Method of determining time of contact between diesel fuel and water

FIELD: chemistry.

SUBSTANCE: method involves taking a sample, concentration of impurities, chromatographic analysis with separation of the concentrate on a capillary column and mass-selective detection while raising temperature from 35°C to 280°C, isolation of tridecane and 1-methylnaphthalene as reference compounds on the chromatogram, calculation of their concentration ratio in the sample and calculation of the time of contact between diesel fuel and water using the formula: x=0.42·y-1.8, where x is the time of contact between diesel fuel and water, h; y=Stridecane/Smethylnaphthalene; Stridecane and Smethylnaphthalene are area of peaks of tridecane and 1-methylnaphthalene on reconstructed chromatograms on selective ions with mass to charge ratio of 85 for tridecane and 145 for 1-methylnaphthalene, which correspond to concentrations of given compounds in the sample.

EFFECT: simple and reliable method with high information content.

1 ex, 1 tbl


The invention relates to the field of environmental and analytical chemistry, in particular to a method for determining the time of contact of diesel fuels with water.

In accordance with the list of certified and temporarily admitted to the use of methods of determining the content of oil products in natural and waste waters is recommended to use the following methods of analytical control: IR - and UV-spektrofotometricheskie, weight, fluorescent and chromatographic methods.

Current state standard GOST R 51797-2001 (Method for detecting the content of oil products) is IR-spectrometric method to determine the concentration of emulsified and dissolved aliphatic, alicyclic and aromatic hydrocarbons (petroleum products) in water. The method allows to determine the total oil content in the water, but not to establish the designated petroleum products (gasoline, kerosene, diesel fuel, etc) and the time of their contact with water.

The method of column chromatography with UV-spectrophotometric end is based on the absorption of aromatic hydrocarbons in the UV region of the spectrum. They make up 30% of the amount of petroleum hydrocarbons, and their share may increase substantially as the relatively rapid consumption by microorganisms aliphatic carbohydrate is childbirth. Thus, when using this method increases the accuracy of the TM when identifying the chronic pollution. (Golubeva M.L. Spectrophotometric determination of oil and oil products in the water. Sanitary-chemical control in the field of protection of water bodies. - M.: Medicine, 1964. P.142-146).

The method of column chromatography with gravimetric (weight) ending is often used in laboratories for the analysis of natural waters and industrial effluents. However, using the gravimetric method can be difficult due to the loss of volatile components of the NP in the sample preparation. Also significant interference to the use of the method create halogenated hydrocarbons included in the NP (PNDF 14.1:7.116-97. The method of measurement of mass concentration of oil products in samples of natural and treated wastewater by the method of column chromatography with a gravimetric finish. M, 1997).

In the recommended techniques (Definition of index of liquid petroleum products in the water. ISO 9377-2:2000 // Drinking water. 2001. No. 5. P.17-21; Korenman YA, žilina SURDS, V. Fokin. Chromatographic determination of oil products in natural and mineral waters // Chemistry and technology of water. 2005. V.27. No. 2. Pp.163-172) described detection methods, chromatographic identification of petroleum products in natural and mineral waters. Meth is water enables you to install a high quality accessory (fractional composition of petroleum products by the appearance of the chromatograms ("fingerprints"). To reliably determine variety of facilities recommended to create a working Atlas the most likely contaminants. This suggests a comparison with known standards (samples) of petroleum products and leads to difficulties in their primary identification in the operational monitoring of water. This method is applicable when the dispersed, dissolved portion of the oil in water similar in composition to the original, which is possible only with fresh dirt, when oil products are not susceptible to degradation.

Fluorescent method is based on measuring fluorescence of polycyclic aromatic hydrocarbons included in the NP. Methods based on absorption of UV and fluorescent radiation, characterized only aromatic, mainly polycyclic structure, and the absorption coefficients of different aromatic structures can greatly vary. In this regard, the results obtained depend not only on quantity but also on the composition of aromatic compounds, which in turn may differ from the NP of different brands (Drugov US, Rodin A.A. Ecological analysis in oil and oil products. Practical guide. S.-Pb.: Anatoly, 2000, 250 C.)

The known method (Patent RF №2152613, 10.07.2000, Bulletin No. 19) detection of petroleum products in aqueous solutions by the method of LUMIN santoy spectroscopy by assessing the accumulation of oil on aquatic blue-violet glow of fat inclusions crustaceans. The method does not allow to determine the composition of the oil and does not differentiate the process of accumulation of petroleum aquatic organisms due to contact time or increase their concentration in the water.

These methods do not answer the question about the sources of water pollution NP, duration of contact of pollutants with water, when possible secondary pollution of water sources due to the biodegradation of the contaminant in the water. (Yasser Moustafa M. Oriental. Assessment of pollution of waters by oil. J.Chern. 2004. 20, No. 2, s.219-226) in the study of water samples taken at different distances from the Strait of oil, it is noted that with increasing distance from the Strait of reduced total content of the NP in the water and increases the content of polar compounds, which are products of decomposition of the original components. However, the authors are not aware of the use of the obtained data to determine the time of contact of the NP with water.

(Tzing S.H., Chang J.Y., Ghule, A., Chang J.J., Lo C., Ling, Y.C. Simple and fast method of identifying the source of spilled oil using an electronic nose": (Department of Chemistry, National Tsing Hua University, Hsinchu 300, Taiwan). Rapid Commun. Mass Spectrom 2003. 17, No. 16, 1873-1880) offers a simple and fast method of identifying the source of spilled oil using two types of "electronic nose", acting on the basis of different principles. For PR the constituent multicomponent analysis recommended multi-sensor device with a resolution in space, allowing on the basis of the graphic image to set the source, and quick time-chromatography-mass spectral analysis of the composition of the sample. Because we are talking about multi-component mixtures of compounds of different nature and biochemical properties, the results are unlikely to be unambiguous and applicable to any kind of NP.

Closest to the invention to the technical essence and the achieved result is the method of determining the time of contact of gasoline with water (the Method for determining the time of contact of gasoline with water (authors Gordienko, B.C., Kantor LI, Tsybysheva L.G. and others, patent No. 2324930, application No. 2006128560). In this way the duration of the gasoline in the water is determined by the ratio of the concentration of the most volatile and less volatile components (frames) in a given time. As reference points selected characteristic and is constantly present in gasoline aromatic hydrocarbons, toluene and 1,2,4-trimethylbenzene (1,2,4-TMB). Selected frames belong to the same class of organic compounds of similar chemical properties and resistance to biodegradation, easily dispersed in water and therefore longer hold it. Changes in the concentration of frames in continuous contact with gasoline water only due to their volatility. The timing of contact of the fuel with the ode is made on a pre-identified dependency relationships concentrations (response detector) frames from time gasoline in the water in these climatic conditions. Selective determination of these compounds in water is carried out after pre-concentration of volatile impurities in the vapor phase of water and chromatographic separation on columns with a highly polar stationary phase. The method is relatively simple, but is applicable only to determine in water volatile fractions of NP (gasoline).

Thus, in the literature not found a simple and reliable method for determining the time of contact of diesel fuels with water.

Diesel fuel (DF) is a mixture of hydrocarbons (HC), wikipaedia in the range of 240-360°C and a density of 0.82 is 0.86 g/cm3. The main components of the DT - alkanes, isoalkanes, alkenes, cycloalkanes, aromatic hydrocarbons and PAHs.

The authors propose a method for determining the time of contact of diesel fuels with water.

The invention consists in the selective determination of the content of one of the most characteristic and is constantly present in diesel fuels limit HC - tridecane (13) and one of PAHs 1 - methylnaphthalene (frames) and determining the relationships of their concentrations. The timing of contact of the fuel with water are made on a pre-identified according to the ratio of frames from the time of diesel fuel in the water.

Selected compounds differ in physico-chemical properties and the ability to biodegra the emission in water. Changes in the concentration of tridecane in the water due to biological decomposition occurs very quickly, compared to 1-methylnaphthalene, because alkanes are more available for microbial oxidation than aromatic hydrocarbons (Brodsky, Surico L. F., Finkelstein SI, Basmanov BP, Yankevich M.I., Yakovlev V.I., Golovlev L.A. Recycling of oil in soil and water microbial cells. Microbiology. 1995. So 64, No. 3, s-398). Therefore, the rate of change of their concentration in the water in time will be different. This difference of speed of biodegradation of selected compounds of the basis for determining the time of contact with water two varieties DT - winter (DZ) and summer (DL) (see table 1). Quantitative determination of the sample components in the water is conducted by a method GC / MS with prior extraction extraction and concentration of organic impurities from water. The concentration of the reference compounds measured at the reconstructed chromatograms of selective ions. The separation of ions takes place in accordance with the ratio of ion mass to charge (m/z): for tridecane m/z=85, for 1-methylnaphthalene m/z=142.

The concentration of the reference compound (S) in the sample correspond to the squares of their peaks on the chromatogram (S).

Table 1
The contact time, hWithtridecan/S1-Mentaly

The dependence relationship Withtridecan/S1-Mentalyfrom time diesel fuel in the water under the above conditions:



x - contact time diesel fuel with water, including

The obtained dependence is applicable to estimate the time of contact of diesel fuels two varieties of water.

Largest relationship of concentrations (response) frames at a given time (Ctridecan/C1-Mentaly) and installed according to x=0,42·1,8you can estimate the time of contact of diesel fuels of different brands of water, and if this river with a known velocity, the distance from the pollution source.

The proposed method is carried out in the following sequence.

A water sample taken in a glass bowl. The volume of the sample should be not less than 0.5 DM3. Quantitative determination of the sample components in the water is conducted by a method GC / MS with prior extraction preconcentration limited-volatile organic impurities. Identification of the components of the concentrate of impurities was performed using a gas chromatograph HP 6890N and mass-selective detector 5973 inert firm "Agilent". Chromatographic separation was obtained concentrate was carried out on a capillary column HP-5MS (30 m × 0.25 mm × 0.25 μm) when programming thermostat temperature columns from 35°C at a rate of 20°C/min to 60°C and with a speed of 6°C/min to 280°C (10 min), (Tsource=230°C, TCOI=250°C). The method of ionization - electron impact (70 eV). The calculation of the concentration is AI (peak area) of the reference compounds were reconstructed chromatograms of selective ions (for tridecane m/z=85, for 1-methylnaphthalene m/z=142).

The chromatogram of the sample are suggested by the authors of reference compounds, tridecan and 1-methylnaphthalene and calculate the ratio of the response (concentration) of the detector tridecane 1-methylnaphthalene (Ctridecan/C1-Mentaly). The obtained values are used to calculate the contact time of diesel fuel with water previously found dependency


where y=(Ctridecan/S1-Mantalini),

x - contact time diesel fuel with water.

Example 1. Select 0,5 DM3water samples from wells Baimak district and conduct extraction concentration; 0,5 DM3the sample is acidified with 10% hydrochloric acid to pH 2, add 50 g of sodium chloride and 10 cm methylene chloride. Shake for 2 minutes, the Extract dried with sodium sulfate and then concentrated in thermostat to 50 mm3. Concentrate the sample is introduced into the evaporator gas chromatograph and separated on a capillary column HP-5MS (30 m × 0.25 mm × 0.25 μm) when programming thermostat temperature columns from 35°C at a rate of 20°C/min to 60°C and with a speed of 6°C/min to 280°C (10 min), (Tsource=230°C, TCOI=250°C).

On the chromatogram find reference compounds (see table 2).

Table 2
IndexRetention time, minThe peak area, mV·c

Calculated by the chromatogram attitude



As required by the authors according to x=0,42·-1,8

find x=0,42·0,41-1,8,

x=2.1 hours contact time of diesel fuel with water.

In the middle reaches of the river 2.8 km/hour distance to the source of the spill will be 2.8 km/h 2,1 h = 5,9 km

Example No. 2. Select 0,5 DM3water samples R. White and analyzed as in example 1. Get the chromatogram of water sample, which does not find one of the reference compounds. In the absence of one of the frames make a conclusion about the water pollution anthropogenic admixtures another source, not diesel fuel.

The method for determining the time (duration) contact diesel fuels with water, including sampling, the concentration of impurities chromatographic analysis by separation concentrate on capillary column and mass-selective detection with the rise of temperature from 35 to 280°C, the selection to chromate the gram as reference compounds tridecane and 1-methylnaphthalene, calculation relationships of their concentrations in the sample and calculating the time of contact of diesel fuels with water according to the formula:
where x is the time of contact of diesel fuels with water, h;
Stridecanand S1-methylnaphthalenesquare peaks tridecane and 1-methylnaphthalene in the reconstructed chromatograms for selective ions with mass-to-charge 85 for tridecane and 142 for 1-methylnaphthalene, corresponding to the concentrations of these compounds in the sample.


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2 ex, 3 tbl

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2 ex, 3 tbl

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1 ex, 1 tbl

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2 tbl, 2 ex

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2 tbl, 2 ex

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2 tbl, 2 ex

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4 tbl, 3 ex