Richtigkeit bei der Bestimmung von Spurenelementen in Lebensmitteln mit der Graphitrohrtechnik AAS

Ohne Zusammenfassung

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Accuracy of the graphite furnace AAS for trace determinations in foodstuffs

     

Potentiometrische Titration von Sulfat, Barium und Strontium mit Hilfe einer bleisensitiven Elektrode

Zusammenfassung Die bleisensitive Elektrode der Fa. Orion spricht neben Bleiionen auch auf Sulfationen an. Dies ermöglicht die potentiometrische Titration von Sulfat mit Bariumperchlorat sowie die Titration von Barium und Strontium mit Natriumsulfat. Der günstigste pH-Bereich liegt zwischen 5 und 7. Titriermedium sind Dioxan-Wasser-Gemische. Die Verfahren sind sehr empfindlich und erlauben in allen Fällen die Titration bis herab zu 5·10^–4 mMol.Anwendungsbeispiele für die Bestimmung von Schwefel in organischen Verbindungen nach Schöniger- oder Wickbold-Verbrennung sind angegeben.

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Potentiometric titration of sulphate, barium and strontium by means of a lead-sensitive electrode

The Orion lead electrode was found to be responsive not only to lead ions but to sulphate ions, too. This offers possibilities to titrate sulphate with barium perchlorate and reversely barium and strontium with sodium sulphate. The useful pH range is 5–7. Dioxan-water mixtures serve as solvents. The described methods are highly sensitive and allow determinations down to 5×10^–4 millimoles.Examples are given for the determination of sulphur in organic samples after combustion according to Schöniger or Wickbold.

     

A Sensitive Spectrophotometric Determination of Nitrite in Water and Soil

A highly sensitive spectrophotometric method for the determination of nitrite in water and soil has been developed. The reaction of nitrite with acidified potassium iodide to liberate iodine which oxidizes leuco‐crystal violet (LCV) to form crystal violet having absorption maxima at 590 nm forms the bases of this method. In aqueous medium the system obeys Beer's law in the range of 0.1 to 1.0 μg per 25 mL (0.004–0.04 ppm), while in an extractive system the range is 0.025–0.25 μg in 100 mL (0.00025–0.0025 ppm). The molar absorptivity and Sandell's sensitivity were found to be 1.54 × 10⁶ 1 mol^?1 cm^?1 and 44 pg cm^?2, respectively.     

Indirect polarographic determination of phosmet O,O-Dimethyl-S-(phthalimidomethyl)dithiophosphate

Summary An indirect polarographic method for the determination of phosmet was elaborated. It is based on the fact that N-hydroxymethylphthalimide formed by the reaction of phosmet with sulphuric acid is polarographically active and exhibits a behaviour during electrolysis at a Hg dropping-electrode similar to that of phthalimide. The method has been applied to the determination of phosmet in apples. The sensitivity is 0.1 ppm.

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Indirekte polarographische Bestimmung von Phosmet O,O-Dimethyl-S-(phthalimidomethyl)dithiophosphat

Zusammenfassung Das Verfahren beruht darauf, daß N-Hydroxymethylphthalimid, das bei der Reaktion von Phosmet mit Schwefelsäure gebildet wird, polarographisch aktiv ist und sich bei der Elektrolyse mit der Quecksilber-Tropfelektrode ähnlich wie Phthalimid verhält. Die Methode wurde zur Bestimmung von Phosmet in Äpfeln angewandt. Die Empfindlichkeit beträgt 0,1 ppm.

     

Interferences in the determination of aluminium by means of atomic absorption spectrophotometry

Summary The following substances have been investigated with regard to their interfering effect in the determination of aluminium by atomic absorption spectrophotometry: HCl, H₂SO₄, HNO₃, H₃PO₄, alkali and alkaline earth metals, Cu, Fe, Zn, Ni, Mn, Co, Mo, Ti, Cr, V, Si. Ternary systems with La have been examined also. Si exerts a strong depressive effect, whereas other elements in certain concentration ranges exhibit positive effects.

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Störungen bei der atomabsorptionsspektralphotometrischen Bestimmung von Aluminium

Zusammenfassung Folgende Substanzen wurden hinsichtlich einer möglichen Beeinflussung der Aluminiumbestimmung untersucht: HCl, H₂SO₄, HNO₃, H₃PO₄, Alkalimetalle, Erdalkalimetalle, Cu, Fe, Zn, Ni, Mn, Co, Mo, Ti, Cr, V, Si. Ternäre Systeme mit La wurden ebenfalls geprüft. Si übt eine stark depressive Wirkung aus, während andere Elemente in bestimmten Konzentrationsbereichen positiv wirken.

Lecture given on the 2nd Czechoslovak Conference on Flame Speotroscopy, Zvíkov, June 5–8, 1973.     

Titrimetric determination of octacyanotungstate(IV) ions with N-bromosuccinimide

Summary N-Bromosuccinimide has been successfully applied in the determination of 1–50 mg of W(CN)₈ ^4–in approximately 6 M hydrochloric acid using Naphthol Blue Black indicator. The average error is ±0.42% and the average standard deviation is ±0.06 mg. The method is not applicable to the determination of Mo(CN) ₈ ^4– ions. Tetrakis-(N-hydro-2-carbocyclic acid-pyridinium)octacyanotungstate(IV) and -molybdate(IV) were used as primary standards for the preparation of standard Mo(IV) and W(IV) solutions. The composition of the latter compounds was verified by analysis and single crystal X-ray data were obtained.

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Titrimetrische Bestimmung von Octacyanowolframat(IV)-ionen mit N-Bromsuccinimid

Zusammenfassung N-Bromsuccinimid wurde mit Erfolg zur Bestimmung von 1–50 mg W(CN)₈ ^4–-Ionen in ungefähr 6 M Salzsäure mit Naphthol-Blau-Schwarz als Indicator verwendet. Der mittlere Fehler beträgt ±0,42 %, die mittlere Abweichung ±0,06 mg. Die Methode ist nicht brauchbar für die Bestimmung von Mo(CN)₈ ^4–-Ionen. Tetrakis(N-hydro-2-carbonylsäure-pyridinium) octacyanowolframat(IV) und -molybdat(IV) wurden als Primärstandards für die Herstellung von Standard-Mo(IV)- und -W(IV)-Lösungen benutzt. Die Zusammensetzung dieser Verbindungen wurde durch Analyse kontrolliert und die Einkristall-Röntgen-Daten wurden festgestellt.

     

Low-Cost Potentiometric Sensor for Chloride Measurement in Continuous Industrial Process Control

Recently, the new updates in legislation about drinking water control and human health have increased the demand for novel electrochemical low-cost sensors, such as potentiometric ones. Nowadays, the determination of chloride ion in aqueous solutions has attracted great attention in several fields, from industrial processes to drinking water control. Indeed, chloride plays a crucial role in corrosion, also influencing the final taste of beverages, especially coffee. The main goal is to obtain devices suitable for continuous and real-time analysis. For these reasons, we investigated the possibility to develop an easy, low-cost potentiometric chloride sensor, able to perform analysis in aqueous mediums for long immersion time and reducing the need of periodic calibration. We realized a chloride ion selective electrode made of Ag/AgCl sintered pellet and we tested its response in model solutions compatible with drinking water. The sensor was able to produce a stable, reproducible, and accurate quantification of chloride in 900 s, without the need for a preliminary calibration test. This opens the route to potential applications of this sensor in continuous, in situ, and real time measurement of chloride ions in industrial processes, with a reduced need for periodic maintenance.     

Assessment of Chemical Composition and Anti-Penicillium Activity of Vapours of Essential Oils from Abies Alba and Two Melaleuca Species in Food Model Systems

The possibilities of the practical utilization of essential oils (EOs) from various plant species in the food industry have attracted the attention of the scientific community. Following our previous studies, the antifungal activities of three further commercial EOs, Melaleuca armillaris subsp. armillaris (rosalina; REO), Melaleuca quinquenervia (niaouli; NEO), and Abies alba (fir; FEO), were evaluated in the present research in respect to their chemical profiles, over four different concentrations, 62.5 μL/L, 125 μL/L, 250 μL/L, and 500 μL/L. The findings revealed that the major compounds of REO, NEO, and FEO were linalool (47.5%), 1,8-cineole (40.8%), and α-pinene (25.2%), respectively. In vitro antifungal determinations showed that the inhibition zones of a Penicillium spp. mycelial growth ranged from no inhibitory effectiveness (00.00 ± 00.00 mm) to 16.00 ± 1.00 mm, indicating a very strong antifungal activity which was detected against P. citrinum after the highest REO concentration exposure. Furthermore, the in situ antifungal efficacy of all EOs investigated was shown to be dose-dependent. In this sense, we have found that the highest concentration (500 µL/L) of REO, NEO, and FEO significantly reduced (p < 0.05) the growth of all Penicillium strains inoculated on the bread, carrot, and potato models. These results indicate that the investigated EOs may be promising innovative agents in order to extend the shelf life of different types of food products, such as bread, carrot and potato.     

Biochemical Characterization and In Vitro Digestibility of Protein Isolates from Hemp (Cannabis sativa L.) By-Products for Salmonid Feed Applications

Hemp (Cannabis sativa L.) processing by-products (hemp cake and hemp seed hulls) were studied for their protein content, extraction of protein isolates (PIs), and their in vitro protein digestibility (IVPD). Crude protein contents of hemp cake and hemp seed hulls were 30.4% and 8.6%, respectively, calculated based on generalized N-to-P conversion factor (N × 5.37). Extraction efficiency of PIs from defatted biomass ranged from 56.0 to 67.7% with alkaline extraction (0.1 M NaOH) followed by isoelectric precipitation (1.0 M HCl). Nitrogen analysis suggested that the total protein contents of PIs extracted using three different alkaline conditions (0.5 M, 0.1 M, and pH 10.0 with NaOH) were >69.7%. The hemp by-product PIs contained all essential amino acids (EAAs) required for fish with leucine, valine, and phenylalanine belonging to the five dominant amino acids. Overall, glutamate was the dominant non-EAA followed by aspartate. Coomassie staining of an SDS-PAGE gel revealed strong presence of the storage protein edestin. High IVPD of >88% was observed for PIs extracted from hemp seeds and by-products when evaluated using a two-phase in vitro gastric/pancreatic protein digestibility assay. PIs extracted from by-products were further tested for their antioxidant activities. The tested PIs showed dose-dependent DPPH radical scavenging activity and possessed strong ORAC values > 650 μM TE/g.