Method for determining amount of detersol-140 additive in motor oils for automobiles

FIELD: technology for controlling quality of motor oils using optical means, in particular, detection of additives in motor oils.

SUBSTANCE: method includes taking a sample, measuring optical density in absorption bands 1604 and 2000 cm-1 during spectrophotometry and following calculation of additive concentration using an experimentally derived formula.

EFFECT: expanded nomenclature of motor oil additives detectable by infrared spectroscopy, and also, possible identification of Detersol-140 only and determining of its amount only, as opposed to total content of all additives present in motor oil.

2 tbl

 

The invention relates to the field of quality control of engine oils using optical means, in particular to methods for determining the quantitative composition, primarily for the determination of additives in motor oils, and may find application in analytical laboratories, laboratories, oil refineries, forensics.

Due to the fact that in modern internal combustion engines of automotive vehicles appeared more intense than before (high forcing, heavy load etc), to motor oils meet strict requirements for their operational properties, to ensure which engine oil add a certain amount of various functional additives (antioxidant, detergent-dispersant, etc.). Lowering the concentration of the additive decreases the level of quality of oil.

The definition not only that, but the amount of additives is important, as they determine the reliability of the engine. One of the additives that improve the detergent-dispersant properties of motor oil, is Demersal-140, which amount in the oil should be from 2 to 3, 5 wt.%. Additive of Demersal-140 is a solution karbonatitovogo of alkylsalicylate calcium, obtained by processing of alkylsalicylate calcium gaseous dioxide the carbon in the presence of the promoter and excess (against stereometria) quantity of calcium hydroxide. (Fuel, lubricants and technical liquids. The range and application. Guide / Iginition, Cymbalista, Saatu and others; Ed. by Vmesnika. Ed. 2-E. - M.: Publishing center "Techinformi", 1999 s-451).

The authors goal was to develop a method for determining the number of additives Demersal-140 in motor oils for motor vehicles. When viewing patent information, scientific-technical literature revealed the following.

The method for determination of additives in oils largest "base number", including potentiometric titration of an alcoholic solution of potassium hydroxide (GOST 11362-96. Petroleum products and lubricants. Neutralization number. The method of potentiometric titration).

The disadvantages of this method is that the additive is determined not differentsirovanno, and in total, and their content is judged indirectly, on the assumption that the higher the base number, the higher the concentration of additives.

There is also known a method of determining the active elements (barium, calcium and zinc)that are included in the composition of additives to oils in the form of metal salts, including the decomposition of metal salts with hydrochloric acid and chelatometric titrovanie barium, calcium and zinc (HOST-68 Additives and oil additives. Method for the determination of barium, calcium and zinc complexometrically the titration).

The disadvantage of this method is that it determines only the active elements of additives, while additives are also of the organic part (for example, karbonitrirovanija alkylsalicylate).

It is known that all alkylsalicylate in the infrared spectrum are characterized by the presence of absorption bands in the range 1640-1530 cm-1(Kazicina L.A., Kupletskaya could BE the Application of UV, IR, NMR spectroscopy in organic chemistry. M.: Moscow state University. University, Chem. 1968, s). Given that Demerol-140 comprises karbonitrirovanija alkylsalicylate calcium, the authors in the study of motor oil quality with this additive has revealed to her the absorption band 1604 cm-1located in a known range.

The closest in technical essence and taken for the prototype is the IR spectroscopic method for determination of polyalkylacrylate in depressant additives to petroleum products, including the preparation of samples with known ratio of polymer, monomer and diesel fuel, the content of which all artificial mixtures of 50 wt.%.

The IR spectrum of the analyzed sample is removed in the area 1850-1050 cm-1and measure the optical density of bands 1735 cm-1and 1170 cm-1. After the base line through the points 1735 cm-1and 1170 cm-1the zero line of the spectrum and measurements according to the respective segments, calculate the concentration of the additive:

WithP=6731lgD1735/D1170-85 (for CPfrom 0 to 60 wt.%) or

WithP=2051lgD1735/D1170+18,2 (for CPfrom 60 to 100 wt.%).

(Methods of analysis, research and testing of petroleum and petroleum products (non-standard methods), part 2, M:its facilities at the Moscow, 1984, s.285-287).

The disadvantage of this method is the limited list of additives whose definition is possible. In addition, the method is time-consuming because of the presence of the intermediate calculation of optical densities and the use of different numerical coefficients in the determination of the concentrations of additives in two ranges.

The technical result of the invention is the expansion of the range determined by IR spectroscopy additives for motor oils.

This technical result is achieved in that in the method for determining the number of additives Demersal-140 in motor oils for motor vehicles, including sampling, spectrophotometrically, measurement of optical density at a given wavelength and the subsequent calculation of the concentration of the additive in mathematical dependence, according to the invention spectrophotometrically the optical density measured absorption bands 1604 cm-1and 2000 cm-1and the concentration of the additive is determined by the following dependencies

,

where C is the concentration of the additive, wt.%;

ΔD=D1604-D2000the difference of optical densities;

D1604- the optical density of the absorption band 1604 cm-1;

D2000- the optical density of the absorption band 2000 cm-1;

a=0,1643 constant experimentally obtained ratio;

b=0,0225 constant experimentally obtained ratio.

To justify a hallmark of samples were prepared, representing the composition of the engine oil with different concentrations of additives Demersal-140 (table 1).

All artificially prepared samples examined by Fourier transform infrared spectrometer AF-1 with a resolution of 2 cm-1in the wavelength range from 4000 to 450 cm-1in the cell of KCl thickness of 0.1 mm at a temperature of 20±2°With sample.

Table 1
The composition of the samples, wt.%
ComponentsSample
No. 1No. 2No. 3No. 4No. 5
Additive of Demersal-140, wt.%22,533,54
Motor oil brand M-z/10V:
And-40A, wt.%91,591,090,590,0to 89.5
Additives:
DF-11, wt.%22222
ACA "D", wt.%1,51,51,51,51,5
KND, wt.%33333

Measure the optical density D1604and D2000. The absorption band of 2000 cm-1is taken to determine the background sample. Determine the difference of optical densities of the absorption bands 1604 cm-1and 2000 cm-1for each sample. Build a graph of the difference of optical densities on the concentration of the additive. For additives of Demersal-140 graph of the difference of optical densities from its concentration has the form of a straight line and can be represented by the equation: ΔD=a+bC, where ΔD=D1604-D2000. By mathematical processing of experimental data, the authors obtained the value of the constant coefficients: a=0,1643; b=0,0225, which allowed us to obtain a formula for calculating the concentration of Pris is DKI of Demersal-140 engine oil:

Substituting the numerical values of the constant coefficients "a" and "b" determine the concentration of additives in the engine oil.

The data obtained is in good agreement with the law of the Bouguer - Lambert - Bera, expressing the relationship of optical density and concentration of the absorbing substance (Kazicina L.A., Kupletskaya could BE the Application of UV, IR, NMR spectroscopy in organic chemistry. M.: Moscow state University. University, Chem. 1968, p.10).

Defining characteristic absorption band 1604 cm-1additives of Demersal-140 and having a mathematical dependence of concentration from the difference of optical densities, the authors investigated samples of motor oil brand M-z/10-In, which was introduced additive of Demersal-140 in a certain number of samples No. 6, 7, 8 (a portion of the additive were weighed on the scales VLR-200 with a multiplier of 0.05 mg providing measurement error 0,010 mg). The results are presented in table 2.

95,9562
Table 2
The results of the study samples of motor oil M-z/10-In with the additive of Demersal-140.
The sample of motor oilNo. 6No. 7No. 8
The concentration of engine oil M-z/10-In, wt.%97,957596,9605
The concentration of additives Demersal-140 in the sample, wt.%2,04253,03954,0438
Measured

options
D16040,2610,2820,308
D20000,0500,0510,052
Asked

options
and0,1643
b0,0225
Settlement

options
ΔD0,2110,2310,256
C, wt.%2,07552,96444,0755

The obtained values of the concentration of the inventive method provide the necessary accuracy of measurement of the concentration of additives Demersal-140. Deviation of the concentration of the additive is within permissible limits.

Thus, the invention extends the range determined by IR spectroscopy additives for motor oils and allows to identify only the additive Demersal-140 in motor oils for automotive vehicles and to determine the number, not the total content of all those present in the engine oil additives, and not its active elements. Given that exploitatio the basic properties of the additives in the engine oil affects not only the content of the active elements, but an organic part of the additive (alkylsalicylate), the contents of which were not previously taken into account for evaluation of the performance properties of engine oils containing the additive Demersal-140, the invention is relevant.

The method for determining the number of additives Demersal-140 in motor oils for motor vehicles, including sampling, spectrophotometrically, measurement of optical density at certain wavelengths and determining the concentration of the additive in mathematical dependence, characterized in that when spectrophotometrically measure the optical density at the absorption bands 1604 cm-1and 2000 cm-1and the concentration of the additive is calculated by the following dependencies:

,

where C is the concentration of the additive, wt.%;

ΔD=D1604-D2000the difference of optical densities;

D1604- the optical density of the absorption band 1604 cm-1;

D2000- the optical density of the absorption band 2000 cm-1;

a=0,1643 constant experimentally obtained ratio;

b=0,0225 constant experimentally obtained ratio.



 

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