JP2009053046A - 炭化水素を主成分とする試料中の水銀を測定する水銀測定装置 - Google Patents
炭化水素を主成分とする試料中の水銀を測定する水銀測定装置 Download PDFInfo
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 371
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 339
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 21
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 17
- 150000002430 hydrocarbons Chemical class 0.000 title abstract description 20
- 239000003463 adsorbent Substances 0.000 claims abstract description 83
- 238000005259 measurement Methods 0.000 claims abstract description 63
- 238000002347 injection Methods 0.000 claims abstract description 32
- 239000007924 injection Substances 0.000 claims abstract description 32
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims description 181
- 239000012159 carrier gas Substances 0.000 claims description 46
- 229910052751 metal Inorganic materials 0.000 claims description 39
- 239000002184 metal Substances 0.000 claims description 39
- 229940008718 metallic mercury Drugs 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 32
- 238000000926 separation method Methods 0.000 claims description 22
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 238000005070 sampling Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 62
- 238000000034 method Methods 0.000 description 44
- 229910052786 argon Inorganic materials 0.000 description 31
- 230000002378 acidificating effect Effects 0.000 description 24
- 239000003795 chemical substances by application Substances 0.000 description 22
- 239000003595 mist Substances 0.000 description 15
- 238000001816 cooling Methods 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 101100484380 Fowlpox virus (strain NVSL) FPV061 gene Proteins 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 239000003915 liquefied petroleum gas Substances 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000003350 kerosene Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 150000002730 mercury Chemical class 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ATZBPOVXVPIOMR-UHFFFAOYSA-N dimethylmercury Chemical compound C[Hg]C ATZBPOVXVPIOMR-UHFFFAOYSA-N 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- TYTHZVVGVFAQHF-UHFFFAOYSA-N manganese(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Mn+3].[Mn+3] TYTHZVVGVFAQHF-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002731 mercury compounds Chemical class 0.000 description 1
- -1 naphtha Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- G01N33/28—Oils, i.e. hydrocarbon liquids
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- G01N2021/3107—Cold vapor, e.g. determination of Hg
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Abstract
【解決手段】水銀測定装置100は、水銀を吸着する第1吸着剤11および水銀を還元する還元剤13が充填されたカラム1と、カラム1に試料を注入する注入器3と、第1吸着剤11を加熱する第1加熱器12と、還元剤13を加熱する第2加熱器と、第2吸着剤17が充填された水銀捕集管18と、水銀捕集管18を加熱する第3加熱器19と、水銀を測定する水銀測定器2と、ガス流路FP1、FP2、FP4と、ガス流路FP1、FP2、FP4のいずれかを選択するための流路切替弁V1〜V3、V5、V6と、第1〜第3加熱器12、14、19、注入器3、流路切替弁V1〜V3、V5、V6および水銀測定器2を制御する制御装置4とを備える。
【選択図】図1
Description
前記水銀捕集管を加熱する第3加熱器と、前記第3加熱器によって加熱され前記水銀捕集管から遊離する金属水銀を試料セルに導入して測定する水銀測定器とを備える。
2 水銀測定器 (水銀原子吸光分析器)
3 注入器
4 制御装置
6 試料交換器
8 水銀測定器 (水銀原子蛍光分析器)
11 第1吸着剤
12 第1加熱器
13 還元剤
14 第2加熱器
17 第2吸着剤
18 水銀捕集管
19 第3加熱器
21、81 試料セル
51 ガス導入口 (第1ガス導入口)
71 ガス導入口 (第2ガス導入口)
100、200 水銀測定装置
FP1 注入・捕集流路
FP2 還元・捕集流路
FP4 測定流路
G1 第1キャリアガス (空気)
G2 第2キャリアガス (アルゴンガス)
S 試料
S1 試料注入工程
S2 捕集・分離工程
S3 水銀還元・捕集工程
S4 金属水銀遊離工程
S5 測定工程
V1、V2、V3、V5、V6、V7 流路切替弁
Claims (6)
- 炭化水素を主成分とする試料中の水銀を測定する装置であって、
水銀を吸着する第1吸着剤および1価と2価の水銀を金属水銀に還元する還元剤が充填されたカラムと、
前記カラムに試料を注入する注入器と、
前記カラムの第1吸着剤を加熱する第1加熱器と、
前記カラムの還元剤を加熱する第2加熱器と、
金属水銀を吸着する第2吸着剤が充填された水銀捕集管と、
前記水銀捕集管を加熱する第3加熱器と、
前記第3加熱器によって加熱され前記水銀捕集管から遊離する金属水銀を試料セルに導入して測定する水銀測定器と、
キャリアガスをガス導入口から導入し、前記第1吸着剤にキャリアガスを流し、ガス導出口からキャリアガスを導出する注入・捕集流路、キャリアガスをガス導入口から導入し、前記第1吸着剤、還元剤および第2吸着剤にキャリアガスを流し、ガス導出口からキャリアガスを導出する還元・捕集流路、ならびにキャリアガスをガス導入口から導入し、前記第2吸着剤および試料セルにキャリアガスを流し、ガス導出口からキャリアガスを導出する測定流路のいずれか1つの流路を形成するガス流路と、
前記ガス流路のいずれか1つを選択するための流路切替弁と、
前記第1加熱器、第2加熱器、第3加熱器、注入器、流路切替弁および水銀測定器を制御する制御装置と、
を備える水銀測定装置。 - 請求項1において、
前記制御装置が、
前記注入器に試料を注入させる試料注入工程と、
前記第1吸着剤に試料中の水銀を捕集させ、揮発性有機物を分離排出させる捕集・分離工程と、
前記第1吸着剤に捕集された水銀を前記第1加熱器に加熱気化させ、前記第2加熱器に前記還元剤を加熱させて1価と2価の水銀を金属水銀に還元させ、金属水銀を前記第2吸着剤が充填された前記水銀捕集管に捕集させる水銀還元・捕集工程と、
前記水銀捕集管を前記第3加熱器に加熱させて金属水銀を前記第2吸着剤から遊離させる金属水銀遊離工程と、
前記水銀捕集管から遊離した金属水銀を前記水銀測定器に測定させる測定工程とを実行する水銀測定装置。 - 請求項2において、
前記制御装置が、
前記金属水銀遊離工程と前記測定工程とを同時に実行する水銀測定装置。 - 請求項1から3までのいずれか一項において、
前記ガス流路が、第1キャリアガスを導入する第1ガス導入口および第2キャリアガスを導入する第2ガス導入口を有し、
前記水銀測定器が水銀原子蛍光分析器である水銀測定装置。 - 請求項4において、
前記試料注入工程、捕集・分離工程および水銀還元・捕集工程では前記第1ガス導入口から第1キャリアガスが導入され、
前記金属水銀遊離工程および測定工程では前記第2ガス導入口から第2キャリアガスが導入され、
前記水銀測定器が水銀原子蛍光分析器である水銀測定装置。 - 請求項1から5までのいずれか一項において、
複数の試料を交換する試料交換器を有し、
前記制御装置が前記試料交換器を制御する水銀測定装置。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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JP2007220138A JP4226049B1 (ja) | 2007-08-27 | 2007-08-27 | 炭化水素を主成分とする試料中の水銀を測定する水銀測定装置 |
CA2697499A CA2697499C (en) | 2007-08-27 | 2008-08-19 | Mercury measuring apparatus for measuring mercury contained in sample composed mainly of hydrocarbon |
PCT/JP2008/002229 WO2009028149A1 (ja) | 2007-08-27 | 2008-08-19 | 炭化水素を主成分とする試料中の水銀を測定する水銀測定装置 |
EP08828417.9A EP2192398B1 (en) | 2007-08-27 | 2008-08-19 | Mercury measuring apparatus for measuring mercury contained in sample composed mainly of hydrocarbon |
US12/674,354 US8223332B2 (en) | 2007-08-27 | 2008-08-19 | Mercury measuring apparatus for measuring mercury contained in sample composed mainly of hydrocarbon |
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JP2007220138A JP4226049B1 (ja) | 2007-08-27 | 2007-08-27 | 炭化水素を主成分とする試料中の水銀を測定する水銀測定装置 |
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JP4226049B1 JP4226049B1 (ja) | 2009-02-18 |
JP2009053046A true JP2009053046A (ja) | 2009-03-12 |
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US (1) | US8223332B2 (ja) |
EP (1) | EP2192398B1 (ja) |
JP (1) | JP4226049B1 (ja) |
CA (1) | CA2697499C (ja) |
WO (1) | WO2009028149A1 (ja) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2012073617A1 (ja) * | 2010-11-30 | 2012-06-07 | 日本インスツルメンツ株式会社 | 水銀分析用の加熱燃焼管、加熱分解装置および水銀分析装置 |
JP2013205128A (ja) * | 2012-03-28 | 2013-10-07 | Kyoto Electron Mfg Co Ltd | 水銀濃度測定装置及び前処理器 |
JP2013205129A (ja) * | 2012-03-28 | 2013-10-07 | Kyoto Electron Mfg Co Ltd | 水銀濃度測定装置及び還元剤劣化検出器 |
JP2015161636A (ja) * | 2014-02-28 | 2015-09-07 | 日本インスツルメンツ株式会社 | 水銀原子蛍光分析装置 |
JP2016065802A (ja) * | 2014-09-25 | 2016-04-28 | 日本インスツルメンツ株式会社 | 水銀を保持するための水銀保持剤ならびにそれを用いる水銀分析方法および水銀分析装置 |
CN108132276A (zh) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | 一种测量气(液)-固相相互作用强度的装置和方法 |
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JP4050577B2 (ja) * | 2002-09-03 | 2008-02-20 | 日本インスツルメンツ株式会社 | 水銀分析装置およびこれに用いるサンプルチェンジャ |
TW547642U (en) * | 2002-12-31 | 2003-08-11 | Chun-Mao Tseng | Ultra-trace automated mercury species analyzer (AMSA) |
JP2004354067A (ja) | 2003-05-27 | 2004-12-16 | Central Res Inst Of Electric Power Ind | ガス中の水銀測定方法および装置 |
TW200813430A (en) * | 2006-08-01 | 2008-03-16 | Brooks Rand Llc | Automated system for detection of chemical compounds |
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Cited By (7)
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WO2012073617A1 (ja) * | 2010-11-30 | 2012-06-07 | 日本インスツルメンツ株式会社 | 水銀分析用の加熱燃焼管、加熱分解装置および水銀分析装置 |
JP2013205128A (ja) * | 2012-03-28 | 2013-10-07 | Kyoto Electron Mfg Co Ltd | 水銀濃度測定装置及び前処理器 |
JP2013205129A (ja) * | 2012-03-28 | 2013-10-07 | Kyoto Electron Mfg Co Ltd | 水銀濃度測定装置及び還元剤劣化検出器 |
JP2015161636A (ja) * | 2014-02-28 | 2015-09-07 | 日本インスツルメンツ株式会社 | 水銀原子蛍光分析装置 |
JP2016065802A (ja) * | 2014-09-25 | 2016-04-28 | 日本インスツルメンツ株式会社 | 水銀を保持するための水銀保持剤ならびにそれを用いる水銀分析方法および水銀分析装置 |
CN108132276A (zh) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | 一种测量气(液)-固相相互作用强度的装置和方法 |
CN108132276B (zh) * | 2016-12-01 | 2020-10-23 | 中国科学院大连化学物理研究所 | 一种测量气(液)-固相相互作用强度的装置和方法 |
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CA2697499C (en) | 2015-09-29 |
US20110299072A1 (en) | 2011-12-08 |
CA2697499A1 (en) | 2009-03-05 |
US8223332B2 (en) | 2012-07-17 |
JP4226049B1 (ja) | 2009-02-18 |
WO2009028149A1 (ja) | 2009-03-05 |
EP2192398A4 (en) | 2016-01-13 |
EP2192398B1 (en) | 2018-10-24 |
EP2192398A1 (en) | 2010-06-02 |
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