Simultaneous Determination of Fluorine and Chlorine in Marine and Stream Sediment by Ion Chromatography Combined with Alkaline Digestion in a Bomb

Fluorine and chlorine are important tracers for geochemical and environmental studies. In this study, a rapid alkaline digestion (NaOH) method for the simultaneous determination of fluorine and chlorine in marine and stream sediment reference samples using ion chromatography is developed. The proposed method suppresses the volatilization loss of fluorine and chlorine and decreases the matrix effects. The results are in good agreement with fluorine ~100%, chlorine ranging from 90 to 95% of the expected concentrations. The detection limits of this method were 0.05 μg/g for fluorine and 0.10 μg/g for chlorine. This method is simple, economical, precise and accurate, which shows great potential for the rapid simultaneous determination of fluorine and chlorine in large batches of geological and environmental samples commonly analyzed for environmental geochemistry studies.

Green Aspects of Ion Chromatography versus Other Methods in the Analysis of Common Inorganic Ions

Due to the increasing environmental awareness of the public, green chemistry has become an important element of environmental protection. In laboratories around the world, millions of analyses of inorganic and organic anions and cations in water and wastewater samples, and solid and gaseous samples are performed daily. Unfortunately, these activities still generate large costs, including environmental costs, which are related to the scale of the studies, the use of toxic chemical reagents, the waste generated, and the energy consumed. The methods used so far for inorganic ion analysis, including classical methods, are increasingly being replaced by instrumental methods, primarily based on ion chromatography. This paper presents the most important advantages and limitations of ion chromatography, and compares them with the costs of classical analyses for the analytes and sample types. Both the financial and environmental costs associated with the determination of common inorganic ions, such as Cl−, NO2−, NO3−, and NH4+, in 1000 environmental samples, were compared using selected reference wet classical methods and ion chromatography. The advantages and limitations of ion chromatography that allow this separation technique to be classified as a green analytical chemistry method have been described herein.

Investigation of per- and polyfluoroalkyl substances (PFAS) in soils and sewage sludges by fluorine K-edge XANES spectroscopy and combustion ion chromatography

For the first time, fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy was applied to detect per- and polyfluoroalkyl substances (PFAS) in various soil and sewage sludge samples. The method can be used to determine the speciation of inorganic and organic fluorides, without pre-treatment of solid samples. Therefore, XANES spectra of several inorganic fluorides as well as selected fluorinated organic compounds were recorded. While inorganic fluorides partially exhibit a variety of sharp spectral features in the XANES spectrum, almost all inspected organofluorine compounds show two distinct broad features at 688.5 and 692.0 eV. Moreover, the peak intensity ratio 688.5 eV/692.0 eV in the PFAS XANES spectrum can be inversely correlated to the chain length of the perfluoro sulfonic acid group. The detection of targeted PFAS by bulk-XANES spectroscopy in combination with linear combination fitting in soils and sewage sludges was not applicable due to the low organic fluorine to total fluorine ratio of the samples (0.01–1.84%). Nonetheless, direct analysis of pure PFAS revealed that analysis of organofluorine species might be achieved in higher concentrated samples. Furthermore, quantitative measurements by combustion ion chromatography (CIC) evaluated as sum parameters extractable organically bound fluorine (EOF) and total fluorine (TF) emphasize that besides soils, sewage sludges are a significant source of organic fluorine in agriculture (154–7209 µg/kg).

A risk-based approach to validation of ion chromatography methods using suppressed conductivity

Ion chromatography (IC) has evolved into one of the most widely used separation techniques of analytical chemistry. Consequently, the number of users of this method is continuously growing. Analysts often assume that widely used guidelines for HPLC method validation in regulated environments routinely apply to IC. This manuscript provides an analysis of the potential shortcomings of traditional approaches to development and validation of IC methods using suppressed conductivity detection and a risk-based alternative approach to these activities. The goal of the alternative approach is a reduction in the risk of erroneous determinations of analytes when IC methods using suppressed conductivity detection are employed.

Aqueous Two-Phase System–Ion Chromatography for Determination of Thiocyanate in Raw Milk

Thiocyanate could effectively inhibit bacteria in milk and extend the shelf life of milk. However, excessive addition will lead to health risks. Therefore, the determination of thiocyanate in raw milk has received a lot of attention, but the determination could be interfered with by other components in raw milk and the pre-treatment of raw milk is complex. In this study, a new pretreatment method combined with ion chromatography (IC) for rapid and sensitive determination of thiocyanate is proposed. An acetonitrile/(NH4)2SO4 aqueous two-phase system (ATPS) was developed for the separation and enrichment of thiocyanate in raw milk. Response surface methodology was performed to optimize the extraction conditions and an efficient pretreatment were obtained using ATPS composed of 42% acetonitrile (w/w) and 16% (NH4)2SO4 (w/w), with the pH 4.7, and the recovery of thiocyanate reached 107.24 ± 0.5%, and the enrichment ratio was 10.74 ± 0.03. IC was used to establish a thiocyanate enrichment method. The linear range was from 0.05 to 15 mg/L and R2 = 0.998, the limit of detection (LOD) was 0.2 μg/L, the limit of quantification (LQD) was 0.6 μg/L. Hence, it is feasible to combine ATPS with IC for the enrichment and determination of thiocyanate in raw milk.

STUDI HIDROGEOKIMIA SUNGAI CITARUM

Sungai Citarum adalah sungai yang terletak di daerah vulkanik dan beriklim tropis. Sungai ini merupakan sungai strategis nasional karena merupakan sungai yang menjadi pasokan air bagi masyarakat maupun industri dan pembangkit listrik. Secara ekonomi sungai ini sangat penting, namun tercemar limbah industri, limbah pertanian dan limbah rumah tangga. Untuk memantau tingkat pencemaran sungai dilakukan analisis hidrogeokimia. Dalam penelitian ini, sampel air dari sungai dianalisis parameter fisis dan kimia serta kandungan ionnya. Analisis kandungan ion dilakukan dengan ion chromatography dan titrasi asam-basa.