Method of determining content of chlorobenzene in natural and waste water using gas chromatography and equilibration vapour analysis

FIELD: chemistry.

SUBSTANCE: method of determining chlorobenzene in natural and waste water using gas chromatography and equilibrium vapour analysis includes determining chlorobenzene on a chromatographic capitally column in a carrier gas current which is nitrogen; generating and detecting the investigated ions formed in a flame with a flame-ionisation detector. The method also includes preparing a basic solution using a more viscous ethylene glycol solvent, hence the basic solution is well preserved for 2 months at temperature in the range of -2°C to -10°C; preparing calibration solutions for chlorobenzene concentration in the range of 0.0003-0.02 mg/dm3; sample preparation, calibrating the chromatograph by perforating the vapour phase of the prepared concentrations; plotting a calibration curve; sample preparation for the analysed water samples; perforating the vapour phase into the evaporator of the chromatograph. The obtained data are processed using ChemStation software which comes in a set with the MAESTRO 7820A chromatographic kit, and qualitative identification and quantitative content of the determined substance is obtained.

EFFECT: improved consistency and accuracy of analysis, shorter duration of the method and easier analysis in environmental monitoring conditions.

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The invention relates to the field of analytical chemistry and can be used to determine the content of chlorobenzene in natural, surface, ground, waste and process waters.

The method of determination in natural and waste waters of chlorobenzene using gas of chromatographie, with the definition of the specified component on capillary chromatography column in a stream of carrier gas, which represents nitrogen; the formation and registration of the flame ionization detector (FID), (FID) detector of the investigated ions in a flame and processing of measurement results by the method of absolute calibration.

The principle of operation of the detector is a flame ionization detector (FID), (FID) is to change the current in the plasma of a hydrogen-oxygen flame when hit in her combustible carbon compounds.

The known method for the gas chromatographic determination of chlorobenzene extraction method (Quantitative chemical analysis of water. The methodology for measuring the content of chlorobenzene in natural and waste waters by gas chromatography. PND F 220-06. M.: NTF "Chromos", 2006 // URLINFOABOUT. URL: http://qlaster.ru/goods/card/210179654/enterprise/73421 - accessed 12.11.2013).

However, the implementation of this method does not provide accurate results for the determination of chlorobenzene. The method proposes to use a range�zones definition from 0.005 to 0.5 mg/DM 3inclusive. Standard for water quality and water fishery from 18.01.10 No. 20, impose requirements on the purity of natural waters: the year-chlorobenzene MPC - 0.001 mg/DM3. Also, this way a long time, not easy to implement sections: "cooking and certified calibration solutions and sample preparation". The method uses methanol as the solvent for preparing the basic solution and hexane as the extractant. These substances are toxic.

The known method of AGONY 4.1.1205-03 (a Collection of guidelines gas Chromatographic determination of benzene, trichloroethylene, toluene, tetrachloroethylene, chlorobenzene, ethylbenzene, m-, p-xylenes, o-xylene, styrene, isopropylbenzene, o-chlorotoluene and naphthalene in the water. The Ministry Of Health. Moscow 2004 // WWW.TEHLIT.RU TECHNICAL LITERATURE. URL: http://www.tehlit.ru/1lib_norma_doc/44/44441 - accessed 12.11.2013).

The implementation of this method requires a large investment of time, provides accurate results for the determination of chlorobenzene. The method is very complex to be executed in the context of environmental monitoring. The measured concentrations of the analytes based on their extraction from dynamic water gas extraction, the solid polymer concentration on the sorbent, followed by thermal desorption, gathermate�tutorial for the separation on a capillary column and detection photoionization detector (PID).

The closest analogue is the RD 52.24.482-2012 (Mass concentration of volatile chlorine substituted hydrocarbons in waters. The measurement technique is gas chromatography method using the analysis of the equilibrium vapor. Techexpert. Electronic Fund legal and normative-technical documentation. URL: http://docs.cntd.ru/document/1200095292 - accessed 12.11.2013), taken as a prototype.

However, as described in the guidance document - version 2 - gas chromatographic method using analysis of the equilibrium pair (PRA) of the sample is pre-concentrated by distillation, continuous in time, cannot provide accurate results in gas chromatographic study of chlorobenzene. For the preparation of certified basic solutions are used toxic solvents isopropyl alcohol, methanol.

The technical problem to be solved by the claimed invention is to improve consistency and accuracy of the analysis, reducing the execution time of the method and ease of implementation analysis in terms of environmental monitoring.

The proposed method allows to solve the problem, to determine the rate of contamination of chlorobenzene in the range of concentrations: the 0.0003-0.02 mg/DM3in accordance with the requirements of water quality and water fishery from 18.01.1 No. 20, instituting the following requirements to the purity of natural waters: chlorobenzene MPC - 0.001 mg/DM3(limiting the rate of harm - Toxicological).

Preparation of calibration samples

As a basic solution of chlorobenzene use of the state security service (the content of the basic substance 100%, if the content of the basic substance less, take this into account), in the form of a solution of ethylene glycol with a concentration of 5*103mg/DM3as shown in table 1.

Ethylene glycol is a viscous substance that retains the volatile components that allows you to store the stock solution of 2 months at a temperature from -2°C. to -10°C. the Mass concentration of the basic solution and the calibration samples (when diluted) is calculated by the formula (1)

where C0is the concentration of the initial solution, V0- the volume of the initial solution, Cxthe concentration of the solution prepared, Vx- volume of the prepared solution (1,106 g/cm3·0,045 cm3)/10 cm3= 0,004977 g/cm3(5*103mg/DM3).

The shelf life of the main solution of 2 months at a temperature from -2°C to -10°C.

An intermediate solution is prepared by dilution from the core solution using distilled, boiled water (5*103mg/DM3*0,020 cm3)/100 cm3= 6.32 per mg/DM3(see PL. 2).

Dissolve� is not stored.

The calibration samples are prepared using distilled, boiled water.

Example. Calibration sample No. 1 - volumetric flask with a capacity of 250 cm3pour water to the mark and select the volume of 0.16 cm3. Then the flask is made of 0.16 cm3the intermediate solution and quickly stir. For volatile components, it is important to make breeding so that there is less loss of the designated substances. Preparation of calibration samples is presented in table 3.

As a basic solution of chlorobenzene use of the state security service (99,9%) in the form of a solution of ethylene glycol with a concentration of 5×103mg/DM3.

Table 1
The name of the componentV (ál) GEOEthylene glycol (ml)P (g/ml)The concentration of the basic solution (mg/cm)
chlorobenzene45,010,01,1065*103mg/DM3

Preparation of intermediate solution

Table 2
NameThe concentration of the basic solution (mg/DM3)V1(cm3the primary solutionV2(cm3) waterThe concentration of the intermediate solution (mg/DM3)
chlorobenzene5*1030,0201001,0

Preparation of calibration samples

Table 3
Name and No. of the sampleThe concentration of the intermediate solution (mg/DM3)V1(cm3) intermediate solutionV2(cm3) waterThe concentration of the calibration sample (mg/DM3)
1 deg. sample1,00,16250,00,00064
2 deg. sample1,00,28250,00,0011
3 deg. sample1,00,7250,00,0028
4 deg. sample1,01,4250,00,0056
5 degrees. sample1,03,45250,00,0138

The establishment of calibration characteristics

10 ml of the calibration mixture is placed in a vial (bottle) sodium sulfate (3 g, calcined at 400°C), hermetically sealed, immediately stirred, incubated in a "binder" (thermostat) at T 80°C - 30 minutes. Then heated headspace syringe taken 1 cm of the gas phase (0.5 cm from the surface of the solution). Injected into the chromatograph evaporator.

Technique PARAMETERS: GC MAESTRO, the carrier gas is nitrogen.

Column NUCOL.

The FID detector.

Flow division 2:1; the Temperature INJ -200°C; flow column (1.5 ml/min; column Temperature: 80°C for 12.5 min; the Temperature detector FID - 250°C; method of 12.5 min retention Time of the analyte 11,530 min.

On capillary column for analysis throughout the range using one of the calibration scale, obtained with solutions No. 1-5. Calibration (calibrate�ovocny) solutions are not stored.

Subsequent analysis of the investigated water samples, sample preparation, is similar to the scheme described the establishment of calibration characteristics.

To obtain the results of measuring the concentration of substances, carried out the analysis of two parallel water samples. Before processing any results, it is necessary to analyze the "single sample with distilled water to ensure no interference and pollution.

The concentration of the substance in water (mg/DM3) is determined by the corresponding calibration graphs using a computer program Chymstation, which is equipped with chromatographic complex MAESTRO A, Agilent. Experienced part of the method of determination of chlorobenzene in natural water are presented in a separate file. The results of mathematical processing of the data according to the results of the practical work presented in tables 4, 5, 6.

This method is illustrated using a typical chromatogram (Fig.1, 2).

Data on the results of empirical studies.

Detection range: chlorobenzene is 0.0003-0.02 mg/DM3.

Measured concentration is 0.001 mg/DM3(chlorobenzene).

chlorobenzene 2,98183
Table 4
The name of the componentSample # With�Argania substances mg/DM3
chlorobenzene10,0011
chlorobenzene40,00108
chlorobenzene70,00109
chlorobenzene100,00106
chlorobenzene130,0011
chlorobenzene160,00107
chlorobenzene190,00111
chlorobenzene220,00108
chlorobenzene250,00104
chlorobenzene280,00116
The arithmetic meanchlorobenzene 0,001089
The relative standard deviation, %

Detection range: chlorobenzene is 0.0003-0.02 mg/DM3.

Measured concentration is 0.006 mg/DM3(chlorobenzene).

td align="justify"> 0,006180
Table 5
The name of the componentSample # Of a substance, mg/DM3
Chlorobenzene20,00586
Chlorobenzene50,00637
Chlorobenzene80,005944
Chlorobenzene110,006014
Chlorobenzene140,006115
Chlorobenzene170,006018
Chlorobenzene200,006054
Chlorobenzene230,005933
Chlorobenzene26
Chlorobenzene290,006155
The arithmetic meanchlorobenzene 0,006063
The relative standard deviation, %chlorobenzene 2,4489

Detection range: chlorobenzene is 0.0003-0.02 mg/DM3.

Measured concentration is 0.01 mg/DM3(chlorobenzene).

Table 6
The name of the componentSample # Of a substance, mg/DM3
Chlorobenzene30,01026
Chlorobenzene60,01043
Chlorobenzene90,01024
Chlorobenzene120,01080
Chlorobenzene150,01082
Chlorobenzo� 180,01098
Chlorobenzene210,01008
Chlorobenzene240,0100
Chlorobenzene270,01066
Chlorobenzene300,01051
The arithmetic meanchlorobenzene 0,010478
Standard deviation, %chlorobenzene 3,17250

Thus, in accordance with the requirements of RMS n/b 5%, the observed confidence interval for the probability P=0,95, also reduced the execution time of the method and increases the convenience of analysis that in the context of environmental monitoring allows you to perform more tests.

Unlike analog, the proposed method ensures compliance with modern requirements (MAC), speed, accuracy and efficiency of the definition of the contaminant component chlorobenzene gas chromatographic method in natural and waste waters.

Method objectified�tion content of chlorobenzene in natural and waste waters using gas chromatography, using the analysis of the equilibrium vapor including definition of chlorobenzene on capillary chromatography column in a stream of carrier gas, which represents nitrogen; the formation and registration of the flame ionization detector of the investigated ions in a flame, characterized in that prepare the stock solution by using a more viscous solvent of ethylene glycol, so the main solution is well maintained 2 months at a temperature from -2°C to -10°C, prepare calibration solutions for the range of concentrations: chlorobenzene is 0.0003-0.02 mg/DM3make sample preparation, graduate chromatograph, piercing the vapour phase of the prepared concentrations, build a calibration curve, perform sample preparation for the studied water samples, the vapour phase pierce into the chromatograph evaporator, the obtained data is processed by computer software ChemStation, which is equipped with chromatographic complex MAESTRO A, and get qualitative identification and quantitative determination of the analyte.



 

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