Method of detecting chloroanilines in aqueous media

FIELD: chemistry.

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.]:

KBr→K++Br-

VG2+VG-⇔VG3-

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:

tx=tx/tarticle,

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.

Table 1
The relative retention times of the analyzed compounds
Substancetx
triptorelin 2,4,6-trichloroaniline0.451
triptorelin 2,4-dichloro-6-bromoaniline0.650
triptorelin 2,6-dichloro-4-bromoaniline0.673
triptorelin 4-chloro-2,6-dibromoanisole0.887
triptorelin 2-chloro-4,6-dibromononane0.908
internal standard1.000
triptorelin 3-chloro-2,4,6-tribromoaniline1.770

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).

Table 2
Equations of the calibration curves of the analyzed components
SubstanceThe equation of the calibration dependenceThe correlation coefficient, R2
2-Chloroanilineρ (g/DM3)=11.991S/Sst+0.1430.9990
3-Chloroanilineρ (g/DM3)=9.422S/Sst+0.0440.9995
4-Chloroanilineρ (g/DM3)=15.556S/Sst+0.176 0.9997
2,4-dichloranilineρ (g/DM3)= 22.37S/Sst+0.1870.9988
2,6-dichloroanilineρ (g/DM3)=17.419S/Sst+0.1860.9980
2,4,6-trichloroanilineρ (g/DM3)=14.316S/Sst+0.0780.9995
- 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

Example 1

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.

Example 2.

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.

Example 3.

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.

Example 4.

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.

Example 5.

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.

Example 6.

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.

Example 7.

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.

Table 3
Examples of the method
# exampleThe content of KBr, %The content of TFW, %The detection limit, µg/DM3The ability of the proposed method
Prototype--1.2-
10.050.855impossible
20.530.06feasible
31.050.05feasible
41.58feasible
52.0100.06feasible
62.5150.05feasible
73.0200.05feasible

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.



 

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EFFECT: improved assay method.

3 tbl

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

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