Method of detecting chloroanilines in aqueous media
SUBSTANCE: chloroanilines are modified into bromine derivatives and extraction concentration and gas-chromatographic detection is carried out. The additional modifier reactant used is trifluoroacetic anhydride in amount of 3-15% of the mass of the extract. Bromine derivatives of chloroanilines are obtained before the extraction concentration step in aqueous medium, in the presence of potassium bromide in amount of 0.5-2.5% of the mass of the water sample.
EFFECT: invention enables to lower the detection limit, increase selectivity of chromatographic separation, reduce the number of steps and duration of the analytical cycle of detecting chloroanilines in water.
3 dwg, 3 tbl, 7 ex
The invention relates to analytical chemistry of organic compounds (concentration and definition) and can be used for sanitary and epidemiological control of drinking waters, water objects that have significance for fisheries, as well as the level of wastewater treatment in various chemical industries.
The closest to the technical nature of the claimed solution is a gas chromatographic method of determining chloraniline [.Schmidt, R.Haas, E. v. Löw, K.Steinbach. Derivatization of aromatic amines with bromine for improved gas chromatographic determination // Chromatographia, - 1998. - Vol.48. No. 5/6. - S-442]. The disadvantages of the prototype are the high detection limits of chloraniline (2-Chloroaniline, 3-Chloroaniline, 4-Chloroaniline, 2,4-dichloroaniline, 2,6-dichloroaniline and 2,4,6-trichloroaniline)associated with inefficient extraction concentration, losses Stripping and evaporation of the organic extract.
The objective of the invention is to develop more effective ways to reduce the detection limit, to increase the selectivity of the chromatographic separation, to reduce the multistage and the analytical cycle definition chloraniline in the water. This is a technical result.
The solution of this problem is achieved in that in the method of determining chloraniline in aquatic environments, including chemical modification of b is aprosodia of chloraniline, extraction preconcentration and gas chromatographic detection, what is new is that as an additional reactant-modifier applied triperoxonane anhydride in the amount of 3-15% by weight of the extract, and bromo derivatives of chloraniline get in front of the stage extraction concentration, in aqueous medium, in the presence of bromide of potassium in an amount of 0.5-2.5% by weight of a water sample.
Getting bromo derivatives of chloraniline in the absence of bromide of potassium is impossible, because in these conditions, molecular bromine is not as pomeroyi agent, and as a strong oxidizing agent, the redox potential of which in the solution reaches 1.1-1.2 C. In the presence of potassium bromide, the potential of an aqueous solution of bromine is reduced to ~0.6 V, which is associated with the formation of ions Br3-[Ksenzenko VI, Stasiewicz DS. Chemistry and technology of bromine, iodine and their compounds. - M.: Chemistry, 1995. - 379 C.]:
Reduced oxidative activity of solutions of bromine in the presence of bromide anions eliminates oxidation of chloraniline, and remaining in the system, molecular bromine, enough for fast and quantitative receipt of bromo derivatives of chloraniline.
Method of determining Chloroaniline in aqueous media includes four stages:
1. Getting bronrott is the breaking of chloraniline (chemical modification, 1 stage) in the water when interacting with bromine in the presence of bromide of potassium. When bromirovanii bromine atoms replace hydrogen atoms of the aromatic nucleus at positions 2, 4 and 6 (NH2band - Deputy of the first kind), not occupied by chlorine atoms. Thus, monochloramine form dibromopropane and dichloraniline - monobromobimane, as confirmed by gas chromatography-mass spectrometry. Figure 1 shows the response of the synthesized 2,6-dichloraniline and mass spectrum of bromo derivatives. Molecular ion (M+) with m/z=239 corresponds to the mass of 4-bromo-2,6-dichloraniline.
At room temperature (20±5°C) reaction of synthesized chloraniline completed within 2 min with the quantitative formation of bromo derivatives of chloraniline.
2. Extraction concentration of bromine derivatives of chloroanilines by the method of solvent extraction. This stage is designed for conversion of bromo derivatives of chloraniline more convenient for subsequent gas chromatographic analysis of the organic phase, increasing their concentration in the extract and separation of interfering components.
Introduction to molecules chloraniline bromine atoms greatly increases their hydrophobicity [Korenman IM Extraction of organic substances. Bitter: Izd-vo Gorkov. state University, 1973. - 158 S.], which provides for the subsequent extraction of the effective izlechenia.eradikation of chloraniline (~95-98%) of the water matrix in the organic phase.
3. Getting trifurcation bromo derivatives of chloraniline (chemical modification, stage 2) in the organic extract when interacting with triperoxonane anhydride. The acylation is carried out for the decontamination adsorption-active amino groups with the aim of improving the chromatographic characteristics of bromo derivatives of chloraniline and increase the sensitivity of their definition (introduction to three fluorine atoms). Fig.2 shows the reaction etilirovany 4-bromo-2,6-dichloraniline and the mass spectrum obtained trifenatate. Molecular ion (M+) with m/z=335 corresponds to the mass of triptoreline 4-bromo-2,6-dichloraniline.
4. Analysis of trifurcation bromo derivatives of chloroanilines by gas chromatography. The obtained derivatives analyzed by capillary gas chromatography with electron capture detector (ECD). The introduction of halogen atoms (bromine and fluorine) in the molecule chloraniline and applications for detection halogenating DEATH provides the maximum sensitivity of their gas chromatographic determination.
The definition of chloraniline in the water performed by the following method. The analyzed water sample placed in the tube with a capacity of 25.0 cm3add 0.12-0.36 g of potassium bromide, which is 0.5-1.5% by weight of a water sample. To the obtained mixture is added 1.0 cm3bromine water is (C(Br 2)=0.015 mol/DM3and bromilow for 2 minutes. To complete the reaction, the synthesized add 1.0 cm3solution of sodium thiosulfate ((PA2S2O3)=0.03 mol/DM3). Next, enter the internal standard is 0.2 cm3an aqueous solution of 4,6-dibromo-1,2-dimethoxybenzene (ρ(4,6-dibromo-1,2-dimethoxybenzene)=1 g/cm3), 1.0 cm3toluene and extracted for 5 minutes with continuous stirring. After separation of phases selected 0.2 cm3extract and enter 6-12 mm3triperoxonane anhydride, which is 5-10% by weight of the extract. The acylation is carried out in a thermostat at 70°C for 30 minutes the resulting triptoreline bromo derivatives of chloraniline analyzed by gas chromatograph with ECD.
Conditions for gas chromatographic determination: detector temperature 320°C, evaporator 320°C, thermostat columns 200°C.; silica capillary column 30 m×0.25 mm×0.25 μm with slightly polar stationary liquid phase (SE-30, SE-52, SE-54), the flow rate of carrier gas (nitrogen, OSC) through a column of 0.8 cm3/min, positive pressure detector 20 cm3/min, the division of the flow of 1:50. Figure 3 shows the chromatogram of a standard solution of chloraniline obtained under the above conditions of sample preparation and chromatographic separation (1 - triptorelin 2,4,6-trichloroaniline, 2 - triptorelin 2,4-dichloro-6-bromoaniline, 3 - triptorelin 2,6-dichloro-4-bromoaniline, 4 - triptorelin 4-chloro-2,6-dibromoanisole, 5 - triptorelin 2-chloro-4,6-dibromononane, 6 - internal standard, 7 - triptorelin 3-chloro-2,4,6-tribromoaniline; the concentration of all components 0.5 µg/DM3).
Identification of bromo derivatives of chloraniline in the analyzed sample of water is performed by relative retention time tx∗:
where txand tarticle- fixed the retention times of components of the sample and internal standard, respectively.
The relative retention times of components of the sample are compared with the relative retention times of the analyzed substances, obtained for a standard solution.
|The relative retention times of the analyzed compounds|
The mass concentration of chloraniline in the analyzed water sample are calculated using equations derived from the calibration graphs for the standard solutions chloraniline (table 2).
|Equations of the calibration curves of the analyzed components|
|Substance||The equation of the calibration dependence||The correlation coefficient, R2|
|2,4-dichloraniline||ρ (g/DM3)= 22.37S/Sst+0.187||0.9988|
|∗- S/Sst- the ratio of the chromatographic peak area of the component to the chromatographic peak area of internal standard (4,6-dibromo-1,2-dimethoxybenzene).|
Examples of the method
The analyzed water sample placed in the tube with a capacity of 25.0 cm3add 0.012 g of potassium bromide, which is 0.05% by weight of a water sample. To the obtained mixture is added 1.0 cm3bromine water ((CH2)=0.015 mol/DM3and bromilow for 2 minutes. To complete the reaction, the synthesized add 1.0 cm3solution of sodium thiosulfate ((PA2S2O3)=0.03 mol/DM3). Next, enter the internal standard is 0.2 cm3an aqueous solution of 4,6-dibromo-1,2-dimethoxybenzene (ρ(4,6-dibromo-1,2-dimethoxybenzene)=1 g/cm3), 1.0 cm3toluene and extracted for 5 minutes with continuous premesis the Institute. After separation of phases selected 0.2 cm3extract and injected with 0.6 mm3triperoxonane anhydride (TFW), which is 0.5% by weight of the extract. The acylation is carried out in a thermostat at 70°C for 30 minutes the resulting triptoreline bromo derivatives of chloraniline analyzed by gas chromatograph with ECD.
The method is not feasible, because the detection limit of chloraniline higher than the prototype.
The content of CVG in the sample - 0.5%, TFW extract - 3%. Analyze as described in example 1. The detection limit is 0.06 ág/DM3. Way feasible.
The content of CVG in the sample-1.0%, TFW extract - 5%. Analyze as described in example 1. The detection limit of 0.05 µg/DM3. Way feasible.
The content of CVG in the sample is 1.5%, TFW extract - 8%. Analyze as described in example 1. The detection limit is 0.06 ág/DM3. Way feasible.
The content of CVG in the sample - 2.0%, TFW extract - 10%. Analyze as described in example 1. The detection limit is 0.06 ág/DM3. Way feasible.
The content of CVG in the sample is 2.5%, TFW extract - 15%. Analyze as described in example 1. The detection limit of 0.05 µg/DM3. Way feasible.
The content of CVG in the sample - 3.0%, TFW extract - 20%. Analyze as described in example 1. The limit of motion is possible - 0.05 µg/DM3. Way feasible.
The results of determination of chloraniline in the water of the proposed method are shown in table 3.
|Examples of the method|
|# example||The content of KBr, %||The content of TFW, %||The detection limit, µg/DM3||The ability of the proposed method|
From examples 1-7 and table 3 it follows that the proposed method for the determination of chloraniline feasible in the range of concentrations of KBr in the sample 0.5-2.5%, TFW extract 3-15%. Further increase in the concentration of KBr, TFWA is impractical because it does not affect the detection limit of chloraniline and leads to excessive reagents. When the content of KBr in the sample is less than 0.5%, TFOY in the extract is less than 3%, bromo derivatives of chloraniline and their triptoreline are formed with semi-quantitative output, and the required sensitivity is not achieved.
Compared with the prototype of the proposed solution has the following advantages:
1. The lower limit of detection chloraniline in water: 0.05 µg/DM3; prototype - 1.2 µg/DM3.
2. Fewer analytical stages is of Tcl: 4; prototype - 7 (3 main: extraction concentration, chemical modification, gas chromatography determination and 3 auxiliary stage: filtering a water sample, evaporation of the organic extract, additional extraction).
3. A smaller amount of a water sample is required for analysis: 25 cm3; prototype - to 1000 cm3.
4. Carrying out the acylation can increase the degree of chromatographic separation of the analyzed compounds: for bromine derivatives of chloraniline it is 60-65%for trifurcation already 90-95%.
5. In the analytical cycle, there is no process of evaporation of the organic extract, leading to distortion of the results of quantitative chemical analysis chloraniline in the water.
6. Less run time analysis: 50 min; prototype - more than 60 minutes
Method of determining chloraniline in aquatic environments, including chemical modification of bromo derivatives of chloraniline, extraction preconcentration and gas chromatographic detection, characterized in that as an additional reactant-modifier applied triperoxonane anhydride in the amount of 3-15% by weight of the extract, and bromo derivatives of chloraniline get in front of the stage extraction concentration in the aqueous medium in the presence of bromide of potassium in an amount of 0.5-2.5% Almassy water samples.
SUBSTANCE: samples undergo crystal structure analysis after drying at temperature 25°C. Changes in the structural state of water are indicated by differences between crystallographic images of dried droplets before and after physical action, which depend on content of liquid-crystal associates.
EFFECT: fast detection of qualitative changes in liquid water under the effect of different factors.
2 ex, 3 dwg
SUBSTANCE: equipment system includes measuring devices connected to a computer. In the system, consisting of one or more sensors, an amplifier, an analogue-to-digital converter (ADC) and a computer, each sensor is a tensoresistor sensor mounted on a horizontal base inside a protective housing and having the end of a flexible elastic sensor plate protruding from the housing, said plate being meant for connection with the top valve of the tested mollusc. The output of each sensor is connected to the input of the amplifier consisting of a zero balancing device, an analogue signal amplifier and a signal shift device connected in series. Each sensor is connected to the bridge circuit of the zero balancing device. The output of the amplifier is connected to the input of a 10 bit ADC whose output is connected to the input of an interfacing device which transmits a digital signal to the input of the computer having special software.
EFFECT: high accuracy and reliability of detection as well as simple design.
2 cl, 3 dwg
SUBSTANCE: isolated during bacteriologic analysis of quality of water for various purposes pathogenic bacteria, additionally potentially pathogenic bacteria with their further identification and normalised indicators of water quality estimation are taken into considereation with further implementation of process of generalisation into a single assessement of microbial risk thresholds, which is performed by calculating first weighted coefficients by formula: An=(P1·V1+P2·V2+…+Pn·Vn). After that, the data obtained are used to calculate integral index by each sanitary and hygienic factor by formula: Estimation of risk by three-level classifier is considered high if values of Rfac are from 0.4 to 1.0 including 0.4 and 1.0, medium if values of Rfac are from 0.2 to 0.4 and low if values of Rfac are from 0 to 0.2, including 0. Estimation of risk by five-level classifier is considered to be very high if values of Rfac are from 0.6 to 1.0, including 0.6 and 1.0, high if values of Rfac are from 0.4 to 0.6, including 0.4, medium if values of Rfac are from 0.2 to 0.4, including 0.2, low or acceptable if values of Rfac are from 0.15 to 0.2, including 0.15 and very low if values of Rfac are from 0 to 0.15. After that the obtained results are used to calculate generalised index of risk of sexually transmitted bacterial intestinal infections CA by formula by three-level classifier it is considered high if values of CA are from 0.4 to 1.0, including 0.4 and 1.0, medium if values of CA are from 0.2 to 0.4, and low if values of CA are from 0 to 0.2, including 0. Estimation of risk by five-level classifier is considered very high if values of CA are from 0.6 to 1.0, high if values of CA are from 0.4 to 0.6, including 0.4, medium if values of CA are from 0.2 to 0.4, including 0.2, low or acceptable if values of CA are from 0.15 to 0.2, including 0.15 and very low if values of CA are from 0 to 0,15.
EFFECT: application of claimed method makes it possible to reduce or prevent morbidity associated with bacterial semination of water.
1 ex, 8 tbl, 1 dwg
SUBSTANCE: bacteriological analysis of water by normalised indicators is performed with determination of pathogenic bacteria, additionally during water analysis determined are potentially pathogenic bacteria and their pathogenic and virulent properties, obtained data are used to estimate probability of infectious process development in people by formula: Hpatogen =(C•(100-Pt)•V•v/r)•T. After that, calculated is integral index of probability of development of bacterial intestinal infections transmitted by water way with direct release of causative agents isolated and identified during microbiological analysis of water by formula: After that, risk of development of bacterial intestinal infections transmitted by water way is carried out, it is considered to be acceptable if its value does not exceed 1x10-5, and microbial risk of development of bacterial intestinal infections transmitted by water way is considered to be low. If its value is from 1x10-5 and lower, microbial risk of development of bacterial intestinal infections transmitted by water way is considered to be high. If its value constitutes more than 1x10-5, risk of water contamination with pathogenic and potentially pathogenic microflora is estimated at population level by formula: Rp=Rv•100000.
EFFECT: application of claimed method makes it possible to reduce or prevent development of intestinal diseases and makes it possible to predict probability of BII development with direct release of bacterial causative agents from water for various purposes, taking into account their species composition and biological properties.
1 ex, 2 tbl
SUBSTANCE: method involves collecting samples directly in the region of functioning of the pond and in the control zone, and then determining content of chemical compounds in the samples and determining main quantitative indicators of components of the aquatic ecosystem based on said content. Quantitative indicators of the biota - number and biomass of phytoplankton, zooplankton and benthos - are also determined in the samples from the control zone and the region of functioning of the pond. The ratio of the quantitative indicators of the biota in the pond region to those in the control zone is then calculated. A reference table of ranges of the calculated chemical indicators of the ratios of components of the aquatic ecosystem is then created while adding rows with ratios of quantitative indicators of the biota into the table. By comparing the calculated ratios with ranges of identical ratios in the reference table, the effect of the pond on the state of the aquatic ecosystem is then determined.
EFFECT: high reliability of results.
1 ex, 4 tbl
SUBSTANCE: during realisation of the method the test objects are soaked in tested solutions, parameters of test objects survivability are registered, and using them, threshold concentrations of tested pesticide toxicity are calculated, besides, pathomorphological modifications are registered in test objects, the average percentage of malformations is calculated, and the threshold concentration of teratogenic impact is established as the pesticide concentration with minimum teratogenic impact at test objects, and extent of pesticides toxicity is estimated on the basis of the threshold concentration coefficient, which is calculated using the formula Kn emb - coefficient of threshold concentrations of pesticides toxicity taking into account their teratogenicity, LC16 - limit concentration of pesticides toxicity causing death of 16% embryos, EterC16 - threshold concentration of teratogenic effect of pesticides. At the same time if values of the coefficient Kn emb >10, the class of pesticides hazard is established as I, i.e. extremely hazardous, 5-10 - the class of pesticides hazard is set as II, i.e. highly hazardous, 1-5 - the class of pesticides hazard is established as III, i.e. hazardous, <1 - the class of pesticides hazard is IV, i.e. moderately hazardous. Test objects are embryos of sturgeons.
EFFECT: increased accuracy and validity of assessment.
2 cl, 1 ex, 6 tbl
SUBSTANCE: enteroviruses are concentrated by introduction into an analysed water sample of a magnetic sorbent microparticles coated with polymeric silicon dioxide with amino poropyl groups in proportions 1:1000-3000 of water sample volume. It is incubated at constant stirring for 1-2 hours. The sorbent is collected with a magnet, a supernatant is removed, and a sorbent-enterovirus complex is produced. Enteroviruses are eluted by 0.5M NaCl and 0.05M Tris (pH-10.5) solution. Enteroviruses are identified by immunochemical, cultural and molecular methods.
EFFECT: high degree of virus concentration in the eluate, decreased amount of the eluating solution.
SUBSTANCE: fixed and mobile monitoring sites equipped with measuring instrumentations are located. Various environmental parameters are registered and subjected to analysis. More specifically, hydrophysical field signals are being registered, chemiluminescence, chromatographic, ion-selective, spectral and radiometric analysis is performed. Besides, bed acoustic impendance is registered, molecular spin interactions of seawater protons are detected, artifacts resulting from the magnetohydrodynamic, bioelectric and concentration effect are detected, synthetic surfactant content in the aquatic environment, chlorophyll concentrations, microorgasnisms, phytoplankton, zooplankton is determined. The collected data is further transferred to the archivers and modeling is performed. In the course of modeling the industrial facility environment and infrastructure is divided into a number of areas and a material balance model and a forecast model are created for each of them. For the purposes of the method implementation a system comprising a water withdrawal line equipped with hydrophysical field sensors, a filtering plant for chlorophyll concentration, a filtering plant with a Seitz funnel for microorganisms sampling, a Nageotte chamber for counting the phytoplankton content, a Bogorov Counting Chamber for enumerating zooplankton, a centrifugal apparatus to determine chlorophyll content, a geophone, spectral sensor of proton spin echo is proposed. Besides, the proposed system comprises devices for chemiluminescence, chromatographic, ion-selective, spectral and radiometric analysis, a radiation spectrometer, an atomic absorption spectrophotometer, an X-ray fluorometric analyser, TV sensors, infrared sensors, heat sensors, a metrological module, a sidescan sonar, multiple-beam echo sounder, water quality evaluator by TropoSample parameters and bed deposits characteristics, a lidar (a light radar), a penetrometer, methane and hydrogen detection sensors.
EFFECT: enhanced functional capabilities.
2 cl, 11 dwg
SUBSTANCE: invention relates to a method of concentrating salicylic acid from aqueous solution, involving extraction with trioctylamine oxide solution in hexane, deposited on foamed polyurethane tablets in amount of 75-80% of the weight of foamed polyurethane.
EFFECT: invention increases concentration coefficient of salicylic acid.
2 tbl, 4 ex
SUBSTANCE: system for rapid biological monitoring and indication consists of measurement-detection, analytical and signal units. The measurement-detection unit is n apparatus for measuring reactions of aquatic indicator organisms, where n=2, 3, 4, for two or more aquarium in which there are indicator organisms, into which water enters from a distributing aquarium, said water being pumped by a pump from the tested underwater horizon of the water body or from water pipe. Parameters of functional characteristics of the indicator organisms are calculated from signals of measuring apparatus coming into the analytical unit which comprises a computer with software, containing a data base of parameters of the state of functional characteristics of different indicator organisms under normal conditions, configured for constant population and editing. Values of the measured parameters are continuously processed by the computer in real time, separately for each individual indicator organism. Upon deviation of average values from standard values, the signal unit is automatically switched off and a three-step alarm signal is generated - upon deviation from the standard on one parameter, on three parameters and on all parameters for all indicator organisms.
EFFECT: high accuracy and reliability of continuous indication of the quality of water.
3 cl, 7 dwg
SUBSTANCE: proposed gas analyser comprises temperature and pressure metres, thermostatting system and fluid thermostat accommodating saturator representing a vertical set of communicating plates and filled with fluid metered component. It additionally incorporates a variable turbulent throttle arranged in tandem with aforesaid saturator and variable turbulent throttle connected in parallel to aforesaid saturator and first throttle, both throttles being operated in supercritical gas efflux conditions.
EFFECT: reduced time of reaching steady-state conditions, higher accuracy, improved dynamic characteristics, simpler design.
SUBSTANCE: present invention can be used in qualitative and quantitative determination of the content of organic compounds of Au, Pt and Pd in rocks of various compositions and concentrated in their organic components. According to the invention, the method involves preparation of a sample of test material, mixing the sample with litharge, fire assay of the sample in a mixture with litharge, dissolving the obtained prill in nitrohydrochloric acid and atomic absorption analysis of the acidic solution. The method is distinguished by that, before mixing the sample with litharge, the sample is mixed with Na or K chloride in ratio of 5% sample to 95% Na or K chloride. Traditional sample preparation methods, where the sample is broken up and dissolved into a solution, lead to loss of the main part of the analysed Au, Pt and Pd, which is in form of organic compounds.
EFFECT: maximum retention of analysed components.
SUBSTANCE: efficiency of filters and devices for purifying household and industrial purpose water is evaluated. A composite index of the overall carbon content in organic compounds with limited volatility is used before and after purification. The overall carbon content is determined using gas chromatography with atomic-emission detection. Determination of the efficiency of purification using a highly sensitive method is invented. In that case the composite index of the overall carbon content correctly reflects the change in the quality of water during treatment.
EFFECT: high sensitivity of the method.
4 ex, 5 tbl
SUBSTANCE: method includes saturation of a noble gas stream by volatile compounds to equilibrium concentrations which is carried out by contact of noble gas with the granulous bed of a stationary phase of solid adsorbates or low-volatile liquids put on solid carrying agents. Device for a method realisation according to the invention consists of the tubular flowing system filled with the granulous bed of a stationary phase with fixed quantity of volatile components. Tubular flowing system is executed, at least, from three consistently connected sections of equal length, first of which is connected to the block of noble gas preparation and has a bigger diameter in comparison with the subsequent.
EFFECT: efficiency upgrading of sorption and denudation processes; simplification of saturation of the flowing system by volatile components.
2 cl, 1 dwg, 1 tbl
SUBSTANCE: at a method realisation the noble gas stream continuously contacts to the granulous bed of the stationary phase consisting from put on corpuscles of the solid carrying agent of a low-volatile liquid. Saturation of a stationary phase by vapours of volatile components is carried out to equilibrium concentrations on entry and exit of the flowing system at the temperature exceeding operating temperatures for gained calibration mixes of various compositions. Device consists of noble gas preparations consistently connected blocks, unit of feeding into of a sample with the evaporator, the temperature-controlled tubular flowing system filled with the granulous bed of a stationary phase and the detector. Tubular flowing system is executed, at least, from three consistently connected sections with equal geometrical sizes, first of which connected with the evaporator of unit of feeding into of sample and has a bigger percent of the solid carrying agent impregnating of a low-volatile liquid in comparison with the subsequent. Detector by means of the additional gas crane is connected with exit and entry of tubular flowing system.
EFFECT: reception of calibration mixes of volatile components.
2 cl, 1 dwg, 1 tbl
FIELD: chemical engineering.
SUBSTANCE: device comprises tank filled with a solution of volatile agents in low-volatile solvent and mixer connected with the inlet of the tank. The mixer is connected with the separator for separating vapor-gas phase from the liquid drops. The inlet of the separator is made of a conical calibrated capillary, and its outlet is connected with the tank. The valve for precise control provides the supply of gas-diluent to the line for discharging the flow saturated with volatile agents.
EFFECT: simplified design.
FIELD: the invention refers to the field of gas industry.
SUBSTANCE: the mode is executed by way of successive bubble contact of a gas flow with two portions of solution of volatile matters in low-volatile solvent. The received gas flow is additionally mixed with a flow of an inert gas-reducer. The consumption of the inert gas-reducer passing through two portions of the solution is changed depending from concentration of volatile matters in the gas flow at the withdrawal out of the second portion of the solution measured with a quality analyzer. The arrangement for execution of the mode has in-series connected a capacity and a thermostatically controlled mixer filled with initial solution of volatile matters in low-volatile solvent. Two throttles of fine regulation are connected with a line for feeding an inert gas-reducer with a regulator of consumption. The outlet of one of the throttles is connected with the line for withdrawal of the gas flow saturated with volatile matters out of the mixer before the quality analyzer located in it. The outlet of the second throttle is connected to the capacity with initial solution. The quality analyzer is switched in a feedback circuit having a block of regulation of consumption of the inert gas-reducer coming into the capacity and the mixer.
EFFECT: increases time of supporting constant concentrations of volatile matters in a gas flow.
2 cl, 1 dwg, 1 tbl
FIELD: chemical industry; devices and the methods for the quick automatic extraction of acetaldehyde and determination of its contents in the probes.
SUBSTANCE: the invention is pertaining to the evaluator for extraction of the acetaldehyde and automatic determination of its contents in the probes in the form of the bars made out of the polyethylene terephthalate. The evaluator contains the desorption bay, the system of the analysis with the separating column for extraction of the acetaldehyde, the system of valves for control over the streams of the fluid mediums in the evaluator, the tool for heating the desorption bay. The desorption bay is made with possibility of its air blowing, locations in it of the indicated probe and the pressure buildup. The desorption bay is connected to the tube used for injection of the gaseous probes, providing the injection of the gaseous probe of the acetaldehyde. The probe of the acetaldehyde then is transferred into the separation column.
EFFECT: the invention ensures the quick automatic extraction of acetaldehyde in the products made out of the polyethylene terephthalate and determination of its contents in the probes.
9 cl, 3 dwg
FIELD: method for producing gas mixtures for testing gas analyzers.
SUBSTANCE: method for producing checking gas mixtures includes desorption of dosed component from adsorbent into carrier gas flow, let at excessive pressure through a vessel filled with adsorbent, wherein preliminarily adsorbed under excessive pressure is a given amount of dosed component. Further, carrier gas flow is let through turbulent throttle mounted serially with vessel, forming at outlet of device the starting flow of checking gas mixture with maximal concentration of component for current filling of adsorbent and gas-carrier pressure set in the vessel. Concentration of component in the flow of checking gas mixture at device outlet is controlled by changing pressure of carrier gas in the vessel and diluting starting flow of checking gas mixture by flow of carrier gas from the source of compressed gas, let through alternating turbulent throttle connected in parallel to vessel and first throttle. Both throttles operate in above-critical mode of gas stream ejection.
EFFECT: possible production of checking gas mixtures with continuous row of values of concentration of dosed component in broad range.
2 cl, 1 dwg
FIELD: analytical chemistry.
SUBSTANCE: analysis of a sample involves its milling, infusion with acetone, filtration of acetone extraction, concentrating and purification by chromatography method. The concentration is purified in column by using a normal-phase sorbent silica gel L 40/100μ and a mixture hexane-acetone (8:2) as a mobile phase. The following chromatography determination is carried out by HPLC method in column filled with sorbent "Nova-Pak C-18" using a mixture acetonitrile-water (7:3) as a mobile phase and a detector based on photodiode array. Method provides enhancing sensitivity of assay. Invention can be used in practice of sanitary-epidemiological stations, chemical-toxicological, veterinary and ecological laboratories.
EFFECT: improved assay method.
FIELD: analytical methods.
SUBSTANCE: invention is dealing with quantitative assay of β,β'-dihydroxydiethyl sulfide in aqueous matrices encountered in mustard gas disposal processes as well as in environmental monitoring. Compound to be assayed is chemically modified via alkyl halide-mediated alkylation reaction in presence of N,N,N-tributyl-N-benzylammonium chloride under heterophase conditions: 40% sodium hydroxide aqueous solution/benzene at 50±5°C for 40±1 min to form chromatography-susceptible derivatives. Sensitivity of determination is 1·10-5 mg/mL at determination error not higher than 25%.
EFFECT: increased determination accuracy.
6 dwg, 1 tbl