CN103439164A - Quick plant or soil water vacuum-extraction method based on microwave heating - Google Patents
Quick plant or soil water vacuum-extraction method based on microwave heating Download PDFInfo
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- CN103439164A CN103439164A CN2013104016004A CN201310401600A CN103439164A CN 103439164 A CN103439164 A CN 103439164A CN 2013104016004 A CN2013104016004 A CN 2013104016004A CN 201310401600 A CN201310401600 A CN 201310401600A CN 103439164 A CN103439164 A CN 103439164A
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Abstract
The invention relates to a quick plant or soil water vacuum-extraction method based on microwave heating. The quick plant or soil water vacuum-extraction method specifically comprises sample pipe microwave heating and water vapor collection, and a connection pipeline, a vacuum system and an extraction system are provided. The process comprises the following steps: quickly putting samples preserved in a frozen state into sample pipes; connecting the sample pipes with the extraction system, and immersing the sample pipes into a liquid nitrogen tank; mounting collection pipes and confirming that the system does not have gas leakage; opening connection valves between the extraction system and the vacuum system and performing vacuumizing; when a vacuum value is lower than 50mTorr, closing the connection valves, so that a mutually communicated high-vacuum closed system can be formed through the sample pipes and the collection pipes; then putting the sample pipes into the liquid nitrogen tank containing liquid nitrogen in a microwave heating cavity, and enabling the collection pipes to be immersed into the liquid nitrogen; switching on a power supply of a microwave heater to start to heat the samples, wherein the collection pipes collect water, which is obtained by evaporation of heating, in the sample pipes; after the water in a plant or soils is completely extracted, taking down the collection pipes, and sealing an opening through a sealing film. The quick plant or soil water vacuum-extraction method is used for D/H and 16O/18O measurement.
Description
Technical field
The present invention relates to a kind of plant or soil moisture fast vacuum method for extracting based on microwave heating, be specifically related to a kind of method for extracting of the moisture for Stable Isotopic Analysis.
Background technology
In plant, the main source of hydrogen and oxygen is water, and the moisture that plants can utilize is mainly from precipitation, the holard, runoff (comprising snow melt) and underground water.The holard, runoff and underground water is at first also all from precipitation, but because the seasonal variations of soil moisture input, evaporation or the difference between soil body moisture and underground water of surface layer make soil moisture produce the isotopics gradient.In general, root system of plant absorbs moisture process and isotopic fractionation does not all occur xylem Water Transportation process subsequently, root with stem in δ D, the δ of water
18δ D, the δ of the water that can absorb for plant in O value and soil
18the O value is close.Therefore can determine the absorption of root system to the holard of separate sources by the isotope ratio of analyzing axis water, understand further the activity of root in soil profile and the difference of plant to the utilization of moisture in natural community.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 moisture that utilizes under varying environment the degree of depth and to the plant of using two above water sources can be quantitatively its shared ratio in the water source that utilizes; But also can study plant water use variation in time, this point is only unascertainable by analyzing the distributions of root system of plant in soil profile.Another vital role of isotope technology is to determine that in soil which Activities of Some Plants root system is the active regions that absorbs 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 the soil layer of its existence, up to the present other method is 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 are the outer wrap electric-heating-wire-heating samples adopted at vacuum specimen tube, owing to being high vacuum in sample hose, have intercepted heat and have conducted to sample, make extraction efficiency not high.Take plant stem as example, and the time that heating is extracted surpasses 2 hours could be complete by the plant moisture extracting.Existing apparatus is to be made by the horminess glass tube sweat soldering in addition, in use, very easily damages.The problem existed for existing apparatus, the present invention proposes new technical scheme more efficiently.
Summary of the invention
The object of the invention is to, a kind of plant or soil moisture fast vacuum method for extracting based on microwave heating is provided, the method is by sample collection, the system leak detection, freezing, vacuumize and heat extraction steps and complete, its process is that the sample that is kept at freezing state is packed in sample hose fast, 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 of opening extraction system and vacuum system vacuumizes, when vacuum values lower than 50mTorr, close the connection valve of extraction system and vacuum system, make sample hose and collection tube 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 the microwave applicator power supply and start heated sample, collect the moisture that is heated and evaporates in collection tube, after the complete extracting of sample moisture, collection tube is taken off from sample, with the sealed membrane sealing, for D/H
16o/
18o measures.
A kind of plant or soil moisture fast vacuum method for extracting based on microwave heating of the present invention, 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: collection can be extracted the plant of 0.2-1.0ml water or the sample of soil, in the sample bottle of should packing into immediately after sample collection, seals and freezing preservation;
B, system leak detection: sample hose (1) is connected with extraction system (10) respectively with collection tube (2), extraction system (10) is connected with vacuum system (14), open vacuum pump (3), when vacuum tightness during 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 to the liquid nitrogen tank (11) of microwave heating chamber (5), and added liquid nitrogen in liquid nitrogen tank (11), sample hose (1) is immersed in to 10-20 minute in liquid nitrogen fully;
D, sample continue freezing, open the vacuum pump switch (12) on vacuum pump (3), open the connection valve (4) be fixed on vacuum system (14) simultaneously, treat the whole system vacustat, and low vacuum, in 50-60mTorr, is closed connection valve (4);
E, the heating extracting, first collection tube (2) is put into to 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 heat energy heated sample pipe (1), automatically control microwave output by sample hose (1) temperature, make sample hose (1) temperature remain on 105-120 ℃, collection tube (2) is collected the moisture that is heated and evaporates from sample hose (1), until moisture is entered in collection tube (2) by complete extracting, in collection process according to the height of collecting moisture, adjust the height of liquid nitrogen in liquid nitrogen tank (8) by continuous interpolation liquid nitrogen, after the heating extracting completes, collection tube (2) is taken off, with cap for special purpose, seal rapidly, stored refrigerated is measured.
In step c by step a sample from refrigerator-freezer takes out, need at room temperature place somewhat and plant, remove diaphragm seal, dry the moisture of sample hose outer wall, and then sample put into to sample hose (1).
Moisture acquisition time in step e in plant roots or stem sample is 30-45 minute, and the moisture acquisition time in pedotheque is 20-30 minute.
In step e, the sample heating-up temperature is measured by infrared mode, and the power stage of FEEDBACK CONTROL microwave, ultrasound wave or far infrared wave, makes sample temperature be controlled at 105-120 ℃.
In the device that described method relates to, an end in vacuum system (14) connects respectively vacuum meter (9) and vacuum pump (3), the other end is the fixing impartial vacuum tube be connected with extraction system (10) of arranging respectively, be provided with valve (4) on vacuum tube, one end of extraction system (10) is connected with impartial several sample hoses (1) of arranging, and its other end is connected with impartial several collection tubes (2) of arranging.
In the device that described method relates to, the fixing microwave applicator (7) in the bottom of microwave heating chamber (5) one sides, sample hose (1) is put into liquid nitrogen tank (11), again liquid nitrogen tank (11) is put into to microwave heating chamber (5), be fixed with infrared sensor (6) in the lower end of sample hose (1), collection tube (2) is put 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) screw and are connected with sample hose (1) and collection tube (2) employing screw socket mode.
Plant, soil moisture fast vacuum method for extracting based on microwave heating of the present invention, wherein:
In sample collection, sampling quantity is determined according to the water cut assessment of plant or soil, generally can extract 0.2-1.0ml water, is advisable, and in the sample hose (1) of should packing into immediately after sample collection, seals and freezing preservation;
In the system leak detection, before extracting moisture, whether check system is airtight, concrete grammar is that sample hose (1) all is connected with extraction system (10) respectively with collection tube (2), open vacuum pump (3) and connect system, when vacuum tightness during lower than 60mTorr, close vacuum, whether the vacuum meter (9) of observing extraction system changes;
Freezing sample, after systems inspection completes, take out sample hose (1), put into after gathering and the sample of freezing preservation, again sample hose (1) is put into to microwave heating chamber (5), liquid nitrogen tank (11) adds liquid nitrogen, and sample hose (1) is immersed in to 10-20 minute in liquid nitrogen fully;
Vacuumize: sample continues freezing, open successively connection valve (4) fixing between vacuum pump switch (12) and vacuum system (14) and extraction system (10), treat the whole system vacustat, generally vacuum tightness will, lower than 50-60mTorr, be closed connection valve (4);
The heating extracting, first collection tube (2) is put into to the liquid nitrogen tank (8) that liquid nitrogen is housed, open microwave heating controller (7) power supply (13) heated sample pipe (1), pipe (1) temperature is controlled microwave output automatically per sample, make sample hose (1) temperature remain on 105-120 degree centigrade until the extracting fully of moisture quilt, the moisture that sample hose (1) evaporates is entered in collection tube (2) by extracting, this process is different and determine per sample, plant roots generally, stem is 30-45 minute, soil is 20-30 minute, adjust the height of liquid nitrogen tank (8) in collection process according to the situation of collecting moisture, and continuous annex solution nitrogen, after the heating extracting completes, collection tube (2) is taken off, with cap for special purpose, seal rapidly, stored refrigerated is for D/H,
16o/
18o measures.
For validity and the feasibility of checking microwave heating extraction process, by test result can further obtain demonstration in Table:
| Sequence number | The technical indicator title | Parameter before functional development | Estimate the parameter reached after functional development |
| 1 | The extracting time | 120-150 minute | 30-45 minute |
| 2 | Sample number | 5-6/time | 8-16/ |
| 3 | The |
6×10-3mbar·L/sec | 2×10-3mbar·L/sec |
| 4 | End vacuum pressure: | <1.5mbar | <1.2mbar |
Plant or soil moisture fast vacuum method for extracting based on microwave heating of the present invention, 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, for extensive sample is tested and is laid a good foundation fast, the invention provides a kind of quick, easy, economic plant, soil moisture extracting method, the present invention is described in detail in detail by the following examples.
The accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation.
Embodiment
The extracting of embodiment 1(plant moisture fast vacuum)
Preparation facilities: the end in vacuum system 14 connects respectively vacuum meter 9 and vacuum pump 3, the other end is the fixing impartial vacuum tube be connected with extraction system 10 of arranging respectively, be provided with valve 4 on vacuum tube, several sample hoses 1 employing screw socket modes that one end of extraction system 10 is arranged with equalization screw and are connected, and its other end screws and is connected with impartial several collection tubes 2 employing screw socket modes of arranging; The fixing microwave applicator 7 in the bottom of microwave heating chamber 5 one sides, sample hose 1 is put into liquid nitrogen tank 11, again liquid nitrogen tank 11 is put into to microwave heating chamber 5, the lower end of several sample hoses 1 of arranging in equalization is fixed with respectively infrared sensor 6, and collection tube 2 is put into liquid nitrogen tank 8; The pipeline of extraction system 10 is formed by the materials processing of monoblock melting TFE copolymer;
Sample collection: collection can be extracted the plant sample of 0.2-1.0ml water, in the sample bottle of should packing into immediately after sample collection, seals and freezing preservation;
System leak detection: sample hose 1 is connected with extraction system 10 respectively with collection tube 2, extraction system 10 is connected with vacuum system 14, open vacuum pump 3, when vacuum tightness during lower than 60mTorr, close vacuum pump 3, observe vacuum meter 9 in extraction system and whether change, if the speed that vacuum meter 9 readings raise is very fast, illustrative system gas leakage, inspection is got rid of to system fully airtight step by step;
Freezing sample: sample hose 1 is taken out, by the plant sample that gathers from refrigerator-freezer takes out, need at room temperature place somewhat and plant, remove diaphragm seal, and dry the moisture of outer wall, the plant sample in the sample bottle of packing into takes out, put into sample hose 1, again sample hose 1 is put into to the liquid nitrogen tank 11 of microwave heating chamber 5, and added liquid nitrogen in liquid nitrogen tank 11, sample hose 1 is immersed in to 10-20 minute in liquid nitrogen fully;
Sample continues freezing, open the vacuum pump switch 12 on vacuum pump 3, open the connection valve 4 be fixed on vacuum system 14 simultaneously, treat the 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, not gas leakage of system, if the speed that vacuum meter 9 readings raise is very fast, illustrative system gas leakage, inspection is got rid of to system fully airtight step by step;
The heating extracting, before heating, close connection valve 4, adopt the screw socket mode to screw extraction system 10 and connect collection tube 2, again collection tube 2 is put into to liquid nitrogen tank 8, and add liquid nitrogen in liquid nitrogen tank 8, then open the power supply 13 on microwave heating controller 7, adopt microwave, ultrasound wave or far infrared wave produce heat energy heated sample pipe 1, manage per sample 1 temperature and automatically control microwave output, make sample hose 1 temperature remain on 105-120 ℃, collection tube 2 is collected the moisture that is heated and evaporates from sample hose 1, until moisture is entered in collection tube 2 by complete extracting, plant roots, it is 30-45 minute that stem is collected the moisture time, in collection process according to the height of collecting moisture, adjust the height of liquid nitrogen in liquid nitrogen tank 8 by continuous interpolation liquid nitrogen, after the heating extracting completes, collection tube 2 is taken out, with cap for special purpose, seal rapidly, while Deng the moisture of collecting, all being melted into aqueous water, water transport is arrived in the ampoule of sealing, and seal with sealed membrane, whole process is wanted rapidly, guarantee that moisture does not leak and evaporation, and with numeral or English numbered samples, stored refrigerated is measured.Attention: must be careful in the process of handling sample hose 1 and collection tube 2, avoid the damage system.
The extracting of embodiment 2(soil moisture fast vacuum)
Preparation facilities is undertaken by embodiment 1;
Sample collection: collection can be extracted the pedotheque of 0.2-1.0ml water, in the sample bottle of should packing into immediately after sample collection, seals and freezing preservation;
System leak detection: sample hose 1 is connected with extraction system 10 respectively with collection tube 2, extraction system 10 is connected with vacuum system 14, open vacuum pump 3, when vacuum tightness during lower than 60mTorr, close vacuum pump 3, observe vacuum meter 9 in extraction system and whether change, if the speed that vacuum meter 9 readings raise is very fast, illustrative system gas leakage, inspection is got rid of to system fully airtight step by step;
Freezing sample: sample hose 1 is taken out, by the pedotheque that gathers from refrigerator-freezer takes out, need at room temperature place somewhat and plant, remove diaphragm seal, and dry the moisture of outer wall, will put into glass wool on pedotheque to avoid that soil particle is extracted into to system, put into sample hose 1, again sample hose 1 is put into to the liquid nitrogen tank 11 of microwave heating chamber 5, and added liquid nitrogen in liquid nitrogen tank 11, sample hose 1 is immersed in to 10-15 minute in liquid nitrogen fully;
Sample continues freezing, open the vacuum pump switch 12 on vacuum pump 3, open the connection valve 4 be fixed on vacuum system 14 simultaneously, treat the 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, not gas leakage of system, if the speed that vacuum meter 9 readings raise is very fast, illustrative system gas leakage, inspection is got rid of to system fully airtight step by step;
The heating extracting, before heating, close connection valve 4, adopt the screw socket mode to screw the collection tube 2 of connection extraction system 10, again collection tube 2 is put into to liquid nitrogen tank 8, and add liquid nitrogen in liquid nitrogen tank 8, then open the power supply 13 on microwave heating controller 7, adopt microwave, ultrasound wave or far infrared wave produce heat energy heated sample pipe 1, manage per sample 1 temperature and automatically control microwave output, make sample hose 1 temperature remain on 105-120 ℃, collection tube 2 is collected the moisture that is heated and evaporates from sample hose 1, until moisture is entered in collection tube 2 by complete extracting, moisture acquisition time in pedotheque is 20-30 minute, in collection process according to the height of collecting moisture, adjust the height of liquid nitrogen in liquid nitrogen tank 8 by continuous interpolation liquid nitrogen, after the heating extracting completes, collection tube 2 is taken out, with cap for special purpose, seal rapidly, while Deng the moisture of collecting, all being melted into aqueous water, water transport is arrived in the ampoule of sealing, and seal with sealed membrane, whole process is wanted rapidly, guarantee that moisture does not leak and evaporation, and with numeral or English numbered samples, stored refrigerated is measured.Attention: must be careful in the process of handling sample hose 1 and collection tube 2, avoid the damage system.
Claims (7)
1. plant or the soil moisture fast vacuum method for extracting based on microwave heating, 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), 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: collection can be extracted the plant of 0.2-1.0ml water or the sample of soil, in the sample bottle of should packing into immediately after sample collection, seals and freezing preservation;
B, system leak detection: sample hose (1) is connected with extraction system (10) respectively with collection tube (2), extraction system (10) is connected with vacuum system (14), open vacuum pump (3), when vacuum tightness during lower than 60 mTorr, 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 to the liquid nitrogen tank (11) of microwave heating chamber (5), and added liquid nitrogen in liquid nitrogen tank (11), sample hose (1) is immersed in to 10-20 minute in liquid nitrogen fully;
D, sample continue freezing, open the vacuum pump switch (12) on vacuum pump (3), open the connection valve (4) be fixed on vacuum system (14) simultaneously, treat the whole system vacustat, and low vacuum, in 50-60 mTorr, is closed connection valve (4);
E, the heating extracting, first collection tube (2) is put into to 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 heat energy heated sample pipe (1), automatically control microwave output by sample hose (1) temperature, make sample hose (1) temperature remain on 105-120 ℃, collection tube (2) is collected the moisture that is heated and evaporates from sample hose (1), until moisture is entered in collection tube (2) by complete extracting, in collection process according to the height of collecting moisture, adjust the height of liquid nitrogen in liquid nitrogen tank (8) by continuous interpolation liquid nitrogen, after the heating extracting completes, collection tube (2) is taken off, with cap for special purpose, seal rapidly, stored refrigerated is measured.
2. method according to claim 1, is characterized in that in step c step a sample need at room temperature placing somewhat and planting from refrigerator-freezer takes out, and removes diaphragm seal, dries the moisture of sample hose outer wall, and then sample is put into to sample hose (1).
3. method according to claim 1, is characterized in that the moisture acquisition time in plant roots in step e or stem sample is 30-45 minute, and the moisture acquisition time in pedotheque is 20-30 minute.
4. method according to claim 1, is characterized in that in step e, the sample heating-up temperature is measured by infrared mode, and the power stage of FEEDBACK CONTROL microwave, ultrasound wave or far infrared wave, makes sample temperature be controlled at 105-120 ℃.
5. method according to claim 1, it is characterized in that in the related device of the method, an end in vacuum system (14) connects respectively vacuum meter (9) and vacuum pump (3), the other end is the fixing impartial vacuum tube be connected with extraction system (10) of arranging respectively, be provided with valve (4) on vacuum tube, one end of extraction system (10) is connected with impartial several sample hoses (1) of arranging, and its other end is connected with impartial several collection tubes (2) of arranging.
6. method according to claim 1, it is characterized in that in the related device of the method, the fixing microwave applicator (7) in the bottom of microwave heating chamber (5) one sides, sample hose (1) is put into liquid nitrogen tank (11), again liquid nitrogen tank (11) is put into to microwave heating chamber (5), be fixed with infrared sensor (6) in the lower end of sample hose (1), collection tube (2) is put into liquid nitrogen tank (8).
7. method according to claim 1, it is characterized in that in the related device of the method, 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) screw and are connected with sample hose (1) and collection tube (2) employing screw socket mode.
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| CN106770375A (en) * | 2016-12-31 | 2017-05-31 | 新疆拓荒者信息科技有限公司 | A kind of microwave moisture content sampling instrument |
| CN106701894A (en) * | 2017-02-10 | 2017-05-24 | 盎亿泰地质微生物技术（北京）有限公司 | Preprocessing method for soil sample for detection of hydrocarbon oxidizing bacteria in oil and gas microbial exploration |
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| 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 |
| 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 |
| CN111983188A (en) * | 2020-08-13 | 2020-11-24 | 中国科学院南京地理与湖泊研究所 | Soil water extraction and stable isotope composition analysis 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 |
| CN113125470A (en) * | 2021-04-20 | 2021-07-16 | 南京晓庄学院 | Utilize microwave remote sensing monitoring soil moisture equipment |
| 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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