Nickel spectrophotometric determination

Burke and Yoe (8) described the simultaneous spectrophotometric determination of cobalt and nickel in acidic ethanol. An analogous procedure in acidic dimethylformamide (DMF) was described by Ayers and Annand (3). By simultaneously solving Beer s law equations, the concentration of each metal can be determined (Eqs. 1 and 2). In general, the results of these two methods were similar. However, Burke and Yoe (8) found that iron and copper interfered with the measurement while Ayers and Annand (3) found interference from manganese. 

An alternative to qdt, (.S )-2-(3-mercaptoquinoxalinyl)thiourinium, is stable and soluble in aqueous ethanol solutions unlike qdt (27). At pH 10 in ammonia-ammonium chloride buffer, this reagent hydrolyzes to qdt. (5)-2-(3-Mercapto-quinoxalinyl)thiourinium has been used for the simultaneous detection of nickel and cobalt and the determination of palladium (27, 28). A related reagent, 6-nitro-(S)-2-(3-mercaptoquinoxalinyl)thiourinium has also been used in metal analysis (7). This reagent is hydrolyzed in ammonia buffer to generate 6-nitro-2,3-quinoxalinedithiol (nqdt). Following adjustment to pH 2.0, the mixture is extracted with methyl isobutyl ketone and spectrophotometrically analyzed. 6-Nitro-(5)-2-(3-mercaptoquinoxalinyl)thiourinium has been used for the simultaneous spectrophotometric determination of nickel and cobalt by the quantification of [Ni(nqdt)2]2 (710 nm, e = 20,700 L mol 1cm 1) and [Co(nqdt)2]2 (530 nm, e = 40,000 L moE cm-1), respectively. 

The methods described in detail in Section 36.2, or only mentioned, have been used as follows for spectrophotometric determination of palladium the thio-Michler s ketone — in silver, copper, and anodic slime [32], in catalysts [31] with thiosemicarbazide derivatives — in water [44] and alloys [46] with palladium-carbon powder — with a-benzilmonoxime [48] with PAR — in catalysts and ores [58] with thiazolylazo derivatives — in Ni-Al catalysts [63] with 5-Br-PADAP — in titanium alloys with pyridylazo derivatives - in nickel alloys [68] with sulphonitrophenol - in silver alloys [70] with Arsenazo III — in iron and meteorites and with Palladiazo — in catalysts, minerals, silica gel, and calcium carbonate [78]. 

F. Albertus, A. Cladera, E. Becerra, V. Cerda, A robust multi-syringe system for process flow analysis. Part 3. Time based injection applied to the spectrophotometric determination of nickel(II) and iron speciation, Analyst 126 (2001) 903. 

Different components such as reactors, detectors and mini-columns can be added to or removed from the manifold in order to improve system performance but the strategy can lead to occurrence of the Schlieren effect. Reactor interchange has been used to attain two different analytical signals under two different sample handling conditions, thus allowing the implementation of differential kinetics. The feasibility of this approach was demonstrated in relation to the spectrophotometric determination of cobalt and nickel in steels [110]. The method involved complexation with citrate followed by time-dependent dissociation and reaction with 4-(2-pyridylazoresorcinol). 

The spectrophotometric determination of cobalt and nickel using 2-hydroxybenzaldehyde thiosemicarbazone [48]. 

Since the pioneering work of Chimside et al. on the spectrophotometric determination of boron in metallic nickel [23], electrolytic dissolution has been exploited for the direct analysis of several solid conductive materials, including metals, ores and alloys. 

Spectrophotometric determination of the extractable content of chromium, lead, nickel and zinc in sewage sludges. A similar strategy to the above-mentioned [355] was used but different standard solution streams were involved. Matrix effects were successfully overcome [356],... 

R. Kuroda, T. Mochizuki, Continuous spectrophotometric determination of copper, nickel and zinc in copper-base alloys by flow-injection analysis, Talanta 28... 

RET/HUM] Retajczyk, T. F., Flume, D. N., Spectrophotometric determination of the stability constant of nickel(II) bromide in lithium bromide medium, Tek. Hoegsk. Handl., 264, (1972), 219-226. Cited on pages 140,153,156,265,356. 

R. Kuroda and T. Mochizuki, Continuous Spectrophotometric Determination of Copper, Nickel and Zinc in Copper-Base Alloys by Flow Injection Analysis. Talanta, 28 (1981) 389. 

L. K. Shpigun, I. Y. Kolotyrkina, and Y. A. Zolotov, Flow-Injection Analysis. Spectrophotometric Determination of Nickel [in Russian]. Zh. Anal. Khim., 41 (1986) 1224. 

The most usual method of spectrophotometric determination of nickel is using the reaction with dimethylglyoxime and an oxidizing agent (bromine, for example) in alkaline solution to form a red soluble complex (445 nm). 

Katiyar, G. S. Haidar, B. C. Rapid extraction and direct spectrophotometric determination of nickel(II) with isonitrosothiocamphor. Indian J. Chem. 1983, 22A, 1084-1085. 

I. Tsukahara and T. Yamamoto. Extraction-spectrophotometric determination of traces of bismuth in lead, copper and nickel metals, and in copper-base alloys with tri-M-octylamine. Analytica Chimica Acta 64 337-344, 1973. 

B.D. Oztiirk, H. FiUk, E. Tiitem, and R. Apak. Simultaneous derivative spectrophotometric determination of cobaltJII) and nickel(II) by dithizone without extraction. Talanta 53 263-269,2000. 

Nickel also is deterrnined by a volumetric method employing ethylenediaminetetraacetic acid as a titrant. Inductively coupled plasma (ICP) is preferred to determine very low nickel values (see Trace AND RESIDUE ANALYSIS). The classical gravimetric method employing dimethylglyoxime to precipitate nickel as a red complex is used as a precise analytical technique (122). A colorimetric method employing dimethylglyoxime also is available. The classical method of electro deposition is a commonly employed technique to separate nickel in the presence of other metals, notably copper (qv). It is also used to estabhsh caUbration criteria for the spectrophotometric methods. X-ray diffraction often is used to identify nickel in crystalline form. 

Spectrophotometric methods may often be applied directly to the solvent extract utilising the absorption of the extracted species in the ultraviolet or visible region. A typical example is the extraction and determination of nickel as dimethylglyoximate in chloroform by measuring the absorption of the complex at 366 nm. Direct measurement of absorbance may also be made with appropriate ion association complexes, e.g. the ferroin anionic detergent system, but improved results can sometimes be obtained by developing a chelate complex after extraction. An example is the extraction of uranyl nitrate from nitric acid into tributyl phosphate and the subsequent addition of dibenzoylmethane to the solvent to form a soluble coloured chelate. 

Discussion. Minute amounts of beryllium may be readily determined spectrophotometrically by reaction under alkaline conditions with 4-nitrobenzeneazo-orcinol. The reagent is yellow in a basic medium in the presence of beryllium the colour changes to reddish-brown. The zone of optimum alkalinity is rather critical and narrow buffering with boric acid increases the reproducibility. Aluminium, up to about 240 mg per 25 mL, has little influence provided an excess of 1 mole of sodium hydroxide is added for each mole of aluminium present. Other elements which might interfere are removed by preliminary treatment with sodium hydroxide solution, but the possible co-precipitation of beryllium must be considered. Zinc interferes very slightly but can be removed by precipitation as sulphide. Copper interferes seriously, even in such small amounts as are soluble in sodium hydroxide solution. The interference of small amounts of copper, nickel, iron and calcium can be prevented by complexing with EDTA and triethanolamine. 

A multiwavelength approach might have been considered as an alternative to chemical derivatisation. Ruddle and Wilson [62] reported UV characterisation of PE extracts of three antioxidants (Topanol OC, Ionox 330 and Binox M), all with identical UV spectra and 7max = 277 nm, after reaction with nickel peroxide in alkaline ethanolic solutions, to induce marked differentiation in different solvents and allow positive identification. Nonionic surfactants of the type R0(CH2CH20) H were determined by UV spectrophotometry after derivatisation with tetrabromophenolphthalein ethyl ester potassium salt [34]. Magill and Becker [63] have described a rapid and sensitive spectrophotometric method to quantitate the peroxides present in the surfactants sorbitan monooleate and monostearate. The method, which relies on the peroxide conversion of iodide to iodine, works also for Polysorbate 60 and other surfactants and is more accurate than a titrimetric assay. 

S. Trevin, F. Bedioui, and F. Devynck, Electrochemical and spectrophotometric study of the behavior of electropolymerized nickel prophyrin films in die determination of nitric oxide in solution. Talanta 43,... 

Nickel has been determined spectrophotometrically in seawater in amounts down to 0.5 xg/l as the dimethylglyoxime complex [521,522], In one procedure [521] dimethylglyoxime is added to a 750 ml sample and the pH adjusted to 9 -10. The nickel complex is extracted into chloroform. After extraction into 1M hydrochloric acid, it is oxidised with aqueous bromine, adjusted to pH 10.4, and dimethylglyoxime reagent added. It is made up to 50 ml and the extinction of the nickel complex measured at 442 nm. There is no serious interference from iron, cobalt, copper, or zinc but manganese may cause low results. 

In another procedure [522] the sample of seawater (0.5-3 litres) is filtered through a membrane-filter (pore size 0.7 xm) which is then wet-ashed. The nickel is separated from the resulting solution by extraction as the dimethylglyoxime complex and is then determined by its catalysis of the reaction of Tiron and diphenylcarbazone with hydrogen peroxide, with spectrophotometric measurement at 413 nm. Cobalt is first separated as the 2-nitroso-1-naphthol complex, and is determined by its catalysis of the oxidation of alizarin by hydrogen peroxide at pH 12.4. Sensitivities are 0.8 xg/l (nickel) and 0.04 xg/l (cobalt). 

After adjusting to 2 mol 1 1 in hydrochloric acid, 500 ml of the sample is adsorbed on a column of Dowex 1-XS resin (Cl form) and elution is then effected with 2 M nitric acid. The solution is evaporated to dryness after adding 1M hydrochloric acid, and the tin is again adsorbed on the same column. Tin is eluted with 2 M nitric acid, and determined in the eluate by the spectrophotometric catechol violet method. There is no interference from 0.1 mg of aluminium, manganese, nickel, copper, zinc, arsenic, cadmium, bismuth, or uranium any titanium, zirconium, or antimony are removed by ion exchange. Filtration of the sample through a Millipore filter does not affect the results, which are in agreement with those obtained by neutron activation analysis. 

In a method for the determination of copper, nickel, and vanadium in seawater, Shijo et al. [840] formed complexes with 2-(5-bromo-2 pyridylazo)-5-(N-propyl-N-sulfopropylamino) phenol and extracted these from the seawater with a xylene solution of capriquat. Following back-extraction into aqueous sodium perchlorate, the three metals were separated on a C is column by HPLC using a spectrophotometric detector. 

In a standard official method [50], the plant material is prepared for analysis by either digestion with 60% wlw perchloric acid, 70% wlw nitric acid, 1 3 mlv, and digestion of the residue with 2 M hydrochloric acid, or by dry combustion at 500 °C followed by extraction of the residue with 6 M hydrochloric acid. The concentration of nickel in these extracts is determined by AAS at 232.0 nm employing either background correction, or by an AA spectrophotometric procedure involving formation of the nickel ammonium pyrrolidiniedithio-carbamate followed by chloroform extraction. 

Arsenic (Note The atomic absorption spectrophotometric graphite furnace methods for arsenic, lead, mercury, and nickel in this monograph were developed at the National Marine Fisheries Service (NMFS) Southeast Fisheries Science Center, Charleston Laboratory, for the determination of these trace element contaminants in materials derived from fish oil. This method is intended for the quantitation of arsenic, lead, mercury, and nickel in marine oils at levels as low as 0.10 pg/g for arsenic and for lead and as low as 0.50 (xg/g for mercury and for nickel.)... 

The thiocyanate method has been used for determining cobalt in vitamin B12 [94], steel [24,94], and nickel [25]. Cobalt present in considerable amounts in alloys with aluminium, nickel, chromium, manganese, copper, and iron was determined by the differential spectrophotometric analysis [95]. 

The most impoitant spectrophotometric reagents for determining nickel are dioximes, which give specific and fairly sensitive methods. An example of a very sensitive method is one using the azo reagent 5-Br-PADAP. 

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