RU2731818C1 - Method for rapid analysis of additives, lubricants, industrial fluids, including waste ones (embodiments) - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: group of inventions relates to rapid analysis of additives, lubricants, industrial fluids, including spent liquids, for assessing the actual state of internal combustion engines, transmissions, compressors and other equipment. Universal indicator for express-analysis of content of additives and serviceability of lubricating materials, obtained by impregnating fibrous materials with dimensions of 30 × 40 mm or 8 × 80 mm water-and-alcohol solution of the following composition, g: methyl orange 0.05–0.3; methyl red 0.15–0.3; bromthymol blue 0.3–50; alizarin yellow P 0.1–0.3; phenolphthalein 0.01–0.1; malachite green 0.01–0.05; red cabbage broth 5–20; cherry infusion or alcohol cherry infusion 0–5; tetraethylammonium bromide 0–9.0 as fixing agent; aqueous solution of ethyl or isopropyl alcohol 914.95–994.32 at temperatures of 10–60 °C. Invention also describes a method for rapid analysis of additive content and operability of lubricants and a method for rapid analysis of the actual state of equipment.

EFFECT: higher accuracy and reliability of rapid analysis.

10 cl, 3 tbl, 38 ex, 21 dwg

Description

The invention relates to an express analysis of additives, lubricants, technical fluids, including spent ones, using a universal indicator, as well as to a method for performing an express analysis of the actual state of internal combustion engines, transmissions, compressors, etc. (technology).

The analysis of additives, lubricants, technical fluids, including used ones, requires a laboratory with expensive equipment and specialists, and the assessment of the state of equipment is fraught with difficulties, since this requires diagnostic equipment and disassembly of individual units and assemblies.

An alternative to this is the fundamental possibility of an indirect assessment of the state of technology by express analysis of additives, fresh and used lubricants and technical fluids.

In this regard, there is a great need for a simple, prompt and economical way to assess the quality of additives (for manufacturers of additives, lubricants), lubricants, technical fluids, including used ones, as well as assessing the state of technology by analyzing the lubricants and technical liquids (for operators),

A known method for assessing the quality of lubricating oil (ed. St. USSR No. 1337743, G01N 21/78, 31/22, 1987), which consists in processing the analyzed oil sample with an alcohol-toluene-aqueous solution of inorganic acid in the presence of an indicator, followed by comparison of the color of the solution with a standard. In this case, the analyzed drop sample of oil is introduced into a solution of hydrochloric acid with a concentration of 0.0005-0.005 mol / dm ³ , and the ratio of the volume of the solution and the mass of the injected sample is determined depending on the minimum allowable base number. The disadvantages of this method for determining the base number include the use of an alcohol-toluene-aqueous solution of hydrochloric acid, which complicates the method and increases the danger of its implementation; low accuracy in determining the values of indicators, since with base number values of the controlled oil sample of 2.5-3.5 mg KOH / g there are no noticeable color gamut transitions, no color difference is detected. When determining the base number in dirty oils, dark brown or black shades prevail, it is almost impossible to determine the color.

There is a known method for determining the base number of engine oils (RF patent No. 2183018, G01N 31/22, G01N 21/78, G01N 33/28, G01N 33/30, 06/15/2001), which consists in the fact that the analyzed drip oil sample is introduced into a mixture consisting of 71 ± 1% distilled water and 29 ± 1% solvent, and the solvent consists of 50% toluene and 50% isopropanol, and the indicator is a blue ribbon filter paper impregnated with a 0.5% aqueous solution of bromothymol blue. The base number is determined using a color scale. The disadvantages of this method for determining the base number include the use of distilled water. In the process of its storage and use, the pH of water changes, regardless of the conditions of storage and receipt, which ultimately causes a large error in the accuracy of determining the base number of the oil. When dipped in a 0.5% solution of bromothymol blue and held for 1 minute, filter paper is not uniformly impregnated, since 0.5% is not sufficiently concentrated.

A known method of obtaining an acid-base indicator strip by impregnating filter chromatographic paper with solutions of acid-base indicators (SU 524534 D21F 11/14, 1976). The disadvantage of the indicator paper obtained by these methods is the weak fixation of the indicator on the cellulose carrier, the washing out of the indicator from the paper into the analyzed solution, as well as the erosion of the color color of the indicator paper upon contact with the analyzed solution, which reduces the accuracy of pH determination due to the zones arising due to the capillary effect. different colors of the indicator.

A known method of producing acid-base indicator paper for determining pH in the range of 5-9 by processing filter paper with a mixture of reagents containing 0.0012 g of methyl red, 0.016 g of bromothymol blue, 2.40 g of polyvinyl alcohol, 0.04 g of polyoxyethylene sorbinate monolaurate, in 40 ml 35% ethanol (Patent GB 922606, 1963). The disadvantage of the method for producing acid-base indicator paper is the complexity of obtaining polyoxyethylene sorbitan monolaurate, and the composition of the impregnating solution itself is complex and insufficiently reproducible, since it consists of a mixture of fixers.

A known method of producing acid-base indicator paper for determining the pH of a solution (SU 1127935 D21H 1/46, D21H 3/80, C01N 31/22, 1984) by impregnating chromatographic paper with a solution of an acid-base indicator and fixer, which is used as 0.3 ÷ 1.8% solution of sodium sulfate in 40-60% ethanol. The disadvantage of the method for producing acid-base indicator paper is the limited area of its application, only for pH 5-9, in the range of color transitions from yellow at pH 5 to dark blue at pH 9 through yellow-green and green-blue tones.

A close known method is RF patent No. 2399050 G01N 33/28, G01N 21/78, B01N 39/18, D21N 27/08, 10.09,2010 g, "Test environment for express analysis of engine oils in internal combustion engines" ... The invention relates to a test medium for express analysis of engine oils in internal combustion engines, having a density of 50.0 to 200.0 g / m ² , containing, based on the total weight of the test medium, from 70.0 to 98.0% by weight of cotton pulp from 0.0 to 25.0% by weight of cellulose and from 0.5 to 30.0% by weight of silicic acid and / or at least a silicate salt. Another invention relates to a method for the rapid analysis of engine oils in internal combustion engines, in which a drop of the engine oil to be examined is applied to the test medium according to the invention and allowed to penetrate into the test medium and then, in order to determine the condition of the engine, the test result is compared in an advantageous way with at least one reference picture. Also presented is a method for performing an express analysis of the actual state of an internal combustion engine using the above test environment. The disadvantage of this method is the difficulty of obtaining a test medium from cellulose, cotton and silicic acid, and the method does not allow to determine the quality of fresh additives and lubricants when they are purchased from a color chromatogram.

Close to the known methods (RF patent No. 2464368 D21F 11/14, G01N 31/22, 20.10.2012) the claimed method is a method of obtaining a universal acid-base indicator paper UKOIB for determining pH in the range of 0-10 by impregnating filter chromatographic paper with a solution a mixture of acid-base indicators and a tetraalkylammonium halide fixer with a content of 0.2-2.0 wt. % in solution, while the solution of a mixture of acid-base indicators and fixer is brought to yellow with 0.1 N sodium hydroxide solution. The disadvantage of this method of producing acid-base indicator paper is the difficulty of obtaining an impregnating solution containing a toxic fixer and sodium hydroxide solution, the inapplicability of indicator paper for determining the base number of a lubricant and additive. Close of the known methods to the claimed one in terms of the achieved effect is the method (prototype, patent RF2484462 G01N 33/28, G01N 21/78, G01N 31/22, 20.10.2012) carried out by processing a drop sample of oil with a solvent consisting of 50% toluene and 50% of isopropanol, in the presence of filter paper impregnated with an aqueous solution of bromothymol blue, followed by comparison of its color with a standard, a drop sample of oil is introduced into a mixture consisting of 70% of a 20% aqueous solution of ethyl alcohol and 30% solvent, a solution of bromothymol blue is taken in 1%, the filter paper, after exposure to bromothymol blue, is blotted with a cotton cloth and dried in a horizontal position. The disadvantages of this method for determining the base number include the use of toxic toluene as a solvent and one type of indicator. Given the state of the art, the objective of the invention is to identify the best methods for assessing the state of internal combustion engines, transmissions, compressors, etc. (technology), to develop a universal indicator for determining the quality of additives, lubricants, technical fluids, including waste fluids, increasing the accuracy of express analysis based on base number, using available reagents. This, as well as other tasks that are not named, but can be isolated from the issues considered here as independent or inevitably follow from them, are solved using a universal indicator on a paper or fabric substrate with all the features of claim 1 and claim 1 of the present claims ... Appropriate options proposed according to the invention for the use of a universal indicator are described in the dependent claims related to claims 1 and 2 of the claims. Independent claim 2 concerning the method protects a particularly preferred mode of action in the express analysis of additives, lubricants, technical fluids and working lubricants and technical fluids in internal combustion engines, transmissions, compressors, etc. (technology). Due to the optimal composition of the universal indicator, wt%: methyl orange 0.05-0.3, methyl red 0.15-0.3, bromothymol blue 0.3-50, alizarin yellow P 0.1-0.3, phenolphthalein 0.01-0.1, malachite green 0 , 01-0.05, red cabbage decoction 5-20, cherry decoction or its alcoholic infusion 0-5, tetraethylammonium bromide 0-9.0 (as a fixer), an aqueous solution of ethyl or isopropyl alcohol 914.95-994.32 on the fabric or paper, it is possible, not without another predictable, to make the universal indicator available for the express analysis of additives, lubricants and technical fluids (upon purchase), as well as lubricants and fluids that work in technology, which make it possible to obtain, at least qualitatively, their assessment states. At the same time, additional advantages flow from the proposed method: The universal indicator proposed according to the invention can be produced in a simple and economical way on an industrial scale; The universal indicator proposed according to the invention, in a short time gives unambiguously interpretable conclusions about the quality of additives, lubricants, technical fluids (upon purchase, before using in technology), as well as on lubricants and fluids operating in technology, to get an idea of the state of their systems ( lubrication, cooling, etc.) and friction units, which can only be done using expensive laboratory and diagnostic equipment;

The universal indicator proposed according to the invention allows a relatively accurate determination of the quality of fresh additives, lubricants, technical fluids, including those working in technology. Fake (low-quality) additives, lubricants, technical fluids, as well as their aging during operation (increase in viscosity, oxidation, etc.), contamination of the lubricant, in particular with mechanical impurities, fuel, coolant (water, glycols ), fuel combustion residues (soot, carbon deposits). Thus, defects and shortcomings of systems and friction units of technology can be established at an early stage;

With the help of an express analysis of the additive, lubricant, technical fluid, using a universal indicator, the user identifies a fake (poor-quality product upon purchase). And according to the express analysis of lubricants and technical fluids working in technology, it detects at an early stage defects in the systems and friction units of technology;

With the help of the express analysis of the lubricant, technical fluid using the universal indicator proposed according to the invention, the user can in a simple way determine the operating time of the lubricant, technical fluids and their timely replacement;

The versatile indicator according to the invention provides a simple and effective way to check the optimum efficiency and optimum combustion of fuel in an internal combustion engine. Thus, the negative impact of technology on the environment is prevented, due to too high fuel consumption or increased emission of harmful substances;

The universal indicator, proposed according to the invention, allows the rapid analysis of any technique using lubricants and technical fluids.

The universal indicator according to the invention has a paper or fabric backing.

A universal indicator was prepared by impregnating paper or fabric in pre-prepared solutions of indicators with close pH intervals of the color transition, having different colors in this interval. Based on literary sources, patents, we studied the recipes for obtaining indicators by impregnating various papers and fabrics in indicator solutions and decoctions, alcohol solutions of vegetables, berries and fruits. This listing does not limit the use of equivalent chemical indicators and indicators derived from vegetables, berries and fruits; therefore, more affordable, cheaper and non-toxic reagents, alcoholic tinctures and decoctions from vegetables, berries, fruits and a substrate for indicators from available papers and fabrics were used.

In the course of preparing a method for obtaining a universal indicator, 47 indicator solutions of various names and concentrations were prepared, including 12 decoctions and alcoholic tinctures of vegetables, berries and fruits. 7 types of different papers and 4 types of fabrics were used as the indicator substrate. After preliminary express analyzes of more than 100 types of additives, lubricants and technical fluids, 8 indicators were selected for testing, including decoctions of red cabbage and cherries or its alcohol tincture for impregnating four types of paper, one type of fabric and four types of well-known indicator strips, 5 names additives, 23 types of lubricants, technical fluids, mineral and synthetic base oils.

During the tests, GOST 33776-2016 was used to determine pH, acidity and alkalinity. for determination of base number GOST 11362-76, for determination of acid number GOST5985-79. To determine the base number of samples of motor oils and additives in the base oil, we used a reference scale of base numbers prepared according to the method of OOO "Khimmotolog",

Table 1 shows 8 indicators used to prepare solutions.

Known universal indicators, which are a combination of several monochromatic indicators with different intervals of pH color transition. For example, the commercially available PKC universal indicator is a mixture of seven indicators: bromcresol purple, bromcresol green, methyl orange, tropeolin, phenolphthalein, thymol blue and bromothymol blue. This indicator, depending on pH, has the following color: at pH = 1 - raspberry, pH = 2 - pinkish-orange, pH = 3 - orange, pH = 4 - yellow-orange, pH = 5 yellow, pH = 6 - greenish yellow, pH = 7 - yellow-green, pH = 8 - green, pH = 9 - blue-green, pH = 10 - grayish-blue.

To carry out tests and obtain a universal indicator (universal indicator strip) for the express analysis of additives, lubricants, technical fluids, including used ones, eight universal solutions were prepared by mixing known reagents and boiling known indicator strips in a decoction of red cabbage.

Sample 1, A solution for paper impregnation was prepared, for which methyl orange 0.2 g, methyl red 0.15 g, bromothymol blue 0.3 g, alizarin yellow P 0.3 g, phenolphthalein 0.1 g, malachite green 0.05 g, red cabbage decoction 2 g were dissolved, cherry decoction 3 g, tetraethylammonium bromide 9.0 g (as a fixer) 984.9 g 50% aqueous ethanol solution by weight. The resulting orange solution was brought to yellow by adding 0.1 N sodium hydroxide solution.

Sample 2. A solution for paper impregnation was prepared, for which methyl orange 0.1 g, methyl red 0.3 g, bromothymol blue 3 g, alizarin yellow P 0.1 g, phenolphthalein 0.05 g, malachite green 0.05 g, red cabbage decoction 5 g were dissolved, tetraethylammonium bromide 6.0 g, in 985.4 g of 90% aqueous ethanol solution, without adding 0.1 N sodium hydroxide solution.

Samples 3-5 were prepared without adding sodium hydroxide.

Sample 3. A solution for paper impregnation was prepared, for which methyl orange 0.05 g, methyl red 0.5 g, bromothymol blue 10 g, alizarin yellow P 0.05 g, phenolphthalein 0.01 g, malachite green 0.01 g, red cabbage decoction 10 g were dissolved, sirtovaya infusion of cherries 3.0 g in 977.38 g. 95% aqueous solution of ethanol.

Sample 4. A solution for paper impregnation was prepared by dissolving methyl red 0.3 g, bromothymol blue 50 g, alizarin yellow P 0.01 g, malachite green 0.01 g, red cabbage decoction 20 g, in 929.68 g 90% water isopropyl alcohol solution.

Further, four samples were prepared on the basis of a decoction of red cabbage. We cut 100 g of red cabbage into a saucepan, poured 300 g of distilled water into it and boiled it until a concentrated solution of 50 g was obtained.

Sample 5. 5 grams of the solution was poured into the crucible, 3 strips of indicator red litmus tube were lowered into the crucible and boiled for 5 minutes, the strips were removed, washed with 5 g of ethanol and the extract was returned to the crucible.

Sample 6. 5 grams of red cabbage solution was poured into the crucible, 3 strips of the universal indicator PND 50-975-84 produced by Lahem were lowered and boiled for 5 minutes, the strips were removed, washed with 5 g of ethanol and the extract was returned to the crucible.

Sample 7. In the crucible, poured 5 grams of red cabbage solution, lowered 3 strips of Rottinger indicator and boiled for 5 minutes, removed the strips, washed them with 5 g of ethanol and returned the extract to the crucible.

Sample 8. 5 grams of red cabbage solution was poured into the crucible, 3 strips of the PKC indicator were lowered and boiled for 5 minutes, the strips were removed from the crucible and survived in a test tube, washed with 5 g of ethanol and the rinsing (solution) was returned to the crucible.

The obtained samples of indicator solutions (each separately) were impregnated with "Blue Ribbon" filter paper, or white writing paper GOST R ISO 9705-2000, or newsprint, GOST 6445-74 or cloth, dried for 10-20 minutes, cut into strips of size 30 × 40 mm. or 8 × 80 mm and placed in a sealed bag. Using the obtained indicator solutions, eight types of test strips and two samples of impregnation were made: a universal indicator strip PND 50-975-84 produced by Lahem with cherry decoction, No. 9; and a universal indicator strip RKS of Russian production, No. 10.

Within the framework of the present invention, decoctions of berries and vegetables can be used either individually or in a mixture with other known indicators, depending on the acidity and alkalinity of the test product.

For the express analysis of additives, lubricants, technical: fluids, including waste, using a universal indicator, we offer two options.

According to option 1, fresh motor oils were tested: flushing Novoil-PZ, alkaline number 4.5 mg KOH / g; Toyota SAE 5W40, base number 6.0 mg KOH / g; Lukoil 10 W40, 8.0 mg KOH / g; Gazpromneft 10W40, base number 9.0 mg KOH / g; M-14 G ₂ TsS, base number 10.2 mg KOH / g. Waste engine oils: Toyota 5W40, base number 2.5 mg KOH / g; Lukoil 10W40 base number 3.5 mg KOH / g. Base oils: polyalphaolefin with a viscosity of 12 cSt at 100 ° C and mineral oils with a viscosity of 8 cSt at 100 ° C; additive S-300 in polalphaolefin oil (ratio 1:50 mass).

According to option 2, in addition to the aforementioned oils, additives, lubricants and technical fluids were additionally tested: Additive S-300 according to TU BY 390401182.023-2012; Additive C-5A according to TU 38 101146-77; Additive TsTs-7 according to TU 0257-001-96449839-2007; Additive T-43 according to TU 0257-002-40065452-97; Additive Anglamol 99 from Lubrizol; Gazpromneft 5W40, base number 8.9 mg KOH / g; Automatic transmission oil TOTEK Astra Robot-Automatic base number 3.5 mg KOH / g; Waste oil for automatic transmission TOTEK Astra Robot-Automatic base number 1.8 mg KOH / g; Transmission oil SAE 75 W90; Waste gear oil SAE 75 W90; Mineral oil MS-20; Mineral oxidized oil MS-20; Mineral oil I-12A; Synthetic polyalphaolefin oil; Brake Fluid Brake Fluid DOT 4 by Castrol; Compressor oil Lukoil stabio synthetic 46; Coolant G12-40; Cooling liquid Tosol-40.

The quality of the used reagents, lubricants and technical fluids was checked in the accredited laboratory of LLC "HTTs UAI" in Ufa.

Express analysis of the performance of engine oils, including those used by the base number, option 1, was carried out at temperatures of 20-25 ° C as follows. A 4 ml syringe was poured into a transparent glass container with a volume of at least 10 ml. gasoline or solvent "Nefras", 2 ml. ethyl alcohol with water in a ratio of 2: 3 vol. (or vodka), dipped indicator paper into it. The mixture was agitated until a clear yellow color was formed. Then one drop of the analyzed product was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. The base number of fresh (and used) engine oil was determined from the change in the color of the aqueous layer of the solution according to the reference scale. The reference scale for determining the base number of a test product has been compiled by numerous tests of lubricants with known base numbers using the quality reagents and indicators in the examples provided. For engine oils, the color in the indicator solution is distributed according to the reference scale developed by OOO Khimmotolog, as follows: yellow color - less than 1 mg KOH / g; light green - 1.5 ÷ 2.0 mg KOH / g, bright green - 2.5 ÷ 3.0 mg KOH / g, light blue - 3.5 ÷ 4.5 mg KOH / g, blue color - 5.0 ÷ 6.5 mg KOH / g, light purple - 7 ÷ 8.5 mg KOH / g, purple - 9.0 ÷ 10 mg KOH / g, dark purple more than 10 mg KOH / g. Changing the brands of gasoline, Nefras solvent and the ratio of alcohol, water within the specified limits does not lead to an inaccuracy in determining the base number of engine oil. The accuracy of the color transition and the convergence of the color of the solution is increased by observing the used methods of OOO "Khimmotolog" and temperature (room temperature), the method of preparing the indicator and the duration of the analysis and comparison with the reference scale of the base number.

Below are examples of tests, while they should not affect in any way to limit the idea of the invention.

Example 1. In a glass transparent container with a volume of at least 10 ml. 4 ml of gasoline AI-80, 2 ml were poured from a syringe. ethyl alcohol with water in a ratio of 2: 3 vol. (or vodka), immersed in it filter paper "Blue Ribbon" soaked in a solution (methyl orange 0.2 g, methyl red 0.15 g, bromothymol blue 0.3 g, alizarin yellow P 0.3 g, phenolphthalein 0.1 g, malachite green 0.05 g , decoction of red cabbage 2 g, decoction of cherry 3 g, tetraethylammonium bromide 9.0 g, (as a fixer) 984.9 g of 50% aqueous solution of ethanol, 0.1 N sodium hydroxide solution was added dropwise to the resulting solution until yellow color sample 1). The mixture was agitated until a clear yellow color was formed. Then one drop of fresh Novoil PZ motor oil was added to it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the light blue color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 4.5 mg KOH / g, which is consistent with the base number according to the quality passport for the tested flushing engine oil Novoil PZ.

Example 2. In a glass transparent container with a volume of at least 10 ml. 4 ml was poured from a syringe. solvent Nefras 40/70, 2 ml. vodka, dipped indicator paper soaked in solution (methyl orange 0.1 g, methyl red 0.3 g, bromothymol blue 3 g, alizarin yellow P 0.1 g, phenolphthalein 0.05 g, malachite green 0.05 g, red cabbage decoction 5 g, tetraethylammonium bromide 6.0 g, in 985.4 g of 90% aqueous ethanol solution, sample 2). The mixture was agitated until a clear yellow color was formed. Then one drop of fresh Toyota SAE 5W40 engine oil was added to it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the blue color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 6 mg KOH / g, which is consistent with the base number according to the quality passport for the tested Toyota SAE 5W40 engine oil.

Primerz, Into a glass transparent container with a volume of at least 10 ml, 4 ml was poured from a syringe. gasoline AI-92, 2 ml. vodka, dipped indicator paper soaked in a solution (methyl orange 0.05 g, methyl red 0.5 g, bromothymol blue 10 g, alizarin yellow P 0.05 g, phenolphthalein 0.01 g, malachite green 0.01 g, decoction of red cabbage 10 g, tetraethylammonium bromide 3.0 g, in 977.38 g of 96% aqueous ethanol solution, sample 3). The mixture was agitated until a clear yellow color was formed. Then one drop of fresh engine oil Lukoil SAE 10W40 was introduced into it, the mixture was again shaken for 1-2 minutes and defended for 1-3 minutes. Based on the light blue color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 8 mg KOH / g, which is consistent with the base number according to the quality passport for the tested Lukoil SAE 10W40 engine oil.

Example 4, Into a glass transparent container with a volume of at least 10 ml, poured from a syringe 4 ml, AI 95 gasoline, 2 ml, vodka, dipped indicator paper impregnated with a solution (methyl red 0.3 g, bromothymol blue 50 g, alizarin yellow P 0.01 g, malachite green 0.01 g, red cabbage decoction 20 g, tetraethylammonium bromide 1.0 g in 928.68 g of 90% aqueous ethanol solution, sample 4). The mixture was agitated until a clear yellow color was formed. Then one drop of fresh engine oil Gazpromneft 10W40 was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the violet color of the aqueous layer of the solution, the base number was determined according to the standard scale, which was 9 mg KOH / g, which is consistent with the base number according to the quality passport for the tested engine oil Gazpromneft 10W 40.

Example 5. In a glass transparent container with a volume of at least 10 ml, poured from a syringe 4 ml, solvent Nefras 80/120, 3 ml. vodka, dipped indicator paper impregnated with a solution (sample 5), the mixture was shaken until a transparent yellow color was formed. Then one drop of fresh motor oil 14 G ₂ TsS was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. The base number was determined according to the dark purple color of the aqueous layer of the solution according to the reference scale, which was 10.2 mg KOH / g, which is consistent with the base number according to the quality passport for the tested engine oil 14 G ₂ CS.

Example 6. In a glass transparent container with a volume of at least 10 ml. 4 ml was poured from a syringe. solvent Nefras 80/120, 2 ml. vodka, dipped indicator paper soaked in the solution (sample 6). The mixture was agitated until a clear yellow color was formed. Then one drop of used Toyota 5W40 engine oil was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the bright green color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 2.5 mg KOH / g, which is consistent with the base number of the oil obtained according to GOST 11362-76.

Example 7. In a glass transparent container with a volume of at least 10 ml. poured 4 ml. solvent Nefras 80/120, 3 ml. vodka, dipped indicator paper soaked in the solution (sample 7). The mixture was agitated until a clear yellow color was formed. Then one drop of used Lukoil 10W40 motor oil was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the light blue color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 3.5 mg KOH / g, which is consistent with the base number of the oil obtained according to GOST 11362-76.

Example 8. In a glass transparent container with a volume of at least 10 ml. 4 ml was poured from a syringe. solvent Nefras 80/120, 4 ml. vodka, dipped indicator paper impregnated with a solution (according to the prototype). The mixture was agitated until a clear yellow color was formed. Then one drop of fresh oil for an automatic transmission TOTEK Astra Robot-Automatic was introduced into it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the green color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 3.5 mg KOH / g, which is consistent with the base number according to the quality passport for the tested fresh oil for an automatic transmission TOTEK Astra Robot-Avtomat.

Example 9, Into a glass transparent container with a volume of at least 10 ml. 4 ml was poured from a syringe. solvent Nefras 80/120, 4 ml. vodka, dipped indicator paper soaked in the solution (sample 8). The mixture was agitated until a clear yellow color was formed. Then one drop of used oil for the automatic transmission TOTEK Astra Robot-Avtomat was added to it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the light green color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 2.0 mg KOH / g, which is consistent with the base number of the oil obtained according to GOST 11362-76.

Example 10. 4 ml was poured from a syringe into a glass transparent container with a volume of at least 10 ml. solvent Nefras 80/120, 3 ml. vodka, dipped indicator paper soaked in the solution (sample 5). The mixture was agitated until a clear yellow color was formed. Then one drop of the S-300 additive in a solution of polyalphaolefin oil (in a ratio of 1:50 mass) was added to it. The mixture was again shaken for 1-2 minutes and left to stand for 1-3 minutes. Based on the blue color of the aqueous layer of the solution, the base number was determined according to the reference scale, which was 5 mg KOH / g, which is consistent with the base number obtained according to GOST GOST 11362-76.

Example 11 (according to the prototype, patent RF2484462). In the analyzed drop sample of engine oil, Gazpromneft SAE 10W 40 is injected into a mixture consisting of 70% 20% distilled water and 30% solvent consisting of 50% toluene and 50% isopropanol; filter paper impregnated with 1 is used as an indicator. , 0% solution of bromothymol blue. The base number was determined according to the color standard scale, according to the light purple color it was 8.0 mg KOH / g, which is inconsistent with the base number of the oil (9.0 mg KOH / g), obtained according to GOST 11362-76. The tests were carried out at temperatures of 25 ° C.

The results of the analysis of oils, including those used by the proposed method according to the first option, are shown in Table 2.

In many cases, it is more convenient to use for the analysis of additives, lubricants, including spent ones, not mixed solutions with an indicator, but a universal indicator, therefore we offer the second variant of the method. When conducting preliminary tests of drop samples with a universal indicator of additives, lubricants and technical fluids, including spent ones, it was found that the spot consists mainly of a core and characteristic three zones, which is consistent with the generally accepted methods of a drop test. The main distinguishing feature of the proposed method from the known ones is a universal indicator on paper or fabric in the form of a square measuring 30 × 40 mm or a strip of 8 × 80 mm, which makes it possible to obtain a chromatogram in color format and evaluate the quality of fresh additives, lubricants and technical fluids, including spent and assess the state of technology, at least qualitatively.

Option 2. Examples of express analysis of additives, engine, transmission oils, technical fluids, including waste, are given in examples 12-38.

Example 12. On the filter paper "Blue Ribbon" impregnated with an indicator solution (sample 1), at a temperature of 60 ° C, a drop of the C-300 additive is applied, which, due to the forces of surface tension and wetting, leaves a sedimentary chromatogram in the form of a core and three zones of colored precipitation: core blue; 1st diff. a zone around the perimeter of the core in the form of a dark blue ring; 2nd diff. zone light orange turning into dark orange, 3rd diff. a zone in the form of a light orange ring, formed as a result of the reaction of the elements of the additives with the indicator solution. In fig. 1 standard sedimentary chromatogram of the original S-300 additive corresponding to TU BY 390401182.023-2012, which, by comparing the color of radial sedimentary chromatograms, can be used to check the quality of a new batch of S-300 additive during incoming inspection. If the color of the core and the zones of the radial sedimentary chromatogram of the tested additive S-300 does not match with the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 13. On white writing paper GOST R ISO 9705-2000 impregnated with an indicator solution (sample 2), at a temperature of 50 ° C, a drop of an additive CD-7 is applied, which, due to the forces of surface tension and wetting, leaves a radial sedimentary chromatogram in the form of a core and three zones of colored precipitation: the core is light yellow with a bright green tint; 1st diff. the ring-shaped area is dark orange; 2nd diff. the zone is light orange; 3rd diffusion zone in the form of a light orange ring), formed as a result of the reaction of additive elements with an indicator solution. In fig. 2 is a reference radial sedimentary chromatogram of the original TsD-7 additive corresponding to TU 0257-001-96449839-2007, which, by comparing the size and color of radial sedimentary chromatograms, can be used to check the quality of a new batch of TsD-7 additive during the incoming inspection. If the color of the zones of the sedimentary chromatogram of the tested additive TsD-7 does not match with the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 14. On newsprint paper. GOST 6445-74 impregnated with an indicator solution (sample 3), at a temperature of 45 ° C, a drop of the T-43 additive is applied, which, due to the forces of surface tension and wetting, leaves a radial sedimentary chromatogram in the form of a core and three zones of colored precipitation: the core is light yellow, a dark orange spot inside the kernel; 1st diff. the ring-shaped area is dark red; 2nd diff. the zone is dark orange with yellow blotches; 3rd diff. area in the form of an orange ring. According to the results of the analysis in an accredited laboratory, the additive is original and the color transitions of the additive elements formed as a result of the reaction of the additives with the indicator can be used as a standard for checking the quality of a new batch of T-43 additive during the incoming inspection. If the color of the zones of the sedimentary chromatogram of the tested additive T-43 does not match with the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 15. A drop of Anglamol 99 additive is applied to the Blue Ribbon filter paper impregnated with an indicator solution (sample 4) at a temperature of 25 ° C. in the form of a core and three colored zones: The core is blurred white, inside the core there is a spot of light orange color; 1st diff. zone is yellow; 2nd diffusion zone is dark yellow; 3rd diffusion zone in the form of a red ring. In fig. 3 standard radial sedimentary chromatogram of the original Anglamol 99 additive corresponding to the quality certificate of the manufacturer "Lubrizol", which, by comparing it with the radial sedimentary chromatogram of the Anglamol 99 additive from the new batch, will allow the size and color of the zones during the incoming control to reveal a fake (low-quality additive). To confirm the result of the rapid analysis of the drop sample, the additive sample is sent to the laboratory to check the quality indicators established by the additive passport.

Example 16. A drop of original fresh engine oil Toyota SAE 5W40 from EKKSOP MOBIL is applied to the Blue Ribbon filter paper impregnated with an indicator solution (sample 5) at a temperature of 25 ° C, which, due to surface tension forces and wetting, leaves a radial color sedimentary chromatogram in form: the core is light green; 1st diff. zone in the form of a yellow-orange ring; 2nd diff. zone orange; 3rd diff. the zone is light orange, formed as a result of the reaction of the elements of the additives with the indicator solution. A clear perimeter of the core, in which the additive elements are concentrated due to the pressure of the droplet weight and the diffusion of the oil base with the additive elements to the perimeter. Then, due to adsorption and capillary diffusion, the additive elements, depending on the diffusion rate, form the second and third zones that differ in color. According to the results of the analysis in an accredited laboratory, Toyota SAE 5W40 engine oil is original, Fig. 4 and the color transitions of the additive elements formed as a result of the reaction with the indicator can be used as a reference for checking the quality of a new batch of Toyota SAE 5W40 engine oil during the incoming inspection. If the color of the sedimentary chromatogram zones of the tested Toyota SAE 5W40 engine oil changes in comparison with the analyzed one, it is rejected or analyzed in the laboratory to confirm the quality indicators established by the passport.

Example 17. On white writing paper GOST R ISO 9705-2000 impregnated with an indicator solution (sample 6), at a temperature of 2 ° C, a drop of the original fresh Lukoil SAE 10W40 engine oil produced by PJSC Lukoil is applied, which, due to the forces of surface tension and wetting leaves a radial sedimentary chromatogram in the form of: core - green; 1st diff. zone in the form of a greenish-orange ring; 2nd diff. the zone is dark orange; 3rd diff. the zone is light orange, impregnated with a base paint base. A clear perimeter of the core, in which the additive elements are concentrated due to the pressure of the droplet weight and the diffusion of the oil base with the additive elements to the perimeter. Then, due to adsorption and capillary diffusion, the additive elements, depending on the diffusion rate, form the second and third zones that differ in color. According to the results of the analysis in an accredited laboratory, the Lukoil SAE 10W40 engine oil is original and the color transitions of the additive elements formed as a result of the reaction with the indicator can be used as a standard for checking the quality of a new batch of Lukoil SAE 10W40 engine oil during the incoming inspection. If the color of the zones of the sedimentary chromatogram of the tested Lukoil SAE 10W40 engine oil changes in comparison with the analyzed one, it is rejected or analyzed in the laboratory to confirm the quality indicators established by the passport.

Example 18. On newsprint paper, GOST 6445-74 impregnated with an indicator solution (sample 7), at a temperature of 25 ° C, a drop of original fresh engine oil Gazpromneft 10W 40 of PJSC Gazpromneft is applied, which, due to the forces of surface tension and wetting, leaves a radial sedimentary chromatogram in the form: the core is greenish-blue; 1-yadif. Zone in the form of a blue-orange ring; 2nd diff. the zone is dark orange; 3rd diff. the zone is light orange, impregnated with a base paint base. A clear perimeter of the core, in which the additive elements are concentrated due to the pressure of the droplet weight and the diffusion of the oil base with the additive elements to the perimeter. Then, due to adsorption and capillary diffusion, the additive elements, depending on the diffusion rate, form the second and third zones that differ in color. In fig. 5 reference radial sediment chromatogram of the original engine oil Gazpromneft SAE 10W40 corresponding to the quality certificate of the manufacturer of PJSC Gazpromneft, which, by comparing radial sediment chromatograms, can be used to check the quality of a new batch of engine oil Gazpromneft SAE 10W40 during the incoming inspection. If the color of the zones of the radial sedimentary chromatogram of the tested Gazpromneft SAE 10W40 engine oil changes in comparison with the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport. Figures 14, 15, 16 and 17 show chromatograms of Gazpromneft SAE 10W40 engine oil diluted with synthetic polyalphaolefin oil, which clearly confirms the change in the oil chromatogram, which can be used to determine a fake. According to statistics, high-quality lubricants are counterfeited by diluting them with base or cheap oil.

Example 19. On the filter paper "Blue Ribbon" impregnated with a 0.5% aqueous solution of bromothymol blue (according to the prototype, RF patent No. 2484462), at a temperature of 25 ° C, a drop of original fresh engine oil of Gazpromneft 10W 40 is applied, which, thanks to the forces of surface tension and wetting leaves a radial sedimentary chromatogram in the form: core-greenish; 1st diff. Zone in the form of a greenish-orange ring; 2nd diff. the zone is dark orange; 3rd diff. the zone is light orange, impregnated with a base oil base. An indistinct core perimeter was obtained, in which additive elements are concentrated. The zones of the sedimentary chromatogram have indistinct, pale color transitions, in contrast to example No. 19 and Fig. 4, by which it is difficult to determine the presence of additives and the normalized base number by comparison with the reference chromatogram.

Example 20. On paper, GOST 12026-76 impregnated with an indicator solution (sample 8), at a temperature of 25 ° C, a drop of original fresh engine oil for diesel engines M-14 G ₂ TsS produced by PJSC NK Rosneft is applied, which, thanks to the forces surface tension and wetting leaves a radial sedimentary chromatogram in the form: core - blue-blue; 1st diff. zone in the form of a dark orange ring; 2nd diff. zone orange; 3rd diff. the zone is light orange, impregnated with a base oil base. A clear perimeter of the core, in which the additive elements are concentrated due to the pressure of the droplet weight and the diffusion of the oil base with the additive elements to the perimeter. Then, due to adsorption and capillary diffusion, the additive elements, depending on the diffusion rate, form the second and third zones that differ in color. In fig. 6 is a reference radial sedimentary chromatogram of the original engine oil M-14 G ₂ TsS corresponding to the quality certificate of the manufacturer of PJSC NK Rosneft, which, by comparing the radial sediment chromatograms, can be used to check the quality of a new batch of M-14 G ₂ TsS engine oil during incoming inspection. In the event of a change in the color of the zones of the radial sedimentary chromatogram of the tested engine oil M-14 G ₂ TsS with a standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established by the passport. Figures 18, 19, 20 and 21 show the chromatograms of M-14 G ₂ TsS engine oil diluted with synthetic polyalphaolefin oil, which clearly confirms the change in the oil chromatogram, which can be used to determine a fake. According to statistics, high-quality lubricants are counterfeited by diluting them with base or cheap oil.

Example 21. On paper, GOST 12026-76 impregnated with an indicator solution (sample 1), at a temperature of 25 ° C, a drop of Toyota 5W40 engine oil from EKKSON MOBIL is applied to the engine for 240 hours. Radial sedimentary chromatogram in the form of a core and three zones. The core is the zone corresponding to the darkest homogeneous part of the oil spot on the filter, dark brown with a shade of blue, in which insoluble impurities are noticeable. The first diffusion zone is annular, lighter in color than the central core, formed as a result of the passage of insoluble impurities through the pores of the paper filter. The ring size is small, indicating a low detergent / dispersant content in the oil. The second zone of oxidized oil is annular from yellow to light brown in color and contains soluble products of oil and fuel oxidation. The third zone of clean oil is orange, which characterizes the presence of fuel by increasing the area of the oil stain applied to the filter. Oil analysis showed a sharp decrease in base number to 2.5 mg / KOH / g. and a decrease in viscosity by 17%. According to the oil stain analysis, the engine oil is not suitable for further use.

Example 22. On white writing paper GOST R ISO 9705-2000 impregnated with an indicator solution (sample 2), at a temperature of 25 ° C, a drop of Lukoil 10W40 engine oil produced by PJSC Lukoil is applied for 236 operating hours, a radial sedimentary chromatogram in the form of a core and three zones of precipitation. The core is a zone corresponding to the darkest homogeneous part of the oil spot on the filter, dark brown with shades of blue, in which insoluble impurities are noticeable. The diffusion zone is an annular zone of a lighter color than the central core. Formed as a result of the passage of insoluble impurities through the pores of the paper filter. The ring size is small, indicating a low detergent / dispersant content in the oil. The oxidized oil zone is an annular zone with a color ranging from yellow to light brown. It contains soluble oil and fuel oxidation products. A zone of clean oil with a perimeter with a color developing indicator paper. A pronounced black edging of the core and a significant decrease in the core and diffusion zone indicate the presence of water. There is fuel in the oil because the clean oil zone has increased; the light brown color of the zone indicates that the oil has oxidized. Oil analysis showed a sharp decrease in base number to 3.5 mg / KOH / g. According to the oil stain analysis, the engine oil is not suitable for further use.

Example 23. A drop of fresh oil for an automatic transmission TOTEK Astra Robot-Automatic manufactured by Totek LLC is applied to the filter paper "Blue Ribbon" soaked in an indicator solution (sample 3), at a temperature of 25 ° C, which, due to the forces of surface tension and wetting leaves a radial sedimentary chromatogram in the form of a greenish-yellow core with a clear perimeter and three zones of colored precipitation: brown; orange and light orange soaked in oil. The oil complies with the manufacturer's quality passport, therefore, by comparing radial sediment chromatograms in color and size, it can be used to check the quality of a new batch of oil for an automatic transmission TOTEK Astra Robot-Avtomat during incoming inspection. If the color of the sedimentary chromatogram zones of the tested oil for the automatic transmission TOTEK Astra Robot-Avtomat is changed with the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 24. A drop of fresh SAE 75W90 gear oil from Addinol is applied to a white cotton chintz fabric according to GOST 29298-2005, impregnated with an indicator solution (sample 4), at a temperature of 30 ° C, which leaves a radial sedimentary chromatogram in the form of a light yellow core with a clear: dark orange perimeter, in which additive elements are concentrated due to the pressure of the drop weight and diffusion of the oil base with additives to the perimeter and three zones of colored precipitation: translucent light crimson; light orange; orange-raspberry color soaked in oil. In fig. 7 reference radial sediment chromatogram of fresh SAE 75 W90 gear oil complying with the Addinol manufacturer's quality data sheet, which, by comparing radial sediment chromatograms in color and size, can be used to check the quality of a new batch of fresh SAE 75W90 gear oil during incoming inspection. If the color of the zones of the sedimentary chromatogram of the tested fresh SAE 75 W90 transmission oil differs from the standard, it is rejected or analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 25. A drop of used SAE 75 W90 gear oil is applied to the Blue Ribbon filter paper soaked in an indicator solution (sample 5) at a temperature of 35 ° C, which leaves a radial sediment chromatogram in the form; a dark kernel with specks of a light yellow hue, mechanical impurities are noticeable; two zones of brown precipitation; orange; translucent light orange. The oil worked in terms of mileage, 24 thousand km, in the gearbox of a Mitsubishi passenger car, the analysis of the oil did not reveal any rejection indicators, and according to the pattern, the color of the kernel is close to the color of the kernel of fresh oil in example 24, further use is recommended.

Example 26. A drop of fresh brake fluid Brake Fluid DOT 4 from Castrol is applied to a white cotton chintz fabric according to GOST 29298-2005, impregnated with an indicator solution (sample 3), at a temperature of 30 ° C, which leaves a radial sedimentary chromatogram in the form of a white core and three zones of colored precipitation: yellow: red and light orange impregnated with oil, fig. 8. The oil complies with the manufacturer's quality certificate, therefore, by comparing radial sediment chromatograms in color and size, it can be used to check the quality of a new batch of Brake Fluid DOT 4 from Castrol. If the color of the zones of the sedimentary chromatogram of the tested oil changes by the obtained chromatogram (reference), it is rejected and analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 27. A drop of polyalphaolefin oil with a viscosity of 12 cSt at 100 ° C is applied to the filter paper "Blue ribbon" soaked in an indicator solution (sample 5, orange) at a temperature of 40 ° C, which leaves a radial chromatogram on the painted surface of the indicator strip in in the form of a yellow-green kernel and a zone along the perimeter of the kernel in the form of a dark orange spot, which disappears after drying. By comparing this radial chromatogram in color and size with the chromatogram of the new fresh polyalphaolefin oil being inspected during the incoming inspection, its quality can be assessed. If the color and size of the chromatogram zones of the tested fresh polyalphaolefin oil with the standard differ, it is rejected and analyzed in the laboratory to confirm the quality indicators established by the passport.

Example 28. A drop of MC-20 oil with a viscosity of 19.5 cSt at 100 ° C is applied to the filter paper "Blue ribbon" soaked in an indicator solution (sample 6, orange) at a temperature of 50 ° C, the surface of the indicator strip in the form of a yellow-green core and a zone along the perimeter of the core in the form of a ring of dark orange color. It can be used as a reference radial chromatogram of high-quality MC-20 oil, corresponding to the manufacturer's quality passport according to the analyzed parameters. By comparing radial chromatograms in color and size, you can check the quality of a new batch of fresh MC-20 oil during incoming inspection. If the color and size of the chromatogram zones of the checked fresh MC-20 oil differ with the standard, it is rejected and analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 29. On the filter paper "Blue ribbon" impregnated with an indicator solution (sample 6), at a temperature of 30 ° C, a drop is applied, oxidized in laboratory conditions, MC-20 oil, which left a radial chromatogram on the painted surface of the indicator in the form of a yellow core and a zone around the perimeter of the core in the form of a ring of dark orange color. We compare the radial chromatogram in color and size with the standard (chromatogram according to example 28), there are noticeable differences in the size and color of the nucleus. The time of absorption and spreading of a drop of oil is 1.2 times longer than the formation of a reference chromatogram. Analysis of the oxidized oil showed an increased acid number by 12% and a viscosity by 27% compared to fresh MC-20 oil according to the oil quality certificate.

Example 30. A drop of original fresh motor oil for diesel engines M-14 G ₂ TsS is applied to the universal indicator paper PND50-975-84 manufactured by Lahem, size 6 × 75, impregnated with an indicator solution of cherry decoction, sample 9, at a temperature of 60 ° C, which, due to the forces of surface tension and wetting, leaves a sedimentary chromatogram on a strip of paper in the form of four zones of colored precipitates of a blue-blue (part of) the core and three zones: 1st in the form of a dark orange ring: 2nd orange; 3rd light orange, formed as a result of the reaction of the elements of the additives with the indicator solution. The sediment chromatogram of the original engine oil M-14 G ₂ TsS corresponds in the width of the zones and the color to the reference Fig. 6 (example 20), which, also by comparing sediment chromatograms, can be used to check the quality of a new batch of M-14 G ₂ TsS engine oil during the incoming inspection. The disadvantage of using the universal indicator paper PND50-975-84 produced by Lahem, impregnated with an indicator solution of a decoction of cherries, is the small size of 6 × 75 millimeters on which stripes of zones, their width and color are visible. For convenient use of a small universal test strip, a drop of the test oil is applied to the left end of the strip, which is installed horizontally. In this position, the oil with additives, due to the forces of surface tension and wetting, moves to the right side, leaving a sedimentary chromatogram with four diffusion bands.

Example 31. On a universal indicator paper RKS of Russian production, impregnated with an indicator solution, sample 4 (Sample 4 was chosen, since the size and color of the chromatogram stripes were disrupted on sample 9. The disadvantage of using universal indicator paper RKS impregnated with indicator solution of cherry decoction is its small the size on which the stripes of zones, their width and color are poorly visible.), at a temperature of 60 ° C, a drop of original fresh engine oil for diesel engines M-14 G ₂ TsS is applied, which, due to the forces of surface tension and wetting, leaves a sedimentary chromatogram in the form of four zones of colored precipitation, blue-blue (part of) the core and three zones: 1st in the form of a dark orange ring; 2nd orange; 3rd light orange, formed as a result of the reaction of the elements of the additives with the indicator solution. The sediment chromatogram of the original engine oil M-14 G ₂ TsS corresponds in the width of the zones and the color to the reference Fig. 6 (example 20), which, also by comparing sediment chromatograms, can be used to check the quality of a new batch of M-14 G ₂ TsS engine oil during the incoming inspection. For convenient use of a small universal test strip, a drop of the test oil is applied to the left end of the strip, which is installed horizontally. In this position, the oil with additives, due to the forces of surface tension and wetting, moves to the right side, leaving a sedimentary chromatogram with a core and four diffusion bands.

Example 32. At the tip of a strip of filter paper "Blue Ribbon" measuring 8 × 80 mm. impregnated with an indicator solution (sample 3), at a temperature of 25 ° C, a drop of original fresh engine oil for diesel engines M-14 G ₂ TsS is applied, the strip is set in a vertical position with the oiled tip down, thanks to the forces of surface tension and wetting, the oil rises up the strip , leaving a sedimentary chromatogram on a strip of paper in the form of four colored precipitates: green (part of) the core and three zones: 1st in the form of a smoothly passing light green color to brown; 2nd in the form of a thin yellow stripe; 3rd brown, impregnated with oil, formed as a result of the reaction of additive elements with indicator solution. Due to gravity, precipitation zones are smaller and more saturated colors. Thus, according to example 31, you can check the quality of the additives and the performance of lubricants and technical fluids during the incoming inspection and current diagnostics of equipment.

Example 33. At the tip of a strip of filter paper "Blue Ribbon" measuring 8 × 80 mm. impregnated with an indicator solution (sample 3), at a temperature of 25 ° C, a drop of mineral base oil (a mixture of MS-20 and I-12A) with a viscosity of 19.5 cSt, mixed with 2% of the mass. S-300 additives, 2% CD-7 additive and 0.5% C-5A additive, the strip is set in a vertical position with the oiled tip down, due to the forces of surface tension and wetting, the oil rises up the strip, leaving a sedimentary chromatogram on the paper strip in the form of four colored precipitates, a green-blue (part of) the core and three zones: 1st in the form of a smoothly passing light green color to yellow-orange; 2nd in the form of a thin strip of crimson color; 3rd light orange impregnated with oil formed as a result of the reaction of additive elements with indicator solution. Due to the overcoming of gravity during the diffusion of additive elements to the top along the indicator strip, the precipitation zones are smaller and more saturated colors. Thus, using example 33 and reference drawings of additives, we see that the color of the zones of the chromatogram on the indicator strip is mainly determined by the detergent-dispersant, antioxidant and antiwear additives,

Example 34. At the tip of a strip of filter paper "Blue Ribbon" measuring 8 × 80 mm. impregnated with an indicator solution (sample 2), at a temperature of 30 ° C, a drop of the original fresh compressor oil Lukoil Stabio Synthetic 46 is applied, the strip is set in a vertical position with the oiled tip down, due to the forces of surface tension and wetting, the oil rises up the strip, leaving on the strip of paper sedimentary chromatogram in the form of four colored precipitates, yellow-green (part of) the core and three zones: 1st in the form of a smoothly passing light green to yellow-orange; 2nd in the form of a thin strip of crimson color; 3rd light orange impregnated with oil formed as a result of the reaction of additive elements with indicator solution. Due to gravity, precipitation zones are smaller and more saturated colors. Thus, according to example 34, it is possible to check the quality and performance of the oil during the incoming inspection and the current diagnostics of the compressor.

Example 35. On the tip of a strip of filter paper "Blue tape" measuring 8 × 80 mm, impregnated with an indicator solution (sample 4), at a temperature of 30 ° C, a drop of Lukoil Stabio Synthetic 46 compressor oil that has worked in the Sullair compressor for 246 hours is applied, the strip is set in vertical position with the oiled tip down, due to the forces of surface tension and wetting, the oil rises up the strip, leaving a sedimentary chromatogram on the strip of paper in the form of four colored precipitates, a light green (part of) core with inclusions of mechanical impurities and three zones: 1st yellow orange; 2nd in light orange; The third is orange-crimson soaked in oil. Due to gravity, precipitation zones are smaller and more saturated colors. The analysis of the oil showed that it is efficient, the viscosity increased by 6%, the diameter of the wear scar by 3%. Thus, according to example 35, you can check the quality and operability of the oil during the incoming inspection and the current diagnostics of the compressor.

Example 36. On white writing paper GOST R ISO 9705-2000 impregnated with an indicator solution (sample 9), at a temperature of 50 ° C, a drop of blue Tosol-40 coolant with an alkalinity of 10 cm ³ is applied. The obtained chromatogram, Fig. 9: The kernel is light green; the first zone is yellow; the second is red. Before testing, the quality of the coolant was analyzed in the laboratory, so the obtained chromatogram can be used as a reference. If the color and size of the chromatogram zones of the tested Tosol-40 coolant with the standard differ, it is rejected and analyzed in the laboratory to confirm the quality indicators established by the passport.

Example 37. On white writing paper GOST R ISO 9705-2000 impregnated with an indicator solution (sample 10), at a temperature of 50 ° C, a drop of antifreeze G12-40 of light orange color, with an alkalinity of 5.8 cm ³ is applied. The obtained chromatogram: The core is light yellow; the first zone is yellow; the second is orange; the third zone is brown. Before testing, the quality of the coolant was analyzed in the laboratory, so the obtained chromatogram can be used as a reference. In the case of a difference in the color and size of the chromatogram zones of the tested coolant - G12-40 with a standard, it is rejected and analyzed in the laboratory to confirm the quality indicators established in the passport.

Example 38. A drop of fresh Toyota SAE 5W40 engine oil is applied to white writing paper GOST R ISO 9705-2000 at room temperature, fig. 11. On writing paper GOST R ISO 9705-2000 at room temperature apply a drop of spent 240 moto / hour. engine oil Toyota SAE 5W40, fig. 12. A drop of spent 240 moto / hour is applied to a universal indicator with a substrate made of GOST R ISO 9705-2000 paper at room temperature. engine oil Toyota SAE 5W40, fig. 13. Compare fig. 11 with fig. 4. In fig. 11 colorless oil stain, which disappears after drying. In Fig. 4, we see a chromatogram of an oil with distinctive features of the color of the core, diffusion zones and sizes indicating the presence of additives in it. Compare Fig. 12 with fig. 13. In fig. 12 the oil spot has a dark core and a lighter diffusion zone. From this figure, it is difficult to determine the additives remaining in it, and therefore the performance of the oil. In fig. 13, we see a chromatogram of the oil with the distinctive features of the presence of additives in it and by the increased size of the 3rd diffusion zone (in comparison with the 3rd diffusion zone in Fig. 12) of the fuel, by which, at least qualitatively, it is possible to determine its performance. It was found that the spreading rate of the oil and the increased area of the chromatogram in Fig. 13 is higher than the drop sample of fresh Toyota SAE 5W40 engine oil in Figure 4. This gives information about a decrease in the viscosity of the engine oil due to the ingress of fuel. Accordingly, according to the method proposed according to the invention, the viscosity of the oil is measured in an advantageous way, by the time of penetration and spreading of the test sample into the substrate of the universal indicator.

Analysis of the tests performed revealed one feature common to all examples. In the first ten minutes, the core has a rich color, indicating the presence of active chemical elements of the additives, in the next 60 minutes, light tones appear in the center of the core, then a dark brown or dark green ring appears around the core. Further, we see on chromatograms, depending on the chemical elements in the additives and their reaction with the chemical products that make up the universal indicator, up to 3 or more colored diffusion zones can be formed, which increases the accuracy of the express analysis.

Therefore, it is important for the user to see the stain formation process in the first 10 minutes. This will make it more likely for him to determine by the color coloration (in the first minutes they are more saturated) and the spreading rate of the spot and its size, a fake. So in fig. 19 in the fake oil M-14G ₂ TsS, obtained by diluting only 10% with base oil, we see a significant difference in the chromatogram color and core size from the chromatogram of the original oil in Fig. 18. If you mix high-quality oil with cheap engine oil with other additives in an amount of up to 10% by weight, then a fake will also be revealed by the appearance of other colors (due to the presence of other chemical elements of the additives). Figuratively speaking, the proposed method allows the color of the chromatogram to reveal a fly in the ointment in a barrel of honey.

During the preparation of the application for the invention, they also tested lubricating coolants, hydraulic oils, heat carriers and aqueous solutions, found the possibility of obtaining reference chromatograms on a universal indicator in accordance with all the features of the claims, to identify counterfeits by color, core size and diffusion zones of the subject product. The results of the express analysis are shown in Blitz 3.

According to the description of the tests performed and the examples given in the text, the preparation and use of a universal indicator for the express analysis of additives, lubricants, technical fluids, including used ones, is clear to the specialist. Mainly, the proposed method is used (second option) for express analysis of fresh additives, lubricants of technical fluids upon purchase and before use, as well as lubricants and technical fluids, worked out in technology for the qualitative determination of defects in it. In this case, a drop of the first (or second) test additive or lubricant or technical fluid, preferably in the form of a dot, is applied to the universal indicator according to at least one of the above-mentioned claims and allows it to penetrate into the universal indicator.

The present invention, already in terms of the rate of increase in the chromatogram and drying on a universal indicator substrate, gives information about the viscosity of the additive, lubricant and technical fluid. When testing a lubricant that has worked in technology, the long absorption of the lubricant and technical fluid into the universal indicator indicates its oxidation. Accordingly, according to the method according to the invention, it is predominantly measured, the time of penetration of the test sample into the substrate of the universal indicator.

By evaluating the chromatogram: the color, the size of the zones, the rate of their increase, the presence of mechanical impurities, coolants, water on it, the user receives information concerning:

- the viscosity of the lubricant or technical fluid, which is determined at least qualitatively;

- the oxidation state of the lubricant or technical fluid, which is determined at least qualitatively;

- the proportion of carbon deposits in the lubricant, which is determined at least qualitatively;

- the presence of water in the lubricant or technical fluid, which is determined at least qualitatively;

- the content of glycol in the engine oil, which is determined at least qualitatively;

- under certain conditions, the dilution of the engine oil with fuel, which is predominantly determined at least qualitatively;

- the content of dust, mechanical impurities in the lubricant or technical fluid, which are determined at least qualitatively;

For this purpose, the chromatogram of the lubricant or technical fluid is advantageously compared with at least a reference chromatogram.

In this case, the chromatograms show in a reasonable way the levels of the presence and condition of the additive, lubricants, technical fluids and allow the specialist and the user to draw conclusions from the rapid analysis performed to the same extent.

For example, the discrepancy between the chromatograms of additives, lubricants, technical fluids in the color and size of diffusion zones, the time of their manifestation indicates the absence in the required amount of chemical elements that determine the detergent-dispersant, antioxidant, antiwear and other properties and the presence of other chemical elements that are not included in the formulation of original additives, lubricants, technical fluids (in the case of mixing with cheap additives and lubricants). Residues from the combustion process (carbon deposits in engine oil) indicate poor injection, poor mixture formation, improper operation of the high pressure fuel pump, uneven air supply for mixing with fuel or improper operation leading to contamination of the engine and engine oil, as well as oil passages, to a decrease in operating ranges, to engine overheating or to increased wear of rubbing surfaces.

The inoperative condition of the lubricant can be explained, for example, by too old lubricant or technical fluid, the presence of mechanical impurities, wear products, glycol or water, formed acids, with an increased flow of breakthrough gases into the crankcase due to wear of the piston rings and piston.

The presence of fuel in the engine oil, for example, can be caused by insufficient injection due to poor injector operation, carburetor, defect or clogging of the injector, improper ignition, fast driving with a cold engine, driving over short distances that lead to increased fuel consumption, malfunction electronic control unit, to the dilution of motor fuel and, as a result, to the danger of overheating of the cylinder head, to a decrease in the lubricity of the engine oil or to increased wear of rubbing surfaces (pistons, cylinders).

Water and glycol can enter, for example, due to a seal failure in the cylinder head, microcracks in the cooling jacket, due to moist air or condensation in an unheated engine. A possible consequence of this will be the oxidation of the engine oil, an increase in its viscosity, temperature and wear of friction units.

In all cases described above, it is recommended to check for possible causes and carry out an oil change. Express analysis should be repeated after a run of 10 to 500 km. To make sure that the defects have been completely eliminated.

Conducted express analyzes showed that the formation of chromatograms depends on the viscosity, temperature and size of the applied drop of lubricant and or technical liquid on the universal indicator. Optimal conditions are considered: application of the 1st or second drop on the universal indicator at temperatures of 10-60 ° С; waiting for the formation of the chromatogram 1-180 minutes. The results obtained are documented and used to improve the quality of the lubricant and its performance in technology.

The formulations of additives, lubricants, brake and coolants of their oil bases are constantly being improved, this introduces a change in the color of the core and diffusion zones and the proposed method allows you to distinguish an original high-quality oil from a fake. The most common counterfeit of a lubricant, technical fluid, is dilution with base oil base and cheap oil. Figure 15 shows how the dilution of engine oil Gazpromneft SAE 5W40 affects. When diluted by 25% with base oil, the core of the chromatogram turns from a greenish-blue color to light green with a dark ring (perimeter) when passing into the first diffusion zone, while the size of the core and the color of the pattern zones decreases, and the third diffusion zone increases. Even when the engine oil M-14 G ₂ TsS is diluted by only 10% with polyalphaolefin oil, Fig. 19 you can find a fake. It is very important to apply the first or second drop of the test sample on a strictly horizontally located universal indicator, since the third and further drops and their sizes affect the size of the chromatogram and the color shades of the core and diffusion zones. There are minor distinctive features of chromatograms on a universal indicator made of cloth and paper. Temperature has a definite effect on the size of the core and diffusion zones. Therefore, it is recommended to carry out tests with a universal indicator on one type of substrate and one temperature in the range of 10-60 ° C. The formation of the size of the nucleus and diffusion zones of the chromatogram occurs within 1-180 minutes, after which they are photographed and stored in a dark place in a sealed bag.

Based on the test results, two variants of the method are proposed: 1. Express analysis of the base number and performance of engine oils, including waste; 2, Express analysis and performance of additives, motor, transmission oils (lubricants), technical fluids, including used ones. At the same time, due to the presence in the composition of solutions of well-known indicators of decoctions and alcoholic tinctures of vegetables and berries, fruits reacting with chemical elements of additives, the accuracy of evaluating the values of the base number increases, which makes it possible to determine the base number of fresh engine oil and carry out timely oil changes to deteriorate its detergent -dispersive properties. The universal indicator paper obtained by the proposed method has an orange color and has contrasting color transitions on the scale, the strength of fixing the indicators, the absence of erosion and greater stability of the resulting color after contact with the analyzed samples of additives, lubricants, technical fluids, including used ones. Using a reference scale and a chromatogram, the quality, originality of the additive, and the base number of the lubricant, including the used one, are determined with great accuracy. In addition, the developed universal indicator can be used along with known indicators for determining the pH and alkalinity of solutions.

Sources of information

1. USSR author's certificate No. 1337743, G01N 21/78, 31/22, 1987

2. RF patent No. 2183018, G01N 31/22, G01N 21/78, GG1N 33/28, G01N 33/30, 15.06.2001

3. Copyright certificate SU No. 524534 D21F 11/14. 1976 year

4. Copyright certificate SU 1127935 D21H 1/46, C01N 31/22, 07.12.84 g.

5. Patent GB 922606, 1963

6. RF patent No. 2399050 G01IN 33/28, G01N 21/78, B01N 39/18, D21N 27/08, 09/10/2010

7. RF patent No. 2464368 D21F 11/14, G01N 31/22, 20.10.2012,

8. RF patent No. 2464462 G01N 33/28, G01N 21/78, G01N 31/22, 2.

Claims (10)

1. A universal indicator for the express analysis of the content of additives and the performance of lubricants, characterized in that the universal indicator is obtained by impregnating fibrous materials with dimensions of 30 × 40 mm or 8 × 80 mm with a water-alcohol solution of the following composition, g: methyl orange 0.05- 0.3; methyl red 0.15-0.3; bromothymol blue 0.3-50; alizarin yellow P 0.1-0.3; phenolphthalein 0.01-0, .1; malachite green 0.01-0.05; decoction of red cabbage 5-20; decoction of cherries or alcoholic infusion of cherries 0-5; tetraethylammonium bromide 0-9.0 as a fixing agent; an aqueous solution of ethyl or isopropyl alcohol 914.95-994.32 at temperatures of 10-60 ° C. 2. A method for express analysis of the content of additives and the performance of lubricants, including those used, by the base number, by applying a drop sample of the analyzed material to the indicator, characterized in that the universal indicator according to claim 1 is used as an indicator. 3. The method according to claim 2, characterized in that the express analysis is carried out by processing a drop sample of an additive with a base oil, or a lubricant, or a technical liquid with a mixture of an aqueous solution of alcohol and a solvent in the presence of a universal indicator, followed by comparing the color of the mixture with a standard, and the analyzed drop sample is introduced into a mixture consisting of 30-33% vol. ethyl alcohol with water in a ratio of 2: 3 vol. and 67-70% vol. gasoline AI-80, or AI-92, or AI-95 or solvent Nefras 40/70 or Nefras 80/120 in the presence of a universal indicator. 4. The method according to claim 3, characterized in that by comparing the color of the reagent mixture with a drop of the product, in the presence of a universal indicator, with the color of the reference scale for determining the base number, the base number of the additive in the mixture with base oil, lubricant and technical fluid is determined. 5. The method according to claim 2, characterized in that a drop of an additive, or a lubricant, or a technical liquid is applied to the universal indicator, and after 1-180 minutes the size, color of the core, diffusion zones of the obtained chromatogram are determined, and by their ratio by comparison with the reference chromatogram is used to judge the quality and performance of the additive, lubricant and technical fluid. 6. The method according to p. 5, characterized in that in order to improve the quality of the chromatogram and the accuracy of determining the performance of additives, lubricants and technical fluids, an aqueous-alcoholic solution of indicators, a decoction of red cabbage 5-20% of the mass. and a decoction of cherries or an alcoholic infusion of cherries 0-5% of the mass. 7. The method according to claim 5, characterized in that the filter paper "Blue tape", or white writing paper, or newsprint paper, or chintz cloth, with dimensions of 30 × 40 mm or 8 × 80 mm, is used as a substrate for the universal indicator, which is impregnated with solutions with certain concentrations of indicators at temperatures of 10-60 ° C, which is dried at room temperature and placed in a sealed bag. 8. The method according to claim 5, characterized in that the chromatogram of the drop is compared with the chromatogram of the reference, taking into account the size of the nucleus or part of the nucleus in the case of using a narrow strip of a universal indicator, the size of diffusion zones, color and their growth rate. 9. The method according to p. 5, characterized in that, at least qualitatively determine: the viscosity of a lubricant or technical liquid by the diffusion rate, size and color of the third diffusion zone of the chromatogram; the degree of oxidation of the lubricant or technical fluid - the presence in the second diffusion zone of color gradations from yellow to dark brown; the proportion of carbon deposits or mechanical impurities in engine oil - by the presence of black particles visible to the eye in the core; the presence of water in the lubricant or technical fluid - by the black edging of the core and a significant decrease in the core and diffusion zone; fuel availability - by the size of the outer ring. 10. A method for carrying out an express analysis of the actual state of technology, in which the method of express analysis of a lubricant operating in the technique according to claim 2 is used.

Images