Method of fluid analysis for metals - products of deterioration of parts and mechanisms, washed these liquids

 

(57) Abstract:

The invention relates to the field of analytical chemistry and can be used to determine the content of an impurity in a variety of special fluids, such as oil, fuel and hydraulic fluids in various industries where these fluids are used. The technical result of the invention is to reduce the error analysis associated with the particle size of the impurity metals - wear products. The inventive method comprises preparing a sample for analysis, preparation of standard samples, construction of calibration graphs, measurement of the concentration of the detected elements, with a sample pre-centrifuged, the precipitate is placed in a separating funnel with a clean analyzed by liquid and after the sedimentation of particles selected volumes of fluid with a narrow classes of particles that are analyzed on the calibration curve corresponding to the known size of the particles, and the concentration of elements in the sample is calculated as the total mass of the element divided by the initial volume of the analyzed fluid. 2 Il.

The invention relates to the field of analytical chemistry and can be used to determine the content of CA is s industry, where these fluids are used.

The method for determination of metallic impurities in organic media /1/, which includes the excitation of the sample induction-coupled plasma and introduction to plasma combined solvent for the sample and sample comparisons. When the sample preparation samples and compare them add a mixture of orthoxylene and acetic anhydride at a volume ratio of 10:1-1:1.

The known method of atomic-absorption determination of vanadium and molybdenum /2/, including their transfer to the complex compound with an organic reagent, which is used as M-cinnamylpiperazine, extraction of the complex in toluene at a ratio of aqueous and organic phases 50:1 and the atomization of the extract in the presence of 2.5-3 M solution of ammonium fluoride.

The known method of atomic absorption analysis solutions /3/ by microcentrifuge defined element on the surface of the helix. When the sample solution is passed through the coil atomizer flow velocity of 0.1-0.3 m/min for 0.1 to 15 minutes while rotating the glass with a solution of the sample around its vertical axis.

The closest analogue is the method of determining the concentration of metals in working aberavon characteristics according to the standard samples, the atomization of the oil samples. Calculated average arithmetic value measurements separately for each of the analyzed elements. On the calibration graphs are simple averages of the measurements are translated into the concentration of the respective element.

The disadvantage of this method is the high error analysis associated with the particle size of the impurity metal wear products. As the particles of metal impurities wear products of units and mechanisms, washed by oil, have a different configuration and size, it has a noticeable effect on the time of their deposition in the sample. The settling velocity of particles increases with their size and with decreasing viscosity of the fluid when it is heated. And because the sample of the working oil is unknown, the average particle size of wear products, to choose the nature of the dependence of the signal, and hence the calibration chart on which I hope the content of the element in the particles and, respectively, in the sample, it is not possible.

The aim of the invention is to reduce uncertainty analysis associated with the particle size of the impurity metal wear products.

The goal of doom, construction of calibration graphs, measurement of the concentration of the detected elements, sample pre-centrifuged, the precipitate is placed in a separating funnel with a clean analyzed by liquid and after the sedimentation of particles selected volumes of fluid with a narrow classes of particles that are analyzed on the calibration curve corresponding to the known size of the particles, and the concentration of elements in the sample is calculated as the total mass of the element divided by the initial volume of the analyzed liquid.

The method is as follows.

Prepare the reference samples with different particle size (average particle size 5 μm, 10 μm and 20 μm) with the same copper content. Construct calibration graphs (Fig. 1), reflecting the dependence of the signal from the metal content in the oil. As can be seen from the graphs, the angle of direct significantly dependent on the average particle size. Because in real samples the particle size is unknown, model samples with different particle size by mixing the specimen with a particle size of 5, 10, 15 μm in the ratio of 1:1:1.

The oil sample was diluted 2 times with clean gasoline and centrifuged. Loose sediments wear on the diameter of deposited faster and after some time the particles, depending on size, are distributed over the entire height of the oil column. This is followed by the deposition of particles and determine the amount of oil with a specified particle size, which corresponds to the narrow particle size class, which was previously calculated and evaluated using comebacks. The dependence of deposition time in the oil particles of copper oxide on their diameter is shown in Fig. 2.

Thus prepared sample of the oil with particles of a given size can be analyzed by the calibration graphs, based on the standard samples of known particle size.

The proposed method can be used to analyze fuel and hydraulic fluid, applying for diluting the liquid with a certain viscosity.

Sources of information taken into account:

1. Auth.St. USSR N 1087848 G 01 N 21/73, 1982

2. Auth.St. USSR N 1456888 G 01 N 21/74, 1987

3. Auth.St. USSR N 1259162, G 01 N 21/74, 1985

4. Certificate of methods of measuring the concentration of products of wear on equipment of the type ISF in the diagnosis engines. M, GosNII GA, 1993, S. 6-10 (prototype).

Method of fluid analysis for metals - products of deterioration of parts and mechanisms, washed these fluids, including the concentration of the detected elements, characterized in that the sample pre-centrifuged, the precipitate is placed in a separating funnel with a clean analyzed by liquid and after the sedimentation of particles selected volumes of fluid with a narrow classes of particles that are analyzed on the calibration curve corresponding to the known size of the particles, and the concentration of elements in the sample is calculated as the total mass of the element divided by the initial volume of the analyzed fluid.

 

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