CN107845585B - On-line pollution monitoring system and method - Google Patents
On-line pollution monitoring system and method Download PDFInfo
- Publication number
- CN107845585B CN107845585B CN201610833793.4A CN201610833793A CN107845585B CN 107845585 B CN107845585 B CN 107845585B CN 201610833793 A CN201610833793 A CN 201610833793A CN 107845585 B CN107845585 B CN 107845585B
- Authority
- CN
- China
- Prior art keywords
- sample
- line
- monitoring system
- pollution monitoring
- transmission
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67242—Apparatus for monitoring, sorting or marking
- H01L21/67253—Process monitoring, e.g. flow or thickness monitoring
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an online pollution monitoring system and method. The on-line pollution monitoring system of the present invention is characterized by comprising: a sampling unit (100) that introduces a chemical through a line connected to a point where the chemical is used, stored, or supplied, and generates a transmission sample to be transmitted; and a main system (200) receiving the transmission sample from the sampling unit and analyzing the transmission sample by the analyzer, wherein the main system is radially connected to a transmission line (300) through a plurality of sampling units arranged in a dispersed manner, and the non-reactive gas of the transmission sample is transmitted in an encapsulated state in the transmission line at the front and rear.
Description
Technical Field
The present invention relates to an On-line contamination monitoring system and method, and more particularly, to a system and method for On-line monitoring of contamination of chemicals used in a semiconductor manufacturing process or the like in real time.
Background
Currently, in the advanced manufacturing industry such as semiconductor manufacturing processes, very small amounts of contamination are the most important cause of profitability and productivity. Thus, when an extremely small amount of a contamination source is analyzed in real time in a production process, a large number of defects caused by contamination can be prevented, and yield and productivity can be improved.
However, production equipment in the manufacturing industry of semiconductors and the like is distributed on a mass production line, and the points where monitoring of chemicals is required are also distributed over a wide area due to the long distance between tanks in the chemical manufacturing industry. In order to monitor the chemical, an analyzer is provided at each of the monitoring points dispersed as shown above, but there is a problem that it involves a considerable investment in a relatively expensive analyzer.
As a solution to this problem, when one analyzer is disposed at a distance substantially in the middle of the monitoring point and a sampling unit is provided for sampling at each point and transferring the sample to the analyzer, a system sharing the analyzers at high cost can be configured. However, when the reliability or efficiency of a system that transfers a sample collected by the above-described method to an analyzer and analyzes the sample is reduced, there is a problem that the topology (topology) cannot be applied.
The above-described problems and problems of the prior art have been explained, but the knowledge of the problems and problems is not known to those of ordinary skill in the art of the present invention.
Disclosure of Invention
The invention aims to provide an online pollution monitoring system and method, which can transmit a sample from a plurality of monitoring points to an analyzer for analysis and can ensure reliability and efficiency.
An online pollution monitoring system of an embodiment of the present invention includes: a sampling unit that introduces a chemical through a line connected to a point where the chemical is used, stored, or supplied and generates a sample to be transferred (hereinafter referred to as "transfer sample"); and a main system receiving the transmission sample from the sampling unit and analyzing the transmission sample by an analyzer, wherein the main system is radially connected to a transmission line through a plurality of sampling units arranged in a dispersed manner, and the transmission sample is transmitted in a packaged state with the non-reactive gas positioned in front and rear of the transmission line.
For the online contamination monitoring system, the sampling unit dilutes the introduced chemical with deionized water to generate the reduced viscosity of the transmission sample.
For the online pollution monitoring system, the primary system comprises: and a pretreatment unit for evaporating the liquid of the transmission sample to leave contaminants and recovering the remaining contaminants with a recovery solution to produce a recovered sample (hereinafter referred to as a "recovered sample") in a state where the transmission sample is accommodated in the pretreatment vessel.
The online pollution monitoring system further comprises: a test solution supply part supplying a test solution to the sampling unit, wherein the sampling unit allows the test solution to be transmitted through the transmission line while being tested by the analyzer when a result of the transmission sample analyzed by the analyzer is detected as contamination.
An online pollution monitoring method according to an embodiment of the present invention is an online pollution monitoring method performed in an online pollution monitoring system, wherein the online pollution monitoring system includes: a sampling unit that introduces a chemical through a line connected to a point where the chemical is used, stored, or supplied and generates a sample to be transferred (hereinafter referred to as "transfer sample"); a main system receiving the transmission sample from the sampling unit and analyzing the transmission sample by an analyzer, wherein the main system is radially connected to a transmission line through a plurality of sampling units arranged in a dispersed manner, and the transmission sample is transmitted in a packaged state with a non-reactive gas located in front and rear of the transmission line, the online contamination monitoring method comprising the steps of: a first step in which the host system receives the transmission sample for analysis; a second step of, in a case where it is detected that the analysis result in the first step is contaminated, the sampling unit transmitting a test solution through the transmission line, and the main system performing analysis; a third step of judging that the contamination monitoring system is abnormal in a case where the analysis result in the second step is different from the prediction of the test solution.
The online pollution monitoring system and the online pollution monitoring method have the following effects that samples are transmitted to the analyzer from a plurality of monitoring points and analyzed, and reliability and efficiency can be ensured.
An embodiment of the present invention has an effect that when the introduced chemical is transferred by a sealing method, a transfer sample with a reduced viscosity is generated by diluting with deionized water and transferred, thereby enabling smooth, efficient and reliable transfer of the sample.
An embodiment of the present invention has an effect that the preprocessor dish is formed of a material through which infrared rays are transmitted, and a heater for heating the preprocessor dish is performed in a lamp type, whereby the temperature of the preprocessor dish is not greatly increased, and thus, rapid cooling is possible, and thus, contamination analysis of a sample can be rapidly performed.
An embodiment of the present invention has an effect of performing evaporation of a solution of a sample and recovery using a recovery solution, ensuring that the composition, density, and the like of a matrix are the same, and in addition, automatically performing this process in a closed state rather than an open state, thereby ensuring the accuracy of analysis while enabling the acquisition of stability.
An embodiment of the present invention has an effect of preventing production interruption due to wrong contamination information in advance by providing a test solution supply part for supplying a test solution to a sampling unit, transmitting the test solution through the same transmission line by the sampling unit and performing a test by an analyzer when a result of a transmission sample analyzed by the analyzer is detected as contamination.
Drawings
FIG. 1 is a diagram illustrating the overall topology of the online pollution monitoring system of the present invention;
FIG. 2 is a diagram illustrating an exemplary transmission line 300 and a transmission sample A transmitted through the transmission line 300 according to an embodiment of the present invention;
FIG. 3 is a block diagram of a sampling unit 100 according to an embodiment of the present invention;
fig. 4 is a block diagram showing the structure of a main system 200 of an embodiment of the present invention;
fig. 5 is a diagram showing a structure of the preprocessing section 220 according to an embodiment of the present invention;
fig. 6 is a diagram showing a structure of an introduction part 230 according to an embodiment of the present invention;
fig. 7 is a diagram showing the structure of the test solution supply part 260 according to an embodiment of the present invention.
Description of the symbols
100: the sampling unit 200: main system
210: sample receiving portion 220: pretreatment unit
230: introduction section 240: analyzer
250: the control unit 260: test solution supply part
300: transmission line
Detailed Description
Embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily practice the invention. The present invention may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. In the drawings, portions that are not related to the description are omitted for the sake of clarity, and like reference numerals and signs are used for like portions throughout the specification.
FIG. 1 is a drawing illustrating the overall topology of the online pollution monitoring system of the present invention.
An online pollution monitoring system of an embodiment of the present invention includes: a plurality of sampling units 100 arranged in a dispersed manner; a main system 200 radially connected to the plurality of sampling units 100 distributed via a transmission line 300; and a transmission line 300 connecting the sampling unit 100 and the main system 200.
The sampling unit 100 introduces a chemical through an introduction line (not shown) connected to a point where the chemical is used, stored, or supplied (mainly in a liquid state), i.e., a monitoring point, and generates a sample (hereinafter referred to as "transmission sample") transmitted through the transmission line 300.
The monitoring points include, for example, Wet process (Wet process) equipment, Chemical Supply devices, pipes, tanks (Tank) and the like in a factory floor (FAB Area), a Service Area (Service Area) or a Chemical Supply Area (Chemical Supply Area) of a semiconductor manufacturing plant, process equipment, pipes, tanks (Tank) and the like in a Chemical manufacturing plant, and the like.
The sampling unit 100 is located in the vicinity of the monitoring point, automatically takes a sample of the chemical used, stored or supplied, and transfers the sample in a quick time to the host system where the analyzer is located. The specific structure of the sampling unit 100 is described in fig. 3 and its description.
The host system 200 receives the transmission sample from the sampling unit 100 through the transmission line 300 to be analyzed by the analyzer. The main system 200 receives the samples transmitted from the plurality of sampling units 100, analyzes the samples, reports whether the analysis result is one or more of contamination, a kind of contamination, or a concentration/content of contamination, and gives an alarm to a user.
The transfer process from the monitoring point to the main system and the transfer process in the main system are all closed systems (closed systems) and are carried out by an on-line delivery (on-line delivery) structure.
In addition, in order to improve the efficiency of the online contamination monitoring system, more sampling units 100 need to be connected to one main system 200, and thus, the distance from the sampling unit 100 to the main system 200 is 100m to 300 m.
Methods for transporting samples of chemicals in the liquid state over long distances are known in two general categories.
The first method is a method of filling all the transfer lines and transferring them like short distance transportation. The above-described method has high reliability, but has a problem that the amount of sample to be sampled is proportional to the transport distance, which causes a very large problem, and the efficiency is reduced.
The second method is a method of vaporizing a chemical in a liquid state and transferring the vaporized sample, and the method has an advantage of improving efficiency as described above, but has a problem that contaminants (main metal components) contained in the chemical are adsorbed to the transfer line during the transfer.
Fig. 2 is a diagram illustrating an example of a transmission line 300 and a transmission sample a transmitted through the transmission line 300 according to an embodiment of the invention.
According to the present invention, a sample is transferred to a transfer line, and a transfer sample a in a liquid state is transferred in a state where a high-pressure non-reactive gas G is enclosed in front and rear thereof in the transfer line 300. The non-reactive gas is N2 or Ar, etc. The transmission sample is pressurized by the high-pressure non-reactive gas at both sides, and the transmission sample is intermittently transmitted while maintaining a packaged state in the transmission line 300.
The inner diameter d of the transmission line is 0.5 mm-1.6 mm, when the inner diameter is too large, the problem that the packaged transmission sample is damaged exists, and when the inner diameter is too small, the problem that the transmission quantity is small and the transmission efficiency is reduced exists.
Fig. 3 is a structural diagram of the sampling unit 100 according to an embodiment of the invention.
The sampling unit 100 includes: DI Vessel (Vessel) 110, sample Vessel (Vessel) 120, injection valve 130, sensors S11, S12, S13 and medium pressure gate valves V11-V18.
The sampling unit performs a function of introducing a chemical on-line through a line connected to a monitoring point, maintaining the introduced chemical as it is or diluting the introduced chemical with deionized water, thereby reducing viscosity to generate a transmission sample, and transmitting the generated transmission sample through the transmission line 300. The sampling unit receives the test solution supplied from a test solution supply unit (260; see fig. 4 and 7) located near the sampling unit or the main system 200, and transmits the test solution through the transmission line 300.
Preferably, the DI vessel and the sample vessel are coil-shaped vessels, and particularly, the sample vessel is formed in a coil shape, and when temporarily stored chemicals are washed by deionized water supplied through the DI vessel, the washing can be rapidly performed.
The sample vessel 120 temporarily stores a quantitative chemical introduced from a monitoring point through the medium pressure gate valve V17.
The sensors S11, S12, S13 are optical sensors or proximity sensors capable of at least distinguishing one from another and detecting liquids such as deionized water, chemicals, or test solutions and non-reactive gases such as N2.
The injection valve 130 has, for example, six ports, and both ends of the transfer ring (Delivery Loop) 140 are connected to the two ports, and has a port for receiving the pressurized non-reactive gas such as N2 supplied thereto, a port connected to a Drain system (Drain), a port connected to the transfer line 300, and a port connected to the sample vessel 120 through a medium pressure gate valve V18.
The injection valve 130 is switched between two positions, a loading Position (LoadPosition) and a Delivery Position (Delivery Position), under the control of a control section 250 or the like located in the main system 200. Preferably, the volume of the transfer ring 140 is greater than the volume of the sample vessel 120 or the volume of the sample vessel 120 in combination with the DI vessel 110.
The DI vessel 110, sample vessel 120 and transfer ring 140 are connected in series by means of one or more medium pressure gate valves and injection valves (when the injection valves are in the loading position), in the order of the DI vessel, sample vessel and transfer ring. Thus, when the deionized water temporarily stored in the DI vessel 110 and the chemical temporarily stored in the sample vessel 120 are transferred to the transfer ring 140 and filled, the deionized water washes the chemical of the sample vessel 120, and the chemicals are not left and can be completely transferred to the transfer ring 140. When the chemicals are temporarily stored in the sample vessel 120, a set amount is stored, and Loss (Loss) occurs in the middle, which is not desirable, but is entirely transferred to the transfer ring 140 without residue according to the structure.
Next, the operation of the sampling unit 100 will be explained.
First, chemicals are introduced from a monitoring point through the medium pressure gate valve V17, and the medium pressure gate valves V11, V14, and V17 are opened. The introduction of the chemical is performed by applying a positive pressure to the chemical itself, or by using a pump (not shown) provided in a Drain system (Drain), or the like. The chemical introduced in the initial step of introduction passes through the sample vessel 120, is discharged from the drain system through the intermediate pressure gate valve V14 and the intermediate pressure gate valve V11, and after a certain amount of chemical is discharged, the intermediate pressure gate valve is closed to fill the sample vessel 120 by an amount corresponding to the volume thereof (precisely, by an amount corresponding to the space between the adjacent intermediate pressure gate valves, and in reality, the distance between the intermediate pressure gate valves adjacent to the sample vessel is designed to be very close to each other). The normal introduction of the chemical is confirmed by the sensor S12.
Before the chemical is filled into the sample vessel 120, the intermediate pressure gate valves V16, V12, V14, and V18 are opened, and the DI vessel 110 and the sample vessel 120 are emptied by a non-reactive gas such as N2 with the injection valve 130 set to the loading position.
In case dilution is required, the DI vessel 110 is filled with deionized water DI for use. The intermediate pressure gate valves V15, V12, V11 are opened, initially deionized water flows through the DI vessel 110 to the Drain system (Drain), and after a certain amount is drained, the intermediate pressure gate valves are closed to fill the DI vessel 110 with deionized water.
The dilution ratio is set by the volume ratio of the sample vessel to the DI vessel, and the filled chemical moves with the deionized water to fill the transfer ring 140 connected to the injection valve 130 at one end. As shown in the drawing, the position of the injection valve 130 must be a loading position (loading position) by using a gas pressure such as N2, a pump, or the like, and the state where the sample is filled in the transfer ring 140 is detected by a sensor S13. As described above, the chemicals temporarily stored in the sample vessel 120 and the DI water temporarily stored in the DI vessel 110 are moved from the loading position of the injection valve 130 and filled into the transfer ring 140 to become a transfer sample.
One feature of the present invention is the delivery of a sample of a selectively diluted chemical. The sampling unit 100 selectively dilutes the introduced chemicals with deionized water to produce a reduced viscosity transport sample for transport. Since chemicals such as sulfuric acid and phosphoric acid have high viscosity, they cannot be smoothly transported by the encapsulation method of the present invention, and thus, a large amount of time is consumed in transportation and Loss (Loss) is caused in transportation. According to a feature of the present invention, when the sample is transferred by the encapsulation method, the sample of chemicals such as sulfuric acid and phosphoric acid is diluted and transferred, which has an effect of transferring the sample more smoothly, efficiently and reliably.
And, the transmission sample filled into the transfer ring 140 is rapidly transmitted mostly long distance by the transmission line 300, thereby being transmitted to the main system 200. For this, first, the injection valve 130 is switched to a transfer Position (Delivery Position) in which the transfer sample at the transfer ring is transferred through the transfer line 300 when a non-reactive gas such as N2 or Ar is pressurized by high pressure as shown in the lower side of the drawing. The transfer sample filled into the transfer ring 140 is pushed by the non-reactive gas at the transfer position of the injection valve 130 and transferred through the transfer line 300. At this time, the sample a is transferred in the transfer line 300 as illustrated in fig. 2.
In addition, for the inspection, the sampling unit 100 fills the inspection solution from the inspection solution supply part 260 located near or at the master system 200 to the transfer ring 140 through the medium pressure gate valve V13, and at this time, opens the medium pressure gate valves V13, V14, and V18, and fills the inspection solution to the transfer ring 140 with the injection valve 130 being at the loading position. The test solution is, for example, a standard solution that introduces a contaminant into a specific chemical, and the type and concentration of the contaminant are known in advance.
And, after the transmission of the transmission sample, the internal channel of the sampling unit 100 is washed by deionized water or chemicals. For example, when the intermediate pressure gate valves V16, V12, V14, and V18 are opened, deionized water DI is flowed to a Drain system (Drain) and cleaned with the injection valve 130 being in the loading position.
After the transfer of the transfer sample is performed, the transfer line 300 is cleaned with deionized water or chemicals. For example, after deionized water is loaded into the transfer ring 140, a process of transferring the deionized water is performed several times. One sampling unit 100 takes samples from a plurality of monitoring points and transfers the samples, and a plurality of structures as shown in fig. 3 are formed.
Fig. 4 is a block diagram showing the structure of a main system 200 according to an embodiment of the present invention.
The host system 200 includes: a sample receiving part 210, a pretreatment part 220, an introduction part 230, an analyzer 240, a control part 250, and a test solution supply part 260.
The sample receiving part 210 receives transmission samples from the connected plurality of sampling units 100 through the transmission line 300. For example, one end of the transfer line 300 of the sample receiving portion 210 or a line extending therefrom includes a line or the like for transferring a transferred sample received by a cylinder-shaped vessel (not shown below) and a vessel hanging from the inside to the preprocessing portion 220 to be described later, and has a number of vessels corresponding to the number of transfer lines, or the number of vessels corresponding to each group of transfer lines.
The pretreatment unit 220 is connected to the sample receiving unit 210, and in a state where the specimen to be transferred from the sample receiving unit 210 is received and accommodated in a pretreatment dish, the liquid for transferring the specimen is evaporated to leave the contaminant, and the recovered specimen (hereinafter, referred to as "recovered specimen") is generated using the remaining contaminant as a recovery solution.
The introduction part 230 is located at the rear end of the pretreatment part 220 and introduces a quantitative recovered sample into the analyzer 240, and performs functions of supplying a standard solution for calibration of the other analyzer 240 and selectively diluting the recovered sample with deionized water.
The analyzer 240 is a well-known device for analyzing a substance present in a sample, analyzes whether or not contamination occurs, a kind of the contamination, a concentration or a content of the contamination, and the like, and is HPIC, ICPMS, ICP-AES, AAS, HPLC, CE, UV-vis, fluoroscience, and the like, and is preferably ICP-MS.
The control section 250 controls the respective sections of the main system 200 and the sampling unit 100, for example, receives a sensing signal from a sensor, connects the signal to an analyzer, and controls a medium pressure gate valve, an injection valve, and the like. The test solution supply part 260 performs a function of supplying a test solution (standard solution) to the sampling unit 100 for testing.
Fig. 5 is a diagram showing a structure of the preprocessing section 220 according to an embodiment of the present invention.
The pretreatment section 220 evaporates the liquid of the transmission sample and leaves contaminants in a state where the transmission sample is accommodated in the pretreatment vessel 221, and generates a sample ("recovered sample") in which the left contaminants are recovered by the recovery solution. The pretreatment section 220 heats a sample of the chemical, evaporates to remove the liquid, and leaves only the contaminants of the metal components, recovered and analyzed.
The preprocessing section 220 includes: the preprocessor dish 221, the external dish (Outer Vessel) 222, the Heater (Heater) 223, the Cooler (Cooler) 224, the first injection valve 225, the second injection valve 226, and a plurality of medium-pressure gate valves (V21, V22, V23, etc.) have a heating and cooling function, a function of quantitatively supplying a recovery solution, a function of introducing a quantitative sample, and a function of transferring and washing a preprocessed sample.
The preprocessor vessel 221 is made of quartz, PTFE, PFA, or PEEK, has infrared transmittance, transmits at least infrared rays from the heater 223, and is preferably made of a chemical resistant and heat resistant material. Further, the lower portion of the pre-processor dish 221 is U-shaped or V-shaped, so that a small amount of the collected sample can be easily introduced into the analyzer.
The exterior of the preconditioner vessel 221 is surrounded by an outer vessel 222 and contains liquid that overflows from the preconditioner vessel 221.
The heater 223 evaporates and concentrates the liquid of the sample contained in the pre-processor dish 222, preferably evaporating all the liquid and leaving only contaminants such as metals.
The heater 223 uses a lamp type heater such as infrared IR or Halogen (Halogen). The chemical-resistant plastic material is deformed at about 250 to 300 degrees, but when the lamp heater applies radiant heat, only the sample located inside the preconditioner vessel 221 is heated without a large increase in the temperature of the preconditioner vessel 221 made of plastic having excellent chemical resistance. Further, the problem that cooling is necessary when the temperature of the preprocessor dish becomes high, but generally, the cooling time takes longer than the temperature rise, and thus, the online (On-line) sample processing is not suitable, can be solved.
According to one feature of the present invention, the preprocessor dish is formed of an infrared ray transmitting material, and the heater for heating the preprocessor dish is manufactured in a lamp type, thereby having an effect that the temperature of the preprocessor dish is not greatly increased, thereby enabling rapid cooling, and thus enabling rapid contamination analysis of a sample.
In addition to the lamp type heater 223, a total heat heater, a carbon heater, a Peltier (Peltier), a microwave (microwave), a hot n2, or the like can be generally used.
The first injection valve 225 is used to introduce a sample (transfer sample) into the preconditioner vessel 221, and the second injection valve 226 is used to introduce a recovery solution into the preconditioner vessel 221.
The recovery solution is used to melt the dried sample (contaminants) and a set volume of recovery solution is supplied to the preconditioner dish 221. When the recovered solution is a metal contaminant, an acid series such as nitric acid or hydrofluoric acid + hydrogen peroxide can be used.
Next, the operation of the preprocessing unit 220 according to an embodiment of the present invention will be described.
First, the transferred sample is transferred from the vessel of the sample receiving part 210 to the pre-processor vessel 221, and at this time, a first injection valve (injection valve) 225, a quantitative pump system, or the like is used to introduce a quantitative sample. For example, the sample is loaded to the sample loop of the injection valve at the loading position of the first injection valve 225, and the loaded sample is transferred to the pre-processor dish 221 at the injection position by means of the structure 227 pressurized by the non-reactive gas, or the like.
And, the sample of the pre-processor dish 221 is heated by the energy of the heater 223, evaporating the liquid and leaving only the contaminants to be analyzed. When the liquid of the sample is evaporated, only the contaminants within the sample remain at the bottom of the pre-processor dish 221, and when the remaining contaminants are recovered by the recovery solution of less amount than the transferred sample, a concentration effect can be obtained. Examples of the liquid (chemical) to be evaporated are sulfuric acid, phosphoric acid, hydrofluoric acid, ammonium hydroxide, IPA, and the like.
And, the pre-processor dish 221 is cooled by the cooler 224, and the pre-processor dish 221 heated for drying the sample must be cooled for the accuracy of the recovery. As described above, the lamp type is easily cooled, and is also easily cooled by the dispersion of a gas such as N2. As another cooling method, a method using cooling water, a method using a Peltier element, or the like can be used.
And, in order to analyze the contaminants remaining in the preprocessor dish 221, the contaminants are recovered as a recovery solution. Before supplying the recovery solution, the pretreater dish 221 must be cooled to room temperature, and a second injection valve 226, a constant-volume pump system, or the like is used as shown in the figure to introduce a constant-volume recovery solution. For example, the recovery solution is loaded on the sample loop of the injection valve at the loading position of the second injection valve 226, and the loaded recovery solution is transferred to the pre-processor dish 221 by means of a structure 228 pressurized by a non-reactive gas, or the like at the injection position. A set volume of the recovery solution, nitric acid or hydrofluoric acid + hydrogen peroxide, etc., is supplied to the preconditioner dish to melt the dried sample.
The collected sample (collected sample) is transferred to an analyzer through an introduction portion and analyzed. In a state where the medium pressure gate valve V23 is opened, the collected sample in the cuvette 221 is loaded on a sample loop coupled to a third injection valve 231 of an introduction part 230 (see fig. 6) described below, and then transferred to the analyzer 240. For loading the sample ring, gas pressurization or pumping or the like is used.
After the pretreatment and transfer of the sample, the moving path and the pretreatment vessel are cleaned to achieve initialization. In order to improve washing efficiency, the vessel is formed in an overflow type structure (over flow type) with an outer vessel 222 so as to surround the pre-processor vessel 221. The heater 223 is formed outside or inside the external vessel 224, and in the case of being formed outside, the external vessel 224 is also made of an infrared ray transmitting material. The preconditioner dish can be occasionally rinsed with deionized water or a rinse solution to maintain a clean condition.
According to a feature of the invention, a pre-treatment function for the sample is added. The chemical sample components are present in various properties such as organic, acidic, and basic properties. When pollutants with the same concentration have different characters, the analysis results are different. The main components of the chemical product differ from each other in the matrix, and thus, differences occur in the sample introduction process, differences in the interference influence during analysis, and the like. Even if the same properties are obtained, the above-described effects occur due to density and component differences. Further, sometimes the concentration of the contaminant in the sample is too low, and the analysis by the analyzer may not be easily performed.
According to one feature of the present invention, evaporation of a solution using a sample and recovery of a recovered solution are performed, whereby the matrix is equal in composition, density, and the like, and the process is automatically performed not in an open state but in a closed state, thereby achieving the accuracy of analysis and obtaining stability.
Fig. 6 is a diagram showing a structure of the introduction part 230 according to an embodiment of the present invention.
The introduction part 230 is located at the rear end of the pretreatment part 220, introduces a quantitative recovery sample into the analyzer 240, performs the functions of supplying a standard solution for the scale of the other analyzer 240 and selectively diluting the recovery sample as deionized water.
The recycle sample is loaded from the pre-processor dish of the pre-processing part 220 to the sample ring at the loading position of the third injection valve 231, and the recycle sample loaded to the sample ring is moved to the analyzer 240 side by pushing deionized water at the injection position by the quantitative pump P22.
The T-pipe 233 is provided on the route leading to the analyzer, and when the collected sample is led to the analyzer 240, deionized water is selectively led to the T-pipe 233 by the quantitative pumps P21 to dilute the collected sample, and the dilution ratio is determined according to the amount (flow rate) of deionized water pushed by each quantitative pump.
The standard solution is loaded to the sample ring of the fourth injection valve 232 at the loading position of the fourth injection valve 232, and the standard solution loaded as deionized water is pushed by the metering pump at the injection position, supplied to the analyzer 240 and calibrated to the analyzer 240.
The sensors S21 and S22 are disposed near the sample loop, and detect the sample or standard solution filled in the sample loop.
Fig. 7 is a diagram showing the structure of the test solution supply part 260 according to an embodiment of the present invention.
The test solution supply part 260 is a device that supplies a test solution to the sampling unit 100, and when the result of analyzing the transmission sample by the analyzer is detected as contamination, the sampling unit 100 transmits the test solution again through the transmission line 300 and performs a test by the analyzer.
As an embodiment, the test solution supply part 260 is included in the main system 200, and the system can be more efficiently formed by supplying the test solution from the test solution supply part 260 to each sampling unit 100 through the supply line 310.
The test solution (standard solution) is filled into the test solution tank 261 by a pump P shown by opening medium-pressure gate valves V24, V27 or by pressurization or depressurization, and the filling of the test solution is confirmed by a sensor (optical sensor, proximity sensor, etc.) S23.
And, the test solution filled into the test solution tank 261 opens the medium pressure gate valves V26, V29 and is transferred through the transfer line 300 by pressurizing the non-reactive gas such as N2 for supply to the sampling unit 100. The transferred test solution is finally stored to a delivery loop (delivery loop) of the sampling unit 100 through a valve, and then transferred to the main system again through the transfer line 300 and analyzed. The test solution transferred to the main system is analyzed and the result is judged through a general analysis sequence.
In describing the main operation process around the inspection process, as shown below, the control of the main process is performed by the control section 250 of the main system 200.
Generally, when each sampling unit 100 transmits a sample to the host system 200, the host system 200 receives the transmitted sample for analysis.
However, when contamination is detected based on the analysis result, the control part 250 of the main system 200 gives a first alarm to the user, so that the test solution supply part 260 located at the main system 200 or the like supplies the test solution (standard solution) to the corresponding sampling unit 100, the sampling unit 100 transmits the test solution through the same transmission line 300 for the test, and the main system 200 analyzes the received test solution. That is, a standard solution containing a contaminant of known kind and concentration is transferred from the sampling unit to the main system through the same path, and analyzed by the same analysis method as the previous analysis.
And when the analysis result of the transmitted test solution is different from the prediction of the test solution, judging that the pollution monitoring system is abnormal. And when the analysis result is the same as the prediction of the test solution, judging that the pollution monitoring system is normal. For example, when a contaminant different from the contaminant contained in the test solution or the same type of contaminant is detected but the concentration of the contaminant contained in the test solution indicates that a difference exceeding a predetermined range is present, it is determined that an abnormality is present in the contamination monitoring system.
And when the pollution monitoring system is judged to be normal, the sample of the chemical product is analyzed again, and when the analysis result is confirmed to be pollution again, a second alarm is sent out, and the generation is stopped. And when the pollution monitoring system is judged to be abnormal, the abnormal condition of the pollution monitoring system is sent to a user for alarming.
In the production line, the pollution problem is closely related to the yield and productivity, and must be managed with great importance. If contamination is detected, the production process must be interrupted to prevent a number of undesirable phenomena from occurring. However, when the contamination analysis result is not reliable, a large loss is caused by production interruption due to an erroneous analysis result.
According to one feature of the present invention, there is an effect that a test solution supply portion is provided which supplies a test solution to a sampling unit, and when a result of analyzing a transmission sample by an analyzer is detected as contamination, the sampling unit transmits the test solution through the same transmission line and is inspected by the analyzer, and a problem of production interruption due to transmission of an erroneous contamination alarm can be prevented from occurring.
Claims (16)
1. An on-line pollution monitoring system is characterized in that,
the method comprises the following steps:
a sampling unit that introduces a chemical through a line connected to a point where the chemical is used, stored, or supplied, and generates a transfer sample to be transferred;
a host system receiving the transmission sample from the sampling unit to be analyzed by an analyzer,
wherein the main system is radially connected with the transmission line through a plurality of sampling units which are distributed and configured,
in the transmission line, the non-reactive gas for transmitting the sample is positioned in front and at the back and is transmitted in an encapsulated state;
further comprising: a test solution supply part supplying a test solution to the sampling unit,
the sampling unit transmits the test solution through the transmission line to be tested by the analyzer when the result of analyzing the transmission sample by the analyzer is detected as contamination.
2. The on-line pollution monitoring system of claim 1,
the inner diameter of the transmission line is 0.5mm to 1.6mm, and the transmission sample is transmitted in a state of being pressurized by the non-reactive gas.
3. The on-line pollution monitoring system of claim 1,
the sampling unit dilutes the introduced chemical with deionized water to generate the reduced viscosity of the transmission sample.
4. The on-line pollution monitoring system of claim 3,
the sampling unit includes:
a sample vessel temporarily storing the introduced quantitative chemical;
a DI vessel temporarily storing the measured amount of deionized water.
5. The on-line pollution monitoring system of claim 4,
the sampling unit further includes:
an injection valve for connecting two ends of the transfer ring with the two ports,
i) moving and filling the chemical temporarily stored in the sample vessel and the deionized water temporarily stored in the DI vessel from the loading position of the injection valve to the transfer ring to become the transfer sample,
ii) pushing the transfer sample filled to the transfer ring through the non-reactive gas and transferring through the transfer line at the transfer position of the injection valve.
6. The on-line pollution monitoring system of claim 5,
the DI vessel, the sample vessel and the transfer ring are connected in series by means of one or more valves, connected in the order of the DI vessel, the sample vessel and the transfer ring.
7. The on-line pollution monitoring system of claim 5,
the DI vessel and the sample vessel are coil-shaped vessels.
8. The on-line pollution monitoring system of claim 1,
the host system includes:
a pretreatment part evaporating the liquid of the transmission sample while leaving contaminants in a state where the transmission sample is accommodated in the pretreatment dish, and generating a recovery sample recovering the contaminants left by the recovery solution.
9. The on-line pollution monitoring system of claim 8,
the pre-treatment part comprises a lamp type heater,
the preprocessor is transparent to infrared rays and at least transmits infrared rays transmitted from the heater.
10. The on-line pollution monitoring system of claim 9,
the pre-processor vessel is made of quartz, PTFE, PFA or PEEK.
11. The on-line pollution monitoring system of claim 8,
the lower part of the preprocessor dish is U-shaped or V-shaped.
12. The on-line pollution monitoring system of claim 8,
the host system includes:
an introduction section which is located at the rear end of the pretreatment section and which introduces a quantitative recovered sample to the analyzer,
there is a tee that selectively introduces deionized water into the path introduced through the analyzer for diluting the recovered sample.
13. The on-line pollution monitoring system of claim 8,
the host system further includes:
and a control part for controlling each part of the main system and the plurality of sampling units.
14. The on-line pollution monitoring system of claim 1,
the test solution supply portion is formed at the main system,
the test solution is supplied from the test solution supply portion to each sampling unit through a supply line.
15. An on-line pollution monitoring method is an on-line pollution monitoring method executed in an on-line pollution monitoring system, and the on-line pollution monitoring system comprises: a sampling unit that introduces a chemical through a line connected to a point where the chemical is used, stored, or supplied, and generates a transfer sample to be transferred; a main system receiving the transmission sample from the sampling units and analyzing the transmission sample by an analyzer, wherein the main system is radially connected to a transmission line through a plurality of the sampling units arranged in a dispersed manner, and the transmission sample is transmitted in an encapsulated state with the non-reactive gas located in front and rear of the transmission sample in the transmission line,
the method comprises the following steps:
a first step in which the host system receives the transmission sample and analyses it;
a second step of, when it is detected that the analysis result at the first step is contamination, the sampling unit transmitting a test solution through the transmission line, and the main system performing analysis;
a third step of judging that there is an abnormality in the contamination monitoring system when the analysis result of the second step is different from the prediction of the test solution.
16. The on-line pollution monitoring method according to claim 15,
further comprising: and a third step of judging that the contamination monitoring system is normal when the analysis result of the second step is the same as the prediction of the test solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610833793.4A CN107845585B (en) | 2016-09-20 | 2016-09-20 | On-line pollution monitoring system and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610833793.4A CN107845585B (en) | 2016-09-20 | 2016-09-20 | On-line pollution monitoring system and method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107845585A CN107845585A (en) | 2018-03-27 |
| CN107845585B true CN107845585B (en) | 2021-07-16 |
Family
ID=61656827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610833793.4A Active CN107845585B (en) | 2016-09-20 | 2016-09-20 | On-line pollution monitoring system and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107845585B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112666046B (en) * | 2020-11-30 | 2022-10-28 | 义乌市清源检测有限公司 | Water quality detection device based on viscosity detection |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005152714A (en) * | 2003-11-21 | 2005-06-16 | Mitsubishi Heavy Ind Ltd | Hazardous substance treatment system and treatment graduation judgment method for matter contaminated with hazardous substance contaminated matter |
| CN1928565A (en) * | 2005-09-05 | 2007-03-14 | 株式会社日立高新技术 | Automatic analyzer |
| CN101221127A (en) * | 2007-10-26 | 2008-07-16 | 河北省电力研究院 | Concurrent measuring method for multiple metallic elements in transformer oil |
| KR101368485B1 (en) * | 2012-09-28 | 2014-03-03 | 주식회사 위드텍 | On-line monitoring system for ultrapure water |
| WO2015174562A1 (en) * | 2014-05-14 | 2015-11-19 | 주식회사 위드텍 | Pollutant monitoring device |
| WO2016144107A1 (en) * | 2015-03-12 | 2016-09-15 | 엔비스아나(주) | Substrate contaminant analysis device and substrate contaminant analysis method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101497641B1 (en) * | 2013-05-28 | 2015-03-03 | 엔비스아나(주) | Apparatus for analyte sampling, method of analyte sampling and analyte sampling analysis system |
-
2016
- 2016-09-20 CN CN201610833793.4A patent/CN107845585B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005152714A (en) * | 2003-11-21 | 2005-06-16 | Mitsubishi Heavy Ind Ltd | Hazardous substance treatment system and treatment graduation judgment method for matter contaminated with hazardous substance contaminated matter |
| CN1928565A (en) * | 2005-09-05 | 2007-03-14 | 株式会社日立高新技术 | Automatic analyzer |
| CN101221127A (en) * | 2007-10-26 | 2008-07-16 | 河北省电力研究院 | Concurrent measuring method for multiple metallic elements in transformer oil |
| KR101368485B1 (en) * | 2012-09-28 | 2014-03-03 | 주식회사 위드텍 | On-line monitoring system for ultrapure water |
| WO2015174562A1 (en) * | 2014-05-14 | 2015-11-19 | 주식회사 위드텍 | Pollutant monitoring device |
| WO2016144107A1 (en) * | 2015-03-12 | 2016-09-15 | 엔비스아나(주) | Substrate contaminant analysis device and substrate contaminant analysis method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107845585A (en) | 2018-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20220252630A1 (en) | System for collecting liquid samples | |
| US11493523B2 (en) | Automated system for safe sample collection, transfer, and analysis | |
| US20210382022A1 (en) | System for collecting liquid samples | |
| TWI808094B (en) | Automated system for remote inline concentration of ultra-low concentrations in pure chemicals | |
| US11761860B2 (en) | System for collecting liquid samples and transporting over distances while maintaining a liquid sample segment | |
| TWI801481B (en) | Systems and methods for icpms matrix offset calibration | |
| US10048173B2 (en) | Apparatus for analyte sampling, method of analyte sampling and analyte sampling analysis system | |
| CN105738287B (en) | Water Test Kits | |
| US20240112900A1 (en) | Automated system for remote inline concentration and homogenization of ultra-low concentrations in pure chemicals | |
| CN107845585B (en) | On-line pollution monitoring system and method | |
| JP7405777B2 (en) | System for prioritization of collecting and analyzing liquid samples | |
| WO2011100823A1 (en) | Interface to a mass spectrometer | |
| EP1523665A1 (en) | Remote analysis using aerosol sample transport | |
| TWI619946B (en) | Online pollution monitoring system and operation method thereof | |
| CN102269663A (en) | ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) online sampling device and online monitoring method of metal impurities | |
| KR101809702B1 (en) | On-line Contamination Monitoring System and Method using it | |
| KR102357430B1 (en) | Sample pretreatment apparatus and sample pretreatment method | |
| JP7514303B2 (en) | Remote automated chemical switching system for use with automated sampling equipment. | |
| US20220252562A1 (en) | Monitoring system and monitoring method | |
| TW202346825A (en) | On-line analysis system and method for specialty gasses | |
| KR20170011805A (en) | Particle analysis system for manufacturing semiconductor and method using the same | |
| WO2023229463A1 (en) | Measuring system for measuring an ion concentration in a process liquid using capillary electrophoresis and method therefor | |
| KR20050018649A (en) | Remote analysis using aerosol sample transport |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |