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ISSN 2522-1841 (Online) ISSN 0005-2531 (Print)
UDC 543.42:546.74:54.412. 2
STUDY OF COMPLEX FORMATION OF Ni (II) WITH AZODERIVATIVES PIROHALLOLA IN THE PRESENCE OF CATIONIC SURFACE
ACTIVE SUBSTANCES
1 12 3
M.Tsintsadze , Ts.Tsignadze-Panchvidze , V.I.Mardanova , R.E.Mammadova ,
F.M.Chyragov2
1Georgian Technical University, Tbilisi, Georgia 2Baku State University, Baku, Azerbaijan 3Kazakh branch of Baku State University
Received 27.12.2022 Accepted 22.02.2023
The effect of the third components of cationic surfactants - chloridecetylpyridinium (CPCl), cetylpyridini-um bromide (CPBr), cetyltrimethylammonium bromide (CPMABr) for complexation of nickel (II) with 4-(2', 3', 4'-trihydroxyphenyl) -3-sulfo-5-chlorophenylazo benzene (R). Same- (NiR) and mixed-ligand complex compounds (Ni (II) -RCPCl, Ni (II) -RCPBr and Ni (II) -RCPMABr) are formed at pH 6, 4, 4 and 4, respectively. All complexes are formed immediately after mixing the solutions of the components and differ in stability. The ratio of the reacting components in the composition of same- (1: 1) and mixed-ligand (1: 1: 1) complexes are established. The interval of obedience to Beer's law is determined. The coefficients of the calibration curve equation are determined by the method of least squares. Complexation of nickel (II) is expressed by linear dependence of A = f (c) is. Stability constants of same- (NiR) and mixed-ligand complexes (Ni (II) -RCPCl, Ni (II) -RCPBr and Ni (II) -RCPMABr) are calculated. Under optimal conditions of complexation, Ni-R was titrated with a solution of third components (CPCl, CPBr and CPMABr) by conductometric method. The influence of foreign ions on complexation of nickel (II) with R in the absence and in the presence of third components was studied. A technique has been developed for the spectrophotometric determination of microquantities of nickel in the waters of the Akstafa and Jogaz rivers of the Kazakh region of the Republic of Azerbaijan.
Keywords: nickel (II), azocompounds, mixed-ligand complex, cetylpyridinium chloride, cetylpyridinium bromide, cetyltrimethylammonium bromide.
doi.org/10.32737/0005-2531-2023-2-146-153
Introduction
As is known, in modern times, nickel is widely used in electrical engineering, radio engineering and the chemical industry. In addition, nickel is used in the production of metal coatings due to its high corrosion resistance and retention of mechanical and physical properties at extreme temperatures. Nickel is used as a catalyst in the hydrogenation of organic compounds. Adding a small amount of nickel to steel increases its durability and corrosion resistance. Compared to other transition metals, nickel is moderately toxic element and still at low concentration causes a general toxic effect on the human body, causing diseases of the nasopharynx and lungs, malignant tumors and dermatological discs. It was assumed that nickel is necessary for plants and some domestic animals. Nickel-containing
wastewater is harmful after penetration into water. Therefore, the development of cost-effective, simple and rapid methods for the determination of nickel with high sensitivity and selectivity is considered an urgent task. Nickel(II) tends to form stable colored complexes with organic reagents containing donor sulfur, nitrogen, and oxygen atoms [1-5]. The most important photometric reagents include dioximes, especially di-methylglyoximes, which have long been used as the most important reagents in the study of mixed ligand nickel compounds [6-14]. Recently, the use of nitrogen compounds for the determination of nickel in complex natural and industrial objects has been expanding [15-17]. The photometric analysis method stands out among the known methods of analytical chemistry due to its simplicity and cost-effectiveness. From
this point of view, the development of methods distinguished by their high metrological characteristics is always an urgent issue.
Purpose of this work: in the presented work, the complexformation of nickel (II) with 4-(2', 3',4'-trihydroxyphenyl)-3-sulfo-5-chloro-phenylazo benzene (R) in the presence of cati-onic surfactants - cetylpyridinium chloride (CPCl), bromide cetylpyridinium (CPBr), cetyl-trimethylammonium bromide (CPMABr) was investigated by photometric method.
Experimental part
Solutions and reagents
The reagent was synthesized according to the method {18], its composition and structure established by the methods of elemental analysis and IR spectroscopy.
Cl
C12H9O7N2SQ
Calculated: % C - 39.94, H - 2.49, N - 7.77, O - 31.07, Cl - 9.85; S - 8.88. Found: % C - 39.99, H - 2.57, N - 7.84, O -31.14, Cl - 9.91, S - 8.93.
We used 1 • 10-3 M ethanol solution of the reagent and water-ethanol solutions (3: 7) of the third components, which were prepared by dissolving their exact weighed portions. A solution of nickel (II) ion was prepared from Ni-SO47H2O by dissolving an accurately weighed portion in water. Acetate-ammonia buffer solutions were used to create the required acidity. All reagents used are of analytical grade at least.
Apparatus
The absorbances of the solutions was measured on a Lamda 40 spectrophotometer (Perkin Elmer) and a KFK-2 photocolorimeter in a cuvette with a layer thickness of 1 cm. The acidity of the buffer solutions was measured on a PHS-25 ion meter adjusted with standard buffer solutions. The specific electrical conduc-
tivity of the solutions was measured on a KEL-1M2 conductometer.
Results and discussions
The absorption spectrum of the reagent was extracted in a wide range of acidity. Experiment shows that two maxima are observed in the absorption spectrum of the jet. Based on literature data [19, 20], we believe that small values of the wavelength in azo derivatives of py-rogallol characterize the quinonehydrazone form, and large values characterize the maximum illumination of the azo form. We found that R (in ethyl alcohol) at pH 6 has an absorption band with a maximum (A= 495 nm). Under these conditions, it forms a complex with nickel (II) (absorption maximum at 521 nm). The study of the obtained complex in the presence of cetylpyridinium chloride (CPCl), cetylpyri-dinium bromide (CPBr), cetyltrimethylammo-nium bromide (CPMABr) in a wide pH range showed that under the influence of the third component, a mixed-ligand complex of Ni (II) R-CPCl with a maximum light absorption X= 544 nm, Ni (II) R-CPBr X = 538 nm and for Ni (II) R-CTMABr X= 549 nm are formed. The color of the reagent and complexes depends on the pH of the medium, therefore, the absorption spectra during complexation were studied against the background of the control experiment R-CPCl, R-CPBr and R-CTMABr. Under the influence of third components, a batho-chromic effect is observed in all the resulting mixed-ligand complexes. It can be seen from the spectra of the complexes isolated on a spec-trophotometer that, under the influence of third components, a bathochromic effect is observed in all the formed mixed-ligand complexes (Figure 1).
It is known from the literature that, depending on the nature of the functional groups that make up the organic molecule, one aromatic nucleus is positively charged and the other is negatively charged, resulting in the interaction of these nuclei. As a result, a bathochromic shift is observed in the light spectrum of the lig-and.
250 300 350 400 450 500 550 600 650
Fig. 1. Absorption spectra of solutions of complexes with nickel (II): 1 -Ni(II) R, 2 - Ni (II) R - CPCl, 3 - Ni(II) R - CPBr, 4 - Ni(II) R -CPMABr, CNi =4 • 10-5 M, CR =1 • 10-4 M
Fig. 2. The dependence of the abrorbances of solutions of the complexes of Ni (II) on pH: 1 - Ni(II) R, 2 - Ni(II) R - CPMABr, 3 - Ni(II) R - CPBr, 3 - Ni(II) R -CPCl. CNi =4-10-5 M ; CR =1 • 10-4 M
The study of the dependence of the ab-sorbances on the pH of the solution showed that when interacting with cetylpyridinium chloride, cetylpyridinium bromide, cetyltrime-thylammonium bromide, the optimal conditions of complexation shift into an acidic medium at pH 6, 4, 4 and 4 in complexes, respectively (Figure 2).
To select the optimal conditions, the in-
fluence of the concentration of reactants, temperature and the influence of time on the formation of a binary and mixed-ligand complexes was studied. The yield of the Ni (II) -R complex is maximum at a concentration of 8 • 10-5 M R, Ni(II) R - CPCl at 810-5 M R and 5.2-10-5 M CPCl, Ni (II) R - CPBr at 810-5 MR and 4.8-10-5 M CPBr, Ni (II) R-CPMABr at 810-5 M R and 4-10-5 M CPMABr. All complexes are
formed immediately after mixing the solutions of the components and differ in stability.
The stability constants and the ratio of the components in the composition of the complexes were established by the methods of isomolar series, the Starick-Barbanel's relative yield method, and the method of equilibrium shift [21].
Starick-Barbanel's relative yield method allows accurate estimation of stoichiometric coefficients and can be applied to any stoichio-metric reaction, regardless of the stability of the concentration of the interacting substances. The ratio of the components in the NiR complex is 1: 1 (Figure 3).
The study showed that the ratio of components in mixed-ligand complexes is 1:1:1.
Molar coefficients of light absorption, linearity interval of the graduated graphs for the determination of nickel (II), as well as other an-
149
alytical characteristics of the reagents are given in Table 1.
To establish the influence of the stability of associates and their complexes on the detection limit of nickel(II), the coefficients of the calibration graph equation were determined using the least squares method [22].
f ^ A = a£ C + nb \ S AC = aS C2 + b£ C
Here, A is the optical density of the complex, C is the concentration of nickel (^g/ml), n is the number of experiments. The coefficients of the equation of the calibration curve were determined by the method of least squares. In the complexation of nickel (II), the dependence A = f (c) is expressed by the following linear equations.
4 1
V,
Ni, ml
Fig. 3. Determination of the composition of the Ni-R complex by the method of isomolar series: CNi =410-5 M; CR =110-4 M, VNi+VR=5 ml, pH=6, 5=490 nm.
2
3
4
3
2
VR.ml
Table 1. Spectrophotometric characteristics of nickel (II) complexes
Complex pH ^max, nM E-10-4, L/mol-SM Me:R Obedience to Beer's law, mkg/mL lgP
Ni(II)R 6 521 0.866±0.04 1:1 0,374-2,72 9.04±0.04
Ni(II)R-CPCl 4 544 1,62±0.03 1:1:1 0,12-2,32 10,39 ±0,05
Ni(II)R-CPBr 4 538 1,54±0.02 1:1:1 0,12-2,32 10,26±0.05
Ni(II)R-CPMABr 4 549 1,68±0.03 1:1:1 0,07-2,32 10,62±0.04
A=(0,17±0,02)c+(6,8±0,11)10 A=(0,26±0,0l)c+ (3,5±0,09)10-A= (0,34±0,02)c+(5,6±0,09)10-A= (0,41±0,0l)c+(4,2±0,06)10
-2
Ni(II)R Ni(II)R-CPCl Ni(II)R-CPBr Ni(II)R-CPMABr
As can be seen, with an increase in the slope angle (a) of the linear equations, the molar absorption coefficients of the complexes increase.
Under optimal conditions of complexation, Ni-R was titrated with a solution of third components (CPCl, CPBr, and CPMABr) by the con-ductometric method [23] (Table 2).
The results show that the lower is the specific electrical conductivity, the greater is the stability of the complexes.
The effect of foreign ions on the com-plexation of nickel (II) with R in the absence and in the presence of third components has been studied. It was found that in the presence of third components, the selectivity of complex-ation reactions significantly increa-ses (Table 3). These reagents are more selective for the spectrophotometric determination of nickel (II) in comparison with the reagents known from the literature [1].
Table 2. Results of conductometric titration of a Ni-R solution with a solution of the third components (CPCl, CPBr
and CPMABr (m-104 Ohm-1cm-1)
—mL 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
R 1.89 1.85 1.82 1.79 1.76 1.73 1.70 1.69 1.69 1.69
R - CPCl 1.76 1.71 1.69 1.67 1.65 1.55 1.53 1.53 1.53 1.53
R - CPBr 1.84 1.81 1.79 1.74 1.69 1.59 1.56 1.56 1.56 1.56
R - CPMABr 1.62 1.58 1.56 1.53 1.49 1.37 1.33 1.33 1.33 1.33
Table 3. Permissible ratios of foreign ions to nickel (II) when it is determined in the form of same- and mixed-ligand complexes (error 5%) ____
Foreign ions R R - CPQ R - CPB R - CPMABr 2-[(2-merkaptophenyl imino) metyl]phenol [1]
Na(I) * * * * 300
K(I) * * * * 300
Mg(II) 248 414 414 828 250
Ca(II) 207 690 270 690 250
Ba(II) 236 2364 472 2364
Zn(II) 224 224 448 448 300
Cd(II) 215 366 215 1931 50
Co(II) 61 464 215 464 20
Cu(II) ** 110 110 22 20
Mn(II) 28 940 190 940 200
Al(III) 5 93 47 93 250
Fe(III) 10 193 193 193 20
Cr(III) 179 258 258 539 20
Pb(II) 71 142 142 71
V(V) 35 176 88 176
W(VI) 197 635 634 952
Mo(VI) 331 828 372 828
F- 319 6379 6379 6379
С2О42- 22 422 217 422
HPO42- 617 1234 617 1234 300
Lemon acid 116 231 462 462
Wine acid 517 2506 2506 2506
Thiourea 1310 1572 1310 1572
Note: * - interferes; ** - does not interfere.
A technique has been developed for the spectrophotometric determination of micro-quantities of nickel in the waters of the Akstafa and Jogaz rivers of the Kazakh region of the Republic of Azerbaijan.
Determination of nickel(II) in the rivers "Akstafa" and "Dzhogaz" of the Kazakh region of the Republic of Azerbaijan.
Analysis technique
For analysis, 1 liter of water was taken from the river bank. The water was evaporated without boiling and a precipitate formed. The resulting precipitate was dissolved in 5 ml
Conclusion
1. To determine nickel by spectropho-tometric method, the azo derivative of pirohallola was used in the presence of third components.
2. The complex compounds of nickel with a reagent in the presence of third components were studied spectrophotomet-rically, the optimal conditions for complex formation and characteristics of the complexes (pHopt, Opt, molar absorption coefficients, composition of complexes, interval of obedience to Beer's law, stability constant) were determined. It was determined that in the presence of the third component, some analytical parameters increase.
3. Under optimal conditions for complex formation, Ni-R was titrated with a solution of third components (CPCl, CPBr, and CPMABr) by the conductometric method. The results show that the lower the electrical conductivity, the greater the stability of the complexes.
4. The effect of foreign ions and masking substances on complexation reactions was studied. It was found that reactions with modified forms of the reagents are characterized by higher selectivity. Alkali metals
HNO3 and transferred to a 50 ml flask and diluted to the mark with distilled water. When nickel(II) is determined by the photometric method, an aliquot of the resulting solution is placed in a 25 ml flask, 2 ml of 110-3 M R and 2 ml of 1-10-2 M CTMABr are added, and diluted to the mark with pH 4. The optical density of solutions is measured at X= 490 nm in a cuvette with l = 1 cm on KFK-2 relative to the test solution. The correctness of the procedure was checked using the ICP-OES thermo ICAP 7400 Duo instrument. The results are presented in Table 4.
and ions Ca(II), Ba(II), Mn(II), Cr(III), Cd(II) do not interfere with the determination of nickel(II).
5. These methods are highly sensitive and selective. It is a very rapid and a simple technique A technique has been developed for the spectrophotometric determination of microquantities of nickel in the waters of the Akstafa and Jogaz rivers of the Kazakh region of the Republic of Azerbaijan.
References
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II Water sample 0.188±0.004 0.194±0.004
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Ni(II)-IN PIROQALLOLUN AZO TÖROMOLORI ILO KATION SOTHl AKTIV MADDOLORLOR l§TlRAKINDA KOMPLEKSOMOLOGOTIRMOSININ TODQlQl
M.Tsintsadze, Ts.Tsiqnadze-Pançvidze. V. l. Mardanova, RE.Mammadova, F.M. Çiraqov
Kationik sathi aktiv maddalarin ûçûncû komponentlarinin - setilpiridinium xlorid (CPCl), setilpiridinium bromid (CPBr), setiltrimetilamonium bromid (CPMABr) nikelin (II) 4-(2', 3'-trihid- 4') ila komplekslaçmasina tasiri. 3-sulfo-5-xlorofenilazobenzol (R). Binar- (NiR) va qariçiq liqand komplekslari (Ni(II)-RCPCl, Ni(II)-RCPBr va Ni(II)-RCPMABr) müvafiq olaraq pH 6, 4, 4 va 4-da amala galir. Bütün komplekslar komponentlarin mahlullarini qançdirdiqdan darhal sonra amala galir va sabitdir. Binar (1:1) va qariçiq-liqandli (1:1:1) komplekslarin komponentlari nisbati müayyan edilmiçdir. Beer qanununa tabeçilik intervali müayyan edilir. Daracali ayrinin tanlik amsallari an kiçik kvadratlar üsulu ila müayyan edilir. Nikelin (II) kompleks formalaçmasi A = f (C) xatti asililigi ila ifada edilir. Binar (NiR) va qançiq-liqandli komplekslarin (Ni(II)-RCPCl, Ni(II)-RCPBr va Ni(II)-RCPMABr) davamliliq sabitlari hesablanmiçdir. Kom-pleksamalagalmanin optimal çaraitinda Ni-R kondüktometrik üsulla ûçûncû komponentlarin (CPCl, CPBr va CPMABr) mahlulu ila titrlanmiçdir. Ûçûncû komponentlar olmadiqda va mövcud olduqda nikelin(II) R ila komplekslaçmasina kanar ionlarin tasiri tadqiq edilmiçdir. içlanmiç metodika Azarbaycan Respublikasinin Qazax vilayatinda Agstafa va Cogaz çaylanmn sulannda nikelin miqdarinin spektrofotometrik tayini ûçûn tatbiq edilmiçdir.
Açar sözlzr: nikel(JJ), azo ЬЫэ§тэ1эп, qariçiq liqand kompleksi, setilpiridinium xlorid, setilpiridinium bromid, setil-trimetilammonium bromid.
ИССЛЕДОВАНИЕ КОМПЛЕКСООБРАЗОВАНИЯ Ni (II) С
АЗОПРОИЗВОДНЫЕ ПИРОГАЛЛОЛА В ПРИСУТСТВИИ КАТИОННЫХ ПОВЕРХНОСТНО-
АКТИВНЫХ ВЕЩЕСТВ
М.Цинцадзе, Ц.Цигнадзе-Панчвидзе, В.И.Марданова, Р.Э.Мамедова, Ф.М.Чирагов
Влияние третьих компонентов катионных ПАВ - хлорида цетилпиридиния (СРС1), бромида цетилпиридиния (СРВг), бромида цетилтриметиламмония (СРМАВг) на комплексообразование никеля (II) с 4-(2', 3', 4'-тригидроксифенил)-3 -сульфо-5-хлорфенилазобензол (Я). Одно- (№Я) и разнолигандные комплексные соединения (№(П)-ЯСРС1, Ni(II)-RCPBr и Ni(II)-RCPMABr) образуются при рН 6, 4, 4 и 4 соответственно. Все комплексы образуются сразу после смешения растворов компонентов и отличаются стабильностью. Установлено соотношение реагирующих компонентов в составе однолигандных (1:1) и разнолигандных (1:1:1) комплексов. Определен интервал соблюдения закона Бера. Коэффициенты уравнения калибровочной кривой определяются методом наименьших квадратов. Комплексообразование никеля (II) выражается линейной зависимостью А = f (С) is. Рассчитаны константы устойчивости однолигандных (№Я) и разнолигандных комплексов (№ (II) -ЯСРС1, № (II) -ЯСРВг и № (II) -ЯСРМАВг). При оптимальных условиях комплексообразования №-Я титровали раствором третьих компонентов (СРС1, СРВг и СРМАВг) кондуктометрическим методом. Изучено влияние посторонних ионов на комплексообразование никеля (II) с Я в отсутствие и в присутствии третьих компонентов. Разработана методика спектрофотометрического определения микроколичеств никеля в водах рек Акстафа и Джогаз Казахского района Азербайджанской Республики.
Ключевые слова: никель (II), азосоединения, разнолигандный комплекс, хлорид цетилпиридиния, бромид цетилпиридиния, бромид цетилтриметиламмония.
