SU1206659A1 - Method of determining alkylenephosphonic acids - Google Patents

Abstract

The invention relates to analytical chemistry, in particular to the definition of alkylene phosphonic acids, and can be used in the analysis of natural waters and air. The purpose of the invention is to increase the selectivity of the method. The determination is carried out by treatment of the sample with manganese sulfate, hydrogen peroxide, arylamine at pH 4.5-6.5 in the presence of a titanium salt. Manganese sulphate is used in an amount to establish an excess concentration of 2-10 - 1-10 M. Photographic solution is obtained. (The ions M (II), cobalt (II), nickel (II), EDTA, ..NTA do not interfere with the determination. Table 3. Table 3 ao O) ate; O

Description

 one

The invention relates to analytical chemistry, and specifically to methods for the kinetic determination of alkylene phosphonic acids (ROS).

The aim of the invention is to increase the selectivity of the method by increasing the selectivity of the activating effect of alkylene phosphonic acids on the redox reaction.

Example 1. V1ML of river water was injected with 1 µg of hydroxyethylene diphosphonic acid (HSPD), 0.5 ml of W of a solution of hydrogen peroxide, 0.5 ml of a 0.1 M solution of manganese sulfate, 0.1 ml of a solution of titanium (IV) with content of 10 μg / l l, 1 ml of W of acetate buffer solution with pH 5.5, water up to 4.5 ml, 0.5 ml of 0.1 M solution of O-phenylenediamine. At the same time, a calibration curve is constructed; for this, B five tubes are injected, respectively, O, 1.0; 2.0; 4.0 and 10.0 µg HEDP and all of the indicated reagents, as well as water up to 4.5 ml. 0.5 ml 0.1 M O-Phenylenediamine solution (plenty of 5 ml solution volume) is poured into all tubes, the solutions are stirred by shaking, and after 30 minutes they are photometted on a photo-electrocolorimeter with a blue light filter (440 nm) in 1 cm cuvettes. The content of HEDP found on the calibration curve is 1.1 μg. The relative standard deviation of the four definitions is 0.10.

Example 2. K1ML of the analyzed solution containing 10 μg of nitrilotrimethylene phosphonic acid (NTF), add 0.5 ml of 1M hydrogen peroxide solution, 1 ml of 0.01M solution of manganese sulfate, 0.5 ml of titanium solution (W) with a content of 1 μg / ml , 1 ml of 1M acetate buffer solution with pH 5.5 and water up to 4.5 ml, 0.5 ml of a 0.1M solution of o-phenylenediamine. At the same time, a calibration curve is constructed; for this, 0 are entered into five tubes, respectively; 1.0; 2.0; 4.0 and 10.0 µg NTF and all of the indicated reagents, as well as water up to 4.5 ml. 0.5 ml of 0.1 M O-phenylenediamine (total volume of solution is 5 ml) is poured into all tubes, the solutions are stirred by shaking, and after 30 minutes they are photometted using a photoelectric colorimeter with a blue light filter (440 nm) in 1 cm cuvettes. For calibration curve found

ten

20

25

066592

9µg NTF. The relative standard deviation of the five measurements is 0.08.

Example 3. K1ml of the analyzed solution containing 5 μg HEDP is added 0.5 ml of W hydrogen peroxide solution, 0.1 ml of 0.01 M manganese sulfate solution, 0.1 ml of titanium solution (M /).

10 μg / ml, 1 ml of 1 M acetate buffer solution with pH 4.5, water to 4.5 ml, 0.5 ml of 0.1 M solution of h-aminophenol. Next, proceed as in example 1. According to the calibration curve,

J5 constructed in Example 1, 5 μg HEDP was found. The relative standard deviation of the five measurements is 0.12.

Example 4. K1 ml of the test solution containing 1 μg NTF is added 0.5 ml of W of hydrogen peroxide solution, 0.4 ml of 0.01 M manganese sulfate solution, 0.5 ml of titanium (IV) solution with a content of 1 μg / ml, 1 ml of W of acetate buffer solution with pH 6.5, water up to 4.5 ml, 0.5 ml of 0.1 M solution of O-aminophenol. Then they proceed as in example 2. According to the calibration curve, Q fica, built in example 2, 1.1 μg NTF were found. The relative standard deviation of four measurements is 0.13.

Example 5. To 1 ml of the analyzed solution containing 10 μg HEDP, 0.5 is poured. ml of hydrogen peroxide solution, 0.5 ml of 0.02 M manganese sulfate solution, 0.2 ml of titanium solution (IV) with a content of 10 μg / ml, 1 ml of III of acetate buffer solution with a pH of 6.5, water. Do4,5mp, 0, 5mpO, 1 M solution of g-phenylenediamine. Next, proceed as in example 1. According to the calibration curve, built in example 1,

5 found 5.2 μg HEDP. The relative standard deviation of the five measurements is 0.10.

Example 6. K1ml of the analyzed solution containing 5 μg

50 NTF, poured 0.5 ml of 1M solution. hydrogen peroxide, 0.5 ml of 0, W of manganese sulphate solution, 0.5 ml of titanium (N) solution with a content of 1 μg / ml, 1 ml of 1 M acetate bu55 fer solution of pH 4.5, water up to 4.5 ml, 0.5 ml of 0.1 M solution of al-acid. Next, proceed as in example 2. According to the calibration curve, 35

40

4.9 microns of NTF were found in Example 2, the relative standard deviation of four measurements is 0.12.

Table 1 shows the ranges of pH values and manganese (II) sulfate concentrations implemented in Examples 1-6, and Table 2 gives examples of the determination of alkylene phosphonic acids under conditions other than optimal.

When the pH value is less than 4.5 and more than 6.5 and when the concentration of manganese (H) is less than 2 to 10 m, the detection sensitivity decreases by 30-40%; when the concentration of manganese is more than 110 M, precipitation of manganese compounds () and closure of the solutions are possible. by strangers. metal ions, which makes it impossible to determine the ROS by the proposed method.

Table 3 shows the characteristics of the known and proposed methods.

From the data of table 3 it is clear that the known method. does not allow to determine practically important phosphonic acids of NTP and HEDP, and the proposed

2 1

2066594

The method is universal - it allows you to define not only NTF. HEDP, but also other phosphonic acids (GMDTP, DFT, etc.). In this case, the determination of phosphonic acids by the proposed method does not interfere with comparable amounts of manganese ions (C), cobalt (H), nickel (I), EDTA, NTA, i.e. The method is more selective than known.

1b

Claims (1)

Invention Formula The method of determining alkylenephosphonic acids by treating the sample being analyzed with manganese sulfate, an oxidizing agent and a reducing agent, followed by photometry of the solution obtained, characterized in that, in order to increase the selectivity of the method, hydrogen peroxide is used as an oxidizing agent; , 5 in the presence of a titanium salt (W), and manganese sulphate is taken in an amount to establish an excess concentration of 2-10. Table 1 Known method O-Dianisidine, potassium periodate, manganese (A) 1 -10 Leukosobenie p / fuchsin, potassium periodate, manganese (t) The proposed method Iron (I, Ш), lyuminr1y (iij), (3-5) 10 Copper (IG) ) Other phosphonic acids are inhibitors, their definition is impossible. It is also possible to determine GMDTF, DFT, etc. Editor I.Nikolaychuk Compiled by V.Gladkov Tehred O. Niece Proofreader L. Pilipenko Order 8702/44 Circulation Subscription VNIIPI USSR State Committee on affairs of invention 14 and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5 Branch PPP Patent, Uzhgorod, st. Project, 4 Table 2 6 6 Manganese (E), copper (P), iron (1, g), cobalt (I), NTA, EDTA Manganese (I) copper (), iron (H, i) aluminum (W), cobalt (IL), NTA, EDTA IDF ) ADMF ") NTF OEDF