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A survey of 32 paper and board materials intended for food contact has been undertaken. Sample composition was analysed to identify chemicals with a potential to migrate to foods. Representative materials covering a range of uses such as aqueous and fatty foods, and use at ambient and elevated temperatures, were obtained from industry. The samples were examined in their unfinished state, even where the final form would have included lamination to plastics, printing, or other treatments. A comprehensive and systematic analytical approach was applied which included determination of volatiles by headspace GC-MS, extraction using water, ethanol and chloroform with subsequent analysis by GC-MS and HPLC, and multi-element screening by ICP-MS. The solvent extracts were also weighed to determine the total amount of material available for migration. A large number of volatile substances were identified with alkyl and aryl aldehydes predominating in the majority of samples. Substances identified in solvent extracts included 2,6-di-tert-butyl-4-hydroxytoluene (BHT), di-tert-butylphenol, benzophenone, 4,4'-bis(dimethyl amino) benzophenone (Michler's ketone), triphenyl methane, bicyclohexylphenylphenanthrene carboxylic acid (and its methyl ester) and abietic acid. Levels of these substances were however generally below 1 mg/kg paper. Of the inorganic elements, arsenic and mercury were not detected above the limits of determination of 1.8 and 0.4 mg/kg respectively in any of the 10 samples examined. Cadmium was detected in teabag tissue and in unbleached Kraft paper at 0.3 mg/kg. Chromium was present in seven samples at 1.1-7.8 mg/kg, whilst lead was present in nine of the 10 samples at levels ranging from 0.3 to 5.9 mg/kg.
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PMID:Migration studies from paper and board food packaging materials. 1. Compositional analysis. 905 81

Scandium, gallium and vanadium contents in plants is on the ppm level, although plants from industrial areas can show higher concentrations of these elements. In Department of Analytical Chemistry of Silesian University there have been elaborated new, sensitive, spectrophotometric methods of determination of scandium, gallium and vanadium using Chrome Azurol S (CAS) and Sterinol (ST). The aim of this study was the application of these methods in analysis of cultivated plants from polluted regions. White cabbage from Upper Silesia was chosen. Because the spectrophotometric methods are not selective, scandium, gallium and vanadium should be preliminary separated from interfering elements. The solvent reaction was applied for the isolation from main and trace components of investigated material. Tienoiltrifluoracetone solution in xylene was used for the extraction of scandium, mesithyloxide for vanadium and n-butyl acetate--for gallium. Interfering and not separated Fe(III) was isolated using the extraction with acetylacetone solution in CHCl3 in the case of scandium and the reduction to Fe(II) by ascorbic acid in the case of gallium and vanadium. Due to influence of Fe(II) on the vanadium determination, KCN was used as a masking agent directly after the reduction. Scandium, gallium and vanadium were determined in 6 independent samples of white cabbage after dry or wet mineralization and contents of these leemnets were found from calibration graphs. Obtain results were checked by the internal standard addition method and Atomic Emission Spectrometry Method (ICP AES). The amounts of gallium and vanadium in white cabbage from Upper Silesia District determined by elaborated methods are in good correlation with a literature data, although the contents of vanadium are on the toxic level. The scandium concentration is higher than in plants from not industrial areas. The standard recovery is satisfactory. The Atomic Emission Spectrometry Method gave comparable results. The proposed the spectrophotometric methods are sensitive, precise and economical too, because they require only small amounts of reagents and simple not expensive apparatus. The methods can be recommended for many laboratories to the analytical control of white cabbage and after adaptation to the other plant material analysis.
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PMID:[Spectrophotometric determination of scandium,gallium and vanadium in white cabbage leaves]. 956 4

A method has been developed for the separation of the entire group of rare-earth elements from high-purity calcium chloride by countercurrent chromatography, and subsequent determination of the elements by ICP-MS. A solution of diphenyl[dibutylcarbamoylmethyl]phosphine oxide in chloroform (0.5 mol L(-1)) has been chosen as reagent for the extraction and preconcentration of trace rare-earth elements from aqueous 5% CaCl2 solution, 3 mol L(-1) in HNO3 and 0.1 mol L(-1) in HClO4. The analytes are back-extracted into a small volume of water and the aqueous eluate is subjected to ICP-MS measurements. The performance characteristics of the procedure developed have been checked by use of the standard addition technique and a real CaCl2 sample (Merck product) has been analyzed. The results obtained demonstrate the applicability of countercurrent chromatography to the determination of ultratrace elements.
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PMID:Group separation of trace rare-earth elements by countercurrent chromatography for their determination in high-purity calcium chloride. 1158 97

In addition to determination of total selenium in nuts, the element distribution among different fractions (lipid extract, low molecular weight, and protein fractions), and speciation analysis were studied. Improved precision for total selenium determination was observed after elimination of lipids. Because selenium was not detected in any of the lipid extracts obtained from the different types of nuts (ICP-MS), in each determination and/or speciation procedure used in this work lipids were extracted (chloroform-methanol, 2:1) and discarded before analysis. In agreement with previously reported data, high selenium levels were found in Brazil nuts (those purchased without shells contained approximately a quarter the content than those purchased with shells) and significantly lower levels in walnuts, cashews, and pecans nuts. Low-molecular-weight compounds were extracted with perchloric acid (0.4 mol L(-1)) to furnish a fraction containing 3 to 15% of the total selenium in different types of nuts. The proteins were isolated from nut samples by dissolution in 0.1 mol L(-1) sodium hydroxide and subsequent precipitation with acetone. They were then dissolved in phosphate buffer pH 7.5. Analysis of protein fractions focused on selenium in two possible states - weakly and firmly bound to proteins. Results obtained for Brazil nuts by size-exclusion chromatography with on-line ICP-MS detection, in the absence and in the presence of beta-mercaptoethanol, showed that approximately 12% of total selenium was weakly bound to proteins. To obtain information about firmly bound selenium, the protein extracts were hydrolyzed enzymatically with proteinase K. Speciation was performed by means of ion-pairing HPLC-ICP-MS. The primary species found in all types of nuts was Se-methionine (19-25% of total selenium for different types of nuts).
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PMID:HPLC-ICP-MS determination of selenium distribution and speciation in different types of nut. 1217 80

The purpose of this in vitro study was to evaluate the mineral contents of root-canal dentin before and after treatment with two commonly used gutta-percha solvents: chloroform and halothane. Twenty extracted human premolars, whose crowns and apical thirds had been removed, were used. Pulp tissues were removed and the teeth were randomly divided into two groups including 10 teeth each. Root canals were enlarged with Gates Glidden burs (#1, 2, and 3). Dentin chips were obtained and saved in plates to serve as a control. Root-canal-dentin walls were then treated with chloroform or halothane for 15 min. Dentin chips were again obtained using Gates Glidden burs (#4, 5, and 6). The levels of five elements, calcium, phosphorus, magnesium, potassium, and sulfur, in each specimen were analyzed using ICP-AES (inductively coupled plasma atomic emission spectrometry) technique. Changes in the levels of the chemical elements were recorded. Differences between the groups were statistically analyzed using Mann-Whitney U test. There was a significant decrease in Ca level and significant increase in Mg level after treatment with halothane (p < 0.05). There was a significant increase in Mg level after treatment with chloroform. The changes in other elements levels after treatment with gutta-percha solvents were minimal and statistically not significant (p > 0.05). As a result it was concluded that gutta-percha solvents have effect on mineral contents of root dentin.
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PMID:Effect of gutta-percha solvents on mineral contents of human root dentin using ICP-AES technique. 1476 Sep 10

In this work the quantitative determination and analytical speciation of arsenic were undertaken in different types of nuts, randomly purchased from local markets. The hardness of the whole nuts and high lipid content made the preparation of this material difficult for analysis. The lack of sample homogeneity caused irreproducible results. To improve the precision of analysis, arsenic was determined separately in nut oil and in the defatted sample. The lipids were extracted from the ground sample with the two portions of a mixture of chloroform and methanol (2:1). The defatted material was dried and ground again, yielding a fine powder. The nut oil was obtained by combining the two organic extracts and by evaporating the solvents. The two nut fractions were microwave digested, and total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained for oils from different types of nuts showed element concentration in the range 2.9-16.9 ng g(-)(1). Lower levels of arsenic were found in defatted material (<0.1 ng g(-)(1) with the exception of Brazil nuts purchased with and without shells, 3.0 and 2.8 ng g(-)(1) respectively). For speciation analysis of arsenic in nut oils, elemental species were extracted from 2 g of oil with 12 mL of chloroform/methanol (2:1) and 8 mL of deionized water. The aqueous layer, containing polar arsenic species, was evaporated and the residue dissolved and analyzed by ion chromatography-ICP-MS. The anion exchange chromatography enabled separation of As(III), dimethylarsinic acid (DMAs(V)), monomethylarsonic acid (MMAs(V)), and As(V) within 8 min. Several types of nuts were analyzed, including walnuts, Brazil nuts, almonds, cashews, pine nuts, peanuts, pistachio nuts, and sunflower seeds. The recovery for the speciation procedure was in the range 72.7-90.6%. The primary species found in the oil extracts were As(III) and As(V). The arsenic concentration levels in these two species were 0.7-12.7 and 0.5-4.3 ng g(-)(1), respectively. The contribution of As in DMAs(V) ranged from 0.1 +/- 0.1 ng g(-)(1) in walnuts to 1.3 +/- 0.3 ng g(-)(1) in pine nuts. MMAs(V) was not detected in almonds, peanuts, pine nuts, sunflower seeds, or walnuts, and the highest concentration was found in pistachio nuts (0.5 +/- 0.2 ng g(-)(1)).
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PMID:Speciation of arsenic in different types of nuts by ion chromatography-inductively coupled plasma mass spectrometry. 1503 Jan 96

The ultrasonically induced degradations of nickel(II) 2,9,16,23-tetraphenoxy-29H, 31H-phthalocyanine and vanadyl 2,9,16,23-tetraphenoxy-29H, 31H-phthalocyanine in a biphasic system consisting of chloroform and water are investigated. Decolourisation of the organic phase containing the metallo-phthalocyanines is found to occur rapidly (approximately minutes for 8 ml of ca. 5 microM solution). Analysis of the aqueous solute via ICP-OES, reveals significant amounts of the released nickel ultimately transfers into the aqueous phase but at a rate much slower than that of decolourisation, whereas the vanadium remains within the organic phase suggesting only partial degradation despite efficient decolourisation.
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PMID:Ultrasonically induced phthalocyanine degradation: decolouration vs. metal release. 1515 64

A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os.
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PMID:Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction. 1796 32

In this work, different analytical speciation schemes have been used to study the reduction of Cr(VI) by a chromate-resistant strain of filamentous fungi Ed8 (Aspergillus sp), indigenous to contaminated industrial wastes. As demonstrated previously, this strain has the capability to reduce chromate present in the growth medium without its accumulation in the biomass, yet the reduced chromium end-products have not been characterized. Liquid growth medium, initially containing 50 mg L(-1) Cr(VI), was analyzed for Cr(III)/Cr(VI) and for total Cr at different time intervals (0-24 h) after inoculation with fungi. Three hyphenated procedures, based on the Cr(III)-EDTA formation and species separation by anion-exchange or ion-pairing reversed-phase chromatography with ICP-MS or DAD detection were used. The results obtained for Cr(VI) in each case were consistent, demonstrating efficient reduction of chromate during 24 h of Ed8 growth. However, pre-column complexation with EDTA did not ensure complete recovery of the reduced forms of chromium in the above procedures. An alternative speciation scheme, based on extraction of Cr(VI)-benzyltributylammonium bromide (BTAB) ion pairs into chloroform and subsequent determination of residual chromium by ICP-MS has provided evidence on the effective conversion of chromate into reduced chromium species in the growth medium. The results indicate the feasibility of using Ed8 strain for chromate bioremediation purposes. Analytically it can be concluded that speciation of chromium in biological systems should not be limited to its two most common oxidation states, because the actual reduced chromium species are not converted quantitatively to Cr(III)-EDTA.
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PMID:Analytical speciation of chromium in in-vitro cultures of chromate-resistant filamentous fungi. 1866 54

Strontium has been determined in a human serum reference material by ICP-MS and by NAA. By ICP-MS, results for (88)Sr and (86)Sr in both 10- and 5-fold diluted serum were in good agreement. For (88)Sr the precision was better than 3% and the detection limit was 0.05 mug/l. under the conditions used. The results were 25.5 mug/l. in the liquid serum or 0.281 mug/g in the lyophilized reference material. In the NAA the (87m)Sr produced was radiochemically separated by extraction with oxine in chloroform. The precision was about 10% and the detection limit 0.02-0.05 mug/g.
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PMID:Determination of strontium in human serum by inductively coupled plasma mass spectrometry and neutron activation analysis: A comparison. 1896 26


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