DK177351B1 - A method of determining catalytic fines in an oil - Google Patents

A method of determining catalytic fines in an oil Download PDF

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Publication number
DK177351B1
DK177351B1 DKPA201100964A DKPA201100964A DK177351B1 DK 177351 B1 DK177351 B1 DK 177351B1 DK PA201100964 A DKPA201100964 A DK PA201100964A DK PA201100964 A DKPA201100964 A DK PA201100964A DK 177351 B1 DK177351 B1 DK 177351B1
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DK
Denmark
Prior art keywords
oil
nmr
determination
aluminum
pulse
Prior art date
Application number
DKPA201100964A
Other languages
English (en)
Inventor
Ole Noergaard Jensen
Original Assignee
Nanonord As
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
Priority to DKPA201100964A priority Critical patent/DK177351B1/en
Application filed by Nanonord As filed Critical Nanonord As
Priority to EP12856813.6A priority patent/EP2795301B1/en
Priority to SG11201403074YA priority patent/SG11201403074YA/en
Priority to BR112014014077A priority patent/BR112014014077A2/pt
Priority to US14/364,361 priority patent/US20140361774A1/en
Priority to JP2014546320A priority patent/JP2015500489A/ja
Priority to DK12856813.6T priority patent/DK2795301T3/da
Priority to US14/364,102 priority patent/US9714909B2/en
Priority to PCT/DK2012/050452 priority patent/WO2013087076A1/en
Priority to CN201280069391.1A priority patent/CN104115006A/zh
Priority to JP2014546319A priority patent/JP2015500488A/ja
Priority to EP12856597.5A priority patent/EP2791661A4/en
Priority to KR1020147019272A priority patent/KR20140128959A/ko
Priority to PCT/DK2012/050456 priority patent/WO2013087077A1/en
Application granted granted Critical
Publication of DK177351B1 publication Critical patent/DK177351B1/en
Priority to HK15103845.4A priority patent/HK1203610A1/xx

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26Oils; Viscous liquids; Paints; Inks
    • G01N33/28Oils, i.e. hydrocarbon liquids
    • G01N33/2829Mixtures of fuels
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G01N24/082Measurement of solid, liquid or gas content
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • G01N24/085Analysis of materials for the purpose of controlling industrial production systems

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analytical Chemistry (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Catalysts (AREA)

Claims (10)

1. Fremgangsmåde til udførelse af en kvantitativ og/eller kvalitativ bestemmelse af katalysatorrester (Eng: Catalytic fines) i brændselsolie, hvor fremgangsmåden omfatter bestemmelse af aluminium ved anvendelse af NMR 5 og kvantitativ og/eller kvalitativ bestemmelse af de katalysatorrester på baggrund af aluminiumsbestemmelsen, hvor fremgangsmåden fortrinsvis omfatter bestemmelse af aluminium i form af aluminiumisotopen 27AI ved udførelse af mindst en NMR-måling på en del af olien, tilvejebringelse af mindst et NMR-spektrum fra NMR-målingen/-erne og udførelse af mindst en 10 kvantitativ og/eller kvalitativ aluminiumsbestemmelse.
2. Fremgangsmåde ifølge krav 1, hvori NMR-målingen udføres in-line eller semi-in-line, omfattende udførelse af NMR-målingen ombord på en motordreven enhed, såsom et fartøj, hvor NMR-målingen fortrinsvis udføres på olien i en strømmende tilstand.
3. Fremgangsmåde ifølge et af de forudgående krav, hvori NMR-målingen omfatter samtidig udsættelse af olie-delen for et magnetfelt B og en flerhed af radiofrekvens-energi-pulser E (RF-pulser) og modtagelse af electromagnetiske signaler fra aluminumsisotoperne, hvor metoden fortrinsvis omfatter bestemmelse af mængden af aluminium-isotoper i test-delen, hvori 20 magnetfeltet B er mindst omkring 1 Tesia, såsom mindst omkring 1,2 Tesia, såsom mindst omkring 1,4 Tesia, såsom mindst omkring 1,6 Tesia.
4. Fremgangsmåde ifølge et af de forudgående krav, hvori NMR-målingen omfatter samtidig udsættelse af olie-delen for et magnetfelt B og en exciterende RF-puls med frekvenser, der er valgt for at excitere et kernespin 25 for mindst en del af aluminum-isotoperne, hvor den exciterende RF-puls fortrinsvis har en båndbredde (spænd over et frekvensområde), som er tilstrækkelig til at excitere mindst et kernespin (spin-overgang) for i det væsentlige alle aluminium-isotoper i olie-delen, hvor den exciterende RF-puls' frekvensområde omfatter en båndbredde på mindst omkring 1 MFIz. DK 177351 B1 2
5. Fremgangsmåde ifølge et af de forudgående krav, hvori fremgangsmåden omfatter bestemmelse af mindst en relaxationshastighed for en exciteret aluminiumsisotop valgt blandt mindst en spin-lattice - TI relaxationshastighed og ved mindst en spin-spin - T2 relaxationshastighed.
6. Fremgangsmåde ifølge et af de forudgående krav, hvori NMR-målingen omfatter samtidig udsættelse af olie-delen for et magnetfelt B og en flerhed af RF-pulser, hvor RF-pulserne omfatter i. en exciterende RF-puls, og ii. mindst en gen-fokuserende RF-puls, 10 hvori den exciterende RF-puls er i form af en 90° puls og den eller de genfokuserende RF-pulser er i form af 180° puls/-er, hvor fremgangsmåden fortrinsvis omfatter at udsætte olie-delen for en flerhed af RF-pulser, et eller flere gen-fokuserende RF-puls-tog, hvor den eller de gen-focuserende RF-puls/-er tilvejebringes med et ekko-delay-tidsrum efter den exciterende RF-15 puls på omkring 50 ms eller mindre.
7. Fremgangsmåde ifølge et af de forudgående krav, hvori den kvantitative og/eller kvalitative aluminumsbestemmelse udføres ved at tilvejebringe en kalibreringsoversigt over kendte aluminiumsindeholdende forbindelser og valgfrit over mængderne heraf i olie.
8. Fremgangsmåde ifølge et af de forudgående krav, hvori fremgangsmåden yderligere omfatter udførelse af en natriumbestemmelse fra målingen på olie-delen ved anvendelse af NMR, udførelse afen vanadiumbestemmelse fra målingen på olie-delen ved anvendelse af NMR og/eller udførelse af en kobberbestemmelse fra målingen på olie-delen ved 25 anvendelse af NMR.
9. Fremgangsmåde ifølge et af de forudgående krav, hvori fremgangsmåden omfatter DK 177351 B1 3 i. udførelse af en kvantitativ og/eller kvalitativ bestemmelse af katalysatorrester i olien; ii. udsættelse af olien for en ekstraktion af katalysatorrester i en separator, der fungerer med et antal driftsparametre omfattende tryk, 5 strømningshastighed og temperatur; iii. udførelse af en kvantitativ og/eller kvalitativ bestemmelse af katalysatorrester i olien; iv. sammenligning af de bestemmelser, der blev foretaget før ekstraktionen med den bestemmelse, der blev foretaget efter ekstraktionen med 10 henblik på at bestemme separatorens ydelse; og v. justering af en eller flere af separatorens driftsparametre baseret på bestemmelsen af separatorydelsen.
10. System egnet to bestemmelse af katalysatorrester i en brændselsolie ifølge et af kravene 1-9, hvor systemet omfatter et NMR-spektrometer, en 15 digital hukommelse, der lagrer en kalibreringsoversigt omfattende kalibreringsdata til kalibrering af de ved NMR-spektrometeret opnåede NMR-spektra, og en computer, der er programmeret til at analysere de af NMR-spektrometeret opnåede NMR-spektra ved anvendelse af kalibreringsoversigten og udførelse af mindst en kvantitativ og/eller kvalitativ 20 bestemmelse af katalysatorrester, hvor systemet er indrettet til i. udførelse af en kvantitativ og/eller kvalitativ bestemmelse af katalysatorrester i olien; ii. udsættelse af olien for en ekstraktion af katalysatorrester i en separator, 25 der fungerer med et antal driftsparametre omfattende tryk, strømningshastighed og temperatur; DK 177351 B1 4 iii. udførelse af en kvantitativ og/eller kvalitativ bestemmelse af katalysatorrester i olien; iv. sammenligning af de bestemmelser, der blev foretaget før ekstraktionen med den bestemmelse, der blev foretaget efter ekstraktionen med 5 henblik på at bestemme separatorens ydelse; og v. justering af en eller flere af separatorens driftsparametre baseret på bestemmelsen af separatorydelsen.
DKPA201100964A 2011-12-12 2011-12-12 A method of determining catalytic fines in an oil DK177351B1 (en)

Priority Applications (15)

Application Number Priority Date Filing Date Title
DKPA201100964A DK177351B1 (en) 2011-12-12 2011-12-12 A method of determining catalytic fines in an oil
PCT/DK2012/050452 WO2013087076A1 (en) 2011-12-12 2012-12-07 A method for quantitative determination of sodium in petroleum fuel
BR112014014077A BR112014014077A2 (pt) 2011-12-12 2012-12-07 método para realizar uma determinação quantitativa e/ou qualitativa de finos catalíticos em óleo combustível, e, sistema apropriado para determinar finos catalíticos em um óleo combustível
US14/364,361 US20140361774A1 (en) 2011-12-12 2012-12-07 Method for quantitative determination of sodium in petroleum fuel
JP2014546320A JP2015500489A (ja) 2011-12-12 2012-12-07 油中の触媒微粒子を測定する方法
DK12856813.6T DK2795301T3 (da) 2011-12-12 2012-12-07 En fremgangsmåde til at bestemme katalytisk finstof i en brændselsolie
EP12856813.6A EP2795301B1 (en) 2011-12-12 2012-12-07 A method of determining catalytic fines in a fuel oil
SG11201403074YA SG11201403074YA (en) 2011-12-12 2012-12-07 A method of determining catalytic fines in an oil
CN201280069391.1A CN104115006A (zh) 2011-12-12 2012-12-07 一种测定油中的催化剂粉末的方法
JP2014546319A JP2015500488A (ja) 2011-12-12 2012-12-07 石油燃料中のナトリウムを定量するための方法
EP12856597.5A EP2791661A4 (en) 2011-12-12 2012-12-07 PROCESS FOR THE QUANTITATIVE DETERMINATION OF SODIUM IN OIL-BASED FUEL
KR1020147019272A KR20140128959A (ko) 2011-12-12 2012-12-07 오일 내의 촉매 파인들을 결정하는 방법
PCT/DK2012/050456 WO2013087077A1 (en) 2011-12-12 2012-12-07 A method of determining catalytic fines in an oil
US14/364,102 US9714909B2 (en) 2011-12-12 2012-12-07 Method of determining catalytic fines in an oil
HK15103845.4A HK1203610A1 (en) 2011-12-12 2015-04-21 A method of determining catalytic fines in an oil

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DK201100964 2011-12-12
DKPA201100964A DK177351B1 (en) 2011-12-12 2011-12-12 A method of determining catalytic fines in an oil

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DK177351B1 true DK177351B1 (en) 2013-02-11

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DKPA201100964A DK177351B1 (en) 2011-12-12 2011-12-12 A method of determining catalytic fines in an oil
DK12856813.6T DK2795301T3 (da) 2011-12-12 2012-12-07 En fremgangsmåde til at bestemme katalytisk finstof i en brændselsolie

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US (1) US9714909B2 (da)
EP (1) EP2795301B1 (da)
JP (1) JP2015500489A (da)
KR (1) KR20140128959A (da)
CN (1) CN104115006A (da)
BR (1) BR112014014077A2 (da)
DK (2) DK177351B1 (da)
HK (1) HK1203610A1 (da)
SG (1) SG11201403074YA (da)
WO (1) WO2013087077A1 (da)

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EP2795301B1 (en) 2018-03-21
EP2795301A4 (en) 2015-09-09
DK2795301T3 (da) 2018-06-14
HK1203610A1 (en) 2015-10-30
SG11201403074YA (en) 2014-07-30
CN104115006A (zh) 2014-10-22
BR112014014077A2 (pt) 2017-06-13
US9714909B2 (en) 2017-07-25
EP2795301A1 (en) 2014-10-29
US20140333304A1 (en) 2014-11-13
KR20140128959A (ko) 2014-11-06
JP2015500489A (ja) 2015-01-05
WO2013087077A1 (en) 2013-06-20

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