![]() Method for automatic real-time analysis of an organic pollutant.
专利摘要:
The present invention relates to a method of the automatic real-time analysis system of an organic contaminant using a real-time solid phase microextraction GC or solid phase microextraction GC / MS analysis system, the method comprising the steps of: a step of continuously providing a sample for receiving a sample bottle in time a sample delivery line formed in the real-time solid phase microextraction GC or solid phase microextraction GC / MS analysis system; and a step for analyzing the sample; whereby the sample is constantly provided in real time, so that a generation time of a highly concentrated organic contaminant can be detected accurately and quickly and thus a corresponding subsequent measure can be taken. 公开号:CH711779B1 申请号:CH00348/17 申请日:2015-09-23 公开日:2019-09-30 发明作者:Choi In-Cheol;Chung Hyen-Mi;Jheong Weon-Hwa;Kwon Oh-Sang;Jeong Dong-Hwan;Park Su-Jeong;Cho Yang-Seok 申请人:Republic Of Korea Ministry Of Environment National Institute Of Environmental Res; IPC主号:
专利说明:
Step to analyze a sample CH 711 779 B1 Description Field of the Invention The present invention relates to a method for automatic real-time analysis of an organic contaminant using a real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system, by means of which the real-time, constant taking of a sample also using an existing analysis device a generation time of a high concentration of a harmful, organic pollutant can be recognized quickly and precisely and a suitable countermeasure can be taken in a water treatment plant, etc. PRIOR ART Due to industrialization and urbanization, environmental pollution has long emerged as social problems, while at the same time the systematic monitoring of drinking water quality, e.g. Protection of the drinking water supply source, administration and regulation of the plants for the discharge of the pollutants etc., become strict within the national framework. A basis for these controls is a quick and accurate measurement of the contaminants in the water. Since a quick water quality measurement in the drinking water supply sources associated with drinking water, purified water and tap water, etc. can enable a quick water purification process, it is even more important in view of safety. Organic contaminants managed by the water supply system include dozens of types of substances, such as volatile organic compounds, agrochemicals, disinfection by-products as well as tasting and malodorous substances, etc. Since these organic pollutants have harmful effects on human health or have a direct effect on the quality of tap water by causing an aesthetic problem, it is necessary to fill such pollutants fully and to manage entirely. Recently, the tasting and malodorous substances (geosmin, 2-MIB (methylisoborneol)) are increasingly being increased by the pollutants of this type in their concentration and production frequency flowing into the water treatment plant, because the algal bloom due to climate changes, e.g. Rises in water temperature and changes in rainfall patterns, etc., are caused more and more. Therefore, by using a water purification material such as e.g. powdery activated carbon, etc., in the water treatment plant and thus by taking quick countermeasures to less than an odor threshold before they can flow into a water supply network, so that customer complaints can be avoided. This requires more complete administration. In the current water treatment plants, the tasting and malodorous substances are analyzed in the normal state once or less per day and only when the high concentration of the same occurs twice a day, but it is currently not easy to measure a constantly changing water quality manually and thus take a countermeasure to the rapid water purification process. It is necessary to add in real time the volatile organic compounds and agrochemicals, both of which arise in emergency situations, such as leak accidents in chemical plants, roll-over accidents of tankers transporting the chemicals, in the water supply network, as well as the disinfection by-products, which only arise in small quantities during the water purification process monitor, but only manual measurement can take place, which is why it is difficult to combat such contaminants by rapid detection. In order to solve these problems, efforts have so far been made to monitor the water quality in real time. For example, various technologies for real-time monitoring of water quality have been proposed by the following South Korean registration patents: Registration Patent no. KR 10-0 901 779 (2.6.2009) with the title “Internet-based monitoring and control system for measuring water quality”, registration patent no. KR 10-0 522 764 (12.10.2005) with the designation "Device for real-time monitoring of water quality and method for controlling the same", registration patent no. KR 10-1 406 884 (5.6.2014) with the title "Multi-wavelength analysis-based online system for measuring water quality for the real-time detection of organic contaminants in water", and registration patent no. KR 10-1 253 251 (4.4.2013) with the designation "Device and method for real-time monitoring and control of substances that cause taste and smell for the purpose of water purification". But most of the above prior art patents relate to the measurement of the basic parameters of water quality (e.g. water temperature, pH, turbidity, electrical conductivity of a residual chlorine, etc.) or of the total index parameters of organic materials (e.g. total organic carbon (TOC), chemical oxygen demand (COD), etc.), some of which relate to the method for real-time measurement of certain organic contaminants. In these patents, however, methods are used which are different from existing analysis devices or by combining the different expensive equipment with one another, which consequently leads to the disadvantage that accuracy, reliability and economy are reduced and operation and administration are made more difficult. CH 711 779 B1 As mentioned above, the organic pollutants in the water, e.g. tasting and malodorous substances etc., furthermore are analyzed even more frequently. However, the registration patents describe the combination of the separate expensive equipment with one another, which is why this is uneconomical and can only be operated and managed in a complicated manner. As a widespread device for analyzing an organic pollutant in water, an analysis device consisting of a solid-phase microextraction device and a gas chromatography mass spectrometry analysis device is currently used extensively, but the degree of utilization of this analysis device is too low and so new devices have to be rebuilt, which is consequently inconvenient Leads to problems. DISCLOSURE OF THE INVENTION Object of the Invention The object of the present invention is to solve the problems and / or disadvantages summarized above and found in the known technologies. With the present patent application, an arrangement for the automatic real-time analysis of an organic pollutant in water is described, by means of which a practical analysis system is developed by automating all measurement processes of the respective sizes of the organic pollutant in the water using an analysis device that has been widely used for manual analysis which enables measurement results to be used to manage water quality quickly in real time, certain organic pollutants, such as tasting and malodorous substances, volatile organic compounds, agrochemicals and disinfection by-products etc., to be analyzed in real time, measuring these contaminants in a controllable degree of concentration (several ng / L levels in the case of the tasting and malodorous substances) as well as reliable measured values, economical maintenance and easy to assemble and operate. SOLUTION OF THE OBJECT OF THE INVENTION In order to solve the problems summarized above and identified in the known technologies, the present application relates to a method according to claim 1. [0012] Furthermore, an arrangement according to the present application additionally has the following features, which are specially designed such that they can be suitably attached to an analysis device previously used: a sample bottle; a heating block that can perform temperature control and stirring; a sample supply and discharge unit; a water drainage pipe; a sample supply amount control line; and a flow path changing means that can change the flow of the sample depending on a program; and can thus be driven in one piece in the existing analyzer so that the organic contaminants, e.g. tasting and malodorous substances in the water, can be constantly analyzed in real time and thus a time of production of a highly concentrated, organic contaminant can be quickly recognized and a suitable countermeasure can be taken. Effect of the invention It can further be provided by means of the arrangement according to the application for the automatic real-time analysis of an organic contaminant in water that a desired degree of measurement sensitivity with regard to the organic contaminants can be obtained from the capacity of the sample bottle and by means of a heating and stirring means of the heating block can, without using other expensive and complicated equipment and chemicals, the arrangement according to the invention can also be easily installed in the existing analysis device and can achieve simple operation and maintenance and high efficiency and practicality. In addition, it can advantageously be provided by means of the arrangement according to the application for the automatic real-time analysis of an organic contaminant in the water that several sample bottles are provided on the heating block, so that the water quality can be checked in different positions as an object to be analyzed. BRIEF DESCRIPTION OF THE DRAWINGS It shows: 1 is a flowchart to illustrate a method for analysis according to the present invention, 2 is a side view of a real time solid phase micro extraction GC or solid phase micro extraction GC / MS analysis system according to the present application, 3 is a perspective view of a connection relationship between a heating block and a sample bottle of the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system according to the present application, CH 711 779 B1 Fig. 4 is a sectional view through section A-A in Fig. 3; Fig. 5 is a sectional view through section B-B in Fig. 3; 6 shows a state in which a sample is provided for the sample bottle in real-time solid-phase microextraction GC or solid-phase microextraction GC / MS analysis system; 7 shows another state in which the sample is taken (concentrated / extracted) from the real-time solid phase microextraction GC or solid phase microextraction GC / MS analysis system according to the present application; and 8 shows a further state in which the sample is removed from the sample bottle in real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system according to the present application. PREFERRED EMBODIMENTS OF THE INVENTION As can be seen in FIG. 1, it is provided according to the invention that the method for the automatic real-time analysis system of an organic pollutant using a real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system comprises the following method steps: a step to continuous, timely provision of a sample for holding a sample bottle via a sample feed line 42 formed in real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system 100; and a step of analyzing the sample by taking and analyzing the sample through an analyzer 10 which is provided from a solid phase micro extraction device 11 for extracting a small quantity of a sample of the real time solid phase micro extraction GC or solid phase micro extraction GC / MS analysis system 100 is used, and a gas chromatography mass spectrometry analysis device 12, which is designed to receive the sample extracted by the solid-phase microextraction device 11 and to analyze the sample containing organic contaminants qualitatively and quantitatively. Therefore, it can be provided by means of the analysis method according to the invention for carrying out a sample analysis through the above-mentioned method steps that the analysis of the water quality to be analyzed is made possible by the continuous circulation of the sample without congestion and thus by providing it in real time, of course at the same time, a point in time at which an event of the water quality itself arises can be quickly identified by means of the constant analysis and thus a countermeasure can be taken, and also by means of the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system 100 used in the analysis the separate equipment can be easily mounted on the previously used analyzer, so that the existing equipment can be used unchanged, which can therefore improve efficiency. The present invention is explained in more detail below. Furthermore, it can be provided according to the invention that the analyzer 10, which consists of a solid-phase micro-extraction device 11 for extracting a small quantity of a sample of the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system 100 and one used in the present invention Gas chromatography mass spectrometry analysis device 12, which is designed to receive the sample extracted by the solid-phase microextraction device 11 and to analyze this sample containing organic contaminants qualitatively and quantitatively, is designed in such a way that further equipment on the analysis device 10 from the above Solid phase micro extraction device 11 for extracting the small quantity of the sample of the existing, ie above-mentioned analysis system 100 and the above gas chromatography mass spectrometry analyzer 12 are additionally mounted so that the sample can be provided continuously in real time. A structure of the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system 100 of this kind is explained in more detail below. First of all, as can be seen in FIG. 2, an analysis device 10 has a solid-phase micro-extraction device 11, which is used to extract a small quantity of a sample, and a gas chromatography mass spectrometry analysis device 12, which receives the sample extracted by the solid-phase micro-extraction device 11 and this sample containing the organic pollutants is analyzed qualitatively and quantitatively. Even if the solid-phase microextraction device 11 is not shown in detail in the figure, it is designed in such a way that a fiber that can absorb the sample is inserted into or from a needle of a syringe for the removal (concentration / extraction) of a sample or can be removed so that the sample to be analyzed can be removed by means of the syringe needle, then this syringe needle inserted into a sample introduction part (not shown in the figure) formed in the gas chromatography-mass spectrometry analysis device 12 and finally the sample can be analyzed qualitatively and quantitatively. CH 711 779 B1 In particular, gas chromatography of the above gas chromatography-mass spectrometry analysis device 12 is known for separating the substances mixed in the sample from the sample itself, and if a mass spectrometer is used as a detector in addition to gas chromatography, then such a generic type It is provided that a molecular mass of the separated substances can be precisely recognized to five decimal places and thus the mixed substances contained in the sample can be separated from one another and analyzed qualitatively and quantitatively. In order to analyze the sample in this way, it is provided in this advantageous embodiment that the solid-phase microextraction device 11 is usually attached to an upper side of the gas chromatography mass spectrometry analysis device 12. In addition, in this advantageous embodiment, as can be seen in FIGS. 2 to 5, it is provided that a heating block 20 between the solid-phase microextraction device 11 and the gas chromatography-mass spectrometry analysis device 12 of the above analysis device 10, in particular on the top of the gas chromatography -Mass spectrometry analysis device 12 is arranged, wherein a plurality of sample bottle seat recesses 21 are formed on an inside of the heating block and wherein the heating block itself is provided in its entirety with a heating means 22 and temperature sensor 23 for heating. It can be provided in this embodiment that the plurality of sample bottle seat recesses 21 are arranged at a certain distance from one another and that a magnetic or oscillating stirring means 24 is additionally enclosed within the heating block 20. In addition, in this embodiment, as can be seen in FIGS. 2 to 5, it is provided that a sample bottle 30 can rest against the sample bottle seat recesses 21 formed in the above heating block 20, with a receptacle 31 for receiving on an inside of the sample bottle a sample to be used for checking the water quality is designed so that the sample received by the receptacle 31 is absorbed by the solid-phase microextraction device 11 of the above-mentioned analysis device 10. It is advantageously provided that the receptacle 31 of the above sample bottle 30 is so large in capacity that it can accommodate a quantity between 100 and 150 ml, but this is not particularly limited. Of course, a plug (not shown in the figure) is formed on an upper side of the sample bottle 30, which plug can close the sample bottle and through which the needle of the syringe can pass. In the sample bottle 30 are also a sample feed 32, which serves to feed the sample 31 to the sample, and a sample discharge 33, which serves to remove the sample received in the receptacle 31 after the sample for analysis from the Analyzer 10 was removed (concentrated / extracted). It is advantageously provided that the sample feed 32 is formed at the upper end of a side surface of the sample bottle 30, but this is not particularly limited, wherein it is also advantageously provided that the sample discharge 33 for easy removal of the sample at the bottom End of the side surface of the sample bottle 30 is formed. In addition, in this advantageous embodiment, it is provided that a sample supply and removal unit 40 is connected to the sample bottle 30 and thus can supply and remove the sample. It is provided, as can be seen in FIG. 3, that a sample feed line 42 is constructed in the sample feed and removal unit 40, which is connected to the sample feed 32 of the sample bottle 30, with a sample feed line 42 in this sample feed line 42. Control valve 42a is constructed, by means of which the sample can be supplied or blocked. That is, it is designed such that one end of the sample supply line 42 is connected to the sample bottle 30, while another end thereof is connected to a line of a medium that an analyst wishes to analyze, i.e. of an object that the analyst wants to check for its water quality, e.g. Raw water (from water, lake, etc.), processed water in the water treatment system, treated water, etc. is connected, so that the sample can be provided in real time to the receptacle 31 formed in the sample bottle 30. In this case, in a section which is connected to a position of the sample supply line 42 in which the analyst wants to check the water quality, a pump 42b can additionally be arranged, which can convey the fluid (the sample). In addition, a washing line (not shown in the figure) is additionally arranged at the end of the sample supply line, which can supply a washing water for washing the interior of the sample bottle 30, or the end is connected to a section to which the washing water is supplied, so that this washing water can be fed to the sample bottle. In contrast, it is designed such that a water discharge line 50 is connected to the above sample supply line 42, so that new sample can always be provided to the sample supply line. Here, the water discharge line 50 is formed such that it branches off from the sample supply line 42, i.e. that it is between a position in which the water quality should be checked and that in the CH 711 779 B1 Sample supply line 42 arranged sample supply control valve 42a is arranged, but it is even more advantageous that it is arranged directly upstream of the sample supply control valve 42a. In contrast, it is provided in this advantageous embodiment of the invention that a component is provided to enable the quantitative analysis, which can be filled with a certain amount of the sample bottle 30 to be supplied to the sample. For this purpose, the sample bottle 30 has a sample supply amount control unit 34, which is designed to be able to receive the specific amount of sample by means of the receptacle 31, the sample supply amount control unit 34 being arranged on a side surface of the sample bottle 30. However, it is advantageously provided that the sample supply quantity control unit is arranged at an exact height at which the receptacle 31 can be completely filled with the sample, so that only the specific quantity of sample can be accommodated in the receptacle 31. Furthermore, it can additionally be provided that a sample supply quantity control line 60 has a sample supply quantity control valve 61, which connects the sample supply quantity control line with the sample supply quantity control unit 34 formed in the sample bottle 30. It can advantageously be provided that the above-mentioned valves are designed to be electronically controlled, similar to an electromagnetic valve, so that they can be opened or closed by the control of a control unit C. The analysis method according to the invention is described in more detail below, which can be carried out by means of the real-time solid-phase microextraction GC or solid-phase microextraction GC / MS analysis system 100, which has the structure mentioned above. 1. Step for providing a sample First, the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system 100 is the one that can analyze the organic pollutants in the water automatically in real time using the analysis device 10 that has been used previously , and must be set up in locations or laboratories etc. within the corresponding water quality test zones in order to use the test water, e.g. treated water, raw water and processed water, which are processed in a water treatment plant, e.g. Water treatment plant, arises to check its water quality. Thereafter, the test water is provided in real time via the sample supply line 42, which is formed in the sample supply and removal unit 40 and is connected to the sample supply 32 of the sample bottle 30. The supply process by means of which the test water is supplied to the sample bottle 30 via the sample supply line 42 takes place in such a way that the conventional control unit C opens the sample supply control valve 42a arranged in the sample supply line 42 so that the test water can be made available to the sample bottle, 5, while a sample discharge control valve 43a of a sample discharge line 43 which is arranged in the sample supply and discharge unit 40 connected to the sample discharge 33 of the sample bottle 30, and a water discharge control valve 51 of a water discharge line connected to the sample supply line 42 50 are controlled in a closed state, so that the receptacle 31 of the sample bottle 30 is filled with the sample as the test water. It is possible that the sample provided via the sample feed line 42 is provided by means of a conventional pump 42a or is moved by a water pressure arising from the purified water or raw water. In this way, does the amount of sample filled in the sample bottle 30 reach a certain quantity, i.e. a position on which the sample supply quantity control unit 34 of the sample bottle 30 is formed, then the excessive sample supply quantity control line 60 provided via the sample supply quantity control unit 34 is discharged to the outside, so that only the specific quantity of sample in the receptacle 31 is filled. 2. Step for analyzing a sample If the determined quantity of sample is filled in the above-mentioned manner, the sample supply control valve 42a arranged in the sample supply line 42 and the sample supply quantity control valve 61 arranged in the sample supply quantity control line 60 are controlled by the control unit C closed and thus the receptacle 31 inside the sample bottle 30 is separated from the outside, as can be seen in FIG. 7, so that a sampling (concentration extraction) can be carried out by the analysis device 10 and an analysis work can be carried out, while the sample which is continuously provided via the sample feed line 42 can be carried out by the Opening the water discharge control valve 51 of the water discharge line 50 can be discharged via this water discharge line 50. An effect can be achieved by means of the water discharge line 50 that the sample existing in the sample supply line 42 can only be left over by the quantity to be provided in real time. CH 711 779 B1 [0050] That is, the object of the invention was to identify, by analyzing the sample supplied in real time, the point in time at which the organic contaminants are superfluous within the sample, as explained above. Therefore, the above water discharge pipe 50 has been introduced, whereby it acts in such a way that the sample existing in the sample supply pipe 42 is maintained only by the quantity to be provided in real time and thus can be analyzed in real time. Thereafter, a needle of the solid phase micro extraction device 11 for concentrating / extracting the sample is positioned in a head space within the sample bottle 30. In contrast, the heating block 20 receiving the above sample bottle 30 is heated to the temperature suitable for the analysis (regulated according to the analysis size) and, if necessary, the stirring means 24 is operated so that the organic contaminants removed from the receptacle 31 of the sample bottle 30 Can move sample well into the head space within the sample bottle 30. Thereafter, the solid phase microextraction device 11 of the analysis device 10 is operated and thus absorbs the sample of the sample bottle 30, so that this sample is then inserted into the gas chromatography mass spectrometry analysis device 12 and thus the analysis work of the same is carried out. During the process in which the work is performed by the analyzer 10, the constant supply of the sample to the sample bottle 30 is of course carried out by means of the components as mentioned above. If the analysis work is completed by the analysis device 10, then the sample received in the other sample bottle 30 can then be analyzed in succession. In contrast, the sample of the sample bottle 30, from which the analyzer 10 has taken the sample to be analyzed, by opening the sample discharge control valve 43a of the sample discharge line 43, which is connected to the sample discharge 33 formed in the sample bottle 30, and the The sample supply quantity control valve 61 of the sample supply quantity control line 60 is discharged to the outside, as can be seen in FIG. 8, the new sample then being made available again via the sample supply line 42, and the sample remaining in the receptacle 31 of the sample bottle 30 is thus discharged via the sample discharge line 43 , so that thereafter, in a state in which the sample discharge control valve 43a is closed, the sample supply amount control valve 61 of the sample supply amount control line 60 is closed. In this way, the procedures for taking up and analyzing the sample can therefore be carried out repeatedly. Since the sample provided via the sample supply line 42 of the sample supply and removal unit 40 represents the one that is provided in real time, the real-time sampling and the sample analysis are carried out by the analysis device 10 in succession, so that an increase in the concentration of the organic pollutants occurs quickly recognized and constant analysis can be made possible. In contrast, a plurality of sample bottles 30 can be formed on the heating block 20. Only the sample can be taken from any position, however, the one sample supply and removal unit 40 connected to any sample bottle 30 is arranged in the processed water, while the other sample supply and removal unit 40 connected to the other sample bottle 30 is arranged in the raw water is arranged, etc., so that the sample analysis can be carried out simultaneously by the analyzer in different positions. In addition, it is designed according to the invention in such a way that the above sample bottle 30 is designed in terms of its capacity in a size between approximately 100 and 150 ml, so that a sufficient amount of organic contaminants can be included therein, the temperature being maintained by the heating means 22 and the temperature sensor 23 of the heating block 20 and the extraction (concentration / extraction) of the sample can be carried out effectively by the stirring means 24, which consequently also leads to an advantage that a sufficient degree of analysis sensitivity during the analysis of the sample by the analysis device 10 without operation Inserting the separate reaction chemicals can be obtained. In particular, if the analysis of the sample represents a process for automatic real-time analysis of the tasting and malodorous substances of the sample, then the arrangement according to the invention has the advantage that, in addition to the chemical analysis by the analysis device 10, a sensory analysis work can also be carried out in parallel which the human being actually smells at the sample and thus analyzes. As mentioned above, it can be provided that the existing equipment is used unchanged by installing the separate equipment in the analyzer, the sample being continuously provided in real time and thus a point in time at which an event occurs is quickly recognized, so that a quick countermeasure can be taken, and at the same time the present invention can easily be applied to the existing analyzer 10, so that it is not necessary to introduce new equipment, which consequently can lead to an economically very useful effect. It should be noted that the above-mentioned embodiments describe only one advantageous embodiment, the present invention can be changed and carried out in various forms. CH 711 779 B1
权利要求:
Claims (3) [1] LIST OF REFERENCE NUMBERS [0062] C: control unit 10: analyzer 11: Solid phase micro extraction means 12: Gas chromatography mass spectrometry analyzer 20: heating block 21: Sampler-seat recess 22: Heating means 23: temperature sensor 24: Rührungsmittel 30: Sampler 31: admission 32: sample feed 33: sample withdrawal 34: Sample feed rate control unit 40: Sample supply and removal unit 42: Sample supply line 42a: Sample supply control valve 42b: pump 43: Sample withdrawal line 43a: Samples discharge control valve 50: Water discharge line 51: Drainage control valve 60: Sample feed rate control line 61: Sample feed rate control valve 100: Real-time solid phase micro extraction GC or solid phase micro extraction GC / MS analysis system claims 1. A method for automatic real-time analysis of an organic contaminant using a real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system, the method comprising the following method steps: a step of continuously, timely providing a sample for inclusion in a sample bottle via a sample delivery line (42) formed in real time solid phase micro extraction GC or solid phase micro extraction GC / MS analysis system (100); and a step for analyzing a sample, in that the sample is taken and analyzed via an analysis device (10) which consists of a solid-phase microextraction device (11) which is used for extracting a certain quantity of a sample of the real-time solid-phase microextraction GC or solid-phase microextraction GC / MSAnalysesystems (100), and a gas chromatography-mass spectrometry analysis device (12), which is designed to receive the sample extracted by the solid-phase micro-extraction device (11) and to analyze the organic contaminant sample qualitatively and quantitatively, CH 711 779 B1 characterized in that the real-time solid-phase micro-extraction GC or solid-phase micro-extraction GC / MS analysis system comprises the following features for the constant implementation of the step for analyzing a sample just after the continuous, real-time implementation of the step for providing a sample: an analysis device (10), which consists of a solid-phase micro-extraction device (11) for extracting a certain quantity of a sample, and a gas chromatography mass spectrometry analysis device (12) which is designed to obtain the sample extracted by the solid-phase micro-extraction device (11) and this the organic There is a qualitative and quantitative analysis of the sample containing contaminants; a heating block (20) which is arranged on an underside of the solid-phase microextraction device (11) which forms the analysis device (10) and which has a plurality of sample bottle seat recesses (21) as well as a heating means (22) and a temperature sensor (23) on the inside thereof; at least one sample bottle (30), each of which rests on the sample bottle seat recesses (21) of the heating block (20), and a receptacle (31) for receiving a sample which is formed on the inside thereof, a sample feeder (32) for this serves to feed the sample to be analyzed in real time to the receptacle (31) and has a sample removal (33) which serves to remove the sample from the receptacle (31); a sample supply and removal unit (40) which comprises a sample supply line (42) which is connected to the sample supply (32) of the sample bottle (30) and a sample supply control valve (42a) for supplying the sample, and a sample discharge line ( 43), which is connected to the sample discharge (33), which is designed to discharge the sample of the receptacle (31) formed in the sample bottle (30), and has a sample discharge control valve (43) for removing the sample ; a water discharge line (50) which is connected to the sample supply line (42) formed in the sample supply and discharge unit (40) and has a water discharge control valve (51) for real-time provision of the sample to the sample bottle (30); and a control unit C for controlling the above control valves. [2] 2. The method according to claim 1, characterized in that a stirring means (24) is additionally enclosed within the heating block (20), which serves to stir the sample within the receptacle (31) of the sample bottle (30) resting on the sample bottle seat recess (21) , [3] 3. The method according to claim 1, characterized in that one end of the sample supply line (42) of the sample supply and removal unit (40), which is connected to the sample supply (32) of the sample bottle (30), on a water treatment system to be analyzed or on Examination water including raw water and processed water is connected, a pump (42b) being additionally provided to provide the sample to the sample bottle (30).
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公开号 | 公开日 WO2016052913A1|2016-04-07| US20170205382A1|2017-07-20| KR101507019B1|2015-03-31|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 KR0166195B1|1995-10-09|1999-05-01|송원오|Apparatus for examing water automatically using cylinder type syringe unit| DE19933017A1|1999-03-26|2001-01-18|Gerstel Systemtechnik Gmbh|Solid phase micro-extrusion and analysis procedures| JP2003315219A|2002-04-22|2003-11-06|Asahi Kasei Corp|Apparatus for screening diffusion speed of volatile substances| KR100997526B1|2008-03-11|2010-12-03|정병길|A automatic control system implementing measuring water quality for sewage treatment plants| KR100964219B1|2009-10-01|2010-06-17|주식회사 제일그린시스|automatic cleaning device of automatic measure for the quality of water for Monitoring Water Pollution|
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申请号 | 申请日 | 专利标题 KR1020140131482A|KR101507019B1|2014-09-30|2014-09-30|Real-time Automatic Analyzing method for Organic Pollutants of Fluid by using of Solid-Phase MicroExtraction-Gas Chromatograph(Gas Chromatograph/Mass Spectrometer Analyzing System| PCT/KR2015/010023|WO2016052913A1|2014-09-30|2015-09-23|Real-time automatic analysis method, for organic contaminant, using real-time spme-gc or spme-gc/ms analysis system| 相关专利
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