scholarly journals Fast Analysis of Water Samples for Trace Amount of Crystal Violet Dye Based on Solid Phase Extraction Using Nanoporous SBA-3 prior to Determination by Fiber Optic-Linear Array Detection Spectrophotometry

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Azam Azarkohan ◽  
Farzaneh Shemirani ◽  
Mahrouz Alvand
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Crystal Violet ◽  
Water Samples ◽  
Fiber Optic ◽  
Linear Array ◽  
Solid Phase ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Array Detection

A solid phase preconcentration procedure using SBA-3 nanosorbent for the fast separation and preconcentration of crystal violet (CV) in water samples by fiber optic-linear array detection spectrophotometry (FO-LADS) is presented. Experimental parameters including pH, sample volume, amount of sorbent, type, volume, and concentration of eluent that affect the recovery of crystal violet have been optimized. Under optimized experimental conditions, analytical parameters including limit of detection, linear working range, and relative standard deviation have also been determined. A preconcentration factor of 200 was achieved in this method. In the initial solution, the detection limit for CV was found as 1.3 μg L−1. Under optimal conditions maximum adsorption capacity was obtained as 344.83 mg g−1. Also, the relative standard deviation was less than ±1.3% (n=5). The presented procedure was applied to the determination of crystal violet in water samples (fish, fish farming water, and river water) with good results.

scholarly journals Determination of Bentazone in Waters by Solid-Phase Spectrofluorimetry

1996 ◽  
Vol 79 (2) ◽  
pp. 567-570 ◽  
Author(s):  
José Luis Vilchez ◽  
Diego Torres-Bustos ◽  
Rosario Blanc ◽  
Alberto Navalón
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Relative Standard Deviation ◽  
Natural Water ◽  
Water Samples ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Relative Standard ◽  
Sensitive Method

Abstract A sensitive method for determining trace amounts of bentazone was developed. The method is based on solid-phase spectrofluorimetry. Bentazone was fixed on a dextran-type anion-exchange gel, and the fluorescence of the gel, packed in a 1 mm thick quartz cell, was measured directly at an excitation wavelength of 338 nm and an emission wavelength of 436 nm by using a solid-phase attachment. The applicable concentration range was 2.0–120.0 μg/L, with a detection limit of 0.4 μg/L. The relative standard deviation at the 30.0 μg/L level was 1.2%. The method was used to determine bentazone in natural water samples. Recoveries were 96.0–102.5%.

scholarly journals Determination of Clopidol Residues in Chicken Tissues by Liquid Chromatography: Collaborative Study

2003 ◽  
Vol 86 (4) ◽  
pp. 685-693 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Solid Phase ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Method Performance ◽  
Chicken Muscle ◽  
Relative Standard

Abstract Eighteen laboratories participated in a collaborative study on the determination of clopidol residues in chicken muscle tissues by liquid chromatography. Of these, results from 16 laboratories which rigorously followed the method were subjected to statistical analysis. The method performance was assessed by all participants using 14 samples of chicken muscle fortified at concentrations ranging from 0.1 to 5.0 mg/kg. In addition, 9 participants each reported results for 6 clopidol-incurred samples in chicken muscle. Test portions were extracted with acetonitrile, and the extracts were purified with alumina and anion exchange resin solid-phase extraction cartridges in sequence. Clopidol was separated by reversed-phase liquid chromatography and quantified at 270 nm. Average recoveries ranged from 81.8 to 85.4%, reproducibility relative standard deviation (RSDR) ranged from 11.9 to 22.6%, and repeatability relative standard deviation (RSDr) ranged from 9.9 to 15.1%. For clopidol-incurred samples at concentrations of 0.100–0.687 mg/kg, the mean determination value range was 0.099–0.659 mg/kg; RSDR was 12.6–19.8%, RSDr was 3.1–8.5%; and HORRAT values were 0.7–1.1. The accuracy and precision of the method are in conformity with the requirements specified by AOAC INTERNATIONAL. The method was adopted Official First Action in April 2003.

Preparation of Adsorbents Based on Dendrimer Modified Silica Gel and its Adsorption Performances for Lead

2013 ◽  
Vol 800 ◽  
pp. 166-172
Author(s):  
Xiong Zhi Wu ◽  
Li Li ◽  
Fei Ping Li ◽  
Wen Ying Jin
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Silica Gel ◽  
Limit Of Detection ◽  
Modified Silica ◽  
Modified Silica Gel ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Separation And Preconcentration

A new sorbent (PAMAM4.0GASG) with gallic acid as functional group has been prepared based on G4.0 polyamidoamine dendrimer modified silica gel (PAMAM4.0SG) and characterized with FTIR. It was employed for selective separation, preconcentration and determination of lead in different samples by flame atomic absorption spectrometry (FAAS). Experimental conditions for effective separation and preconcentration of lead were optimized. The preconcentration factor reaches 200 for lead. The relative standard deviation (R.S.D.) under optimum conditions was 2.1% for 5.0 μg ml1 of Pb (II).The relative standard deviation (R.S.D.) was 2.1% for 5.0 μg ml1 of Pb (II). The limit of detection (LOD) of 0.081μg ml1 was achieved with a sample loading flow rate of 4.2 ml min1 and a 10 ml sample volume in the proposed method. The proposed column enrichment method was applied for the preconcentration/separation and determination of Pb (II) in tap water and river water samples successfully.

scholarly journals On the potential of 2-D-Video Disdrometer technique to measure micro physical parameters of solid precipitation

2015 ◽  
Vol 8 (3) ◽  
pp. 3087-3120
Author(s):  
F. Bernauer ◽  
K. Hürkamp ◽  
W. Rühm ◽  
J. Tschiersch
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Shape Parameter ◽  
Solid Phase ◽  
Shape Descriptors ◽  
Phase Precipitation ◽  
Detailed Characterization ◽  
Matching Algorithm ◽  
Solid Precipitation ◽  
Relative Standard

Abstract. Detailed characterization and classification of precipitation is an important task in atmospheric research. Line scanning 2-D-video disdrometer technique is well established for rain observations. The two orthogonal views taken of each hydrometeor passing the sensitive area of the instrument qualify this technique especially for detailed characterization of non symmetric solid hydrometeors. However, in case of solid precipitation problems related to the matching algorithm have to be considered and the user must be aware of the limited spacial resolution when size and shape descriptors are analyzed. This work has the aim of clarifying the potential of 2-D-video disdrometer technique in deriving size, velocity and shape parameters from single recorded pictures. The need of implementing a matching algorithm suitable for mixed and solid phase precipitation is highlighted as an essential step in data evaluation. For this purpose simple reproducible experiments with solid steel spheres and irregularly shaped styrofoam particles are conducted. Self-consistency of shape parameter measurements is tested in 40 cases of real snow fall. As result it was found, that reliable size and shape characterization with a relative standard deviation of less than 5% is only possible for particles larger than 1 mm. For particles between 0.5 and 1.0 mm the relative standard deviation can grow up to 22% for the volume, 17% for size parameters and 14% for shape descriptors. Testing the adapted matching algorithm with a reproducible experiment with styrofoam particles a mismatch probability of less than 2.5% was found. For shape parameter measurements in case of real solid phase precipitation the 2DVD shows self-consistent behavior.

scholarly journals Multiresidue Determination of Pesticides in Drinking and Related Waters by Solid-Phase Extraction and Liquid Chromatography with Ultraviolet Detection: Interlaboratory Study

2002 ◽  
Vol 85 (2) ◽  
pp. 375-383 ◽  
Author(s):  
François van Hoof ◽  
Peter van Wiele ◽  
Françoise Acobas ◽  
Jean-Luc Guinamant ◽  
Auguste Bruchet ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Solid Phase Extraction ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tap Water ◽  
Phase Extraction ◽  
Relative Standard ◽  
Styrene Divinylbenzene

Abstract As part of a project funded by the European Commission (EC) for the development and evaluation of multiresidue methods for analysis of drinking and related waters, 17 European laboratories evaluated a method using styrene–divinylbenzene copolymer solid-phase extraction followed by liquid chromatography with diode array detection. The main aim of the study was to evaluate whether the method meets the requirements of EC Drinking Water Directive 98/83 in terms of accuracy, precision, and detection limit for 21 pesticides according to the following requirements: limit of detection, ≤0.025 μg/L; accuracy expressed as recovery, between 75 and 125%; and precision expressed as repeatability relative standard deviation of the method, <12.5%, and as reproducibility relative standard deviation of the method, <25%. Analyses for unknown concentrations were performed with commercial bottled and tap waters. All laboratories were able to achieve detection limits of 0.01 μg/L for all pesticides except pirimicarb (0.02 μg/L). The criteria for repeatability were met for all compounds. Terbutryn in bottled water and carbendazim in tap water did not meet the criteria for reproducibility. In terms of accuracy, the method met the requirements for all pesticides in both matrixes, except for metamitron. However, several compounds (linuron, terbutryn, propazine, metobromuron, and isoproturon) showed recoveries slightly below 75%.

scholarly journals A sensitive and specific solid-phase extraction–gas chromatography–tandem mass spectrometry method for the determination of 11 haloacetic acids in aqueous samples

2018 ◽  
Vol 24 (5) ◽  
pp. 375-383 ◽  
Author(s):  
Aziz Kinani ◽  
Jérôme Olivier ◽  
Adrien Roumiguières ◽  
Stéphane Bouchonnet ◽  
Said Kinani
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Standard Deviation ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
Solid Phase ◽  
Haloacetic Acids ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Relative Standard

A method for the analysis of 11 haloacetic acids in water samples has been developed. It involves enrichment of the target analytes from water samples by solid-phase extraction, derivatization to methyl esters, and gas chromatography coupled with tandem mass spectrometry determination. Gas chromatography conditions were optimized for a good separation of all haloacetic acids in a short runtime. Data were acquired in the multiple reaction monitoring mode. Six solid-phase extraction sorbents among the most widely used in environmental analysis were tested. Bakerbond SDB was retained because it has been shown to provide the best results for a large class of targeted haloacetic acids. The performances of the developed method have been assessed according to the French Standard NF T 90-210. The calibration curves for all the studied haloacetic acids had consistent slopes with r2 values > 0.99. Quantification limits between 0.01 and 0.50 µg l−1 were achieved. Satisfactory repeatability (relative standard deviation ≤ 14.3%) and intermediate precision (relative standard deviation ≤ 15.7%) were obtained. Applied to the analysis of 15 untreated water samples collected from three rivers, the method allowed the detection of five haloacetic acids including monochloroacetic acid (in 100% of the samples, <0.5–1.85 µg l−1), dichloroacetic acid (87%, <0.05–0.22 µg l−1), trichloroacetic acid (93%, <0.05–0.52 µg l−1), dibromoacetic acid (53%, <0.01–0.40 µg l−1), tribromoacetic acid (20%, <0.05–0.14 µg l−1), and bromodichloroacetic acid (6%, < 0.05 µg l−1).

scholarly journals Using nanometer TiO2 modified with cetyl trimethyl ammonium bromide for separation and preconcentration of Parathion in water sample

2016 ◽  
Vol 17 (2) ◽  
pp. 362-371
Author(s):  
Haghighe Fathi ◽  
Robab Soltani-Jigheh ◽  
Saeed Hemmati
Keyword(s):  
Water Samples ◽  
Cetyl Trimethyl Ammonium Bromide ◽  
Solid Phase ◽  
Environmental Water ◽  
Sample Volume ◽  
Ammonium Bromide ◽  
Base Line ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Cetyl Trimethyl Ammonium

In this work, nanometer TiO2 modified by cetyl trimethyl ammonium bromide (CTAB) was used as adsorbent for solid-phase extraction (SPE) of Parathion in environmental water samples. Adsorbed Parathion was then desorbed with different eluents and determined by gas chromatography (GC)/flame ionization detection. Greater selectivity, resolution, and sensitivity have been seen by GC compared with other methods. Parameters that might influence the extraction efficiency, such as the eluent type and its volume, adsorbent amount, sample volume, sample pH and sample flow rate, were optimized. Under the optimized extraction conditions with toluene as the eluent, the experimental results showed the excellent linearity of Parathion (R2 &gt; 0.99) over the range of 0.01–0.8 μg/mL, and the relative standard deviation was 6.3% (n = 5). The detection limit of the proposed method could reach 0.024 ng/mL based on the ratio of chromatographic signal to base line noise (S/N = 3). Recovery of 93% was achieved with spiked water samples. The method was successfully applied to the analysis of surface water samples.

scholarly journals Interlaboratory Study of a Multiresidue Gas Chromatographic Method for Determination of Organochlorine and Pyrethroid Pesticides and Polychlorobiphenyls in Milk, Fish, Eggs, and Beef Fat

2002 ◽  
Vol 85 (6) ◽  
pp. 1398-1409 ◽  
Author(s):  
François Bordet ◽  
Dary Inthavong ◽  
Jean-Marc Fremy ◽  
D Aspe ◽  
T Durand ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Solid Phase ◽  
Food Samples ◽  
Interlaboratory Study ◽  
Electron Capture Detection ◽  
Precision Data ◽  
Relative Standard ◽  
Pyrethroid Pesticides

Abstract An interlaboratory study was conducted to validate a gas chromatographic (GC) method for determination of 21 organochlorine pesticides, 6 pyrethroid pesticides, and 7 polychlorobiphenyl (PCB) congeners in milk, beef fat, fish, and eggs. The method was performed at low contamination levels, which represent relevant contents in food, and is an extension of the European standard (method NF-EN-1528, Parts 1–4). It enlarges the applicable scope of the reference EN method to pyrethroid pesticides and proposes the use of solid-phase extraction (SPE) as a cleanup procedure. Cryogenic extraction was made, and SPE cleanup was performed with 2 successive SPE cartridges: C18 and Florisil®. After injection of the purified extract onto a GC column, residues were measured by electron capture detection. Food samples (liquid milk, beef fat, mixed fish, and mixed eggs) were prepared, tested for homogeneity, and sent to 17 laboratories in France. Test portions were spiked with 27 pesticides and 7 PCBs at levels from 26 to 45, 4 to 27, 31 to 67, and 19 to 127 ng/g into milk, eggs, fish, and fat, respectively. Based on results for spiked samples, the relative standard deviation for repeatability ranged from 1.5 to 6.8% in milk, 3 to 39% in eggs, 4.5 to 12.2% in fish, and 7 to 13% in fat. The relative standard deviation for reproducibility ranged from 33 to 50% in milk, 29 to 59% in eggs, 31 to 57% in fish, and 30 to 62% in fat. This method showed acceptable intra- and interlaboratory precision data, as corroborated by HORRAT values at low levels of pesticide and PCB contamination. The statistical evaluation of the results was performed according to the International Organization for Standardization (ISO; ISO 3534 standard) and 5725-2 Guideline.

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