KR20120077703A

KR20120077703A - Sulfuric acid clean-up process centrifuging with teflon vial

Info

Publication number: KR20120077703A
Application number: KR1020100139764A
Authority: KR
Inventors: 최기인
Original assignee: 한국세라믹기술원
Priority date: 2010-12-31
Filing date: 2010-12-31
Publication date: 2012-07-10

Abstract

PURPOSE: A sulfuric acid treating method based on centrifugation with a Teflon vial is provided to increase the precision of experiment by eliminating remaining sulfuric acid on the wall of a separating funnel. CONSTITUTION: A sulfuric acid treating method includes the following: an organic solvent extracting agent is prepared(S20); the organic solvent extracting agent is injected into a centrifuging vial(S21); sulfuric acid is added into the organic solvent extracting agent(S22); a mixed solution is obtained and kept(S23); the mixed solution is centrifuged(S24); and an organic solvent layer is separated from the centrifuged solution(S25). The organic solvent extracting solution includes hexane. The centrifuging vial is based on Teflon.

Description

Sulfuric acid clean-up process centrifuging with Teflon Vial}

The present invention relates to a method for treating sulfuric acid in organic solvent extracts, and more particularly to a more improved method for treating sulfuric acid which can be commonly used for pretreatment of organic solvent extracts for analysis of harmful pollutants.

The pollutant purification process using sulfuric acid is a process for removing organic substances acting as an obstacle during the pretreatment and analysis of trace harmful pollutants such as dioxins, and is widely applied to the pretreatment and analysis of hazardous substances.

1 is a schematic of a conventional exemplary sulfuric acid treatment process.

Referring to FIG. 1, a solvent extract such as hexane (S10) is transferred to a separatory funnel (S11), concentrated sulfuric acid is added (S13) for about 10 minutes, shaken (S14), and then left for about 30 minutes (S15), followed by an aliquot. Sulfuric acid in the bottom of the funnel is removed (S16). Then, concentrated sulfuric acid is added again (S13) to remove sulfuric acid under the separating funnel after shaking and standing, and this operation is repeated several times to ten times until the coloring of the sulfuric acid becomes thin.

At this time, by treating the sample extracted with an organic solvent such as hexane with concentrated sulfuric acid, polar compounds such as lipids, amines and aldehydes, which are interfering substances in the extract, can be removed, and in the process As it breaks down, the sulfate layer turns dark brown.

However, the purification process using sulfuric acid generates a lot of waste sulfuric acid used in the purification process, so the operation is very cumbersome, and there are many problems for the safety of the tester during the waste liquid treatment. The disadvantage is that the test operation time becomes very long due to time.

In addition, since the sulfuric acid layer simply moves to the lower portion of the separating funnel by gravity sedimentation, not only does it take a long time to separate the layers, but also the sulfuric acid remains on the upper surface of the separating funnel.

In order to solve the above problems of the prior art, an object of the present invention is to provide a sulfuric acid treatment method that facilitates the operation in the sulfuric acid purification process, while reducing the time required for separation.

In order to achieve the above technical problem, the present invention comprises the steps of preparing an organic solvent extract; Injecting the organic solvent extract into a centrifuge vial; Adding sulfuric acid to the solvent extract; Standing the mixed solution to which the sulfuric acid is added; Centrifuging the mixed solution; And separating the upper organic solvent layer from the mixed solution separated by centrifugation.

In the present invention, the solvent of the organic solvent extract may include hexane.

In the present invention, the centrifugal vial is preferably made of Teflon material.

In addition, in the present invention, the sulfuric acid addition step to the centrifugation step may be repeated one or more times after the centrifugation step.

According to the present invention, the centrifugation process is applied to reduce the settling time that is typically required for the sulfuric acid treatment process by about 30 minutes or more per time.

In addition, as described above, residual sulfuric acid deposited on the wall of the separatory funnel, which is difficult to remove through the conventional sulfuric acid treatment process, can be removed by centrifugation, thereby contributing to the improvement of experimental precision.

1 is a view schematically showing a conventional sulfuric acid treatment method.
2 is a view schematically showing a sulfuric acid treatment method according to an embodiment of the present invention.
3 is a view schematically showing a sulfuric acid treatment method according to another embodiment of the present invention.

Hereinafter, with reference to the drawings will be described a preferred embodiment of the present invention.

2 is a view schematically showing a sulfuric acid treatment method of the present invention.

Referring to the drawings, first, an appropriate amount of sample extracted with an organic solvent such as hexane is prepared (S20). The amount of sample may be appropriately selected, and about 10-30 ml may be used considering the capacity of the vial described later.

Next, the solvent extract is transferred to a vial of about 50 ml volume (S21). In the present invention, the vial is preferably formed of a Teflon material. Vials made of Teflon have a strong resistance to sulfuric acid.

Subsequently, 5-10 ml of concentrated sulfuric acid is added to the vial (S22), and the reaction is shaken for about 10 minutes (S23). When the reaction is completed, the vial is placed in a centrifuge and centrifuged for about 5 minutes (S24).

Subsequently, the upper organic solvent layer of the sample having been centrifuged is extracted and used for the next purification process (S25).

In the present invention, centrifugal separation is used without using a conventional separation filter. According to this, the high-density sulfate layer in which polar compounds such as lipids, amines and aldehydes in the organic solvent extract are dissolved does not simply drop by gravity sedimentation but moves by force under the vial by centrifugal force. Accordingly, it is possible to drastically reduce the time required for fixing in the conventional method.

In addition, in the conventional separation filter method, sulfuric acid may remain on the top wall of the funnel, whereas in the present invention, the sulfuric acid layer is forcibly separated from the sulfuric acid layer so that the treatment efficiency due to the residual sulfuric acid is not reduced.

Meanwhile, as described above, the centrifugation for separation of the sulfate layer may be performed once, but the centrifugation may be performed one or more times depending on the degree of coloring of the treated sulfate layer.

3 is a schematic view illustrating a case where centrifugation is performed one or more times.

Referring to Figure 3, the solvent extract is transferred to centrifuge vials (S20, S21), concentrated sulfuric acid is added (S22), followed by shaking for about 10 minutes (S23), the centrifuge is mounted in a centrifuge, and then centrifuged. The process of performing (S24) is as described above.

If the lower sulfate layer is dark brown as a result of centrifugation, sulfuric acid is added to the centrifuge vial again (S22), and shaking (S23) and centrifugation (S24) are performed. This process may be repeated an appropriate number of times depending on the degree of coloring of the sulfate layer. However, in the case of the present invention, the sulfuric acid layer can be completely separated even with a small number of repetitions (2 to 3 times) compared to the conventional separation filter method.

In addition, when the centrifugation is repeated in the present invention, the solvent extract may be performed by separating the solvent extract of the upper layer centrifuged in the centrifugation step and adding sulfuric acid thereto.

Although preferred embodiments of the present invention have been described above with reference to the drawings, these embodiments do not limit the present invention. Those skilled in the art can modify it or replace some means, and such changes or modifications fall within the scope of the present invention without departing from the technical spirit of the present invention.

Claims

Preparing an organic solvent extract;
Injecting the organic solvent extract into a centrifuge vial;
Adding sulfuric acid to the solvent extract;
Standing the mixed solution to which the sulfuric acid is added;
Centrifuging the mixed solution; And
The organic solvent extract sulfuric acid purification method comprising the step of separating the upper organic solvent layer from the mixed solution centrifuged.

The method of claim 1,
The organic solvent extract is an organic solvent extract sulfuric acid purification method characterized in that it comprises hexane.

The method of claim 1,
The centrifugal vial is a teflon material, characterized in that the organic solvent extract sulfuric acid purification method.

The method of claim 1,
After the centrifugation step, the sulfuric acid purification step of the organic solvent extract, characterized in that the step of repeating the centrifugation step one or more times.