TWI619946B - Online pollution monitoring system and operation method thereof - Google Patents

Online pollution monitoring system and operation method thereof Download PDF

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TWI619946B
TWI619946B TW105128454A TW105128454A TWI619946B TW I619946 B TWI619946 B TW I619946B TW 105128454 A TW105128454 A TW 105128454A TW 105128454 A TW105128454 A TW 105128454A TW I619946 B TWI619946 B TW I619946B
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sample
vessel
pollution monitoring
monitoring system
sampling unit
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TW201812304A (en
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田弼權
成墉益
朴準虎
朴泓榮
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非視覺污染分析科學技術有限公司
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Abstract

本發明的線上污染監測系統特徵在於,包括:取樣單元,通過與使用、存儲或供應化學製品的點連接的線而導入化學製品,並生成要傳輸的樣品;主系統,從取樣單元接收傳輸樣品而通過分析儀分析,其中,主系統通過分散配置的多個取樣單元與傳輸線而呈放射狀連接,在傳輸線內,傳輸樣品的非反應性氣體位於前後而以封裝的狀態傳輸。The online pollution monitoring system of the present invention is characterized by comprising: a sampling unit that introduces a chemical by a line connected to a point of using, storing or supplying a chemical, and generates a sample to be transferred; and a main system that receives the transmitted sample from the sampling unit In the analysis by the analyzer, the main system is radially connected to the transmission line by a plurality of sampling units arranged in a distributed manner, and in the transmission line, the non-reactive gas of the sample is transported in the package state.

Description

線上污染監測系統及方法Online pollution monitoring system and method

本發明涉及線上污染監測系統及方法,更具體地涉及一種即時對在半導體製造工藝等中使用的化學製品污染進行線上(On-line)監測的系統及方法。The present invention relates to an online pollution monitoring system and method, and more particularly to a system and method for on-line monitoring of chemical contamination used in semiconductor manufacturing processes and the like.

當前,在半導體製造工藝等尖端製造產業,極微量的污染為收益率與生產力最重要的原因。由此,在生產工藝中,當即時對極微量的污染源實施分析時,能夠通過防止因污染而發生的大量的不良,從而,謀求提高收益率及生產力。At present, in the cutting-edge manufacturing industries such as semiconductor manufacturing processes, extremely small amounts of pollution are the most important causes of profitability and productivity. Therefore, in the production process, when a very small amount of pollution source is analyzed in real time, it is possible to improve the yield and productivity by preventing a large number of defects caused by the pollution.

但,半導體等製造業的生產裝備分散配置於大規模生產線上,化學製品製造業也因槽體之間的距離遠,需要對化學製品監測的點也分散在寬廣的區域。為了監測化學製品,在每個如上所示分散的各個監測點上設置分析儀,但其存在伴隨極大投資相當昂貴的分析儀的問題。However, the production equipment of semiconductors and other manufacturing industries are distributed in large-scale production lines, and the chemical manufacturing industry is also far away from the distance between the tanks, and the points that need to be monitored for chemicals are also dispersed in a wide area. In order to monitor the chemicals, the analyzer is placed at each of the various monitoring points dispersed as shown above, but it suffers from the problem of a very expensive analyzer that is extremely expensive to invest.

作為解決該問題的解決方案,將一個分析儀大致設置在監測點的中間距離之後,設置供在各個點上採取樣本之後傳輸至分析儀的取樣單元時,能夠構成共用高成本的分析儀的系統。但,在將按照如上所述方法採取的樣本傳輸至分析儀而進行分析的系統的可靠性或效率性降低時,存在無法適用該拓撲結構(topology)的問題。As a solution to this problem, after an analyzer is placed approximately at the intermediate distance of the monitoring point, a system for sharing a high-cost analyzer can be constructed when a sampling unit for transmitting samples to the analyzer at each point is set. . However, when the reliability or efficiency of a system in which a sample taken by the method as described above is transmitted to an analyzer is lowered, there is a problem that the topology cannot be applied.

對於上述現有技術問題及課題進行了說明,但對於該問題及課題的認識並非本發明的技術領域普通技術人員瞭解。The above-mentioned prior art problems and problems have been described, but the knowledge of the problems and the problems is not known to those skilled in the art of the present invention.

發明要解決的技術問題Technical problem to be solved by the invention

本發明的目的為提供一種線上污染監測系統及方法,將樣本由多個監測點傳輸至分析儀進行分析,並能夠確保可靠性與效率性。It is an object of the present invention to provide an in-line pollution monitoring system and method for transmitting samples from a plurality of monitoring points to an analyzer for analysis and ensuring reliability and efficiency.

本發明的技術方案在於:The technical solution of the invention lies in:

本發明的一實施例的線上污染監測系統包括:取樣單元,通過與供使用、存儲或供應化學製品的點連接的線導入化學製品並生成要傳輸的樣品(下面稱為“傳輸樣品”);主系統,從取樣單元接收傳輸樣品而通過分析儀進行分析,其中,主系統通過分散配置的多個取樣單元與傳輸線而呈放射狀連接,在傳輸線內,傳輸樣品的非反應性氣體位於前後,而以封裝的狀態傳輸。An online pollution monitoring system according to an embodiment of the present invention includes: a sampling unit that introduces a chemical to a sample to be transported by a line connected to a point for use, storage, or supply of a chemical (hereinafter referred to as "transfer sample"); The main system receives the transmitted sample from the sampling unit and analyzes it by the analyzer. The main system is radially connected to the transmission line by a plurality of sampling units arranged in a distributed manner. In the transmission line, the non-reactive gas for transmitting the sample is located before and after. It is transmitted in the state of the package.

對於線上污染監測系統,取樣單元將導入的化學製品通過去離子水稀釋而生成降低黏度的傳輸樣品。For an in-line contamination monitoring system, the sampling unit dilutes the introduced chemical with deionized water to produce a reduced viscosity transport sample.

對於線上污染監測系統,主系統包括:預處理部,將傳輸樣品容納於前置處理器皿的狀態下,蒸發傳輸樣品的液體而剩下污染物,並將剩下的污染物通過回收溶液而生成回收的樣品(下面稱為“回收樣品”)。For the online pollution monitoring system, the main system includes: a pre-processing unit that stores the transport sample in the state of the pre-processor vessel, evaporates the liquid of the sample to leave the contaminant, and generates the remaining contaminant through the recovery solution. The recovered sample (hereinafter referred to as "recovered sample").

線上污染監測系統還包括:檢驗溶液供應部,將檢驗溶液供應至取樣單元,其中,當檢測出通過分析儀分析的傳輸樣品的結果為污染時,取樣單元使得通過傳輸線傳輸檢驗溶液,而通過分析儀檢驗。The online pollution monitoring system further includes: a test solution supply unit that supplies the test solution to the sampling unit, wherein when the result of detecting the transmitted sample analyzed by the analyzer is contamination, the sampling unit causes the test solution to be transmitted through the transmission line, and passes the analysis Instrument inspection.

本發明的一實施例的線上污染監測方法是一種線上污染監測系統中執行的線上污染監測方法,其中,線上污染監測系統,包括:取樣單元,通過與供使用、存儲或供應化學製品的點連接的線導入化學製品並生成要傳輸的樣品(下面稱為“傳輸樣品”);主系統,從取樣單元接收傳輸樣品而通過分析儀進行分析,其中,主系統通過分散配置的多個取樣單元與傳輸線而呈放射狀連接,在傳輸線內,傳輸樣品的非反應性氣體位於前後,而以封裝的狀態傳輸,該線上污染監測方法,包括如下步驟:第一步驟,主系統接收傳輸樣品而分析;第二步驟,在檢測出在第一步驟中的分析結果為污染的情況下,所述取樣單元通過傳輸線傳輸檢驗溶液,並且,主系統進行分析;第三-一步驟,在第二步驟中的分析結果與檢驗溶液的預測不同的情況下,判斷污染監測系統出現異常。An online pollution monitoring method according to an embodiment of the present invention is an online pollution monitoring method implemented in an online pollution monitoring system, wherein the online pollution monitoring system includes: a sampling unit connected to a point for use, storage or supply of chemicals The line introduces the chemical and generates a sample to be transported (hereinafter referred to as "transfer sample"); the main system receives the transmitted sample from the sampling unit and is analyzed by the analyzer, wherein the main system passes through a plurality of sampling units of the distributed configuration The transmission line is radially connected. In the transmission line, the non-reactive gas for transmitting the sample is located before and after, and is transmitted in a package state. The line pollution monitoring method comprises the following steps: in the first step, the main system receives the transmission sample for analysis; a second step, in the case where it is detected that the analysis result in the first step is contamination, the sampling unit transmits the test solution through the transmission line, and the main system performs analysis; the third-first step, in the second step When the analysis result is different from the prediction of the test solution, it is judged that the pollution monitoring system appears Often.

參照附圖對本發明的實施例進行具體說明,以使本發明所屬技術領域的技術人員容易實施。但,本發明能夠以各種不同的形式實現,並非限定於在此說明的實施例。並且,在附圖中,為了明確說明本發明,而省略了與說明無關的部分,通過整個說明書,對於相似的部分使用相似的名稱及附圖標記。The embodiments of the present invention will be specifically described with reference to the accompanying drawings in order to facilitate the invention. However, the invention can be embodied in a variety of different forms and is not limited to the embodiments described herein. Further, in the drawings, in order to clearly explain the present invention, portions that are not related to the description are omitted, and similar names and reference numerals are used for the similar portions throughout the specification.

圖1為例示本發明的線上污染監測系統的整個拓撲結構的附圖。1 is a diagram illustrating the entire topology of an in-line pollution monitoring system of the present invention.

本發明的一實施例的線上污染監測系統包括:多個取樣單元(100),分散配置;主系統(200),通過傳輸線(300)與分散配置的多個取樣單元(100)而呈放射狀連接;傳輸線(300),連接取樣單元(100)與主系統(200)之間。An online pollution monitoring system according to an embodiment of the present invention includes: a plurality of sampling units (100) arranged in a distributed manner; and a main system (200) radiating through a transmission line (300) and a plurality of sampling units (100) arranged in a distributed manner Connection; a transmission line (300) connected between the sampling unit (100) and the main system (200).

取樣單元(100)通過與使用、存儲或供應化學製品(主要為液體狀態)的點,即監測點連接的導入線(未圖示)而導入化學製品,並生成通過傳輸線(300)傳輸的樣品(下面稱為“傳輸樣品”)。The sampling unit (100) introduces the chemical by introducing a line (not shown) connected to the point of use, storage or supply of the chemical (mainly liquid state), that is, the monitoring point, and generates a sample transmitted through the transmission line (300). (hereinafter referred to as "transfer sample").

監測點,例如,半導體製造工廠的工廠區(FAB Area)、服務區(Service Area)或化學製品供應區(Chemical Supply Area)的濕法加工(Wet Porcess)設備、化學製品供應裝置、配管、槽體(Tank)等,化學製品製造工廠的工藝設備、配管、槽體(Tank)等。Monitoring points, for example, Wet Porcess equipment, chemical supply equipment, piping, tanks in a FAB Area, a Service Area, or a Chemical Supply Area of a semiconductor manufacturing plant Tank, etc., process equipment, piping, tanks, etc. of chemical manufacturing plants.

取樣單元(100)位於監測點的附近,自動採取使用、存儲或供應的化學製品的樣品,並在快的時間內將樣品傳輸至分析儀所處的主系統。對於取樣單元(100)的具體結構,在圖3及其說明部分進行敘述。The sampling unit (100) is located near the monitoring point and automatically takes samples of the chemical used, stored or supplied and transmits the sample to the main system where the analyzer is located in a fast time. The specific structure of the sampling unit (100) will be described in Fig. 3 and its description.

主系統(200)通過傳輸線(300)從取樣單元(100)接收傳輸樣品而通過分析儀分析。主系統(200)接收從多個取樣單元(100)傳輸的樣品而進行分析,對分析結果是否為污染、污染物的種類或污染物的濃度/含量中一個以上進行報告,並向使用者發出報警。The main system (200) receives the transmitted sample from the sampling unit (100) through the transmission line (300) and analyzes it by the analyzer. The main system (200) receives the samples transmitted from the plurality of sampling units (100) for analysis, and reports whether the analysis result is one or more of pollution, type of pollutants, or concentration/content of the pollutants, and issues to the user Call the police.

由監測點至主系統的移送過程與主系統內的移送過程全部為封閉系統(close system),通過線上傳輸(on-line delivery)結構進行。The transfer process from the monitoring point to the main system and the transfer process in the main system are all closed systems, which are carried out by an on-line delivery structure.

另外,為了提高線上污染監測系統的效率,需要將更多的取樣單元(100)與一個主系統(200)連接,由此,從取樣單元(100)至主系統(200)的距離為100m至300m。In addition, in order to improve the efficiency of the online pollution monitoring system, it is necessary to connect more sampling units (100) with one main system (200), whereby the distance from the sampling unit (100) to the main system (200) is 100 m to 300m.

長距離運輸現有液體狀態的化學製品的樣品的方法熟知的大致為兩種。Methods for transporting samples of existing liquid state chemicals over long distances are generally well known.

第一種方法為如短距離運輸一樣全部填充傳輸線並移送的方式。如上所述的方式的可靠性高,但存在必須要採取的樣品的量與傳輸距離成比例而造成非常大的問題,進而降低效率的問題。The first method is a method of completely filling and transferring a transmission line as in short-distance transportation. The reliability of the above-described method is high, but there is a problem that the amount of the sample that must be taken is proportional to the transmission distance, causing a very large problem, thereby reducing the efficiency.

第二種方法為將液體狀態的化學製品汽化並傳輸發生了汽化的樣品的方式,如上所述的方式具有提高效率性的優點,但發生包含於化學製品的污染物(主要金屬成分)在傳輸過程中吸附於傳輸線的問題。The second method is a method of vaporizing a chemical in a liquid state and transporting a sample in which vaporization has occurred, and the manner as described above has an advantage of improving efficiency, but the occurrence of contaminants (main metal components) contained in the chemical is transmitted. The problem of adsorption to the transmission line during the process.

圖2為顯示本發明的一實施例的傳輸線(300)與通過傳輸線(300)傳輸的傳輸樣品(A)的示例圖。2 is a diagram showing an example of a transmission line (300) and a transmission sample (A) transmitted through a transmission line (300) according to an embodiment of the present invention.

根據本發明,將樣品傳輸至傳輸線,並在傳輸線(300)內,液體狀態的傳輸樣品(A)以高壓的非反應性氣體(G)位於前後而封裝的狀態傳輸。非反應性氣體為N2或Ar等。傳輸樣品因位於兩側的高壓的非反應性氣體施壓,在傳輸線(300)內,傳輸樣品保持封裝的狀態並間歇地傳輸。According to the present invention, the sample is transported to the transmission line, and in the transmission line (300), the transport sample (A) in the liquid state is transported in a state in which the high-pressure non-reactive gas (G) is located before and after. The non-reactive gas is N2 or Ar or the like. The transport sample is pressurized by a high-pressure, non-reactive gas located on both sides, and within the transmission line (300), the transport sample remains in a packaged state and is intermittently transported.

傳輸線的內徑(d)為0.5mm~1.6mm,在內徑太大時,存在封裝的傳輸樣品發生破損的問題,在內徑太小時,存在傳輸量小,降低傳輸效率的問題。The inner diameter (d) of the transmission line is 0.5 mm to 1.6 mm. When the inner diameter is too large, there is a problem that the package transmission sample is broken. When the inner diameter is too small, there is a problem that the transmission amount is small and the transmission efficiency is lowered.

圖3為本發明的一實施例的取樣單元(100)的結構圖。3 is a structural diagram of a sampling unit (100) according to an embodiment of the present invention.

取樣單元(100)包括:DI器皿(Vessel)(110)、樣品器皿(Vessel)(120)、注射閥(130)、感測器(S11、S12、S13)及中壓閘閥(V11~V18)。The sampling unit (100) includes: a DI vessel (110), a sample vessel (Vessel) (120), an injection valve (130), a sensor (S11, S12, S13), and a medium pressure gate valve (V11 to V18). .

取樣單元執行如下功能,通過與監測點連接的線而線上導入化學製品,將所導入的化學製品保持原樣或通過去離子水稀釋,從而,降低黏度而生成傳輸樣品,將所生成的傳輸樣品通過傳輸線(300)傳輸。並且,取樣單元接收由位於取樣單元附近或主系統(200)的檢驗溶液供應部(260;參照圖4及圖7)供應的檢驗溶液,而通過傳輸線(300)傳輸。The sampling unit performs the following functions: introducing a chemical on the line through a line connected to the monitoring point, leaving the introduced chemical as it is or diluting it with deionized water, thereby reducing the viscosity to generate a transport sample, and passing the generated transport sample through Transmission line (300) transmission. And, the sampling unit receives the inspection solution supplied from the inspection solution supply portion (260; see FIGS. 4 and 7) located near the sampling unit or the main system (200), and is transported through the transmission line (300).

DI器皿(110)通過中壓閘閥(V15)而接收所供應的去離子水,能夠暫時存儲定量去離子水,而且,N2等非反應性氣體通過中壓閘閥(V16)推動暫時存儲於DI器皿(110)的去離子水。樣品器皿(120)及DI器皿(110)為線圈(coil)或容器(container)等形狀,具有定量的體積(volume)。The DI vessel (110) receives the supplied deionized water through the medium pressure gate valve (V15), and can temporarily store the quantitative deionized water, and the non-reactive gas such as N2 is temporarily stored in the DI vessel through the medium pressure gate valve (V16). (110) Deionized water. The sample vessel (120) and the DI vessel (110) are in the shape of a coil or a container and have a quantitative volume.

優選地,DI器皿及樣品器皿為線圈狀的器皿,尤其,將樣品器皿形成為線圈狀,將暫時存儲的化學製品借助通過DI器皿供應的去離子水清洗時,能夠快速執行清洗。Preferably, the DI vessel and the sample vessel are coil-shaped vessels, and in particular, the sample vessel is formed into a coil shape, and the temporarily stored chemical can be quickly cleaned by washing with deionized water supplied through the DI vessel.

樣品器皿(120)暫時存儲由監測點通過中壓閘閥(V17)導入的定量化學製品。The sample vessel (120) temporarily stores the quantitative chemical introduced by the monitoring point through the intermediate pressure gate valve (V17).

感測器(S11、S12、S13)為光感測器或接近感測器,至少能夠相互區分並檢測去離子水、化學製品或檢驗溶液等液體與N2等非反應性氣體。The sensors (S11, S12, S13) are photo sensors or proximity sensors capable of distinguishing at least one another and detecting a liquid such as deionized water, a chemical or a test solution, and a non-reactive gas such as N2.

注射閥(130)例如,具有六個口,傳遞環(Delivery Loop)(140)的兩端與兩個口連接,並具有接收所供應的N2等被加壓的非反應性氣體的口、與排水系統(Drain)連接的口、與傳輸線(300)連接的口、通過中壓閘閥(V18)而與樣品環(120)連接的口。The injection valve (130) has, for example, six ports, and two ends of a delivery loop (140) are connected to the two ports, and have a port for receiving a pressurized non-reactive gas such as N2 supplied, and a drain. The port connected to the system (Drain), the port connected to the transmission line (300), and the port connected to the sample ring (120) through the intermediate pressure gate valve (V18).

注射閥(130)根據位於主系統(200)的控制部(250)等控制而轉換裝載位置(Load Position)與傳輸位置(Delivery Position)兩個位置。優選地,傳遞環(140)的體積大於樣品器皿(120)的體積或樣品器皿(120)與DI器皿(110)合起來的體積。The injection valve (130) switches between the load position and the delivery position according to a control unit (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) combined with the DI vessel (110).

DI器皿(110)、樣品器皿(120)及傳遞環(140)借助一個以上中壓閘閥與注射閥(注射閥為裝載位置時)而串聯連接,按DI器皿、樣品器皿及傳遞環的順序連接。由此,將暫時存儲於DI器皿(110)的去離子水與暫時存儲於樣品器皿(120)的化學製品傳輸並填充至傳遞環(140)時,去離子水清洗樣品器皿(120)的化學製品,並且,不會殘留化學製品並能夠全部傳輸至傳遞環(140)。當將化學製品暫時存儲於樣品器皿(120)時,存儲設定的量,中間發生損耗(Loss)時,並非為所希望的,但根據所述結構而不發生殘留地全部傳輸至傳遞環(140)。The DI vessel (110), the sample vessel (120) and the transfer ring (140) are connected in series by means of more than one medium-pressure gate valve and the injection valve (when the injection valve is in the loading position), and are connected in the order of the DI vessel, the sample vessel and the transfer ring. . Thus, the chemistry of the sample vessel (120) is cleaned by deionized water when the deionized water temporarily stored in the DI vessel (110) and the chemical temporarily stored in the sample vessel (120) are transferred and filled into the transfer ring (140). The article, and without leaving the chemical and capable of being completely transferred to the transfer ring (140). When the chemical is temporarily stored in the sample vessel (120), the set amount is stored, and loss (Loss) occurs in the middle, which is not desirable, but is not completely transferred to the transfer ring according to the structure. ).

下面,對取樣單元(100)的運行進行說明。Next, the operation of the sampling unit (100) will be described.

首先,由監測點通過中壓閘閥(V17)而導入化學製品,開啟中壓閘閥(V11、V14、V17)。化學製品的導入通過賦予化學製品本身的正壓,或使用設置於排水系統(Drain)的泵(未圖示)等而執行。在導入的初期步驟中所導入的化學製品經過樣品器皿(120)而通過中壓閘閥(V14)及中壓閘閥(V11)而由排水系統排出,在排出一定量之後,關閉中壓閘閥,填充與樣品器皿(120)的體積對應的量(正確的為與相鄰的中壓閘閥之間的空間對應的量,在現實中,與樣品器皿相鄰的中壓閘閥之間的距離設計地非常接近)。通過感測器(S12)確認化學製品被正常導入的情況。First, the chemical is introduced from the monitoring point through the medium pressure gate valve (V17), and the medium pressure gate valve (V11, V14, V17) is opened. The introduction of the chemical is performed by applying a positive pressure to the chemical itself or by using a pump (not shown) or the like provided in a drain system (Drain). The chemical introduced in the initial step of the introduction passes through the sample vessel (120) and is discharged by the drainage system through the intermediate pressure gate valve (V14) and the intermediate pressure gate valve (V11). After discharging a certain amount, the medium pressure gate valve is closed and filled. The amount corresponding to the volume of the sample vessel (120) (correctly the amount corresponding to the space between adjacent medium-pressure gate valves, in reality, the distance between the medium-pressure gate valves adjacent to the sample vessel is designed very Close). It is confirmed by the sensor (S12) that the chemical is normally introduced.

並且,在將化學製品填充至樣品器皿(120)之前,打開中壓閘閥(V16、V12、V14、V18),在將注射閥(130)作為裝載位置的狀態下,利用N2等非反應性氣體而騰空DI器皿(110)及樣品器皿(120)。Further, the intermediate pressure gate valve (V16, V12, V14, V18) is opened before the chemical is filled into the sample vessel (120), and the non-reactive gas such as N2 is used in a state where the injection valve (130) is used as the loading position. And vacate the DI vessel (110) and the sample vessel (120).

在需要稀釋的情況下,將去離子水(DI)填充至DI器皿(110)而使用。打開中壓閘閥(V15、V12、V11),在初期,去離子水通過DI器皿(110)而流至排水系統(Drain),在排出一定量之後,關閉中壓閘閥而將去離子水填充至DI器皿(110)。Deionized water (DI) is filled into the DI vessel (110) for use in the case where dilution is required. Open the medium pressure gate valve (V15, V12, V11). At the beginning, the deionized water flows through the DI vessel (110) to the drainage system (Drain). After discharging a certain amount, the medium pressure gate valve is closed to fill the deionized water to DI vessel (110).

稀釋比例通過樣品器皿與DI器皿的體積比例而設定,所填充的化學製品與去離子水移動而填充至與一端的注射閥(130)連接的傳遞環(140)。填充的方式如附圖所示,使用N2等氣體加壓或泵等,注射閥(130)的位置必須為裝載位置(load position),樣品被填充至傳遞環(140)的情況通過感測器(S13)檢測。如上所示,將暫時存儲於樣品器皿(120)的化學製品與暫時存儲於DI器皿(110)的去離子水由注射閥(130)的裝載位置移動並填充至傳遞環(140)而成為傳輸樣品。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. The filling method is as shown in the drawing, using N2 or other gas pressurization or pump, etc., the position of the injection valve (130) must be the load position, and the sample is filled into the transfer ring (140) through the sensor. (S13) Detection. As indicated above, the chemical temporarily stored in the sample vessel (120) and the deionized water temporarily stored in the DI vessel (110) are moved by the loading position of the injection valve (130) and filled into the transfer ring (140) to be transported. sample.

本發明的一個特徵為有選擇地稀釋化學製品的樣品而傳輸。取樣單元(100)將所導入的化學製品有選擇地通過去離子水稀釋,生成降低黏度的傳輸樣品而傳輸。硫酸、磷酸等化學製品因黏度高,將其直接通過本發明的封裝方法傳輸時,無法順暢推動,由此,存在傳輸中浪費大量時間並傳輸中造成損耗(Loss)的問題。根據本發明的一個特徵,在通過封裝方法傳輸時,稀釋硫酸、磷酸等化學製品的樣品而傳輸,具有能夠更順暢有效並可靠得傳輸樣品的效果。One feature of the invention is the selective dilution of a sample of the chemical for transport. The sampling unit (100) selectively dilutes the introduced chemical by deionized water to produce a reduced viscosity transport sample for transport. Since a chemical such as sulfuric acid or phosphoric acid has a high viscosity and is directly transported by the encapsulation method of the present invention, it cannot be smoothly pushed, and thus there is a problem that a lot of time is wasted in transmission and loss (Loss) is caused during transmission. According to a feature of the present invention, when a sample of a chemical such as sulfuric acid or phosphoric acid is diluted and transported by the encapsulation method, it has an effect of being able to transmit the sample more smoothly and efficiently and reliably.

並且,填充至傳遞環(140)的傳輸樣品通過傳輸線(300)而大部分長距離快速傳輸,從而,傳輸至主系統(200)。為此,首先,注射閥(130)轉換為傳輸位置(Delivery Position),在傳輸位置的狀態下,在圖面下側所示,通過高壓對N2或Ar等非反應性氣體施壓時,位於傳遞環的傳輸樣品通過傳輸線(300)傳輸。在注射閥(130)的傳輸位置通過非反應性氣體推動填充至傳遞環(140)的傳輸樣品,並通過傳輸線(300)傳輸。並且,此時,在傳輸線(300)內,傳輸樣品(A)的情況如圖2說明所示。Also, the transport sample filled to the transfer ring (140) is quickly transmitted over most of the long distance through the transmission line (300), thereby being transmitted to the host system (200). To this end, first, the injection valve (130) is converted into a delivery position (Delivery Position), and in the state of the transmission position, as shown on the lower side of the drawing, when a non-reactive gas such as N2 or Ar is pressed by a high pressure, it is located. The transport sample of the transfer ring is transmitted through the transmission line (300). The transport sample filled to the transfer ring (140) is pushed by the non-reactive gas at the transfer position of the injection valve (130) and transported through the transfer line (300). Further, at this time, the case where the sample (A) is transported in the transmission line (300) is as shown in FIG.

另外,為了檢驗,取樣單元(100)通過中壓閘閥(V13)而將檢驗溶液從位於附近或位於主系統(200)的檢驗溶液供應部(260)而填充至傳遞環(140),此時,打開中壓閘閥(V13、V14、V18),在將注射閥(130)作為裝載位置的狀態下,將檢驗溶液填充至傳遞環(140)。檢驗溶液例如是一種將污染物進入特定化學製品,而預先知曉污染物的種類及濃度的標準溶液。In addition, for inspection, the sampling unit (100) fills the test solution (260) from the test solution supply portion (260) located nearby or located in the main system (200) through the intermediate pressure gate valve (V13), at this time, The medium pressure gate valve (V13, V14, V18) is opened, and the test solution is filled into the transfer ring (140) with the injection valve (130) as the loading position. The test solution is, for example, a standard solution that introduces contaminants into a particular chemical while knowing in advance the type and concentration of the contaminant.

並且,在將傳輸樣品進行傳輸之後,取樣單元(100)的內部通道通過去離子水或化學製品清洗。例如,打開中壓閘閥(V16、V12、V14、V18),在將注射閥(130)作為裝載位置的狀態下,將去離子水(DI)流至排水系統(Drain)而清洗。Also, after the transport sample is transported, the internal passage of the sampling unit (100) is cleaned by deionized water or chemicals. For example, the medium-pressure gate valves (V16, V12, V14, and V18) are opened, and the deionized water (DI) is flowed to the drain system (Drain) to be cleaned with the injection valve (130) as the loading position.

在進行傳輸樣品的傳輸之後,傳輸線(300)利用去離子水或化學製品清洗。例如,將去離子水裝載至傳遞環(140)之後,執行多次反復傳輸的過程的方法。並且,一個取樣單元(100)從多個監測點採取樣品而傳輸,形成多個如圖3所示的結構。After the transfer of the transport sample, the transfer line (300) is cleaned with deionized water or chemicals. For example, a method of performing a process of repeated transmissions after loading deionized water to the transfer ring (140). And, a sampling unit (100) transmits samples from a plurality of monitoring points to form a plurality of structures as shown in FIG.

圖4為顯示本發明的一實施例的主系統(200)的結構的框圖。4 is a block diagram showing the structure of a main system (200) according to an embodiment of the present invention.

主系統(200)包括:樣品接收部(210)、預處理部(220)、導入部(230)、分析儀(240)、控制部(250)及檢驗溶液供應部(260)。The main system (200) includes a sample receiving unit (210), a pre-processing unit (220), an introduction unit (230), an analyzer (240), a control unit (250), and a test solution supply unit (260).

樣品接收部(210)通過傳輸線(300)從連接的多個取樣單元(100)接收傳輸樣品。例如,樣品接收部(210)的傳輸線(300)的一端或由此延伸的線包含供從向內部垂掛的缸形的器皿(下面未圖示)與器皿接收的傳輸樣品移送至將下文敘述的預處理部(220)的線等,並具有與傳輸線的數量對應,或按傳輸線的組分別對應的數量的器皿。The sample receiving portion (210) receives the transport sample from the connected plurality of sampling units (100) through the transmission line (300). For example, one end of the transmission line (300) of the sample receiving portion (210) or a line extending therefrom includes a transport sample for receiving from a cylinder-shaped vessel (not shown) suspended inside from the vessel and transported to the vessel to be described later. The line of the pre-processing unit (220) or the like has a number of vessels corresponding to the number of transmission lines or corresponding to the group of transmission lines.

預處理部(220)與樣品接收部(210)連接,在將接收從樣品接收部(210)移送的傳輸樣品容納於前置處理器皿的狀態下,蒸發傳輸樣品的液體,留下污染物,並將留下的污染物作為回收溶液而生成回收的樣品(下面稱為“回收樣品”)。The pre-processing unit (220) is connected to the sample receiving unit (210), and evaporates the liquid of the sample to be transported, leaving the contaminant, in a state in which the transport sample received from the sample receiving unit (210) is received in the pre-processor vessel. The remaining contaminants are used as a recovery solution to produce a recovered sample (hereinafter referred to as "recycled sample").

導入部(230)位於預處理部(220)的後端,並將定量的回收樣品導入分析儀(240),執行供應用於其它分析儀(240)的刻度的標準溶液與有選擇地通過去離子水稀釋回收樣品的功能。The introduction portion (230) is located at the rear end of the pretreatment portion (220), and introduces a quantitative recovered sample into the analyzer (240), performs a standard solution for supplying the scale for the other analyzer (240), and selectively passes Ion water dilution to recover the function of the sample.

分析儀(240)為對存在於樣品內的物質進行分析的公知的設備,分析是否發生污染、污染物的種類、污染物的濃度或含量等,並且,為HPIC、ICPMS、ICP-AES、AAS、HPLC、CE、UV-vis、Fluorescence等,優選的為ICP-MS。The analyzer (240) is a well-known device for analyzing substances present in the sample, and analyzes whether or not pollution, the type of the contaminant, the concentration or content of the contaminant, and the like, and is HPIC, ICPMS, ICP-AES, AAS. HPLC, CE, UV-vis, Fluorescence, etc., preferably ICP-MS.

控制部(250)控制主系統(200)的各個部分與取樣單元(100),例如,接收由感測器的傳感信號並與分析儀連接,控制中壓閘閥及注射閥等。檢驗溶液供應部(260)執行將檢驗溶液(標準溶液)供應至取樣單元(100)而用於檢驗的功能。The control unit (250) controls each part of the main system (200) and the sampling unit (100), for example, receives the sensing signal from the sensor and is connected to the analyzer, and controls the intermediate pressure gate valve and the injection valve. The test solution supply section (260) performs a function of supplying a test solution (standard solution) to the sampling unit (100) for inspection.

圖5為顯示本發明的一實施例的預處理部(220)的結構的附圖。Fig. 5 is a view showing the configuration of a preprocessing section (220) according to an embodiment of the present invention.

預處理部(220)在將傳輸樣品容納於前置處理器皿(221)的狀態下,蒸發傳輸樣品的液體並留下污染物,並生成將通過回收溶液而回收留下的污染物的樣品(“回收樣品”)。預處理部(220)對化學製品的樣品進行加熱,蒸發而去除液體,並且,僅留下金屬成分的污染物,並回收而分析。The pre-processing section (220) evaporates the liquid of the sample to be transported while leaving the transport sample in the pre-processor vessel (221) and leaves a contaminant, and generates a sample of the contaminant to be recovered by recovering the solution ( "Recycling samples"). The pretreatment section (220) heats the sample of the chemical, evaporates to remove the liquid, and leaves only the contaminants of the metal component, and recovers and analyzes.

預處理部(220)包括:前置處理器皿(221)、外部器皿(Outer Vessel)(222)、加熱器(Heater)(223)、冷卻器(Cooler)(224)、第一注射閥(225)、第二注射閥(226)與多個中壓閘閥(V21、V22、V23等),具有加熱及冷卻功能、定量供應回收溶液功能、導入定量樣品功能及移送及清洗預處理樣品的功能。The pre-processing section (220) includes: a front processor vessel (221), an outer vessel (Outer Vessel) (222), a heater (223), a cooler (224), a first injection valve (225). The second injection valve (226) and the plurality of medium-pressure gate valves (V21, V22, V23, etc.) have the functions of heating and cooling, quantitatively supplying the recovered solution, introducing the quantitative sample function, and transferring and cleaning the pre-treated sample.

前置處理器皿(221)的材質為石英、PTFE、PFA或PEEK,具有紅外線透過性,至少透過自加熱器(223)的紅外線,偏好耐化學性及耐熱性材質。並且,前置處理器皿(221)的下部為U字形或V字形,由此,易於將少量的回收樣品導入至分析儀。The material of the front processor plate (221) is quartz, PTFE, PFA or PEEK, which has infrared transmittance, at least infrared rays transmitted from the heater (223), and prefers chemical resistance and heat resistance. Further, the lower portion of the front processing vessel (221) has a U-shape or a V-shape, whereby it is easy to introduce a small amount of the recovered sample to the analyzer.

前置處理器皿(221)的外部被外部器皿(222)環繞,並且,容納由前置處理器皿(221)溢出的液體。The exterior of the front processor vessel (221) is surrounded by an outer vessel (222) and houses the liquid overflowing by the pre-processor vessel (221).

加熱器(223)對容納於前置處理器皿(222)的樣品的液體蒸發並濃縮,優選地,蒸發所有液體並僅留下金屬等污染物。The heater (223) evaporates and concentrates the liquid contained in the sample of the pre-processor vessel (222), preferably, evaporates all of the liquid and leaves only contaminants such as metals.

加熱器(223)使用紅外線(IR)或鹵素(Halogen)等燈式加熱器。對於耐化學性塑膠材質,大致在250度~300度左右發生變形,但燈式加熱器施加輻射熱時,由耐化學性優秀的塑膠形成的前置處理器皿(221)的溫度不會發生大地增加,而僅加熱位於前置處理器皿(221)的內部的樣品。並且,也能夠解決當前置處理器皿的溫度變高時必須冷卻,但一般地因冷卻時間比升溫花費更長時間,不適應線上(On-line)樣品處理等問題。The heater (223) uses a lamp heater such as infrared (IR) or halogen (Halogen). For chemical resistant plastic materials, the deformation is about 250 to 300 degrees. However, when the radiant heat is applied to the lamp heater, the temperature of the front processor (221) formed of plastic with excellent chemical resistance does not increase greatly. Only the sample located inside the front processor vessel (221) is heated. Further, it is also possible to solve the problem that cooling is required when the temperature of the current processing vessel becomes high. However, generally, the cooling time takes longer than the temperature rise, and the problem of on-line sample processing is not satisfied.

根據本發明的一個特徵,將前置處理器皿由紅外線透過性材質形成,並將對前置處理器皿進行加熱的加熱器製造為燈式,由此,具有如下效果,未極大增加前置處理器皿的溫度,由此,能夠快速冷卻,從而,能夠快速進行樣品的污染分析。According to a feature of the present invention, the front processor vessel is formed of an infrared ray transmissive material, and the heater for heating the front processor vessel is made into a lamp type, thereby having the following effects without greatly increasing the front processor vessel. The temperature, by which, enables rapid cooling, thereby enabling rapid contamination analysis of the sample.

並且,加熱器(223)除了使用燈式之外,一般能夠使用全熱加熱器、碳加熱器、帕爾貼(Peltier)、微波(microwave)、hotN2等。Further, in addition to the lamp type, the heater (223) can generally use a full heat heater, a carbon heater, a Peltier, a microwave, a hotN2, or the like.

第一注射閥(225)用於將樣品(傳輸樣品)導入前置處理器皿(221),第二注射閥(225)為用於將回收溶液導入至前置處理器皿(221)。The first injection valve (225) is for introducing a sample (transfer sample) into the front processor vessel (221), and the second injection valve (225) is for introducing the recovery solution to the front processor vessel (221).

回收溶液用於融化乾燥的樣品(污染物),設定體積的回收溶液被供應至前置處理器皿(221)。回收溶液為金屬污染物時,能夠利用硝酸或氫氟酸+過氧化氫等酸系列。The recovered solution is used to melt the dried sample (contaminant) and the set volume of the recovered solution is supplied to the pre-treatment vessel (221). When the recovered solution is a metal contaminant, an acid series such as nitric acid or hydrofluoric acid + hydrogen peroxide can be used.

下面,對本發明的一實施例的預處理部(220)的動作進行說明。Next, the operation of the preprocessing unit (220) according to an embodiment of the present invention will be described.

首先,將傳輸樣品由樣品接收部(210)的器皿傳輸至前置處理器皿(221),此時,使用圖示的第一注射閥(injection valve)(225)或定量泵系統等,以用於導入定量的樣品。例如,在第一注射閥(225)的裝載位置將樣品裝載至注射閥的樣品環,在注射位置上借助通過非反應性氣體施壓的結構(227)等而將裝載的樣品移送至前置處理器皿(221)。First, the transport sample is transported from the vessel of the sample receiving portion (210) to the pre-processor vessel (221), at which time, using the illustrated first injection valve (225) or a metering pump system, etc., For the introduction of quantitative samples. 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 front by the structure (227) or the like pressurized by the non-reactive gas at the injection position. Processor vessel (221).

並且,利用加熱器(223)的能量而加熱前置處理器皿(221)的樣品,蒸發液體並僅留下要分析的污染物。當樣品的液體被蒸發時,僅樣品內的污染物留在前置處理器皿(221)的底部,當通過少於傳輸樣品的量的回收溶液而回收所留下的污染物時,能夠獲得濃縮效果。例如,被蒸發的液體(化學製品)為硫酸、磷酸、氫氟酸、氫氧化銨、IPA等。Also, the sample of the front processor vessel (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 in the sample remain at the bottom of the pre-treatment vessel (221), and when the contaminant remaining is recovered by the recovery solution less than the amount of the sample transferred, the concentration can be obtained. effect. For example, the liquid (chemical) to be evaporated is sulfuric acid, phosphoric acid, hydrofluoric acid, ammonium hydroxide, IPA, or the like.

並且,利用冷卻器(224)而對前置處理器皿(221)進行冷卻,用於乾燥樣品而加熱的前置處理器皿(221)必須冷卻,以用於回收的準確性。如上所述,燈式易於冷卻,並且,通過N2等氣體的分散也容易冷卻。對於其它的冷卻方式,能夠採用利用冷卻水的方式或利用Peltier元素的方式等。Also, the front processor vessel (221) is cooled by a cooler (224), and the heated front processor vessel (221) for drying the sample must be cooled for accuracy of recovery. As described above, the lamp type is easy to cool, and is easily cooled by dispersion of a gas such as N2. For other cooling methods, a method using cooling water or a method using a Peltier element can be employed.

並且,為了對殘留在前置處理器皿(221)的污染物進行分析而作為回收溶液回收。在供應回收溶液之前,前置處理器皿(221)必須冷卻至常溫,為了導入定量回收溶液而使用圖示的第二注射閥(226)或定量泵系統等。例如,在第二注射閥(226)的裝載位置將回收溶液裝載在注射閥的樣品環,在注射位置借助通過非反應性氣體而施壓的結構(228)等將所裝載的回收溶液移送至前置處理器皿(221)。將設定體積的回收溶液供應至前置處理器皿而融化乾燥的樣品,回收溶液為硝酸或氫氟酸+過氧化氫等。Further, in order to analyze the contaminants remaining in the pre-processor vessel (221), it is recovered as a recovery solution. The pretreatment vessel (221) must be cooled to normal temperature before the recovery solution is supplied, and the second injection valve (226) or the metering pump system or the like shown in the figure is used in order to introduce the quantitative recovery solution. For example, the recovery solution is loaded in 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 injection site by means of a structure (228) or the like pressurized by a non-reactive gas. Front processor plate (221). The set volume of the recovered solution is supplied to the front processor vessel to melt the dried sample, and the recovered solution is nitric acid or hydrofluoric acid + hydrogen peroxide.

並且,所回收的樣品(回收樣品)經過導入部而移送至分析儀進行分析。在開啟中壓閘閥(V23)的狀態下,前置處理器皿(221)的回收樣品被裝載至與下面所述的導入部(230;參照圖6)的注射閥(231)結合的樣品環,之後移送至分析儀(240)。對於裝載樣品環,使用氣體施壓或泵等而執行。Then, the collected sample (recovered sample) is transferred to the analyzer through the introduction portion for analysis. In the state where the intermediate pressure gate valve (V23) is opened, the recovered sample of the front processor vessel (221) is loaded to the sample loop combined with the injection valve (231) of the introduction portion (230; see Fig. 6) described below. It is then transferred to the analyzer (240). For loading the sample loop, it is performed using gas pressure or a pump or the like.

在樣品的預處理與移送後,清洗移動路徑與前置處理器皿而達到初期化。為了提高清洗效率,器皿形成為溢流式的結構(over flow type),具有外部器皿(222)以使環繞前置處理器皿(221)。加熱器(223)形成於外部器皿(224)的外部或內部,對於形成於外部的情況,外部器皿(224)也由紅外線透過性材質構成。前置處理器皿能偶利用去離子水或清洗液清洗,從而保持清潔狀態。After pre-treatment and transfer of the sample, the moving path and the pre-processor vessel are cleaned to achieve initialization. To improve cleaning efficiency, the vessel is formed in an over flow type with an outer vessel (222) to surround the front processor vessel (221). The heater (223) is formed outside or inside the outer vessel (224), and the outer vessel (224) is also made of an infrared permeable material when it is formed outside. The front processor can be cleaned with deionized water or cleaning solution to keep it clean.

根據本發明的一個特徵,增加對樣品的預處理功能。化學製品樣品的成分以有機性、酸性、鹼性等各種性質存在。相同濃度的污染物存在各不相同的性狀時,分析結果不同。該化學製品的主要成分因矩陣不同,而發生樣品導入過程中的差異、分析時幹擾影響差異等。並且,即使為相同的性狀,但因密度及成分差異,而發生如上所述的影響。並且,間或因樣品內的污染物的濃度太低,也存在不易於利用分析儀進行的分析的情況。According to one feature of the invention, the pre-treatment function of the sample is increased. The components of the chemical sample exist in various properties such as organic, acidic, and basic. When the same concentration of contaminants has different traits, the analysis results are different. The main components of the chemical are different in matrix, and the difference in the sample introduction process and the difference in interference during analysis are caused. Further, even if they are of the same trait, the effects as described above occur due to the difference in density and composition. Also, there may be cases where the concentration of the contaminants in the sample is too low, and there is also an analysis that is not easily performed by the analyzer.

根據本發明的一個特徵,執行利用樣品的溶液的蒸發與回收溶液的回收,由此,矩陣的成分及密度等相同,而且,並非以開放狀態而是密閉狀態自動執行該過程,由此,具有達到分析的準確度,同時得到穩定性的效果。According to a feature of the present invention, the evaporation of the solution using the sample and the recovery of the recovery solution are performed, whereby the composition and density of the matrix are the same, and the process is not automatically performed in an open state but in a sealed state, thereby having Achieve the accuracy of the analysis while achieving the effect of stability.

圖6為顯示本發明的一實施例的導入部(230)的結構的附圖。Fig. 6 is a view showing the configuration of an introduction portion (230) according to an embodiment of the present invention.

導入部(230)位於預處理部(220)的後端,將定量回收樣品導入至分析儀(240),執行用於其它分析儀(240)的刻度的標準溶液的供應及有選擇地作為去離子水稀釋回收樣品的功能。The introduction portion (230) is located at the rear end of the pretreatment portion (220), introduces the quantitatively recovered sample to the analyzer (240), performs the supply of the standard solution for the calibration of the other analyzer (240), and selectively acts as a Ion water dilution to recover the function of the sample.

在第一注射閥(231)的裝載位置上從預處理部(220)的前置處理器皿將回收樣品裝載至樣品環,在注射位置上通過定量泵(P22)推動去離子水而將裝載至樣品環的回收樣品移送至分析儀(240)側。The recovered sample is loaded from the front processing vessel of the pretreatment portion (220) to the sample loop at the loading position of the first injection valve (231), and the deionized water is pushed by the metering pump (P22) at the injection position to be loaded to The recovered sample of the sample loop is transferred to the side of the analyzer (240).

在導入至分析儀的路徑上具有T字管(233),將回收樣品導入至分析儀(240)時,有選擇地利用定量泵(P21)而將去離子水導入至T字管(233),稀釋回收樣品,且稀釋比例根據各個定量泵推動的去離子水的量(流量)決定。A T-tube (233) is provided on the path to the analyzer, and when the recovered sample is introduced into the analyzer (240), the metering pump (P21) is selectively used to introduce the deionized water into the T-tube (233). The sample is diluted and recovered, and the dilution ratio is determined according to the amount (flow rate) of deionized water pushed by each metering pump.

在第二注射閥(232)的裝載位置上標準溶液被裝載至第二注射閥(232)的樣品環,在注射位置上通過定量泵而推動作為去離子水而裝載的標準溶液,供應至分析儀(240)並對分析儀(240)進行刻度。At the loading position of the second injection valve (232), the standard solution is loaded to the sample loop of the second injection valve (232), and the standard solution loaded as deionized water is pushed by the metering pump at the injection position, and supplied to the analysis. The meter (240) scales the analyzer (240).

感測器(S21、S22)接近設置於樣品環,檢測填充至樣品環的樣品或標準溶液。The sensor (S21, S22) is placed close to the sample loop to detect a sample or standard solution filled to the sample loop.

圖7為顯示本發明的一實施例的檢驗溶液供應部(260)的結構的附圖。Fig. 7 is a view showing the structure of a test solution supply portion (260) according to an embodiment of the present invention.

檢驗溶液供應部(260)為將檢驗溶液供應至取樣單元(100)的裝置,將傳輸樣品通過分析儀分析的結果檢測為污染時,取樣單元(100)將檢驗溶液通過傳輸線(300)而再次傳輸,並通過分析儀進行檢驗。The test solution supply portion (260) is a device for supplying the test solution to the sampling unit (100), and when the result of the analysis of the transport sample by the analyzer is detected as contamination, the sampling unit (100) passes the test solution through the transfer line (300) again. Transfer and test by analyzer.

作為一實施例,檢驗溶液供應部(260)包含於主系統(200)而構成,從檢驗溶液供應部(260)通過供應線(310)將檢驗溶液供應至各個取樣單元(100),系統能夠更有效地形成。As an embodiment, the test solution supply portion (260) is included in the main system (200), and the test solution is supplied from the test solution supply portion (260) to the respective sampling units (100) through the supply line (310), and the system can Formed more efficiently.

檢驗溶液(標準溶液)通過打開中壓閘閥(V24、V27)並顯示的泵(P)或利用加壓或減壓而填充至檢驗溶液箱(261),對於填充檢驗溶液的情況通過感測器(光感測器、接近感測器等)(S23)確認。The test solution (standard solution) is filled into the test solution tank (261) by opening the medium pressure gate valve (V24, V27) and displaying the pump (P) or by pressurizing or depressurizing, and passing the sensor for filling the test solution (Photosensor, proximity sensor, etc.) (S23) Confirmation.

並且,填充至檢驗溶液箱(261)的檢驗溶液,打開中壓閘閥(V26、V29)並通過對N2等非反應性氣體加壓而通過傳輸線(310)傳輸,以用於供應至取樣單元(100).傳輸的檢驗溶液通過閥而最終存儲至取樣單元(100)的傳遞環(delivery loop),之後,再次通過傳輸線(300)傳輸至主系統並進行分析。被傳輸至主系統的檢驗溶液通過普通分析順序而分析及判斷結果。And, the test solution filled into the test solution tank (261) is opened, the medium pressure gate valve (V26, V29) is opened and transmitted through the transmission line (310) by pressurizing a non-reactive gas such as N2 for supply to the sampling unit ( 100). The transmitted test solution is finally stored in the delivery loop of the sampling unit (100) through the valve, and then transmitted again to the main system through the transmission line (300) and analyzed. The test solution transmitted to the main system is analyzed and judged by the ordinary analysis sequence.

在對圍繞檢驗過程的主要運行過程進行說明時,如下所示,主要過程的控制通過主系統(200)的控制部(250)執行。In explaining the main operation process surrounding the inspection process, as shown below, the control of the main process is performed by the control section (250) of the main system (200).

一般而言,各個取樣單元(100)將樣品傳輸至主系統(200)時,主系統(200)接收傳輸樣品而分析。In general, when each sampling unit (100) transmits a sample to the host system (200), the host system (200) receives the transmitted sample for analysis.

但,根據該分析結果而檢測污染時,主系統(200)的控制部(250)向使用者發出第一次報警,使位於主系統(100)等的檢驗溶液供應部(260)將檢驗溶液(標準溶液)供應至相應取樣單元(100),取樣單元(100)通過相同的傳輸線(300)傳輸檢驗溶液,以用於檢驗,並且,主系統(200)對所接收的檢驗溶液進行分析。即,將包含知曉種類及濃度的污染物的標準溶液通過相同的路徑由取樣單元傳輸至主系統,通過與之前分析相同的分析方法進行分析。However, when the contamination is detected based on the analysis result, the control unit (250) of the main system (200) issues a first alarm to the user, so that the test solution supply unit (260) located at the main system (100) or the like will check the solution. (Standard solution) is supplied to the corresponding sampling unit (100), the sampling unit (100) transmits the inspection solution through the same transmission line (300) for inspection, and the main system (200) analyzes the received inspection solution. That is, a standard solution containing contaminants of known species 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.

當所傳輸的檢驗溶液的分析結果與對檢驗溶液的預測存在差異時,判斷污染監測系統存在異常。當分析結果與檢驗溶液的預測相同時,判斷污染監測系統正常。例如,檢測與包含於檢驗溶液的污染物不同種類的污染物,或污染物的種類相同,但包含於檢驗溶液的污染物的濃度顯示存在超過規定範圍的差異時,判斷污染監測系統存在異常。When there is a difference between the analysis result of the transmitted test solution and the prediction of the test solution, it is judged that there is an abnormality in the pollution monitoring system. When the analysis result is the same as the prediction of the test solution, it is judged that the pollution monitoring system is normal. For example, when the type of contaminant different from the contaminant contained in the test solution or the type of the contaminant is detected, but the concentration of the contaminant contained in the test solution indicates that there is a difference exceeding the prescribed range, it is judged that the pollution monitoring system is abnormal.

當判斷污染監測系統正常時,對化學製品的樣品進行再次分析,再次確認分析結果為污染時,發出第二次報警,並終止生成。並且,判斷污染監測系統存在異常時,將污染監測系統的異常情況向使用者發車報警。When it is judged that the pollution monitoring system is normal, the chemical sample is re-analyzed, and when the analysis result is confirmed as contamination, a second alarm is issued and the generation is terminated. Moreover, when it is determined that there is an abnormality in the pollution monitoring system, the abnormal situation of the pollution monitoring system is sent to the user to give an alarm.

在生產線上,污染問題與收益率及生產力存在密切關聯,必須進行非常重要地管理。假如,檢測污染時,必須中斷生產工藝,而防止發生大量不良現象。但,當污染分析結果不存在可靠性時,反而會因錯誤的分析結果而因生產中斷而造成極大損失。On the production line, pollution problems are closely related to profitability and productivity and must be managed very importantly. If pollution is detected, the production process must be interrupted to prevent a large number of undesirable phenomena. However, when there is no reliability in the results of the pollution analysis, it will cause a great loss due to the interruption of production due to the wrong analysis result.

根據本發明的一個特徵,具有如下效果,具有檢驗溶液供應部,其將檢驗溶液供應至取樣單元,並且,當將傳輸樣品通過分析儀分析的結果檢測為污染時,取樣單元通過相同的傳輸線傳輸檢驗溶液,並通過分析儀而檢驗,能夠對因發送錯誤的污染報警而造成生產中斷的問題防患於未然。According to a feature of the present invention, there is an effect of having a test solution supply portion that supplies a test solution to a sampling unit, and, when the result of the analysis of the transport sample by the analyzer is detected as contamination, the sampling unit transmits through the same transmission line The test solution is inspected by an analyzer, and it is possible to prevent the problem of production interruption due to the transmission of an erroneous pollution alarm.

本發明的有益效果在於:The beneficial effects of the invention are:

本發明的一實施例的線上污染監測系統及方法具有如下效果,將樣本從多個監測點傳輸至分析儀並進行分析,能夠確保可靠性與效率性。The online pollution monitoring system and method according to an embodiment of the present invention has an effect of transmitting samples from a plurality of monitoring points to an analyzer and performing analysis, thereby ensuring reliability and efficiency.

本發明的一實施例具有如下效果,將所導入的化學製品以封裝的方法傳輸時,通過去離子水稀釋而生成降低黏度的傳輸樣品並傳輸,由此,能夠更順暢、有效且可靠地傳輸樣品。An embodiment of the present invention has an effect of generating a transport sample having a reduced viscosity and transferring it by diluting with deionized water when transporting the introduced chemical product, thereby enabling smoother, more efficient, and more reliable transport. sample.

本發明的一實施例具有如下效果,將前置處理器皿通過紅外線透過的材料形成,將對前置處理器皿加熱的加熱器以燈式進行,由此,未極大增加前置處理器皿的溫度,從而,能夠快速冷卻,因而,能夠快速進行樣品的污染分析。An embodiment of the present invention has the following effects: the front processing vessel is formed by a material that transmits infrared rays, and the heater that heats the front processing vessel is lighted, thereby not greatly increasing the temperature of the front processing vessel. Thereby, rapid cooling can be performed, and thus, contamination analysis of the sample can be performed quickly.

本發明的一實施例具有如下效果,執行對樣品的溶液的蒸發與利用回收溶液的回收,保證矩陣的成分及密度等相同,另外,以密閉的狀態而非開放的狀態自動執行該過程,由此,保證分析的準確度,同時能夠獲取穩定性。An embodiment of the present invention has the effects of performing evaporation of a solution of a sample and recovery of a recovery solution, ensuring that the composition and density of the matrix are the same, and automatically performing the process in a closed state rather than an open state, This ensures the accuracy of the analysis while achieving stability.

本發明的一實施例具有如下效果,具有將檢驗溶液供應至取樣單元的檢驗溶液供應部,當檢測出通過所述分析儀分析的傳輸樣品的結果為污染時,取樣單元通過相同的傳輸線而傳輸檢驗溶液,並通過分析儀進行檢驗,對於因錯誤的污染情報而造成生產中斷的情況防患於未然。An embodiment of the present invention has an effect of supplying a test solution to a sampling solution supply unit of a sampling unit, and when detecting that the result of the transport sample analyzed by the analyzer is contamination, the sampling unit transmits through the same transmission line. The test solution is tested by an analyzer to prevent production interruptions due to incorrect contamination information.

100:取樣單元 110:DI器皿 120:樣品器皿 130:注射閥 140:傳遞環 200:主系統 210:樣品接收部 220:預處理部 221:前置處理器皿 222:外部器皿 223:加熱器 224:冷卻器 225、226、231、232:注射閥 227:借助通過非反應性氣體施壓的結構 230:導入部 233:T字管 240:分析儀 250:控制部 260:檢驗溶液供應部 261:檢驗溶液箱 300:傳輸線 310:供應線 P21、P22:定量泵 d:內徑 G:非反應性氣體 A:傳輸樣品 P:泵 S11、S12、S13、S21、S22、S23:感測器 V11~V18 、V21、V22、V23、V24、V26、V27、V29:中壓閘閥100: sampling unit 110: DI vessel 120: sample vessel 130: injection valve 140: transfer ring 200: main system 210: sample receiving portion 220: pre-processing portion 221: pre-processor tube 222: external vessel 223: heater 224: Cooler 225, 226, 231, 232: injection valve 227: structure 230 by pressure applied by non-reactive gas: introduction portion 233: T-tube 240: analyzer 250: control portion 260: inspection solution supply portion 261: inspection Solution tank 300: Transmission line 310: Supply line P21, P22: Dosing pump d: Inner diameter G: Non-reactive gas A: Transfer sample P: Pumps S11, S12, S13, S21, S22, S23: Sensors V11~V18 , V21, V22, V23, V24, V26, V27, V29: medium voltage gate valve

圖1為例示本發明的線上污染監測系統的整體拓撲結構的附圖; 圖2為顯示本發明的一實施例的傳輸線與通過傳輸線而傳輸的傳輸樣品的示例圖; 圖3為本發明的一實施例的取樣單元的結構圖; 圖4為顯示本發明的一實施例的主系統的結構的框圖; 圖5為顯示本發明的一實施例的預處理部的結構的附圖; 圖6為顯示本發明的一實施例的導入部的結構的附圖; 圖7為顯示本發明的一實施例的檢驗溶液供應部的結構的附圖。1 is a view showing an overall topology of an in-line pollution monitoring system of the present invention; FIG. 2 is a view showing an example of a transmission line and a transmission sample transmitted through a transmission line according to an embodiment of the present invention; Figure 4 is a block diagram showing the structure of a main system according to an embodiment of the present invention; and Figure 5 is a view showing the structure of a pre-processing unit according to an embodiment of the present invention; BRIEF DESCRIPTION OF THE DRAWINGS FIG. 7 is a view showing the structure of a test solution supply portion according to an embodiment of the present invention.

Claims (17)

一種線上污染監測系統,其特徵在於, 包括: 一取樣單元,通過與使用、存儲或供應一化學製品的一點連接的線而導入該化學製品,並生成要傳輸的一傳輸樣品; 一主系統,從該取樣單元接收該傳輸樣品而通過一分析儀分析, 其中,該主系統通過分散配置的多個該取樣單元與一傳輸線而呈放射狀連接, 在該傳輸線內,該傳輸樣品的一非反應性氣體位於前後而以封裝的狀態傳輸。An online pollution monitoring system, comprising: a sampling unit for introducing the chemical through a line connected to a point of using, storing or supplying a chemical, and generating a transport sample to be transported; Receiving the transport sample from the sampling unit for analysis by an analyzer, wherein the main system is radially connected to a plurality of the sampling units in a dispersed manner, and a non-reactive one of the transport samples is transmitted in the transmission line The gas is transported in a packaged state before and after it. 根據申請專利範圍1所述的線上污染監測系統,其特徵在於, 該傳輸線的內徑為0.5mm~1.6mm,該傳輸樣品以借助該非反應性氣體施壓的狀態傳輸。The online pollution monitoring system according to the invention of claim 1, wherein the transmission line has an inner diameter of 0.5 mm to 1.6 mm, and the transport sample is transported in a state of being pressurized by the non-reactive gas. 根據申請專利範圍1所述的線上污染監測系統,其特徵在於, 該取樣單元將導入的該化學製品通過一去離子水稀釋而生成降低黏度的該傳輸樣品。The online pollution monitoring system according to claim 1, wherein the sampling unit dilutes the introduced chemical product with a deionized water to generate the transport sample having reduced viscosity. 根據申請專利範圍3所述的線上污染監測系統,其特徵在於, 該取樣單元包括: 一樣品器皿,暫時存儲導入的定量的該化學製品; 一去離子水(DI)器皿,暫時存儲定量的該去離子水。The online pollution monitoring system according to claim 3, wherein the sampling unit comprises: a sample vessel for temporarily storing the introduced quantitative chemical; and a deionized water (DI) vessel for temporarily storing the quantitative amount of the chemical Deionized water. 根據申請專利範圍4所述的線上污染監測系統,其特徵在於, 該取樣單元還包括: 一注射閥,供一傳遞環的兩端與兩個口連接, i)從該注射閥的裝載位置將暫時存儲於該樣品器皿的化學製品與暫時存儲於該DI器皿的該去離子水移動並填充至該傳遞環而成為該傳輸樣品, ii)在該注射閥的一傳輸位置將填充至該傳遞環的該傳輸樣品通過該非反應性氣體推動並通過該傳輸線傳輸。The online pollution monitoring system of claim 4, wherein the sampling unit further comprises: an injection valve for connecting two ends of a transfer ring to the two ports, i) from a loading position of the injection valve The chemical temporarily stored in the sample vessel is moved with the deionized water temporarily stored in the DI vessel and filled into the transfer ring to become the transport sample, ii) a transfer position to be filled at the transfer valve of the injection valve The transferred sample is pushed by the non-reactive gas and transmitted through the transmission line. 根據申請專利範圍5所述的線上污染監測系統,其特徵在於, 該DI器皿,該樣品器皿及該傳遞環借助一個以上閥而串聯連接,該述DI器皿、該樣品器皿及該傳遞環的順序連接。The online pollution monitoring system according to claim 5, wherein the DI vessel, the sample vessel and the transfer ring are connected in series by means of one or more valves, and the DI vessel, the sample vessel and the transfer ring are sequentially arranged. connection. 根據申請專利範圍5所述的線上污染監測系統,其特徵在於, 該DI器皿及該樣品器皿為一線圈狀器皿。The online pollution monitoring system according to claim 5, wherein the DI vessel and the sample vessel are a coiled vessel. 根據申請專利範圍1所述的線上污染監測系統,其特徵在於, 該主系統包括: 一預處理部,在將該傳輸樣品容納於一前置處理器皿的狀態下,蒸發該傳輸樣品的液體,而留下一污染物,並生成通過一回收溶液回收留下的污染物的一回收樣品。The online pollution monitoring system of claim 1, wherein the main system comprises: a pre-processing unit that evaporates the liquid for transporting the sample while the transfer sample is contained in a front processing vessel A contaminant is left behind and a recovered sample of the contaminant left by a recovery solution is generated. 根據申請專利範圍8所述的線上污染監測系統,其特徵在於, 該預處理部包括燈式加熱器, 該前置處理器皿具有紅外線透過性,至少透過由該加熱器傳來的一紅外線。The online pollution monitoring system according to claim 8, wherein the pretreatment portion includes a lamp heater having infrared ray permeability and transmitting at least an infrared ray transmitted from the heater. 根據申請專利範圍9所述的線上污染監測系統,其特徵在於, 該前置處理器皿的材質為石英、PTFE、PFA或PEEK。The online pollution monitoring system according to claim 9 is characterized in that the material of the front processing vessel is quartz, PTFE, PFA or PEEK. 根據申請專利範圍8所述的線上污染監測系統,其特徵在於, 該前置處理器皿的下部為U字形或V字形。The online pollution monitoring system according to claim 8, wherein the lower portion of the front processor vessel has a U-shape or a V-shape. 根據申請專利範圍8所述的線上污染監測系統,其特徵在於, 該主系統包括: 一導入部,位於該預處理部的後端,並將定量的該回收樣品導入至該分析儀, 具有一T字管,有選擇地將一去離子水導入至通過該分析儀導入的一路徑,而用於稀釋該回收樣品。The online pollution monitoring system according to claim 8, wherein the main system comprises: an introduction portion located at a rear end of the pretreatment portion, and introducing the quantitative sample to the analyzer, having one A T-tube selectively introduces a deionized water into a path introduced by the analyzer for diluting the recovered sample. 根據申請專利範圍8所述的線上污染監測系統,其特徵在於, 該主系統還包括: 一控制部,控制該主系統的各個部分與多個該取樣單元。The online pollution monitoring system according to claim 8 is characterized in that the main system further comprises: a control unit that controls each part of the main system and a plurality of the sampling units. 根據申請專利範圍1所述的線上污染監測系統,其特徵在於, 還包括:一檢驗溶液供應部,將一檢驗溶液供應至該取樣單元, 當通過該分析儀對該傳輸樣品分析的結果檢測為污染時,該取樣單元將該檢驗溶液通過該傳輸線傳輸,通過該分析儀檢驗。The online pollution monitoring system according to claim 1, further comprising: a test solution supply unit that supplies a test solution to the sampling unit, and the result of analyzing the transmitted sample by the analyzer is detected as When contaminated, the sampling unit transmits the test solution through the transmission line and is inspected by the analyzer. 根據申請專利範圍14所述的線上污染監測系統,其特徵在於, 該檢驗溶液供應部形成於該主系統, 通過供應線將該檢驗溶液從該檢驗溶液供應部供應至各個該取樣單元。The online pollution monitoring system according to claim 14, wherein the test solution supply portion is formed in the main system, and the test solution is supplied from the test solution supply portion to each of the sampling units through a supply line. 一種線上污染監測方法,是一種線上污染監測系統中執行的線上污染監測方法,該線上污染監測系統包括:一取樣單元,通過與使用、存儲或供應一化學製品的一點連接的線而導該化學製品,並生成要傳輸的一傳輸樣品;主系統,從該取樣單元接收該傳輸樣品而通過一分析儀分析,其中,該主系統通過分散配置的多個該取樣單元與一傳輸線而呈放射狀連接,在該傳輸線內,該傳輸樣品的一非反應性氣體位於前後而以封裝的狀態傳輸,該線上污染監測方法特徵在於, 包括如下步驟: 一第一步驟,該主系統接收該傳輸樣品並分析; 一第二步驟,當檢測在該第一步驟的分析結果為污染時,該取樣單元將一檢驗溶液通過該傳輸線傳輸,並且,該主系統進行分析; 一第三-一步驟,當該第二步驟的分析結果與對該檢驗溶液的預測不同時,判斷該污染監測系統存在異常。An online pollution monitoring method is an online pollution monitoring method implemented in an online pollution monitoring system, the online pollution monitoring system comprising: a sampling unit that conducts the chemistry through a line connected to a point of using, storing or supplying a chemical product An article, and a transmission sample to be transmitted; a main system, receiving the transmission sample from the sampling unit and analyzing by an analyzer, wherein the main system is radially distributed by a plurality of the sampling units and a transmission line Connecting, in the transmission line, a non-reactive gas of the transport sample is transported in a packaged state before and after, the online pollution monitoring method is characterized in that the method comprises the following steps: a first step, the main system receives the transmitted sample and a second step, when detecting that the analysis result in the first step is contamination, the sampling unit transmits a test solution through the transmission line, and the main system performs analysis; a third-first step, when When the analysis result of the second step is different from the prediction of the test solution, the pollution monitoring system is judged There is an abnormality. 根據申請專利範圍16所述的線上污染監測方法,其特徵在於, 還包括:一第三-二步驟,當該第二步驟的分析結果與對該檢驗溶液的預測相同時,判斷該污染監測系統正常。The online pollution monitoring method according to claim 16, further comprising: a third-two step, determining the pollution monitoring system when the analysis result of the second step is the same as the prediction of the test solution normal.
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