and application of high-abundance oxygen-18 carbon dioxide |
| CN113758991A (en) * | 2021-09-10 | 2021-12-07 | 北京善为正子医药技术有限公司 | Purity detection method of high-abundance oxygen-18 water |
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| CN100348976C (en) | 2007-11-14 |
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Effective date of registration: 20060804 Address after: 200062 Shanghai Yunling Road No. 345 Applicant after: Shanghai Research Institute of Chemical Industry Co-applicant after: Shanghai Lianhong Isotope Technology Co., Ltd. Address before: 200062 Shanghai Yunling Road No. 345 Applicant before: Shanghai Research Institute of Chemical Industry |
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Address after: 200062 Shanghai Yunling Road No. 345 Co-patentee after: Shanghai Lianhong Isotope Technology Co., Ltd. Patentee after: Shanghai Chemical Research Institute Co., Ltd. Address before: 200062 Shanghai Yunling Road No. 345 Co-patentee before: Shanghai Lianhong Isotope Technology Co., Ltd. Patentee before: Shanghai Research Institute of Chemical Industry |