Method of extraction of the volatile substances from the water medium

FIELD: ecology; hydrochemistry; analytical chemistry; methods of extraction of the volatile organic substances from the water medium.

SUBSTANCE: the invention is pertaining to the field of ecology, hydrochemistry, analytical chemistry and may be used for extraction of the organic compounds from the water mediums, in particular, from the mineral waters including sulfide mineral waters. For realization of the method of extraction of the volatile organic substances from the water medium into the organic dissolvent conduct the joint condensation of the extracted substance produced as a result of distillery and the vapor of the dissolvent. For production of the joint condensate they gate the vapor-shaped dissolvent through the water sample or preliminary add it into the water sample with the subsequent distillation. The organic dissolvent is chosen from the following row: ethanol, acetonitrile, acetone, hexane. The method ensures the single-stage extraction of the dissolved organic substances into the dissolvents, the unlimited their mixing with the water, reduction of the thermal action on the researched sample, the increase of the extraction ratio.

EFFECT: the invention ensures the single-stage extraction of the dissolved organic substances into the dissolvents, their unlimited mixing with the water, the reduced the thermal action on the researched sample, the increased extraction ratio.

2 cl, 1 tbl, 5 ex

 

The invention relates to hydrochemistry, analytical chemistry, ecology and can be used to select, research the dissolved natural and man-made organic substances in water objects, including mineral waters.

The known method [1], where volatile organic compounds extracted from water samples by steam distillation. The two options are: the steam distillation are either directly from the flask with the sample water through boiling; or to produce steam and feed it to the sample used the steam generator.

However, this method has several disadvantages:

- analyzed water sample during the procedure, it is necessary to heat at +105-110°To avoid condensation of water vapor in the volume of the sample;

for hydrophilic, water soluble substances (low molecular weight fatty acids, phenols, amines and others) requires a considerable excess of the volume of distillate in relation to the original sample (5-10 times), or chemical modification of the sample (the change in pH and the like) before the distillation procedure that may cause undesired chemical transformations in the system.

The technical result is the improvement of economic indicators, with the exception of mnogostadiinost, a significant reduction of thermal effects on the investigated sample with a simultaneous increase in the degree of extraction, the possibility of the regulation of the efficiency of extraction by varying the polarity of the used organic solvent.

This is achieved by the fact that organic matter is extracted from water into an organic solvent (for example, ethanol, acetonitrile, acetone, carbon tetrachloride, diethyl ether, hexane, etc.) by cocondensation as the result of steam distillation of the solvent having a boiling point below the boiling point of the sample.

The method is carried out in two variants as follows.

Option 1:

The analyzed water sample volume of 300 cm3placed in a glass conical flask with rack type KNX capacity of 750 cm3. Add 80 cm3organic solvent (ethanol, acetonitrile, acetone, carbon tetrachloride and others)make glass capillaries to promote vaporization. The flask with the mixture is placed on a heater, electric stove. Collect installation for the distillation of glass is attached to the flask nozzle type H2 CS 29/32-14/23 GOST 9425-71 with thermometer up to 150°, laboratory refrigerator type HPT 400 14/23 GOST 9499-70 and alonger type AI CS 14/23-60 GOST 9425-71. The contents of the flask is brought to a boil. The Stripping end, when the condensation temperature on thermometer reaches 90-92°C. the resulting distillate contains extracted from water with organic substances.

Option 2:

Collect the installation of glass for steam distillation [1], pouring in a steam generator, an organic solvent (ethane is l, acetonitrile, acetone, carbon tetrachloride, diethyl ether, hexane and other). In a flask with a capacity of 1000 cm3for shepherd fluid place a sample of the investigated water volume 700-750 cm3. The temperature of the water bath is adjusted to 90-92°C. Carry out the distillation, directing the solvent vapor from the steam generator in water volume. Collect the condensate solvent in the amount of 50-70 cm3or more (to increase the degree of extraction), containing extracted from water with organic substances.

Example 1.

In a flask shepherd liquid was placed 700 g of a standard solution of propionic acid in distilled water with a mass concentration of 2.8 ág/g In the steam generator poured 350 cm3fresh ethyl alcohol (96°). Carried out the steam distillation of ethanol for option 2 (see above). The mass of the obtained distillate was 43.8, by gas chromatography on the chromatograph M-3700 detector ionization in the flame found that the concentration of propionic acid in cocondensate equal to 23.7 ág/g Thus, in the model experiment, the degree of extraction of propionic acid from aqueous solution was 23,7×43,8:2,8:700×100%=53%.

Example 2.

In a flask shepherd liquid was placed 750 g of sulfide mineral water scvt (Matsesta, Sochi). In the steam generator poured 350 cm3acetonitrile mark "x is mikeski clean. Made the steam distillation of acetonitrile under option 2 (see above). The mass of the obtained cocondensate amounted to 44.5, the Method converts high-performance liquid chromatography microcolumn chromatograph "milikhrom-4" when multi-wave detection (220, 230, 240, 250 and 270 nm) detected several unidentified chemical compounds. As eluent used 80% solution of acetonitrile in water. On column length of 80 mm, an inner diameter of 2 mm, phase C-18 (5 μm) for 18°With the retention volumes of the substances were, respectively, 119, 157, 183, 263 and 1556 µl.

Example 3.

The sample solution of ortho - and para-cresol in water volume of 300 cm3at concentrations 66,3 and 91.5 ág/cm3accordingly placed in a glass conical flask with rack type KNX capacity of 750 cm3. Add 10 cm3ethanol, making glass capillaries to promote vaporization. The flask with the mixture is placed on a heater, electric stove. Collect installation for the distillation of glass is attached to the flask nozzle type H2 CS 29/32-14/23 GOST 9425-71 with thermometer up to 150°, laboratory refrigerator type HPT 400 14/23 GOST 9499-70 and alonger type AI CS 14/23-60 GOST 9425-71. The contents of the flask is brought to boiling by steam distillation of ethanol for option 1 (see above). The Stripping end, when the condensation temperature on those whom mometer reaches 95-97° C. the resulting distillate mass 13,62 g (density 0,9527 g/cm3contains extracted from water organic matter: ortho-cresol 380,22 µg/cm3and para-cresol 215,91 µg/cm3. The degree of extraction of ortho-cresol was 380,22×13,62×100/0,9527×66,3×300=27,3%, and para-cresol, respectively 215,91×13,62×100/0,9527×91,5×300=11.2 per cent.

Example 4.

To study and compare the extracting ability of various organic liquids for the proposed method of extraction of target components used carbon tetrachloride. Unlike ethanol and acetonitrile he is a non-polar solvent.

The analyzed sample solution of organic acids in water by volume 302 cm3placed in a glass conical flask with rack type KNX capacity of 750 cm3. Acids: acetic 162,3 µg/cm3, propionic - 144,1 µg/cm3and oil - RUB 145.1 mg/cm3. Add 20 cm3carbon tetrachloride, make glass capillaries to promote vaporization. Organic solvent, without mixing with water, is under a layer of an aqueous solution, because its density is higher than water. The flask with the sample placed on the heater - electric tile. Collect installation for the distillation of glass is attached to the flask nozzle type H2 CS 29/32-14/23 GOST 9425-71 with thermome the rum to 150° With laboratory refrigerator type HPT 400 14/23 GOST 9499-70 and alonger type AI CS 14/23-60 GOST 9425-71. The contents of the flask is brought to a boil - 65-67°by steam distillation of carbon tetrachloride for option 1 (see above). Pair of carbon tetrachloride in the form of bubbles penetrate the layer of water and is condensed in the refrigerator. The Stripping end, when the condensation temperature on thermometer begins to rise sharply. The obtained distillate mass 31,65 g (density 1,595 g/cm3contains butyric acid at a concentration of 8.8 mg/cm3, acetic and propionic acids were not detected (sensitivity to GC-analysis was not worse than 0.5 ág/cm3). The degree of extraction of butyric acid 8,8×31,65×100/1,595×RUB 145.1×302=0,4%.

Example 5.

Order direct demonstration of the advantages of the proposed method over the closest analogue in the efficiency of allocation of organic substances from water studied the content of carboxylic acids With2- C6in the gas-vapor phase by heating the sample with pre-addition of organic solvent in the volume of the sample and without it.

The analyzed sample solution of organic acids in water is prepared in a two-dimensional tubes with a capacity of 25 cm3. In one of the flasks while cooking add 95%(vol.) ethanol in the amount of 0.85 ml penicillin bottles 15 momaday aliquots of 5 ml of the prepared mixtures, sealed with a rubber stopper. For tight fixing of the tube is fixed in a special metal clip container used Protasova analysis. Then put exactly 5 minutes (stopwatch) each vial in turn on a boiling water bath (100°). Take 1 ml of the vapor phase through a rubber tube piercing medical syringe and conducted her research using gas chromatography chromatograph M-3700(DIP) with column 15% Carbowax 20M Chromaton AW-DMCS (0,315-0,400), L=1.0 m, d=4 mm. The results of the determination of the concentration of acids is presented in table 1

480±36,6
Table 1.

The results of a comparative study of the vapor phase above the aqueous solution of carboxylic acid at 100°C.
ExperienceThe content of organic acids in the gas-vapor phase, mg/ml
C2With3With4With5With6
An aqueous solution of carboxylic acids70±17,4150±13,8190±16,8260±29,9320±34,0
An aqueous solution of carboxylic acids when added to a sample of 3% ethanol114±6,0280±and 31.7340±44,9590±52,5
Note: the Content of organic acids in both experiments was

acetic acid (C2) 324 m kg/ml

- propionic (C3) 368 µg/ml

- oil (C4) 287 µg/ml

- walerianowo (C5) 304 µg/ml

- nylon (C6) 305 mg/ml

Thus, a preliminary introduction to the volume of the aqueous solution of aliphatic acid With2-C6ethanol in the amount of 3% of the volume of the sample leads to the increase of their content in the gas-vapor phase when heated to 100°With on average 80%.

The proposed method allows to:

- perform a direct one-step extraction of dissolved organic substances in solvents, infinitely miscible with water, ethanol, acetonitrile, acetone and the like);

- significantly reduce the effects of temperature (15-25° (C) in the investigated sample in comparison with the traditional method of steam distillation;

- reduce material, energy and labor costs;

- exclude prior chemical modification of the water sample, if the target organic substances are hydrophilic chemical compounds;

- to increase the degree of extraction of the target organic substances from water;

- to regulate the efficiency of extraction of target components by ranged the project polarity organic solvent.

Bibliography

1. Stepin D. Technology laboratory experiment in chemistry: Textbook. manual for schools. M.: Chemistry, 1999, p.á305-314.

1. The method of extracting volatile organic compounds from the water environment, including the release of dissolved organic substances from water by distillation the distillation with steam, wherein the steam generator or the water injected organic solvent for cocondensate vapor of the solvent with the extracted substance.

2. The method according to claim 1, characterized in that the organic solvent is selected from a range of ethanol, acetonitrile, acetone, hexane.



 

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