JP3804798B2 - Evaporation supply device for liquid organometallic compounds - Google Patents

Description

  The present invention relates to an apparatus for vaporizing and supplying a liquid organometallic compound to an inductively coupled plasma (Electrically Coupled Plasma) emission spectrometer (ICP).

In recent years, metal organic chemical vapor deposition (MOCVD) using an organometallic compound has attracted attention as a crystal growth method for compound semiconductors. The MOCVD method is one of crystal growth means often used for producing an epitaxial thin film of a compound semiconductor. For example, (CH ₃ ) ₃ Ga, (CH ₃ ) ₃ In, (CH ₃ ) ₃ Al, etc. The organic metal compound is used as a raw material, and the crystal growth of the thin film is performed by utilizing the thermal decomposition reaction.

  Since the quality of the semiconductor thin film obtained by MOCVD depends greatly on the chemical purity of the organometallic compound used as a raw material, from the beginning of this technology to the present, there has always been a higher purity organometallic compound. I have been asking.

  However, organometallic compounds are very difficult to handle because of their very strong chemical activity and toxicity, and it is still difficult to say that a method for analyzing trace impurities in organometallic compounds has been established.

  Most of the methods for analyzing trace impurities of organometallic compounds that have been reported so far use ICP as the analyzer, but the form of organometallic compound at the time of ICP measurement and introduction of organometallic compound into ICP As methods / apparatuses, the following six types of methods are broadly known.

<1> Hydrolysis method: After hydrolyzing an organometallic compound, the obtained aqueous solution is aerosolized with a nebulizer and supplied to an ICP torch.
[For example, Journal of Crystal Growth 77 (198
6) 47-54]
<2> Solution method: A method in which a mixed solution of an organometallic compound diluted with a solvent such as xylene is aerosolized with a nebulizer and supplied to an ICP torch.
[For example, ANALYST, MAY 1990, VOL. 115]
<3> Flow Injection method: an organometallic compound is mixed with diethyl ether,
Once the adduct is formed, it is passed through a nebulizer to make an aerosol. next,
By introducing the aerosol into a membrane drying tube, diethyl ether was removed from the system, and only the remaining organometallic compound was supplied to the ICP torch.
[For example, Spectrochimica Acta. Vol. 44B, no. 1
0, pp. 1041-1048, 1989]
<4> Electrothermal Vaporization method: 3,000 instantaneously
A method in which an organometallic compound is placed in a heater capable of raising the temperature to about 0 ° C., and the generated organometallic compound vapor is entrained with a carrier gas and directly introduced into the ICP torch.
[For example, JOURNAL OF ANALYTICAL ATOMIC SP
ECTROMETRY, DECEMBER 1994, VOL. 9]
<5> Direct vapor introduction method: A method in which a carrier gas is blown into an organometallic compound sealed in a SUS container, and the resulting organometallic compound vapor is directly introduced into the ICP torch.
[For example, Journal of Electronic Materials,
Vol. 18, no. 5, 1989]
<6> Exponential Dilution Method: A predetermined amount of an organometallic compound is put in a heater and heated, and the generated organometallic compound vapor is directly I by carrier gas.
Method to introduce to CP torch.
[For example, EUROPIAN PATENTION APPLICATION, EP04
47747A2]

  The above six methods have advantages and disadvantages, and none of them are analytical methods for completed organometallic compounds / introduction methods to ICP, but i) no pretreatment of organometallic compounds is necessary, ii) organometallic compounds Because it can be analyzed without diluting, high-sensitivity analysis is possible, iii) there is no change in concentration of impurities over time, and iv) the amount of sample required for measurement is very small. The Exponential Dilution method is said to be excellent.

  However, when such an Exponential Dilution method is used, for example, it is necessary to sample the organometallic compound from a container filled with the organometallic compound using a dispenser such as a syringe. Human body may be damaged due to poisoning, burns, etc. when introduced into the heater, ii) Organometallic compounds may be contaminated during sampling operation, iii) Repeated sampling every analysis There was a problem such as having to.

European Patent Application No. 447747 Journal of Crystal Growth 77 (1986) 47-54 ANALYST, MAY 1990, VOL. 115 Spectrochimica Acta. Vol. 44B, no. 10, pp. 1041-1048, 1989 JOURNAL OF ANALYTICAL ATOMIC SP ECTROMETRY, DECEMBER 1994, VOL. 9 Journal of Electronic Materials, Vol. 18, no. 5, 1989

  The present invention has been made in view of the above circumstances, and not only can safely handle organometallic compounds that are harmful to the human body, but can be reproduced with very high sensitivity even if only a very small amount of expensive organometallic compounds are used. An object of the present invention is to provide an apparatus for vaporizing and supplying a liquid organometallic compound capable of performing reliable ICP analysis.

As a result of intensive studies to achieve the above object, the present inventors have 1) vaporize a liquid raw material from a liquid raw material container filled with a liquid organometallic compound through a liquid mass flow controller for controlling the flow rate of the liquid raw material. A liquid feed path connected to the vaporizer;
2) a carrier gas path connected to the vaporizer from a carrier gas source via a carrier gas mass flow controller;
3) Further, the flow rate control of the calibration standard gas is performed in the gas path leading to the sample inlet of the inductively coupled plasma (ICP) through an inline monitor installed on the downstream side of the vaporizer. By connecting a gas path equipped with a mass flow controller for gas necessary for the operation, sampling of complicated and dangerous liquid organometallic compounds by a dispenser such as a syringe becomes unnecessary, and the safety to the human body is greatly improved. In addition to avoiding contamination during sampling, ICP analysis with extremely high sensitivity and high reproducibility is possible even with a very small amount of expensive organometallic compound. The apparatus for vaporizing and supplying a liquid organometallic compound of the invention can generate a plurality of calibration standard gases simultaneously. As a result, it is possible to perform qualitative and quantitative analysis of a wide range of impurities instantaneously, and as a result, it is possible to perform ICP analysis that is extremely safe, extremely sensitive, and highly reproducible. The present invention has been made.

Accordingly, the present invention provides the following vaporization supply apparatus.
[I] (1) A liquid source container containing a liquid organometallic compound, a vaporizer for vaporizing the liquid organometallic compound, and the container and the vaporizer are connected to control the flow rate of the liquid organometallic compound. A liquid material path in which a liquid mass flow controller is installed,
(2) a carrier gas source, a carrier gas path connecting the carrier gas source and the vaporizer, and having a carrier gas mass flow controller interposed therebetween;
(3) a sample gas path in which one end is connected to the gas outlet path of the vaporizer and the other end is connected to the sample inlet of the inductively coupled plasma emission spectrometer, and an inline monitor is interposed;
(4) A standard gas for controlling the flow rate of the calibration standard gas by connecting the gas cylinder filled with the calibration standard gas and the gas cylinder and a required part downstream of the in-line monitor interposition position of the sample gas path. A vaporizing and supplying apparatus for a liquid organometallic compound, characterized in that it comprises a standard gas path in which a mass flow controller is interposed
[II] The vaporization according to (1), wherein a plurality of standard gas cylinders for calibration are provided, and a plurality of standard gas passages each including a standard gas mass flow controller for controlling the flow rate of these standard gases are provided. Feeding device.

  The liquid organometallic compound vaporization supply device of the present invention was completely gasified by gasifying with a vaporizer after accurately measuring and controlling the flow rate of the liquid organometallic compound filled in the raw material container with a mass flow controller. By confirming the concentration of the organometallic compound gas with an in-line monitor, it is possible to always introduce an organometallic compound gas having an accurate concentration into the ICP apparatus. In addition, since the calibration standard gas can be directly supplied to the ICP apparatus, it is possible to perform in-line qualitative and quantitative analysis of the impurity concentration remaining in the organometallic compound gas. Therefore, the sampling operation of a complicated and dangerous liquid organometallic compound by a dispenser such as a syringe is not required, and not only the safety to the human body is greatly improved, but also contamination during sampling can be avoided, or Even if only a very small amount of expensive organometallic compound is used, ICP analysis with very high sensitivity and high reproducibility becomes possible.

Embodiments and examples of the invention

Hereinafter, the present invention will be described in more detail with reference to the drawings.
FIG. 1 shows an embodiment of a vaporized supply apparatus for a liquid organometallic compound according to the first invention of the present invention. In the figure, 1 is a liquid raw material container for storing a liquid organometallic compound (MO), 2 is an argon gas, etc. The carrier gas source 3 is a vaporizer. G1 is a liquid source path connecting the liquid source container 1 and the vaporizer 3, and a liquid mass flow controller MFC-1 for controlling the flow rate of the liquid organometallic compound is interposed in the path G1. At the same time, on-off valves V1 and V2 are provided upstream and downstream from the MFC-1 interposition position, respectively. In addition, the edge part by the side of the container 1 of the said path | route G1 is comprised as a dip tube, and the front-end | tip is immersed in the organometallic compound. G2 is a carrier gas path connecting the carrier gas source 2 and the vaporizer 3, and a carrier gas mass flow controller MFC-2 for controlling the flow rate of the carrier gas is interposed in this path G2, and this medium is connected to this path G2. An on-off valve V3 is interposed upstream from the mounting position. Further, G3 is a path connecting the container 1 and the carrier gas source 2, and is equipped with a pressure regulator 4 on the upstream side and an open / close valve V4 on the downstream side.

  Reference numeral 10 denotes an ICP device, and the gas outlet path of the vaporizer 3 and the sample inlet of the ICP device 10 are connected by a sample gas path G4. An in-line monitor 5 is interposed in the path G4, and an open / close valve V5 is interposed further downstream. Reference numeral 11 denotes a plasma torch, 12 denotes an injector, 13 denotes an RF coil, and 14 denotes a plasma flame.

  Reference numeral 6 denotes a gas cylinder filled with a calibration standard gas. This gas cylinder 6 is located between the inline monitor 5 interposition position and the open / close valve V5 interposition position of the sample gas path G4 by a standard gas path G5. Connected to the site. Here, in the path G5, a pressure regulator 4 ′, a standard gas mass flow controller MFC-3 for controlling the flow rate of the calibration standard gas, and an opening / closing valve V6 are sequentially provided from the upstream side to the downstream side. Yes. In this case, one end of the standard gas path G5 is connected to the carrier gas source 2 at the downstream side of the position where the opening / closing valve V6 is interposed, and the opening / closing valve V7 and the gas mass flow are sequentially connected from the upstream side toward the downstream side. The other end of the carrier gas path G6 in which the controller MFC-4 and the open / close valve V8 are respectively connected is connected, and the pressure regulator 4 ′ interposition position and the MFC-3 interposition position of the standard gas path G5 are connected. One end is connected to the carrier gas source 2 and the other end of the carrier gas path G7 in which the open / close valve V9 is interposed is connected to the intermediate portion. Further, a purge path G8 in which the open / close valve V10 is interposed is branched at a portion between the MFC-3 interposed position and the open / close valve V6 interposed position in the standard gas path G5.

  Note that a purge path G9 having an opening / closing valve V11 is also branched between the inline monitor 5 insertion position and the opening / closing valve V5 insertion position of the sample gas path G4.

  The vaporizer 3 has a gas-liquid mixing part and a nozzle part arranged in close proximity to each other and mixes a liquid organometallic compound with a carrier gas while controlling the flow rate in the gas-liquid mixing part. The liquid mixture is discharged from the nozzle portion in a sprayed state to vaporize the liquid organometallic compound, and the organometallic compound gas generated by the vaporization is taken out from the gas outlet path downstream of the nozzle portion together with the carrier gas. It is. Further, the vaporizer 3 is provided with a heater, and the organometallic compound gas can be efficiently and stably gasified.

  The in-line monitor 5 is a device that measures the raw material concentration in the gas path G4, and is arranged to check whether the raw material gas concentration supplied to the ICP is a set value. The measurement principle is that an organometallic compound gas is passed through an infrared absorption cell built in the in-line monitor 5 to measure infrared absorption peculiar to the gas with an infrared detector and convert it into a concentration. . Here, the organometallic compound gas whose concentration has been measured is directly introduced into the ICP 10 via the gas path G4. In order to further stabilize the concentration of the organometallic compound gas in the gas path, the organometallic compound gas may be used as necessary. It is effective to perform gas purging from the path G9 with the on-off valve V5 closed and the on-off valve V11 opened.

  In addition, there is a possibility that some pressure fluctuation may occur at the time of valve switching. In order to reduce this, as shown in FIG. 2, a double block valve (pneumatic operation valve) in which the open / close valves V5 and V11 are integrated. By using (Equation), the supply path can be changed instantaneously without pressure fluctuation.

  The calibration standard gas is a reference gas necessary for quantifying the concentration of impurities remaining in the liquid organometallic compound (MO), but the compound containing the same element as the impurity to be analyzed has a high purity. It is prepared by diluting with argon gas and precisely analyzing the gas concentration with a high-performance analyzer such as API-MS (Atmosphere Pressure Ionization-Mass Spectrometer). The calibration standard gas is introduced into the ICP through the path G5 having the standard gas mass flow controller MFC-3 interposed. At this time, the flow rate of gas supplied to the ICP is arbitrarily set by the mass flow controller MFC-3. By changing, a calibration curve of impurity concentration to be analyzed (impurity concentration vs. ICP peak sensitivity) can be created.

  A compound that can be used as a calibration standard gas contains a target metal, has an appropriate vapor pressure, and does not cause a complicated chemical change even when various kinds of compounds are mixed. Tetramethylsilane and tetramethylgerman are preferred when impurities are to be measured. The gas for diluting the compound is optimally argon, and its concentration is 0.1 to 1,000 ppm, preferably 1 to 100 ppm. The calibration standard gas must be calibrated with a high-performance analyzer such as API-MS for an accurate metal concentration. The calibration standard gas passes through the mass flow controller MFC-3 and is introduced into the ICP to measure the peak intensity corresponding to each element. The calibration curve obtained from the peak intensity and the standard gas concentration is used as a calibration curve. By using it, the impurity concentration in the organometallic compound gas can be accurately obtained.

  In order to further stabilize the concentration of the calibration standard gas in the gas path, it is effective to perform gas purging from the path G8 with the on-off valve V6 closed and the on-off valve V10 opened as necessary. .

  In addition, there is a possibility that some pressure fluctuation may occur at the time of valve switching. In order to reduce this, as shown in FIG. 3, a double block valve (pneumatic operation valve) in which the open / close valves V6 and V10 are integrated. By using (Equation), it is possible to change the supply path instantaneously without pressure fluctuation.

  When the organometallic compound gas or the calibration standard gas is transported through the piping path, the organometallic compound or the metal component is adsorbed on the inner wall of the piping, which may have a memory effect and adversely affect the analysis result. Therefore, in order to eliminate this influence, a pipe from the downstream side of the vaporizer 3 in the path G4 to the inline monitor 5, a pipe from the downstream side of the inline monitor 5 to the ICP 10, and an open / close valve V6 in the path G5 It is preferable to attach a heater 7 such as a tape heater to the downstream pipe, the downstream pipe of the opening / closing valve V8 of the path G6, and the upstream pipe of the path G9.

  In order to instantaneously remove the memory effect of the calibration standard gas, the purge gas can be flowed from the path G6 through the opening / closing valve V7, the gas mass flow controller MFC-4, and the opening / closing valve V8.

  FIG. 4 shows an embodiment of the second invention. In this example, gas cylinders 6a and 6b respectively filled with two kinds of calibration standard gases are arranged. The gas cylinders 6a and 6b are respectively provided with pressure regulators 4′a and 6a sequentially from the upstream side toward the downstream side. 4′b, standard gas mass flow controllers MFC-3a and MFC-3b for controlling the standard gas flow rate, and one end of standard gas paths G5a and G5b interposing the open / close valves V6a and V6b are connected. The other ends of the paths G5a and G5b are connected to one end of the standard gas supply path G5c, and the other end of the path G5c is a portion between the inline monitor 5 interposition position and the opening / closing valve V5 interposition position of the sample gas path G4. It is connected to the. The paths G5a and G5b are connected to paths G6 and G7 that interpose valves V8a, V8b, V9a, and V9b, respectively, and purge paths G8a and G8b that intervene valves V10a and V10b are branched. Other configurations are the same as those in FIG.

  Note that the number of calibration standard gases may be three or more, and in this case, a standard gas path similar to the above may be provided in these cylinders.

  Since the calibration standard gas corresponds to the type of impurities to be analyzed, the number of elements necessary for the analysis is finally required. In order to simplify the equipment, a standard gas for multi-element calibration should be prepared in which all the metal-containing compounds to be measured are charged in a single pressure vessel. A non-volatile compound may be produced, or it may be changed to another compound. Therefore, it becomes necessary to divide the stable compounds into several groups even if they are mixed with each other, and a plurality of calibration standard gases and supply paths corresponding thereto are required. In view of the above, it is desirable that the type of calibration standard gas, the number of gas mass flow controllers used, and the gas path are 2-5 systems.

  Furthermore, the liquid organic metal compound vaporization supply apparatus of the present invention is a pipe length of the liquid raw material path G1 from the liquid raw material container 1 filled with the liquid organic metal compound (MO) of the first and second inventions to the vaporization apparatus 3. By using a pipe having an outer diameter of 1/8 inch or less, and using the main valve V1 attached to the raw material container 1 as small as possible, The dead volume in the controller MFC-1, the vaporizer 3, the main valve V1, or the liquid source path G1 can be minimized.

  In the apparatus for vaporizing and supplying a liquid organometallic compound of the present invention, the flow rate of the liquid organometallic compound (MO) raw material supplied to the vaporizing apparatus 3 from the liquid mass flow controller MFC-1 of the first and second inventions is 0. 005 to 1 g / min, more preferably 0.01 to 0.1 g / min, and the flow rate of the carrier gas supplied to the vaporizer 3 is 10 to 3,000 ml / min, more preferably 50 to The range is 1,000 ml / min.

  Furthermore, in the apparatus for vaporizing and supplying a liquid organometallic compound according to the present invention, the flow rate of the mass flow controller MFC-3 for standard gas according to the first and second inventions is 0.1 to 100 ml / min, more preferably 1 to 10 ml. / The range is every minute.

  By opening the open / close valve V3 and passing the carrier gas through the carrier gas mass flow controller MFC-2 for which the carrier gas flow rate has been set in advance, the carrier gas is transferred from the vaporizer 3 to the ICP via the gas path G4 via the inline monitor 5. Will be transported. The result of the ICP measurement performed in this state is defined as a blank.

  By passing the carrier gas adjusted to a predetermined pressure by the pressure regulator 4 to the liquid source container 1 via the opening / closing valve V4, the internal pressure in the liquid source container 1 is increased. When the main valve V1 is opened in this state, the liquid organometallic compound (MO) passes from the dip tube through the main valve V1 to the vicinity of the liquid mass flow controller MFC-1, but when the opening / closing valve V2 is further opened, the liquid The organometallic compound reaches the liquid mass flow controller MFC-1, and simultaneously starts the flow rate control.

  As a result, the liquid organometallic compound (MO) having a constant flow rate is supplied to the vaporizer 3 through the path G1, and is diluted with the carrier gas transported in large quantities from the carrier gas mass flow controller MFC-2. The organometallic compound that has been mixed and instantaneously heated to a predetermined temperature, for example, 150 ° C. in the vaporizer 3 and completely gasified is transported at high speed to the in-line monitor 5 through the path G4.

  The in-line monitor 5 measures the concentration of the organometallic compound gas diluted and mixed in the carrier gas, and determines whether or not the concentration is a predetermined concentration. The organometallic compound gas discharged from the in-line monitor 5 is introduced into the ICP 10 through the opening / closing valve V5 from the path G4.

  Further, in order to accurately quantify the amount of impurities in the organometallic compound gas, the calibration standard gas is introduced into the ICP 10 via the standard gas mass flow controller MFC-3 and further via the path G4 from the path G5. be able to.

  Here, the liquid organometallic compound (MO) to be subjected to ICP analysis is not particularly limited as long as it is used as a raw material for MOCVD, but so-called compound semiconductor materials such as III-V and II-VI semiconductors. It has a remarkable effect on trace analysis.

  Specific compound names include trimethyl (ethyl) gallium, trimethyl (ethyl) indium, trimethyl (ethyl) aluminum, dimethyl (ethyl) zinc, tertiary butylphosphine, tertiary butylarsine, and the like. It is not limited, and all compounds can be analyzed as long as they are liquid organometallic compounds, organic compounds, metal hydride compounds, metal halide compounds that have a slight vapor pressure at normal temperature and normal pressure. . However, analysis is basically impossible unless the metal impurity to be analyzed has vapor pressure and cannot be transported by carrier gas.

More specifically, the operation example of the apparatus is as follows.
First, the ICP-AES plasma torch is turned on to confirm that the plasma is combusting stably. The on-off valve V5 is opened, and the flow rate of the carrier gas (argon) is controlled by the gas mass flow controller MFC-2. The flow rate of the carrier gas is set to 500 to 700 ml / min necessary for stably burning the argon plasma. At this time, the carrier gas is supplied to the ICP through the vaporizer 3 and the in-line monitor 5.

After setting the pressure of the pressure regulator 4 to 2 kg / cm ² , the on-off valve V9 is closed, and after opening the main valve V1, the main valve V4 is gradually opened. When the on-off valve V2 is opened in this state, the liquid mass flow controller MFC-1 immediately starts the flow control, and starts supplying the liquid organometallic compound at a constant flow rate to the vaporizer 3. The set value of the mass flow controller MFC-1 for liquid is in the range of 0.01 to 0.1 g / min.

  The liquid organometallic compound (MO) that has reached the vaporizer 3 is diluted and mixed here with a large amount of carrier gas, but is further heated to 150 ° C. with a heater, so that it can be monitored in-line from the path G4. Transported at high speed up to 5. The organometallic compound gas whose concentration is measured by the in-line monitor 5 is directly introduced into the ICP from the gas path G4 via the opening / closing valve V5. In order to further stabilize the concentration of the organometallic compound gas in the gas path. For this, it is effective to perform gas purging for about 2 to 5 minutes from the path G9 with the on-off valve V5 closed and the on-off valve V11 opened. In addition, there is a possibility that some pressure fluctuation may occur at the time of this valve switching. In order to alleviate this, a double block valve (air operated type) in which the open / close valves V5 and V11 are integrated as shown in FIG. By using, the supply path can be changed instantaneously without pressure fluctuation.

  In this way, by supplying an organometallic compound gas whose concentration and flow rate are clearly defined to the ICP, it is possible to perform an ICP analysis that is quick, highly accurate, and extremely safe for the human body.

  The compound that can be used for the calibration standard gas is preferably one that contains the target metal, has an appropriate vapor pressure, and does not cause complex chemical changes to each other even when various types of compounds are mixed. Tetramethylsilane and tetramethylgerman are preferred when silicon impurities are to be measured. The gas for diluting the compound is optimally argon, and its concentration is 0.1 to 1,000 ppm, preferably 1 to 100 ppm. The calibration standard gas must be calibrated with a high-performance analyzer such as API-MS for the exact metal concentration. The calibration standard gas passes through the mass flow controller, and is introduced into the ICP via the path G5 and further through G4, whereby the peak intensity corresponding to each element is measured. This peak intensity and the standard gas concentration By using the calibration curve obtained from the above, the impurity concentration in the organometallic compound gas can be accurately determined.

  In order to further stabilize the concentration in the gas path of the calibration standard gas, it is effective to perform gas purging for about 2 to 5 minutes from the path G8 with the on-off valve V6 closed and the on-off valve V10 opened. is there. In addition, there is a possibility that some pressure fluctuation may occur when switching the valve. In order to alleviate this, as shown in FIG. 3, a double block valve (air operated type) in which the open / close valves V6 and V10 are integrated. ) Can be used to change the supply path instantly without pressure fluctuation.

  Furthermore, since the liquid organometallic compound vaporization supply apparatus of the present invention can simultaneously generate a plurality of calibration standard gases, a wide range of qualitative and quantitative analysis of impurities can be instantaneously performed. In this case, the chemical reaction of each compound used for the standard gas can be prevented by dividing the calibration standard gas into a plurality of systems.

  As a result, it is possible to perform ICP analysis with extremely high safety, extremely high sensitivity, and high reproducibility.

It is a schematic block diagram which shows one Example of this invention. It is a schematic block diagram which shows the other Example of this invention. It is a schematic block diagram which shows another Example of this invention. It is a schematic block diagram which shows another Example of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Liquid raw material container 2 Carrier gas source 3 Vaporizer 4 Pressure regulator 5 In-line monitor 6 Standard gas cylinder for calibration 7 Heater 10 ICP apparatus MFC-1 to MFC-4 Mass flow controllers V1 to V11 Opening and closing valves G1 to G9

Claims (2)

(1) A liquid raw material container containing a liquid organometallic compound, a vaporizer for vaporizing the liquid organometallic compound, and a liquid for controlling the flow rate of the liquid organometallic compound by connecting the container and the vaporizer A liquid material path with a mass flow controller,
(2) connecting a carrier gas source, the carrier gas source and the vaporizer;
A carrier gas path in which a mass flow controller for carrier gas is interposed;
(3) a sample gas path in which one end is connected to the gas outlet path of the vaporizer and the other end is connected to the sample inlet of the inductively coupled plasma emission spectrometer, and an inline monitor is interposed;
(4) A standard gas for controlling the flow rate of the calibration standard gas by connecting the gas cylinder filled with the calibration standard gas and the gas cylinder and a required part downstream of the in-line monitor interposition position of the sample gas path. A vaporization supply device for a liquid organometallic compound, comprising a standard gas path in which a mass flow controller for a gas is interposed. The vaporization supply apparatus according to claim 1, further comprising a plurality of standard gas passages in which a plurality of standard gas cylinders for calibration are arranged and a standard gas mass flow controller for controlling the flow rate of these standard gases is provided.

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