CN101587100B - Method for determining benzene compounds in coked lean and fat oil by capillary gas chromatography - Google Patents
Method for determining benzene compounds in coked lean and fat oil by capillary gas chromatography Download PDFInfo
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- CN101587100B CN101587100B CN2008101977329A CN200810197732A CN101587100B CN 101587100 B CN101587100 B CN 101587100B CN 2008101977329 A CN2008101977329 A CN 2008101977329A CN 200810197732 A CN200810197732 A CN 200810197732A CN 101587100 B CN101587100 B CN 101587100B
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Abstract
The invention provides a method for determining benzene compounds in coked lean and fat oil by capillary gas chromatography. The method mainly comprises the following steps: establishing a condition of the capillary gas chromatography; determining a quantitative internal standard substance; calculating content of the benzene compounds; and calculating the content of lean oil or fat oil. Compared with the conventional method, the method has high accuracy, rapidness, convenience and non-pollution, reduces operation intensity for workers, greatly improves the work environment, improves work efficiency, can be used for production control for coking enterprises, and provides the accurate and convenient experimental method for field analysis and operation regulation for factories.
Description
Technical field
The present invention relates to that coking industry is poor, the assay method of benzene-like compounds in the rich oil.
Background technology
At present, coke-oven gas reclaims crude benzol and adopts washing oil to absorb the crude benzol method usually, and washing oil is one of chemical products of extracting from coal tar, is made up of more than 70 kinds of organic compounds.Washing oil absorbs crude benzol technology and comprises washing oil suction benzene and rich oil de-benzene two procedures.It is to absorb benzene hydrocarbon with washing oil washing coal gas that washing oil is inhaled benzene, and the washing oil that has absorbed benzene hydrocarbon is called rich oil.Rich oil de-benzene is to distillate the benzene hydrocarbon that is dissolved in the rich oil with steamed, and the washing oil behind the rich oil de-benzene is called oil-poor, understands the distribution situation of benzene-like compounds in the lean and fat oil, can in time grasp the tower effect that coking is reclaimed the production control situation of crude benzol workshop section and washed the benzene tower.What traditional coking was poor, the assay method of benzene-like compounds adopts in the rich oil is the way of distillation, this method complex operation, moisture should not take off to the greatest extent, when water and oily azeotropic, be very easy to overflow, cause the analytical equipment severe contamination, be difficult to clean, analysis time long (about 50 minutes), error is bigger, easily pollutes the healthy of working environment and grievous injury analyst in the sample analysis process.
Summary of the invention
The purpose of this invention is to provide the method for benzene-like compounds in a kind of, rich oil poor with quick, accurate, the pollution-free mensuration coking of capillary gas chromatography, can improve the test job environment, the attended operation personnel's is healthy.
Purpose of the present invention is realized by following scheme:
According to the organic trait of benzene-type products and the difference on chemical constitution, adopt efficient capillary chromatography (instrument selection gas chromatograph AgiLent-6820), can be with benzene, toluene, P-xylene, m-xylene in poor, the rich oil, o-xylene effectively separates and accurately quantitatively.
Concrete scheme is:
This method comprise the benzene-like compounds capillary gas chromatography condition in poor, the rich oil of setting up, quantitatively internal standard compound determine that concrete steps are:
(1) foundation of capillary gas chromatography condition
Chromatographic condition is: chromatographic column: quartz elastic capillary tube post, 5% diphenyl, 15～30 meters * 0.25 millimeter～0.32 millimeter * 0.20～0.35 micron of 95% dimethyl polysiloxane;
Post flow N
2: 2.0～3.5 ml/min
Column temperature-temperature programme: initial temperature 40 degree～70 degree, kept 0～3 minute, be warming up to 100 degree with 50 degree/minute clock rate, kept 0.5 minute; With 60 degree/minute temperature programme to 250 degree, kept 5 minutes again;
Vapourizing temperature: 250 degree～300 degree;
Detected temperatures: 200 degree～250 degree;
Hydrogen flowing quantity: 25～60 ml/min;
Air mass flow: 250～600 ml/min;
Air: hydrogen=10:1
Tail wind drift amount: 20～40 ml/min;
Split ratio is 30～50:1;
Sample size: 0.2～0.8 microlitre;
(2) quantitative internal standard compound determines
Internal standard compound is positive nonane, purity: greater than 95.0%;
(3) cubage of benzene-like compounds
X
i％＝(A
i/A
s)×f
i(m
s/M)×100％
＝(A
i/A
s)×f
i×K×100％
In the formula:
X
iThe content of-certain component materials, %;
A
iThe peak area of-certain component materials;
A
s-positive nonane area;
f
iThe relative correction factor of-certain component materials;
m
sThe quality of-internal standard compound: volume * density * internal standard compound purity; Positive nonane density is 0.73 grams per milliliter;
The quality of M-sample: volume * density; Poor, rich oil average density is 1.063 grams per milliliters;
K-m
s/M；
(4) cubage of oil-poor or rich oil
Y
Poor, rich oil%=∑ X
i%.
The concrete value of above-mentioned GC conditions is: column temperature-temperature programme: initial temperature 50 degree, kept 1 minute, and be warming up to 100 degree with 50 degree/minute clock rate, kept 0.5 minute; With 60 degree/minute temperature programme to 250 degree, kept 5 minutes again; Post flow (N
2): 2.8 ml/min; Vapourizing temperature, detected temperatures: 250 degree; Hydrogen flowing quantity: 40 ml/min; Air mass flow: 400 ml/min; Tail wind drift amount: 25 ml/min; Split ratio is 30:1; Sample size is 0.4 microlitre.
The relative correction factor of above-mentioned certain component materials is the variation range of benzene,toluene,xylene content in, the richness poor according to our unit, prepares one group of standard specimen that contains internal standard compound.Measure each 3 microlitre of benzene,toluene,xylene respectively with 10 microliter syringes and bring in the sample dottle pin sample bottle in 12 milliliters, add the positive nonane of 3 microlitres respectively and 5 milliliters of acetone diluted are standby; Sample introduction 0.4 microlitre obtains corresponding chromatogram respectively under above-mentioned experiment condition, is handled obtaining benzene, toluene, P-xylene, m-xylene, o-xylene relative correction factor by chromatographic work station.
This assay method is quick, environmentally safe, and the accuracy height, the recovery of standard model is between 106.08%～120.11%, and the standard deviation rich oil is 0.07322%, and oil-poor is 0.007841%, and coefficient of variation rich oil is 3.85%, oil-poor is 3.00%.Show that thus this assay method degree of accuracy and precision meet the requirements, show that simultaneously this method of testing is feasible.
Description of drawings
Fig. 1 is a lean and fat oil standard specimen chromatogram; Horizontal ordinate-time (branch); Ordinate-response (millivolt);
Fig. 2 is the sample chromatogram; Horizontal ordinate-time (branch); Ordinate-response (millivolt);
Above accompanying drawing is under above-mentioned chromatographic run condition, the stratographic analysis figure that standard specimen, sample are analyzed and recorded with internal standard method.
Embodiment
The invention will be further described with embodiment below:
Get 100 milliliters of oil-poor or rich oil samples, in 250 milliliters of wide-necked bottles,, left standstill 20 minutes with 20 gram solid sodium hydroxide dehydrations.Getting after 0.5 milliliter of dehydration oil-poor or rich oil sample with 1 milliliter of transfer pipet brings in the sample dottle pin sample bottle in 12 milliliters, add 5 milliliters of acetone and the positive nonane of 3 microlitres, shake up (coming and going 5-10 time), get 0.4 microlitre sample, under the chromatography test condition of regulation, carry out test analysis with micro syringe.
Data processing is as follows:
Formula: X
i%=(A
i/ A
s) * f
i(m
s/ M) * 100%
＝(A
i/A
s)×f
i×K×100％
The content Y of oil-poor or rich oil
Poor, rich oil%=∑ X
i%
The density of positive nonane is 0.73 grams per milliliter, and purity is 95%; Average density poor, rich oil is 1.063 grams per milliliters,
K＝m
s/M＝0.003×0.73×0.95/0.5×1.063＝0.3913
A
s＝171.52
1.A
Benzene=44.765 f
Benzene=1.317
X
Benzene%=(44.765/171.52) * 1.317 * 0.3913 * 100=0.1345
2.A
Toluene=20.21 f
Toluene=1.043
X
Toluene%=(20.21/171.52) * 1.043 * 0.3913 * 100=0.0409
3.A
P-xylene=15.72 f
P-xylene=0.7814
X
P-xylene%=(15.72/171.52) * 0.7814 * 0.3913 * 100=0.0280
4.A
M-xylene=11.604 f
M-xylene=0.5196
X
M-xylene%=(11.604/171.52) * 0.5196 * 0.3913 * 100=0.0137
5.A
O-xylene=13.971 f
O-xylene=0.7838
X
O-xylene%=(13.971/171.52) * 0.7838 * 0.3913 * 100=0.0344
By formula Y
Oil-poor%=∑ X
i%
=X
Benzene%+X
Toluene%+X
P-xylene%+X
M-xylene%+X
O-xylene%
＝0.1345+0.0409+0.0280+0.0137+0.0344
＝0.2515
Claims (3)
1. the method for benzene-like compounds in, the rich oil poor with the capillary gas chromatography coking is characterized in that: this method comprise the benzene-like compounds capillary gas chromatography condition in poor, the rich oil of setting up, quantitatively internal standard compound determine that concrete steps are:
(1) foundation of capillary gas chromatography condition
Chromatographic condition is: chromatographic column: quartz elastic capillary tube post, 5% diphenyl, 15～30 meters * 0.25 millimeter～0.32 millimeter * 0.20～0.35 micron of 95% dimethyl polysiloxane;
Post flow N
2: 2.0～3.5 ml/min;
Column temperature-temperature programme: initial temperature 40 degree～70 degree, kept 0～3 minute, be warming up to 100 degree with 50 degree/minute clock rate, kept 0.5 minute; With 60 degree/minute temperature programme to 250 degree, kept 5 minutes again;
Vapourizing temperature: 250 degree～300 degree;
Detected temperatures: 200 degree～250 degree;
Hydrogen flowing quantity: 25～60 ml/min;
Air mass flow: 250～600 ml/min;
Air: hydrogen=10: 1
Tail wind drift amount: 20～40 ml/min;
Split ratio is 30～50: 1;
Sample size: 0.2～0.8 microlitre;
(2) quantitative internal standard compound determines
Internal standard compound is positive nonane, purity: greater than 95.0%;
(3) cubage of benzene-like compounds
X
i％＝(A
i/A
s)×f
i(m
s/M)×100％
＝(A
i/A
s)×f
i×K×100％
In the formula:
X
iThe content of-certain benzene-like compounds, %;
A
iThe peak area of-certain benzene-like compounds;
A
s-positive nonane area;
f
iThe relative correction factor of-certain benzene-like compounds;
m
sThe quality of-internal standard compound: volume * density * internal standard compound purity; Positive nonane density is 0.73 grams per milliliter;
The quality of M-sample: volume * density; Poor, rich oil average density is 1.063 grams per milliliters;
K-m
s/M；
(4) cubage of benzene-like compounds in the oil-poor or rich oil
Y
Poor, rich oil%=∑ X
i%.
2. by the method for benzene-like compounds in described, the rich oil poor of claim 1 with the capillary gas chromatography coking, it is characterized in that: the concrete value of above-mentioned GC conditions is: column temperature-temperature programme: initial temperature 50 degree, kept 1 minute, be warming up to 100 degree with 50 degree/minute speed, kept 0.5 minute; With 60 degree/minute temperature programme to 250 degree, kept 5 minutes again; Post flow N
2: 2.8 ml/min; Vapourizing temperature, detected temperatures: 250 degree; Hydrogen flowing quantity: 40 ml/min; Air mass flow: 400 ml/min; Tail wind drift amount: 25 ml/min; Split ratio is 30: 1; Sample size is 0.4 microlitre.
3. by the method for benzene-like compounds in described, the rich oil poor of claim 1 with the capillary gas chromatography coking, it is characterized in that: the relative correction factor of above-mentioned certain component materials is the variation range according to benzene,toluene,xylene content in poor, the rich oil, prepare one group of standard specimen that contains internal standard compound, measure each 3 microlitre of benzene,toluene,xylene respectively with 10 microliter syringes and bring in the sample dottle pin sample bottle in 12 milliliters, add the positive nonane of 3 microlitres respectively and 5 milliliters of acetone diluted are standby; Sample introduction 0.4 microlitre obtains corresponding chromatogram respectively under above-mentioned experiment condition, is handled obtaining benzene, toluene, P-xylene, m-xylene, o-xylene relative correction factor by chromatographic work station.
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|---|---|---|---|
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|---|---|---|---|
| CN2008101977329A CN101587100B (en) | 2008-11-20 | 2008-11-20 | Method for determining benzene compounds in coked lean and fat oil by capillary gas chromatography |
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| CN101587100B true CN101587100B (en) | 2011-10-26 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323369A (en) * | 2011-08-08 | 2012-01-18 | 宝钢集团新疆八一钢铁有限公司 | Gas chromatography determination method of benzene content in lean and rich oil |
| CN105136940A (en) * | 2015-10-15 | 2015-12-09 | 宣化钢铁集团有限责任公司 | Determining method for initial boiling point and final boiling point of coking-light benzene |
| CN108226360A (en) * | 2018-01-05 | 2018-06-29 | 四川环科检测技术有限公司 | A kind of method for measuring acetone in air |
| CN112630335A (en) * | 2020-12-16 | 2021-04-09 | 马钢奥瑟亚化工有限公司 | Method for determining contents of benzene, toluene and xylene in coal tar light oil fraction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428605A (en) * | 2001-12-27 | 2003-07-09 | 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 |
| CN1740785A (en) * | 2005-09-23 | 2006-03-01 | 清华大学 | Method for predicting deep oil-gas reservoir by BTEX anomaly in sea-bottom shallow sediment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428605A (en) * | 2001-12-27 | 2003-07-09 | 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 |
| CN1740785A (en) * | 2005-09-23 | 2006-03-01 | 清华大学 | Method for predicting deep oil-gas reservoir by BTEX anomaly in sea-bottom shallow sediment |
Non-Patent Citations (1)
| Title |
|---|
| 张杰.洗苯塔前后贫、富油中粗苯含量的测定方法研究.《科技情报开发与经济》.2008,第18卷(第30期),136-138. * |
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