Determination of thiosulphate in the presence of dithionite and sulphite

To determine thiosulphate in the presence of dithionite and sulphite, iodine dissolved in potassium bromide solution is used to oxidize thiosulphate to tetrathionate, and dithionite and sulphite to sulphate. The tetrathionate generated from the thiosulphate is then oxidized with potassium bromate-potassium bromide solution in the presence of hydrochloric acid. The bromine consumption of the tetrathionate is measured by titration of the excess of bromine with sodium thiosulphate after the addition of potassium iodide. For each equivalent of iodine used to determine thiosulphate by the Wollak method, fourteen equivalents of bromine are used to determine thiosulphate by this method.     

Coulometric Determination of Total Cyanide in Effluent and Wastewater

Abstract

A simple procedure for the determination of low levels of total cyanide in effluent samples has been developed. After distillation of the cyanide from the sample, as hydrocyanic acid, the cyanide is determined with coulometrically generated iodine using a biamperometric end point detection system. As little as 0.06mg/l total cyanide can be measured using the procedure. The method obviates the need for calibration curves and does not require special reagents.

Silver (I) was determined to be an effective catalyst for the decomposition of bound cyanides in the distillation procedure.     

Solvent extraction studies of addition compounds of metal halides and triphenylphosphine, -arsine and -stibine : Detection of palladium

Palladium, is very efficiently extracted as PdI₂·₂(C₆H₅)₃Sb from weakly acidic medium, containing excess of iodide with a solution, of triphenylstibinc in cyclohexane. A test for the detection of palladium is described based on this property. In the presence of sulfite and in the absence of cyanide, which inhibits the reaction, the test is specific. A pink to red color develops in the organic layer enabling the identification of as little as 0.07 μg- Pd.     

The use of iodate and periodate with iodide in the potentiometric titration of arsenite,sulfide, and sulfite with mercury (II)

A new potentiometric method is adopted for the accurate microdetermination of arsenite, sulfide and sulfite. The reductant is added to a known excess of standard iodate or periodate properly acidified with sulfuric acid. To the brown solution containing iodine equivalent to the reductant, an excess of standard iodide solution is added followed by titrating unreacted iodide with mercury (II) potentiometrically using the silver amalgam as indicator electrode. The potential breaks which averaged 350 mV per 0.1 ml of 0.05 M titrant were sharp enough for the precise determination of end points, and hence the high accuracy of the present method. In addition, besides simplicity and rapidity the stoichiometry of the reaction between iodate or periodate with the above reductants is still maintained even with the very low concentration.     

Determination of total inorganic iodine in seawater by cathodic stripping square wave voltammetry

A method has been designed for the reduction of iodate to iodide in seawater and subsequent determination of total dissolved iodine as iodide by cathodic stripping square wave voltammetry. The pH of the sample is lowered to about 1-2 and iodate is reduced to iodide with sodium sulfite under this acidic condition. The pH of the sample is then raised to 8-9 before the concentration of iodide is measured.     

Solvent extraction studies of addition compounds of metal halides and triphenylphosphine, -arsine and -stibine : Part II. Spectrophotometric determination of palladium

Palladium extracted with a cyclohexane solution of triphenylarsine from weakly acidie medium containing excess iodide and sulfite, can be determined spectrophotometrically by measuring the; absorbance of the organic extract at 325 mμ. The optimum range of concentration was found to be 1 to 4 p.p.m. of palladium in the final dilution, Except for cyanide and large amounts of titanium(IV) and zirconium(IV), which inhibited the reaction, no other ion among the 41 tested interfered under the given conditions.     

A novel and efficient method for the synthesis of α-aminonitriles by the reaction of aminals with trimethylsilyl cyanide catalyzed by iodine

Iodine, was found to be a practical and novel catalyst for the reaction of aminal and trimethylsilyl cyanide under mild and neutral reaction condition to afford the corresponding α-aminonitriles in high yields and short reaction times. Trimethylsilyl iodide derived in situ from elemental iodine and trimethylsillyl cyanide catalyzed this conversion.     

Gaseous catalysts for end-point indication in titrimetric analysis in the microgram range with iodide and bromide as catalysts

A new technique for end-point detection in titrations with bromate is described. The first drop in excess causes evolution of bromine which is swept by nitrogen into an indicator vessel. There, the bromine reacts with iodide to form iodine which catalyzes the cerium(IV)—arsenic(III) reaction or with sulfite to form bromide which catalyzes the permanganate—iodine reaction. Microgram amounts of antimony(III) or arsenic(III) can be determined.     

Bismuthiol as an analytical reagent

Summary Lead can be determined from its Bismuthiol II complex volumetrically by dissolving it in an excess of EDTA at a p_H of about 10 and titrating the excess of the EDTA against a magnesium or lead solution. In the same way silver can be determined by dissolving the complex in an excess of cyanide and back titrating the excess against a standard silver nitrate with iodide as the indicator. The results of the former are fairly accurate while those due to latter are highly satisfactory with silver less than 20 mg. With higher amounts of silver, however, the results are within +2%.Part VIII see Z. analyt. Chem. 156, 103 (1957).     

Determination of ascorbic acid by iodate using iodine cyanide end point; indirect determination of vanadium, and colorimetric determination of ascorbic acid

Summary Two methods for the determination of ascorbic acid are described. The first employs titration with iodate in presence of cyanide and hydrochloric acid and starch indicator with two end points, corresponding to the formation of iodine after reduction to iodide and conversion of iodine to iodine cyanide respectively. The titration is applied to the indirect determination of vanadium(V). In the second method ascorbic acid is treated with excess ferric solution and the ferrous iron formed is determined colorimetrically by ortho-phenanthroline.

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Zusammenfassung Zwei Verfahren zur Ascorbinsäurebestimmung werden beschrieben. Bei dem ersten wird in Gegenwart von KCN und Salzsäure sowie von Stärke als Indicator mit Jodatlösung titriert. Dabei werden zwei Endpunkte erhalten, die der Reduktion von Jodat zu Jodid und damit verbundener Jodbildung bzw. der Umwandlung des Jods in JCN entsprechen. Diese Titration wird auch zur indirekten Bestimmung von Vanadium(V) verwendet. Bei dem zweiten Verfahren wird die Ascorbinsäure mit überschüssiger Eisen(III)-lösung behandelt und das gebildete zweiwertige Eisen colorimetrisch mit o-Phenanthrolin bestimmt.

     

Highly Selective and Sensitive Triiodide PVC‐Based Membrane Electrode Based on a New Charge Transfer Complex of 2‐(((2‐(((E)‐1‐(2‐Hydroxyphenyl) Methylidine) Amino) Phenyl) Imino) Methyl) Phenol for Nano‐Level Monitoring of Triiodide

Abstract

A highly selective and sensitive triiodide sensor based on a 2‐(((2‐(((E)‐1‐(2‐hydroxy phenyl) methylidine) amino) phenyl) imino) methyl) phenol with iodine (CTC) as membrane carrier was developed. The electrode revealed a Nernstian behavior over a very wide triiodide‐ion concentration range (5.0×10^?8–1.0×10^?2 M), and relatively low detection limit (3.0×10^?8 M). The potentiometric response is independent of the pH of solution in the pH range of 3.0–10.0. The electrodes manifest advantages of low resistance, very fast response (<12 s), and most importantly, good selectivities relative to a wide variety of inorganic and organic anions, including iodide, bromide, chloride, fluoride, sulfite, sulfate, cyanide, thiocyanate, and acetate. In fact, the selectivity behavior of the proposed triiodide ion‐selective electrode shows great improvements compared to the previously reported electrodes for the triiodide ion. The proposed membrane sensor can be used for at least 6 months without any significant divergences in the potential. The electrode was successfully applied as an indicator electrode in the titration of triiodide with thiosulfate ion.     

Analysis of Impurities in Commercial Fluorene by Synchronous Nonprotected Room-Temperature Phosphorescence

Abstract

The applicability of nonprotected room-temperature phosphorescence (NP-RTP) in real samples is demonstrated in this work. In this methodology only two reagents, potassium iodide and sodium sulfite, were used to obtain the phosphorescent signals. Synchronous phosphorimetry was used to enhance sensitivity. Analyses of dibenzofuran, acenaphthene, and fluorene were carried out in a sample of impure fluorene.     

Indirect amplification method for determining mercury by direct-current polarography. Application to organomercury compounds

An amplification method for the determination of 0.5–70 ppm (2.5 × 10⁻⁶ to 3.5 × 10⁻⁴ M) of Hg(II) is described. Hg(II) is reacted with a slight excess of KI, and the excess iodide is oxidized by bromine water and measured polarographically as iodate with sixfold amplification. Alternatively, the iodate formed is reacted to liberate iodine which is then reduced to iodide, and again oxidized to yield six iodate ions for every iodide ion originally present;

2. Microdetermination of Mercury in Organomercurial Compounds

polarographic reduction requires 36 electrons. Oxidation of the excess iodide with periodate yields four iodate ions for every iodide ion and therefore allows 24-fold amplification.Microdetermination of mercury in organomercurials is achieved using the sixfold method following closed flask combustion: the average percentage error for 10 determinations is ±0.40 and the time required for one sample run is 45 min.     

Photometric titration of total iodine at trace levels in concetrated chloride solutions

The method is based on reduction of total iodine (10^?7?10^?5 M), to iodide with sulphite in acidic solution. The excess of sulphur dioxide is removed by bubbling with nitrogen, and the resulting solution is titrated spectrophotometrically with a standard solution of iodate, the absorbance being measured at 230 nm. Some Italian table salts, iodized or common, were analyzed for their iodide and total iodine content.     

Determination of ultratrace iodide in aqueous solution with a piezoelectric detector

Iodide is oxidized to iodate and, after destruction of excess oxidant, iodine is formed on addition of excess of iodide. This is extracted into toluene and detected by adsorption on the silver-plated electrode of the piezoelectric crystal. The resulting frequency change of the dry crystal after removal from the toluene is proportional to iodide concentration over the range 0.6–127 μg l^?1. No significant interferences were caused by other ions except bromide. The mechanism of iodine adsorption is investigated by cyclic voltammetry.     

Titrimetric determination of microgram amounts of lead by thiocyanate amplification after precipitation as lead hexathiocyanatochromate(III)

Lead (25–200 μg) is precipitated as Pb₃[Cr(SCN)₆]₂. The filtered precipitate is treated with 10% carbonate solution, and the thiocyanate dissolved is oxidized by iodine to sulphate at pH 8.2. After acidification, the excess of iodine is extracted into chloroform, and the iodide ion retained in the aqueous solution is amplified by bromine oxidation and subsequent treatment with more iodide. The method provides 152 iodine atoms for each original lead ion. Only Bi³⁺ and Cu²⁺ interfere seriously.     

Solvent-specific reduction of Na<Subscript>2</Subscript>PtI<Subscript>6</Subscript> in acetone

Oxidation state of iodide complexes of Pt^II and Pt^IV in large excess of NaI with respect to platinum in water and acetone solution has been determined by means of ¹⁹⁵Pt NMR spectroscopy. In acetone, iodide complexes of Pt^IV are almost quantitatively reduced into Pt^II, and iodine is bound in a poorly soluble polymeric complex with sodium iodide and acetone. Iodometric titration has revealed the formation of equivalent amount of iodine. Reduction of platinum has not been observed in aqueous medium.     

Spectrophotometry -Kinetic Determination of Thioketones

Abstract

A spectrophotometric-kinetic method is proposed for the assay of thioketones. The method is based on the catalysis of the sodium azide-iodine-starch reaction by thiourea at concentrations from 10 to 100 ppb. The course of the reaction is monitored spectrophotometrically by the reduction of iodine to iodide using starch iodine indicator.     

Spectrophotometric determination of <Emphasis Type="Italic">L</Emphasis>-ascorbic acid in pharmaceuticals

A simple and sensitive spectrophotometric method for the determination of L-ascorbic acid with leuco crystal violet is proposed. The determination is based on the oxidation of analyte by potassium iodate. The colourless oxidation products were formed in the quantity equivalent to iodide ions. The iodide ions react with the excess of iodate ions in acidic medium, to form free iodine which oxidized leuco crystal violet (LCV) to the liberated crystal violet (CV ⁺) dye, showing maximum absorption at 588 nm. The absorbance was measured at pH of 4.1–4.2 in 1 cm cuvettes. Beer’s law was obeyed in the concentration range 0.5–4.0 μg/mL. The molar absorptivity of the coloured compound is 4.14 × 10⁴ L/mol cm for L-ascorbic acid. The analytical parameters were optimized and the method was successfully applied to the determination of L-ascorbic acid in pharmaceuticals. The results were compared with those obtained by methods proposed in Polish Standard.