CN104698115A - Method for measuring content of n-alkanes in liquid paraffin - Google Patents
Method for measuring content of n-alkanes in liquid paraffin Download PDFInfo
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- CN104698115A CN104698115A CN201510068226.XA CN201510068226A CN104698115A CN 104698115 A CN104698115 A CN 104698115A CN 201510068226 A CN201510068226 A CN 201510068226A CN 104698115 A CN104698115 A CN 104698115A
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Abstract
The invention discloses a method for measuring the content of n-alkanes in liquid paraffin. The problem that only the content of n-alkanes is measured in the prior art is solved. The method comprises the following steps: measuring the percentage composition of n-alkanes in liquid paraffin and the content of isoparaffin and accurately analyzing the carbon number distribution of the n-alkanes. According to the technical key points, the method comprises the following steps: taking a sample with the injection volume of 0.2 microL, verifying the n-alkanes according to the order of the boiling points by virtue of a hydrogen flame detector by using an elastic quartz capillary column coated with a fixing solution OV-101 under an experimental temperature meeting condition and adopting a temperature programming method, so as to obtain the chromatographic peaks of n-alkanes and non-normal alkanes, and performing peak area normalization quantification. Therefore, the separation effect of the n-alkanes in the liquid paraffin on the OV-101 elastic quartz capillary column can be achieved.
Description
Technical field
The present invention relates to petrochemicals detection technique field, is a kind of assay method utilizing vapor-phase chromatography to carry out tracer liquid paraffin normal paraffin content specifically.
Background technology
Whiteruss is a kind of important industrial chemicals, and whiteruss proterties is colourless transparent oil liquid, cannot not observe aobviously fluorescence in the sunlight.Odorless tasteless under room temperature, after heating, slightly oil is smelly, is obtained through decompression distillation by heavy oil.Principal ingredient is the potpourri of C16-C20 n-alkane composition.A series of chemical products can be obtained, as chlorinated paraffin, farm chemical emulgent, fatty alcohol, the synthetic detergent that can be degraded, plastic plasticizer, fertilizer additive and cosmetics, protein concentrate etc. from it.Sometimes white oil is also known as liquid wax.But structure exist significantly different.Be that the light distillate such as kerosene, diesel oil is refined through molecular sieve and cold press dewaxing, the concentrated sulphuric acid, alkali cleaning, make after washing.According to cut, liquid paraffin,light and Paraffin liquid heavy can be divided into, and the various n-alkane monomer of C11 to C18 or the potpourri of several n-alkane.The volatilization character of each n-alkane, kinematic viscosity are different, have thus derived various application.Light wax is generally containing c9-c13, and heavy wax is generally containing c13-c16.We adopt OV 1 fused-silica capillary column with Agilent 7890 type gas chromatograph for this reason, achieve the effect be better separated, and each analysis only needs 57.5 minutes, except obtaining normal paraffin content, also obtains the carbon number distribution of n-alkane.Although can measure existing China Petrochemical Industry rower SH/T0410-92, need two instruments, be not suitable with the needs of a large amount of sample analysis.Normal paraffin content can only be measured to China Petrochemical Industry rower SH/T0412-92.Now this is improved.
Summary of the invention
Object of the present invention: be exactly the assay method that a kind of whiteruss normal paraffin content is provided for existing Problems existing, to determine normal paraffin content quickly and accurately, and the carbon number distribution of n-alkane.
The object of the invention is to realize by following technical solution:
Test determination step comprises: set by the chromatographic condition of gas chromatograph: body of first ventilating, rear energising;
Carrier gas is nitrogen, and purity is greater than 99.99% (V/V); Combustion gas is hydrogen, and purity is greater than 99.99% (V/V); Combustion-supporting gas is air, through silica gel and 5A molecular sieve drying, purification; Standard specimen: nC12, nC13, nC14, nC15, nC16, (chromatographically pure)
Start intensification order: detecting device, injection port, column temperature, column oven heats up and should arrange when the former two's temperature is greater than column oven preset temperature; All do not exceed specified maximum temperature; The initial 130 DEG C of maintenances (5min) of column temperature, then rise to 240 DEG C with 4 DEG C/min, keep 25min;
Temperature of vaporization chamber 280 ~ 300 DEG C;
Detector temperature 280 ~ 300 DEG C;
Hydrogen flowing quantity: 30ml/min;
Air mass flow: 300 ~ 500ml/min scope 400ml/min;
N2: inlet pressure 25.9psi;
Split ratio: 30:1
Apply this condition to measure sample, carry out quantitatively by normalization method to each n-alkane recorded, each n-alkane peak area recorded and isoparaffin peak area are added together, and quantitatively calculate by normalization, computing formula is as follows:
In formula: the percentage composition (weight) of n-alkane in W%--whiteruss;
A
positive structure-n-alkane peak area sum;
A
isomery-isoparaffin peak area sum.
Principle of work: this method adopts the method for temperature programme.Concerning each wish analysis bank is divided, there is an optimum column temperature, for the multi-component blend sample of wide boiling range, select the heating mode be suitable for by experiment, to reach desirable separating effect.
Qualitative analysis: in whiteruss, n-alkane is by carbon number continuous distribution, elasticity OV-101 capillary column is pressed boiling point order and flows out, the large peak in chromatogram is n-alkane, and peak-to-peak small peak is isoparaffin.
Quantitative test: the sample size of this invention is 0.2uL, because excessive concentration, sample signal is strengthened, makes chromatographic peak broaden simultaneously, be unfavorable for the separation of sample, cause pillar to transship, make result inaccurate.Concentration is too low, and sample signal is too weak, and each component area is too little, makes result inaccurate.Therefore, through debugging, sample size is the accurate separation that 0.2uL is applicable to this capillary column.
The method adopts normalization method to carry out quantitatively.The method is easy, and accurately, the change of operating conditions (as flow velocity, column temperature) is less to quantitative Influence on test result.This can realize n-alkane better separating effect on OV-101 fused-silica capillary column in whiteruss.
The method and technology scheme of the positive structure content of liquid wax of the present invention is: use vapor-phase chromatography, and wherein, chromatographic column adopts fused-silica capillary column, long 30m, interior painting OV-101 immobile liquid, and flame ionization ditector selected by detecting device; Carrier gas is High Purity Nitrogen.
When nitrogen is carrier gas, the sensitivity of hydrogen flame detector is high, and the range of linearity is wide.When air is combustion-supporting gas, it provides necessary oxygen, also plays a CO simultaneously
2and H
2the purging effect that the comburants such as O are taken away, usual air velocity is 10 times of hydrogen flow rate.Be generally 300 ~ 500ml/min scope, be optimized for 400ml/min.
Sensing chamber's temperature must more than 120 DEG C, and due to combustion of hydrogen, produce a large amount of water vapor, water vapor can not be discharged from detecting device with steam condition, is condensed into water, and resistance is declined, and sensitivity reduces, and noise increases.The sensitive sensitivity temperature influence of major part detecting device is little, therefore detector temperature can refer to the maximum temperature setting of chromatographic column, and need not accurate optimization.Detecting device preference temperature 280 DEG C ~ 300 DEG C in the present invention, optimum temperature is 300 DEG C.
The selection of column temperature: make material both be separated completely, does not make again peak shape expand, trails.Column temperature generally selects each component boiling point medial temperature or lower.When analyzed component boiling spread is very wide, now adopts temperature programme way, can satisfactory result be obtained.The initial 130 DEG C of maintenances (5min) of column temperature of the present invention, then rise to 240 DEG C with 4 DEG C/min.
Temperature of vaporization chamber is selected: higher than sample component maximum boiling point 30 ~ 50 DEG C or higher than column temperature 30 ~ 70 DEG C, peak shape favorable reproducibility, illustrates that vaporization makes proper temperature.Temperature of vaporization chamber of the present invention can select 280 ~ 300 DEG C, and optimum temperature is 300 DEG C.
It is exactly the gas produced of vaporizing after sample enters injection port that split ratio is selected, and enters chromatographic column and the ratio of discharging injector.Because the gas that sample vaporization produces can not enter chromatographic column completely, be separated, then enter detecting device detection.1), the volume containing the sample of chromatographic column is not infinitely great, and too much sample enters chromatographic column and can overload, and causes separation efficiency to decline, and peak distortion is trailed, also can serviceable life.Go out so part will be shunted.2), because after chromatographic column thinner samples vaporization generation gas expansion, moment can not enter chromatographic column, but have the individual time quickly, but can not be oversize, otherwise bands of a spectrum can spectrum width.So some will be shunted in time.The split ratio selected in the present invention is 30:1.
The advantage that the present invention has and positive technique effect are: n-alkane data described in this patent, for paraffin resource rational utilization, the exploitation of paraffin processing technology and the allotment of special wax all most important.Normal paraffin content is important product quality data and technology controlling and process index.Our unit's whiteruss take diesel oil as raw material, and through isopropyl alcohol-urea dewaxing, obtain the whiteruss containing n-alkane, the normal paraffin content of this whiteruss is more than 90%.The present invention adopts quartz capillary column can analyze normal paraffin content fast, and can the large quantitative analysis collected specimens of continuous print, accuracy rate 100%.OV-101 fused-silica capillary column is made up of 100% dimethyl silicone polymer, non-polar stationary phase, there is excellent chemical inertness, sample component is separated, by the optimization to chromatogram column operation condition by boiling point height, use this chromatogram column analysis normal paraffin content, chromatogram figure is out attractive in appearance, and each Component seperation effect is very good, and baseline wander is little, measurement result accuracy rate is high, reproducible.In this chromatographic column, can normal paraffin content be measured, the carbon number distribution of n-alkane can also be obtained.This measuring speed is fast, applied range.
Accompanying drawing explanation
Fig. 1 is that whiteruss n-alkane of the present invention and isoparaffin are at chromatographic column separating effect spectrogram.(large peak is n-alkane, and peak-to-peak small peak is isoparaffin).
The present invention to be described in further detail by example below in conjunction with accompanying drawing; but following example is only the present invention's example wherein; do not represent the rights protection scope that the present invention limits, the scope of the present invention is as the criterion with claims.
Embodiment
1) reagent and material:
Combustion gas: hydrogen: purity can reach 99.99%.Thered is provided by hydrogen generator;
Carrier gas: nitrogen: purity can reach 99.99%.Thered is provided by high-pressure cylinder, after decompression, enter clarifier, removing impurity and water.Nebulizer gas pressure and flow is controlled respectively again by pressure maintaining valve and needle valve.Chromatographic column is entered by vaporizer;
Combustion-supporting gas: air, through silica gel and 5A molecular sieve drying, purification; Thered is provided by our unit's pressurized air;
Standard specimen: nC12, nC13, nC14, nC15, nC16 (chromatographically pure);
2) instrument
Gas chromatograph: Agilent 7890 type gas chromatograph, is furnished with flame ionization ditector;
Chromatographic column: OV-101 fused-silica capillary column, long 30m, internal diameter 0.32mm, thickness 0.3um.PE company N931-6025.
3) experimental procedure:
Chromatographic condition sets:
First open hydrogen generator, treat that pressure reaches 0.3Mpa, open nitrogen, air;
First set column temperature: initial 130 DEG C, keep (5min), then rise to 240 DEG C with 4 DEG C/min, keep 25min, when analyzed component boiling spread is very wide, now adopt temperature programme;
Temperature of vaporization chamber: 300 DEG C, suitable temperature of vaporization chamber can ensure that sample gasifies rapidly, does not cause again sample to decompose.Peak shape favorable reproducibility illustrates that temperature of vaporization chamber is suitable.Preference temperature is 280 DEG C ~ 300 DEG C;
The temperature of detecting device FID is 300 DEG C, can ensure sample gasification and not decompose just.Selectable temperature 280 DEG C ~ 300 DEG C.
Hydrogen flowing quantity: 30ml/min; Hydrogen flowing quantity is excessive, unstability of base line.The optimum flow ratio of nitrogen and hydrogen is between 1:1 ~ 1:1.5.
Nitrogen flow: 30ml/min
Air mass flow: 400ml/min; General hydrogen and air mass flow are than being 1:10.Flow velocity is too small, and oxygen-supplying amount is not enough, and response is low; Flow velocity is excessive, and make flame unstable, noise increases; It is generally 300 ~ 500ml/min scope.
N2: inlet pressure 25.9psi
Split ratio: 30:1; General soap film flowmeter is measured.The present invention inputs on N2000 workstation.
Sample size is: 0.2uL; Sample size is excessive, and peak broadens, and retention changes, can not be quantitative.Sample size is too small, and detector sensitivity is inadequate, can't check.Sample size selects 0.18uL ~ 0.22uL.
Vaporizer sample introduction sealing gasket, after sample introduction 10 ~ 20 times, should change in time.
In finished pot collected specimens, get 0.2uL sample with 1uL syringe, under operation condition of chromatogram, carry out stratographic analysis;
After 57.5 minutes, sample analysis terminates, and process data, print (preview) result.If retention time, not to upper, inputs correct retention time according to standard spectrogram, then print (preview) result.According to the chromatomap as described in Fig. 1 (c10 ~ c22 separating effect figure on a column), calculate normal paraffin content, quantitatively calculate the n-alkane in sample, quantivative approach adopts normalization method.
Shutdown order: first close hydrogen generator, open atmospheric valve; After column compartment temperature drops to room temperature, close nitrogen, air, Shutdown Hosts, close workstation.
Apply this kind of method to adopt liquid wax sample to liquid wax apparatus and measure, carry out quantitatively by normalization method to each n-alkane recorded, the each n-alkane peak area recorded and isoparaffin peak area are added together, and quantitatively calculate by normalization, computing formula is as follows:
In formula: the percentage composition (weight) of n-alkane in W%--whiteruss;
A
positive structure-n-alkane peak area sum;
A
isomery-isoparaffin peak area sum;
Table 1 is normal paraffin content (c10 ~ c22) tables of data
| Title | The total area | (peak area) normal paraffin content |
| C10 | 0.00000 | 0.0000 |
| C11 | 194.74829 | 0.4095 |
| C12 | 6449.66748 | 13.5624 |
| C13 | 7417.96680 | 15.5986 |
| C14 | 7159.43311 | 15.0549 |
| C15 | 6971.58643 | 14.6599 |
| C16 | 6441.07080 | 13.5443 |
| C17 | 5481.09326 | 11.5257 |
| C18 | 3007.13672 | 6.3234 |
| C19 | 914.80359 | 1.9237 |
| C20 | 191.99327 | 0.4037 |
| C21 | 52.05544 | 0.1095 |
| C22 | 17.49260 | 0.0368 |
| Total amount | 93.1524 |
From then on figure can find out that the normal paraffin content of this time experiment is 93.2%, and the content of isoparaffin is 6.8%.
Claims (4)
1. the assay method of whiteruss normal paraffin content, is characterized in that: test determination step comprises:
The chromatographic condition of gas chromatograph is set: body of first ventilating, rear energising;
Carrier gas is nitrogen, and purity is greater than 99.99% (V/V); Combustion gas is hydrogen, and purity is greater than 99.99% (V/V); Combustion-supporting gas is air, through silica gel and 5A molecular sieve drying, purification; Standard specimen: nC12, nC13, nC14, nC15, nC16 (chromatographically pure)
Start intensification order: detecting device, injection port, column temperature, column oven heats up and should arrange when the former two's temperature is greater than column oven preset temperature; All do not exceed specified maximum temperature; The initial 130 DEG C of maintenances (5min) of column temperature, then rise to 240 DEG C with 4 DEG C/min, keep 25min;
Temperature of vaporization chamber 280 ~ 300 DEG C;
Detector temperature 280 ~ 300 DEG C;
Hydrogen flowing quantity: 30ml/min;
Air mass flow: 300 ~ 500ml/min scope;
N2: inlet pressure 25.9psi;
Split ratio: 30:1
Apply this condition to measure sample, carry out quantitatively by normalization method to each n-alkane recorded, each n-alkane peak area recorded and isoparaffin peak area are added together, and quantitatively calculate by normalization, computing formula is as follows:
In formula: the percentage composition (weight) of n-alkane in W%--whiteruss;
A
positive structure-n-alkane peak area sum;
A
isomery-isoparaffin peak area sum;
Selected gas chromatograph Agilent 7890 type gas chromatograph is also furnished with the gas chromatograph of flame ionization ditector; Chromatographic column: OV-101 fused-silica capillary column, long 30m, internal diameter 0.32mm, thickness 0.3um, PE company N931-6025.
2. the assay method of whiteruss normal paraffin content according to claim 1, is characterized in that: air mass flow is 400ml/min.
3. the assay method of whiteruss normal paraffin content according to claim 1, is characterized in that: detecting device preference temperature is 300 DEG C.
4. the assay method of whiteruss normal paraffin content according to claim 1, is characterized in that: temperature of vaporization chamber selects 300 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106404954A (en) * | 2016-08-31 | 2017-02-15 | 北京彤程创展科技有限公司 | Method for measuring carbon number distribution in petroleum wax |
| CN107817302A (en) * | 2017-09-27 | 2018-03-20 | 中国石油天然气集团公司 | A kind of gas chromatography analysis method of petroleum hydrocarbon component |
| CN107966499A (en) * | 2016-10-19 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of method by near infrared spectrum prediction crude oil carbon number distribution |
| CN109030645A (en) * | 2018-07-20 | 2018-12-18 | 山西潞安纳克碳化工有限公司 | A kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil |
| CN111272936A (en) * | 2020-03-13 | 2020-06-12 | 中国石油大学(华东) | Method for dividing crude oil biodegradation grade by using n-alkane residual rate |
| CN111289667A (en) * | 2020-03-13 | 2020-06-16 | 中国石油大学(华东) | Method for dividing crude oil biodegradation grade by using normal paraffin loss rate |
| CN113267576A (en) * | 2021-05-14 | 2021-08-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for measuring n-isoparaffin content and carbon number distribution in wax by using gas chromatography |
| CN114965792A (en) * | 2022-06-14 | 2022-08-30 | 宁夏滨泽新能源科技有限公司 | Analysis method for rapidly detecting content of C4-C22 alkane |
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Cited By (12)
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|---|---|---|---|---|
| CN106404954A (en) * | 2016-08-31 | 2017-02-15 | 北京彤程创展科技有限公司 | Method for measuring carbon number distribution in petroleum wax |
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| CN107966499A (en) * | 2016-10-19 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of method by near infrared spectrum prediction crude oil carbon number distribution |
| CN107966499B (en) * | 2016-10-19 | 2023-05-05 | 中国石油化工股份有限公司 | Method for predicting crude oil carbon number distribution by near infrared spectrum |
| CN107817302A (en) * | 2017-09-27 | 2018-03-20 | 中国石油天然气集团公司 | A kind of gas chromatography analysis method of petroleum hydrocarbon component |
| CN107817302B (en) * | 2017-09-27 | 2020-05-08 | 中国石油天然气集团公司 | Gas chromatography analysis method for petroleum hydrocarbon components |
| CN109030645A (en) * | 2018-07-20 | 2018-12-18 | 山西潞安纳克碳化工有限公司 | A kind of method of carbon number distribution and n-alkane normal olefine in detection coal oil |
| CN111272936A (en) * | 2020-03-13 | 2020-06-12 | 中国石油大学(华东) | Method for dividing crude oil biodegradation grade by using n-alkane residual rate |
| CN111289667A (en) * | 2020-03-13 | 2020-06-16 | 中国石油大学(华东) | Method for dividing crude oil biodegradation grade by using normal paraffin loss rate |
| CN111272936B (en) * | 2020-03-13 | 2022-05-13 | 中国石油大学(华东) | Method for dividing crude oil biodegradation grade by using n-alkane residual rate |
| CN113267576A (en) * | 2021-05-14 | 2021-08-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for measuring n-isoparaffin content and carbon number distribution in wax by using gas chromatography |
| CN114965792A (en) * | 2022-06-14 | 2022-08-30 | 宁夏滨泽新能源科技有限公司 | Analysis method for rapidly detecting content of C4-C22 alkane |
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