Pyrohydrolysis as a sample preparation method for the subsequent halogen determination: A review.

The use of pyrohydrolysis as a sample preparation method for further halogen determination is extensively discussed in this review, covering studies published in the last 30 years. This method is compatible with both organic (such as cellulose, fossil fuels, carbon nanotubes, and graphite) and inorganic (such as rocks, silicates, alumina, and nuclear fuels) matrices. It has also been used for samples with different organic matter content, such as coal, mineral supplements, and soil. Sample masses vary greatly and are dependent on organic matter content in the samples, ranging from 50 mg to up to 500 mg for organic samples, and up to 4 g to inorganic samples. Different additives, such as V2O5 and cellulose, or flame retardants, such as silica, could also be used to improve analyte recovery using pyrohydrolysis. Dilute alkaline solutions or even water have been used as absorbing solutions, with mainly NaOH, NH4OH, and mixtures of NaHCO3 and Na2CO3 being applied. Furthermore, pyrohydrolysis is compatible with detection techniques such as ion chromatography, inductively coupled plasma mass spectrometry, ion selective electrode, inductively coupled plasma optical emission spectrometry, energy-dispersive X-ray fluorescence spectrometry, spectrophotometry, and isotope ratio mass spectrometry. Other advantages usually related to this method are the low residual carbon concentration of digests and the low residue generation. A critical comparison with alkaline extraction, alkaline fusion, Schöniger oxygen flask combustion, combustion bomb and microwave-induced combustion is also provided.

Ultrasound: a suitable technology to improve the extraction and techno-functional properties of vegetable food proteins.

Vegetable-based proteins may be extracted from different sources using different extraction methods, among them, ultrasound-assisted extraction stands out. This review presents the current knowledge on ultrasound-assisted extraction (UAE) and the functional properties of extracted vegetable proteins. Ultrasound generates cavitation in a liquid medium, defined as gas and vapor microbubbles collapse under pressure changes large enough to separate them in the medium. Cavitation facilitates the solvent and solid interaction, increasing yield and reducing extraction periods and temperature used. Moreover, ultrasound treatment changed extracted protein properties such as solubility, hydrophobicity, emulsifying and foam, water and oil absorption capacity, viscosity, and gelatinization. Ultrasound-assisted extraction is a promising technique for the food technology sector, presenting low environmental impact, lower energy and solvent consumption, and it is in accordance with green chemistry technology and sustainable concepts.

A new and feasible analytical method using reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for further determination of Nickel in hydrogenated vegetable fat.

A new and simple method for Ni determination in hydrogenated vegetable fat (HVF) has been developed using a RP-DLLME sample preparation procedure for further determination by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrophotometry (GFAAS). The RP-DLLME procedure includes simultaneous microextraction and preconcentration of Ni in HVF, using 5.0 g of HVF preheated (75 °C) and diluted in 5.0 mL of xylene, with the addition of a dispersant/extractant mixture (n-propanol/dilute HNO3). The sample was manually stirred and centrifuged and the aqueous phase was collected for further Ni determination by FAAS and GFAAS. RP-DLLME was carried out using only 700 µL of n-propanol and 300 µL of 2.0 mol L-1 HNO3. The recovery varied from 93.3% to 101.5% for HVF. The LODs and LOQs were 40 and 90 ng g-1 for FAAS, and 0.41 and 1.36 ng g-1 for GFAAS. The proposed analytical method is viable and this is the first application of RP-DLLME to solid fat samples, with Ni determination as an example of application. This method consumes small amounts of reagents, with lower toxicity as compared to microwave decomposition. Furthermore, the key features of the RP-DLLME method include simplicity of operation, high sample mass, reduced reagent consumption, and use of diluted HNO3 as an extractant.