Method for combined detection of transition metal ions in natural and waste water through high-performance liquid chromatography

FIELD: chemistry.

SUBSTANCE: invention can be used for simultaneous determination of content of ions of transition metals Fe(III), Fe(II), Cu, Pb, Zn, Ni, Co, Cd, Mn in natural, surface, waste, underground water and water extracts of saline soil. High-performance liquid chromatography is used for simultaneous determination of content of ions with separation of the ions in a chromatographic column in eluent flow. The eluent consists of a solution of sodium octane sulphonate, sodium hydrotartrate and acetonitrile in dionised water. Mixing is then carried out in a post-column reaction module with a reagent which is a solution of PAR ([4-(2-pyridylazo) resorcinol], glacial acetic acid and aqueous ammonia in deionised water. Further, the difference in optical absorption of the eluent and complexes of the determined ions with the added reagent is detected using spectrophotometric detector in the visible spectrum at 520 nm.

EFFECT: increased accuracy, faster simultaneous determination of content of transition metal ions in natural, surface, waste, underground water and water extracts of saline soil.

2 tbl

 

The invention relates to the field of analytical chemistry and can be used for simultaneous determination of the content of transition metal ions Fe(III), Fe(II), Cu, Pb, Zn, Ni, Co, Cd, Mn in natural, surface, waste, underground waters and water extracts of saline soils. Actual use of the invention in the analysis of associated wastewater, oil and gas industry. The presence of ions of iron and other transition metals can be explained as the result of corrosion of downhole equipment. Oxide iron(III) in groundwater usual composition is present in the form of colloids in concentrations of a few mg/DM3, ferrous iron(II) exists in ionic form, in the absence of oxygen in a sustainable and can meet in quantities of several tens of mg/DM3. When disposing of the wastewater in the oil and gas industry by pumping the wastewater in deep horizons there is a restriction on the content in the industrial iron(III), which is able to degrade the injection well due to sludging. Known spectrophotometric, atomic absorption and other methods for the determination of these metal ions, such as [1-3]. As a rule, is determined by one of the above mentioned ions, others interfere with the determination, require the prior removal or masking. For each component the and required extensive range of expensive chemicals. Iron ions are determined summarily, as total iron. The application of the method of high performance liquid chromatography provides a simple, rapid and highly sensitive method for the separation and determination of the content of transition metal ions. Manufacturers liquid chromatograph offer a chromatographic column for the separation and determination of transition metal ions, publish corporate information releases with examples of use of its products [4-7]. But the international standards organization (ISO) to determine the heavy metals they are missing.

Also known chromatographic method for the simultaneous determination of ions of cadmium, lead, zinc, Nickel and copper (patent of Russian Federation №2037824 IPC 6 G01N 30/06, publ. 19.06.1995,) [8] pre-treatment of the sample by the combined diethyldithiocarbamate sodium dividing Filatov metals in the chromatographic column in the flow of the mobile phase (eluent)containing acetonitrile, water and chloroform, and the subsequent UV-detection components. The disadvantages of this method include the need for prior sample preparation and is not wide enough set of transition metals for simultaneous determination.

The essence of our invention: for fast, simultaneous determination soda is a place of transition metal ions, and for iron ions in different oxidation States is used HPLC using chromatographic complex Waters Alliance with the separation of ions through column chromatography Delta-Races With 18 firms Waters or equivalent from another manufacturer in the current offer us eluent. Eluent is prepared by serial dilution in a liter of deionized water, 2 mmol octanesulfonate sodium, 35 mmol hydrotartrate of sodium and 50 ml of acetonitrile. The rate of elution of 0.8 ml/min, temperature 25°C. After separation of the metal ions come in poleconomy reaction module, where it is mixed with poleconomy reagent with the formation of colored complexes. The reagent is prepared by serial dilution in deionized water and 0.2 mmol of PAIRS ([4-(2-pyridylazo) resorcinol]), 1 mol of glacial acetic acid and 3 mol of water of ammonia. The feed rate into the reaction module reagent 0.5 ml/min, temperature 25°C. is Applied spectropho-tematicheskie detector to register the difference between the optical absorptions of eluent and complexes of defined ion reagent in the visible spectrum radiation at λ=520 nm. The amount of injection from 1 to 100 μl. The analysis duration 25 minutes. The range of measurement of mass concentration for different transition metal ions from 0.1 to 20 mg/DM3. More concentrated analyzed water samples of Rabba who are. Sample preparation is diluted canned according to GOST R 51592 samples of the investigated water solution of nitric acid in deionized water at a concentration of 0.01 mol/DM3. For preparation of calibration solutions of mixtures of ions of transition metals used state standard (GSO) of aqueous solutions of individual ions with a mass concentration of 1.0 mg/cm3. For calibration of the required aliquots GSO diluted in nitric acid in a concentration of 0.01 mol/DM3. Prepared a series of solutions recommended nominal ion concentration in the calibration solutions are shown in table 1

Cu
Table 1
The name ionMass concentration of the ion in solution, mg/DM3
Solution No. 1Solution No. 2Solution No. 3Solution No. 4Solution No. 5Solution No. 6
Fe(III)0,21,02,04,010,020,0
0,10,51,02,05,010,0
Pb0,50,51,02,05,010,0
Zn0,10,51,02,05,010,0
Ni0,10,51,02,05,010,0
Co0,10,51,02,05,010,0
Cd0,10,51,02,05,010,0
Fe(II)*0,21,02,0 4,010,020,0
Mn0,10,51,02,05,010,0
Note - Calibration solutions of Fe(II) is prepared according to GOST 4212. The calibration of Fe(II) is carried out separately. Solutions used freshly prepared.

The content of the transition metal ions are calculated from the calibration graphs on the computer program, which is completed with chromatographic complex Alliance Waters. Examples of determination of transition metal ions in industrial underground gas storage are given in table 2.

Table 2
The name of the objectDefined metals, mg/DM3
Fe(III)CuPbZnNiCoCdFe(II)Mn
Sandy-Umecka UGS 25,110,36OTC1,350,29OTCOTC5,43OTC
Elano-Kurdiska UGS203,20to 2.29OTC1,260,28OTCOTC32,80OTC
Stepnovskoe UGS145,801,69OTC0,310,39OTCOTC19,39OTC
Algayskom rayons field SLE 1122,40OTCOTC0,032,50OTC38,20213,804,30

Bibliography

[1] the PND f 14.1:2:4.139-98. The method of measurement of the masses of the o concentrations of iron, cobalt, manganese, copper, Nickel, silver, chromium and zinc in samples of drinking water and waste water by atomic absorption spectrometry. - M.: State Committee of the Russian Federation on environmental protection, 1998, (edition of 2004).

[2] the PND f 14.1:2.2-95. The method of measurement of mass concentration of total iron in natural and waste waters by the photometric method with on-phenantroline. - M.: the Ministry of environment protection and natural resources of the Russian Federation, 1995 (edition of 2004).

[3] USSR GOST 4011-72 drinking Water. Methods of measuring the mass concentration of total iron. - M.: Publishing house of standards,

[4] parts Catalog, chromatography columns and accessories Waters (Waters quality parts, chromatography columns and supplies catalog), 2006-2007, s.

[5] Dmiso, JAL. Comparison of methods of exchange and obraniakowi chromatography for determination of transition metal ions (D. Michaud and J. Krol. A comparison of exchange and reverse phase chromatographie for transition metal ion analysis). Lab. Highlights (Lab Highlights), 0393 4/89 - Waters.

[6] Warren, JAL. Application software WISE: Optimizing mixed eluent tartrate/citrate for the analysis of transition metals (V.Warren, J.Krol. Application of WISE Software: Optimization of a tartrate / citrate blended eluent for transition metal analysis). Lab. Highlights (Lab Highlights). 0413 6/89 - Water.

[7] the Determination of transition metals by ion chromatography (De-Terminanions of Transitions Metals by Ion Chromatography). Technical Note 10. - Dionex.

[8] the Description of the patent RU №2037824 IPC 6 G01N 30/06. The method of simultaneous qualitative and quantitative determination of cadmium, lead, zinc, Nickel and copper. / Sosnina M.V., Motylev S.M. 1995

The method of simultaneous determination in natural and waste waters ions iron(II), iron(III), copper, lead, zinc, Nickel, cobalt, cadmium, manganese using high-performance liquid chromatography separation of the ions on the chromatographic column in the current eluent consisting of an aqueous solution octanesulfonate sodium, hydrotartrate sodium and acetonitrile, and subsequent mixing in polukolonnoy reaction module with the reagent, representing aqueous solution PAIRS ([4-(2-pyridylazo)resorcinol], glacial acetic acid and aqueous ammonia; registration spectrophotometric detector differential optical acquisitions eluent and complexes defined ions with the reagent in the visible spectrum radiation at a = 520 nm.



 

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