JPH0155404B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a nonvolatile content measuring device suitable for use in analyzing various volatile samples such as benzene, naphthalene, and anthraquinone.

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 such non-volatile content, a principle as shown in FIG. 1 is known, for example. That is,
A liquid reservoir 2 is provided in a furnace core tube 1 whose one end is closed with a silicone rubber stopper 7, a sample container 3 is placed in the tube, nitrogen or helium gas is pressurized through an inert gas inlet 4, and the gas is discharged through the same outlet 5. However, during this period, the electric tube furnace 6 is heated under control by the temperature control section 8.

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. In addition, it is difficult to operate the sample container 3 in and out, and it is relatively difficult to control the temperature.
It has drawbacks such as difficulty in obtaining accurate measurement values, and has not yet been fully put into practical use.

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

The inventors of the present invention have focused on the above-mentioned situation and have conducted extensive research in order to improve the above-mentioned drawbacks, and as a result, have combined a vertical furnace core tube with a removable cap from which a sample holder is suspended. The inventors have discovered that the above-mentioned drawbacks can be overcome, and have arrived at 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 is closely connected, and an inert gas inlet is provided. On the other hand, a collection bottle for collecting flocculated gas having an inert gas outlet at the upper end 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 non-volatile content measuring device has a structure in which the bottle can be sealed with an inert gas by communicating with the bottle.

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

FIG. 2 is an overall schematic diagram showing an example of the device of the present invention;
Figure 3 is an enlarged view of the main parts.

In the above figure, reference numeral 9 indicates a vertical furnace core tube, and a heating device 14 is installed around the outer circumference of the tube to heat and maintain the inside of the tube at a predetermined temperature, and a sample holder 18 is installed at the upper end. A suspended removable cap 16 is closely connected via the hermetic joint 15, while at the lower end a collection bottle 10 for collecting condensed gas having an inert gas outlet 13 is likewise connected to the hermetic joint 15. are closely connected through the

Here, the vertical furnace core tube 9, cap 16, and collection bottle 10 are all made of heat-resistant tempered glass, such as Pyrex glass or Vycor glass, and the airtight joints 15 of each part are airtight. A silicon packing 15a or the like is used to improve the properties.

In the above configuration, the sample holder 1
As shown in the figure, the cap 16 suspending the 8 is connected to a flow rate regulating valve 23, a pressure gauge 22, and a flow meter 21 for inert gas such as nitrogen gas, helium gas,
It is connected to an inlet pipe for Arcon gas, etc., and has an inert gas inlet 12, which is shown in an enlarged view in FIG. In order to set the sample container 11 at a predetermined position in the furnace core tube 9, the sample receiving part 19 is made of wire knitted into a basket shape and equipped with a non-slip part 19' as shown in FIG. 3B. There is.

However, of course, the inert gas inlet 12 can also be connected to the vertical furnace tube 9 without having to be connected to the cap 16, in which case at least the sample container 11 in the furnace core tube 9 can be connected. It is important to provide it above the position.

In addition, in the figure, 17 is a thermocouple thermometer, which is attached to the sample container 11 in order to accurately set and detect the temperature of the sample part.
The furnace core tube 9 is inserted from the side and attached at a position in contact with or in a nearby position (in the figure, the latter position), and the furnace core tube 9 on the outer periphery of the sample part is further provided with a viewing window 20 to visually check the progress. is provided.

The above description is based on the embodiment apparatus shown in FIGS. 2 and 3, but the apparatus of the present invention is of course
It goes without saying that the invention is not limited to this explanation, and that various design changes may be made as appropriate without departing from the purpose.

FIG. 4 shows, as an example, another embodiment for suspending the sample holder.
A configuration is used in which a thermocouple thermometer 17 is assembled at the lower end of which a sample container 11 is held, and an inert gas inlet 12 is opened on the side of the furnace core tube 9 and is connected to the side of the furnace core tube 9. The mechanism is such that an inert gas is introduced. In addition, in the same figure, Figures 2 and 3
The same reference numerals as in the figure indicate the same parts.

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

First, in the apparatus as described above, an inert gas such as nitrogen gas is introduced through the inert gas inlet 12, and the temperature of the sample container is set to a predetermined temperature using the heating device 14. On the other hand, sample container 11
Accurately weigh and store the required sample in the chamber.

After making preparations in this way, the joint 15 between the furnace core tube 9 and the cap 16 of the apparatus is removed, the sample holder 18 is taken out, the weighed sample container 11 is placed on the sample receiving part 19, and the sample is placed again. Insert the holder 18 into the furnace core tube 9 and connect the joint 15
The cap 16 is closely connected to the furnace core tube 9 and fixed with a stopper (not shown).

Next, after the fixation is completed, the accommodated sample is heated in that state for a required period of time. At this time, most of the volatile components are in the flocculated gas collection bottle 1.
0, and a part of it is released to the outside from the inert gas outlet 13 along with the nitrogen gas. on the other hand,
The nonvolatile components remain in the sample container 11 as they are.

When the heating is finished, the sample holder 18 is taken out again in the same manner as before, the sample container 11 is removed, and after cooling to room temperature, its weight is measured.

This heating operation, cooling, and weight measurement are repeated, and when it is confirmed that the weight of the sample container after heating is constant, the measurement operation is ended.

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

Non-volatile content % = C-A/B-A x 100 However, A: Weight of empty sample container B; Weight of sample container with sample C: Weight of sample container with sample after heating When determining the composition ratio of a compound, it is necessary to accurately measure the nonvolatile components and correct the area percentage ratio, but by using the device of the present invention, this correction can be performed accurately. In particular, it is possible to adjust the vaporization chamber temperature of the gas chromatograph and the temperature for non-volatile content measurement within ±5° C., and extremely reliable correction values can be obtained.

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

(Measurement example) Using a measuring device equipped with the sample holder shown in Figure 4, nitrogen gas is supplied from the inert gas inlet.
The sample was introduced at a flow rate of 50 ml/min, and the temperature of the sample container was set to 300°C using a heater.

And, on the other hand, approximately
200 mg of crude 1-aminoanthraquinone was placed and accurately weighed. The weight of the sample container was 102.08 mg.The weight of the sample container including the sample was 313.72 mg.

Next, remove the connection between the furnace core tube and the cap of the device, take out the sample holder, place the weighed sample container on the sample receiver, and reinsert it into the furnace core tube.
Both were securely fixed with a stopper.

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, and 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, cooling, and weight measurement were performed again, and it was confirmed that the weight of the sample container after heating was constant. This weight was 118.36 mg.

As a result, it was found that the nonvolatile content in the initial crude 1-aminoanthraquinone was 7.7%.

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 this is a so-called assembly method, each part can be removed freely, each instrument can be cleaned easily and easily, and the sample container can be easily inserted and removed, providing excellent operability.Furthermore, the furnace core tube is vertical. Therefore, aggregated substances do not accumulate in the pipe, and it can withstand repeated use over a long period of time.It has a very convenient advantage, and as mentioned above, the adjustment accuracy is good and extremely reliable correction values can be obtained. It has a great effect.

In particular, according to the device of the present invention, since the inert gas inlet is located above the sample container position and the inert gas flows only in one direction from above to below, volatile matters are always dispersed downward, and the sample (weighed) In addition, substances with a relatively high boiling point that volatilize in the heating device are cooled in a collection bottle.
Since it becomes a liquid or solid and is collected, there is no adverse effect on sample preparation, and it has extremely excellent effects especially in terms of safety and hygiene.

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 flow rate control, pressure gauge, flow meter, heating source temperature 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 drawings]

Fig. 1A is a principle diagram of the non-volatile content measuring device, B is a partially enlarged view thereof, Fig. 2 is an overall conceptual diagram showing an example of the non-volatile content measuring device according to the present invention, and Fig. 3 is a diagram of the non-volatile content measuring device according to the present invention. In the figure showing one example of a sample holder, A is a schematic front view showing a part of the internal structure, and B is a plan view of a sample receiving part. Moreover, FIG. 4 is an explanatory diagram of the internal structure of another embodiment of the non-volatile content measuring device of the present invention. 9... Vertical furnace core tube, 10... Collection bottle, 11...
Sample container, 12...Inert gas inlet, 13...Inert gas outlet, 14...Heating device, 15...Joint part, 15a...Silicon gasket, 16...Cap, 18...Sample holder, 19... ...Sample receiving section.

Claims (1)

[Scope of Claims] 1. A flocculated gas collection device in which a removable cap with a sample holder suspended is closely connected to the upper end of a vertical furnace core tube having a heating device around it, and an inert gas outlet at the lower end. In addition to tightly joining the bottles, 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, and the cap and the vertical furnace core tube are connected to each other. A non-volatile content measuring device characterized in that a collection bottle is communicated with the system so that an inert gas can be sealed and circulated through the system. 2. The non-volatile content measuring device according to claim 1, wherein a silicone packing is used for each connection between the cap, the vertical furnace core tube, and the vertical furnace core tube and the collection bottle. 3. The nonvolatile content measuring device according to claim 1 or 2, wherein the cap, the vertical furnace core tube, and the collection bottle are each made of glass.