CN1088191C - Chromatographic column for analysis of three-component oil in tar and using method - Google Patents
Chromatographic column for analysis of three-component oil in tar and using method Download PDFInfo
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- CN1088191C CN1088191C CN 96119618 CN96119618A CN1088191C CN 1088191 C CN1088191 C CN 1088191C CN 96119618 CN96119618 CN 96119618 CN 96119618 A CN96119618 A CN 96119618A CN 1088191 C CN1088191 C CN 1088191C
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Abstract
The present invention relates to a chromatographic column used for analyzing three-component oil in tar oil and a using method thereof. The present invention is characterized in that a filling material in a stainless steel pipe is formed by mixing glycol polyester adipate and 6201 according to a certain weight ratio; the chromatographic column is used under the conditions that column temperature is from 150 to 200 DEC C, vaporization temperature is from 250 to 290 DEG C, detection temperature is from 200 to 290 DEG C, supporting gas pressure is from 0.05 to 0.06MPa, the flow quantity of combustion gas is from 40 to 80 ml/portion, the flow quantity of combustion-supporting gas is from 160 to 200 ml/portion, etc. The present invention used for analyzing three-component oil in tar oil has the advantages of high speed, high accuracy rate, confidence degree being higher than 95%, no pollution timely production guidance and low cost, and the using period of the chromatographic column can reach 1 to 2 years.
Description
The present invention relates to a kind of gas chromatographic column and using method that is used for analyser, especially belong to the analysis of mixed triolein in the tar.
Before the present invention, analyze the method for the mixed triolein in the tar, mainly be to carry out distillation test, with the mixed triolein in the way of distillation analysis tar, it exists not enough: the one, and complicated operation, analytical cycle is long, need one hour more than, also will do the naphthalene content test in addition, can not in time instruct production; The 2nd, owing to contain a large amount of carcinogenic substances in the tar, in still-process, can produce noxious odor, contaminated environment, harmful to operator's health, easily cause occupational illness; As adopt capillary column to carry out the analysis of sample, and though post is imitated height, good separating effect, peak shape is many, quantitatively accurately, and its cost price costliness, every meter about four, 50 yuan, uneconomical, and little, the easy obstruction of capillary caliber, should not on producing, apply.
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of and both do not pollute the environment, human body is worked the mischief, can make good separating effect again, analytical cycle is short, cost is low, the operating period can reach gas chromatographic column and the using method in 1～2 year.
The object of the present invention is achieved like this: the gas chromatographic column that is used for analyzing the tar mixed triolein, form by stainless-steel tube and inserts, immobile liquid in the inserts adopts the adipate glycol polyester, carrier adopts 40～80 purposes 6201, weight ratio when carrier 6201 skins are coated with stain immobile liquid adipate glycol polyester is an immobile liquid: carrier=15: 100, and it is stirred evenly.
The using method that adopts the inserts gas chromatographic column of this kind proportioning is to be that 100～200 ℃, vapourizing temperature are that 250～290 ℃, detected temperatures are that 200～290 ℃, nebulizer gas pressure are that 0.05～0.06Mpa and its flow are that 69ml/min, burning gases are hydrogen in the gas chromatography column temperature, and its flow is that the flow of 40～80ml/min, combustion air is 160～200ml/min, decays to 2
1～3, sensitivity is 10
7～9Condition under use.
Description of drawings is as follows:
Fig. 1 is a kind of be used for the analyzing gas chromatographic column of tar mixed triolein and gas chromatogram of analytical approach
Be described in further detail as follows below in conjunction with embodiment: the pipe of chromatographic column is a stainless steel material, it is of a size of: Φ 3mm * 1m, inserts immobile liquid adipate glycol polyester and mesh size 6201 carriers between 50～70 orders are formulated by its weight ratio 15: 100, constantly stir when being coated with stain.Service condition when it is analyzed is to be that 185 ℃, detected temperatures be 250 ℃, vapourizing temperature at 290 ℃, nebulizer gas pressure are that 0.06Mpa and its flow are that the flow of 69ml/min, burning hydrogen is that the flow of 35ml/min, combustion-supporting gas air is 170ml/min, sample size 0.6ul at chromatogram column temperature, adopts the CDMC-1E chromatographic data processor to carry out data processing.Under these conditions, the mixed triolein fraction is carried out qualitative analysis, its result such as table 1 and Fig. 1.
By table 1 as can be known, within 10 minutes, the chromatograph method just can be analyzed each fractional composition in the mixed triolein (indenes, the benzene first is fine, naphthalene, beta-methylnaphthalene, alpha-methyl-naphthalene, biphenyl, acenaphthene, dibenzofuran, fluorenes) come out, and has shortened the time greatly than the way of distillation.
The t check is carried out in the chromatographic column accuracy: the configuration standard specimen, the correction area normalization method replication of employing band correction factor 10 times carries out the t check with the result, to check chromatographic reliability, the results are shown in Table 2.
As shown in Table 2, the t of each component in the mixed triolein standard specimen
RealAll less than the theoretical value t=2.26 that measures frequency n=10 o'clock, degree of confidence reaches 95% to assay, illustrates that the matching degree of measured value and true value is fine, is reliable with the gc analysis mixed triolein.
Measure precision with chromatogram repeatability, randomly draw 6 standard specimens, each sample replication 5 times the results are shown in Table 3.
By table 3 as seen, each measures the standard deviation and the relative standard deviation of material, check the allowed band that Kaiser proposes about the chromatogram ration analysis relative standard deviation, as seen the relative standard deviation of each material is far smaller than this setting, simultaneously, the permissible error when observing degree of confidence 95%, each material all ± (0.5～1.0%), favorable reproducibility is described, adopts its precision of mixed triolein in the chromatography analysis tar good.
Employing the present invention analyzes the mixed triolein in the tar, and analytical cycle is short, only 10 minutes, accuracy height, and degree of confidence reaches more than 95%, and non-environmental-pollution improves operating personnel's condition, compares with adopting the kapillary packed column, and is with low cost.
The retention time of table 1. mixed triolein fraction each component
Table 2. mixed triolein standard specimen t check results
Table 3. fraction precision measurement result
| The | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Title | Unknown material | Indenes | The benzene first is fine | Naphthalene | Methylnaphthalene | Biphenyl | Acenaphthene | Dibenzofuran | Fluorenes |
| Boiling point ℃ | - | 183.1 | 190.7 | 217.9 | 243.0 | 254.9 | 276.9 | 285.1 | 297.9 |
| Retention time | 0.43 | 0.61 | 0.87 | 1.37 | 1.94 | 2.87 | 4.07 | 6.07 | 8.40 |
| Form | Actual concentration | Revise concentration | Absolute error | Relative error | Standard deviation | t Real |
| Indenes | 3.18 | 3.172 | -0.008 | 0.25 | 0.0670 | 0.378 |
| The benzene first is fine | 2.25 | 2.246 | -0.004 | 0.18 | 0.0370 | 0.342 |
| Naphthalene | 45.47 | 45.381 | -0.089 | 0.196 | 0.5889 | 0.478 |
| Beta-methylnaphthalene | 8.11 | 8.078 | -0.032 | 0.39 | 0.1970 | 0.514 |
| Alpha-methyl-naphthalene | 8.05 | 8.049 | -0.001 | 0.01 | 0.2160 | 0.015 |
| Biphenyl | 13.23 | 13.195 | -0.035 | 0.26 | 0.1940 | 0.570 |
| Acenaphthene | 9.73 | 9.759 | 0.029 | 0.298 | 0.1290 | 0.711 |
| Dibenzofuran | 7.02 | 7.049 | 0.410 | 0.41 | 0.1140 | 0.804 |
| Fluorenes | 2.97 | 2.978 | 0.269 | 0.269 | 0.0437 | 0.579 |
Claims (3)
1, a kind of gas chromatographic column that is used for analyzing the tar mixed triolein, form by stainless-steel tube and inserts, it is characterized in that the immobile liquid in the inserts adopts the adipate glycol polyester, carrier adopts 6201, weight ratio when carrier 6201 skins are coated with stain immobile liquid adipate glycol polyester is an immobile liquid: carrier=15: 100, and it is stirred evenly.
2, a kind of gas chromatographic column that is used for analyzing the tar mixed triolein according to claim 1, the mesh size that it is characterized in that carrier 6201 is 40～80 orders.
3, a kind of method of utilizing the described gas chromatographic column of claim 1 to analyze mixed triolein in the tar, the temperature that it is characterized in that gas chromatographic column is controlled at 150～200 ℃, gasification temperature is controlled at 250～290 ℃, detected temperatures is controlled at 200～290 ℃, and nebulizer gas pressure is that 0.05～0.06Mpa, flow are that 69ml/min, burning gases hydrogen flowing quantity are that the flow of 40～80ml/min, combustion air is 160～250ml/min, decay 2
1～3, sensitivity is 10
7～9Condition under use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96119618 CN1088191C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysis of three-component oil in tar and using method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96119618 CN1088191C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysis of three-component oil in tar and using method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1165296A CN1165296A (en) | 1997-11-19 |
| CN1088191C true CN1088191C (en) | 2002-07-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96119618 Expired - Fee Related CN1088191C (en) | 1996-09-01 | 1996-09-01 | Chromatographic column for analysis of three-component oil in tar and using method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI700491B (en) * | 2015-11-20 | 2020-08-01 | 日商日立高新技術科學股份有限公司 | Calibration method for gas analysis device and gas analysis device |
-
1996
- 1996-09-01 CN CN 96119618 patent/CN1088191C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI700491B (en) * | 2015-11-20 | 2020-08-01 | 日商日立高新技術科學股份有限公司 | Calibration method for gas analysis device and gas analysis device |
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| Publication number | Publication date |
|---|---|
| CN1165296A (en) | 1997-11-19 |
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