Analytical control of silica glass production. Voltammetric determination of titanium and iron in raw materials and silica glass samples

Adsorptive stripping voltammetric (AdSV) methods are presented for the determination of titanium and iron in quartz and silica glass samples obtained after pressure decomposition. Mandelic acid and catechol were used as complexing agents for titanium and iron, respectively. The method for titanium determination is based on the catalytic effect of chlorate ions. An insoluble residue remaining after decomposition of quartz and silica glass samples in HF+H2SO4 mixture was checked by energy-dispersive X-ray analyses. ET-AAS was applied as a reference method to AdSV measurements.     

Stepwise complexometric determination of aluminium, titanium and iron concentrations in silica sand and allied materials

Background  

This study aimed at measuring the quantities of Al, Ti and Fe in silica sand and allied materials employing a complexometric method in the same analyte and a stepwise indirect titration with EDTA. The method involves the complexation of Al, Ti and Fe with excess EDTA and the selective de-complexation of TiO-EDTA and Al-EDTA complexes with tartaric acid and NaF respectively. In addition to its simplicity, rapidity and accuracy, the proposed method does not require the use of a separation technique or any sophisticated instrumentation.     

分光光度法同时测定硅石中的铁和铝

在邻二氮菲(Phen)、铬天青S(CAS)和十四烷基二甲基苄基氯化铵(TDMBA)的共同存在下,于pH 5～6的酸性介质中,铁、铝分别生成Fe-Phen和Al-CAS-TDMBA络合物,用同一份试液,在波长510 nm测定铁,在625 nm测定铝,两种络合物互不干扰。用该法可同时测定硅石中的铁和铝。     

Voltammetric determination of iron(II) and iron(III) in standard rocks and other materials

Voltammetry at a rotating platinum electrode in concentrated electrolyte solutions containing HCl and LiCl is described for simultaneous determinations of iron(II) and iron(III) in a variety of materials. Applications of the method to some U.S. Geological Survey standard rocks, a Georgian clay, and an iron-containing multiple vitamin tablet are described. For materials which can be dissolved without altering the original iron(II)/ iron(III) ratio, this method enables the two valence states to be determined rapidly and simultaneously. The technique is precise (r.s.d. ≈ 2%) and relatively free from interference, and requires only a recording d.c. polarograph.     

Voltammetric determination of arsenic in high iron and manganese groundwaters

Determination of the speciation of arsenic in groundwaters, using cathodic stripping voltammetry (CSV), is severely hampered by high levels of iron and manganese. Experiments showed that the interference is eliminated by addition of EDTA, making it possible to determine the arsenic speciation on-site by CSV. This work presents the CSV method to determine As(III) in high-iron or -manganese groundwaters in the field with only minor sample treatment. The method was field-tested in West-Bengal (India) on a series of groundwater samples. Total arsenic was subsequently determined after acidification to pH 1 by anodic stripping voltammetry (ASV). Comparative measurements by ICP-MS as reference method for total As, and by HPLC for its speciation, were used to corroborate the field data in stored samples. Most of the arsenic (78 ± 0.02%) was found to occur as inorganic As(III) in the freshly collected waters, in accordance with previous studies. The data shows that the modified on-site CSV method for As(III) is a good measure of water contamination with As. The EDTA was also found to be effective in stabilising the arsenic speciation for longterm sample storage at room temperature. Without sample preservation, in water exposed to air and sunlight, the As(III) was found to become oxidised to As(V), and Fe(II) oxidised to Fe(III), removing the As(V) by adsorption on precipitating Fe(III)-hydroxides within a few hours.     

Properties and production of F-doped silica glass

Fluorine-doped silica glass is an optical material with high transmission in the vacuum ultraviolet region, specifically at 157 nm. This feature, along with low thermal expansion and ease of polishing make it the material of choice for the photomask substrate for the 157 nm lithography node. We report the synthesis of fluorine-doped silica glass using various dopants. Characterization of the glasses was achieved by measuring vacuum UV and IR spectra and by refractive index measurements. Transmission and refractive index are both found to depend on fluorine concentration.     

Voltammetric determination of copper in water samples digested by ozone

The applicability of ozone as a digestion agent in voltammetric trace metal analysis of water samples was investigated. It was shown that ozone efficiently destroys dissolved organic matter, causing a significant decrease of the concentration of surface active substances in the sample, thus enabling voltammetric measurements. Ozonolysis times of 30 and 60 min were sufficient for the treatment of river water and biologically treated wastewater samples, depending on their organic load, prior to voltammetric determination of copper using a solid gold electrode.     

Colorimetric determination of iron in titanium alloys

There is need for an improved method for the determination of iron in titanium alloys. In this paper a colorimetric method using o-phenanthroline is proposed. The method is applicable to the range of 0.02 to 9 per cent. iron. Two modifications of a basic procedure are described. One modification, applicable to ordinary titanium alloys, is a direct method. A second modification, applicable to alloys containing large amounts of certain alloying elements, calls for a prior separation of the iron by an ether extraction. In a direct method a one gram sample is dissolved in hydrochloric acid and an aliquot of the solution taken. Hydroxylamine and ammonium tartrate are added, the pH of the solution is adjusted by the addition of sodium acetate, and o-phenanthroline added. A study was made to find the best pH and optimum amount of o-phenanthroline for the development of the color.     

2. The raw materials of CA 2.1 Wood as natural raw materials for cellulose acetate production

The molecular arrangement of wood cell wall is described in relation to the physical and mechanical properties of wood. The chemical composition of wood is also summarized to illustrate the heterogeneity in distribution of cell wall constituents to use wood plup fibers judiciously as natural raw materials for cellulose acetate production.     

Hazard in reaction of titanium raw materials with sulphuric acid

The reaction of ilmenite titanium raw material with sulphuric acid was investigated in ‘hazard’ type calorimetric system. The investigations show the essential influence of initial temperature, particle size distribution and concentration of sulphuric acid on rate and heat power of reaction and determine the limits of safety of the process and also its efficiency.     

Synthesis of rutile titanium dioxide from Russian raw materials

The conditions of the structure formation of rutile titanium dioxide from titanium dioxide (anatase) and titanium hydroxide isolated by thermolysis from the titanium compound (NH₄)₂TiO(SO₄)₂ · H₂O and by thermal hydrolysis of a titanium sulfate(IV) solution, respectively, were studied. It was shown that the mechanical activation of the studied powders causes, in addition to a decrease in the initial grain size, deep destructuring with the formation of the transition phase, which, in the process of the subsequent high-temperature treatment, functions as a matrix for the formation of rutile. The research results will be used for the development of a new variant of the technology for the synthesis of titanium dioxide, which is an important component of compositions for polymeric materials—in particular, the K-300-61 and K-153 adhesives.     

Voltammetric determination of pentachlorophenol with a silica gel-modified carbon paste electrode

Summary The anodic voltammetric behaviour of pentachlorophenol at a silica gel-modified carbon paste electrode in aqueous solution is reported. Adsorption of the fungicide onto the electrode under open-circuit conditions is followed by application of either differential or square wave voltammetry. The results obtained by differential pulse voltammetry at pH 2.9, with a modifier concentration of 10% and accumulation times of 120 and 300 s, allowed the development of a method to determine pentachlorophenol in the ranges of 1.0×10⁻⁶–1.0×10⁻⁵ and 1.0×10⁻⁷–1.0×10⁻⁶ mol l⁻¹. The relative standard deviation is 2.6% for a concentration of 2.0×10⁻⁷ mol l⁻¹, with a detection limit of 1.8×10⁻⁸ mol l⁻¹ (5 ppb). The effect of other chlorophenols was studied. The results obtained by square wave voltammetry showed a behaviour typical of an irreversible electron transfer. Amplitude, step height and frequency were optimised, taking into account the resolution of the voltammetric response. No improvement in sensitivity was obtained with respect to DPV. Good results were obtained by applying the proposed differential-pulse voltammetric method to the determination of pentachlorophenol in a commercial fungicide.     

Catalytic flow-injection determination of reactive iron in non-acidified water samples.

A flow-injection determination method was proposed for the speciation of reactive species of iron in non-acidified water samples. Iron was determined by the spectrophotometric monitoring of the iron-catalyzed oxidation of o-phenylenediamine with hydrogen peroxide. The reactive iron was characterized as Fe3+ and Fe(III)Li(3-in), where i = 1 or 2 for a unidentate ligand and i = 1 for a bidentate ligand (L(n-)) from the chemical equilibria of hydroxo, oxalato and fluoro Fe(III) complexes. A useful parameter was also proposed to check the reliability of the determination when suffering the adsorption of iron on the inner wall of a PTFE tube of a flow-injection system. Under the optimized FIA condition and by measuring the peak height, a linear calibration curve of iron was obtained up to 0.1 mg L(-1) with a detection limit of 0.1 microg L(-1). The proposed method was successfully applied to the speciation of reactive and unreactive iron in tap- and river-water samples.     

Analytical determination of mercury in medicinal and waste water samples

Tris(2-ethylhexyl)phosphate (TEHP) is proposed as an extractant for mercury salicylate. Optimum extraction conditons are developed and the method is used for determinations of mercury in medicinal and waste water samples.     

Peculiarities of foam glass synthesis from natural silica-containing raw materials

Journal of Thermal Analysis and Calorimetry - The primary source of the power for marine industry comes from large two-stroke low-speed marine diesel engines. The more severe emission regulations...     

Characterisation of raw materials for production of ceramics

The aim of this paper is to characterize some raw materials used for ceramics material production. Five samples of clay have been analyzed. It has been carried out a patterned sampling in a quarry in Rosarno (South Italy). Chemical-physical properties on clay samples are determined. Test pieces have been prepared and physical properties after firing are determined by DSC thermal analysis, XRD analysis and X-ray fluorescence. It is important to note the high amount of Fe₂O₃. The mixture principally contains quartz, illite and oligoclase. It has been observed the colour and the shape after firing: predominant colour is red. In this case the clay has been used in mixtures covered with glazes. The colour of internal clay is hidden by opaque of glazes. The analysed raw materials can be used in a slip for single fired red tiles. The A2sp clay produces best ceramics at 1000°C.     

Sequential determination of iron and titanium by flow-injection analysis

A flow-injection method has been developed for the sequential spectrophotometric determination of iron and titanium using 3,4 dihydroxybenzoic acid as chromogenic reagent. The system involves the sequential measurement of the absorbances of the complexes at 380 and 570 nm. The system is designed using a simultaneous injection of sample and reagent into separate carrier streams. The proposed method is characterized by a precision of about 2%, a sampling rate of about 50 samples per hour, and a reagent consumption of 200 mul (0.50% solution) per sample. It is relatively free of interferences and was used for the sequential determination of titanium and iron in rocks.     

Voltammetric determination of mesalazine in pharmaceutical preparations and biological samples using boron-doped diamond electrode

Voltammetric method for the determination of non-steroidal anti-inflammatory drug mesalazine (5-ASA) is presented for the first time using boron-doped diamond electrode (BDDE). 5-ASA provides one well-developed SWV oxidation peak at about ?900 mV (vs. saturated silver/silver chloride reference electrode) on BDDE. Britton-Robinson buffer (pH 7.0) was chosen as an optimal supporting electrolyte for the determination of 5-ASA using square wave voltammetry (SWV). Parameters of SWV were developed and low limit of detection (7.0 × 10^?7 mol L^?1) was reached. In addition, relative standard deviation of repeated measurements (c _5-ASA = 5 × 10^?5 mol L^?1, RSD_M = 2.7%) and relative standard deviation of repeated determinations (RSD_D < 1.5%) were calculated and confirm obtained good results. Applicability of the proposed method was verified by an analysis of a pharmaceutical preparation and spiked human urine.