CN111024864A - Liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene and determination method and application thereof - Google Patents
Liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene and determination method and application thereof Download PDFInfo
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- CN111024864A CN111024864A CN201911424459.3A CN201911424459A CN111024864A CN 111024864 A CN111024864 A CN 111024864A CN 201911424459 A CN201911424459 A CN 201911424459A CN 111024864 A CN111024864 A CN 111024864A
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Abstract
The invention discloses a liquid chromatograph for simultaneously measuring hydrocarbon composition and fatty acid methyl ester content in aviation kerosene and a measuring method and application thereof. The liquid chromatograph has a simple structure and high automation degree, can simultaneously determine the hydrocarbon composition and the fatty acid methyl ester content in the aviation kerosene, can detect the fatty acid methyl ester with the content limit of 5.0mg/kg in the aviation kerosene, and can be used as a reference standard for simultaneously determining the trace fatty acid methyl ester and the hydrocarbon composition in the aviation kerosene.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene, and a determination method and application thereof.
Background
Aviation kerosene is one of petroleum products, mainly composed of hydrocarbon compounds in different fractions, and is mainly used as fuel for aviation turbine engines, and has the following characteristics: the high-altitude performance and the combustion performance are good, the complete and stable combustion can be ensured, the carbon deposit is small, the smoke is less, the air resistance is not generated in the high-altitude flight, and the evaporation loss is small; low freezing point and good low-temperature fluidity; low sulfur and mercaptan sulfur content, low corrosivity and no odor; the smoke point is high, the glow value is proper, and the flame radiation capability is proper; the stability is good, the product is not easy to deteriorate when stored at normal temperature, and the generated colloid sediment is less at higher use temperature; deep refining degree, good cleanness, and good lubricity and abrasion resistance. Meanwhile, the aviation kerosene has no low saturated vapor pressure, has good thermal stability and can meet the requirement of supersonic high-altitude flight. In recent years, with the rapid development of economy, the demand for aviation kerosene has increased.
Aviation kerosene is a special fuel, and because the aviation kerosene and other fuels share one storage and transportation system in the links of pipe transportation, storage and the like, cross contamination cannot be completely avoided. With the commercial application, the risk of mixing trace Fatty Acid Methyl Ester (FAME) in the aviation kerosene is increasing. It is generally considered safe that the content of Fatty Acid Methyl Esters (FAME) in the aviation kerosene is less than 5 ppm. When the concentration of fatty acid methyl esters is sufficiently high, it can affect the thermal stability of the jet fuel. In addition, the pollution of fatty acid methyl ester can also affect the freezing point and the colloid of the aviation kerosene, so that the operation failure of the aviation engine is caused, and even the aviation kerosene is flamed out.
At present, the standard methods for determining trace Fatty Acid Methyl Ester (FAME) in aviation kerosene mainly comprise: IP585 and IP 590. The determination principle of the IP585 gas chromatography mass spectrometry is that a polar column is adopted to separate fatty acid methyl ester compounds and nonpolar hydrocarbon compound matrixes in aviation kerosene, and characteristic ions are selected for quantitative analysis. The principle of the IP590 liquid chromatography evaporation-refraction detector method is that fatty acid methyl ester compounds are separated from other fatty acid methyl ester compounds by a polar column, an evaporation-refraction detector is adopted, and quantification is carried out by an external standard method. The two methods can only carry out quantitative analysis on trace fatty acid methyl ester in the aviation kerosene. The method for measuring the group composition or the aromatic hydrocarbon content in the aviation kerosene mainly comprises the following steps: a fluorescence indicator adsorption method for measuring GB/T11132 liquid petroleum product hydrocarbons; high performance liquid chromatography of a differential refractometer for measuring the aromatic hydrocarbon content of NB/SH/T0939 aviation fuel and petroleum fractions. There is no standard method for simultaneous determination of trace fatty acid methyl esters and hydrocarbon compositions.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a liquid chromatograph for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content in aviation kerosene, a determination method and application thereof.
The invention is realized by the following steps:
in a first aspect, the invention provides a liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene, the liquid chromatograph comprising a sample injection device, a switching element, a first liquid chromatographic column, a second liquid chromatographic column and a detector; the liquid chromatograph has a first state and a second state;
the liquid chromatograph is in a first state, and the sample introduction device, the switching element, the first liquid chromatographic column, the second liquid chromatographic column and the detector are sequentially connected; the liquid chromatograph is in a second state that the first liquid chromatographic column is reversely connected behind the second liquid chromatographic column by rotating the switching element, and the sample feeding device, the switching element, the second liquid chromatographic column, the first liquid chromatographic column and the detector are sequentially connected in the second state of the liquid chromatograph.
In a second aspect, the present invention further provides a method for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content in aviation kerosene, comprising the following steps: separating and detecting a sample to be detected by adopting the liquid chromatograph, wherein the sample to be detected is aviation kerosene, and hydrocarbons in the aviation kerosene comprise saturated hydrocarbon, monocyclic aromatic hydrocarbon and bicyclic aromatic hydrocarbon;
adjusting the liquid chromatograph to be in a first state, enabling a sample to be detected to pass through a sample injection device, entering a first liquid chromatographic column along with a mobile phase, enabling hydrocarbons to completely flow out of the first liquid chromatographic column and enter a second liquid chromatographic column, and rotating a switching element when the fatty acid methyl ester does not flow out of the first liquid chromatographic column, enabling the liquid chromatograph to be in a second state that the first liquid chromatographic column is reversely connected behind the second liquid chromatographic column, enabling the fatty acid methyl ester to be firstly reversely blown to a detector for detection, then enabling the hydrocarbons to be separated into saturated hydrocarbons, monocyclic aromatic hydrocarbons and bicyclic aromatic hydrocarbons through the second liquid chromatographic column, then enabling the hydrocarbons to flow to the detector for detection through the reversely connected first liquid chromatographic column.
In a third aspect, the invention also provides the use of the above-mentioned determination method for determining a petroleum fraction containing or not containing fatty acid methyl esters and having a distillation range of 150 ℃ to 350 ℃;
preferably, the petroleum fraction includes any one of jet fuel and jet fuel.
The invention has the following beneficial effects:
the invention provides a liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene and a determination method and application thereof, wherein the liquid chromatograph at least comprises a switching element, a first liquid chromatographic column and a second liquid chromatographic column, the liquid chromatograph is adjusted to be in a first state in the determination process of the hydrocarbon and fatty acid methyl ester content in the aviation kerosene, a sample to be determined enters the first liquid chromatographic column along with a mobile phase through a sample introduction device, the hydrocarbon completely flows out of the first liquid chromatographic column and enters the second liquid chromatographic column, and when the fatty acid methyl ester does not flow out of the first liquid chromatographic column, the switching element is rotated to enable the liquid chromatograph to be in a second state after the first liquid chromatographic column is reversely connected to the second liquid chromatographic column, the fatty acid methyl ester is firstly reversely blown to a detector for detection, and then the hydrocarbon is separated into saturated hydrocarbon through the second liquid chromatographic column, Monocyclic aromatic hydrocarbon and bicyclic aromatic hydrocarbon pass through a first liquid chromatographic column which is reversely connected, and finally flow to a detector for detection, so that the simultaneous determination of the hydrocarbon composition and the fatty acid methyl ester content in the aviation kerosene is realized.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a liquid chromatograph in the present invention, and a solid line shows a schematic structural diagram of the liquid chromatograph in a first state, and a broken line shows a schematic structural diagram of the liquid chromatograph in a second state;
FIG. 2 is a flow chart of an analysis of a liquid chromatograph in a first state according to the present invention;
FIG. 3 is a flow chart of an analysis of a liquid chromatograph in a second state according to the present invention;
FIG. 4 is a high performance liquid chromatogram obtained by measurement in an example of the present invention.
Icon: 10-liquid chromatography; 11-a pump; 12-a sample injector; 13-a six-way valve; 131-a first communication port; 132-a second communication port; 133-a third communication port; 134-a fourth communication port; 135-fifth communication port; 136-sixth communication port; 14-a first liquid chromatography column; 15-a second liquid chromatography column; 16-differential refractive detector.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
The following describes the liquid chromatograph 10 for simultaneously measuring the hydrocarbon composition and the fatty acid methyl ester content of the aviation kerosene, and the measuring method and application thereof in the embodiment of the present invention, specifically, the switching element is a six-way valve (a four-way valve, an eight-way valve, etc. may also be used).
The liquid chromatograph 10 for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content of the aviation kerosene provided by the embodiment of the invention comprises a pump 11, an injector 12, a six-way valve 13, a first liquid chromatographic column 14, a second liquid chromatographic column 15 and a differential refraction detector 16.
The six-way valve 13 includes a first communication port 131, a second communication port 132, a third communication port 133, a fourth communication port 134, a fifth communication port 135, and a sixth communication port 136, which are arranged in this order in the clockwise direction.
The pump 11 is connected to the injector 12, and the liquid chromatograph 10 has a first state for feeding liquid (shown by a solid line in fig. 1) and a second state for detection (shown by a broken line in fig. 1), and the transition between the first state and the second state is realized by rotating the six-way valve 13.
In the first state, the liquid outlet of the sample injector 12 communicates with the second communication port 132 of the six-way valve 13 and communicates with the liquid inlet of the first liquid chromatography column 14 via the first communication port 131. The liquid outlet of the first liquid chromatography column 14 communicates with the fourth communication port 134 and with the liquid inlet of the second liquid chromatography column 15 via the third communication port 133. The liquid outlet of the second liquid chromatography column 15 is communicated with the differential refractive detector 16 through a fifth communication port 135 and a sixth communication port 136 in sequence.
After the six-way valve 13 is rotated to the second state for detection, the positions (positions in the entire apparatus) of the six communication ports of the six-way valve 13 are not changed, but the communication conditions of the six communication ports with each other are changed. In the second state, the liquid outlet of the sample injector 12 communicates with the second communication port 132 of the six-way valve 13 and communicates with the liquid inlet of the second liquid chromatography column 15 via the third communication port 133. The liquid outlet of the second liquid chromatography column 15 communicates with the fifth communication port 135 and with the liquid inlet of the first liquid chromatography column 14 via the fourth communication port 134. The liquid outlet of the first liquid chromatography column 14 is communicated with the differential refractive detector 16 through the first communication port 131 and the sixth communication port 136 in this order.
In other words, in the second state, after the first liquid chromatography column 14 is connected to the second liquid chromatography column 15 in the opposite direction, the sample to be measured and the mobile phase both flow through the second liquid chromatography column 15 and then flow through the first liquid chromatography column 14.
The idea of designing the liquid chromatograph provided in the embodiment of the invention is as follows: at present, for the detection of biodiesel containing fatty acid methyl ester, a conventional liquid chromatograph is mostly adopted, wherein only one liquid chromatograph column is included, however, fatty acid methyl ester is a mixture containing a large number of different components, and in the detection process, the fatty acid methyl ester cannot be quantitatively detected due to long peak emergence time, broadened chromatographic peak and the like of the fatty acid methyl ester, but the liquid chromatograph in the embodiment of the invention can be adopted to well solve the above problems because: before the fatty acid methyl ester flows out of the first liquid chromatographic column 14, the six-way valve 13 is rotated to enable the liquid chromatograph 10 to be in the second state, so that the fatty acid methyl ester flows out of the chromatographic column before the hydrocarbon components, and the fatty acid methyl ester flows out of the chromatographic column in the dead time of chromatographic detection, thereby greatly shortening the detection time and obviously improving the detection accuracy.
In some embodiments, the first liquid chromatography column 14 is an amino column or a cyano column. The second liquid chromatography column 15 is also an amino column or a cyano column.
Specifically, in the same liquid chromatograph 10, the first liquid chromatography column 14 and the second liquid chromatography column 15 may be both an amino column or both a cyano column or either one of the amino column and the cyano column.
In the present invention, the column length of the first liquid chromatography column 14 and the column length of the second liquid chromatography column 15 may be, for example, 10 to 300mm, for example, 10mm, 100mm, 150mm, 200mm, 250mm and 300 mm.
In some preferred embodiments, the column length of the first liquid chromatography column 14 may be 10-50 mm, such as 10mm, 30mm and 50 mm. The column length of the second liquid chromatography column 15 may be 100-300 mm, for example, 100mm, 150mm, 200mm, 250mm and 300 mm. The substances in the sample to be detected can be fully separated and eluted within the optimal length range, and the detection result has high accuracy.
It is worth noting that in the present invention, the second liquid chromatography column 15 has a longer column length than the first liquid chromatography column 14. In some embodiments, the column length of the first liquid chromatography column 14 may be 30mm, and correspondingly, the column length of the second liquid chromatography column 15 may be 250 mm.
In some preferred embodiments, the detector is any one of a differential refraction detector, an ultraviolet detector, an evaporative refraction detector, and a fluorescence detector.
In addition, the invention also provides a method for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content in the aviation kerosene, which comprises the following steps: the liquid chromatograph 10 provided by the invention is used for separating and detecting a sample to be detected.
The sample to be tested can comprise fatty acid methyl ester or hydrocarbon alone or can also comprise fatty acid methyl ester and hydrocarbon simultaneously. The hydrocarbons may include, for example, saturated hydrocarbons, monocyclic aromatics, and bicyclic aromatics.
It is worth mentioning that the term "monocyclic aromatic hydrocarbon" (MAH) as used in the present invention refers to compounds which have a longer retention time than most non-aromatic hydrocarbons but a shorter retention time than most bicyclic aromatic hydrocarbons on a particular polar column, such as benzene, tetralin and higher cycloalkylbenzenes (e.g. octahydrophenanthrene), thiophene, styrene, and conjugated polyenes, etc.; "bicyclic aromatic" (DAH) means that the retention time is longer than most monocyclic aromatics on a particular polar column.
During the measurement, the liquid chromatograph 10 is first adjusted to be in the first state, and the sample to be measured and the mobile phase sequentially enter the first liquid chromatography column 14 through the pump 11, the sample injector 12, the second communication port 132 and the first communication port 131, and sequentially enter the second liquid chromatography column 15 through the liquid outlet of the first liquid chromatography column 14 and the fourth communication port 134 and the third communication port 133. The analysis flow of this process is shown in FIG. 2, i.e., the sample to be measured and the flow phase flow through the pump 11, the sample injector 12, the first liquid chromatography column 14, the second liquid chromatography column 15 and the differential refraction detector 16 in turn.
Before the fatty acid methyl ester flows out of the first liquid chromatography column 14, the six-way valve 13 is rotated to bring the liquid chromatograph 10 into the second state, and the liquid outlet of the sample injector 12 is communicated with the second communication port 132 of the six-way valve 13 and with the liquid inlet of the second liquid chromatography column 15 through the third communication port 133. The liquid outlet of the second liquid chromatography column 15 communicates with the fifth communication port 135 and with the liquid inlet of the first liquid chromatography column 14 via the fourth communication port 134. The liquid outlet of the first liquid chromatography column 14 is communicated with the differential refractive detector 16 through the first communication port 131 and the sixth communication port 136 in this order. That is, after the first liquid chromatographic column 14 is reversely connected to the second liquid chromatographic column 15, the fatty acid methyl ester is firstly blown back to the differential refractive detector 16 for detection, then the hydrocarbons are separated into saturated hydrocarbons, monocyclic aromatic hydrocarbons and bicyclic aromatic hydrocarbons through the second liquid chromatographic column 15, then the hydrocarbons pass through the reversely connected first liquid chromatographic column 14, and finally the hydrocarbons flow to the detector 16 for detection.
The analytical flow of this process is shown in FIG. 3, i.e., in the column section, the sample to be measured and the mobile phase flow through the second liquid chromatography column 15 and the first liquid chromatography column 14 in turn, and then to the differential refractive index detector 16.
The invention adopts external standard method to quantify. The standard substances adopted by the hydrocarbons are
The standard substance used for (fatty acid methyl ester) is typically (BD100), and pure fatty acid methyl ester can be used, and the time for the fatty acid methyl ester to flow out of the first liquid chromatography column 14 is determined according to the reagents tested in the experimental process of the inventor, and then the time for the fatty acid methyl ester to flow out of the sample to be tested is determined.
In the present invention, the mobile phase includes at least one of n-heptane, n-pentane and isopropanol. Isocratic elution is adopted in the determination process, namely, the flow velocity of the mobile phase is kept unchanged all the time in the determination process. In the present invention, the flow rate of the mobile phase during isocratic elution may be, for example, 0.1 to 2.0mL/min, and accordingly, the measurement time may be 15 to 30 min.
Under the matching of the flow velocity range and the determination time, the condition that a chromatographic peak has tailing or has poor resolution can be avoided, and all substances can be fully separated.
Preferably, the sample volume of the sample to be tested in the embodiment of the present invention may be 10 to 50 μ L. The sample amount can enable the peak area of the chromatographic peak of each substance in the chromatogram obtained by detection to be moderate.
In the embodiment of the invention, the column temperature is 20-40 ℃, so that the peak can be rapidly generated, the retention time is shortened, and the accurate quantitative analysis result can be obtained.
The embodiment of the invention also provides an application of the determination method, such as the determination of fatty acid methyl ester with or without and petroleum fraction with distillation range of 150-350 ℃;
preferably, the petroleum fraction includes any one of jet fuel and gas fuel.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The present embodiment provides a liquid chromatograph 10 for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content in aviation kerosene, which includes a pump 11, an injector 12, a six-way valve 13, a first liquid chromatography column 14, a second liquid chromatography column 15, and a differential refraction detector 16.
The six-way valve 13 includes a first communication port 131, a second communication port 132, a third communication port 133, a fourth communication port 134, a fifth communication port 135, and a sixth communication port 136, which are arranged in this order in the clockwise direction.
The pump 11 is connected to the injector 12, and the liquid chromatograph 10 has a first state for feeding liquid and a second state for detection, and transition between the first state and the second state is performed by rotating the six-way valve 13.
In the first state, the liquid outlet of the sample injector 12 communicates with the second communication port 132 of the six-way valve 13 and communicates with the liquid inlet of the first liquid chromatography column 14 via the first communication port 131. The liquid outlet of the first liquid chromatography column 14 communicates with the fourth communication port 134 and with the liquid inlet of the second liquid chromatography column 15 via the third communication port 133. The liquid outlet of the second liquid chromatography column 15 is communicated with the differential refractive detector 16 through a fifth communication port 135 and a sixth communication port 136 in sequence.
After the six-way valve 13 is rotated to the second state for detection, the positions (positions in the entire apparatus) of the six communication ports of the six-way valve 13 are not changed, but the communication conditions of the six communication ports with each other are changed. In the second state, the liquid outlet of the sample injector 12 communicates with the second communication port 132 of the six-way valve 13 and communicates with the liquid inlet of the second liquid chromatography column 15 via the third communication port 133. The liquid outlet of the second liquid chromatography column 15 communicates with the fifth communication port 135 and with the liquid inlet of the first liquid chromatography column 14 via the fourth communication port 134. The liquid outlet of the first liquid chromatography column 14 is communicated with the differential refractive detector 16 through the first communication port 131 and the sixth communication port 136 in this order.
Wherein the first liquid chromatography column 14 is an amino column with a length of 30mm, and the second liquid chromatography column 15 is an amino column with a length of 250 mm.
The method for simultaneously determining the hydrocarbon composition and the fatty acid methyl ester content in the aviation kerosene by utilizing the liquid chromatograph comprises the following steps: firstly, the liquid chromatograph is injected, the instrument flow path is as shown in fig. 2, the mobile phase and flow rate of the liquid chromatograph are kept unchanged, the mobile phase and sample pass through the injector 12 by the pump 11, enter the first liquid chromatographic column 14 after passing through the six-way valve 13, and then enter the first liquid chromatographic column 14
After the fatty acid methyl ester enters the second liquid chromatographic column 15 through the first liquid chromatographic column 14 and before the fatty acid methyl ester does not flow out of the first liquid chromatographic column 14, the six-way valve 13 is rotated, the instrument flow path is as shown in fig. 3, at this time, after the first liquid chromatographic column 14 is reversely connected with the second liquid chromatographic column 15, the fatty acid methyl ester on the first liquid chromatographic column 14 is firstly reversely blown to the detector, and then the saturated hydrocarbon, the monocyclic aromatic hydrocarbon and the bicyclic aromatic hydrocarbon sequentially flow out and enter the differential refraction detector 16.
Measurement results
1. And performing liquid chromatography measurement on the aviation kerosene containing fatty acid methyl ester and hydrocarbons, wherein the liquid chromatography measurement result is shown in figure 4, in the figure 4, the peak 1 is the fatty acid methyl ester, the peak 2 is saturated hydrocarbon, the peak 3 is monocyclic aromatic hydrocarbon, and the peak 4 is bicyclic aromatic hydrocarbon. Therefore, the determination method provided by the embodiment of the invention can be used for separating fatty acid methyl ester, saturated hydrocarbon, monocyclic aromatic hydrocarbon and bicyclic aromatic hydrocarbon in the aviation kerosene, can realize complete separation of all substances, and is favorable for accurately determining the content of each substance by a detector.
2. The quantitative result of the bicyclic aromatic hydrocarbon in the article to be tested and the determination result of NB/SH/T0939-2016 in the embodiment of the invention are shown in Table 1.
TABLE 1 measurement of bicyclic aromatic hydrocarbons and NB/SH/T0939-2016
As can be seen from table 1 above: the quantitative result of the bicyclic aromatic hydrocarbon in the article to be detected in the embodiment of the invention is compared with the determination result of NB/SH/T0939-2016, and no obvious difference exists.
3. The results of the determination of the aromatic content in aviation kerosene containing different concentrations of fatty acid methyl esters in the examples of the present invention are shown in table 2.
TABLE 2 determination of aromatic content in aviation kerosene containing different concentrations of fatty acid methyl esters
Remarking: and the measurement results of the monocyclic aromatic hydrocarbon and the bicyclic aromatic hydrocarbon are calculated according to the actual sample weight of the aviation kerosene.
As can be seen from table 2 above: the quantitative results for aromatics in the examples of the invention were not affected by the addition of fatty acid methyl esters.
4. The results of the measurements of the contents of different amounts of methyl esters of fatty acids added to the test article of the present invention are shown in Table 3.
TABLE 3 results of measurements of aviation kerosene with various contents of fatty acid methyl esters
As can be seen from table 3 above: in the embodiment of the invention, for the quantitative result of the fatty acid methyl ester, the difference between the theoretical value and the measured value is small, which indicates that the accuracy rate of the determination of the fatty acid methyl ester is high.
5. The detection limit and quantification limit data for the fatty acid methyl ester assay in the test article of the present invention are shown in table 4.
Table 4 detection limit and quantitation limit data for fatty acid methyl ester assays
Remarking: in this example, the data is obtained by repeating the measurement 7 times for a aviation kerosene sample having a fatty acid methyl ester content of 30 mg/kg.
As can be seen from table 4 above: the limit of quantification of fatty acid methyl ester in the examples of the present invention was as low as 5.0 mg/kg.
Compared with the prior art, the embodiment provided by the invention has the following advantages:
1) the determination method realizes the simultaneous determination of the hydrocarbon composition and the fatty acid methyl ester content of the aviation kerosene containing fatty acid methyl ester.
2) The quantitative range of the determination of the fatty acid methyl ester by the determination method is wide, and the determination of the constant amount to the trace amount of the fatty acid methyl ester in the aviation kerosene can be realized.
3) The determination does not need to pre-separate the sample, has no consumable, and can save the experiment cost.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A liquid chromatograph for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene is characterized by comprising a sample injection device, a switching element, a first liquid chromatographic column, a second liquid chromatographic column and a detector; the liquid chromatograph has a first state and a second state;
when the liquid chromatograph is in a first state, the sample feeding device, the switching element, the first liquid chromatographic column, the second liquid chromatographic column and the detector are sequentially connected; make through rotating the switching element the liquid chromatograph is first liquid chromatography column dock in second state behind the second liquid chromatography column, just the liquid chromatograph is under the second state, the sampling device switching element the second liquid chromatography column first liquid chromatography column with the detector connects gradually.
2. The liquid chromatograph of claim 1, wherein the first liquid chromatography column is an amino column or a cyano column and the second liquid chromatography column is an amino column or a cyano column;
preferably, the column length of the first and second liquid chromatography columns is 10-300 mm;
more preferably, the column length of the first liquid chromatography column is 10-50 mm, and the column length of the second liquid chromatography column is 100-300 mm.
3. The liquid chromatograph of claim 1, wherein the sample injection device comprises a pump and a sample injector, wherein an outlet of the pump is connected to an inlet of the sample injector, and wherein an outlet of the sample injector is connected to an inlet of the switching element.
4. The liquid chromatograph of claim 1, wherein the detector is any one of a differential refraction detector, an ultraviolet detector, an evaporative refraction detector, and a fluorescence detector.
5. A method for simultaneously determining hydrocarbon composition and fatty acid methyl ester content in aviation kerosene is characterized by comprising the following steps: separating and detecting a sample to be detected by using a liquid chromatograph according to any one of claims 1 to 4, wherein the sample to be detected is aviation kerosene, and hydrocarbons contained in the aviation kerosene comprise saturated hydrocarbon, monocyclic aromatic hydrocarbon and bicyclic aromatic hydrocarbon;
adjust liquid chromatograph is first state, the sample to be measured passes through sampling device gets into along with the mobile phase first liquid chromatography column, in hydrocarbons flows out completely first liquid chromatography column gets into second liquid chromatography column, and fatty acid methyl ester has not flowed yet during first liquid chromatography column, rotate switching element makes liquid chromatograph is first liquid chromatography column connect in reverse in second state after the second liquid chromatography column, fatty acid methyl ester is earlier by the blowback extremely the detector detects, then hydrocarbons pass through second liquid chromatography column separation becomes saturated hydrocarbon, monocyclic aromatic hydrocarbon, dicyclic aromatic hydrocarbon, again connect in reverse first liquid chromatography column, flow to finally the detector detects.
6. The method of claim 5, wherein the mobile phase comprises at least one of n-heptane, n-pentane, and isopropanol.
7. The method according to claim 5, wherein the determination is performed by isocratic elution, and the flow rate of the mobile phase during isocratic elution is 0.1-2 mL/min.
8. The method according to claim 5, wherein the measurement time is 15-45 min and the column temperature is 20-40 ℃.
9. The method of claim 5, wherein the method has a limit of quantitative detection of fatty acid methyl esters in jet fuel as low as 5.0 mg/kg.
10. Use of a method for simultaneous determination of the hydrocarbon composition and the fatty acid methyl ester content in aviation kerosene according to any one of claims 5 to 9, wherein said method is used for determination of a petroleum fraction containing or not containing fatty acid methyl esters and having a distillation range of 150 ℃ to 350 ℃;
preferably, the petroleum fraction includes any one of jet fuel and jet fuel.
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