Digestion device for analyzing trace metal elements in high-purity quartz

Abstract

The utility model discloses a digestion device for analyzing trace metal elements in high-purity quartz, and relates to the technical field of equipment for analyzing trace metal elements in quartz, the digestion device comprises a digestion unit, the digestion unit comprises a PFA tank body, the PFA tank body is internally provided with a reaction cavity, and the reaction cavity is internally provided with a reaction cavity; a gas inlet pipe, a gas outlet pipe and a liquid adding pipe which are respectively communicated with the reaction cavity are arranged on the PFA tank body, a gas inlet valve and a gas outlet valve are respectively arranged on the gas inlet pipe and the gas outlet pipe, and a sealing cover is arranged at the liquid adding end of the liquid adding pipe. The PFA tank body is used as the reaction cavity, the appearance is transparent, the reaction completion condition in the reaction cavity is convenient to observe, the PFA tank body is resistant to high temperature and strong acid, metal elements are prevented from being dissolved out of the reaction tank and hydrofluoric acid, and the analysis accuracy of trace metal elements in quartz is improved.

Description

Technical Field

[0001] The present application relates to the technical field of equipment for analyzing trace metal elements in quartz, and in particular to a digestion device for analyzing trace metal elements in high-purity quartz. Background Art

[0002] Existing technologies often use inductively coupled plasma mass spectrometry (ICP-MS) or inductively coupled plasma optical emission spectroscopy (ICP-OES) to analyze trace metals in high-purity quartz. Both methods require that the quartz solid be processed into a liquid before sampling and testing can be achieved. The principle of processing quartz is often to utilize the reaction of quartz (SiO2) with hydrofluoric acid (HF) to form gaseous silicon tetrafluoride (SiF4) and water. However, due to the material of the reaction tank, the quality of hydrofluoric acid, and the reaction conditions that require heating, this reaction is often prone to introducing external metal element contamination, affecting the accuracy of the analysis.

[0003] In the prior art, the equipment for generating gaseous silicon tetrafluoride (SiF4) and water by the reaction of quartz (SiO2) and hydrofluoric acid (HF) mainly includes platinum crucibles and polytetrafluoroethylene reaction tanks. During the reaction, the quartz is first calcined in a Class 1000 clean room with a platinum crucible, and then hydrofluoric acid is added to the polytetrafluoroethylene reaction tank for microwave digestion. However, the powder material of the polytetrafluoroethylene main body has a large specific surface area and cannot be processed by melt injection molding. Therefore, more metal elements are often precipitated therein, and the acid removal process after digestion is also prone to metal element contamination. It requires extremely high proficiency of the operator and is difficult to stably complete the content of 10 -9 (ppb level) and below metal element analysis process. Utility Model Content

[0004] The present application aims to solve at least one of the technical problems existing in the prior art. To this end, the present application provides a digestion device for analyzing trace metal elements in high-purity quartz.

[0005] The purpose of this application can be achieved through the following technical solutions:

[0006] The present application provides a digestion device for analyzing trace metal elements in high-purity quartz, the digestion device comprising at least one digestion unit, each of the digestion units comprising a PFA tank body, the PFA tank body comprising a reaction chamber, an air inlet pipe, an air outlet pipe, and a liquid adding pipe respectively connected to the reaction chamber being installed on the PFA tank body, the air inlet pipe and the air outlet pipe being respectively provided with an air inlet valve and an air outlet valve, and the liquid adding end of the liquid adding pipe being provided with a sealing cover.

[0007] In one or more embodiments of the present application, a plurality of digestion units are arranged in parallel, the air inlet ends of the air inlet pipes of the plurality of digestion units are connected by a first connecting pipe, and the air outlet pipes of the plurality of digestion units are connected by a second connecting pipe.

[0008] In one or more embodiments of the present application, the air inlet pipe, the air outlet pipe and the liquid adding pipe are installed on the PFA tank through a four-way joint and communicate with the reaction chamber.

[0009] In one or more embodiments of the present application, the liquid adding end of the liquid adding tube is funnel-shaped.

[0010] In one or more embodiments of the present application, the digestion device further includes a heater configured to heat the PFA tank.

[0011] Preferably, a heating groove is provided on the upper surface of the heater, and the heating groove is configured to accommodate at least the bottom of the PFA tank.

[0012] Preferably, the heater is a graphite heating digester.

[0013] In one or more embodiments of the present application, the air inlet pipe is a PFA tube; and / or the air outlet pipe is a PFA tube; and / or the liquid adding pipe is a PFA tube.

[0014] Beneficial effects:

[0015] In the present application, an air inlet pipe, an air outlet pipe and a liquid adding pipe connected to the reaction chamber are provided, so that when adding reaction liquid (such as hydrofluoric acid) to the reaction chamber, high-purity nitrogen can also be introduced into the reaction chamber through the air inlet pipe during the reaction to protect the gas in the acid-catching process, so as to avoid the pollution of external particles and metal elements caused by open volatilization, and to accelerate the speed of hydrofluoric acid evaporation. The present application sets a plurality of digestion units in parallel, and the air inlet ends of the air inlet pipes of the plurality of digestion units are connected by a first connecting pipe, and the air outlet pipes of the plurality of digestion units are connected by a second connecting pipe, so that the gas flowing out of the plurality of digestion units can be centrally recovered and processed, thereby improving work efficiency and reducing recovery costs. The present application also uses a PFA tank body as a reaction chamber, which is transparent in appearance and is convenient for observing the completion of the reaction inside the reaction chamber, and the PFA tank body is resistant to high temperatures and strong acids, which avoids the dissolution of metal elements from the reaction tank in hydrofluoric acid and improves the accuracy of trace metal element analysis in quartz. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The present application will be further described below with reference to the accompanying drawings.

[0017] Figure 1 This is a schematic structural diagram of a digestion unit in one of the embodiments of the present application;

[0018] Figure 2 is a cross-sectional view of a digestion unit in one embodiment of the present application;

[0019] Figure 3 It is a structural schematic diagram of a digestion device consisting of three digestion units in one embodiment of the present application.

[0020] Description of reference numerals:

[0021] 1. PFA tank; 2. Air inlet pipe; 3. Air outlet pipe; 4. Liquid adding pipe; 5. Air inlet valve; 6. Air outlet valve; 7. Sealing cover; 8. First connecting pipe; 9. Second connecting pipe; 10. Four-way connector; 100. Digestion unit. DETAILED DESCRIPTION

[0022] The following will be combined with the accompanying drawings in the embodiments of this application to clearly and completely describe the technical solutions in the embodiments of this application. Obviously, the embodiments described are only part of the embodiments of this application, not all of the embodiments. Based on the embodiments of this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0023] In some embodiments, see Figure 1 and Figure 2 As shown, the present application provides a digestion device for analyzing trace metal elements in high-purity quartz, which is used to process the chemical reaction between high-purity quartz and hydrofluoric acid to precipitate the metal elements contained in the high-purity quartz.

[0024] The digestion device includes a digestion unit 100, which includes a PFA tank body 1. The PFA tank body 1 has a reaction chamber. The PFA tank body 1 is equipped with an air inlet pipe 2, an air outlet pipe 3 and a liquid adding pipe 4 respectively connected to the reaction chamber. The air inlet pipe 2 and the air outlet pipe 3 are respectively provided with an air inlet valve 5 and an air outlet valve 6, and the liquid adding end of the liquid adding pipe 4 is provided with a sealing cover 7.

[0025] In the present application, the PFA tank 1 is made of PFA material. PFA material is a high-performance polymer material and belongs to a fluorine-containing polymer (for example, perfluoropropyl perfluorovinyl ether and polytetrafluoroethylene copolymer) with excellent chemical stability, high temperature tolerance, low friction coefficient and good biocompatibility.

[0026] Before the reaction, the PFA tank 1 is first cleaned with ultrapure water, and then high-purity hydrofluoric acid is added to the reaction chamber of the PFA tank 1 from the liquid feeding end of the liquid feeding tube 4. After heating to 110°C for pretreatment, the PFA tank 1 is cleaned again with ultrapure water;

[0027] During the reaction, add the quartz sample into the PFA tank 1, close the air inlet valve 5 and the air outlet valve 6, open the sealing cover 7, add 5 to 10 times the mass of high-purity hydrofluoric acid (49%) into the reaction chamber from the liquid feeding end of the liquid feeding tube 4, close the sealing cover 7, heat to 100 ° C, and react until the quartz particles disappear;

[0028] After the reaction is complete, high-purity nitrogen is introduced from the air inlet end of the air inlet pipe 2 and the air inlet valve 5 and the air outlet valve 6 are opened. The temperature is raised to 110° C. and acid removal treatment is performed in a high-purity nitrogen atmosphere until the liquid in the reaction chamber disappears. The sealing cover 7 is then opened, and a 2% high-purity nitric acid solution with a mass of 5 to 10 times that of quartz is added from the liquid adding end of the liquid adding pipe 4 to extract the metal elements. The extract can be used for trace metal element analysis by inductively coupled plasma mass spectrometry or inductively coupled plasma spectrometry.

[0029] In some embodiments, the air inlet pipe 2 is made of PFA tube; and / or, the air outlet pipe 3 is made of PFA tube; and / or, the liquid adding pipe 4 is made of PFA tube, so as to prevent the metal elements precipitated in the air inlet pipe 2 and / or the air outlet pipe 3 and / or the liquid adding pipe 4 from flowing into the extract during the reaction process and affecting the accuracy of the metal content in the extract.

[0030] Preferably, in this embodiment, the air inlet pipe 2, the air outlet pipe 3 and the liquid adding pipe 4 are all made of PFA material.

[0031] In some embodiments, see Figure 1 and Figure 2 As shown, the liquid adding end of the liquid adding tube 4 is funnel-shaped, which is convenient for adding the reaction liquid.

[0032] In some embodiments, see Figure 1 and Figure 2 As shown, to facilitate installation of the air inlet pipe 2, air outlet pipe 3, and liquid addition pipe 4 on the PFA tank body 1, a four-way joint 10 is sealed over the opening of the PFA tank body 1. The air inlet pipe 2, air outlet pipe 3, and liquid addition pipe 4 are sealed and plugged into the other three openings of the four-way joint 10 to communicate with the reaction chamber. The air inlet pipe 2 and air outlet pipe 3 are plugged into the four-way joint 10 horizontally at both ends; the liquid addition pipe 4 is plugged into the four-way joint 10 vertically from the top, extending through the interior of the four-way joint 10 and at least partially into the reaction chamber.

[0033] In some embodiments, the digestion device further includes a heater (not shown), which is configured to heat the PFA tank 1 .

[0034] Specifically, a heating groove is provided on the upper surface of the heater, and the heating groove is configured to accommodate at least the bottom of the PFA tank body 1 so as to limit the PFA tank body 1 when the heater heats the PFA tank body 1 to prevent the PFA tank body 1 from tipping over.

[0035] Exemplarily, the heater is a graphite heating digester.

[0036] In some embodiments, see Figure 3 As shown, multiple digestion units 100 are arranged in parallel so that multiple groups of high-purity quartz can be processed simultaneously. Specifically, the digestion device also includes a first connecting pipe 8 and a second connecting pipe 9. The air inlet ends of the air inlet pipes 2 of the multiple digestion units 100 are connected through the first connecting pipe 8, and the air outlet pipes 3 of the multiple digestion units 100 are connected through the second connecting pipe 9. During the reaction, the external gas source can simultaneously provide high-purity nitrogen to the air inlet pipes 2 of the multiple digestion units 100 through the first connecting pipe 8, and the gas in the air outlet pipe 3 of each digestion unit 100 can be discharged centrally through the second connecting pipe 9, realizing centralized treatment.

[0037] The above is a detailed description of an embodiment of the present application. However, the content is only a preferred embodiment of the present application and cannot be considered to limit the scope of implementation of the present application. All equivalent changes and improvements made within the scope of the present application should still fall within the scope of the patent application.

[0038] It should be noted that the terms "first", "second" and similar terms used in this application do not indicate any order, quantity or importance, but are only used to distinguish different components. The descriptions of the directions of "left", "right", "left side", "right side", "upper", "lower", "top", "bottom" and so on in this application are all defined based on the relationship between the orientations or positions shown in the accompanying drawings. They are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the structure must be constructed and operated in a specific orientation. Therefore, they cannot be understood as limitations on this application. In the description of this application, the meaning of "multiple" is more than two, unless otherwise clearly and specifically defined.

[0039] In the description of this application, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to direct connections, indirect connections through an intermediate medium, or internal communication between two components. Those skilled in the art will understand the specific meanings of these terms in this application based on specific circumstances.

Claims

1. A digestion device for analysis of trace metal elements in high-purity quartz, characterized in that: The digestion device includes at least one digestion unit, each of which includes a PFA tank body, a reaction chamber provided therein, an air inlet pipe, an air outlet pipe, and a liquid adding pipe respectively connected to the reaction chamber, the air inlet pipe and the air outlet pipe are respectively provided with an air inlet valve and an air outlet valve, and a sealing cap is provided at the liquid adding end of the liquid adding pipe; A plurality of the digestion units are arranged in parallel, the air inlet ends of the air inlet pipes of the plurality of digestion units are connected via a first connecting pipe, and the air outlet pipes of the plurality of digestion units are connected via a second connecting pipe.

2. The digestion device according to claim 1, characterized in that The air inlet pipe, the air outlet pipe and the liquid adding pipe are installed on the PFA tank body through a four-way joint and are communicated with the reaction chamber.

3. The digestion device according to claim 1, characterized in that The liquid adding end of the liquid adding tube is funnel-shaped.

4. The digestion device according to claim 1, characterized in that The air inlet pipe is a PFA pipe; and / or the air outlet pipe is a PFA pipe; and / or the liquid adding pipe is a PFA pipe.

5. The digestion device according to any one of claims 1 to 4, characterized in that: The digestion device further includes a heater configured to heat the PFA tank.

6. The digestion device according to claim 5, characterized in that: A heating groove is provided on the upper surface of the heater, and the heating groove is configured to accommodate at least the bottom of the PFA tank.

7. The digestion device according to claim 5, characterized in that: The heater is a graphite heating digester.

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