CN1164647A - Chromatographic column for analysising anthracene oil in tar and using method - Google Patents
Chromatographic column for analysising anthracene oil in tar and using method Download PDFInfo
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- CN1164647A CN1164647A CN 96119617 CN96119617A CN1164647A CN 1164647 A CN1164647 A CN 1164647A CN 96119617 CN96119617 CN 96119617 CN 96119617 A CN96119617 A CN 96119617A CN 1164647 A CN1164647 A CN 1164647A
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Abstract
The present invention relates to a chromatographic column for analysizing anthracence oil in tar and its use method. It is characterized by that the filler in stainless steel tube is made up by using SE-30 as stationary liquid and chromosorb W as supporter according to the weight ratio of 95:100, and said chromatographic column is used under the conditions of that column temp. is 190-250 deg.C, vaporization temp. is 280-320 deg.C, detection temp. is 200-270 deg.C, pressure of carrier gas is 0.03-0.1 MPa, flow rate of burning hydrogen gas is 16-145 ml/min and flow rate of combustion-supporting air is 83-358 ml/min. Said invention possesses quick analysizing speed, high accuracy (above 95%), low cost, and has no environmental pollution, and its service time can be up to 1-2 years.
Description
The present invention relates to the chromatograph analytical approach, especially belong to chromatographic column and the using method of analyzing carbolineum in the tar.
Before the present invention, analyze the carbolineum in the tar, mainly take the way of distillation, it exists not enough: complicated operation, analytical cycle is long, promptly needs about one hour, and serious environment pollution is harmful to operating personnel's health, for a long time in this work, easily sends out occupational illness.Also once had the people to repay pilot production with packed column gas chromatography post method when analyzing carbolineum, but success, life cycle is only month surplus.
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of simple to operate, non-environmental-pollution, analysis carbolineum component fast, accurately, it analyzes data degree of confidence up to chromatographic column and using method on 95%.
The object of the present invention is achieved like this: the chromatographic column that is used for analyzing tar carbolineum, form by stainless-steel tube and inserts, immobile liquid SE-30 in its inserts and the weight proportion of carrier Chromosorbw are 9.5: 100, constantly stir, so that carrier Chromosorbw appearance is coated with SE-30 is even.Be used for analyzing the using method of the chromatographic column of tar carbolineum, be the temperature of chromatographic column is controlled at 190～250 ℃, detected temperatures is controlled at 200～270 ℃, vapourizing temperature is controlled at 280～320 ℃, nebulizer gas pressure is controlled at 0.03～0.1MPa, the flow of burning gases hydrogen is 16～145ml/ branch, and the flow of combustion air is 83～358ml/ branch, decays to 2
1～3, sensitivity 10
7～9
Be described in further detail as follows below in conjunction with embodiment: chromatographic column is a stainless steel material, and it is of a size of φ 3 * 2m, and the immobile liquid SE-30 of inserts is 9.5: 100 with the weight proportion of carrier Chromosorb w when mixing.Chromatographic column be at the column temperature of chromatographic column at 230 ℃, vapourizing temperature at 300 ℃, detected temperatures at 250 ℃, carrier gas N
2Flow be 20ml, the flow of combustion air is the 160ml/ branch, burning gases H
2Flow be the 43.90ml/ branch, the decay 2
2, sensitivity is 10
8, chromatographic data processor when operation be 5 in peak width, slope for test oneself, minimum area is 200 square millimeters, change ginseng time into 0, be that 0.8 minute, stand-by time are that 18 minutes, sample size are that 0.2uL, carbolineum sample amount are 0.4uL locking time.Under these conditions, carbolineum is carried out the chromatogram quantification analysis result, see Fig. 1 and table 1.
From the carbolineum The qualitative analysis as can be seen, the key component in the carbolineum was isolated before 10 minutes, only had just to separate out about 16 minutes.Therefore the residence time fixes on 18 minutes for well.
In order to verify the accuracy of chromatogram analysis data, utilize institute to join standard specimen, adopt and revise area normalization method replicate determination ten times, carry out the t check and calculate, see Table 2.
As seen from Table 2, the t of each material check result of calculation all is 95% o'clock theoretical value t=2.26 less than degree of confidence, illustrates that the compound degree of measured value and actual value is fine.Utilize the degree of confidence of carbolineum data in the stratographic analysis tar to reach more than 95%, illustrate that the data of analyzing with the present invention are accurately and reliably.
In order to verify the precision of chromatographic data, 6 obtained each samples of random sampling are carried out 5 tests, the results are shown in Table 3.
As seen, the actual standard deviation is far smaller than the theoretical standard deviation that allows, and illustrates that the precision of this analytical approach is fine from table 3.
Employing the present invention analyzes the carbolineum in the tar, and simple to operate, analytical cycle is no more than 18 minutes, and has accomplished to analyze fast, accurately, reliably, degree of confidence reaches more than 95%, and is free from environmental pollution, improved operating personnel's condition of work, occupational illness is difficult for taking place, and life cycle can reach 1～2 year.
The analysis result of table 1 carbolineum standard specimen
| Sequence number | The component title | Relative correction factor fi | Theoretical value % | The mean value % of 10 measurement results | Error % | |
| Absolute error | Relative error | |||||
| ??1 | Naphthalene | ??1.062 | ??4.668 | ????4.661 | ??0.007 | ??0.15 |
| ??2 | The alpha+beta methylnaphthalene | ??1.006 | ??14.647 | ????14.611 | ??0.036 | ??0.246 |
| ??3 | Biphenyl | ??1.027 | ??4.518 | ????4.636 | ??-0.118 | ??2.61 |
| ??4 | 2,6+1,3 dimethylnaphthalenes | ??1.155 | ??5.275 | ????5.185 | ??0.09 | ??1.706 |
| ??5 | Acenaphthene | ??1.045 | ??7.590 | ????7.664 | ??-0.074 | ??0.975 |
| ??6 | Dibenzofuran | ??1.250 | ??9.121 | ????9.034 | ??0.087 | ??0.954 |
| ??7 | Fluorenes | ??0.845 | ??9.373 | ????9.367 | ??0.00 | ??0.062 |
| ??8 | Phenanthrene+anthracene+carbazole | ??1 | ??24.890 | ????24.917 | ??-0.027 | ??0.108 |
| ??9 | The methylphenanthrene anthracene | ??0.9226 | ??7.383 | ????7.360 | ??0.023 | ??0.312 |
| ??10 | The firefly anthracene | ??1.155 | ??6.824 | ????6.845 | ??-0.021 | ??0.308 |
| ??11 | Pyrene | ??1.217 | ??5.715 | ????5.717 | ??-0.002 | ??0.035 |
The t check of table 2 carbolineum standard specimen
Table 3. fraction precision measurement result
Claims (2)
1, a kind of chromatographic column that is used for analyzing tar carbolineum is made up of stainless-steel tube and inserts, it is characterized in that immobile liquid SE-30 in the inserts and the weight proportion of carrier Chromosorbw are 9.5: 100, stirs when the two is mixed.
2, a kind of using method that is used for analyzing the chromatographic column of tar carbolineum is characterized in that temperature in chromatographic column is controlled at 190～250 ℃, vapourizing temperature and is controlled at 280～320 ℃, detected temperatures to be controlled at flow that 200～270 ℃, nebulizer gas pressure are controlled at 0.03～0.1MPa, burning gases hydrogen be that the flow of 16～145ml/ branch, combustion air is 83～358ml/ branch, decay 2
1～3, sensitivity 10
7～9Condition under use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96119617A CN1090760C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysising anthracene oil in tar and using method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96119617A CN1090760C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysising anthracene oil in tar and using method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1164647A true CN1164647A (en) | 1997-11-12 |
| CN1090760C CN1090760C (en) | 2002-09-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN96119617A Expired - Fee Related CN1090760C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysising anthracene oil in tar and using method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786935A (en) * | 2010-02-26 | 2010-07-28 | 曲靖众一精细化工股份有限公司 | Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil |
| CN103604886A (en) * | 2013-11-26 | 2014-02-26 | 武汉钢铁(集团)公司 | Method for determining content of anthracene in coked industrial anthracene oil by using capillary tube chromatography |
| CN107367568A (en) * | 2017-07-31 | 2017-11-21 | 内蒙古中煤蒙大新能源化工有限公司 | A kind of method of hydrocarbon content in quick analysis gaseous sample |
-
1996
- 1996-09-01 CN CN96119617A patent/CN1090760C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786935A (en) * | 2010-02-26 | 2010-07-28 | 曲靖众一精细化工股份有限公司 | Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil |
| CN101786935B (en) * | 2010-02-26 | 2012-12-12 | 曲靖众一精细化工股份有限公司 | Method for extracting fluorene, anthracene and carbazole from mixed anthracene oil |
| CN103604886A (en) * | 2013-11-26 | 2014-02-26 | 武汉钢铁(集团)公司 | Method for determining content of anthracene in coked industrial anthracene oil by using capillary tube chromatography |
| CN107367568A (en) * | 2017-07-31 | 2017-11-21 | 内蒙古中煤蒙大新能源化工有限公司 | A kind of method of hydrocarbon content in quick analysis gaseous sample |
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| Publication number | Publication date |
|---|---|
| CN1090760C (en) | 2002-09-11 |
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