In geological samples

The quantitative imaging capability of the NMP is one of the major strengtiis of the teclmique. The advanced state of the databases available for PIXE [21, 22 and 23] allows also for the analysis of layered samples as, for example, in studying non-destmctively the elemental composition of fluid inclusions in geological samples. 

The X-ray determination of REE in geological samples is normally complicated by the relatively low concentrations of the REE, their complex X-ray spectra, the high concentration of matrix elements and the lack of reference standards with certified values for REE. A rapid and sensitive ion exchange and X-ray fluorescence procedure for the determination of trace quantities of rare earths is described. The REE in two U.S.G.S. standards, two inhouse synthetic mixtures and three new Japanese standards have been determined and corrections for inter-rare earth element interferences are made. 

DETERMINATION OF TRACE ELEMENTS IN GEOLOGICAL SAMPLES BY MAGNETIC SECTOR ICP-MS... 

Inductively coupled plasma-mass spectrometry (ICP-MS) is a multielement analytical method with detection limits which are, for many trace elements, including the rare earth elements, better than those of most conventional techniques. With increasing availability of ICP-MS instalments in geological laboratories this method has been established as the most prominent technique for the determination of a large number of minor and trace elements in geological samples. 

In addition to the aforementioned methods, TLC in combination with other instrumental techniques have also been used for quantification of inorganic species. For example, two-dimensional TLC coupled with HPLC has been utilized for the separation and quantification of REEs in nuclear fuel fission products using silaiuzed silica gel as layer material [60]. In another interesting method, REEs in geological samples have been determined by ICP-AAS after their preconcentration by TLC on Fixion plates [32]. TLC in combination with neutron activation has been used to determine REE in rock samples on Eixion 50 x 8 layers with the sensitivity limit of 0.5 to 10 pg/g for 10- to 30-mg samples [41]. A combination of TLC and A AS has been utilized for the isolation and determination of zinc in forensic samples [27]. 

Merritt WR, Champion PJ, Hawkings RC (1957) The half-life of °Pb. Can J Phys 35 16 Pickett DA, Mnrrell MT, Williams R.W (1994) Determination of femtogram qnantities of protactinium in geological samples by thermal ionization mass spectrometry. Anal Chem 66 1044-1049 Robert J, Miranda CF, Mnxart R (1969) Mesure de la periode dn protactininm-231 par microcalorimetrie. Radiochim Acta 11 104-108... 

Pickett DA, Murrell MT, Williams RW (1994) Determination of femtogram quantities of protactinium in geologic samples by thermal ionization mass spectrometry. Anal Chem 66 1044-1049 Pietruszka AJ, Carlson RW, Hauri EH (2002) Precise and accurate measurement of Ra- °Th- U disequilibria in volcanic rocks using plasma ionization multicollector mass spectrometry. Chem Geol 188 171-191... 

Volpe AM, Olivares JA, Murrell MT (1991) Determination of radium isotope ratios and abundances in geologic samples by thermal ionization mass spectrometiy. Anal Chem 63 913-916... 

This review highlights the important potential of U-series disequilibria in understanding the continental alteration and related mass transfers. The recent analytical developments, including TIMS and MC ICP MS techniques, for measuring small amounts of U, Th and Ra in geologic samples, offer today new possibilities and new perspectives for analysing U-series disequilibria in weathering profiles and river waters, and could lead to new and, as yet, unanticipated advances in the field of continental alteration. 

Danzer K, Schron W, Drefiler B, Jagemann K-U (1998) Matrix sensitivity of solid sampling AAS. Determination of zinc in geological samples. Fresenius J Anal Chem 361 710... 

Dulski, P. (1994). Interferences of oxide, hydroxide and chloride analyte species in the determination of rare earth elements in geological samples by inductively coupled plasma-mass spectrometry. Fresenius Journal of Analytical Chemistry 350 194-203. 

Jarvis, K. E. and Williams, J. G. (1993). Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) a rapid technique for the direct, quantitative determination of major, trace and rare-earth elements in geological samples. Chemical Geology 106 251—262. 

Riolo J, Ludwig B, Albtecht P, Synthesis of ting C monoaromatic steroid hydrocarbons occurring in geological samples. Tetrahedron Letters 26 2697— 2700, 1985. 

The identification of compounds using powder diffraction is useful for qualitative analysis, such as mixtures of small crystals in geological samples. It also gives a rough check of the purity of a sample—but note that powder diffraction does not detect amorphous products or impurities of less than about 5%. 

W.-M. Yang and Z.-M. Ni, The possibility of standardless analysis in graphite furnace atomic absorption spectrometry determination of gold in geological samples, Spectrochim. Acta, Part B, 51(1), 1996, 65-73. 

Many [M(dik)4] complexes are volatile, especially those that contain fluorinated diketonate ligands. Mass spectra and gas chromatographic behavior of several of these complexes have been studied (see Table 10). Isenhour and coworkers240 241 have employed fluorinated diketonates in mass spectrometric procedures for determination of Zr and Zr/Hf ratios in geological samples. The most intense peak in mass spectra of [M(dik)4] complexes is [M(dik)3]+. Sievers et al.242 have used gas chromatography of metal trifluoroacetylacetonates to separate Zr from Al, Cr and Rh. However, attempts to separate [Zr(tfacac)4] and [Hf(tfacac)4] by gas chromatography were unsuccessful. Zirconium and hafnium can be separated by solvent extraction procedures that employ fluorinated diketones.105 [M(dik)4] (M = Zr or Hf dik = acac, dpm, tfacac or hfacac) have been used as volatile source materials for chemical vapor deposition of thin films of the metal oxides.243,244... 

Grudpan, K., Jakmunee, J., and Sooksamiti, R, Flow-injection in-valve solid-phase extraction spectrophotometric determination of uranium in geological samples, Lab. Rob. Autom., 10, 25-31, 1998. 

Broadhead, M., Broadhead, R., and Hager, J.W. (1990) Laser sampling ICP-MS semi-quantitative determination of sixty-six elements in geological samples. Atomic Spectroscopy 11, 205-209. 

Y. S. Chung, R. M. Barnes, Determination of gold, patinum, palladium and silver in geological samples by inductively coupled plasma atomic emission spectrometry after poly(dithiocarbamate) resin pre-treatment,. /. Anal. Atom. Spectrom., 3 (1988), 1079D 1082. 

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