Method of simultaneous determination of diehtylene glycol and methanol in natural and sewage water by method of liquid chromatography

FIELD: chemistry.

SUBSTANCE: method of simultaneous determination of methanol and diethylene glycol in natural and sewage water by LC method with separation of said components in chromatographic column in flow of eluent, which represents sulphuric acid solution in deionised water with molar concentration 2.5 mmole/dm3; registering difference of indices of refraction of eluent solution and solutions, which contain target components and processing results of measurements by method of absolute calibration. Sample preparation does not require dilution of analysed water sample up to content of target components 10 g/dm3, more concentrated samples are diluted with deionised water.

EFFECT: quickness and simultaneousness of determination of diethylene glycol and methanol content.

 

The invention relates to the field of analytical chemistry and can be used for simultaneous determination of methanol and diethylene glycol (deg) in surface, ground, waste and process waters. Actual use of the invention in the analysis of associated wastewater, oil and gas industry. Methanol is used to prevent the formation of solid crystalline compounds gas with water in technological processes gas industry, as an inhibitor of hydrate formation in systems of gas production. In waters associated gas condensate fields can reach significant values. Diethylene glycol (deg) in the gas industry is widely used for gas dehydration when preparing it for transportation. Therefore, sewage gas industry objects associated with the extraction, storage and transportation of natural gas containing methanol and diethylene glycol. Waste water is treated and disposed of via injection into deep aquifers groundwater. When pumping the residual amount of methanol should not exceed 40 g/DM3; diethylene glycol 4 g/DM3[1].

Currently, there are various methods for determination of methanol in water. Among the chemical methods that photometric with chromotrope acid, titrimetric with bichromate of potash in to the amount of oxidant. Apply rapid instrumental methods: method infrared spectrometry; method voltammetry [2] and gas chromatography methods [3; 4]. On the website LLC Econix-Expert. The production and supply of laboratory equipment and instruments [2] proposed voltammetric analyzer for the determination of small quantities of methanol (0.05 to 10 mg/DM3) and deg (0.5 to 10 mg/DM3in waste water in unelaborated conditions. In gas chromatography method [3] uses a Packed column containing polychrome coated with a solution of 1, 2, 3 Tris (beta-tzanetaki) propane. The analysis is performed in a stream of inert carrier gas, column temperature of 60-70°C, evaporator 100-150°C.

Also known the method according to the patent of Russian Federation №2273850, IPC G01N 30/02, publ. 10.04.2006 [4], in which the chromatographic method used Packed column containing diatomite-modified polyglycerol obtained temperature processing of glycerol over 40 hours. For the analysis of the methanol from the water sample is distilled off and washed with organic solvents from interfering with the analysis of compounds, the column temperature 80°C, evaporator 150°C.

For diethylene glycol offer determination method iodometric titration and gas chromatography determination [5]. Used for the analysis of the Packed column containing Polisorb-1 Nanase who is important to him polyethylene glycol, the column temperature of 190-200°C, evaporator 290°C.

Gas chromatography does not allow simultaneous determination of the content of diethylene glycol and methanol due to the significant differences in physico-chemical properties of these compounds, which require different temperature conditions analysis. High temperature, presence of oxygen in the presence of metals contribute to the partial destruction of the designated components.

The essence of our invention: for rapid and simultaneous determination of methanol and diethylene glycol used liquid chromatography using a chromatographic complex Waters Alliance separation of the components in the chromatographic column SH1011 firm "Shodex" or similar ready column from another manufacturer in the current eluent, representing a sulfuric acid solution with a molar concentration of 2.5 mmol/DM3. Eluent is prepared from standard-titre sulfuric acid dilution in deionized water. The rate of elution of 0.8 cm3/min, temperature 30°C. is Applied refractometric detector for the registration of the refractive index difference between the eluent solutions and solutions containing desired components. The amount of injection from 1 to 100 μl. The analysis duration 16 minutes. The range of measurement of mass concentration for methane is from 0.01 to 100 g/DM 3for diethylene glycol from 0.001 to 100 g/DM3. The sample preparation does not require dilution of the investigated water until the content of the designated components 10 g/DM3more concentrated samples diluted with deionized water. Sampling is carried out according to GOST 51592-2000. Methanol is biochemically unstable connection, so samples should be stored and transported in cooled to 3-5°C or frozen. The shelf life of solutions 5 days.

For preparation of calibration solution mixture of methanol and DAG, using individual reagents brand "chemically pure for chromatography. Prepare a series of calibration solutions of mixtures of methanol and diethylene glycol breeding individual components in deionized water, get a solution with a mass concentration in accordance with table 1. Solutions to use freshly prepared.

Table 1
Component nameMass concentration of the component in solution, g/DM3
Solution No. 1Solution No. 2Solution No. 3Solution No. 4 Solution No. 5Solution No. 6
Methanol0,0010,010,11,05,010,0
Deg0,0010,010,11,05,010,0

The content of methanol and deg calculated using calibration graphs on the computer program, which is completed with chromatographic complex Alliance Waters. Examples of definitions of methanol and deg in the industrial underground storage of gas, made by the proposed method and performed by gas chromatographic methods GOST R 51104-97 (for methanol) and GOST 19710-83 (deg) are given in table 2.

Table 2
The name of the objectDefined components, g/DM3
methanoldiethylene glycol
In the proposed method is ke According to GOST R 51104-97By the proposed methodAccording to GOST 19710-83
Sandy-ë UGS2,992,070,230,03
Elano-Kurdiska UGS16,2411,84of 5.064,91
Stepnovskoe UGS45.99 per34,287,164,92

Bibliography

[1] STO Gazprom 18-2005 Hydroecological monitoring in specialized landfills placement of liquid waste in the gas industry. // OOO Scientific-research Institute of natural gases and gas technologies - VNIIGAZ. - M.: OOO promotional center gas industry, 2005

[2] LTD Website Econix-Expert. The production and supply of laboratory equipment and instruments. URL: http : //ionomer.ru (accessed on 10.02.2012)

[3] GOST R 51104-97 Gases Russian region liquefied hydrocarbon exported. Technical conditions. - M.: Russian State Standard. 1997

[4] the Description of the patent RU 2273850 the PC G01N 30/88. The method of determination of methyl alcohol in water. / Akhmetov TI, Kiyanenko GV, Gatiatullina L., Sultanova AM // OAO "Nizhnekamskneftekhim", 2005

[5] GOST 19710-83 ethylene Glycol. Technical conditions. - M: STANDARTINFORM, 2006.

The method of simultaneous determination in natural and waste waters methanol and diethylene glycol by liquid chromatography with components separation on a chromatographic column in the current eluent consisting of an aqueous solution of sulfuric acid, registration refractometric detector refractive index difference between the eluent solution and solutions containing methanol and diethylene glycol.



 

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