JP2013520654A - 包括二次元ガスクロマトグラフ法による模擬蒸留 - Google Patents
包括二次元ガスクロマトグラフ法による模擬蒸留 Download PDFInfo
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- 238000004088 simulation Methods 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- KUPLEGDPSCCPJI-UHFFFAOYSA-N tetracontane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC KUPLEGDPSCCPJI-UHFFFAOYSA-N 0.000 description 2
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- 238000012512 characterization method Methods 0.000 description 1
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/46—Flow patterns using more than one column
- G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
- G01N30/463—Flow patterns using more than one column with serial coupling of separation columns for multidimensional chromatography
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/78—Detectors specially adapted therefor using more than one detector
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8682—Group type analysis, e.g. of components having structural properties in common
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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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- 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
- G01N33/2823—Raw oil, drilling fluid or polyphasic mixtures
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- G01N33/2835—Specific substances contained in the oils or fuels
- G01N33/287—Sulfur content
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Abstract
【選択図】図2
Description
2DGC(GC×GC)システムは、LECO corp.(St. Joseph, Michigan, USA)により製造されるpeagus 4Dであり、これは、注入口、カラム、および検出器で構成されるAgilent 6890ガスクロマトグラフ(Agilent Technology、Wilmington, DE)からなる。100−バイアルトレイのオートサンプラーを有するスプリット/スプリットレス注入口システムが、用いられた。二次元キャピラリーカラムシステムは、非極性の第一カラム(BPX−5、30メートル、内径0.25mm、膜厚1.0μm)、および極性(BPX−50、3メートル、内径0.25mm、膜厚0.25μm)の第二カラムを用いる。両キャピラリーカラムとも、SGE Inc.(Austin, TX)の製品である。Zoex技術(Zoex Corp、Lincoln, NE)に基づいたデュアルジェットサーマルモジュレーションアセンブリ[dual jet thermal modulaion assembly]は、液体窒素で冷却された「トラップ−リリース[trap−release]」型デュアルジェットサーマルモジュレーターであり、これは、これら二つのカラム間に設置される。水素炎イオン化検出器(FID)および硫黄化学発光検出器(SCD)(GE analytical Inc.)が、信号を検出するのに用いられる。試料1.0マイクロリットルが、300℃で、スプリット75:1で注入口から注入された。キャリヤーガスは、1.0ml/分の流れである。オーブンは、60℃(0分保持、および3℃/分の昇温)から、300℃(0分保持)へプログラム制御された。全GC運転時間は、80分であった。モジュレーション時間は、10秒であった。検出器のサンプリング速度は、100Hzであった。データ取得後、それは、LECOソフトウェアパッケージ(機器に付属される)による定性および定量分析で処理された。表示−品質クロマトグラムは、データを二次元画像へ変換することによって完成された。これは、商業プログラム(「Transform」(Research System Inc.、Boulder, CO))によって処理された。二次元画像は、更に、「PhotoShop」(Adobe System Inc.、San Jose, CA)によって処理されて、公表可能画像が作成された。模擬蒸留転換は、デジタルデータをエクセルファイルへエクスポートすることによって為され、模擬蒸留曲線は、関連するエクセルのセルを合計することによって作成された。温度較正は、ノルマルパラフィン混合物を用いて、参照保持時間が、同じ実験条件下に作成されることによって為された。
ディーゼル温度沸騰範囲の炭化水素混合物の、GC×GCまたは2DGC−FIDクロマトグラムである。
硫黄化学発光検出器(SCD)が、GC×GC(または、2DGC)へ取り付けられるか、または既存の水素炎イオン化検出器と一体化される場合には、化合物区分またはタイプによる硫黄種の内訳を、決定することができる。同様に、炭化水素検出器(FID)の信号について上記されるように、2DGCからの硫黄の信号は、個々の硫黄分子タイプの模擬蒸留曲線を作成するのに用いられることができる。
Claims (8)
- 石油ストリームの蒸留を、包括二次元ガスクロマトグラフ法によって模擬する方法であって、
a)前記石油ストリームを二次元ガスクロマトグラフで分離して、極性を温度の関数として決定する工程、および
b)前記二次元ガスクロマトグラフを所定温度で積分して、信号強度を温度の関数として決定する工程
を含む方法。 - 前記温度は、第一次元の保持時間であり、前記極性は、第二次元の保持時間であることを特徴とする請求項1に記載の方法。
- 前記第一次元の保持時間は、沸点であることを特徴とする請求項2に記載の方法。
- 前記信号強度は、重量%であることを特徴とする請求項1に記載の方法。
- 前記信号強度は、モル%であることを特徴とする請求項1に記載の方法。
- 前記積分工程は、石油原料ストリーム中の飽和分、一環芳香族、二環芳香族および三環芳香族の重量%を与えることを特徴とする請求項4に記載の方法。
- 前記積分工程は、非炭素元素含有化合物のモル%を与えることを特徴とする請求項5に記載の方法。
- 前記非炭素元素含有化合物は、硫黄含有化合物を含むことを特徴とする請求項7に記載の方法。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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US33850010P | 2010-02-19 | 2010-02-19 | |
US61/338,500 | 2010-02-19 | ||
US13/021,061 US9176102B2 (en) | 2010-02-19 | 2011-02-04 | Simulation distillation by comprehensive two-dimensional gas chromatography |
US13/021,061 | 2011-02-04 | ||
PCT/US2011/024679 WO2011103042A1 (en) | 2010-02-19 | 2011-02-14 | Simulation distillation by comprehensive two-dimensional gas chromatography |
Publications (2)
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JP2013520654A true JP2013520654A (ja) | 2013-06-06 |
JP5789619B2 JP5789619B2 (ja) | 2015-10-07 |
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JP2012553952A Expired - Fee Related JP5789619B2 (ja) | 2010-02-19 | 2011-02-14 | 包括二次元ガスクロマトグラフ法による模擬蒸留 |
Country Status (9)
Country | Link |
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US (1) | US9176102B2 (ja) |
EP (1) | EP2537024B1 (ja) |
JP (1) | JP5789619B2 (ja) |
CN (1) | CN102782489A (ja) |
AU (1) | AU2011218340B2 (ja) |
CA (1) | CA2788539C (ja) |
MY (1) | MY164062A (ja) |
SG (1) | SG182556A1 (ja) |
WO (1) | WO2011103042A1 (ja) |
Cited By (1)
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KR101499488B1 (ko) * | 2014-02-06 | 2015-03-09 | 한국과학기술연구원 | 기체크로마토그래피를 이용한 유종분석방법 및 장치 |
Families Citing this family (7)
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CN102749405B (zh) * | 2012-07-23 | 2014-05-14 | 中国石油天然气股份有限公司 | 石油样品中五环三萜烷类化合物的定量分析方法 |
US9863898B2 (en) * | 2013-12-18 | 2018-01-09 | Exxonmobile Research And Engineering Company | High temperature simulated distillation |
US20160061786A1 (en) * | 2014-08-28 | 2016-03-03 | Exxonmobil Research And Engineering Company | Compositional analysis of high boiling point mixtures by comprehensive two-dimensional gas chromatography |
CN106053673A (zh) * | 2016-07-29 | 2016-10-26 | 神华集团有限责任公司 | 一种测定锅炉系统水中氢含量的方法及其应用 |
CA3041782A1 (en) | 2016-11-18 | 2018-05-24 | Exxonmobil Research And Engineering Company | Systems and methods for generating a petroleum model of composition using two-dimensional gas chromatography |
SG11202010987YA (en) | 2018-06-26 | 2021-01-28 | Exxonmobil Res & Eng Co | Methods for separating wax products from hydrocarbon feedstreams |
US11401471B2 (en) * | 2018-12-19 | 2022-08-02 | ExxonMobil Technology and Engineering Company | Simulated distillation using gas chromatography with vacuum ultraviolet detection |
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2011
- 2011-02-04 US US13/021,061 patent/US9176102B2/en active Active
- 2011-02-14 CN CN2011800097529A patent/CN102782489A/zh active Pending
- 2011-02-14 CA CA2788539A patent/CA2788539C/en not_active Expired - Fee Related
- 2011-02-14 EP EP11745081.7A patent/EP2537024B1/en not_active Not-in-force
- 2011-02-14 AU AU2011218340A patent/AU2011218340B2/en not_active Ceased
- 2011-02-14 JP JP2012553952A patent/JP5789619B2/ja not_active Expired - Fee Related
- 2011-02-14 WO PCT/US2011/024679 patent/WO2011103042A1/en active Application Filing
- 2011-02-14 SG SG2012052494A patent/SG182556A1/en unknown
- 2011-02-14 MY MYPI2012003365A patent/MY164062A/en unknown
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US20080163672A1 (en) * | 2004-11-15 | 2008-07-10 | Frank Cheng-Yu Wang | Method of Analyzing Basestocks for Low Temperature Properties |
US20070137481A1 (en) * | 2005-12-20 | 2007-06-21 | Jan Blomberg | Method to measure olefins in a complex hydrocarbon mixture |
US20090282897A1 (en) * | 2008-05-14 | 2009-11-19 | Fabrice Bertoncini | Method of determining physico-chemical properties of a petroleum sample from two-dimensional gas chromatography |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101499488B1 (ko) * | 2014-02-06 | 2015-03-09 | 한국과학기술연구원 | 기체크로마토그래피를 이용한 유종분석방법 및 장치 |
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CN102782489A (zh) | 2012-11-14 |
AU2011218340B2 (en) | 2014-10-23 |
EP2537024A1 (en) | 2012-12-26 |
US9176102B2 (en) | 2015-11-03 |
AU2011218340A1 (en) | 2012-09-06 |
WO2011103042A1 (en) | 2011-08-25 |
CA2788539C (en) | 2016-08-16 |
EP2537024A4 (en) | 2013-08-07 |
EP2537024B1 (en) | 2017-04-26 |
MY164062A (en) | 2017-11-15 |
JP5789619B2 (ja) | 2015-10-07 |
SG182556A1 (en) | 2012-08-30 |
CA2788539A1 (en) | 2011-08-25 |
US20110209525A1 (en) | 2011-09-01 |
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