Green Determination of Total Iron in Water by Digital Image Colorimetry

A green iOS digital image colorimeter was fabricated for the determination of total iron in natural water. A mobile application operating on an iOS device was designed using Euclidean distance theory to perform iron determination. The application records the components of the color by storing red, green, and blue values as well as calculating the hue, saturation, brightness, and gray values using standard color theory. The component values obtained from the images of orange solutions of iron(II) complex with 1,10-phenanthroline were collected in a database and used for evaluation of the total iron concentration in water samples. Under the optimal conditions for solid-phase extraction used for sample preconcentration, the enrichment factor was 8.18. The iron concentration was determined by this device for concentrations from 0.01 to 1.0?ppm. The iOS digital image colorimeter achieved a limit of quantitation of 0.1?ppm. The accuracy and precision of the iOS digital image colorimeter were validated using a certified reference material, riverine water. The instrumentation was used for the analysis of natural water samples.     

Colorimetric analysis of water and sand samples performed on a mobile phone

Analysis of water and sand samples was done by reflectance measurements using a mobile phone. The phone's screen served as light source and front view camera as detector. Reflected intensities for white, red, green and blue colors were used to do principal component analysis for classification of several compounds and their concentrations in water. Analyses of colored solutions and colorimetric reactions based on widely available chemicals were performed. Classification of iron(III), chromium(VI) and sodium salt of humic acid was observed using reflected intensities from blue and green light for concentrations 2-10 mg/l. Addition of complex forming sodium salt of ethylenediaminetetraacidic acid enabled the discrimination of Cu(II) ions in the 2-10 mg/l concentration range based on reflection of red light. An alternate method using test strips for copper solutions with the phone as reader also demonstrated a detection limit of 2 mg/l. Analysis of As(III) from 25 to 400 μg/l based on reflection of red light was performed utilizing the bleaching reaction of tincture of iodine containing starch. Enhanced sensitivity to low concentrations of arsenic was obtained by including reflected intensities from white light in the analysis. Model colored sand samples representing discoloration caused by the presence of arsenic in groundwater were analyzed as a complementary method for arsenic detection.     

FTIR, XRD, and DSC analysis of the rosemary extract effect on polyethylene structure and biodegradability

The purpose of this research study was evaluation of the utility of two common multivariate techniques, agglomerative cluster analysis (CA) and principal component analysis (PCA), as supplementary means of detecting incompatibilities, which can occur between active pharmaceutical ingredients and excipients at the preformulation stage of a solid dosage form. For the detection of incompatibilities between atenolol (beta blocker) and selected excipients (mannitol, lactose, starch, methylcellulose, β-cyclodextrin, meglumine, chitosan, polyvinylpyrrolidone and magnesium stearate), the thermogravimetry (TG), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) were chosen. The results have shown that compatibility between atenolol and an excipient can be identified in a CA dendrogram by two large clusters, from which one groups an excipient and physical mixtures with a high concentration of the excipient. Another cluster encompasses atenolol and mixtures with a high content of the drug. In the PCA plot, all samples are located along the first principal component axis (PC1), beginning from a single component located with the most negative PC1 value, through mixtures with gradually varying concentration of both ingredients, till the second component located close to the most positive PC1 values. The results have shown that CA and PCA fulfil their role as supporting techniques in the interpretation of the data acquired from the TG curves, and the obtained data are compatible with the results of DSC and FTIR analyses.     

A robust multi-syringe system for process flow analysis. Part 3. Time based injection applied to the spectrophotometric determination of nickel(II) and iron speciation.

A new software-controlled time-based system for sample or reagent introduction in process flow injection analysis was developed. By using a multi-syringe burette coupled with one multi-port selection valve, the time-based injection of precise known volumes was accomplished. Characteristics and performance of the injection system were studied by injecting an indicator in a buffered carrier. Two multi-syringe time-based injection (MS-TBI) systems were implemented: first, the injection of a sample in a multiple-channel manifold where the sample would sequentially merge and react with different reagents, and second, the sequential injection of several solutions (sample and reagents) into a particular flowing stream. The first system was applied to the spectrophotometric determination of nickel(II) in diluted samples from the acidic nickel ore leaching process, by using ammonium citrate as carrier, a saturated solution of iodine as oxidizing agent and alkaline dimethylglyoxime as chromogenic reagent. The sampling frequency attained was 57 h-1. Determinations on process samples compared well at the 95% confidence level with the reference values obtained by ICP-OES. The second time-based injection system was applied to the speciation of iron. Total iron and iron(II) concentrations were separately and sequentially determined using 1,10-phenanthroline in acetic buffer medium as reagent. The developed manifold allowed the optional use of two different carrier solutions, containing or not containing ascorbic acid, for performing the separate determinations. Also, in the sequential procedure, plugs of reducing carrier were alternatively intercalated before the sample injections used for total iron determinations. Sampling frequencies of 68 injections per hour were routinely used. Accuracy was assessed by analyzing synthetic known mixtures of Fe(III) and Fe(II) standard solutions. Recoveries of 98-100.5% with a maximum relative standard deviation of 3.6% were found. Results obtained for various samples of fertilizers agreed well with those attained by the standard batch procedure.     

Principal Component‐Wavelet Neural Network as a Multivariate Calibration Method for Simultaneous Determination of Iron,Nickel, and Cobalt

Abstract

Principal component‐artificial neural network (PC‐ANN) and principal component‐wavelet neural network (PC‐WNN) are applied for simultaneous determination of iron(II), nickel(II), and cobalt(II). A simple and selective spectrophotometric method for simultaneous determination of iron(II), nickel(II), and cobalt(II) based on formation of their complexes with 1‐(2‐pyridylazo)‐2‐naphtol (PAN) in micellar media is described. Although the complexes of Fe(II), Ni(II), and Co(II) with reagent show a spectral overlap, they have been simultaneously determined by PC‐ANN and PC‐WNN. The results obtained by the two methods were compared and it was shown that in PC‐WNN, the convergence speed was faster and the root mean square error of prediction set was also smaller than PC‐ANN. Interference effects of common anions and cations were studied and the proposed method was also applied satisfactorily to the determination of Fe(II), Ni(II) and Co(II) in synthetic samples.     

Determination of trace levels of iron in a seawater sample using isotope dilution/inductively coupled plasma mass spectrometry.

An analytical method for trace levels of iron in a seawater sample using isotope dilution ICP-MS was developed. Preconcentration of iron and the removal of major elements in seawater such as alkali and alkaline-earth elements can be carried out quickly using a chelating resin disk by adjusting the sample pH to 3. The collision cell option of the ICP-MS instrument method was used to improve the performance of the instrument for iron measurements since ArO and ArN interferences could be reduced using this analytical method. About 4 ml min(-1) helium, as the collision gas, were introduced into the cell. 40Ar14N and 40Ar16O which interfere with 54Fe and 56Fe in water had their amounts decreased by 5 orders of magnitude. Then, the isotope dilution method was used for iron determination below ng g(-1) level of trace iron in four environmental reference materials (river water standard sample JAC-0031 (Japan Soc. for Analytical Chemistry), estuarine standard sample SLEW-2 (NRC Canada) and seawater standard samples CASS-3 and NASS-5 (NRC Canada)) were measured. Good agreement between analytical results and certified values of reference materials was obtained, which confirmed the effectiveness of this method.     

A Simple and Cheap Device for Colorimetric Determination of Serum Iron

A simple and cheap device for colorimetric determination of serum iron and TIBC (total iron‐binding capacity) was devised. The proposed device employs an LED as a light source and a common light dependent resistor (LDR) as a detector. This device functions on the basis of the light intensity received by LDR, connected to a digit multimeter, yielding resistance readings. The serum, standard, and blank solutions were prepared according to the kits instructions and introduced into the colorimeter with a disposable syringe. The iron content of the serum was calculated from the resistance difference of serum and standard solutions. The precision of the method was assessed with two commercially available serum‐based chemistry controls. The values obtained with the proposed device indicated that the serum iron concentrations correlated well with the values obtained with the commercial automated analyzer. The calibration graph was linear for iron concentrations up to 90 μmol/L (500 μg/dL). The proposed fabricated colorimeter is considerable cheaper, requires smaller sample volumes, and is suitable for serum iron assay.     

Phase morphology of blends of polycarbonate with poly(methyl methacrylate-co-cyclohexyl methacrylate), and of polycarbonate with poly(methyl methacrylate) by solid state nuclear magnetic resonance,differential scanning calorimetry,and transmission electron microscopy

The miscibility of polycarbonate (PC) with poly(methyl methacrylate-co-cyclohexyl methacrylate) (PMCHM) and with poly(methyl methacrylate) (PMMA) was studied by nuclear magnetic resonance (NMR) ¹H spin-lattice relaxation time in the rotating frame (¹H T_1p), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). A blend of PC/PMCHM (50/50 wt/wt) with the acrylic component PMCHM, a copolymer of PMMA and poly(cyclohexyl methacrylate) (80/20 wt/wt), shows only one T_1p value, which indicates high miscibility in this blend. A blend of PC/PMMA (50/50 wt/wt) shows two ¹H T_1p values, which are similar to those of the homopolymers PC and PMMA. These results indicate high immiscibility. The “domain size” calculated from NMR results of the miscible blend PC/PMCHM is approximately 40 Å. The results of DSC and TEM are similar to the NMR results. However, TEM results show the presence of 3% PC domains in the PC/PMCHM blend, which are not seen by NMR or DSC. Those PC domains are approximately 500 Å. A strong intramolecular repulsion in the copolymer PMCHM and specific intermolecular interactions between PC and PMMA may explain the miscibility in the PC/PMCHM system. © 1994 John Wiley & Sons, Inc.     

链解缠结聚对苯二甲酸乙二酯的结晶行为研究

采用冷冻萃取聚对苯二甲酸乙二酯(PET)溶液(0.1～10g/dL7种不同浓度,3种不同性能溶剂)的方法制备了解缠结PET试样.与链相互穿透且缠结的熔体骤冷试样相比,解缠结PET试样的结晶能力明显增强,且随着制样溶液浓度的降低,链间解缠结程度增加,PET的结晶能力逐渐增强,有序结构含量明显增加,但是如果制样溶液浓度太低,溶液中链间距离太大,则又不利于萃取过程中链间的有序堆砌而结晶.采用接触浓度c*附近的溶液,既可确保链间的有效解缠结又有利于链间的有序堆砌而结晶.PET的结晶能力甚至还受制样所用溶剂性能的影响,这是因为溶剂性能影响了溶液中链间的相互作用以及链的解缠结程度.     

Separation and preconcentration of iron(II) and iron(III) from natural water on a melamine-formaldehyde resin

A combined method for the preconcentration and selective spectrophotometric determination of both valencies of iron, i.e., Fe(II) and Fe(III), down to 0.4 mug l(-1) has been developed. Iron(III) from synthetic and natural water samples has been concentrated on a melamine-formaldehyde resin at pH 5; iron(II) was not retained under identical conditions. The oxidized iron was concentrated on a second resin column. The iron in both columns was eluted with 1 M HCl solution and separately analyzed by the 1,10-phenanthroline-citrate spectrophotometric method. The effect of pH, adsorption and elution rates, and interferences on the developed procedure were investigated. Metal ions that can be retained by the resin at moderate concentrations, e.g., Al(3+), do not cause interference in more dilute solutions encountered in natural water samples. At least 160-fold volume enrichment can be easily obtained using an adsorption flowrate of 50 ml min(-1). A hydrothermal water sample was analyzed by the recommended procedure and by a literature method, and the results were statistically compared by t- and F-tests.     

Equilibrium in-fiber standardization method for determination of sample volume by solid phase microextraction

This paper describes an in-fiber standardization method by Solid Phase Microextraction (SPME) for the determination of a sample volume. After loading a specific amount of standard, the volumetric standard, on a PDMS-coated fiber (n(0)), the fiber was exposed in the headspace of sample vials containing different volumes of water. The amount of standard that remained on the fiber after equilibrium (n(f)), which was determined with gas chromatography/mass spectrometry (GC/MS), depends on the volume of the sample. Naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, 1-ethylnaphthalene, and 2-ethylnaphthalene were chosen as volumetric standards based on theoretical calculations. The effect of loading time, exposure time, and exposure temperature were investigated. The effect of the matrix was also studied, analyzing both water and wine samples. Precision and accuracy of the method were obtained for each standard in both water and wine. The partition coefficients of the compounds between the fiber and the sample (K(fs)) and between the headspace and the sample (K(hs)) were obtained by plotting n(0)/n(f)versus sample volume.     

Determination of total tin in river water by hydride generation-atomic absorption spectrometry

Summary The total tin in river water was determined by hydride generation-atomic absorption spectrometry in sulphuric acid medium. The water was concentrated with nitric and sulphuric acids. Interference from copper and iron was eliminated by extracting copper with a carbon tetrachloride solution of zinc dibenzyldithiocarbamate and by complexing iron with 1,10-phenanthroline in solution. The acidities of the sample solutions were checked by weighing the residue in the flasks during the acid digestion so that the acidities of the sample solutions became approximately equal to those of the calibration solutions. When a 1,000 mg/l tin(IV) solution was diluted with water, the hydrolysed tin could not be determined entirely as the total tin by acidification with sulphuric acid, but it could be recovered completely by digestion even after 5 days. Thus digestion is essential when determining the total tin in water.     

The Application of Modulated Temperature Power Compensation DSC to the Characterisation of Polymer Blends

A modulated temperature power compensated differential scanning calorimeter, MTDSC, has been built from a standard Perkin-Elmer DSC model-2 such that a computer generated voltage has been applied to induce a sinusoidal change in sample temperature superimposed on a linear heating rate. The effect of amplitude of the temperature fluctuation, modulation period and block temperature on the reversibility has been assessed from the Lissajous diagram of heat flow vs. sample temperature. From their reproducibility and symmetry the most effective conditions for operating the MTDSC has been deduced. The specific heat of sapphire has been measured using these operational conditions for comparison with conventional DSC. Phase separated blends of polycarbonate (PC) and polyethylene terephthalate (PET) have been analysed. This revised version was published online in August 2006 with corrections to the Cover Date.     

An on-line flow-injection microwave-assisted mineralization and a precipitation/dissolution system for the determination of molybdenum in blood serum and whole blood by electrothermal atomic absorption spectrometry

An on-line flow injection (FI) precipitation–dissolution system with microwave-assisted sample digestion has been developed for the electrothermal atomic absorption spectrometry (ETAAS) determination of trace or ultratrace amounts of molybdenum in human blood serum and whole blood samples. After the exposure of the sample to microwave radiation, the on-line precipitation of molybdenum was achieved by the merging-zone of a 0.5-ml plug of sample with a plug of potassium ferrocyanide, which were carried downstream with a solution of 0.5 mol l⁻¹ of HNO₃. The interfering effects of iron and copper were minimized by the introduction of a flow of a 5% (w/v) sodium potassium tartrate (for iron) and 2% (w/v) of thiourea (for copper and zinc) in a 5% (v/v) ammonia and 2% (v/v) ammonium chloride solution previous to the precipitation reaction. The reddish-brown precipitate of molybdenyl ferrocyanide was collected on the walls of a knotted reactor. The precipitate was dissolved with the introduction of 1 ml of a 3.0 mol l⁻¹ NaOH solution and the best performance in terms of detection limit and precision was achieved when a sub-sample of 140 μl was collected in a capillary of a sampling arm assembly, to introduce 20 μl volumes into the atomizer by means of positive displacement with air through a time-based injector. A detection limit (3σ) of 0.1 μg Mo l⁻¹ using an aqueous standard solution was obtained. The method is quantitative and is applied over the range 0.2–20.0 μg Mo l⁻¹. The precision of the method evaluated by ten replicate analyses of aqueous standard solutions containing 0.5 and 1.0 μg Mo l⁻¹ was 2.8 and 3.1% (relative standard deviation, RSD) (for n=5), respectively. Whereas, the precision evaluated by five replicate analysis of a serum and a whole blood sample were 3.3 and 3.8% RSD. An enrichment factor of ca. 3.5 was achieved with the introduction of 0.5 ml aqueous standard solutions at a sample flow rate of 1.0 ml min⁻¹. Recoveries of spiked molybdenum in blood serum and whole blood were in the ranges 96–102 and 94–98%, respectively. The results obtained for two human whole blood certified reference materials were in good agreement with the indicative values.     

Determination of the rare earth elements in natural waters by isotope-dilution mass spectrometry

A method is described for the determination of ten rare earth elements (La, Ce, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu) in natural waters by isotope-dilution mass spectrometry. A 1-l sample is used for sea water, and proportionately less for other natural waters. The rare earth elements are extracted by co-precipitation with hydrated iron (III) oxide and purified on a single cation-exchange column, with hydrochloric and nitric acids as eluents. Final measurements are from a triple Re/ Ta filament in the mass spectrometer, run automatically under computer control. Relative standard deviations are better than 4% for the analysis of standard solutions, with accuracy in the same range. The analytical blank is low ( <0.03 pmol, 4 pg, for Nd) producing a sample/blank concentration ratio greater than 100 for all ten rare earth elements when determined in a 1-l seawater sample. Concentration depth profiles are given for an ocean water and normalised abundance patterns for three natural waters.     

Rapid and highly sensitive determination of low-molecular-weight carbonyl compounds in drinking water and natural water by preconcentration HPLC with 2,4-dinitrophenylhydrazine.

The aim of this research was to develop a simple procedure for a highly sensitive determination of low-molecular-weight (LMW) carbonyl compounds in drinking water and natural water. We employed a preconcentration HPLC system with 2,4-dinitrophenylhydrazine (DNPH) for the determination of LMW carbonyl compounds. A C-18 reverse-phase preconcentration column was used instead of a sample loop at the sample injection valve. A 0.1 - 5.0 mL portion of the derivatized sample solution was injected with a gas-tight syringe, and a 15% acetonitrile aqueous solution was pushed through the preconcentration column to remove the unreacted excess DNPH, which caused serious interference in the determination of formaldehyde. The detection limits were 1 - 3 nM with a relative standard deviation of 2 - 5% for 20 nM standard solutions (n = 5). The calibration curves were essentially unaffected by coexisting sea salts. Applications to commercial mineral water, tap water, river water, pond water and seawater are presented.     

Analysis of structure transition and compatibility of PTT/PC blend without transesterification

Poly(trimethylene terephthalate)/polycarbonate (PTT/PC) blends were prepared by solvent mixing to avoid transesterification during high temperature blending. The influences of compositions on the thermal behavior, crystallization morphology and structure of the blends were studied. FTIR results indicated that there was no COO linking to two phenyl groups on each side chain and DSC results supported no transesterification reaction. DSC curves showed that T _c and T _mc increased to maximum range when PC contents were between 7 wt%-15 wt%, however, T _m decreased constantly with the increase of PC contents. It was observed from POM that PTT spherulitic morphology and crystallization kinetics were obviously influenced by the change of PC contents. Structural evolutions during cooling were investigated by SAXS which showed L _c of PTT remained a constant with different PC contents and also fixed during crystallization, nevertheless, it revealed a maximum value of L _nc for sample PTT₉₃. It was concluded that PC chains could be permeated into not only amorphous crystallite structure but also amorphous lamellae structure and 7 wt% PC content was supposed to be the “proper” penetration amount into PTT lamellae structure which led to a maximum capacity of amorphous lamellar layer. Fringedmicelle crystal model was adopted to illustrate semi-crystalline physical structures of the blend in two kinds of component aggregation states.     

Application of internal standardization to rapid coprecipitation technique using lanthanum phosphate for flame atomic absorption spectrometric determination of iron and lead.

By applying an internal standardization, we could use a rapid coprecipitation technique using lanthanum phosphate as a coprecipitant for preconcentration of iron(III) and lead in their flame atomic absorption spectrometric determination. Indium as an internal standard was added to the initial sample solution together with lanthanum and phosphoric acid; the coprecipitation of iron(III) and lead was then carried out at pH about 3. After measuring the atomic absorbances of iron, lead, and indium in the final sample solution, we determined the contents of iron(III) and lead in the original sample solution by using the internal standardization with indium. In this method, complete collection of the precipitate was not required after the coprecipitation of iron(III), lead, and indium, because the ratio of the recovery of iron(III) or lead to that of indium was almost constant regardless of the recovery of the precipitate. This method was simple and rapid, and was available for the determination of 2-300 micrograms L-1 of iron(III) and 5-400 micrograms L-1 of lead in some water samples.     

Solid-phase extraction of some heavy metal ions on a double-walled carbon nanotube disk and determination by flame atomic absorption spectrometry

A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.     

Kinetics of the light-driven aqueous autoxidation of sulfur(IV) in the absence and presence of iron(II)

The photochemical autoxidation of aqueous, acidic sulfur(IV) solutions was studied in the absence and presence of iron(II) by a newly introduced technique using a diode-array spectrophotometer, in which the same light source is used to drive and detect the reaction. Based on detailed kinetic and stoichiometric data sets, a non-chain mechanism is proposed for the autoxidation of sulfur(IV). In this mechanism, excited hydrated sulfur dioxide, *H2O.SO2, first reacts with O2 to form peroxomonosulfate ion, HSO5-, which rapidly oxidizes another H2O.SO2 to give hydrogensulfate ion as a final product. In the presence of iron(II), the formation of iron(III) was detected, which can be interpreted through the simultaneous contribution of two additional pathways: some of the HSO5- formed oxidizes iron(II) instead of sulfur(iv), and *H2O.SO2 also reacts directly with iron(II) to yield iron(III). This mechanism provides a sufficient quantitative interpretation of all experimental observations.