ICP-AES ANALYSIS OF HIGH-PURITY ARSENIC

I.I. Evdokimov, V.G. Pimenov, D.A. Fadeeva

Аннотация


The arc discharge atomic emission spectrometry method with pre-concentration of impurities is mainly used for multi-element analysis of high-purity arsenic. Spark ionization mass-spectrometry and neutron activation analysis are applied less often. The use of spark ionization mass-spectrometry and neutron activation analysis is quite problematic at the present time. Arc discharge atomic emission spectrometry in combination with pre-concentration of impurities makes it possible to determine the impurities at the level of 10−8-10−4 % mass. At the same time the number of the determined impurities is reduced (e.g., P, S, Sb, Se, Te are getting lost during concentration by matrix sublimation) with the increase in the duration of the analysis.

Thus, at the present time the express multi-element techniques of analysis of arsenic which can provide the determination of wide range of impurities at the level of 10−7-10−5 % mass. (according to the modern requirements), including the elements P, S, Sb, Se and Te (with volatility close to that of the matrix) are actually absent. In the present paper the capabilities of available and widely used method of inductively-coupled plasma atomic emission spectrometry are estimated for analysis of high-purity arsenic. The matrix interference was investigated in the process of spraying the solutions with arsenic concentration up to 150 mg/mL into inductively-coupled plasma. It was found that in order to attain low limits of quantification of impurities it is expedient to analyze sample solutions with arsenic concentration ~100 mg/mL. It does not present a problem technically. Preparation of samples in chemically resistant vials of PFA (PerFluoroAlkoxy polymer) and the use of additionally purified reagents (water, nitric acid) made it possible to decrease the effect of contaminations on the limits of quantification of most impurities. A technique for determination of 39 elements in high-purity arsenic has been developed. The diapason of determined impurities includes the most abundant metals (Al, Ca, Cu, Mg, Fe) and Si, as well as the elements usually getting lost during concentration by matrix sublimation (B, P, S, Sb, Se, Te). The limits of quantification (as well as the limits of detection) of impurities in arsenic are equal ~10−7-10−5 % mass. If necessary, the range of impurities can be widened in view of the possibilities of inductively-coupled plasma atomic emission spectrometry, the possibilities of the suggested sample preparation technique and the availability of the corresponding standard solutions of the determined elements.

Key words: high-purity arsenic, determination of impurities, inductively coupled plasma atomic emission spectrometry.

DOI:http://dx.doi.org/10.15826/analitika.2015.19.1.006


Полный текст:

PDF (Russian)

Литература


Rtskhiladze V.G. Mysh'iak [Arsenic]. Moscow, Metallurgiia, 1969, 187 p. (in Russian).

OST 6-12-112-73. Mysh'iak metallicheskii dlia poluprovodnikovykh soedinenii os.ch. [Industrial Standard 6-12-112-73. Ultrapure metallic arsenic for semiconductor products]. Moscow, Ministerstvo khimicheskoi promyshlennosti, 1973, 27 p. (in Russian).

Deviatykh G.G., Churbanov M.F. Vysokochistye khal'kogeny. Monografiia [High-purity chalcogenides. Monograph]. Nizhnii Novgorod, Izdatel'stvo NNGU, 1997, 244 p. (in Russian).

Nemodruk A.A. Analiticheskaia khimiia mysh'iaka [Analytical chemistry of arsenic]. Moscow, Nauka, 1976, 224 p. (in Russian).

Maslennikov B.M., Romanova L.V. [Spectral and spectrochemical determination of copper, iron, antimony, and phosphorus in arsenic]. Metody analiza veshchestv vysokoi chistoty [Methods for analysis of high-purity substances]. Moscow, Nauka, 1965, pp. 228-230. (in Russian).

Maslova A.I., Trofimov N.V., Romanova L.V., Novoselova L.M. [Spectrographic analysis of high-purity arsenic]. Poluchenie i analiz chistykh veshchestv [Production and analysis of pure substances]. Gor'kii, GGU, 1982. Рp. 73-75 (in Russian).

Solodovnik S.M., Goriushina V.G., Brodskaia V.D., Nazarova M.G., Lushina V.K. [A Spectrographic method for the analysis of arsenic of high purity after chemical concentration of impurities]. Zhurnal analiticheskoi khimii [Journal of Analytical Chemistry], 1967, vol. 22, no. 7, pp. 1054-1057 (in Russian).

Vlasov V.S., Popova G.D., Krasnikova G.V., Iudelevich I.G. [The spectral analysis of metallic arsenic using extraction]. Zavodskaia laboratoriia [Industrial laboratory], 1973, vol. 39, no. 9, pp. 1048-1050 (in Rusian).

Otmakhov 3.I., Chashchina O.V., Slezko N.I. [The use of ion exchange resins for the concentration of impurities of arsenic and arsenic trichloride]. Zavodskaia laboratoriia [Industrial laboratory], 1969, vol. 35, no. 6, pp. 685-687 (in Russian).

Karpel' N.G., Shaparova V.V., Shtif S.L. [The spectral determination of impurities in arsenic, gallium arsenide and silicon carbide]. Metody analiza veshchestv vysokoi chistoty [Methods for analysis of high-purity substances]. Moscow, Nauka, 1965, pp. 224-228 (in Russian).

Shelpakova I.R., Rossin A.E., Chanysheva T.A., Shcherbakova O.I., Krbchkov V.G. [Atomic-emission determination of impurities in high-purity arsenic with preliminary distillation of base in the form of oxide]. Vysokochistye veshchestva [High-Purity Substances], 1991, no. 5, pp. 170-175 (in Russian).

Pimenov V.G., Bondarenko A.V. [Atomic emission analysis of high-purity arsenic with the concentration of impurities by matrix distillation from the electrode with a nozzle]. Analitika i kontrol' [Analysis and control], 2002, vol. 6, no. 1, pp. 33-39 (in Russian)

Saprykin A.I., Nenashev B.G. [Study of ultrapurification of arsenic by spark source mass-spectrometry]. Vysokochistye veshchestva [High-Purity Substances], 1993, no. 2. pp. 91-103 (in Russian).

Kuz'min N.M., Vlasov V.S., Bokova T.A. [Radioactivation Analysis of Arsenic]. Zhurnal analiticheskoi khimii [Journal of Analytical Chemistry], 1972, vol. 27, no. 9, pp. 1807-1810 (in Russian).

Gaivoronskii P.E., Pimenov V.G. [Apparatus for purifying liquids from non-volatile impurities]. Zavodskaia laboratoriia [Industrial laboratory], 1984. vol. 50, no. 6. pp. 20-21 (in Russian).

Lidin R.A., Molochko V.A., Andreeva L.L. Khimicheskie svoistva neorganicheskikh veshchestv [Chemical properties of inorganic substances]. Moscow, Khimiia, 1996, 480 s. (in Russian).

Mocak J., Bond A.M., Mitchell S., Scollary G. A statistical overview of standard (IUPAC and ACS) and new procedures for determining the limits of detection and quantification: Application to voltammetric and stripping techniques. IUPAC Technic al Report 1997. Pure and Applied Chemistry, 1997, vol. 69, pp. 297-328.

GOST R 54500.3–2011/ Rukovodstvo ISO/MEK 98–3:2008. Neopredelennost' izmereniia. Chast' 3. Rukovodstvo po vyrazheniiu neopredelennosti izmereniia [State Standard R 54500.3–2011/ ISO/IEC Guide 98–3:2008. Uncertainty of measurement. Part 3: Guide to the expression of uncertainty in measurement]. Moscow, Standartinform Publ., 2012, 101 p. (in Russian).

Tsygankova A.R., Makashova G.V., Shelpakova I.R. [The element's spectral lines intensity dependence on ICP-plasma power and argon flow rate]. Metody i ob"ekty khimicheskogo analiza [Methods and objects for chemical analysis], 2012, vol. 7, no. 3, pp. 138-142 (in Russian).

Bekov G.I., Boitsov A.A., Bol'shov M.A., Grinzaid E.L., Drobyshev A.I., Zil'bershtein Kh.I., Katskov D.A., Petrov A.A., Podmoshenskaia S.V., Prudnikov E.D., Iufa B.Ia. Spektral'nyi analiz chistykh veshchestv. 2-e izd., pererab. i dop. [Spectral analysis of pure substances. 2nd ed.]. St. Petersburg, Khimiia Publ., 1994, 336 p. (in Russian).

Zelentsova L.V., Iudelevich I.G. [Atomic absorption analysis of high-purity arsenic]. Zhurnal analiticheskoi khimii [Journal of Analytical Chemistry], 1983. vol. 38, no. 8, pp. 1404-1407 (in Russian).


Ссылки

  • На текущий момент ссылки отсутствуют.