Search results for "Calibration curve"

The Fractal Approach to Secondary Mechanisms in SEC

2007

Abstract Size‐exclusion chromatography (SEC) is one of the most used experimental techniques to characterize polymers in solution; it has been applied to interpret the elution behaviour of many polymer‐solvent systems in five types of column packings. The experimental data have revealed that the classical universal calibration is not accomplished. Deviations from a unique curve are a consequence of two effects: entropic (exclusion by size) and enthalpic (binary and ternary interactions between solvent, polymer, and gel), which results in secondary mechanisms accompanying the main “ideal” SEC separation mechanism. Therefore, three approaches of building a calibration curve have been compared…

Solution properties of polyelectrolytes

1991

Abstract Chromatographic data for sodium polystyrene sulphonate were obtained on both silica- and polymer-based size-exclusion supports using mobile phases of various pH and ionic strength. Deviations of the elution volume were observed towards both lower and higher values relative to the reference calibration graph obtained with uncharged standards. An empirical correlation is proposed in order to account for all the secondary effects observed. The general applicability of this correlation was further tested for chromatographic data obtained for a series of peptides and proteins on a silica-based support under very different eluent conditions. Deviations from ideal elution behaviour such a…

Flow-injection spectrophotometric determination of amino acids based on an immobilised copper(II) -zincon system

1993

Abstract The flow-injection spectrophotometric determination of different amino acids was carried out by reaction with copper(II) ions entrapped in a polymeric material and filling a packed-bed reactor; the released copper(II), complexed with the amino acid, reacted with zincon in a basic medium producing a blue colour that was monitored at 600 nm. The method was applied to determine the contents of different amino acids in pharmaceutical formulations. The calibration graph for glycine was linear over the range 0.5–20 μg ml −1 with a relative standard deviation of 0.8% ( n = 6) at 10 μg ml −1 and a sample throughput of 108 h −1 .

The fractal calibration method applied to the characterization of polymers in solvent mixtures and in mixed gel packings by SEC.

2007

The size-exclusion chromatographic (SEC) behaviour of different solvent/polymer systems in three packing sets has been analysed from fractal considerations. The three-column sets studied are specifically formed by: (i) 'pure' micro-styragel, (ii) 'mixed' TSK Gel H(HR + XL + HR) and (iii) mixed TSK Gel H(XL + HR + XL). The experimental data reveals that in most of the systems assayed the classical universal calibration (UC) is not fulfilled, denoting the existence of secondary effects accompanying the main SEC mechanism. In order to obtain an accurate characterization of different polymers eluted in solvent mixtures and/or mixed packings, the use of a reliable and trusted calibration curve i…

1996

An iterative, approximative procedure is presented, to calibrate the determination of molar masses of polymers with gel-permeation chromatography, additionally using viscometry, and transformations, according to Benoit's concept of universal calibration, even if only polymers with broad molar mass distribution are available. The calculated (intermediate) values of the average molar masses from each step of iteration converge to final values. With at least two fractions of the polymers to be analyzed, and with measured intrinsic viscosities of the fractions, a calibration curve of gel-permeation chromatography and Mark-Houwink's constants can be determined. Assumptions for the use of the cal…

1996

Developing an artificial oxygen carrier for use in humans, we polymerize native haemoglobin and myoglobin, using bifunctional, amino group specific cross-linkers, to soluble, so-called hyperpolymers. These polymers, like other polymerized globular proteins, are members of a new class of macromolecues which consist of macromolecular base units. They all have, due to the mechanisms of the chemical reaction, broad distributions of molecular weights. Fractions of hyperpolymers of human haemoglobin were obtained by employing preparative gel-permeation (size-exclusion) chromatography. The calibration curve of analytical gel-permeation chromatography (GPC) for haemoglobin hyperpolymers was determi…

FIA-Fluorimetric assembly for the determination of noradrenaline hydrochloride by a solid-phase reactor with immobilized hexacyanoferrate(III)

1997

An FIA assembly provided with immobilized hexacyanoferrate(III) is proposed for the fluorimetric determination of noradrenaline hydrochloride. The oxidative reagent is immobilized by means of a strong anion-exchange resin. The FIA manifold is very simple and the calibration graph is linear over the range 0.5–75mgl−1 noradrenaline hydrochloride with an r.s.d of 0.88% (17 replicates) and a sample throughput of 84h−1. Foreign compounds such as NaCl, sucrose, lactose and sodium sulfate caused no significant errors. The procedure is applied to the determination of noradrenaline in a medicinal formulation.

A multiresidue analytical method for trace level determination of antibiotics and antiretroviral drugs in wastewater and surface water using SPE-LC-M…

2016

An analytical method for simultaneous determination of seven commonly used antibiotics and three antiretrovirals in surface water and urban wastewater at the ng L−1 level has been developed. The method involves concentration and clean-up by solid phase extraction (SPE) followed by identification and quantification by liquid chromatography tandem mass spectrometry (LC-ESI-MS/MS). The use of matrix-matched calibration curves constructed by spiking surface water was evaluated for quantification and compared with the internal standard method using isotopically labelled compounds. The method gave absolute recoveries of 41–116% with most of the compounds having recoveries >50%. The LOQs ranged fr…

Dating archaeological copper/bronze artifacts by using the voltammetry of microparticles.

2014

A method for dating copper/bronze archaeological objects aged in atmospheric environments is proposed based on the specific signals for cuprite and tenorite corrosion products measured through the voltammtry of microparticles method. The tenorite/cuprite ratio increased with the corrosion time and fitted to a potential law that yielded a calibration curve usable for dating purposes.