Ion-exchange separation and spectrophotometric determination of boron in geological materials

Various dissolution techniques were investigated for total rocks and minerals and the best approach found was alkaline fusion. Boron in silicates was rendered chemically reactive by fusion with potassium carbonate, the fusion cake was extracted with water and borate was isolated by Amberlite XE-243 boron-selective resin. The Amberlite XE-243 resin was utilized to separate microgram amounts of boron from natural waters (fresh to hypersaline) and salt cores. Borate was eluted with 2 M hydrochloric acid and determined by spectrophotometry of the carminic acid complex at 620 nm in either 94% sulphuric acid or sulphuric/acetic acid (20:80) medium, or preferably, as the azomethine-H ion-association complex at pH 5.2 (415 nm), depending on the sensitivity required. Good precision and accuracy were obtained on several international standard rocks with an average relative standard deviation of 1.37%.     

Ion-exchange separation and spectrophotometric determination of vanadium in environmental samples

A selective and sensitive method for the extraction and spectrophotometric determination of vanadium(V) in microgram quantities is described. The molar absorptivity of the yellow vanadium(V)-caffeic acid-Aliquat 336 extract is 1.3 x 10(4) 1.mole(-1).cm(-1) at 370nm. The method is compared with the atomic-absorption spectrometric method and applied to the trace determination of vanadium in steel, alloys, a rock and environmental samples.     

Ion-exchange separation and spectrophotometric determination of titanium in biological materials

Summary A combined anion-exchange-spectrophotometric method has been worked out for the determination of titanium in biological materials. The sample is dry-ashed at 420°C. The ash (ca. 0.5 g) is then decomposed with a mixture of nitric, perchloric and hydrofluoric acids, and is finally taken up in hydrochloric acid. The titanium is collected by anion-exchange on an Amberlite CG 400 (SCN^–) column from 1 M thiocyanate — 1 M hydrochloric acid solution and eluted with 4 M hydrochloric acid. Titanium is subsequently determined spectrophotometrically with diantipyrylmethane. Results of the determination of titanium in various materials of biological origin and in two NBS standard biological samples are compiled. Standard deviations are in the range of 3–9% (2.4% in synthetic mixtures).

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Spurenbestimmung von Titan in biologischem Material durch Kombination von Anionenaustauscher-Trennung und Spektralphotometrie

Zusammenfassung Bei der vorgeschlagenen Methode wird die Probe bei 420° C trocken verascht, die Asche mit einer Mischung von Salpeter-, Perchlor- und Flußsäure aufgeschlossen und in Salzsäure aufgenommen. Titan wird dann aus 1 M Thiocyanat-Salzsäurelösung an dem Anionenaustauscher Amberlite CG 400 (SCN^–) adsorbiert und mit 4M Salzsäure eluiert. Danach erfolgt die spektralphotometrische Bestimmung mit Diantipyrylmethan. Das Verfahren wurde auf synthetische Gemische, verschiedenartige biologische Materialien und zwei NBS-Standardsubstanzen angewendet. Die Standardabweichungen liegen im Bereich von 3–9% (2,4% für synthetische Gemische).

     

The preconcentration, separation and spectrophotometric determination of traces of silicate

A method for the determination of traces of silicate based on the use of a strong base anion exchange in a preconcentration step and a batch-reactive stripping agent technique prior to spectrophotometric determination has been proposed. The reaction of molybdate and silicate in acidic solution to form 12-molybdosilicic acid permits recoveries exceeding 90% in analyzing solutions containing 0.02 to 0.1 μg of silicon/ml.     

Combined anion-exchange separation and spectrophotometric determination of traces of titanium in sea water

Summary Traces of titanium in sea water have been preconcentrated by anion-exchange from acidified samples in the presence of thiocyanate. Titanium adsorbs strongly on a column of Amberlite CG 400 (SCN^–) and can be stripped easily by elution with 2 M hydrochloric acid — 1.5% hydrogen peroxide solution. Titanium in the effluent is determined spectrophotometrically with diantipyrylmethane as colour reagent. The combined method allows to determine traces of titanium very selectively and sensitively in sea water as well as non-saline water on a 41 sample basis. The method yields a coefficient of variation of 7% at a titanium level of 0.4 g per l.

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Kombinierte Anionenaustauscher-Trennung und spektralphotometrische Bestimmung von Titanspuren in Meerwasser

Zusammenfassung Titanspuren wurden in Gegenwart von Thiocyanat durch Anionenaustausch aus der angesäuerten Probe angereichert. Titan wird an Amberlite CG 400 (SCN^–) stark adsorbiert und kann durch Elution mit 2M HCl — 1,5% H₂O₂ leicht abgelöst werden. Im Eluat wird es spektralphotometrisch mit Diantipyrylmethan bestimmt. Die kombinierte Methode gestattet eine selektive und empfindliche Bestimmung in einer 41-Probe von Meer- oder auch Süßwasser. Für einen Gehalt von 0,4 g Ti/l beträgt der Variationskoeffizient 7%.

     

A selective lon-exchange separation and spectrophotometric determination of traces of copper in silicate rocks

Summary A combined cation-exchange separation-spectrophotometric procedure has been worked out for the accurate determination of traces of copper in silicate rocks. Silicates are opened up with sulfuric and hydrofluoric acids. The residue is taken up into a 0.5 M hydrochloric acid −0.05 M oxalic acid −1% hydrogen peroxide solution and loaded on a strongly acidic cation-exchange resin column. Polyvalent ions including ferric ions do not adsorb on the column, while copper (II) retains together with divalent metal ions as well as aluminum (III). Copper (II) can selectively be eluted by a small volume of 0.05 M thiosulfate solution. This fraction is sufficiently pure to allow a direct spectrophotometric determination of copper with Na-DDTC without the addition of tartrate and EDTA as masking agents. Quantitative results are quoted for the determination of copper in international standard rocks of the Geological Survey of Japan (GSJ) and the U.S. Geological Survey (USGS).     

Kinetic spectrophotometric determination of traces of sulfide

A method for the determination of sulfide based on the addition reaction of sulfide with magenta at pH 7 and 25 degrees C is described. The decrease in absorbance of magenta at 540 nm, its lambda(max), over a fixed time is proportional to the concentration of sulfide over the range of 25-2500 ng ml(-1). The limit of detection was found to be 15 ng ml(-1). Ten replicate analysis of a sample solution containing 1.5 mug ml(-1) sulfide gave a relative standard deviation of 0.8%. The effects of various cations and anions on sulfide determination have been reported and procedures for removal of interferences have been described.     

Atomic-absorption spectrophotometric determination of traces of manganese with thenoyltrifluoroacetone

An atomic-absorption spectrophotometric method for the determination of traces of manganese in solution with thenoyltrifluoroacetone (TTA) is described. Manganese(II) is extracted with 0.01M TTA in methyl isobutyl ketone (MIBK) at pH 9.5. The atomic-absorption of the organic phase at 279.5 nm is measured. Except for chromium, iron, hafnium, niobium, nickel, rhodium, tin, titanium and zirconium, microquantities of many other cations and anions do not interfere. Iron can be removed by MIBK extraction before the TTA extraction. The sensitivity of the method was 1.6 ng/ml for 1% absorption in aqueous solution. The method was successfully applied to the analysis of environmental waters. Manganese in the filtered fractions of water samples was reliably determined with relative standard deviations of 7% at the 5 mug/l. level and 1% at 50 mug/l.     

Chemical separation and determination of traces of phosphorus

Summary A rapid procedure for the concentration of highly diluted aqueous solutions containing traces of phosphorus (down toca. 0.0025 p. p. m.) is described. The method is based upon (a) selective carrying of P(V) by ignited BaSO₄ or SrSO₄ in presence of a suitable charge determining cation, (b) stripping the carried phosphorus quantitatively in small volume of HC1 solution. The phosphorus concentrate is then spectrophotometrically determined by the molybdenum blue method, and the amount of the trace element in the original sample is estimated by applying a radiometric correction factor. Conditions have been worked out for applying the method in presence of the following interfering ions: As(III) (400 p. p. m.), Al³⁺ (200 p. p. m.), Fe³⁺ (200 p. p. m.), and over 1000 p. p. m. of each of Ca²⁺, Mg²⁺, Cu²⁺, Mn²⁺ and Cr³ ions. The net recovery (uncorrected) of phosphorus in the concentrated form comes toca. 98–99%, and the net error of estimation after correction can be minimised to the limit of accuracy of spectrophotometric determination.

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Zusammenfassung Die rasche Anreicherung von Phosphorspuren (zirka 0,0025 ppm) aus hochverdünntea wäßrigen Lösungen wurde beschrieben. Sie beruht a) auf der selektiven Adsorption von P(V) an geglühtes BaSO₄ oder SrSO₄ in Gegenwart eines geeigneten Kations; b) auf der quantitativen Überführung des adsorbierten Phosphors in ein kleines Volumen Salzsäure. Der angereicherte Phosphor wird dann nach der Molybdänblaumethode bestimmt und die Menge des in der ursprünglichen Probe enthaltenen Spurenelementes mit einem radiometrischen Korrekturfaktor ermittelt. Die Arbeitsbedingungen bei Anwesenheit der störenden Ionen As(III) (400 ppm), Al(III) (200 ppm), Fe(III) (200 ppm) und über je 1000 ppm Ca, Mg, Cu(II), Mn(II) und Cr(III) wurden ermittelt. Die unkorrigierte Ausbeute an Phosphor in der angereicherten Form beträgt etwa 98 bis 99%, der Fehler nach der Korrektur entspricht der Genauigkeitsgrenze der spektrophotometrischen Bestimmung.

     

Kinetic spectrophotometric determination of traces of iron(II)

A simple method for the selective and sensitive kinetic spectrophotometric determination of iron (II) is described. The method is based on the oxidation reaction of reduced phenolphthalein by periodate in alkaline media. The change in absorbance was measured using the fixed time method. The effect of different variables on the reaction was investigated and optimum conditions were obtained. The calibration curve was linear in the range 50–3000 ng/mL, and a detection limit of 17 ng/mL was obtained. The relative standard deviation of ten replicate determinations of 200 ng/mL of Fe(II) was 1.2%. The determination of Fe(II) in the presence of a 50-fold amount of Fe(III) could be carried out. This article was submitted by the authors in English.     

ET-AAS determination of traces of As, Sb and Sn in pure gold after matrix separation with hydrazine

Summary The possibilities of ET-AAS using the graphite furnace or the tungsten coil atomizer were compared by the trace As, Sb and Sn determination in the chloride-containing solution resulting after gold reduction with hydrazine. It was found that the tungsten coil atomizer tolerates higher concentrations of chloride ions than the conventional graphite furnace.     

Anion-exchange enrichment and spectrophotometric determination of traces of gallium in natural waters

Summary Traces of Ga in sea and fresh water have been enriched by anion-exchange from an acidified sample in the presence of thiocyanate. Gallium adsorbs strongly on a column of Amberlite CG 400 and can be stripped with a NaOH-NaCl solution. Gallium in the effluent is purified by anion-exchange from HCl and determined spectrophotometrically with Rhodamine B as colour reagent. The combined method allows to determine traces of Ga in sea water as well as fresh water on a 101 sample basis. The standard deviation is about 17% at a Ga level of 0.01 g/l.

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Anreicherung durch Anionenaustausch und spektralphotometrische Bestimmung von Galliumspuren in Meerwasser

     

Photochronometric determination of traces of gold(III)

Summary A method for the determination of traces of gold is based on the catalytic effect of Au(III) on the reduction of Ag(I) with Fe(II). The time elapsing from the addition of the Fe(II) solution to the appearance of a certain precipitation (determined photometrically) is measured and the Au content is read from a calibration curve. Interferences are caused by halogen and cyanide ions and by oxidizing agents. 45 ng of Au could be determined with a maximum error of 2.5 ng.

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Zusammenfassung Ein Verfahren zur Spurenbestimmung von Gold beruht auf der durch Goldionen katalysierten Reduktion von Silberionen mit Eisen(II). Hierbei wird die Zeit gemessen, die bis zum Auftreten einer gewissen Niederschlagsdichte vergeht, die photometrisch bestimmt wird. Der Goldgehalt ergibt sich aus einer Eichkurve. Halogen- und Cyanidionen sowie Oxydationsmittel verursachen Störungen. 45 ng Gold konnten mit einem Fehler von höchstens 2,5 ng wiedergefunden werden.