CN104634756B - Sample injector for measuring properties of high-condensation wax oil and application thereof - Google Patents

Sample injector for measuring properties of high-condensation wax oil and application thereof Download PDF

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Publication number
CN104634756B
CN104634756B CN201310552547.8A CN201310552547A CN104634756B CN 104634756 B CN104634756 B CN 104634756B CN 201310552547 A CN201310552547 A CN 201310552547A CN 104634756 B CN104634756 B CN 104634756B
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sealing gasket
wax oil
quartz
sample
oil
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CN104634756A (en
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孙甲
胡卫平
徐新良
孟伟
展江宏
宋自力
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Petrochina Co Ltd
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Petrochina Co Ltd
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Abstract

The invention relates to a sample injector for measuring the property of high-condensation wax oil; a near infrared instrument sample cell clamping piece, an oil-resistant rubber sealing gasket, a quartz wound sheet, a polytetrafluoroethylene sealing gasket, a sample cell, a positioning bolt and a quartz scraping sheet; installing an oil-resistant rubber sealing gasket on the surface of the near-infrared instrument sample pool clamping piece, installing a quartz wound piece on the oil-resistant rubber sealing gasket, installing a polytetrafluoroethylene sealing gasket on the quartz wound piece, then connecting and fixing the outer instrument sample pool clamping piece, the oil-resistant rubber sealing gasket, the quartz wound piece and the polytetrafluoroethylene sealing gasket by using a positioning bolt, and forming a sample pool in a space surrounded by the quartz wound piece, the polytetrafluoroethylene sealing gasket and the positioning bolt; heating and softening or liquefying the wax oil which can not be sampled at normal temperature, injecting the wax oil into the sample pool of the sample injector, cooling the sample to the normal temperature, solidifying and forming, putting the whole sample injector into a near-infrared instrument, directly measuring to obtain a wax oil near-infrared spectrogram, establishing near-infrared wax oil property model basic data, and obtaining the property evaluation of the wax oil.

Description

A kind of injector for measuring high solidifying wax oil property and its application
Technical field
The present invention relates to a kind of special injector of near infrared spectrometer and its application method for measuring high solidifying wax oil property
Background technology
According to relevant authority patent information inquiry system and literature query system, correlation technique situation of the present invention is found such as Under:
Patent 1(Application publication number 201120393038.1)Detector for asphaltene in wax oil fraction, Sinopec Fushun Petrochemical Research Institute of limited company.
The invention provides a kind of detector for asphaltene in wax oil fraction, including it is solvent tank, flask, bottle,suction, true Empty pump and control system;Solvent stock tank top is with the outlet with vavuum pump with pipeline connection, and solvent tank sets solvent to discharge Mouthful, the entrance of solvent outlet and flask is with pipeline connection, and drag sets opening, and the opening is with bottle,suction entrance with pipe fitting Connection, the entrance of bottle,suction sets filter membrane, and the outlet of bottle,suction connect with vavuum pump, control system including liquid level detector with Controller, bottle,suction sets the liquid level detector of detection bottle,suction liquid level, and liquid level detector is connected with controller with circuit mode, Controller is connected with vavuum pump with circuit mode.Compared with prior art, the present apparatus is used for the survey of N.heptane insolubles in wax oil It is fixed, semi-automation can be achieved, reduces the health caused due to solvent volatilization on human body and environmental pollution influence, improves work Efficiency and detection quality.
Document 1SH/T0509-2010 asphalt compound mensuration methods come determine the asphalitine of wax oil, saturation point, fragrance point, The property data of colloid.
Sample is settled out asphalitine with normal heptane, after filtering, flowed back the solvable point for removing and being mingled with precipitation with normal heptane, Again with toluene backflow dissolving precipitation, obtains asphalitine.By depitching matter partial adsorbates on chromatography on alumina post, positive heptan is used successively Alkane, toluene, toluene-ethano expansion are washed out, and correspondence obtains saturation point, fragrance point, colloid, with accuracy rate is poor, reproduction degree is low, The limitations such as operation difficulty is high, dangerous big, personnel cost and equipment and instrument cost height, the test period is 82 hours.
Found by background technology situation related to this technology in Research Literature, the problem of being primarily present is:Measurement in the past The measure device of wax oil studies on asphaltene as described in the content of patent 1 there is provided a kind of detector for asphaltene in wax oil fraction, including Solvent tank, flask, bottle,suction, vavuum pump and control system;Solvent stock tank top is connected with the outlet with vavuum pump with pipeline Lead to, solvent tank setting solvent outlet, the entrance of solvent outlet and flask is with pipeline connection, and drag sets opening, The opening is connected with bottle,suction entrance with pipe fitting, and the entrance of bottle,suction sets filter membrane, and the outlet of bottle,suction is connected with vavuum pump, Control system includes liquid level detector and controller, and bottle,suction sets the liquid level detector of detection bottle,suction liquid level, level sensing Device is connected with controller with circuit mode, and controller is connected with vavuum pump with circuit mode.For N.heptane insolubles in wax oil Measure, can be achieved semi-automation, reduce due to solvent volatilize human body is caused health and environmental pollution influence, improve Operating efficiency and detection quality.
This assay device structures for measuring wax oil asphalitine are complicated, cost is high, installation steps are more, using poisonous and hazardous Chemical reagent is more, big to human health damage, the shortcomings of require high to operating personnel.
Conventional wax oil asphalitine, saturation point, fragrance point, the property data analysis test method of colloid are bibliography 1 Asphalt compound mensuration method SH/T0509-2010 determines the property number of the asphalitine of wax oil, saturation point, fragrance point, colloid According to.
Sample is settled out asphalitine with normal heptane, after filtering, flowed back the solvable point for removing and being mingled with precipitation with normal heptane, Again with toluene backflow dissolving precipitation, obtains asphalitine.By depitching matter partial adsorbates on chromatography on alumina post, positive heptan is used successively Alkane, toluene, toluene-ethano expansion are washed out, and correspondence obtains saturation point, fragrance point, colloid,
This method for measuring wax oil property is complicated, step is more, endangered using poisonous and hazardous chemical reagent, to health Evil is big, require high to operating personnel, accuracy rate is poor, reappear that degree is low, operation difficulty is high, it is dangerous greatly, personnel cost and equipment The limitations such as instrument cost height, the test period is the shortcomings of test period is long within 82 hours.
The assay device structures of measurement wax oil asphalitine were complicated in the past, cost is high, installation steps are more, using poisonous and hazardous Chemical reagent is more, big to human health damage, the shortcomings of require high to operating personnel.
The method of measurement wax oil property was complicated in the past, step is more, endangered using poisonous and hazardous chemical reagent, to health Evil is big, require high to operating personnel, accuracy rate is poor, reappear that degree is low, operation difficulty is high, it is dangerous greatly, personnel cost and equipment Instrument cost is high, the test period is 82 hours, the shortcomings of test period is long.
The content of the invention
It is an object of the invention to provide a kind of injector for measuring high solidifying wax oil property and its application.One kind coordinates near-infrared The special injector and its application method of the high condensation point wax oil of apparatus measures, the atlas of near infrared spectra for measuring high condensation point wax oil, So as to obtain the data of the characteristic absorption peak of high condensation point wax oil, basic data is provided to set up near-infrared wax oil property model, is entered And obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, using coordinating, nir instrument measurement is high The special injector and its application method of condensation point wax oil can overcome measurement wax oil property equipment therefor and application method in the past Shortcoming, with structures and methods are simple, cost is low, install and operating procedure is few, precision is high, use poisonous and hazardous chemical reagent Less, harm to health is small, require low to operating personnel.Accuracy rate is high, it is high to reappear degree, operation difficulty is low, danger Small, personnel cost and equipment and instrument cost are low, the test period is greatly shortened by 1 hour, the advantages of test period is short.
Injector composition of the present invention has:Near infrared spectrometer sample cell fastener, oil resistant rubber sealing gasket, quartz wound piece, Polytetrafluoroethylene sealing gasket, sample cell, bolt, quartz scrape tabletting;
Installed on the surface of near infrared spectrometer sample cell fastener and quartz is installed on oil resistant rubber sealing gasket, oil resistant rubber sealing gasket Create piece, polytetrafluoroethylene sealing gasket be installed and then with bolt by near infrared spectrometer sample cell fastener, oil resistant on quartz wound piece Rubber gasket, quartz wound piece, polytetrafluoroethylene sealing gasket are connected, in quartz wound piece, polytetrafluoroethylene sealing gasket, positioning Sample cell is formed in the space that bolt is surrounded.
The wax oil that can not will be sampled at normal temperatures, heats and softens or injects the special Autosampler pond after liquefying, Sample cell is struck off with glass scraper tabletting under sample softening or liquefaction, after sample is cooled to normal temperature cure shaping, in stone Test sample region is formed in the space that English wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, basic data is provided to set up near-infrared wax oil property model, And then obtain the evaluation conclusions such as the property of wax oil.
, can be by usually not using the special injector and its application method for coordinating nir instrument to measure high condensation point wax oil The wax oil that can be sampled at normal temperatures, realizes and injects the special injector after heating and softening, glass is used under sample soft state Glass tabletting strikes off sample cell, after sample is cooled to normal temperature cure shaping, is put into nir instrument, carries out direct measurement, can be with The wax oil atlas of near infrared spectra of coincidence measurement requirement is obtained, so that the data of the characteristic absorption peak of high condensation point wax oil are obtained, to build Vertical near-infrared wax oil property model provides basic data, and then obtains the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, using coordinating, nir instrument measurement is high The special injector and its application method of condensation point wax oil can overcome measurement wax oil property equipment therefor and application method in the past Shortcoming, with structures and methods are simple, cost is low, install and operating procedure is few, precision is high, use poisonous and hazardous chemical reagent Less, harm to health is small, require low to operating personnel.Accuracy rate is high, it is high to reappear degree, operation difficulty is low, danger Small, personnel cost and equipment and instrument cost are low, the test period is greatly shortened by 1 hour, the advantages of test period is short.
Brief description of the drawings
The injector schematic diagram of the high solidifying wax oil property of Fig. 1 measurements.
Fig. 2 quartz scrapes tabletting schematic diagram.
Wherein:1 near infrared spectrometer sample cell fastener, 2 oil resistant rubber sealing gaskets, 3 oily rubber gaskets, 4 polytetrafluoroethylene (PTFE) are close Packing, 5 sample cells, 6 bolts, 7 quartz scrape tabletting.
Embodiment
Injector composition of the present invention has:Near infrared spectrometer sample cell fastener 1, oil resistant rubber sealing gasket 2, quartz wound piece 3rd, polytetrafluoroethylene sealing gasket 4, sample cell 5, bolt 6, quartz scrape tabletting 7;
Install on oil resistant rubber sealing gasket 2, oil resistant rubber sealing gasket 2 and install on the surface of near infrared spectrometer sample cell fastener 1 Quartz wound piece 3, quartz wound piece 3 on install polytetrafluoroethylene sealing gasket 4 then with bolt by outer instrument sample cell fastener 1, Oil resistant rubber sealing gasket 2, quartz wound piece 3, polytetrafluoroethylene sealing gasket 4 are connected, in quartz wound piece, teflon seal Sample cell 5 is formed in the space that pad, bolt are surrounded.
The wax oil that can not will be sampled at normal temperatures, heats and softens or injects the special Autosampler pond 5 after liquefying, Sample cell is struck off with glass scraper tabletting 7 under sample softening or liquefaction, after sample is cooled to normal temperature cure shaping, in stone Test sample region is formed in the space that English wound piece 3, polytetrafluoroethylene sealing gasket 4, bolt 6 are surrounded.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener 1 It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, basic data is provided to set up near-infrared wax oil property model, And then obtain the evaluation conclusions such as the property of wax oil.
Embodiment 1:
Kazakhstan's train wax oil colloid property measurement
Using the special injector for coordinating nir instrument to measure high condensation point wax oil, first by near infrared spectrometer sample cell fastener Installed on surface and quartz wound piece is installed on oil resistant rubber sealing gasket, oily rubber gasket, polytetrafluoroethyl-ne is installed on quartz wound piece Alkene sealing gasket and then with bolt that outer instrument sample cell fastener, oil resistant rubber sealing gasket, quartz wound piece, polytetrafluoroethylene (PTFE) is close Packing is connected, and sample cell is formed in the space that quartz wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded.
By Kazakhstan's train wax oil that can not be sampled at normal temperatures, injected after being heated to 80 DEG C of softenings or liquefaction The special Autosampler pond, strikes off sample cell with glass scraper tabletting under sample softening or liquefaction, treats that sample is cooled to After 30 DEG C of curing moldings, test sample area is formed in the space that quartz wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded Domain.
Special injector is integrally put into nir instrument, nir instrument is 1. fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, basis is provided to set up near-infrared wax oil colloid property model Data, and then obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, utilize homemade cooperation nir instrument Measure the high special injector of condensation point wax oil to obtain high condensation point wax oil atlas of near infrared spectra, fill up national and foreign standards Lack the blank of high solidifying wax oil spectrogram in spectrum picture library.
Embodiment 2:
The mixed gatch asphalitine property measurement of Kelamayi North SinKiang
Special injector is used, oil resistant rubber sealing gasket, oily rubber first will be installed on the surface of near infrared spectrometer sample cell fastener Quartz wound piece is installed on sealing gasket, polytetrafluoroethylene sealing gasket is installed and then with bolt by outer instrument sample on quartz wound piece Product pond fastener, oil resistant rubber sealing gasket, quartz wound piece, polytetrafluoroethylene sealing gasket are connected, in quartz wound piece, polytetrafluoroethyl-ne Sample cell is formed in the space that alkene sealing gasket, bolt are surrounded.
By the Kelamayi North SinKiang mixed gatch that can not be sampled at normal temperatures, noted after being heated to 70 DEG C of softenings or liquefaction Enter the special Autosampler pond, sample cell is struck off with glass scraper tabletting under sample softening or liquefaction, treat that sample is cooled down To 40 DEG C of curing moldings, created in quartz and test sample area is formed in piece, the space that polytetrafluoroethylene sealing gasket, bolt are surrounded Domain.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, base is provided to set up near-infrared wax oil asphalitine property model Plinth data, and then obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, utilize homemade cooperation nir instrument The atlas of near infrared spectra of high condensation point wax oil can be obtained by measuring the high special injector of condensation point wax oil, can fill up national and foreign standards light Lack the blank of high solidifying wax oil spectrogram in spectrogram storehouse.
Embodiment 3:
Eastern boundary oil field Huoshaoshan wax oil aromatic hydrocarbons property measurement
Using the special injector for coordinating nir instrument to measure high condensation point wax oil, first by near infrared spectrometer sample cell fastener Installed on surface and quartz wound piece is installed on oil resistant rubber sealing gasket, oily rubber gasket, polytetrafluoroethyl-ne is installed on quartz wound piece Alkene sealing gasket and then with bolt that outer instrument sample cell fastener, oil resistant rubber sealing gasket, quartz wound piece, polytetrafluoroethylene (PTFE) is close Packing is connected, and sample cell is formed in the space that quartz wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded.
By the eastern boundary oil field Huoshaoshan wax oil that can not be sampled at normal temperatures, injected after being heated to 90 DEG C of softenings or liquefaction The special Autosampler pond, strikes off sample cell with glass scraper tabletting under sample softening or liquefaction, treats that sample is cooled to After 45 DEG C of curing moldings, test sample area is formed in the space that quartz wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded Domain.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, basis is provided to set up near-infrared wax oil aromatic hydrocarbons property model Data, and then obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, use homemade cooperation nir instrument The atlas of near infrared spectra of high condensation point wax oil can be obtained by measuring the high special injector of condensation point wax oil, fill up national and foreign standards spectrogram Lack the blank of high solidifying wax oil spectrogram in storehouse.
Embodiment 4:
Middle oil transport Amy gram wax oil saturation point property measurement
It will first be installed on the surface of near infrared spectrometer sample cell fastener and stone be installed on oil resistant rubber sealing gasket, oily rubber gasket English wound piece, on quartz wound piece polytetrafluoroethylene sealing gasket is installed and then with bolt by outer instrument sample cell fastener, oil resistant rubber Glue sealing gasket, quartz wound piece, polytetrafluoroethylene sealing gasket are connected, in quartz wound piece, polytetrafluoroethylene sealing gasket, positioning spiral shell Sample cell is formed in the space that bolt is surrounded.
The wax oil that can not will be sampled at normal temperatures, heats and softens or injects the special Autosampler pond after liquefying, Sample cell is struck off with glass scraper tabletting under sample softening or liquefaction, after sample is cooled to normal temperature cure shaping, in stone Test sample region is formed in the space that English wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, base is provided to set up near-infrared wax oil saturation point property model Plinth data, and then obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, utilize homemade cooperation nir instrument The atlas of near infrared spectra that the special injector of high condensation point wax oil measures high condensation point wax oil is measured, meet that analysis process quickly analyzes will Ask.
Embodiment 5:Black petrochemical industry wax oil saturation point property measurement
By the black petrochemical industry wax oil that can not be sampled at normal temperatures, special injector sample is injected after being heated to 100 DEG C of liquefaction Product pond, sample cell is struck off under sample liquefaction with glass scraper tabletting, after sample is cooled to normal temperature cure shaping, in quartz Test sample region is formed in the space that wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded.
Special injector is integrally put into nir instrument, nir instrument is fixed on near infrared spectrometer sample cell fastener It is interior, instrument power source is connected, after carrying out direct measurement after instrument stabilizer, the wax oil near infrared spectrum of coincidence measurement requirement can be obtained Figure, so as to obtain the data of the characteristic absorption peak of high condensation point wax oil, base is provided to set up near-infrared wax oil saturation point property model Plinth data, and then obtain the evaluation conclusions such as the property of wax oil.
For normal temperature solid-state, it is impossible to inject the high condensation point wax oil of liquid sample pool, utilize homemade cooperation nir instrument The atlas of near infrared spectra that the special injector of high condensation point wax oil measures high condensation point wax oil is measured, meet that analysis process quickly analyzes will Ask.

Claims (1)

1. a kind of application for the injector for measuring high solidifying wax oil property, it is characterised in that:The injector is by near infrared spectrometer sample Pond fastener, oil resistant rubber sealing gasket, quartz wound piece, polytetrafluoroethylene sealing gasket, sample cell, bolt, glass scraper tabletting group Into;Installed on the surface of near infrared spectrometer sample cell fastener and quartz wound piece be installed on oil resistant rubber sealing gasket, oil resistant rubber sealing gasket, Polytetrafluoroethylene sealing gasket is installed on quartz wound piece, then with bolt by near infrared spectrometer sample cell fastener, oil resistant rubber Sealing gasket, quartz wound piece, polytetrafluoroethylene sealing gasket are connected, in quartz wound piece, polytetrafluoroethylene sealing gasket, bolt Sample cell is formed in the space surrounded;
The application of the injector of the high solidifying wax oil property of measurement includes:The wax oil that can not will be sampled at normal temperatures, heating The Autosampler pond is injected after softening or liquefaction, sample cell is struck off with glass scraper tabletting under sample softening or liquefaction, After sample is cooled to normal temperature cure shaping, in the space that quartz wound piece, polytetrafluoroethylene sealing gasket, bolt are surrounded Form test sample region;
Injector is integrally put into nir instrument, is fixed on near infrared spectrometer sample cell fastener in nir instrument, instrument is connected Device power supply, after carrying out direct measurement after instrument stabilizer, obtains wax oil atlas of near infrared spectra, so as to obtain the feature of high condensation point wax oil The data of absworption peak, set up near-infrared wax oil property model basic data, and then obtain the properties evaluations conclusion of wax oil.
CN201310552547.8A 2013-11-08 2013-11-08 Sample injector for measuring properties of high-condensation wax oil and application thereof Active CN104634756B (en)

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CN112730636B (en) * 2019-10-28 2022-06-03 中国石油天然气股份有限公司 Heavy oil four-component separation method

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