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 The Solid Phase Extraction of Some Metal Ions Using Palladium Nanoparticles Attached to Silica Gel Chemically Bonded by Silica-Bonded N-Propylmorpholine as New Sorbent prior to Their Determination by Flame Atomic Absorption Spectroscopy

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
M. Ghaedi ◽  
M. Rezakhani ◽  
S. Khodadoust ◽  
K. Niknam ◽  
M. Soylak
Keyword(s):  
Electron Microscopy ◽  
Metal Ions ◽  
Silica Gel ◽  
Solid Phase ◽  
Food Samples ◽  
Natural Food ◽  
Modified Silica Gel ◽  
Flame Atomic Absorption ◽  
Relative Standard

In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4–2.7 ng mL−1. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL−1) in different natural food samples.

scholarly journals Determination of gold, palladium and copper by flame atomic absorption spectrometry after preconcentration on silica gel modified with 3-(2-aminoethylamino)propyl group

2005 ◽  
Vol 3 (2) ◽  
pp. 252-262 ◽  
Author(s):  
Mustafa Imamoglu ◽  
Ali Aydin ◽  
Mustafa Dundar
Keyword(s):  
Silica Gel ◽  
Volume Flow Rate ◽  
Absorption Spectrometry ◽  
Rate Matrix ◽  
Modified Silica ◽  
Modified Silica Gel ◽  
Flame Atomic Absorption ◽  
Ft Ir ◽  
Preconcentration Method

AbstractA preconcentration method of gold, palladium and copper based on the sorption of Au (III), Pd (II) and Cu (II) ions on a column packed with 3-(2-aminoethylamino)propyl bonded silica gel is described. The modified silica gel was synthesized and characterized by FT-IR and C, H, N elemental analysis. At column preconcentration, the effects of parameters such as pH, volume, flow rate, matrix constituents of solutions and type of eluent on preconcentration of gold, palladium and copper were studied. The recoveries of Au (III), Pd (II) and Cu (II) were 98.93±0.51, 98.81±0.36 and 99.21±0.42 % at 95 % confidence level, respectively. The detection limits (δ) of the elements were 0.032, 0.016 and 0.012 μg ml−1, respectively. The preconcentration method was applied for determination of gold and palladium in certified reference material SARM 7B and copper in river and synthetic seawater by FAAS. Gold, palladium and copper were determined with relative error lower than 10 %.

Determination of diltiazem based on the reduction of Cu(II)–BCA complexes in micellar medium

2010 ◽  
Vol 88 (6) ◽  
pp. 533-539 ◽  
Author(s):  
Larissa Zuppardo Lacerda Sabino ◽  
Daniele Cestari Marino ◽  
Horacio Dorigan Moya
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Confidence Level ◽  
Limit Of Detection ◽  
Calibration Graph ◽  
Micellar Medium ◽  
Solution Ph ◽  
Simple Method ◽  
Relative Standard

A simple method was developed for determining microquantities of diltiazem, based on the reduction of copper(II) in buffered solution (pH 7.0) and the use of a micellar medium containing 4,4′-dicarboxy-2,2′-biquinoline acid. The copper(I) produced reacts with 4,4′-dicarboxy-2,2′-biquinoline acid and the complexes formed are spectrophotometrically measured at 558 nm. A typical calibration graph shows good linearity (r = 0.993) from 20 to 100 μg mL–1 of diltiazem. The limit of detection and relative standard deviation were calculated as 12 μg mL–1 (99% confidence level) and 3.5% (40 μg mL–1; n = 6), respectively, with a mean recovery value of 96.5% found in pharmaceutical dosages. A straightforward and effective way to recycle the reagents is addressed. The hazardous aspects of the Cu(I)–BCA reaction are presented as well.

Study on the Kinetic Spectrophotometric Determination of Selenium (IV) on Oxidation of Neutral Red with Potassium Periodate and its Application

2012 ◽  
Vol 610-613 ◽  
pp. 446-451
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Neutral Red ◽  
Optimum Conditions ◽  
Hair Samples ◽  
Relative Standard ◽  
Kinetic Spectrophotometric

Based on the oxidation of neutral red by KIO4 in 3.2×10-4 mol/L sulfuric acid solution, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of neutral red at 530 nm with a fixed-time method. The decrease in the absorbance of neutral red is proportional to the concentration of Se(IV) in the range 0.0–8.0 µg/L with a fixed time of 4–6 min from the initiation of the reaction. The limit of detection is 0.36 µg/L Se(IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 81.60 kJ/mol. The relative standard deviation for the determination of 0.1 and 0.2 µg/mL Se(IV) was 2.1 and 1.9 %, respectively. The method has been successfully applied to the determination of Se (IV) in tea and human hair samples with the relative standard deviation of 0.33 %–1.5 % and the recovery of 97.5 %–103.5 %.

Kinetic Spectrophotometric Determination of Selenium (IV) by its Catalytic Effect on the Oxidation of Acid Chrome Blue K by Hydrogen Peroxide

2012 ◽  
Vol 538-541 ◽  
pp. 2358-2363 ◽  
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang
Keyword(s):  
Hydrogen Peroxide ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Acid Chrome Blue K ◽  
Good Agreement

Based on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid solution, while 1,10-phenanthroline (phen) acts as an activator, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of ACBK at 524 nm with a fixed-time method. The decrease in the absorbance of ACBK is proportional to the concentration of Se (IV) in the range 0.06–1.0 µg/L with a fixed time of 4–10 min from the initiation of the reaction. The limit of detection is 0.018 µg/L Se (IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 62.30 kJ/mol. The relative standard deviation for 11 replicate determination of 0.01 and 0.02 µg/25mL selenium (III) was calculated to be 2.3 % and 2.0 %, respectively. Combined with sulphydryl dextrane gel (SDG) separation and enriching, the method has been successfully applied to the determination of Se (IV) in foodstuff samples with the relative standard deviation of 1.1 %–3.7 % and the recovery of 99.0 %–104.0 %, the results are in good agreement with those provided by HG-AAS method.

scholarly journals Liquid Chromatographic Method with Immunoaffinity Column Cleanup for Determination of Ochratoxin A in Barley: Collaborative Study

2000 ◽  
Vol 83 (6) ◽  
pp. 1377-1383 ◽  
Author(s):  
A Catherine Entwisle ◽  
Alison C Williams ◽  
Peter J Mann ◽  
Philip T Slack ◽  
John Gilbert
Keyword(s):  
Standard Deviation ◽  
Ochratoxin A ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Collaborative Study ◽  
Immunoaffinity Column ◽  
Low Level ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted to evaluate a liquid chromatographic (LC) method with immunoaffinity column cleanup for determination of ochratoxin A. The method was tested at 3 concentration levels of ochratoxin A in barley, which represent possible future European regulatory limits. The test portion was extracted with acetonitrile–water by blending at high speed. The extract was filtered, diluted with phosphate-buffered saline (PBS), and applied to an ochratoxin A immunoaffinity column. The column was washed with water and the ochratoxin A eluted with methanol. The solvent was then evaporated and the residue redissolved in injection solvent. After injection of this solution onto reversed-phase LC column, ochratoxin A was measured by fluorescence detection. Eight samples of low level naturally contaminated barley and 2 samples of blank barley (ochratoxin A not found at the limit of detection of 0.2 μg/kg at the signal-to-noise ratio of 3 to 1) were sent, along with ampules of ochratoxin A, calibrant, and spiking solutions, to 15 laboratories in 13 different European countries. Test portions were spiked with ochratoxin A at levels of 4 ng/g, and recoveries ranged from 65 to 113%. Based on results for spiked samples (blind duplicates) and naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) ranged from 4 to 24%, and the relative standard deviation for reproducibility (RSDR) ranged from 12 to 33%. The method showed acceptable within- and between-laboratory precision, as evidenced by HORRAT values, at the low level of determination for ochratoxin A in barley.

Rapid determination of fosetyl-aluminium in commercial pesticide formulations by high-performance liquid chromatography

2014 ◽  
Vol 68 (6) ◽  
Author(s):  
Helen Karasali ◽  
Konstantinos Kasiotis ◽  
Kyriaki Machera
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Hplc Method ◽  
Negative Ion ◽  
Rp Hplc ◽  
Relative Standard

AbstractAn isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL−1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSDr) was lower than the RSDr, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.

scholarly journals Spectrophotometic Determination of Caffeine and Vitamin B6 in Selected Beverages, Energy/Soft Drinks and Herbal Products

2021 ◽  
Vol 28 (1) ◽  
pp. 22-29
Author(s):  
A.L. Ogunneye ◽  
O.O. Banjoko ◽  
M.R. Gbadamosi ◽  
O.H. Falegbe ◽  
K.H. Moberuagba ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Vitamin B6 ◽  
Limit Of Detection ◽  
Soft Drinks ◽  
Sensitivity Limit ◽  
Limit Of Quantification ◽  
Herbal Products ◽  
Relative Standard

In this study, a simple, sensitive and reproducible spectrophotometric technique has been developed and validated for the determination of caffeine and vitamin B6 in beverages, energy/soft drinks and herbal products. The determination of caffeine and vitamin B6 in the respective samples were carried out at maximum (λmax) absorbance of 272 and 290 nm respectively. The method was validated in terms of linearity, sensitivity (limit of Detection (LOD) and limit of Quantification (LOQ), accuracy (% Recovery), precision (relative standard deviation). The method was linear from (4-20 µg/ml and 50 - 250 µg/ml with r 2 of 0.9991 and 0.9996 for vitamin B6 and caffeine respectively. The accuracy of the method ranged from 99.48 - 101.42% for caffeine and 99.94% - 102.35% for vitamin B6. The detection limit and quantification limit were 0.192 µg/ml and 0.640 µg/ml for vitamin B6 while 0.0155 µg/ml and 0.0518 µg/ml was obtained for caffeine. The method for the two analytes was found to be precise as the percentage relative standard deviation was below 5%. Therefore, the method proposed in this study is rapid, suitable and can be used as a quality control index for caffeine and vitamin B6 in beverages, energy/soft drinks and herbal products in industries. Keywords: Caffeine, Vitamin B6, Beverages, Energy/Soft drinks, Herbal products, Spectrophotometry

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

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