Multi-element trace determinations in pure alkaline earth fluoride powders by high-resolution ICP-MS using wet-chemical sample preparation and laser ablation

Abstract

Four alternative analytical procedures for the determination of ten important trace impurities (Mg, Cr, Fe, Cu, Zn, Sr, Zr, Cd, Ba, and Pb) in pure alkaline earth fluoride powders were applied using high-resolution inductively coupled plasma mass spectrometry (ICP-MS). Two procedures are based on a wet-chemical microwave digestion with boric acid and quantification by the standard addition technique and isotope dilution mass spectrometry (IDMS), respectively. In addition, analyses are also performed by laser ablation as a direct solid sampling technique applying matrix-matched external calibration as well as isotope dilution of the powdered sample. For most elements good agreement between the different methods is found. Detection limits for laser ablation vary between 0.05 ng g(-1) for Zr and 20 ng g(-1) for Mg. They are about one to two orders of magnitude lower than those of the wet-chemical procedures, which is mainly due to the high dilution factor during the sample preparation step. Advantages and restrictions of the different analytical procedures are discussed with respect to their routine applicability. Due to its relatively high accuracy, low detection limits, and time-efficiency LA-ICP-IDMS is the preferred choice if no standard reference materials are available.

Use of Sol−Gels as Solid Matrixes for Trace Analysis by UV Laser Ablation and Laser-Enhanced Ionization Detection

“…Using ZrX-based calibration pellets and indium as the internal standard, the Pb concentration in the NIST 1632c Bituminous Coal CRM sample was measured at 3.72 μg·g -1 , a 2% deviation from the 3.79 μg·g -1 certified value. A 3σ limit of detection of 60 ng/g was calculated for Pb, which compares well with results obtained in other laboratories by different techniques. ,−

3 SEM photographs of particles ablated from ZrX-based materials and collected on Nucleopore filters. (A) ZrX only; (B) ZrX-based calibration standard; (C) ZrX-based NIST sample.

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Taxonomic and geographic influences on fish otolith microchemistry

“…The micromilled powders are dissolved and then analysed with SB‐ICPMS for elemental concentrations, or with isotope‐ratio mass spectrometry to determine stable isotope ratios. The advantage of micromill sampling for the determination of the elemental composition is the greater stability and precision afforded by SB‐ICPMS compared with laser ablation (LA) – ICPMS (Tibi and Heumann ). However, contamination from the milling procedure may be problematic (Arslan and Secor ).…”