JPH07151653A - Sample kit and sampling/analyzing method - Google Patents

Abstract

PURPOSE:To provide a sample kit which can be transferred in clean state from a measuring position to an analyzing position. CONSTITUTION:A unit for capturing gas/particle component in the air, a suction unit, and an exhaust unit are coupled into a set and housed in a nonmetallic portable box 10 thus providing a sample kit which can be transferred easily by human power or a light car. The capturing unit, the suction unit, and the exhaust unit are cleaned at a place of required cleanliness and then the units are coupled, as a set, through a tube thus providing a sample kit. The sample kit is housed in a nonmetallic portable box 10 in order to protect against contamination and transferred to a measuring position.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sampling kit used for sampling and analysis in a clean room and the like and a method of using the same.

[0002]

2. Description of the Related Art In recent years, as semiconductor circuit patterns have become finer and the devices have become higher in density and higher in integration, the importance of making the manufacturing process clean has increased.

Factors that cause a reduction in cleanliness include various factors such as peeling contamination of clean room members, corrosion contamination of equipment materials, dust contamination due to equipment maintenance work, and new dust contamination associated with the expansion of automation of automatic conveyance equipment. It is becoming more and more difficult, and its analysis is becoming more and more difficult. By controlling the behavior and state by locating the source and components of the generation, the performance and reliability of the product will be greatly improved.

Up to now, it has been reported that clean room air and outdoor air are sampled and analyzed by using ultrapure water as an absorbing liquid. It is not enough. Further, when it comes to analysis of clean room air, the analysis sensitivity needs to be in the range of ng / m ³ , and therefore an analytical instrument without contamination and a highly sensitive measuring instrument are needed. In order to carry out these analyses, advanced technology that makes full use of instruments and equipment is also essential.

[0005] In sampling, especially in a clean room, the required level of analysis is extremely small, so unless you are an analytical engineer who is well trained and trained in this kind of analysis, the sample (absorption liquid) may be in the middle of sampling. Will be contaminated with more than the amount of analytical components, and the accuracy of analysis will be lost. However, clean rooms that require analysis of ultra-trace amounts of impurities in the ng / m ³ level in air are mainly used by leading-edge companies such as semiconductor manufacturers, and products, equipment, manufacturing processes, etc. in such clean rooms are In most cases, it is confidential to the outside world. For this reason, some companies are reluctant to have outside measurement engineers enter the clean room to perform sampling work.

The conventional sampling operation procedure is as follows. The absorption bottle, absorption liquid, suction pump, connecting tube, and other equipment are carried separately to the sampling destination. Enter the sampling destination (in a clean room), put the absorbing solution in the absorption bottle, and connect the absorption bottle and suction pump with the connecting tube. All connection operations are done manually by the sampling engineer. Aspirate for a fixed time at a constant suction flow rate. The sampling engineer adjusts the suction pump. After sampling is complete, remove all connected absorption bottles and suction pumps. Put the absorbing solution (which will be the analytical sample) in the absorption bottle into another container, then take it back and perform the measurement.

In these operations, the level to be analyzed is g.
In the case of (gram) and mg (milligram), the amount of contamination from the operation is negligible even if the sampling person is not selected. However, when the detection level is extremely small amount of μg (microgram) and ng (nanogram), the amount of contamination in the sampling operation may be much larger than the target component amount depending on the person performing the sampling operation. .

In order to prevent contamination in such a sampling operation, a highly skilled engineer who has acquired attention to contamination in performing micro trace analysis at the μg to ng level and a technique for sampling so as not to contaminate. Will become indispensable. Also, if a person other than such a highly skilled technician performs sampling, a system that does not cause contamination by the person sampling the sample is required.

[0009]

In the conventional sampling, the sample after sampling is exposed to the outside air and contaminated during transportation. When a sampling operator manually performs the operation as in the conventional case, in a place where sampling is performed (in a clean room), an absorption liquid is put into an absorption bottle, and in an operation of connecting the absorption bottle-aspiration pump with a connection tube, There is a very high possibility that the absorption liquid is contaminated by the operation of taking in and out the absorption liquid at this sampling location, and in many cases, the absorption liquid is contaminated. In addition, the air to be sampled is discharged from the absorption bottle containing the absorption liquid to the outside through a suction pump, but when exhausted into the clean room, dust is generated from the suction pump or the absorption liquid is a dilute acidic solution. Since the exhaust gas after being absorbed becomes acidic, exhausting it to a clean room as it is may adversely affect the manufacturing process.

[0010]

SUMMARY OF THE INVENTION In the present invention, a sampling kit that can be moved from a sampling place to an analysis place in a clean state so that the sampling equipment does not come into direct contact with the outside air during transportation, and this sampling kit. It is an object of the present invention to provide a method for easily performing sampling and analysis at a remote place using a kit.

For this purpose, the present invention is a non-metallic device that is capable of collecting gas and particle components in the air and connecting a collecting device, a suction device, and an exhaust device into a set and transporting these devices. It has a configuration of a sampling kit that is housed in a flexible box and can be easily transported by human power or light vehicle. Further, the above-mentioned collection device may be composed of an absorption bottle having an absorption liquid and a suction port provided with a cap, the suction device may be equipped with a suction pump, and the exhaust device may be equipped with an exhaust tube. The suction pump used here is preferably a constant flow rate type, and may be further equipped with a flow meter. In addition, this exhaust system neutralizes the exhaust after passing through the absorption bottle using dilute acid solution as the absorption liquid, and prevents dust in the suction pump from reducing the cleanliness in the clean room and collecting dust. In addition, an exhaust treatment bottle containing the exhaust treatment liquid may be provided.

The collecting instrument, the suction device, and the exhaust device are connected by a tube having a valve, and the valve can open and close the flow path between the devices and the instrument. In addition, the box containing this sampling kit is packed with vinyl to prevent contamination during transportation,
In addition, it may be stored in a dedicated outer box and transported.

Further, according to the present invention, in the method for sampling and analyzing gas / particle components in air, a collecting instrument and a suction device capable of collecting gas / particle components in air at a place having a required cleanliness, and Clean the exhaust system and put these instruments into a set to connect them with tubes to make a sampling kit, store it in a non-metallic box that can be transported without contamination, and transport the sample kit to the sampling location for cleaning. Open this box and perform the necessary operations in this state, perform sampling with the sampling kit still connected in the box, and store the sampling kit again in this box to prevent contamination after sampling. , Carry this sampling kit even in a place away from the sampling place for analysis.

In this sampling kit, the collection device may include an absorption bottle having an absorption liquid and a suction port covered with a cap, the suction device may have a suction pump, and the exhaust device may have an exhaust tube. . Further, the exhaust device may include an exhaust treatment bottle having an exhaust treatment liquid, and may be connected between the suction pump and the exhaust tube. In addition, in this sampling and analysis method, in order to prevent contamination during transportation, a box containing a sampling kit in which a collection device, a suction device and an exhaust device are connected together and connected by a tube is further packed with vinyl. It may be packed from the top in a dedicated outer box.

As the material of the equipment and the equipment which come into contact with the sampling air and the absorbing liquid, a material having an elution amount equal to or less than the total amount of trapped target impurities in the air to be trapped is used. And the elution amount is the time (days) required for sampling by filling the same collection device with the same collection liquid that collects the target impurities (target component to be analyzed).
After leaving it for the same period, analyze and confirm.

[0016]

With these configurations, in the present invention, a box containing a sampling kit, which is obtained by connecting a collecting instrument, a suction device, and an exhaust device in advance, is brought to a sampling place, the box is opened, and the box is opened. Inside, a sampling kit is connected and set to a predetermined arrangement for sampling to perform sampling. After sampling, set the sampling kit in this box for transportation, store it in the box, and transport it to the analysis site. At the analysis site, open the box again and collect the absorbent from the absorption bottle in the sampling set for analysis.

[0017]

The present invention will be described in more detail with reference to the accompanying drawings. Note that these examples are one of the embodiments according to the present invention, and the present invention is not limited to these embodiments.

1 to 4 show a first embodiment of a sampling kit according to the present invention, and FIG. 5 shows a second embodiment of the present invention. Note that the description common to each embodiment will be omitted.

In FIG. 1, 1 is a suction port for sucking gas in the air, and 2 is a sealing cap for covering the suction port during transportation. The suction port 1 can be moved in a box 10 described later, and can project from an opening 11 provided in a part of the box for sucking outside air at the time of sampling. 3 is an absorption bottle that has an absorption liquid selected according to the sampled gas or analyte, such as transparent quartz glass or borosilicate glass that has a low content of metal impurities and almost no elution or adsorption of components. Made of glass.

A suction pump 4 is of a double diaphragm type in this embodiment.
As shown in FIG. 2, this suction pump 4 has this box 1
A control unit 9 is arranged corresponding to an opening provided in a part of the box 0, and can be operated from the outside of the box 10. The control unit 9 is provided with an operation switch, a timer switch, a display device, a flow rate adjusting dial, a flow rate meter and the like.

Reference numeral 5 denotes an exhaust treatment bottle having an exhaust treatment liquid. When the sampled air is exhausted from the absorption bottle 3 containing the absorption liquid to the outside of the box 10 via the suction pump 4, the suction pump 4 discharges the air. Against the dust and the exhaust gas of acid that passes through the absorption liquid of the dilute acid solution in the absorption bottle 3,
In this embodiment, the exhaust treatment bottle 5 contains ultrapure water for dust and dilute alkaline solution for acid exhaust. Further, 6 is an exhaust tube joint for discharging exhaust gas to the outside. If necessary, an exhaust tube is connected to the exhaust tube joint 6, and the end of the exhaust tube is lowered to the grating or brought to an appropriate exhaustable place.

Reference numeral 7 is a tube made of Teflon or silicon for connecting these devices, and a cock 8 which is one type of valve made of Teflon attached to the tube 7.
Between the suction port 1 and the absorption bottle 3, the absorption bottle 3 and the suction pump 4
During, the suction pump 4 and the exhaust processing bottle 5, and between the exhaust processing bottle 5 and the exhaust tube joint 6 are opened and closed between the respective devices. With this cock, there is no need to connect each device in a clean room as in the conventional case, and each device is connected in advance with a tube 7 at the assembly site of the sampling kit, and these cocks 8 close the flow path. If this is done, it will be less likely to be contaminated during transportation or to move, leak or mix the processing liquid between each equipment, etc.
Moreover, by simply opening these cocks 8 at the time of sampling, the sampling state can be set without worrying about contamination of each instrument by the sampling operator.

The groups of the suction port 1, the absorption bottle 3, etc. and the groups of the suction pump 4, the exhaust bottle 5, etc. are set on different mounts so that the tip of the suction port 1 projects out of the box 10. The frame 12 on which the suction port 1 and the suction bottle 3 are set is slidable inside the box 10 so that the tip of the suction port 1 can project from the opening 11 of the box 10.

Numeral 10 is a non-metallic box for accommodating these devices as a group and is preferably sized so that a person can easily carry them.

These instrument and device materials also include resins,
In particular, polyethylene resin, polypropylene resin, poly-4-methylpentene-1 resin, polystyrene resin,
Polyvinyl chloride resin, fluorine resin, methacrylic acid ester resin, acrylonitrile resin, polyamide resin, polycarbonate resin, polyether resin,
It may be a thermoplastic polyester resin, or a mixture selected from two or three or more.

When the above-mentioned sampling equipment is stored in this box 10, it is carried out in a clean room having a cleanness equal to or higher than the clean room at the sampling place. Then, outside the clean room, it is packed with vinyl from above, and further housed in a dedicated outer container made of PP resin. In this embodiment, this packed outer container preferably has a size and weight of a trunk that can be manually transported, and can be easily moved from a sampling kit assembly place to a sampling place by a human carrier or a carrier such as a courier. Be transported to.

The sampling kit moved to the sampling place is unpacked from its outer container and vinyl, and carried into a clean room where it is sampled according to a predetermined cleaning procedure.

After the sampling kit carried in is installed at the sampling place, the lid 13 of the box 10 can be opened. At this time, sampling workers use the gloves attached to this sampling kit to prevent contamination. Then, the gantry 12 on which the suction port 1 and the absorption bottle 3 are placed is slid in the box 10 toward the opening 11 provided in the box 10 so that the suction port 1 projects from the opening 11. Next, the cocks 8 that are provided in the tubes 7 that connect the respective devices and that close the flow paths are opened.

The lid 1 of the box 10 is then understood as seen from the perspective view of the upper part of the sampling kit in the box of FIG.
3 is closed and the protrusion 14 provided inside the lid 13 is engaged with the notch 15 provided at the upper portion of the gantry 12 to fix the gantry 12 to the box 10 at the time of sampling. There is another notch 16 on the upper part of the gantry 12, which is closed when the gantry 12 is sliding to the rear inside the box 10 when being transported, so that the notch 16 and the protrusion of the lid 13 are closed. This is to prevent the suction port 1 from projecting from the opening 11 by engaging with 14 and fixing the pedestal 12 so as not to move inside the box 10. The exhaust tube joint 6 and the power cord of the suction pump 4 are removed from the side of the box 10. An exhaust tube is connected to the exhaust tube joint 6 as necessary as described above. The power cord of the suction pump 4 is connected to a predetermined power source.

The operation switch of the control unit 9 of the suction pump 4 is operated to operate the suction pump 4. At this time, the timer switch is set to a predetermined time for sampling and is linked. The flow rate is also set to a predetermined value by adjusting the flow rate adjusting dial and using a flow meter.

After the lapse of a predetermined sampling time, the suction pump 4 is stopped by the operation switch, the sealing cap 2 is attached to the suction port 1, and each cock 8 is closed.
Slide the gantry 12 inside the box 10, close the lid 13 and engage the protrusion 14 inside the lid 13 with the other notch 16 on the top of the gantry 12, fix it so that it will not move during transportation, and suck. Remove the power cord of the pump 4 and the exhaust tube joint 6 and collect them on the side of the box 10.

The sampling kit stored in the box 10 is taken out of the clean room, and the box 10 is repackaged with the above-mentioned vinyl and the outer box in the reverse order of unpacking and transported to the analysis place.

The sampling kit transported to the analysis site is removed from the outer box container and vinyl,
In the clean room, the absorbing liquid is taken out from the absorbing bottle 3 and each required analysis is performed.

In the above embodiment, in order to pull the suction port 1 out of the box 10, the frame on which the suction port 1 and the absorption bottle 3 are mounted is slid in the box 10. Only 1 is slidably installed inside the box 10 and connected by a tube, and this suction port 1
It may be configured such that only the end of the box is slid so that the tip of the box is projected from the box 10 to be fixed, and the box is retracted from the box during transportation.

FIG. 5 shows a second embodiment of the present invention. In this embodiment, the main structure is the same as that of the first embodiment, and a reference bottle 17 having a reference liquid is further provided in the box 10 as compared with the first embodiment. The reference bottle 17 is made of the same material as the absorption bottle 3, and the reference liquid is the same as the absorption liquid, and the reference liquid 17 is placed in a sealed state on the reference liquid. With this configuration,
By simultaneously analyzing the components of the reference liquid in the reference bottle 17 during the analysis of the absorption liquid, the elution amount of the absorption bottle into the absorption liquid can be known, and the accuracy of the analysis result can be further improved.

In each of the embodiments, an inverted U-shaped device may be installed inside the box and liquids different from each other may be put in the respective ends in order to confirm the fall. As a result, if the liquid falls over during transfer, these liquids are mixed and the fall can be confirmed. Further, the box itself may have a double structure so that the power source of the exhaust tube and the suction pump is easy to carry and the sampling equipment is not contaminated, and these instruments may be put in one of them. Although the above is concerned with sampling air in a clean room, it should be understood that the apparatus of the present invention can also be used to analyze ambient air for internal and external comparisons. It should be noted that a clean room designed for class 1000 or less requires a cleanness on the order of ng, and it is preferable that the sampling kit of the present invention is fully equipped with vinyl and an outer box for transportation.

[0037]

[Effect] In the present invention, the epoch-making thing is that the assembly of the first sampling kit is performed by a worker who is skilled in the analysis of cleanliness, and the sampling is performed by the person in charge of each company in a confidential place of each company. It is easy to carry out without worrying about contamination that would adversely affect the sampling equipment and the measurement results, and further, the analysis can be appropriately carried out by a skilled worker at a place away from the confidentiality of each company. That is, each company can measure a high degree of cleanliness without putting an outside person in the place of confidentiality.

[Brief description of drawings]

FIG. 1 is a configuration diagram of a first embodiment of a sampling kit according to the present invention.

FIG. 2 is a perspective view of the outer shape of the box during transportation of the sampling kit of FIG.

3 is an overall view of the inside of the sampling kit of FIG.

FIG. 4 is a perspective view showing the upper part of the sampling kit in the box of the sampling kit of FIG. 1.

FIG. 5 is a configuration diagram of a second embodiment of a sampling kit according to the present invention.

[Explanation of symbols]

 1 Suction Port 2 Sealing Cap 3 Absorption Bottle 4 Suction Pump 5 Exhaust Treatment Bottle 6 Exhaust Tube Joint 7 Tube 8 Cock 9 Suction Pump Controller 10 Box 11 Box Opening 12 Frame 13 Box Lid 14 Protrusions 15, 16 Notch 17 Reference Bottle

Claims (23)

[Claims] 1. A collection device capable of collecting gas / particle components in air, a suction device and an exhaust device are connected to form a set, and these devices are housed in a transportable non-metallic box. , A sampling kit that enables easy transportation by human power or light vehicle. 2. The sampling kit according to claim 1, wherein the collection device includes an absorption bottle for containing an absorption liquid and a suction port shielded from the outside by a cap. 3. The sampling kit according to claim 1, wherein the suction device is composed of a suction pump. 4. The exhaust device according to claim 1, wherein the exhaust device includes an exhaust tube and / or an exhaust treatment bottle having an exhaust treatment liquid, and is arranged after the suction device. Sampling kit. 5. The tube is used to connect the collecting device, the suction device, and the exhaust device, and each flow path is opened and closed by a valve attached to a main part of the tube. Item 5. The sampling kit according to any one of items 1 to 4. 6. The sampling kit according to claim 1, wherein the box is made of resin to prevent contamination from the box. 7. The suction port is movably installed, is fixedly housed inside the box at the time of transportation, and is fixed so as to project from an opening provided in the box at the time of sampling. The sampling kit according to any one of 1 to 6. 8. The suction port, the collection device group, the suction device, and the exhaust device group are set on different mounts, and the tip of the suction port projects outside the box during preparation before sampling. When the suction port is moved so that the suction port and the collection tool are set inside the box, the tip of the suction port is projected from the opening of the box. , The pedestal is fixed by closing the lid of the box during sampling, and the pedestal is fixed by closing the lid of the box with the suction port retracted from the opening and stored in the box during transportation. 7. The structure according to claim 1, wherein
The sampling kit according to any one of 1. 9. An operating glove is attached so that a sampling operator can operate the sampling kit without contamination.
The sampling kit according to any one of 1. 10. The sampling according to any one of claims 1 to 9, wherein the sampling kit is further wrapped in vinyl and housed in a dedicated outer box to prevent contamination during transportation. kit. 11. The device according to claim 1, wherein the device is made of a material having an elution amount equal to or less than the total amount of trapped target impurities in the air to be trapped.
0. The sampling kit according to any one of 0. 12. The material of the device is borosilicate glass,
The sampling kit according to claim 1, wherein the sampling kit is made of glass such as quartz glass. 13. The material of the device is polyethylene resin, polypropylene resin, poly-4-methylpentene-1 resin, polystyrene resin, polyvinyl chloride resin, fluorine resin, methacrylic acid ester resin, acrylonitrile. 12. A resin, a polyamide resin, a polycarbonate resin, a polyether resin, a thermoplastic polyester resin, or a mixture of two or more selected from three or more. The sampling kit according to any one of 1. 14. The sampling kit according to claim 1, further comprising a reference bottle having a reference liquid. 15. The sampling kit according to claim 1, further comprising a tipping confirmation device. 16. The sampling kit according to claim 15, wherein the falling confirmation device has an inverted U shape, and has different liquids at both ends thereof. 17. A sampling device, a suction device, and an exhaust device capable of collecting gas / particle components in air at an assembly place having a required cleanliness in a method for sampling and analyzing gas / particle components in air. The sample kit is cleaned and stored in a non-metallic box that can be transported so as not to be contaminated by connecting these instruments as a set and connecting them with a tube to transport the sample kit from the assembly site to the sampling site. Open the box and perform necessary operations in a clean state, perform sampling with the sampling kit still connected in the box, and put the sampling kit in the box to prevent contamination after sampling. And the analysis can be carried by transporting the sampling kit at a location remote from the sampling location. And a sampling and analysis method characterized by. 18. The sampling and analysis method according to claim 17, wherein the collection device includes an absorption bottle having an absorption liquid and a suction port covered with a sealing cap. 19. The sampling and analysis method according to claim 17, wherein the suction device has a suction pump. 20. The exhaust device comprises an exhaust tube and / or an exhaust treatment bottle having an exhaust treatment liquid, and is arranged after the suction device.
9. The sampling and analysis method according to any of 9. 21. The absorption liquid is put in the absorption bottle in a clean room in advance so that the collected sampling set can be easily handled and sampled without being contaminated by the minimum necessary operations, The exhaust treatment liquid is put in an exhaust treatment bottle, and further, the tube is used to connect between the collecting instrument, the suction device, and the exhaust device, and the tube is operated by operating a valve provided on the tube. The flow path is set in a closed state, and at the time of sampling, the sampling operator opens the projection of the suction port to the outside of the box and opens the flow path of the tube by operating a valve provided on the tube. 21. The method according to claim 17, wherein the exhaust device is connected to the outside and the suction device is set and driven. Sampling and analysis methods listed. 22. The box containing the sampling kit in which the collection device, the suction device and the exhaust device are connected together by a tube is further packed in vinyl, and then is packed in a dedicated outer box for transportation. The sampling and analysis method according to any one of claims 17 to 21, which further prevents contamination at the time. 23. The sampling and analysis method according to claim 17, wherein the sampling kit further comprises a reference bottle having a reference liquid.