CN210923212U - Device suitable for organic matter of soil is got rid of - Google Patents

Abstract

The utility model discloses a device suitable for organic matter of soil gets rid of, include: the sample containing unit is made of a high-temperature-resistant, corrosion-resistant and transparent material and is used for containing a soil sample; a sample protection unit for closing a mouth of the sample containing unit; the gas discharge unit comprises a gas discharge channel arranged on the sample containing unit and/or the sample protection unit and is used for discharging gas generated by the soil sample out of the sample containing unit; the experiment and detection unit at least comprises a heating box capable of accommodating the sample accommodating unit and a high-temperature-resistant gas detection probe arranged at the gas discharge unit; the utility model discloses a device suitable for organic matter of soil gets rid of can get rid of soil sample organic matter completely, avoids the phenomenon of the inorganic carbon attached sample of ashing process production simultaneously, and experimental apparatus is simple and easy, has reduced the experiment cost and has improved the efficiency that organic matter got rid of.

Description

Device suitable for organic matter of soil is got rid of

Technical Field

The utility model belongs to adopt the dry ash method to get rid of the relevant equipment field of soil organic matter, concretely relates to device suitable for soil organic matter gets rid of.

Background

Soil organic matters are one of the important components, influence and restriction of the soil organic matters on vegetation growth are involved in research, and a method for measuring various organic matters is formed. Among them, organic carbon is a representative example of organic matters, and the most commonly used measurement methods include a dry burning method and a wet burning method. The principle of the dry burning method is to convert organic matters into a form of carbon dioxide, measure the concentration of the carbon dioxide and then obtain the content of the organic matters; the principle of the wet burning method is mainly that according to the characteristic that organic matters are easy to oxidize, a chemical reagent is added to perform an oxidation reaction, and the content of the oxides is measured so as to determine the content of the organic matters. However, some studies need to obtain the ion concentration and isotope composition in soil, and organic matters prevent the soluble components from being fully dissolved in the sample, so that the experiment is greatly disturbed. In order to avoid the influence of organic matters in the soil sample dissolving process, organic matters are removed before the sample is dissolved. Similar to organic matter determination, organic matter removal typically includes dry and wet firing methods. The dry burning method is mainly to convert a sample into carbon dioxide gas at a high temperature (500-. At present, both dry burning and wet burning methods have certain disadvantages in the organic matter removing process. The dry burning method is greatly influenced by inorganic carbon, carbon dioxide gas formed by high-temperature combustion cannot be discharged in time, and the formed inorganic carbon is attached to a soil sample to prevent the soluble components of the sample from being dissolved. The influence of the wet combustion method on soil organic matters mainly comprises the following steps: firstly, organic matters cannot be fully oxidized, for example, the effect of hydrogen peroxide on treating soil with high organic matter content is poor; secondly, the possibility of damaging the ion composition in the soil exists in excessive chemical agents; thirdly, the experimental operation is complex, the time required for the oxidation reaction is long, and the difficulty of removing organic matters is increased. The device fully considers the defect that carbon dioxide gas can not be removed in the dry burning method experiment process, designs a simple and efficient crucible device for removing organic matters, improves the efficiency of removing the organic matters in the soil, and solves the key problem that the soluble components in the soil are affected by organic matters in the dissolving process.

SUMMERY OF THE UTILITY MODEL

In view of this, the utility model aims at providing a simple and easy efficient soil organic matter remove device, and the main technical problem who solves includes: 1. the device is simple and easy to design, consists of transparent quartz crucibles of different models, and can simultaneously complete organic matter removal experiments of a plurality of samples. 2. The crucible device has the characteristics of high temperature resistance and corrosion resistance, can fully exert the advantages of a dry burning method, can discharge carbon dioxide gas generated by converting organic matters in time, and prevents inorganic carbon generated in an ashing process from being attached to a sample. 3. And a gas monitoring system is installed, so that the carbon dioxide gas generated in the experimental process is detected in real time, and the adverse effect caused by incomplete ashing or excessive ash is avoided. 4. The device can be also suitable for removing organic matters of other samples, such as plant samples, rock mineral samples, food and the like.

In order to realize the technical purpose, the utility model discloses a technical scheme as follows:

an apparatus suitable for organic matter removal from soil comprising:

the sample containing unit mainly comprises a crucible, the crucible is made of transparent quartz, and the sample containing unit has the advantages of high temperature resistance, corrosion resistance, full completion of ashing, visual identification of ashing degree, and judgment of whether an ashing experiment is completed or not according to the fact that a sample in the crucible is changed into white or grey white;

the sample protection unit comprises a crucible cover matched with a crucible, and the sample protection unit mainly has the following functions: (1) the sample amount loss in the ashing process is prevented; (2) the sample is prevented from being polluted by external substances;

the gas discharge unit mainly comprises a gas vent I and a gas vent II on the sample containing unit; the diameter of exhaust hole I and exhaust hole II is 2mm, all is located the cylinder both sides, and two gas vent docks and forms gas discharge channel promptly. The main functions of the gas discharge unit are: (1) fully discharging carbon dioxide gas generated in the sample ashing process out of the crucible; (2) gas is discharged from the side surface, so that secondary pollution to the sample is avoided;

experiment and detecting element mainly includes that muffle furnace heating cabinet installation gas monitoring probe (high temperature resistant), gives gaseous detection device with gas emission information transfer through the sensor, ensures that the carbon dioxide gas that the ashing experiment produced discharges completely.

The utility model has the advantages that: the utility model discloses a device suitable for organic matter of soil gets rid of can get rid of soil sample organic matter completely, avoids the phenomenon of the inorganic carbon attached sample of ashing process production simultaneously, and experimental apparatus is simple and easy, has reduced the experiment cost and has improved the efficiency that organic matter got rid of. In addition, the gas monitoring probe and the gas detection device can monitor gas generated in the experimental process in real time, avoid manual inspection of an ashing experimental process, and improve the continuity of the experiment.

Drawings

The present invention can be further illustrated by the non-limiting examples given in the accompanying drawings;

FIG. 1 is a schematic structural view of the crucible of the present invention after being engaged with a crucible cover;

FIG. 2 is a schematic structural view of the crucible of the present invention when separated from the crucible cover;

fig. 3 is a schematic view of the overall structure of the present invention.

Detailed Description

In order to make the present invention better understood by those skilled in the art, the technical solutions of the present invention are further described below with reference to the accompanying drawings and examples.

As shown in figure 1, the structure of the crucible and the crucible cover of the utility model is schematically shown, the sample holding unit comprises transparent quartz crucibles with different specifications, the diameter of the bottom of the crucible is 15mm, 20mm or 25mm, the height of the crucible is 45mm, 55mm or 60mm, and the thickness of the crucible is 2-5 mm. The sample protection unit comprises a crucible cover, is matched with the crucible, and has an inner diameter of 20mm, 25mm or 30mm and the like. The gas discharge unit consists of a vent I on the crucible and a vent II on the crucible cover, and the diameter of the vent I is 2 mm.

As shown in figure 2, the exhaust holes I and II are respectively positioned on two sides of the upper port of the crucible and two sides of the crucible cover, the two exhaust holes are butted to successfully form an exhaust channel, the crucible cover is rotated, and the gas exhaust is stopped when the exhaust port of the crucible is closed and the crucible cover is contacted with the outside.

As shown in fig. 3, the experimental heating units (4 and 5) and monitoring units (6-8) include a high temperature heating muffle (4) and an integrated gas monitoring system. The experimental sample is heated at high temperature by the sample heating box (5), the gas monitoring probe (for example, ES10B11-EX/H high-temperature combustible gas detection alarm) (6) is installed on the sample heating box (5) and used for monitoring gas generated in the experimental process, and the data sensor (7) transmits the signal collected by the gas monitoring probe (ES10B11-EX/H) (6) to the gas detector (8) to complete the real-time automatic monitoring of the gas in the experimental process.

Adopt the utility model discloses an organic matter remove device gets rid of when organic matter in the soil, earlier with the sample hold place the crucible in, arrange the heating in the muffle furnace after having adjusted gas discharge channel, install gas monitoring system, begin the ashing experiment to gas detector can not monitor gas discharge and be given first place, accomplishes the experiment, opens the muffle furnace and examines ashing back sample, whether further confirm that the ashing experiment is fully accomplished.

Taking the following example of removing organic matters of a deposited sludge soil sample and retaining silicate components of the sample as an example, the experimental steps are cleaning before the device, pretreating the sample, containing and incinerating the sample, post-treating the sample and cleaning after the device respectively. The method mainly comprises the following steps:

1. cleaning before installation

Respectively cleaning a sample holding unit (crucible) and a sample protection unit (crucible cover) before holding a sample, wherein the used reagent comprises 50% of aqua regia (HNO)₃: HCl 1:3), 50% HNO₃And Milli-Q water. The method comprises the following specific steps: (1) adding 50% aqua regia into the experimental crucible and the crucible cover, heating and boiling for 24h, and washing with Milli-Q water for three times; (2) adding 50% of HNO₃Heating and boiling for 24h, and washing with Milli-Q water for three times; (3) adding Milli-Q, boiling for 24 hr, washing for three times, and oven drying.

2. Sample pretreatment

And (3) sieving the soil sample by a 200-mesh sieve to remove impurities, placing the soil sample in an oven, sealing and drying for 24 hours, and removing water in the soil.

3. Sample holding and ashing experiment

The soil sample after pretreatment is uniformly loaded into the sample containing unit (2) by using the sample weighing paper, so that the sample is prevented from remaining on the crucible wall in the sample loading process. The sample protection unit (1) is placed on the sample holding unit (2), and the sample protection unit is rotated to align the gas discharge units (3 and 3') to form a gas discharge channel. And a gas monitoring probe (6) is arranged on the muffle furnace heating box (5) and is connected with the gas monitoring probe, the data sensor (7) and the gas detector (8).

The experimental steps are as follows: (1) placing a crucible device (figure 1) which contains a sample and is well adjusted with a gas discharge channel in a muffle furnace (figure 3), and rotating the crucible device to stagger gas discharge ports of adjacent crucible devices so as to prevent mutual interference in the ashing process; (2) opening a muffle furnace, adjusting the temperature to 500 ℃, and heating the crucible; (3) starting a data sensor and a gas detector, and monitoring carbon dioxide gas generated in the experimental process until the gas monitor does not detect the gas; (4) checking the color of a sample in a crucible in the muffle furnace, considering that the ashing experiment is finished when the color of the sample is white or grey white, and otherwise, continuously heating the sample; (5) and after the sample is incinerated, closing the muffle furnace to naturally cool the sample, and opening the muffle furnace to take out the cooled crucible.

4. Sample post-treatment

And transferring the ashed sample in the crucible to a beaker, adding 1N acetic acid, fully vibrating, heating and dissolving for 24h, centrifuging the whole solution, placing the sample insoluble in the acetic acid at the bottom of the beaker, and filtering out supernatant to obtain the sample only containing the silicate component.

5. Post-cleaning of the apparatus

The method comprises the following specific steps: (1) adding Milli-Q water to clean the crucible and the crucible cover for three times; (2) adding 50% aqua regia, boiling for 24 hr, and washing with Milli-Q water for three times; (3) adding 50% of HNO₃Heating and boiling for 24h, and washing with Milli-Q water for three times; (4) adding Milli-Q, boiling for 24 hr, washing for three times, and oven drying.

The above description of the specific embodiments is only intended to facilitate the understanding of the method of the present invention and its core idea. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, the present invention can be further modified and modified, and such modifications and modifications also fall within the protection scope of the appended claims.

Claims (4)

1. An apparatus suitable for organic matter removal from soil, comprising:

the sample containing unit is made of a high-temperature-resistant, corrosion-resistant and transparent material and is used for containing a soil sample;

a sample protection unit for closing a mouth of the sample containing unit;

the gas discharge unit comprises a gas discharge channel arranged on the sample containing unit and/or the sample protection unit and is used for discharging gas generated by the soil sample out of the sample containing unit;

the experiment and detection unit at least comprises a heating box capable of accommodating the sample accommodating unit and a high-temperature-resistant gas detection probe arranged at the gas discharge unit.

2. The apparatus of claim 1, wherein the apparatus comprises: the sample containing unit is a plurality of crucibles with different specifications; the sample protection unit is a crucible cover which can be matched with the crucible.

3. The apparatus of claim 2, wherein the apparatus comprises: the opening and closing of the gas discharge passage can be controlled.

4. An apparatus according to claim 3, wherein the apparatus comprises: the gas discharge unit comprises a gas discharge hole I arranged at the upper part of the side wall of the crucible and a gas discharge hole II arranged on the side wall of the crucible cover; the crucible cover can rotate to enable the exhaust holes I and the exhaust holes II to be overlapped to open the exhaust channel, or rotate to enable the exhaust holes I and the exhaust holes II to be staggered to close the exhaust channel.

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