CN1629632A - Group composition analysis method for hydrocarbon series of residual oil and bitumen - Google Patents
Group composition analysis method for hydrocarbon series of residual oil and bitumen Download PDFInfo
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Abstract
A group composition analysis method to resid and asphalt hydrocarbon is to add a treated silica gel into a chromatographic post to be added with treated Al2O, weigh resid or asphalt accurately and put them into the chromatographic post then put Al2O in it. Normal heptane is put into the post and flown paraffinsection is collected, the matched solution of normal heptane and dichloromethane is put into the post to collect the flown aromatic section, the solution of matched by dichlormethane and THF is put in it to collect the gel section. The receiving bottles are completely extracted and weighed accurately, the increased weight of each is net for each preparation section and the result is got by compute.
Description
Technical field
The invention belongs to a kind of post liquid chromatography analytical approach, relate in particular to a kind of analytical approach that residual oil, pitch are carried out the group composition of hydrocarbon system
Background technology
Coal, the existing history for a long time of petroleum refining, long course has been experienced in corresponding tar, mink cell focus, pitch analysis too, product for the lightweight part adopts gas chromatography and high performance liquid chromatography better to solve, but to bad always solutions such as heavy oil residue, pitches.For the residual oil that reaches over thousands of kind of compound, pitch class heavy product, primarily should be the problem analysis that solves the group composition of hydrocarbon system.The classification of so-called group composition mainly is to divide according to functional group's feature of compound, and wherein, only having the straight chain of carbon, hydrogen and the compound of side chain is alkane; What have carbon, hydrogen and form JI key-aromatic ring is aromatic hydrocarbons; It is colloid or non-hydrocarbon system that aromatic hydrocarbons or ring have oxygen, nitrogen sulphur etc. heteroatomic; Have extremely long two keys and molecular weight very big be bituminous matter.Strictly speaking, this is a kind of than broad classification, is the method that a kind of enrichment section is divided, yet, for this complex object be, be used to instruct explained hereafter and technical study, this is absolutely necessary.
Four early stage, classical big hydrocarbon group composition analysis method [ASTM D-2007, PA (1986)], there is some deficiency in it, it is appropriate to thermosol hexane solvend is made PONA analysis, and in fact, except the hexane solvend of sample, remainder still exists the problem analysis of group composition, particularly residual oil, asphalt product.This classical way is all excessive aspect sample size, solvent load, as, the toluene consumption of flushing aromatic hydrocarbons reaches hundreds of milliliters, causes the bigger pollution to operator and environment; The foundation of the simulation PONA analysis of standard pure sample also lacks.Thin layer-hydrogen flame method also can be carried out PONA analysis (chromatogram magazine,, 17 volumes, 4 phases, 372-375 page or leaf in 1999).The advantage of the method: (1), sample are dissolved in strong polarity thing (as tetrahydrofuran) part all can carry out four big hydrocarbon type tests, and this point had had breakthrough than in the past.PONA analysis scope to asphalt product enlarges to some extent, analyzes more representative.(2) sample and solvent load are few, poison little, analysis operation rapidly, convenient, instrumentation.But the deficiency of its maximum is to prepare enrichment section branch, do for Infrared spectroscopy, nuclear magnetic resonance, trace element analysis etc. and further deeply analyze and examine, and this is that the modern science development is necessary.
Summary of the invention
The purpose of this invention is to provide a kind of method of residual oil, pitch being carried out the PONA analysis of hydrocarbon system.
Analytical approach of the present invention comprises the steps:
(1) carrier pre-service, sample add
Silica gel for chromatography is activated 4-5 hour down for 180 ± 10 ℃ in muffle furnace; After the cooling, take by weighing 1.6 ± 0.1 grams and add in the chromatographic columns back and add 1.2 ± 0.1 and restrain in 400 ± 10 ℃ of aluminium oxide of 4-5 hour of activation down, accurately weighing 0.1100 ± 0.0100 gram pitch or residual oil sample inserted in the chromatographic column, adds 0.6 ± 0.1 gram aluminium oxide again;
Aforesaid silica gel is the 100-200 order, and subsidiary factory of Haiyang Chemical Plant, Qingdao produces.
Aforesaid chromatographic column is 90 millimeters of glass pipe ranges, and is interior through 6 millimeters, and the bottom reducing is 0.7 millimeter.
Aforesaid aluminium oxide is 0.047-0.147mm, Chinese Medicine group, and Shanghai chemical reagents corporation produces.
(2) chromatographic analysis process
(1) the 1st preparation section, the flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask, gets 20 milliliters of normal heptanes, divides 4 times and adds and collect the alkane section that flows out;
(2). the 2nd preparation section, the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask, by normal heptane: methylene chloride is 35 milliliters of the obtain solutions of 1: 2.5 volume ratio, divides the aromatic hydrocarbons section of 7 addings and collection outflow;
(3). the 3rd preparation section, the flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask, by methylene chloride: tetrahydrofuran is 30 milliliters of the solution of volume ratio preparation in 1: 3, divides the colloid section of 6 addings and collection outflow;
(4). the drying of preparation section branch and true amount: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60 ℃, solvent is drained and weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section;
(5). the computing formula of the group composition of hydrocarbon system
Alkane content (W%) in the sample=(the net increase weight/raw sample amount of alkane receiving flask) * 100%
Arene content in the sample (W%)=(the net increase weight/raw sample amount of aromatic hydrocarbons receiving flask) * 100%
(the W%=(the net increase weight/raw sample amount of nonhydrocarbon receiving flask) * 100% of gum level in the sample
Sample medium pitch matter content (W%)=100%-alkane content (W%)-arene content (W%)-non-hydrocarbon content (W%)
Use pure sample that the inventive method is carried out
Checking
1, selecting pure sample product 24 alkane (analyzes purely, Koch-ligh Laboratory company produces, and content is greater than 99%) is that the simulation of stable hydrocarbon is represented; Dibenzo [ah] anthracene (is analyzed pure.Fluka AG.Chem company produces.Content is greater than 98%) be the simulation representative of aromatic hydrocarbons; (content is greater than 99.0% for antifebrin.Shanghai chemical reagents corporation of Chinese Medicine group produces) be the representative of colloid; What standard application was represented in bitum simulation is the tetrahydrofuran insoluble of " Taiyuan Iron and Steel Co. " coal-tar pitch.
With 24 alkane, dibenzo [ah] anthracene, antifebrin, the tetrahydrofuran insoluble of coal-tar pitch and their potpourri weighing, the numerical value of institute's weighing sees Table 1.
Take by weighing silica gel 1.6 ± 0.1 grams and add in the chromatographic column, add 1.2 ± 0.1 gram aluminium oxide again.Load weighted pure sample product are inserted respectively in the chromatographic column, add 0.6 ± 0.1 gram aluminium oxide.The flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask.Get 20 milliliters of normal heptanes, divide to add and collect the alkane section (the 1st preparation section) that flows out for 4 times.The flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask.Preparation normal heptane/methylene chloride is 35 milliliters of the solution of 1/2.5 volume ratio, divides to add and collect the aromatic hydrocarbons section that flows out (the 2nd preparation section) for 7 times.The flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask.Preparation methylene chloride/tetrahydrofuran is 30 milliliters of the solution of 1/3 volume ratio, and its volume ratio is.Divide and add and collect the colloid section (the 3rd preparation section) that flows out for 6 times.. prepare section drying of dividing and really measure: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section.
2, addition and the collecting amount according to preparation can calculate and obtain the recovery and standard deviation, and concrete data can be referring to table 1.
The result is clearly visible from table 1, and the pure sample experiment presents the high recovery and low standard deviation.Mixing the recovery mean value join the sample experiment is 99.756%, and the standard deviation average be-0.1001%, and the pure sample recovery of testing is an average 99.443% separately, and the standard deviation average is-0.2.545%,
3, ultimate analysis-infrared spectrum-nuclear magnetic resonance examining to resolution
3.1. chromatographic resolution rate
The used instrument of ultimate analysis is Vario EL organic element analyzer (German FA EAS company), FT-80A nuclear, magnetic resonance device (U.S. Varian company).With the 9# compound sample is example, and its alkane section, aromatic hydrocarbons section, nonhydrocarbon (colloid) section have been carried out ultimate analysis, and the element theory value content of this measurement result and original molecule amount relatively can be weighed the size of resolution, and comparing data is listed in table 2.
Clearly visible by table 2, the measured value of the carbon that each collection section is divided, hydrogen, nitrogen content and carbon, hydrogen, the nitrogen content value (theoretical value) of corresponding pure sample are very approaching, therefore examine the clear zoning that the preparation section is divided from the ultimate analysis angle.
3.2. examining of Infrared spectroscopy coupled columns liquid chromatography resolution
Respectively 24 alkane, dibenzo [ah] anthracene and antifebrin pure sample are carried out Infrared spectroscopy, again each section branch (the 1st, the 2nd, the 3rd preparation section) of collecting through chromatographic column is carried out Infrared spectroscopy, compare collection of illustrative plates, can judge the chromatographic resolution rate of separating column.Used instrument is that EXCALIBUR SERIES infrared spectrometer (U.S. Diglab company) 4000 is to 500cm
-1Scope interscan transmitance reaches 64 times, and resolution is 4cm
-1
With the 10# compound sample is example, and typical comparison diagram is shown in Fig. 1.Label is that 1 figure is the infrared spectrogram of antifebrin pure sample among Fig. 1, and label is that 2 figure is the infrared spectrogram of the 3rd preparation section (colloid).Label is that 3 figure is the infrared spectrogram of dibenzo [ah] anthracene pure sample among Fig. 1, and label is that 4 figure is the infrared spectrogram of the 2nd preparation section (aromatic hydrocarbons).Label among Fig. 1 is that 5 figure is the infrared spectrogram of 24 alkane pure samples, and label is that 6 figure is the infrared spectrogram of the 1st preparation section (alkane).
Clearly visible from Fig. 1, diffuse reflectance infrared spectroscopy that the preparation section is divided and corresponding pure sample diffuse reflectance infrared spectroscopy are identical, and this shows that the post liquid chromatography has high chromatographic resolution rate.
Spectral resolution is examined 3.3. the hydrogen nuclear magnetic resonance analysis of spectrum is checked colors
Used instrument is FT-80A nuclear magnetic resonance analyser (U.S. Varian company).24 alkane, dibenzo [ah] anthracene and antifebrin pure sample are carried out nuclear magnetic resonance spectroscopy, the nmr spectrum that obtains compare with the collection of illustrative plates of collecting each section branch through chromatographic column, can judge the chromatographic resolution rate.With the 10# compound sample is example, and comparison diagram is shown in Fig. 2, and label is that 1 figure is the hydrogen nuclear magnetic resonance spectrogram of antifebrin pure sample among Fig. 2, and number in the figure is that 2 figure is that the 3rd preparation section is divided the hydrogen nuclear magnetic resonance spectrogram of (colloid).The figure of the label 3 among Fig. 2 is the hydrogen nuclear magnetic resonance spectrogram of dibenzo [ah] anthracene pure sample, and the figure of label 4 is the hydrogen nuclear magnetic resonance spectrogram of the 2nd preparation section (aromatic hydrocarbons).The figure of the label 5 among Fig. 2 is hydrogen nuclear magnetic resonance spectrograms of 24 alkane pure samples, and the figure of label 6 is the hydrogen nuclear magnetic resonance spectrogram of the 1st preparation section (alkane).
Clearly visible from Fig. 1, nuclear magnetic resonance that each preparation section is divided and corresponding pure sample the hydrogen spectrogram of nuclear magnetic resonance identical, this reconfirms that used post liquid chromatography has high chromatographic resolution rate.
Above-mentioned ultimate analysis, Infrared spectroscopy and nuclear magnetic resonance spectroscopy result have confirmed all sidedly that not only method center pillar liquid chromatography has high chromatographic resolution rate, and this is the assurance of sample separation.In addition, confirmed that also institute's construction method has analysis and two functions of preparation type, the section that experiment provides divides a preparation amount to guarantee that Other Instruments is used.
The present invention compared with prior art has following advantage:
1. body of the present invention has shown advanced hydrocarbon system's classificating thought: in this method as simulated compound-dibenzanthracene [ah], antifebrin.In hexane, be insolubles, but be present in the pitch really, so this method is more comprehensive to the sign of sample, advanced, science.The present invention is based upon on the experiment basis of simulation pure sample; Analysis to full pattern is also examined with other modern instrument, and therefore, method has substantial theoretical foundation.
2.. the present invention has good adaptability to residual oil and pitch class sample: because the present invention has the advantages that to analyze the preparation type of holding concurrently, analyze the foundation that data can be used as the process exploitation of asphalt product, prepare enrichment section branch, do for Infrared spectroscopy, nuclear magnetic resonance, trace element analysis etc. and further deeply analyze and examine.Pitch class sample lacks capable analytical approach always, and this law has remedied some shortcomings, is the method with actual application value.
3. in should inventing, solvent for use toxicity is little, consumption is few, is the method for " green, safety and economy ".
Description of drawings
Fig. 1 is the comparison diagram of the infrared spectrum of the infrared spectrum of collect after chromatographic column is separated three preparation sections of 24 alkane, dibenzo [ah] anthracene and antifebrin mixing pure sample and original each pure sample.Fig. 2 is three comparison diagrams that prepare the proton nmr spectra of section proton nmr spectra that divides and original each pure sample that 24 alkane, dibenzo [ah] anthracene and antifebrin mixing pure sample are collected after chromatographic column is separated.Fig. 3 is the infrared spectrogram of 13# pitch sample the 1st preparation section (alkane), and Fig. 4 is the infrared spectrogram of 13# the 2nd preparation section (aromatic hydrocarbons), and Fig. 5 is the infrared spectrogram of 13# the 3rd preparation section (colloid).
Embodiment
Embodiment 1: be numbered 11# (pitch sample), it derives from coal and catalytic cracked oil pulp refines the processing product altogether.In its technological process, coal: oil=1: 1, used the catalyzer of iron content.
Take by weighing silica gel 1.614 grams and add in the chromatographic column, add 1.103 gram aluminium oxide again.Sample 0.1103 gram is inserted in the chromatographic column, adds 0.5622 gram aluminium oxide.The flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask.Get 20 milliliters of normal heptanes, divide 4 addings.. the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask.35 milliliters of preparation normal heptane/methylene chloride (1/2.5) solution divide 7 times and add and collect the aromatic hydrocarbons section that flows out.The flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask.30 milliliters of preparation methylene chloride/tetrahydrofuran (1/3) solution, its volume ratio is.Divide 6 times and add and collect the colloid section that flows out.. prepare section drying of dividing and really measure: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section.The process of another parallel sample identical (summary), gained the results are shown in table 3.
Embodiment 2: being numbered the residual oil sample of 12#, is the refinery cracked oil distillation bottoms that obtains
Take by weighing silica gel 1.700 grams and add in the chromatographic column, add 1.183 gram aluminium oxide again.Sample 0.1211 gram is inserted in the chromatographic column, adds 0.5982 gram aluminium oxide.. the flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask.Get 20 milliliters of normal heptanes, divide 4 addings.. the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask.35 milliliters of preparation normal heptane/methylene chloride (1/2.5) solution divide 7 times and add and collect the aromatic hydrocarbons section that flows out.The flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask.30 milliliters of preparation methylene chloride/tetrahydrofuran (1/3) solution, its volume ratio is.Divide 6 times and add and collect the colloid section that flows out.. prepare section drying of dividing and really measure: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section.The process of another parallel sample identical (summary), gained the results are shown in table 3.
Embodiment 3: be numbered 13# (pitch sample), it is that coal and catalytic cracked oil pulp refine the toluene insolubles of handling product, coal in its technological process altogether: oil=1: 1, useless catalyzer.
Take by weighing silica gel 1.512 grams and add in the chromatographic column, add 1.233 gram aluminium oxide again.Sample 0.10561 gram is inserted in the chromatographic column, adds 0.5822 gram aluminium oxide.. the flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask.Get 20 milliliters of normal heptanes, divide 4 addings.. the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask.35 milliliters of preparation normal heptane/methylene chloride (1/2.5) solution divide 7 times and add and collect the aromatic hydrocarbons section that flows out.The flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask.30 milliliters of preparation methylene chloride/tetrahydrofuran (1/3) solution, its volume ratio is.Divide 6 times and add and collect the colloid section that flows out.. prepare section drying of dividing and really measure: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section.The process of another parallel sample identical (summary), gained the results are shown in table 3.
Embodiment 4: sample number into spectrum is the rock asphalt in special upright nit lake.
Take by weighing silica gel 1.531 grams and add in the chromatographic column, add 12983 gram aluminium oxide again.Sample 0.1143 gram is inserted in the chromatographic column, adds 0.6912 gram aluminium oxide.. the flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask.Get 20 milliliters of normal heptanes, divide 4 addings.. the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask.35 milliliters of preparation normal heptane/methylene chloride (1/2.5) solution divide 7 times and add and collect the aromatic hydrocarbons section that flows out.The flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask.30 milliliters of preparation methylene chloride/tetrahydrofuran (1/3) solution, its volume ratio is.Divide 6 times and add and collect the colloid section that flows out.. prepare section drying of dividing and really measure: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section.The process of another parallel sample identical (summary), gained the results are shown in table 3.
Table 1 pure sample is joined sample and is compared with the section of purchasing branch measurement result
Join sample pure reagent weighing configuration assay content standard deviation recovery % numbering
g W
1％ W
2％
Independent pure sample 24 alkane 0.0547 100 98.095-1.905 98.095 1#
24 alkane 0.0508 100 97.964-2.036,97.964 2#
Dibenzo [ah] anthracene 0.0420 100 98.095-1.805 98.095 3#
Dibenzo [ah] anthracene 0.0442 100 97.964-2.036 97.964 4#
Antifebrin 0.0875 100 97.600-2.400 97.600 5#
Antifebrin 0.0365 100 96.438-3.562 96.438 6#
Tetrahydrofuran insoluble 0.0395 100 94.937-5.063 94.937 7#
Tetrahydrofuran insoluble 0.0387 100 98.450-1.550 98.450 8#
On average-2.545 97443
Mix pure sample 24 alkane 0.0311 27.154 26.658-0.496 98.173 9#
Dibenzo [ah] anthracene 0.0259 22.629 20.909-1.720 92.399 9#
Antifebrin 0.0314 27.402 26.843-0.559 97.853 9#
Tetrahydrofuran insoluble 0.0261 22.815 24.790 1.975 108.657 9#
Mix pure sample 24 alkane 0.0285 26.571 25.638-0.933 96.489 10#
Dibenzo [ah] anthracene 0.0294 27.402 26.843-0.559 97.960 10#
Antifebrin 0.0247 23.024 22.642-0.382 98.341 10#
Tetrahydrofuran insoluble 0.0247 23.003 24.886 1.883 108.186 10#
Average 0.1001 99.756
(compound sample)
Standard deviation: W
2%-W
1%, recovery %:W
2%/W
1%
Table 2 pure sample product compare with the ultimate analysis of the section of purchasing
Relatively 24 alkane preparation section dibenzo [ah] anthracene prepares section antifebrin preparation section
Carbon content, C% 85.714 84.695 94.964 93.170 71.111 72..32
Hydrogen content, H% 14.286 13.710 5.036 5.550 6.667 6.595
Oxygen level, O% 11.852 10.990
Nitrogen content, N% 10.370 10.095
The hydrocarbon system of table 3 residual oil, pitch full pattern (W%) measurement result
Sample number project stable hydrocarbon aromatic hydrocarbons gum asphalt
11# measures (1) 5.496 60.154 17.327 17.023
Measure (2) 4.986 58.230 20.128 15.855
Average W% 5.241 59.191 18.727 16.439
Deviation % 0.255 0.961 1.401 0.584
12# measures (1) 9.950 21.379 52.906 15.765
Measure (2) 8.001 22.087 52.348 17.554
Average W% 8.975 21.733 52.627 16.659
Deviation % 0.974 0.354 0.279 0.895
13# measures (1) 7.375 66.379 23.659 2.586
Measure (2) 8.497 67.984 20.850 2.668
Average W% 7.936 67.182 22.254 2.627
Deviation % 0.561 0.802 1.404 0.041
14# measures (1) 5.496 60.154 17.327 17.023
Measure (2) 4.986 58.230 20.928 15.855
Average W% 5.241 59.191 19.128 16.439
Deviation % 0.255 0.961 1.800 0.584
Claims (4)
1, the PONA analysis method of a kind of residual oil, pitch hydrocarbon system is characterized in that comprising the steps:
(1) carrier pre-service, sample add
Silica gel for chromatography is activated 4-5 hour down for 180 ± 10 ℃ in muffle furnace; After the cooling, take by weighing 1.6 ± 0.1 grams and add in the chromatographic columns back and add 1.2 ± 0.1 and restrain in 400 ± 10 ℃ of aluminium oxide of 4-5 hour of activation down, accurately weighing 0.1100 ± 0.0100 gram pitch or residual oil sample inserted in the chromatographic column, adds 0.6 ± 0.1 gram aluminium oxide again;
(2) chromatographic analysis process
(1) flushing of alkane and collection in the sample: after the chromatographic column vertical fixing of getting ready, bottom inserts a dry section of crossing of accurate weighing and divides receiving flask, gets 20 milliliters of normal heptanes, divides 4 times and adds and collect the alkane section that flows out;
(2). the flushing of aromatic hydrocarbons and collection in the sample: after treating that normal heptane has been collected alkane, change another receiving flask, by normal heptane: methylene chloride is 35 milliliters of the obtain solutions of 1: 2.5 volume ratio, divides 7 times and adds and collect the aromatic hydrocarbons section that flows out;
(3). the flushing of colloid and collection in the sample: after treating that the aromatic hydrocarbons section has been collected, change another receiving flask, by methylene chloride: tetrahydrofuran is 30 milliliters of the solution of volume ratio preparation in 1: 3, divides the colloid section that adds and collect outflow for 6 times;
(4). the drying of preparation section branch and true amount: above-mentioned three receiving flasks are put into the air extractor that temperature is lower than 60C, solvent is drained and weight, accurate each receiving flask of weighing, the weightening finish of each receiving flask is each net weight for preparing section;
(5). the computing formula of the group composition of hydrocarbon system
Alkane content (W%) in the sample=(the net increase weight/raw sample amount of alkane receiving flask) * 100%
Arene content in the sample (W%)=(the net increase weight/raw sample amount of aromatic hydrocarbons receiving flask) * 100%
(the W%=(the net increase weight/raw sample amount of nonhydrocarbon receiving flask) * 100% of gum level in the sample
Sample medium pitch matter content (W%)=100%-alkane content (W%)-arene content (W%)-non-hydrocarbon content (W%)
2, the PONA analysis method of a kind of residual oil as claimed in claim 1, pitch hydrocarbon system is characterized in that described silica gel is the 100-200 order, and subsidiary factory of Haiyang Chemical Plant, Qingdao produces.
3, the PONA analysis method of a kind of residual oil as claimed in claim 1, pitch hydrocarbon system is characterized in that described chromatographic column is 90 millimeters of glass pipe ranges, and interior through 6 millimeters, the bottom reducing is 0.7 millimeter.
4, the PONA analysis method of a kind of residual oil as claimed in claim 1, pitch hydrocarbon system is characterized in that described aluminium oxide is 0.047-0.147mm, Chinese Medicine group, and Shanghai chemical reagents corporation produces.
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| US4671103A (en) * | 1985-04-08 | 1987-06-09 | Exxon Chemical Patents Inc. | Method for determining crude oil fouling by high performance liquid chromatography |
| CN1118702C (en) * | 1999-05-24 | 2003-08-20 | 中国科学院山西煤炭化学研究所 | High-efficiency liquid-phase chromatographic analysis of asphaltine |
| CN1181340C (en) * | 2001-12-27 | 2004-12-22 | 中国科学院山西煤炭化学研究所 | Analysis method of hydrocarbon composition in asphalt, heavy oil and tar |
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