CN1566944A - Method for analyzing composition of refinery gas by employing multiple column parallel gas-chromatography instrument - Google Patents
Method for analyzing composition of refinery gas by employing multiple column parallel gas-chromatography instrument Download PDFInfo
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Abstract
A multiple parallel columns gas chromatographic analysis method for the refinery gas components, comprises the following: to flow air sample into four parallel chromatogram columns A to D each with an independent air-in mouth and gas chromatographic device, wherein, A to C has top separating column and back-blowing system; to measure oxygen, nitrogen, methane, or carbon monoxide by column A; to measure carbon dioxide, ethylene, ethane or sulfureted hydrogen by column B; to measure C-[3]-C-[4] hydrocarbon and C-[5] alkyl hydrocarbon by column C; to measure all components of sample air by column D by the relevant values in each column calculated by computer and to get relevant value in column D and altogether calculate the each component value of the sample.
Description
Technical field
The present invention is a kind of method of utilizing the parallel gas chromatograph analytical gas of multicolumn to form.Specifically, be on the parallel chromatograph of multicolumn, to measure the method that refinery gas is formed with the expansion normalization method.
Background technology
The refinery gas analysis is the conventional analysis project of petrochemical field, and its composition is the significant data that instructs process condition and carry out technology Calculation.Refinery gas generally includes permanent gases and hydro carbons, and permanent gases mainly contains: oxygen, nitrogen, carbon monoxide, carbon dioxide etc., hydro carbons mainly comprises C
1～C
4Lower carbon number hydrocarbons and C
5～C
7Lighter hydrocarbons.Refinery gas is divided into catalytic reforming (CR) gas, catalytic cracked gas, thermal cracking gas etc. according to the processing technology difference, and the composition of different process institute aerogenesis is also inequality.Using more general means of testing at present is the multidimensional gas chromatographic analytical approach that adopts many valves of multicolumn combination technique, the characteristics of these class methods are that many root chromatogram columns are switched the back series connection by valve, and then obtain an analysis of spectra by the detecting device detection by quantitative, the general correction normalization method that adopts carries out quantitative test, all needs 15～45 minutes approximately analysis times.
In recent years, the fine inner diameter capillary column express-analysis technology parallel fast gas chromatograph analysis system of the polychromatic spectrum post that grows up that combines with the chip micro-processing technology provides the analytical approach of another kind of refinery gas.Owing to adopted the design of pre-column blowback parallel detection, analytical cycle is shortened greatly, only be 160 seconds.But the parallel analysis mode of polychromatic spectrum post obtains many analysis of spectra of each chromatographic column.Existing method all is according to many chromatograms that provide, and the external standard method that adopts single-point or multiple spot to proofread and correct is carried out quantitative test.So-called external standard analytical approach promptly is to test forming known standard gas sample earlier, obtain analyzing in each analysis of spectra the peak area value of component, then under same test condition, gas to be measured is tested, the peak area value of each component is wherein compared with the peak area of the corresponding component of standard gas, can obtain each components contents of gas to be measured.The normalization method that external standard adopts is to carry out normalizing according to the component concentration that records to calculate, can not adopt the correction normalizing, because proofreading and correct normalization method can only all occur just can using in same spectrogram by all components in sample, that is to say, be under the situation that tested gas all components all distillates in same chromatographic column could be effectively.
The analytical approach of the outer marking quantitative that the parallel chromatograph of above-mentioned multicolumn adopts is a kind of absolute quantivative approach.In the practical application, each mensuration all need be used standard sample, and wants the each chromatographic run condition of analyzing of strict control, guarantees consistent with the standard sample test condition.Therefore, stability of instrument and analyst's operant level is had relatively high expectations.Since the operating conditions of chromatogram during test, as the response performance of detecting device, column temperature, flow velocity, sample size, post effects etc. are difficult to identical, therefore occur bigger error easily.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts expansion normalization method analysis of refinery gases to form with the parallel chromatograph of multicolumn, this method standard gas sample consumption is few, simple to operate and quick, accurate.
The present invention is a benchmark with a related chromatographic column of the parallel chromatogram of multicolumn, detection response with reference to other chromatographic column, try to achieve the detection response of related each component of chromatographic column, adopt the expansion normalization method to try to achieve each component concentration then, solved each component of related chromatographic column is difficult to determine each component response owing to mixed peak problem effectively.Compare with external standard method, the present invention has reduced the use amount of standard gas sample to greatest extent, has reduced application cost, has avoided the influence to analysis result of sample size and chromatographiccondition, has increased test accuracy.
The method that the parallel gas chromatographic analysis refinery gas of multicolumn provided by the invention is formed comprises the steps:
(1) sample gas is fed in the gas chromatography with four parallel chromatographic column A～D detects, each chromatographic column all has independently injection port and detecting device, wherein chromatographic column A～C all has pre-separation post and blowback system, oxygen, nitrogen, methane and/or carbon monoxide in the chromatographic column A test sample gas, chromatographic column B detects carbon dioxide, ethene, ethane and/or sulfuretted hydrogen, and chromatographic column C detects C
3～C
4Hydro carbons and C
5Alkane, chromatographic column D test sample gas all components,
(2) determine in the ratio of each component overall response value of each the component response that detects in each chromatographic column spectrogram of A～C and detection and the chromatographic column D spectrogram respectively summation with A～corresponding response of C chromatographic column detected components, thereby determine the response of each component in chromatographic column D spectrogram
(3) according to the response of each component in chromatographic column D spectrogram, try to achieve each components contents in the sample with the correction normalization method.
Description of drawings
Fig. 1 is the spectrogram of chromatographic column A when analyzing catalytic cracked gas in the example of the present invention.
Fig. 2 is the spectrogram of chromatographic column B when analyzing catalytic cracked gas in the example of the present invention.
Fig. 3 is the spectrogram of chromatographic column C when analyzing catalytic cracked gas in the example of the present invention.
Fig. 4 is the spectrogram of chromatographic column D when analyzing catalytic cracked gas in the example of the present invention.
Embodiment
Four parallel chromatographic columns are capillary chromatographic column in the described chromatograph, and wherein chromatographic column D is that wall is coated with stain open pipe capillary column, and chromatographic column A～C is porous layer open pipe capillary column.Each chromatographic column mutually and connect, injection port all communicates with total injection port, used detecting device is thermal conductivity detector (TCD).For satisfying the needs of different component gas analysis, the different stationary phase of each chromatographic column filling.The stationary phase of chromatographic column A is the 5A molecular sieve, and the stationary phase of its pre-separation post is the NaX molecular sieve, 0.32 millimeter of column internal diameter, 30 microns of thickness; The stationary phase of chromatographic column B is Porpark U, and the stationary phase of its pre-separation post is Porpark Q, 0.32 millimeter of column internal diameter, 10 microns of thickness; The stationary phase of chromatographic column C and its pre-separation post is aluminium oxide, 0.32 millimeter of column internal diameter, 8 microns of thickness; The stationary phase of chromatographic column D is OV-1,0.15 millimeter of column internal diameter, 2 microns of thickness.
The pre-separation post of described chromatographic column will not need the component analyzed and the component of interference analysis to be retained in wherein, make need the component stream measured by analysis post detect.Retained fraction in the pre-separation post is discharged system by back-flushing valve.Can determine the retained fraction of each pre-separation post by the adjustment blowback time.In addition, the component that the pre-separation post will need not be measured is removed, and makes each chromatographic column measure different components targetedly, can shorten omnidistance analysis time.Chromatographic column A pre-separation post of the present invention is used for the component of retained gas sample except that permanent gas and methane, and the retained fraction of chromatographic column B pre-separation post is the above all components of C4, and the retained fraction of chromatographic column C pre-column is the above heavy constituent of C5 alkene.Chromatographic column D does not have the pre-separation post, so all components all has response in the sample gas in this post spectrogram, available peak area is represented, but lighter gas composition, as permanent gases be lower than C
5Hydrocarbon in this spectrogram, be prone to mixed peak, can not directly calculate each component concentration with the correction normalization method.Therefore, be respectively determine the ratio of the overall response value of the response of each chromatographic column detected components and this chromatographic column detected components by the analysis of spectra of A～C post, that determines A～C post detected components again on the analysis of spectra of related chromatographic column D goes out the zone, peak.By each regional peak area summation, calculate the actual peak area that each component is occupied in the D spectrogram, calculate each component concentration with the expansion normalization method again.Concrete grammar is as follows:
Each component response of A～C post accounts for the ratio of the total component response of this chromatographic column
In the formula, R
XiThe peak area of arbitrary component i that-A～C chromatographic column detects accounts for the number percent that this chromatographic column detects each component total peak area,
X-A, B or C chromatographic column,
S
iThe peak area of arbitrary component i that-X chromatographic column detects,
∑ S
XEach component peaks area summation that-X chromatographic column detects.
On the spectrogram of chromatographic column D, determine to go out the zone, peak, total peak area and R that each regional peak area is added and obtains corresponding to A, B, C chromatographic column detected components
XiMultiply each other, promptly obtain the peak area value of arbitrary component in the gas sample, promptly
Si(D)＝S
X×R
Xi
Si in the formula (D)-arbitrary component i shared actual peak area in the D spectrogram,
S
XIn-D the spectrogram corresponding to the total peak area of X chromatographic column detected components,
When refinery gas is analyzed, for C
5The above component of alkene generally only provides total content.That is to say, only need the C in the chromatographic column D spectrogram
5Alkene, C
6The peak area of above hydrocarbon component adds and gets final product,
S
D＝∑S
C5＝+∑S
C6+
S
DC in the-D spectrogram
5Alkene, C
6The peak area of above hydrocarbon component and,
∑ S
C5=-C
5Olefin peaks area summation,
∑ S
C6+-C
6Above hydrocarbon peak area summation.
In the said method, each chromatographic column of A～C carry out total peak area add with component Ying Yuqi occur to mix the component at peak in chromatographic column D corresponding region consistent.
Determined the actual peak area value Si (D) of each component on chromatographic column D in the gas sample, the area normalization method of the promptly available correction up factor obtains each components contents.
Y in the formula
iThe percentage composition of-arbitrary component i,
f
i-i component is with respect to the volume correction factor of primary standard substance,
The d-dilution gfactor, the percentage composition sum of other component except that not carrying out normalizing calculating component.
Arbitrary component i is with respect to the relative correction factor f of primary standard substance described in the normalization method
iTry to achieve by following formula:
Fi-is a relative correction factor in the formula, i.e. the ratio of certain component and the absolute correction factor of primary standard substance;
Wi/Si-is the absolute correction factor of arbitrary component i, and Wi is the volume content of component i, and Si is its peak area;
Wm/Sm-is the absolute correction factor of primary standard substance, and Wm is the volume content of primary standard substance, and Sm is the primary standard substance peak area.
The assay method of relative correction factor is that preparation contains the standard gas sample that desire is surveyed gas and primary standard substance earlier, under the analysis condition identical, detect with refinery gas, the response that obtains each component in each chromatographic column is a peak area, and the computing formula of each component concentration in the standard gas and the described relative correction factor of peak area substitution can be tried to achieve fi.
In the inventive method, the testing conditions of chromatographic column A is 110 ℃, 0.1925MPa, and the testing conditions of chromatographic column B is 90 ℃, 0.1995MPa, and the testing conditions of chromatographic column C is 120 ℃, 0.2065MPa, and the testing conditions of chromatographic column D is 60 ℃, 0.189MPa.
Refinery gas of the present invention refers to hydrogen, oxygen, nitrogen, C
1～C
4Alkane, C
2～C
4Alkene and a small amount of C
5Alkane, alkene and C
6Above heavy constituent also have amounts of carbon dioxide, carbon monoxide in addition.Comprise catalytic reforming (CR) gas, catalytic cracked gas, coking gas, steam cracking gas etc.If the present invention is used for the analysis of rock gas or other mixed gas, can suitably selects for use in A～D chromatographic column one or two to carry out gas composition according to gas composition and measure.
In actual applications, relative correction factor only needs once just can reuse with standard gas sample mensuration, need not often measure, and makes the standard specimen consumption be reduced to minimum.Each component calculated by peak area formula draw of gas sample is become software, only need control chromatographic operating conditions during mensuration,, can carry out the express-analysis test refinery gas with the injection port of working sample injecting chromatograph.
Further specify the present invention below by example, but the present invention is not limited to this.
Example 1
Use the parallel quick gas chromatograph of Agilent 3,000 four posts of Agilent company.Four analytical columns are capillary chromatographic column, and except that D is that wall is coated with the stain open tubular column, all the other are the porous layer open tubular column.Chromatographic column A pre-separation post stationary phase is the NaX molecular sieve, and 2 meters of column lengths, analytical column stationary phase are the 5A molecular sieve, 10 meters of column lengths, 0.32 millimeter of column internal diameter, 30 microns of thickness; Chromatographic column B pre-column is Porpark Q, and 1 meter of column length, analytical column are Porpark U, 8 meters of column lengths, 0.32 millimeter of column internal diameter, 10 microns of thickness; Chromatographic column C pre-column and analytical column stationary phase are aluminium oxide, and 1 meter of pre-column length is analyzed 10 meters of column lengths, 0.32 millimeter of column internal diameter, 8 microns of thickness; Chromatographic column D is the OV-1 post, long 10 meters, and 0.15 millimeter of column internal diameter, 2 microns of thickness.
Press the standard gas sample of catalytic cracked gas component preparation known content,, obtain in the standard sample each component with respect to the relative correction factor f of primary standard substance isobutane with standard sample injecting chromatograph injection port
iAdopting helium during test is carrier gas, and the operating conditions of each chromatographic column sees Table 1.Standard gas sample is formed and each component relative correction factor f
iValue sees Table 2.
With catalytic cracked gas sample injecting chromatograph injection port to be measured, to operate by table 1 condition, each chromatographic column analysis of spectra of the A～D that obtains is seen Fig. 1～4 successively.
Fig. 1 is the spectrogram of chromatographic column A, and the component that chromatographic column A detects is oxygen, nitrogen, methane and carbon monoxide.Peak area Si and each component peaks area summation ∑ S by described each component
ANumber percent try to achieve R
Ai, wherein i represents arbitrary component that post A detects.
By that analogy, by the spectrogram of chromatographic column B shown in Figure 2, try to achieve the peak area Si and the detected components peak area summation ∑ S of each detected components of post B
BNumber percent R
Bi, wherein i represents arbitrary component that chromatographic column B detects, and is carbon dioxide, ethene, ethane and sulfuretted hydrogen.Component identical with Fig. 1 component among Fig. 2 is not calculated, as methane, air (main oxygen and the nitrogen of analyzing wherein).
By chromatographic column C spectrogram shown in Figure 3, try to achieve the peak area Si and the peak area summation ∑ S of each detected components
CNumber percent R
Ci, wherein i represents arbitrary component that chromatographic column C detects, and is propylene, propane, normal butane, isobutane, anti-butylene, n-butene, isobutylene, maleic, isopentane, 1,3 butadiene.
Fig. 4 is the spectrogram of chromatographic column D, and all components of gaseous sample all goes out the peak among this figure, but permanent gas and C
4Following component occurs mixing the peak, determines the zone of chromatographic column A, B, C detected components, in the drawings respectively with A, B, C mark, C in the gas sample
5Alkene and C
6The peak of above hydrocarbon component promptly obtains S by shown in the D district with D zone other peak area adduction except that isopentane
D, respectively the peak area addition in A, B, C zone is obtained S again
A, S
B, S
C
The peak area of each component in Fig. 4 that chromatographic column A detects
S
Ai(D)＝R
Ai×S
A
The peak area of each component in Fig. 4 that chromatographic column B detects
S
Bi(D)＝R
Bi×S
B
The peak area of each component in Fig. 4 that chromatographic column C detects
S
Ci(D)＝R
Ci×S
C
By following formula the area normalization method that the peak area value of each component on the D spectrogram carries out the correction up factor is obtained each components contents.Analysis result sees Table 2.
Dilution gfactor d is the percentage composition sum of other component beyond the deduction hydrogen in the formula.
Table 1
Component concentration, body % 0.01～100
Passage label A B C D
Carrier gas helium, 0.56MPa
Detected temperatures, ℃ 110 90 120 60
Pressure before the post, MPa 0.1925 0.1995 0.2065 0.189
Time swap, second 20
Sample injection time, millisecond 25 25 25 20
The blowback time, second 87 4-
Detector sensitivity is low
Working time, second 160
Table 2
Gas content, volume %
Project fi
Standard gas refinery gas
Hydrogen 10.9 10.30--
Nitrogen 35.009 35.49 2.03
Methane 8.16 8.06 2.28
Carbon monoxide 0.574 0.58 1.85
Carbon dioxide 3.07 3.09 1.50
Ethene 10.71 10.82 1.55
Ethane 10.31 10.66 1.50
Propylene 10.20 10.06 1.19
Propane 4.98 4.90 1.14
Isobutane 2.047 2.04 1
Normal butane 1.58 1.55 0.96
N-butene 0.808 0.80 1.01
Isobutylene 1.05 1.05 1.04
1,3 butadiene 0.50 0.50 1.09
Isopentane 0.102 0.10 0.858
Amount to 100 100---
Claims (8)
1, the method for the parallel gas chromatographic analysis refinery gas composition of a kind of multicolumn comprises the steps:
(1) sample gas is fed in the gas chromatography with four parallel chromatographic column A～D detects, each chromatographic column all has independently injection port and detecting device, wherein chromatographic column A～C all has pre-separation post and blowback system, oxygen, nitrogen, methane and/or carbon monoxide in the chromatographic column A test sample gas, chromatographic column B detects carbon dioxide, ethene, ethane and/or sulfuretted hydrogen, and chromatographic column C detects C
3～C
4Hydro carbons and C
5Alkane, all components in the chromatographic column D test sample gas,
(2) determine in the ratio of each component overall response value of each the component response that detects in each chromatographic column spectrogram of A～C and detection and the chromatographic column D spectrogram respectively summation with A～corresponding response of C chromatographic column detected components, thereby determine the response of each component in chromatographic column D spectrogram
(3) according to the response of each component in chromatographic column D spectrogram, try to achieve each components contents in the sample with the correction normalization method.
2, in accordance with the method for claim 1, it is characterized in that described four parallel chromatographic columns are capillary chromatographic column.
3, in accordance with the method for claim 2, it is characterized in that chromatographic column D is that wall is coated with stain open pipe capillary column, chromatographic column A～C is porous layer open pipe capillary column.
4, in accordance with the method for claim 1, it is characterized in that each chromatographic column detecting device is a thermal conductivity detector (TCD).
5, in accordance with the method for claim 2, the stationary phase that it is characterized in that chromatographic column A is the 5A molecular sieve, and the stationary phase of its pre-separation post is the NaX molecular sieve, 0.32 millimeter of column internal diameter, 30 microns of thickness; The stationary phase of chromatographic column B is Porpark U, and the stationary phase of its pre-separation post is Porpark Q, 0.32 millimeter of column internal diameter, 10 microns of thickness; The stationary phase of chromatographic column C and its pre-separation post is aluminium oxide, 0.32 millimeter of column internal diameter, 8 microns of thickness; The stationary phase of chromatographic column D is OV-1,0.15 millimeter of column internal diameter, 2 microns of thickness.
6, in accordance with the method for claim 1, the testing conditions that it is characterized in that chromatographic column A is 110 ℃, 0.1925MPa, the testing conditions of chromatographic column B is 90 ℃, 0.1995MPa, and the testing conditions of chromatographic column C is 120 ℃, 0.2065MPa, and the testing conditions of chromatographic column D is 60 ℃, 0.189MPa.
7, in accordance with the method for claim 1, it is characterized in that proofreading and correct correction factor used in the normalization method and be the relative correction factor of each component with respect to primary standard substance, its value is determined by the standard gas sample that test contains primary standard substance.
8, in accordance with the method for claim 7, it is characterized in that described primary standard substance is selected from isobutane or n-butene.
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| CN1301407C (en) * | 2005-01-21 | 2007-02-21 | 大连交通大学 | Oxygen availability gas-phase chromatography detecting method and apparatus for aerating tank |
| CN100409009C (en) * | 2005-06-22 | 2008-08-06 | 中国石油化工股份有限公司 | Analyzer for mixed gas containing O2, N2 and H2 |
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| CN103954715A (en) * | 2014-04-15 | 2014-07-30 | 华东师范大学 | Gas chromatograph for refinery gas analysis |
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| CN1301407C (en) * | 2005-01-21 | 2007-02-21 | 大连交通大学 | Oxygen availability gas-phase chromatography detecting method and apparatus for aerating tank |
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| US7823439B2 (en) | 2007-11-15 | 2010-11-02 | Midwest Research Institute | Method for identifying the composition of a sample |
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| CN102650625B (en) * | 2011-02-28 | 2013-12-25 | 中国石油化工股份有限公司 | Component analyzer for hydrocarbon gas mixture with oxygen compounds |
| CN102650624B (en) * | 2011-02-28 | 2013-12-25 | 中国石油化工股份有限公司 | Analysis method for hydrocarbon gas mixture with oxygen compounds |
| US10823644B2 (en) | 2013-02-28 | 2020-11-03 | TricornTech Taiwan | Real-time on-site gas analysis network for ambient air monitoring and active control and response |
| US10859474B2 (en) | 2013-02-28 | 2020-12-08 | TricornTech Taiwan | Real-time on-site gas analysis network for ambient air monitoring and active control and response |
| CN103954715A (en) * | 2014-04-15 | 2014-07-30 | 华东师范大学 | Gas chromatograph for refinery gas analysis |
| CN103954715B (en) * | 2014-04-15 | 2015-05-20 | 华东师范大学 | Gas chromatograph for refinery gas analysis |
| CN105181851A (en) * | 2015-10-13 | 2015-12-23 | 神华集团有限责任公司 | Method for testing oxynitride in environment |
| CN106153431A (en) * | 2016-07-21 | 2016-11-23 | 中国科学院山西煤炭化学研究所 | The detection method of a kind of quick mensuration raw gas composition and device thereof |
| CN114428121A (en) * | 2020-09-09 | 2022-05-03 | 中国石油化工股份有限公司 | Containing high concentration H2Quantitative detection device and method for all components of natural gas of S |
| CN114428121B (en) * | 2020-09-09 | 2024-04-09 | 中国石油化工股份有限公司 | High-concentration H 2 S-type natural gas full-component quantitative detection device and method |
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