JP2002323414A - Quantity-of-residue measuring instrument - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a quantity-of-residue measuring instrument that can quickly measure the quantities of residues left on the surfaces of a washed container and member. SOLUTION: This instrument measures the quantity of the residue 12 left on the surface of, for example, a container 11 which is an object to be measured. The instrument is provided with an aspirator 13 which closely adheres to the surface 11a of the container 11 in a watertight state, a pressure reducing means (not shown in the figure) which reduces the pressure in the aspirator 13, and a vaporizing means 14 which vaporizes the residue 12 sucked into the aspirator 13. This instrument is also provided with a measuring means (mass spectrometer) 50 which measures the produced vapor 15.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a residue measuring device capable of quickly measuring residues remaining on the surfaces of containers and members that have been subjected to a cleaning treatment.

[0002]

2. Description of the Related Art For example, in electrical equipment such as transformers and capacitors, polychlorinated biphenyls (PCBs) having excellent insulating properties have been used as insulating oils. Since these PCBs have an adverse effect on the human body and the environment, their use and production as well as insulators for the above-mentioned electrical equipment are currently prohibited.
For this reason, in the above-mentioned electric equipment and the like using PCBs as insulating oil, the insulating oil is extracted from the inside and subjected to detoxification treatment, and at the same time, members such as containers and components of PCBs with residual adhesion are cleaned. ing.

[0003] In the cleaning treatment of a member having PCBs remaining thereon, conventionally, the member is immersed in an organic solvent such as n-hexane and subjected to ultrasonic cleaning to obtain a concentration of PCBs remaining on the surface of the member. Is repeated until the value becomes equal to or less than a specified value (10 μg / m ² ) (usually about 5 to 6 times).

[0004]

Thereafter, in order to check whether the cleaning is good, for example, a predetermined area is wiped with absorbent cotton or the like, and the wiped material is extracted with an organic solvent to measure a residual amount. An inspection is performed and a predetermined value (for example, in the case of PCB, the surface concentration is 10 μg /
m ² ). However,
There is a problem in that the wipe test requires time and effort and cannot be performed quickly. As a result, when a large amount of harmful substances such as PCBs are processed, a simple and quick determination method is desired.

[0005] In addition to the PCB, when it is necessary to confirm the presence or absence of residual substances in a container and quickly judge the suitability of cleaning, the conventional so-called wiping test takes time, and the emergence of alternative analysis means. Is desired.

[0006] Further, there is a demand not only for the cleaning object but also for measuring the residual amount of PCB such as a member to which PCB has adhered. However, the residual P is extracted by using an organic solvent as described above.
When extracting and analyzing CB, it takes time and effort, and there is a demand for quick measurement.

SUMMARY OF THE INVENTION In view of the above problems, an object of the present invention is to provide a residue measuring apparatus capable of quickly measuring the residue remaining on the surface of a member such as a container subjected to a cleaning treatment and its components. .

[0008]

According to a first aspect of the present invention for solving the above-mentioned problems, there is provided a residue amount measuring apparatus for measuring a residual amount of a residual substance of an object to be measured. A suction device, a pressure reducing means for reducing the pressure inside the container, a vaporizing means for vaporizing a residual substance from the outside of the container, and a measuring means for measuring the vaporized measurement object. The residue amount measuring device is characterized in that:

According to a second aspect of the present invention, there is provided a residue measuring apparatus for measuring a residual amount of a residual substance in an object to be measured. A substantially hemispherical bowl-shaped suction container, a decompression means for depressurizing the inside of the container, a means for introducing a high-temperature gas for vaporization for evaporating a residual substance from the outside into the container, and a vaporization by the introduced high-temperature gas A residual amount measuring apparatus comprising: a measuring means for measuring an object to be measured.

A third aspect of the present invention is the residue measuring apparatus according to the first or second aspect, wherein the vaporization of the residual analysis is performed by introducing a high-temperature inert gas from the outside.

According to a fourth aspect, in the first or second aspect, there is provided a residue amount measuring apparatus, wherein the vaporization of the measuring means is performed by heating a heating means provided in the suction device.

According to a fifth aspect of the present invention, in the first or second aspect, there is provided an apparatus for measuring the amount of residues, wherein a feed pipe for feeding the vaporized measurement object to the measuring means is kept warm.

According to a sixth aspect of the present invention, in the first or second aspect, the measuring means is a mass spectrometer.

According to a seventh aspect of the present invention, there is provided the residue measuring apparatus according to the first or second aspect, wherein the object to be measured is a substance after cleaning of the adhered substance on which the PCB is adhered.

An eighth invention is the residue measuring apparatus according to the second invention, wherein the object to be measured is a member to which the PCB is adhered or a wiping object obtained by wiping the PCB.

A ninth aspect of the present invention is a method for measuring the amount of residue, wherein the amount of PCB adhered to a cleaned product after the cleaning step of the PCB processing equipment is measured using the first to seventh residue amount measuring devices. .

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described, but the present invention is not limited thereto.

[First Embodiment] FIG. 1 is a schematic sectional view of an apparatus for measuring the amount of residues according to the present embodiment, and FIG. 2 is a drawing showing the measurement state. As shown in these drawings, the residue amount measuring device 10 according to the present embodiment includes:
This is a device for measuring the residual amount of the residual substance (for example, PCB) 12 remaining on the surface of the container 11 which is the object to be measured, for example, which is in close contact with the surface 11a of the container 11 which is the object to be measured in a watertight manner. Aspirator 13, depressurizing means (not shown) for decompressing the interior of the aspirator 13, vaporizing means 14 for vaporizing the residual substance in the aspirator 13, and measuring means for measuring the vaporized substance 15 (for example, mass (Analysis device) 50.

In the present embodiment, in the present embodiment, the suction device 13 is made of a material such as a fluororesin (for example, “Teflon (trademark)” that improves the adhesion to the container 11 by changing the material of the lower opening edge 13 a of the hemispherical skirt. No.))) and other materials to improve watertightness so as to shut off the outside. Further, the pressure inside the suction device 13 is reduced by 1 to 760 to
rr, preferably 5 to 200 torr.

Here, in the present embodiment, a feed pipe 16 for feeding the mass spectrometer 50 for analyzing the vapor 15 is provided at the upper end opening of the suction device 13.
An introduction pipe 18 for introducing a high-temperature inert gas 17 is inserted into the supply pipe 16 so that the high-temperature inert gas 17 is introduced into the suction device 13.

As the inert gas 17 to be introduced, for example, helium (He), nitrogen (N ₂ ) or the like is preferably used. Further, the gas is supplied to the gas for 100 to 2 so that the residual substance is vaporized.
It is heated to about 00 ° C. In the present invention,
The vaporizing means is not limited to the present embodiment, and for example, a vaporizing means may be provided inside for vaporizing.

Further, in order to prevent the vaporized residual substance from adhering to the inside of the feed pipe 16 in the course of being introduced into the analyzer, the outer circumferences of the feed pipe 16 and the suction device 13 are heated, for example, by heating means ( Heating means 19 provided with a nichrome wire or the like is used.

FIG. 3 is a perspective view of the container as viewed from the opening side.
And measuring the residual concentration using the opening D as a predetermined opening diameter.
Are doing. For example, taking a PCB as an example, a transformer
The residual concentration on the surface of the container is 10 μg / m ^TwoStipulated
And the component parts etc. are less than 0.01mg / kg
Stipulated.

[Second Embodiment] FIG. 4 is a schematic sectional view of a residue measuring apparatus according to a second embodiment. As shown in FIG. 4, the residue amount measuring apparatus 10 according to the present embodiment includes a measuring object such as a container piece, an insulator, various crushed pieces, a coil (including a cut piece) or the like constituting a transformer or a capacitor. An apparatus for measuring the residual amount of a residual substance (for example, PCB) 12 remaining on the surface of a measurement object 21, a flat plate 22 having a smooth surface on which the measurement object 11 is placed, and a watertight state with the flat plate 22 Suction device 1
3, depressurizing means (not shown) for depressurizing the inside of the suction device 13, and vaporizing means 1 for evaporating the residual substance in the suction device 13
4 and a mass spectrometer 50 which is a measuring means for measuring the vaporized residual substance 15.

In the present embodiment, an infrared heater 23 is provided inside the suction device, and the inner surface of the suction device 13 is a reflection surface that reflects the infrared light well.

In the measurement, an object to be measured is placed on the flat plate 22, the object is covered with a suction device, and the pressure is reduced by an external pressure reducing means to a predetermined pressure. The substance is being vaporized.

According to the residual amount measuring apparatus of the present embodiment, the apparatus of the first embodiment is in direct contact with the apparatus of the first embodiment to measure the residual concentration on the surface. The residual amount of the object can be measured.

The object to be measured in the present embodiment is not limited to the member after cleaning, but may be, for example, a member to which PCB is adhered or a harmful substance such as a wiped object obtained by wiping harmful substances such as PCB. The amount may be measured.

[Third Embodiment] FIG. 5 is an example of a schematic diagram of a mass spectrometer for measuring the residue of the residue measuring apparatus according to the present embodiment. As shown in FIG. 5, an organic halide detection device 50 according to the present embodiment is shown.
Is a detection device for detecting the concentration of the organic halide in the vaporized residue, a capillary column 54 which is a sample introduction means for continuously leaking the vaporized substance 51 into the vacuum chamber 52 and introducing it as a molecular beam 53, A laser irradiation means 54 for irradiating the leaked molecular beam 53 with a laser beam 55 for laser ionization, a converging section 56 composed of a plurality of ion electrodes for converging the laser ionized molecules, and selectively concentrating the converged molecules. It comprises an ion trap 57 and a time-of-flight mass spectrometer 60 provided with an ion detector 59 for reflecting ions emitted at a constant period by a reflectron 58 and detecting the reflected ions. . Then, from the comparison of the signal intensities detected by the detector 59, the PCB concentration of the measurement target can be obtained. The measured PCB concentration is sent to a cleaning facility or a monitoring command room to monitor the suitability of cleaning in the cleaning process.

FIGS. 6A and 6B show signals from the ion detector which detected PCB. Here, the horizontal axis is the flight time (second), and the vertical axis is the ion signal intensity (V). FIG. 2B is an enlarged view of FIG. 6A for the 4-chlorine PCB. By using this measurement system, the detection sensitivity of the PCB concentration is 0.01 mg / N.
High sensitivity and rapid analysis with m ³ and detection time within 1 minute is possible.

[Fourth Embodiment] Next, a PCB detoxification treatment facility using a residue amount measuring apparatus of the present invention will be described with reference to FIG. As shown in FIG.
The B detoxification processing system is a harmful substance treatment system for detoxifying an object to be treated on which a harmful substance, PCB is attached, contained, or stored. A separation means 1004 for separating the harmful substance 1002 from the container 1003 to be stored, and a pretreatment means 1006 having one or both of the disassembly means 1005 for disassembling the constituent materials 1001a, b,. Core separating means 1007 for separating a core 1001a, which is a constituent material of the object to be processed, in the preprocessing means 1006 into a coil 1001b and an iron core 1001c; Coil separating means 10
08, the iron core 1001c separated by the core separation means 1008 and the metal container (container body and lid etc.) 1003 separated by the disassembly means 1005 and the copper wire 1001 separated by the coil separation means 1008
a cleaning means 1011 for cleaning d with a cleaning liquid 1010; a harmful substance decomposition processing means 1013 for decomposing one or both of a cleaning waste liquid 1012 after cleaning and a harmful substance 1002 separated by the pretreatment means; PC remaining on the surface of containers 1002 and inorganic materials 1008 such as coils and iron cores cleaned in 1011
And a measuring means 1016 for measuring the B concentration with the above-described measuring device.

The harmful substances to be detoxified in the present invention include, in addition to PCBs, for example, vinyl chloride sheets, hazardous waste paints, waste fuels, hazardous chemicals, waste resins, untreated explosives and the like. However, as long as it is a harmful substance caused by environmental pollution, it is not limited thereto.

Examples of the object to be treated in the present invention include, for example, transformers and capacitors using PCB as an insulating oil, and storage containers for storing paints that are harmful substances. It is not limited.

Also, in the ballast for fluorescent lamps, PCB has been conventionally used, so that it is necessary to perform detoxification treatment. In this case, since the capacity is small, it is not necessary to perform pretreatment and directly to the separation means 1009. Detoxification treatment can be performed by charging.

When the harmful substance is a liquid or the like,
Detoxification processing is performed by directly charging the harmful substance decomposition processing means 1013, and the stored container can be processed by detoxification processing of the constituent materials. It is necessary to confirm that the liquid after the treatment is 3 ppb or less, which is the PCB discharge standard. Although various decomposing apparatuses can be used for the configuration of the harmful substance processing means 1013, it is more preferable to use a high-temperature and high-pressure hydrothermal decomposition apparatus using sodium carbonate.

FIG. 8 schematically shows a hydrothermal apparatus. As shown in FIG. 8, the hydrothermal decomposition apparatus 120 includes a cylindrical primary reactor 122 provided with a cyclone separator 121, and a PC.
B, a pressurizing pump 124 for pressurizing the processing liquid 123 of H ₂ O and NaOH, and a preheater 125 for preheating the mixed liquid
, A secondary reactor 126 having a configuration wound with piping, and a cooler 1
27 and a pressure reducing valve 128. Further, a gas-liquid separator 129 and an activated carbon tank 130 are disposed downstream of the pressure reducing valve 127, and the exhaust gas (CO ₂ ) 131
Is discharged from the chimney 132 to the outside, and the wastewater (H ₂ O, Na
Cl) 133 is separately subjected to drainage treatment as needed. In addition, H ₂ is supplied to the piping 134 of the PCB that becomes the processing liquid 123.
O and NaOH are each introduced. The oxygen pipe 135 is directly connected to the primary reactor 125.

In the above apparatus, the pressure inside the primary reactor 122 is increased to 26 MPa by pressurization by the pressurizing pump 124. Further, the preheater 125 preheats the mixed treatment liquid 123 of PCB, H ₂ O and NaOH to about 300 ° C. Further, oxygen is jetted into the primary reactor 122, and the temperature rises to 380 ° C to 400 ° C due to internal reaction heat. The cyclone separator 121 includes a primary reactor 122
The large Na ₂ CO ₃ crystal particles precipitated inside are separated, and the fine particles of Na ₂ CO ₃ are sent to the secondary reactor 126. The operation of the cyclone separator 121 prevents the secondary reactor 126 from being blocked. By this stage, the PCB
Causes a dechlorination reaction and an oxidative decomposition reaction,
1, CO ₂ and H ₂ O. Next, in the cooler 127, the fluid from the secondary reactor 126 is cooled to 100 ° C.
At the same time, the pressure is reduced to atmospheric pressure by the pressure reducing valve 128 at the subsequent stage. Then, the CO ₂ and steam and the treated water are separated by the gas-liquid separator 129, and the CO ₂ and steam pass through the activated carbon tank 130 and are discharged into the environment.

The PCB processing system according to the present embodiment comprises a container 1002 and a coil
This is for determining the concentration of PCB adhering to the surface of an inorganic substance 1008 such as an iron core.

By providing this measuring system, it is possible to quickly and efficiently monitor the suitability of the cleaning in the cleaning process. As a result, the disassembly process can be performed while always monitoring whether the cleaning process is being performed properly. If a cleaning defect is found, the cleaning process can be performed again. Eliminating pollutants to the outside, and taking environmentally friendly measures.

[0040]

As described above, according to the first aspect of the present invention, there is provided a residue amount measuring device for measuring a residual amount of a residual substance of an object to be measured, wherein the apparatus is provided in a watertight state. A suction device that is in close contact with the container, a pressure reducing unit that reduces the pressure in the container, a vaporizing unit that vaporizes a residual substance in the container from outside, and a measuring unit that measures the vaporized measurement target. Therefore, harmful substances remaining on the surface of the measurement object can be quickly measured.

According to a second aspect of the present invention, there is provided a residue measuring apparatus for measuring a residual amount of a residual substance in an object to be measured, wherein the flat plate on which the object is mounted is in close contact with the flat plate in a watertight state. A substantially hemispherical bowl-shaped suction container, a depressurizing means for depressurizing the inside of the container, a means for introducing a high-temperature gas for vaporizing a residual substance from the outside into the container, and the introduced high-temperature gas. Since it is provided with a measuring means for measuring the vaporized measurement target, the residual amount of the harmful substance can be easily and quickly measured even when the measurement target is not a smooth surface or even in a component (fragment, etc.). .

According to the third invention, in the first or second invention, the vaporization of the residual analysis is performed by introducing a high-temperature inert gas from the outside. Hazardous substances remaining on the surface of the object to be measured can be quickly measured by performing the measurement quickly.

According to the fourth aspect, in the first or second aspect, since the vaporization of the measuring means is performed by heating the heating means provided in the suction device, the heating means is provided without providing the inert gas introducing means. By means, harmful substances can be vaporized.

According to a fifth aspect of the present invention, in the first or second aspect, the feed pipe for feeding the vaporized measurement object to the measuring means is kept warm, so that vaporized harmful substances are contained in the feed pipe. High precision analysis can be performed without adhesion.

According to the sixth aspect, in the first or second aspect, since the measuring means is a mass spectrometer, it is possible to analyze harmful substances with high accuracy.

According to the seventh aspect, in the first or the second aspect, since the object to be measured is the one after cleaning of the adhered substance on which the PCB is adhered, it is possible to quickly measure the residual amount of the PCB. it can.

According to an eighth aspect, in the second aspect, the object to be measured is a member to which a PCB is attached or a PCB
Therefore, the residual amount of the PCB and the remaining amount of the wiped object can be quickly measured.

According to the ninth aspect of the present invention, the amount of PCB attached to the cleaned product after the cleaning process of the PCB processing equipment is measured using the first to seventh residual amount measuring devices. The residual amount can be quickly measured without requiring such time.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view showing an example of a residue amount measuring device according to a first embodiment.

FIG. 2 is a perspective view illustrating an example of a residue amount measuring device according to the first embodiment.

FIG. 3 is a perspective view showing an example of a residue amount measuring device according to the first embodiment.

FIG. 4 is a perspective view illustrating an example of a residue amount measuring apparatus according to a second embodiment.

FIG. 5 is a schematic diagram of an organic halide detection device according to a third embodiment.

FIG. 6 is a graph showing measurement results of low chlorine PCB.

FIG. 7 is a schematic diagram of a PCB detoxification processing system according to a fourth embodiment;

FIG. 8 is a schematic diagram of a hydrothermal decomposition apparatus.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Residual amount measuring apparatus 11 Container 12 Residual substance (for example, PCB) 13 Aspirator 14 Vaporizing means 15 Vaporized substance 22 Flat plate 23 Infrared heater 50 Measurement means (for example, mass spectrometer)

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2G052 AB22 AC11 AD32 AD42 AD52 CA04 CA12 CA14 DA01 DA13 EB01 EB11 GA24 JA07 JA08 JA09

Claims (9)

[Claims] 1. A residue amount measuring device for measuring a residual amount of a residual substance of an object to be measured, comprising: a suction device which is in close contact with the object to be measured in a watertight state; An apparatus for measuring the amount of residue, comprising: vaporizing means for vaporizing a residual substance from the outside in the container; and measuring means for measuring the vaporized measurement target. 2. A residue amount measuring apparatus for measuring a residual amount of a residual substance of an object to be measured, comprising: a plate on which the object to be measured is placed; and a substantially hemispherical shape which is in tight contact with the plate in a watertight state. A bowl-shaped suction container, a decompression means for depressurizing the inside of the container, a means for introducing a high-temperature gas for vaporization for evaporating a residual substance from the outside into the container, and a measuring object vaporized by the introduced high-temperature gas. A residue measuring device, comprising: a measuring means for measuring. 3. The apparatus according to claim 1, wherein the residual analysis is performed by introducing a high-temperature inert gas from the outside. 4. An apparatus according to claim 1, wherein said measuring means is vaporized by heating a heating means provided in said suction device. 5. The residual amount measuring apparatus according to claim 1, wherein a supply pipe for supplying the vaporization measurement target to the measurement unit is kept warm. 6. The residual amount measuring apparatus according to claim 1, wherein the measuring means is a mass spectrometer. 7. The residual amount measuring apparatus according to claim 1, wherein the object to be measured is a substance after cleaning of the adhered substance to which the PCB is adhered. 8. The residual amount measuring apparatus according to claim 2, wherein the object to be measured is a member to which PCB is attached or a wiped object obtained by wiping PCB. 9. A PC for a cleaned product which has been subjected to a cleaning process of a PCB processing facility using the residue amount measuring apparatus according to claim 1.
A method for measuring the amount of residues, wherein the amount of B is measured.