Automated Sequential‐injection Chemiluminescence Determination of Glucosamine Sulphate via Luminol‐Hydrogen Peroxide System

A highly sensitive automated sequential‐injection chemiluminescence (SIA‐CL) method for determination of glucosamine sulphate (GLS) was developed. The goal of the present work is the evaluation of the enhancement effect of the investigated drug glucosamine sulphate on the chemiluminescence reaction between luminol and H₂O₂ in alkaline medium of 1.0 × 10^?2 mol L^?1 sodium hydroxide at pH 11. The experimental conditions affecting the CL reaction such as the sequence of the reagents, concentrations, flow rate and aspirated volumes of reactants were systematically investigated and optimized. Under optimum conditions 50 μL of 1.0 × 10^?3 mol L^?1 luminol, 30 μL of a GLS test solution and 50 μL of 1.0 × 10^?2 mol L^?1 H₂O₂ were used and the luminescing zone was pushed into the detector at a flow rate 100 μL s^?1. The proposed method recorded high sensitivity, accuracy and simplicity that could be clarified as linear concentration range 1.0‐2000 ng mL^?1 with rectilinear part (r = 0.9992, n = 9) and limit of detection 0.3 ng mL^?1, along with relative standard deviation 1.3%. It was found that the developed method can be used directly to determine the investigated drug GLS in its pharmaceutical dosage forms and in spiked serum and urine by diluting the samples for a 1000 fold. The obtained results were statistically analyzed and compared with those obtained by the reported method.     

Ionic strength effect on the liquid–liquid extraction of zinc(II) and cadmium(II) from sulphate medium by 1-phenyl-3-methyl-4-benzoylpyrazol-5-one in chloroform

The liquid–liquid extraction of zinc(II) and cadmium(II) from sulphate medium by 1-phenyl-3-methyl-4-benzoylpyrazol-5-one (HPMBP) in chloroform is studied. The ionic strength effect of the aqueous phase shows that the extraction of the metal increases with decreasing concentration of sulphate. At initially of about 10^?4?M with three different sulphate concentrations 0.033, 0.16 and 0.33?M in the aqueous phase, Zn(II) and Cd(II) are extracted as the complexes Zn(PMBP)₂ and Cd(PMBP)₂. Sulphate complexes of Zn(II) and Cd(II) are formed in the aqueous phase. The metal–sulphate interaction has been made in evidence by using the Debye–Huckel extended limiting law of ionic activity coefficient.     

A Field Effect Transistor Sensitive to the Phenobarbical Anion

Abstract

A field effect transistor sensitive to the phenobarbital anion is described. The response is Nernstian between 10^?1 mol 1^?1 and 10^?4 mol 1^?1 in the absence of added hydroxide, and 10^?1 mol 1^?1 to 10^?3 mol 1^?1 in the presence of added hydroxide. Selectivities over sulphate, chloride, nitrate, hydrogen phosphate have been determined and speed of response and stability are greater than the corresponding coated wire electrode.     

Determination of trace levels of sulphate in water using flow-injection and in-line preconcentration

Sulphate is preconcentrated on a strong anion-exchange resin and determined using the effect of sulphate ions on the complexation of methylthymol blue and barium. A computer-controlled flow-injection analyser is used to automate the whole procedure. The resin has two functions: it preconcentrates sulphate and also separates sulphate from divalent cations that may interfere in the determination step. The system can handle 30 samples per hour and has a working range from 25 to 1000 μg 1^?1 of sulphate. Lower detection limits can be obtained by changing the preconcentration conditions. The effect of both anionic and cationic interferents was studied.     

Screening of chemiluminescent systems for the determination of some biologically important organic compounds

Screening tests are described for the development of chemiluminescence systems (oxidizing systems) capable of detecting biological organic compounds. The light emission depends strongly on the oxidizing systems employed. Acidic permanganate system gives rise to light emission for many compounds, including catechols, catecholamines, triphenols and indoles. The following oxidizing systems led specifically to chemiluminescence for hydroquinone, adrenaline or phenylpyruvic acid: 10^?1 M thiosulphate with 10^?1 M sodium hydroxide and 10^?4 M Ag (I), 0.3 % hydrogen peroxide with 10^?3 M sodium hydroxide/50% acetonitrile and 10^?4 M Fe (II), and 0.3% hydrogen peroxide with 10^?2 M sodium hydroxide/10^?2 M didodecyldimethylammonium bromide and 10^?4 M Co(II), respectively.     

Improvements to CO<Subscript>2</Subscript> headspace biodegradability test

This study proposes changes to the design and evaluation of the CO₂ headspace test, which is used as a simple method for assessment of the complete biodegradability of surfactants. It presents a modified equation for the calculation of biodegradation. It is proposed that the solution of 7 mol L^?1 sodium hydroxide commonly used in the process involving alkalinisation of the vial contents be replaced with 15 mol L^?1 sodium hydroxide. The use of the higher hydroxide concentration leads to a significant reduction in the value of the blank CO₂ headspace test.     

Speciation of butyltins in fish and sediment by means of gas chromatography with flame photometric detection

A modified method for the determination of tributyl-, dibutyl-, and monobutyl-tin in fish and sediment samples is proposed. The samples are digested with hydrochloric acid and the butyltin compounds are extracted into a tropolone solution in pentane and pentylated by a Grignard reaction. The products are cleaned up by washing with a sodium hyrdoxide solution, dried over sodium sulphate, concentrated by evaporation and analysed by gas chromatography with flame photometric detection, using an interence filter at 610 nm. Problems peculiar to the fish and sediment samples are overcome by this improved clean-up procedure. The limit of detection for tributyltin in fish is 0.04 m?g g^?1 and the reproducibility at 0.06 μg g^?1, expressed as the relative standard deviation, is 6.8%. Contaminated sediment samples were found to contain the mixed methylbutyl-tin compounds Me₂BuSn⁺ and MeBu₂Sn⁺.     

Single-column ion chromatography of weak inorganic acids for materials and process characterization

Single-column ion chromatography allows the separation and direct conductometric detection of anions of weak inorganic acids. Mixtures containing borate, silicate, germanate, fluoride and chloride can be resolved by using a resin-based anion-exchange column and a 0.06 g l^?1 sodium hydroxide/2.5 × 10^?5 M sodium benzoate eluent. Judicious selection of sample preparation and of eluent composition is important. Glasses are analyzed for boron and fluoride by fusion with sodium hydroxide, suitable dilution and use of a benzoate eluent. Results on standard glasses are in good agreement with certified values. The separation of arsenite and arsenate in a gold plating bath is outlined.     

The determination of sulphate in natural waters by inductively-coupled plasma emission spectrometry

Sulphate is determined simultaneously with other constituents by using inductively-coupled plasma emission spectrometry; the intensity of the 180.73-nm sulphur line is monitored. At a forward power of 1100 W, under compromise conditions, a 3 s detection limit of 0.08 mg l^-1 sulphate and a precision of 0.8% RSD at the 200 mg l^-1 sulphate level were obtained. A small spectral interference from calcium is overcome by software corrections, and good agreement is demonstrated between the proposed method and spectrophotometric sulphate measurements for a variety of natural waters including seawater.     

Study on the Color Reaction of Silver with 2‐(2‐Quinolylazo)‐5‐Dimethylaminoaniline and its Application

A new chromogenic reagent, 2‐(2‐quinolylazo)‐5‐dimethylaminoaniline (QADMAA) was synthesized. A highly sensitive, selective and rapid method for the determination of silver based on the rapid reaction of silver(I) with QADMAA was developed. In the presence of pH = 6.5 sodium citrate‐sodium hydroxide buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with silver to form a violet complex of a molar ratio 1:2 (silver to QADMAA). The molar absorptivity of the complex is 1.26 × 10⁵ L. mol^?1.cm^?1 at 570 nm. Beer's law is obeyed in the range of 0.01–0.6 μg/mL. The relative standard deviation for eleven replicate samples of 0.2 μg/mL silver is 1.76%. This method was applied to the determination of silver in water with good results.     

Extraction And Spectrophotometric Determination Of Cadmium Based On The Formation Of A Ternary Complex With Cadion And 1, 10-Phenanthroline

Abstract

Cadmium ion reacts with cadion and 1, 10-phenanthroline to form a 1:1:2 orange-red ternary complex in 0.5N sodium hydroxide medium. The complex is extracted by chloroform and has a molar absorptivity of 9.2 × 10⁴ l. mole^?1. cm^?1 at 490 nm. A method is developed for the determination of cadmium in electroplating waste water.     

Liquid–liquid microextraction and spectrophotometric determination of anionic surfactants using Astra Phloxine FF

A novel and simple procedure for determination of anionic surfactants has been developed. The method is based on the reaction of sodium dodecyl sulphate (SDS) with Astra Phloxine FF reagent at pH 3–8, followed by liquid–liquid microextraction of the formed ion associate into an organic phase containing a mixture of carbon tetrachloride and dichloroethane (4:1, v/v) and subsequent UV-Vis detection at 555 nm. The calibration plot was linear in the range 0.006–0.29 mg L^?1 of SDS. The limit of detection (LOD), calculated based on 3s, is 0.002 mg L^?1. The method was applied to the determination of anionic surfactants in real wastewater samples.     

Kinetics and mechanism of base-catalyzed cleavage of some bicyclo[4.2.0.]octa-1,3,5-trien-7-one (benzocyclobuten-1(2H)-one) derivatives

The kinetics of cleavage of 3-hydroxybicyclo[4.2.0]octa-1,3,5-trien-7-ones in aqueous sodium hydroxide, and of the alkoxy and acetoxy analogues in methanolic sodium methoxide solution, were examined under pseudo-first-order reaction conditions. The dependence of the rate upon the basicity of the solvent, whether measured by H_? or by [OR^?], reflects the possible structure of the transition state. The deduced mechanism is also supported by the effects of substituents upon the reaction rate. The relative amounts of the volatile reaction products derived from o-toluic acid and from phenylacetic acid are understood in terms of the substituent effect upon the relative stabilities of the carbanions.     

An improved method for the spectrophotometric determination of fluoride by addition of sodium dodecyl sulphate to the fluoride/lanthanum (III)/Alizarin fluorine blue system

The conventional spectrophotometric method for the determination of fluoride, based on the fluoride/lanthanum(III)/alizarin fluorine blue ternary complex, is improved by addition of sodium dodecyl sulphate. In 15% (v/v) acetone medium, the absorbance of the binary reagent complex is decreased and the reaction time is only 3 min under sonication. Beer's Law is obeyed at 574 nm for fluoride concentrations in the ranges 0.075–0.30 and 0.20–1.2 mg 1^?1; the apparent molar absorptivities are (1.6 ± 0.1) × 10⁴ and (1.5 ± 0.1) × 10⁴ mol^?1 cm^?1 fluoride levels, respectively. This method is applied to the determination of fluoride in bottled mineral waters.     

Production and characterization of surfactant-stable fungal keratinase from <Emphasis Type="Italic">Gibberella intermedia</Emphasis> CA3-1 with application potential in detergent industry

Surfactant-stable keratinases with good properties are promising candidates for extensive applications in detergent industries. A novel fungal keratinase-producing strain, Gibberella intermedia CA3-1, is described in this study. The keratinase production medium was optimized and composed of 10 g L^?1 of wool powder, 5 g L^?1 of tryptone, 10 g L^?1 of maltodextrin and 0.5 g L^?1 of NaCl. Keratinase activity was increased up to 109 U mL^?1 from 15 U mL^?1 by culture optimization. The optimal reaction pH and temperature of the enzyme were 9.0 and 60°C, respectively. The keratinase activity could be improved by sodium dodecyl sulphate (SDS), and it remained stable in the presence of several surfactants and commercial detergents. G. intermedia keratinase was proved to completely remove blood stains from cotton cloth when combined with detergents. These findings indicate that this fungal keratinase is a promising catalyst for the application in detergent industry. To our knowledge, this is the first report on keratinase production by Gibberella genus.     

Über basische Aluminiumsalze und ihre Lösungen. XVI. Kinetische Untersuchungen an niederbasischen Aluminiumchloridlösungen

Basic Aluminum Salts and their Solutions. XVI. Kinetic Studies on Low Basic Aluminum Chloride Solutions Basic aluminum chloride solutions of low basicity were prepared by different methods and investigated by means of the ferrone kinetics. In solutions prepared by expulsion of hydrogen chloride or addition of solid sodium carbonate preferably dimeric cations are formed. In solutions prepared by addition of sodium hydroxide solution or sodium carbonate solution only at very low basicity small quantities of dimeric ions are formed, at increasing basicity tridecameric ions arise. An explanation of this behaviour is given, involving the action of hydroxide ions and a possible formation of the dihydroxy-aluminum complex. The rate constant for the reaction of the dimeric ions with the ferrone reagent was determined to be k = 0.97 ± 0.06 min^?1.     

The solubility of uranium(IV) hydrous oxide in sodium hydroxide solutions under reducing conditions

The solubility of hydrous UO₂ in sodium hydroxide solutions containing sodium dithionite and/or Zn metal powder as reductants has been measured. The results provide no firm evidence for any amphoteric behavior of U(IV) but do set an upper limit of K ≤ 2 x 10^?23 for the hypothetical reaction:

The results provide no evidence for such a reaction.     

Sorption Catalytic Determination of Copper(II) and L-α-alanine on Mg-, Al-Layered Double Hydroxides

Mg-, Al and Mg-, Cu-, Al-layered double hydroxides well-known synthetic hydrotalcite-like sorbents, were used for the first time as carriers for indicators in the sorption catalytic determination of copper(II) and L-α-alanine. Mg-, Al and Mg-, Cu-, Al-layered double hydroxides were synthesized by coprecipitation and characterized using infrared spectroscopy, X-ray diffraction, and scanning electron microscopy. The adsorption of 0.50?mg?L^?1 copper(II) solution by Mg-, Al-layered double hydroxides followed a pseudo-second-order model with an equilibrium sorption capacity of 24.2?×?10^?3?mg?g^?1 (3.8?×?10^?4?mmol g^?1) and a reaction rate constant of 4.2?g mg^?1?min^?1. Mg-, Al-layered double hydroxide tablets were prepared and used for sorption concentration and subsequent sensitive and selective sorption catalytic determination of 5.5?×?10^?3 to 1.0?mg?L^?1 copper(II) at the sorbent phase. The method was used for the analysis of natural water. A method was developed for the determination of α-alanine in Mg-, Cu-, Al-layered double hydroxide tablets with a limit of detection of 4.0?×?10^?3 mol?L^?1. In addition, thin layers of Mg-, Cu-, Al-layered double hydroxide were used to separate α-alanine and determine α-amino acids by thin-layer chromatography.     

Spektrochemische bestimmung von sulfat bzw. Chlorid mit roentgenfluoreszenz nach anreicherung durch mitfällung an BaCrO4 BZW. AgSCN aus verdünnten lösungen

Sulphate and chloride are quantitatively co-precipitated from dilute solutions (10^?5- 10^?4M) with BaCrO₄ and AgSCN respectively, and determined in the precipitate by X-ray fluorescence spectroscopy. Ratios of count-rates I_S/I_Cr and I_Cl/I_Sfor the appropriate K_α-lines are used for quantitative evaluation by comparison with reference standards prepared the same way. The method enables both sulphate and chloride to be determined in 50–100 ml of tap-water with a reproducibility of about 3%.     

Spectrophotometric Determination of 8-Hydroxyquinoline (Oxine) in Aqueous Solution by Azo Dye Formation with Diazotized p-Aminoacetophenone

Abstract

A sensitive spectrophotometric method for the determination of oxine in aqueous solution is investigated. It is based on the reaction of the analyte with diazotized p-aminoacetophenone to form, in the presence of sodium hydroxide, an intense cherry-red water-soluble and stable azo dye which shows maximum absorption at 520 nm. The linear absorbance plot with the concentration indicates that Beer's law is adhered over the range 10–100μg of oxine in a final volume of 25 ml, i.e., 0.4–4 ppm, with a molar absorptivity of 3.37 × 10⁴ 1mol^?1 cm^?1, a relative error of +0.44 to –1.12%, and a relative standard deviation of 0.54–2.9%, depending on the level of analyte concentration. The optimum conditions affecting the color reaction and interference due to foreign organic compounds have been examined.