JPS6082102A - Refining apparatus of reagent - Google Patents

Abstract

PURPOSE:To refine a quartz corrosive reagent with an inexpensive apparatus by using a ''Teflon'' material at the part of the apparatus in contact with the reagent. CONSTITUTION:An original liquid reagent 6 is charged into a reagent storage tank 4 made of ''Teflon'' which is placed on a hot plate 7 and heated. A gaseous nitrogen is blown into the reagent storage tank through a gas washing bottle 1 and a ''Teflon'' tube 3. The evaporated reagent is cooled by a cooler pipe 9 made of ''Teflon'' through a ''Teflon'' tube 8, and the refined reagent is collected in a collecting bottle 11 made of ''Teflon''.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for purifying a solution-like reagent such as an acid by a distillation method.

Along with the demand for higher purity materials due to advances in the electronics industry, atomic crab industry, and various materials industries, there is an even stronger need for improvements in ultratrace component analysis technology in material measurement technology. The recent rapid development of analytical equipment has made it possible to analyze ultratrace components using wet chemical analysis, but due to the problem of so-called contamination, in which target components are mixed in with the reagents used for analysis, blank values for analysis are high. In many cases, it is still not possible to analyze ultratrace components. Currently, high-purity reagents for the electronics industry or for measuring hazardous metals are commercially available, but they are not of sufficient purity for use in ultratrace component analysis, and need to be further purified depending on the purpose of use. . Conventionally, quartz double-stage distillation equipment and quartz non-boiling distillation equipment have been used to prepare high-purity reagents, but since these equipment is made of quartz, it cannot be used with quartz corrosive substances such as hydrofluoric acid. It has drawbacks such as difficulty in purifying the reagent, expensive equipment, and the need for a large installation space.

SUMMARY OF THE INVENTION An object of the present invention is to provide a new reagent purification apparatus that can purify quartz corrosive reagents, can be assembled at low cost, and can be disassembled and stored when not in use.

In the reagent purification device of the present invention, a reagent storage tank section having two conduits in the upper lid is heated on a hot plate, the generated reagent vapor is expelled with a cleaned inert gas introduced from one conduit, and the other conduit is expelled. It has a structure in which the condensed purified reagent is guided from a conduit to a cooling pipe installed in a cooling tank part to a collection bottle part, and all parts that come into contact with the reagent are made of Teflon.

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to drawings showing one embodiment.

FIG. 1 is a sectional view showing an embodiment. An appropriate amount of reagent stock solution 6 is put into a reagent storage tank 4 made of Teflon.

Two Teflon conduits are attached to the upper lid 5 of the storage tank. Conduit 3 connects to nitrogen gas washing bottle 1, and conduit 8
are connected to cooling tubes 9, the tips of each conduit being below and above the reagent liquid level. The storage tank is heated by placing it on a hot plate 7, and the generated reagent vapor is introduced from a conduit 8 into a Teflon cooling pipe 9 to be condensed, and the condensed purified reagent is collected in a Teflon collecting bottle 11. In this case, if the reagent boils, reagent droplets will be generated and the purification efficiency will deteriorate, so the reagent is heated at a temperature that does not boil. Nitrogen gas is blown through the conduit 3 in order to efficiently send out the generated reagent vapor. Nitrogen gas may also contain impurities, so it is washed through an air washing bottle. The air washing bottle contains a washing liquid 2 such as concentrated sulfuric acid. The cooling pipe 9 is placed in a cooling tank 10. The cooling tank 10 contains ice and water.

Dry ice - Contains a cooling agent such as ethanol.

The cooling tubes are coiled to increase cooling efficiency. Cover the mouth of the collection bottle with a Teflon sheet to prevent contamination from the outside. Table 1.2 shows the results when commercially available highest purity nitric acid and hydrofluoric acid were distilled to 11"ij using the apparatus shown in Figure 1. The distillation rate was approximately 20 fnl/hour, although it depended on the temperature of the hot plate. As shown in Table 1.2, the concentration of each impurity was reduced to 1/1 with nitric acid by distillation purification.
．． It was reduced to 1/1.1 to 1/4 with 5 to IA 8° hydrofluoric acid.

FIG. 2 shows a sectional view of the reagent storage tank portion of the device that is an improved version of the device shown in FIG. In FIG. 2, the conduits 3 and 8 of FIG. 1 have been improved. In conduit 3, tip table 1. Since the concentration of impurities in nitric acid before and after distillation is cylindrical, large bubbles are continuously generated when nitrogen gas is blown into the nitric acid, which tends to generate reagent droplets and reduces purification efficiency. The tip of the conduit 12 has a hole 21 with a large number of pores, and since bubbles are continuously generated, nitrogen gas can be gently blown into the conduit 12. Therefore, generation of reagent droplets can be suppressed. Since the reagent droplets that entered the tube '98 are directly sent to the cooling tube, the purification efficiency decreases. Since the conduit 13 is equipped with a trap 14 redundantly filled with Teflon scraps, the reagent droplets are collected here, and only the reagent vapor is sent to the 1' container, thereby achieving commercial purification efficiency. Monkey. As shown in FIG. 2, by using a dedicated system, the purification efficiency could be increased several times compared to the device shown in FIG.

Various types of cooling parts other than those shown in FIG. 1 are conceivable for the cooling section and cooling tank section. A sectional view of this embodiment is shown in FIG. The third factor has a double tube structure. The cooling pipe part 5 is made of a transparent material and is incorporated into the cooling pipe part I6. A coolant 17 is circulating in the cooling tank s16. By using this cooling tube section, the distillation rate was faster because the condensed reagents did not stagnate.

In the apparatus shown in FIGS. 1 and 2, each part can be disassembled, so the apparatus need only be assembled when necessary, and can be disassembled and stored when not in use. Therefore, no special installation space is required. It is also cheaper to assemble than a quartz distillation device.

As shown in the examples above, the reagent purification apparatus of the present invention enables distillation purification of quartz corrosive reagents, which could not be performed with conventional quartz distillers. Became. Furthermore, this device has the advantage of being inexpensive to assemble and easy to disassemble, requiring no special installation space.

[Brief explanation of the drawing]

FIG. 1 is a sectional view showing an embodiment of the device of the present invention. In fig. 1...Air washing bottle, 2...Cleaning liquid such as concentrated sulfuric acid, 3.
...Teflon conduit, 4...Teflon acid storage tank, 5
...upper lid. 6... Acid stock solution, 7... Hot plate, 8... Teflon conduit, 9... Teflon cooling pipe, 10... Cooling tank, 11... Teflon collection bottle, 2nd The figure is a sectional view of an acid storage tank portion of a device showing another embodiment. In the figure, 12, 13... Teflon conduit, 14... trap, and FIG. 3 is a sectional view showing another embodiment of the cooling pipe section and the cooling tank section. In fig. 15... Teflon cooling pipe, 16... Cooling tank, 17
...coolant. O l Figure: /P 2 Figure O 3 Figure

Claims (1)

[Claims] The reagent storage tank section, which has two conduits in the upper lid, is heated on a vent plate, and the generated reagent vapor is expelled with a cleaned inert gas introduced from one conduit, and then transferred to the cooling tank section from the other conduit. It is configured to introduce the condensed loaded reagent into the installed cooling pipe section and guide it from the cooling pipe section to the collection bottle section, and is characterized in that all parts that come into contact with the reagent are constructed using Teflon material. Reagent purification equipment.