Test determination of aluminum, beryllium, and cationic surfactants using phenolcarboxylic acids of the triphenylmethane series immobilized on cloths from synthetic and natural fibers

We consider the use of cloth matrices from viscose and cotton fibers bearing phenolcarboxylic acids of the triphenylmethane series immobilized by adsorption in chemical test methods of analysis. Chrome Azurol S, Sulfochrome, and Eriochrome Cyanine R were used for immobilization. It was found that the reagents are weakly retained on cellulose matrices. The degree of retention varied from 10 to 60%. It was observed that the reagent complexes of metal ions exhibited enhanced adsorbability on the matrices. Cloths with immobilized Chrome Azurol S were used in the test determination of 0.0005–0.5 mg/L beryllium and 0.0005–1.0 mg/L aluminum. When the reaction products were preconcentrated on the cloth from 100 mL of a test solution, the detection limit was 0.0001 mg/L. Procedures were developed for determining 0.1–100 mg/L aluminum and 0.02–0.6 mg/L beryllium in solutions using cloth test strips encapsulated into a polymeric film. It was demonstrated that Sulfochrome and Eriochrome Cyanine R immobilized on cloths can be used to determine 0.01–1 and 1–1000 mg/L cationic surfactants.     

2,3,7-Trihydroxyfluorones immobilized on cellulose matrices in test methods for determining rare elements

It was shown that 2,3,7-trihydroxyfluorones immobilized by adsorption on cellulose matrices can be used as reagents for the test determination of Mo(VI), Ti(IV), Ge(IV), Hf(IV), Nb(V), Ta(V), W(VI), Bi(III), V(IV), and Zr(IV). The change of the protolytic and complexing properties of trihydroxyfluorones immobilized on cellulose matrices was considered in comparison to corresponding properties in a solution. It was found that the reactions of trihydroxyfluorones with rare elements on cellulose matrices and in a solution exhibit similar effects upon the addition of cetylpyridinium. These effects are the bathochromic shift of the absorption maxima of the reagents and their complexes with analytes and the extension of the range of optimum acidity for complex formation. The complexation of salicylfluorones with the titanium(IV) in solution and on cellulose paper was studied by IR spectrometry. Phenylfluorone immobilized on a mixed-fiber cloth as used in test determinations of (mg/L) 0.05–5 Ti(IV), V(IV), Hf(IV), Nb(V), and Mo(VI); 0.01–5 Ge(IV) and Zr(IV); 0.05–1 Bi(III) and W(VI); and 0.1–5 Ta(V) by the color intensity of the indicator matrix after passing through 20 mL of a test solution. It was shown that phenylfluorone immobilized on cellulose paper can be used to determine (mg/L) 0.05–50 Ti(IV), 0.5–1000 Ge(IV), 0.5–500 Zr(IV), 5–200 Bi(III), 0.1–50 Mo(VI), 0.1–1000 V(IV), 0.1–100 Nb(V), 0.1–800 Hf(IV), 1–100 Ta(V), and 1–800 W(VI) by the length of the colored zone of a test strip after it was brought into contact with a test solution.     

Determination of molybdenum using 1,5-diphenylcarbazone immobilized on silica

The sorption of 1,5-diphenylcarbazone on highly dispersed silica from toluene and acetone-hexane (1:4) solutions was studied. The nature of the bonding of the reagent with the surface of silica gel was studied by absorption spectrometry. A solid-phase reagent is proposed for the sorption-diffuse-reflection and visual test determinations of down to 0.025 and 0.05 μg/L molybdenum(VI), respectively. The procedures were used for the determination of molybdenum in sea salt and a medicinal preparation.     

Measurements of kineic parameters of inorganic pyrophosphatase by flow-injection procedures

Two flow-injection systems were designed for characterizing the enzymatic hydrolysis of pyrophosphate by inorganic pyrophosphatase (EC 3.6.1.1). By using a molybdenum(VI) reagent the selective determination of a product, orthophosphate, in the presence of pyrophosphate was made. An anion exchange column was employed for the simultaneous determination of both the substrate and the product with a molybdenum(V)/molybdenum(VI) reagent. The effects of magnesium concentration and reaction temperature on the enzyme activity were determined. The Michaelis constant and maximum velocity at 25°C and pH 7.2 were evaluated. K_m was ca. 3 μM.     

Spectrophotometry Determination of Molybdenum with N-Cyanoacylacetaldehyde Hydrazone

N-cyanoacylacetaldehyde hydrazone (CAAH), which is a laboratory synthetic reagent, is proposed as a new reagent for spectrophotometry determination of microamounts of molybdenum at λ_max 790 nm. The reagent forms 1:1 blue coloured complex with molybdenum (VI) in phosphoric acid solution. The stable blue colour is obtained finally after changing from yellow to green. The colour development depends on temperature, time and concentration of phosphoric acid. This reagent is applied for the determination of molybdenum in steel alloys and the results are satisfactory.     

Kinetic spectrophotometric determination of traces of molybdenum(VI) by its inhibitory effect on the oxidation of 4-hydroxycoumarine by potassium permanganate.

The present paper describes a simple, selective and sensitive kinetic method for the determination of trace amounts of molybdenum(VI) based on its inhibitory effect on the reaction oxidation of 4-hydroxycoumarine by KMnO(4) in the presence of hydrochloric acid, at pH 1.75 at 25 degrees C. The rate of the indicator reaction was followed spectrophotometrically by measuring the decrease in the absorbance of KMnO(4) at 525 nm. The development method includes optimization of the reagent concentration and temperature. The calibration graph was linear in the range of concentrations from 20 to 200 ng/cm(3) of molybdenum(VI). The probable relative error was in the interval 3.10 - 10.52% for the concentration range of 200 - 20 ng/cm(3) molybdenum(VI), respectively. The interference effects of the foreign ions were determined to assess the selectivity of the method. The developed method was found to have relatively good selectivity, sensitivity, simplicity and rapidity. The proposed method was applied to the determination of molybdenum(VI) in a particular type of steel and alloy (hastelloy).     

1-Phenyl-3-methyl-4-benzoylpyrazol-5-one as a group-extraction reagent for spectrophotometric determination of trace elements

1-Phenyl-3-methyl-4-benzoylpyrazol-5-one has been examined as a regent for detection and solvent extraction of metal ions. The reagent seems to be promising as a group-extraction reagent for the spectrophotometric determination of copper, nickel, cobalt, manganese, zinc, chromium(VI) and molybdenum(VI).     

Spectrophotometric Determination of Trace Amounts of Molybdenum in Steel and Pure Iron with a New Chromogenic Reagent Dimethoxyhydroxyphenylflurone

ABSTRACT

A simple method for the direct determination of trace molybdenum in low alloy steel and pure iron with selectivity and sensitivity is reported. In the presence of TritonX-100 and sulphuric-phosphoric acid medium, a new chromogenic reagent dimethoxyhydroxyphenyl-flurone (DMHPF) forms a red complex with molybdenum(VI). The molar absorptivity is obeyed from the range of 0? 8 μg/25 ml for molybdenum(VI). Most of metal ions and 35000-fold amounts of iron do not interfere with the determination of molybdenum. The proposed method has been successfully used for the determination of trace amounts of molybdenum in steel and pure iron specimens.     

Triphenyltetrazolium chloride as a new analytical reagent for molybdenum(VI): Application to plant analysis

Solvent extraction of molybdenum(VI) ion associate with triphenyltetrazolium chloride (TTC) has been studied. TTC was proposed as reagent for the spectrophotometric determination of micro amounts of molybdenum(VI) at λ_max 250 nm. The optimum conditions for extraction of molybdenum(VI) as an ionassociation complex with TTC has been determined. Beer’s law is obeyed in the range of 0.5–10 μg/mL molybdenum(VI). The molar absorptivity of the ion-pair is 1 × 10⁶ L/mol cm. The sensitivity of the method is 9.6 × 10⁻⁵ μg/cm². The characteristic values for the extraction equilibrium and the equilibrium in the aqueous phase are: distribution constant K _D = 32.64, extraction constant K _ex = 2.19 × 10¹⁰ association constant β = 6.71 × 10⁸. The interferences of different cations, anions on molybdenum(VI) determination were also investigated. A sensitive and selective method for the determination of microquantities of molybdenum(VI) has been developed. The determination was carried out without preliminary separation of molybdenum. A novel procedure of molybdenum(VI) extraction and spectrophotometric determination in different plant samples was examined.     

Spectrophotometric determination of trace molybdenum in plants and seeds with 3,5-dibromo-4-hydroxyphenylflurone

A novel spectrophotometric method based on a new reagent, 3,5-dibromo-4-hydroxyphenylflurone, was developed for the determination of molybdenum in plants and seeds. 3,5-Dibromo-4-hydroxyphenylflurone showed outstanding analytical characteristics for spectrophotometric determination of molybdenum. The reaction conditions are simple and stable. In 0.2 mol l(-1) phosphoric acid medium (which can combine with iron and other metal ions and greatly improves the selectivity of the color system), molybdenum(VI) reacts with 3,5-dibromo-4-hydroxyphenylflurone to form a 1:2 red complex with an absorption maximum at 530 nm, the color reaction can completed in 2 min and the absorbance of the molybdenum complex remains stable for at least 72 h at room temperature. Its stability constant is 1.21 x 10(28) at 25 degrees C. Beer's law is obeyed over the range 0-0.6 microg ml(-1) Mo(VI). The reagent has very high sensitivity and selectivity; the molar absorptivity of the complex is 1.35 x 10(5) 1 mol(-1) cm(-1) and the limit of quantification, the limit of detection and relative standard deviation (n = 10) were found to be 6.7 ng ml(-1), 2.2 ng ml(-1) and 1.01%, respectively. Cu (50000-fold), Fe (20000-fold), K (20000-fold), NH4+ (20000-fold), Mg (15000-fold), Zn (10000-fold), Na (10000-fold), Al (4000-fold), Ca (25000-fold), Mn (2000-fold), Ce (500-fold), Cr (400-fold) and Bi (200-fold) do not interfere with the determination of trace levels of molybdenum up to the excesses indicated. The selectivity is much superior to that of other published methods. The proposed method was applied to the direct determination of molybdenum in plants and seeds with satisfactory results. The synthesis of the reagent and conditions of color reaction were studied in detail.     

Consecutive sorption of molybdenum(VI) and chromium(VI) from a single sample onto fiber materials filled with an anion exchanger and their solid-phase determination with phenylfluorone and diphenylcarbazide

We have considered the possibility of the sorption-spectrometric determination of molybdenum(VI) with phenylfluorone and chromium(VI) with diphenylcarbazide from a single sample by consecutive sorption from different media onto fiber materials filled with an AV-17 anion exchanger. The dependences of analytical signals of molybdenum and chromium on the sorption conditions (pH of the initial solution, NaCl concentration, sizes of the support disc, agitation time) have been studied in the batch mode. The conditions of analytical signal registration have been determined and the analytical ranges have been established (0.01–0.06 μg/mL for Cr and 0.02–0.2 μg/mL for Mo). It has been demonstrated that molybdenum and chromium can be determined at their ratios from 1: 1 to 5: 1 from a single sample after chromium sorption from 0.1 M HCl and molybdenum sorption at pH 4 by diffuse-reflection spectroscopy or visual test. The selectivity of molybdenum and chromium determination in the presence of interfering ions has been studied.     

Determination of molybdenum(VI) by differential pulse polarographic technique using 4-(2-hydroxy phenyl ethaminodiol), benzene-1,3-diol(4-2-HPEDB-1,3,D)

A novel analytical reagent 4-(2-hydroxy phenyl ethaminodiol), benzene-1,3-diol(4-2-HPEDB-1,3,D) was synthesized for the determination of molybdenum(VI). The present paper reveals the detailed study of electroanalytical behaviour for [Mo-(4-2-HPEDB-1,3,D)] complex under optimized conditions. The peak obtained for [Mo-(4-2-HPEDB-1,3,D)] prevent the interference of foreign ions which shows the sensitivity of the proposed method. The linearity was maintained at the concentration range of 0.5–200 μg/mL at pH 4.5 with correlation factor 0.9997. The present method was successfully applied for the analysis of molybdenum(VI) in biological fluids and plant material. The results obtained from the proposed method show good agreement with reference method.     

Determination of trace molybdenum in vegetable and food samples by spectrophotometry with p-carboxyphenylfluorone

A new highly sensitive and selective chromogenic reagent, p-carboxyphenylfluorone (p-CPF), was studied for spectrophotometric determination of trace molybdenum. In 0.36 mol L(-1)phosphoric acid medium, p-CPF reacts with molybdenum(VI) to form a 1:3 red complex, which has a sensitive absorption peak at 531 nm. Under optimal conditions, the reaction of molybdenum(VI) with p-CPF completed rapidly and absorbance remains almost constant for at least 24 h. Molybdenum(VI) obeyed Beer's law in the range 0-2.0 microg mL(-1); the apparent molar absorption coefficient, Sandell's sensitivity and the limit of detection were found to be 1.03 x 10(5) L mol(-1) cm(-1), 1.028 ng cm(-2)and 0.73 ng mL(-1) respectively; the effect of various foreign ions were examined in detail. It was found that most coexisting ions can be tolerated in considerable amounts, especially 800 mg of Mn(II), 200 mg of Mg(II), Fe(II), Co(III), Ni(II) and Cd(II), 50 mg of Ca(II) and Al(III), 25 mg of Cu(II) and Fe(III), 10 mg of Hg (II), La(III), Bi(III), Pb(II) and Zn(II) don't interfere with the determination of molybdenum(VI). The proposed method is very simple, sensitive and selective, it has been applied to determine molybdenum in vegetable and food samples with a very high precision and accuracy. Moreover, the synthesis of the reagent and the conditions of the colour reaction were also studied in detail.     

Carminic acid as a reagent for the spectrofluorimetric determination of molybdenum and tungsten-I Development of procedures

Carminic acid forms red fluorescent complexes with molybdenum(VI) and tungsten(VI) which provide spectrofluorimetric methods for the determination of these metals in the range 0.1–0.9 ppm and 0.4–0.36 ppm at pH 5.2 and 4.6 respectively. The optimum conditions for the analytical procedures have been established, and the effects of a wide range of cations and anions have been investigated. The reagent forms 1:1 complexes with both molybdenum and tungsten, and the conditional stability constants have been evaluated.     

Pyrocatechol Violet in New Optical Methods for Determining Molybdenum(VI)

The complexation of molybdenum(VI) with Pyrocatechol Violet (PCV) in the absence or presence of a cationic surfactant, cetyltrimethylammonium (CTMA), was studied. Conditions for the preconcentration of molybdenum(VI) as its PCV complex on adsorbents of different nature were found. Concentration factors were at least 67 at a liquid phase volume of 20 mL and for an adsorbent sample of 0.3 g. Chromaticity characteristics of complexes were determined in the solution and on the adsorbent. It was shown that the PCV complex of molybdenum(VI) in the presence of CTMA can be used in the analysis of low-molybdenum samples. A test scale for the semiquantitative determination of molybdenum was obtained.     

Azo compounds as reagents for the voltammetric determination of molybdenum(VI)

Linear sweep voltammograms of Lumogallion IREA (pH 2), Magneson IREA (pH 2), 4-(2-pyridylazo)resorcinol (pH 4.8), and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (pH 4.8) in the presence of molybdenum(VI) exhibit peaks at potentials more negative than the potentials of reduction peaks of the reagents by approximately 0.1 V. In all of the above cases, the heights of these peaks linearly increased with an increase in the concentration of molybdenum(VI) in the range from 5 x 10^-7 to 2.5 x 10^-6 M; thus, these peaks can be used for the determination of molybdenum. The simultaneous proportional decrease in the heights of the cathodic peaks of the reagents can be used for indirect determination of molybdenum(VI). The limits of detection without preliminary accumulation at a dropping mercury electrode with a drop time of 5 s are (1.5-3.9) x 10^-7 M, depending on the nature of the reagent and the technique used for determining the concentration.     

A New Method for the Microdetermination of Molybdenum (VI) in Steel,Biological Materials and Waters

Abstract

A method is presented for the trace analysis of molybdenum (VI) in standard steel sample, plant tissues, animal tissues, and natural waters. The method is based on the extractive separation of molybdenum from complex matrices by chelating it with a new reagent N-p-methoxypheny1-2-furylacrylohydroxamic acid (MFHA) into isoamyl alcohol followed by spectrophotometric determination, Eight other new hydroxamic acids were studied for the same purpose and MFHA was chosen as it was the most sensitive of these as well as the other hydroxamic acids reported previously, The method enables rapid and reliable analysis of molybdenum at ppb lelvels in environmental matrices.     

Microdetermination of molybdenum by an automatic reaction-rate method

An automatic reaction-rate method is described for the microdetermination of molybdenum; the method is based on the hydrogen peroxide-iodide reaction which is catalyzed by molybdenum. The effect of reagent concentrations was studied and the maximum tolerable amounts of interfering ions were determined. Procedures for the determination of 0.01–0.15 μg and 0.1–1.0 μg molybdenum per milliliter are given ; 0.036–2.5 μg of molybdenum could be determined with relative errors of about 2%.     

Speciation, liquid-liquid extraction, sequential separation, preconcentration, transport and ICP-AES determination of Cr(III), Mo(VI) and W(VI) with calix-crown hydroxamic acid in high purity grade materials and environmental samples

A new functionalized calix[6]crown hydroxamic acid is reported for the speciation, liquid-liquid extraction, sequential separation and trace determination of Cr(III), Mo(VI) and W(VI). Chromium(III), molybdenum(VI) and tungsten(VI) are extracted at pH 4.5, 1.5 M HCl and 6.0 M HCl, respectively with calixcrown hydroxamic acid (37,38,39,40,41,42-hexahydroxy7,25,31-calix[6]crown hydroxamic acid) in chloroform in presence of large number of cations and anions. The extraction mechanism is investigated. The various extraction parameters, appropriate pH/M HCl, choice of solvent, effect of the reagent concentration, temperature and distribution constant have been studied. The speciation, preconcentration and kinetic of transport has been investigated. The maximum transport is observed 35, 45 and 30 min for chromium(III), molybdenum(VI) and tungsten(IV), respectively. For trace determination the extracts were directly inserted into the plasma for inductively coupled plasma atomic emission spectrometry, ICP-AES, measurements of chromium, molybdenum and tungsten which increase the sensitivity by 30-fold, with detection limits of 3 ng ml⁻¹. The method is applied for the determination of chromium, molybdenum and tungsten in high purity grade ores, biological and environmental samples. The chromium was recovered from the effluent of electroplating industries.     

Direct gravimetric determination of molybdenum(VI) in presence of other ions and its application to alloy steel

N-o-Toluoyl-N-o-tolylhydroxylamine has been synthesized and employed successfully as a gravimetric reagent for direct determination of molybdenum(VI). The dried complex (110-120 degrees ) has definite composition, MoO(2)(C(15)H(14)O(2)N)(2). The method is quite simple, rapid, sensitive and gives reproducible results. The precipitation is quantitative at room temperature over a wide range of acidity. The reagent is highly selective and the method is satisfactory for analysing alloy steels.