The determination of metals in organic compounds

Summary A comprehensive review of the methods available for the determination of metals in organic compounds has been made. The following metals have been considered:—sodium, potassium, lithium, rubidium, caesium, magnesium, calcium, barium, strontium, boron, thallium, silicon, germanium, antimony, bismuth, tin, lead, selenium, tellurium, silver, gold, osmium, platinum, copper, cadmium, zinc, mercury, vanadium, chromium, iron, cobalt, nickel, niobium, tantalum, rhenium, titanium, zirconium and uranium.

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Zusammenfassung Eine vollständige Übersicht über Methoden zur Bestimmung von Metallen in organischen Verbindungen wird gegeben. Für folgende Metalle werden Methoden beschrieben: Natrium, Kalium, Lithium, Rubidium, Cäsium, Magnesium, Calcium, Barium, Strontium, Bor, Thallium, Silicium, Germanium, Antimon, Wismut, Zinn, Blei, Selen, Tellur, Silber, Gold, Osmium, Platin, Kupfer, Cadmium, Zink, Quecksilber, Vanadium, Chrom, Eisen, Kobalt, Nickel, Niob, Tantal, Rhenium, Titan, Zirkonium und Uran.

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Résumé On donnait une revue complète des méthodes valables pour le dosage des métaux dans des substances organiques. Des méthodes sont décrites pour les métaux suivants: sodium, potassium, lithium, rubidium, caesium, magnésium, calcium, barium, strontium, bore, thallium, silicium, germanium, antimoine, bismuth, étain, plomb, sélénium, tellure, argent, or, osmium, platine, cuivre, cadmium, zinc, mercure, vanadium, chrome, fer, cobalt, nickel, niobe, tantale, rhenium, titane, zirconium et urane.

     

Elemental content in wheat products of Al-Qusim region, Saudi Arabia using the INAA technique

Wheat is one of the most grown crops in Saudi Arabia. It is grown in various regions of the country. Accurate knowledge of the elemental concentrations in wheat and its products (bran and flour) is of great importance from a nutritional point of view. Wheat samples were obtained from the Al-Qusim region, 300 km northwest of Riyadh, and analyzed. Up to 50 elements (Al, Sb, As, Ba, Br, Cd, Ca, Cs, Cl, Cr, Co, Cu, Ga, Au, Hf, In, I, Ir, Fe, Mg, Mn, Hg, Mo, Ni, K, Rb, Sc, Se, Ag, Na, Sr, Ta, Te, Th, Sn, Ti, W, U, V, Zn, Zr, Ce, Dy, Eu, La, Lu, Nd, Sm, Tb and Yb) were determined in the wheat products. It was observed that the elemental content of bran was much higher than that of white flour.     

Strategy for water analysis using ICP-MS

The developed strategy permits determination in three steps of sixty-seven elements using inductively coupled plasma mass spectrometry (ICP-MS). Sodium, Mg, Si, S, Cl, K, and Ca are determined in a first step; B, Al, P, Cr, Fe, Mn, Ni, Cu, Zn, As, Se, Ag, Cd, Sb, Ba, Hg, and Pb are determined in a second step; and Li, Be, Ti, V, Co, Ga, Ge, Br, Rb, Sr, Y, Zr, Nb, Mo, Sn, Te, I, Cs, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Pt, Au, Tl, Bi, Th, and U are analyzed in a third step. The figures of merit obtained are adequate to carry out water quality monitoring and other hydrochemical studies, such those based in the application of hydrochemical fingerprinting to water management.     

Traceability along the production chain of Italian tomato products on the basis of stable isotopes and mineral composition

The paper shows the variability of stable isotope ratios and mineral composition in tomato and derivatives along the production chain (juice, passata and paste) in order to evaluate the possibility of tracing their geographical origin. The ratios (13)C/(12)C, (15)N/(14)N, (18)O/(16)O, D/H, (34)S/(32)S and the content of Li, Be, B, Na, Mg, Al, P, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Mo, Ag, Cd, Sn, Sb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Tm, Yb, Ir, Tl, Pb, U and of nitrates, chlorides, sulphates and phosphates were measured by Isotope Ratio Mass Spectrometry, Inductively Coupled Plasma Mass Spectrometry and Ion Chromatography, respectively. The tomato products were from three Italian regions - Piedmont, Emilia Romagna, and Apulia. By applying linear discriminant analysis on 17 of these parameters (Gd, La, Tl, Eu, Cs, Ni, Cr, Co, δ(34)S, δ(15)N, Cd, K, Mg, δ(13)C, Mo, Rb and U) excellent discrimination among products from the three regions was achieved. Irrespective of the processing technology, over 95% of the samples were correctly reclassified in cross-validation into the production site. The use of these parameters will allow the development of analytical control procedures that can be used to check the geographical provenance of Italian tomatoes and products derived from them.     

Synthesis of 2‐Arylquinazolin‐4(3H)‐ones by N‐Aryl Benzamidines with Aromatic Carbonates

The reaction of N‐aryl benzamidines 1a , 1b , 1c , 1d , 1e , 1f , 1g , 1h , 1i , 1j , 1k , 1l , 1m , 1n with diphenyl carbonate 2a or ethyl phenyl carbonate 2b synthesized 2‐arylquinazolin‐4(3H)‐ones 3a , 3b , 3c , 3d , 3e , 3f , 3g , 3h , 3i , 3j , 3k , 3l , 3m , 3n in simple and safe process with good yields (71–90%). It was suggested that different electron‐donating substituent in N‐aryl benzamidines 1a , 1b , 1c , 1d , 1e , 1f , 1g , 1h , 1i , 1j , 1k , 1l , 1m , 1n afforded similar effect to the yields of 2‐arylquinazolin‐4(3H)‐ones 3a , 3b , 3c , 3d , 3e , 3f , 3g , 3h , 3i , 3j , 3k , 3l , 3m , 3n . In these reactions, N‐aryl benzamidines 1a , 1b , 1c , 1d , 1e , 1f , 1g , 1h , 1i , 1j , 1k , 1l , 1m , 1n built up intermediate compounds by nucleophilic addition to carbonates 2 to give annulation products 3a , 3b , 3c , 3d , 3e , 3f , 3g , 3h , 3i , 3j , 3k , 3l , 3m , 3n , following to cyclization involving the elimination of ethanol/phenol.     

Der Nachweis organischer Farbstoffe durch Mikrosublimation. II Besonderer Teil

Zusammenfassung Folgende organische Farbstoffe, die entweder als Pulver oder auch als Ausfärbung oder als Druck vorlagen, gaben kennzeichnende Sublimate:Indischgelb G, Dianilgelb G, die Hansagelbsorten 10 G, 5 G, 5 G transparent, 3 G, G, G transparent, GGR extra, GR, 3 R, Litholechtgelb RN, Helioechtgelb 6 GL, Litholechtorange RN, Permanentrot R extra, Litholechtscharlach RN (Hansarot B), Litholechtscharlach B, Permanentrot FRL, Autolrot BL, Autolrot RLP, Brillant-Indigo BASF, Indanthrengelb G, Indanthrenbraun G, Indanthrenblau RSN, Indanthrenviolett FFBN, Indanthrengelb 7 GK, Indanthrenbrillantorange GR, Indanthrenbrillantorange RK.

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Summary The following organic dyestuffs which were present either as powders or as dyed or printed material, gave characteristic sublimates:Indian yellow G, dianil yellow G, the 10 G, 5 G, 5 G transparent, 3 G, G, G transparent, GGR extra, GR, 3 R brands of Hansa yellow, lithol-fast yellow RN, helio-fast yellow 6 GL, lithol-fast orange RN, permanent red R extra, lithol-fast scarlet RN (Hansa red B), lithol-fast scarlet B, permanent red FRL, autol red BL, autol red RLP, brilliant indigo BASF, indanthrene yellow G, indanthrene brown G, indanthren blue RSN, indanthrene violet FFBN, indanthrene yellow 7 GK, indanthrene brilliant orange GR, indanthrene brilliant orange RK.

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Résumé Les pigments organiques suivants, qui étaient à notre disposition, soit comme poudre, soit comme colorisation ou comme impression, donnèrent des sublimés caractéristiques:Indischgelb G, Dianilgelb G, les sortes de Hansagelb 10 G, 5 G, 5 G transparent, 3 G, G, G transparent, GGR extra, GR, 3 R, Litholechtgelb RN, Helioechtgelb 6 GL, Litholechtorange RN, Permanentrot R extra, Litholechtscharlach RN (Hansarot B). Litholechtscharlach B, Permanentrot FRL, Autolrot BL, Autolrot RLP, Brillant-Indigo BASF, Indanthrengelb G, Indanthrenbraun G, Indanthrenblau RSN, Indanthrenviolett FFBN, Indanthrengelb 7 GK, Indanthrenbrillantorange GR, Indanthrenbrillantorange RK.

     

NAA and ICP analysis of obsidian from Central Europe and the Aegean: Source characterisation and provenance determination

INAA and ICPES are compared for their discriminative power in obsidian source characterisation. Geological samples from the Aegean and Carpathian sources were analysed for Na, Sc, Fe, Co, Rb, Sb, Cs, Ba, La, Ce, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th, U by INAA and for B, Na, Mg, Al, K, Ca, Sc, Ti, Mn, Fe, Zn, Y, Yr, Cs, Ba, La, Ce, Sm, Eu, Gd, Tb, Yb, Lu, Hf by two ICPES procedures. It is shown that all techniques work successfully, however, INAA is more efficient in the chemical discrimination of neighbouring sources.     

A systematic neutron activation analysis of peat from Burundi

Mean concentrations of Al, As, Au, Ba, Br, Ca, Ce, Cl, Co, Cr, Cs, Cu, Eu, Fe, Ga, Hf, Ho, I, K, La, Lu, Mg, Mn, Na, Pr, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Ti, Th, V, W, Yb, and Zr, determined in 6 samples of peat from Burundi, were equal to 3911, 1.7, 0.025, 33, 21, 472, 14, 55, 4.2, 16, 0.43, 14, 0.27, 14675, 1. 2, 1.5, 0.09, 2.9, 203, 5.6, 0.29, 745, 20, 70, 1.5, 13, 2.1, 6.5, 0.8, 6, 0.4, 0.2, 2.9, 392, 15.7, 0.43, 0.09 and 101 ppm resp. The peat in Burundi contain approximately the same concentrations of elements as the peat in other countries. It is enriched in Br and depleted in Ca, K, Mn, Na, Sr and Yb.     

Systematic study of the solvent extraction of metal oxinates

The extraction of 32 metals (Be, Mg, Ca, Sr, Ba, Sc, La, Ti, Zr, Th, V, Nb, Cr, Mo, W, U, Mn, Fe, Co, Ni, Pd, Cu, Ag, Zn, Cd, Hg, Al, Ga, In, Tl, Pb and Bi) with oxine solution has been studied. The effects of pH, oxine concentration and water-soluble complexing agents (oxalic acid, tartaric acid, hydrocyanic acid, nitrilotriacetic acid, ethylenediaminetetraacetic acid and 1,2-diaminocyclohexanetetraacetic acid) have been investigated. From these results the extraction constants and stability constants ot the metal complexes with the various complexing agents investigated have been calculated.     

Determination of trace element impurities in aspirin tablets by neutron activation analysis

Twenty five trace and minor elements (aluminium, arsenic, barium, bromine, cerium, chlorine, cobalt, chromium, cesium, europium, iron, hafnium, potassium, magnesium, manganese, sodium, rubidium, antimony, scandium, selenium, strontium, thorium, titanium, vanadium and zinc) in five different Egyptian aspirin brands (Aspo, Askin, Aspocid, Aspeol and Rivo) have been determined by instrumental neutron activation analysis. It has been concluded that the concentration of arsenic, barium, bromine, cobalt, chromium, iron (except in Aspocid), magnesium, manganese, rubidium, selenium, strontium and zinc in the Egyptian brands is below or within the concentration range reported for these elements in 16 American aspirin and aspirin-like brands.     

Trace element profile of a wild edible mushroom (Suillus granulatus)

Seventeen elements, Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, V, and Zn (macroelements and trace elements) were investigated by Atomic Spectrometries on a particular wild edible mushroom collected in the central region of Argentina during 2 different years in the same season. The metal content profile in Suillus granulatus samples is given. The found quantities of Na, K, Ca, Mg, Fe, P, V, and Al were 0.40, 10.84, 0.48, 0.30, 0.57, 4.24, 0.18, and 1.23 g/kg dry weight, respectively. The levels of Li, Cu, Zn, Cd, Co, Ni, Cr, and Mn were 0.98, 23.02, 22.30, 0.26, 0.16, 1.17, 0.90, and 28.75 mg/kg dry weight, respectively. Pb was not detected at the investigated levels. The results indicate that the levels of metals in the analyzed samples are not considered to be a health risk. In order to demonstrate the validity of our method, a recovery study was performed with acceptable results.     

Excretion of biotrace elements using the multitracer technique in mice

A radioactive multitracer solution obtained from the nuclear reaction of selenium with 25 MeV/nucleon⁴⁰Ar ions was applied to the investigation of the trace elements behavior in feces and urine of mouse. The excretion rates of 23 elements, Na, K, Rb, Mg, Ca, Sr, Ga, As, Sc, V, Cr, Mn, Co, Fe, Zn, Y, Zr, Mo, Nb, Tc, Ru, Ag and In were simultaneously detected under strictly identical experimental conditions, in order to clarify the excretion behavior of the elements in mice. Fecal and urinary excretion rates of the elements in mice reached the highest value separately at 48 and 24 hours. The total excretion of Mo, Tc and Co within 96 hours were all larger, more than 60%. Accumulative excretion rates of Ca, Nb, Mg, Sr, V, Sc, Na, Cr, Fe, Ag, Mn and Zr were 60-30%. The total rates of Ru, K, As, Zn, Rb, Y, Ga and In were less than 30%, and low excretion. The main excretion pathway of Mo, Co, Mg, Fe and Ag was through urine, and Na, K, As and Rb were eliminated from the body also in urine. But fecal excretion of Tc, Nb, Sr, Y, Ru, and In were larger than urinary excretion, and Ca, Sc, Mn, Zr, Zn were eliminated from the body in feces.     

INAA and ICP-MSHS: Metal pollutants in fish tissues Nile tilapia (<Emphasis Type="Italic">Oreochromic niloticus</Emphasis>) in Pampulha Lake,Belo Horizonte city,Minas Gerais State,Brazil

Pampulha Lake, Minas Gerais, Brazil, is being polluted via its tributaries, Sarandi and Ressaca. Instrumental neutron activation analysis and inductively coupled plasma mass spectrometry high resolution were applied to determine Al, As, B, Ba, Co, Cr, Cs, Cu, Fe, K, Mg, Mn, Mo, Na, P, Pb, Rb, Zn and Ti in Nile tilapia fish, Oreochromis niloticus. The organs analyzed were: intestine, spleen, heart, testicle, kidney, liver, gills and muscle. The results demonstrated relatively high concentrations of Al, Co, Cu, Fe, P and Ti in gills, Al and Cu in liver, Al in intestine and Fe in muscle and spleen.     

Major,minor and trace element mass fractions determined using ED-XRF,WD-XRF and INAA for five certified clay reference materials: NCS DC 60102–60105; NCS DC 61101 (GBW 03101A, 03102A, 03103, and 03115)

Major, minor and trace element mass fractions were determined using wavelength dispersive and energy dispersive X-ray fluorescence and instrumental neutron activation analysis for five clay certified reference materials (NCS DC 60102–60105, 61101) distributed by the National Research Center for Certified Reference Materials in China. We report mass fractions for 10 major and the following 29 minor and trace elements: As, Ba, Ce, Co, Cr, Cs, Cu, Eu, Hf, La, Lu, Nb, Nd, Ni, Pb, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Th, U, V, Y, Yb, Zn, and Zr.     

Determination of impurities in titanium and titanium oxide by radiochemical neutron activation analysis

A radiochemical neutron activation analysis has been applied to 2N–4N grade titanium metal and its oxide. Twenty two impurities were separated in a group from scandium by a radiochemical separation method using cation exchange resin with HBr and HCl. The contents of the elements were calculated by a single comparator method using two monitors. The analytical results agree well within 10% deviation with those obtained by instrumental method. Eighteen elements, Na, Fe, Co, As, Se, Sr, Mo, Sb, La, Eu, Tb, Yb, Lu, Hf, Ta, W, Th and U, are determined in titanium oxides and 17 elements, Na, Cr, Fe, Co, Se, As, Zr, Mo, Sb, Cs, Ce, Tb, Yb, Hf, Ta, W and Th, in titanium metals.     

Polynuclear heterocyclic compounds. XIX. Reduction of 3,3,6,6-tetramethyloctahydroacridine-1,8-diones

Reduction in alcohol solution, using hydrogen at atmospheric pressure and platinum oxide catalyst, of 3, 3, -6, 6-tetramethyl-1, 2, 3, 4, 5, 6, 7, 8-octahydroacridine-1, 8-dione and its 9-phenyl derivative gives the corresponding 3, 3, 6, 6-tetramethyl-1, 2, 3, 4, 5, 6, 7, 8, 9, 10-decahydroacridine-1, 8-dione and its 9-phenyl derivative.For part XVIII see [1].     

Intercomparison of moss reference material by different multi-element techniques

An intercomparison of data obtained for a moss reference material (Hylocomium splendens) used as biomonitor of atmospheric deposition by different multi-element techniques is presented. In total 43 elements (Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Zr, Ag, Sn, Sb, I, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Tm, Yb, Lu, Hf, Ta, W, Au, Th, U) were determined using inductively coupled plasma-mass spectrometry (ICP-MS), conventional instrumental neutron activation analysis (INAA), epithermal neutron activation analysis (ENAA) and as well as shorttime neutron activation analysis without and with a⁶LiD-converter. Advantages and drawbacks of each method are discussed. The introduction of moss reference materials for atmospheric multi-element deposition studies involving nuclear analytical techniques is strongly recommended.     

Determinations de traces dans les semi-conducteurs par activation neutronique

Résumé On décrit la détermination de traces dans le germanium, le silicium et le sélénium. En appliquant des techniques gamma spectrométriques, précédées ou non de séparations chimiques il est possible de doser les éléments suivants dans (1) germanium: As, Cu, Au, Ga, Zn, Hg, Cr, Sn, Sb, Co, In, Ni, Ir, Se, Sc, Ag, Ta, Hf et U; (2) silicium: P, Au, Sb, Ga, Fe, K, Cr, Mo, Sn, As, Co, In, Zn, Cu, W, Ta, Na, Eu, Sm, La, Sc et T1; (3) sélénium: Cl, Br, I, P, S, Te, Na, K, Cr, Fe, Co, Cu, Zn, Ga, Sc, Ag, Cd, La, W, Au et Tl. Les concentrations et ou limites de détections varient de quelques parties par million à 10⁻³ parties par milliard.     

Identification and differentiation of barbiturates, other sedative-hypnotics and their metabolites in urine integrated in a general screening procedure using computerized gas chromatography-mass spectrometry

A gas chromatographic-mass spectrometric procedure is described for the identification and differentiation of sedative-hypnotics and their metabolites in urine. The following 24 barbiturates and thirteen other hypnotics could be detected: acecarbromal, allobarbital, amobarbital, aprobarbital, barbital, brallobarbital, bromisoval, (sec)butabarbital, butalbital, butobarbital, carbromal, clomethiazole, crotylbarbital, cyclobarbital, cyclopentobarbital, diethylallylacetamide, dipropylbarbital, glutethimide, guaifenesin, ethinamate, heptabarbital, hexobarbital, meprobamate, methaqualone, metharbital, methohexital, methylphenobarbital, methyprylone, pentobarbital, phenobarbital, propallylonal, pyrithyldione, secobarbital, thiobutabarbital, thiopental, vinbarbital and vinylbital. The procedure presented is integrated in a general screening procedure (general unknown analysis) for several groups of drugs detecting over 300 drugs and over 1000 of their metabolites. It includes cleavage of conjugates by acid hydrolysis, isolation by liquid-liquid extraction, derivatization by acetylation, separation by capillary gas chromatography, and identification by computerized mass spectrometry. Using mass chromatography with the selected ions m/z 83, 117, 141, 167, 169, 207, 221 and 235, the presence of barbiturates, other hypnotics and/or their metabolites was indicated. The identity of positive signals in the reconstructed mass chromatograms was confirmed by a visual or computerized comparison of the stored full mass spectra with the reference spectra. The sample preparation, mass chromatograms, reference mass spectra and gas chromatographic retention indices are documented.