An automated method for the determination of low-level kjeldahl nitrogen in water and waste water

An entirely automated system for low level Kjeldahl nitrogen determination in water samples is described. Samples are continuously digested at 300 °C with sulfuric acid and hydrogen peroxide to convert the organic nitrogen to ammonia, which is determined colorimetrically with sodium salicylate and sodium dichloroisocyanurate (as chlorine source). The method has a range of 10–500 μg Nl^-1 with good precision and accuracy.     

Use of Potentiometry with Imposed Current for the Determination of Chlorine in Breakpoint Chlorination

Abstract

An investigation of the use of potentiometric titrations with imposed current, in order to identify break-point curves, has been carried out. The influence of temperature and/or conctact times has been evaluated. In ammonia chlorine mixtures determination of ammonia have been performed before and after addition of sulfite, as dechlorination agent, and results have been compared with potentiometric titrations of combined chlorine.     

Interaction of 7-Chloro-9-methylthio-3-phenylpyrimido[5,4-f][1,2,4]triazolo[3,4-b][1,3,4]thiadiazepine with Some Nucleophiles

The reactions of 7-chloro-9-methylthio-3-phenylpyrimido[5,4-f][1,2,4]triazolo[3,4-b][1,3,4]thiadiazepine (1) with some nucleophiles have been studied. Substitution of the chlorine atom with hydrogen occurs with ammonia in DMSO to give 9-methylthio-3-phenylpyrimido[5,4-f][1,2,4]triazolo[3,4-b][1,3,4]thiadiazepin-7(8H)-one. With a methanolic solution of ammonia the 7-methoxy derivative is formed. Reaction of compound 1 with an excess of sodium methoxide in methanol gave 6,7-dimethoxy-9-methylthio-3-phenyl-5,6-dihydropyrimido[5,4-f][1,2,4]triazolo[3,4-b][1,3,4]thiadiazepine. The corresponding 7-substituted derivatives were obtained when compound 1 was heated with morpholine or 2-(dimethylamino)ethylamine. The azomethine bond of the thiadiazepine ring is reduced by sodium borohydride to give the corresponding 5,6-dihydro derivatives.     

Simultaneous Determination of Sodium,Potassium, and Ammonium Ions by Automated Direct Potentiometry

Abstract

Sodium, potassium and ammonium ions, in concentration ranges of natural and waste water samples, have been simultaneously determined by direct potentiometry, using sodium, potassium, and ammonia ion-sensitive electrodes. The results are printed out as concentration units directly from an automated continuous -flow system with on-line minicomputer and printer. The optimum sampling rate is 20 samples or 60 determinations per hour. Various water samples have been analyzed and the results compared to those obtained by the standard methods. The lower detection limits were 0.1 ppm for Na⁺ and NH₄ ⁺ and 1.0 ppm for K⁺. The values of standard deviation were < 10%, with the exception of the lowest concentrations. The relative error was in the range of ± 2%. The correlation of standard and proposed methods was very good.     

Determination of phenols in waters using micro-pumped multicommutation and spectrophotometric detection: an automated alternative to the standard procedure

An automated and greener spectrophotometric procedure has been developed for the determination of phenol in water at 700 nm. The method uses the reaction between phenol, sodium nitroprusside, and hydroxylamine hydrochloride in a buffered medium at pH 12.3. The flow manifold comprises four solenoid micro-pumps employed for sample and reagent introduction into the reaction coil and to transport the colored product formed to the detector. The linear dynamic range was 50–3,500 ng mL⁻¹ (R = 0.99997; n = 6) and the method provided a limit of detection (3σ) of 13 ng mL⁻¹. The sampling throughput was estimated to be 65 measurements per hour and the coefficient of variation was 0.5% (n = 10) for a 1.0 μg mL⁻¹ phenol concentration. Recoveries of 92–105% were obtained for phenol determination in spiked water samples at concentration levels from 50 to 5,000 ng mL⁻¹. The use of multicommutation reduced the reagent consumption 25-fold, the sample consumption 225-fold, and the waste generation 30-fold compared with the batch procedure. The proposed method is an environmentally friendly alternative to the official 4-aminoantipyrine method since it avoids the use of chloroform.     

Automated Determination of Arsenic,Selenium, Antimony,Bismuth and Tin by Atomic Absorption Utilizing Sodium Borohydride Reduction

Abstract

An automated system for the determination of arsenic, selenium, antimony, bismuth and tin is described. These elements and their compounds are reduced with sodium borohydride to the corresponding hydride. Sensitivity of the automated system is comparable and in most cases better than the manual technique. The automated method was found superior to the manual with respect to reproducibility and ease of operation.     

The spectrophotometric determination of ammonia in natural waters with particular reference to sea-water

The conditions for the precise spectrophotometric determination of microgram amounts of ammonia by means of the sodium phenate-hypochlorite method of RUSSELL have been investigated. Several modifications of her procedure have been introduced, particularly in the time and temperature used for development of the blue colour. BEER'S Law is obeyed up to a concentration of 2 mg NH₄-N/1 and ammonia can be determined with a standard deviation of 0.7%. The method can be used for the determination of up to at least 6 mg NH₄-N/l if recourse is made to a calibration curve. The interference of a number of inorganic ions has been studied, none of those which occur in natural fresh waters causes any marked diminution of the colour. The method can, therefore, be employed directly for the determination of ammonia in fresh waters. The most serious interferences are produced by copper and hydroxylamine. Hydrazine, however, does not interfere with the determination of ammonia unless it is present to the extent of at least 500 times the weight of the ammonia.The phenate-hypochlorite method cannot be used for the direct estimation of ammonia in sea-water owing to the interference of magnesium and calcium ions. The ammonia is therefore separated from the sea-water by a preliminary distillation under reduced pressure in a slow current of air as suggested by KROGH. A metaborate buffer has been employed for the liberation of the ammonia, and the optimum conditions of alkalinity for its separation determined. If two distillation apparatus are used concurrently 40–50 samples of sea-water may be examined per day with a standard deviation of less than 1 mg NH₄-N/m³Amino acids and urea do not interfere in either the sodium phenate-hypochlorite procedure or the distillation.     

Trace-Level Determination of Phenol by Liquid Chromatography with On-Line Precolumn Technology and Fluorescence Detection

Abstract

A strongly basic anion-exchange resin is used for the trace enrichment and automated sample handling of phenol, with subsequent determination by reversed-phase liquid chromatography with fluorescence detection. Because of the presence of high concentrations of ionic compounds in the water samples tested, phenol is first trapped on a relatively long precolumn filled with a highly hydrophobic packing material; during this step, (in) organic anions which are not retained, are flushed to waste. In the next step, phenol is desorbed from this column at high pH and sorbed in a small zone (“peak compression”) on a short precolumn containing the anion exchanger.

In the analysis of tap and river water samples, the detection limit was found to be 10ppt (1:10¹¹).     

Direct and mediated electrochemical oxidation of ammonia on boron-doped diamond electrode

Direct (non-mediated) electrochemical oxidation of ammonia on boron-doped diamond (BDD) electrode proceeds mainly at high pH (> 8) via free ammonia (NH₃) oxidation. To enhance ammonia oxidation on BDD at low pH (< 8), where mainly ammonium (NH₄⁺) is present, oxidation of ammonia was mediated by active free chlorine. In this process, electro-generated in situ active chlorine rapidly reacts with ammonia instead of being further electro-oxidized to chlorate at the electrode surface. Thus, active chlorine effectively removes ammonia from an acidic solution, while the formation of by-products such as chlorate and possibly perchlorate is minimized.     

An evaluation of trace element analysis in the forensic investigation of fibre samples

The use of trace element analysis in the forensic examination of fibres has been investigated. Samples of both natural and synthetic fibres have been analysed to show that it is possible to both identify and discriminate between samples that would, by present methods, be considered indistinguishable. A number of wool garments of predetermined trace element composition were sent for wear for a period of nine months. The conditions and frequency of wear and cleaning were reported to enable their effect upon the trace element composition of these garments to be determined. The wool samples were analysed by both short (30 min) and long (50 hrs) irradiations in a reactor flux of about 10¹² n·cm⁻²·sec⁻¹. This permitted the concentrations of the elements such as sodium, chlorine, iodine, manganese, cobalt and chromium to be determined. Both sodium iodide and lithium drifted germanium detectors were used to measure the induced activity of the wool samples. The composition of a range of acrylic fibres from a variety of sources has also been examined using a sodium iodide detector. The concentrations of sodium chlorine, bromine, managese, copper, aluminium, titanium, indium and barium were determined in these samples.     

Thin Layer Chromatographic Method for Rapid Identification and Quantification of Corticosteroid Sodium Phosphates in Pharmaceutical Preparations

Abstract

A rapid and inexpensive thin layer chromatography (TLC) procedure for the assay of dexamethasone sodium phosphate (DSP) and betamethasone sodium phosphate (BSP) persent in pharmaceutical preparations is described. Free steroids liberated after alkaline phosphatase reaction is isolated by TLC on silica gel layer and estimated after elution with ethanol. Assay of unesterified steroids and identification of the preservatives like methyl or propyl parabenzoates, phenol, benzyl alcohol etc. may also be carried out by this method without any additional cost. Possibility of using this method for other corticosteroid sodium phosphates (CSP) are discussed.     

Indicator Papers in Test Methods of Visual Colorimetry

Compounds for the impregnation of indicator papers were proposed for the determination of ammonia, aniline, phenol, active chlorine, chromium(VI), nickel, nitrites, and pH of natural waters, soils, and atmospheric precipitation by test methods. The determination is performed by the intensity or tint of the test liquid after the introduction of prepared indicator papers. Test procedures were developed for the determination of the above components in air and natural and waste waters. The relative standard deviation is no higher than 50%.     

A Method to Prepare Highly Effective Chlorinated Sodium Phosphate

Abstract

The chlorinated sodium phosphate is a kind of detergent containing bleaching agent for warewashing, disinfectant and bleaching agent. The active chlorine is an effective composition for this purpose.     

Determination of Ammonia in Water Using Flow Injection Analysis with Automatic Pervaporation Enrichment

Abstract

An automated ammonia monitoring system has been developed by putting a pervaporation unit in an enrichment cycle used in flow injection analysis mode. In the proposed system, an enrichment cycle was equipped to enable the adjustment for the measuring range of ammonium by controlling the duration of the enrichment circulation. Therefore, the system was capable to determine ammonia in both the surface water with low ammonia concentration and the ammonia-rich wastewater with the linear dynamic range of 0.05–15 mg l^?1 and 15–50 mg l^?1, respectively. The relative standard deviations were less than 1.9% and the quantification limit is as low as 0.03 mg l^?1. The sampling frequency is 8–10 h^?1.     

An Automated Method for the Determination of Arsenic and Antimony

Abstract

An automated method for determining arsenic and antimony by atomic absorption spectrophotometry based on the evolution of the corresponding hydride by sodium borohydride is reported. This method is rapid and sensitive, and is most suitable for the routine monitoring of the arsenic and antimony levels in surface and ground water, as well as in polluted water.     

Syntheses of Novel Hexahomotrithiacalix[3]arenes

The first synthesis of the C ₃ -symmetrical p-tert-butylhexahomotrithiacalix[3]arene 7d via one-pot procedure by the reaction of 2,6-bis(chloromethyl)-p-tert-butylphenol 8d with sodium sulfide nanohydrate under high-dilution conditions is reported. Also, hexahomotrithiacalix[3]arenes 7d-f (where d-f designate the type of the substituents R at the p-positions of the phenolic rings: d, R=t-Bu; e, R=CH₃; f, R=Cl) were synthesized via a convergent approach in good yield by the [2+1] cyclization reaction of 2,6-bis(chloromethyl)phenol monomers 8d-f and bis(chloromethyl)phenol dimers 15d-f in presence of sodium sulfide nanohydrate under high-dilution conditions. The structures of 7d-f were determined by ¹H, ¹³C NMR, MS and elemental analysis. A preliminary study of the binding properties of 7d with alkali- and heavy metal cations using biphasic picrate extraction method showed only weak abilities to bind the cations examined.     

Influence of Different Redox Conditions on the Biodegradation of the Pesticide Metabolites Phenol and Chlorophenols

Abstract

The fate and behaviour of phenol and monochlorophenols during bankfiltration and underground passage with variable redox conditions were investigated. A model ecosystem was used consisting in laboratory filter columns filled with natural underground material and operated with natural aerobic and anaerobic groundwater to create different redox situations.

The test substances (phenol, 2-chlorophenol, 3-chlorophenol, 4-chlorophenol) were added continuously to the infiltrating water and their concentration in the filter effluents determined. Beside the redox conditions other factors known to affect microbial degradation processes like the substrate concentration and the underground material were varied stepwise.

Phenol was degraded under both, aerobic and anaerobic conditions. The presence of oxygen is more favourable to degradation; no lag phase was observed under aerobic conditions. In a sulfate reducing environment, phenol could only be degraded after microbial adaptation. The length of the lag phase was strongly influenced by the substrate concentration and the undergroundmaterial. Prior contact with phenol resulted in a shorter lag phase.

Monochlorophenols behaved almost persistent in the model system. Degradation could only be observed in a test filter that provided a more active microbial population due to prior adaptation to phenol and a more favourable underground material.     

Novel Reaction Route Including Enzymic Reaction For A Synthesis Of A Branched Polysaccharide

Abstract

Stereoselective synthesis of α-D-glucosyl-branching polysaccharide by chemical and enzymic reactions was investigated. Ring-opening polymerization of 1,6-anhydro-3-O-benzoyl-2,4-di-O-benzyl-β-D-glucopyranose (1) with PF₅ as catalyst at low temperature gave a highly stereoregular polymer, which was converted to 2,4-diO-benzyl-(1→6)-α-D-glucopyranan by debenzoylation with sodium methoxide. The polymer was glucosylated according to the glycosyl imidate method. Deprotection of the branched polysaccharide was carried out with sodium in liquid ammonia at -78 °C to give a (1→6)-α-D-glucopyranan having α-D-glucopyranosyl and β-D-glucopyranosyl branches. Only the β-D-glucopyranosyl branch of the polymer was completely removed by enzymatic hydrolysis by the use of cellulase to provide stereoregular (1→6)-α-D-glucopyranan having an α-D-glucopyranosyl branch at the C-3 position. Polymers were characterized by optical rotation, NMR spectroscopy, GPC, and X-ray diffractometry.     

Analysis of Urea Nitrogen in the Presence of Ammonia Using an Ammonia Gas Sensitive Electrode

Abstract

This report describes a method for the determination of ammonia and urea in raw sewage samples using an Orion Ammonia Gas-Sensing Electrode. Urea is determined by potentiometrically measuring the ammonia produced following exhaustive hydrolysis by urease and subtracting the amount of ammonia present before enzymatic hydrolysis. The recovery of urea from raw sewage samples using the procedure herein described is shown to be nearly Quantitative.     

The Thin-Layer Chromatographic Separation of Halogenated Fumigants as Ammonium Halides and Their Subsequent Determination by Meca

Abstract

A method is described for the determination of several pesticides containing bromine and chlorine by molecular emission cavity analysis (MECA). The pesticides were decomposed in an oxygen flask and the combustion products dissolved in aqueous ammonia. The ammonium halides were separated by TLC using microcrystalline cellulose adsorbent. After scraping from the TLC plates and dissolving in water the separated components were quantitated by MECA using either the InBr (Λ_max = 376 nm) or the InCl (Λ_max = 360 nm) emission bands. Recoveries of over 96% were obtained. Soils fortified with l, 2-dibromo-3-chloropropane at levels of 5–25 ppm were extracted using shaking and distillation procedures. Subsequent analysis showed that the shaking extraction gave a recovery of 92% compared to 85% from acid refluxing.