JP2600617Y2 - Closed container for chemical analysis - Google Patents

Description

[Detailed description of the invention]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a closed vessel for chemical analysis used for quantitative analysis of volatile chemical substances by gas chromatography.

[0002]

2. Description of the Related Art When a chemical substance is decomposed at a high temperature and a volatile decomposition product generated at that time is quantitatively analyzed, an ordinary cap container is used to remove the substance when the cap is opened. Volatilization prevents accurate measurement. Therefore, in order to collect a product or the like without dissipating, a closed container for chemical analysis as shown in FIG. 2 has conventionally been used. In a conventional hermetic container for chemical analysis, the upper surface of a main body container 1 made of glass is covered with a rubber film 21, and an annular cap 22 having a hollowed center is screwed to a container mouth portion to make a rubber film 21.
Is brought into close contact with the mouth of the main body container 1. When collecting and measuring the sample B, the sample suction needle A of the sample is pierced through the rubber film 21 and the sample B in the main body container 1 is collected.

[0003]

In the case of such a conventional closed container for chemical analysis, there is a problem that the rubber film 21 once pierced by the suction needle A has a poor sealing property and can hardly be reused.

The present invention has been made to solve the above-mentioned problems, and an object of the present invention is to provide a closed container for chemical analysis which can easily collect a component to be measured with little volatilization loss and can be used repeatedly.

[0005]

An analytical sealed container for chemical analysis according to the present invention, which has been made to achieve the above object, will be described with reference to FIG. 1 corresponding to an embodiment.化学Chemistry of the present invention
The analytical closed container for analysis has a container body 1, an inner cap 2 screwed to the container body 1 and having a center hole 6, and an outer cap 8 screwed to the inner cap 2 and having a center hole 9. ,
The O-ring 3 is compressed and interposed between the container body 1 and the inner cap 2, and the hermetic rubber packing 10 for closing the center hole 6 of the inner cap 2 is provided with both center holes 6 of the inner cap 2 and the outer cap 8. 9 high temperature high
It can be used repeatedly under rolling .

A needle guide tube 14 is preferably inserted into the hermetically sealed rubber packing 10 so as to be surrounded by a center hole of the outer cap 8. The hermetic rubber packing 10 is formed of soft rubber, and the lower surface is covered with a chemical resistant rubber 13.
It is preferable that the chemical-resistant rubber 13 closes the center hole 9 of the inner cap 2 on the container body side.

[0007]

When the sample B to be measured is filled in the container body and sealed with the inner cap 2, the sample B is prevented from being radiated by the O-ring 3.

When the outer cap 8 is attached, the suction needle A is pierced into the sealed rubber packing 10 into the container body 1, and then the suction needle A is withdrawn from the sealed rubber packing 10, the through hole of the needle is sealed. Remains in packing 10. When the outer cap 8 is tightened to the inner cap 2, the through hole opened by the suction needle A is compressed and closed between the center hole 6 of the inner cap 2 and the center hole 9 of the outer cap 8.

[0009]

Embodiments of the present invention will be described below. FIG. 1 is a half sectional view of the closed container for chemical analysis of the present invention. As shown in FIG. 1, a synthetic resin inner cap 2 is screwed into the mouth of a glass bottomed main body container 1 whose inner bottom surface is reduced in a mortar shape. An elastic packing 4 on which an O-ring 3 is fitted is provided on the back side of the inner cap 2, and is interposed between the elastic cap 4 and the mouth of the main container 1.

The elastic packing 4 is a disk made of hard tetrafluoroethylene having high chemical resistance, and has a central portion 5 which hangs down and has a through hole at the center thereof.
Thin edges are extended outwardly from the front and back surfaces of the disk, and annular grooves having a U-shaped cross section are formed in the circumferential portion. The O-ring 3 is fitted in the annular groove and is compressed between the container body 1 and the inner cap 2.

A center hole 6 is opened in the top plate of the inner cap 2. The center hole 6 has a step formed by narrowing the mouth at the lower end portion in the thickness direction of the top plate. On the upper surface of the inner cap 2, an annular protrusion 7 is raised around the center hole 6. The inner cap 2 has a thread groove on the outer circumference,
The outer cap 8 is screwed there. Outer cap 8
, A center hole 9 is formed in the top plate at a position directly above the center hole 6 of the inner cap 2.

Between the center hole 6 of the inner cap 2 and the center hole 9 of the outer cap 8, a hermetically sealed rubber packing 10 for closing the center hole 6 of the inner cap 2 is sandwiched. The sealing rubber packing 10 is formed of a soft rubber having a convex cross section with the small diameter portion 11 on the lower side and the large diameter portion 12 on the upper side.
2 is sandwiched between the upper end of the annular projection 7 of the inner cap 2 and the periphery of the lower surface of the center hole 9 of the outer cap 8. Small diameter part 1
Numeral 1 enters the inside of the center hole 6 of the inner cap 2, the tip of which is covered with a chemical resistant rubber 13, and abuts on the above-mentioned step to close the container body 1 side. Sealed rubber packing 10
In the large-diameter portion 12, a needle guide pipe 14 is provided upright with the pipe channel being surrounded by the center hole 9 of the outer cap 8. The needle guide pipe 14 is connected to the upper surface of the collar 15 by a reduced-diameter cylindrical pipe 16 having a vertical opening. This reduced-diameter cylindrical tube 16
Has an inner diameter that is reduced in a mortar shape downward. The lower surface of the collar 15 is connected to a needle hole tube 17 vertically communicating with the conduit of the reduced diameter cylindrical tube 16, and the needle hole tube 17 is connected to the large diameter portion 12 of the hermetically sealed rubber packing 10 to the depth of the collar 15. It pierces vertically.

The outer diameter of the reduced-diameter cylindrical tube 16 substantially coincides with the inner diameter of the center hole 9 of the outer cap 8, and is inscribed in the center hole 9 and protrudes upward from the center hole 9. Is in contact with the upper surface of the collar 15 of the needle guide tube 14. The outer cap 8 presses the upper surface of the sealing rubber packing 10 through the lower surface of the collar 15.

The outer cap 8 is provided with two screw holes with a center hole 9 interposed therebetween, and a gap adjusting screw 18 is screwed up and down so as to be able to move up and down. The gap adjusting screw 18 is formed by an embedded screw.

A sample B to be measured is filled in a glass bottomed main body container 1 and sealed with an inner cap 2 and an outer cap 8. A suction needle A for collecting a sample is inserted into a tightly-sealed rubber packing 10 from a channel of a needle guide pipe 14 inscribed in a center hole 9 of an outer cap 8, and a sample B vaporized in the main body container 1. Aspirate. The collected sample B is
For example, it is sent to a measuring device such as gas chromatography.

When the suction needle A is pulled out of the needle guide tube 14, a through hole for the needle remains in the hermetically sealed rubber packing 10, but it is closed when the outer cap 8 is tightened. Outer cap 8
The gap adjusting screw 18 prevents overtightening.

The suction needle A is guided by a needle guide pipe 14 which vertically penetrates the pipe, and the hermetically sealed rubber packing 1 is provided.
0, the suction needle A is vertically inserted into the container body 1. Even though the sealing rubber packing 10 is formed of soft rubber, the lower surface is formed of the chemical resistant rubber 13, so that even if the corrosive reagent is filled in the container body 1, the sealing rubber packing 10 may be corroded. There is no.

Example 1 2.0 ml of toluene was filled in a glass body container 1 having an inner volume of 5 ml, and sealed with an inner cap 2 and an outer cap 8 having the above structure. Then, each was heated for 1 hour at each predetermined temperature, and the amount of volatilization was measured.

Next, the suction needle A was repeatedly pierced 50 times and pulled out, and thereafter the volatilization amount was measured in the same manner.

Table 1 shows the results before piercing the suction needle A together with the predetermined heating temperature. Table 2 shows the results after the suction needle A was repeatedly pierced 50 times, together with the predetermined heating temperature.

[0021]

[Table 1]

[0022]

[Table 2]

Examples 2-5 Instead of toluene, Tables 2 and 3
The same procedures as in Example 1 were carried out except that each of the substances shown in Table 1 was filled.

Comparative Example 1 2.0 ml of xylene was charged into a conventional closed vessel for chemical analysis having a content of 5 ml as shown in FIG. 2, sealed, heated at 150 ° C. for one hour, and the internal pressure and the volatilization amount were measured. It was measured. Next, the suction needle A for sampling was once pierced, pulled out, and the internal pressure and the amount of volatilization were measured again. Table 3 shows the results.

[0025]

[Table 3]

The sealed container for chemical analysis used in the examples was found to have a remarkable sealing force as compared with the sealed container for chemical analysis used in the comparative example.

At that time, the internal pressure was raised to 10 at a temperature of 250 ° C.
It was found that even when the pressure was increased to kg / cm ^2, sufficient airtightness was obtained.

[0028]

As described in detail above, the sealed container for chemical analysis of the present invention has high sealing performance even under high temperature and high pressure. Even if the suction needle is repeatedly pierced a considerable number of times, the hermeticity is hardly reduced. Therefore, low-boiling-point decomposition products and the like can be quantified with high precision without volatilization loss. The component to be measured can be easily collected, and the measurement can be automated. Long-term repeated use is also possible.

[Brief description of the drawings]

FIG. 1 is a half sectional view showing one embodiment of a sealed container for chemical analysis to which the present invention is applied.

FIG. 2 is a half sectional view showing one embodiment of a conventional sealed container for chemical analysis.

[Explanation of symbols]

1 is a main body container, 2 is an inner cap, 3 is an O-ring, 4
Is an elastic packing, 5 is a center part, 6 is a center hole of an inner cap, 7 is an annular projection, 8 is an outer cap, 9 is a center hole of an outer cap, 10 is a sealing rubber packing, 11 is a small diameter part,
12 is a large diameter portion, 13 is a chemical resistant rubber, 14 is a needle guide tube, 15 is a collar, 16 is a reduced diameter cylindrical tube, 17 is a needle hole tube,
18 is a gap adjusting screw, A is a suction needle, and B is a sample.

Continuation of the front page (56) References JP-A 1-148859 (JP, U) JP-A 63-21841 (JP, U) JP-A 63-152640 (JP, U) JP-A 4-24044 (JP) , U) Japanese Utility Model Showa 62-50729 (JP, U) Japanese Utility Model Application Hei 2-105862 (JP, U) (58) Fields investigated (Int. Cl. ⁶ , DB name) G01N 1/00 101 G01N 1/10 G01N 1/22 G01N 35/02 B01L 3/00

Claims (3)

(57) [Scope of request for utility model registration] A container body, an inner cap screwed into the container body and having a center hole, and an outer cap screwed into the inner cap and having a center hole, between the container body and the inner cap. O- ring is interposed compressed into high temperature high pressure seal plug rubber packing for closing the center hole of the inner cap, characterized in that is provided sandwiched between the two center hole of the inner cap and outer cap Bottom, enable repeated use
Sealed container for scientific analysis . 2. The sealed container for chemical analysis according to claim 1, wherein a needle guide pipe is inserted into the hermetically sealed rubber packing so as to be surrounded by a center hole of the outer cap. 3. The sealing rubber packing is made of soft rubber, and the lower surface thereof is covered with a chemical resistant rubber, and the chemical resistant rubber closes the container body side of the center hole of the inner cap. 3. The sealed container for chemical analysis according to 1 or 2.