Sample preparation method for major‐element analyses of carbonate rocks by X‐ray spectrometry

Abstract

A sample preparation method is described which permits fast and accurate wavelength‐dispersive, x‐ray fluorescence analysis of ten major oxides in carbonate rocks. The sample is first ground into a fine powder, then calcined, its loss‐on‐ignition (LOI) is determined and finally it is fused into a glass disc with lithium tetraborate at 1100°C using a 1:10 sample‐to‐flux ratio. Geological reference standards and synthetic standards are used for calibration. Matrix effects are corrected empirically using Lachance‐Traill correction algorithms. The accuracy and precision of the method were assessed by the analysis of several NBS carbonate reference standards.

Chemical Characterisation of Geological Raw Materials Used in Traditional Ceramics

“…-Determination of the remaining elements. Silicon, Al, Fe, Ca, Mg, Na, K, Ti, Zr, Hf, P, Sr, As, Mn, S and Cl were determined by XRF (Baker 1982, van Zyl 1982, Hickson and Juras 1986, Rouseau and Bouchard 1986, Anderson 1987, King and Vivit 1988, Feret 1990, Gazulla et al 1991, Conture et al 1993, Buhrke et al 1998, Obenauf 2002).…”

“…Silicon, Al, Fe, Ca, Mg, Na, K, Ti, Zr, Hf, P, Sr, As, Mn, S and Cl were determined by XRF (Baker 1982, van Zyl 1982, Hickson and Juras 1986, Rouseau and Bouchard 1986, Anderson 1987, King and Vivit 1988, Feret 1990, Gazulla et al 1991, Conture et al 1993, Buhrke et al 1998, Obenauf 2002). Silicon, Al, Fe, Ca, Mg, Na, K, Ti, Zr, Hf, P, Sr, As, Mn, S and Cl were determined by XRF (Baker 1982, van Zyl 1982, Hickson and Juras 1986, Rouseau and Bouchard 1986, Anderson 1987, King and Vivit 1988, Feret 1990, Gazulla et al 1991, Conture et al 1993, Buhrke et al 1998, Obenauf 2002).…”

“…In the case of Cl, sample preparation was in the form of pellets (van Zyl 1982, Hickson and Juras 1986, Anderson 1987, King and Vivit 1988, because in bead preparation, Cl would volatilise due to the high temperatures involved and high Cl volatility. The XRF measurement conditions used for Cl are given in Table 2.…”

“…The chemical characterisation of ceramic raw materials can be carried out by the following analytical techniques: X-ray fluorescence spectrometry (XRF), thermogravimetry (TG), gravimetry (G), inductively coupled plasma-atomic emission spectrometry (ICP-AES), potentiometry (P), coulometry (C) and atomic absorption spectrometry (AAS) (Bertin 1984, King and Vivit 1988, Knockman 1989, Bennett and Oliver 1992, Goto and Tatsumi 1996, Corumluoglu and Guadagnino 1997, Dhawan and Suri 1999, Coedo et al 2002.…”

Bead‐releasing agents used in the preparation of solid samples as beads for WD‐XRF measurement

“…A literature search showed that the following additives are used as bead-releasing agents: NaI, LiBr, NH 4 I, LiI, and LiF [5][6][7][8]. However, studies also show that the use of a release agent may interfere in the WD-XRF measurement of a fused bead sample if the release agent contains an analyte element, or if it produces matrix effects (absorption and strengthening) or line overlap [9].…”