JPS6130767A - Measurement for concentration of ethyleneglycol - Google Patents

Measurement for concentration of ethyleneglycol

Info

Publication number
JPS6130767A
JPS6130767A JP15342184A JP15342184A JPS6130767A JP S6130767 A JPS6130767 A JP S6130767A JP 15342184 A JP15342184 A JP 15342184A JP 15342184 A JP15342184 A JP 15342184A JP S6130767 A JPS6130767 A JP S6130767A
Authority
JP
Japan
Prior art keywords
tube
concentration
reaction tube
formaldehyde
reaction
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
JP15342184A
Other languages
Japanese (ja)
Inventor
Tsutomu Kikuta
菊田 勉
Koji Uzawa
鵜沢 孝次
Kuniaki Matsunobu
邦明 松延
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.)
Tokyo Gas Co Ltd
Gastec Corp
Original Assignee
Tokyo Gas Co Ltd
Gastec Corp
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 Tokyo Gas Co Ltd, Gastec Corp filed Critical Tokyo Gas Co Ltd
Priority to JP15342184A priority Critical patent/JPS6130767A/en
Publication of JPS6130767A publication Critical patent/JPS6130767A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Biophysics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

PURPOSE:To measure the concentration of ethyleneglycol in a conduit handily and quickly, by oxidizing ethyleneglycol in a gas for color reaction of the resulting aldehyde to measure the concentration thereof depending on the length of the colored layer thereof. CONSTITUTION:A measuring apparatus is so arranged to oxidize ethyleneglycol to form formaldehyde. For example, it is made up of a reaction tube 1 holding an oxidizing agent 2 comprising sodium periodate, an assay tube 4 holding a detection agent 5 comprising hydroxylaminephosphate, for instance, which detects and causes a color reaction of formaldehyde, a connection tube 7 and a gas sampler. Then, the reaction tube 1 is connected to an errect tube 10 of a conduit 9 through a connection tube 11. A sample gas is oxidized with the reaction tube 1 to form formaldehyde which is colored with the assay tube 4. Thus, the length of the resulting colored layer is measured to facilitate the measurement of the concentration of ethyleneglycol.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は都市ガス供給用等の導管に於いて、その接合部
に於けるガス漏洩を防止するために用いるエチレングリ
コールの濃度測定方法に関するものである。
Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for measuring the concentration of ethylene glycol used to prevent gas leakage at joints in pipes for supplying city gas, etc. It is.

(従来の技術およびその問題点) 都市ガス供給用等の導管に於いて、麻をパツキンとして
用いた接合部からのガスの漏洩を防止するだめに、導管
内にエチレングリコールを注入し、前記パツキンをこの
エチレングリコールで一定に湿らせておくことが行なわ
れており、そこでエチレングリコール蒸気が一定濃度以
上かどうかを導管の一定間隔毎に測定する必要がある。
(Prior art and its problems) In order to prevent gas leakage from the joints of city gas supply pipes using hemp as packing, ethylene glycol is injected into the pipes and the packing is made of hemp. The conduit is kept constantly moistened with this ethylene glycol, and it is necessary to measure whether the ethylene glycol vapor is above a certain concentration at regular intervals along the conduit.

従来、かかるエチレングリコール蒸気の濃度測定には機
器分析、特にガスクロマトグラフィーが主に使われてい
るが、この方法ではサンプリングから濃度測定までの操
作に時間と熟練を要し、また携帯用としての持運びが不
可能である等、簡便性並びに迅速性に欠け、また高価で
あるという欠点がある。
Conventionally, instrumental analysis, particularly gas chromatography, has been mainly used to measure the concentration of ethylene glycol vapor, but this method requires time and skill from sampling to concentration measurement, and is not portable. It has drawbacks such as being unable to be carried, lacking in simplicity and speed, and being expensive.

本発明は以上の従来の欠点を解消し、導管内のエチレン
グリコール濃度の測定を簡便に、しかも迅速に行なえる
ようにすることを目的とするものである。以下詳述する
と次の通りである。
It is an object of the present invention to overcome the above-mentioned conventional drawbacks and to make it possible to measure the ethylene glycol concentration in a conduit simply and quickly. The details are as follows.

(発明の構成および作用) 符号1は反応管であり、該反応管1中にはエチレングリ
コールを酸化してホルムアルデヒドを生成する酸化剤2
を保持する。酸化剤2としてば倒えば過ヨウ素酸ナトリ
ウム〔NaIO4) 、過ヨウ素酸カリウム〔K工04
〕、過マンガン酸カリウム〔KMnO4〕等の溶液をシ
リカゾル、活性アルミナ等の担体に吸着し乾燥させたも
のを用いる。そして反応管1はこの酸化剤20両端側を
例えば多孔質プラスチック、綿、グラスウール、金網等
の通気性隔壁3で保持し、管体の両端を溶封等によって
封止して保存する。4は定量管であり、該定量管4中に
はホルムアルデヒドを検知して呈色する検知剤5を保持
する。検知剤5としては例えばリン酸ヒドロキシルアミ
ン〔(NH2OH)3・H3P0. ]、クフロモトロ
ブ(C10H6”a208S2 ・2 H20]等の溶
液をシリカゾル、ケイ砂、″ガラス粒、アルミナ等の担
体に吸着し乾燥させたものに適宜の呈色試薬を加えたも
のを用いる。そして定量管4は、かかる検知剤5を透明
な管体に入れ、反応管1と同様な通気性隔壁6で該検知
剤50両端側を保持し、管体の両端を溶封等によって封
止して保存する。
(Structure and operation of the invention) Reference numeral 1 denotes a reaction tube, and in the reaction tube 1 there is an oxidizing agent 2 that oxidizes ethylene glycol to produce formaldehyde.
hold. Oxidizing agent 2 is sodium periodate [NaIO4], potassium periodate [K-04]
], a solution of potassium permanganate [KMnO4] or the like is adsorbed onto a carrier such as silica sol or activated alumina and dried. The reaction tube 1 is stored by holding both ends of the oxidizing agent 20 with air-permeable partition walls 3 made of porous plastic, cotton, glass wool, wire gauze, etc., and sealing both ends of the tube by melt sealing or the like. 4 is a quantitative tube, and the quantitative tube 4 holds a detection agent 5 that detects formaldehyde and develops a color. As the detection agent 5, for example, hydroxylamine phosphate [(NH2OH)3.H3P0. ], Kufuromotolob (C10H6"a208S2 ・2H20), etc. is adsorbed onto a carrier such as silica sol, silica sand, "glass grains, alumina, etc. and dried, and an appropriate coloring reagent is added to the solution.Then, quantitative determination is performed. The tube 4 is constructed by putting the detecting agent 5 in a transparent tube body, holding both ends of the detecting agent 50 with an air-permeable partition wall 6 similar to that of the reaction tube 1, and sealing both ends of the tube body by melt sealing or the like. save.

かかる構成に於いて本発明は、使用時に前記反応管1と
定量管4の両端を開口し、該反応管1のm個aと定量管
4の一側a′を例えばシリコンゴムいて該ガス採取器8
により導管9内のガスを採取する。かかるサンプルガス
の採取は例えば導管9の適所に設けた立管10に接続管
11を介して反応管1の他側すを接続することにより容
易に行なうことができる。
In such a configuration, the present invention opens both ends of the reaction tube 1 and the quantitative tube 4 during use, and connects the m pieces a of the reaction tube 1 and one side a' of the quantitative tube 4 with silicone rubber, for example, to collect the gas. Vessel 8
The gas inside the conduit 9 is sampled. Such sampling of the sample gas can be easily carried out, for example, by connecting the other side of the reaction tube 1 to a standpipe 10 provided at an appropriate position of the conduit 9 via a connecting tube 11.

しかしてサンプルガスは反応管1、定量管4を順次通過
してガス採取器8に至るのであるが、ガス中のエチレン
グリコールは反応管1を通過する際、酸化剤2で酸化さ
れ、ホルムアルデヒドが生成する。例えば酸化剤として
過ヨウ素酸ナトリウム〔Na工04〕を用いた場合には
次反応式によりホルムアルデヒぜが生成する。
Thus, the sample gas passes through the reaction tube 1 and the metering tube 4 in order and reaches the gas sampling device 8. When the ethylene glycol in the gas passes through the reaction tube 1, it is oxidized by the oxidizing agent 2, and formaldehyde is generate. For example, when sodium periodate (Na-04) is used as an oxidizing agent, formaldehyde is produced according to the following reaction formula.

02H602+Na工04−→2HCHO+Na工03
+H20次いでこのホルムアルデヒドはサンプルガスと
共に定量管4を通過する際、検知剤5と反応して一側a
′から他側b′に向ってこれを呈色、即ち発色または変
色させる。例えば検知剤にリン酸ヒドロキシルアミン〔
(NH2OH)3・H3P04)を用いた場合には次反
応式により、リン酸が生成し、かかるリン酸により呈色
する前記呈色試薬により赤褐色に変色させろことができ
る。
02H602+Na work 04-→2HCHO+Na work 03
+H20 Next, when this formaldehyde passes through the metering tube 4 together with the sample gas, it reacts with the detection agent 5, and one side a
' to the other side b', that is, develops or changes color. For example, the detection agent is hydroxylamine phosphate [
(NH2OH)3.H3P04), phosphoric acid is produced according to the following reaction formula, and the color can be changed to reddish brown using the coloring reagent that is colored by the phosphoric acid.

3HOHO+(NH2OH)3・H3PO4→30H2
NOH−1−H3PO,−1−3H20このように本発
明は、サンプルガス中に含まれるエチレングリコールを
反応管1に於いて酸化してホルムアルデヒドを生成させ
、次いでかかるホルムアルデヒドにより定量管4の一側
a′から他側b′に向って呈色させるものであって、こ
の呈色層   ′の長さはホルムアルデヒドの濃度、即
ちサンプルガス中のエチレングリコールの濃度に対応す
るので、この呈色層の長さにより、かかる濃度を測定す
ることができる。この際、定量管4の管体に、予め既知
濃度のエチレングリコールを用いて反応させた場合の呈
色層の長さに対応して検量線を作成し、濃度目盛12を
設けておけば濃度を具体的数値として容易に確認するこ
とができる。
3HOHO+(NH2OH)3・H3PO4→30H2
NOH-1-H3PO, -1-3H20 Thus, in the present invention, ethylene glycol contained in a sample gas is oxidized in the reaction tube 1 to produce formaldehyde, and then one side of the quantitative tube 4 is oxidized with the formaldehyde. The length of this coloring layer ′ corresponds to the concentration of formaldehyde, that is, the concentration of ethylene glycol in the sample gas. Depending on the length, such concentration can be measured. At this time, if a calibration curve is prepared in advance in the tube body of the quantitative tube 4 corresponding to the length of the colored layer when reacting with ethylene glycol of a known concentration, and a concentration scale 12 is provided, the concentration can be easily confirmed as concrete numerical values.

以上の本発明を都市ガス供給用の導管に適用した場合に
は、保安上の目的で混入された付臭剤が前述の測定に妨
害を及ぼす場合がある。即ち、現在都市ガスの付臭剤と
しては、ターシャルブチルメルカプタン(TBM )や
テトラヒドロチオフェン(THT )等が広く用いられ
ているが、このうち特にTBMは分解して定量管4内の
反応に妨害を及ぼす。
When the present invention described above is applied to a city gas supply conduit, the odorant mixed in for security purposes may interfere with the above-mentioned measurement. That is, tertiary butyl mercaptan (TBM) and tetrahydrothiophene (THT) are currently widely used as odorants for city gas, but TBM in particular decomposes and interferes with the reaction inside the metering tube 4. effect.

かかる妨害は、反応管1に前記酸化剤と共にガス付臭剤
の除去剤を保持することにより防止することができる。
Such interference can be prevented by holding a gas odorant remover together with the oxidizing agent in the reaction tube 1.

例えばTBMに対する除去剤として塩化第2水銀(Hg
C12)を用いると、次反応式で示すように分解しない
安定な錯化合物 (((!H3)30E+ −Hg(!1 〕と塩酸とな
り、塩酸は担体のシリカゲル等に吸着され、定量管4に
於けるホルムアルデヒドの反応に妨害な及ぼさない。
For example, mercuric chloride (Hg) is used as a remover for TBM.
When C12) is used, as shown in the following reaction formula, a stable complex compound ((!H3)30E+ -Hg(!1 ) that does not decompose and hydrochloric acid is formed, and the hydrochloric acid is adsorbed on the carrier silica gel etc. It does not interfere with the reaction of formaldehyde in the process.

(C!H3)3C!SH+HgC!1□→(OH3)3
0S −Hg01−1− HC!1(発明の効果) 本発明は以上の通り、エチレングリコールの酸化反応と
、かかる酸化反応によって生成するホルムアルデヒドに
よる呈色反応を合理的に用いてエチレングリコール濃度
を定量するものであり、即ち反応管と定量管並びにガス
採取器やこれらを接続する接続管だけで測定することが
できるので、従来の機器分析に比較して遥かに安価で、
しかも簡便性、迅速性を備え、携帯用として少量のガス
採取量で容易に、しかも即座に所定の濃度測定を行なえ
るという大きな効果がある。このため広範囲での測定を
必要とする導管的測定用として最適である。しかも本発
明は簡単な構造のものを用いるので、性能維持のための
保守が容易で、故障等の発生も極少であるという利点も
ある。特に本発明は反応管と定量管を個別に構成してい
るので、これらを一体に構成するものと比較してそれら
中の物質相互の反応による不都合を効果的に防止し、正
確な反応と長期的な保存等を可能とする・という特徴が
ある。
(C!H3)3C! SH+HgC! 1□→(OH3)3
0S -Hg01-1- HC! 1 (Effects of the Invention) As described above, the present invention is for quantifying ethylene glycol concentration by rationally using the oxidation reaction of ethylene glycol and the coloring reaction caused by formaldehyde produced by the oxidation reaction. Since it can be measured using only a quantitative tube, a gas sampler, and a connecting tube that connects these, it is much cheaper than conventional instrumental analysis.
In addition, it is simple and quick, and has the great effect of being portable and allowing a predetermined concentration to be measured easily and immediately with a small amount of gas sampled. For this reason, it is ideal for pipe measurements that require measurement over a wide range. Moreover, since the present invention uses a simple structure, maintenance to maintain performance is easy, and there are also advantages in that the occurrence of failures and the like is minimized. In particular, in the present invention, since the reaction tube and the quantitative measurement tube are configured separately, compared to a configuration in which they are configured as one unit, inconveniences caused by reactions between the substances in them can be effectively prevented, and accurate reactions and long-term results can be achieved. It has the characteristic that it enables storage etc.

【図面の簡単な説明】[Brief explanation of the drawing]

第3図は測定状態説明図である。 符号1・・反応管、2・・酸化剤、3,6・通気性隔壁
、4・・・定量管、5・・検知剤、7・・・接続管、8
・・・採取器、9・・・導管、1o・立管、1・1・・
・接続管。
FIG. 3 is an explanatory diagram of the measurement state. Code 1: Reaction tube, 2: Oxidizing agent, 3, 6: Air permeable partition, 4: Quantitative tube, 5: Detecting agent, 7: Connecting tube, 8
...Collector, 9... Conduit, 1o Standpipe, 1.1...
・Connection pipe.

Claims (2)

【特許請求の範囲】[Claims] (1)エチレングリコールを酸化してホルムアルデヒド
を生成する酸化剤を保持、封止した反応管と、ホルムア
ルデヒドを検知して呈色する検知剤を保持、封止した定
量管を設け、使用時に前記反応管と定量管の両端を開口
し、該反応管の一側と定量管の一側を接続すると共に、
該定量管の他側にガス採取器を接続し、該ガス採取器に
より前記反応管の他端から所定量吸引したサンプルガス
を、まず該反応管を通過させ、ガス中のエチレングリコ
ールを酸化してホルムアルデヒドを生成させた後、定量
管を通過させて呈色させ、呈色層の長さにより濃度を測
定することを特徴とするエチレングリコールの濃度測定
方法
(1) A reaction tube that holds and seals an oxidizing agent that oxidizes ethylene glycol to produce formaldehyde, and a metering tube that holds and seals a detection agent that detects formaldehyde and develops a color, are installed, and the reaction tube is Opening both ends of the tube and the quantitative tube, and connecting one side of the reaction tube and one side of the quantitative tube,
A gas sampling device is connected to the other side of the metering tube, and a predetermined amount of sample gas sucked from the other end of the reaction tube by the gas sampling device is first passed through the reaction tube to oxidize the ethylene glycol in the gas. A method for measuring the concentration of ethylene glycol, which comprises: generating formaldehyde, passing it through a quantitative tube to develop a color, and measuring the concentration based on the length of the colored layer.
(2)エチレングリコールを酸化してホルムアルデヒド
を生成する酸化剤と共に、ガス付臭剤の除去剤を保持、
封止した反応管と、ホルムアルデヒドを検知して呈色す
る検知剤を保持、封止した定量管を設け、使用時に前記
反応管と定量管の両端を開口し、該反応管の一側と定量
管の一側を接続すると共に、該定量管の他側にガス採取
器を接続し、該ガス採取器により前記反応管の他端から
所定量吸引したサンプルガスを、まず該反応管を通過さ
せ、その中のエチレングリコールを酸化してホルムアル
デヒドを生成させると共に付臭剤を除去した後、定量管
に至らせて呈色させ、呈色層の長さにより濃度を測定す
ることを特徴とするエチレングリコールの濃度測定方法
(2) Holds an oxidizing agent that oxidizes ethylene glycol to produce formaldehyde, as well as a gaseous odorant remover;
A sealed reaction tube and a sealed quantitative tube holding a detection agent that detects formaldehyde and develops a color are provided, and when in use, both ends of the reaction tube and quantitative tube are opened, and one side of the reaction tube and the quantitative tube are connected. One side of the tube is connected, and a gas sampling device is connected to the other side of the metering tube, and a predetermined amount of sample gas sucked from the other end of the reaction tube by the gas sampling device is first passed through the reaction tube. , ethylene glycol is oxidized to produce formaldehyde, the odorant is removed, and then the ethylene is passed through a metering tube to develop a color, and the concentration is measured by the length of the colored layer. How to measure glycol concentration
JP15342184A 1984-07-24 1984-07-24 Measurement for concentration of ethyleneglycol Pending JPS6130767A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15342184A JPS6130767A (en) 1984-07-24 1984-07-24 Measurement for concentration of ethyleneglycol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15342184A JPS6130767A (en) 1984-07-24 1984-07-24 Measurement for concentration of ethyleneglycol

Publications (1)

Publication Number Publication Date
JPS6130767A true JPS6130767A (en) 1986-02-13

Family

ID=15562134

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15342184A Pending JPS6130767A (en) 1984-07-24 1984-07-24 Measurement for concentration of ethyleneglycol

Country Status (1)

Country Link
JP (1) JPS6130767A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6451860U (en) * 1987-09-29 1989-03-30

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5929749A (en) * 1982-08-12 1984-02-17 Honda Motor Co Ltd Compensating method of trouble detection in instrumental system of suction air quantity parameter sensor for internal-combustion engine
JPS5965763A (en) * 1982-10-08 1984-04-14 Gastec:Kk Measuring method of average concentration of carbon monoxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5929749A (en) * 1982-08-12 1984-02-17 Honda Motor Co Ltd Compensating method of trouble detection in instrumental system of suction air quantity parameter sensor for internal-combustion engine
JPS5965763A (en) * 1982-10-08 1984-04-14 Gastec:Kk Measuring method of average concentration of carbon monoxide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6451860U (en) * 1987-09-29 1989-03-30

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