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Investigation of catalytic effects of Al(III), Sc(III), Y(III) on generation of cadmium vapor in the presence of potassiumcyanide

Al(III), Sc(III), Y(III) elementlerinin potasyum siyanür varlığında kadmiyum buharı üretimine katalitik etkilerinin incelenmesi

  1. Tez No: 772039
  2. Yazar: AHMET ÇELİK
  3. Danışmanlar: PROF. DR. ZİKRİ ARSLAN
  4. Tez Türü: Yüksek Lisans
  5. Konular: Kimya, Chemistry
  6. Anahtar Kelimeler: Belirtilmemiş.
  7. Yıl: 2015
  8. Dil: İngilizce
  9. Üniversite: Jackson State University
  10. Enstitü: Yurtdışı Enstitü
  11. Ana Bilim Dalı: Analitik Kimya Ana Bilim Dalı
  12. Bilim Dalı: Belirtilmemiş.
  13. Sayfa Sayısı: 76

Özet

The objective of this study was to develop new chemical vapor generation methods for the determination of cadmium by ICP-MS. Cadmium forms volatile species when reacted with strong reducing agents, such as sodium borohydride (NaBH4). Nevertheless, the efficiency of Cd vapor generation is very poor in comparison to other vapor or hydride forming elements, such as arsenic and selenium, and mercury. Various chelating and catalytic agents have been utilized to alleviate the interferences. Among those Co-thiourea system has been popular despite its moderate efficiency and rigorous control of the experimental conditions. First row transitions metal ions have also been found to improve the generation of volatile Cd species in the presence of potassium cyanide (KCN). In this study, performances of three trivalent cations, including aluminum, Al(III), scandium, Sc(III) and yttrium, Y(III) that are known as hard Lewis acids, were investigated on generation of volatile Cd species for determination of Cd by ICP-MS. Potassium cyanide was used as masking ligand to alleviate the interferences of common transition metals and hydride forming elements. The performances of Al(III), Sc(III) and Y(III) were examined in the presence of KCN. An online chemical vapor generation manifold was built and the experimental variables influencing Cd vapor generation, such as the type and concentration of acid(s), the concentrations of KCN and Al(III), Sc(III) and Y(III), and NaBH4, the lengths of mixing tubings, the flow rates of sample solution and carrier gas were examined using a univariate method. The optimum medium for vapor generation was 4% (v/v) HCl. A concentration of 1% (m/v) KCN was sufficient for maintaining vapor generation efficiency. Optimum signals were obtained with 0.1 mol L-1 Al(III) and 0.06 mol L-1 Sc(III), and 0.08 mol L-1 Y(III). A concentration of 3% (m/v) NaBH4 solution provides the highest efficiency in Cd vapor generation. Under the optimum conditions, an enhancement of 20-, 20- and 17-fold was obtained with Al(III), Sc(III) and Y(III), respectively. The detection limits (3s) were 5.2 6.3 and 7.8 ng L-1 (ppt) for 111Cd isotope. The effects of the transition metals, alkaline earth elements, and hydride forming elements were investigated for Al(III) - KCN, Sc(III) - KCN and Y(III) – KCN systems. In all scenarios, Cu, Fe, Pb and Se induced depressive effects on Cd vapor generation. The effects of Cu and Se were marginal, while those of Fe(III) and Pb(II) were highly influential on the vapor generation. The methods were successfully applied to the determination of Cd by ICP-MS in several certified reference materials, including seawater (CASS-4), estuarine water (SLEW-3), bone ash (SRM 1400) and domestic sludge (SRM 2781). External calibration was used in seawater and estuarine water analyses. Concentrations of Fe and Pb were high in bone ash and domestic sludge samples; therefore, analyses were performed with standard additions calibration using the CVG-ICP-MS procedures

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