JPH04122457A - Constant temperature bath with shaking mechanism - Google Patents

Abstract

PURPOSE:To permit the time required for the decomposition of inorg. matter to be shortened by adding a shaking mechanism to a constant temp. bath used at the time of decomposing the inorg. matter by pressure decomposition method. CONSTITUTION:A pressure decomposition container storage shelf 3 is divided by shelves 12 to receive a plurality of storing cases 11 and so constructed as to be reciprocally rockably movable about a rotary shaft 4. In a shaking mechanism, a link 14 is freely rotatably mounted to a disk plate 13 attached to the rotary shaft of a motor 2 and the other end of this link 14 is in engagement with a slider 15 provided on the rotary shaft 4. In this structure, by rotating a motor 2, the storage shelf 3 can be rockably moved about the rotary shaft 4. The disc plate 13 is provided with a plurality of link holding holes 16 to change the stopping position of the link 14, whereby the rocking angle of the storage shelf 3 can be changed. In this way various kinds of samples can be decomposed in a stationary condition without shaking action and in a shaking condition.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a constant temperature bath with a shaking mechanism used for chemical decomposition of inorganic substances.

(Conventional technique) Conventionally, when chemically decomposing inorganic substances, the sample containing the inorganic substance to be decomposed is placed in a pressure decomposition container, and this pressure decomposition container is placed in a constant temperature bath maintained at a constant temperature. The reaction is promoted by allowing it to stand still.

However, when the reaction is left in a constant temperature bath,
There was a problem in that it took a long time to decompose inorganic substances.

For this reason, hena1. chim, hecta, 47 (19
69) “DECOMPO3ITIO” on p517-527
N BY PRESSURE IN 1N0RGANI
CANALYSIS'', J. DOLEZAL et al. disclose an attempt to shorten the time required for reaction by rotating a pressurized decomposition vessel within a constant temperature bath.

(Problem to be Solved by the Invention) However, although the apparatus of J. DOLEZAL et al. mentioned above can shorten the time required to decompose inorganic substances,
The acid or decomposition solution used leaks from the seal of the Teflon container inside the pressure decomposition container, corrodes the metal pressure decomposition container, contaminates the sample, and causes loss of decomposition solution, leading to complete sample decomposition. There was a problem that the liquid could not be obtained.

An object of the present invention is to solve the above-mentioned problems and provide a constant temperature bath with a shaking mechanism that can shorten the time required for decomposing inorganic substances and perform reactions with less contamination.

(Means for Solving the Problems) A constant temperature chamber with a shaking mechanism of the present invention includes: a constant temperature chamber; a pressurized decomposition container storage shelf provided inside the constant temperature chamber and having a rotation axis for shaking; ;Put it on the rotating shaft of the pressurized decomposition container storage shelf.
The apparatus is characterized by comprising: a shaking mechanism that shakes the storage shelf; and a storage box that is stored in the pressurized decomposition container storage shelf and holds the pressurized decomposition containers inside.

(Function) In the above-mentioned configuration, since the pressure decomposition container storage shelf is shaken by the shaking mechanism, the pressure decomposition container is rocked in the thermostatic chamber, and the reaction is accelerated, but the decomposition acid or decomposition There is no liquid leakage, and it is possible to achieve the constant temperature bath that is free from contamination and can complete the reaction in a short time, which is the objective of the present invention.

The rotational motion of the shaker and motor is converted into vertical motion by a link, and the pressurized decomposition container storage shelf in the thermostatic chamber is swung through the drive shaft, thereby causing the pressurized decomposition containers in the storage shelf to be swung. I will do it.

(Example) FIG. 1 is a perspective view showing an example of a constant temperature bath of the present invention. In FIG. 1, a constant temperature bath 1 is composed of a bath main body 1a, a lid portion 1h, and a control portion 1c.

A motor 2, which forms part of the shaking mechanism, is mounted on the upper surface of the tank body 1a. Further, inside the tank body 1a, a pressurized decomposition container storage shelf 3 is rotatably attached to a support body 5 via a rotation shaft 4 for shaking.

FIGS. 2(a) and 2(b) are a side view and a front view partially showing the configuration of an example of the pressurized decomposition container storage shelf 3 used in the thermostatic chamber 1 of the present invention. As shown in FIGS. 2(a) and 2(b), the storage shelf 3 is partitioned into shelves 12 for accommodating a plurality of storage boxes 11, and is swingable by reciprocating around the rotation axis 4. It is configured. The shaking mechanism consists of motor 2 and disk 13.
, a link 14, and a slider 15.

FIG. 3 is a diagram showing in detail the configuration of an example of a shaking mechanism used in the constant temperature bath 1 of the present invention. The shaking mechanism is constructed by rotatably attaching a link 14 to a disc 13 attached to the rotating shaft of the motor 2, and engaging the other end of this link 14 with a slider 15 provided on the rotating shaft 4. ing. With this configuration, by rotating the motor 2, the pressurized decomposition container storage shelf 3 can be swung around the rotation axis 4. In addition, as shown in Fig. 3, the disk 1
3 is provided with a plurality of link fixing holes 16, and by changing the fixing position of the link 14, the swinging angle of the pressurized decomposition container storage shelf 3 is changed.

Actually, various samples were decomposed in a static state without shaking and in a state with shaking using the thermostatic chamber of the present invention described above.
The degradation rate was quantified. The results are shown in Table 1.

The decomposition operation and the determination of the decomposition rate are as follows.

Decomposition procedure Weigh 0.100 to 1.000 g of the sample, which had been previously dried at 105°C for 2 hours and left to cool in a desiccator, into a Teflon container, add various types of vinegar or alkali, and cover with a Teflon lid. Put on the cloak and tighten it tightly. This is heated at a certain temperature for a certain period of time.

Quantitative force for decomposition rate■After leaving the pressure decomposition container to cool, carefully remove the screwed jacket, add approximately 50ml of water to the Teflon container in several portions,
Leave it in the tray until nitrite and nitric acid gases are no longer generated. This sample solution is suction-filtered using a membrane filter, and the filter paper from which the residue adhering to the membrane filter and suction funnel has been wiped is transferred to a platinum crucible of known mass. After being incinerated at low temperature with a Bunsen burner, the mass is measured. . After that, the decomposition rate (wt
%).

Decomposition rate (4%) - ((Amount of sample weighed - Amount of residue after treatment) / Amount of sample weighed) , it can be seen that the decomposition efficiency becomes better when shaking is added using the constant temperature bath of the present invention.

In Table 1, for α-alumina sample No. 3, the relationship between temperature and decomposition rate is shown in Figure 4, the relationship between time and decomposition rate is shown in Figure 5, and the relationship between shaking angle and decomposition rate is shown in Figure 6. The relationship between the number of shaking and the decomposition rate is shown in FIG. 7. These results show that the higher the temperature, the longer the time, the greater the shaking angle, and the greater the number of shaking, the higher the decomposition rate.

The present invention is not limited only to the embodiments described above,
Many variations and changes are possible. For example, in the two embodiments, the shaking mechanism is composed of a disk rotated by a motor, a link, and a slider, but the present invention is not limited to this configuration, and it goes without saying that other configurations may be used.

(Effects of the Invention) As is clear from the above explanation, according to the present invention, by adding a shaking mechanism to a constant temperature bath used when decomposing inorganic substances by the pressure decomposition method, inorganic substances can be The time required for decomposition can be shortened, moreover, almost complete decomposition can be achieved with a simple process, and since only shaking is required, there is no contamination of foreign matter into the sample, and inorganic matter can be decomposed with extremely little contamination.

[Brief explanation of the drawing]

Fig. 1 is a perspective view showing the structure of an example of the thermostatic oven of the present invention, and Figs. 2 (a) and (b) partially show the structure of an example of the pressurized decomposition container storage shelf used in the thermostatic oven of the invention. 3 is a diagram showing in detail the configuration of an example of the shaking mechanism used in the thermostatic chamber of the present invention, and FIG. 4 is a diagram showing the relationship between temperature and decomposition rate of Example Sample No. 3. Graph, Figure 5 is a graph showing the relationship between time and decomposition rate for Example Sample No. 3, Figure 6 is a graph showing the relationship between shaking angle and decomposition rate for Example Sample No. 3, Figure 7 is Example Grat/temperature bath 1b showing the relationship between the number of shaking and decomposition rate of sample No. 3...Lid 2...Motor 4...Rotating shaft 11...Storage box 13...Disc 15 ...It's a slide duff. ] a... Tank body 1c... Control part 3... Pressurized decomposition container storage shelf 5... Support body 12... Shelf 14... Link 16... Link fixing hole Fig. 2 ( a) (b) Figure 4 Figure 5 Time (hr) Figure 7

Claims (1)

[Claims] 1. A constant temperature chamber; A pressurized decomposition container storage shelf provided inside the constant temperature chamber and having a rotating shaft for shaking; A pressurized decomposition container storage shelf that is attached to the rotating shaft of the pressurized decomposition container storage shelf and shakes the storage shelf. 1. A constant temperature bath with a shaking mechanism, comprising: a shaking mechanism for holding the pressurized decomposition containers;