KR20040059205A - Apparatus for automatic preprocessing volatile organic compound - Google Patents

Abstract

PURPOSE: A volatile organic compound automatic pretreatment apparatus is provided, to allow the volatile organic compounds of waste matters to be inputted, extracted and analyzed automatically in a short time and precisely without variation of analyzed result. CONSTITUTION: The automatic pretreatment apparatus comprises a sample container(110) loading and sealing waste sample; a holder part loading the sample container; an extraction part(140) inputted into the sample container to extract volatile organic compounds; a weighing part inputting a solvent in the sample container; an automatic stirring part stirring the sample inside the sample container together with the solvent; a solvent storing tank(200) storing a solvent; a transfer valve part(180) transferring the volatile organic compounds extracted into gas state in the sample container to an analysis device; a transfer part(190) connecting the transfer valve part with the analysis device; a channel washing valve(101) washing a weight part and a solvent input channel from a carrying gas storing tank(300); a carrying gas supply valve(102) supplying a carrying gas to the extraction part(140); a solvent supply valve(103) supplying a solvent through the weighing part from a solvent storing tank(200); a solvent input valve(104) inputting a solvent from the weighing part to the extraction part; a control part(210) controlling the operation of motors of each unit, temperature and the valves; and a computer connected with the control part for controlling the each unit and outputting the result.

Description

Apparatus for automatic preprocessing volatile organic compound

The present invention relates to an automatic pretreatment apparatus for the analysis of volatile organic compounds in the waste generated in each process of the steel mill, and more particularly, to quickly and accurately analyze volatile organic compounds, which are environmental pollutants in the waste generated in each process of the steel mill. It relates to a volatile organic compound automatic pretreatment device for.

In general, steel mills have several steps to produce steel products from raw material processing to rolling processes. In this process, wastewater generated by each process is purified to be discharged through the steel plant's own purification facilities. The purification of wastewater has a process of decomposition using microbial propagation, in which contaminants in wastewater, such as lead, mercury, cadmium (hereinafter referred to as "heavy metals"), etc., are benzene, toluene, xylene, Trichloroethylene, tetrachloroethylene (hereinafter referred to as "volatile organic compound") and the like precipitate with the microorganism and solidify. The steel mill analyzes the composition and content of the contaminants in the solidified wastewater and wastewater, and predicts the extent to which the contaminants contained in the waste are eluted after landfill disposal in advance. It is utilized to

Figure 2 is a perspective view showing the configuration of a volatile organic compound analysis device according to the prior art

FIG. 1 is a schematic view showing a dissolution test method for analyzing volatile organic compounds according to the prior art. As shown in FIG. 1, as a pretreatment method for analyzing volatile organic compounds according to the related art, wastes determined by the government in accordance with the Waste Management Act Enforcement Decree The dissolution test method is used to pretreat the waste samples collected in each process. Waste dissolution test is a test method that predicts in advance how much environmental pollutants contained in workplace wastes will be eluted after landfill disposal. Samples are collected, weighed, separated from sample, solvent production, solvent addition, container sealing, shaking It is a test method that is used as judgment data to determine the designated waste or landfill method for nine wastes among designated wastes.

Normally, the waste dissolution test method prescribed in the Enforcement Decree of the Waste Management Act is as follows.

First, accurately measure the weight of the solid or semi-solid sample taken from each process to at least 50g.

Secondly, hydrochloric acid is added to distilled water to prepare a solvent solution so that the acidity is 5.8-6.3Ph.

Third, the solvent solution and the sample are mixed in a sealed container so as to be 10 times as large as the sample, and mounted in a horizontal reciprocating stirrer.

Fourth, the number of stirring is 200 times per minute, the amplitude is 4 ~ 5cm and stirred for 6 hours.

Fifth, the resultant was filtered through a glass fiber filter paper of 100 [㎛], and the filtrate was used as a dissolution test sample.

Sixth, if filtration is difficult, centrifugation is performed, and the supernatant is taken as a sample for dissolution test.

The analysis of the sample extracted through this process is divided into volatile and non-volatile, and the non-volatile is analyzed the composition and content of heavy metals in the sample using an ion plasma analyzer or an atomic absorption analyzer, the volatility is the application number 10- The composition and content of volatile organic compounds in the sample were analyzed using the thermal desorption sample injection device and gas chromatography ion trap analyzer of volatile organic compounds specified in 1999-0020001 and Application No. 10-2001-80036.

In the conventional method of pretreatment by waste dissolution test, as shown in FIG. 2, since the volatile organic compounds in the sample are extracted in the aqueous state by the syringe 50 or the like, the gas chromatography ion trap analysis apparatus 20 is analyzed. In order to use the thermal desorption separation tube 12 of the thermal desorption sample injection device 10, the process of separating the extract 60 in an aqueous state into a gaseous state.

This separation process includes a sample collector 13 for collecting the extracted sample, a heat desorption separator tube 12 for supplying a transport gas from the transport gas reservoir 40 to the collected sample, and rapidly desorption of the sample by heat. And a sample dryer 15 for drying the sample heat-desorbed from the thermal desorption separation tube, and the gaseous sample is separated through the sample inlet 21 of the gas chromatography ion trap analysis apparatus 20. Is injected into the analysis.

However, the pretreatment method for the analysis of the conventional volatile organic compounds as described above has the following problems.

First, agitation, which takes the most time among pretreatment methods by waste dissolution test of waste samples collected in each steel mill process, is for the extraction of heavy metals in the sample. Analysis of the composition and content of has a problem that is delayed for more than 6 hours, which is a treatment time for the extraction of heavy metals. Therefore, during the pretreatment process, the volatile organic compound, that is, the composition, already extracted from the waste sample is lost, resulting in a deviation of the analysis result obtained by analyzing the same.

Second, in the conventional waste dissolution test, all the processes are performed by the operator's manual work, and thus, deviations occur during the preparation and addition of the solvent solution, and the filtration and supernatant extraction process of the finished sample is extracted. Even when the supernatant sample is injected into the thermal desorption sample injection device 10 for gas chromatography analysis, personal deviation occurs, and all such manual deviation causes the deviation of the final analysis result.

Third, since the volatile organic compounds in the sample are extracted in an aqueous solution state in the conventional waste dissolution test, the thermal desorption separation of the thermal desorption sample injection device 10 for analysis by using the gas chromatography ion trap analysis device 20 Using the tube 12, the extract 60 in aqueous solution should be subjected to a process of separating it into a gaseous state. However, since the thermal desorption separation tube 12 is washed by the transport gas supplied from the transportation gas reservoir 40, the volatile organic compounds extracted in the separation process are fixed to the inner wall of the thermal desorption separation tube 12 and lost or previously thermal desorption. Since the composition and content of the volatile organic compounds extracted by the contaminants stuck to the inner wall of the separator 12 are different, there is a problem of deteriorating the accuracy and reliability of the analysis results.

Therefore, the present invention has been made to solve the above problems, the present invention is a method of pretreatment of contaminants in the waste of each steel mill, the pre-treatment and extraction process of volatile organic compounds faster and more accurate By eliminating the deviation and eliminating the injection process of the thermal desorption sample injector, it automatically performs the pretreatment and extraction process of the waste sample and the injection of the analysis device, thereby fundamentally eliminating the causes of personal deviation and process variation by worker. The present invention provides an automatic pretreatment apparatus for volatile organic compounds.

Figure 1 is a working overview showing the dissolution test method for the analysis of volatile organic compounds according to the prior art

Figure 2 is a perspective view showing the configuration of a volatile organic compound analysis device according to the prior art

Figure 3 is a perspective view showing the overall configuration of the automatic volatile organic compound pretreatment apparatus according to an embodiment of the present invention

Figure 4 is a perspective view showing a connection state of the automatic volatile organic compound pretreatment apparatus according to an embodiment of the present invention and the conventional gas chromatography ion trap analysis device

5 is a connection block diagram of the automatic volatile organic compound pretreatment apparatus according to the present invention

Figure 6a and Figure 6b is a longitudinal cross-sectional view showing the configuration of the sample container according to the present invention

7a and 7b is a perspective view and a cross-sectional view showing the structure of the extraction unit according to the present invention

7c and 7d are sectional views showing the flow path of the extraction unit according to the present invention.

8A and 8B are cross-sectional views showing the flow path of the metering valve according to the present invention.

Figure 9 is an exploded perspective view showing the configuration of the holder portion and the automatic stirring portion according to the present invention

10 is an exploded perspective view showing the structure of the metering unit according to the present invention;

Figure 11a is a perspective view showing the structure of the transfer valve unit according to the present invention

11B and 11C are cross-sectional views showing a flow path of a transfer valve according to the present invention.

12 is a cross-sectional view showing the structure of the transfer unit according to the present invention;

<Description of the symbols for the main parts of the drawings>

100: automatic pretreatment device 101: flow path cleaning valve 102: transport gas supply valve

103: solvent supply valve 104: solvent injection valve 105: flow path distributor

106: upper fixing plate 107: lower fixing plate 108: sample

110: sample container 120: holder portion 121: holder motor

122: motor holder 123: holder cup 124: drain

125: gear coupling 126: holder coupling 127: gear bar

128: gear bar fixing ring 129: gear bar bearing 130: gear bar holder

140: extraction unit 141: injector 142: extraction valve

143: transport gas inlet 144: transport gas outlet 145: extraction unit fixture

146: heater 147: temperature detector 150: metering unit

151: piston motor 152: motor holder 153: gear couple

154: gear bar 155: piston coupling 156: metering valve

157: graduated syringe 158: metering unit holder 159: piston

160: gear bar fixing ring 161: gear bar bearing 162: gear bar fixing

163: piston fixing pin 170: automatic stirring portion 171: rotating magnet

172: stirring motor 173: motor holder 174: support

175: stirring magnet 180: transfer valve portion 181: transfer valve

182,193: heater 183: temperature detector 184: thermal cover

190: transfer unit 191: transfer unit connection nut 192: transfer unit fixing feet

194: temperature detector 195: thermostat 196: flow path

197: inlet connecting nut 198: inlet fixing feet 200: solvent reservoir

201: water level monitoring window 210: control unit 300: transport gas storage

400: analysis device 410: gas chromatography

411: Sample inlet 412: Separator 413: Heater

420: connector 421: ion trap analyzer 500: computer

In order to achieve the above object, the present invention provides an automatic pretreatment apparatus for a volatile organic compound, comprising: a sample container capable of loading and sealing a waste sample; A holder portion for loading a sample container; An extraction unit which is introduced into the sample container and extracts volatile organic compounds; A metering unit for injecting a solvent into the sample container; An automatic stirring unit for stirring the sample in the sample container together with the solvent; A solvent reservoir for storing the solvent; A transfer valve unit for transferring the volatile organic compound extracted in the gas state in the sample container to the analysis device; A transfer unit connecting the transfer valve unit and the analyzer; A flow path cleaning valve for cleaning the metering unit and the solvent injection path from the transport gas reservoir; A transport gas supply valve for supplying a transport gas to the extraction unit; A solvent supply valve for supplying a solvent from the solvent reservoir through a metering unit; A solvent injection valve for injecting a solvent from the metering unit into the extraction unit; A control unit for controlling motor driving and temperature control of each element and control of the valve; The present invention provides an automatic pretreatment apparatus for volatile organic compounds, which is connected to a control unit of an automatic pretreatment apparatus, controls each element and is configured by a computer that is responsible for outputting the analysis results from the analysis apparatus.

The objects, features and advantages of the present invention will be more readily understood by reference to the accompanying drawings and the following detailed description.

Hereinafter, the configuration and operation of the present invention with reference to the accompanying drawings in detail as follows.

3 is a perspective view showing the overall configuration of the automatic volatile organic compound pretreatment apparatus according to an embodiment of the present invention, the automatic pretreatment apparatus 100 of the present invention is a sample container 110 that can be sealed by weighing a sample, A holder unit 120 for loading a sample container, an extraction unit 140 that is introduced into the sample container to extract volatile organic compounds, a metering unit 150 for injecting a solvent into the sample container, and a sample in the sample container. The automatic stirring unit 170 for stirring the solvent together with the solvent, the solvent reservoir 200 storing the solvent, and changing the flow path to send the volatile organic compound extracted in the gas state in the sample container to the analyzer, and In order to prevent adsorption of the volatile organic compounds extracted in the container, the transfer valve unit 180 having a heater is connected to maintain the high temperature, and the transfer valve unit and the analyzer are connected to each other. Transport unit 190 which is automatically injected into the analysis device to perform the analysis, flow path cleaning valve 101 for cleaning the metering unit and the solvent injection flow path from the transport gas reservoir, transport for supplying the transport gas to the extraction unit A gas supply valve 102, a solvent supply valve 103 for supplying a solvent from the solvent reservoir through the metering section, a solvent injection valve 104 for injecting solvent from the metering section into the extraction section, and a motor drive of each element And a controller 210 in charge of temperature control and valve control.

Figure 4 is a perspective view showing a connection state of the automatic volatile organic compound automatic pretreatment apparatus according to an embodiment of the present invention and the conventional gas chromatography ion trap analysis device, Figure 5 is a connection block of the automatic volatile organic compound pretreatment apparatus according to the present invention As a figure, it will be described in detail with reference to the following description of the operation of the present invention.

6A and 6B are longitudinal cross-sectional views showing the configuration of the sample container according to the present invention, wherein the sample container 110 of FIG. 3 is closed with a bottle 111 made of glass, as shown in FIG. 6. Consists of, the stopper is composed of a rubber film inner mold 113, which is possible to insert the outer portion 112 and the extraction portion of the plastic material and easy to seal.

7a and 7b are a perspective view and a cross-sectional view showing the structure of the extraction unit according to the present invention, Figure 7c and 7d is a cross-sectional view showing a flow path of the extraction unit according to the present invention, the extraction unit 140 of FIG. As shown in FIG. 1, an injector 141 for injecting a solvent into the sample container 110 and an extraction valve 142 which is responsible for opening and closing of the flow path of the solvent and the transport gas, as shown in FIGS. 7C and 7D. ), A transport gas inlet 143 located on left and right sides of the injector, a transport gas outlet 144, and an extraction unit fixing unit 145, and as shown in FIG. 7B, a heater embedded to enable heating of the extraction unit. 146 and a temperature detector 147 for detecting the temperature of the extraction section.

8A and 8B are cross-sectional views showing the flow path of the metering valve according to the present invention, and FIG. 10 is an exploded perspective view showing the structure of the metering unit according to the present invention. The metering unit 150 of FIG. 3 is shown in FIG. As described above, the graduated syringe 157 capable of measuring the amount of the solvent to be injected into the sample container, the piston 159 for injecting or discharging the solvent into the graduated syringe, and the piston of the graduated syringe are moved up and down. Piston motor 151 to be fixed, the fixed base 152 for fixing the piston motor, the piston motor gear bar 154 connected to the piston motor to convert the rotational movement to vertical movement, and the gear couple connecting the piston motor and the gear bar Ring 153, a piston coupling 155 for coupling the piston motor gear bar to move the piston up and down, and a metering valve for opening and closing the flow path of the metering unit as shown in Figs. 156) and the metering section A fixed stand 158, a fixed stand 162 for fixing the gear bar, a bearing 161 for the rotation of the gear bar, and a fixing ring 160 for fixing the bearing and the fixed stand.

9 is an exploded perspective view showing the configuration of the holder portion and the automatic stirring portion according to the present invention, wherein the holder portion 120 of FIG. 3 is a holder cup 123 for loading a sample container, as shown in FIG. In addition, the holder motor 121, which can raise or lower the sample container to the extraction part position, a holder 122 for fixing the holder motor, a gear coupling 125 for connecting the holder motor and the gear bar, and the holder motor The holder motor gear bar 127 connected to convert the rotational movement into a vertical motion, the holder coupling coupled to the holder motor gear bar 126 to move the holder cup up and down, and is generated when washing the extraction unit after extraction It consists of a drain port 124 for drainage of the waste water, a fixing stand 130 for fixing the gear bar, a bearing 129 for the rotation of the gear bar, and a fixing ring 128 for fixing the bearing and the fixing stand.

As shown in FIG. 9, the automatic stirring unit 170 of FIG. 3 includes a rotating magnet 171 with a magnet, a stirring motor 172 for rotating the rotating magnet, and a fixing stand 173 for fixing the stirring motor. And a support 174 for supporting the fixed base, and a stirring magnet 175 which rotates together by the magnetic field in the sample container 110 when the rotating magnet 171 is rotated by the stirring motor.

11A is a perspective view illustrating a structure of a transfer valve unit according to the present invention, and FIGS. 11B and 11C are cross-sectional views illustrating a flow path of a transfer valve according to the present invention, and the transfer valve unit 180 of FIG. 3 is illustrated in FIG. 11A. As described above, the transfer valve 181, the transfer valve heater 182 for heating the transfer valve to 120 ° C, the transfer valve temperature detector 183 for detecting the temperature of the transfer valve, and the temperature for maintaining the temperature of the transfer valve 11B and 11C, the transfer valve 181 is connected to the extraction unit 140 and the transfer unit 190 by switching the flow path.

12 is a cross-sectional view showing the structure of the transfer unit according to the present invention, wherein the transfer unit 190 of FIG. 3 connects the transfer valve 181 and the sample inlet 411 of the analysis device 400 as shown in FIG. A flow path 196, a transfer part connecting nut 191 for connecting the flow path and the transfer valve 181, a fixing pit 192 for fixing the connection nut and the flow path, and a transfer part heater 193 for heating the transfer part. A transfer part temperature detector 194 for detecting the temperature of the transfer part, a thermostat 195 for keeping the transfer part warm, an inlet connection nut 197 for connection with a sample inlet of the analyzer, a connection nut and a flow path It consists of a fixing foot 198 for fixing.

Referring to the operation of the automatic pretreatment apparatus of the present invention configured as described above are as follows.

Figure 4 shows the configuration of the volatile organic compound automatic pretreatment device 100 and the conventional gas chromatography ion trap analysis device 400 according to the present invention, the waste sample 108 collected in each steel mill process is weighed at 50g By loading in the sample container 110 specified in the present invention. At this time, the stirring magnet 175 for stirring is added together, and the sample container loaded with the sample 108 is sealed and mounted in the holder cup 123. The holder cup 123 equipped with the sample container is raised so that the extraction unit 140 is introduced into the sample container via the rubber membrane 113 of the sample container stopper by driving the holder motor 121.

At this time, the extraction unit 140, as shown in Figure 5, the transport gas from the transport gas reservoir 300 through the transport gas supply valve 102 and the extraction valve 142 through the transport gas inlet 143 of the extraction unit Flows and the flow path is cleaned. In addition, the transport gas flows through the flow path cleaning valve 101, the metering valve 156, and the solvent injection valve 104 to wash the flow path of the metering unit 150.

In FIG. 9, the holder cup 123 on which the sample container 110 is loaded has a holder motor gear bar for converting the driving motion of the holder motor 121 and the rotational motion of the holder motor into vertical motion to precisely control the rotation speed ( 127 is precisely raised to the position of the extraction unit 140.

As shown in FIG. 5, when the extraction unit 140 is introduced into the sample container 110 by raising the holder cup 123, the washing of the flow path of the transport gas is stopped. Instead, the solvent reservoir 200 accurately fills a certain amount of solvent in the metering unit 150 via the solvent supply valve 103 and the metering valve 156.

In FIG. 4, the solvent reservoir 200 is a container for storing a solvent necessary for the pretreatment of the sample, and the solvent is well diluted with the volatile substance contained in the solid sample 108 using distilled water having an acidity of 6 Ph. To assist in the extraction. The solvent reservoir 200 has a water level monitoring window 201 to easily check the remaining amount of solvent, when the water level is lowered to replenish distilled water.

In FIG. 10, the metering unit 150 is a graduated syringe 157 capable of metering, which enables accurate metering of the solvent required by the movement of the piston 159 connected to the piston motor 151 for precisely controlling the rotation speed. Done.

When a certain amount of solvent is filled in the metering unit 150 in this way, as shown in FIG. 5, the solvent supply valve 103 is closed, and the solvent in the metering unit of the metering valve 156 is shown in FIG. 8. The flow path is injected into the extraction unit 140 via the solvent injection valve 104 and the extraction valve 142. When all the solvent in the metering unit 150 is injected, the solvent injection valve 104 is closed, and the transport gas is injected into the extraction unit 140 through the transport gas supply valve 102 and the extraction valve 142 again, and the sample It helps to mix the sample 108 and the solvent in the vessel 110. In addition, the rotating magnet 171 is rotated by the driving of the stirring motor 172 of the automatic stirring unit 170, the stirring is added together with the sample 108 in the sample container 110 by the rotating magnetic field of the rotating magnet 171. The magnet 175 is rotated together to agitate the sample 108 and the solvent in the sample container 110.

In FIG. 9, the automatic stirring unit 170 rotates the rotating magnet 171 with magnets at both ends at 120 rpm by the stirring motor 172 which is a DC motor, and is generated by the rotation of the rotating magnet 171. The stirring magnet 175 injected together with the sample 108 in the sample container 110 is rotated together by the magnetic field, thereby stirring the sample 108 and the solvent in the sample container 110.

In addition, as shown in Figure 7b, because the characteristics of the volatile sample is maintained at a temperature higher than the room temperature is helpful for extraction, the sample in the sample container by the heater 146 built in the extraction unit 140 during the stirring of the sample 50 It is maintained by heating to ℃.

After the sample 108 and the solvent are mixed with the transport gas and stirred for 10 minutes by the automatic stirring unit 170, most of the volatile organic compounds contained in the sample 108 in the form of gas in the sample container 110. It is extracted and exists.

As shown in FIG. 5 in the sample container 110 in which the extracted volatile organic compounds are present, a transport gas is injected through the transport gas supply valve 102, and as shown in FIGS. 7C and 7D, an extraction valve When the flow path of 142 is switched, the volatile organic compounds in the sample container 110 are sucked through the transport gas inlet 143 and the transport gas outlet 144 of the extraction unit 140 to the transport valve unit 140. When the transfer valve 181 of the transfer valve unit 180 is operated to switch the flow path from the automatic pretreatment device 100 to the analysis device 400, the volatile organic matter in the gas state extracted in the sample container 110 is moved. The compound is automatically injected into the sample inlet 411 of the analyzer 400 through the transfer unit 181 through the transfer valve 181 along the transport gas.

In FIG. 4, the transfer valve unit 180 connects the automatic pretreatment device 100 and the analysis device 400, the transport gas is always flowing, and the separator tube heater of the analysis device 400 maintained at 120 ° C. 413 is maintained and is maintained at 120 ° C by the built-in heater 182 to prevent the extracted volatile organic compounds from adsorbing in the middle.

When the automatic pretreatment device 100 and the analyzer 400 are connected by the operation of the transfer valve unit 180, the gaseous volatile organic compound is quickly passed through the transfer unit 190 together with the transport gas. 400). The transfer unit 190 is also maintained at 150 ° C. by the built-in heater 193 to match the temperature conditions with the separator tube heater 413 of the analyzer 400 and to prevent the volatile organic compounds from being cooled and adsorbed in the middle. do.

The extract automatically injected through the sample inlet 411 of the analysis device 400 is transferred to the ion trap analysis unit 421 through the connection part 420 via the separation tube 412 and the automatic analysis is performed.

In FIG. 4, the computer 500 receives an analysis result from the analysis device 400, outputs the result to the screen, and is connected to the control unit 210 of the automatic preprocessing device 100 to automatically control each element.

On the other hand, in the automatic pretreatment device 100, when the extracted volatile organic compounds are transferred to the analysis device 400, the holder cup 123 loaded with the sample container 110 is lowered, the operator finished the sample container (110) Is removed from the holder cup (123).

In addition, as shown in FIG. 5, the transport gas flows from the transport gas reservoir 300 through the transport gas supply valve 102 and the extraction valve 142 through the transport gas inlet 143 of the extraction unit 140. The cleaning gas flows through the flow path cleaning valve 101, the metering valve 156, and the solvent injection valve 104 to clean the flow path of the metering unit 150.

After the analysis is completed in the analysis device 400, the operator instructs the pre-processing of the next sample through the computer 500, in the pre-processing device 100, the holder cup 123 is raised without the sample container 110 As shown in FIG. 5, a predetermined amount of solvent is injected into the metering unit 150 from the solvent reservoir 200 through the solvent supply valve 103 and the metering valve 156. When the solvent is injected into the metering unit 150, the solvent supply valve 103 is closed, and the piston 159 of the metering unit 150 is lifted up and passes through the solvent injection valve 104 and the extraction valve 142. The solvent in 150 washes the flow path through the extraction unit 140 and is drained through the drain hole 124 of the holder cup 123.

After the cleaning of the flow path by the solvent, the transport gas from the transport gas reservoir 300 through the transport gas supply valve 102 and the extraction valve 142 through the transport gas inlet 143 of the extraction unit 140 Flow to clean the flow path. In addition, the transport gas flows through the flow path cleaning valve 101, the metering valve 156, and the solvent injection valve 104 to clean the flow path of the metering unit 150.

As described above, the present invention provides a method for pretreatment of contaminants in the wastes of steel mills, in which the pretreatment and extraction of volatile organic compounds is performed more quickly and accurately to eliminate deviations in analysis results and to obtain extracts in the conventional aqueous solution. By automating the pretreatment process to extract volatile organic compounds in a gaseous state, the injection process of the thermal desorption sample injection device 10 for the extraction of an aqueous solution sample is omitted, and the pretreatment and extraction process of the waste sample and the injection of the analysis device are automatically performed. By doing so, it is possible to provide an automatic pretreatment apparatus for a volatile organic compound that fundamentally eliminates personal variation occurrence factors and process variation factors caused by workers.

According to the present invention, in the method of pretreatment of pollutants in the waste of each steel mill process, by providing an automatic pretreatment apparatus 100 for the extraction process of volatile organic compounds, the analysis of pollutants faster and more accurate The advantage of eliminating the deviation of the result can be obtained.

In addition, by automating the manual pretreatment process to obtain an aqueous solution extract through a conventional waste dissolution test method to extract the volatile organic compounds in a gas state, the injection process of the thermal desorption sample injection device 10 for the extraction of the aqueous solution sample By omitting and automatically preprocessing and extracting waste samples and injecting analytical equipment, fundamentally eliminating personal deviations and process deviations by workers, and dramatically shortening the pretreatment time of volatile organic compounds. You can expect to do it.

Claims (9)

In the automatic pretreatment apparatus of volatile organic compounds, A sample container 110 capable of loading and sealing waste samples; A holder part 120 capable of loading a sample container; An extraction unit 140 that is introduced into the sample container to extract volatile organic compounds; A metering unit 150 for introducing a solvent into the sample container; An automatic stirring unit 170 for stirring the sample in the sample container together with the solvent; A solvent reservoir 200 for storing a solvent; A transfer valve unit 180 for transferring the volatile organic compounds extracted in the gas state in the sample container to the analysis device 400; A transfer unit 190 connecting the transfer valve unit and the analysis device; A flow passage washing valve 101 for washing the metering unit 150 and the solvent injection passage from the transport gas reservoir 300; A transport gas supply valve 102 for supplying a transport gas to the extraction unit 140; A solvent supply valve 103 for supplying a solvent from the solvent reservoir 200 through the metering unit 150; A solvent injection valve 104 for injecting a solvent from the metering unit 150 into the extraction unit 140; A controller 210 which is in charge of motor driving and temperature control of each element and control of the valve; An automatic pretreatment apparatus for volatile organic compounds, comprising: a computer (500) connected to the control unit (210) of the automatic pretreatment apparatus to control each element and to output an analysis result from the analysis apparatus. The method of claim 1, wherein the sample container 110, Consists of a glass bottle 111 and a cap capable of sealing, The stopper is an automatic pretreatment apparatus for a volatile organic compound, characterized in that the plastic material is made of an outer portion 112 and the extraction portion is easy to seal the inner rubber membrane (113). The method of claim 1, wherein the holder portion 120, A holder cup 123 for loading the sample container 110, A holder motor 121 capable of raising or lowering the sample container to a location of the extraction unit 140; Fixing table 122 for fixing the holder motor, A gear coupling 125 connecting the holder motor and the gear bar; A holder motor gear bar 127 connected to the holder motor and converting a rotational movement into a vertical movement; A holder coupling 126 coupled to the holder motor gear bar to move the holder cup up and down; A drain 124 for draining the wastewater generated when the extraction part is washed after the extraction is finished, Fixing rod 130 for fixing the gear bar, A bearing 129 for rotating the gear bar; Automatic pretreatment device of a volatile organic compound, characterized in that consisting of a fixed ring (128) for fixing the bearing and the holder. The method of claim 1, wherein the extraction unit 140, Injector 141 for injecting a solvent into the sample container 110, Extraction valve 142 for opening and closing the flow path of the solvent and transport gas, A transport gas inlet 143 and a transport gas outlet 144 positioned on left and right sides of the injector, Fixing table 145 for fixing the extraction unit, A heater 146 embedded to enable heating of the extraction unit; Automatic pretreatment device of a volatile organic compound, characterized in that consisting of a temperature detector (147) for detecting the temperature of the extraction unit. The method of claim 1, wherein the metering unit 150, A graduated syringe 157 capable of measuring the amount of solvent to be injected into the sample container 110, A piston 159 for injecting or discharging the solvent into the graduated syringe, A piston motor 151 for moving the piston of the graduated syringe up and down, Fixing table 152 for fixing the piston motor, A piston motor gear bar 154 connected to the piston motor and converting a rotational movement into a vertical movement; A gear coupling 153 connecting the piston motor to the gear bar; A piston coupling 155 coupled to the piston motor gear bar to move the piston up and down; A metering valve 156 for opening and closing the flow path of the metering unit; Fixing table 158 for fixing the metering unit, Fixing rod 162 for fixing the gear bar, A bearing 161 for rotating the gear bar; Automatic pretreatment device of volatile organic compounds, characterized in that consisting of a fixing ring 160 for fixing the bearing and the stator. The method of claim 1, wherein the automatic stirring unit 170, Rotating magnet 171 with a magnet, A stirring motor 172 for rotating the rotating magnet; Fixing stand (173) for fixing the stirring motor, A support 174 for supporting the fixture; When the rotating magnet 171 is rotated by the stirring motor, automatic pretreatment apparatus for volatile organic compounds, characterized in that consisting of a stirring magnet 175 to be rotated together by a magnetic field in the sample container (110). The method of claim 1, wherein the solvent reservoir 200, A container for storing the solvent necessary for the pretreatment of the sample, the solvent is a distilled water of 6Ph acidity, and has a water level monitoring window 201, the automatic pretreatment of volatile organic compounds, characterized in that the remaining amount of solvent can be easily identified Device. The method of claim 1, wherein the transfer valve unit 180, A transfer valve 181 capable of switching the flow path, A transfer valve heater 182 for heating the transfer valve to 120 ° C .; A transfer valve temperature detector 183 for detecting a temperature of the transfer valve; Automatic pretreatment device of volatile organic compounds, characterized in that consisting of a heat insulating cover (184) for maintaining the temperature of the transfer valve. The method of claim 1, wherein the transfer unit 190, A flow path 196 connecting the transfer valve 181 and the sample inlet 411 of the analyzer 400; A transfer part connecting nut 191 for connecting the flow path and the transfer valve 181, Fixing feet 192 for fixing the connection nut and the flow path, A transfer part heater 193 for heating the transfer part; A transfer unit temperature detector 194 for detecting a temperature of the transfer unit; Insulating body 195 for the insulation of the transfer unit, An inlet connecting nut 197 for connection with a sample inlet of the analyzer; An automatic pretreatment apparatus for volatile organic compounds, characterized in that the coupling nut and the fixing feet (198) for fixing the flow path.