JPS58135457A - Measuring apparatus of nonvolatile matter - Google Patents

Abstract

PURPOSE:To prevent the stagnation of flocculated matters in a pipe and also, to carry out easily washing of each instrument and insertion and extraction of a sample vessel, by combining a core pipe of a vertical type furnace with a freely detachable cap suspending a sample holder. CONSTITUTION:A heating device 14 heating and keeping the inside of a pipe at a prescribed temperature, is provided around the outer circumference of a vertical type furnace core pipe 9 and a freely detachable cap 16 suspending a sample holder 18 is joined closely to the upper end of the device 14 through an airtight joining part 15. On one hand, a collection bottle 10 for collecting a condensed gas having an inactive gas exit 13 is joined to the lower end of the device 14 through the part 15 in the same way. An inactive gas is introduced from an inactive gas entrance 12 at use time. And, the holder 18 is taken out by unfastening the part 15 of the pipe 9 and the cap 16, and the holder 18 is inserted into the pipe 9 again and said holder is fixed by the part 15 after placing a sample vessel 11 stored a weighed sample in a sample receiving part 19 and then, the sample is heated for the necessary time.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a nonvolatile content measuring device suitable for use in the analysis of various volatile samples such as carbon dioxide.

Generally, when determining the quality, composition, etc. of these volatile samples using the area percentage method of a gas chromatograph, it is necessary to measure the nonvolatile content and correct the analytical values.

Currently, as a method for measuring non-volatile content, for example,
The knowledge principle shown in the figure is known. That is, the furnace core tube (1'l has a liquid reservoir +
21? A sample container (3) is placed in the tube, and nitrogen or helium gas is injected through the inert gas inlet (4) and discharged through the same outlet (5).
6) is a method in which heating is controlled by a temperature control unit (81).

However, with this method, volatile matter generated by heating the sample accumulates in the tube, making it difficult to withstand repeated use over a long period of time, and because the liquid reservoir and electric tubular furnace are integrated, cleaning the equipment is difficult. There are disadvantages such as difficulty in controlling the sample container (3), difficulty in handling the sample container (3), and difficulty in controlling the temperature, making it difficult to obtain accurate measured values. However, it has not yet reached the point where it can be fully put into practical use.

Therefore, the analysis of volatile samples currently tends to lack accuracy, and it is desired to develop a means for obtaining accurate analytical values.

The inventors of the present invention have focused on this situation and have conducted extensive research to improve the above-mentioned shortcomings. As a result, it was discovered that the above drawbacks could be overcome by combining a vertical furnace core tube and a removable cap with a suspension/pull holder, leading to the present invention.

That is, the features of the present invention are based on a vertical furnace core tube with a heating device around it, a removable cap with a sample holder suspended from the upper end of the core tube, tightly joined to the core tube, and an inert gas inlet. - A collection bottle for collecting flocculated gas provided at the upper end of the inert gas outlet is closely connected to the lower end of the furnace core tube, and the cap, the vertical furnace core tube, and the collection bottle are closely connected to the lower end of the furnace core tube. The nonvolatile content measuring device has a structure in which a collecting bottle is connected to the bottle and can be sealed with an inert gas.

Hereinafter, the present invention will be explained in more detail based on the accompanying drawings.

Is Figure 2 an example of the device of the present invention? Fig. 3 is an enlarged view of the main parts.

In the above figure, (9) indicates a vertical furnace core tube, and a heating device (141) is installed around the outer periphery of the tube to heat and maintain the inside of the tube at a predetermined temperature. A removable cassop (16) suspending from the holder is closely connected via an airtight joint (15)', and a collection bottle for condensed gas collection having an inert gas outlet (131) is attached at the lower end. αO) are similarly closely joined via an airtight joint 0ω.

Here, the vertical furnace core tube (9), cap θ6), and collection bottle (10) are all made of heat-resistant tempered glass, such as Noquilenx glass or Vycor glass, and the airtight joints of each part A silicon packing (15a) or the like is used for a9 to ensure good airtightness.

In the above configuration, the sample holder 〇 & ke hanging cap Oe is the flow rate adjustment valve 1, as shown in the figure.
It is connected to the inert gas introduction pipe, such as nitrogen gas, helium gas, alcon gas, etc., which is equipped with a pressure gauge and a flow meter t2D, and the inert gas population a'zrwx is shown in an enlarged view in Fig. 3. On the other hand, the sample holder 〇81 suspended from the cap is made of stainless steel wire, etc.
In order to set the sample container 0υ in a predetermined position in the furnace core tube (9), a wire is woven into a basket shape at the lower end of the furnace core tube (9).
It has a sample receiving part (1) as shown in FIG. 3 (b) attached with 191"k.

However, of course, it is also possible to connect the inert gas port (121 to the vertical furnace core tube (9) without the need to connect it to the cap 06), and in this case, at least the furnace core tube (9) can be connected to the vertical furnace core tube (9).
) It is important to install the sample container above the 0υ position.

In addition, 07) in the figure is a thermocouple thermometer, and in order to accurately set and detect the temperature of the sample part, there is a furnace core tube ( 9) It is installed by being penetrated from the side, and the furnace core tube (9) on the outer periphery of the sample part is further provided with a viewing window (a) for viewing the progress.

The above description is based on the embodiment device shown in FIGS. 2 and 3, but the device of the present invention is of course not limited to this description, and various modifications may be made as appropriate without departing from the purpose. Needless to say, design changes are allowed.

As an example, FIG. 4 shows another embodiment of the suspension of the sample holder, and the sample holder α
Insert a thermocouple thermometer (1
7) is assembled and the sample container αυ is held at its lower end, and the inert gas population Q21
is a mechanism in which an inert gas is introduced from the side of the furnace core tube (9) by opening at the side of the furnace core tube (9). In this figure, the same reference numerals as in FIGS. 2 and 3 indicate the same parts.

The apparatus of the present invention has the above-mentioned configuration, and the manner in which the apparatus is used will now be described.

First, in the device as described above, the inert gas inlet (121
Introduce an inert gas such as nitrogen gas, and heat the IJII thermal device Q.
41, the sample container temperature is set to a predetermined temperature. On the other hand, a required sample is accurately weighed and stored in the sample container (111).

After making preparations in this way, remove the joint 09 between the furnace core tube (9) and the cap (15), take out the sample holder Q8, place the weighed sample container αυ on the sample receiver full Q'l, After that, insert the sample holder α into the furnace core tube (9) again, tightly connect the cap to the furnace core tube (9) using the joint Q51, and attach the stopper (not shown).
Fix it with.

Next, after the fixation is completed, the housed sample is heated in that state for a required period of time. At this time, most of the volatile components accumulate at the bottom of the flocculation gas collection bottle (IQl),
A part of the gas is discharged to the outside from the inert gas outlet a3 along with the nitrogen gas. On the other hand, non-volatile components remain as they are in the weight of the sample container.

When the heating is finished, the sample holder 08 is taken out again in the same way as before, and the sample container 3 (lυ) is removed, cooled to room temperature, and its weight t'' is measured.

Then, this heating operation and cooling zero weight measurement are repeated, and when it is confirmed that the salting of the sample container after heating is constant, the measurement work is completed.

From this result, the nonvolatile content in the sample is calculated using the following formula to obtain the required appropriate analytical value.

However, A: weight of empty sample container B; weight of sample container with sample included C: weight of sample container with sample after heating, that is, when determining the composition ratio of a compound by the area percentage method of gas chromatography, for example, it is difficult to accurately determine the nonvolatile components. It is necessary to measure and correct the area percentage ratio, but by using the above-mentioned apparatus of the present invention, this correction can be performed accurately. The temperature can be adjusted to within ±5° C., and extremely reliable correction values can be obtained.

Below, we will show examples of actual measurements of non-volatile content using the apparatus of the present invention.

(Measurement example) Using a measuring device equipped with a sample holder shown in Figure 4, 50 mt7t of nitrogen gas was supplied from the inert gas inlet.
;p, and set the temperature of the sample container part to 300℃ using a heating heater.
rnf/ crude 1-aminoanthraquinone and weighed accurately. The weight of the sample container is 102.08 The weight of the sample container including the fermentation sample is S l 3.72 m? Q Next, remove the connection between the furnace core tube and camp of the device, take out the sample holder, place the weighed sample container above on the sample receiver, reinsert it into the furnace core tube, and secure both with the stopper. Fixed.

When the sample was heated in this state for 30 minutes, most of the volatile components remained in the collection bottle, some of them were accompanied by nitrogen gas and released to the outside from the inert gas outlet, while non-volatile components remained in the sample container. remained.

The sample holder was removed from the sample as described above, the sample container was removed, and the weight was measured after cooling to room temperature.

Next, the above-mentioned heating and cooling 1 weight measurement was carried out again to confirm that the weight of the sample container after heating was constant. Its weight was l l B, 36 mp.

As a result, it was found that the nonvolatile content in the initial crude 1-aminoanthraquinone was 7%.

As described above, the device of the present invention uses a vertical furnace core tube, a removable cap with a sample holder suspended at the upper end is closely connected, and a collection bottle for collecting coagulated gas is closely connected to the lower end. Since it is a so-called assembly method, each part can be easily removed, making it possible and easy to clean each instrument, and it is easy to insert and remove sample containers, making it easy to operate.
Moreover, since the furnace core tube is vertical, aggregated substances do not accumulate inside the tube, and it can withstand repeated use over a long period of time.
This method has many advantageous advantages, and, as mentioned above, has the remarkable effect of providing highly reliable correction values with good adjustment accuracy.

In addition, the device of the present invention is particularly intended for the measuring section of the device during actual operation, which consists of a measuring section and a control section. It can be easily combined with a flow rate control, a pressure gauge, a flow meter, a heating source m degree indicator, etc., and is suitable for use and extremely suitable for industrialization, and is expected to be put into practical use in the future.

[Brief explanation of the drawing]

Figure 1 (F) is a principle diagram of the non-volatile content measuring device; Figure (B) is a partially enlarged view thereof. Figure 2 is an overall conceptual diagram showing an example of the non-volatile content measuring device according to the present invention. Figure 4 shows an example of the sample holder of the invention, in which (a) is a schematic front view showing a part of the internal structure, and (b) is a plan view of the sample receiving part. It is an internal structure explanatory diagram showing another example. (9)... Vertical furnace core tube, 001... Collection bottle. aυ... Sample container, 02... Inert gas inlet. Q31...Inert gas outlet, 04...Heating device. 051...M combination Wr, (15a)...Silicon gasket. Q61...Cap, 01G...Sample holder. θ9... Sample receiving part. Cν) 2nd eye

Claims (1)

[Claims] / A removable cap with a sample holder suspended at the upper end of a vertical furnace core tube having a heating device around it is closely connected to the flocculated gas, and an inert gas outlet is provided at the bottom of the tube. The collection bottle' (r) is closely connected and an inert gas inlet for introducing an inert gas into the vertical furnace core tube is provided at least above the position of the sample container suspended by the sample holder. A non-volatile content measuring device characterized in that a shaped furnace core tube and a collection bottle are connected to each other so that an inert gas can be sealed and circulated in the system. 2. A cap, a vertical furnace core tube, and a vertical furnace. A non-volatile content measuring device according to claim 1, in which a silicon gasket is used for each joint between the core tube and the collection bottle. 3. A patent in which the cap, the vertical furnace core tube, and the collection bottle are each made of glass. Non-volatile 1 according to claim 1 or 2
minute measuring device.