KR102357430B1 - Sample pretreatment apparatus and sample pretreatment method - Google Patents

Abstract

The present invention relates to a chemical pretreatment technology, and more particularly, in order to analyze chemicals contained in air, high-purity gas, chemical gas, liquid, and an analysis sample of a semiconductor substrate, etc., the chemical is transferred to a separate container before being introduced into the analyzer. to a sample pretreatment device configured to perform pretreatment by performing evaporation, dilution and dissolution, and the like, and a sample pretreatment method using the same.
In order to achieve the above technical object, the sample pre-processing apparatus and method of the present invention are for pre-processing a sample solution containing an analysis target material before providing it to an analyzer, and include an internal space in which the sample solution to be pre-treated is supported. used chemical vessel; and a heating unit that heats the sample solution supported on the chemical vessel unit to evaporate the solvent to form chemical fume, and discharges the chemical fume formed by the heating unit and supplies an alternative solvent to the chemical vessel unit to form a pretreatment sample solution.

Description

SAMPLE PRETREATMENT APPARATUS AND SAMPLE PRETREATMENT METHOD

The present invention relates to a sample pre-processing apparatus and a sample pre-processing method, and more particularly, introducing a sample solution into an analyzer to analyze chemicals contained in an analysis sample such as air, high-purity gas, chemical gas, liquid, and semiconductor substrate. It relates to a sample pretreatment apparatus and a sample pretreatment method equipped to transfer a sample solution to a separate container and perform pretreatment by performing room temperature/high temperature chemical reaction, evaporation, and dilution dissolution.

Air, high-purity gas, chemical gas, liquid, etc. may contain metals and metal compounds, which have adverse effects such as harmful effects on the human body, as well as atmospheric or various gases containing metals and metal compounds. However, when it is used at the manufacturing site, it causes a problem that the test result or the state of the product deteriorates.

In particular, in the semiconductor device manufacturing process, if any impurity exists even in a trace amount, its characteristics are greatly affected. Problems such as lowering the yield of the entire semiconductor device may occur. Therefore, in order to improve the characteristics of the semiconductor device, it is necessary to suppress the impurity content as low as possible, and it is absolutely necessary to accurately analyze the impurity concentration as a premise for technological improvement activities to suppress the impurity amount.

For this reason, continuous real-time contamination monitoring of chemical gases used in wafer processes for manufacturing semiconductor devices is required. In order to analyze chemical gases in the analyzer, it is necessary to pre-process the sample according to the practically impossible characteristics of direct analysis and the demand for improvement of analysis accuracy.

As such, for example, chemical samples used in the process on the peninsula are destructive analysis methods such as atomic absorption spectroscopy and inductively coupled mass spectroscopy (ICP-mass spectroscopy) or total reflection fluorescence X-ray analysis ( It can be analyzed by non-destructive analysis methods such as total X-ray fluorescent analyzer). Usually, the solvent of the analysis sample prepared for the chemical analysis of the total amount of metal and metal components in the solution is often unsuitable for the analyzer, so the solvent needs to be removed or replaced.

As a prior art, for chemical pretreatment, pretreatment was performed on the sample through manual sample transfer, high temperature chemical reaction, evaporation, and dilution and dissolution, and this prior art can prevent damage to the human body due to harmful chemicals, differences between analyzers, etc. There may be disadvantages, and there is no technical means to smoothly transfer the residual analyte to the analyzer after evaporating the solvent, which is inconvenient, and the reliability of the analysis data due to sample contamination and reduced repeatability due to exposure of chemicals to the atmosphere after dilution and dissolution There were difficulties in lowering the

Accordingly, the present invention is to improve the conventional problems as described above, and by transferring the sample solution containing the analyte to a separate container for pretreatment and then transferring the pretreated pretreatment sample solution to the analyzer, failure/damage of the analyzer An object of the present invention is to provide a sample pre-processing apparatus and a sample pre-processing method for reducing probability and preventing sample contamination to increase analysis reliability.

In order to achieve the above technical object, a sample pre-processing device according to an embodiment of the present invention is a sample pre-processing device for pre-processing a sample solution containing an analyte before providing it to an analyzer, and the sample solution to be pre-treated is supported. a chemical vessel unit having an internal space; and a heating unit that heats the sample solution supported in the chemical vessel unit to evaporate the solvent to form chemical fume, and discharges the chemical fume formed by the heating unit and supplies an alternative solvent to the chemical vessel unit to form a pretreatment sample solution.

In addition, the sample pre-processing apparatus according to an embodiment of the present invention is provided with a chemical entrance to the vessel cover, which is located and coupled to the upper portion of the chemical vessel, so as to introduce the sample solution into the chemical vessel or to discharge the chemical fume. can be

In addition, in the sample preprocessing apparatus according to an embodiment of the present invention, the chemical entrance may include: a first chemical entrance for transferring an external sample solution to the inside of the chemical vessel; a second chemical entrance for discharging the internal chemical fume to the outside; A third chemical entrance to transport the alternative solvent; may be configured to include.

In addition, in the sample pre-processing apparatus according to an embodiment of the present invention, the heating unit is formed in a shape surrounding the outside of the chemical vessel unit, the vessel guide formed of a heat conductor; and a heater installed in the vessel guide to heat the sample solution carried in the chemical vessel unit.

In addition, the sample pre-processing apparatus according to an embodiment of the present invention is connected to the discharge part of the chemical vessel part at the lower end of the chemical vessel part, and a first valve for transferring the pretreatment sample solution inside the chemical vessel part to the analyzer. A valve assembly configured to include; may be further provided.

In addition, in the sample pre-processing apparatus according to an embodiment of the present invention, the valve assembly may include: a second valve for injecting washing water; A third valve serving as a passage for discharging a solution inside the chemical vessel unit; may be configured to include.

In addition, in the sample pre-processing apparatus according to an embodiment of the present invention, the valve assembly, a fourth valve for introducing a gas for stirring from the lower side of the chemical vessel; may be configured to include.

In addition, in the sample pretreatment apparatus according to an embodiment of the present invention, the chemical vessel part is formed in a detachable structure and mounted on the sample pretreatment apparatus before performing the pretreatment process to prepare for pretreatment.

In addition, the sample pre-processing apparatus according to an embodiment of the present invention may further include a cooling unit to prevent overheating of the chemical vessel unit in the process of forming the chemical fume by the heating unit.

In addition, the sample pretreatment method according to an embodiment of the present invention is a sample pretreatment method for pretreatment before providing a sample solution containing an analyte to the analyzer. The sample solution to be pretreated is introduced into the internal space of the chemical vessel unit. introduction step; and a chemical fume discharge step of heating the introduced sample solution by a heating unit to evaporate the solvent of the sample solution and discharge it in the form of chemical fume; and a pretreatment sample forming step of supplying an alternative solvent to the chemical vessel unit to form a pretreatment sample solution. In addition, after the pretreatment sample forming step, a pretreatment sample transfer step of transferring the pretreatment sample solution inside the chemical vessel unit to the analyzer through the first valve connected to the chemical vessel unit at the lower end of the chemical vessel unit; can

In addition, in the sample pretreatment method according to an embodiment of the present invention, in the step of discharging the chemical fume, the solvent of the sample solution is evaporated by the heating unit to prevent overheating of the chemical vessel in the process of discharging it in the form of chemical fume. For this, the cooling unit may be additionally driven.

In addition, in the sample pretreatment method according to an embodiment of the present invention, the pretreatment sample forming step includes an alternative solvent supply step of supplying an alternative solvent to the chemical vessel unit; while supplying the alternative solvent or supplying the alternative solvent After this is completed, it may be configured to introduce gas for stirring from the lower side of the chemical vessel part.

In addition, the sample pretreatment method according to an embodiment of the present invention, before the introduction step or after the pretreatment sample forming step, a cleaning step of supplying cleaning water to clean the internal space of the chemical vessel part; may be configured to include.

According to the means for solving the above problems, the sample preprocessing apparatus according to the present invention is configured to include a chemical vessel part and a heating part so as to provide a separate container to perform pretreatment of the sample solution in the container, and the heating part By discharging the chemical fumes formed by the process and supplying an alternative solvent to the chemical vessel part to form a pretreatment sample solution, the pretreatment operation of the sample solution is efficiently processed to shorten the analysis time and process time, and the solvent of the sample solution is replaced with an alternative solvent By replacing it with the analyzer, damage to the analyzer can be reduced and the lifespan of the analyzer can be extended. In addition, there are advantages such as prevention of sample contamination due to exposure to air by automating manual operations, securing the safety of the analyst, and improving processing capacity (capacity) due to 24-hour operation.

It should be understood that the effects of the present invention are not limited to the above-described effects, and include all effects that can be inferred from the configuration of the invention described in the detailed description or claims of the present invention.

1 is a plan view illustrating the overall configuration of a pre-processing sampler including a sample pre-processing apparatus of the present invention.
2 is an overall cross-sectional view of a sample pre-processing apparatus according to an embodiment of the present invention.
3 is a perspective view of a chemical cover part of the sample pre-processing apparatus according to an embodiment of the present invention;
4 is a view of various examples of chemical tubes that are introduced into the chemical vessel unit in the sample pre-processing apparatus according to an embodiment of the present invention.
5 is a detailed structure of the upper structure of the chemical vessel and the sealing member in the sample pre-processing apparatus according to an embodiment of the present invention.
6 is a schematic diagram of a detachable structure of a sample pre-processing apparatus according to an embodiment of the present invention.
7 is a modified example of a sample pre-processing apparatus according to an embodiment of the present invention.
8 is a schematic diagram of a detachable structure in a modified embodiment of the sample pre-processing apparatus according to an embodiment of the present invention.
9 is an exemplary view of the use of the valve assembly in the sample pre-processing apparatus according to an embodiment of the present invention.

Hereinafter, the present invention will be described with reference to the accompanying drawings. However, the present invention may be embodied in several different forms, and thus is not limited to the embodiments described herein.

Throughout the specification, when a part is said to be “connected (connected, contacted, coupled)” with another part, it is not only “directly connected” but also “indirectly connected” with another member interposed therebetween. "Including cases where In addition, when a part "includes" a certain component, this means that other components may be further provided, rather than excluding other components, unless otherwise stated.

The terminology used herein is used only to describe specific embodiments, and is not intended to limit the present invention. The singular expression includes the plural expression unless the context clearly dictates otherwise. In the present specification, terms such as “comprise” or “have” are intended to designate that a feature, number, step, operation, component, part, or combination thereof described in the specification exists, but one or more other features It should be understood that this does not preclude the existence or addition of numbers, steps, operations, components, parts, or combinations thereof.

As used herein, the term 'sample', 'sample solution', or 'sample solution' refers to a liquid fluid in which a substance to be analyzed (hereinafter, 'analytical substance') is dissolved or dispersed. At this time, when the sample solution is introduced into the sample pre-processing device, it is sufficient if it is in a liquid state, and the analyte is collected or dissolved from air, high-purity gas, chemical gas, liquid, semiconductor substrate, etc. and is present in the sample solution. In addition, as used herein, 'chemical' is a word that refers to a chemical substance, and includes not only process chemicals used in the process, but also 'sample' or 'sample solution' or fume gas generated by heating the sample solution. It may be a word, and it can be clearly understood from the context.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings.

1 is an explanatory view illustrating the overall configuration of a pretreatment sampler 100 including a sample pretreatment apparatus of the present invention, a sample pretreatment apparatus 110 and a heater controller 120 , a first chemical storage tank 130 , and a medicine vessel 140 , the second drug storage tank 150 , the utility 160 , and may be configured to include an eggplant bottle 170 , but is not limited thereto. In addition, the analysis apparatus 200 illustrated by way of example includes an automatic calibration function and may include an ICPMS for measuring metal contamination levels, such as a contaminant analysis apparatus used in a semiconductor production process, but is limited thereto. It may be configured by replacing or exchanging a conventional analysis device.

The sample pre-processing apparatus 110 according to an embodiment of the present invention is located on one side of the pre-processing sampler 100, receives a sample solution containing an analyte from an external flow path, and holds a predetermined capacity in a container provided in the apparatus. and performs a pre-treatment function of diluting the sample solution supported in the container by heating and evaporating the sample solution with a pre-treatment solution so that the analyzer can analyze it with a heater located outside the container. At this time, the fume gas or inert gas for purge purpose generated when the sample solution is heated may be discharged through the exhaust port provided at the upper end of the sample pre-treatment device, and the pre-processed sample is transferred to a valve or valve assembly connected to the discharge pipe at the bottom of the sample pre-treatment device. can be transferred to the analyzer.

In order to perform such a pre-processing function, the sample pre-processing device 110 includes a chemical vessel unit that supports a predetermined amount of a sample solution and a heating unit that heats the sample solution of the chemical vessel unit. A first chemical inlet for injecting a sample from the outside into the chemical vessel in the sample preprocessing apparatus, a second chemical inlet for discharging fume gas, and a third chemical inlet for injecting an alternative solvent may be provided in the vessel cover of the chemical vessel. , if necessary, may be provided with a fourth chemical inlet through which the inert gas is injected. In addition, an additional configuration may be included, and details will be described later.

On the other hand, the heater controller 120 of the pre-processing sampler 100 performs a function of controlling the heater of the sample pre-processing apparatus 110, for example, may be configured to apply a control algorithm such as PID control. As described above, the present invention provides a sample pretreatment device ( 110), such as temperature stability improvement, can be implemented.

In addition, the first chemical storage tank 130 of the pretreatment sampler 100 may be used as a chemical for dissolving metal contaminants remaining on the inner surface of the vessel by remaining solidified by evaporation of the solvent during the sample pretreatment process. At this time, if necessary, it can be used by diluting each other at an appropriate ratio by adjusting the concentration of the two or other chemicals.

In addition, the chemical vessel 140 of the pretreatment sampler 100 is configured to store a standard solution required for the calibration of the analyzer. For example, a metal standard of a certain concentration is dissolved in a nitric acid solution diluted to a concentration of 2%, and it is used for calibration of the analyzer by diluting it at a certain ratio if necessary.

In addition, the second chemical storage tank 150 of the pretreatment sampler 100 is used for cleaning the pretreatment vessel, the vessel, and the solution transfer pipe as a whole. For example, it can be used when the same chemical as that of the first drug storage tank is stored in a thick concentration and the central supply of the chemical is not smooth. In addition, nitric acid, hydrofluoric acid, etc. are stored and when solid residue is generated, it can be used as a concentrated aqueous solution for quick cleaning. It can also be used after dilution as needed. At this time, if necessary, it can be used by diluting each other at an appropriate ratio by adjusting the concentration of the two or other chemicals.

In addition, the utility 160 of the pretreatment sampler 100 is a configuration used for sample transfer, cleaning, etc., and may be used, for example, to provide nitrogen gas, cooling water, ultrapure water, and valve opening/closing air.

In addition, the eggplant bottle 170 of the pretreatment sampler 100 may be used with a central supply of an analysis sample as a configuration for manually or manually loading a chemical sample required for analysis. In the case of pretreatment of certain specific chemicals, for example, HCDS, only the pretreatment time takes 4 hours or more in total, and for this purpose, it may be used to prepare the next sample. It may be formed in a structure in which an analyst puts a sample required for analysis in an eggplant bottle and uses it by mounting and connecting to the equipment. That is, FIG. 1 shows the implementation to use four pre-treatment heaters at the same time.

The sample pre-processing apparatus according to an embodiment of the present invention may have a detailed structure as shown in the overall cross-sectional view in FIG. It is possible to implement a pretreatment function of heating the included sample solution to remove the unwanted solvent and diluting the remaining solute with an appropriate alternative solvent.

In order to perform the pretreatment function, the sample pretreatment apparatus of the present invention includes a chemical vessel unit 10 having an internal space for supporting a sample solution introduced from the outside, and heating the sample solution carried in the chemical vessel unit to heat the solvent. It is configured to include a heating unit that evaporates to form a chemical fume, and discharges the chemical fume formed by the heating unit and supplies an alternative solvent to the chemical vessel unit to form a pretreatment sample solution to perform the pretreatment process.

In the present invention, the sample, the sample solution, or the sample solution may be a solution containing contaminants of the substrate, and vapor phase decomposition (VPD) is performed to analyze the contaminants of the substrate, so that an etching solution and/or a scan solution It may be a sample solution in a state in which contaminants are collected. In this case, the etching solution is a solution for bulk etching the wafer, which is the substrate to be analyzed, and may be a solution containing hydrofluoric acid, nitric acid, or ultrapure water. The scan solution is a solution supplied or recovered by the nozzle to scan the substrate or to collect contaminants on the substrate. If necessary, the scan solution may be a solution commonly used in a normal scan, and a solution containing hydrofluoric acid, hydrogen peroxide or ultrapure water can be

In the sample preprocessing apparatus of the present invention, the chemical vessel unit 10 has an internal space to store the sample solution and perform dilution and mixing with an alternative solvent, and at the lower end of the chemical vessel unit 10, A discharge part 11 providing a passage role to discharge the solution may be provided. Here, the capacity and thickness of the chemical vessel part are not particularly limited, and for example, a capacity of 14 ml and a thickness of 2 mm may be used. In addition to the form illustrated by way of example in the drawings, the shape of the container can be changed for the convenience of the user, and the lower end of the container is inclined so that the loaded solution can be discharged through the discharge unit 11 .

In general, a semiconductor manufacturing process is performed using various gases such as harmful gas or hydrogen, or various flammable gases, corrosive foreign substances, and harmful substances containing toxic components are generated in large amounts during the process. Since these corrosive foreign substances and harmful substances are highly reactive to metals and general plastics, and there is a possibility of causing another contamination, the chemical vessel part 10 is corroded or oxidized by the sample solution containing these corrosive foreign substances and harmful substances, contamination, etc. In order to avoid this, it may be formed by selecting any one or more from materials such as Teflon material, for example, PTFE (Polytetrafluoroethylene), PFA (Perfluoroalkoxy), and FEP (Fluorinated ethylene propylene), and preferably made of PTFE.

The sample pre-processing apparatus of the present invention provides chemical inlets 21, 22, 23 for transferring external chemicals into the chemical vessel unit 10 or discharging chemicals inside the chemical vessel unit to the outside of the chemical vessel unit 10. It may be provided in the vessel cover unit 20 that is located and coupled to the upper portion of the. Here, the chemical entrance is a first chemical entrance 21 for transferring the external sample solution to the inside of the chemical vessel unit, a second chemical entrance 22 for discharging the internal chemical fume to the outside, and a agent for transferring an alternative solvent 3 chemical entrances 23 may be included. In addition, the chemical inlet is a fourth chemical inlet 24 for introducing a purge gas such as an inert gas into the chemical vessel unit 10, or a fifth chemical inlet 25 for introducing a chemical for an auxiliary function such as cleaning. It may be configured to further include. In this case, the chemical entrance may include a valve for opening and closing the flow path, although the structure is not shown in detail in the drawing. In FIG. 2, three chemical entrances 21, 22, and 23 are illustrated by way of example, but this is exemplary and the user can further add or reduce the number of chemical entrances according to convenience and purpose, and other than the vessel cover part It can also be formed on location.

On the other hand, the chemical entrance and exit may be additionally provided with a tube body to assist the entry and exit of each chemical. That is, as exemplarily shown in FIG. 3( a ), a tube body 21a is provided at the chemical entrance into which a sample solution or an alternative solvent is introduced, and the sample solution introduced into the internal space of the chemical vessel 10 or It is possible to guide the flow of an alternative solvent or the like. At this time, it is preferable that the lower part of the tube body 21a is formed as an inclined end, as shown in FIG. 4(b), so that the sample solution is ejected toward the bottom or the filling sample solution rather than the inner wall of the chemical vessel part 10. The tube bodies 22a and 23a for introducing a solvent or washing water into the inside of the chemical vessel part 10 are formed as inclined ends with the lower part facing the inner wall so as to be ejected toward the inner wall as shown in Fig. 4(c), or Fig. 4(d). ), it is preferable to have a structure in which an outlet hole is formed in the lower side to be ejected in the lateral direction, thereby collecting the solute or residue of the inner wall of the chemical vessel 10 and flowing.

In addition, although the user may configure one chemical entrance to perform two or more functions, it is preferable to individually perform one function in consideration of the possibility of sample and drug contamination, the complexity of the flow line, and the inconvenience. In addition, the chemical entrance and / or tube may be configured to include a Teflon material to avoid internal corrosion, sample contamination, and the like.

The sample pre-processing apparatus of the present invention may include a vessel cover unit 20 to seal the internal space of the chemical vessel unit 10 , and may include a chemical entrance to the vessel cover unit 20 . At this time, the chemical vessel part 10 and the vessel cover part 20 may be fixed to each other by a fastening means 27 to maintain a sealed state, and a combination of bolts, nuts, clamps, etc. may be used as the fastening means. . A seating groove 13 for seating a portion of the sealing member 15 is formed on at least one side of the mutual coupling portion of the vessel cover 20 and the chemical vessel 10, and the sealing member 15 is formed of an elastic material. ) can be seated in the groove 13 to further enhance the stability of the sealing structure.

Here, the sealing member 15 is in the form of an O-ring, and its cross-section may have various shapes, and all commonly used materials such as natural rubber, synthetic rubber, and synthetic resin can be used, and the sealing member 15 ) may further include a protrusion (15a) to further enhance the sealing performance.

In the sample preprocessing apparatus of the present invention, the heating unit for heating the sample solution supported on the chemical vessel unit to evaporate the solvent to form chemical fume includes a heater 30 . The heater 30 is configured to heat the sample solution carried in the internal space of the chemical vessel unit 10 from the outside of the chemical vessel unit 10 , and may be, for example, a micro heater. The heater 30 transfers heat to the inside of the chemical vessel part 10 on which the sample solution is supported to evaporate the solvent of the sample solution, for example, performs a heating function in a temperature range of 0 to 250 ° C. And, it is good not to exceed a predetermined upper limit temperature, for example, a maximum of 250°C according to the material of the chemical vessel part. If the temperature of the heater 30 exceeds 250° C., the chemical vessel 10 provided inside the heater may be damaged or deformed, thereby affecting the chemical pretreatment process. Although not shown in the drawings, the sample pre-processing apparatus of the present invention is provided with a temperature sensing unit (not shown) to enable temperature control of the heater, and based on this, the temperature control of the heater is implemented by the heater controller 120 described above, and the apparatus For safety, etc., it may be equipped with a time setting function.

On the other hand, the chemical vessel part 10 of the present invention may be formed of a material such as Teflon to be thermally and chemically stable. When the chemical vessel part 10 is heated in direct contact with the heater, it is exposed to local overheating. Therefore, there may be a possibility that the chemical vessel unit 10 may be damaged or the service life may be shortened. In order to prevent this, the vessel guide 40 may be provided between the heater 30 and the chemical vessel unit 10 . The vessel guide 40 is formed in a shape that surrounds the outside of the chemical vessel part without a gap, and is preferably made of a heat conductor to facilitate heat conduction, and can be used by selecting from commonly used heat conductors such as metal materials. and is not particularly limited.

The sample pre-processing apparatus according to the present invention, in addition to being operated in a state in which the chemical vessel unit 10 and the like are installed together with the heating unit, is formed and configured in a detachable structure as shown in FIG. 6 to perform the pre-treatment process. It may have a form used for pretreatment by being installed in the sample pretreatment device before. That is, as shown in FIG. 6(a), the chemical vessel part 10 and the vessel cover part 20 are coupled to each other by the fastening means 27 and transported, and the vessel guide 40 as shown in FIG. 6(b). ) to perform a pre-treatment function by mounting the chemical vessel part 10 in the seating space provided inside.

In addition to the convenience of using one heating part in common when the chemical vessel part 10 is formed in a structure detachable from the heating part, the replacement of damaged or worn parts inside the sample preprocessing apparatus of the present invention is possible. It can be easy. In particular, it is easy to dismantle or assemble the chemical vessel part that is constantly exposed to chemical gases and chemicals and requires periodic replacement, and provides convenience in terms of device management such as cleaning.

The sample preprocessing apparatus according to the present invention, as a modified embodiment, may be configured to additionally include a cooling unit, and the cooling unit has a function of preventing overheating of the chemical vessel unit in the process of forming chemical fume by the heating unit carry out Here, the cooling unit 50 of the sample pre-processing apparatus according to the present invention forms a closed space surrounding the outside of the heating unit as exemplarily shown in FIG. 7 , and forms a closed space of the cooling unit 50 . By introducing the refrigerant, the refrigerant flows to the outer shell of the heater 30, and as a result, the temperature of the outer wall of the chemical vessel unit 10 is driven so as not to exceed a predetermined temperature (eg, 250° C.).

At this time, a refrigerant injection pipe 51 and a refrigerant discharge pipe 52 through which a refrigerant can enter and exit are provided on one side of the outer wall of the sample pretreatment apparatus, and the refrigerant may be water or the like. In addition, since the temperature of the outer wall of the chemical vessel is sufficiently high while the cooling unit is not driven and the cooling unit blocks heat leakage so that the chemical can be smoothly evaporated, the inner wall of the cooling unit 50 has an insulating material to prevent heat loss. (60) may be further provided.

In addition, in the case of having a cooling unit, the sample pretreatment apparatus according to the present invention is formed in a detachable structure as shown in FIG. It may have a form that is installed in the sample pretreatment device before performing the pretreatment process by being configured and used for pretreatment. That is, as shown in FIG. 8(a), the chemical vessel part 10 and the vessel cover part 20 are coupled to each other by the first fastening means 27 and transported, and the vessel guide as shown in FIG. 8(b). After the chemical vessel part 10 is mounted in the seating space provided on the inside of the 40, a pre-processing function is performed. At this time, it is preferable to fasten the chemical vessel part 10 and the like by the second fastening means 28 to stably maintain the mounting state. The effect due to the detachable structure as described above is substantially the same as that of FIG. 6 , and thus the corresponding description is cited.

As shown in FIGS. 2 and 7, the sample pre-processing apparatus according to an embodiment of the present invention is connected to the discharge unit 11 of the chemical vessel unit 10 at the lower end of the chemical vessel unit 10, and a valve assembly 70 including a valve for transferring the pretreatment sample solution inside the chemical vessel to the analyzer. In addition, a connection for flowing an external chemical or gas into the inside of the chemical vessel unit or discharging a fluid inside the chemical vessel unit to the outside may be implemented.

By way of example, when the function and structure of the valve assembly 70 are further described using FIG. 9 , the valve assembly provides a first valve ( 71) may be included. At this time, a flow detection sensor 71a may be additionally included to confirm whether the sample has been moved to the analyzer. In addition, the valve assembly 70 may include a second valve 72 providing a flow path connected to the chemical vessel part 10 so that an inert gas, for example, nitrogen can move. In a predetermined step, the nitrogen gas introduced through the second valve moves to the chemical vessel part 10 on which the solution is supported and floats in the form of air bubbles, which are used so that the alternative solvent and the solute are evenly mixed in the pretreatment process. Also, in the cleaning step, the contaminants remaining on the chemical vessel can be wiped off well. In addition, the valve assembly 70 may include a third valve 73 that provides a flow path through which washing water, such as ultrapure water, is introduced. The ultrapure water is easily controlled by a user to move in any one or a plurality of directions of the first valve, the second valve, the fourth valve, and the chemical vessel part for the purpose of cleaning, so that it is possible to perform a cleaning function. The valve assembly 70 may include a fourth valve 74 that provides a flow path for discharging a solution, etc. inside the chemical vessel unit in a cleaning process. It is driven so that residual solution or washing water can be discharged to the outside.

Hereinafter, a method of pre-processing a sample solution containing an analyte using the sample pre-processing apparatus of the present invention will be described in detail.

A sample pretreatment method according to an embodiment of the present invention includes an introduction step of introducing a sample solution to be pretreated into an internal space of a chemical vessel; and a chemical fume discharge step of heating the introduced sample solution by a heating unit to evaporate the solvent of the sample solution and discharge it in the form of chemical fume; and a pretreatment sample forming step of supplying an alternative solvent to the chemical vessel unit to form a pretreatment sample solution.

Looking at each step in detail, in the introduction step, a sample solution of a predetermined volume is introduced into the chemical vessel part 10 through the chemical entrance 21 and the tube 21a, and in the chemical fume discharge step, it is provided inside the device The heater 30 of the heated part heats the outer wall of the chemical vessel part 10 to a temperature of, for example, 0 to 250° C., and the heat transferred to the inside evaporates the solvent of the sample solution.

Meanwhile, in the chemical fume discharging step, the cooling unit 50 may be additionally driven to prevent overheating of the chemical vessel unit in the process of evaporating the solvent of the sample solution by the heating unit and discharging it in the form of chemical fume. This is to prevent deformation or damage of the chemical vessel part by providing a refrigerant such as water around the heater 30 and the vessel guide 50 and forcibly cooling it quickly.

In addition, in the chemical fume discharge step, when evaporation to an appropriate level is completed, an inert gas may be injected through the chemical inlet 22 to perform a purge function. At this time, the inert gas is not particularly limited, such as nitrogen or argon gas. The injected inert gas purges unnecessary chemical fumes that exist inside the chemical vessel unit 10, such as vapor generated when the sample solvent is evaporated, and is discharged through the chemical inlet 23 and the tube 23a.

In the pretreatment sample forming step, the residue (solute of the sample solution) remaining in the chemical vessel part 10 is diluted by an alternative solvent introduced from any one of the chemical entrances to form a pretreatment sample solution. At this time, the gas for stirring from the lower side of the chemical vessel part through the second valve 72 of the valve assembly 70 while supplying the substitute solvent in the alternative solvent supply step of supplying the substitute solvent to the chemical vessel unit or after the supply of the substitute solvent is completed dilution and mixing by an alternative solvent can be supplemented by introducing As such, the pretreatment sample solution formed by the pretreatment sample formation step is then moved to the analyzer through a valve connected to the analyzer to perform analysis.

The sample pretreatment method according to an embodiment of the present invention may include a cleaning step of supplying cleaning water to clean the internal space of the chemical vessel before the introduction step or after the pretreatment sample forming step. This is to set the flow direction of washing water such as ultrapure water supplied through the third valve 73 of the valve assembly 70 to perform a desired function by using the open/close state of other valves. That is, in a state in which the internal space of the chemical vessel unit can be exhausted, the washing water flows into the internal space of the chemical vessel unit to perform a washing function for the chemical vessel unit, and in the state in which the first valve 71 is opened, the washing water flows into the internal space of the chemical vessel unit. It flows to the side and performs a cleaning function for the corresponding flow path, and in the state in which the fourth valve 74 is opened, the washing water washes the internal flow path of the valve assembly and is discharged to the outside, thereby performing a cleaning function for the corresponding discharge flow path. .

In addition, the description of the present invention described above is for illustration, and those of ordinary skill in the art to which the present invention pertains will understand that it can be easily modified into other specific forms without changing the technical spirit or essential features of the present invention. will be able Therefore, it should be understood that the embodiments described above are illustrative in all respects and not restrictive. For example, each component described as a single type may be implemented as distributed or divided, and likewise components described as distributed or divided may also be implemented in a combined form within the scope of those of ordinary skill in the art. have. In addition, the steps of the method may be performed singly or performed multiple times in combination with at least one other step.

The scope of the present invention is indicated by the following claims, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included in the scope of the present invention.

110: sample pretreatment device
10: chemical vessel part 11: discharge part
20: vessel cover portion 27: first fixture
28: second fixture
30: heating unit 40: vessel guide
50: body housing 60: insulation material
70: valve assembly
100: HCDS pretreatment sampler
120: heater controller 130: first chemical storage tank
140: drug vessel 150: second drug storage tank
160: utility 170: eggplant bottle
200: contaminant analysis device

Claims (13)

A sample pretreatment device for pre-treating a sample solution containing an analyte before providing it to an analyzer,
a chemical vessel unit having an internal space in which a sample solution to be pre-treated is supported; and
It consists of including; a heating unit for evaporating the solvent by heating the sample solution supported on the chemical vessel unit to form a chemical fume;
The chemical fumes formed by the heating unit are discharged and an alternative solvent is supplied to the chemical vessel unit to form a pretreatment sample solution,
a first valve connected to the chemical vessel unit at the lower end of the chemical vessel unit and transferring the pretreatment sample solution inside the chemical vessel unit to the analyzer; Alternatively, a second valve for injecting washing water into the chemical vessel; a third valve serving as a passage for discharging the solution inside the chemical vessel; a fourth valve for introducing a stirring gas from the lower side of the chemical vessel; A sample pre-processing apparatus, characterized in that it further comprises; a valve assembly comprising at least any one of.
According to claim 1,
A sample pre-processing apparatus, characterized in that a chemical entrance is provided in the vessel cover portion that is positioned and coupled to the upper portion of the chemical vessel unit to introduce the sample solution into the chemical vessel unit or discharge chemical fumes.
3. The method of claim 2,
The chemical entrance may include: a first chemical entrance for transferring an external sample solution to the inside of the chemical vessel; a second chemical entrance for discharging the internal chemical fume to the outside; A sample pretreatment device, characterized in that it includes; a third chemical entrance for transferring an alternative solvent.
According to claim 1,
The heating unit,
a vessel guide formed to surround the outside of the chemical vessel unit and formed of a heat conductor; and
A sample pre-processing apparatus comprising: a heater installed in the vessel guide to heat the sample solution carried in the chemical vessel unit.
According to claim 1,
The chemical vessel part is formed in a detachable structure and is mounted on the sample pre-processing device before performing the pre-processing process to prepare for pre-treatment.
According to claim 1,
Sample preprocessing apparatus, characterized in that the cooling unit is additionally provided to prevent overheating of the chemical vessel unit in the process of forming the chemical fume by the heating unit.
In the sample pretreatment method for pretreatment before providing a sample solution containing an analyte to the analyzer,
an introduction step of introducing a sample solution to be pre-treated into the internal space of the chemical vessel; and
a chemical fume discharging step of heating the introduced sample solution by a heating unit to evaporate the solvent of the sample solution and discharging it in the form of chemical fume;
and a pretreatment sample forming step of supplying an alternative solvent to the chemical vessel part to form a pretreatment sample solution;
After the pretreatment sample forming step, a pretreatment sample transfer step of transferring the pretreatment sample solution inside the chemical vessel portion to the analyzer through the first valve connected to the chemical vessel portion at the lower end of the chemical vessel portion; characterized in that it is further provided sample pretreatment method.
8. The method of claim 7,
The chemical fume discharge step is,
Sample pretreatment method, characterized in that the cooling unit is additionally driven to prevent overheating of the chemical vessel unit in the process of evaporating the solvent of the sample solution by the heating unit and discharging it in the form of chemical fume.
8. The method of claim 7,
A sample pretreatment method comprising a; supplying washing water to clean the internal space of the chemical vessel before the introduction step or after the pretreatment sample forming step.
In the sample pretreatment method for pretreatment before providing a sample solution containing an analyte to the analyzer,
an introduction step of introducing a sample solution to be pre-treated into the internal space of the chemical vessel; and
a chemical fume discharging step of heating the introduced sample solution by a heating unit to evaporate the solvent of the sample solution and discharging it in the form of chemical fume;
and a pretreatment sample forming step of supplying an alternative solvent to the chemical vessel part to form a pretreatment sample solution;
The pretreatment sample forming step is
A sample pretreatment method comprising a; alternative solvent supply step of supplying an alternative solvent to the chemical vessel unit, wherein a gas for stirring is introduced from the lower side of the chemical vessel part while the alternative solvent is supplied or after the replacement solvent supply is completed. delete delete delete

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