JP2004093372A - Online automatic gas chromatographic measurement apparatus for formalin - Google Patents

Online automatic gas chromatographic measurement apparatus for formalin Download PDF

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Publication number
JP2004093372A
JP2004093372A JP2002255297A JP2002255297A JP2004093372A JP 2004093372 A JP2004093372 A JP 2004093372A JP 2002255297 A JP2002255297 A JP 2002255297A JP 2002255297 A JP2002255297 A JP 2002255297A JP 2004093372 A JP2004093372 A JP 2004093372A
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JP
Japan
Prior art keywords
formalin
sample
gas chromatograph
hot water
switching device
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP2002255297A
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Japanese (ja)
Inventor
Katsue Chikamatsu
親松 勝栄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Gas Chemical Co Inc
Original Assignee
Mitsubishi Gas Chemical Co Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Gas Chemical Co Inc filed Critical Mitsubishi Gas Chemical Co Inc
Priority to JP2002255297A priority Critical patent/JP2004093372A/en
Publication of JP2004093372A publication Critical patent/JP2004093372A/en
Pending legal-status Critical Current

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Abstract

<P>PROBLEM TO BE SOLVED: To provide an automatic gas chromatographic measurement apparatus for formalin measurement capable of efficiently measuring online formalin-containing samples sampled from the sampling positions of a formalin reaction device and continuously fed via flow passage pipes. <P>SOLUTION: A gas chromatograph is provided with a sample select device having both a flow passage switching device for automatically taking the formalin-containing samples into the gas chromatograph and a device for flowing hot water into the flow passage pipes on the downstream side of the the flow passage switching device. The pipes are heated and washed by using the sample select device to prevent the deposition of the sample components from blocking the pipes and affecting the next measurement values. <P>COPYRIGHT: (C)2004,JPO

Description

【0001】
【発明の属する技術分野】
本発明は、ホルマリン反応装置の各サンプリング箇所から採取され、各流路配管を経由して連続して送られて来るホルマリン含有サンプルを、流路切り替え装置を用いて自動的にガスクロマトグラフ中に取り込み測定するホルマリン測定用のオンライン自動ガスクロ測定装置に関するものである。
【0002】
【従来の技術】
従来、オンラインによるホルマリンのガスクロ測定装置は、サンプル配管の保温に電熱ヒーター等を使用し外部から加熱する方法がとられていた。しかしながら、このような方法では、配管の加温が十分になされていないとホルマリンの多量体の析出などによる閉塞トラブルが起きてしまい、いったん配管が詰まるとその洗浄が大変で高濃度サンプルでは特に注意が必要であった。また、各サンプリング箇所から送られて来るホルマリン含有サンプルが、ホルマリンの濃度やその他の成分の組成および濃度を異にする多様なものであるため、測定実施毎に前回測定の影響を除くため時間を掛けて置換する必要があり、置換不足のケースも多く、多頻度での測定を阻む要因ともなっていた。
【0003】
【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、ホルマリン反応装置の各箇所より採取された多流路オンラインサンプルを自動的に分析するガスクロ測定装置を提供することにある。
【0004】
【課題を解決するための手段】
本発明者は、ホルマリン反応装置より採取したホルマリン含有サンプルを自動的に精度良くオンラインで分析するガスクロ測定装置について鋭意研究を重ねた結果、該ガスクロ装置に、流路切り替え装置からサンプル注入器2までの配管及びサンプル注入器2に加温と洗浄のために温水を流すことができ、サンプル切り換えの間に温水を流す動作をするサンプルセレクト装置を付帯させ、内部に35℃以上、100℃未満の温水を流しすことで、従来の装置外部から加熱する方法を用いた場合よりも析出トラブルが少なく効率的にホルマリン濃度の測定を行うことができることを見い出した。また、装置内部に当該温度範囲の温水を流すことによって、サンプルセレクト装置からサンプル注入器までの配管及び注入器の洗浄も兼ねることができるため、サンプリング流路の置換不足に伴なう次回測定値への影響も解消できることを見い出し本発明に到達した。
【0005】
本発明は、(1)ガスクロマトグラフ1、ホルマリン含有サンプルを該ガスクロマトグラフ1に注入するサンプル注入器2、ホルマリン反応装置の各サンプリング箇所から各流路配管を経由して連続して送られて来るホルマリン含有サンプルを自動的に該ガスクロマトグラフ1内に取り込むための流路切り換え装置と該流路切り替え装置以降の各流路配管内に温水を流す装置を有するサンプルセレクト装置3、各駆動部を制御するプログラムコントローラー4、計測演算制御ユニット5から構成されることを特徴とする、ホルマリンのオンライン自動ガスクロ測定装置、(2)サンプルセレクト装置3が、サンプル析出と次回測定値への影響が生じないように、流路切り替え装置からサンプル注入器2までの配管及びサンプル注入器2に加温と洗浄のために温水を流すことができ、サンプル切り換えの間に温水を流す動作をする装置である、(1)記載のホルマリンのオンライン自動ガスクロ測定装置に関するものである。
【0006】
【発明の実施の形態】
本発明は、ホルマリン反応装置の工程監視のために用いるガスクロマト法によるオンライン自動分析装置に関する。ホルマリン装置の各サンプリング箇所につながる複数個の流路を経由し連続して送られて来る多流路オンラインサンプルを、サンプル流路の切り換えや内部に温水を流せるサンプルセレクト装置3を通じて、サンプルをガスクロマトグラフに注入するサンプル注入器2へ導入して、ガスクロマトグラフで分析する自動ガスクロ分析装置である。
【0007】
オンラインで分析するホルマリン含有サンプル中に含まれるホルマリン濃度は、高濃度から低濃度まで多種にわたるので、サンプル自体の温度が下がるとサンプル中に含まれるホルマリン多量体の析出などによる閉塞トラブルが増加するので、サンプル温度を下げない工夫が必要である。また高濃度から低濃度まで混在するサンプル中のホルマリン濃度を精度良く測定するためには、流路配管内の置換を充分行わないと高濃度の影響が生じて正確な分析ができない。温水の通液は、サンプル置換の効果をあげるために、測定毎にサンプル置換を行う際に実施することによって、加温と同時に前サンプルを洗浄することができる。このように、本発明の装置は、オンラインによるホルマリン反応装置の工程監視装置として好適に用いられるガスクロ法による自動測定システムである。
【0008】
【発明の効果】
本発明の装置及び方法を用いることにより、サンプルリング配管の閉塞や配管内残留成分による測定値への妨害を回避できるため、ホルマリン反応装置の各部より採取したサンプルをオンラインで自動的に多頻度かつ速い応答速度で計測することが可能となり、工業的に大変有用である。
【図面の簡単な説明】
【図1】本発明の測定装置
【符号の説明】
1:ガスクロマトグラフ
2:サンプル注入器
3:サンプルセレクト装置
4:プログラムコントローラー
5:計測演算制御ユニット
[0001]
TECHNICAL FIELD OF THE INVENTION
According to the present invention, a formalin-containing sample that is collected from each sampling point of a formalin reaction apparatus and continuously sent through each flow path pipe is automatically taken into a gas chromatograph using a flow path switching device. The present invention relates to an online automatic gas chromatograph for measuring formalin to be measured.
[0002]
[Prior art]
Conventionally, an on-line formalin gas chromatograph has been used in which a sample pipe is heated externally using an electric heater or the like to keep the temperature of the sample pipe. However, in such a method, if the piping is not sufficiently heated, blockage troubles such as precipitation of formalin multimers may occur. Was needed. In addition, since the formalin-containing samples sent from each sampling point are various with different concentrations of formalin and other components, the time required to remove the influence of the previous measurement must be taken each time measurement is performed. It is necessary to multiply and replace, and in many cases, replacement is insufficient, which has been a factor that hinders frequent measurement.
[0003]
[Problems to be solved by the invention]
An object of the present invention is to solve the above-mentioned problems in the prior art, and to provide a gas chromatograph that automatically analyzes a multi-channel online sample collected from each part of a formalin reactor.
[0004]
[Means for Solving the Problems]
The present inventor has conducted intensive studies on a gas chromatograph that automatically and accurately analyzes a formalin-containing sample collected from a formalin reactor on-line. As a result, the gas chromatograph has a flow path switching device to a sample injector 2. Hot water for heating and washing can be supplied to the piping and the sample injector 2 and a sample select device for performing the operation of flowing the hot water during the sample switching is provided. It has been found that, by flowing hot water, formalin concentration can be measured more efficiently with less precipitation trouble than when a conventional method of heating from outside the apparatus is used. In addition, by flowing hot water within the temperature range within the device, the piping from the sample select device to the sample injector and the injector can also be washed, so that the next measurement value due to insufficient replacement of the sampling flow path. The present inventors have found that the influence of the present invention can be eliminated, and reached the present invention.
[0005]
The present invention provides (1) a gas chromatograph 1, a sample injector 2 for injecting a formalin-containing sample into the gas chromatograph 1, and a continuous feed from each sampling point of a formalin reactor via each flow path pipe. The sample select device 3 having a channel switching device for automatically taking the formalin-containing sample into the gas chromatograph 1 and a device for flowing hot water into each channel pipe after the channel switching device, and controls each drive unit. A formalin on-line automatic gas chromatograph measuring device, which is composed of a program controller 4 and a measurement calculation control unit 5 so that the sample selection device 3 does not affect sample deposition and the next measurement value. In addition, the piping from the flow path switching device to the sample injector 2 and the sample injector 2 are heated. For cleaning can flow hot water, it is a device that operates to flow a hot water between the sample switching relates Automatic online gas chromatography measuring apparatus formalin according (1).
[0006]
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention relates to an on-line automatic analyzer by a gas chromatography method used for monitoring a process of a formalin reactor. A multi-channel online sample that is continuously sent through a plurality of channels connected to each sampling point of the formalin device is subjected to gas chromatography through a sample selection device 3 that can switch sample channels and flow hot water inside. This is an automatic gas chromatograph which is introduced into a sample injector 2 for injecting into a chromatograph and is analyzed by a gas chromatograph.
[0007]
The concentration of formalin contained in formalin-containing samples to be analyzed online varies from high to low, so if the temperature of the sample itself drops, clogging problems due to precipitation of formalin multimers contained in the sample will increase. It is necessary to devise a method that does not lower the sample temperature. In addition, in order to accurately measure the formalin concentration in a sample mixed from a high concentration to a low concentration, if the replacement in the flow path piping is not sufficiently performed, the effect of the high concentration occurs and accurate analysis cannot be performed. The hot water is passed when the sample replacement is performed for each measurement in order to increase the effect of the sample replacement, so that the previous sample can be washed at the same time as the heating. As described above, the apparatus of the present invention is an automatic measurement system by a gas chromatography method which is suitably used as an on-line process monitor of a formalin reaction apparatus.
[0008]
【The invention's effect】
By using the apparatus and method of the present invention, it is possible to avoid clogging of the sampling pipe and interference with measured values due to residual components in the pipe, so that samples collected from each part of the formalin reactor are automatically and frequently used online and frequently. Measurement can be performed at a high response speed, which is very useful industrially.
[Brief description of the drawings]
FIG. 1 is a measurement apparatus of the present invention.
1: gas chromatograph 2: sample injector 3: sample selector 4: program controller 5: measurement operation control unit

Claims (2)

ガスクロマトグラフ1、ホルマリン含有サンプルを該ガスクロマトグラフ1に注入するサンプル注入器2、ホルマリン反応装置の各サンプリング箇所から各流路配管を経由して連続して送られて来るホルマリン含有サンプルを自動的に該ガスクロマトグラフ1内に取り込むための流路切り換え装置と該流路切り替え装置以降の各流路配管内に温水を流す装置を有するサンプルセレクト装置3、各駆動部を制御するプログラムコントローラー4、計測演算制御ユニット5から構成されることを特徴とする、ホルマリンのオンライン自動ガスクロ測定装置A gas chromatograph 1, a sample injector 2 for injecting a formalin-containing sample into the gas chromatograph 1, and a formalin-containing sample that is continuously sent from each sampling point of a formalin reactor via each flow path pipe are automatically generated. A sample select device 3 having a channel switching device for taking in the gas chromatograph 1 and a device for flowing hot water into each channel pipe after the channel switching device, a program controller 4 for controlling each drive unit, measurement calculation A formalin automatic gas chromatograph measuring apparatus characterized by comprising a control unit 5. サンプルセレクト装置3が、サンプル析出と次回測定値への影響が生じないように、流路切り替え装置からサンプル注入器2までの配管及びサンプル注入器2に加温と洗浄のために温水を流すことができ、サンプル切り換えの間に温水を流す動作をする装置である、請求項1記載のホルマリンのオンライン自動ガスクロ測定装置。Flowing hot water for heating and washing in the pipe from the flow path switching device to the sample injector 2 and the sample injector 2 so that the sample select device 3 does not affect sample deposition and the next measurement value. The formalin on-line automatic gas chromatograph measuring apparatus according to claim 1, wherein the apparatus performs an operation of flowing hot water during sample switching.
JP2002255297A 2002-08-30 2002-08-30 Online automatic gas chromatographic measurement apparatus for formalin Pending JP2004093372A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2002255297A JP2004093372A (en) 2002-08-30 2002-08-30 Online automatic gas chromatographic measurement apparatus for formalin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2002255297A JP2004093372A (en) 2002-08-30 2002-08-30 Online automatic gas chromatographic measurement apparatus for formalin

Publications (1)

Publication Number Publication Date
JP2004093372A true JP2004093372A (en) 2004-03-25

Family

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