JP4603786B2 - Chemical substance monitoring device and chemical substance monitoring method - Google Patents

Description

  The present invention relates to a method for stabilizing sensitivity and improving quantitative accuracy of a mass spectrometer used in a chemical substance monitoring apparatus.

  The effects of exhaust gas discharged from waste incineration facilities and facilities for treating hazardous substances such as polychlorinated biphenyl (PCB) on the human body and the environment have become a problem. In setting up and operating these treatment facilities, consideration for the surrounding environment, residents, and workers is indispensable. For this reason, it is essential to monitor online whether these facilities are operating normally and whether the working environment atmosphere inside these facilities or the ambient air around these facilities is not contaminated. It has become.

  A chemical monitoring method and monitoring apparatus capable of selectively monitoring organic chlorine compounds such as dioxins and dioxin precursors in exhaust gas and a combustion furnace using the same are described in, for example, Patent Document 1. ing.

  Patent Document 1 discloses a sample analysis monitor device capable of performing measurement while correcting the concentration of a measurement target substance in a gas containing various contaminants, and capable of highly accurate analysis, and a combustion furnace using the same. 2.

  In corona discharge, the direction of sample introduction to the corona discharge region and the direction in which ions are extracted by corona discharge are almost opposite to each other, improving ion generation efficiency, and using atmospheric pressure chemical ionization mass using an ion source using corona discharge An analyzer is described in Patent Document 3.

JP 2000-162189 A

JP 2001-147216 A JP 2001-93461 A

  With chemical substance monitoring equipment using mass spectrometers, exhaust gas discharged from waste incineration facilities, exhaust gas discharged from various chemical decomposition facilities, harmful gases in the atmosphere of the surrounding environment, etc. In the case of measuring the concentration of the sample, there is a problem that the sensitivity of the measurement substance is greatly lowered due to the influence of the contaminant contained in the sample gas.

  In order to stabilize the sensitivity and improve the quantitative accuracy, it is necessary to weaken the influence of moisture, which is a main component of the contaminant.

  In Patent Document 2, when the concentration of contaminant components is high, the sensitivity of the measurement object is remarkably lowered, and the measurement accuracy deteriorates, air whose flow rate is controlled is introduced into the ion source inlet, and the exhaust gas is discharged. Although it is described that the influence of contaminant components can be weakened by diluting, what is the specific description regarding stabilization of sensitivity and improvement of quantitative accuracy by controlling the moisture concentration in the sample gas? Nor.

  An object of the present invention is to provide a chemical substance monitoring apparatus and a chemical substance monitoring method capable of highly accurate analysis.

  The present invention has been made to solve the above-described problems. The moisture concentration is monitored, and the amount of dry air introduced into the sample gas is adjusted so that the moisture concentration in the sample gas is approximately 1% or less. In this way, the sample gas diluted with dry air is introduced into the ion source and the moisture concentration is controlled to prevent the fluctuation of the sensitivity of the measurement target substance due to the influence of contaminants and achieve high-accuracy measurement.

  The chemical substance monitoring device according to the first configuration of the present invention performs an ion source part that generates ions of a measurement target substance in a sample gas, an introduction pipe that introduces the sample gas into the ion source part, and mass analysis of ions. It has a mass spectrometer and a first pipe for introducing dry air for diluting the sample gas into the introduction pipe. Ions of the substance to be measured are detected under the condition that dry air is introduced into the introduction pipe so that the moisture concentration in the sample gas introduced into the ion source is approximately 1% or less.

  The chemical substance monitoring device of the first configuration is further arranged in the first pipe and means for controlling the flow rate of the dry air, and the inside of the introduction pipe or the exhaust pipe for exhausting the ion source part, Detecting means for detecting the moisture concentration in the gas inside the introduction pipe or the exhaust pipe. Based on the output of the detection means, the flow rate of the dry air is controlled. Moreover, it has the apparatus which produces | generates the dry air whose water concentration is about 1% or less, and this apparatus is connected to 1st piping.

  The chemical substance monitoring apparatus of the first configuration further controls the second pipe for introducing the standard substance for measuring the concentration of the measurement target substance into the introduction pipe, and the flow rate of the standard substance flowing through the second pipe. The ionization efficiency of the standard substance is substantially equal to the ionization efficiency of the measurement target substance. The substance to be measured is ionized by an atmospheric pressure chemical ion source that is used as an ion source and is ionized by corona discharge under atmospheric pressure. When the measurement target substance is PCB and when the positive ion of the measurement target substance is generated in the ion source part, tetrachlorobenzene or pentachlorobenzene is used as the standard substance, and when the negative ion of the measurement target substance is generated in the ion source part, Trichlorophenol is used as a standard substance. The concentration of the measurement target substance is determined based on the measured ion intensity of the standard substance and the measurement target substance.

  According to the first configuration, the measurement target substance in the sample can be quantified with an accuracy of 10% or less by using an inexpensive standard substance.

  The chemical substance monitoring apparatus of the second configuration of the present invention performs ion analysis of an ion source part that generates ions of a substance to be measured in a sample gas, an introduction pipe that introduces the sample gas into the ion source part, and ion mass spectrometry. It has a mass analyzer, a first pipe for introducing dry air for diluting the sample gas into the introduction pipe, and a control means arranged in the first pipe for controlling the flow rate of the dry air. Under the condition that the flow rate of the dry air introduced into the introduction pipe is controlled by this flow rate control means so that the moisture concentration in the sample gas introduced into the ion source portion is approximately 5% or less, Ion detection is performed.

  According to the second configuration, the measurement target substance in the sample can be quantified with an accuracy of 200% or less by using an inexpensive standard substance.

  The chemical substance monitoring device of the third configuration according to the present invention exhausts the ion source part that generates ions of the substance to be measured in the sample gas, the introduction pipe that introduces the sample gas into the ion source part, and the ion source part. An exhaust pipe, a mass analyzer for performing mass analysis of ions, a first pipe for introducing dry air for diluting the sample gas into the introduction pipe, and a first pipe disposed in the first pipe for controlling the flow rate of the dry air 1 flow control means, a second pipe for introducing a standard substance for measuring the concentration of the substance to be measured into the introduction pipe, and a second flow rate arranged in the second pipe for controlling the flow rate of the standard substance Control means, detection means arranged inside the exhaust pipe and detecting moisture concentration in the gas inside the exhaust pipe, and moisture in the sample gas introduced into the ion source based on the output of the detection means The first flow is such that the concentration is approximately 1% or less. And means for controlling the control means. The concentration of the measurement target substance is determined based on the ionic strength of the standard substance and the target substance. The moisture concentration of the dry air introduced into the introduction pipe is managed so as to be approximately 1% or less. One end of the introduction pipe is connected to the exhaust pipe of the PCB decomposition processing apparatus, and the sample gas is introduced into the introduction pipe from the exhaust pipe. Alternatively, one end of the introduction pipe is disposed inside a chemical agent treatment chamber that performs chemical agent detection or chemical agent decomposition treatment, and the sample gas is introduced from one end into the introduction pipe. The other end of the introduction pipe is connected to the ion source unit. Further, the sample gas is collected from the outdoor atmosphere by a gas collecting means.

  According to the third configuration, the measurement target substance in the sample can be quantified with an accuracy of 10% or less by using an inexpensive standard substance.

  The chemical substance monitoring apparatus of the fourth configuration according to the present invention performs an ion source part that generates ions of a substance to be measured in a sample gas, an introduction pipe that introduces the sample gas into the ion source part, and mass analysis of ions. This detection unit has a mass analysis unit and a detection means that is disposed inside the introduction pipe or the exhaust pipe that exhausts the ion source part and detects the moisture concentration in the gas inside the introduction pipe or the exhaust pipe. The sensitivity of the detected ions is corrected by the value of the moisture concentration detected by the means.

  In the chemical substance monitoring method of the present invention, the sample gas is caused to flow through the introduction pipe connected to the ion source section, the sample gas is introduced into the ion source section, and the first pipe connected to the introduction pipe. The first flow rate control means controls the flow rate of the dry air having a moisture concentration of approximately 1% or less, and the step of introducing the dry air for diluting the sample gas into the introduction pipe is connected to the introduction pipe. A step in which the flow rate of the standard substance for measuring the concentration of the measurement target substance contained in the sample gas is controlled by the second flow rate control means arranged in the second pipe, and the standard substance is introduced into the introduction pipe. In the gas inside the exhaust pipe for exhausting the ion source unit, the step of generating ions of the measurement target substance and the standard material in the ion source unit, the step of performing mass analysis of the ions generated in the ion source unit Detecting the moisture concentration of A step of controlling the first flow rate control means so that the moisture concentration in the sample gas introduced into the ion source is approximately 1% or less based on the detected moisture concentration; And determining the concentration of the substance to be measured based on the intensity of the ions. According to this method, the measurement target substance in the sample can be quantified with an accuracy of 10% or less by using an inexpensive standard substance.

  According to the present invention, it is possible to provide a chemical substance monitoring apparatus and a chemical substance monitoring method that prevent a reduction in sensitivity of a measurement target substance due to the influence of moisture, which is a main component of a contaminant substance, eliminate a quantification error, and have high quantification accuracy. it can.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

  FIG. 1 is a diagram illustrating a schematic configuration example of a chemical substance monitoring apparatus applied to a PCB processing facility according to the first embodiment of the present invention.

  As shown in FIG. 1, the measurement target gas is introduced from the exhaust gas line 1 of the PCB processing facility 60 into the introduction pipe 2 (heated to about 200 ° C.). The sample gas introduced from the exhaust gas line 1 is introduced into the ionization section 3 through the introduction pipe 2 after removing fine dust such as dust and mist with the filter 16. The gas passing through the ionization unit 3 is sucked by the pump 7 and exhausted using the exhaust line 19. The flow rate of the gas flowing through the exhaust line 19 is controlled by the mass flow controller 12. Since a gas flow rate of about 1 to 3 L / min is sufficient for the mass spectrometer, the excess flow rate is exhausted using the bypass line 18. The flow rate of the gas flowing through the bypass line 18 is controlled by the mass flow controller 6. The exhaust gas that has passed through the pump 7 passes through the activated carbon 8, and the PCB and the standard sample contained in the exhaust gas are adsorbed by the activated carbon 8 and safely exhausted.

  The standard sample 17 is introduced into the introduction pipe 2 via the standard sample generator 5 using the dry air produced by the dry air production apparatus 14 as a carrier gas. Since the generation amount of the standard sample is influenced by the flow rate of the mass flow controller 13, the adjustment of the introduction amount of the dry air into the introduction pipe 2 is performed using an introduction system by another mass flow controller 15. Here, the dry air produced by the dry air production apparatus 14 is used as the carrier gas for introducing the standard sample 17, but the standard sample may be introduced using air or an air cylinder. The concentration of the standard sample is set to be approximately the same as the average concentration of the substance to be measured in the sample gas measured in advance by GC / MS or the like.

  The shape of the standard sample generator 5 may be any shape as long as the evaporated standard sample is mixed with the dry air flowing from the dry air production apparatus 14, but the amount of the standard sample generated is influenced by the temperature. In order to receive strongly, it is important to wind a heater around the standard sample generator 5 and control the temperature to be constant. The hole diameter and shape of the container in which the standard sample is placed may be determined so that the target concentration can be generated according to the evaporation amount of the standard sample. If there are a plurality of substances to be measured and it is desired to add a plurality of standard samples in accordance with them, a plurality of containers containing standard samples may be placed in the standard sample generator 5.

  As the ion source used in the ionization unit 3, atmospheric pressure chemical ionization, chemical ionization, electron impact ionization, plasma ionization, glow discharge ionization, and the like are used. Here, the ion source using the corona discharge described in Patent Document 3 was used, but in this ion source, the sample introduced into the ionization portion is opposite to the direction in which ions generated in the vicinity of the needle electrode travel by the electric field. In other words, when flowing toward the needle electrode, ions of the measurement object can be efficiently ionized. In the embodiment of the present invention, the flow of the sample toward the needle electrode is 10 mL / min or more. Ions ionized by the ionization unit are introduced into the mass analysis unit 4 and processed by the data processing unit 9. The analysis result 70 by the data processing unit 9 is sent to the PCB processing facility 60.

  There are various contaminants in the sample gas, and the sensitivity of the measurement target substance varies due to the influence of the contaminants. The influence of moisture, which is a major component among contaminants, is large, and it is important to control the moisture concentration. Therefore, the sample gas is diluted by introducing the atmosphere into the dry air production apparatus 14, producing dry air, controlling the flow rate by the mass flow controller 15, and introducing it into the introduction pipe 2. The moisture concentration of the sample gas is measured by the hygrometer 11 provided in the exhaust line 19, and the value is sent to the controller 10. The controller 10 and the mass flow controller 15 control the flow rate of the dry air, and the moisture concentration of the sample gas. Manage. However, when there is no possibility that the measurement target substance is adsorbed to the hygrometer, or when there is no generation of a component that affects the measurement from the hygrometer itself, the distance from the dry air introduction unit 50 to the ionization unit 3 May be provided.

  Dry air may be introduced using an air cylinder, but the capacity of air cylinders is limited and frequent replacement is required. Is good. Various apparatuses can be used as the dry air production apparatus 14, and for example, a refrigeration air dryer, an adsorption air dryer, a membrane air dryer, or the like can be used.

  A refrigeration air dryer uses a refrigeration cycle formed of a compressor (refrigerator), a condenser, an expansion valve, an evaporator, and other electrical parts, and allows the compressed air to pass through the evaporator and the moisture in the compressed air. To obtain dry air.

  In the adsorption type air dryer, a special moisture adsorbent is used, the adsorbent is filled into the chamber, compressed air is introduced into the chamber, and dry air is obtained from the outlet side.

  In the membrane air dryer, the hollow fiber membrane formed with a polymer membrane that is easy to permeate moisture and difficult to permeate air uses the difference in concentration and pressure, taking advantage of the fact that water vapor permeation is significantly faster than oxygen and nitrogen. To remove water vapor. Compressed air is introduced into the hollow fiber membrane filter, only water vapor is discharged to the outside, and dry air is obtained on the outlet side.

  FIG. 2 is a diagram showing a schematic configuration example of an adsorption air dryer used in the chemical substance monitoring apparatus of the embodiment of the present invention. Compressed air is introduced into the adsorption column filled with the adsorbent, becomes dry air, and is discharged from the adsorption column. When the adsorbent adsorbs a certain amount of water, the water adsorbability is lost. Therefore, two or more adsorption columns filled with the adsorbent are provided and used by switching. The adsorption column with poor adsorbability is regenerated by drying with a heater or another method.

  In the configuration shown in FIG. 2, the compressed air is introduced into the adsorption column 26 filled with the adsorbent through the three-way valve 23, and the dry air is discharged from the adsorption column 26. Part of the dry air from which moisture has been removed by the adsorption column 26 by adjusting the purge air control valve 30 is introduced into the adsorption column 27, the adsorption column 27 is dried and regenerated, and discharged from the purge air discharge port of the valve 25. . When the dehumidifying performance of the adsorption column 26 is reduced, the three-way valve 23 is switched to introduce compressed air into the adsorption column 27, and the purge air control valve 30 is adjusted to remove a portion of the dried air from the adsorption column 27. Is introduced into the adsorption column 26, the adsorption column 26 is dried and regenerated, and discharged from the purge air discharge port of the valve 24. By repeating this operation alternately in the adsorption column 26 and the adsorption column 27, the adsorbent is automatically regenerated, and the dry air is continuously discharged from the purge air discharge port. The gas flow in each part is adjusted by valves 24 and 25 and check valves 28 and 29.

  FIG. 3 is a diagram showing a schematic configuration example of a chemical substance monitoring apparatus applied to a PCB processing facility according to the second embodiment of the present invention.

  In the configuration shown in FIG. 1, dry air is introduced into both the standard sample generator 5 and the introduction pipe 2. However, in the configuration shown in FIG. 3, the dry air is not introduced into the standard sample generator 5 and is dried. Dry air from the air production apparatus 14 is introduced into the introduction pipe 2. Air is introduced into the standard sample generator 5 via the pump 20, the activated carbon 21 and the mass flow controller 13.

  FIG. 4 is a diagram illustrating a schematic configuration example of a chemical substance monitoring apparatus applied to a PCB processing facility according to the third embodiment of the present invention. In the configuration shown in FIG. 4, the dry air is not introduced into the introduction pipe 2 but the dry air from the dry air production apparatus 14 is introduced into the standard sample generator 5 via the mass flow controller 13. When the change in the moisture concentration of the sample gas is not large and the moisture concentration range can be grasped and the sample gas may be diluted by introducing a certain amount of dry air, as shown in FIG. A configuration without a controller is also possible.

  For example, it is known that the moisture concentration of the sample gas is in the range of 4.5 to 5%, the moisture concentration in the dry air to be used is 0.5%, and the introduction amount of the sample gas is 1.0 L / min. When the introduction amount of the standard sample (dry air) is 1.0 L / min, the moisture concentration upstream of the ion source is reduced to 0.9 to 1.0% when the introduction amount of the dry air is 7.0 L / min. can do. In this case, the amount of dry air introduced is fixed.

  When the substance to be measured is PCB, the sensitivity is affected by the moisture concentration.

  FIG. 5 is a schematic configuration diagram of an example of an apparatus used for confirming experimentally a decrease in sensitivity due to the influence of PCB water concentration in the example of the present invention.

  In the standard sample generator 5, as a standard sample 17, PCB (polychlorobiphenyl), 1,2,4,5-tetrachlorobenzene (TeCB: 1,2,4,5-tetrachlorobenzen), pentachlorobenzene (PeCB: Bpentachlorobenzen) To generate a certain amount of standard sample vapor. The vapor of the standard sample is sent to the introduction pipe 2 by dry air (the flow rate is controlled by the mass flow controller 13). On the other hand, 0 to 10% of water vapor (the flow rate is controlled by the mass flow controller 32) generated by the humidifier 35 is introduced into the introduction pipe 2.

  The sample gas in which water vapor is added to the vapor of the standard sample is ionized by the ionization unit 3 and subjected to mass analysis by the mass analysis unit 4. In the ionization unit 3, an atmospheric pressure chemical ionization method was used, and as the mass analysis unit 4, an ion trap type mass spectrometer was used.

  As the sample gas, KC300 (mainly PCB of 3-4 chloride) and KC600 (mainly 5-7 chloride) are used as the sample gas. Degree.

FIG. 6 is a diagram showing an example of an experimental result showing a decrease in sensitivity due to the influence of moisture concentration when PCB is measured in the positive ionization mode from the apparatus shown in FIG. 5 in the embodiment of the present invention.
The horizontal axis in FIG. 6 indicates the water concentration W. The vertical axis in FIG. 6 is a signal intensity ratio defined by detected signal intensity I (W) / detected signal intensity I (W = 0). As is apparent from FIG. 6, the signal intensity ratios of PCB, TeCB, and PeCB for each chloride show different behaviors.

  FIG. 7 is a diagram showing an experimental result example of the change in the moisture concentration of the signal intensity ratio of PCB to TeCB obtained in the example of the present invention. The vertical axis in FIG. 7 indicates the signal intensity ratio of PCB to TeCB at a moisture concentration W, and the relative ratio with the signal intensity ratio of PCB to TeCB at 1 at a moisture concentration W = 0 as a correction coefficient.

  FIG. 8 is a diagram showing an experimental result example of the change in the moisture concentration of the signal intensity ratio of PCB to PeCB obtained in the example of the present invention. The vertical axis in FIG. 8 shows the signal intensity ratio of PCB to PeCB at a moisture concentration W, and the relative ratio with the signal intensity ratio of PCB to PeCB at 1 at a moisture concentration W = 0 as a correction coefficient.

  7 and 8, the closer the relative ratio is to 1, the more the signal intensity changes of PCB and TeCB, and PCB and PeCB are equal.

  6, 7, and 8, in the apparatus shown in FIGS. 1 and 3, when the measurement target substance is PCB, the moisture concentration in the sample gas is set to 1% when the quantitative accuracy is to be within ± 10%. If it is desired that the quantitative accuracy be within ± 200%, the water concentration in the sample gas may be controlled within 5%.

  If the sensitivity change of the measurement target substance according to the change in the moisture concentration can be grasped in advance and the correction coefficient according to the moisture concentration has been obtained, the configuration for diluting the sample gas by introducing dry air is eliminated, Sensitivity correction can also be performed using a moisture concentration measured by a hygrometer and a correction coefficient corresponding to the moisture concentration.

  FIG. 9 is a diagram showing a schematic configuration example of a chemical substance monitoring apparatus applied to a PCB processing facility according to the fourth embodiment of the present invention. In the configuration shown in FIG. 9, the dry air production apparatus 14, the controller 10, and the mass flow controller 15 are omitted from the configuration of the apparatus shown in FIG.

  For example, when a sample gas having a water concentration of 5% is measured in the positive ionization mode using pentachlorobenzene (PeCB) as a standard sample, the concentration of tetrachloride PCB is as follows. The addition concentration of PCB of 4 chloride and PeCB is A μg / Nm 3, and the signal intensity when the water concentration is W = 0 (the signal intensity of PCB of 4 chloride / the signal intensity of PeCB) is B. From the results shown in FIG. 8, when the relative ratio regarding tetrachloride PCB / PeCB when the water concentration W = 0 is 1, the relative ratio regarding PCB tetrachloride / PeCB when the water concentration is 5% is 1.66. Therefore, the concentration of 4-chloride PCB when the moisture concentration is 5% is AxB / 1.66.

The configuration shown in FIGS. 1, 3, 4, and 9 shows an example in which the exhaust gas from the exhaust gas line of the PCB processing facility is introduced and analyzed, but the working environment air in the PCB processing facility, the PCB processing facility It is also possible to replace the PCB processing facility 60 with a chemical agent processing facility 70 in the configuration shown in FIGS. 1, 3, 4, and 9.

  FIG. 10 is a diagram showing a schematic configuration example of a chemical substance monitoring apparatus applied to a chemical drug processing facility which is a fifth example of the present invention and detects a chemical drug or decomposes a chemical drug.

  In the configuration shown in FIG. 10, the PCB processing facility 60 is replaced with the chemical agent processing facility 70 in the configuration shown in FIG. 3, and the line for introducing the standard sample is omitted. Needless to say, the exhaust gas from the chemical agent treatment facility 80, the working environment air in the chemical agent treatment facility 80, and the ambient air of the chemical agent treatment facility 80 can be introduced and analyzed.

  Furthermore, it is needless to say that the chemical agent treatment facility 80 can be replaced with a hazardous material treatment facility, an explosive material treatment facility, or the like in the configuration shown in FIG.

  Even when analyzing dangerous substances, explosives, and chemical agents, monitoring the moisture concentration, adjusting the amount of dry air introduced, and managing the moisture concentration can cause fluctuations in the sensitivity of the measurement target substance due to the influence of contaminants. Is important to prevent. When there is little fluctuation in ionization efficiency and the measurement target substance can be measured stably, it is possible to eliminate the line for introducing the standard sample as shown in FIG. 10 and reduce the cost. It is also important to consider the safety of workers and the protection of the surrounding environment at hazardous substance decomposition treatment facilities.

  In the embodiment described above, when monitoring the exhaust gas from the PCB processing facility, the hazardous material processing facility, the explosive material processing facility, the chemical agent processing facility, the working environment air in the processing facility, and the ambient air of the processing facility, In addition to the analysis result 70, it is also important to add information for stopping the processing apparatus when the measurement target substance detects a predetermined reference value or more based on the analysis result 70.

  According to the present invention, it is possible to provide a chemical substance monitoring apparatus and a chemical substance monitoring method that reduce sensitivity associated with the influence of contaminants, eliminate quantitative errors, and have high quantitative accuracy.

BRIEF DESCRIPTION OF THE DRAWINGS The figure which is Example 1 of this invention, and shows the schematic structural example of the chemical substance monitoring apparatus applied to the PCB processing facility. The figure which shows the schematic structural example of the adsorption type air dryer used with the chemical substance monitoring apparatus of the Example of this invention. The figure which is Example 2 of this invention, and shows the schematic structural example of the chemical substance monitoring apparatus applied to the PCB processing facility. The figure which is Example 3 of this invention, and shows the schematic structural example of the chemical substance monitoring apparatus applied to the PCB processing facility. In the Example of this invention, the schematic block diagram of an example of the apparatus used in order to confirm the sensitivity fall by the influence of the moisture concentration of PCB by experiment. The figure which shows the example of an experimental result which shows the sensitivity fall by the influence of a moisture concentration at the time of measuring PCB in positive ionization mode from the apparatus shown in FIG. 5 in the Example of this invention. The figure which shows the experimental result example of the change of the moisture concentration of the signal intensity ratio with respect to TeCB of PCB obtained in the Example of this invention. The figure which shows the experimental result example of the change of the moisture concentration of the signal intensity ratio with respect to PeCB of PCB obtained in the Example of this invention. The figure which is Example 4 of this invention, and shows the schematic structural example of the chemical substance monitoring apparatus applied to the PCB processing facility. The figure which is Example 5 of this invention, and shows the example of schematic structure of the chemical substance monitoring apparatus applied to the chemical chemical | medical agent processing plant | facility which detects a chemical chemical | medical agent or decomposes | disassembles a chemical chemical.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Exhaust line, 2 ... Introduction piping, 3 ... Ionization part, 4 ... Mass analysis part, 5 ... Standard sample generator, 6, 12, 13, 15, 32 ... Mass flow controller, 7, 20 ... Pump, 8, 21 ... activated carbon, 9 ... data processing unit, 10 ... controller, 11 ... hygrometer, 14 ... dry air production device, 16 ... filter, 17 ... standard sample, 18 ... bypass line, 19 ... exhaust line, 23 ... three-way valve, 24 , 25 ... Valve, 26, 27 ... Adsorption column, 28, 29 ... Check valve, 30 ... Purge air control valve, 35 ... Humidifier, 50 ... Dry air introduction part, 60 ... PCB processing facility, 70 ... Analysis result, 80 ... Chemical agent treatment facility.

Claims (14)

An ion source for generating PCB ions in the sample gas;
An introduction pipe for introducing the sample gas into the ion source;
A mass spectrometer for performing mass analysis of the ions;
A data processing unit for processing data by the mass analyzing unit;
A first pipe for introducing dry air for diluting the sample gas into the introduction pipe ;
Means for controlling the flow rate of the dry air disposed in the first pipe,
It means for controlling the flow rate, chemical monitoring apparatus characterized by moisture concentration of the sample gas introduced into the ion source section introduces the drying air into the inlet pipe to be 1% or less . In chemical monitoring apparatus according to claim 1, arranged inside the exhaust pipe for exhausting the inside or the ion source portion of the front Symbol introduction pipe, moisture in the air inside of the inlet conduit or the exhaust pipe A chemical substance monitoring apparatus comprising: a detecting means for detecting a concentration ; and the means for controlling the flow rate controls the flow rate of the dry air based on an output of the detecting means. In chemical monitoring apparatus according to claim 1, the chemical has a device for generating the drying air the moisture concentration is 1% or less, the said apparatus characterized by being connected to the first pipe Monitor device. The chemical substance monitoring apparatus according to claim 1, wherein a standard substance generating apparatus that generates a standard substance for measuring the concentration of the PCB , a second pipe that introduces the standard substance into the introduction pipe, chemical monitoring apparatus characterized by chromatic and means for controlling the flow rate of the reference material to be supplied to the second pipe. 5. The chemical substance monitoring apparatus according to claim 4, wherein the ion source section is an atmospheric pressure chemical ion source that is ionized by corona discharge under atmospheric pressure. In chemical monitoring apparatus according to claim 4, standards of occurrence of said reference material generating apparatus, if the previous SL ion source for generating positive ions of the PCB, a Te Tiger chlorobenzene or pentachlorobenzene, wherein when generating the negative ions of the PCB in the ion source unit, chemical monitoring device, characterized in that the Application Benefits chlorophenol. In chemical monitoring apparatus according to claim 4, wherein the data processing unit, based on the intensity of the ionic strength and the PCB of ion-of the standard substance, and determining the concentration of the PCB Chemical substance monitoring device. An ion source for generating PCB ions in the sample gas;
An introduction pipe for introducing the sample gas into the ion source;
An exhaust pipe for exhausting the ion source;
A mass spectrometer for performing mass analysis of the ions;
A data processing unit for processing data by the mass spectrometry unit;
A first pipe for introducing dry air for diluting the sample gas into the introduction pipe;
First flow rate control means for controlling the flow rate of the dry air disposed in the first pipe;
A second pipe for introducing a standard substance for measuring the concentration of the PCB into the introduction pipe;
Second flow rate control means for controlling the flow rate of the standard substance disposed in the second pipe;
A detecting means arranged inside the exhaust pipe and detecting a moisture concentration in a gas inside the exhaust pipe;
Based on the output of the detection means, means for controlling the first flow rate control means so that the moisture concentration in the sample gas introduced into the ion source section is 1 % or less,
The data processing unit, based on the intensity of the ions of the strength of the ion-of the standard PCB, chemical monitoring apparatus characterized by determining the concentration of the PCB. 9. The chemical substance monitoring apparatus according to claim 8, wherein the moisture concentration of the dry air introduced into the introduction pipe is 1 % or less. In chemical monitoring apparatus according to claim 8, one end of the introduction pipe is connected to an exhaust pipe of PCB decomposition treatment apparatus, the other end of the pre-Symbol introduction pipe, characterized in that it is connected to the ion source region Chemical substance monitoring device. 9. The chemical substance monitoring apparatus according to claim 8, further comprising means for collecting the sample gas from the outdoor atmosphere. In chemical monitoring apparatus according to claim 8, one end of the inlet conduit into the interior of the chemical drug treatment chamber for detecting or decomposition treatment of chemicals chemical agents is arranged, the other end of the pre-Symbol introduction pipe the ion A chemical substance monitoring device connected to a source part. One end of which is connected to the exhaust pipe of the PCB decomposition processing apparatus, and the introduction pipe through which the sample gas is introduced;
An ion source connected to the other end of the introduction pipe and generating PCB ions contained in the sample gas;
An exhaust pipe for exhausting the ion source;
A mass spectrometer for performing mass analysis of the ions;
A data processing unit for processing data by the mass analyzing unit;
A first pipe for introducing dry air for diluting the sample gas into the introduction pipe;
First flow rate control means arranged in the first pipe for controlling the flow rate of the dry air;
A standard substance for measuring the concentration of the PCB substance connected to the introduction pipe between the exhaust pipe and the connection part of the introduction pipe, and the connection part of the first pipe and the introduction pipe is introduced. A second pipe to be introduced into the pipe;
Second flow rate control means for controlling the flow rate of the standard substance disposed in the second pipe;
Detecting means that is disposed inside the exhaust pipe and detects a moisture concentration in a gas inside the exhaust pipe;
Based on the output of the detection means, means for controlling the first flow rate control means so that the moisture concentration in the sample gas introduced into the ion source section is 1 % or less,
Wherein the data processing unit, wherein the intensity of ion-standard material and strength of the ions of the PCB material, chemical monitoring apparatus characterized by determining the concentration of the PCB. A sample gas is caused to flow through an introduction pipe connected to the ion source unit, and the sample gas is introduced into the ion source unit;
The first flow control means disposed in the first pipe connected to the inlet conduit, the moisture concentration is controlled flow rate of 1 percent or less is dry air, the dry air is said to dilute the sample gas A process to be introduced into the introduction pipe;
The flow rate of the standard substance for measuring the concentration of PCB contained in the sample gas is controlled by the second flow rate control means arranged in the second pipe connected to the introduction pipe. A step of introducing into the introduction pipe, a step of generating ions of the PCB in the ion source unit,
Performing mass analysis of the ions;
Detecting the moisture concentration in the gas inside the exhaust pipe for exhausting the ion source part;
A step of controlling the first flow rate control means based on a moisture concentration detected in the gas so that a moisture concentration in the sample gas introduced into the ion source unit is 1 % or less;
Based on the intensity of the ionic strength and the PCB of ion-of the reference material, chemical monitoring method characterized by a step of determining the concentration of the PCB.

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