The method of determining characteristics of trace metals in lubricating oils, fuels and special liquids
(57) Abstract:The invention relates to the field of analytical chemistry. For measuring the characteristics and concentration of metallic impurities in the form of separate particles, the analyzed object in a spray form is fed into the plasma gas discharge in atmospheric pressure with such speed that the particles of metal impurities included in the analytical zone one by one. The prepared sample is optionally dissolved in an organic solvent, determine the number of particles in the initial and dissolved samples, the ratio of their number to determine the coefficient that measures the quality of the working oil, the average particle size is assessed according to the distribution of the particles obtained by analysis of dissolved samples, and taking into account the number of particle traces and their elemental composition determine the level of wear of individual units of machines and mechanisms. The technical result - the possibility of rapid determination of the concentration, medium size, number of particles and the elemental composition of each particle. 3 table. The invention relates to the field of analytical chemistry, namely to the study and analysis of materials with special optical liquids, such as lubricating oil, fuel and hydraulic fluid, the degree of wear of the engines, machines and mechanisms for assessing the quality of lubricating oil, in tribological studies.There is a method of determining the content of iron working in oils /1/. The method is based on filtering oil contains particles of iron through the multilayer filter material, with subsequent review of the magnetic properties of the filter material by means of the magnetic field and the distribution of iron between the layers of the filter septum is judged on the dispersion of particles of iron.There is a method of determining the degree of contamination of lubricating oils /2/. Select a sample of predetermined volume, heat it to a predetermined temperature, optionally measure the rate of temperature rise of the oil, placed in a sample calibrated conduit through which is passed a current of a specified value, measure the resistance of the conductor and the rate of change of resistance of the conductor and calculate the ratio of the rate of change in resistance of the conductor to the speed increase of the oil temperature, which determine the degree of contamination of the oil.There is a method of determining the characteristics of mi is m follows. Enter the sample in the spectral source with speed, providing with a given probability separate in time the recording of signals from each particle analyzed impurities, prepared samples and the comparison samples, while imposing a sample in the form of an aerosol into the plasma torch of cyclone type, register the optical signal radiation at two or more measurement channels, each of which is configured to analytical line radiation of one metal, convert the optical signals into electrical impulses, measure them, determine the mass of individual metal particles traces of contaminants on the pulse and calibration characteristics for the signals registered at the same time on each channel determine the mass ratio of the respective metals, which taking into account the stoichiometric ratio of metals set the particle count particle count of individual traces, the content of metal wear particles and average particle diameter, which determine the level of wear of machines and mechanisms.The closest analogue is the way to determine the distribution of particles in suspension in a gaseous dispersion medium in size, and, the alley the evaporation zone Shine pulsating stream of light containing radiation line of the analyzed element, convert the signal into an electrical impulse acquisitions and analyze amplitude analyzer or integrate the electrical signals from the set of particles passing the evaporation zone during the exposure.The result of integration is taken as the analytical parameter and is proportional to the content of impurities in the analyzed sample.It is known that when the lubricating oil is heated, light fractions evaporate and the oil formed small particles of coke, which stick metal particles, forming a complex ensemble consisting of several particles, bonded Cox. In the analysis of the scintillation method, this ensemble will be registered as one large particle complex composition. Thereby inflated the average particle size and distorted their elemental composition. The concentration of the elements remains unchanged. This makes a significant error in determining the mean size of particles in the oil and affect the evaluation engine wear.Object of the present invention is to provide a way to reduce their iagnostic engines.The problem is solved in that in the method are prepared sample is injected sample with speed, providing with a given probability separate in time the recording of signals from each particle analyzed impurities, in the form of an aerosol spray into the cyclone-type plasmatron, register optical radiation signals simultaneously on two or more measurement channels, each of which is configured to analytical line radiation of one metal, convert the optical signals into electrical impulses, measure them, additionally prepared sample is dissolved in an organic solvent, determine the number of particles in the initial and dissolved samples, the ratio of their number to determine the coefficient, assessing the quality of the working oil, the average particle size is assessed according to the distribution of the particles obtained by analysis of dissolved samples, and based on the number of particles of the trace elemental composition of the particles determine the level of wear of individual units of machines and mechanisms, implementing run diagnostics engines.Run diagnostics wear of engines based on the possibility of registration of complex particles and otodectes the traditional analysis allows to determine the physical connection of particles of various metals (Nalepa and Nadira), which are additional signs when run diagnostics.The method is as follows:
Selected samples of the investigated oil volume of 20-50 ml mix thoroughly with the help of ultrasound or mechanical stirrer, are placed in a glass centrifuge and centrifuged for 60 minutes at a rotational speed of 4000 rpm Centrifugation separates particles of metal having a higher density of metal dissolved in oil and in molecular form. In the sediment fall only particles of metals included in the liquid from the outside. The additive metals, including leguminosarum remain in the upper layer, which is removed after centrifugation. The top layer of oil, not containing particle impurities are removed with a pipette. And remove so as not to capture the selected residue, leaving as little oil in a glass. Then in a glass add the selected diluent, in which there are no elements to analyze on which to prepare the comparison samples, the mixture was mixed thoroughly and poured into the container for analysis.Pre-prepared sample using an ultrasonic atomizer is turned into fine ash. Ranostay of liquid droplets and particles of metals, the flow of carrier gas is continuously injected into the plasma gas discharge microwave plasma torch cyclone type, the temperature of which is about 5200 K.When a particle enters the plasma, it is heated, evaporated and the resulting atomic pairs is excited, i.e., an outbreak (scintillation) particles. The rate at which the sample is selected based, so that particles of the metal trace amounts received in plasma sequentially one after another.The radiation of the atomic vapor through the condenser enters the spectral device. Decomposed into a spectrum of radiation polychromator is registered at the output of the photomultipliers.The pulse duration of the radiation particles is proportional to the time spent plasma and is 1-10 MS, and the amplitude or area of the pulse - evaporated mass of the particle. Therefore, at the output of the photomultipliers are a sequence of pulses of different amplitudes and durations. Electrical pulses from the photomultipliers is coming to an analog-to-digital Converter and processed by the computer.Special calibration characteristics, the computer determines the concentration of metal wear particles and the concentration of rastvorennoe size, their composition and quantity. The following 1 ml of oil is diluted with an organic solvent, strongly shaken for 3 min and analyzed by the same method. For processing 1 ml butter take 1-2 g of solvent. The solvent may be used tetrachlorethylene. The ratio of the number of particles detected in the analysis of the original oil to the number of particles registered in the analysis of oils, solvent-treated, determine the factor reflecting the quality of the oil. The higher the ratio, the higher the quality of the oil, i.e., the closer it for their consumer qualities to broken oil. On the elemental composition of individual particles and their sizes provide useful diagnostics of engines.Example. As an example of useful diagnostics of engines considered engine PS-90.Identification of complex particles with alloys of nodes shown in the table.1.The figures for the chemical element symbol indicate the percentage of this element in the alloy.As follows from the table.1, the complex particles may be a symptom of one or another node.So, in case of detection of particles such as Fe(Cr 12), which may belong to e detected particles Fe(W 9), Cu(Zn 34), Al(Cu 5) in concentrations exceeding a certain value, it is possible to draw a conclusion about the wear of the bearings. If the detected particles of Ti and Mg(Al 9) - not fixed the starter.In addition it is observed that with increasing wear in the oil increases the number of complex particle - naklab. With the increase noticeably with minor wear on the engine during the operating time of several thousand hours. The ratio of the number of complex particle-naklab NCuFethe number of particles of pure metal NCuand NFeyou can assess the dynamics of wear components and assemblies of the engine, which is confirmed by the data given in table.2
As can be seen from the table.2, in the destruction of the site dramatically increases the number of particles of pure metal and the number of particles of naklab.An example of application of the method to estimate the average size and degree of contamination of the oil are presented in table.3
As can be seen from the table. 3, with respect To the number of particles found in the original oil, to the number of particles detected in the dissolved oil depends on the oil developments. The more fresh oil from the engine SO this relationship more. In this respect it is possible to judge the suitability of the oil for further work.The present invention may find application is the same, road transport and other industries.Sources of information taken into account:
1. Auth.St. The USSR 1770902 G 01 N 33/30,19902. Auth.St. The USSR 431451 C 01 N 33/28,19733. RF application 96102385/25, G 01 N 21/73 19964. U.S. patent 3825345 G 01 J 3/30, G 01 N 15/02 1974 (prototype). The method of determining characteristics of trace metals in lubricating oils, fuels and special liquids, characterized in that the prepared sample is injected sample with speed, providing with a given probability separate in time the recording of signals from each particle analyzed impurities, in the form of an aerosol spray into the cyclone-type plasmatron, register optical radiation signals simultaneously on two or more measurement channels, each of which is configured to analytical line radiation of one metal, convert the optical signals into electrical impulses, measure them, additionally prepared sample is dissolved in an organic solvent, determine the number of particles in the initial and dissolved samples, the ratio of their number to determine the coefficient that measures the quality of the working oil, the average Rasma particle traces, the elemental composition of the particles, determine the level of wear of individual units of machines and mechanisms, run through the diagnostics engine.
FIELD: spectral analysis.
SUBSTANCE: method uses one-electrode high-frequency plasma charge in mode of alternating pulses. In accordance to direction of gas along, perpendicularly or oppositely to plasma-generating electrode different constructions of device burners are used. Recording of radiation spectrums is performed in direction dependent on type of used spectrometer: perpendicular to said generated charge for slit spectrometer and in parallel for diaphragm spectrometer.
EFFECT: higher sensitivity, lower costs.
2 cl, 4 dwg
FIELD: engines; testing methods.
SUBSTANCE: invention relates to methods of determining parameters of simple wear particles consisting of one element and complex wear particles consisting of several elements found in oil system of engine for determining type of developing defect. According to proposed method, parameters of all wear particles found in oil system of engine are considered at one to failure. In sample of lubricating oil taken from rear drive box, amount of metal wear particles is determined and parameter of these particles, i.e. elementary content, and mean size of particles of each element in oil sample, concentration of dissolved metal and metal in wear particles are found. Simultaneously with taking oil sample, wash-out sample from main oil filter is taken and parameters of wear particles in this sample are measured and reference values of ratings of wear particles are calculated in form of ratio of simple and complex particles in wash-out sample, amount of particles of each element and amount of complex particles of definite composition in total amount of particles washed from oil filter, rating of wear particles of definite element and rating of complex particles are determined. Basing of relationship of values of parameters of wear particles in samples of oil and oil filter wash-out samples type of developing defect in engine oil system is determined.
EFFECT: improved information content when determining type of developing defect in engine oil filter.
SUBSTANCE: invention relates to atomic emission spectral analysis. The method includes sample introduction into aflame of plasma, registration of the sequence of atomic emission spectrum during the flow of the sample into the plasma, calculation of the intensity of the analytical spectral line of the desired element depending on the arrival time of the sample into the flame of the plasma, determining by the calibration dependence of concentration of the desired element in the sample, and determining the distribution of particles of the sample by mass. The concentration of all the desired elements is determined simultaneously due to the fact that each spectrum sequence is recorded in the spectral range, including the analytical spectral line of the desired elements. Calculation of the intensity of the analytical spectral lines in carried out in each spectrum taking into account the background under the line, after this the dependence concentration of the desired element is obtained from the arrival time of the sample into the plasma, and as per the indicated dependencies the mass of the particles and the concentration of the desired elements in the particles are determined.
EFFECT: providing simultaneous determination of the distribution of particles by mass in a dispersed sample.
6 cl, 4 dwg, 2 tbl
FIELD: instrument making.
SUBSTANCE: device to detect and identify chemical compounds includes chamber of analysed chemical compound entry, chamber of ions analyser, analyser of ions connected to device of data processing. Also device comprises membrane permeable for analysed compounds and arranged between specified chambers, system for supply of sample comprising analysed compound, source of ionisation. Besides, device includes facilities of connection to systems of provision of working atmospheres of chambers, sources of supply and sources of electric working fields. Besides, membrane is arranged with possibility to form ions of analysed chemical compounds on its surface as it is exposed to electromagnet radiation or flow of particles, and source of ionisation is set with the possibility to send electromagnet radiation or flow of particles directly at surface of membrane. At the same time source of ionisation is arranged in the form of source of electromagnet radiation optically joined via scanning device with surface of membrane.
EFFECT: increased sensitivity of method to detect organic compounds, simplified process to produce ions of analysed chemical compounds, reduced requirements to parametres of laser and expanded field of method application and device to detect and identify chemical compounds.
29 cl, 5 dwg
SUBSTANCE: invention refers to medicine and aims at treating necrotic ulcers of oral mucosa in patients with multiple myeloma. Luminal-dependent chemiluminescence of oral fluid is conducted to determine fluorescence light sum and maximum flash. If the light sum value is within the range of 1.02 to 6.6 standard units, and the maximum flash value is 0.7 to 2.5 standard units, the toothpaste Lacalut fluor is used 2 times a day and solcoseryl dental adhesive paste 4 times a day after meals and before bedtime to relieve symptoms completely. The light sum value 8.3 to 13.5 standard units and the maximum flash value 3.4 to 4.2 standard units, the toothpaste Colgate total propolis is used 2 times a day and the film preparation Oblecol three times a day to relieve symptoms completely.
EFFECT: use of the invention reduces a length of epithelisation of necrotic ulcers of oral mucosa.
SUBSTANCE: gas, liquid and solid-body burners, connected in order of application to fitting and HF generator by platform movement, are separately placed in device for spectral analysis of substance composition on platform on HF generator.
EFFECT: invention makes it possible to carry out analysis of atomic composition of gas, liquid and solid substances by means of single device.
SUBSTANCE: invention relates to spectral analysis and can be used in biological and clinical diagnostic laboratories for monitoring state of health of patients. Method for laser nuclear emission spectral analysis of hair includes treatment of analysed sample at stages of water washing, drying and thermal treatment at next tool method of determining content of metals using pilot laser for accurate selection of radiation zone of inspected sample. At that, during whole process of treatment analysed sample controlled part stays in capsule volume less than 10 mql, and stages of heat treatment are combined and reduced to few minutes at state of sample to its carbonisation at 285 ± 5 °C, in process of which recorded losses of volatile components contained in exhaust gases with hydrocarbon matrix, using their source of excitation of six-jet plasmatron that is followed by laser irradiation of charred test in subsequent staged treatment spectrum analytic signals obtained during implementation of both methods of spectra excitation.
EFFECT: higher accuracy of hair analysis due to control chemical composition of exhaust gases.
1 cl, 1 dwg
SUBSTANCE: invention refers to medicine, namely to medical diagnostics of the presence of acetone in the expired air of a patient. Method of measuring concentration of acetone in the expired air is based on measuring the level of acetone content according by the discharge emission lines at low pressure of the expired air sample of a patient with setting of the concentration of water steams, determined by the parameters of glow discharge. Proposed device consists of discharge tube with the discharge in the pumped through the tube of the expired air of a patient combined with visible wavelength range spectrometer and with a possibility of decoding and interpretation of emission spectra. Using the invention provides the possibility of non-invasive control of glucose content in diabetic's blood by measurement of acetone concentration in the expired air in real time.
EFFECT: invention provides to increase accuracy and measuring sensitivity of acetone impurities concentration in the expired air of a patient, as well as to simplify the design and to expand the range of devices of this purpose.
2 cl, 5 dwg
FIELD: chemical industry; petrochemical industry; analysis of the materials by the chemical methods.
SUBSTANCE: the invention is pertaining to the field of analysis of the materials by the chemical methods (by titration, with utilization of chemical indicators), containing the organic compounds of magnesium and may be used in chemical and a petrochemical industry at exercising control over the quality of petroleum. The invention provides, that magnesium chloride from the oil test is produced by impregnation of the ash-free filter with the tested oil with its subsequent incineration up to the complete ashing. Then the ash is dissolved in 30-40 cm3 of the weak 6 Mole/dm3 solution of hydrochloric acid. The produced solution id boiled within 15-20 minutes, transferred by a spray of the distilled water into the graduated flask. Take the aliquot, in which add the distilled water and neutralize it with ammonia (dropwise) up to pH=10.0, introduce the ammoniacal buffered solution and the indicating device the chromogen black ЕТ-100 and titrate 0.025 Mole/cm3 with the B-trilonum solution till the change of the a crimson-violet color into blue- pale blue, and quantity of magnesium (in mass%), is determined by the empirical formula. The invention allows to reduce the time duration for determination of the contents of magnesium, to improve the labor conditions due to exclusion from the process of the toxic and flammable benzole without reduction of requirements on toxicity and reliability of the produced results.
EFFECT: the invention ensures reduction of the time for determination of the contents of magnesium, improvement of the labor conditions, exclusion from the process of the toxic and flammable benzole without reduction of requirements to toxicity and reliability of the produced results.
FIELD: analytical methods.
SUBSTANCE: invention is intended for use as a means of metrologically supporting measurement techniques in determination of total alkaline number of motor oils and lubricating materials. This means is represented by composition containing 75-84% liquid hydrocarbons, 0.05-6% water-soluble alkali component, and 15-20% aliphatic alcohol. Use of standard specimen allows performing reliable estimation of quality of motor oils and lubricating materials by accessible acid-base titration technique requiring no special instrumentation equipment.
EFFECT: simplified analytical procedure.
SUBSTANCE: invention relates to the field of testing petroleum derivatives, in particular to testing hygroscopicity of aviation synthetic oils, and can be utilized in institutions engaged in development and application of lubricating oils for aircraft techniques and for estimating changes in quality conditions of aviation synthetic oils from tendency of oils to water absorption under operation conditions. In a method of estimating hygroscopicity of oils from amount of absorbed water, including sampling oil, keeping sample at specified relative humidity and temperature in presence of distilled water, and then calculating amount of absorbed water using thus obtained dependence, additionally calculating content of water in initial sample (C0), specifying keeping time (t) for sample of oil at specified relative humidity and temperature, and calculating amount of absorbed water (C1) in oil sample from mathematic dependence taking into consideration experimentally found maximum water solubility constant (Cmax) and constant coefficient (ka) for particular kinds of aviation synthetic oils.
EFFECT: reduced determination time and labor expenditure for determination, increased sensitivity of method under oil operation conditions without losses in accuracy and reproducibility.
1 dwg, 3 tbl