CN220120510U - Pretreatment device for solid sample mercury isotope analysis determination - Google Patents

Pretreatment device for solid sample mercury isotope analysis determination Download PDF

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CN220120510U
CN220120510U CN202321604909.9U CN202321604909U CN220120510U CN 220120510 U CN220120510 U CN 220120510U CN 202321604909 U CN202321604909 U CN 202321604909U CN 220120510 U CN220120510 U CN 220120510U
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heating
sample
mercury
heating pipe
solid sample
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张辉
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Institute of Geochemistry of CAS
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Institute of Geochemistry of CAS
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Abstract

The utility model relates to the technical field of mercury sampling analysis, in particular to a pretreatment device for solid sample mercury isotope analysis and determination. The device includes sample support, heating pipe, heating furnace, catalytic tube, reaction tank and zero gas pitcher, the sample support sets up heating pipe one end, just be provided with the air inlet on the heating pipe, the heating pipe other end with catalytic tube connects, the catalytic tube is provided with second heating device outward, the heating furnace sets up the heating pipe middle part, and right the heating pipe heats, catalytic tube lets in confined in the reaction tank, reaction tank top export with zero gas pitcher intercommunication. By introducing the secondary heating and catalysis processes of the sample, the sample pretreatment method of the solid sample mercury isotope analysis is unified, the full and complete conversion and oxidation preservation of mercury in the sample are ensured, and the precision and accuracy of the solid sample mercury isotope analysis measurement are improved.

Description

Pretreatment device for solid sample mercury isotope analysis determination
Technical Field
The utility model relates to the technical field of mercury sampling analysis, in particular to a pretreatment device for solid sample mercury isotope analysis and determination.
Background
With the rapid development of mercury isotope analysis technology in recent years, the method has been widely applied to the fields of geology, environment, archaeology and the like. The migration and conversion process of mercury in a sample can be analyzed according to the fractionation mechanism of mercury isotopes, thereby researching various environmental processes and characteristics. However, a series of pre-treatments of the sample are required before mercury isotope analysis determination can be performed using a multi-receiving inductively coupled plasma mass spectrometer (MC-ICP-MS). For a solid sample, firstly, mercury in the sample is required to be digested and extracted by a wet chemical method, or is required to be completely transferred into an oxidizing solution for preservation by high-temperature thermal analysis, then the mercury is reduced into elemental mercury by a reducing reagent, and then the elemental mercury enters MC-ICP-MS for mercury isotope determination. The pretreatment method of the solid sample does not have unified standards and a relatively perfect pretreatment device. Therefore, in the process of measuring the solid sample mercury isotopes, the sample injection and heating modes are not uniform, mercury in the sample is insufficient in oxidation reduction and is easy to pollute by the external atmosphere, the sample treatment efficiency is low, and errors are easy to generate.
At present, pretreatment methods for solid sample mercury isotope analysis mainly comprise two types: firstly, a chemical digestion method comprises the steps of electric plate digestion, microwave digestion, water bath digestion and the like, wherein the principle is that a certain amount of samples are taken, specific strong acid solution (hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, perchloric acid and the like) is added, then the samples are fully dissolved in a heating and microwave mode and the like, mercury in the samples is fully oxidized, supernatant or washing liquid is transferred to a volumetric flask and then added with a fixing liquid, and after the volume is fixed, the samples are uniformly shaken, and the mercury isotopes are analyzed by a next machine. And secondly, a pyrolysis method is mainly to put a sample into a muffle furnace, heat the sample at a high temperature of 500-1000 ℃, fully convert mercury in the sample into elemental mercury to be separated out through high temperature, load the elemental mercury into a strong acid solution through carrier gas for oxidation fixation, and finally take samples to reduce the elemental mercury into elemental mercury through a reducing agent for measuring mercury isotopes on a machine.
Because the form of mercury in a solid sample is complex, the pretreatment of the solid sample by the digestion method is complicated, a large amount of chemical reagents are needed to be prepared, human errors and reagent blanks are easy to introduce, different samples need to be digested by different acids, and the risk that the digestion is incomplete and the mercury in the sample is not completely oxidized exists. In addition, the digestion process needs professional experimenters and is carried out in a fume hood, so that the ordinary people can hardly complete the digestion process, and waste gas and waste liquid generated in the experiment process are harmful to human bodies. The pyrolysis method is an effective pretreatment method for analyzing solid sample mercury, however, at present, a sample injection mode and a heating pipe structure are not unified, and no secondary heating and catalysis are carried out on analysis gas (carrier gas) before the sample enters an oxidation solution, so that mercury in the sample is converted into elemental mercury incompletely, the oxidation solution is not isolated from the external atmosphere, and the atmospheric mercury solution in the environment is dissolved into the oxidation solution, so that analysis and research of mercury isotopes are affected.
Disclosure of Invention
First, the technical problem to be solved
The utility model aims to solve the technical problems that mercury in a sample is insufficient in oxidation and reduction and is easy to be polluted by the outside atmosphere due to non-uniform sample injection and heating modes.
(II) technical scheme
In order to solve the technical problems, the utility model provides a pretreatment device for solid sample mercury isotope analysis and determination, which comprises a sample support, a heating pipe, a heating furnace, a catalytic pipe, a reaction tank and a zero gas tank, wherein the sample support is arranged at one end of the heating pipe, an air inlet is arranged on the heating pipe, the other end of the heating pipe is connected with the catalytic pipe, a second heating device is arranged outside the catalytic pipe, the heating furnace is arranged in the middle of the heating pipe and is used for heating the heating pipe, the catalytic pipe is introduced into the closed reaction tank, and an outlet at the top of the reaction tank is communicated with the zero gas tank.
Further, the second heating device is a heating wire sleeved outside the catalytic tube, and the heating wire is used for carrying out secondary heating on the catalytic tube.
Further, a sealing plug is arranged at one end of the sample support, a wedge-shaped socket matched with the sealing plug is arranged at one end of the heating pipe, and the sample support is inserted into the wedge-shaped socket through the sealing plug and is connected with one end of the heating pipe.
Further, vaseline is coated on the sealing plug and/or the wedge-shaped socket.
Further, the other end of the sample holder is provided with a groove.
Further, the catalyst in the catalytic tube adopts silicon carbide.
Further, the oxidation reagent in the reaction tank adopts anti-aqua regia.
Further, the mercury absorbing material in the zero gas tank adopts activated carbon.
(III) beneficial effects
The technical scheme of the utility model has the following advantages: by introducing the secondary heating and catalysis processes of the sample, the sample pretreatment method of the solid sample mercury isotope analysis is unified, the full and complete conversion and oxidation preservation of mercury in the sample are ensured, and the precision and accuracy of the solid sample mercury isotope analysis measurement are improved. The traditional wet chemical digestion method is abandoned, the consumption of samples and reagents and the production of waste liquid and waste gas are greatly reduced, and human errors and reagent errors are reduced.
Drawings
FIG. 1 is a schematic structural diagram of a pretreatment device for solid sample mercury isotope analysis determination according to the present utility model;
in the figure: 1. a sample holder; 2. heating pipes; 3. a heating furnace; 4. a catalytic tube; 5. a reaction tank; 6. zero gas tank; 7. an air inlet; 8. a heating wire; 9. and (5) sealing plugs.
Detailed Description
The following describes in further detail the embodiments of the present utility model with reference to the drawings and examples. The following examples are illustrative of the utility model and are not intended to limit the scope of the utility model.
In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
Referring to fig. 1, the utility model provides a pretreatment device for solid sample mercury isotope analysis and determination, which comprises a sample holder 1, a heating pipe 2, a heating furnace 3, a catalytic pipe 4, a reaction tank 5 and a zero gas tank 6. Sample holds in palm 1 and sets up heating pipe 2 one end, just be provided with air inlet 7 on the heating pipe 2, air inlet 7 can connect 1/4 inch teflon pipe and oxygen hose intercommunication, guarantees the continuous import of oxygen, the export of heating pipe 2 is designed to connectable 1/4 inch teflon pipe, the heating pipe 2 other end pass through teflon pipe with catalysis pipe 4 is connected, catalysis pipe 4 is provided with the second heating device outward, heating furnace 3 sets up heating pipe 2 middle part, and right heating pipe 2 heats, catalysis pipe 4 lets in confined in the reaction tank 5, the export of reaction tank 5 top with zero gas pitcher 6 intercommunication. The sample holder 1, the heating pipe 2 and the reaction tank 5 are all made of quartz materials, and other pipe fittings and connecting pieces are all made of quartz or Teflon materials, so that the adsorption of the materials to mercury is prevented; the heating furnace 3 is designed as a tube heating furnace 3 suitable for a new type of heating tube 2, and the temperature can be programmed.
When the mercury sample pretreatment method is used, the heating furnace 3 is used for heating the solid sample on the sample holder 1 in the heating pipe 2, so that mercury in each form in the solid sample is converted into elemental mercury, and then the elemental mercury enters the catalytic tube 4 along with oxygen introduced from the air inlet 7, and as the catalytic tube 4 is provided with a secondary heating device, the sample pretreatment method for mercury isotope analysis of the solid sample is unified through the secondary heating and catalytic process of the introduced sample, the full and complete conversion and oxidation preservation of mercury in the sample are ensured, and the precision and accuracy of mercury isotope analysis measurement of the solid sample are improved. Meanwhile, the traditional wet chemical digestion method is abandoned, mercury in the gas separated out from the reaction tank 5 can be discharged into the atmosphere after being filtered by the zero gas tank 6, and mercury in the external atmosphere entering the reaction tank 5 can also be filtered, so that pollution and interference of the external atmospheric mercury to an oxidation solution are ensured, consumption of samples and reagents and production of waste liquid and waste gas are greatly reduced, and human errors and reagent errors are reduced.
In some embodiments, the second heating device is a heating wire 8 sleeved outside the catalytic tube 4, the heating wire 8 is used for performing secondary heating on the catalytic tube 4, the heating wire 8 can adopt resistance type heating, and the resistance is heated by introducing direct current, so that the heating purpose is achieved.
In some embodiments, a sealing plug 9 is disposed at one end of the sample holder 1, a wedge-shaped socket matched with the sealing plug 9 is disposed at one end of the heating tube 2, and the sample holder 1 is inserted into the wedge-shaped socket through the sealing plug 9 and connected with one end of the heating tube 2, so that external atmosphere cannot enter the heating tube 2. Further, the sealing plug 9 and/or the wedge-shaped socket are/is coated with vaseline, which enhances the tightness between the sealing plug 9 and the wedge-shaped socket.
In some embodiments, the other end of the sample holder 1 is provided with a recess for receiving a solid sample that has been ground to a powder.
In some embodiments, the catalyst in the catalytic tube 4 is made of silicon carbide or a high temperature refractory material such as compliant fragments.
In some embodiments, the oxidizing agent in the reaction tank 5 adopts anti-aqua regia (a mixture of concentrated nitric acid and concentrated hydrochloric acid according to a volume ratio of 1:3), and other strong oxidizing agents can be sampled according to the subsequent analysis requirements.
In some embodiments, the mercury absorbing material in the zero gas tank 6 is activated carbon, or other mercury absorbing material.
The foregoing is merely a preferred embodiment of the present utility model, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the technical principles of the present utility model, and these modifications and variations should also be regarded as the scope of the utility model.

Claims (8)

1. The pretreatment device for the solid sample mercury isotope analysis determination is characterized by comprising a sample support, a heating pipe, a heating furnace, a catalytic pipe, a reaction tank and a zero gas tank, wherein the sample support is arranged at one end of the heating pipe, an air inlet is formed in the heating pipe, the other end of the heating pipe is connected with the catalytic pipe, a second heating device is arranged outside the catalytic pipe, the heating furnace is arranged at the middle part of the heating pipe and is used for heating the heating pipe, the catalytic pipe is led into the reaction tank which is sealed, and an outlet at the top of the reaction tank is communicated with the zero gas tank.
2. The pretreatment device for solid sample mercury isotope analysis measurement according to claim 1, wherein the second heating device is a heating wire sleeved outside the catalytic tube, and the heating wire is used for carrying out secondary heating on the catalytic tube.
3. The pretreatment device for solid sample mercury isotope analysis and determination according to claim 1, wherein a sealing plug is arranged at one end of the sample holder, a wedge-shaped socket matched with the sealing plug is arranged at one end of the heating pipe, and the sample holder is inserted into the wedge-shaped socket through the sealing plug and is connected with one end of the heating pipe.
4. A pretreatment device for solid sample mercury isotope analysis assay according to claim 3, wherein the sealing plug and/or the wedge-shaped socket is coated with petrolatum.
5. A pretreatment device for solid sample mercury isotope analysis assay according to claim 3, wherein the other end of the sample holder is provided with a groove.
6. The pretreatment device for solid sample mercury isotope analysis assay according to claim 1, wherein the catalyst in the catalytic tube is silicon carbide.
7. The pretreatment device for solid sample mercury isotope analysis assay according to claim 1, wherein the oxidizing agent in the reaction tank is anti-aqua regia.
8. The pretreatment device for solid sample mercury isotope analysis assay according to claim 1, wherein the mercury absorbing material in the zero gas tank is activated carbon.
CN202321604909.9U 2023-06-21 2023-06-21 Pretreatment device for solid sample mercury isotope analysis determination Active CN220120510U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321604909.9U CN220120510U (en) 2023-06-21 2023-06-21 Pretreatment device for solid sample mercury isotope analysis determination

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321604909.9U CN220120510U (en) 2023-06-21 2023-06-21 Pretreatment device for solid sample mercury isotope analysis determination

Publications (1)

Publication Number Publication Date
CN220120510U true CN220120510U (en) 2023-12-01

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202321604909.9U Active CN220120510U (en) 2023-06-21 2023-06-21 Pretreatment device for solid sample mercury isotope analysis determination

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