JP2012181092A - Heating concentrator, and heating concentration method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a heating concentrator capable of inhibiting impurities from mixing with a sample liquid to be concentrated by heating, and a heating concentration method.SOLUTION: The heating concentrator has: a heating and concentrating container 12 having a container body 25 storing a liquid sample 11 and including a first open surface 25b through which steam of the liquid sample 11 passes to a top edge 25A, and a tap 26 provided on the top edge 25A of the container body 25 and including a second open surface 26a through which the steam of the liquid sample 11 passes; a lid 14 arranged on the top edge 25A of the container body 25 so as to close the first open surface 25b and confronting the second open surface 26a with a discharge part 29 placed at the second open surface 26a therebetween; and heating means 16 for heating the heating and concentrating container 12.

Description

  The present invention relates to a heating concentration apparatus and a heating concentration method for concentrating a liquid sample containing trace components by heating.

As IC (Integrated Circuit) becomes finer, wet cleaning is required to improve impurity removal capability and impurity removal efficiency.
In recent years, the purity of wet cleaning semiconductor chemicals has increased, and now the level has reached ppt and sub-ppt (ppq). At the same time, there is a need for a microanalysis technique for evaluating chemical solutions.

  In the conventional microanalysis technique, since the sensitivity on the analyzer side is insufficient depending on the type of metal element to be measured, it is difficult to analyze the ppt order. Therefore, as one means that can solve this problem, concentration of the liquid sample is performed and analysis sensitivity is improved. Improvements are being made.

For example, Patent Document 1 discloses a heating concentration including a beaker containing a liquid sample, an aluminum block having a recessed portion for accommodating the beaker, and a coil heater provided in the aluminum block so as to surround the beaker. An apparatus is disclosed.
In the heating and concentration apparatus described in Patent Document 1, the upper end of the beaker is opened, and the vapor of the liquid sample is discharged to the outside of the beaker through the upper end of the beaker. Thereby, the liquid sample is concentrated.

JP 2001-305031 A

However, in the heating and concentration apparatus described in Patent Document 1, since the upper end of the beaker is opened to the atmosphere, there is a problem that impurities (including metal and the like) are easily mixed into the beaker from the upper end side of the beaker.
As described above, when impurities are mixed in the liquid sample, impurities remain in the concentrated sample liquid, so that the microanalysis cannot be performed accurately.

  Then, an object of this invention is to provide the heating concentration apparatus and the heating concentration method which can suppress that an impurity mixes in the sample liquid concentrated by heating.

  In order to solve the above-described problem, according to the invention according to claim 1, there is provided a heating and concentration apparatus for concentrating a liquid sample containing a trace component by heating, containing the liquid sample, and vapor of the liquid sample at an upper end A container body having a first open surface through which the liquid sample passes, and a heating and concentration container provided at the upper end of the container body and having a spout with a second open surface through which the vapor of the liquid sample passes, A lid that is disposed at the upper end of the container body so as to close the first open surface, and that has a gap between the pouring spout and faces the second open surface; There is provided a heating and concentration apparatus comprising heating means for heating a container for use.

  Moreover, according to the invention which concerns on Claim 2, the said cover body has the protrusion part which protrudes from the lower surface of the said cover body in the outer periphery of the said cover body, The heating concentration apparatus of Claim 1 characterized by the above-mentioned. Is provided.

  According to a third aspect of the present invention, there is provided the heating and concentrating apparatus according to the second aspect, wherein the lid is circular and the protrusion is ring-shaped. The

  According to the invention of claim 4, an inert gas supply pipe made of a fluororesin that supplies an inert gas of high purity, a connection member provided so as to penetrate the lid, and the connection The heating concentration apparatus according to claim 1, further comprising: a supply pipe connecting member that connects the inert gas supply pipe to the member.

  According to the invention of claim 5, the connection member has a cylindrical shape protruding from the upper surface of the lid body and has a first threaded portion, and the supply pipe connection member is the first The heating and concentrating device according to claim 1, further comprising a second screw portion that is screwed to the screw portion.

  Moreover, according to the invention which concerns on Claim 6, the recessed part was provided in the position facing the said spout among the said cover bodies, The heating of any one of Claims 1 thru | or 5 characterized by the above-mentioned. A concentrator is provided.

  The invention according to claim 7 provides the heating and concentration apparatus according to claim 6, wherein the recess is a groove extending from the center of the lid to the outer periphery of the lid. Is done.

  The invention according to claim 8 is characterized in that it comprises a gap formed between the recess and the spout and has a discharge part for discharging the vapor of the liquid sample. A heat concentration apparatus according to 6 or 7 is provided.

  Further, according to the invention according to claim 9, a step portion that accommodates the upper end of the heating and concentration container is provided in a portion of the lid that faces the heating and concentration container. Claim | item 1 thru | or 8 WHEREIN: The heating concentration apparatus of any one is provided.

  According to a tenth aspect of the present invention, the material of the heating and concentration vessel is a high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less. A heating concentration apparatus according to item 1 is provided.

  According to an eleventh aspect of the present invention, in any one of the first to tenth aspects, the material of the lid is high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less. The described heating concentration apparatus is provided.

  Moreover, according to the invention which concerns on Claim 12, the said high purity inert gas is 99.9999 vol%, The heating concentration apparatus of any one of Claims 4 thru | or 11 characterized by the above-mentioned. Provided.

  Moreover, according to the invention which concerns on Claim 13, it has a handle provided in the outer wall of the said container main body, The heating concentration apparatus of any one of Claims 1 thru | or 12 characterized by the above-mentioned is provided. .

  According to the invention of claim 14, the heating means includes a quartz case and a heater accommodated in the quartz case, and the heater coil is attached to the quartz tube. 14. The heating and concentration apparatus according to claim 1, wherein the heating and concentration apparatus is a coated halogen heater.

  According to a fifteenth aspect of the invention, the heating means includes an opaque quartz plate that is accommodated in the quartz case and on which the heater is placed. 14 is provided.

  According to the invention of claim 16, the control unit for adjusting the temperature of the heater, and an electric wire having one end connected to the heater and the other end connected to the control unit. The heating and concentrating device according to claim 14 or 15, wherein the electric wire is covered with a heat-shrinkable tube made of a fluororesin.

  The invention according to claim 17 is the method for heating and concentrating a liquid sample using the heating and concentration apparatus according to any one of claims 1 to 16, wherein the liquid sample is placed in the container body. The container for heating and concentrating by the heating means, the step of disposing the lid on the upper end of the container main body, making the first and second open surfaces face the lid, and the heating means. And heating the liquid sample, and discharging the vapor of the liquid sample from the gap to the outside of the heating and concentration container.

  The invention according to claim 18 is characterized in that the liquid sample is heated in a state where a high-purity inert gas is supplied into the container body and the space in the container body is at a positive pressure. A heating concentration method according to claim 17 is provided.

  According to a nineteenth aspect of the present invention, the high-concentration synthetic quartz having an impurity metal concentration of 1 ppb or less is used as the material for the heat concentration container. Is provided.

  Further, according to the invention of claim 20, as the material of the lid, high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less is used. The described heat concentration method is provided.

  In addition, according to the invention of claim 21, the high-purity inert gas has a purity of 99.9999 vol% or more, and the heat concentration according to any one of claims 17 to 20, A method is provided.

  According to the heating and concentrating apparatus of the present invention, the lid is disposed at the upper end of the container main body so as to close the first open surface, and is opposed to the second open surface by interposing a gap between the spout. By having the body, it is possible to prevent impurities from being mixed into the liquid sample from above the first and second open surfaces. Thereby, since impurities contained in the concentrated liquid sample are reduced, it is possible to accurately perform microanalysis using the concentrated liquid sample.

  In addition, according to the heating and concentration method of the present invention, the liquid sample is poured into the container body, and then a lid is disposed on the upper end of the container body so that the first and second open surfaces and the lid face each other. Next, the liquid sample is heated by the heating means through the heating and concentration container, and the lid body disposed opposite to the first and second open surfaces is used to detect the liquid sample from above the first and second open surfaces. Impurities can be prevented from being mixed into the liquid sample. Thereby, since impurities contained in the concentrated liquid sample are reduced, it is possible to accurately perform microanalysis using the concentrated liquid sample.

It is a perspective view which shows schematic structure of the heating concentration apparatus which concerns on embodiment of this invention. It is sectional drawing of the container for heating concentration and a cover body which are arrange | positioned on the heating means shown in FIG. It is a top view of the container for heating concentration shown in FIG. It is sectional drawing of the AA line direction of the container for heating concentration shown in FIG. It is the side view which looked at the container for heating concentration shown in FIG. It is a top view of the cover body shown in FIG. It is a figure which shows the cross section of the CC line direction of the cover body shown in FIG. 6, and the container for heating concentration. It is a top view of the halogen heater which comprises the heating means shown in FIG.1 and FIG.2.

  Embodiments to which the present invention is applied will be described below in detail with reference to the drawings. The drawings used in the following description are for explaining the configuration of the embodiment of the present invention, and the size, thickness, dimensions, and the like of each part shown in the drawings are different from the dimensional relationship of an actual heating concentration apparatus. There is a case.

(Embodiment)
FIG. 1 is a perspective view showing a schematic configuration of a heating and concentration apparatus according to an embodiment of the present invention, and FIG. 2 is a cross-sectional view of a heating and concentration container and a lid arranged on the heating means shown in FIG. It is.
Referring to FIGS. 1 and 2, the heating and concentration apparatus 10 of the present embodiment is an apparatus that concentrates a liquid sample 11 containing trace components by heating, and includes a heating and concentration container 12, a handle 13, and a lid. 14, connection member 15, heating means 16, control unit 17, covered electric wire 18, inert gas supply pipe 19, supply pipe connection member 21, and inert gas supply source 23.

  FIG. 3 is a plan view of the heating and concentration container shown in FIG. 2, and FIG. 4 is a cross-sectional view of the heating and concentration container shown in FIG. FIG. 5 is a side view of the heating and concentration container shown in FIG.

Referring to FIGS. 1 to 5, the heating and concentration container 12 has a container body 25 and a spout 26.
Referring to FIG. 2, the container body 25 is a container that stores the liquid sample 11. 2 and 4, the container body 25 has a cup shape in which the upper end 25 </ b> A side is an open end (a shape whose width becomes narrower from the upper end 25 </ b> A of the container body 25 toward the bottom surface of the container body 25). Yes. The container body 25 has, at its upper end 25A, a first open surface 25b that passes when the vapor of the heated liquid sample 11 evaporates. The first open surface 25b is substantially circular.

Referring to FIG. 3, the upper end 25A of the container body 25 has a ring shape. The diameter _{R 1} of the upper end 25A of the container body 25, for example, can be set to 110 mm.
2-5, the upper end surface 25a of the container main body 25 is a flat surface. Referring to FIG. 2, the upper end surface 25a of the container body 25 is in contact with the lid body 14 in a state where no gap is formed.

  Referring to FIGS. 2 to 5, the spout 26 is provided at the upper end 25 </ b> A of the container body 25 and has a second open surface 26 a through which the vapor of the liquid sample 11 passes. The spout 26 functions as a spout for pouring the concentrated liquid sample 11 into another container (for example, a vial). The spout 26 is disposed so as to protrude outside the container body 25. Referring to FIG. 2, the spout 26 is disposed at a position lower than the upper end surface 25 a of the container body 25.

  As a result, as shown in FIG. 2, the lid 14 is placed between the recess 32 provided in the lid 14 and the spout 26 in a state where the lid 14 is placed on the heating and concentration container 12. The discharge part 29 comprised by the clearance gap between the recessed part 32 and the spout 26 which were provided in is formed. Via this discharge part 29, the vapor generated from the liquid sample 11 by heating is discharged to the outside of the heating and concentration container 12.

Referring to FIGS. 2 to 5, the tip 26 </ b> A of the spout 26 has an acute angle shape and is disposed at the lowest position of the spout 26.
Thus, the concentrated liquid sample 11 can be easily transferred to another container (for example, a vial) by making the shape of the spout 26 an acute angle.

As a material of the heating and concentrating container 12, for example, high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less can be used. The impurity metal concentration (also referred to as “metal impurity concentration”) in the present application is the impurity concentration of a metal contained in high-purity synthetic quartz.
Thus, by using high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less as the material constituting the heating and concentration vessel 12, it is included in the material constituting the heating and concentration vessel 12 when the liquid sample 11 is concentrated. Since elution of the impurity metal can be suppressed, the liquid sample 11 can be prevented from being contaminated by the impurity metal.

Referring to FIGS. 3 and 5, the handle 13 is provided on the outer wall of the container body 25. The handle 13 is plate-shaped. In this way, by providing the handle 13 on the outer wall of the container body 25, the heated concentration container 12 can be easily handled. Therefore, the liquid sample 11 concentrated by heating is transferred to another container (for example, a vial). At this time, it is possible to prevent impurities from being mixed into the concentrated liquid sample 11.
Further, when the liquid sample 11 concentrated by heating is transferred to another container (for example, a vial), the upper end 25A of the heating and concentration container 12 is not held by a person, so that it adheres to the person's hand. It is possible to suppress the impurities that have been mixed into the liquid sample 11.

6 is a plan view of the lid shown in FIG. 2, and FIG. 7 is a diagram showing a cross-section in the CC line direction of the lid shown in FIG. 6 and a container for heating and concentration.
Referring to FIGS. 6 and 7, the lid body 14 has a circular plate shape in plan view. Referring to FIG. 2, the lid body 14 is disposed so that the upper end surface 25 a of the container body 25 and the lower surface 14 b of the lid body 14 are in contact with each other when the liquid sample 11 is heated and concentrated.
The lid body 14 has a shape that can be opposed to the first and second open surfaces 25b and 26a. If the diameter _{R 1} of the upper end 25A of the container body 25 is 110 mm, the diameter _{R 2} of the lid 14 can be, for example, to 170 mm.

  In this way, by providing the lid body 14 disposed so as to be in contact with the upper end surface 25a of the container body 25, and making the lid body 14 opposed to the first and second open surfaces 25b and 26a. In addition, it is possible to prevent impurities from being mixed into the liquid sample 11 from above the heating and concentration container 12.

  With reference to FIGS. 6 and 7, the lid body 14 includes a stepped portion 14 </ b> A, a protruding portion 31, and a recessed portion 32. 14 A of level | step-difference parts are recessed parts which can be accommodated in the upper part 25A (upper end of the container 12 for heating concentration) of the container main body 25, and are formed in the part facing the container 12 for heating concentration in the cover body 14. FIG. By providing such a stepped portion 14 </ b> A, it is possible to prevent the lid 14 from being displaced from the upper end of the heating and concentration container 12.

Referring to FIG. 7, the protruding portion 31 is provided on the outer peripheral edge of the lid body 14 so as to protrude from the lower surface 14 b of the lid body 14. The protrusion 31 has a ring shape.
As described above, the protrusions 31 that protrude from the lower surface 14b of the lid 14 and have a ring shape are provided on the outer peripheral edge of the lid 14 so that impurities can be introduced into the heating and concentration container 12 from the outside of the heating and concentration apparatus 10. Can be prevented from being mixed.

The recess 32 is provided in the lid 14 at a position facing the spout 26. When the lid 14 is placed on the heating and concentration container 12, the recess 32 is disposed to face the spout 26. The recess 32 is a groove extending from the center of the lid body 14 to the outer peripheral edge of the lid body 14.
As described above, by providing the recess 32 (groove in the case of the present embodiment) disposed opposite to the spout 26, the vapor generated when the liquid sample 11 is heated and concentrated is passed through the discharge unit 29. Thus, the high-purity inert gas supplied into the heating and concentration container 12 can be easily discharged to the outside of the lid body 14 via the discharge portion 29. I can escape. Further, by letting the high purity inert gas escape to the outside of the lid body 14 through the discharge part 29, the lid body 14 can be prevented from wobbling due to the pressure of the inert gas.

In the present embodiment, the case where only one groove is provided as an example of the recess 32 has been described as an example, but a plurality of grooves may be provided in the lid body 14.
In the present embodiment, the groove 32 is described as an example of the recess 32, but a plurality of hole-shaped recesses may be provided instead of the groove.

As the material of the lid 14, high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less is preferably used. The impurity metal concentration (also referred to as “metal impurity concentration”) in the present application is the impurity concentration of a metal contained in high-purity synthetic quartz.
Thus, by using high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less as the material constituting the lid body 14, elution of impurity metals contained in the material constituting the lid body 14 can be suppressed. The liquid sample 11 can be prevented from being contaminated by the impurity metal.

  6 and 7, the connection member 15 is provided so as to penetrate the center of the lid body 14. The connecting member 15 has a cylindrical shape protruding from the upper surface 14a of the lid body 14 and has a first screw portion 15A. As the connection member 15, for example, a flare joint made of Teflon (registered trademark) and quartz can be used.

Referring to FIG. 2, the heating means 16 includes a quartz case 33, an opaque quartz plate 34, a heater fixing quartz rod 35, and a halogen heater 36 as a heater.
The quartz case 33 includes a quartz case body 33A and a quartz cover 33B. The quartz case body 33 </ b> A accommodates an opaque quartz plate 34, a heater fixing quartz rod 35, and a halogen heater 36.
The quartz cover 33B is attached to the quartz case body 33A in a detachable state. On the upper surface of the quartz cover 33B, the heating and concentration container 12 is placed.
Thus, by using the quartz case 33 as a component of the heating means 16, it is possible to suppress the generation of metal fume during heating.

The opaque quartz plate 34 is disposed on the bottom surface of the quartz case body 33A. A halogen heater 36 is placed on the opaque quartz plate 34.
Thus, by providing the opaque quartz plate 34 on the bottom surface of the quartz case body 33A, it becomes possible to radiate the heat of the halogen heater 36 to the heating and concentration container 12, and thus the liquid sample 11 is efficiently heated. can do.
Further, by providing the opaque quartz plate 34, heat transmission from the quartz case body 33A can be prevented. As a result, it is possible to prevent melting of plastic or the like constituting the draft located below the opaque quartz plate 34.

  The heater fixing quartz rod 35 is fixed on an opaque quartz plate 34. The heater fixing quartz rod 35 is a member for regulating the position of the halogen heater 36 on the opaque quartz plate 34.

FIG. 8 is a plan view of the halogen heater constituting the heating means shown in FIGS. 1 and 2.
2 and 8, the halogen heater 36 has a structure in which a heater coil 37 (for example, nichrome wire) made of metal is covered with a quartz tube 38, and the position is defined by a quartz rod 35 for fixing the heater. In this state, it is placed on an opaque quartz plate 34.
Thus, by covering the heater coil 37 made of metal with the quartz tube 38, it is possible to suppress the generation of metal fume from the heater coil 37 during heating. Thereby, the metal contamination of the liquid sample 11 at the time of concentration can be suppressed.

  Referring to FIG. 2, the heating means 16 having the above-described configuration heats the liquid sample 11 accommodated in the heating and concentration container 12 placed on the quartz cover 33B. Concentrate.

  Referring to FIGS. 1 and 8, the control unit 17 is electrically connected to the heater coil 37 via the covered electric wire 18. The control unit 17 has a temperature adjustment dial 39 for adjusting the temperature of the halogen heater 36.

1 and 8, the covered electric wire 18 includes an electric wire 41 and a heat-shrinkable tube 42 made of a fluorine resin. The electric wire 41 is made of metal. The electric wire 41 has one end connected to the heater coil 37 and the other end connected to the control unit 17. The electric wire 41 is covered with a heat-shrinkable tube 42 made of a fluorine resin. As the fluorine resin heat shrinkable tube 42, for example, a Teflon (registered trademark) heat shrinkable tube can be used.
Thus, by covering the wire 41 made of metal with the heat-shrinkable tube 42 made of fluororesin, it is possible to suppress metal fume generated from the wire 41 when the halogen heater 36 is heated. Thereby, the metal contamination of the liquid sample 11 at the time of concentration can be suppressed.

  Referring to FIGS. 1 and 2, the inert gas supply pipe 19 is made of Teflon (registered trademark), one end is connected to an inert gas supply source 23, and the other end is connected to a supply pipe. The member 21 is attached to the connecting member 15. As the inert gas supply pipe 19, for example, a Teflon (registered trademark) tube can be used.

The inert gas supply pipe 19 supplies the high-purity inert gas supplied from the inert gas supply source 23 to the space 44 formed between the liquid surface 11 a of the liquid sample 11 and the lid body 14. Thus, the pressure of the container body 25 in which the liquid sample 11 is stored is set to a positive pressure.
In this way, the pressure of the container body 25 in which the liquid sample 11 is stored is set to a positive pressure, and impurities are mixed into the liquid sample 11 through the discharge portion 29 formed between the lid 14 and the spout 26. Can be suppressed.

  Referring to FIGS. 1 and 2, the supply pipe connecting member 21 is provided at the other end of the inert gas supply pipe 19. The supply pipe connecting member 21 is provided with a second threaded portion 21A that is screwed with the first threaded portion 15A of the connecting member 15, and is configured to be detachable from the connecting member 15.

Referring to FIGS. 1 and 2, the inert gas supply source 23 is a device that supplies a high purity inert gas (purge gas), and is connected to one end of the inert gas supply pipe 19.
As a high purity inert gas (purge gas), for example, nitrogen (N ₂ ) having a purity of 99.9999 vol% or more can be used. Further, other inert gases such as Ar and He may be used as long as the purity is comparable.
In addition, the density | concentration used by this invention has shown the volume density | concentration. Therefore, in the following description, “vol%” is simply expressed as “%”.

As described above, by using nitrogen (N ₂ ) having a purity of 99.9999% or more as the high-purity inert gas, the liquid sample 11 can be prevented from being contaminated by impurities contained in the inert gas.

  According to the heating and concentrating device of the present embodiment, the upper end 25A of the container body 25 is disposed so as to close the first open surface 25b, and a gap (discharge portion 29) is formed between the second open surface 26a. By having the lid 14 that opposes the second open surface 26b with the interposition of impurities, it is possible to prevent impurities from being mixed into the liquid sample 11 from above the first and second open surfaces 25b, 26a. . Thereby, microanalysis can be accurately performed using the concentrated liquid sample 11.

  Further, as the material of the heating and concentrating container 12 and the material of the lid body 14, high-purity synthetic quartz (in other words, a material having a high purity and difficult to elute the impurity metal) having an impurity metal concentration of 1 ppb or less is used. Thus, the contamination of the liquid sample 11 by the impurity metal contained in the material of the heating and concentrating container 12 and the material of the lid 14 can be suppressed.

Next, with reference to FIG. 2, the heating and concentration method of the present embodiment using the heating and concentration apparatus 10 shown in FIG. 1 will be described.
First, the container 12 for heating and concentration and the lid 14 are sufficiently washed. Next, the liquid sample 11 containing a trace component (component to be measured) is poured into the container body 25. Next, the lid body 14 is arranged on the container body 25 so that the upper end 25A of the container body 25 is accommodated in the stepped portion 14A, and the first and second open surfaces 25b, 26a and the lid body 14 are opposed to each other. Let Thereby, it can suppress that an impurity mixes into the liquid sample 11 from the upper direction of the 1st and 2nd open surfaces 25b and 26a, and can prevent the position of the cover body 14 from shifting | deviating with respect to the container main body 25. FIG.

  Moreover, when arrange | positioning the cover body 14 on the container main body 25, it arrange | positions so that the 2nd open surface 26a and the recessed part 32 may oppose. Thereby, the discharge part 29 is formed between the second open surface 26 a and the recess 32.

  Next, the high-purity inert gas is supplied to the space 44 in the container main body 25 through the inert gas supply pipe 19, so that the space 44 in the container main body 25 is set to a positive pressure. Thereby, it can suppress that an impurity penetrate | invades in the container 12 for heat concentration through the discharge part 29. FIG.

Next, the vapor of the liquid sample 11 is discharged from the discharge unit 29 to the outside of the heating and concentration container 12 by heating the liquid sample 11 through the heating and concentration container 12 by the quartz hot plate 16 (heating means). To do. Thereby, the concentration of the liquid sample 11 proceeds. At this time, the temperature at which the liquid sample 11 is heated is adjusted by rotating the temperature adjustment dial 39 shown in FIG.
Thereafter, the concentrated liquid sample 11 is transferred to another container (for example, a vial). Next, after the pretreatment of the concentrated liquid sample 11 is performed, a trace component contained in the concentrated liquid sample 11 is analyzed by the analyzer.

  According to the heating and concentration method of the present embodiment, the first and second open surfaces 25b and 26a and the lid body 14 are opposed to each other, and the space 44 in the container body 25 is made positive pressure by a high purity inert gas. Thus, by concentrating the liquid sample 11 by heating, it is possible to prevent impurities from entering the liquid sample 11 from the outside of the heating and concentration container 12. Thereby, microanalysis can be accurately performed using the concentrated liquid sample 11.

  The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to such specific embodiments, and within the scope of the present invention described in the claims, Various modifications and changes are possible.

(Example)
With reference to FIG.1 and FIG.2, the heating concentration method by the Example of this invention is demonstrated.
First, the heating and concentration container 12 and the lid body 14 are washed with electronic industrial hydrochloric acid which is a cleaning liquid, and then the electronic industry hydrochloric acid adhered to the heating and concentration container 12 and the lid body 14 with ultrapure water. Washed away.
High purity synthetic quartz having an impurity metal concentration of 1 ppb or less was used as a material for the heating and concentration container 12 and the lid 14.
Next, 140 g of high-purity hydrogen peroxide water (concentration 31%, impurity metal concentration of 100 ppt or less) was poured into the container body 25 of the heating and concentrating container 12 as the liquid sample 11. Next, the lid body 14 was disposed on the upper end 25 </ b> A of the container body 25, and the first and second open surfaces 25 b and 26 a and the lid body 14 were opposed to each other.

Next, nitrogen (N ₂ ) having a purity of 99.9999% or more, which is a high-purity inert gas (purge gas), is supplied to the space 44 in the container body 25 via the inert gas supply pipe 19. The space 44 in 25 was set to a positive pressure. The supply amount of nitrogen was 1 L / min. The purge time was 40 minutes.

  Next, the high-temperature hydrogen peroxide solution as the liquid sample 11 was heated for 2 hours by adjusting the heating temperature with the temperature adjustment dial 39 of the control unit 17. Thereafter, 7 g of 0.1 N nitric acid was used as a pretreatment, and the high-purity hydrogen peroxide solution was concentrated 20 times. Using this ICP-MS (Inductively Coupled Plasma Mass Spectrometer) as an analysis device, impurity elements (B, Na, Mg, Al, K, Ca contained in high-purity hydrogen peroxide water that has been concentrated 20 times. , Cr, Mn, Fe, Co, Cu) were measured. The results are shown in Table 1.

(Reference example)
With reference to FIG.1 and FIG.2, the heating concentration method of a reference example is demonstrated.
First, the heating and concentration container 12 is washed with electronic industrial hydrochloric acid as a cleaning solution, and then the heating and concentration container 12 is washed with ultrapure water. The container 12 for heating and concentration was washed. High purity synthetic quartz having an impurity metal concentration of 1 ppb or less was used as the material for the heating and concentration vessel 12.
Next, 140 g of high-purity hydrogen peroxide water (concentration 31%, impurity metal concentration is 100 ppt or less) is poured as the liquid sample 11 into the container body 25 of the heat-concentration container 12, and the upper end of the heat-concentration container 12 is opened. . In other words, the lid 14 was not disposed at the upper end of the heating and concentration container 12.

Next, the high-temperature hydrogen peroxide solution as the liquid sample 11 was heated for 2 hours by adjusting the heating temperature with the temperature adjustment dial 39 of the control unit 17.
At this time, since the upper end of the heating and concentrating container 12 was opened, the vapor generated by heating evaporated into the atmosphere via the first and second open surfaces 25b and 26a.
Thereafter, 7 g of 0.1 N nitric acid was used as a pretreatment, and the high-purity hydrogen peroxide solution was concentrated 20 times. Using this ICP-MS (Inductively Coupled Plasma Mass Spectrometer) as an analysis device, impurity elements (B, Na, Mg, Al, K, Ca contained in high-purity hydrogen peroxide water that has been concentrated 20 times. , Cr, Mn, Fe, Co, Cu) were measured. The results are shown in Table 1.

(About analysis results of Examples and Reference Examples)
Table 1 shows the results of measuring the impurity concentration contained in the concentrated liquid samples of Examples and Reference Examples.
Referring to Table 1, the concentration of Cu was not different between the example and the reference example, but elements other than Cu (B, Na, Mg, Al, K, Ca, Cr, Mn, Fe, Regarding Co), the concentration of the reference example was higher than the concentration of the example. In particular, for B (boron), the concentration of the reference example was about 14 times the concentration of the example.

From the above results, the lid 14 is disposed at the upper end of the heating and concentrating container 12 and the space 44 in the container body 25 is positively opened with a high purity inert gas (nitrogen (N ₂ ) having a purity of 99.9999% or more). It has been confirmed that the use of the pressure has the effect of suppressing the mixing of impurities into the liquid sample 11.

  The present invention is applicable to a heating concentration apparatus and a heating concentration method for concentrating a liquid sample containing a trace component by heating.

DESCRIPTION OF SYMBOLS 10 ... Heat concentration apparatus, 11 ... Liquid sample, 11a ... Liquid level, 12 ... Heat concentration container, 13 ... Handle, 14 ... Lid body, 14a ... Upper surface, 14b ... Lower surface, 15 ... Connection member, 15A ... 1st Screw part, 16 ... quartz hot plate, 16a ... lower surface, 17 ... control unit, 18 ... covered electric wire, 19 ... inert gas supply pipe, 21 ... supply pipe connecting member, 21A ... second screw part, 23 ... non-use Active gas supply source, 25 ... container body, 25a ... upper end surface, 25A ... upper end, 25b ... first open surface, 26 ... spout, 26a ... second open surface, 26A ... tip, 29 ... gap, 31 ... Projection, 32 ... penetrating part, 33 ... quartz case, 33A ... quartz case body, 33B ... quartz cover, 34 ... opaque quartz plate, 35 ... quartz rod for fixing heater, 36 ... halogen heater, 37 ... Heater co Le, 38 ... a quartz tube, 39 ... temperature adjusting dial, 41 ... wire, 42 ... fluororesin-made heat shrinkable tubing, 44 ... space, _{R 1,} R 2 _... diameter

Claims (21)

A heating concentration device for concentrating a liquid sample containing a trace component by heating,
A container body that contains the liquid sample and has a first open surface through which the vapor of the liquid sample passes, and a second body that is provided at the upper end of the container body and through which the vapor of the liquid sample passes. A heating and concentration container having a spout with an open surface;
A lid that is disposed at the upper end of the container body so as to close the first open surface, and that has a gap between the spout and faces the second open surface;
Heating means for heating the container for heating and concentration;
A heating and concentrating device comprising:   The heating and concentrating apparatus according to claim 1, wherein the lid has a protruding portion that protrudes from a lower surface of the lid on an outer peripheral edge of the lid. The lid is circular,
The heating and concentrating apparatus according to claim 2, wherein the protruding portion has a ring shape. An inert gas supply pipe made of fluororesin that supplies an inert gas of high purity;
A connecting member provided so as to penetrate the lid,
A supply pipe connection member for connecting the inert gas supply pipe to the connection member;
The heating concentration apparatus according to claim 1, wherein The connection member has a cylindrical shape protruding from the upper surface of the lid body, and has a first threaded portion,
The heating and concentrating apparatus according to claim 1, wherein the supply pipe connecting member has a second threaded portion that is screwed with the first threaded portion.   The heating and concentrating apparatus according to any one of claims 1 to 5, wherein a concave portion is provided at a position facing the pouring spout in the lid.   The heating and concentrating apparatus according to claim 6, wherein the concave portion is a groove extending from the center of the lid body to an outer peripheral edge of the lid body.   The heating and concentrating apparatus according to claim 6 or 7, wherein the heating and concentrating apparatus is configured by a gap formed between the concave portion and the spout and has a discharge portion for discharging the vapor of the liquid sample.   The step part which accommodates the upper end of the said container for heating concentration is provided in the part facing the said container for heating concentration among the said cover bodies, The any one of Claims 1 thru | or 8 characterized by the above-mentioned. Heating concentration device.   The heating and concentrating apparatus according to any one of claims 1 to 9, wherein the material for the heating and concentrating container is high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less.   The heating concentration apparatus according to any one of claims 1 to 10, wherein the material of the lid is high-purity synthetic quartz having an impurity metal concentration of 1 ppb or less.   The heating concentration apparatus according to any one of claims 4 to 11, wherein the high-purity inert gas is 99.9999 vol%.   The heating concentration apparatus according to any one of claims 1 to 12, further comprising a handle provided on an outer wall of the container body. The heating means has a quartz case and a heater accommodated in the quartz case,
The heating and concentrating apparatus according to any one of claims 1 to 13, wherein the heater is a halogen heater in which a heater coil is covered with a quartz tube.   15. The heating and concentration apparatus according to claim 14, wherein the heating means includes an opaque quartz plate that is accommodated in the quartz case and on which the heater is placed. A control unit for adjusting the temperature of the heater;
One end is connected to the heater and the other end is connected to the control unit; and
The heating and concentrating apparatus according to claim 14 or 15, wherein the electric wire is covered with a heat-shrinkable tube made of a fluorine resin. A method for heating and concentrating the liquid sample using the heating and concentrating device according to any one of claims 1 to 16,
Pouring the liquid sample into the container body;
Disposing the lid on the upper end of the container body, and opposing the first and second open surfaces and the lid;
Heating the liquid sample via the heating and concentration container by the heating means, and discharging the vapor of the liquid sample from the gap to the outside of the heating and concentration container; and
The heating concentration method characterized by including.   18. The heating and concentration method according to claim 17, wherein the liquid sample is heated in a state in which a high-purity inert gas is supplied into the container body and the space in the container body is at a positive pressure.   19. The heat concentration method according to claim 17 or 18, wherein high purity synthetic quartz having an impurity metal concentration of 1 ppb or less is used as a material for the heat concentration container.   20. The heat concentration method according to any one of claims 17 to 19, wherein high purity synthetic quartz having an impurity metal concentration of 1 ppb or less is used as a material of the lid.   The heating concentration method according to any one of claims 17 to 20, wherein the high-purity inert gas has a purity of 99.9999 vol% or more.

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