Method of determining dispersity of emulsion fuels

FIELD: investigating or analyzing materials.

SUBSTANCE: method comprises direct visualization of image, which is formed in microscopic observation, processing the images, and determining the quality of the emulsion from the histogram of the water drop distribution in the fuel, mean size of drops, and dispersion of the results. The fuel sample of high viscosity is heated up to 50-60°С.

EFFECT: enhanced reliability of determining.

1 cl, 4 dwg, 1 tbl, 2 ex

 

The invention relates to the field of quality control of emulsion fuels, can be used to control the receipt and storage of water-based fuels and applies to fuel consisting of liquid petroleum products, resins and water.

There is also known a method for determining the dispersion of the emulsion by measuring the optical density of the emulsion on fotoelektrokalorimetry ck-2 and calculated by the equation Geller (USSR 1754192, 15.08.1992).

Closer to the invention is a method of determining the dispersion of the water fuel emulsions (VTE), including:

1. The determination of the period of stability during laboratory storage of VTE in glass tubes (20 cm3with a visual assessment of coalescence by measuring the time from the moment of preparation and staging of VTE deposited to allocate 1% of the dispersed phase. This method allows to estimate the time during which there is the emulsion.

2. The definition of “rheological” stability when stored in glass cylinders (250 cm3) under normal conditions, consisting in periodic determination (after 1 hour in microemulsion, the size of the dispersed phase of more than 0.01 μm, and 24 hours in microemulsions, the size of the dispersed phase of less than 0.01 μm) kinematic viscosity of the emulsion in the middle layer.

3. Thermochromics stability when the cycle is logical up to 50± 2°With thermostat and cooled to -12±2°in the cryostat sample VTE in laboratory conditions with a visual assessment of coalescence.

4. Evaluation of thermal stability with increasing temperature 10 cm3VTE in the glass tube (20 cm3). When heated VTE with a speed of 1°With 1 min visually estimated the emergence of a clear phase boundary (Luneva CENTURIES and other Chimmotologie, the materials of the seminar, the Society “Knowledge”, RSFSR, Moscow house of scientific and technical propaganda, M., 1990, s-132).

The disadvantages of the known methods is the duration analysis using expensive equipment, as well as the relatively low accuracy.

The purpose of this invention is to eliminate these drawbacks.

This goal is achieved by a method for determining the dispersion of emulsion fuels by direct visualization of the image forming microscopic observation, with further computer processing and evaluation of the quality of the emulsion by the histogram distribution of water droplets in the fuel volume, the average value of the droplet size and the RMS deviation of the results. In the case of high-viscosity fuel sample is preferably heated to 50-60°C.

The method allows to measure the water droplets in the fuel size 1-400 microns.

The way the wasp is estlat as follows:

The sample is withdrawn from the top layer of the fuel. The number of samples 1-2 ml of Sample is placed in the form of a drop on a glass slide. Further actions depend on the viscosity of the fuel. If the fuel has a high viscosity, glass slide before applying a drop of oil heated to 50-60°With, put a drop of fuel and served quickly cover glass. If the viscosity of the fuel is low, the sample is prepared without heating the glass. For analysis prepare 3 preparation of fuel. In all cases, the analytical sample is prepared immediately prior to testing.

The mixture is placed on the object table of the optical microscope in transmitted light. The microscope is equipped with the analyzer, polarizer and the device phase contrast. The setup diagram is shown in figure 1 and algorithm analysis in figure 2.

The results of determination accept:

1. A histogram of the distribution of water droplets in the fuel volume

2. The average droplet size

3. Standard deviation

Prepare at least 3 of the preparation of the same sample. The number of recorded objects are not less than 10000, which is sufficient to obtain reproducible results point method of analysis. For the final result to determine the arithmetic mean of 3 parallel measurements, provided they are positive statistical test is about the Fisher test.

Example 1

Qualitative analysis of emulsion fuels.

As objects selected 2 samples of emulsion fuels: 1 sample obtained from oil and 30% water in a conventional mixer, 2 - fuel from the fuel oil with 30% of the water received in the rotary mechanical disperser.

Analysis of images obtained by imaging drugs (figure 3), allows to establish that the emulsion 1 heterogeneous, contains water droplets large and medium sizes. Emulsion 2 homogeneous and contains no gaps and large drops. Determination of water content in the surface layer of the fuel during the day showed that emulsion 1 is unstable, the water content in the surface layer decreases. The water content in the fuel 2 remains constant during the day. During the day emulsion 1 splits, and emulsion 2 remains stable.

Example 2

Definition of dispersion of the fuel during storage

Fuel is drawn from fuel oil with 20% water. Analyzed the changes in dispersion of the fuel during storage for 10 days. Qualitative analysis of emulsions as freshly prepared and after storage, indicating their high homogeneity and the absence of elements of the bundle.

The results of the quantitative analysis are summarized in table 1. The distribution pattern of water droplets in size for all the studied emulsions (figure 4) is the same and has a distinct maximum (5-10 μm). P and stored for 1 day emulsion become more homogeneous (narrows the distribution of droplet sizes), the average droplet size not changed significantly, reduces the content of large droplets (>10 μm) and increases the amount of drops with dimensions of 1.6-5 and 5-10 microns.

Longer storage (10 days) leads to a slight increase in average droplet size and partial redistribution of smaller droplets (1.6 to 5 mm) in a drop of 5-10 microns.

Thus, the proposed method allows you to quickly and accurately analyzes VTE in the moment, or after a specified retention period.



Table 1

Statistical data on the composition of the emulsions during storage
SampleStatistical data on the composition of emulsions
DminmcmDmaxmcmDcfmcmSKON
Freshly prepared emulsion1,6383,41,9916700
After 1 day1,6263,71,97to 16,460
After 10 days1,6384,12,1214165
Dmin, μm is the minimum droplet size

Dmax, the km - the maximum droplet size

Dcp, micron average size drops

RMSE is the root mean square deviation

N - number of objects

1. The method for determining the dispersion of emulsion fuels, including direct visualization of the image, characterized in that the direct visualization of the image forming microscopic observation with further computer processing and evaluation of the quality of the emulsion by the histogram distribution of water droplets in the fuel volume, the average value of the droplet size and the RMS deviation of the results.

2. The method according to claim 1, characterized in that the viscosity of the fuel sample is heated to 50-60°C.



 

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