Method of determining content of diesel fuel in lubricating oil of internal combustion engine

FIELD: chemistry.

SUBSTANCE: method of determining content of diesel fuel in lubricating oil of an internal combustion engine involves the following stages: preparing a mixture which contains an oil sample and C5 hydrocarbon, such as C5 alkane; injecting the mixture into the injector (11) of gas chromatograph (10); obtaining chromatographs of the sample; determination of the firs parametre M, which characterises peak area related to C5 hydrocarbon, such as C5 alkane, determination the second parametre C, which characterises area of at least one peak, related to a hydrocarbon, which characterises diesel fuel; and determination of content T of diesel fuel using formula (I): where a and b are constants, which define equation y=ax+b of a calibrating straight line of the ratio of the second to the first parametres as a function of content of diesel fuel.

EFFECT: increased accuracy and reliability of analysis.

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The technical field to which the invention relates.

The invention relates to the analysis of lubricating oils, and in particular to the determination of fuel oil internal combustion engine.

The level of technology

Methods of analysis of the content of the diesel fuel in the lubricating oil are known, but are not quite satisfactory, especially in relation to the accuracy of the analysis. The reason lies in the difficulty of differentiation between diesel fuel, which contains mainly saturated and unsaturated hydrocarbons from C6to C25and lubricating oil, which contains mainly saturated and unsaturated hydrocarbons from C20to C50. Requires a very high degree of reliability of results, particularly for the development of engines equipped with particle filters.

Disclosure of inventions

The aim of the invention is to solve some of these problems. Thus, the invention provides a method of determining the content of the diesel fuel in the lubricating oil of the internal combustion engine, comprising the following stages:

- the formation of a mixture containing the sample of lubricating oil, and hydrocarbon, C5such as alkane C5in a predetermined ratio;

the injection of the mixture into the injector of the gas chromatograph;

- obtaining the chromatogram of the analyzed sample;

- the definition of the first parameter M, which characterizes the peak area of the chromatogram associated with the hydrocarbon, C5such as alkane C5,

- definition of the second parameter C describing the area, at least one peak of the chromatogram associated with the hydrocarbon characterizing diesel;

- definition of the content T of diesel fuel in the analyzed sample by the following formula:

where a and b are constants that determine the equation y=ax+b of the calibration straight line correlation between the second and the first parameters as a function of content of diesel fuel.

Other features and advantages of the invention will be clear from the description which is given to him later in this document the purpose of evidence, but not of limitation, with reference to the accompanying drawings, in which:

- figure 1 schematically illustrates the chromatograph according to the prior art;

- figure 2 illustrates the examples of the parameters of the chromatograph used in the context of the invention;

- figure 3 explains an example of the calibration straight line.

The invention provides a definition of the content of the diesel fuel in the sample of lubricating oil of the internal combustion engine. To form a mixture containing a sample of the Academy of Sciences of litereature lubricating oils and hydrocarbon, C 5such as

C5alkane, in a predetermined ratio. The sample is injected and receive the chromatogram of the sample. Define the parameter characterizing the peak area of hydrocarbon, C5that is the parameter characterizing the peak associated with hydrocarbon characterizing diesel fuel. Based on the results of the calibration of these parameters define the content of a diesel fuel sample.

In this patent application the term "hydrocarbon, Cn" belongs to the family of isomeric compounds with n more than 5.

Figure 1 explains the chromatograph of the prior art. The chromatograph 10 includes an injector 11 for the analyzed products, the separation column 12 to divide the analyzed products, the detector 13 of the said products and the device 14 to receive the gaseous combustion products.

Various compounds analyzed products pass through the separation column 12 at different points in time. The detector 13 is, for example, a flame ionization detector known in the art, and has a flame fed by gases generated in the device 14. This device 14 is, for example, a reservoir of distilled water and the electrolysis device containing distilled water, in which are immersed two electrodes 16 and 17. These electrodes are supplied source : the ohms of electrical energy 18. Hydrogen and oxygen are formed on the electrodes and provide a flame ionization detector oxygen and hydrogen through the tube 19. The detector 13 also receives gas for transferring products in the separation column, such as hydrogen, helium or nitrogen. The detector 13 measures the intensity generated during combustion of compounds derived from the column 12. Energy intensity varies according to the presence or absence of compounds in the cell. The chromatogram is prepared to provide, for example, the intensity as a function of time.

The invention proposes to make the mixture containing the sample of lubricating oil and hydrocarbon, C5such as alkane C5in a predetermined ratio. The mixture is introduced into the injector of the chromatograph. Get the chromatogram of the analyzed sample. Determine a first parameter characterizing the peak area associated with the hydrocarbon, C5. Determine a second parameter characterizing the area, at least one peak associated with hydrocarbon characterizing diesel fuel. The content of Tonnes of diesel fuel in the analyzed sample is calculated by the following formula:

where a and b are constants that determine the calibration straight line chromatograph, usually defined by C/M=a×T+b. Nab is emer, the parameters are proportional to the amplitudes or peak areas of the chromatogram.

The second parameter may, for example, be a function of height or peak area associated with hydrocarbon belonging to the group from C6to C25.

You can assume the calculated approximate content of diesel fuel, considering the second option, which is a function only of the peak hydrocarbon With20. Then in this approximation it is possible to identify peaks, in which the hydrocarbons will be taken into account in the parameter C for the calculation of content of diesel fuel. The number of significant peaks can thus be a function of the calculated approximation.

Mainly, the second parameter can characterize the space of several peaks associated with the respective hydrocarbon belonging to the group from C20to C25.

To account for the relative area of different compounds in different conditions chromatography was carried out factor With mostly correct to communicate concentration of the compound C5with the desired value. In particular, C can be determined by the following formula: C=α·C0/[S5],

C0 is the peak area associated with the hydrocarbon, C5such as alkane C5that is a correction factor for concentration standard, and [C5] is it what centrala hydrocarbon, C 5in a sample.

Formed mixture may contain a predetermined proportion of carbon disulphide. The function of carbon disulphide is the dilution of the pure mixture of oil+C5with a view to their homogeneous mixing and receiving fluid and a fluid medium, which separation is facilitated. In addition, carbon disulfide mostly invisible to the detector, even in large quantities. Therefore, the carbon disulfide does not interfere with the detection of diesel fuel and oil.

The calibration straight line is preferably prepared in advance with the same type of diesel fuel and the same type of oil as in the analyzed sample.

To pre-determine the equation of the calibration straight line can be the following stage. Are several standard mixtures containing lubricating oil and diesel fuel in various predetermined ratios, and hydrocarbon, C5such as alkane C5in a predetermined ratio.

The content of the diesel fuel in the standard sample will be denoted by t0. For each standard mixture:

in the injector of the gas chromatograph impose a standard mixture;

- get the chromatogram of the standard mixture;

- define the first parameter M0, characterizing the peak area of the chromatogram associated with the hydrocarbon, C5such as alkane C5 ;

determine a second parameter C0, which characterizes the peak area of the chromatogram associated with the hydrocarbon characterizing diesel fuel.

Of pairs of parameters obtained for the different obtained mixtures (which can be represented by points t0 X and C0/M0 Y)determine the constants a and b. Constants a and b receive, for example, if we take as a calibration straight line straight line that best fits the various received pairs.

The chromatogram can be obtained using a flame ionization detector, which allows the calculation node to perform the integration of the chromatogram to calculate the area of each peak.

Example conditions for implementing the method according to the invention will be hereinafter given in detail.

Can be used with the following device:

- gas chromatograph, preferably providing accurate programming and control of temperature and pressure in the column. Chromatograph preferably supplied with helium, air, industrial quality and hydrogen quality N55;

- non-polar capillary column sold by Chrompack under the brand name CF Syl 19 cb, having a length of 10 m, the diameter of 0.53 mm, a thickness of 1 μm;

- 2-meter predalone free from silicon dioxide which has a glass connecting piece, the contraction in the ith connection with capillary column;

- flame ionization detector (FID);

device integration in the form of a computer using software sold under the reference NRCAM in the next version after A;

- nizkotemperaturnyi injector to column, mainly to regulate the pressure, and automated injection device having at least 8 positions, recommended 100-position switch;

- scales with a precision of 0.1 mg;

- vibration table for mixing and homogenization of the samples.

Can use the following reagents:

- carbon disulphide (CS2), such as sold by Prolabo analytical quality Normapur;

- pentane (C5), having a purity of more than 99%;

industrial diesel fuel without additives;

- fresh oil type ALEA A2/B2 15W40.

Can use the following standard samples. Prepare a mixture of fresh oil/diesel fuel having the following relative mass content of diesel fuel: 1, 2, 3, 4, 5, 6, 7, 8, 10, 12 and 15%.

To increase the accuracy of the calibration is preferably used for data standards fresh diesel fuel and fresh butter, which correspond, respectively, diesel fuel and oil, which was used to obtain samples.

For each standard sample Khujand is performed following stages of preparation:

- a portion of the oil corresponding to the title by weight, selected from the flask and weighed. Its weight will be denoted m1;

- selected and placed in the flask volume of diesel fuel needed to get his title by weight. The weight of the mixture oil-diesel fuel will be denoted m2;

the mixture is vigorously shaken for at least for 10 minutes on the vibration table to homogenization.

Then the standard specimens are subjected to a process described below for samples.

For each sample analyzed oils are the following stages of preparation:

- select 1.7 ml of the analyzed sample and then weighed. The mass of this sample will be denoted m3. It may be taken as an additional sample if the mass does not correspond to the interval of expected values;

- to analyze the sample, add 20 ml of pentane. Pentane store and pick at ambient temperature. The mass of the mixture will be denoted m4;

the mixture was immediately diluted by adding 5 ml of carbon disulfide (CS2), the flask containing the mixture almost immediately hermetically sealed to limit evaporation of the solvent CS2;

- the resulting mixture is stirred using a vibratory table for approximately 1 is displaced so that to homogenize the mixture. Then thus obtained mixture is diluted with CS275% by volume, and it is ready for injection box in the chromatograph;

- optional, to increase the retention time of the mixture last poured into the sampler volume of 2 ml to provide so small dead volume as possible. The sealing cover can bend when opening the sampler. Fill as many samplers as needed for the analyzed mixtures;

- Inuktitut 0,5 ál using an automatic injector.

Of course, volumes and masses are given only as a guide, you can use other values.

Next will be described an example of the chromatographic analysis. During this analysis, the carrier gas in the separation column is helium. The temperature of thermostat chromatograph and the program pressure helium can be set according to the chart shown in figure 2. The temperature of the injector is controlled so that in advance to monitor the temperature program 10°C in accordance with the progress of thermostat. The flow rate of the carrier gas in the column due to program pressure helium. The chromatograph is controlled by regulation of the pressure.

For chromatograph used by the applicant during the test, the flow rate of hydrogen in the detector was RA is approximately 30 ml/min, and the flow rate of air in the detector was equal to 400 ml/min, with an accuracy of up to 10 ml/min

To integrate the peaks of the various compounds used the following stage of the chromatographic cycle:

- integration part of the standard pentane was carried out between t=22 seconds, and t=33 seconds;

- integrating parts of carbon disulfide (CS2) was carried out, except C20between t=33 s and t=37 min and 40 sec. The connection between C5and C20belong exclusively to diesel fuel;

- integration between calls C20and C22part of diesel fuel exclusively carried out between t=37 min and 40 sec and t=44 min and 15 sec;

- integration between calls C22and C24part of diesel fuel exclusively carried out between t=44 min and 15 sec and t=51 min and 15 sec;

- integration between calls C24and C25part of diesel fuel exclusively carried out between t=51 min and 20 sec and t=54 min and 20 sec;

- integration between parts of the oil from C25was carried out between t=54 min and 20 sec and t=97 min.

Primarily, the integration times for the various compounds are adjusted in accordance with the deterioration of the column.

The obtained chromatogram analyzed with the aim of identifying the areas of the peaks associated with different connections. Principles which may that A0 is the area allocated to standard pentane, A1 is the area associated with carbon disulphide, A2 is the area associated with up to C20exclusively, A3 is the area associated with up to C22exclusively, A4 is the area associated with up to C24exclusively, and A5 is the area associated with up to C25only.

Mainly, the concentration of the standard pentane associated with the entered value. The area belonging to different connections (or family of compounds), can thus be calculated regardless of the conditions chromatography was carried out.

Fixed area A0 is calculated as follows:

Weight of pentane equal to m4-m3. Then the concentration of pentane [C5]=(m4-m3)/m4. Considering [Ci] introduced concentration (for example, 0,0066), then: A0'=A0·[Ci]/[C5].

Obtaining a calibration curve as follows:

weighted actual content of diesel fuel is g=(m2-m1)/m2;

- for each area Ai, where i is between 1 and 4, build the graph of the straight line corresponding approximately

for example, by the method of least squares. Expressing the equation of the straight line in the form y=aix+bidetermine the value of iand bi. From those same standards thus obtained 4 calibration straight lines. The sample points and the calibration curve is given in figure 3.

Similarly carry out the integration for the analyzed sample with the aim of identifying the areas A0', A1, A2, A3 and A4. Then, for i between 1 and 4 rely relationships

Based on these relations and the calibration straight lines, determine the content of diesel fuel according to the following formula:

If lubricant is known, account only for the calculation of content of diesel fuel for i=1.

For certain oils, which slightly overlap with the heavy components of diesel fuel, a result that should be taken into consideration, determined in accordance with the content of diesel fuel received for i=1. For example, if this value is between 0 and 2%, take into account the value obtained for i=1; if this value is between 2 and 10%, take into account the value obtained for i=2; if this value is between 10 and 20%, take into account the value obtained for i=3; if this value is more than 20%, take into account the value obtained for i=4. Also consider joint elution of diesel fuel.

Because some oils have a characteristic structure (e.g. the, if the basic mixture is C16)may require selective integration. Such integration may, in particular, to exclude the area of the peaks corresponding to the considered connection, and requires a separate calibration.

Mainly, the temperature profile and pressure profile chromatograph periodically correct according to the standards that affect the solution containing the hydrocarbon, C5C20-C26and C30. For example, alkanes C5C20-C26and C30can be used with, for example, 60 mg of each of these compounds in 5 ml CS2. Also take into account the wear of the column and changes in the retention time.

Mainly, the new calibration straight lines receive for each new column used in the chromatograph.

This method allows to separate oil from diesel fuel by dividing their hydrocarbon, Cnn varies from 6 to 50, on the hydrocarbons constituting the family of saturated and/or unsaturated compounds. This method is not a separation connections for connection, and is a division of a family of hydrocarbon-based compounds (saturated and/or unsaturated) from the collection of hydrocarbon-based compounds (saturated and/or unsaturated).

1. The method of determining the content of the diesel tank is VA in the lubricating oil of the internal combustion engine, characterized in that it comprises the following stages:
the preparation of a mixture containing the sample of lubricating oil and a hydrocarbon, C5such as alkane C5in a predetermined ratio;
the introduction of the mixture into the injector (11) CG (10);
obtaining a chromatogram of the analyzed sample;
determining the first parameter M, which characterizes the peak area of the chromatogram associated with the hydrocarbon, C5such as alkane C5,
determining a second parameter C describing the area, at least one peak of the chromatogram associated with the hydrocarbon characterizing diesel;
the determination Tonnes of diesel fuel in the analyzed sample by the following formula:

where a and b are constants that determine the equation y=ax+b of the calibration straight line correlation between the second and the first parameters as a function of content of diesel fuel.

2. The method according to claim 1, wherein the second parameter characterizes the area, at least one peak of the chromatogram associated with a hydrocarbon group
C6to C25.

3. The method according to claim 2, in which the approximation of the content of diesel fuel is calculated as a function of the second parameter C describing the area of the peak associated with the hydrocarbon, C20chromate is grams, and then the corrected content of diesel fuel is calculated as a function of the second parameter C describing the area of several peaks associated with the corresponding hydrocarbons selected from the group of C20to C25while the number of peaks is a function of the calculated approximation.

4. The method according to claim 2, in which the second parameter characterizes the area of several peaks associated with the corresponding hydrocarbons selected from the group of C20to C25.

5. The method according to claim 1, wherein the second parameter receives the following formula: C=α·C0/[C5], where C0 is the peak area associated with the hydrocarbon, C5such as alkane C5α is a correction factor on the concentration of the standard and [C5] is the concentration of hydrocarbon, C5in a sample.

6. The method according to claim 1, characterized in that the formed mixture contains carbon disulfide at a predetermined value.

7. The method according to any of the preceding paragraphs, including the preliminary stage of determining the equation of the calibration straight line, in which:
are several standard mixtures containing lubricating oil and diesel fuel in various predetermined ratios, and hydrocarbon, C5such as alkane C5in a predetermined ratio;
for each of the th standard mix:
the standard mixture was injected into the injector (11) CG (10);
get the chromatogram of the standard mixture;
determine the first parameter M0, characterizing the peak area of the chromatogram associated with the hydrocarbon, C5such as alkane C5;
determine a second parameter C0, which characterizes the peak area of the chromatogram associated with the hydrocarbon characterizing diesel;
on the basis of pairs of first and second parameters obtained for different standard mixtures, determine the a and b parameters of the calibration straight line.

8. The method according to claim 1, in which each chromatogram obtained using a flame ionization detector (13) and in which the current node performs the integration of the chromatogram to calculate the area of each peak of the chromatogram.



 

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3 cl, 3 ex, 2 tbl

FIELD: physics.

SUBSTANCE: chromatographic separator of mixed gases and vapours contains three columns with one used to regenerate sorbent layer from heavy mix fraction, and two others used to separate mixture and remove light fraction. Columns are sectioned. Each section is filled sorbent selective to components of separated substance. Light and heavy fraction exhaust lines after fraction tanks through collector and driven switch elements are added with chromatographic modules each containing three columns with one used to regenerate sorbent layer from heavier fraction and two others used to separate mixture and remove light fraction components. Columns are sectioned. Each section is filled sorbent selective to components of separated substance and moving under carrier gas height supplied from the first section and exhausted from the last through offtake passing through column and filled motionless sorbent layer. Number of chromatographic modules to separate binary fractions is proportional to number of these fractions in multicomponent separated mixture. Modules process variable, including temperature, separated fraction volume, sorbent selectivity, column diameter and length are individual.

EFFECT: higher efficiency and productivity of compound multicomponent mixture separation.

1 dwg

FIELD: chemistry.

SUBSTANCE: novel chemical compound - 4-(4-cyanophenyl)-4'-(4-hydroxyhexyloxy)-benzylidenaniline, which possessing liquid crystalline properties, has wider temperature range of mesophase existence, higher temperature of passing into isotropic liquid (>200°C), demonstrates higher structural selectivity with respect to positional isomers of organic compounds.

EFFECT: increasing gas chromatographic column efficiency and reducing time of separation of positional isomers of organic compounds.

1 ex, 1 tbl

FIELD: chemistry; mechanics.

SUBSTANCE: device consists of serially connected detector, an analytical column, evaporator, device for preparing and inputting samples, as well as a holder for solid samples, three-way tap, the input of which has nozzle for inlet of the carrier gas, while its outputs are connected to the case of an airlock chamber and the solid samples holder respectively. The airlock chamber consists of a case and a swivel head, which have a cylindrical channel of the same diameter. The case of the airlock chamber is fixed to the evaporator such that, the cylindrical channel of the case is a continuation of the channel of the evaporator, and the swivel head is fixed to the case with provision for rotation by a 90° angle. The solid samples holder is in form of container with a calibrated opening.

EFFECT: increased authenticity of identification with simplification of the device and its use at the same time.

2 dwg

FIELD: chemical engineering; medical engineering.

SUBSTANCE: method involves plotting two chromatograms one of which is based on radioactivity (No 1) and the other one on ultraviolet absorption (No 2) or on radioactivity (No 1) and on fluorescence (No 2) and chromatogram specific relative to ultraviolet absorption (No 3) or relative to fluorescence (No 3). Material quality is estimated to be the more high the more close studied labeled compound peak shape is to trapezoid shape on the third chromatogram.

EFFECT: high accuracy of the method.

8 dwg

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