JP2004279260A - Liquefied gas online analysis system - Google Patents

Liquefied gas online analysis system Download PDF

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Publication number
JP2004279260A
JP2004279260A JP2003072156A JP2003072156A JP2004279260A JP 2004279260 A JP2004279260 A JP 2004279260A JP 2003072156 A JP2003072156 A JP 2003072156A JP 2003072156 A JP2003072156 A JP 2003072156A JP 2004279260 A JP2004279260 A JP 2004279260A
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Japan
Prior art keywords
sample
liquefied gas
liquefied
liquid state
sampling
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JP2003072156A
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Japanese (ja)
Inventor
Katsue Chikamatsu
勝栄 親松
Tetsuo Igarashi
哲夫 五十嵐
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Mitsubishi Gas Chemical Co Inc
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Mitsubishi Gas Chemical Co Inc
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Priority to JP2003072156A priority Critical patent/JP2004279260A/en
Publication of JP2004279260A publication Critical patent/JP2004279260A/en
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Abstract

<P>PROBLEM TO BE SOLVED: To sample and analyze a sample in a liquefied state online in a manufacturing plant, a storage plant, etc. for handling a liquefied gas, such as dimethyl ether, methyl amine, propane, cyanogen chloride, hydrocyanic acid, liquefied petroleum gas (LPG) liquefied by compression/refrigeration or a composition containing the liquefied gas. <P>SOLUTION: A thermally controlled low temperature tank is provided so as to sample the sample in the liquefied state and supply it to an analysis apparatus, and the tank includes pressure-proof flow path piping and a sampling apparatus. Only the required quantity of the sample can be collected by handling the sample in the liquefied state, and a sensitive and efficient online analysis can be implemented. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

【0001】
【発明の属する技術分野】
本発明は、液化ガス(常温常圧下ではガス状を呈する気体が圧縮あるいは同時に冷却することで液体になるガスをさし、以下液化ガスという)又は液化ガスを含有する組成物からなる試料を液体の状態でサンプリングし分析するためのオンライン分析システムに関する。このようなオンライン分析システムは、液化ガス又は液化ガスを含有する組成物を原料とする製造設備、或いは貯蔵設備等をオンラインで監視、制御する上で有用である。
【0002】
【従来の技術】
従来、液化ガス又は液化ガスを含有する組成物からなる試料を分析する場合、試料をガス化したうえでサンプリングし分析していた(例えば、特許文献1参照)。そのため、該試料をオンラインで分析するためには、試料を連続的且つ完全にガス化する装置が必要なうえに、分析に用いなかった余剰なガス化した試料を元の反応装置に戻すには困難さが伴うため、何らかの方法を講じて廃棄する必要があった。例えば、大気に廃棄する場合には環境上の問題があり、しかも原料の損失を伴うため非効率なシステムになっていた。
【0003】
【特許文献1】
特開平7−20012号公報
【0004】
【発明が解決しようとする課題】
本発明の目的は、従来技術における上記したような課題を解決し、圧縮・冷却することで液体にすることができるジメチルエーテル、メチルアミン、プロパン、塩化シアン、シアン化水素、液化石油ガス(LPG)等の、液化ガス又は液化ガスを含有する組成物を取り扱う製造設備や貯蔵設備等において、試料を液体の状態でオンラインでサンプリングし分析できるようにすることにある。これによって、予め試料をガス化する装置や工程が必要なくなり、余剰の試料は液体状態のままで元の製造設備や貯蔵設備等に戻すことができるようになるため、生産の効率化や原単位の向上につながる。
【0005】
【課題を解決するための手段】
本発明者は、液化ガス又は液化ガスを含有する組成物からなる試料を液態状態のままでサンプリングし分析できる装置について鋭意研究を重ねた結果、該試料を液体状態にすることができる温度にコントロールされた低温槽内に、該試料を液体状態にすることができる耐圧配管と、該試料を液体状態でサンプリングできるサンプリング装置を設置することで、液化ガス又は液化ガスを含有する組成物を取り扱う製造設備や貯蔵設備等をオンラインで簡便且つ効果的に監視、制御できることを見いだし、本発明に到達した。
【0006】
すなわち、本発明は、液化ガス又は液化ガスを含有する組成物からなる試料を液体の状態のままオンラインでサンプリングして分析する(1)(2)示す液化ガスオンライン分析システムに関する。
(1)液化ガス又は液化ガスを含有する組成物からなる試料を液体の状態でサンプリングできる装置、及び該試料を分析できる分析装置から構成される、液化ガスオンライン分析システム。
(2)液化ガス又は液化ガスを含有する組成物からなる試料を液体の状態でサンプリングできる装置において、該試料を液体の状態にすることができる温度にコントロールされた低温槽内に、該試料を液体の状態にすることができる圧力を維持できる配管、及び該試料を液体の状態でサンプリングできるサンプリング装置を設置してある、(1)記載の液化ガスオンライン分析システム。
【0007】
【発明の実施の形態】
本発明の装置は、液化ガス又は液化ガスを含有する組成物からなる試料を、液体状態に保てるように温度コントロールされた低温槽、該低温槽内に配置された耐圧配管及びサンプリング装置を有している(図1)。サンプリングされた液体試料は、低温槽外の近接した分析装置、例えばガスクロマトグラフ、液体クロマトグラフ、或いはカールフィッシャー水分測定装置等に導入して分析される。
【0008】
【実施例】
以下、本発明の実施例を示すが本発明はこれにより限定されるものではない。実施例1
液化ガスであるジメチルエーテル(沸点−23.6℃)を製造する装置において、製品組成をオンラインで測定するため本発明の装置を使用した。サンプリング用のバイパスラインとして製品槽に付設したブラインで保冷された試料配管を、温度コントロールが可能な低温槽内(−10℃〜5℃)の耐圧配管(耐圧2MPa仕様)及びサンプリング装置に連結させ、循環している反応混合液の一部を必要なタイミング(装置変動時は短時間間隔で、安定時は長時間間隔)でサンプリング装置内にあるサンプリングコックを作動させて、分析目的によって1〜50μlの試料をサンプリングし、この液体状の試料を、近接した分析用のガスクロマトグラフ装置(株式会社島津製作所製GC−14Bシリーズ)に導入して分析した。また、別系統では同様にしてサンプリングした試料を、低温槽に近接した液体クロマトグラフ装置(株式会社日立製作所製L−7000シリーズ)に導入して分析した。
【0009】
【発明の効果】
本発明の装置により、液化ガス又は液化ガスを含有する組成物からなる試料を液体状態のままオンラインで取り扱うことが可能となり、従来のように試料を予めガス化する必要がなくなり、分析測定に伴う装置及び工程の簡略化や余剰サンプルの廃棄問題を解消することができる。
【図面の簡単な説明】
【図1】本発明のシステム
【符号の説明】
1:低温槽
2:サンプリング装置
3:分析装置
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a liquefied gas (hereinafter, referred to as a liquefied gas, which is a gas that becomes a liquid by compressing or simultaneously cooling a gas that is in a gaseous state at normal temperature and normal pressure), or a liquid gas-containing sample. The present invention relates to an on-line analysis system for sampling and analyzing in a state. Such an online analysis system is useful for online monitoring and control of a production facility or a storage facility that uses a liquefied gas or a composition containing a liquefied gas as a raw material.
[0002]
[Prior art]
Conventionally, when analyzing a sample made of a liquefied gas or a composition containing a liquefied gas, the sample has been gasified and then sampled and analyzed (for example, see Patent Document 1). Therefore, in order to analyze the sample online, a device for continuously and completely gasifying the sample is required, and in order to return the excess gasified sample not used for analysis to the original reactor, Because of the difficulties, it was necessary to take some measures and dispose of them. For example, disposal in the atmosphere has an environmental problem, and is accompanied by a loss of raw materials, resulting in an inefficient system.
[0003]
[Patent Document 1]
Japanese Patent Application Laid-Open No. Hei 7-20012
[Problems to be solved by the invention]
SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems in the prior art and to provide a liquid such as dimethyl ether, methylamine, propane, cyanogen chloride, hydrogen cyanide, liquefied petroleum gas (LPG) which can be made liquid by compression and cooling. Another object of the present invention is to make it possible to sample and analyze a sample in a liquid state online in a manufacturing facility or a storage facility that handles a liquefied gas or a composition containing a liquefied gas. This eliminates the need for a device or process for gasifying the sample in advance, and allows the excess sample to be returned to the original manufacturing facility or storage facility in a liquid state, thereby improving production efficiency and reducing unit consumption. Leads to improvement.
[0005]
[Means for Solving the Problems]
The present inventors have conducted intensive research on an apparatus capable of sampling and analyzing a sample made of a liquefied gas or a composition containing a liquefied gas in a liquid state, and as a result, controlled the temperature at which the sample can be turned into a liquid state. By installing a pressure-resistant pipe that can convert the sample into a liquid state and a sampling device that can sample the sample in a liquid state in a cooled low-temperature bath, a liquefied gas or a composition containing a liquefied gas is manufactured. The inventors have found that facilities and storage facilities can be easily and effectively monitored and controlled online, and have reached the present invention.
[0006]
That is, the present invention relates to a liquefied gas online analysis system described in (1) and (2), in which a sample made of a liquefied gas or a composition containing a liquefied gas is sampled and analyzed online in a liquid state.
(1) A liquefied gas online analysis system comprising a device capable of sampling a sample made of a liquefied gas or a composition containing a liquefied gas in a liquid state, and an analyzer capable of analyzing the sample.
(2) In an apparatus capable of sampling a sample made of a liquefied gas or a composition containing a liquefied gas in a liquid state, the sample is placed in a low-temperature bath controlled at a temperature at which the sample can be turned into a liquid state. The liquefied gas online analysis system according to (1), further comprising a pipe capable of maintaining a pressure capable of bringing the liquid state, and a sampling device capable of sampling the sample in a liquid state.
[0007]
BEST MODE FOR CARRYING OUT THE INVENTION
The apparatus of the present invention has a low-temperature tank whose temperature is controlled so that a sample made of a liquefied gas or a composition containing a liquefied gas can be kept in a liquid state, a pressure-resistant pipe disposed in the low-temperature tank, and a sampling device. (FIG. 1). The sampled liquid sample is introduced into a nearby analyzer outside the low-temperature chamber, such as a gas chromatograph, a liquid chromatograph, or a Karl Fischer moisture meter, and analyzed.
[0008]
【Example】
Hereinafter, examples of the present invention will be described, but the present invention is not limited thereto. Example 1
In an apparatus for producing dimethyl ether (boiling point -23.6 ° C.) as a liquefied gas, the apparatus of the present invention was used to measure the product composition online. A sample pipe cooled by a brine attached to a product tank as a bypass line for sampling is connected to a pressure-resistant pipe (withstand pressure of 2 MPa) in a low-temperature tank (-10 ° C to 5 ° C) capable of controlling temperature and a sampling device. The sampling cock in the sampling device is operated at a necessary timing (a short time interval when the device fluctuates, and a long time interval when the device is stable) by circulating a part of the circulating reaction mixture. A 50 μl sample was sampled, and this liquid sample was introduced into a nearby analytical gas chromatograph (GC-14B series manufactured by Shimadzu Corporation) for analysis. In another system, a sample sampled in the same manner was introduced into a liquid chromatograph (L-7000 series manufactured by Hitachi, Ltd.) adjacent to the low-temperature bath and analyzed.
[0009]
【The invention's effect】
The apparatus of the present invention enables a sample made of a liquefied gas or a composition containing a liquefied gas to be handled online in a liquid state, eliminating the need for the sample to be gasified in advance as in the related art, and accompanying the analytical measurement. It is possible to simplify the apparatus and the process and eliminate the problem of discarding the surplus sample.
[Brief description of the drawings]
FIG. 1 shows a system of the present invention.
1: Low temperature tank 2: Sampling device 3: Analysis device

Claims (2)

液化ガス又は液化ガスを含有する組成物からなる試料を液体の状態でサンプリングできる装置、及び該試料を分析できる分析装置から構成される、液化ガスオンライン分析システム。A liquefied gas online analysis system comprising a device capable of sampling a sample made of a liquefied gas or a composition containing a liquefied gas in a liquid state, and an analyzer capable of analyzing the sample. 液化ガス又は液化ガスを含有する組成物からなる試料を液体の状態でサンプリングできる装置において、該試料を液体の状態にすることができる温度にコントロールされた低温槽内に、該試料を液体の状態にすることができる圧力を維持できる配管、及び該試料を液体の状態でサンプリングできるサンプリング装置を設置してある、請求項1記載の液化ガスオンライン分析システム。In a device capable of sampling a sample made of a liquefied gas or a composition containing a liquefied gas in a liquid state, the sample is placed in a low-temperature bath controlled at a temperature capable of bringing the sample into a liquid state. The liquefied gas online analysis system according to claim 1, further comprising a pipe capable of maintaining a pressure capable of controlling the pressure, and a sampling device capable of sampling the sample in a liquid state.
JP2003072156A 2003-03-17 2003-03-17 Liquefied gas online analysis system Pending JP2004279260A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009020031A (en) * 2007-07-13 2009-01-29 Taiyo Nippon Sanso Corp Liquefied gas sampling container
CN104865043A (en) * 2015-05-07 2015-08-26 中国石油大学(华东) Liquefied natural gas (LNG) low-temperature flowing characteristic experimental device
CN105043817A (en) * 2015-06-04 2015-11-11 中国科学院上海应用物理研究所 Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution
CN113759075A (en) * 2021-10-13 2021-12-07 山东京博石油化工有限公司 Method for detecting water content of 1-octene used for POE production

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009020031A (en) * 2007-07-13 2009-01-29 Taiyo Nippon Sanso Corp Liquefied gas sampling container
CN104865043A (en) * 2015-05-07 2015-08-26 中国石油大学(华东) Liquefied natural gas (LNG) low-temperature flowing characteristic experimental device
CN104865043B (en) * 2015-05-07 2017-03-15 中国石油大学(华东) A kind of LNG cold flow characteristics experimental provision
CN105043817A (en) * 2015-06-04 2015-11-11 中国科学院上海应用物理研究所 Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution
CN113759075A (en) * 2021-10-13 2021-12-07 山东京博石油化工有限公司 Method for detecting water content of 1-octene used for POE production

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