The method of determining lower alkylamines followed
(57) Abstract:Use: analytical chemistry control content lower alkylamines followed in the environment. The inventive method comprises preparing an aqueous solution of the sample, the processing of aqueous extraction-alleluya mixture, in which a mixture of 0.5 to about 4. % solution of dichloroacetylene in an inert organic solvent, in the presence of a solution of a carbonate of an alkali metal concentration of 0.5 to 2 mol/L. table 2. The invention relates to analytical chemistry and can be used to control volatile alkylamines followed in the environment.There is a method of quantitative determination of volatile amines by transferring them from solution into the gas phase in the form of free bases in a sealed vessel when interacting with an excess of alkali, followed by gazohromatografirovaniem gas phase  .A drawback of the analysis of amines in the form of reason is the low accuracy of determination due to adsorption losses of reactive amines on the contacting surfaces of the vessel and device for vapor dosing, evaporator and sorbent XP is by gas chromatography determination of primary and secondary amines in the form of pentafluorobenzene derivatives  , which is the conversion of amines into their derivatives with simultaneous extraction of the obtained amino derivatives by treatment with an aqueous solution of the sample for 10 min extraction-alleluya mixture followed by gas chromatography of the extract amino derivatives.The disadvantage of this method is the low performance analysis.The aim of the invention is to increase productivity analysis.The aim is achieved in that in the method of determining lower alkylamines followed by preparing an aqueous solution of amino, processing the obtained aqueous extraction-alleluya mixture in the presence of a carbonate of an alkali metal and gazohromatografirovaniem obtained extract amino derivatives, the extraction reaction of acylation is carried out with the use of a solution of a carbonate of an alkali metal concentration of 0.5-2 mol/l, and as extraction-alleluya use a mixture solution of dichloroacetylene in an inert organic solvent in the following ratio of components, about. % : dichloroacetylene 0.5 to 4; organic solvent - rest.Use as extracts is the rate of component, and the proposed content of the carbonate of the alkali metal in the aqueous phase provides significant productivity analysis due to the higher reactivity of the proposed mixture under conditions for the analytical determination of micro-quantities of the investigated substances.When the content of the carbonate of the alkali metal in the aqueous phase below 0.5 mol/l is sharply reduced the output of one of the lower alkylamines followed - methylamine, which leads to a decrease in the sensitivity analysis (table. 1), the upper bound of the range (2 mol/l) determined from the properties of solubility of Na2CO3in the water. The proposed ratio of components extraction-alleluya mixture is also associated with conditions to ensure the maximum output of the analyzed compounds. When the content of dichloroacetylene in an organic solvent is less than 0.5. % or more than about 4. % decreases the output of most of the analyzed compounds (table. 2).P R I m e R 1. To 1 ml of a mixture of hydrochloride amines 0.5% sulfuric acid containing 4.0 µg of methylamine (MA), 0.8 µg dimethylamine (DMA), 4 g of ethylamine (EA) and 1.0 μg of diethylamine (deja), add 1 ml of a solution of Na2CO3a concentration of 1 mol/l and 1 ml of freshly prepared allerease, the organic layer is separated and 2 µl of toluene extract is injected into the chromatograph evaporator Color-100". Chromatographic analysis is performed on a glass column (0.3 x 300 cm), filled with sorbent Chromatin-super with 15% PEG-20 M (0.2 to 0.25 mm) at a temperature of column 170aboutC. the results of the analysis of the content of the analyzed components amounted to 4.0 µg MA (100% ), of 0.79 ág DMA (99% ), and 3.8 µg EA (95% ), of 0.96 ág deja (96% ).P R I m m e R 2. To 1 ml of a mixture of hydrochloride amines 0.5% sulfuric acid containing 0.4 µg MA, 0.08 µg DMA, 0.4 µ g EA and 0.1 µg deja add 1 ml of 1 M Na2CO3and 1 ml of freshly prepared alleluya mixture (0.5% solution dichloroacetylene in toluene). Further processing and chromatographic analysis carried out analogously to example 1. The results of the analysis are found to be 0.4 µg MA (100% ), 0,079 µg DMA (99% ), of 0.42 µg EA (105% ) and 0,091 µg deja(91% ). (56) 1. USSR author's certificate N 1051422, CL G 01 N 30/00, 1983.2. Ripley B. D. et al. Gas chromatographic determination of Primary and Secundary Amines as Pentafloorbenzamide Derivates. - J. Assoc. off. Anal. Chem. 1982, v. 65, N 2, p. 1066-1072. The METHOD of DETERMINING LOWER alkylamines followed by preparing an aqueous solution of the sample, processing aqueous extraction-alleluya mixture in the presence of carbonate Sch the purpose of improving performance, the concentration of the solution of the carbonate of an alkali metal chosen from 0.5 to 2 mol/l, and as extraction-alleluya use a mixture solution of dichloroacetylene in an inert organic solvent in the following ratio of components, about. % :
Dichloroacetylene 0,5 - 4
Organic solvent Else
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for synthesis of ester perfluorinated derivative by using a chemical reaction. This reaction represents the fluorination reaction of the parent compound as a raw, the reaction of chemical conversion of fragment of ester perfluorinated derivative to yield another ester perfluorinated derivative or the interaction reaction of carboxylic acid with alcohol under condition that at least one or reagent, i. e. carboxylic acid or alcohol, represents a perfluorinated compound wherein indicated perfluorinated derivative of ester represents a compound comprising a fragment of the formula (1):
with a boiling point 400°C, not above. The reaction time for carrying out abovementioned chemical reaction is sufficient to provide the required yield of ester perfluorinated derivative and wherein this yield of ester perfluorinated compound is determined by the gas chromatography method by using a nonpolar column. Also, invention relates to a method for pyrolysis of ester perfluorinated derivative with a boiling point 400°C, not above, to yield the dissociation product wherein this product represents a derivative of acyl fluoride or ketone and wherein pyrolysis time is sufficient to provide the required degree of conversion of ester perfluorinated derivative and wherein the indicated conversion degree of ester perfluorinated derivative is determined by gas chromatography method by using a nonpolar column. Also, invention relates to a method for analysis of ester perfluorinated derivative with a boiling point 400°C, not above, that involves analysis of ester perfluorinated derivative in a sample containing ester perfluorinated derivative by gas chromatography method by using a nonpolar column wherein ester perfluorinated derivative represents compound comprising a fragment of above given formula (1).
EFFECT: improved method of synthesis.
8 cl, 1 dwg, 2 ex
FIELD: instrument engineering.
SUBSTANCE: device for generating flow of vapor-gas mixture with preset concentration of vapor has vessel partially filled with fluid, second vessel provided with branch pipes for supply and removal of gas, and vapors of fluid pipeline-leak. One of vessels is connected with gas discharge forcer; fluid vapors pipeline-leak connects both vessels. Vessel, partially filled with fluid, is mounted inside second vessel. Pipeline-line, connecting both vessels, is totally placed inside second vessel. Device is also provided with additional discharge forcer for adjusting concentration of fluid vapor in second vessel. Granulated filler is introduced into vessel partially filled with fluid. Device is also provided with gas analyzer for providing gas concentration in space of second vessel.
EFFECT: higher precision of keeping of preset concentration of vapor; improved efficiency of vapor concentration control and adjustment.
FIELD: instrument engineering.
SUBSTANCE: invention is designed for calibrating gas analyser detectors, according to which there prepared is calibration substance solution with concentration A=By/k (%) as per Henry constant value k (mg/m %) at calibration temperature and as per the specified value of calibration substance mass concentration in calibration steam/gas mixture By (mg/m). After the solution has been introduced into the vessel in quantity enough for fully saturated equilibrium calibration steam/gas mixture to appear above the solution surface, the sensor calibration is carried out by means of mixture; at that, mixture concentration is changed by means of direct proportional change of solution concentration by diluting concentrated reference solution of calibration substance with analytical accuracy up to the specified concentration value A (%). There also proposed is the device for realising this method, which includes a solution point for preparing calibration solution with analytical accuracy, vessel with thermostatic device for obtaining steam/gas mixture with constant concentration corresponding to Henry law; at that, solution point includes graduated dose metre, graduated diluter, mixer with a reducer, capacity with solvent, and reference container with reference solution, which is stabilised with a gate valve meant for multiple use of container, and vessel with thermostatic device consists of thermometre and heat-insulating cover plate with an inlet branch pipe containing a normally closed return valve and a pusher for valve opening.
EFFECT: decrease of calibration substance losses; accuracy and reproducibility of metrological performance, and meeting requirements of industrial and ecological safety.
6 cl, 2 dwg
SUBSTANCE: vapour-gas mixture source has a mixer which has connecting pieces for inlet and outlet of the vapour-gas mixture. The vapour-gas mixture source also has a diffusion pipe filled with working fluid and an auxiliary pipe designed for filling the diffusion pipe with working fluid. Part of the diffusion pipe is filled with substance which retains the working fluid. The level of working fluid in the auxiliary pipe is lower than the level of substance in the diffusion pipe. The substance which retains the working fluid used can be sand, granular material with particle size between 10 and 10000 mcm, porous substances, e.g. ceramic metal etc.
EFFECT: more accurate measurement and maintenance of concentration of the vapour-gas mixture coming out of the source, provision for constant diffusion flow of vapour of working fluid into the mixer.
11 cl, 2 dwg
SUBSTANCE: invention relates to laboratory methods of analysis and deals with method of quantitative determination of manganese, lead and nickel in bile by method of atomic-absorption analysis with atomisation in flame. Essence of method lies in the following: sampling of bile is carried out during duodenal probing, after that it is frozen, and unfrozen at room temperature, homogenisation of bile by mixing being performed already at partial soft unfreezing. After that, sampling of homogenised bile is carried out for preparation for analysis, concentrated nitric acid is introduced into it with volume ratio 1:1, mixture is kept at room temperature, then heated and further mixture is kept for not less than 2.5 hours at room temperature. In order to obtain analyte, to obtained mixture added is concentrated hydrogen peroxide in volume ratio 1:1 to volume of bile sample volume, analyte is heated, after that cooled to room temperature. After that by method of atomic-absorption spectrometry, using graduated diagram, quantitative content of particular type of metal: manganese, lead and nickel is determined in analyte.
EFFECT: invention allows increasing accuracy of quantitative determination of manganese, lead and nickel in bile.
FIELD: engines and pumps.
SUBSTANCE: proposed method is based on application of simplified model of intake of admixtures into cabin which allows for only oil decomposition products in gas turbine engine. Major portion of air samples, 95-97%, required for identification and quantitative determination of oil decomposition products, is sampled on surface from device simulating oil decomposition conditions including air temperature and pressure at point of sampling from engine compressor, and oil stay time in hot zone.
EFFECT: decreased time of in-flight experiments and that of surface analysis of samples.
1 cl, 1 ex, 1 tbl, 1 dwg
SUBSTANCE: invention relates to analytical chemistry, particularly to methods of determining benzoic acid, and describes a method for quantitative determination of benzoic acid from a methyl derivative thereof - methyl ether in aqueous matrices with determination sensitivity of 5.0·10-5 mg/cm3 with determination error of not more than 25%. The method is characterised by that quantitative determination of benzoic acid is carried out using a chromatographic method with flame-ionisation detection and includes the following steps: extraction concentration of an analyte with benzene in water samples acidified with 25% sulphuric acid solution to pH 1-3 while adding sodium chloride until a saturated solution is obtained, conducting a benzoic acid methylation reaction with diazomethane to obtain a derivative - methyl ether of benzoic acid and determining the formed methyl ether of benzoic acid by a chromatographic method with flame-ionisation detection.
EFFECT: method provides high sensitivity, selectivity and easy implementation during quantitative determination of benzoic acid in aqueous media and enables use thereof in practice in factory analytical laboratories, central laboratories of chemical companies and chemical-toxicology laboratories.
1 ex, 3 tbl
SUBSTANCE: device for preparing control gas mixtures comprises a gas mixer, at least one channel for supplying target gas to the gas mixer, at least two channels for supplying the diluent gas to the gas mixer, and the channel for output of the gas mixture from the gas mixer. And in each channel for supplying gas to the gas mixer the mass flow controller of gas and a solenoid valve are mounted successively, at least in one channel for supplying the diluent gas to the gas mixer the gas humidifier and the solenoid valve are mounted successively. In each of the channels equipped with the gas humidifier at least one bypass pipeline with the additional solenoid valve is mounted. and the output of the gas flow controller of this channel is connected to the input of the additional pipeline which output is connected to the output of the last solenoid valve, and at the input of the target gas and the input of the diluent gas at least one filter is mounted, which outputs are connected to the inputs of manually operated valves.
EFFECT: possibility of operational automated obtaining the dry or moist gas mixture, and reliable obtaining of the given values of concentrations of gas mixtures at the output of the device.
SUBSTANCE: each blood sample is analysed twice. A fresh blood sample is centrifuged at 2,000 rpm for 5 min. The samples are separated in plasma fractions and formed elements. A solid-phase plasma extraction is performed by sequential passing of 100% acetonitrile, plasma, distilled water, 50% acetonitrile solution under vacuum through a cartridge with Oasis HLB 3 cc sorbent. The cartridge with the sorbent is dried under vacuum, and 100% methylene chloride is passed through the sorbent. An aliquot portion of the produced extract is chromatographed. Producing the extract of formed elements is ensured by dispersed solid-phase extraction: by adding 100% acetonitrile thereto and agitating intensively. That is followed by adding a number of QuECHeRS salts for extraction, agitating, centrifuging for 10 minutes at 2,000 rpm; that is accompanying by forming 3 layers; an upper layer is transferred to another test tube, which contains a number of QuECHeRS salts for purification; the layers are centrifuged at 2,000 rpm; the upper layer is sampled. Plasma and formed elements extracts are analysed by Agilent 1200 liquid chromatograph with a fluorimetric detector on Zorbax column 50 mm long and having an inner diameter of 4.6 mm with Eclipse PAH C18 sorbent at column temperature 27°C; a movable phase is presented by mixed acetonitrile and water at flow rate 1.5 cm3/min and optimising elution in the gradient mode (supplying the movable phase of 60 vl % to 68 vl % of acetonitrile for 1 min, increasing 60 vl % to 68 vl % of acetonitrile for 3 min, increasing 68 vl % to 70 vl % for 0.5 min, increasing acetonitrile 70 vl % to 90 vl % for 1.5 min, increasing acetonitrile 90 vl % to 100 vl % for 4.5 min, supplying 100% acetonitrile for 1.5 min, reducing acetonitrile to 60 vl % and supplying 60% acetonitrile for 4 min to balance the column). An excitation wavelength of the fluorimetric detector makes 265 nm, and an emission wavelength makes 412 nm. A calibration chart is used to quantify benz(a)pyrene in plasma and formed elements separately, while the results are summed up.
EFFECT: invention provides high sensitivity of the method and ensures selectivity in a combination with its accessibility for routine analyses.
3 cl, 6 tbl, 1 ex
SUBSTANCE: invention relates to medicine, namely to experimental pharmacology, and can be used for quantitative determination of carnosine in tissues and physiological liquids. Determination of carnosine in biological materials is carried out by highly-selective mass spectrometry method using electrospray ionization. At that, deproteinization of blood plasma should be preliminary carried out using 10 % aqueous solution of trichloroacetic acid. Then aliquot of internal standard solution of L-alanyl-carnosine is added to deproteinizated sample. And separation of extraction products is performed at reversed-phase chromatographic column 4.6×150 mm with temperature separation of 35 °C and eluent feed rate 0.7 ml/min. Used eluent is 10 mM ammonium acetate, acidified with glacial acetic acid to pH 3.7, and mixture of acetonitrile with 10 mM ammonium acetate in ratio of 90:10, taken in ratio of 10:90, respectively. Detection of carnosine is carried out by four child ions with m/z 110.0, 156.1, 180.0, 210.1, formed as result of molecular ion carnosine disintegration with m/z 227.1. Concentration of carnosine is calculated by chromatographic peak carnosine area relation to L-alanyl-carnosine internal standard peak area.
EFFECT: invention provides highly selective and sensitive gas chromatography/mass-spectrometric method for quantitative determination of carnosine in biological substrates.
1 cl, 6 dwg, 2 tbl, 1 ex