CN111189743A - Experimental device for measuring content of carbonate in soil and operation method - Google Patents
Experimental device for measuring content of carbonate in soil and operation method Download PDFInfo
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- CN111189743A CN111189743A CN202010147074.3A CN202010147074A CN111189743A CN 111189743 A CN111189743 A CN 111189743A CN 202010147074 A CN202010147074 A CN 202010147074A CN 111189743 A CN111189743 A CN 111189743A
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- 239000002689 soil Substances 0.000 title claims abstract description 60
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 60
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 claims description 4
- 230000008030 elimination Effects 0.000 claims description 3
- 238000003379 elimination reaction Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 239000007789 gas Substances 0.000 description 43
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000005259 measurement Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000003221 volumetric titration Methods 0.000 description 3
- 229910021532 Calcite Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 239000002681 soil colloid Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 229910052806 inorganic carbonate Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000004856 soil analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/18—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by allowing the material to react
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses an experimental device for determining the content of carbonate in soil and an operation method, wherein the device comprises a gas generating device and a gas collection measuring device which are connected, wherein the gas generating device comprises a suction filter bottle, a large rubber plug arranged on the suction filter bottle, an acid burette and a rubber tube; the gas collection measuring device comprises a left gas measuring pipe and a right gas measuring pipe, hoses are respectively sleeved at bottom pipe orifices of the left gas measuring pipe and the right gas measuring pipe, the hoses at the bottom ends of the left gas measuring pipe and the right gas measuring pipe are connected through a three-way pipe with a piston, and a beaker is placed below the three-way pipe; the gas production device is connected with the gas collection measuring device through a U-shaped test tube. The device adopts common instruments in a common chemical laboratory as parts, has simple structure, easy assembly, high air tightness, convenient experimental operation and accurate and stable experimental result, and can be well applied to the determination of the content of the carbonate in the soil.
Description
Technical Field
The invention relates to the technical field of soil research, in particular to an experimental device for measuring the content of carbonate in soil in a common chemical laboratory and an operation method.
Background
In the research of soil, the physicochemical property of soil is often needed to be measured, and in the soil detection, the soil is often measured firstlyThe content of the soil carbonate is one of important bases for judging the basic properties and fertility level of the soil because the soil carbonate has close relations with the soil pH value, the existence form and the effective degree of soil nutrient elements and the soil colloid properties. In addition, in soil analysis work, the carbonate content of soil is the basis for selecting an analysis method when measuring a plurality of items. The inorganic carbonate in the soil is mainly insoluble calcite (CaCO)3) And dolomite (CaCO)3·MgCO3) Generally, calcite is taken as the main component, so that the determination of the carbonate content of the soil is mainly to determine the calcium carbonate content of the soil.
The analysis methods commonly used for measuring soil carbonate at home and abroad for a long time include a volumetric titration method and an air-measuring method. The volumetric titration method is to add a certain amount of standard acid solution into the soil to make it react with carbonate, and the excessive acid is dripped back with standard alkali solution, and the method does not need special equipment and is often used as a rapid measurement method, but the method has high result and large error, and is more obvious to saline-alkali soil, mainly because the hydrogen ions in the standard acid exchange with the metal cations on the soil colloid, so the consumed acid amount is not only the function of carbonate in the soil, which is the main problem of volumetric titration method. The gas method is to measure CO released by the reaction of soil sample and acid2The method has become a national standard method in western Europe, eastern Europe and other countries, has been taken as a professional standard recommended by the soil society in the United states, and has been listed as a national standard in the middle of the 80 s. The gas quantity method adopts a temperature atmospheric pressure correction calculation method which is inconvenient to operate, the temperature and the atmospheric pressure are required to be measured for conversion in each test, the equipment is complicated, the calculation is complex, and a soil sample and a reference substance (CaCO) are adopted3Reagent) CO production by plotting a standard curve2The volume is substituted into the direct calculation result, so that the equipment and the calculation process are simplified, the measurement precision is improved, and the gas method operation tends to be more standardized. In the prior literature and patent, most of the devices for measuring soil carbonate by gas method are based on CO generated by reaction2Calculating soil carbonate content by volume, e.g.Baoshidan who compiled in A book of soil Agrochemistry analysis (third edition) to determine CaCO by a set of gas method3The apparatus of (1). However, the currently disclosed device has many problems in equipment assembly or operation methods, the parts used by the device are numerous, the parts are not common in common chemical laboratories, the parts are difficult to collect and assemble, some parts need to be specially ordered, the purchase cost is high, the air tightness of the device is not easy to guarantee, the corresponding operation method has complicated flows and is not easy to master, the explanation of the operation steps and the test principle is incomplete and detailed, and the soil research work of the laboratory personnel in common chemical laboratories is greatly limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the experimental device and the operation method for measuring the content of the soil carbonate, the device adopts common instruments in a common chemical laboratory as parts, has simple structure and easy assembly, improves the integral air tightness of the device by simplifying the device, simplifies the experimental operation, provides complete and detailed operation steps and cautions, has accurate and stable experimental results after multiple times of experimental detection, and can be well applied to the measurement of the content of the soil carbonate.
The technical scheme adopted by the invention is as follows: an experimental device for measuring the content of carbonate in soil comprises a gas generating device and a gas collecting measuring device which are connected, wherein the gas generating device comprises a suction bottle, a large rubber plug arranged on the suction bottle, an acid burette and a rubber tube; the gas collection measuring device comprises a left gas measuring pipe and a right gas measuring pipe, hoses are respectively sleeved at bottom pipe orifices of the left gas measuring pipe and the right gas measuring pipe, the hoses at the bottom ends of the left gas measuring pipe and the right gas measuring pipe are connected through a three-way pipe with a piston, and a beaker is placed below the three-way pipe; the gas production device is connected with the gas collection measuring device through a U-shaped test tube.
Further, the one end of rubber tube is connected with the suction flask, and the other end is connected with the inlet end of U type test tube, the end of giving vent to anger of U type test tube is connected with left gas measuring pipe to it is sealed through little rubber buffer.
Further, the capacity of each of the left and right air measuring tubes is 100ml, and the set height of the left and right air measuring tubes is maintained on the same horizontal line.
Further, a hole is formed in the large rubber plug on the suction bottle, and the aperture of the hole is slightly smaller than the pipe diameter of the pipe nozzle at the bottom of the acid burette.
Furthermore, the gas production device and the gas collection measuring device are fixed by an iron stand.
An operation method for measuring the content of carbonate in soil by using an experimental device for measuring the content of carbonate in soil comprises the following steps:
step 1: disconnecting the rubber tube from the suction bottle, closing a piston of the three-way tube, adding a colored sulfuric acid solution into the right gas measuring tube, enabling the liquid levels of the left and right gas measuring tubes to rise below a zero scale by the added sulfuric acid solution, adjusting the heights of the two tubes to enable the liquid levels to be flush at the same reading, and keeping the liquid levels of the two tubes unchanged for a moment;
step 2: opening a large rubber plug on the suction filtration bottle, taking down the suction filtration bottle for cleaning, and cleaning for 2-3 times by using deionized water;
and step 3: taking soil in a suction filter flask, recording the soil mass M, if a sample is attached to the wall of the suction filter flask when being poured into the suction filter flask, flushing the sample on the wall of the suction filter flask into the bottom of the suction filter flask by using a small amount of deionized water, and slightly shaking the suction filter flask to uniformly disperse the sample on the bottom of the suction filter flask;
and 4, step 4: connecting the rubber tube with a suction filter bottle, tightly plugging a large rubber plug into the suction filter bottle, and observing that the liquid level of a left air measuring tube is lower than that of a right air measuring tube because the large rubber plug is plugged, and standing for a moment, wherein the liquid levels of the two tubes are kept still;
and 5: opening the large rubber plug, observing the liquid levels of the two tubes to be slowly leveled, indicating that the air tightness of the device is good, if the liquid levels of the two tubes cannot be kept low at the left and high at the right before the large rubber plug is opened but are slowly leveled, indicating that the device leaks air, and checking the air leakage position by applying an elimination method and sealing;
step 6: recording the liquid level reading a of the left air measuring pipe at the moment1；
And 7: adding a proper amount of hydrochloric acid solution into the acid type burette, and recording the reading b of the liquid level of the acid type burette1；
And 8: tightly plugging a large rubber plug into the suction bottle, and recording the liquid level descending number c of the left air measuring pipe;
and step 9: holding the bottle mouth of the suction filter bottle by a right hand finger, controlling a piston of the acid burette by the left hand finger to enable the hydrochloric acid solution to slowly drop into the suction filter bottle, meanwhile, slightly shaking the suction filter bottle by the right hand to enable a sample to fully react with the hydrochloric acid solution, observing the slow drop of the liquid level of the left air measuring pipe, adjusting the piston of the three-way pipe to enable the liquid level of the right air measuring pipe to be slightly higher than the liquid level of the left air measuring pipe all the time, preventing the liquid level in the right air measuring pipe from being too high to cause overflow, standing for a moment after the hydrochloric acid solution is added, and when the liquid level of the left air measuring pipe stops dropping, slightly shaking the suction filter bottle by the hand intermittently for;
step 10: slowly adjusting the piston of the three-way pipe to make the liquid levels of the left and right air measuring pipes parallel and level, and recording the reading a of the liquid level of the left air measuring pipe at the moment2And at this point the acid burette level reading b2；
Step 11: opening the large rubber plug, taking down the suction bottle, and cleaning for the next test;
step 12: calculating the CO produced2Volume, front and rear liquid level changes of left air measuring tube to (a)2-a1) The amount of hydrochloric acid solution added is (b)2-b1) CO produced2The volume amount is V ═ a2-a1)-(b2-b1)-c；
Step 13: calculation of CaCO by Standard Curve method3The content is as follows: weighing standard CaCO on electronic balance3Samples 0.01g, 0.02g, 0.04g, 0.06g, 0.08g, 0.10g were tested for the corresponding CO according to the above procedure2The amount of production; drawing a standard curve by using a computer to generate a standard curve equation and an R square value, wherein the R square value is required to be at least 3 and 9, otherwise, adjusting the experiment operation to re-determine the standard curve;
step 14: CO produced by soil sample2Substituting the volume V into a standard curve equation to obtain CaCO3Mass m, CaCO in soil sample3The content is as follows:
compared with the prior art, the invention has the beneficial effects that: the device adopts common instruments in a common chemical laboratory as parts, has simple structure, easy assembly, high air tightness and convenient experimental operation, provides a complete and detailed operation method, has accurate and stable experimental results after multiple experimental detections, and can be well applied to the determination of the content of the carbonate in the soil.
Drawings
FIG. 1 is a schematic structural diagram of an experimental device for determining the content of carbonate in soil according to the present invention.
Wherein: 1-a suction filter bottle, 2-a large rubber plug, 3-an acid burette, 4-a rubber tube, 5-a U-shaped test tube, 6-a small rubber plug, 7-a left air measuring tube, 8-a right air measuring tube, 9-a hose, 10-a three-way tube and 11-a beaker.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further explained with reference to the accompanying drawings and examples, which are only for the purpose of explaining the present invention and do not limit the scope of the present invention.
As shown in fig. 1, an experimental device for determining the content of carbonate in soil comprises a gas generating device and a gas collecting measuring device which are connected with each other, wherein the gas generating device and the gas collecting measuring device are fixed by an iron stand.
The gas production device comprises a suction bottle 1, a large rubber plug 2 installed on the suction bottle 1, an acid burette 3 and a rubber tube 4, wherein the capacity of the suction bottle 1 is 250ml, the acid burette 3 is communicated with the interior of the suction bottle 1, and the acid burette 3 is fixed with the suction bottle 1 through the large rubber plug 2, the large rubber plug 2 on the suction bottle 1 is provided with a hole, the hole diameter is slightly smaller than the pipe diameter of the pipe mouth at the bottom of the acid burette 3, and the glass pipe mouth is inserted by the elasticity of the rubber plug 2 to ensure the gas tightness. The gas collection measuring device comprises a left gas measuring pipe 7 and a right gas measuring pipe 8, the capacity of the left gas measuring pipe 7 and the capacity of the right gas measuring pipe 8 are both 100ml, the setting heights of the left gas measuring pipe 7 and the right gas measuring pipe 8 are kept on the same horizontal line, hoses 9 are sleeved at the bottom pipe openings of the left gas measuring pipe 7 and the right gas measuring pipe 8 respectively, the hoses 9 at the bottom ends of the left gas measuring pipe 7 and the right gas measuring pipe 8 are connected through a three-way pipe 10 with a piston, and a beaker 11 is placed below the three-way pipe 10 to collect liquid.
Produce gas device and gas collection measuring device and be connected through U type test tube 5 to it is sealed through little rubber buffer 6, the one end of rubber tube 4 is connected with suction bottle 1, and the other end is connected with U type test tube 5's inlet end, U type test tube 5's the end of giving vent to anger is connected with left gas buret 7 to it is sealed through little rubber buffer 6.
The invention provides an experimental device for measuring the content of carbonate in soil, which utilizes the principle that hydrochloric acid and carbonate react in a gas production device to generate CO2Collecting and determining the CO produced by a gas-collecting measuring device2Volume, converted carbonate content, chemical reaction formula is CaCO3+2HCl→CaCl2+H2O+CO2×) and the specific operation method is as follows:
step 1: disconnecting the rubber tube 4 from the suction filtration bottle 1, closing a piston of the three-way tube 10, adding a colored sulfuric acid solution (about 0.5mol/L, adding a few drops of methyl red indicator, and preparing in advance and placing in a volumetric flask for standby) into the right measuring air tube 8, enabling the liquid levels of the left measuring air tube 7 and the right measuring air tube 8 to rise below a zero scale by the added sulfuric acid solution, adjusting the heights of the two tubes to enable the liquid levels to be aligned at the same reading, and keeping the liquid levels of the two tubes unchanged for a moment;
step 2: opening the large rubber plug 2, taking down the suction filtration bottle 1 for cleaning, and cleaning for 2-3 times by using deionized water;
and step 3: measuring 0.1-1.0g of soil (dried and sieved by a 100-mesh sieve) in a suction filter flask 1, recording the soil mass M, if a sample is attached to the wall of the suction filter flask 1 when poured into the suction filter flask, flushing the sample on the wall of the suction filter flask into the bottom of the suction filter flask by using a small amount of deionized water, and slightly shaking the suction filter flask 1 to uniformly disperse the sample at the bottom of the suction filter flask, so that the subsequent reaction is uniform and sufficient, and the test error is reduced;
and 4, step 4: connecting the rubber tube 4 with the suction filtration bottle 1, tightly plugging the large rubber plug 2 into the suction filtration bottle 1, leading the liquid level of the left air measuring tube 7 to descend due to the plugging of the large rubber plug 2, observing that the liquid level of the left air measuring tube 7 is lower than that of the right air measuring tube 8, standing for a moment, and keeping the liquid levels of the two tubes still;
and 5: opening the large rubber plug 2, observing the liquid levels of the two tubes to be slowly restored to be level, indicating that the air tightness of the device is good, if the liquid levels of the two tubes cannot be kept low at the left and high at the right before the large rubber plug 2 is opened, but are slowly level, indicating that the device leaks air, and checking the air leakage position and sealing the air leakage position by applying an elimination method, particularly carefully checking whether the air leakage exists at the connection position of the large rubber plug 2, the small rubber plug 6 and the rubber tube 4 with a glass instrument;
step 6: record the reading a of the liquid level of the left air measuring tube 7 at the moment1；
And 7: adding a proper amount of hydrochloric acid solution (1:3, prepared in advance and placed in a volumetric flask for later use) into the acid type burette 3, and recording the liquid level reading b of the acid type burette 31；
And 8: tightly inserting a large rubber plug 2 into the suction bottle 1, and recording the liquid level drop number c (usually about 2 ml) of the left air measuring pipe 7;
and step 9: holding the bottle mouth of the suction filter bottle 1 by a right hand finger (reducing the influence of body temperature), controlling a piston of the acid burette 3 by the left hand finger to enable the hydrochloric acid solution to slowly drop into the suction filter bottle 1, meanwhile, slightly shaking the suction filter bottle 1 by the right hand to enable a sample to fully react with the hydrochloric acid solution, observing the slow drop of the liquid level of the left air measuring pipe 7, adjusting the piston of the three-way pipe 10 to enable the liquid level of the right air measuring pipe 8 to be slightly higher than the liquid level of the left air measuring pipe 7 all the time, not enabling the liquid level in the right air measuring pipe 8 to be too high to cause overflow, adding the hydrochloric acid solution and then standing for a moment, and when the liquid level of the left air measuring pipe 7 stops dropping, shaking the suction filter bottle 1 slightly by hand;
step 10: slowly adjusting the piston of the three-way pipe 10 to enable the liquid levels of the left and right air measuring pipes to be parallel and level (so as to ensure that the upper parts of the liquid levels of the two air measuring pipes are atmospheric pressure), recording the reading a of the liquid level of the left air measuring pipe 7 at the moment2And at this point the acid burette 3 level reading b2；
Step 11: opening the large rubber plug 2, taking down the suction filtration bottle 1, and cleaning for the next test;
step 12: calculating the CO produced2Volume, front and rear liquid level changes of the left air measuring tube 7 to (a)2-a1) The amount of hydrochloric acid solution added is (b)2-b1) The factors causing the liquid level change of the left air measuring pipe 7 include: CO produced by the reaction2Hydrochloric acid solution and the volume into which the large rubber stopper 2 is inserted, so that CO is generated2The volume amount is V ═ a2-a1)-(b2-b1)-c；
Step 13: calculation of CaCO by Standard Curve method3The content is as follows: weighing standard CaCO on electronic balance3Samples (analytically pure) 0.01g, 0.02g, 0.04g, 0.06g, 0.08g, 0.10g (required to be accurate to 0.001g, and actual soil sample CaCO can also be considered3Content adjustment gradient range), respectively determining corresponding CO according to the above operation steps2The amount produced. With CaCO3Mass m is the abscissa, corresponding to the CO produced2Drawing a standard curve by using a computer with the volume V as a vertical coordinate to generate a standard curve equation and an R square value, wherein the R square value is required to be at least 3 and 9, and otherwise, adjusting the experiment operation to re-determine the standard curve;
step 14: CO produced by soil sample2Substituting the volume V into a standard curve equation to obtain CaCO3Mass m, CaCO in soil sample3The content is as follows:
in the above embodiment, the following matters need to be noted during the operation:
1) when the three-way pipe 10 is not used, the piston of the three-way pipe 10 is opened to enable the colored sulfuric acid solution to flow out, the colored sulfuric acid solution is collected and stored for next use, and the acid burette 3 is sealed to prevent the hydrochloric acid solution from volatilizing.
2) Before each experiment, whether the liquid level of each tube is proper or not should be checked, the current reaction needs to be enough, and if the reaction is not finished and the liquid is used up, the sample should be re-measured.
3) The test has strict requirement on the air tightness of the device, all parts are tightly plugged when being assembled, the punching diameter of the rubber plug is slightly smaller than that of the glass tube, and the glass tube is inserted by utilizing the elasticity of the rubber plug so as to ensure that the device is airtight.
4) The measurement is carried out under the condition that the temperature and the air pressure are relatively constant as much as possible, so that the correction of the temperature and the air pressure can be omitted, and the error caused by the environmental influence is reduced.
5) To prevent CO2It is continuously absorbed by water and should be read immediately after the reaction is complete.
6) Within the allowable range of the test, the more the soil sample is weighed, the smaller the measurement error is, and in order to reduce the measurement error, if CO generated by the reaction is2The amount is less, and some soil samples are recommended to be properly taken for measurement.
The embodiments of the present invention are disclosed as the preferred embodiments, but not limited thereto, and those skilled in the art can easily understand the spirit of the present invention and make various extensions and changes without departing from the spirit of the present invention.
Claims (6)
1. The utility model provides an experimental apparatus of survey soil carbonate content which characterized in that: the device comprises a gas generating device and a gas collection measuring device which are connected, wherein the gas generating device comprises a suction filter bottle, a large rubber plug arranged on the suction filter bottle, an acid burette and a rubber tube, the acid burette is communicated with the interior of the suction filter bottle, and the acid burette is fixed with the suction filter bottle through the large rubber plug;
the gas collection measuring device comprises a left gas measuring pipe and a right gas measuring pipe, hoses are respectively sleeved at bottom pipe orifices of the left gas measuring pipe and the right gas measuring pipe, the hoses at the bottom ends of the left gas measuring pipe and the right gas measuring pipe are connected through a three-way pipe with a piston, and a beaker is placed below the three-way pipe;
the gas production device is connected with the gas collection measuring device through a U-shaped test tube.
2. The experimental facility for determining the carbonate content of soil according to claim 1, wherein: the one end of rubber tube is connected with the suction flask, and the other end is connected with the inlet end of U type test tube, the end of giving vent to anger of U type test tube is connected with left gas metering pipe to it is sealed through little rubber buffer.
3. The experimental facility for determining the carbonate content of soil according to claim 1, wherein: the capacity of the left air measuring pipe and the capacity of the right air measuring pipe are both 100ml, and the set height of the left air measuring pipe and the set height of the right air measuring pipe are kept on the same horizontal line.
4. The experimental facility for determining the carbonate content of soil according to claim 1, wherein: the big rubber stopper on the suction bottle is provided with a hole, and the aperture is slightly less than the pipe diameter of acid burette bottom mouthpiece.
5. The experimental facility for determining the carbonate content of soil according to claim 1, wherein: the gas production device and the gas collection measuring device are fixed by an iron stand.
6. An operating method for measuring the carbonate content of soil by using the experimental device as claimed in any one of claims 1 to 5, which is characterized by comprising the following steps:
step 1: disconnecting the rubber tube from the suction bottle, closing a piston of the three-way tube, adding a colored sulfuric acid solution into the right gas measuring tube, enabling the liquid levels of the left and right gas measuring tubes to rise below a zero scale by the added sulfuric acid solution, adjusting the heights of the two tubes to enable the liquid levels to be flush at the same reading, and keeping the liquid levels of the two tubes unchanged for a moment;
step 2: opening a large rubber plug on the suction filtration bottle, taking down the suction filtration bottle for cleaning, and cleaning for 2-3 times by using deionized water;
and step 3: taking soil in a suction filter flask, recording the soil mass M, if a sample is attached to the wall of the suction filter flask when being poured into the suction filter flask, flushing the sample on the wall of the suction filter flask into the bottom of the suction filter flask by using a small amount of deionized water, and slightly shaking the suction filter flask to uniformly disperse the sample on the bottom of the suction filter flask;
and 4, step 4: connecting the rubber tube with a suction filter bottle, tightly plugging a large rubber plug into the suction filter bottle, and observing that the liquid level of a left air measuring tube is lower than that of a right air measuring tube because the large rubber plug is plugged, and standing for a moment, wherein the liquid levels of the two tubes are kept still;
and 5: opening the large rubber plug, observing the liquid levels of the two tubes to be slowly leveled, indicating that the air tightness of the device is good, if the liquid levels of the two tubes cannot be kept low at the left and high at the right before the large rubber plug is opened but are slowly leveled, indicating that the device leaks air, and checking the air leakage position by applying an elimination method and sealing;
step 6: recording the liquid level reading a of the left air measuring pipe at the moment1；
And 7: adding a proper amount of hydrochloric acid solution into the acid type burette, and recording the reading b of the liquid level of the acid type burette1；
And 8: tightly plugging a large rubber plug into the suction bottle, and recording the liquid level descending number c of the left air measuring pipe;
and step 9: holding the bottle mouth of the suction filter bottle by a right hand finger, controlling a piston of the acid burette by the left hand finger to enable the hydrochloric acid solution to slowly drop into the suction filter bottle, meanwhile, slightly shaking the suction filter bottle by the right hand to enable a sample to fully react with the hydrochloric acid solution, observing the slow drop of the liquid level of the left air measuring pipe, adjusting the piston of the three-way pipe to enable the liquid level of the right air measuring pipe to be slightly higher than the liquid level of the left air measuring pipe all the time, preventing the liquid level in the right air measuring pipe from being too high to cause overflow, standing for a moment after the hydrochloric acid solution is added, and when the liquid level of the left air measuring pipe stops dropping, slightly shaking the suction filter bottle by the hand intermittently for;
step 10: slowly adjusting the piston of the three-way pipe to make the liquid levels of the left and right air measuring pipes parallel and level, and recording the reading a of the liquid level of the left air measuring pipe at the moment2And at this point the acid burette level reading b2；
Step 11: opening the large rubber plug, taking down the suction bottle, and cleaning for the next test;
step 12: calculating the CO produced2Volume, front and rear liquid level changes of left air measuring tube to (a)2-a1) The amount of hydrochloric acid solution added is (b)2-b1) CO produced2The volume amount is V ═ a2-a1)-(b2-b1)-c；
Step 13: calculation of CaCO by Standard Curve method3The content is as follows: weighing standard CaCO on electronic balance3Samples 0.01g, 0.02g, 0.04g, 0.06g, 0.08g and 0.10g, respectively, of the corresponding CO, determined according to the above-mentioned procedures2Generating the yield, drawing a standard curve by using a computer, generating a standard curve equation and an R square value, wherein the R square value is required to be at least 3 and 9, and otherwise, adjusting the experiment operation to re-measure the standard curve;
step 14: CO produced by soil sample2Substituting the volume V into a standard curve equation to obtain CaCO3Mass m, CaCO in soil sample3The content is as follows:
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| CN112147036A (en) * | 2020-09-23 | 2020-12-29 | 上海化工研究院有限公司 | Device and method for testing constant-temperature substance gas-releasing reaction capability when meeting water |
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| CN112147036A (en) * | 2020-09-23 | 2020-12-29 | 上海化工研究院有限公司 | Device and method for testing constant-temperature substance gas-releasing reaction capability when meeting water |
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