CN110470749A - A method of the analysis thick aromatic hydrocarbons boiling range of carbon ten - Google Patents
A method of the analysis thick aromatic hydrocarbons boiling range of carbon ten Download PDFInfo
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- CN110470749A CN110470749A CN201810450299.9A CN201810450299A CN110470749A CN 110470749 A CN110470749 A CN 110470749A CN 201810450299 A CN201810450299 A CN 201810450299A CN 110470749 A CN110470749 A CN 110470749A
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- retention time
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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
Abstract
The present invention relates to Measurement of distilled process fields, disclose a kind of method for analyzing the thick aromatic hydrocarbons boiling range of carbon ten, wherein, the described method includes: (1) is under conditions of linear temperature program, with the retention time of each component in gas chromatograph for determination C5-C44 normal paraffin mixture standard sample, and obtain boiling point-retention time correction curve；(2) under testing conditions identical with step (1), the thick aromatic hydrocarbons sample of carbon ten is detected with gas chromatograph, the thick aromatic hydrocarbons sample of the carbon ten obtains chromatogram after entering detector, carries out slice integral to the chromatogram, obtains sample Percent yield-retention time relation curve；(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines boiling point corresponding to corresponding sample Percent yield to get the boiling range of the thick aromatic hydrocarbons of carbon ten is arrived.Method analysis time of the invention is short, and easy to operate, environmental pollution is small, and more efficient, associated maintenance is easier.
Description
Technical field
The present invention relates to Measurement of distilled process fields, and in particular, to a method of the analysis thick aromatic hydrocarbons boiling range of carbon ten.
Background technique
The thick aromatic hydrocarbons of carbon ten produced in different oil refining devices has different purposes, the predominantly comprehensive benefit of the thick aromatic hydrocarbons of carbon ten
With and its deep processing product it is different, by the parting core index using 210 DEG C of recovery volumes as the thick aromatic hydrocarbons of carbon ten, be arranged I, II
Two models.
The boiling range method of the GB/T6536 measurement thick aromatic hydrocarbons of carbon ten is: taking 100mL sample, is steamed with certain distillation speed
It evaporates, records initial boiling point, distillation yield 5%, 10%, 90% and midbarrel and do or the thermometer of decomposition point or the end point of distillation
Reading, data obtain boiling range after being corrected.This method labor efficiency is low, high to analyst's skill requirement, causes serious pollution to the environment.
Summary of the invention
The purpose of the present invention is overcome in the prior art measure the thick aromatic hydrocarbons boiling range of carbon ten method low efficiency, it is heavy-polluted lack
It falls into, a kind of method for analyzing the thick aromatic hydrocarbons boiling range of carbon ten is provided.
To achieve the goals above, the present invention provides a kind of method for analyzing the thick aromatic hydrocarbons boiling range of carbon ten, wherein the method
Include:
(1) under conditions of linear temperature program, with gas chromatograph for determination C5-C44 normal paraffin mixture standard sample
The retention time of each component in product, and obtain boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), the thick aromatic hydrocarbons sample of carbon ten, the carbon are detected with gas chromatograph
Each component in ten thick aromatic hydrocarbons samples is successively separated by boiling point, into detector after obtain chromatogram, to the chromatogram carry out
Slice integral, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines phase
Boiling point corresponding to the sample Percent yield answered is to get the boiling range for arriving the thick aromatic hydrocarbons of carbon ten.
The method of the invention analysis time is short, easy to operate, and environmental pollution is small, more efficient, the phase of instrument analysis
It is easier to close maintenance；Also, compared with standard method (GB/T6536), the result of this method is essentially identical to the weight of standard method
Renaturation and reproducibility.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of method for analyzing the thick aromatic hydrocarbons boiling range of carbon ten, wherein the described method includes:
(1) under conditions of linear temperature program, with gas chromatograph for determination C5-C44 normal paraffin mixture standard sample
The retention time of each component in product, and obtain boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), the thick aromatic hydrocarbons sample of carbon ten, the carbon are detected with gas chromatograph
Each component in ten thick aromatic hydrocarbons samples is successively separated by boiling point, into detector after obtain chromatogram, to the chromatogram carry out
Slice integral, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines phase
Boiling point corresponding to the sample Percent yield answered is to get the boiling range for arriving the thick aromatic hydrocarbons of carbon ten.
In the present invention, " sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve "
Refer to when obtaining reservation corresponding to corresponding sample Percent yield from the sample Percent yield-retention time relation curve
Between, then from boiling point-retention time correction curve boiling point corresponding to the retention time is found, corresponding sample can be obtained
Boiling point corresponding to Percent yield.
In the present invention, the condition of the linear temperature program includes: chromatogram column temperature: initial temperature is 55-65 DEG C, with
The heating rate of 34-36 DEG C/min is warming up to 350-360 DEG C；Temperature of vaporization chamber: initial temperature is 100-110 DEG C；With 34-36
DEG C/min rate rises to 350-360 DEG C, and constant temperature 1-2min；Detection room temperature: 350-360 DEG C of constant temperature.In above-mentioned linear program
Under conditions of heating, the thick aromatic hydrocarbons boiling range of carbon ten measured can be made more acurrate.
In the present invention, the C5-C44 normal paraffin mixture standard sample can be commercially available, such as can be
The Sinopec Research Institute of Petro-Chemical Engineering trade mark is the commercially available product of DX-1k.If commercially available C5-C44 normal paraffin mixture
Standard sample excessive concentration is unable to accurate calibration, then measures again after can diluting standard sample.
In the present invention, " carrying out slice integral to the chromatogram " in step (2) usually can be by gas-chromatography work
Make the included function in station to implement.
In the present invention, in step (1) and step (2), the detector of gas chromatograph is preferably hydrogen flameionization detection
Device.
In the present invention, the condition of the gas-chromatography can be the selection of this field routine, under preferable case, gas-chromatography
The condition of instrument can also include: that carrier gas is helium, flow 25-27mL/min；Combustion gas is hydrogen, flow 34-36mL/min；
Combustion-supporting gas is argon gas, flow 340-360mL/min.
In the present invention, the chromatographic column in gas chromatograph is nonpolar gas chromatographic column.The chromatographic column is conducive to detect
The boiling range of the thick aromatic hydrocarbons of multi-component carbon ten.
In the present invention, the sample volume of the gas chromatograph can be determined according to appearance situation, the gas chromatograph
Sample volume it is too many, will lead to and occur tack peak in gas phase spectrogram, spectrogram inaccuracy, and the sample volume of the gas chromatograph is too
Few, the peak area occurred in gas phase spectrogram is too small or chromatographic column cannot respond to, and can not obtain accurate data.Preferable case
Under, in step (1) and step (2), the sample volume of gas chromatograph is 1.4-1.6mL.
The present invention will be described in detail by way of examples below.In following embodiment and comparative example,
Gas chromatograph is the product of agilent company model 7890A；
The product that gas chromatographic column in gas chromatograph is agilent company model HP-1；
Chromatographic work station is the Simdis data processing software of AC analysis and Control Co., Ltd, Holland；
The detector of gas chromatograph is flame ionization ditector；
C5-C44 normal paraffin mixture standard sample is purchased from Sinopec Research Institute of Petro-Chemical Engineering, trade mark DX-
1k；
The thick aromatic hydrocarbons sample 1 of carbon ten comes from China petroleum Chemicals Co., Ltd. Town Hai Lian Hua branched Corporation disproportionation device；
The thick aromatic hydrocarbons sample 2 of carbon ten comes from Sinopec Group's Yangtze petrochemical industry branch company aromatic device.
Embodiment 1
(1) condition of linear temperature program is set on gas chromatograph are as follows: initial temperature is 65 DEG C, with 36 DEG C/min
Heating rate be warming up to 360 DEG C；Temperature of vaporization chamber: initial temperature is 110 DEG C；360 DEG C are risen to 36 DEG C/min rate, and permanent
Warm 2min；Detection room temperature: 360 DEG C of constant temperature.Carrier gas is helium, flow 27mL/min；Combustion gas is hydrogen, flow 36mL/
min；Combustion-supporting gas is argon gas, flow 360mL/min.After gas chromatograph brings into operation, by autosampler by 1.6mL
C5-C44 normal paraffin mixture standard sample inject gas chromatograph, measure C5-C44 normal paraffin mixture standard sample
The retention time of middle each component obtains boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), by autosampler by the thick aromatic hydrocarbons sample 1 of carbon ten of 1.6mL
Inject gas chromatograph, each component in the thick aromatic hydrocarbons sample 1 of the carbon ten is successively separated by boiling point, into detector after obtain color
Spectrogram carries out slice integral to the chromatogram, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines phase
Boiling point corresponding to the sample Percent yield answered is to get the boiling range for arriving the thick aromatic hydrocarbons 1 of carbon ten.The results are shown in Table 1.
Embodiment 2
(1) condition of linear temperature program is set on gas chromatograph are as follows: initial temperature is 55 DEG C, with 34 DEG C/min
Heating rate be warming up to 350 DEG C；Temperature of vaporization chamber: initial temperature is 100 DEG C；350 DEG C are risen to 34 DEG C/min rate, and permanent
Warm 1min；Detection room temperature: 350 DEG C of constant temperature.Carrier gas is helium, flow 25mL/min；Combustion gas is hydrogen, flow 35mL/
min；Combustion-supporting gas is argon gas, flow 350mL/min.After gas chromatograph brings into operation, by autosampler by 1.4mL
C5-C44 normal paraffin mixture standard sample inject gas chromatograph, measure C5-C44 normal paraffin mixture standard sample
The retention time of middle each component obtains boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), by autosampler by the thick aromatic hydrocarbons sample 2 of carbon ten of 1.4mL
Inject gas chromatograph, each component in the thick aromatic hydrocarbons sample 2 of the carbon ten is successively separated by boiling point, into detector after obtain color
Spectrogram carries out slice integral to the chromatogram, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines phase
Boiling point corresponding to the sample Percent yield answered is to get the boiling range for arriving the thick aromatic hydrocarbons 2 of carbon ten.The results are shown in Table 1.
Embodiment 3
(1) condition of linear temperature program is set on gas chromatograph are as follows: initial temperature is 60 DEG C, with 35 DEG C/min
Heating rate be warming up to 355 DEG C；Temperature of vaporization chamber: initial temperature is 105 DEG C；355 DEG C are risen to 35 DEG C/min rate, and permanent
Warm 1min；Detection room temperature: 355 DEG C of constant temperature.Carrier gas is helium, flow 26mL/min；Combustion gas is hydrogen, flow 34mL/
min；Combustion-supporting gas is argon gas, flow 340mL/min.After gas chromatograph brings into operation, by autosampler by 1.5mL
C5-C44 normal paraffin mixture standard sample inject gas chromatograph, measure C5-C44 normal paraffin mixture standard sample
The retention time of middle each component obtains boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), by autosampler by the thick aromatic hydrocarbons sample 2 of carbon ten of 1.5mL
Inject gas chromatograph, each component in the thick aromatic hydrocarbons sample 2 of the carbon ten is successively separated by boiling point, into detector after obtain color
Spectrogram carries out slice integral to the chromatogram, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, determines phase
Boiling point corresponding to the sample Percent yield answered is to get the boiling range for arriving the thick aromatic hydrocarbons 2 of carbon ten.The results are shown in Table 1.
Embodiment 4-6
Embodiment 4-6 repeats all processes of embodiment 1 respectively, detects the repeatability and reproduction of the method for the invention
Property.
Comparative example 1-3
Measure the thick aromatic hydrocarbons sample 1 of carbon ten, the thick aromatic hydrocarbons sample 2 of carbon ten and the thick aromatic hydrocarbons sample 3 of carbon ten respectively according to GB/T6536
Boiling range, the results are shown in Table 1.
Comparative example 4
The thick aromatic hydrocarbons boiling range of carbon ten is analyzed according to the method for embodiment 1, unlike, the item of linear temperature program is not used
Temperature condition is directly arranged in part on gas chromatograph are as follows: chromatogram column temperature is 350-360 DEG C；Temperature of vaporization chamber is 350-360
DEG C, and constant temperature 1-2min；Detection room temperature: 350-360 DEG C of constant temperature.The results are shown in Table 1.
Table 1
The measurement result of the method for the invention and the measurement result of GB/T6536 are basic it can be seen from the result of table 1
It is identical.The method of the invention has preferable repeatability and reproduces it can be seen from embodiment 1 and the result of embodiment 4-6
Property.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (6)
1. a kind of method for analyzing the thick aromatic hydrocarbons boiling range of carbon ten, which is characterized in that the described method includes:
(1) under conditions of linear temperature program, in gas chromatograph for determination C5-C44 normal paraffin mixture standard sample
The retention time of each component, and obtain boiling point-retention time correction curve；
(2) under testing conditions identical with step (1), the thick aromatic hydrocarbons sample of carbon ten is detected with gas chromatograph, the carbon ten is thick
Each component in aromatic hydrocarbons sample is successively separated by boiling point, into detector after obtain chromatogram, the chromatogram is sliced
Integral, obtains sample Percent yield-retention time relation curve；
(3) sample Percent yield-retention time relation curve is associated with boiling point-retention time correction curve, is determined corresponding
Boiling point corresponding to sample Percent yield obtains the boiling range of the thick aromatic hydrocarbons of carbon ten.
2. according to the method described in claim 1, wherein, the condition of the linear temperature program includes: chromatogram column temperature: initial
Temperature is 55-65 DEG C, is warming up to 350-360 DEG C with the heating rate of 34-36 DEG C/min；Temperature of vaporization chamber: initial temperature is
100-110℃；350-360 DEG C, and constant temperature 1-2min are risen to 34-36 DEG C/min rate；Detect room temperature: constant temperature 350-360
℃。
3. method according to claim 1 or 2, wherein in step (1) and step (2), the detector of gas chromatograph is
Flame ionization ditector.
4. method according to claim 1 or 2, wherein the condition of gas chromatograph further include: carrier gas is helium, flow
For 25-27mL/min；Combustion gas is hydrogen, flow 34-36mL/min；Combustion-supporting gas is argon gas, flow 340-360mL/min.
5. method according to claim 1 or 2, wherein the chromatographic column in gas chromatograph is nonpolar gas chromatographic column.
6. method according to claim 1 or 2, wherein in step (1) and step (2), the sample volume of gas chromatograph is
1.4-1.6mL。
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2018
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|---|---|---|---|---|
| EP0833155A1 (en) * | 1996-09-12 | 1998-04-01 | Exxon Research And Engineering Company | Determining true boiling point curves for a crude oil or fraction |
| CN101275932A (en) * | 2007-03-30 | 2008-10-01 | 中国石油化工股份有限公司 | Pulse micro-inverse product yield on-line simulation distil analysis method |
| WO2011115678A1 (en) * | 2010-03-19 | 2011-09-22 | Thiosolv, L.L.C. | Systems and processes for improving distillate yield and quality |
| CN103995061A (en) * | 2013-02-20 | 2014-08-20 | 中国石油化工股份有限公司 | Analysis method for hydrocarbon composition of diesel fraction and heavy oil fraction in micro-reaction liquid product |
| CN104569257A (en) * | 2014-12-23 | 2015-04-29 | 武汉钢铁(集团)公司 | Gas chromatograph determination method of coking scrubbing oil distillation range |
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