Method of determining tin (iv)

FIELD: chemistry.

SUBSTANCE: method of determining tin (IV) in an aqueous solution involves extraction of tin (IV) ions. Extraction is carried out by adding antipyrine, sulphosalicylic acid and calcium chloride with concentration of 0.60, 0.35 and 2 mol/l, respectively, to the solution. After phase separation, morin solution is added to the extract to form a fluorescent tin and morin complex, followed by measurement of fluorescence of the obtained solution using liquid analyser Fluorat2-3M to determine concentration of tin (IV).

EFFECT: quantitative detection of tin ions and simple analysis.

1 dwg, 1 ex

 

The invention relates to the field of analytical chemistry, and in particular to methods of determining ion tin (IV).

The way to determine the micro-ion tin (IV) includes removing it from the aqueous solution containing antipyrine and sulfosalicylic acid, which form the extraction stratifying system. Adding potassium chloride to the system antipyrine - sulfosalicylic acid - water provides quantitative extraction of tin ions. To determine the content of tin in the water after extraction shifted to the fluorescent compound with Maureen and analyze the resulting solution fluorimetric method for the fluid analyzer "Fluorat 2-3M. Thus, we receive the fullness of the extracted ion tin (IV), safe working conditions, simplification and cheapening of the process of analysis through the use of water-soluble extraction stratifying systems.

There is a method of determining the micro-ion tin (II), including removing it from the solution existentiality, benzoic acid and pyrocatechin purple in the presence of chloroethanol acid and quantitative registration spectrophotometric method (Degtev M.I., Poroshina, NV New variant of the extraction-photometric determination of tin (II) without the use of organic solvent is / Zavodskaya laboratoriya. Diagnostics of materials. 2011. T. No. 5. P.9-11). The disadvantages of the method include the need for heating systems up to 70-80°C and the use of an expensive reagent (existentiality) or its synthesis, which increases the complexity of the process.

Closest to the invention to the technical essence and the achieved result is a method for determination of tin, which involves a preliminary extraction of iodide complex tin from solutions of carbon tetrachloride, reextraction in the presence of sulfuric acid, the introduction organicheskoi dye basic blue, complexing ligandinduced and carboxymethyl cellulose and the subsequent photomatrixovina formed ion associate. (A.S. USSR №1386892 IPC G013122, publ. 07.04.1988,)

The disadvantage of the prototype: the multistage and the complexity of the analysis, the use of toxic organic solvents.

The objective of the invention is to develop an effective method for the concentration and quantitative detection of ions of tin (IV) with water stratifying system with the participation of antipyrine and sulfosalicylic acid, achieving completeness of extraction, improving the safety of working conditions by eliminating organic solvents, cheaper and significantly simplifies the process of analysis.

Set for the ache is achieved by the characteristics specified in the claims in common with the prototype, such as the method of determination of tin (IV) in aqueous solution, including extraction of ions of tin (IV) and distinctive, essential features such as the extraction of the ion tin (IV) are added to a solution of antipyrine, sulfosalicylic acid and potassium chloride with a concentration of 0.60; 0.35 and 2 mol/l, respectively, and after separation of the phases to the extract add Morin solution for formation of a fluorescent complex compounds of tin with Maureen and provide measurements of fluorescence of the resulting solution by means of a fluid analyzer "Fluorat 2-3M for determining the concentration of tin (1U).

These characteristics individually and all together aimed at solving the problem and are significant. The use of the proposed combination of characteristics in the prior art was not found, therefore the proposed solution meets the patentability criteria of "novelty".

One set of new essential features with a common, known, provides a solution to the problem is not obvious to a person skilled in this technical field and demonstrates compliance of the claimed technical solution to the patentability criterion of "inventive step".

The technical result - quantitative detection of tin ions due to the formation of water is Oh stratifying system and the simplification of the method of analysis due to the exclusion of organic solvents.

In common with the prototype is the use of extraction to opredeleniya tin (1U), and the difference is the use of extraction stratifying system phenazone - sulfosalicylic acid, after separation of the phases to the extract add Morin solution for formation of a fluorescent complex compounds of tin with Maureen and provide measurements of fluorescence of the resulting solution by means of a fluid analyzer "Fluorat 2-3M for determining the concentration of tin (1U).

The mixture of substances - antipyrine and sulfosalicylic acid in certain molar ratios (3:1,5-2,0) is a liquid, sparingly soluble in water, so in the system of phenazone - sulfosalicylic acid - water there is a separation into two liquid phases. The reason for the separation is the acid-base interaction between the components of an aqueous solution. The optimal number of antipyrine and sulfosalicylic acid equal 0,0060 and 0,0035 mol, respectively, in 10 ml of an aqueous solution that provides the most convenient for the subsequent analysis of the amount of the produced phase (1.4 to 1.9 ml). When the number of sulfosalicylic acid does not occur delamination aqueous solution, and the surface of the organic lower phase is reduced. The optimal concentration of potassium chloride is 2 mol/l (Fig.). Less soda is the content of KCl does not provide quantitative extraction of tin ions in the lower phase, more - leads to a decrease in the fluorescence of the complex tin (IV) with Maureen. In Fig. shows the dependence of the degree of extraction of ions of tin (IV) concentration in KS1 system phenazone-sulfosalicylic acid - water (CAnt=0.6 mol/l, CSSA=0.4 mol/l).

The invention is illustrated by description of a specific, but not limiting, example implementation.

Example. Neutral or slightly acidic solution containing 90 mcg tin (IV)add 1,129 g antipyrine, 0,763 g sulfosalicylic acid, 1.48 g of KCl, bring the total volume of the system with deionized water to 10 ml and intensively shaken for 1 min After stratification and separation of the phases to extract poured 3 ml of ethanol, 4 ml of 1 mol/l HCl solution prepared in deionized water, and 1 ml of 0.1%solution of Morin in ethanol, bring the volume of solution with deionized water to 15 ml and peremeshivayte 30 minutes to carry out the measurement on the analyzer liquid "Fluorat 2-3M. The concentration of tin is automatically determined using a calibration based, established in memory of the analyzer.

From the description and practical application of the present invention to specialists will be obvious and other private forms of its implementation. The description and examples are considered to illustrate the invention, the essence of which and the amount of patent is rittany defined in the following claims the set of essential features and their equivalents.

Method for determination of tin (IV) in aqueous solution, including extraction of ions of tin (IV), characterized in that the extraction of ions of tin (IV) are added to a solution of antipyrine, sulfosalicylic acid and potassium chloride with a concentration of 0.60; 0.35 and 2 mol/l, respectively, and after separation of the phases to the extract add Morin solution for formation of a fluorescent complex compounds of tin with Maureen and provide measurements of fluorescence of the resulting solution by means of a fluid analyzer "Fluorat 2-3M for determining the concentration of tin (IV).



 

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