Andriana Surleva

A modified ninhydrin micro-assay for determination of total cyanogens in plants.

Indirect quantification of total cyanogenic compounds (cyanogens) in plants was studied using a novel ninhydrin-based spectrophotometric micromethod. The ninhydrin-cyanide system obeys Beers law in the range from 20 μg L(-1) to 800 μg L(-1) CN(-) with molar absorptivity ε=1.4×10(5) L mol(-1)cm(-1). Recovery at 100 μg L(-1) CN(-) was 100.5±0.1% and LOD and LOQ were 8 and 22 μg L(-1), respectively. The conditions for ninhydrin reagent preparation were discussed. The extraction and separation solutions, extraction and incubation time, and solvent volume were also investigated for maximum recovery of total cyanogens. 0.1% NaHCO3 was used as an extraction solvent for cyanide formed after enzymatic hydrolysis of cyanogens. The procedure was suitable for samples containing more than 90 mg CN(-)/100 g sample. When cyanogen concentrations were lower, the resulted cyanide was separated by microdiffusion in a Conway cell. Water was used as a hydrolysis medium and a donor solvent, while 2% Na2CO3 as an absorbing solution. Total cyanogen content in plum and almond kernels, as well as apple and flax seeds was determined.

A new generation of cyanide ion-selective membranes for flow injection application: Part III. A simple approach to the determination of toxic metal-cyanide complexes without preliminary separation.

A new flow injection approach to total weak acid-dissociable (WAD) metal-cyanide complexes is proposed, which eliminates the need of a separation step (such as gas diffusion or pervaporation) prior to the detection. The cornerstone of the new methodology is based on the highly selective flow-injection potentiometric detection (FIPD) system that makes use of thin-layer electroplated silver chalcogenide ion-selective membranes of non-trivial composition and surface morphology: Ag(2+delta)Se(1-x)Te(x) and Ag(2+delta)Se. An inherent feature of the FIP-detectors is their specific response to the sum of simple CN(-)+Zn(CN)(4)(2-)+Cd(CN)(4)(2-). For total WAD cyanide determination, ligand exchange (LE) and a newly developed electrochemical pre-treatment procedure for release of the bound cyanide were used. The LE pre-treatment ensures complete recovery only when the sample does not contain Hg(CN)(4)(2-). This limitation is overcome by implementing electrochemical pre-treatment which liberates completely the bound WAD cyanide through cathodic reduction of the complexed metal ions. A complete recovery of toxic WAD cyanide is achieved in the concentration range from 156 microg L(-1) up to 13 mg L(-1). A three-step protocol for individual and group WAD cyanide speciation is proposed for the first time. The speciation protocol comprises three successive measurements: (i) of non-treated, (ii) LE-exchange pre-treated; (iii) electrochemically pre-treated sample. In the presence of all WAD complexes this procedure provides complete recovery of the total bound cyanide along with its quantitative differentiation into the following groups: (1) Hg(CN)(4)(2-); (2) CN(-)+Cd(CN)(4)(2-)+Zn(CN)(4)(2-); (3) Cu(CN)(4)(3-)+Ni(CN)(4)(2-)+Ag(CN)(2)(-). The presence of a 100-fold excess in total of the following ions: CO(3)(2-), SCN(-), NH(4)(+), SO(4)(2-) and Cl(-) does not interferes. Thus the proposed approach offers a step ahead to meeting the ever increasing demand for cyanide-species-specific methods. The equipment simplicity makes the procedure a good candidate for implementing in portable devices for in-field cyanide monitoring.

Ninhydrin-based spectrophotometric assays of trace cyanide

Abstract The extreme toxicity of cyanide, its wide industrial application as well as its continued illegal use generate research interest in different fields of science, imposing multidisciplinary approach to study cyanide poisoning. We show here that the reaction between cyanide and ninhydrin can be performed at ambient conditions; however, the ninhydrin reagent has to be freshly prepared in oxygen free solvent. Besides, we show that the reading of the absorbance at 485 nm might be more suitable and reliable than that at 590 nm, where the pH-dependent blue colored cyanide-ninhydrin adduct is less stable. Ninhydrin-based color reagent can be used to quantify the cyanide released from plant seeds. In sodium carbonate medium, the proposed assay is fast, cheap and environmentally friendly

Evaluation of ICP-OES Method for Heavy Metal and Metalloids Determination in Sterile Dump Material

This study is aimed at development of an analytical method for the determination of heavy metals and arsenicin waste material from barite recovery by dual view inductively coupled plasma optical emission spectrometry (ICP-OES) after wet digestion. Aquaregia open digestion method was used for sample preparation. A soil certified reference material was used to study the efficiency of wet digestion procedure applied to sterile dump material. The sensitivity, accuracy, and precision of the method were determined. The achieved detection limits are: Arsenic (As) 0.80; Copper (Cu) 0.29; Lead (Pb) 0.29; Zink (Zn) 0.30; Cadmium (Cd) 0.11; Chromium (Cr) 0.09; Nickel (Ni) 0.02, mg.kg-1.The developed method is applied for the determination of hazardous metals and arsenic in sterile dump material from closed barite mine in the region of Tarnita-Suceava, Romania.

Contribution to Casein Determination by UV Spectrophotometry

Abstract In the present paper, the interaction between copper ions and proteins is presented, in order to elaborate a simple and rapid spectrophotometric assay of casein in milk. Under alkaline conditions, copper ions form the biuret complex with the proteins, which can be used in protein determination. Although very specific, the biuret method is less sensitive. Using insoluble copper phosphate, casein is able to extract copper ions, with which it forms the biuret complex, while either the complex or copper ions could be determined in the ultraviolet range. Indeed, an increased absorbance of biuret complex at 215 nm was found. Nevertheless, copper ions can be determined in UV as well, their concentration being proportional to that of casein. When used tetraglycine instead casein, mass spectrometric measurements at pH higher than 11 revealed the formation of complexes with many copper ions bound to each peptide bond-containing molecule. Nevertheless, on diluting the biuret solution the complex may dissociate leading to very complex UV spectra that should be further studied.

Manufacturing parameters influencing fire resistance of geopolymers: A review

Geopolymers exhibit various unique properties and characteristics, including high compressive strength, high temperature stability, and low thermal conductivity. As a relatively new and perspective material, the behavior of geopolymers subjected to high temperatures is being intensively studied nowadays. This review summarizes the recent achievements in the development of geopolymer-based fire resistance materials. Technological parameters, which influence thermal behavior of geopolymer-based materials, are also discussed. Besides that, recent applications of geopolymers according to their composition are presented.

Improved ninhydrin-based reagent for spectrophotometric determination of ppb levels of cyanide

ABSTRACT Cyanide is an extremely severe poison that has been raising concerns and controversies regarding its toxic effects on humans and the environment. A short-term human exposure to elevated levels can induce coma or death. Toxic effects occur at blood cyanide concentrations of 0.05 mg/dL, while death can occur at levels of 0.3 mg/dL. Numerous law and systems regulate cyanide levels in various environments. To exemplify, the maximum contamination limit imposed by United States Environmental Protection Agency in drinking water is 200 µg/L, while the European Union presents a lower limit of 50 µg/L. Ninhydrin has proved to be an effective color reagent for the spectrophotometric determination of trace levels of cyanide. This article reports a ninhydrin-based color reagent that was employed in cyanide determination involving real samples of water, cigarette smoke, urine, and cyanogenic plants, achieving an appropriate sample pretreatment procedure for cyanide liberation and separation. The reaction between cyanide and ninhydrin is fast enough to be performed at ambient conditions, but the ninhydrin reagent must be freshly prepared in oxygen-free solvent. Beers law is obeyed in the range between 20 and 400 ppb CN− (r = 0.992; N = 7) with molar absorptivity of 1.4 × 105 L mol−1 cm−1 and limit of detection of 8 ppb cyanide. Recovery at 100 ppb CN− was (100.5 ± 0.1) %, whereas precision was 1.7%. Also, absorbance at 485 nm proved to be temperature-dependent, with a maximum at ambient conditions. Throughout all measurements, the ninhydrin-based assay proved to be reliable, economical and environmentally friendly. Significance of the assay for the determination of cyanide in the field of environmental forensics, as well as its potential aid in elucidating incidents with legal consequences are highlighted.

Spectrophotometric study of competitive complexation equilibria involving overlapped spectral responding species: Determination of the stability constant of bismuth-pyrophosphate complex

AbstractSpectrophotometric study of competitive complex formation equilibria involving overlapped spectral responding species applying a simple and versatile algorithm was carried out. The algorithm involves multivariable regression for calculation of equilibrium concentrations from multiwavelength data and mass action law for the stability constant calculation. The used regression functions are part of common statistical software. Stability constants and complex stoichiometry of competing equilibria were simultaneously determined. The species concentration profiles at several spectral overlapping and α-coefficient of competing reaction were obtained. Non-absorbing bismuth — pyrophosphate (PPh) system was studied as a competitive reaction of bismuth — 4-(2-Pyridylazo) resorcinol (PAR) complex. The formation of Bi-PPh complex with 1:1 stoichiometry was proved in the studied concentration region (CBi = 1×10−5 mol L−1; CPPh = 5×10−6 − 1×10−4 mol L−1). The stability constant of the complex at pH 1 and µ = 1.0 have been determined: logβ = 4.2±0.2.