CN103439164B - Based on plant or the soil moisture fast vacuum method for extracting of microwave heating - Google Patents
Based on plant or the soil moisture fast vacuum method for extracting of microwave heating Download PDFInfo
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- CN103439164B CN103439164B CN201310401600.4A CN201310401600A CN103439164B CN 103439164 B CN103439164 B CN 103439164B CN 201310401600 A CN201310401600 A CN 201310401600A CN 103439164 B CN103439164 B CN 103439164B
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Abstract
The present invention relates to a kind of plant based on microwave heating, soil moisture fast vacuum method for extracting, specifically comprise sample hose by microwave heating, moisture vapor is collected, connecting line, vacuum system and extraction system, its process is loaded fast in sample hose by the sample being kept at freezing state, sample hose is connected with extraction system, and sample hose is immersed in liquid nitrogen tank, install collection tube and confirm that system is air tight, the connection valve opening extraction system and vacuum system vacuumizes, when vacuum values is lower than 50mTorr, close connection valve, sample hose and collection tube is made to form the high vacuum enclosed system of a mutual UNICOM.Then sample hose is placed in and is equipped with in the liquid nitrogen tank of liquid nitrogen in microwave heating chamber, collection tube is made to be immersed in liquid nitrogen, open microwave applicator power supply and start heated sample, the moisture evaporated that to be heated from sample hose is collected in collection tube, after complete for the moisture in plant or soil extracting, collection tube is taken off, seals with sealed membrane, for D/H
16o/
18o measures.
Description
Technical field
The present invention relates to a kind of plant based on microwave heating or soil moisture fast vacuum method for extracting, be specifically related to a kind of moisture method for extracting for Stable Isotopic Analysis.
Background technology
In plant, the main source of hydrogen and oxygen is water, and the moisture that plant can utilize is mainly from precipitation, the holard, runoff (comprising snow melt) and underground water.The holard, runoff and underground water are initial also all from precipitation, but make soil moisture produce isotopics gradient due to the seasonal variations of soil moisture input, the evaporation of surface layer or the difference between soil body moisture and underground water.In general, root system of plant absorbs moisture process and xylem Water Transportation process subsequently and all isotopic fractionation does not occur, namely root with δ D, the δ of water in stem
18can for δ D, δ of the water of plant absorption in O value and soil
18o value is close.Therefore can determine the absorption of root system to the holard of separate sources by the isotope ratio analyzing axis water, understand the activity of root in soil profile further and in natural community plant to the difference of the utilization of moisture.In whole growth course, plant not only utilizes a kind of water source (comprising atmospheric precipitation, the holard, underground water etc.).Utilize stable isotope technology not only can measure plant under various circumstances utilized moisture the degree of depth and to use the plant at two or more water source can quantitatively its utilize ratio shared by water source; But also plant water use change in time can be studied, this point is unascertainable by means of only analyzing the distribution institute of root system of plant in soil profile.Another vital role of isotope technology to determine that in soil which Activities of Some Plants root system is the most active regions absorbing moisture.Because root system of plant spreads all over whole soil profile usually, but this does not also mean that root system all shows moisture picked-up activity in its soil layer existed, up to the present other method is then difficult to address this problem, and the precondition addressed these problems is that the complete moisture sample that can obtain different parts detects for stable isotope.
Current plant, soil moisture extracting method adopt the outer wrap electric-heating-wire-heating sample at vacuum specimen tube, owing to being high vacuum in sample hose, having intercepted heat and conducted to sample, made extraction efficiency not high.For plant stem, the time that heating is extracted could by complete for plant moisture extracting more than 2 hours.In addition existing apparatus is made up of horminess glass tube sweat soldering, very easily damages in using.For existing apparatus Problems existing, the present invention proposes new technical scheme more efficiently.
Summary of the invention
The object of the invention is to, a kind of plant based on microwave heating or soil moisture fast vacuum method for extracting are provided, the method is by sample collection, system is hunted leak, freezing, vacuumize and heat extraction steps and complete, its process is loaded fast in sample hose by the sample being kept at freezing state, sample hose is connected with extraction system, and sample hose is immersed in liquid nitrogen tank, install collection tube and confirm that system is air tight, the connection valve opening extraction system and vacuum system vacuumizes, when vacuum values is lower than 50mTorr, close the connection valve of extraction system and vacuum system, sample hose and collection tube is made to form the high vacuum enclosed system of a mutual UNICOM.Then collection tube is immersed in liquid nitrogen, then sample hose is placed in microwave heating chamber, open microwave applicator power supply and start heated sample, in collection tube, collect the moisture evaporated that to be heated from sample, after the complete extracting of sample moisture, collection tube is taken off, with sealed membrane sealing, for D/H
16o/
18o measures.
A kind of plant based on microwave heating of the present invention or soil moisture fast vacuum method for extracting, the device related in the method is by vacuum system (14), vacuum pump (3), vacuum meter (9), valve (4), vacuum pump switch (12), extraction system (10), microwave applicator (7), sample hose (1), collection tube (2), liquid nitrogen tank (8), liquid nitrogen tank (11), microwave heating chamber (5), infrared sensor (6) form, and concrete operations follow these steps to carry out:
A, sample collection: gather and can extract the plant of 0.2-1.0ml water or the sample of soil, should load immediately in sample bottle after sample collection and seal and freezen protective;
B, system are hunted leak: be connected with extraction system (10) respectively with collection tube (2) by sample hose (1), extraction system (10) is connected with vacuum system (14), open vacuum pump (3), when vacuum tightness is lower than 60mTorr, close vacuum pump (3), observe vacuum meter (9) in extraction system and whether change;
C, freezing sample: sample hose (1) is taken out, put into the sample that step a gathers, again sample hose (1) is put into the liquid nitrogen tank (11) of microwave heating chamber (5), and add liquid nitrogen in liquid nitrogen tank (11), sample hose (1) is immersed in 10-20 minute in liquid nitrogen completely;
D, sample continue freezing, open the vacuum pump switch (12) on vacuum pump (3), open the connection valve (4) be fixed in vacuum system (14) simultaneously, treat whole system vacustat, and low vacuum, in 50-60mTorr, closes connection valve (4);
E, heating extracting, first collection tube (2) is put into the liquid nitrogen tank (8) that liquid nitrogen is housed, open the power supply (13) on microwave heating controller (7), adopt microwave, ultrasound wave or far infrared wave produce energy heats sample hose (1), exported by sample hose (1) temperature automatic control microwave, sample hose (1) temperature is made to remain on 105-120 DEG C, collection tube (2) collects the moisture evaporated that is heated from sample hose (1), until moisture is entered in collection tube (2) by complete extracting, according to the height collecting moisture in collection process, by constantly adding the height of liquid nitrogen in liquid nitrogen adjustment liquid nitrogen tank (8), after heating extracting completes, collection tube (2) is taken off, rapid cap for special purpose seals, stored refrigerated measures.
After step a sample being taken out from refrigerator-freezer in step c, at room temperature need place and plant somewhat, remove diaphragm seal, dry the moisture of sample hose outer wall, and then sample is put into sample hose (1).
The moisture collection time in step e in plant roots or stem sample is 30-45 minute, and the moisture collection time in pedotheque is 20-30 minute.
In step e, sample heating temperature is measured by infrared mode, and the power stage of FEEDBACK CONTROL microwave, ultrasound wave or far infrared wave, sample temperature is controlled at 105-120 DEG C.
In the device that described method relates to, vacuum meter (9) and vacuum pump (3) is connected respectively in one end of vacuum system (14), the other end is the fixing impartial vacuum tube be connected with extraction system (10) arranged respectively, vacuum tube is provided with valve (4), several sample hoses (1) that one end and the equalization of extraction system (10) arrange are connected, and several collection tubes (2) that its other end arranges with equalization are connected.
In the device that described method relates to, microwave applicator (7) is fixed in the bottom of microwave heating chamber (5) side, sample hose (1) puts into liquid nitrogen tank (11), again liquid nitrogen tank (11) is put into microwave heating chamber (5), be fixed with infrared sensor (6) in the lower end of sample hose (1), collection tube (2) puts into liquid nitrogen tank (8).
In the device that described method relates to, the pipeline of extraction system (10) is formed by the materials processing of monoblock melting TFE copolymer, and the two ends of extraction system (10) adopt screw socket mode to screw with sample hose (1) and collection tube (2) to be connected.
Plant based on microwave heating of the present invention, soil moisture fast vacuum method for extracting, wherein:
In sample collection, sampling quantity is determined according to the water cut assessment of plant or soil, is generally advisable can extract 0.2-1.0ml water, should loads immediately in sample hose (1) and seal and freezen protective after sample collection;
In system leak detection, before extracting moisture, whether check system is airtight, concrete grammar is connected with extraction system (10) all respectively with collection tube (2) by sample hose (1), open vacuum pump (3) and connect system, when vacuum tightness is lower than 60mTorr, close vacuum, whether the vacuum meter (9) observing extraction system changes;
Freezing sample, after systems inspection completes, takes out sample hose (1), put into the sample of also freezen protective after gathering, again sample hose (1) is put into microwave heating chamber (5), liquid nitrogen tank (11) adds liquid nitrogen, and sample hose (1) is immersed in 10-20 minute in liquid nitrogen completely;
Vacuumize: sample continues freezing, open vacuum pump switch (12) successively and connection valve (4) fixing between vacuum system (14) and extraction system (10), treat whole system vacustat, vacuum tightness lower than 50-60mTorr, will close connection valve (4) under normal circumstances;
Heating extracting, first collection tube (2) is put into the liquid nitrogen tank (8) that liquid nitrogen is housed, open microwave heating controller (7) power supply (13) heated sample pipe (1), manage (1) temperature automatic control microwave per sample to export, sample hose (1) temperature is made to remain on 105-120 degree Celsius until moisture is by complete extracting, the moisture that sample hose (1) evaporates is entered in collection tube (2) by extracting, this process is different per sample and determine, plant roots under normal circumstances, stem is 30-45 minute, soil is 20-30 minute, adjust the height of liquid nitrogen tank (8) according to the situation of collecting moisture in collection process, and continuous annex solution nitrogen, after heating extracting completes, collection tube (2) is taken off, rapid cap for special purpose seals, stored refrigerated is used for D/H,
16o/
18o measures.
For validity and the feasibility of checking microwave heating extraction process, demonstration can be obtained further in Table by test result:
| Sequence number | Technical indicator title | Parameter before functional development | The parameter reached is estimated after functional development |
| 1 | Extraction times | 120-150 minute | 30-45 minute |
| 2 | Sample number | 5-6/time | 8-16/time |
| 3 | System vacuum slip | 6×10-3mbar·L/sec | 2×10-3mbar·L/sec |
| 4 | End vacuum pressure: | <1.5mbar | <1.2mbar |
Plant based on microwave heating of the present invention or soil moisture fast vacuum method for extracting, the superiority of the method is: the moisture after extracting is measured by gas stable isotope mass spectrometer, hydrogen isotope ratio precision is 4 ‰, oxygen isotope ratio precision is 0.1 ‰, the result that method precision detects meets internationally recognized critical field, test fast for extensive sample and lay a good foundation, the invention provides a kind of quick, easy, economic plant, soil moisture extracting method, by the following examples in detail the present invention is described in detail.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation.
Embodiment
Embodiment 1(plant moisture fast vacuum extracting)
Preparation facilities: connect vacuum meter 9 and vacuum pump 3 in one end of vacuum system 14 respectively, the other end is the fixing impartial vacuum tube be connected with extraction system 10 arranged respectively, vacuum tube is provided with valve 4, one end of extraction system 10 and impartial several sample hoses 1 arrange adopt screw socket mode to screw to be connected, and its other end and impartial several collection tubes 2 arranged adopt screw socket mode to screw to be connected; Microwave applicator 7 is fixed in the bottom of microwave heating chamber 5 side, sample hose 1 puts into liquid nitrogen tank 11, again liquid nitrogen tank 11 is put into microwave heating chamber 5, be fixed with infrared sensor 6 respectively in the lower end of several sample hoses 1 of equalization arrangement, collection tube 2 puts into liquid nitrogen tank 8; The pipeline of extraction system 10 is formed by the materials processing of monoblock melting TFE copolymer;
Sample collection: gather the plant sample that can extract 0.2-1.0ml water, should load immediately in sample bottle after sample collection and seal and freezen protective;
System is hunted leak: be connected with extraction system 10 respectively with collection tube 2 by sample hose 1, extraction system 10 is connected with vacuum system 14, open vacuum pump 3, when vacuum tightness is lower than 60mTorr, close vacuum pump 3, observe vacuum meter 9 in extraction system and whether change, if the speed that vacuum meter 9 reading raises is very fast, illustrative system leaks gas, and checks that eliminating is completely airtight to system step by step;
Freezing sample: sample hose 1 is taken out, after the plant sample gathered is taken out from refrigerator-freezer, at room temperature need place and plant somewhat, remove diaphragm seal, and dry the moisture of outer wall, the plant sample loaded in sample bottle is taken out, put into sample hose 1, again sample hose 1 is put into the liquid nitrogen tank 11 of microwave heating chamber 5, and add liquid nitrogen in liquid nitrogen tank 11, sample hose 1 is immersed in 10-20 minute in liquid nitrogen completely;
Sample continues freezing, open the vacuum pump switch 12 on vacuum pump 3, open the connection valve 4 be fixed in vacuum system 14 simultaneously, treat whole system vacustat, low vacuum is in 50-60mTorr, close connection valve 4, wait for 1-2 minute, if vacuum tightness is no more than 100mTorr, then system is not leaked gas, if the speed that vacuum meter 9 reading raises is very fast, illustrative system leaks gas, and checks that eliminating is completely airtight to system step by step;
Heating extracting, before heating, close connection valve 4, adopted by extraction system 10 screw socket mode to screw and connect collection tube 2, again collection tube 2 is put into liquid nitrogen tank 8, and liquid nitrogen is added in liquid nitrogen tank 8, then the power supply 13 on microwave heating controller 7 is opened, adopt microwave, ultrasound wave or far infrared wave produce energy heats sample hose 1, pipe 1 temperature automatic control microwave exports per sample, sample hose 1 temperature is made to remain on 105-120 DEG C, collection tube 2 collects the moisture evaporated that to be heated from sample hose 1, until moisture is entered in collection tube 2 by complete extracting, plant roots, it is 30-45 minute that stem collects the moisture time, according to the height collecting moisture in collection process, by constantly adding the height of liquid nitrogen in liquid nitrogen adjustment liquid nitrogen tank 8, after heating extracting completes, collection tube 2 is taken out, rapid cap for special purpose seals, when being all melted into aqueous water Deng the moisture collected, by water transport in the ampoule of sealing, and seal with sealed membrane, whole process is wanted rapidly, guarantee that moisture does not leak and evaporates, and with numeral or English numbered samples, stored refrigerated measures.Attention: must be careful in the process of loading and unloading sample hose 1 and collection tube 2, avoids damage system.
Embodiment 2(soil moisture fast vacuum extracting)
Preparation facilities is undertaken by embodiment 1;
Sample collection: gather the pedotheque that can extract 0.2-1.0ml water, should load immediately in sample bottle after sample collection and seal and freezen protective;
System is hunted leak: be connected with extraction system 10 respectively with collection tube 2 by sample hose 1, extraction system 10 is connected with vacuum system 14, open vacuum pump 3, when vacuum tightness is lower than 60mTorr, close vacuum pump 3, observe vacuum meter 9 in extraction system and whether change, if the speed that vacuum meter 9 reading raises is very fast, illustrative system leaks gas, and checks that eliminating is completely airtight to system step by step;
Freezing sample: sample hose 1 is taken out, after the pedotheque gathered is taken out from refrigerator-freezer, at room temperature need place and plant somewhat, remove diaphragm seal, and dry the moisture of outer wall, pedotheque will be put into glass wool to avoid soil particle to be extracted into system, put into sample hose 1, again sample hose 1 is put into the liquid nitrogen tank 11 of microwave heating chamber 5, and add liquid nitrogen in liquid nitrogen tank 11, sample hose 1 is immersed in 10-15 minute in liquid nitrogen completely;
Sample continues freezing, open the vacuum pump switch 12 on vacuum pump 3, open the connection valve 4 be fixed in vacuum system 14 simultaneously, treat whole system vacustat, low vacuum is in 50-60mTorr, close connection valve 4, wait for 1-2 minute, if vacuum tightness is no more than 100mTorr, then system is not leaked gas, if the speed that vacuum meter 9 reading raises is very fast, illustrative system leaks gas, and checks that eliminating is completely airtight to system step by step;
Heating extracting, before heating, close connection valve 4, screw socket mode is adopted by extraction system 10 to screw the collection tube 2 of connection, again collection tube 2 is put into liquid nitrogen tank 8, and liquid nitrogen is added in liquid nitrogen tank 8, then the power supply 13 on microwave heating controller 7 is opened, adopt microwave, ultrasound wave or far infrared wave produce energy heats sample hose 1, pipe 1 temperature automatic control microwave exports per sample, sample hose 1 temperature is made to remain on 105-120 DEG C, collection tube 2 collects the moisture evaporated that to be heated from sample hose 1, until moisture is entered in collection tube 2 by complete extracting, the moisture collection time in pedotheque is 20-30 minute, according to the height collecting moisture in collection process, by constantly adding the height of liquid nitrogen in liquid nitrogen adjustment liquid nitrogen tank 8, after heating extracting completes, collection tube 2 is taken out, rapid cap for special purpose seals, when being all melted into aqueous water Deng the moisture collected, by water transport in the ampoule of sealing, and seal with sealed membrane, whole process is wanted rapidly, guarantee that moisture does not leak and evaporates, and with numeral or English numbered samples, stored refrigerated measures.Attention: must be careful in the process of loading and unloading sample hose 1 and collection tube 2, avoids damage system.
Claims (1)
1. the plant based on microwave heating or soil moisture fast vacuum method for extracting, it is characterized in that the device related in the method is by vacuum system (14), vacuum pump (3), vacuum meter (9), valve (4), vacuum pump switch (12), extraction system (10), microwave applicator (7), sample hose (1), collection tube (2), first liquid nitrogen tank (8), second liquid nitrogen tank (11), microwave heating chamber (5), infrared sensor (6) forms, vacuum meter (9) and vacuum pump (3) is connected respectively in one end of vacuum system (14), the other end is the fixing impartial vacuum tube be connected with extraction system (10) arranged respectively, vacuum tube is provided with valve (4), several sample hoses (1) that one end and the equalization of extraction system (10) arrange are connected, several collection tubes (2) that its other end arranges with equalization are connected, microwave applicator (7) is fixed in the bottom of microwave heating chamber (5) side, sample hose (1) puts into the second liquid nitrogen tank (11), again the second liquid nitrogen tank (11) is put into microwave heating chamber (5), infrared sensor (6) is fixed with in the lower end of sample hose (1), collection tube (2) puts into the first liquid nitrogen tank (8), the pipeline of extraction system (10) is formed by the materials processing of monoblock melting TFE copolymer, the two ends of extraction system (10) adopt screw socket mode to screw with sample hose (1) and collection tube (2) to be connected, concrete operations follow these steps to carry out:
A, sample collection: gather and can extract the plant of 0.2-1.0ml water or the sample of soil, should load immediately in sample bottle after sample collection and seal and freezen protective;
B, system are hunted leak: be connected with extraction system (10) respectively with collection tube (2) by sample hose (1), extraction system (10) is connected with vacuum system (14), open vacuum pump (3), when vacuum tightness is lower than 60mTorr, close vacuum pump (3), observe vacuum meter (9) in extraction system and whether change;
C, freezing sample: sample hose (1) is taken out, put into the sample that step a gathers, again sample hose (1) is put into second liquid nitrogen tank (11) of microwave heating chamber (5), and liquid nitrogen is added in the second liquid nitrogen tank (11), sample hose (1) is immersed in 10-20 minute in liquid nitrogen completely, after wherein sample takes out from refrigerator-freezer, at room temperature need place and plant somewhat, remove diaphragm seal, dry the moisture of sample hose outer wall, and then sample is put into sample hose (1);
D, sample continue freezing, open the vacuum pump switch (12) on vacuum pump (3), open the connection valve (4) be fixed in vacuum system (14) simultaneously, treat whole system vacustat, and low vacuum, in 50mTorr, closes connection valve (4);
E, heating extracting, first collection tube (2) is put into the first liquid nitrogen tank (8) that liquid nitrogen is housed, open the power supply (13) on microwave heating controller (7), adopt microwave, ultrasound wave or far infrared wave produce energy heats sample hose (1), exported by sample hose (1) temperature automatic control microwave, sample hose (1) heating-up temperature is measured by infrared mode, and FEEDBACK CONTROL microwave, the power stage of ultrasound wave or far infrared wave, temperature remains on 105-120 DEG C, collection tube (2) collects the moisture evaporated that is heated from sample hose (1), until moisture is entered in collection tube (2) by complete extracting, the moisture collection time in plant roots or stem sample is 30-45 minute, the moisture collection time in pedotheque is 20-30 minute, according to the height collecting moisture in collection process, the height of liquid nitrogen in the first liquid nitrogen tank (8) is adjusted by constantly adding liquid nitrogen, after heating extracting completes, collection tube (2) is taken off, rapid cap for special purpose seals, stored refrigerated measures.
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| CN104359712B (en) * | 2014-10-31 | 2017-01-25 | 河海大学 | Continuous soil moisture pumping device and using method thereof |
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| 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 |
| CN110208042A (en) * | 2019-06-04 | 2019-09-06 | 中国工程物理研究院核物理与化学研究所 | It is a kind of biology sample in tissue free water tritium sampler |
| CN110672367A (en) * | 2019-09-20 | 2020-01-10 | 深圳雨伦环境科技有限公司 | Moisture vacuum extraction device and moisture vacuum extraction method |
| CN111983188B (en) * | 2020-08-13 | 2022-01-21 | 中国科学院南京地理与湖泊研究所 | Soil water extraction and stable isotope composition analysis method |
| CN113125470B (en) * | 2021-04-20 | 2021-11-16 | 南京晓庄学院 | Utilize microwave remote sensing monitoring soil moisture equipment |
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