CN206920275U - A kind of device for determining soil sample calcium carbonate content - Google Patents

A kind of device for determining soil sample calcium carbonate content Download PDF

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Publication number
CN206920275U
CN206920275U CN201720823600.7U CN201720823600U CN206920275U CN 206920275 U CN206920275 U CN 206920275U CN 201720823600 U CN201720823600 U CN 201720823600U CN 206920275 U CN206920275 U CN 206920275U
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soil sample
calcium carbonate
container
carbonate content
reaction vessel
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CN201720823600.7U
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高玉峰
汤昕怡
何稼
顾张翔
王丽亚
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Hohai University HHU
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Hohai University HHU
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Abstract

The utility model discloses a kind of device for determining soil sample calcium carbonate content, including soil sample hydrochloric acid reaction device device and gas collection drainage volume measuring device.Soil sample hydrochloric acid reaction device device is made up of the dress sample pallet of reaction vessel, upper flange disk, top cover, the rotation-controlled being connected with rod member, and gas collection drainage volume measuring device includes container and stereometry container equipped with clear water and oil slick.Soil sample can fully be reacted in reaction vessel with hydrochloric acid, and using air-water displacement method, the volume of clear water namely caused CO2 volumes are flowed into container by determining, you can obtain soil sample calcium carbonate content according to demarcation relation curve.Calcium carbonate content continuous mode of the present utility model is simple and easy to do, and as a result accurately, soil sample will not produce mass loss.

Description

A kind of device for determining soil sample calcium carbonate content
Technical field
The utility model belongs to Soil K+adsorption technical field, is related to a kind of device for determining soil sample calcium carbonate content.
Background technology
Calcium carbonate content method for measuring mainly has following a few classes in soil sample at present:First, to being dried after soil sample pickling and washing Dry measure difference weight, calculates calcium carbonate content.This method is easier, but soil sample easily produces in multiple pickling water-washing process Mass loss, influence the accuracy of result of the test.Second, using closed container gas collection method, measurement soil sample is discharged after dissolving with hydrochloric acid CO2Volume or pressure change, calculate calcium carbonate content.Two shortcomings be present in this method:CO first2It is water-soluble, determine volume Or pressure is less than normal.In addition, injecting hydrochloric acid into the closed container equipped with soil sample, the process liquids occupy partial volume, also can It has impact on the measurement of gas volume and pressure.Third, ICP method (plasma transmitting chromatograph), Atomic absorption (flame graphite furnace) Spectrometer and EDTA titrations, can also determine calcium ion content, the calcium carbonate content in the inverse soil body.But ICP method and original Sub- absorption spectrometer and EDTA titration cost is more expensive, and disodium ethylene diamine tetraacetate can be with most of gold in EDTA titrations Belong to cation and complex reaction occurs, by other ion interferences, influence to determine accuracy.
Utility model content
The defects of the purpose of this utility model is to overcome prior art, there is provided a kind of measure soil sample calcium carbonate content Device, the continuous mode of calcium carbonate content is simple and easy to do, and soil sample will not produce mass loss, and measurement result is more accurate.
To solve the technical problem of prior art, the utility model uses following technical scheme.
A kind of device for determining soil sample calcium carbonate content of the present utility model, it is characterised in that:Including a soil sample hydrochloric acid Reactor and a gas collection drainage volume measuring device;
The soil sample hydrochloric acid reaction device includes the reaction vessel equipped with watery hydrochloric acid, its top flange dish and reaction vessel top cover It is connected by several bolts, described reaction vessel is sealed;One rod member injects through the reaction vessel top cover In described reaction vessel, rod member bottom sets a pallet for being used to hold soil sample, and the pallet can rotate around the shaft;One Blast pipe with exhaust valve and duplex fitting, its one end insert described reaction by the exhaust outlet of reaction vessel top cover In container, in the described gas collection drainage volume measuring device of other end insertion;
The gas collection drainage volume measuring device includes a liquid filled container and an individual with liquid filled container top cover Product measurement container;Clear water and oil reservoir of the liquid filled container built with least 1/2 container height;The left port of one drainpipe is led to Cross in the clear water in the liquid outlet insertion liquid filled container of the liquid filled container top cover, its right output port inserts the cubing container It is interior;Described cubing container wall is provided with volume markings.
Described rotating shaft is driven by an electronic dead slow speed motor.
Switch is provided with described rod member, for controlling the rotation and stopping of pallet.
The lower surface position of described drainpipe right output port is in same level with the oil reservoir liquid level in liquid filled container.
The mouth of pipe and Qi Nei liquid in described blast pipe insertion liquid filled container do not contact.
Compared with prior art, the utility model includes advantages below and beneficial effect:
(1) for the utility model when determining soil sample calcium carbonate content, mass loss is not present in soil sample and continuous mode is easy, Measuring accuracy is high.
(2) when determining, oil slick layer is poured on clear water, avoids CO2It is dissolved in water so that gas volume measure is more smart Really.
(3) soil sample hydrochloric acid reaction device device can be disconnected with gas collection drainage volume measuring device by bilateral, first be poured into Hydrochloric acid, sample is installed, pressure change caused by during being loaded can be avoided by then connecting two agent sets, not interfered with CO2The measurement of volume.
(4) soil sample of the present utility model enters dilute hydrochloric acid solution, quality free of losses by pallet.Soil is controlled by switch manual The beginning of sample and hydrochloric acid reaction, the automatic sample of closed container is realized, sample-adding immediate response causes gas before avoiding instrument assembling Body loss.
(5) the method CO replaced by gas-liquid2Gas volume is measured by clear water volume quantitative, measurement result essence Really.
Brief description of the drawings
Fig. 1 is an a kind of example structure schematic diagram of the device for determining soil sample calcium carbonate content of the utility model.
Fig. 2 is the rotatable tray in use schematic diagram of one embodiment device of the present utility model.
When Fig. 3 is using the embodiment device of the utility model one measure soil sample calcium carbonate content, its CO2Volume and calcium carbonate The demarcation relation curve of quality.
In figure, 1 watery hydrochloric acid, 2 reaction vessels, 3 top flange dish, 4 bolts, 5 rod members, 6 switches, 7 rotating shafts, 8 pallets, 9 rows Tracheae valve, 10 duplex fittings, 11 reaction vessel top covers, 12 liquid filled container top covers, 13 oil reservoirs, 14 liquid filled containers, 15 drainpipes Valve, 16 blast pipes, 17 drainpipes, 18 cubing containers, 19 soil samples.
Embodiment
The utility model is described in further details below in conjunction with accompanying drawing.
As shown in figure 1, it is a kind of example structure signal of device for determining soil sample calcium carbonate content of the utility model Figure.The embodiment device includes:Soil sample hydrochloric acid reaction device device and gas collection drainage volume measuring device.The soil sample hydrochloric acid is anti- Answer device device and gas collection drainage volume measuring device separate, two big device internal pressures are one big before on-test Atmospheric pressure, sample-adding process do not interfere with the measure of gas volume.
The soil sample hydrochloric acid reaction device device includes the reaction vessel 2 equipped with watery hydrochloric acid 1, container top ring flange 3 with it is anti- Container cap 11 is answered, both are connected by bolt 4, realize sealing.
The reaction vessel top cover 11 lays the rod member 5 of insertion container, and the bottom of rod member 5 is the pallet 8 equipped with soil sample 19, support Disk 8 can occur to rotate at a slow speed by the rotary shaft 7 with electronic dead slow speed motor, and rod member 5 is provided with switch 6, can control the rotation of pallet 8 Turn and stop, soil sample 19 is poured into the reaction vessel 2 equipped with hydrochloric acid 1.After instrument assembles, examination can be automatically controlled by switch The beginning tested, avoid instrument unassembled good or throw soil sample during unsealing, immediate response causes gas escape, realizes closed appearance The automatic sample of device.
Exhaust outlet is left on the top of reaction vessel top cover 11, by with valve 9 and the blast pipe of duplex fitting 10 16 It is connected with gas collection drainage volume measuring device.
The gas collection drainage volume measuring device includes liquid filled container 14 and cubing container 17.
Clear water of the liquid filled container 14 built with 1/2-3/4 container heights.More than clear water liquid level it is at least 2cm oil reservoir 13, for completely cutting off CO2With clear water, avoid reacting caused CO2It is dissolved in the water, causes experiment to survey gas flow inclined compared with actual value It is small.
The liquid filled container 14 includes liquid filled container top cover 12, sets air inlet on top cover 12, passes through blast pipe 16 and soil sample Hydrochloric acid reaction case is connected, and blast pipe 16 is inserted inside liquid filled container 14, and the mouth of pipe and will fill liquid in sample container 14 and not enter Row contact, i.e.,:2~5cm more than the liquid level of oil reservoir 13.
The liquid filled container top cover 12 is additionally provided with liquid outlet, is surveyed by the drainpipe 17 with draining tube valve 15 and volume Container 18 is measured to be connected.
In the insertion clear water of drainpipe 17 being connected with liquid outlet in the liquid filled container 14, its left end nozzle position close to The bottom of liquid filled container 14, but do not contact therewith.The internal diameter of drainpipe 17 is thinner, about 2~5mm, to make in air pressure Clear water is pressed into drainpipe 17 under and flow out.
The drainpipe 17 is connected to liquid filled container 14 and cubing container 18, and inside is full of clear water.Surveyed positioned at volume The lower surface position of the right output port of drainpipe 17 in amount container 18 is in same level with the liquid level of oil reservoir 13 in liquid filled container 14, At least it is not less than the horizontal level of the liquid level of oil reservoir 13.So as to avoid in the exhaust process of determination test, its initial level is poor Drainage procedure is had an impact, causes surveyed displacement hull product value phenomenon bigger than normal.
The wall of cubing container 18 is volume markings, can real-time monitored enter liquid volume, final liquid bulk Product is CO caused by reaction2Gas volume.When experiment does not start, in liquid filled container 14 in pressure and cubing container 18 The mouth of pipe pressure of drainpipe 17 balances each other.When reaction produces CO2Afterwards, in liquid filled container 14 pressure increase, clear water under gas pressure, It is pressed into drainpipe 17, and flows into volume measurement device 18, the liquid volume in final volume measurement apparatus 18 produces CO2Volume.The method that liquid volume is surveyed by air-water displacement overcomes CO2Gas volume is unable to the shortcomings that accurate quantification measure.
Using a kind of principle for the device measure soil sample calcium carbonate content for determining soil sample calcium carbonate content of the utility model such as Under:CaCO in soil sample3Reacted with HCl, produce CO2I.e.:
CaCO3+2HCl→CaCl2+H2O+CO2
Caused CO2Measured by gas collection drainage volume measurement device, according to CO2What volume can be reacted completely Calcium carbonate quality, so as to obtain the calcium carbonate content of soil sample.
It is as follows that the utility model determines the step of soil sample calcium carbonate content:
(1) soil sampling 19 is dried, and then claims quality, and soil sample quality is 6g;
(2) watery hydrochloric acid 1 that volume is 60mL, concentration is 2mol/L is poured into reaction vessel 2, it is ensured that the carbon in soil sample 19 Sour calcium and hydrochloric acid reaction are complete.
(3) gas collection drainage volume measuring device is assembled:As shown in Figure 1,1000mL is poured into liquid filled container 14 first Clear water, clear water is highly 2/3 container height, in order to there is the liquid of sufficient amount to discharge.It is subsequently poured into the thick oil of at least 2cm 13, completely cut off gas and clear water, avoid CO2Water is dissolved in, causes institute's measured value less than normal.Air inlet and draining are set on liquid filled container top cover 12 Mouthful, it is connected respectively with soil sample hydrochloric acid reaction device device with cubing container 18 by blast pipe 16 and drainpipe 17.Liquid is filled to hold Oil reservoir does not contact in the mouth of pipe of 14 internal exhaust tube of device 16 and dress sample container 14, positioned at the liquid level above 2cm of oil reservoir 13.Internal drainage pipe 17 nozzle positions do not contact therewith close to the bottom of liquid filled container 14.After covering liquid filled container top cover 12, guarantee and body Clear water is full of in the connected drainpipe 17 of product measurement container 18.The nozzle position of drainpipe 17 and dress liquid in cubing container 18 The liquid level of oil reservoir 13 is equal in container 14, now the internal pressure of liquid filled container 14 and the mouth of pipe of drainpipe 17 in cubing container 18 Locate pressure balance, clear water will not be flowed out by liquid outlet.
(4) sample is filled:Soil sample 19 after weighing is placed on pallet 8, by the reaction vessel top cover with rod member 5 Yu pallet 8 11 are connected with top flange dish 3 by bolt 4, ensure sealing.The top exhaust outlet of reaction vessel top cover 11 is connected with blast pipe 16, Before reaction vessel top cover 11 is not installed, exhaust valve 9 is in open mode, the soil sample hydrochloric acid reaction device dress before on-test Put separate with gas collection drainage volume measuring device, two big device internal pressures are all an atmospheric pressure before on-test Power, sample-adding process do not interfere with the measure of gas volume.Traditional measurement method is overcome to note into the closed container equipped with soil sample Enter hydrochloric acid, liquid occupies partial volume, the shortcomings that causing surveyed gas volume bigger than normal.
After tightening bolt 4, exhaust valve 9 is closed, and blast pipe 16 is surveyed by bilateral 10 and gas collection drainage volume Determine device to be connected.
(5) firing test:After connecting each part by Fig. 1, exhaust valve 9 and drainpipe 15 are opened.Instrument assembles The beginnings that experiment is automatically controlled by switch 6 afterwards, avoid throwing soil sample immediate response during the unassembled good or unsealing of instrument and cause Gas escape, realize the automatic sample of closed container.Now pallet 8 rotates along the rotary shaft 7 with electronic dead slow speed motor, Soil sample 19 is tumbled from pallet 8 into watery hydrochloric acid 1, is fully reacted with hydrochloric acid 1, the loss of soil sample massless.React the CO of generation2By After blast pipe 17 is discharged, into the liquid filled container 14 of sealing.Container internal pressure changes, and clear water enters under gas pressure Drainpipe 17, flow into stereometry container 18.15min after being produced in reaction vessel 2 without obvious bubble, read cubing and hold The volume of clear water, i.e. 338.9mL in device 18, the clear water volume of outflow is CO caused by reaction2Volume.The side replaced by gas-liquid Method causes CO2Gas volume is measured by clear water volume quantitative.
(6) calcium carbonate content and CO are demarcated2The relation of volume:Calcium carbonate 0.5g, 1g, 1.5g, 2g, 2.5g, 3g are taken respectively, By above-mentioned instrument and assay method, CO caused by its difference is determined2Volume, draw calcium carbonate quality and survey CO2Volume relationship Curve, as shown in Figure 3.
(7) calcium carbonate content is calculated:When discharge clear water volume is CO2Volume when being 338.9mL, by calcium carbonate quality with Surveyed CO2Volume calibration relation curve, i.e. obtained by Fig. 3, corresponding calcium carbonate quality is 1.49g.Therefore, the soil sample 19 Calcium carbonate content w is w=CaCO3Quality/quality of soil sample, i.e., 24.83%.
In a word, the utility model proposes a kind of method and its device for determining soil sample calcium carbonate content, solves tradition Measuring method is also easy to produce quality of soil sample loss, liquid occupies the problems such as volume influences gas volume measurement, gas is dissolved in water, can be real Existing closed container automatic sample, measure gas volume using air-water displacement method so that soil sample calcium carbonate content to be measured obtains letter Just, accurate measure.

Claims (5)

  1. A kind of 1. device for determining soil sample calcium carbonate content, it is characterised in that:Collect including a soil sample hydrochloric acid reaction device and one Gas drainage volume measuring device;
    The soil sample hydrochloric acid reaction device includes the reaction vessel (2) equipped with watery hydrochloric acid (1), and its top flange dish (3) is held with reaction Device top cover (11) is connected by several bolts (4), and described reaction vessel (2) is sealed;One rod member (5) passes through institute State reaction vessel top cover (11) to inject in described reaction vessel (2), rod member (5) bottom sets one to be used to hold soil sample (19) Pallet (8), the pallet (8) can around the shaft (7) rotate;One row with exhaust valve (9) and duplex fitting (10) Tracheae (16), its one end are inserted in described reaction vessel (2) by the exhaust outlet of reaction vessel top cover (11), other end insertion In described gas collection drainage volume measuring device;
    The gas collection drainage volume measuring device includes a liquid filled container (14) and one with liquid filled container top cover (12) Individual cubing container (18);The liquid filled container (14) is built with least clear water of 1/2 container height and oil reservoir (13);One The left port of drainpipe (17) is inserted in the clear water in liquid filled container (14) by the liquid outlet of the liquid filled container top cover (12), Its right output port is inserted in the cubing container (18);Described cubing container (18) wall is provided with volume markings.
  2. A kind of 2. device for determining soil sample calcium carbonate content according to claim 1, it is characterised in that described rotating shaft (7) it is driven by an electronic dead slow speed motor.
  3. A kind of 3. device for determining soil sample calcium carbonate content according to claim 1, it is characterised in that described rod member (5) switch (6) is provided with, for controlling the rotation and stopping of pallet (8).
  4. A kind of 4. device for determining soil sample calcium carbonate content according to claim 1, it is characterised in that described drainpipe (17) the lower surface position of right output port is in same level with oil reservoir (13) liquid level in liquid filled container (14).
  5. A kind of 5. device for determining soil sample calcium carbonate content according to claim 1, it is characterised in that described blast pipe (16) mouth of pipe and Qi Nei liquid inserted in liquid filled container (14) does not contact.
CN201720823600.7U 2017-07-07 2017-07-07 A kind of device for determining soil sample calcium carbonate content Active CN206920275U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107219150A (en) * 2017-07-07 2017-09-29 河海大学 A kind of method and its device for determining soil sample calcium carbonate content
CN108490110A (en) * 2018-02-02 2018-09-04 同济大学 A kind of method of the high containing hydrogen silicone oil hydrogen content of rapid and accurate determination
CN111781089A (en) * 2019-04-04 2020-10-16 应急管理部化学品登记中心 Novel sample and water mixing method for measuring gas release rate of substance in water

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107219150A (en) * 2017-07-07 2017-09-29 河海大学 A kind of method and its device for determining soil sample calcium carbonate content
CN108490110A (en) * 2018-02-02 2018-09-04 同济大学 A kind of method of the high containing hydrogen silicone oil hydrogen content of rapid and accurate determination
CN111781089A (en) * 2019-04-04 2020-10-16 应急管理部化学品登记中心 Novel sample and water mixing method for measuring gas release rate of substance in water

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