JP3005283B2 - Tobacco smoke introduction device - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to an apparatus for introducing tobacco smoke, and more specifically, to an apparatus for introducing smoke to a tobacco smoke analyzer.

[Prior Art] The smoke component of tobacco is very wide ranging from a vapor phase component to a medium to high boiling component and a non-volatile component.

At present, to analyze non-volatile components of tobacco smoke components other than non-volatile components by gas chromatography, they are divided into a vapor phase component and a medium-high boiling point component, and analyzed separately. This is because the required setting conditions of the analytical column of the gas chromatograph differ greatly between the above components. For example, if all tobacco smoke is analyzed on a column set for medium and high boiling components, the separation between the components contained in the vapor phase components will be insufficient, and these analysis results will show a peak at the beginning of the retention time. Since it is obtained in an overlapping state, reliable analysis cannot be performed. On the other hand, if all the tobacco smoke is passed through the column set for the vapor phase component, the medium and high boiling components will adhere to the column, making the column unusable.

For the reasons described above, the vapor phase component is analyzed by introducing the smoke passing through the glass fiber filter directly into the gas chromatograph by the gas sampler. In addition, a method of extracting a medium-high boiling point component from a smoke aggregate collected on a glass fiber filter with an organic solvent or the like and then analyzing the extracted component with a gas chromatograph is generally performed.

[Problems to be Solved by the Invention] However, in the above-mentioned conventional analysis method, a considerable amount of the vapor phase component having a relatively high boiling point among the vapor phase components passing through the glass fiber filter is collected by the filter. There is a problem. On the other hand, in the analysis of the middle and high boiling point components, there is a problem that the unstable smoke component changes because the components are collected in the glass fiber filter.

In the analysis of tobacco smoke, it is desirable to analyze the smoke that actually enters the mouth of the smoker, that is, in a fresh state immediately after combustion, but there has been no analysis system that can achieve this.

The present invention has been made in view of such a viewpoint, and an object of the present invention is to provide a device capable of introducing smoke into an analyzer so that smoke immediately after combustion can be analyzed as it is.

[Means for Solving the Problems] In order to achieve the above object, in the cigarette smoke introduction device of the present invention, the outer cylinder provided with the parallel top plate and the bottom plate, and the top plate and the bottom plate A rotor housed in the outer cylinder so as to be rotatable about a vertical axis, and first and second axial through holes formed in the rotor on the same radius with respect to the rotation axis; A carrier gas line connected to the top plate and the bottom plate so as to pass through the first through hole in a series, and the carrier gas line is a part of a line connecting a carrier gas source and a tobacco smoke analyzer. And that the smoking line is connected to the top plate and the bottom plate so as to pass through the second through-hole uniformly, and the smoking line is a part of a line connecting the tobacco sample and the smoker. A position where the second through hole is aligned with the smoking line, and Rotating the rotor so as to reciprocate between the rear gas line and a position where the rear gas line is aligned.

In a preferred embodiment, the rotor is driven to rotate by an actuator connected to the rotation shaft.

[Operation] According to the tobacco smoke introducing apparatus according to the present invention, the carrier gas is flowed to the analyzer through the first through hole of the introducing apparatus before the predetermined number of smoking times of the tobacco sample. On the other hand,
The tobacco sample is attached to the smoking line prior to the predetermined number of times of smoking. Then, a predetermined number of times of smoking is performed by the smoker, and only the smoke of the predetermined number of times of smoking is filled in the second through-hole of the introduction device.

From this state, when the rotor of the introduction device is rotated to reach a position where the second through-hole is aligned with the carrier gas line, the tobacco smoke inside the second through-hole is carried by the carrier gas and enters the analyzer. be introduced. Thereafter, when the required amount of tobacco smoke has been introduced into the analyzer, the rotor is rotated in the opposite direction and returned to the original position where the second through-hole is aligned with the smoking line.

Embodiment FIG. 1 is a diagram showing an entire system incorporating a tobacco smoke introducing apparatus and an analyzing apparatus according to the present invention.
As shown in FIG. 2, the analyzer has two gas chromatographs (hereinafter abbreviated as GC) 12 and 14 each having a known predetermined function (for example, a heating and temperature control mechanism), as shown in FIG.
Both are connected by a connector 16 that connects the respective lines 22.

The first GC 12 has an inert carrier gas (H in this embodiment)
e) Split / splitless injection block 18 for introducing tobacco smoke as a sample gas together with e)
Is arranged. A first sample gas line 22 extends from the injection block 18 into the vessel, where the first sample gas line 22 is first placed.
A column 24 is provided. The first column 24 is set for analysis of middle and high boiling components, and the first GC has a temperature control mechanism (not shown) in the vessel.

A second sample gas line 26 is connected to the first line 22 downstream of the first column 24. The second line 26 is provided with a third column 28 which is a pressure control member.
A first detector 32 is disposed on the second line 26 downstream of the first detector 32. The third column 28 is not for analysis, but is for maintaining the flow rate in the system constant when the flow of the sample gas is switched in a manner described later, so that the pressure loss is equal to that of the second column 38 described later. Is set to Therefore, it is also possible to use a member such as a resistance line member (without mixing) instead of the column as shown.

An inert gas (He) supply first switching line 34 is connected to the second line 26 upstream of the third column 28. line
34 is connected to a predetermined gas source (not shown), and an electromagnetic valve V3 is interposed here.

A second switching line 36 for supplying an inert gas (He) is connected to the first line 22 downstream of the connection position of the second line 26. Line 36 is connected to a predetermined gas source (not shown),
Here, an electromagnetic valve V4 is provided.

Downstream from the connection position of the second switching line 36, the first GC12
The line 22 of the second GC 14 is connected to the line 22 of the second GC 14 by the connector 16.
Is linked to

The second GC 14 is provided with a second column 38. 2nd column 3
8 is set for vapor phase component analysis, and the second GC 14 has an internal temperature control mechanism (not shown). Further, a second detector 42 is provided in the first line 22 downstream of the second column 38.

A tobacco smoke introduction device 52 is connected to the injection block 18 of the first GC 12 outside the device via a line 56. FIG. 3 is a vertical sectional side view showing the introduction device 52, and FIG.
The figure is a plan view thereof.

The introduction device 52 includes a cylindrical outer cylinder 84 attached to the frame 82, and a rotor 86 held in the outer cylinder 84. Outer cylinder
The top and bottom of 84 are a top plate 88 screwed to the outer cylinder 84,
Each is closed by a bottom plate 92. A packing 94 for sealing is provided between the top plate 88 and the bottom plate 92 and the outer cylinder 84 and the rotor 86.

The outer cylinder 84 has heaters 102 at positions shifted by 180 °.
And a temperature sensor 104. The heater 102 and the temperature sensor 104 are connected to a temperature controller 58 outside the introduction device 52 as shown in FIG.

The rotor 86 has two through holes 9 of the same size extending in the axial direction.
6, 98 are formed. The two holes 96 and 98 are arranged at the same radius on the rotor 86 and at positions shifted by 90 degrees.
The top plate 88 and the packing 94 adjacent to the top plate 88 are formed with ports 96s that align with the through holes 96 and ports 98s that align with the through holes 98 at normal times. On the other hand, the bottom plate 92 and the packing 94 adjacent thereto are formed with a port 96d that aligns with the through hole 96 and a port 98d that aligns with the through hole 98 at normal times.

The port 96s of the top plate 88 is connected to the carrier gas line 54b, and the port 96d of the bottom plate 92 is connected to the line 56 communicating with the injection block 18 of the first GC 12. As shown in FIG. 1, a carrier gas (He in this embodiment) is drawn from a gas source by a line 54, and is branched into lines 54a and 54b in a three-way solenoid valve V1. Line 54a is connected directly to the injection block 18, while line 54b
Is connected to port 96s as described above.

The port 98s of the top plate 88 is connected to the suction holder 64, and the bottom plate 9
Connected to line 66 which communicates with 8d smoker 68. holder
A tobacco sample 62 is attached to 64 as shown in FIG.

The shaft shaft 72 of the rotor 86 is integrated with the rotating shaft of the pneumatic actuator 74 on the upper side. For the actuator 74, a pressurized air line 76 is provided in a known manner.
a and 76b are connected so that the rotation direction of the shaft can be selected by using one of the lines. In the present embodiment, the actuator 74 rotates the rotor 86 of the introduction device 52 in both directions within an angle range of 90 ° in the following manner. Pressurized air is drawn from the air source by a line 76, and a three-way solenoid valve V2 supplies
Branched to 6b.

For example, in the state shown in FIG. 4, when pressurized air is supplied to the actuator 74 via the line 76a, the actuator 74 rotates the rotor 86 in the direction of arrow A in FIG. Therefore, the through hole 98 of the rotor 86 is aligned with the ports 96s and 96d, and the line 54 connected to the ports 96s and 96d is
b, communicate with 56. By this operation, the tobacco smoke filled in the through-hole 98 at the previous stage, which was in alignment with the holder 64 and the smoker line 66, is transferred to the carrier gas (He) passing through the lines 54b and 56.
Is introduced into the injection block 18 of the first GC 12. Conversely, when pressurized air is supplied to the actuator 74 via the line 76b from this state, the actuator 74 rotates the rotor 86 in the direction of arrow B in FIG. 4 to return to the original position.

Control of the valves V1, V2 and the smoking device 68 is controlled by the controller 44.
The operation signal is transmitted through the relay box 46. Also valve V
3. Control of V4 is performed by the event program of the control mechanism built in the GC12. The control mechanism of the GCs 12, 14 is linked with the controller 44.

 Next, an outline of the operation of the above system will be described.

First, a temperature raising program for the GCs 12 and 14 is started (provided that an initial set temperature (for example, 40 ° C.) is obtained). Further, the tobacco sample 62 is attached to the smoking device 68 (or another smoking device) without passing through the introduction device 52 to start the smoking device and ignite the tobacco sample 62.

Prior to the predetermined number of times of smoking (for example, the fifth time), the tobacco sample 62 is transferred to the holder 64 above the introduction device 52 to be in the state shown in FIG. Then, the smoker 68 causes the through-hole 98 of the introduction device 52 to fill only the smoke of the predetermined number of times of smoking.

On the other hand, the carrier gas (He) does not first pass through the introduction device 52, but directly through the line 54a.
Pour into 8. Then, as described above, prior to the predetermined number of times of smoking of the tobacco sample 62, V1 is switched, and the carrier gas is supplied from the line 54b to the through hole 96 of the introduction device 52 and the line 56.
To the injection block 18 via.

At the same time as the switching of V1, V3 is opened and V4 is closed, and He gas is introduced from line 34 into the first line 22 of the first GC 12. Thereby, the setting is made so that the sample gas flows to the second column 38 in the second GC 14.

Here, a predetermined number of times of smoking is performed, and the through hole 98 of the introduction device 52 is filled with tobacco smoke. And switch V2,
By the actuator 74, the rotor 86 of the introduction device 52 is
It is rotated in the direction of arrow A in FIG. As a result, the through-hole 98 communicates with the carrier gas line 54b, and the tobacco smoke inside the through-hole 98 is carried by the carrier gas and the first GC 12
Introduced in line 22. The flow of each gas at this time is indicated by a white arrow in FIG.

After a predetermined amount of tobacco smoke has been introduced into the first GC 12, V1 is switched so that the carrier gas again flows directly to the injection block 18 via the line 54a. Immediately thereafter, V2 is switched, and the rotor 86 is rotated in the direction of arrow B in FIG. 4 by the actuator 74 to return the rotor 86 to the original position shown in FIG.

Subsequently, without attaching a cigarette to the holder 64, empty smoking is performed by the smoker 68, and the tobacco smoke through hole 98 of the rotor 86 is cleaned.

In the first GC 12, the sample gas is separated by a first column 24 for analysis of middle and high boiling components, and first, its vapor phase component comes out of the column 24. This vapor phase component is
In the second GC 14, the separation is further clearly performed in the second column 38, and the analysis result is obtained by the second detector 42.

However, since the second column 38 of the second GC 14 is set for use as a vapor phase component, it is impossible to flow the middle and high boiling components coming out of the column 24 following the vapor phase component to the second column 38. This is because, as described above, the middle and high boiling components adhere to the inside of the column 38, making the column unusable.

Therefore, at the point when the medium-to-high boiling point component comes out of the first column 24 (for example, measuring the time when toluene comes out in the preliminary test), V3 is closed and V4 is switched to the open state, and the line
Instead of 34, this time He gas is introduced from the line 36 into the first line 22. By this operation, the sample gas changes its flow according to the flow of the introduced He gas from the line 36,
It starts flowing to line 26. Then, the sample gas passes through the third column 28 which is a pressure control member, and the analysis result in a state where the sample gas is separated by the first column 24 is obtained by the first detector 32. The flow of each gas at this time is indicated by black arrows in FIG.

Example 1 The system shown in FIG. 1 was set under various conditions described below, and a cigarette smoke analysis experiment was performed. The gas chromatograph used was Shimadzu GC-14A (with detector).
These were set as the first and second GCs 12, 14 under the conditions shown in Tables 1 and 2.

Control of the valves V1, V2 and the smoking device 68 is controlled by the controller 44.
The operation signal was transmitted through the relay box 46. On the other hand, valves V3 and V4
Was controlled by an event program of a control mechanism built in the GC12. The temperature of the introduction device 52 was previously set to 100 ° C.

As the smoking device 68, a device having a mechanism capable of repeating smoking at a rate of 35 ml / time for 2 seconds at intervals of at least one minute under standard smoking conditions was used.

The controller 44 used was Shimadzu CR4A, GC12
And has the function of processing and storing the data obtained from 14 and 14, and controls the tobacco smoke analysis system by an event program.

Table 3 shows a time program when a part of tobacco smoke in the latter half of 2 seconds was introduced into the first and second GCs 12 and 14 and analyzed at the time of the fifth smoking.

[Effects of the Invention] According to the tobacco smoke introduction device according to the present invention, the vapor phase component and the middle and high boiling components of tobacco smoke immediately after combustion are simultaneously supplied to the analyzer in a fresh state that enters the actual smoker's mouth. Can be introduced. Here, it is not necessary to separate the components by filtering the tobacco smoke with a glass fiber filter, collecting the medium- and high-boiling components on the filter, and passing the vapor-phase components as in the related art. Therefore, troublesome procedures involved are not required, and a decrease in the analysis accuracy due to the partial collection of the vapor phase component on the filter and the deterioration of the medium and high boiling components during re-evaporation can be prevented. Become like In addition, by combining with a smoker as shown in the illustrated embodiment, only smoke from a predetermined number of times of smoking can be reliably introduced into the analyzer.

[Brief description of the drawings]

FIG. 1 is a diagram showing an entire system incorporating a tobacco smoke introducing apparatus and an analyzing apparatus according to the present invention. FIG. 2 is a diagram showing a gas flow in the tobacco smoke analyzer. FIG. 3 is a vertical sectional side view showing the introduction device, and FIG. 4 is a plan view thereof. 12, 14… GC, 22, 26 …… Sample gas line, 24, 2
8, 38 …… Column, 32, 42 …… Detector, 34, 36 ……
Inert gas line, 44 …… Controller, 46 …… Relay box, 52 …… Introduction device, 58 …… Temperature regulator, 62 ……
Tobacco sample, 68 smoking device, 84 outer cylinder, 86 rotor, 88 top plate, 92 bottom plate, 96, 98 through holes.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Hideki Takahashi 6-2, Umegaoka, Midori-ku, Yokohama-shi, Kanagawa Prefecture Inside the Tobacco Central Research Laboratories of Tobacco Inc. (72) Inventor Atsuko Akagi 5 Dobashi, Miyamae-ku, Kawasaki-shi -6-1 (72) Inventor Masahiro Kawai 2-17-36 Sakaecho, Fuchu-shi, Tokyo (56) References JP-A-1-112974 (JP, A) JP-A-60-76641 (JP, A) (58) ) Surveyed field (Int.Cl. ⁷ , DB name) G01N 1/00-1/02 G01N 30/04

Claims (2)

(57) [Claims] 1. A tobacco smoke introducing device for introducing a sample of tobacco smoke into a tobacco smoke analyzer, comprising: an outer cylinder provided with a parallel top plate and a bottom plate; A rotor housed in the outer cylinder so as to be rotatable about a vertical axis, first and second axial through holes formed in the rotor on the same radius with respect to the rotation axis; A carrier gas line connected to the top plate and the bottom plate so as to pass through the first through hole in a series, and the carrier gas line is a part of a line connecting a carrier gas source and the tobacco smoke analyzer. And a smoking line connected to the top plate and the bottom plate so as to pass through the second through-hole uniformly, and the smoking line is a part of a line connecting the tobacco sample and the smoking device. In cooperation with the carrier gas source and the smoking device A controller for controlling the operation of the tobacco smoke introduction device, the controller comprising: a controller configured to rotate the rotor at a position where the first and second through holes are aligned with the carrier line and the smoking line, respectively. And an initial step of supplying a carrier gas from the carrier gas source to the carrier line, and while the state of the initial step is maintained, the tobacco smoke from the tobacco sample is smoked by the smoking device. A filling step of filling the inside of the second through-hole; rotating the rotor immediately after the filling step, and stopping the rotor at a position where the second through-hole is aligned with the carrier gas line. An introduction step of carrying the tobacco smoke in the second through hole by the carrier gas and introducing it into the tobacco smoke analyzer; And a return step of rotating the rotor to stop the rotor at a position where the first and second through-holes are aligned with the carrier line and the smoking line, respectively. A cigarette smoke introduction device characterized by the following. 2. The apparatus according to claim 1, wherein said rotor is reciprocally moved by a pneumatic actuator connected to a rotating shaft of said rotor.