High Resolution ICP-OES Research Articles

A Fast and Efficient Procedure of Iron Species Determination Based on HPLC with a Short Column and Detection in High Resolution ICP OES.

The optimization and application of a new hyphenated procedure for iron ionic speciation, i.e., high performance liquid chromatography (HPLC) with short cation-exchange column (50 mm × 4 mm) coupled to high resolution inductively coupled plasma optical emission spectrometry (ICP hrOES), is presented in this paper. Fe(III) and Fe(II) species were separated on the column with the mobile phase containing pyridine-2,6-dicarboxylic acid (PDCA). The total time of the analysis was approx. 5 min, with a significantly low eluent flow rate (0.5 mL min-1) compared to the literature. Additionally, a long cation-exchange column (250 mm × 4.0 mm) was used as reference. Depending on the total iron content in the sample, two plasma views were chosen, e.g., an attenuated axial (<2 g kg-1) and an attenuated radial. The standard addition method was performed for the method's accuracy studies, and the applicability was presented on three types of samples: sediments, soils, and archaeological pottery. This study introduces a fast, efficient, and green method for leachable iron speciation in both geological and pottery samples.

Speciation and Enrichment of Cadmium and Lead from Water Samples using Fe3O4/rGO Sorbent in Dispersive Magnetic Micro-Solid Phase Extraction with Inductively Coupled Plasma-Optical Emission Spectroscopy

This work reports the development of dispersive magnetic solid-phase extraction (DMSPE) with high resolution ICP-OES for the pre-concentration of cadmium and lead in water samples. The method uses magnetic reduced graphene oxide (Fe3O4/rGO) as adsorbent. The influences of sample pH, extraction time, desorption solvent and desorption time were evaluated and optimized. In the optimized conditions, linear calibration curves for Cd2+ and Pb2+ were obtained in the range of 10-2000 μg L-1 with correlation coefficients of 0.9996 and 0.9995, respectively. Low detection limits of Cd2+ and Pb2+ were found to be 9.03 μg L-1 and 12.4 μg L-1, respectively. Good relative recovery values, in the range of 91-95% and excellent repeatability of 6.4-9.9%, (n = 3) were obtained. The results revealed that Fe3O4/rGO can be a suitable nanocomposite sorbent in the speciation and pre-concentration of Cd2+ and Pb2+ for tap water and drinking water samples. The method is rapid, selective, reliable and environmentally friendly for the determination of Cd2+ and Pb2+ in water samples.

Challenges in the quality assurance of elemental and isotopic analyses in the nuclear domain benefitting from high resolution ICP-OES and sector field ICP-MS.

Accurate analytical data reinforces fundamentally the meaningfulness of nuclear fuel performance assessments and nuclear waste characterization. Regularly lacking matrix-matched certified reference materials, quality assurance of elemental and isotopic analysis of nuclear materials remains a challenging endeavour. In this context, this review highlights various dedicated experimental approaches envisaged at the European Commission—Joint Research Centre—Institute for Transuranium Elements to overcome this limitation, mainly focussing on the use of high resolution-inductively coupled plasma-optical emission spectrometry (HR-ICP-OES) and sector field-inductively coupled plasma-mass spectrometry (SF-ICP-MS). However, also α- and γ-spectrometry are included here to help characterise extensively the investigated actinide solutions for their actual concentration, potential impurities and isotopic purity.

Improved plutonium concentration analysis in specimens originating from the nuclear fuel cycle using high resolution ICP-OES

High resolution ICP-OES allows for the reliable determination of plutonium in radioactive samples.

Solid phase separation and ICP-OES/ICP-MS determination of rare earth impurities in nuclear grade uranium oxide

A simple, effective and low cost solid phase extraction procedure was standardized for the trace and ultra-trace level determination of rare earth impurities, such as, Ce, Dy, Sm, Gd, Eu, Er etc. which act as neutron poisons, in nuclear grade uranium oxide (U3O8 > 99.9% by weight). The method involves selective separation of these elements as their fluorides with the help of activated charcoal from major uranium matrix followed by determination by ICP-MS and high resolution ICP-OES. The residual uranium content of the solution was <10 μg/mL. The recovery of REEs ranges from 85 to 105%. The method was validated with nuclear grade uranium oxide standards CRM-I to CRM-V (BARC, Mumbai, India) in addition to some synthetic standards. The RSD of the method was ±12% (n = 3).

Promises and pitfalls in the reliable determination of233U using high resolution ICP-OES

This study highlights that the currently employed analytical approach for the ICP-OES determination of 233U at λ = 385.950 nm is neither specific for this U isotope nor reliable and provides potential solutions for a selective and reliable quantification of 233U, 235U, and 238U using high resolution ICP-OES. While being a sensitive U wavelength region, the small isotopic line splitting of 233U (λ = 385.950 nm), 235U (λ = 385.955 nm) and 238U (λ = 385.958 nm) cannot be resolved with any commercial high resolution optical spectrometer. In addition, the width of 5.67 pm of the 233U peak, defined as full width at half maximum, is particularly larger than the 238U peak width of ∼4.3 pm, thus indicating splitting of the 233U emission signal into multiple peaks. In contrast, superior U isotopic information can be obtained from isotope specific emission lines centred around λ = 411.6 nm and λ = 424.4 nm with a spectral distance between 233U and 238U of 25 pm and 39 pm, respectively. The 233U signal of both wavelength regions, however, suffers from a potential interference with thorium that requires peak deconvolution for accurate quantification of 233U.

Validation of isotopic analysis of depleted, natural and enriched uranium using high resolution ICP-OES

Analytical procedures for the reliable determination of uranium isotopes employing a commercially available high resolution (HR)-ICP-OES installed in a glove box were developed and validated. To this end, nine commonly used U emission lines were tested for their potential to provide isotopic splitting of the U signal, thus providing isotopic information. Among all emission lines tested, the wavelength region around 424.4 nm offered the largest spread between individual U signals, i.e.233U, 235U, 236U, and 238U. This study focused specifically on the reliable determination of the abundances of 235U at 424.412 nm and 238U at 424.437 nm in samples containing depleted, natural and slightly enriched U, but also included specimens with rather high (up to ∼90%) 235U enrichments. Appropriate selection of the spectral background and accurate positioning of the peaks proved essential for obtaining reproducible U isotope ratios. The accuracy of the developed methodology was confirmed by the analysis of eight certified isotopic reference materials as well as eight reference samples that have been characterised in an accredited laboratory in-house using TIMS. In addition, this study highlights the potential of the developed HR-ICP-OES procedure for identifying nuclear sources of various U specimens via the analysis of 233U (424.398 nm) and 236U (424.423 nm). In contrast to the commonly used techniques, the methodology applied in this study does neither require the separation of U from the matrix prior to analysis nor the regular analysis of a reference sample with a known isotopic composition to correct for bias effects as it is the case for more sophisticated and precise mass spectrometric measurements. Nevertheless, HR-ICP-OES provides fit for purpose U isotopic information with reasonable accuracy (typically <1.5%) and precision (∼1%) within a few minutes. As such, HR-ICP-OES can be employed as a reliable, fast screening tool to identify the U isotopic composition and as such, complements the more laborious TIMS analysis routinely employed for this purpose.