JP5042918B2 - 絶縁油中のポリ塩化ビフェニル類の分析方法及び分析装置 - Google Patents
絶縁油中のポリ塩化ビフェニル類の分析方法及び分析装置 Download PDFInfo
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2835—Specific substances contained in the oils or fuels
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G01N2030/143—Preparation by elimination of some components selective absorption
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
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Description
(1)絶縁油中のポリ塩化ビフェニル類の濃度を測定するポリ塩化ビフェニル類の分析方法であって、前処理として、ジビニルベンゼン及びメタクリレート系有機モノマーをモノマー成分として含む共重合体の粒子に、ポリ塩化ビフェニル類を含む絶縁油を接触させ、絶縁油中のポリ塩化ビフェニル類と不純物である油分とを分離する工程を含む前記分析方法。
(2)メタクリレート系有機モノマーが、ジオール型水酸基又はジオール型水酸基に変換可能な基を有する前記(1)に記載のポリ塩化ビフェニル類の分析方法。
(3)絶縁油中のポリ塩化ビフェニル類の濃度を測定するための分析装置であって、ジビニルベンゼン及びメタクリレート系有機モノマーをモノマー成分として含む共重合体の粒子が充填された容器を備え、該容器にポリ塩化ビフェニル類を含む絶縁油を通過させることにより該絶縁油中のポリ塩化ビフェニル類と不純物である油分とを分離する分離精製部と、該分離精製部を経た絶縁油についてポリ塩化ビフェニル類の濃度を測定する分析部とを有する前記分析装置。
(4)メタクリレート系有機モノマーが、ジオール型水酸基又はジオール型水酸基に変換可能な基を有する前記(3)に記載のポリ塩化ビフェニル類の分析装置。
(5)容器が、固相抽出用の容器又は液体クロマトグラフに用いる分離カラムである前記(3)又は(4)に記載のポリ塩化ビフェニル類の分析装置。
(6)容器が、液体クロマトグラフに用いる分離カラムであり、該容器に対して溶離液を循環送液するためのリサイクル用バルブを備え、絶縁油から油分が十分に分離されるまでリサイクル送液するように構成された前記(3)〜(5)のいずれかに記載のポリ塩化ビフェニル類の分析装置。
(7)分析部が、ポリ塩化ビフェニル類を保持するためのトラップカラムと、該トラップカラムにポリ塩化ビフェニル類を分取し、濃縮するための第1の切替バルブと、トラップカラムから脱離させたポリ塩化ビフェニル類をガスクロマトグラフに導入するための第2の切替バルブとを有する前記(3)〜(6)のいずれかに記載のポリ塩化ビフェニル類の分析装置。
(8)ヘリウムガスをトラップカラムに流し、トラップカラム中に残存する溶離液及び水分を除去する前記(7)に記載のポリ塩化ビフェニル類の分析装置。
(実施例1)
図2は、ジビニルベンゼン及びメタクリレート系有機ポリマーを含む共重合体の粒子からなる前処理剤を充填したカラムである。ネジ式カラムエンド1によりパイプ2の両端を密閉し、パイプ2内に充填してある前処理剤3を空隙がないように閉じ込めてある。絶縁油試料中に不純物として粒子が混入している場合に、その粒子が前処理剤3の層に混入しないよう、パイプ2の両端にはフィルター4を使用している。これに対し、液体クロマトグラフに接続するために作られているチューブ接続用ネジ穴5を通して前処理剤3に液体が流れ込む。
図6は、実施例2における絶縁油中のPCB分析の操作フローである。この例はクリーンアップ前の油分分解処理と濃縮処理を行わず、絶縁油試料の秤量からガスクロマトグラフ測定までの全工程を自動で行うものである。図7はこれを行なうための絶縁油中のPCB分析装置の概略構成図であり、特に絶縁油中のPCB類と油分とを分離する分離精製部を示している。図8は、絶縁油中のPCB分析装置の、特に分離精製部を経た絶縁油中のPCB濃度を測定する分析部を示す概略構成図である。
さらに別の例として、液体クロマトグラフを使用せずにクリーンアップを行う方法について説明する。ジビニルベンゼン及びメタクリレート系有機モノマーをモノマー成分として含む共重合体の粒子からなる前処理剤を、適当な溶媒とともにビーカーなどガラス容器に入れ、ここに絶縁油試料を加え、一定時間、一定温度にて攪拌することにより試料中のPCBのみを前処理剤に保持させる。その後、ろ過により前処理剤を分離し、PCBを前処理剤から脱離させるための溶媒で処理することによりPCBを回収し測定する。または加熱によりPCBを回収し測定を行う。
2 パイプ
3 前処理剤
4 フィルター
5 チューブ接続用ネジ穴
6 溶離液
7 リサイクル用バルブ
8 ポンプ
9 オートサンプラー
10 クリーンアップ用カラム
11 分離判定検出器
12 リサイクル用バルブ制御部
13 フラクションコレクター
14 加熱脱離装置
15 GC/MS装置
16 リサイクル機能付き液体クロマトグラフ
17 六方バルブ
18 四方バルブ
19 トラップカラム
Claims (6)
- 絶縁油中のポリ塩化ビフェニル類の濃度を測定するポリ塩化ビフェニル類の分析方法であって、前処理として、ジビニルベンゼン及びメタクリレート系有機モノマーをモノマー成分として含む共重合体の粒子に、ポリ塩化ビフェニル類を含む絶縁油を接触させ、絶縁油中のポリ塩化ビフェニル類と不純物である油分とを分離する工程を含み、前記メタクリレート系有機モノマーがジオール型水酸基を有する前記分析方法。
- 絶縁油中のポリ塩化ビフェニル類の濃度を測定するための分析装置であって、ジビニルベンゼン及びメタクリレート系有機モノマーをモノマー成分として含む共重合体の粒子が充填された容器を備え、該容器にポリ塩化ビフェニル類を含む絶縁油を通過させることにより該絶縁油中のポリ塩化ビフェニル類と不純物である油分とを分離する分離精製部と、該分離精製部を経た絶縁油についてポリ塩化ビフェニル類の濃度を測定する分析部とを有し、前記メタクリレート系有機モノマーがジオール型水酸基を有する前記分析装置。
- 容器が、固相抽出用の容器又は液体クロマトグラフに用いる分離カラムである請求項2に記載のポリ塩化ビフェニル類の分析装置。
- 容器が、液体クロマトグラフに用いる分離カラムであり、該容器に対して溶離液を循環送液するためのリサイクル用バルブを備え、絶縁油から油分が十分に分離されるまでリサイクル送液するように構成された請求項2又は3に記載のポリ塩化ビフェニル類の分析装置。
- 分析部が、ポリ塩化ビフェニル類を保持するためのトラップカラムと、該トラップカラムにポリ塩化ビフェニル類を分取し、濃縮するための第1の切替バルブと、トラップカラムから脱離させたポリ塩化ビフェニル類をガスクロマトグラフに導入するための第2の切替バルブとを有する請求項2〜4のいずれかに記載のポリ塩化ビフェニル類の分析装置。
- ヘリウムガスをトラップカラムに流し、トラップカラム中に残存する溶離液及び水分を除去する請求項5に記載のポリ塩化ビフェニル類の分析装置。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2008135013A JP5042918B2 (ja) | 2008-05-23 | 2008-05-23 | 絶縁油中のポリ塩化ビフェニル類の分析方法及び分析装置 |
US12/994,300 US8562910B2 (en) | 2008-05-23 | 2009-05-20 | Method and apparatus for analysis of poly (biphenyl chloride) in electrical insulating oil |
CN200980118693.1A CN102037353B (zh) | 2008-05-23 | 2009-05-20 | 绝缘油中的多氯联苯类的分析方法及分析装置 |
PCT/JP2009/059256 WO2009142232A1 (ja) | 2008-05-23 | 2009-05-20 | 絶縁油中のポリ塩化ビフェニル類の分析方法及び分析装置 |
DE112009001241T DE112009001241T5 (de) | 2008-05-23 | 2009-05-20 | Verfahren und Vorrichtung zur Analyse von Poly(biphenylchlorid) in elektrischem Isolieröl |
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JP5333941B2 (ja) * | 2010-02-04 | 2013-11-06 | 平沼産業株式会社 | 固相抽出装置 |
JP5546644B2 (ja) * | 2010-11-26 | 2014-07-09 | 株式会社日立ハイテクノロジーズ | 油中のポリ塩化ビフェニルの分析方法 |
JP5639513B2 (ja) * | 2011-03-23 | 2014-12-10 | 一般財団法人電力中央研究所 | Pcb抽出装置、並びにこれを用いた、pcb検出装置及びpcb検出方法 |
FR2988620B1 (fr) * | 2012-03-29 | 2014-04-25 | Commissariat Energie Atomique | Dispositif et procede d'extraction de composes contenus dans un echantillon liquide en vue de leur analyse |
CN103194307B (zh) * | 2013-03-14 | 2014-08-27 | 吉林省电力有限公司电力科学研究院 | 循环萃取法分离绝缘油中多氯联苯 |
JP2015224895A (ja) * | 2014-05-26 | 2015-12-14 | 有限会社シマムラテック | 液体クロマトグラフィーにおけるリサイクル分取方法 |
CN215115863U (zh) * | 2020-12-10 | 2021-12-10 | 国网上海市电力公司 | 变压器植物绝缘油中抗氧化剂含量的检测装置 |
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JP4065090B2 (ja) | 1999-09-10 | 2008-03-19 | 財団法人化学物質評価研究機構 | Pcb簡易測定装置 |
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US8562910B2 (en) | 2013-10-22 |
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US20110126609A1 (en) | 2011-06-02 |
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WO2009142232A1 (ja) | 2009-11-26 |
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