JP2000180354A - Measuring method for harmful halogen compound by using surface plasmon resonance - Google Patents
Measuring method for harmful halogen compound by using surface plasmon resonanceInfo
- Publication number
- JP2000180354A JP2000180354A JP35988598A JP35988598A JP2000180354A JP 2000180354 A JP2000180354 A JP 2000180354A JP 35988598 A JP35988598 A JP 35988598A JP 35988598 A JP35988598 A JP 35988598A JP 2000180354 A JP2000180354 A JP 2000180354A
- Authority
- JP
- Japan
- Prior art keywords
- dioxins
- halogen compound
- harmful halogen
- dissolved
- plasmon resonance
- 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.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- 150000002366 halogen compounds Chemical class 0.000 title claims abstract description 20
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 title claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 150000002013 dioxins Chemical class 0.000 abstract description 23
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 15
- 239000007788 liquid Substances 0.000 abstract description 6
- 238000002835 absorbance Methods 0.000 abstract description 5
- 239000013307 optical fiber Substances 0.000 abstract description 5
- 238000005070 sampling Methods 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 10
- 239000000523 sample Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 101000650817 Homo sapiens Semaphorin-4D Proteins 0.000 description 1
- 102100027744 Semaphorin-4D Human genes 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- -1 dioxins) Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はゴミ焼却炉等を含む
各種の廃棄物の焼却施設や工場等で発生する排ガスや廃
液中、固体中に含まれる有害ハロゲン化合物のインライ
ン濃度計測装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an in-line measuring apparatus for the concentration of harmful halogen compounds contained in exhaust gas, waste liquid and solids generated in incinerators and factories of various wastes including refuse incinerators and the like.
【０００２】[0002]
【従来の技術】従来技術の一例として、ゴミ焼却炉等で
発生する有害ハロゲン化合物として、ダイオキシン類を
例に以下に説明する。ゴミ焼却炉等で発生するダイオキ
シン類は排ガスの場合は１００〔ｎｇ／Ｎｍ 3〕程度以
下であり、極めて低濃度である。さらに、ダイオキシン
類の場合には異性体により人体に及ぼす毒性が異なるた
め、ダイオキシン類の個々の異性体について個別に濃度
を求める必要がある。このため、現在時点では排ガス中
のダイオキシン類の直接計測が不可能な状況にある。2. Description of the Related Art As one example of the prior art, a garbage incinerator or the like is used.
Dioxins as harmful halogen compounds generated
An example is described below. Daiki generated in garbage incinerators, etc.
Synths are 100 [ng / Nm when exhaust gas is used. ThreeAbout
Below and very low concentrations. Furthermore, dioxin
In some cases, isomers have different effects on the human body
Individual dioxin isomers
Need to ask. For this reason, at present
It is impossible to measure dioxins directly.
【０００３】上述した極低濃度のダイオキシン類の濃度
を個々の異性体について計測する方法として、従来法で
は高分解能ガスクロマトグラフ／高分解能質量分析計を
用いて計測を実施している。この具体的分析方法につい
ては、試料のサンプリング法や前処理法も含め、厚生省
生活衛生局が取りまとめた「廃棄物処理におけるダイオ
キシン類標準測定分析マニュアル」に詳しく記載されて
いる。[0003] As a method for measuring the concentration of the above-mentioned dioxins at an extremely low concentration for each isomer, in the conventional method, measurement is performed using a high-resolution gas chromatograph / high-resolution mass spectrometer. Details of this specific analysis method, including the sample sampling method and the pretreatment method, are described in detail in the “Manual for Standard Measurement and Analysis of Dioxins in Waste Disposal” compiled by the Ministry of Health and Welfare.
【０００４】[0004]
【発明が解決しようとする課題】この方法は、上述した
高分解ガスクロマトグラフ／高分解能質量分析計を使用
して極低濃度の計測を行う。このため、不純物を前処理
により極力除去する必要があるため、試料の前処理に多
くの時間を要する。このため、分析結果を得るのに要す
る時間は、現状２週間から１ヶ月程度必要であり、ま
た、分析に要する費用も高価であるという課題を抱えて
いた。本発明は上記問題点を解消することを目的とす
る。In this method, an extremely low concentration is measured by using the above-described high-resolution gas chromatograph / high-resolution mass spectrometer. For this reason, since it is necessary to remove impurities as much as possible by pretreatment, much time is required for pretreatment of the sample. For this reason, there is a problem that the time required to obtain the analysis result is currently required from about two weeks to one month, and the cost required for the analysis is high. An object of the present invention is to solve the above problems.
【０００５】[0005]
【課題を解決するための手段】本発明は上記目的を達成
するため、（１）表面プラズモン共鳴を利用して溶媒中
に溶融している有害ハロゲン化合物の紫外線吸収度を増
加させた後、紫外線吸収法を用いて有害ハロゲン化合物
を計測することを特徴とする。また（２）上記（１）に
おいて有害ハロゲン化合物が発生する現場においてオン
ライン計測装置に適用することを特徴とする。In order to achieve the above object, the present invention provides (1) increasing the ultraviolet absorption of a harmful halogen compound dissolved in a solvent using surface plasmon resonance, The method is characterized by measuring harmful halogen compounds using an absorption method. (2) The present invention is characterized in that the method is applied to an online measuring device at a site where a harmful halogen compound is generated in the above (1).
【０００６】本発明によれば、単純な紫外線吸収法では
感度不足のため適用が難しかった紫外線吸収法を、表面
プラズモン共鳴を利用して、溶媒中に溶解している有害
ハロゲン化合物（ダイオキシン類を含む）の紫外線吸収
の吸光度を増加させたことにより、紫外線吸収法での計
測が可能となる。また、表面プラズモン共鳴を利用した
紫外線吸収法をゴミ焼却炉等の有害ハロゲン化合物が発
生する現場において、オンライン計測装置に適用するこ
とが可能になる。According to the present invention, a harmful halogen compound (dioxins, etc.) dissolved in a solvent is removed by utilizing surface plasmon resonance, instead of the ultraviolet absorption method which has been difficult to apply due to lack of sensitivity in a simple ultraviolet absorption method. ), The measurement by the ultraviolet absorption method becomes possible. Further, the ultraviolet absorption method using surface plasmon resonance can be applied to an on-line measurement device at a site where harmful halogen compounds are generated, such as a garbage incinerator.
【０００７】[0007]
【発明の実施の形態】次に本発明法の一実施形態を図面
に基づいて説明する。図１は、本実施形態例の表面プラ
ズモン共鳴を利用した有害ハロゲン化合物の一つである
ダイオキシン類のオンライン計測装置の概念図である。
図１に示したダイオキシン類オンライン計測システムを
用いて、以下に示す方法で排ガス中のダイオキシン類の
濃度計測を実施した。Next, an embodiment of the method of the present invention will be described with reference to the drawings. FIG. 1 is a conceptual diagram of an on-line measurement device for dioxins, which is one of harmful halogen compounds using surface plasmon resonance, according to the present embodiment.
Using the dioxin online measurement system shown in FIG. 1, the concentration of dioxins in the exhaust gas was measured by the following method.
【０００８】分析対象となるダイオキシン類を含む煙道
（１０１）を通過する排ガスは、煙道壁（１０２）から
採取管（１０３）を等速吸引した。本実施例では排ガス
温度が５００℃以上の場合に使用する冷却プローブを使
用した。採取されたダストを含むガスは、捕集部である
インピンジャー（１０４）中でトルエン溶解される。本
実施例では捕集部となるインピンジャーは２本である
が、必要に応じてインピンジャーの数を増やしてもよ
い。捕集部を通過したガスは、空のインピンジャーを通
過して真空ポンプ（１０５）により吸引され、ガス流量
計（１０６）を経て大気に放出した。尚、これらの捕集
部を構成するインピンジャーは恒温槽（１０７）により
５℃程度に保持した。Exhaust gas passing through a flue (101) containing dioxins to be analyzed was suctioned at a constant speed from a flue wall (102) through a sampling pipe (103). In this embodiment, a cooling probe used when the exhaust gas temperature is 500 ° C. or higher is used. The gas containing the collected dust is dissolved in toluene in the impinger (104), which is a collecting part. In this embodiment, the number of the impinger is two, but the number of the impinger may be increased if necessary. The gas that passed through the collection unit passed through an empty impinger, was sucked by a vacuum pump (105), and was discharged to the atmosphere via a gas flow meter (106). In addition, the impinger which comprised these collection parts was hold | maintained at about 5 degreeC by the thermostat (107).
【０００９】ダイオキシン類が溶解したトルエンは、配
管により約２０〔ｃｃ〕が液輸送用ポンプ（１０８）で
吸引しダイオキシン類計測部に導いた。一方、インピン
ジャーへの溶媒の補給は別途、液補給用ポンプ（１０
９）で補給した。About 20 [cc] of toluene in which dioxins were dissolved was sucked by a liquid transport pump (108) through a pipe and led to a dioxins measuring section. On the other hand, the supply of the solvent to the impinger is separately performed by a liquid supply pump (10
Replenished in 9).
【００１０】計測部のサンプル槽（１１０）に導かれた
ダイオキシン類を含むトルエンは、マグネティックスタ
ーラー（１１１）で攪拌した。このサンプル槽上部から
金属薄膜として金を５０〔ｎｍ〕蒸着したプリズム（１
１２）を設置した。一方、光源（１１３）からの光は、
光照射用光プリズム（１１４）で複数の照射用レンズ
（１１５）を経てプリズム（１１２）に照射した。本実
施形態例では、光源としてキセノンランプを使用した
が、レーザを光源として使用することにより、より高感
度な計測が可能である。プリズム中を屈折した光は、金
属蒸着膜が薄いため一部が透過し、金属表面で生じる表
面プラズモンを誘起する。金属膜を透過した光は、表面
プラズモン部分に接近した溶媒中に溶解しているダイオ
キシン類により吸収される。そして、この光は再度、金
属蒸着膜を透過してプリズムの反対側に出射される。こ
の光は偏光板（１１６）を透過した後、集光レンズ（１
１７）で集光して光ファイバー（１１８）を用いて分光
システム（１１９）に導いた。この分光システム（１０
８）では、ダイオキシン類の個々の異性体について光吸
収を生じるな波長で吸光度を計測した。具体的には、
２，３，７，８−ＴＣＤＤの場合、２４５〔ｎｍ〕の波
長を用いて吸光度を評価した。尚、分光システムの制御
と吸光度の計算はコンピュータ（１２０）で実行し、結
果を表示した。尚、サンプル槽（１１０）で計測したダ
イオキシン類を含む溶媒は、必要に応じて排出用ポンプ
（１２１）で排出される。以上の手順により、排ガス中
のダイオキシン類のオンライン計測を可能とした。The toluene containing dioxins led to the sample tank (110) of the measuring section was stirred by a magnetic stirrer (111). A prism (1) on which 50 nm of gold was deposited as a metal thin film from the upper part of the sample tank.
12) was installed. On the other hand, the light from the light source (113)
The light was irradiated to the prism (112) via the plurality of irradiation lenses (115) by the light irradiation optical prism (114). In this embodiment, a xenon lamp is used as a light source. However, by using a laser as a light source, measurement with higher sensitivity is possible. The light refracted in the prism is partially transmitted because the metal deposition film is thin, and induces surface plasmon generated on the metal surface. Light transmitted through the metal film is absorbed by dioxins dissolved in a solvent near the surface plasmon portion. Then, this light again passes through the metal deposition film and is emitted to the opposite side of the prism. This light is transmitted through the polarizing plate (116) and then condensed by the condenser lens (1).
The light was condensed at 17) and guided to a spectroscopy system (119) using an optical fiber (118). This spectroscopy system (10
In 8), the absorbance of each of the dioxins isomers was measured at a wavelength that does not cause light absorption. In particular,
In the case of 2,3,7,8-TCDD, the absorbance was evaluated using a wavelength of 245 [nm]. The control of the spectroscopy system and the calculation of the absorbance were executed by a computer (120), and the results were displayed. The solvent containing dioxins measured in the sample tank (110) is discharged by a discharge pump (121) as necessary. With the above procedure, on-line measurement of dioxins in exhaust gas was made possible.
【００１１】[0011]
【発明の効果】以上のように、本発明によれば、従来紫
外線吸収法では感度不足のため適用が難しかった紫外線
吸収法を、表面プラズモン共鳴を利用して、溶媒中に溶
解している有害ハロゲン化合物（ダイオキシン類を含
む）の紫外線吸収の吸収度を増加させたことにより、紫
外線吸収法での計測を可能としたものであり、通常の分
析法では２週間以上の長時間を有するダイオキシン分析
が、本発明方法を用いることにより１分程度の時間間隔
でサンプリング可能となり、ダイオキシン類のリアルタ
イムに近いモニターを可能にした。As described above, according to the present invention, the ultraviolet absorption method, which had been difficult to apply because of the insufficient sensitivity in the conventional ultraviolet absorption method, was replaced with a harmful substance dissolved in a solvent using surface plasmon resonance. By increasing the absorbance of ultraviolet absorption of halogen compounds (including dioxins), measurement by the ultraviolet absorption method is enabled, and dioxin analysis having a long time of 2 weeks or more in a normal analysis method However, by using the method of the present invention, sampling can be performed at a time interval of about one minute, thereby enabling real-time monitoring of dioxins.
【００１２】また、本発明によれば、ゴミ焼却炉等の有
害ハロゲン化合物が発生する現場において、オンライン
計測装置に適用したことにより、極めて有益である。Further, according to the present invention, it is extremely useful to apply the present invention to an on-line measuring device at a site where harmful halogen compounds are generated such as a garbage incinerator.
【図１】本発明の一実施形態に係るオンライン計測装置
の概念図である。FIG. 1 is a conceptual diagram of an online measurement device according to an embodiment of the present invention.
１０１ 煙道 １０２ 煙道壁 １０３ 採取管 １０４ インピンジャー １０５ 真空ポンプ １０６ ガス流量計 １０７ 恒温槽 １０８ 液輸送用ポンプ １０９ 液補給用ポンプ １１０ サンプル槽 １１１ マグネティックスターラー １１２ プリズム １１３ 光源 １１４ 光照射用光ファイバー １１５ 照射用レンズ １１６ 偏光板 １１７ 集光レンズ １１８ 光ファイバー １１９ 分光システム １２０ コンピュータ １２１ 排出用ポンプ Reference Signs List 101 flue 102 flue wall 103 sampling pipe 104 impinger 105 vacuum pump 106 gas flow meter 107 constant temperature bath 108 liquid transport pump 109 liquid replenishment pump 110 sample tank 111 magnetic stirrer 112 prism 113 light source 114 light irradiation optical fiber 115 irradiation Lens 116 Polarizing plate 117 Condensing lens 118 Optical fiber 119 Spectrum system 120 Computer 121 Discharge pump
フロントページの続き (72)発明者 原 謙治 広島県広島市西区観音新町四丁目６番22号 三菱重工業株式会社広島製作所内 (72)発明者 小笠原 弘明 広島県広島市西区観音新町四丁目６番22号 三菱重工業株式会社広島製作所内 Ｆターム(参考） 2G042 AA01 BB18 BD20 CA01 CB03 EA01 GA01 HA01 HA03 2G059 AA01 AA05 BB04 CC12 DD03 DD05 DD12 DD13 DD17 EE01 EE12 FF03 GG01 HH03 JJ01 JJ11 JJ12 JJ17 JJ19 KK01 MM01 PP01 Continuing on the front page (72) Inventor Kenji Hara 4-62-22 Kannonshinmachi, Nishi-ku, Hiroshima-shi, Hiroshima Mitsubishi Heavy Industries, Ltd. Hiroshima Works (72) Inventor Hiroaki Ogasawara 4-622 Kannonshinmachi, Nishi-ku, Hiroshima-shi, Hiroshima No. F-term in Mitsubishi Heavy Industries, Ltd. Hiroshima Works (reference) 2G042 AA01 BB18 BD20 CA01 CB03 EA01 GA01 HA01 HA03 2G059 AA01 AA05 BB04 CC12 DD03 DD05 DD12 DD13 DD17 EE01 EE12 FF03 GG01 HH03 JJ01 JJ11 JJ01 JJ01 JJ01 JJ01 JJ01 JJ01 JJ01
Claims (2)
溶融している有害ハロゲン化合物の紫外線吸収度を増加
させた後、紫外線吸収法を用いて有害ハロゲン化合物を
計測することを特徴とする表面プラズモン共鳴を利用し
た有害ハロゲン化合物計測方法。1. A surface characterized by measuring the harmful halogen compound using an ultraviolet absorption method after increasing the ultraviolet absorption of a harmful halogen compound dissolved in a solvent using surface plasmon resonance. A method for measuring harmful halogen compounds using plasmon resonance.
いてオンライン計測装置に適用することを特徴とする請
求項１記載の表面プラズモン共鳴を利用した有害ハロゲ
ン化合物計測方法。2. The method for measuring harmful halogen compounds using surface plasmon resonance according to claim 1, wherein the method is applied to an on-line measuring device at a site where harmful halogen compounds are generated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35988598A JP2000180354A (en) | 1998-12-18 | 1998-12-18 | Measuring method for harmful halogen compound by using surface plasmon resonance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35988598A JP2000180354A (en) | 1998-12-18 | 1998-12-18 | Measuring method for harmful halogen compound by using surface plasmon resonance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000180354A true JP2000180354A (en) | 2000-06-30 |
Family
ID=18466800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35988598A Withdrawn JP2000180354A (en) | 1998-12-18 | 1998-12-18 | Measuring method for harmful halogen compound by using surface plasmon resonance |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000180354A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004040270A1 (en) * | 2002-10-23 | 2004-05-13 | Sentronic GmbH Gesellschaft für optische Meßsysteme | Optical sensor |
| EP1373863A4 (en) * | 2001-03-27 | 2005-01-26 | Euro Celtique Sa | Atr crystal device |
| JP2007333485A (en) * | 2006-06-13 | 2007-12-27 | Toyota Central Res & Dev Lab Inc | Biological substance oxidation apparatus and biological substance oxidation measurement method |
| CN105486665A (en) * | 2016-01-26 | 2016-04-13 | 深圳大学 | SPR detection system and method |
-
1998
- 1998-12-18 JP JP35988598A patent/JP2000180354A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1373863A4 (en) * | 2001-03-27 | 2005-01-26 | Euro Celtique Sa | Atr crystal device |
| WO2004040270A1 (en) * | 2002-10-23 | 2004-05-13 | Sentronic GmbH Gesellschaft für optische Meßsysteme | Optical sensor |
| JP2007333485A (en) * | 2006-06-13 | 2007-12-27 | Toyota Central Res & Dev Lab Inc | Biological substance oxidation apparatus and biological substance oxidation measurement method |
| CN105486665A (en) * | 2016-01-26 | 2016-04-13 | 深圳大学 | SPR detection system and method |
| CN105486665B (en) * | 2016-01-26 | 2018-07-31 | 深圳大学 | A kind of SPR detection methods |
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