CN103604886A - Method for determining content of anthracene in coked industrial anthracene oil by using capillary tube chromatography - Google Patents

Method for determining content of anthracene in coked industrial anthracene oil by using capillary tube chromatography Download PDF

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CN103604886A
CN103604886A CN201310604278.5A CN201310604278A CN103604886A CN 103604886 A CN103604886 A CN 103604886A CN 201310604278 A CN201310604278 A CN 201310604278A CN 103604886 A CN103604886 A CN 103604886A
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anthracene
sample
azophenlyene
internal standard
industrial
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CN103604886B (en
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刘翠霞
谢广粤
张贺娟
张广义
黄琮发
王兰
常红兵
刘向勇
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Wuhan Iron and Steel Co Ltd
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Wuhan Iron and Steel Group Corp
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Abstract

The invention provides a method for determining the content of anthracene in coked industrial anthracene oil by using a capillary tube chromatography. The method comprises the following steps: preparing a standard sample; analyzing the prepared standard sample by using the capillary tube chromatography; determining the test sample; and calculating the content of the anthracene in industrial anthracene according to a formula. The method can determine the content of the anthracene in the industrial anthracene simply, conveniently, accurately and reliably. The analyzing time of the whole test sample is not more than 12 minutes, the pre-treatment of the sample is simple and few middle links are needed in the operation process; the chromatography is applied in consideration of an environment-friendly and safe method, so as to reduce the environmental pollution, reduce the morbidity of occupational diseases, remove an electric heating reflowing process and ensure the safety production.

Description

By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum
Technical field
The present invention relates to a kind of chromatograph assay method of material, belong to particularly a kind of method of measuring anthracene content in coking industry carbolineum by micellar electrokinetic capillary chromatography.
Background technology
What in industry standard YB/T 5086-2005 < < industry anthracene, in anthracene content assaying method > >, measure that in industrial anthracene, anthracene content adopts is chemical method.The analysis principle of the method is: anthracene is as conjugated diolefine, in organic solvent chlorobenzene, play addition reaction (9 with maleic anhydride, 10 there is Diels-Alder reaction), need add hot reflux 20 ~ 30 minutes, the cooling rear acid generating with the maleic anhydride hydrolysis of standard solution of sodium hydroxide titration surplus, then be converted into anthracene content according to standard solution of sodium hydroxide consumption.The method analysis time long (nearly 1 hour), the large and complex steps of personal error, adopts chlorobenzene (toxicity is larger) to make solvent environment and operating personnel healthy is all produced to harmful effect.
Due to features such as chromatography have good separating effect, analysis speed is fast, detection sensitivity is high, applied widely and easy and simple to handle, in production, scientific research, teaching, food, environmental protection, universe exploration etc. are multi-field, be used widely.Capillary column claims again open hole capillary column or open-tubular capillary column, internal diameter mostly is 0.1~0.5mm, fixing phase portion and interposition is hollow in the inner, so chromatographic column perviousness is large, resistance to mass tranfer is little, has better separation efficiency, analysis speed faster than packed column.The theoretical cam curve of every meter of column length of conventional packed column is 102~103, capillary column is 103~104, post effect is slightly better than conventional packed column, but the column length of capillary column mostly is the more than 10 times of conventional packed column, total post effect is more much higher than conventional packed column, therefore when Analysis of Complex sample, can show its characteristic.
At present, employing is that chemical method is measured the anthracene content in industrial anthracene.Because adopting chlorobenzene, chemical method makes solvent and maleic acid anhydride reactant, with NaOH titration, anthracene content in industrial anthracene is carried out to quantitative test, toxicity is larger, easily operator's physical and mental health is damaged, and operating process is loaded down with trivial details, analysis time is long, and the general used time is at 40 ~ 50 minutes, and has the artificial drawbacks such as systematic error.
Before the present invention, do not adopt chromatography determination coking industry complex sample, because the pre-service of sample is more difficult, because anthracene in industrial anthracene, phenanthrene, carbazole, firefly anthracene, pyrene, the material such as to bend be the condensed-nuclei aromatics at three rings or Fourth Ring, under general solvent normal temperature, normal means are difficult to it to dissolve completely, therefore cannot carry out stratographic analysis.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of and measure that anthracene content in industrial anthracene is accurate, sample pretreatment simple, it is convenient to measure, analysis time is short, non-environmental-pollution by micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum.
Realize the measure of above-mentioned purpose:
By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: according to actual sample concentration preparation standard specimen, accurately take chromatographically pure anthracene and internal standard compound azophenlyene, the amount that the quality that internal standard compound azophenlyene adds and sample add is basically identical, according to 15 ~ 25 times of anthracene reference material quality, add N, N-dimethylacetamide solvent, pack in the sample bottle with sealing gasket, with whirlpool mixed instrument, be mixed stand-by;
2) prepared standard specimen is analyzed with capillary chromatography, and correction factor is calculated:
A with micro syringe by standard sample solution injecting chromatograph, measure the peak area that can obtain anthracene and internal standard compound azophenlyene, measuring number of times is 2 ~ 3 times, the peak area of anthracene and internal standard compound azophenlyene is got to arithmetic mean substitution formula and calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene;
B calculates anthracene according to the following formula with respect to the area relative correction factor of internal standard compound azophenlyene:
Figure 210916DEST_PATH_IMAGE001
In formula: f i-represent that anthracene is with respect to the area relative correction factor of internal standard compound azophenlyene;
a s -representing the peak area of internal standard compound azophenlyene in standard specimen, unit is: μ Vs or pAs;
a i -representing the peak area of anthracene in standard specimen, unit is: μ Vs or pAs;
m i -representing the quality of anthracene in standard specimen, unit is: g;
m s -representing the quality of internal standard compound azophenlyene in standard specimen, unit is: g;
3) sample is measured:
A accurately takes industrial anthracene sample size and internal standard compound azophenlyene amount, and internal standard compound azophenlyene amount is 25 ~ 45% of industrial anthracene sample size;
B is the industrial anthracene sample and the internal standard compound azophenlyene that take, adds DMA solvent according to 15 ~ 25 times of its industrial anthracene sample weight, packs in the sample bottle with sealing gasket, with whirlpool mixed instrument, is mixed stand-by;
C heats sample bottle in the container being not less than at 80 ℃, and the heat time is no less than 30 seconds, with whirlpool mixed instrument, stirs;
D takes out sample with micro syringe and injects capillary chromatography from sample bottle;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 280 ~ 300 ℃;
Detected temperatures: 250 ~ 300 ℃;
Post flow: 2.0 ~ 3.0mL/min;
Before post, press: 0.05 ~ 1.0 MPa;
H 2flow: 25 ~ 45 mL/min;
Air mass flow: 250 ~ 450 mL/min;
Split ratio: 30 ~ 60:1;
Tail blows: 20 ~ 30 mL/min;
Sample size: 0.5 ~ 1.0 μ L;
Half-peak breadth: 3min;
Smallest peaks area: delete impurity peaks by actual conditions, be not less than 50 μ Vs;
4) according to following formula, calculate the weight percent content value of anthracene in industrial anthracene:
Figure 44005DEST_PATH_IMAGE002
%
In formula:
X i-represent the massfraction of industrial anthracene, unit: %;
A ithe peak area of anthracene in-expression sample, unit: μ Vs or pAs;
A sthe peak area of internal standard compound azophenlyene in-expression sample, unit: μ Vs or pAs;
M sthe quality of internal standard compound azophenlyene in-expression sample, unit: g;
M examinationthe quality of-expression anthracene sample, unit: g.
It is characterized in that: each sample replication is secondary at least, and the arithmetic mean value of getting its replication end value is as measurement result value.
The present invention is compared with prior art: the present invention adopts dissolves that the good solvent of industrial anthracene effect, capillary column are separated, interior gauged method, can be simply, convenient, measure anthracene content in industrial anthracene accurately, reliably, accuracy, precision, automaticity improve a lot.More former method analysis time of the method has great advantage, and the whole sample analysis time is no more than 12 minutes, detection efficiency multiplication (than fast nearly 5 times of former method), and labour productivity is greatly improved.Sample pretreatment is simple, and operating process intermediate link is few, and systematic error reduces greatly.From environmental protection, safety method, consider, chromatographic application has reduced environmental pollution, has reduced the incidence of disease of occupational illness, has removed electrical heating reflux course, has guaranteed safety in production.
Embodiment
Below the present invention is described in detail:
Because the mass percentage content different manufacturers content range of anthracene in industrial anthracene is different, during preparation standard specimen, should consider that the concentration of standard specimen and actual sample concentration are more approaching better.It is applicable to following embodiment.
Embodiment 1
By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: accurately take anthracene reference material 0.0379g, azophenlyene 0.1000g, add 6mLN, N-dimethylacetamide solvent, packs in the sample bottle with sealing gasket, is mixed stand-by with whirlpool mixed instrument;
2) prepared standard sample solution is analyzed with capillary chromatography, and correction factor is calculated:
A gets in 0.5 μ L standard solution inject gas chromatograph and measures with micro syringe, and measuring number of times is 2 times, obtains respectively the average peak area A of anthracene ibe 1560.9282 μ V s, the average peak area A of internal standard compound azophenlyene sbe 3323.5842 μ Vs;
B is by asking correction factor formula
Figure 891876DEST_PATH_IMAGE003
calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene, f i=0.80698;
3) sample is measured:
The industrial anthracene sample mass number that A accurately takes is 0.3000g, and the internal standard compound azophenlyene mass number accurately taking is according to 33% of industrial anthracene sample mass number, therefore internal standard compound azophenlyene mass number is 0.1000g;
B pours the industrial anthracene sample taking and internal standard compound azophenlyene in the sample bottle with sealing gasket into, gets solvent according to 20 times of industrial anthracene sample size, adds 6mL DMA solvent;
The container that C is placed in sample plasma bottle at 82 ℃ heats, and the heat time is 35 seconds, with the even sample of whirlpool mixed instrument;
D gets 0.5 μ L with micro syringe by the sample after mixing and injects capillary gas chromatograph;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 280 ℃;
Detected temperatures: 250 ℃;
Post flow: 2.2mL/min;
Before post, press: 0.058MPa;
H 2flow: 28 mL/min;
Air mass flow: 280 mL/min;
Split ratio: 35:1;
Tail blows: 20 mL/min;
Sample size: 0.5 μ L;
Half-peak breadth: 3min;
Smallest peaks area: 50 μ Vs;
4) according to following formula, calculate the mass percentage content value 2 times of anthracene in industrial anthracene: known: A ibe respectively 9063.6231 μ Vs, 9054.7129 μ Vs, A sbe respectively 6360.5124 μ Vs, 6355.2001 μ Vs, m sbe 0.1000 g, m examinationbe 0.3000 g, f ivalue is 0.8070, corresponding data substitution respectively:
Figure 551527DEST_PATH_IMAGE004
% calculates, the arithmetic mean X of twice ibe 38.3325%
Be that measurement result is the mass percentage content of anthracene in industrial anthracene.
By statistics, this is implemented minute and has only used 8.5 minutes, compare and adopt shortened nearly 42 minutes 50 minutes used times of chemical method, and the data precision of measuring is than adopting chemical method to improve two-decimal.
Above-described embodiment only exemplifies for the best, and is not the restriction to embodiments of the present invention.
Embodiment 2
By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: accurately take anthracene reference material 0.0455g, azophenlyene 0.1050g; Add 7.5mLN, N-dimethylacetamide solvent, packs in the sample bottle with sealing gasket, with whirlpool mixed instrument, is mixed stand-by;
2) prepared standard sample solution is analyzed with capillary chromatography, and correction factor is calculated:
A gets in 0.6 μ L standard solution inject gas chromatograph with micro syringe, and measures, and measuring number of times is 2 times, obtains respectively the average peak area A of anthracene ibe 1732.3580 μ Vs, the average peak area A of internal standard compound azophenlyene sbe 3107.4426 μ Vs;
C is by asking correction factor formula
Figure 510256DEST_PATH_IMAGE003
calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene, f i=0.7772;
3) sample is measured:
The industrial anthracene sample mass number that A accurately takes is 0.3500g, and the internal standard compound azophenlyene mass number accurately taking is according to 30% of industrial anthracene sample mass number, therefore internal standard compound azophenlyene mass number is 0.1050g;
B pours the industrial anthracene sample taking and internal standard compound azophenlyene in the sample bottle with sealing gasket into, gets solvent according to 25 times of industrial anthracene sample size, adds 7.5mL DMA solvent;
The container that C is placed in sample plasma bottle at 80 ℃ heats, and the heat time is 30 seconds, with the even sample of whirlpool mixed instrument;
D gets 0.6 μ L with micro syringe by the sample after mixing and injects capillary gas chromatograph;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 280 ℃;
Detected temperatures: 270 ℃;
Post flow: 2.4mL/min;
Before post, press: 0.062MPa;
H 2flow: 30 mL/min;
Air mass flow: 300 mL/min;
Split ratio: 40:1;
Tail blows: 22 mL/min;
Sample size: 0.6. 0 μ L;
Half-peak breadth: 3min;
Smallest peaks area: 50 μ Vs;
4) according to following formula, calculate the mass percentage content value 2 times of anthracene in industrial anthracene: known: A ibe respectively 8967.2567 μ Vs, 8945.7812 μ Vs, A sbe respectively 6725.8145 μ Vs, 6738.9023 μ Vs, m sbe 0.1050 g, m examinationbe 0.3500 g, f ivalue is 0.7772, corresponding data substitution respectively:
Figure 430807DEST_PATH_IMAGE004
% calculates, the arithmetic mean X of twice ibe 31.0160%,
Be that measurement result is the mass percentage content of anthracene in industrial anthracene.
By statistics, this is implemented minute and has only used 8.3 minutes, compare and adopt shortened nearly 42 minutes 50 minutes used times of chemical method, and the data precision of measuring is than adopting chemical method to improve two-decimal.
Above-described embodiment only exemplifies for the best, and is not the restriction to embodiments of the present invention.
Embodiment 3
By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: accurately take anthracene reference material 0.0519g, azophenlyene 0.1400g; Add 9.2mLN, N-dimethylacetamide solvent, packs in the sample bottle with sealing gasket, with whirlpool mixed instrument, is mixed stand-by;
2) prepared standard sample solution is analyzed with capillary chromatography, and correction factor is calculated:
A gets in 0.8 μ L standard solution inject gas chromatograph and measures with micro syringe, and measuring number of times is 2 times, obtains respectively the average peak area A of anthracene ibe 1797.3326 μ Vs, the average peak area A of internal standard compound azophenlyene sbe 4779.8643 μ Vs;
B is by asking correction factor formula
Figure 918420DEST_PATH_IMAGE003
calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene, f i=0.9858
3) sample is measured:
The industrial anthracene sample mass number that A accurately takes is 0.4g, and the internal standard compound azophenlyene mass number accurately taking is according to 35% of industrial anthracene sample mass number, therefore internal standard compound azophenlyene mass number is 0.14g;
B pours the industrial anthracene sample taking and internal standard compound azophenlyene in the sample bottle with sealing gasket into, gets solvent according to 23 times of industrial anthracene sample size, adds 9.2mL DMA solvent;
The container that C is placed in sample bottle at 85 ℃ heats, and the heat time is 40 seconds, with the even sample of whirlpool mixed instrument;
D gets 0.8 μ L with micro syringe by the sample after mixing and injects capillary gas chromatograph;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 290 ℃;
Detected temperatures: 280 ℃;
Post flow: 2.5mL/min;
Before post, press: 0.070MPa;
H 2flow: 35 mL/min;
Air mass flow: 350 mL/min;
Split ratio: 45:1;
Tail blows: 24 mL/min;
Sample size: 0.8 μ L;
Half-peak breadth: 3min;
Smallest peaks area: 50 μ Vs;
4) according to following formula, calculate the mass percentage content value 2 times of anthracene in industrial anthracene: known, A ibe respectively 8241.6247 μ Vs, 8256.7180 μ Vs, A sbe respectively 7855.2035 μ Vs, 7864.3247 μ Vs, m sbe 0.14 g, m examinationbe 0.4 g, f ivalue is 0.9858, corresponding data substitution respectively
% calculates, the arithmetic mean X of twice ibe 36.2095%
Be that measurement result is the mass percentage content of anthracene in industrial anthracene.
By statistics, this is implemented minute and has only used 8.2 minutes, compare and adopt the used time of chemical method to have shortened nearly 41 minutes with 49 minutes, and the data precision of measuring is than adopting chemical method to improve two-decimal.
Embodiment 4
By micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: accurately take anthracene reference material 0.0603g, azophenlyene 0.1600g; Add 12.5mLN, N-dimethylacetamide solvent, packs in the sample bottle with sealing gasket, with whirlpool mixed instrument, is mixed stand-by;
2) prepared standard sample solution is analyzed with capillary chromatography, and correction factor is calculated:
A gets in 1.0 μ L standard solution inject gas chromatographs and measures with micro syringe, and measuring number of times is 2 times, obtains respectively the average peak area A of anthracene ibe 2228.3071 μ V s, the average peak area A of internal standard compound azophenlyene sbe 3923.5842 μ Vs;
B is by asking correction factor formula
Figure 686842DEST_PATH_IMAGE003
calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene, f i=0.6948
3) sample is measured:
The industrial anthracene sample mass number that A accurately takes is 0.5000g, and the internal standard compound azophenlyene mass number accurately taking is according to 40% of industrial anthracene sample mass number, therefore internal standard compound azophenlyene mass number is 0.2000g;
B pours the industrial anthracene sample taking and internal standard compound azophenlyene in the sample bottle with sealing gasket into, gets solvent according to 25 times of industrial anthracene sample size, adds 12.5mL DMA solvent;
The container that C is placed in sample bottle at 90 ℃ heats, and the heat time is 45 seconds, with the even sample of whirlpool mixed instrument;
D gets 1.0 μ L with micro syringe by the sample after mixing and injects capillary gas chromatograph;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 300 ℃;
Detected temperatures: 290 ℃;
Post flow: 2.6mL/min;
Before post, press: 0.073MPa;
H 2flow: 40 mL/min;
Air mass flow: 400 mL/min;
Split ratio: 50:1;
Tail blows: 25 mL/min;
Sample size: 1.0 μ L;
Half-peak breadth: 3;
Smallest peaks area: 60 μ Vs;
4) according to following formula, calculate the mass percentage content value secondary of anthracene in industrial anthracene: known, A ibe respectively 10334.9169 μ Vs, 10367.2023 μ Vs, A sbe respectively 7916.3725 μ Vs, 7922.5146 μ Vs, m sbe 0.2000 g,
M examinationbe 0.5000 g, f ivalue is 0.6948, corresponding data substitution respectively:
Figure 602846DEST_PATH_IMAGE004
% calculates, the arithmetic mean X of twice ibe 36.3255 %
Be that measurement result is the mass percentage content of anthracene in industrial anthracene.
By statistics, this is implemented minute and has only used 8 minutes, compare and adopt shortened nearly 42 minutes 50 minutes used times of chemical method, and the data precision of measuring is than adopting chemical method to improve two-decimal.
Above-described embodiment only exemplifies for the best, and is not the restriction to embodiments of the present invention.

Claims (2)

1. by micellar electrokinetic capillary chromatography, measure the method for anthracene content in coking industry carbolineum, its step:
1) preparation standard specimen: according to actual sample concentration preparation standard specimen, accurately take chromatographically pure anthracene and internal standard compound azophenlyene, the amount that the quality that internal standard compound azophenlyene adds and sample add is basically identical, according to 15 ~ 25 times of anthracene reference material quality, add N, N-dimethylacetamide solvent, pack in the sample bottle with sealing gasket, with whirlpool mixed instrument, be mixed stand-by;
2) prepared standard specimen is analyzed with capillary chromatography, and correction factor is calculated:
A with micro syringe by standard sample solution injecting chromatograph, measure the peak area that can obtain anthracene and internal standard compound azophenlyene, measuring number of times is 2 ~ 3 times, the peak area of anthracene and internal standard compound azophenlyene is got to arithmetic mean substitution formula and calculate anthracene with respect to the area relative correction factor of internal standard compound azophenlyene;
B calculates anthracene according to the following formula with respect to the area relative correction factor of internal standard compound azophenlyene:
Figure 35318DEST_PATH_IMAGE001
In formula: f i-represent that anthracene is with respect to the area relative correction factor of internal standard compound azophenlyene;
a s -representing the peak area of internal standard compound azophenlyene in standard specimen, unit is: μ Vs or pAs;
a i -representing the peak area of anthracene in standard specimen, unit is: μ Vs or pAs;
m i -representing the quality of anthracene in standard specimen, unit is: g;
m s -representing the quality of internal standard compound azophenlyene in standard specimen, unit is: g;
3) sample is measured:
A accurately takes industrial anthracene sample size and internal standard compound azophenlyene amount, and internal standard compound azophenlyene amount is 25 ~ 45% of industrial anthracene sample size;
B is the industrial anthracene sample and the internal standard compound azophenlyene that take, adds DMA solvent according to 15 ~ 25 times of its industrial anthracene sample weight, packs in the sample bottle with sealing gasket, with whirlpool mixed instrument, is mixed stand-by;
C heats sample bottle in the container being not less than at 80 ℃, and the heat time is no less than 30 seconds, with whirlpool mixed instrument, stirs;
D takes out sample with micro syringe and injects capillary chromatography from sample bottle;
E carries out stratographic analysis under the test condition of regulation:
Analysis condition:
Chromatographic column: model DB-5, is of a size of: 30.00m * 0.32mm * 0.25 μ m;
Detecting device: flame ionization ditector;
Vapourizing temperature: 280 ~ 300 ℃;
Detected temperatures: 250 ~ 300 ℃;
Post flow: 2.0 ~ 3.0mL/min;
Before post, press: 0.05 ~ 1.0 MPa;
H 2flow: 25 ~ 45 mL/min;
Air mass flow: 250 ~ 450 mL/min;
Split ratio: 30 ~ 60:1;
Tail blows: 20 ~ 30 mL/min;
Sample size: 0.5 ~ 1.0 μ L;
Half-peak breadth: 3min;
Smallest peaks area: delete impurity peaks by actual conditions, be not less than 50 μ Vs;
4) according to following formula, calculate the weight percent content value of anthracene in industrial anthracene:
Figure 207673DEST_PATH_IMAGE002
%
In formula: X i-represent the massfraction of industrial anthracene, unit: %;
A ithe peak area of anthracene in-expression sample, unit: μ Vs or pAs;
A sthe peak area of internal standard compound azophenlyene in-expression sample, unit: μ Vs or pAs;
M sthe quality of internal standard compound azophenlyene in-expression sample, unit: g;
M examinationthe quality of-expression anthracene sample, unit: g.
2. the method for measuring grace content in coking industry carbolineum by micellar electrokinetic capillary chromatography as claimed in claim 1, it is characterized in that: each sample replication is secondary at least, and the arithmetic mean value of getting its replication end value is as measurement result value.
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CN1164647A (en) * 1996-09-01 1997-11-12 武汉钢铁(集团)公司 Chromatographic column for analysising anthracene oil in tar and using method

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