CN103592248A - Soil water content colorimetric-determination method - Google Patents

Soil water content colorimetric-determination method Download PDF

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Publication number
CN103592248A
CN103592248A CN201310643783.0A CN201310643783A CN103592248A CN 103592248 A CN103592248 A CN 103592248A CN 201310643783 A CN201310643783 A CN 201310643783A CN 103592248 A CN103592248 A CN 103592248A
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China
Prior art keywords
absorbance
soil
moisture content
soil moisture
solution
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CN201310643783.0A
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杨张青
胡小宁
段铁城
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HENAN NONGDA XUNJIE TEST TECHNOLOGY Co Ltd
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HENAN NONGDA XUNJIE TEST TECHNOLOGY Co Ltd
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Abstract

The invention relates to a soil water content colorimetric-determination method. The soil water content colorimetric-determination method comprises the following steps of 1, carrying out extraction on a soil sample to be detected by a cobalt chloride hexahydrate organic solution having a concentration of 0.1-30g/L as a color developing agent to remove solids and to obtain a solution to be detected, and determining the absorbance of the solution to be detected at the wavelength of 380-680nm, and 2, searching the corresponding soil water content in a built absorbance-soil water content standard curve according to the absorbance obtained by the step 1, or substituting the absorbance obtained by the step 1 into the built absorbance-soil water content standard curve equation and calculating the corresponding soil water content. The soil water content colorimetric-determination method is not influenced by soil types, components, unit weight and disturbance, has an error ratio below 2% is a pervasive soil moisture content detection method, is suitable for fast determination in the field and is suitable for soil water fast-determination in the laboratory.

Description

The colorimetric estimation method of soil moisture content
Technical field
The present invention relates to the assay method of soil moisture content, be specifically related to a kind of colorimetric estimation method of soil moisture content.
Background technology
" setting up a water-saving society, Water Saving Agriculture Development " is that national Major Strategic is disposed.Monitoring farmland moisture condition changes, and carries out water-saving irrigation significant to ensureing China's grain security.Field soil water content detection mode has the distributed monitoring of imbedding at present, and portable moisture detects two classes.Most frequency domain reflection or Time Domain Reflectometry formula Moisture Meter that adopt dielectric principle.Its detection speed is fast, simple to operate, but accuracy of detection is subject to the impact of soil type, composition, unit weight, soil disturbance etc., for flush type, applying this error can be by calibrating and solves with laboratory method contrast on the spot, and for portable use, usually cause even 10~20% significant errors.
The research of soil moisture fast measurement technique, foreign scholar studies starting early.Nineteen twenty-two, Gardner just takes to the research of tensiometer Fast Measurement unsaturated soil tension force; Nineteen thirty-nine Shawbauer starts to utilize the thermoelectricity line resistance of placing into the soil to change the research of carrying out soil moisture Fast Measurement; Nineteen fifty, neutron attenuation method starts to be applied to Quick Measurement soil moisture content; 1976, first Topp and Davis introduced time domain reflectometry the research of soil moisture Quick Measurement; Nineteen eighty-three, Hainsworth test utilizes X ray Quick Measurement soil moisture; 1991, Walley utilized near-infrared method Quick Measurement soil moisture content to obtain certain achievement in research.
In recent years, the soil moisture fast measurement technique of China also has made some progress successively, from traditional oven drying method, progressively develop into fast measurement technique, a lot of scholars and expert try hard to find a kind of applicable China's actual conditions, good and cheap, succinct Fast-Measurement of Soil Water Content easily.Late 1970s Qi, Xian Electronics Science and Technology University has developed SVJ-3 type microwave moisture meter; Nineteen sixty, China also started to utilize in laboratory gamma-rays scenography to measure soil moisture content; Nineteen eighty-two, impedance method is measured soil moisture content and has also been obtained application; In latter stage in 20th century, there is the quick soil surveying technology based on standing wave ratio principle, as time-domain reflectomer, frequency domain reflectometer etc.But these methods and device therefor complicated (microwave method, gamma-rays, NEUTRON METHOD, Near-Infrared Absorption Method) or limited to the adaptability of soil type, and the calibration operation complicated (time domain method, frequency domain method, standing wave ratio method) before using.As everyone knows, soil is a kind of nonuniformity being comprised of inert solid, active solid, solute, gas and water, heterogeneous, dispersion and granular porous system.Because its physical characteristics is complicated, Spatial Variability is large, has caused the difficulty of utilizing above-mentioned Physical to measure moisture.
Within 1963, yellow uncommon pottery is used the moisture (chemistry world 1963.4) in anhydrous cupric sulfate colorimetric method for determining kerosene, in China, propose first to carry out determination of moisture with colourimetry, 1980 Nian Lu galaxy of literary talents are used waterless cobaltous chloride colorimetric method for determining soil moisture (agricultural mechanical journal 1980.12), first colourimetry is used for to determining soil moisture, its principle is that waterless cobaltous chloride is met water pulverize redness, and its reaction is: CoCl 2+ 6H 2o=[Co (H 2o) 6] C1 2, along with the ratio of water and solvent acetone strengthens, colorimetric solution color by blueness to pink conversion.
Colorimetric method for determining soil moisture precision is high, range greatly, be not substantially subject to the impact of soil types, unit weight, proportion and chemical composition etc., but within more than 30 year, effectively do not promoted, its main cause is: the hydration form of cobalt chloride has multiple and phase co-conversion (CoCl 2h 2o (bluish violet) CoCl 22H 2o (aubergine) CoCl 26H 2o (pink) [CoCl 4] 2-(blueness)); The preparation process that cobalt chloride removes water of crystallization needs 220 ℃ to dry 21 hours, makes trouble, and in preservation process, is easy to the moisture absorption after dehydration; Changing than toner color of different water cut, maximum absorption wavelength changes; Soil contrast toner has suction-operated, soil moisture content with than the non-linear relation of the absorbance of toner; Adopt depigmenting agent and centrifugal method, also limited the use occasion of the method and rapidity etc.Perhaps just because of CoCl 2colour developing influence factor too much, belong to reversible balanced reaction, technology is ripe far away, having caused rarely seenly between more than 30 year has a correlative study report.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of colorimetric estimation method that is not subject to the soil moisture content that the factors such as soil type, composition, unit weight, disturbance affect.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The colorimetric estimation method that designs a kind of soil moisture content, comprises the steps:
(1) color solution preparation: get CoCL2 6H2O and be dissolved in organic solvent and be mixed with the organic solution that concentration is 0.1~30g/L, be developer;
(2) liquid soil mixes: get described developer native than mixing by the liquid of 1g:8~12mL with pedotheque to be measured;
(3) native liquid is separated: separated by upper step gained potpourri, remove solid matter, and obtain solution to be measured;
(4) absorbance detection: under the wavelength of 380~680nm, measure the absorbance of above-mentioned solution to be measured;
(5) result is calculated: according to upper step gained absorbance, on absorbance-soil moisture content typical curve of having set up, search corresponding soil moisture content; Or upper step gained absorbance is updated to absorbance-soil moisture content typical curve equation of having set up, tries to achieve corresponding soil moisture content.
In the present invention with cobalt chloride hexahydrate [Co (H 2o) 6] Cl 2blue organic solution as developer, do not carry out drying and dehydrating, can make to reduce decades of times than the preparation time of toner, with [Co (H 2o) 6] Cl 2the CoCl that proposes of the reaction mechanism Yu Lu galaxy of literary talent that sets up of organic solution 2+ 6H 2o=[Co (H 2o) 6] Cl 2difference, but meet equally determination of moisture requirement:
Cobalt chloride hexahydrate is met water may there are two kinds of reversible reaction equilibrium systems:
[Co (H 2o) 6] Cl 2(Chinese red) ten 2EtOH=Co (EtOH) 2Cl 2(blueness)+6H 2o,
In soil, there is Cl -while existing, its equilibrium system is
[Co (H 2o) 6] 2++ 4Cl -(Chinese red)=[COCl 4] 2-+ 6H 2o (blueness)
When moisture increases, balanced type is carried out left, and color is changed to pale red by blueness, makes to shoal than toner blueness, and under certain wavelength, its absorbance and water percentage are the funtcional relationship of negative correlation.
In described step (1), described organic solvent is at least one in acetone, ethanol, ether.
In described step (4), with photoelectric colorimetry instrument, measuring before the absorbance of described solution to be measured, first to prepare penetrability that the solvent of described color solution adjusts photoelectric colorimetry instrument to zero.
The developer of known aqueous rate of take is titer, measure its absorbance and with the dulling luminosity ratio of the typical curve of this titer compared with calculation correction coefficient, instrument and medicament are proofreaied and correct.
The method for building up of described typical curve is as follows:
(1) get the pedotheque Mg of the different known aqueous rate of certain sample size;
(2) according to colorimetric estimation method claimed in claim 1, measure the corresponding absorbance of pedotheque of each known aqueous rate;
(3), according to the corresponding absorbance of the known aqueous rate of pedotheque and upper step gained thereof, matching returns out curvilinear equation C=f (Ax 0), be typical curve equation.
The present invention has actively useful effect:
1. chromogenic agent scope of the present invention very wide (0.5~30g/L), between weight moisture capacity 0~40%, far surpasses specific retesion of soil 30~35%), determination of moisture scope can be extended to the speed survey of paddy field soil sample; The present invention is used more stable than toner concentration scope blue primary color under 0~60 ℃ of environment temperature; Red on the impact of absorbance in allowed band;
2. survey moisture method of the present invention is not subject to the impact of soil type, composition, unit weight, disturbance etc., and error can be controlled in below 2%, is a kind of universality soil moisture content detection method; Both be applicable to on-the-spot speed in the wild and surveyed, be also applicable to laboratory Fast Measurement soil sample moisture.
3. high, the soil sample that can measure low-water-content of the inventive method accuracy of detection, and this just conventional dielectric method be difficult to accomplish; It is microwave heating method that current laboratory is not the most subject to the survey water method that great soil group, unit weight affect, but before and after measuring, all wants the cooperation of precision balance, limited efficiency, and tool is portable; The inventive method is no more than 1% in the absolute error in low water content interval, and speed is fast, efficiency is high, is combined can in 3~5 minutes, completes test with centrifuge method; Can make separately soil moisture measure, also can be used as the additional function of soil nutrient tacheometer.
4. working curve modeling of the present invention can be directly with the filtrate after native liquid separation, can process without colour killing, also can build working curve without the titer of analytical grade reagent preparation, both reduce operation and cost that colour killing is processed, substantially get rid of again the error that soil sample contrast toner adsorption band comes.
5. the present invention proposes a method of cooing titer correction instrument and medicament error of developer, to eliminate the inconsistent error of bringing of real work curve under the built-in working curve of instrument and service condition; When formulating working curve, measure the titer absorbance of known moisture levels, in actual measurement, measure the variation of this titer absorbance, calculate calibration factor, for revising test data; The present invention can make typical curve universalization, makes user exempt typical curve modeling process, improves operating process efficiency and measuring accuracy.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
The colorimetric estimation method of 1 one kinds of soil moisture contents of example, comprises the steps:
(1) developer: take 10.000g cobalt chloride in 1L volumetric flask, dissolve and be settled to 1L with ethanol, shake up standbyly, survey its absorbance;
(2) working curve: prepare respectively water cut and be the mark liquid after 0%, 5%, 10%, 15%, 20%, 25%, 30% colour developing, and on spectrophotometer, test its absorbance, take absorbance as horizontal ordinate, take water cut as ordinate, drawing curve, working curve equation is: y=0.2348x 2-0.6706x+0.5018;
(3) take about 1.00g fresh soil sample in color comparison tube, draw developer 10mL in color comparison tube, firmly shake up, soil is spread out, with filter paper, this soil sample liquid to be measured is filtered in cuvette, standby;
(4) during with survey soil, the developer of known aqueous rate is done the absorbance that titer records, and the ratio of the absorbance of the same water percentage titer during with working curve processed, proofreaies and correct this working curve.This trial correction coefficient is 1, and after proofreading and correct, working curve equation does not become.
(5) measure the absorbance of liquid to be measured, after the automatic substitution of the absorbance of soil sample is proofreaied and correct, the equation of working curve, obtains y=0.643 (mL)
(6) water cut of soil sample is 16.8%.
Example 2: a kind of colorimetric estimation method of soil moisture content, comprises the steps:
(1) developer: take 3.200g cobalt chloride in 1L volumetric flask, with acetone solution and be settled to 1L, shake up standby.
(2) working curve: prepare respectively water cut and be the mark liquid after 0%, 2%, 4%, 6%, 8%, 10%, 15%, 20% colour developing, and on spectrophotometer, test its absorbance, take absorbance as horizontal ordinate, take water cut as ordinate, drawing curve, working curve equation is: y=24.38x 2-48.374x+23.586.
(3) take about 2.000g fresh soil sample in color comparison tube, draw developer 20mL in color comparison tube, firmly shake up, soil is spread out, with filter paper, this soil sample liquid to be measured is filtered in cuvette, standby.
(4) during with survey soil, the developer of known aqueous rate is done the absorbance that titer records, and the ratio of the absorbance of the same water percentage titer during with working curve processed, proofreaies and correct this working curve.This trial correction coefficient is that after 1. corrections, working curve equation does not become.
(5) on spectrophotometer, test the absorbance of above soil sample, absorbance is 0.25.By the equation of the absorbance of soil sample 0.25 substitution working curve, the water cut of trying to achieve this soil sample is 0.130 (mL)
(6) water cut of soil sample is 6.95%.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements, all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.

Claims (5)

1. a colorimetric estimation method for soil moisture content, comprises the steps:
(1) color solution preparation: get CoCL2 6H2O and be dissolved in organic solvent and be mixed with the organic solution that concentration is 0.1~30g/L, be developer;
(2) liquid soil mixes: get described developer native than mixing by the liquid of 1g:8~12mL with pedotheque to be measured;
(3) native liquid is separated: separated by upper step gained potpourri, remove solid matter, and obtain solution to be measured;
(4) absorbance detection: under the wavelength of 380~680nm, measure the absorbance of above-mentioned solution to be measured;
(5) result is calculated: according to upper step gained absorbance, on absorbance-soil moisture content typical curve of having set up, search corresponding soil moisture content; Or upper step gained absorbance is updated to absorbance-soil moisture content typical curve equation of having set up, tries to achieve corresponding soil moisture content.
2. the colorimetric estimation method of soil moisture content according to claim 1, is characterized in that, in described step (1), described organic solvent is at least one in acetone, ethanol, ether.
3. the colorimetric estimation method of soil moisture content according to claim 1, it is characterized in that, in described step (4), with photoelectric colorimetry instrument, measuring before the absorbance of described solution to be measured, first to prepare penetrability that the solvent of described color solution adjusts photoelectric colorimetry instrument to zero.
4. the colorimetric estimation method of soil moisture content according to claim 3, it is characterized in that, the developer of known aqueous rate of take is titer, measure its absorbance and with the dulling luminosity ratio of the typical curve of this titer compared with calculation correction coefficient, instrument and medicament are proofreaied and correct.
5. the colorimetric estimation method of soil moisture content according to claim 1, is characterized in that, the method for building up of described typical curve is as follows:
(1) get the pedotheque Mg of the different known aqueous rate of certain sample size;
(2) according to colorimetric estimation method claimed in claim 1, measure the corresponding absorbance of pedotheque of each known aqueous rate;
(3) according to the corresponding absorbance matching of the known aqueous rate of pedotheque and upper step gained thereof, return out curvilinear equation C=f (Ax 0), be typical curve equation.
CN201310643783.0A 2013-12-05 2013-12-05 Soil water content colorimetric-determination method Pending CN103592248A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN104331639A (en) * 2014-12-01 2015-02-04 中国矿业大学 Indirect soil moisture content obtaining and rapid evaluation method
CN107027485A (en) * 2017-04-28 2017-08-11 道真自治县茂峰中药材发展有限公司 A kind of implantation methods of safflower
CN107047196A (en) * 2017-04-28 2017-08-18 道真自治县云星种植有限责任公司 A kind of implantation methods of the bark of official magnolia
CN109030479A (en) * 2018-08-01 2018-12-18 吴旌旗 A kind of simple type flowerpot soil moisture content detection device
CN109115699A (en) * 2017-06-23 2019-01-01 河南农大迅捷测试技术有限公司 A kind of soil moisture content detection method based on colorimetric estimation technology
CN110220856A (en) * 2019-06-05 2019-09-10 常州大学 The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104331639A (en) * 2014-12-01 2015-02-04 中国矿业大学 Indirect soil moisture content obtaining and rapid evaluation method
CN104331639B (en) * 2014-12-01 2017-09-05 中国矿业大学 A kind of soil moisture content indirect gain and fast appraisement method
CN107027485A (en) * 2017-04-28 2017-08-11 道真自治县茂峰中药材发展有限公司 A kind of implantation methods of safflower
CN107047196A (en) * 2017-04-28 2017-08-18 道真自治县云星种植有限责任公司 A kind of implantation methods of the bark of official magnolia
CN109115699A (en) * 2017-06-23 2019-01-01 河南农大迅捷测试技术有限公司 A kind of soil moisture content detection method based on colorimetric estimation technology
CN109030479A (en) * 2018-08-01 2018-12-18 吴旌旗 A kind of simple type flowerpot soil moisture content detection device
CN110220856A (en) * 2019-06-05 2019-09-10 常州大学 The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil
CN110220856B (en) * 2019-06-05 2021-07-27 常州大学 Method for detecting content of chloride ions in electrodeposition liquid of electrolytic copper foil by flow injection method

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