CN110954391A - Digestion tank for monitoring pretreatment of elements in soil and application - Google Patents
Digestion tank for monitoring pretreatment of elements in soil and application Download PDFInfo
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- CN110954391A CN110954391A CN201911345146.9A CN201911345146A CN110954391A CN 110954391 A CN110954391 A CN 110954391A CN 201911345146 A CN201911345146 A CN 201911345146A CN 110954391 A CN110954391 A CN 110954391A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a digestion tank for element monitoring pretreatment in soil and application thereof. The digestion tank has good sealing performance and pressure-bearing performance. The special digestion tank is utilized to carry out the pretreatment of monitoring elements in the soil by adopting a constant-temperature direct heating method, so that the digestion process is shortened, the use amount of various acids is reduced, a large amount of time and cost are saved, the efficiency is improved, and the environmental pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of contaminated soil monitoring, and particularly relates to a digestion tank for monitoring pretreatment of elements in soil and application thereof.
Background
Monitoring of heavy metals and arsenic and mercury elements in soil is an important content of environmental monitoring, and pretreatment of a soil sample plays a key role in monitoring heavy metals in soil. At present, the monitoring sample treatment of heavy metal elements in soil mainly comprises normal-temperature normal-pressure digestion and microwave digestion. The former method consumes a lot of acid, and requires manual observation and repeated addition of acid, resulting in a large amount of acid agent. The microwave digestion method overcomes the defects of normal temperature and pressure electric heating plate digestion, the usage amount and digestion time of an acid agent are reduced, but a microwave oven for chemical analysis is high in price, temperature control is easy to damage, maintenance cost is high, the amount of samples processed at one time is small, and the microwave digestion method is difficult to be widely applied to actual work generally.
Therefore, how to make the pretreatment operation of the soil sample more convenient, efficient and low-cost becomes a technical problem to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The method has the advantages of complex pretreatment operation, small treatment capacity, high cost and the like of the soil sample in the prior art. The invention provides a digestion tank for monitoring and pretreatment of elements in soil, which comprises the following components:
the digestion tank is made of polytetrafluoroethylene materials and comprises a tank body and a tank cover;
the tank body is of a cylindrical structure, a cavity is formed in the tank body, and the inner bottom of the tank body is of a crescent structure;
the upper opening of the tank body is in threaded connection with the tank cover, the threaded connection part of the tank body is of an external thread structure, and the threaded connection part of the tank cover is of an internal thread structure;
the cover is internally provided with a cover inner pad which is made of expanded polytetrafluoroethylene.
Preferably, the height of the tank body is 90 mm, the outer diameter of the tank body is 40 mm, the wall thickness of the tank body is 7 mm, the central wall thickness of the bottom of the tank body is 10 mm, and the depth of the external thread of the tank body is 15 mm.
The outer diameter of the tank cover is 50 mm, the height of the tank cover is 20 mm, and the depth of the inner wire of the tank cover is 15 mm.
The thickness of the inner pad of the tank cover is 3 mm, the diameter of the inner pad of the tank cover is 39 mm, and the density of the inner pad of the tank cover is 1.8g/cm 3.
Correspondingly, the invention also provides a method for monitoring and pretreating heavy metal elements in soil by using the digestion tank, which comprises the following steps:
(1) placing soil to be detected into the digestion tank;
(2) adding a comprehensive digestion solution into the digestion tank;
(3) putting the digestion tank into a graphite digestion device for constant-temperature heating;
(4) carrying out acid-dispelling treatment on the heated content in the digestion tank;
(5) diluting the content after the acid removing treatment to a constant volume to obtain a pretreatment sample.
Preferably, the comprehensive digestion solution consists of concentrated nitric acid, concentrated hydrochloric acid, concentrated perchloric acid, concentrated hydrofluoric acid and concentrated hydrogen peroxide.
Preferably, in the step (3):
the tank body is connected with the tank cover before the digestion tank is heated, the constant-temperature heating temperature is 180 ℃, and the constant-temperature heating is carried out by using a porous graphite constant-temperature digestion device.
Preferably, in the step (4):
cooling the contents of the digestion tank to room temperature before the acid-removing treatment;
the acid removing treatment specifically comprises the following steps: the lid of the digestion tank was opened, the digestion tank was heated at a constant temperature of 160 ℃ and heating was stopped when the content volume reached 0.2-0.5 ml.
Preferably, in the step (5):
after the contents were cooled to room temperature, the contents were diluted with pure water to a volume of 50 ml.
Correspondingly, the invention also provides a method for monitoring and pretreating arsenic and mercury elements in soil by using the digestion tank, which comprises the following steps:
(1) placing soil to be detected into the digestion tank;
(2) adding aqua regia into the digestion tank;
(3) putting the digestion tank into a graphite digestion device for constant-temperature heating;
(4) diluting the heated contents in the digestion tank to a constant volume to obtain a pre-treatment sample.
Preferably, in the step (3):
the tank body is connected with the tank cover before the digestion tank is heated, the constant-temperature heating temperature is 160 ℃, and the constant-temperature heating is carried out by using a porous graphite constant-temperature digestion device.
Preferably, in the step (4):
after the contents were cooled to room temperature, the contents were diluted with pure water to a volume of 25 ml.
Compared with the prior art, the digestion tank provided by the invention is used for monitoring and pretreating elements in soil, so that the treatment time can be greatly saved, and the dosage of an acid agent required by treatment is reduced. The digestion tank provided by the invention is simple to manufacture, low in cost and good in sealing performance, and does not leak gas under the condition of bearing 2MPa of pressure.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a schematic front structural diagram of a digestion tank for element monitoring pretreatment in soil according to an embodiment of the invention;
fig. 2 is a schematic flow chart of a method for monitoring and pre-treating heavy metal elements in soil according to an embodiment of the present invention;
fig. 3 is a schematic flow chart of a method for monitoring and pre-treating arsenic and mercury in soil according to an embodiment of the present invention.
Detailed Description
The method has the advantages of complex pretreatment operation, small treatment capacity, high cost and the like of the soil sample in the prior art. The invention provides a digestion tank for monitoring and pretreating elements in soil. The technical solution of the present invention will be described clearly and completely with reference to the accompanying drawings in the following embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present application. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
As shown in figure 1, the invention provides a digestion tank for monitoring and pretreatment of elements in soil, which is prepared from polytetrafluoroethylene materials and comprises a tank body and a tank cover.
The tank body is of a cylindrical structure, a cavity is formed in the tank body, and the inner bottom of the tank body is of a meniscus structure, so that liquid residue can be effectively reduced.
The opening at the upper part of the tank body is in threaded connection with the tank cover, the threaded connection part of the tank body is of an external thread structure, and the threaded connection part of the tank cover is of an internal thread structure.
The cover is internally provided with a cover inner pad which is made of expanded polytetrafluoroethylene.
Through the threaded connection jar body cover of enough dark, can effectively strengthen and clear up a jar pressure-bearing capacity, the jar of can still airtight not revealing gas in the pressure-bearing condition can be guaranteed to clear up to the pad in the cover of expanded polytetrafluoroethylene cover simultaneously.
According to a specific implementation scene, the height of a tank body of the digestion tank is 90 mm, the outer diameter of the tank body is 40 mm, the wall thickness of the tank body is 7 mm, the wall thickness of the center of the bottom of the tank body is 10 mm, and the depth of an external thread of the tank body is 15 mm. The outer diameter of the tank cover of the digestion tank is 50 mm, the height of the tank cover is 20 mm, and the depth of the inner thread of the tank cover is 15 mm. The thickness of the inner pad of the digestion tank cover is 3 mm, the diameter of the inner pad of the tank cover is 39 mm, and the density of the inner pad of the tank cover is 1.8g/cm3. The digestion tank provided by the invention has the advantages that the tank body can bear 2MPa pressure, the sealing performance is good, and gas is not leaked under the condition of bearing pressure; the height of the tank body is 90 mm, so that acid removing operation is conveniently carried out after digestion; and the digestion tank is simple to manufacture and low in cost.
Example 2
As shown in FIG. 2, the invention provides a method for monitoring and pretreating heavy metal elements in soil by using the digestion tank, which comprises the following steps:
step 201: and placing the soil to be detected into the digestion tank.
Step 202: and adding the comprehensive digestion liquid into the digestion tank.
The comprehensive digestion solution is prepared by mixing concentrated nitric acid, concentrated hydrochloric acid, concentrated perchloric acid, concentrated hydrofluoric acid and concentrated hydrogen peroxide according to a certain proportion through repeated tests in combination with specific implementation scenes.
Step 203: and (4) putting the digestion tank into a graphite digestion device for constant-temperature heating.
The tank cover is screwed down before the digestion tank is heated by combining a specific implementation scene, so that the tank cover is tightly connected with the tank body, the sealing property of the digestion tank is ensured, the porous graphite constant temperature digestion device is selected for heating in constant temperature heating, and the constant temperature heating temperature is 180 ℃.
Step 204: and (4) carrying out acid-dispelling treatment on the heated content in the digestion tank.
Wherein, the contents in the digestion tank are fully cooled to room temperature before the acid removing treatment by combining with specific implementation scenes; when the acid is removed, the tank cover of the digestion tank is opened, the digestion tank is heated at the constant temperature of 160 ℃, and the heating is stopped when the volume of the content in the digestion tank is reduced to 0.2-0.5 ml.
Step 205: diluting the content after the acid removing treatment to a constant volume to obtain a pretreatment sample.
And in combination with a specific implementation scene, cooling the content in the digestion tank to room temperature after acid-removing treatment, and then diluting with pure water to a constant volume of 50 ml.
Example 3
As shown in fig. 3, the invention provides a method for monitoring and pretreating arsenic and mercury in soil by using the digestion tank, which comprises the following steps:
step 301: and placing the soil to be detected into the digestion tank.
Step 302: adding aqua regia into the digestion tank.
Step 303: and (4) putting the digestion tank into a graphite digestion device for constant-temperature heating.
The tank cover is screwed down before the digestion tank is heated by combining a specific implementation scene, so that the tank cover is tightly connected with the tank body, the sealing performance of the digestion tank is ensured, the porous graphite constant temperature digestion device is selected for heating in constant temperature heating, and the constant temperature heating temperature is 160 ℃.
Step 304: diluting the heated contents in the digestion tank to a constant volume to obtain a pre-treatment sample.
And in combination with a specific implementation scene, after the content in the digestion tank is cooled to room temperature, diluting with pure water to a constant volume of 25 ml.
The present invention will be further described in detail with reference to specific embodiments in conjunction with specific implementation scenarios.
Example 4
In a specific implementation scenario, the invention provides a method for monitoring and pretreating heavy metal elements in soil by using the digestion tank, and the method specifically comprises the following steps:
step 401: accurately weighing 0.2 g of soil sample to be detected and placing the soil sample into a digestion tank.
Step 402: the comprehensive digestion solution is prepared by mixing concentrated nitric acid, concentrated hydrochloric acid, concentrated perchloric acid, concentrated hydrofluoric acid and concentrated hydrogen peroxide according to a certain proportion through repeated tests; the soil sample to be measured is wetted by a small amount of pure water, and then 5.00ml of comprehensive digestion solution is added.
Step 403: screwing down the tank cover of the digestion tank, and putting the digestion tank into a graphite digestion device; wherein, the graphite constant temperature digestion device is porous (20 holes, 40 holes and 60 holes), and the aperture is 43 mm; the digestion tank was directly heated at a constant temperature of 180 ℃ for 2.5 hours.
Step 404: after heating, fully cooling the contents in the digestion tank to room temperature, and then performing acid-dispelling treatment; the pot cover of the digestion pot is opened, and the digestion pot is heated in a porous graphite digestion device at a constant temperature of 160 ℃ to drive acid until the liquid is about the size of the soybean (0.2-0.5 ml).
Step 405: and (3) fully cooling the content of the digestion tank after acid dispelling to room temperature, diluting the content by using pure water, transferring the diluted content into a 50ml volumetric flask, and fixing the volume to 50ml to finally complete the preparation of the sample.
The invention utilizes a special digestion tank and adopts a constant-temperature direct heating method to shorten the digestion process to be within 4 hours. The total amount of the various acids is 5ml, compared with the prior art, the method saves a great deal of time and cost, improves the efficiency and reduces the environmental pollution.
Example 5
In a specific implementation scenario, the invention provides a method for monitoring and pretreating arsenic and mercury in soil by using the digestion tank, and the method specifically comprises the following steps:
step 501: accurately weighing 0.1g of soil sample to be detected in the digestion tank.
Step 502: 5.00ml of aqua regia is added into the digestion tank to be mixed with the soil to be detected.
Step 503: screwing down the tank cover of the digestion tank, and putting the digestion tank into a graphite digestion device; wherein, the graphite constant temperature digestion device is porous (20 holes, 40 holes and 60 holes), and the aperture is 43 mm; the digestion tank was directly heated at a constant temperature of 160 ℃ for 0.5 hour.
Step 504: and (3) fully cooling the contents in the heated digestion tank to room temperature, diluting with pure water, transferring into a 25ml volumetric flask, and fixing the volume to 25ml, thus finally completing the sample preparation.
At present, the pretreatment of arsenic and mercury monitoring samples in soil needs to add 30ml of aqua regia into the soil sample to be detected with the same quantity, and heat the soil sample for two hours at 120 ℃. Since aqua regia is extremely volatile, serious contamination to the laboratory and the outside can occur during the whole experimental process. According to the invention, the soil sample is pretreated by adding 5ml of aqua regia into a special digestion tank and then heating at a constant temperature of 160 ℃ for 0.5 hour, so that the acid consumption is reduced by 80% in the whole experiment, the time is shortened to one fourth, and the experiment efficiency is greatly improved. Because the tank body is sealed, the aqua regia is not easy to escape, and the object to be tested is not lost, thereby protecting the laboratory environment and the external atmospheric environment from acid pollution and improving the accuracy of the experiment.
The specific implementation scenarios of the above embodiments are only used for illustrating the present invention and are not used to limit the scope of the present invention. The above sequence numbers are for illustrative purposes only and do not represent the relative merits of the implementation scenario. Any methods and materials similar or equivalent to those described herein can be used in the practice of the present invention, and the preferred methods and materials are described herein for illustrative purposes only. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The foregoing disclosure is only for the specific implementation of the embodiments of the present invention, and is not intended to limit the present invention in other forms, and the embodiments of the present invention are not limited thereto. Any person skilled in the art may, using the teachings disclosed above, change or modify the equivalent embodiments with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A digestion tank for monitoring pretreatment of elements in soil is characterized by being prepared from polytetrafluoroethylene materials and comprising a tank body and a tank cover;
the tank body is of a cylindrical structure, a cavity is formed in the tank body, and the inner bottom of the tank body is of a crescent structure;
the upper opening of the tank body is in threaded connection with the tank cover, the threaded connection part of the tank body is of an external thread structure, and the threaded connection part of the tank cover is of an internal thread structure;
the cover is internally provided with a cover inner pad which is made of expanded polytetrafluoroethylene.
2. The digestion tank according to claim 1,
the jar body jar height is 90 millimeters, jar external diameter is 40 millimeters, jar body wall thickness is 7 millimeters, jar body bottom center wall thickness is 10 millimeters, jar external silk degree of depth is 15 millimeters.
The outer diameter of the tank cover is 50 mm, the height of the tank cover is 20 mm, and the depth of the inner wire of the tank cover is 15 mm.
The thickness of the inner pad of the tank cover is 3 mm, the diameter of the inner pad of the tank cover is 39 mm, and the density of the inner pad of the tank cover is 1.8g/cm3。
3. A method for monitoring and pre-treating heavy metal elements in soil by using the digestion tank prepared according to the claims 1-4, which is characterized by comprising the following steps:
(1) placing soil to be detected into the digestion tank;
(2) adding a comprehensive digestion solution into the digestion tank;
(3) putting the digestion tank into a graphite digestion device for constant-temperature heating;
(4) carrying out acid-dispelling treatment on the heated content in the digestion tank;
(5) diluting the content after the acid removing treatment to a constant volume to obtain a pretreatment sample.
4. The method of claim 3,
the comprehensive digestion solution consists of concentrated nitric acid, concentrated hydrochloric acid, concentrated perchloric acid, concentrated hydrofluoric acid and concentrated hydrogen peroxide.
5. The method of claim 3, wherein in step (3):
the tank body is connected with the tank cover before the digestion tank is heated, the constant-temperature heating temperature is 180 ℃, and the constant-temperature heating is carried out by using a porous graphite constant-temperature digestion device.
6. The method of claim 3, wherein in step (4):
cooling the contents of the digestion tank to room temperature before the acid-removing treatment;
the acid removing treatment specifically comprises the following steps: the lid of the digestion tank was opened, the digestion tank was heated at a constant temperature of 160 ℃ and heating was stopped when the content volume reached 0.2-0.5 ml.
7. A method according to claim 3, wherein in step (5):
after the contents were cooled to room temperature, the contents were diluted with pure water to a volume of 50 ml.
8. A method for monitoring and pretreating arsenic and mercury in soil by using the digestion tank prepared according to the claims 1-4, which is characterized by comprising the following steps:
(1) placing soil to be detected into the digestion tank;
(2) adding aqua regia into the digestion tank;
(3) putting the digestion tank into a graphite digestion device for constant-temperature heating;
(4) diluting the heated contents in the digestion tank to a constant volume to obtain a pre-treatment sample.
9. The method of claim 8, wherein in step (3):
the tank body is connected with the tank cover before the digestion tank is heated, the constant-temperature heating temperature is 160 ℃, and the constant-temperature heating is carried out by using a porous graphite constant-temperature digestion device.
10. The method of claim 8, wherein in step (4):
after the contents were cooled to room temperature, the contents were diluted with pure water to a volume of 25 ml.
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| CN201911345146.9A CN110954391A (en) | 2019-12-24 | 2019-12-24 | Digestion tank for monitoring pretreatment of elements in soil and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112649276A (en) * | 2020-12-30 | 2021-04-13 | 中国地质大学（武汉） | Method for digesting geological sample by using ammonium bifluoride or ammonium fluoride |
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