KR100993504B1 - Analysis equipment for nitrogen monoxide - Google Patents

Analysis equipment for nitrogen monoxide Download PDF

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KR100993504B1
KR100993504B1 KR1020090094813A KR20090094813A KR100993504B1 KR 100993504 B1 KR100993504 B1 KR 100993504B1 KR 1020090094813 A KR1020090094813 A KR 1020090094813A KR 20090094813 A KR20090094813 A KR 20090094813A KR 100993504 B1 KR100993504 B1 KR 100993504B1
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gas
analyzer
storage tank
supply pipe
ammonia
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이준열
장향자
서봉수
이재준
이진우
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(주)원익머트리얼즈
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)

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Abstract

PURPOSE: An analysis apparatus for nitrogen monoxide is provided to prevent the error of an analysis result by removing ammonia gas from a piping and each apparatus. CONSTITUTION: An analysis apparatus for nitrogen monoxide comprises the following: an ammonia gas storage tank(10); an air storage tank(20); a GC-TCD analysis device(40) analyzing NO, N2, and O2; a FT-IR analysis device(50) analyzing CO, CO2, N2O, CH4, NO2, and H2O; a moisture analysis device(60) analyzing the NO, the N2, and the O2; a He gas tank(100) inserting He gas to a gas supply pipeline(11); a mixing device(110) mixing ammonia gas and air; a reaction device(120) reacting the ammonia gas and the air to produce NO gas; a moisture removal device(130) removing the moisture from the NO gas by freezing; multiple computers(80); and a scrubber(70) discharging the gas in which the analysis is completed.

Description

일산화질소 분석장치{Analysis equipment for nitrogen monoxide}Nitrogen monoxide analyzer {Analysis equipment for nitrogen monoxide}

본 발명은 일산화질소 분석장치에 관한 것으로 상세하게는 에어 가스와 암모니아가스를 혼합장치에서 혼합하고, 반응장치를 통해 반응시켜 일산화질소 가스를 형성하고, 수분제거장치를 통해 일산화질소 가스의 수분을 제거한뒤 분석장치를 통해 분석하며, 분석후 전체 장치와 배관을 He 가스로 청소하고 진공펌프로 완전히 제거하는 구성으로 이루어지는 것을 특징으로 하는 일산화질소 분석장치에 관한 것이다.The present invention relates to a nitrogen monoxide analyzer, and in particular, air gas and ammonia gas are mixed in a mixing apparatus, reacted through a reaction apparatus to form nitrogen monoxide gas, and water is removed from the nitrogen monoxide gas through a moisture removal apparatus. Analyze through the back analysis device, and after the analysis relates to a nitrogen monoxide analysis device characterized in that the configuration consisting of a He gas and the vacuum pump is completely removed.

일반적으로 NO(일산화질소)는 반도체 공정에서 산화막을 증착시킬 때 사용되는 재료로서 사용되며, 대량의 반도체 제조를 위해 NO의 소요는 증가되는 추세이며 널리 이용되고 있다. In general, NO (nitrogen monoxide) is used as a material used when depositing an oxide film in a semiconductor process, and the requirement of NO is increasing and widely used for manufacturing a large amount of semiconductors.

반도체 산업의 발달로 인해 최근 NO 가스의 순도는 점점 더 고순도가 요구되고 있다.Due to the development of the semiconductor industry, the purity of NO gas has been increasingly required in recent years.

NO가스의 수요는 증가되고 있지만 공급되는 양은 전세계적으로 줄어들고 있어 NO 가스의 제조는 반드시 필요한 사업이며 이러한 NO 가스를 제조하는데 있어서 NO 가스와 불순물의 농도를 정확히 평가할 분석 시스템의 개발이 요구되고 있다.The demand for NO gas is increasing, but the quantity supplied is decreasing all over the world. Therefore, the production of NO gas is a necessary business and the development of an analytical system that accurately evaluates the concentration of NO gas and impurities in manufacturing NO gas is required.

상기 문제점을 해결하기 위하여 본 발명은 에어 가스와 암모니아가스를 혼합장치에서 혼합하고, 반응장치를 통해 반응시켜 일산화질소 가스를 형성하고, 수분제거장치를 통해 일산화질소 가스의 수분을 제거한뒤 분석장치를 통해 분석하며, 분석후 전체 장치와 배관을 He 가스로 청소하고 진공펌프로 완전히 제거하는 구성으로 이루어지는 일산화질소 분석장치를 제공하는데 그 목적이 있다.In order to solve the above problems, the present invention mixes air gas and ammonia gas in a mixing apparatus, reacts through a reaction apparatus to form nitrogen monoxide gas, and removes moisture of nitrogen monoxide gas through a moisture removing apparatus, and then analyzes the analysis apparatus. The purpose of the present invention is to provide a nitrogen monoxide analyzer which is configured to clean the entire apparatus and pipes with He gas and completely remove them with a vacuum pump after the analysis.

상기 과제를 해결하기 위한 본 발명은 일산화질소 분석장치에 관한 것으로서 에어 가스와 암모니아가스를 혼합장치에서 혼합하고, 반응장치를 통해 반응시켜 일산화질소 가스를 형성하고, 수분제거장치를 통해 일산화질소 가스의 수분을 제거한뒤 분석장치를 통해 분석하며, 분석후 전체 장치와 배관을 He 가스로 청소하고 진공펌프로 잔류가스를 완전히 제거하도록 구성되어진다.The present invention for solving the above problem relates to a nitrogen monoxide analyzer, the mixture of air gas and ammonia gas in a mixing device, and reacts through a reaction device to form a nitrogen monoxide gas, the moisture removal device of the nitrogen monoxide gas After removing water, it analyzes through analysis device. After analysis, the whole device and pipes are cleaned with He gas, and vacuum pump is used to completely remove residual gas.

본 발명은 암모니아가스와 에어 가스를 혼합하여 일산화질소 가스를 형성하고, 이를 특성에 맞는 분석장치로 분석하므로 정확한 성분 분석이 가능하며, 분석이 끝나면 He 가스를 주입하여 배관과 각 장치의 암모니아 가스를 제거하고, 진공펌프를 이용하여 He 가스를 배관과 장치에서 배출시키므로 다음 분석시에 가스가 섞여 분석결과가 잘못되는 것을 방지하는 효과가 있다.The present invention forms a nitrogen monoxide gas by mixing ammonia gas and air gas, and analyzes it with an analyzer suitable for characteristics, so that accurate component analysis is possible. Remove and discharge the He gas from the pipe and the device by using a vacuum pump, there is an effect to prevent the analysis results are wrong by mixing the gas in the next analysis.

본 발명은 일산화질소를 분석하는 장치에 있어서, 암모니아가스가 저장되어지는 암모니아가스저장탱크(10)와; 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)에 연결되어 에어(Air) 가스를 주입하는 에어(Air) 가스 저장탱크(20); 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, NO, N2, O2를 분석하는 GC-TCD(가스 크로마토그래피) 분석장치(40)와; 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, 상기 GC-TCD 분석장치(40)와 병렬로 연결되고, CO, CO2, N2O, CH4, NO2, H2O를 분석하는 FT-IR(퓨리에 변환 적외선 분광 광도계) 분석장치(50)와; 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, 상기 GC-TCD 분석장치(40) 및 FT-IR 분석장치(50)와 병렬로 연결되고, NO, N2, O2를 분석하는 수분분석장치(60)와; 상기 암모니아가스저장탱크(10)의 바로 뒷 배관에 연결되고, 암모니아가스저장탱크(10)에서 주입되는 암모니아가스를 가스공급배관(11)과 GC-TCD 분석장치(40), FT-IR 분석장치(50) 및 수분분석장치(60)내부에서 제거하기 위한 He가스를 가스공급배관(11)으로 주입하는 He 가스 탱크(100)와; 상기 암모니아가스저장탱크(10)와 에어 가스 저장탱크(20) 후단의 가스공급배관(11)에 설치되어 암모니아가스와 에어가스를 혼합하는 혼합장치(110)와; 상기 혼합장치(110)의 후단에 연결되어 에어가스와 암모니아가스를 반응시켜 NO가스를 생성하는 반응장치(120)와; 상기 반응장치(120)의 후단에 연결되어 NO가스 내에 포함되어진 수분을 동결시켜 제거하는 수분제거장치(130)와; 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60)가 각각 연결되며, 상기 GC- TCD 분석장치(40)와 FT-IR 분석장치 및 수분분석장치(60)의 분석정보를 수신받아 저장하며 표시하는 다수의 컴퓨터(80)와; 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60)와 배출배관(71)으로 연결되어 분석이 완료되어진 가스를 배출하는 스크러버(70);를 포함하여 구성되어진다.The present invention provides a device for analyzing nitrogen monoxide, comprising: an ammonia gas storage tank (10) in which ammonia gas is stored; An air gas storage tank 20 connected to the gas supply pipe 11 connected to the ammonia gas storage tank 10 to inject air gas; A GC-TCD (gas chromatography) analyzer 40 connected to the ammonia gas storage tank 10 and a gas supply pipe 11 to analyze NO, N 2 and O 2; It is connected to the ammonia gas storage tank 10 and the gas supply pipe 11, and connected in parallel with the GC-TCD analysis device 40, CO, CO 2 , N 2 O, CH 4 , NO 2 , H A FT-IR (Fourier Transform Infrared Spectrophotometer) analyzer 50 for analyzing 2 O; It is connected to the ammonia gas storage tank 10 and the gas supply pipe 11, and connected in parallel with the GC-TCD analyzer 40 and the FT-IR analyzer 50, NO, N 2 , O 2 Moisture analysis device 60 for analyzing the; Is connected to the pipe immediately behind the ammonia gas storage tank 10, the ammonia gas injected from the ammonia gas storage tank 10 gas supply pipe 11 and GC-TCD analyzer 40, FT-IR analyzer He 50 and the He gas tank 100 for injecting the He gas for removal in the moisture analysis device 60 into the gas supply pipe (11); A mixing device 110 installed in the gas supply pipe 11 at the rear end of the ammonia gas storage tank 10 and the air gas storage tank 20 to mix ammonia gas and air gas; A reaction device 120 connected to a rear end of the mixing device 110 to generate NO gas by reacting air gas and ammonia gas; A water removal device 130 connected to a rear end of the reaction device 120 to freeze and remove water contained in the NO gas; The GC-TCD analyzer 40, the FT-IR analyzer 50, and the moisture analyzer 60 are connected to each other, and the GC-TCD analyzer 40, the FT-IR analyzer, and the moisture analyzer ( A plurality of computers 80 for receiving, storing, and displaying the analysis information of 60); A scrubber 70 connected to the GC-TCD analyzer 40, the FT-IR analyzer 50, the moisture analyzer 60, and the discharge pipe 71 to discharge the gas for which the analysis is completed; It is constructed.

이러한 상기 암모니아가스저장탱크(10)와 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60) 간의 가스공급배관(11)에 각각의 조절밸브(90)가 설치되어지며, 상기 조절밸브(90)의 전단에 연결되어 상기 스크러버(70)와 연결되어지는 방출배관(72)에 가스 방출밸브(91)가 설치되며, 상기 조절밸브(90)의 전단인 가스공급배관(11)에 연결되며 상기 에어 가스 저장탱크(20)와 연결되는 에어 가스 배관(21)에 에어 가스를 유동시키는 에어 가스 밸브(93)가 설치되어지며, 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)에 암모니아가스를 유동시키는 암모니아가스 밸브(97)가 설치되어진다.Each control valve 90 in the gas supply pipe 11 between the ammonia gas storage tank 10, the GC-TCD analyzer 40, the FT-IR analyzer 50, and the moisture analyzer 60. Is installed, is connected to the front end of the control valve 90, the gas discharge valve 91 is installed on the discharge pipe 72 is connected to the scrubber 70, the front end of the control valve 90 An air gas valve 93 connected to a gas supply pipe 11 and flowing air gas is installed in an air gas pipe 21 connected to the air gas storage tank 20, and the ammonia gas storage tank 10 is provided. The ammonia gas valve 97 for flowing the ammonia gas is installed in the gas supply pipe 11 connected to the).

또한, 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)과 상기 방출밸브(91) 후단의 방출배관(72) 간에 진공배관(31)이 연결되며, 상기 진공배관(31)에 진공밸브(92)가 설치되어지고, 상기 진공밸브(92)의 상에 진공펌프가 설치되어 상기 진공배관(31)과 가스공급배관(11)을 진공상태가 되도록 한다.In addition, a vacuum pipe 31 is connected between the gas supply pipe 11 connected to the ammonia gas storage tank 10 and the discharge pipe 72 at the rear end of the discharge valve 91, and is connected to the vacuum pipe 31. A vacuum valve 92 is installed, and a vacuum pump is installed on the vacuum valve 92 to bring the vacuum pipe 31 and the gas supply pipe 11 into a vacuum state.

그리고, 상기 암모니아가스저장탱크(10)와 연결되어지는 가스공급배관(11)에는 상기 암모니아가스저장탱크(10)에서 유입되는 암모니아가스의 유량을 조절하는 제1 유량조절기(12)가 설치되어지고, 상기 에어 가스 탱크(20)와 연결되어지는 에어 가스 배관(21)에 에어 가스의 유량을 조절하는 제2 유량조절기(22)가 설치되어 진다.In addition, the gas supply pipe 11 connected to the ammonia gas storage tank 10 is provided with a first flow controller 12 for controlling the flow rate of ammonia gas flowing from the ammonia gas storage tank 10. In addition, a second flow controller 22 for adjusting the flow rate of the air gas is installed in the air gas pipe 21 connected to the air gas tank 20.

또한, 스크러버(70)에는 NO, H2O, NH3을 흡착하는 흡착제가 내장되어 상기 배출배관(71)을 통해 배출되어지는 가스가 통과하며 중화되도록 한다.In addition, the scrubber 70 has a built-in adsorbent for adsorbing NO, H 2 O, NH 3 so that the gas discharged through the discharge pipe 71 passes through and neutralized.

그리고, 상기 He 가스 탱크(100)는 혼합장치(110)와 수분제거장치(130)의 양단 가스공급배관(11)에 연결되어지며, 가스공급배관(11)과 연결되어지는 부분에 He 가스 개폐밸브(95)가 설치되고, He 가스 개폐밸브(95)와 He 가스 탱크(100) 간에는 He 가스의 역류를 방지하는 체크밸브(97)가 설치되어진다.In addition, the He gas tank 100 is connected to the gas supply pipe 11 at both ends of the mixing device 110 and the water removal device 130, the He gas opening and closing on the portion connected to the gas supply pipe (11). A valve 95 is provided, and a check valve 97 is provided between the He gas on-off valve 95 and the He gas tank 100 to prevent back flow of He gas.

삭제delete

즉, 본 발명을 좀더 상세하게 설명하면 다음과 같다.That is, the present invention will be described in more detail as follows.

암모니아가스가 저장되어지는 암모니아가스저장탱크(10)에서 배출되어지는 암모니아가스의 유량을 측정하여 조절하는 제1 유량조절기(12)가 암모니아가스저장탱크(10)의 배출구에 설치되어지고, 제1 유량조절기(12)와 연결되어 배출되어지는 암모니아가스를 개폐하는 암모니아가스 밸브(97)가 설치되어진다.A first flow regulator 12 for measuring and adjusting the flow rate of the ammonia gas discharged from the ammonia gas storage tank 10 in which the ammonia gas is stored is installed at the outlet of the ammonia gas storage tank 10, and the first The ammonia gas valve 97 which opens and closes the ammonia gas discharged in connection with the flow regulator 12 is provided.

그리고, 에어 가스가 저장되어진 에어 가스 저장탱크(20)의 배출구에 에어 가스의 유량을 측정하여 조절하는 제2 유량조절기(22)가 설치되고, 제2 유량조절기(22)와 연결되어 배출되어지는 에어 가스를 개폐하는 에어 가스 밸브(21)가 설치 되어 상기 암모니아가스 밸브(97)가 연결되는 가스공급배관(11)에 에어 가스 밸브(21)가 연결되는 배관이 연결되어진다.In addition, a second flow controller 22 is installed at the outlet of the air gas storage tank 20 in which the air gas is stored to measure and regulate the flow rate of the air gas, and is discharged in connection with the second flow controller 22. An air gas valve 21 for opening and closing the air gas is installed, and a pipe for connecting the air gas valve 21 to the gas supply pipe 11 to which the ammonia gas valve 97 is connected is connected.

상기 가스공급배관(11) 상에는 암모니아가스와 에어 가스를 혼합하는 혼합장치(110)가 설치되어지고, 상기 혼합장치(110)에서 혼합되어진 혼합가스가 유입되어 반응되어지는 반응장치(120)가 설치되어지며, 상기 반응장치(120)에서 반응되어진 혼합가스에 포함되어지는 수분을 제거하는 수분제거장치(130)가 설치되어진다.A mixing device 110 for mixing ammonia gas and air gas is installed on the gas supply pipe 11, and a reaction device 120 is installed in which the mixed gas mixed in the mixing device 110 is introduced and reacted. The water removal device 130 for removing water contained in the mixed gas reacted by the reaction device 120 is installed.

상기 수분제거장치(130)에서 배출되어지는 혼합가스가 가스공급배관(11)을 통해 병렬로 연결되어진 NO, N2, O2를 분석하는 GC-TCD(가스 크로마토그래피) 분석장치(40)와, CO, CO2, N2O, CH4, NO2, H2O를 분석하는 FT-IR(퓨리에 변환 적외선 분광 광도계) 분석장치(50)와, NO, N2, O2를 분석하는 수분분석장치(60)로 유입되어 측정되어지고, 이 측정값이 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60)에 연결되는 컴퓨터에 전송되어 표시되어지며, 상기 가스공급배관과 상기 GC-TCD 분석장치(40), FT-IR 분석장치(50), 수분분석장치(60) 간에는 각각 조절밸브(90)가 설치되어 유입되어지는 혼합가스의 양을 조절할 수 있다.GC-TCD (Gas Chromatography) analysis device 40 for analyzing the NO, N2, O2 connected in parallel through the gas supply pipe 11 is mixed gas discharged from the water removal device 130, CO Fourier Transform Infrared Spectrophotometer (FT-IR) Analyzer 50 to analyze CO2, N2O, CH4, NO2, H2O, and Moisture Analyzer 60 to analyze NO, N2, O2 The measured value is transmitted to and displayed on a computer connected to the GC-TCD analyzer 40, the FT-IR analyzer 50, and the moisture analyzer 60, and the gas supply pipe and the GC-TCD analysis are displayed. The control valve 90 is installed between the device 40, the FT-IR analyzer 50, and the moisture analyzer 60 to adjust the amount of the mixed gas introduced therein.

상기 조절밸브(90) 전단의 가스공급배관(11)과 상기 GC-TCD 분석장치(40), FT-IR 분석장치(50), 수분분석장치(60)의 후단에 연결되어 가스를 배출하는 배출배관(72)이 연결되어지고, 상기 배출배관(72)의 끝단에 스크러버(70)가 설치되어 NO, H2O, NH3을 흡착하는 흡착제를 통해 가스를 정화시켜 배출시키게 된다.The gas supply pipe 11 in front of the control valve 90 and the GC-TCD analysis device 40, the FT-IR analysis device 50, the discharge terminal connected to the rear end of the moisture analysis device 60 to discharge the gas A pipe 72 is connected, and a scrubber 70 is installed at the end of the discharge pipe 72 to purify and discharge the gas through an adsorbent that adsorbs NO, H 2 O, and NH 3.

상기 GC-TCD 분석장치(40)의 전단과 수분분석장치(60)의 후단에는 진공배 관(31)이 설치되고, 상기 진공배관(31) 상에는 진공펌프(30)가 설치되어 지며, 상기 진공펌프(30)의 배출구가 상기 배출배관()과 연결되어 가스를 배출시킨다. The vacuum pipe 31 is installed at the front end of the GC-TCD analysis device 40 and the rear end of the water analysis device 60, and the vacuum pump 30 is installed on the vacuum pipe 31. A discharge port of the pump 30 is connected to the discharge pipe () to discharge the gas.

상기 혼합장치(110)의 전단과 수분제거장치(130) 후단에는 가스공급배관(11)이 연결되어지는 부분에 He 가스 탱크(100)가 연결되어 He 가스로 전체 배관에 잔류하는 혼합가스를 배출시키며, 상기 He 가스 탱크(100)의 양단에는 He 가스 개폐밸브(95)가 설치되고, He 가스 개폐밸브(95)와 He 가스 탱크(100) 간에는 He 가스의 역류를 방지하는 체크밸브(97)가 설치되어진다.In front of the mixing device 110 and the rear end of the water removing device 130, the He gas tank 100 is connected to the portion where the gas supply pipe 11 is connected to discharge the mixed gas remaining in the entire pipe as He gas. He gas opening and closing valves 95 are installed at both ends of the He gas tank 100, and a check valve 97 preventing reverse flow of He gas between the He gas opening and closing valve 95 and the He gas tank 100. Is installed.

이러한 본 발명의 장치를 이용하여 일산화질소를 형성한뒤 성분을 측정하고난다음 장치 전체의 배관과 각 장치 내부에 잔류하는 일산화질소 가스를 완전히 배출하는 방법은 암모니아가스 밸브(97)와 에어 가스 밸브(21) 및 조절밸브(90)를 차단하고, He 가스 개폐밸브(95)를 개방하여 He 가스를 장치 전체 배관을 통과시켜 배출배관(72)으로 배출시키고, He 가스 개폐밸브(95)를 차단한뒤 진공배관(31)상에 설치되어진 진공밸브(92)를 개방하여 진공펌프(30)로 배관상에 잔류하는 He 가스를 스크러버(70)로 배출시키게 된다.After forming nitrogen monoxide using the apparatus of the present invention and measuring the components, a method of completely discharging the nitrogen monoxide gas remaining in the piping of the entire apparatus and inside each apparatus includes an ammonia gas valve 97 and an air gas valve. (21) and the control valve (90) are cut off, the He gas open / close valve (95) is opened, and the He gas is discharged to the discharge pipe (72) by passing the entire pipe of the apparatus, and the He gas open / close valve (95) is blocked. After that, the vacuum valve 92 installed on the vacuum pipe 31 is opened to discharge the He gas remaining on the pipe by the vacuum pump 30 to the scrubber 70.

비교예 1 : 고농도 NO가스(99.5%) 분석 Comparative Example 1 Analysis of Highly Concentrated NO Gas (99.5%)

도 1에 도시된 분석장치를 이용하여 반도체용 NO가스 제조에 원료로 사용되는 원료용 NO가스(99.5%)를 분석한 데이터이다. GC-TCD 분석장치(40) 에서는 NO, N2, O2를 분석하였으며 FT-IR 분석장치(50)을 이용하여 N2O, NO2, CO2, CO, CH4를 분석하였다. H2O는 수분분석장치(60)를 이용하였다. It is data analyzing the raw material NO gas (99.5%) used as a raw material to manufacture the NO gas for semiconductors using the analyzer shown in FIG. In the GC-TCD analyzer 40, NO, N 2 and O 2 were analyzed, and N 2 O, NO 2 , CO 2 , CO, and CH 4 were analyzed using the FT-IR analyzer 50. H 2 O was used for the moisture analyzer (60).

실시예 1 내지 3 : NO 제조가스 분석 Examples 1 to 3 NO production gas analysis

실시예 1,2,3은 도 1에 도시된 분석장치와 같이 가스 크로마토그래피(GC-TCD), 퓨리에 변환 적외선 분광 광도계 및 수분분석장치(60)를 이용하여 생성된 NO 제조가스를 분석한 정량분석 데이터이다. Examples 1, 2 and 3 are quantitative analyzes of the NO gas produced using gas chromatography (GC-TCD), a Fourier transform infrared spectrophotometer, and a water analyzer 60 as shown in FIG. Analytical data.

실시예 1은 가스반응 라인부를 통과하여 나온 NO 제조가스를 분석한 데이터이며 실시예 2는 가스반응 라인부 중 수분제거장치(130)를 통과하지 않고 바로 반응장치(120)에서 나온 NO 제조가스를 분석라인으로 통과시켜 분석한 데이터이다.Example 1 is the data analyzing the NO produced gas passed through the gas reaction line portion and Example 2 is the NO produced gas from the reaction device 120 directly without passing through the water removal device 130 of the gas reaction line portion Data analyzed by passing through the analysis line.

실시예 3은 실시예 1에서 나온 NO 제조가스를 정제시스템에 통과시켜 정제한 후 분석한 데이터이다. Example 3 is data analyzed after purifying the NO gas produced in Example 1 through a purification system.

도 1에 도시된 분석장치를 이용하면 불안정한 상태를 가지고 있는 NO 정제가스 및 불순물의 정량 분석이 가능함을 확인하였다.Using the analytical apparatus shown in FIG. 1, it was confirmed that quantitative analysis of NO purified gas and impurities having an unstable state was possible.

표 1TABLE 1

분석기Analyzer GC-TCDGC-TCD 수분분석장치Moisture Analysis Device FT-IFFT-IF 불순물impurities NONO N2 N 2 O2 O 2 H2OH 2 O N2ON 2 O NO2 NO 2 CO2 CO 2 COCO CH4CH4 비교예1Comparative Example 1 99.599.5 1.481.48 N.DN.D. 2222 151151 137137 33 N.D.N.D. 44 실시예1Example 1 46.946.9 36.636.6 2.622.62 6363 227227 265265 6666 4141 N.D.N.D. 실시예2Example 2 43.743.7 39.239.2 3.173.17 153153 276276 312312 9797 5353 1414 실시예3Example 3 92.992.9 0.10.1 N.D.N.D. 5050 178178 139139 3131 2525 N.D.N.D.

(농도단위: GC-TCD=%, FT-IR, 수분분석장치:ppmv)(Concentration unit: GC-TCD =%, FT-IR, moisture analyzer: ppmv)

실시예 1과 실시예 2에서 보면 알 수 있듯이 수분제거장치(130)를 통과한 NO 제조가스와 통과하지 않은 NO 제조가스는 수분 및 다른 불순물에서 많은 차이가 보이는 것을 알 수 있다. As can be seen from Example 1 and Example 2, it can be seen that the NO production gas that passed through the water removal device 130 and the NO production gas that did not pass show a great difference in moisture and other impurities.

도 1은 본 발명에 따른 일산화질소 분석장치의 전체 구성도,1 is an overall configuration diagram of a nitrogen monoxide analyzer according to the present invention,

도 2는 본 발명에 따른 일산화질소 분석장치의 실시예 1에서 FT-IR로 분석한 NO 생성가스의 분석스펙트럼을 나타내는 그래프,2 is a graph showing an analysis spectrum of the NO product gas analyzed by FT-IR in Example 1 of the nitrogen monoxide analyzer according to the present invention;

도 3은 본 발명에 따른 일산화질소 분석장치의 실시예 1에서 GC-TCD로 분석한 NO 생성가스의 분석스펙트럼을 나타내는 그래프,3 is a graph showing an analysis spectrum of the NO product gas analyzed by GC-TCD in Example 1 of the nitrogen monoxide analyzer according to the present invention;

도 4는 본 발명에 따른 일산화질소 분석장치의 실시예 1에서 수분분석장치로 분석한 NO 생성가스의 분석스펙트럼을 나타내는 그림으로 분석 후 10분이 지난 시점을 나타낸 그래프.Figure 4 is a graph showing the analysis spectrum of the NO product gas analyzed by the moisture analyzer in Example 1 of the nitrogen monoxide analyzer according to the present invention 10 minutes after the analysis.

<도면의 주요 부분에 대한 부호의 설명><Explanation of symbols for the main parts of the drawings>

10 : 암모니아가스저장탱크 20 : 에어 가스 저장탱크10: ammonia gas storage tank 20: air gas storage tank

30 : 진공펌프 40 : GC-TCD 분석장치30: vacuum pump 40: GC-TCD analysis device

50 : FT-IR 분석장치 60 : 수분분석장치50: FT-IR analyzer 60: moisture analyzer

70 : 스크러버 80 : 컴퓨터70: Scrubber 80: Computer

90 : 조절밸브 100 : He 가스 탱크90: control valve 100: He gas tank

110 : 혼합장치 120 : 반응장치110: mixing device 120: reactor

130 : 수분제거장치130: water removal device

Claims (7)

일산화질소를 분석하는 장치에 있어서,In the device for analyzing nitrogen monoxide, 암모니아가스가 저장되어지는 암모니아가스저장탱크(10)와;An ammonia gas storage tank 10 in which ammonia gas is stored; 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)에 연결되어 에어(Air) 가스를 주입하는 에어(Air)가스 저장탱크(20);An air gas storage tank 20 connected to the gas supply pipe 11 connected to the ammonia gas storage tank 10 to inject air gas; 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, NO, N2, O2를 분석하는 GC-TCD(가스 크로마토그래피) 분석장치(40)와;A GC-TCD (gas chromatography) analyzer 40 connected to the ammonia gas storage tank 10 and a gas supply pipe 11 to analyze NO, N 2 and O 2 ; 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, 상기 GC-TCD 분석장치(40)와 병렬로 연결되고, CO, CO2, N2O, CH4, NO2, H2O를 분석하는 FT-IR(퓨리에 변환 적외선 분광 광도계) 분석장치(50)와;It is connected to the ammonia gas storage tank 10 and the gas supply pipe 11, and connected in parallel with the GC-TCD analysis device 40, CO, CO 2 , N 2 O, CH 4 , NO 2 , H A FT-IR (Fourier Transform Infrared Spectrophotometer) analyzer 50 for analyzing 2 O; 상기 암모니아가스저장탱크(10)와 가스공급배관(11)으로 연결되며, 상기 GC-TCD 분석장치(40) 및 FT-IR 분석장치(50)와 병렬로 연결되고, NO, N2, O2를 분석하는 수분분석장치(60)와;It is connected to the ammonia gas storage tank 10 and the gas supply pipe 11, and connected in parallel with the GC-TCD analyzer 40 and the FT-IR analyzer 50, NO, N 2 , O 2 Moisture analysis device 60 for analyzing the; 상기 암모니아가스저장탱크(10)의 바로 뒷 배관에 연결되고, 암모니아가스저장탱크에서 주입되는 암모니아가스를 가스공급배관(11)과 GC-TCD 분석장치(40), FT-IR 분석장치(50) 및 수분분석장치(60)내부에서 제거하기 위한 He가스를 가스공급배관(11)으로 주입하는 He 가스 탱크(100)와;It is connected to the pipe immediately behind the ammonia gas storage tank 10, the ammonia gas injected from the ammonia gas storage tank gas supply pipe 11, GC-TCD analysis device 40, FT-IR analysis device 50 And He gas tank 100 for injecting the He gas for removing in the moisture analysis device 60 into the gas supply pipe (11); 상기 암모니아가스저장탱크(10)와 에어 가스 저장탱크(20) 후단의 가스공급 배관(11)에 설치되어 암모니아가스와 에어가스를 혼합하는 혼합장치(110)와;A mixing device 110 installed in the gas supply pipe 11 at the rear end of the ammonia gas storage tank 10 and the air gas storage tank 20 to mix the ammonia gas and the air gas; 상기 혼합장치(110)의 후단에 연결되어 에어가스와 암모니아가스를 반응시켜 NO가스를 생성하는 반응장치(120)와;A reaction device 120 connected to a rear end of the mixing device 110 to generate NO gas by reacting air gas and ammonia gas; 상기 반응장치(120)의 후단에 연결되어 NO가스 내에 포함되어진 수분을 동결시켜 제거하는 수분제거장치(130)와;A water removal device 130 connected to a rear end of the reaction device 120 to freeze and remove water contained in the NO gas; 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60)가 각각 연결되며, 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치 및 수분분석장치(60)의 분석정보를 수신받아 저장하며 표시하는 다수의 컴퓨터(80)와;The GC-TCD analyzer 40, the FT-IR analyzer 50, and the moisture analyzer 60 are connected to each other, and the GC-TCD analyzer 40, the FT-IR analyzer, and the moisture analyzer ( A plurality of computers 80 for receiving, storing, and displaying the analysis information of 60); 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60)와 배출배관(71)으로 연결되어 분석이 완료되어진 가스를 배출하는 스크러버(70);를 포함하여 구성되어지는 것을 특징으로 하는 일산화질소 분석장치.A scrubber 70 connected to the GC-TCD analyzer 40, the FT-IR analyzer 50, the moisture analyzer 60, and the discharge pipe 71 to discharge the gas for which the analysis is completed; Nitrogen monoxide analyzer, characterized in that configured. 제 1항에 있어서,The method of claim 1, 상기 암모니아가스저장탱크(10)와 상기 GC-TCD 분석장치(40)와 FT-IR 분석장치(50) 및 수분분석장치(60) 간의 가스공급배관(11)에 각각의 조절밸브(90)가 설치되어지며, 상기 조절밸브(90)의 전단에 연결되어 상기 스크러버(70)와 연결되어지는 방출배관(72)에 가스 방출밸브(91)가 설치되며, 상기 조절밸브(90)의 전단인 가스공급배관(11)에 연결되며 상기 에어 가스 저장탱크(20)와 연결되는 에어 가스 배관(21)에 에어 가스를 유동시키는 에어 가스 밸브(93)가 설치되어지며, 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)에 암모니아가스를 유동시키는 암모니아가스 밸브(97)가 설치되어지는 것을 특징으로 하는 일산화질소 분석장치.Each control valve 90 is provided in the gas supply pipe 11 between the ammonia gas storage tank 10, the GC-TCD analyzer 40, the FT-IR analyzer 50, and the moisture analyzer 60. Is installed, is connected to the front end of the control valve 90, the gas discharge valve 91 is installed in the discharge pipe 72 is connected to the scrubber 70, the gas that is the front end of the control valve 90 An air gas valve 93 is installed in the air gas pipe 21 connected to the supply pipe 11 and connected to the air gas storage tank 20. The ammonia gas storage tank 10 is installed. Nitrogen monoxide analyzer, characterized in that the ammonia gas valve (97) is installed in the gas supply pipe (11) connected to the flow. 제 2항에 있어서,3. The method of claim 2, 상기 암모니아가스저장탱크(10)와 연결되는 가스공급배관(11)과 상기 방출밸브(91) 후단의 방출배관(72) 간에 진공배관(31)이 연결되며, 상기 진공배관(31)에 진공밸브(92)가 설치되어지고, 상기 진공밸브(92)의 상에 진공펌프가 설치되어 상기 진공배관(31)과 가스공급배관을 진공상태가 되도록 하는 것을 특징으로 하는 일산화질소 분석장치.A vacuum pipe 31 is connected between the gas supply pipe 11 connected to the ammonia gas storage tank 10 and the discharge pipe 72 at the rear end of the discharge valve 91, and a vacuum valve is connected to the vacuum pipe 31. (92) is installed, the vacuum pump is installed on the vacuum valve (92), the nitrogen monoxide analyzing apparatus, characterized in that the vacuum pipe 31 and the gas supply pipe to be in a vacuum state. 제 1항에 있어서,The method of claim 1, 상기 암모니아가스저장탱크(10)와 연결되어지는 가스공급배관(11)에는 상기 암모니아가스저장탱크(10)에서 유입되는 암모니아가스의 유량을 조절하는 제1 유량조절기(12)가 설치되어지고, 상기 에어 가스 탱크(20)와 연결되어지는 에어 가스 배관(21)에 에어 가스의 유량을 조절하는 제2 유량조절기(22)가 설치되어지는 것을 특징으로 하는 일산화질소 분석장치.The gas supply pipe 11 connected to the ammonia gas storage tank 10 is provided with a first flow controller 12 for controlling the flow rate of ammonia gas flowing from the ammonia gas storage tank 10. Nitrogen monoxide analyzer, characterized in that the second flow controller 22 for adjusting the flow rate of the air gas is installed in the air gas pipe (21) connected to the air gas tank (20). 제 1항에 있어서,The method of claim 1, 상기 스크러버(70)에는 NO, H2O, NH3을 흡착하는 흡착제가 내장되어 상기 배출배관(71)을 통해 배출되어지는 가스가 통과하며 중화되도록 하는 것을 특징으로 하는 일산화질소 분석장치.Nitrogen monoxide analyzer, characterized in that the scrubber (70) has a built-in adsorbent for adsorbing NO, H 2 O, NH 3 to neutralize the gas discharged through the discharge pipe (71). 제 1항에 있어서,The method of claim 1, 상기 He 가스 탱크(100)는 혼합장치(110)와 수분제거장치(130)의 양단 가스공급배관(11)에 연결되어지며, 가스공급배관(11)과 연결되어지는 부분에 He 가스 개폐밸브(95)가 설치되고, He 가스 개폐밸브(95)와 He 가스 탱크(100) 간에는 He 가스의 역류를 방지하는 체크밸브(97)가 설치되어지는 것을 특징으로 하는 일산화질소 분석장치.The He gas tank 100 is connected to the gas supply pipe 11 at both ends of the mixing device 110 and the water removal device 130, the He gas opening and closing valve ( And a check valve (97) is provided between the He gas on-off valve (95) and the He gas tank (100) to prevent back flow of the He gas. 삭제delete
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CN102359989A (en) * 2011-07-18 2012-02-22 上海上计群力分析仪器有限公司 Multifunctional catalyst reaction evaluation and characterization device and application thereof
CN104730188A (en) * 2015-01-28 2015-06-24 中国农业科学院植物保护研究所 Gas chromatography analysis method for rapidly detecting nitrous oxide greenhouse gas
CN105067752A (en) * 2015-07-24 2015-11-18 中国科学院重庆绿色智能技术研究院 Program heating analysis equipment and method for testing property of its catalyst
KR101760104B1 (en) 2016-04-06 2017-07-21 (주)에스엔엘코리아 Apparatus for branching gas
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102359989A (en) * 2011-07-18 2012-02-22 上海上计群力分析仪器有限公司 Multifunctional catalyst reaction evaluation and characterization device and application thereof
CN104730188A (en) * 2015-01-28 2015-06-24 中国农业科学院植物保护研究所 Gas chromatography analysis method for rapidly detecting nitrous oxide greenhouse gas
CN105067752A (en) * 2015-07-24 2015-11-18 中国科学院重庆绿色智能技术研究院 Program heating analysis equipment and method for testing property of its catalyst
KR101760104B1 (en) 2016-04-06 2017-07-21 (주)에스엔엘코리아 Apparatus for branching gas
CN115524415A (en) * 2022-09-16 2022-12-27 重庆同辉科发气体有限公司 High-purity nitrous oxide analysis pipeline system
CN115524415B (en) * 2022-09-16 2023-05-30 重庆同辉科发气体有限公司 High-purity nitrous oxide analysis pipeline system

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