Spectrophotometric study of a direct determination of serum calcium

A modification of a direct manual procedure for serum calcium has been developed in which a one-piece color reagent is used. When a micro amount of serum is added to the reagent, rapid and stable color formation occurs enabling the procedure to serve either as a manual stat system of in robotized automatic instrumentation. Total color measurement is not attained in such a procedure owing to the described regressive nature of the reagent blank. However, accurate and linear reaction characteristics are effectively achieved. The use of a low dielectric solvent, EG, served well for repressing the ionization of the blank while allowing linear and reproducible calibration characteristics.     

Comparative chromogenicities and discrepant spectra obtained between a heterogeneous and homogeneous Zimmermann reaction

A spectrophotometric study is shown for two modifications of a 17-KS procedure in which nearly all aqueous reaction media were used. Although the apparent differences in matrices of reaction between the two procedures appear to be minute, a small volume of ethanol for one is substituted for the same volume of methanol in the other, the final alkalinity of the latter procedure is stronger, and the reaction temperature was increased, wide differences in spectral results are found between the two methods. The ethanolic, lower alkalinity procedure is a homogeneous, single-phase reaction while the methanolic, higher-alkalinity procedure is a heterogeneous system in which a precipitation of detergent occurs and the precipitate becomes an integral part of the color reaction. The rate of formation of the ethanolic procedure is variable for the different 17-KS but it is constant in the methanolic procedure. The chromogenicities of color formation between the two procedures differ in that the methanolic system provides uniform and predictable spectra with more equivalent molar absorptivities. Lastly, the methanolic system shows a much greater sensitivity owing, apparently, to a more complete final reaction. This inability to form full color for several compounds in the homogeneous system can be related in some way to the large variations in ability to form that color owing to matrix composition.     

Quantitative Determination of Phthalides in Molecules of Vinyl Polymers and Their Role in Radical Polymerization

The applicability to vinyl polymers of the procedure for quantitative determination of phthalide groups in polymeric molecules from the color of their sulfuric acid solutions was examined. The correlation between the intensity of the color of sulfuric acid solutions of polymers (polymethyl methacrylate, polystyrene) and the content of phthalide fragments incorporated into the polymer molecule was studied systematically on a quantitative level.     

Application of HPTLC Multiwavelength Imaging and Color Scale Fingerprinting Approach Combined with Multivariate Chemometric Methods for Medicinal Plant Clustering According to Their Species

In the current study, multiwavelength detection combined with color scales HPTLC fingerprinting procedure and chemometric approach were applied for direct clustering of a set of medicinal plants with different geographical growing areas. The fingerprints profiles of the hydroalcoholic extracts obtained after single and double development and detection under 254 nm and 365 nm, before and after selective spraying with specific derivatization reagents were evaluated by chemometric approaches. Principal component analysis (PCA) with factor analysis (FA) methods were used to reveal the contribution of red (R), green (G), blue (B) and, respectively, gray (K) color scale fingerprints to HPTLC classification of the analyzed samples. Hierarchical cluster analysis (HCA) was used to classify the medicinal plants based on measure of similarity of color scale fingerprint patterns. The 1-Pearson distance measurement with Ward’s amalgamation procedure proved to be the most convenient approach for the correct clustering of samples. Data from color scale fingerprints obtained for double development procedure and multiple visualization modes combined with appropriate chemometric methods proved to detect the similar medicinal plant extracts even though they are from different geographical regions, have different storage conditions and no specific markers are individually extracted. This approach could be proposed as a promising tool for authentication and identification studies of plant materials based on HPTLC fingerprinting analysis.     

Microchemical urinalysis: IX. Determination of hydroxyproline in urine

A simplified procedure is described for the determination of hydroxyproline in human or monkey urine. In this procedure I ml of urine is subjected in succession to hydrolysis, oxidation, extraction and color development. During these steps impurities and interfering substances are eliminated, thus resulting in a chromophore due to hydroxyproline alone. Thirty-five urine samples can be analyzed in one working day.     

Periodate oxidation analysis of carbohydrates : Part I. Spectrophotometr1c determination of glyoxal in dialdehyde fragments formed from glycosides with 2,4-dinitrophenylhydrazine

A simple procedure for the determination of glyoxal in dialdehyde fragments, formed from glycosides by periodate oxidation, is proposed. By heating sample solutions prepared by dilution of reaction mixtures for periodate oxidation, with an aqueous dimethylsulfoxide solution of 2,4-dinitrophenylhydrazine hydrochloride. followed by addition of an aqueous ethanolic solution of potassium hydroxide, intense color with an absorption maximum at 576 nm developed. The spectrophotoinetric method based on this color reaction makes it possible to determine selectively 1·10^?2–2·10^?1 μmole amounts of conjugated glyoxal without a prior liberation process. Data for glyoxal content obtained by this procedure are discussed in relation to overoxidation.     

A new procedure for fast soft staining of BN‐PAGEs on photosynthetic complexes

We report a fast and sensitive procedure for blue native PAGE staining, in which the conventional staining step with CBB is avoided. After running, a short exposure to a mix of polar protic solvents (ethanol and acetic acid) leads to a fast and selective removal of the dye from the migration front and a specific binding to the protein bands, while the rest undergo a selective and complete background removal, leading to an intense contrast. This single‐step staining–destaining technique is useful in protein samples that bind colored cofactors such as photosystems, which can be selectively discerned by their characteristic green color. After the staining of such samples, the green color persists, while the other unpigmented protein complexes and the molecular standard remain CBB stained, creating a useful reference system for the assignment of the bands. The advantages and chemical basis of this staining procedure are discussed.     

Microdetermination of magnesium in biological fluids

A modified procedure for the spectrophotometric determination of serum magnesium is described in which a direct addition of serum is made to a two-piece color reagent system. One solution contains an optimized concentration of the color reagent Magon, 1-azo-2-hydroxy-3-2-(2,4-dimethylcarboxanilido)-naphthalene-1′-(2-hydroxybenzene-5-sulfonate) sodium salt, in a dimethyl sulfoxide medium for binding magnesium and also EGTA, ethylene-bis(oxyethylenenitrilo)-tetraacetic acid, for binding calcium. The other is an alkaline solution of dilute cyanide to bind copper and iron and provide the optimum reaction pH. By means of these ingredients the simple procedure involves a reaction with serum magnesium while masking the interference of calcium and trace metals and allowing the reaction to take place without either separation or deproteinization steps. Optimized characteristics are shown for a linear reaction involving a variable reaction blank in the procedure where calcium is measured against a blank that is constant in its makeup. The linearity of the procedural reagent blank, with respect to its own concentration, helps attain the required linear results for the overall system and this is described by spectral studies.     

A Test Method for the Determination of Mercury(I, II) on a Polymer Surface

It was found that mercury(I, II) reacts with 5-chloro-2-hydroxy-3-[(tetrahydro-2,4-dithioxo-1,3-thiazin-5-yl)azo]benzenesulphonic acid (tyrodine) in weakly acid solutions in the presence of acetates, formates, and some organic solvents (ethanol and acetone) to give an intensely colored insoluble compound (_max = 600 nm, > 3 × 10⁴). The composition of the solution affected the sensitivity of the color reaction between mercury and tyrodine. A test procedure was developed for the determination of mercury(I, II) on the surface of a polycaproamide membrane with a detection limit of <50 ng in the adsorbent zone. The procedure involves the quantitative and selective adsorption of the mercury complex of tyrodine on the support surface from 0.5 M acetate solutions of pH 3–4 in the dynamic mode; the sample volume was 5–25 mL. Mercury was then determined by the change in the support color using a color scale or by the change in diffuse reflectance at 600 nm. The adsorption of the mercury complex was accompanied by an abrupt change in the color of the support surface from pale crimson (reagent) to stable blue-violet. The test procedure was used in the analysis of an industrial sample of complex composition with a mercury concentration of lower than 0.05%. The determination error (relative standard deviation) was 20%.     

阳离子交换树脂分离-铝试剂分光光度法测定土壤中铝形态

研究了铝试剂光度法测定土壤溶液中铝的最佳条件,着重探讨了共存离子,特别是土壤溶液中的无机离子和有机阴离子对测定铝的影响。采用阳离子交换树脂分离,建立了测定土壤溶液及天然水中铝形态方法。用该法可测定总反应性铝、总单核铝和稳定性单核铝。由总反应性铝减去总单核铝求得酸溶性铝。由总单核铝减去稳定单核铝求得不稳定单核铝。与阳离子树脂交换分离-邻苯二酚紫光度法进行了比较。结果表明：邻苯二酚紫光度法灵敏度较高,但铁的干扰较大。铝试剂光度法灵敏度略低,但铁的干扰较少。阳离子树脂交换分离-铝试剂光度法更适合于测定含铁量比较高的土壤溶液中的铝形态。     

Photometric Determination of N-Phenyl-Substituted Monomaleimides as Aci Forms of Their Nitro Compounds

A procedure is developed for the photometric determination of three N-phenyl-substituted monomaleimides as aci forms of their nitro compounds obtained by preliminary hydrolysis, nitration, and subsequent interaction with alkali. As a result, an intense bright-yellow color of the reaction product is developed.     

A Sensitive Visible Spectrophotometric Method for Copper Using Bis-Substituted Thiocarbamoyl Trisulfides

Abstract

Bis-substituted thiocarbamoyl disulfides (thiuram disulfides) were investigated as chromogenic reagents for the analysis of copper in trichloroacetic acid solutions. It was found that hydrogen peroxide speeded color development, increased color stability and enhanced color intensity in a trichloroacetic acid-alcohol matrix. In the presence of hydrogen peroxide, all copper complexes had molar absorptivities exceeding 30,000. Bis-pentamethylene thiocarbamoyl disulfide was selected as the best commerically available reagent of those investigated. The procedure is almost interference free, silver and mercury being the most serious interference. The sensitivity is 6 × 10^?3 micrograms/cm².     

Polymeric materials with grafted luminescent organosiloxane coatings

A procedure was developed for preparing polymeric materials with grafted luminescence organosiloxane coatings containing conjugates of rare-earth elements with various color spectra.     

Spectrophotometric evaluation of interferences in three iron reactions for the determination of serum total cholesterol

A spectrophotometric and chemical evaluation of reported interferences for three iron reactions for the determinations of serum cholesterol has been presented. It has been shown that all three reactions are affected by various interfering substances, such as 2-thiouracil, nitrate, azide, bromide, diethylstilbesterol, and steroids. Spectral differences between the reactions are probably due to solvent and anion effects.The incorporation of uranyl acetate as a precipitating agent into the ferric acetate-uranyl acetate procedure did not make the results obtained comparable with the Abell-type extract of a very icteric serum. Incorporation of ferrous sulfate does not noticeably affect the intensity or stability of color development with standards.As proposed, the ferric acetate-uranyl acetate procedure for the determination of cholesterol represents a modified iron reagent, but the reaction mechanism and the procedure described for it is neither new nor direct. The use of the ferric acetate reagent for serum cholesterol as opposed to ferric chloride, ferric ammonium chloride, or ferric perchlorate appears to have no real advantages as a color reaction. In fact the reaction is less sensitive while reagent preparation is more tedious, time consuming, and expensive than the ferric chloride procedure. Although no quantitative studies were performed, the only effects that chloride had on the reactions were in the region of 400 nm, a wavelength sufficiently far enough away from the 560-nm peak that it did not affect determinations. The concept that the ferric acetate-uranyl acetate reagent contains only acetate and sulfate anions is nullified as soon as one adds serum to the reagents.     

Colorimetric determination of tantalum in titanium alloys

Experimental work on tantalum-titanium alloys has been handicapped by the lack of accurate methods for the determination of the tantalum. In this paper a colorimetric procedure is proposed for the determination. The tantalum is separated completely from the titanium by two tannin precipitations with an intervening digestion with tannin. The tannin precipitate is ignited, fused with potassium bisulfate and the melt taken up with ammonium oxalate solution. Pyrogallol is then added and the intensity of the yellow color is measured. A study was made of the tantalum pyrogallol color to obtain optimum conditions. Elements that would be found in the usual tantalum-titanium alloys do not interfere with the method. More than 0.0025 gram of niobium interferes by cauaing occlusion of titanium by the tannin precipitate. This causes high results for tantalum, since titanium reacts with pyrogallol to produce a yellow color. The presence of more than 0.0050 gram of tungsten causes high results for tantalum because tungsten is partially precipitated by the tannin and reacts with pyrogallol to produce a yellow color. The proposed method is recommended for tantalum-titanium alloys containing 0.05 to 5 percent, tantalum.     

Semiquantitative and Quantitative Determination of Trace Amount of Phosphate Ion in Water Using Polyurethane Foam Thin -Layer Colorimetry

Abstract

A simple, sensitive and fast method for the colorimetric determination of phosphate ion in water is described.

The method is based on spectrophotometric measurement of the blue molybdoantimony phosphoric acid species sorbed in a polyurethane foam thin-layer for quantitative determination of phosphate ion, or the visual color comparison technique for rapid semiquantitative determination.

The detection limit for the quantitative procedure is 5 μg/1 and for semiquantitative procedure 20 μg/1 for sample volumes of 100 ml and 25 ml, respectively.     

Chromatography of conjugated polymeric carbocations

The separation of a number of homo- and copolyarylenephthalides, which were converted into a colored ionized form, by adsorption chromatography using elution with 96% sulfuric acid was studied. A correlation between the color (degree of conjugation) and the adsorption ability of chromophore groups, which were formed upon the dissolution of the test compounds in H₂SO₄, was found: in the separation of a mixture of two polyarylenephthalides of the same type, a polymer whose chromophore group absorbs in the short-wave-length region of the spectrum was eluted first and the polyarylenephthalide with a deeper color was eluted next. The procedure developed allowed us to analyze the polymers in microgram amounts.     

A Selective Colorimetric Method for the Determination of Penicillins and Cephalosporins with α-Aminoacyl Functions

ABSTRACT

A simple, sensitive and selective colorimetric method is described for the assay of ampicillin, amoxicillin, cephalexin, cefadroxil and cefaclor in their pharmaceutical preparations. The method is based on measuring the color obtained when the alkaline degradation products of these agents are allowed to react with ascorbic acid. The factors affecting the color generation and determination were studied and optimized. The reaction is selective to β-lactam antibiotics having amino acid side-chains with free amino functions and thus allow interference-free quantitation of some preparations containing these agents in combination with other β-lactam agents. The procedure is also successfully adopted as stability-indicating method for cephalosporins. A tentative mechanism of the color reaction is proposed.     

Photometric Determination of Dimaleimides

A procedure was developed for the photometric determination of dimaleimides as the aci form of their nitro compounds obtained after preliminary hydrolysis, nitration, and subsequent interaction with an alkali. The resulting intense bright yellow color of the solution provides highly the sensitive determination of dimaleimides.     

Blister-colorimetric determination of phosphate ions in water,agricultural samples,and biological samples

A procedure was proposed for the determination of phosphate ions in a blister cell (pellet cartridge) with a dry reagent mixture. The procedure is suitable for the quantitative determination of phosphate in different samples using a dry reagent mixture in an ampule or a blister without dissolving the reagents. After an ampule or a blister cell was opened and several drops of a test liquid were added, a color developed, whose intensity was proportional to the concentration of phosphate ions in the solution. The solution was then diluted to 2 mL with water and analyzed by photometry. The composition of the mixture was determined, and the procedure for the quantitative determination of phosphate ions was proposed; the procedure involves the formation and reduction of phosphomolybdic acid and the use of auxiliary reagents. The error of the colorimetric determination of phosphate ions in aqueous solutions, soil extracts, and urine was estimated with the participation of inexperienced operators.