Method of determining weight concentration of lewisite in yperite-containing water by gas-chromatographic method using flame-ionisation detector

FIELD: chemistry.

SUBSTANCE: lewisite is derived in 2-(2-chlorovinyl)-1,3-dithia-2-arsaolan, which is extracted from water by liquid extraction with hexane. Content of lewisite is determined by gas-chromatographic determination of acetylene which is released during alkaline hydrolysis of 2-(2-chlorovinyl)-1,3-dithia-2-arsaolan. The masking action of yperite is eliminated by deriving yperite using ammonia solution in thioethylene glycol.

EFFECT: high sensitivity and reliability of determining lewisite in the presence of yperite on a level which corresponds to sanitary standards.

2 cl, 1 tbl

 

The technical field to which the invention relates.

The invention relates to the field of analytical chemistry, namely the analysis of non-biological materials by physical and chemical methods.

The level of technology

In the practice of chemical environmental control to date, various methods for the detection, identification and quantitative detection of lewisite in natural and man-made environments, different analysis techniques, analytical principles and metrological characteristics. More than 90% of the methods for determining the residual content of skin-naravnih S in different environments (the reaction mass, soil, water, building materials, air) based on gas chromatographic analytical method (GC) using different types of detecting devices: flame photometric (PFD), electron capture (ESD), flame ionization (PID), terminolo (Ted). Due to the high reactivity and lability of lewisite sensitivity of the detecting device GC to it is small and is at the level of 1×10-3%. In this regard, the determination of lewisite on the level of hygiene is carried out with the use of different methods of derivatization. The most common way derivatization is the translation in acetylene at alkaline hydrolysis 30% of the races is a thief NaOH with subsequent analysis of the equilibrium vapor-gas phase using the PID. High volatility and low adsorption capacity of acetylene allow us to determine the lewisite in the water at the level of the MPC. The lack of determination of lewisite on acetylene is the fact that the reaction of formation of acetylene is a group for lewisite and almost all the products of its hydrolysis. For the separation of lewisite from hlorvinilovoj acid using the kinetic method based on the differences in the kinetic regularities of alkaline hydrolysis of lewisite and hlorvinilovoj acid (RU 2163016 C2 "Method separate definitions in the water β-chlorovinyldichloroarsine at MPC and β is chlorovinyldichloroarsine acid"). For the separation of lewisite of all the products of its hydrolysis using the method of solvent extraction (usually as an extractant using diethyl ether in the presence of various vysalivatel (MIM No. 031-02-150-05 "MIM mass concentration of lewisite in water reservoirs by gas chromatography with flame ionization detection", FSUE "GosNIIOKhT". 2005; MIM No. 031-02-281-08 "MIM mass concentration of lewisite in waste water samples by gas chromatography using a flame ionization detector", FSUE "GosNIIOKhT". 2008).

There is a way to determine lewisite in water, in which high sensitivity and selectivity determination is achieved by double the derivatization of lewisite (MIM No. 031-02-196-06 "MIM mass concentration of lewisite in waste water, contains detergents, by gas chromatography", FSUE "GosNIIOKhT". 2006). Within this way before stage solvent extraction (as extractant used hexane in the presence of vicariates sodium chloride) are precolumn lewisite 1,2-atadditional 2-(2-chloride)-1,3-dithia-2-Arsalan (scheme 1):

Translation of lewisite in low volatile 2-(2-chloride)-1,3-dithia-2-arsal allows you to more effectively carry out the stage of concentration of the extract by evaporation him dry. At the final stage of 2-(2-vinyl chloride) 1,3-dithia-2-Arsalan transfer in acetylene treatment of dry extract 30 sodium hydroxide solution in the presence of ethanol (scheme 2).

Thanks to its metrological characteristics (lower limit of detection of lewisite of 1.5×10-4mg/DM3the relative measurement error of ±31%) this method is implemented on the objects on destruction of lewisite. He was selected as the prototype method.

With the undeniable advantages of the prototype method is unacceptable in the case of the presence in the aqueous matrix of mustard gas. Mustard gas is extracted by the same extractants, and lewisite. It was established experimentally that under conditions of excess alkali along with the main hydrolysis product of sulfur mustard - diethylenglycol is formed of impurity soy is inania (presumably, Allen), which by its chromatographic characteristics close to the acetylene. This fact leads to false positive results of determination of lewisite in water containing mustard gas. The study was carried out on an artificial mixture of water (15 ml), lewisite and mustard gas, the method introduced is found. The results are shown in table 1

Table 1
Submitted ×10-6mgFound lewisite (average of four measurements) ×10-6mg
mustard gaslewisiteWithout treatment with ammonium hydroxideTo treatment with ammonium hydroxide
×10-6mg%×10-6mg%
1001001801808585
5050108216 40,681,2
101021210the 9.797
55173403,8368
3,53,5226282,3868
1,51,55,33560,9362,2

Information that reveals the essence of the invention

The present invention is to improve the accuracy, sensitivity, reproducibility and quantitative analysis of lewisite at MPC in water in the presence of mustard gas. The problem is solved in that at the stage of sample preparation is the derivatization of the compound.

The difference of this invention from the prototype method is that the translation of mustard gas in well water-soluble derivative allows us to derive it from the composition of the extract and eliminate thereby preventing influence of mustard gas that bring the to the improvement of the main metrological characteristics of the proposed method and allows to determine the mass concentration of lewisite in the water level of sanitary normative in the joint presence with mustard.

The basis for the development of the proposed method based on the hydrolysis of mustard gas in the slightly alkaline environment of ammonium hydroxide with the formation of diethylenglycol (scheme 3)

The proposed method for quantitative determination of at MPC lewisite in water containing mustard gas, is carried out in the following sequence.

In the vial is placed 15 cm3acidified analyzed samples of water and poured 0.1 ml of 1% solution identicial in acetonitrile. The mixture is treated in the RAS for 5 min add 25% solution of ammonia in water to pH 8-9 and re-treated in the RAS within 3 minutes. Then poured 2 ml of hexane and add 5 g of NaCl. After shaking and settling organic layer selected in penitsillinovy bottle. The extraction was repeated three times, the organic extracts are combined and the solvent evaporated at room temperature in a stream of inert gas to the dry residue. The vial containing the dry residue is sealed using a rubber stopper with Teflon gasket and metal clip. Out of the vial selected 5 ml of air and add 5 ml of 30%sodium hydroxide solution. The vial is placed in the RAS and process for 15 minutes and Then from the bottle take 1 ml of air-vapour phase and injected into the chromatograph evaporator.

The content of lewisite in water samples is determined by the method of absolute gratuitous is. Calculation of mass concentration of lewisite in the analyzed sample of water is performed by the formula

C=Mg×1000/VCR×0,7

where Mgthe number of lewisite, was found in the calibration characteristic, mg;

0,7 - coefficient taking into account the loss of lewisite in the stages of sample preparation.

For the measurement arithmetic mean value of the results of two parallel determinations. The analysis time per sample, taking into account the time of sample preparation does not exceed 60 minutes Lower limit of detection of lewisite by the present method is 1*10-4mg/DM3. The relative error of the methodology does not exceed ±30%.

Thus, the proposed method allows to determine the mass concentration of lewisite in water in the presence of mustard gas at MPC. The proposed method allows to solve the on-site laboratories urgent need to quantify the mass fraction of lewisite at the level of 1*10-4mg/DM3.

1. The method of determining the mass concentration of lewisite in water containing mustard gas, by gas chromatography using a flame ionization detector, including the derivatization of lewisite 2-(2-chloride)-1,3-dithia-2-Arsalan and derivatization of the compound in diethylenglycol, liquid extraction of 2-(2-chloride)-1,3-dithia-2-Arsalan hexane in the presence of sodium chloride, to centrirovannyi extract by evaporation to dryness, the derivatization of 2-(2-vinyl chloride)-1,3-dithia-2-Arsalan in acetylene, gas chromatography determination of acetylene.

2. The method according to claim 1, in which for the Department of mustard gas from lewisite use the derivatization of the compound in diethylenglycol solution of ammonium hydroxide.



 

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2 tbl, 1 ex, 1 dwg

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