title: Determination of trace metallic impurities in high-purity quartz by ion chromatography.
abstract: A method has been developed for the determination of relevant trace impurities (alkali, alkaline and transition metals) in high purity quartz by ion-chromatography. In situ reagent (HF) purification and simultaneous sample dissolution was achieved in a multichannel vapour phase digestion assembly. Twenty-one samples can be digested at a time in this vapour phase system. Significant decrease in the process blank levels for all the analytes was observed. Drastic reduction (250 times) of NH4+ blank was achieved in the described vapour phase digestion, which enables the determination of trace concentration of sodium in high purity quartz. After volatilisation of the matrix and unreacted HF, the clear water leached solutions were injected into an ion-chromatograph equipped with conductivity detector for the determination of alkali and alkaline earth metals. In the case of transition metals, the trace residues were leached with 10 mM HCl and after separation on a mixed bed analytical column (IonPac CS5) were detected by spectrophotometry after post column derivatisation using 4-(2-pyridylazo)resorcinol (PAR). The accuracy of the result was checked by their comparison with those obtained by independent methods like inductively coupled plasma (ICP) MS and ICP atomic emission spectrometry. The achievable detection limits are between 0.4 ng/g (Li) and 22 ng/g (Mn). The application of the method to the determination of the above trace metals in two high-purity-grade quartz samples is demonstrated.
authors.affiliation: National Centre for Compositional Characterisation of Materials, Bhabha Atomic Research Centre, ECIL (PO), Hyderabad City, Andhra Pradesh 500062, India.
authors.forename: K
authors.initials: K
authors.lastname: Dash
authors.forename: K
authors.initials: K
authors.lastname: Chandrasekaran
authors.forename: S
authors.initials: S
authors.lastname: Thangavel
authors.forename: S M
authors.initials: SM
authors.lastname: Dhaville
authors.forename: J
authors.initials: J
authors.lastname: Arunachalam
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D008670:Metals / Q000032:analysis*; D011791:Quartz / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014131:Trace Elements / Q000032:analysis*
chemical_list: D008670:Metals; D014131:Trace Elements; D011791:Quartz