Macro To Nano Spectroscopy

Fluorine, chlorine, bromine, and iodine have been studied in biological samples and other related matrices owing to the need to understand the biochemical effects in living organisms. In this review, the works published in last 20 years are covered, and the main topics related to sample preparation methods and analytical techniques commonly used for fluorine, chlorine, bromine, and iodine determination in biological samples, food, drugs, and plants used as food or with medical applications are discussed. The commonest sample preparation methods, as extraction and decomposition using combustion and pyrohydrolysis, are reviewed, as well as spectrometric and electroanalytical techniques, spectrophotometry, total reflection X-ray fluorescence, neutron activation analysis, and separation systems using chromatography and electrophoresis. On this aspect, the main analytical challenges and drawbacks are highlighted. A discussion related to the availability of certified reference materials for evaluation of accuracy is also included, as well as a discussion of the official methods used as references for the determination of halogens in the samples covered in this review.

Analytical methods for the determination of halogens in bioanalytical sciences: a review

Sample preparation techniques based on combustion reactions in closed vessels - A brief overview and recent applications

Iodine determination in food samples was performed by inductively coupled plasma mass spectrometry (ICP-MS) after digestion by microwave-induced combustion (MIC). Sample masses up to 500 mg of bovine liver, corn starch, milk powder, or wheat flour were completely combusted using the MIC system. Ammonium nitrate (6 mol l−1 solution, 50 μl) was used as an aid for ignition and vessels were charged with 15 bar of O2. The use of H2O, 0.9 mmol l−1 H2O2, 10 to 50 mmol l−1 (NH4)2CO3 and 56 mmol l−1 tetramethylammonium hydroxide was investigated as absorbing solutions, as well as the suitability of performing a reflux step after the combustion process. Digestion of food samples by pressurized microwave-assisted acid digestion, microwave-assisted extraction and conventional extraction of iodine in alkaline solution were also evaluated. Iodine recoveries higher than 99% were obtained using MIC and 50 mmol l−1 (NH4)2CO3 or 56 mmol l−1 tetramethylammonium hydroxide as absorbing solution and with 5 min for the reflux step. Accuracy was evaluated using certified reference materials (bovine muscle, corn bran, and milk powder) and agreement better than 97% was obtained. The limit of quantification by MIC and further ICP-MS determination was 0.002 µg g−1. Blanks were always low and no memory effects were observed. Digestion by MIC allowed the processing of up to eight samples by each run in 25 min with high efficiency of digestion (residual carbon content lower than 1%) providing a suitable medium for further iodine determination by ICP-MS.

Iodine determination in food by inductively coupled plasma mass spectrometry after digestion by microwave-induced combustion.

A procedure coupling acid decomposition and precipitation, using inductively coupled plasma optical emission spectrometry (ICP- OES) is proposed for the determination of Cl, Br and I in milk samples. During the mineralization process in closed and open vessels (microwave ovens), anions are precipitated as salts of low solubility products (AgCl, AgBr and AgI). After separation from digestate solution, precipitates are dissolved with ammonia resulting in a 20% v/v solution. The final solution was directly introduced into the ICP-OES without any damage to the sample introduction system and with no severe spectral interference. Three biological reference materials were used to validate the methodology: Non-Fat Milk Powder SRM 1549 from NIST, Skim Milk Powder RM-151 from BCR and Whole Egg Powder RM 8415, also from NIST. The limits of detection (3σb/s) for Cl, Br and I in the solid sample were 30, 40 and 280 µg g−1 for the closed vessel microwave oven, and 15, 20 and 40 µg g−1 for the open vessel microwave oven, respectively. Relative standard deviations, considering five replicates of sample submitted to the proposed methodology, were 1% for Cl and Br, and 2% for I, when a closed vessel microwave was used. The results for Cl were in good agreement with the certified values (90% confidence level). For Br, recoveries ranged from 87 to 104% for closed vessel microwave oven and from 90 to 102% for open vessel microwave oven. As for I, recoveries ranged from 85 to 98% with a closed vessel microwave oven. Accurate results for determinations in certified materials and good recoveries demonstrated the efficiency of the procedure.

Determination of chlorine, bromine and iodine in milk samples by ICP-OES

This paper describes the development of various new acid sample decomposition methods, as well as an extraction (leaching) method and compares them with the “Schoniger Combustion” technique. The methods have been developed as sample preparation techniques for iodine determination in biological materials, especially in solid samples. ICP-MS (inductively coupled plasma mass spectrometry) and a catalytic technique are employed and discussed for the final determination of iodine concentrations. Accuracy and reliability of the different analytical methods are shown in the examples of different CRMs (certified reference materials) available for iodine. The results of an interlaboratory comparison are specifically presented for the extraction (leaching) method.

Iodine determination in biological materials : Options for sample preparation and final determination

Aufgrund der hohen erreichbaren Temperatur und des hohen Druckes wurde der Hochdruckverascher HPA zur Veraschung von biologischem Material fur die nachfolgende voltammetrische Bestimmung von Spurenelementen getestet. Anhand einiger verschiedener Standard-referenzmaterialien konnte gezeigt werden, das sich dieses Nasveraschungsverfahren in ausgezeichneter Weise fur dieses Einsatzgebiet, bei dem es auf eine vollkommene Zerstorung der organischen Matrix ankommt, eignet. Mit einer Mischung von HNO3 und einer geringen Menge HClO4 und unter Verwendung verschiedener Temperaturprogramme konnte eine Vielzahl von verschiedenartigen biologischen Matrices in geeigneter Weise zerstort werden. Dabei erhaltene Ergebnisse der Spurenelementbestimmungen sowie die Blindwerte des Aufschlusverfahrens werden angegeben.

Einsatz des Hochdruckveraschers HPA nach Knapp [1] für die voltammetrische Bestimmung von Spurenelementen in biologischem Material

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Iodine determination in biological materials : Options for sample preparation and final determination

Einsatz des Hochdruckveraschers HPA nach Knapp [1] für die voltammetrische Bestimmung von Spurenelementen in biologischem Material