JPH10319002A - Exhalation analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To properly and speedily execute countermeasure against contamination and degradation of a column or a detector. SOLUTION: An exhalation analyzer 10 is provided with a column 12 for separating a component included in an exhalation A, a detector 14 for detecting the separated component, a carrier gas solenoid valve 16C for supplying a carrier gas C, a standard gas solenoid valve 16S for supplying a standard gas S, and a control part 18 for controlling operations of the detector 14, the carrier gas solenoid valve 16C, and the standard gas solenoid valve 16S. The control part 18 supplies the carrier gas C to the column 12 and the detector 14 via the carrier gas solenoid valve 16C every time a given time has elapsed or a given analysis count has ended, thereby sensitivity of the detector 14 is inspected, the standard gas S is supplied to the column 12 and the detector 14 via the standard gas solenoid valve 16S, and thereby degree of separation of the column 12 is inspected.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a breath analysis apparatus for analyzing components contained in breath in the medical field, health industry, drunk driving control, drug investigation, and the like.

[0002]

2. Description of the Related Art Conventionally, as described in, for example, JP-A-6-58919, a breath analyzer for collecting and analyzing the breath of a subject has been developed. Breath analyzers are used to analyze breaths for clinical tests in the medical field, monitor patient conditions, measure the working environment and indoor environment in the industrial field, control drunk driving and drugs in the police field, and cause fires in the firefighting field. It is used in a wide range of fields, such as research and health management in the health industry field.

[0003] This breath analyzer uses gas chromatography. The breath analyzer is attached to the main body of the breath analyzer and has an outer peripheral portion covered with a heater. Two carrier gas flow paths respectively connected via a four-way electromagnetic valve, an air cylinder connected to the four-way electromagnetic valve, and a sample measuring section provided in a part of each carrier gas flow path. I have.

[0004] On the downstream side of each sample measuring section, a breathing introduction pump (suction pump) connected via a three-way electromagnetic valve and an exhaust pipe is provided. In addition, two separate columns and the like are connected to the three-way electromagnetic valves described above in parallel and independently of each other.

[0005] In the case of collecting and analyzing exhaled breath from a subject, when the subject exhales into the exhalation collection tube, the exhaled breath is discharged into the exhalation collection tube by the exhalation introduction pump. Exhaled air fills each sample weighing section while being discharged out of the device. Next, when a carrier gas is sent from an air cylinder to each sample measuring section, the exhaled air filled in each measuring section is sent to each separation column, and then each exhaled air is separated by a difference in retention time of each component gas. You. Thereafter, a signal corresponding to each component gas is output from the detector.

Conventionally, an operator has dealt with contamination or deterioration of a column or a detector as follows. First,
Based on the analysis results, it is determined whether the resolution of the column has decreased or the sensitivity of the detector has decreased. If this decrease in the degree of separation or sensitivity is recognized, the temperature and time for conditioning are determined, a conditioning program is input, and conditioning is started. After the conditioning, the standard gas is analyzed this time to judge again whether the column resolution or the sensitivity of the detector has decreased. If no improvement is observed in the degree of separation or sensitivity, it is determined that the column or the detector may have deteriorated.

[0007]

However, the conventional breath analyzer has the following problems because all measures for contamination or deterioration of the column or the detector are manually performed.

[0008] The judgment of contamination / deterioration is extremely delicate,
It depends entirely on the operator's experience and intuition. Therefore, if the operator is unfamiliar, the operator may not notice contamination or deterioration, and in such a case, the analysis accuracy is reduced.

[0009] Since the treatment for contamination and deterioration is troublesome as a whole, the workability has been reduced.

[0010]

SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide a breath analyzer which can carry out a corrective and quick treatment for contamination or deterioration of a column or a detector.

[0011]

A breath analyzer according to the present invention comprises a column for separating components contained in the breath by passing the breath, a detector for detecting the components separated by the column, A carrier gas solenoid valve for supplying a carrier gas to the column and the detector, a standard gas solenoid valve for supplying a standard gas to the column and the detector, a column heater for heating the column, and heating the detector A detector heater; and a control unit for controlling operations of the detector, the carrier gas solenoid valve, the standard gas solenoid valve, the column heater, and the detector heater. The control unit inspects the sensitivity of the detector by supplying a carrier gas to the column and the detector via the carrier gas solenoid valve every time a predetermined time elapses or each time a predetermined number of analyzes is completed. In addition, by supplying a standard gas to the column and the detector via the standard gas solenoid valve, the separation degree of the column is inspected. Further, subsequently, if there is an abnormality in the sensitivity of the detector or the degree of separation of the column, the column heater and the detector while supplying a carrier gas to the column and the detector via the carrier gas solenoid valve. The column and the detector may be conditioned by heating the column and the detector with a heater.

Next, the column separation will be described with reference to FIG. The degree of separation of the two components cannot be determined only by the separation coefficient α (retention ratio of the later-eluted component based on the previous-eluted component, α> 1) and the sharpness of both component peaks (theoretical plate number N). The degree of separation R is used to indicate the degree of separation. In FIG. 7, R is R = 2 (tr ₂ −tr ₁ ) / (W ₁ −
W ₂ ). Note that W ₁ = W ₂ and R is N,
The following equation can be derived as an equation related to α and k ′. R =
( ^N1 / ^2/4 ) [(α-1) / α] [k '/ (k' +
1)]. When R <0.5, the two peaks almost overlap, when R = 1, 2% overlap, and when R = 1.25, 0.5% overlap. At R = 1.5, almost complete separation is possible.

[0013]

FIG. 1 is a block diagram showing one embodiment of a breath analyzer according to the present invention. 2 and 3 show FIG.
2 is a partially enlarged view of the flow path switching valve in FIG. 2, FIG. 2 shows a case where a flow path for exhalation suction is selected, and FIG. 3 shows a case where a flow path for analysis is selected. Hereinafter, description will be made based on these drawings.

The breath analyzer 10 according to the present embodiment has a breath A
, A column 12 for separating components contained in the exhaled air A by passing through, a detector 14 for detecting the components separated by the column 12, and a carrier gas solenoid valve for supplying a carrier gas C to the column 12 and the detector 14. 16C,
A standard gas solenoid valve 16S for supplying a standard gas S to the column 12 and the detector 14, a column heater 12H for heating the column 12, and a detector heater 14H for heating the detector 14.
, Detector 14, carrier gas solenoid valve 16C, standard gas solenoid valve 16S, column heater 12H and detector heater 1
And a control unit 18 for controlling the operation of 4H.

The column 12 is a hollow capillary tube having an inner wall coated with a liquid phase or the like. Detector 1
Reference numeral 4 denotes a photoionization detector that detects components by irradiating ultraviolet rays from an ultraviolet lamp to ionize components. The column heater 12H is a thermostat provided with a heating element (not shown), a temperature sensor, and a temperature controller. Detector heater 14
H includes a heating element (not shown), a temperature sensor, and a temperature controller. The control unit 18 is not shown,
It is provided with sequence control means including a timer and a relay, and data processing means including a microcomputer.

The breath analyzer 10 includes gas cylinders 22C and 22S, a standard gas storage unit 24, and a sample introduction unit 2.
6. A sample introduction section heater 26H, a flow path switching valve 28, a flow path switching valve heater 28H, a sample measuring tube 30, a suction pump 32, a display 34 and the like are additionally provided.

The gas cylinder 22C is filled with a carrier gas C such as helium or nitrogen. Gas cylinder 22
S is filled with a standard gas S composed of a known component. The standard gas S is, for example, a mixture of helium and isoprene and pentane. Standard gas storage 24
Is a storage container for storing the standard gas S in a fixed amount (for example, 500 ml) so as to smoothly supply the standard gas S. The sample introduction unit 26 includes a container that blows exhalation A into the subject and a sample gas that is introduced, a pressure sensor that detects the pressure in the container, and the like. The sample introduction unit heater 26H includes a heating element (and a cooling element if necessary), a temperature sensor, and a temperature controller (not shown). The flow path switching valve 28 is constituted by a rotary valve including ports 1 to 6 shown in FIGS. 2 and 3 and an actuator (not shown), and based on a control signal output from the control unit 18, the exhalation A, the standard gas S, and the carrier gas. C
Switch the flow path. The flow path switching valve heater 40H is
This is a thermostat provided with a heating element (not shown), a temperature sensor, and a temperature controller, and heats the flow path switching valve 28 to a constant temperature. The sample measuring tube 30 is a tube that holds a constant volume of the breath A or the standard gas S. The suction pump 32 is, for example, a diaphragm pump, and sucks the breath A or the standard gas S in the sample introduction unit 26 to fill the sample measuring tube 30.

Next, the exhalation suction operation and the analysis operation, which are the normal operations of the exhalation analyzer 10, will be described.

In the breath analyzer 10, in addition to the analysis, the breath A can be filled into the sample measuring tube 30 and the breath suction can be performed. First, a flow path (FIG. 2) for exhalation suction is selected by the flow path switching valve 28. When the subject blows exhalation A into the sample introduction unit 26, the suction pump 32 operates correspondingly for a predetermined time. At this time, the exhalation A is changed from the sample introduction part 26 → port 6 → port 5 →
It flows in the order of the sample measuring tube 30 → port 2 → port 1 → suction pump 32 → discharge. Thereby, the metering tube 30 is filled with a constant volume of exhaled air A.

Subsequently, a flow path for analysis (FIG. 3) is selected by the flow path switching valve 28. Thereby, the carrier gas C flows through the gas cylinder 22C → port 3 → port 2 → sample measuring tube 30 → port 5 → port 4 → column 12 → detector 14 → discharge, so that the exhalation A filled in the sample measuring tube 30. Also flows with the carrier gas C and passes through the column 12 and the detector 14. Each component contained in the breath A is separated by the column 12 and detected by the detector 14 with a time difference. The detector 14 and the control unit 18 perform qualitative analysis based on the volume (retention volume) or the time (retention time) of the carrier gas C from the time when the exhalation A is injected until the separation zone of each component appears, and the peak area is determined. Alternatively, quantitative analysis is performed from the peak height.

FIG. 4 is a flow chart showing the operation of the control unit 18 in the breath analyzer 10 for contamination or deterioration of the column or the detector. FIG. 5 shows the breath analyzer 10.
5 is a time chart showing a conditioning operation in FIG. FIG. 6 is a table showing the result of comparing the operation and effect of the conventional technology and the present invention. Hereinafter, FIG.
6 through FIG.

Each time a predetermined time elapses or each time the predetermined number of analyses is completed, the inspection of the column 12 and the detector 14 is executed following the above-described analysis operation. The predetermined time is, for example, one day, and the predetermined number of times of analysis is, for example, one span. One span is the number of times of analysis when the same component is continuously analyzed or when continuously analyzed under the same conditions.

First, the sensitivity of the detector 14 is checked by supplying the carrier gas C to the column 12 and the detector 14 via the carrier gas solenoid valve 16C (step 1).
01). At this time, the flow path shown in FIG. 2 is selected by the flow path switching valve 28. The inspection condition is, for example, the column 12
Is 80.degree. C. (the same as during normal analysis), the temperature of the detector 14 is 120.degree. C., and the carrier gas C is helium 6 ml / min. Subsequently, the column 12 is supplied via the standard gas solenoid valve 16S.
Then, by supplying the standard gas S to the detector 14, the degree of separation of the column 12 is inspected. The operation at this time is the same as the above-mentioned exhalation suction operation and analysis operation except that the standard gas S is used instead of the exhalation A (step 10).
2). Subsequently, it is determined whether the sensitivity of the detector 14 and the degree of separation of the column 12 are normal (step 103).
The sensitivity of the detector 14 is such that the slope sensitivity is a constant value (for example, 20
0 μV / min) is normal, and if it is above a certain value, it is abnormal. The degree of separation of the column 12 is normal if it is equal to or more than a certain value, and abnormal if it is equal to or less than the certain value.
This constant value of the degree of separation is, for example, if the standard gas S is a mixture of helium and isoprene and pentane,
1.5.

If the sensitivity of the detector 14 or the degree of separation of the column 12 is abnormal, the column heater 12H and the detector heater 14H are supplied while supplying the carrier gas C to the column 12 and the detector 14 via the carrier gas solenoid valve 16C. The column 12 and the detector 14 are heated to perform conditioning of the column 12 and the detector 14 (Step 104). Conditioning conditions include, for example, the temperatures of the column 12 and the detector 14 as shown in FIG. 5, and the carrier gas C is helium 6 ml / min. Subsequently, the sensitivity of the detector 14 is checked again (step 10).
5) Check the degree of separation of the column 12 (step 10)
6) It is determined whether the sensitivity of the detector 14 and the degree of separation of the column 12 are normal (step 107). Detector 1
If the sensitivity of No. 4 or the degree of separation of the column 12 is abnormal, the fact is displayed on the display 34. If the sensitivity of the detector 14 is abnormal, the content of the display is, for example, "Check or replace the detector because the detector may be deteriorated." If abnormal, for example, "Check or replace the column because the column may be deteriorated." Subsequently, by executing the automatic shutdown (step 109),
All operations end.

On the other hand, if there is no abnormality in steps 103 and 107, the automatic shutdown is executed (step 109), whereby all the operations are completed.

[0026]

According to the breath analyzer of the first or second aspect, every time a predetermined time elapses or each time a predetermined number of analyzes is completed,
Since the sensitivity of the detector and the degree of separation of the column are automatically inspected, extremely sensitive contamination / deterioration can be accurately determined without depending on the operator. As a result, it is possible to prevent the operator from overlooking the contamination and deterioration due to an unfamiliar operator, thereby improving the analysis accuracy. Moreover, the automation makes it easy for anyone to operate, so that the workability can be improved.

According to the breath analyzer of the present invention, if the sensitivity of the detector or the resolution of the column is abnormal, the conditioning of the column and the detector is automatically performed, so that the manual operation is troublesome. Since complicated operations can be avoided, workability can be further improved.

[Brief description of the drawings]

FIG. 1 is a configuration diagram showing one embodiment of a breath analyzer according to the present invention.

FIG. 2 is a partially enlarged view showing a flow path switching valve in FIG. 1 when a flow path for exhalation suction is selected.

FIG. 3 is a partially enlarged view showing a flow path switching valve in FIG. 1 when a flow path for analysis is selected.

FIG. 4 is a flowchart showing an operation of a control unit for contamination / deterioration of a column or a detector in the breath analyzer of FIG. 1;

5 is a time chart showing a conditioning operation in the breath analyzer of FIG. 1. FIG.

FIG. 6 is a table showing the results of comparing the operation and effect of the conventional technique and the present invention.

FIG. 7 is a waveform chart for explaining a column separation degree.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Breath analyzer 12 Column 12H Column heater 14 Detector 14H Detector heater 16C Carrier gas solenoid valve 16S Standard gas solenoid valve 18 Control part A Expiration C Carrier gas S Standard gas

Claims (2)

[Claims] 1. A column that separates components contained in a breath by passing the breath, a detector that detects the components separated by the column, and a carrier that supplies a carrier gas to the column and the detector. A gas solenoid valve, a standard gas solenoid valve for supplying a standard gas to the column and the detector, a column heater for heating the column, a detector heater for heating the detector, the detector, and the carrier gas solenoid. A control unit that controls the operation of the valve, the standard gas solenoid valve, the column heater, and the detector heater. By supplying a carrier gas to the column and the detector, the sensitivity of the detector is inspected, and the standard gas solenoid valve By supplying the standard gas to the column and the detector through, examining the degree of separation of the column, the breath analyzer. 2. A column for separating components contained in the breath by passing the breath, a detector for detecting the components separated by the column, and a carrier for supplying a carrier gas to the column and the detector. A gas solenoid valve, a standard gas solenoid valve for supplying a standard gas to the column and the detector, a column heater for heating the column, a detector heater for heating the detector, the detector, and the carrier gas solenoid. A control unit that controls the operation of the valve, the standard gas solenoid valve, the column heater, and the detector heater. By supplying a carrier gas to the column and the detector, the sensitivity of the detector is inspected, and the standard gas solenoid valve By supplying a standard gas to the column and the detector via the above, the separation degree of the column is inspected, and if there is an abnormality in the sensitivity of the detector or the separation degree of the column, through the carrier gas solenoid valve. A breath analyzer that conditions the column and the detector by heating the column and the detector with the column heater and the detector heater while supplying a carrier gas to the column and the detector.