JP5287320B2 - Odor measuring device - Google Patents

Description

  The present invention relates to an odor measuring apparatus capable of performing determination and evaluation by a measurer smelling an odor component in a sample.

  In order to analyze an odor component in a sample, analyzers such as a gas chromatograph (GC) and a gas chromatograph mass spectrometer (GC / MS) are widely used. Such an analyzer detects substances that cannot be felt by the human sense of smell, so it is necessary to actually determine whether or not the components separated by the column smell. For this purpose, GC and GC / MS (referred to as “sniffing GC” in this specification, but sometimes referred to as sniffing GC, etc.) having an odor sniffing port are conventionally known ( (See Patent Documents 1 and 2, Non-Patent Documents 1 and 2).

  FIG. 2 is a schematic flow path configuration diagram of the sniffing GC described in Patent Document 1. In this sniffing GC, the carrier gas supplied from the carrier gas cylinder 1 is regulated to a predetermined gas pressure by the pressure regulating unit 2 and flows to the column 4 through the sample introduction unit 3 such as a sample vaporizing chamber. Then, the carrier gas exits from the column 4 and passes through the main flow path 7 and is introduced into a detector 5 such as a mass spectrometer. At the end of the sub flow path 8 branched from the main flow path 7 by the splitter 6 provided at the outlet of the column 4, an odor sniffing port 9 is provided.

  The smell sniffing port 9 is a funnel-shaped instrument for detecting an odor component by the sense of smell of the measurer. The measurer sniffs the gas discharged from the smell sniffing port 9, but when the measurer takes almost the same time to inhale and exhale, it takes about half of the time to smell. It is a dead period that cannot be felt. The number of normal breaths at rest is said to be about 12-20 times per minute for adults, and the respiratory cycle is 3-5 seconds. Of these, for about 1.5 to 2.5 seconds, which is about half, gas is released from the smell sniffing port 9, but the measurer cannot sniff. Therefore, the odor component contained in the gas released at this time may cause the detection of smell sniffing.

  These problems include, for example, (1) how to breathe so as to shorten the time when the measurer exhales, and (2) the timing when the measurer smells while looking at the detection results (chromatogram, etc.) by the detector. A certain degree of improvement can be expected by taking measures such as In order to assist the method (2), in the apparatus described in Patent Document 2, when a peak appears on the chromatogram obtained by the detector, the measurement person is notified by display or voice. Yes.

  However, since the time for the measurer to exhale cannot be zero in the first place, it is difficult to completely eliminate the detection of the odor component. Further, depending on the odor component, there may be a case where a peak does not appear in the detection result of the detector, but in the method (2), in such a case, detection is missed. In addition, any of the methods described above places excessive tension or psychological burden on the operator, which may affect accurate judgment.

Japanese Patent Laying-Open No. 2005-274416 (FIG. 2, paragraphs [0002]-[0003]) JP 2008-170333 A

“Introduction and application of gestell scent device”, [online], Agilent Technologies, Inc. [Search February 5, 2009], Internet <URL: http://www.chem-agilent.com/appnote /applinote.php?pubno=MS-200711-004p> "GC-O System Sniffer9000", [online], Prime Tech Co., Ltd. [Search February 5, 2009], Internet <URL: http://www.primetech.co.jp/search/detail.asp? pid = 30002>

  The present invention has been made in order to solve the above-mentioned problems, and the object of the present invention is to prevent the measurer from sniffing the odor components separated by the column and place an excessive burden on the measurer. An object of the present invention is to provide an odor measuring apparatus having a smell sniffing function that can avoid this.

In order to solve the above problems, the present invention includes a separation unit that separates various odor components in a sample gas in a time direction, and a gas discharge for a measurer to smell the odor components separated by the separation unit. In an odor measuring apparatus comprising a discharge port,
a) After the gas continuously supplied during the predetermined period including the odor component separated by the separation unit is stored in the gas reservoir, the gas is delivered to the discharge port during a period shorter than the predetermined period. by the intermittent supply gas discharging control means of the gas which is continuously fed through the separation unit prior Symbol discharge port,
b) Notification that notifies the measurer synchronized with the intermittent gas discharge so that the measurer can breathe in accordance with the intermittent gas discharge period from the discharge port by the gas discharge control means. Means,
It is characterized by having.

  The separation unit is typically a chromatographic column, but depending on the type of odor component, a collection tube using a heat desorption method can also be used.

  In the odor measuring apparatus according to the present invention, the gas containing the odor component separated in time by the separation unit is continuously supplied to the gas discharge control means. Usually, a gas emitted from a separation unit such as a column is branched into a plurality by a splitter, one is introduced into a detector such as a mass spectrometer, and the other is supplied to a gas discharge control means. Therefore, the gas supplied to the gas discharge control means is a part of the gas emitted from the separation unit, but the supply is continuous in time.

Gas discharge control means compressed gas is continuously supplied, as described above, intermittently supplied to the discharge port at a predetermined period. In general, this period is set to a period that is comfortable for the measurer to breathe. Therefore, gas is discharged from the discharge port for a certain period, and gas discharge is stopped for the next certain period. The notification means notifies by display, sound, vibration, etc. so as to indicate the timing at which gas is discharged from the discharge port or the discharge stops. The measurer breathes in accordance with this notification, so that the gas can be sucked when the gas is discharged from the discharge port, and can be exhaled when the gas discharge is stopped.

In odor measuring device according to the present invention, the gas discharge control means, after the reservoir gas is continuously supplied for a predetermined period including the separated odor components in the separation section, from the gas the predetermined period gas reservoir and sends the to the discharge port even during a short period, i.e. that having a kind of buffer. As the gas reservoir, for example, a syringe capable of sucking and discharging gas by driving a plunger can be used.

Further, since the gas containing the odor component separated by the separation unit is supplied even during the period in which the gas is delivered from the gas reservoir to the discharge port, it is necessary to prevent the gas from escaping. Therefore, the gas discharge control means is an auxiliary gas that temporarily stores the gas that is continuously supplied including the odor component separated by the separation unit during the period in which the gas is delivered from the gas reservoir to the discharge port. It is good to set it as the structure which has a reservoir in the front | former stage of the said gas reservoir. That is, it is possible to by the configuration of connecting a buffer for storing the gas in series to rather compress a leakage gas is continuously supplied.

As another configuration, connects the buffer for storing the gas in parallel, to perform sending the other buffer to the compressed gas to the discharge port, the operation of alternately while accumulated gas into one buffer It can also be considered.

The human respiratory cycle varies from person to person. Further, if the components in the gas when compressed gas is continuously supplied is mixed, the period clogging of intermittent gas delivery would be decided detection resolution of odor component with a period of respiration. Therefore, in the odor measuring apparatus according to the present invention, the measurement person adjusts at least one of the intermittent gas discharge period, the gas discharge period, and the gas discharge stop period from the discharge port by the gas discharge control means. It is preferable to further include an instruction unit.

  With this configuration, the measurer appropriately adjusts the intermittent gas discharge period so that his / her breathing is not excessive, or the separation performance of the odor component in the separation unit is poor (temporarily adjacent two in time) When the time interval of the odor component is narrow), the intermittent gas discharge cycle can be adjusted to be short.

  According to the odor measuring apparatus of the present invention, gas is discharged from the discharge port (smell sniffing port) only when the measurer inhales, and all odor components contained in the original sample gas are discharged from the discharge port. Since it is contained in the exhaled gas, it is possible to prevent the smell of odor components from being leaked by the measurer. In addition, the measurer only needs to breathe in accordance with the notification from the device, and it is guaranteed that there is no need to smell the breathing period, so there is excessive tension and psychological burden on the measurer. Will not be forced. Conventionally, the measurer has required a certain degree of experience and training to perform breathing appropriate for the measurement. However, according to the present invention, even an inexperienced person can perform an appropriate measurement. It is advantageous for cost reduction.

BRIEF DESCRIPTION OF THE DRAWINGS The schematic block diagram of the smell smell part in the smell measuring apparatus which is one Example of this invention. The general | schematic channel block diagram of a general smell sniffing GC. The schematic timing diagram which shows operation | movement of each part of the smell smell part of FIG.

Hereinafter, an odor measuring apparatus according to an embodiment of the present invention will be described with reference to the accompanying drawings.
The basic configuration of the odor measuring apparatus of the present embodiment is as shown in FIG. 2 described above, and the odor sniffing part A indicated by a dotted line in FIG. 2 has a characteristic configuration shown in FIG. That is, FIG. 1 is a schematic configuration diagram of an odor sniffer in the odor measuring apparatus of the present embodiment.

  In FIG. 1, a first three-way joint 10, a first valve 13, and a second three-way are provided in a sub-flow channel 8 through which a sample gas from a column outlet (not shown) flows by being branched by a splitter 6. A joint 14 and a second valve 15 are provided. A syringe-like first syringe 11 is connected to the auxiliary flow path 8 by the first three-way joint 10, and a second syringe 16 is connected to the auxiliary flow path 8 by the second three-way joint 14. In the first syringe 11, the plunger 11 a inserted in the barrel is pressed by an appropriate external pressure (for example, atmospheric pressure), and the plunger 11 a slides according to the relationship between the external pressure and the internal pressure of the barrel. The first syringe 11 is provided with a top dead center sensor 12 for detecting that the plunger 11a has reached the top dead center. On the other hand, in the second syringe 16, the plunger 16a is reciprocally driven in the barrel by a drive source 17 including a motor or the like.

  The control unit 20 including a CPU, a ROM, a RAM, and the like receives a detection signal from the top dead center sensor 12, opens and closes the first valve 13 and the second valve 15, and controls the plunger 16 a by the drive source 17. Control each sliding operation. Further, the control unit 20 sends a control signal to the breathing instruction unit 21 including a display unit 22 such as a lamp, a voice output unit 23, and the like. The control unit 20 achieves control as described later by operating a control program stored in advance in a ROM or the like on the CPU.

  In the odor measuring apparatus according to the present embodiment, when a sample to be measured is introduced into the carrier gas by the sample introduction unit 3, the gas vaporized from the sample is carried into the column 4 along the carrier gas flow, and the column 4 The various odor components (gas components) in the gas are separated in the time direction and flow out of the column 4 while passing through the column 4. The operation of the smell sniffing part when the sample gas containing the separated odor component is continuously supplied to the sub-channel 8 will be described with reference to FIG. FIG. 3 is a schematic timing chart showing the operation of each part of the smell sniffer shown in FIG.

  In a state where the sample gas is continuously supplied from the splitter 6 to the sub-channel 8, the control unit 20 closes the first valve 13 at time t1. At this time, as will be described later, almost no gas remains in the first syringe 11, and the plunger 11a is at the bottom dead center position. Since the pressure of the sample gas flowing through the auxiliary flow path 8 is higher than the external force applied to the plunger 11a of the first syringe 11, the sample gas flows into the barrel of the first syringe 11 while pushing up the plunger 11a. Thereby, the internal volume (sample gas amount) of the first syringe 11 increases as shown in FIG. When the first syringe 11 is filled with the sample gas at time t2, the plunger 11a reaches the top dead center, which is detected by the top dead center sensor 12.

  Upon receiving a detection signal from the top dead center sensor 12 as shown in FIG. 3D, the control unit 20 closes the second valve 15 and opens the first valve 13. Thereby, the auxiliary flow path 8 from the splitter 6 to the second syringe 16 is connected. Furthermore, the control unit 20 controls the drive source 17 so as to pull out the plunger 16a of the second syringe 16 in the pushed state at a predetermined constant speed. As the plunger 16 a is pulled out, the sample gas accumulated in the first syringe 11 until just before that and the sample gas newly flowing into the auxiliary flow path 8 from the splitter 6 are sucked into the second syringe 16. As a result, the internal volume (sample gas amount) of the second syringe 16 increases as shown in FIG. On the other hand, as the sample gas in the first syringe 11 is sucked, the plunger 11a is drawn into the barrel so as to be balanced with the sample gas, and its internal volume (sample gas amount) decreases as shown in FIG. To do.

  If the control unit 20 controls the drive source 17 so as to pull out the plunger 16a for a predetermined time T2, the first valve 13 is closed while the second valve 15 is opened at time t3. Thereby, the flow path connecting the splitter 6 and the first syringe 11 and the second syringe 16 is blocked, while the second syringe 16 and the sniffing port 9 are connected. Then, the control unit 20 controls the drive source 17 so as to push the plunger 16a of the second syringe 16 into the barrel at a predetermined constant speed. Then, the sample gas accumulated in the second syringe 16 immediately before that is pushed out and discharged from the sniffing port 9 through the second valve 15 as shown in FIG.

  Time t3 is the same as time t1 in terms of control operation. That is, at the time t3, the sample gas is no longer in the first syringe 11 due to the suction by the second syringe 16 immediately before that, and the first valve 13 is closed at the time t3, and at the same time, supplied through the splitter 6 The new sample gas thus added starts to accumulate in the first syringe 11.

  As shown in FIGS. 3B, 3E, and 3G, the discharge of the sample gas from the sniffing port 9 is stopped while the second valve 15 is closed, and the second valve 15 is opened, During the period in which the plunger 16a of the second syringe 16 is being pushed in, the sample gas is discharged from the sniffing port 9. The sample gas discharged from the sniffing port 9 after time t3 is the sample gas supplied to the sub-flow channel 8 through the splitter 6 during the period T immediately before it. That is, the discharge of the sample gas from the smell sniffing port 9 is intermittent with periodicity, but part of the sample gas continuously supplied from the splitter 6 to the sub-channel 8 is not wasted. All are used for discharge from the sniffing port 9. Therefore, all odor components contained in the sample gas are discharged from the odor sniffing port 9.

  As described above, the control unit 20 controls the opening / closing operation of the two valves 13 and 15 and the driving of the plunger 16a of the second syringe 16 to thereby intermittently and periodically discharge the sample gas from the odor sniffing port 9. In synchronization with this, for example, the lamp of the display unit 22 is turned on during the discharge period T1 to inform the measurer in real time of the sample gas discharge period T1 and the discharge stop period T2. In period T2, a control signal is sent to turn off the lamp. Further, the sound output unit 23 may be controlled to output a notification sound that informs the sample gas discharge period and the discharge stop period. Of course, instead of simply turning on / off the lamp, a display mode may be used in which the position of the elapsed time in each of the sample gas discharge period T1 and the discharge stop period T2 is notified more finely.

  The measurer who smells smells his / her breathing cycle so that he / she inhales during the sample gas discharge period T1 and exhales during the sample gas discharge stop period T2 by watching this display or listening to the notification sound. Match the cycle of intermittent discharge of sample gas. Then, the measurer judges the presence or absence of the odor when sucking the sample gas discharged from the odor sniffing port 9, and records the scent sensory strength and the odor. In parallel with the smell sniffing measurement by such a measurer, the detection of the odor component for the same sample gas is executed by the detector 5, and the result is represented by, for example, a chromatogram, a mass spectrum, a mass chromatogram or the like. By combining these chemical analysis results with the smell smell measurement results by the measurer, identification and evaluation of odor components in the sample are performed.

  As described above, the general human breathing cycle is 3 to 5 seconds, and if the cycle of intermittent discharge of the sample gas is adjusted to this, breathing without difficulty is possible. Of course, since there are individual differences in the respiratory cycle, it is preferable that the sample gas discharge period and the discharge stop period can be adjusted within an appropriate range. The time of the discharge stop period can be adjusted, for example, by adjusting the position of the top dead center of the first syringe 11 or the flow rate of the sample gas supplied from the splitter 6 to the sub-flow channel 8. On the other hand, the time of the discharge period can be adjusted by the pushing speed of the plunger 16a of the second syringe 16, for example. Therefore, it is preferable to provide an input unit for the measurer to set each time and cycle, and to provide a function for adjusting the above elements according to the time and cycle set from the input unit. Thereby, for example, the measurer can adjust the cycle of intermittent discharge of the sample gas to the natural breathing cycle.

  As described above, in this smell sniffing part, the components supplied during the period T shown in FIG. 3 are mixed in the second syringe 16, so that the two odor components adjacent in time separated by the column 4 are mixed. If the time interval is shorter than the respiratory cycle, they may be mixed and discharged from the sniffing port 9. That is, the time resolution of the sniff measurement is determined by the intermittent discharge cycle of the sample gas. Therefore, it is conceivable to limit the maximum time of the intermittent ejection cycle so that the intermittent ejection cycle is shorter than the time interval at which two components that are temporally adjacent on the chromatogram appear. Of course, such a restriction is unnecessary if the separation performance of the column 4 is sufficiently high.

  In the above embodiment, only the sample gas is discharged during the gas discharge period from the smell sniffing port 9, but the time during which the sample gas is pushed out from the second syringe 16 and discharged from the sniffing port 9 is further compressed, and the sample gas is discharged. You may make it discharge the gas for purifying the inside of a clean air or a nostril continuously after exhaling. That is, the sample gas is exhaled from the sniffing port 9 in the first half of the period when the measurer inhales, and clean air or cleaning gas is exhaled from the sniffing port 9 in the second half of the period of inhaling breath. During the period in which the measurer exhales, the gas ejection may be stopped, or clean air or purified gas may be exhaled in the same manner as in the above embodiment. Since the nostril of the measurer is washed with clean air or clean gas, it is expected that the burden on the nose will be reduced and the accuracy of smell sniffing will be increased.

  Moreover, in the said Example, when connecting the 1st syringe 11 and the 2nd syringe 16 in series to the single subchannel 8, and discharging the sample gas from the 2nd syringe 16, the 1st stage of the front | former stage is carried out. The sample gas newly supplied to the syringe 11 was stored. A function similar to this is that two syringes are arranged in parallel, and when the sample gas is discharged from one syringe to the sniffing port, the sample gas newly supplied to the other syringe is stored. It is obvious that the operation can be realized by alternately performing the operations. However, in this case, it is necessary to forcibly drive the plunger with a motor or the like for both of the two syringes.

  Further, the above-described embodiment is an example of the present invention, and it is apparent that the present invention is encompassed in the scope of claims of the present application even if appropriate modifications, corrections and additions are made within the scope of the present invention.

DESCRIPTION OF SYMBOLS 1 ... Carrier gas cylinder 2 ... Pressure regulation part 3 ... Sample introduction part 4 ... Column 5 ... Detector 6 ... Splitter 7 ... Main flow path 8 ... Sub flow path 9 ... Smell sniffing port 10 ... 1st three-way joint 11 ... 1st syringe 11a ... plunger 12 ... top dead center sensor 13 ... first valve 14 ... second three-way joint 15 ... second valve 16 ... second syringe 16a ... plunger 17 ... drive source 20 ... control unit 21 ... breathing instruction unit 22 ... display unit 23 ... Audio output part

Claims (3)

In an odor measurement apparatus comprising: a separation unit that separates various odor components in a sample gas in a time direction; and a discharge port through which gas is discharged so that a measurer can smell the odor component separated by the separation unit.
a) After the gas continuously supplied during the predetermined period including the odor component separated by the separation unit is stored in the gas reservoir, the gas is delivered to the discharge port during a period shorter than the predetermined period. by the intermittent supply gas discharging control means of the gas which is continuously fed through the separation unit prior Symbol discharge port,
b) Notification that notifies the measurer synchronized with the intermittent gas discharge so that the measurer can breathe in accordance with the intermittent gas discharge period from the discharge port by the gas discharge control means. Means,
An odor measuring apparatus comprising: The odor measuring device according to claim 1 ,
The gas discharge control means is an auxiliary for temporarily storing a gas continuously supplied including an odor component separated by the separation unit during a period in which the gas is sent from the gas reservoir to the discharge port. An odor measuring apparatus having a gas reservoir in a stage preceding the gas reservoir. The odor measuring device according to claim 1 or 2 ,
The apparatus further comprises an adjustment instruction means for the measurer to adjust at least one of a period of intermittent gas discharge from the discharge port by the gas discharge control means, a gas discharge period, or a gas discharge stop period. Odor measuring device.

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