Determination of Lead in Lime-preserved Egg by Microwave Digestion and Flame Atomic Absorption Spectroscopy

[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Determination of Iron in Layered Crystal Sodium Disilicate and Sodium Silicate by Flame Atomic Absorption Spectrometry with Boric Acid as a Matrix Modifier

The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry （FAAS） were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.

Chemical Analysis of Magnesia and Magnesia-Alumina Refractory Materials——Flame atomic absorption spectrometric method for determination of calcium oxide content

1 Scope This standard specifics the determination of calcium oxide coutent by flame atomic absorption spectrometric method.

Flow-Injection Flame Atomic Absorption Determination of Hexavalent Chromium with On-Line Preconcentration on an Anion Imprinted Polymer

A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn packed with Cr(VI)-imprinted poly(4-vinyl pyridineco-2-hydroxyethyl methacrylate) placed into a flow injection system. Hexava-lent chromium was eluted with a small volume of diluted hydrochloric acid into the nebulizer-burner system of a flame atomic absorption spectrometer. An enrichment factor of 550 and a 3σ detection limit of 0.04 μg·L-1 along a sampling frequency of 4 h-1 at a sample flow rate of 3.5 mL·min-1. The relative standard deviation is 2.9% for 1 μg·L-1 Cr(VI) (n = 11). The flow injection system proposed has the advantage of being simpler because the use of expensive and sophisticated instruments is avoided. Ease of use, continuous process and selectivity make this method suitable for Cr(VI) determination in different environmental samples such as sea and river waters, soils and sediments.

A novel method for the determination of trace copper in cereals by dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with flame atomic absorption spectrometry

A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient（r） of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.

Determination of Copper by Flame Atomic Absorption Spectrometry after Preconcentration with Activated Carbon Impregnated with a New Schiff Base

A simple and reliable method for the extraction and determination of trace amounts of copper（Ⅱ） ions using activated carbon （AC） impregnated by a new Schiff base 5-[（4-heptyloxyphenyl）azo]-N-（4-propyloxyphenyl）-salicylaldimine （HPPS） and atomic absorption spectrometry is presented. Recovery efficiency and the influence of pH value, volume of sample solution, effect of different eluents, and interfering ions were evaluated. The limit of detection （3σ） was 2.62 ng.mL^-1 and the relative standard deviation （n=10） was 1.5%. Under optimum conditions, the copper ions were concentrated 25 fold using 250 mL of sample solution and 10 mL of eluent. This procedure has been successfully applied to the determination of copper in different water samples.

Determination of Manganese in Tri Calcium Phosphate (TCP) by Atomic Absorption Spectrometry

Tricalcium phosphate Anhydrous Powder typically contains less than 10 ppm (mg/Kg) (w/w) manganese. This level can be determined utilizing Flame Atomic Absorption Spectrometer (AAS) and standard based on known standards. A number of analytical methods are presently used for the analysis of metals in the biochemical. The instrumental techniques available are Inductively Coupled Plasma (ICP/MS), X-Ray Fluorescence, UV-VIS Spectrophotometry, and Atomic Absorption Spectrometry. Flame AA has gained widespread acceptance as an analytical technique and is used for many applications. In this study, we have determined the amount of manganese metal present in Tricalcium Phosphate (TCP) using Flame Atomic Absorption Spectrophotometer. The method has high precision and accuracy. The percent recovery was found to be 99.8% for spiked sample. The results meet the requirement.

Dental Erosion by Beverages and Determination of Trace Elements in Teeth by Atomic Absorption Spectrometry

The analysis of trace elements in human tooth for use as biomarkers continues to generate considerable interest in environmental and bioanalytical studies, medical diagnostic and forensic science. This study investigated concentrations of essential and toxic elements (Zn, Cu, Pb, Ni, Co and Cd) using flame atomic absorption spectroscopy (FAAS) and (Na and K) flame atomic emission spectroscopy (FAES) in human tooth obtained from Misan province, Iraq. The influence of smoking habits and born children on the levels of trace elements in additional to dental erosion by some beverages in the tooth samples were investigated. The overall of mean concentrations of (Zn 185.2 ppm, Cu 36.11 ppm, Pb 18.63 ppm, Ni 13.44 ppm, Co 3.45 ppm, and Cd 0.58 ppm, Na 11.683 ppm and K 115.27 ppm), (Zn 178.243 ppm, Cu 35.877 ppm, Pb 15.64 ppm, Ni 12.89 ppm, Co 3.421 ppm, Cd 0.455 ppm, Na 11,558.04 ppm and K 114.04 ppm) in smokers and non-smokers tooth groups respectively, (Zn 81.12 ppm, Cu 24.37 ppm, Pb 11.18 ppm, Ni 13.68 ppm, Co 3.32 ppm, Cd 0.44 ppm, Na 8227 ppm and K 76.42 ppm), (Zn 80.58 ppm, Cu 24.30 ppm, Pb 10.86 ppm, Ni 12.74 ppm, Co 2.71 ppm, Cd 0.23 ppm, Na 8165 ppm and K 72.80 ppm) in mothers and wives tooth groups respectively. However the w/w% loss of tooth immersed in following order of beverages (green tea, black tea, cinnamon, hibiscus, vinegar and citrus aurantifolia (9.09, 9.68, 12.36, 15.01, 16.77 and 17.38), (8.19, 8.25, 9.76, 13.37, 14.02 and 15.33) in smokers and non-smokers groups respectively, (11.25, 11.47, 13.30, 15.75, 19.58, and 20.91), (8.31, 7.96, 11.39, 13.49, 17.40, and 17.67) in mothers and wives groups respectively. However, there is a statistically significant variance found Zn (tcal 5.029, ttab 2.131), Pb (tcal 4.8538, ttab 2.131), Ni (tcal 5.243, ttab 2.131), Cd (tcal 3.9062, ttab 2.131) and Na (tcal 3.0832, ttab 2.131) between smokers and non-smokers tooth groups. However, the Co (tcal 2.7403, ttab 2.131) also shows statistically significant variance between mothers and wives groups. There is no statistically significant variance in w/w% loss after immersed the tooth in some beverages but in general it was higher in smokers than non-smokers and in mothers higher than wives.

Preconcentration and Separation of Trace Copper in Water Samples with Nanometer-Size TiO_2 Colloid and Determination by FAAS

A new absorbent of nanometer-size TiO2 colloid for Cu（Ⅱ ） was studied in this work. The adsorption rate could reach above 99% when the pH values were at the range of 5-6. The adsorption balance time, adsorption capacities, and the eluent were investigated. A novel method of trace Cu（ Ⅱ ） preconcentration and separation with nanometer-size titanium dioxide colloid and determination by flame atomic absorption spectrometry （FAAS） was advanced. The detection limit （3a） of the method was 1.15 μg · L^-1, and the relative standard deviation （R.S.D） was 1.53% （n=6）. Environmental sample experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 95.9% and 97.8%.

Releasing of Cupric Ion of Three types of Copper-bearing Intrauterine Contraceptive Device in Simulated UterineFluid

Objective To compare the cupric ion releasing in vitro o.f the three IUDs. Methods The stability o.f cupric ion releasing o.f IUDs including TCu 380.4 IUD （TCu 380A）, Multiload Cu375 IUD （MCu 375） and Yuangong 365 copper-bearing indomethacin-releasing IUD （Yuangong 365） by the determination of cupric ion releasing in simulated uterine fluid. The simulated uterine fluid was used for releasing media. Copper ion was determined by flame atomic absorption spectrometer. Results The cupric ion releasing of three IUDs were instable at the beginning and tend to be stable gradually. In the stable phase, the average level of cupric ion releasing of TCu380A, MCu375 and Yuangong 365 were 4.25±2.71-7.62±6.42 μg, 4.92±1.23 -8.62±3.08 μg and 2.19±0.40-4.68±1.66 μg, respectively. TCu380A had higher instable releasing level than those of Yuangong 365 （P〈0. 05）. Conclusion TCu 380.4 and MCu 375 showed a ＂burst release＂ during the first few days and the.former was of great significance（P〈0.05）. The initial cupric ion releasing of Yuangong 365 appeared to be the lowest, followed by MCu375 and TCu380A in a releasing order

TiO_2 nanotubes:A novel solid phase extraction adsorbent for the sensitive determination of nickel in environmental water samples

A novel method was developed for the sensitive determination of nickel in environmental water samples by using TiO2 nanotubes, a new nanomaterial, as solid phase extraction absorbent. In general, TiO2 nanomaterials were often used for catalytic degradation of pollutants in environmental field, and only a very few application in environmental analytic chemistry. In present work, TiO2 nanotubes was firstly used for the enrichment of nickel and the factors would influence the preconcentration performance were optimized. Under the optimal conditions, TiO2 nanotubes exhibited its good enrichment capacity for nickel and the detection limit of the proposed method was 1 ng· mL^-1. The proposed method was validated with real water samples, and excellent results were obtained with the spiked recoveries in the range of 94.4-99.2%, respectively.

Levels of Selected Essential and Non-Essential Metals in the Soil and Ginger (<i>Zingiber officinale</i>) Cultivated in Wolaita Zone, Ethiopia

Ginger (Zingiber officinale) is an important spice and medicinal plant used in different parts of the world. The objective of current study was to determine the level of essential and non-essential metals in ginger and its correlation with concentration of metals in the supporting soil. The level of K, Na, Ca, Mg, Mn, Fe, Zn, Cu, Co, Cd and Pb in soil and ginger cultivated in the selected districts of Wolaita zone, Southern Ethiopia were determined using flame atomic absorption spectrometry. A 0.5 g ginger sample was digested using a mixture of 4 ml HNO3 and 1.5 ml HClO4 at 210°C for 150 minutes, and a 0.5 g soil sample was digested employing a mixture of 6 ml aqua-regia and 1 ml H2O2 at 280°C for 150 minutes. The metal concentrations range in dry weight basis for ginger samples is decreasing in the order: K (1691 - 3487 mg/kg) > Mg (701 - 1583 mg/kg) > Ca (862 - 1476 mg/kg) > Na (398 - 776 mg/kg) > Mn (325 - 672 mg/kg) > Fe (6.14 - 11.92 mg/kg) > Zn (5.30 - 10.09 mg/kg) > (0.12 - 0.23 mg/kg) for Pb. The concentration of Cd, Cu and Co in ginger samples were below the limit of detection. The results revealed that ginger has the ability to accumulate relatively higher amounts of K and Mg among the determined essential metals. The soil samples have been found to be acidic pH, sandy clay loam in texture, a very low electrical conductivity and moderate level of (CEC, organic carbon, available phosphorus and total nitrogen). Although, a positive correlation between the levels of K, Mg, Zn, Mn in ginger and soil samples were observed. All the non-essential metals analyzed in this study were below the permissible ranges set by FAO/WHO.

Determination of Selected Essential and Non-Essential Metals in Three Types of Teff (<i>Eragrostis tef</i>) Cultivated in Southern Ethiopia

Teff (Eragrostis tef) is used to supply staple food “injera” for many Ethiopians. The present study was aimed toward determining the extent of selected metals that can exist in three types of teff cultivated in selected districts of southern Ethiopia. The level of those metals was determined by flame atomic absorption spectrometry. The optimized wet digestion procedure was evaluated employing a spiking method and an acceptable percentage recovery of (91.1% - 108.9%) has been obtained for metals in the teff. Oven dried 1 g of teff samples were digested using 5 mL of HNO3 and 1 mL of HClO4 at 300°C for 3 hours. The result indicated that the mean concentration of metals (in mg/kg dry weight basis) in teff samples were found to be from 1206.9 to 1768.9 of Ca, 2463.9 to 2554.7 of Mg, 82.6 to 109.9 of Na, 2879 to 3075 of K, 207.4 to 239.5 of Fe, 55.9 to 100.4 of Mn, 27.1 to 87.1 of Zn, 5.4 to 45.5 of Cu and 0.118 to 0.130 of Pb respectively. However, Cd is below the method detection limit. A statistical analysis of variance revealed that there was a significant difference (p ≤ 0.05) between the mineral content in three teff types and teff from the three districts. Red teff had higher essential metal contents except Cu followed by brown teff. Strong positive correlation was recognized between Mg with Ca and K, the rest have moderate or weak correlation. Further study has been done on the mineral contents of similar variety or three types of teff with the soil analysis from different locations.

Determination and Degradation of Potassium Bromate Content in Dough and Bread Samples Due to the Presence of Metals

Potassium bromate (PB) is used in bread making as an agent of maturation;however, it is classified as a potential carcinogen. In the present study, a rapid, simple, precise and accurate testing method has been developed to determine the level of bromate ions in bread, which is based on a reaction of bromate ions with iodide ions in acidic medium to produce iodine (I2). The absorbance of iodine (I2) was measured at 352 nm, and bromate ions reacted with iodide during the first 3 minutes after initiation of the reaction. The proposed method has been successfully applied to the determination of bromate ions in commercial bread. In this work, we found that bromate ions alone degraded at about 400°C, however, during bread making they degraded at 150°C - 200°C, this mightbe due to the presence of metals [Fe, Mg, Zn, Mn, Cu and Al] in flour which served as catalysts. In this study we found that the use of two grams (2 g) of PB per bag flour (60 kg) was safe.

A magnetic adsorbent based on salicylic acid-immobilized magnetite nano-particles for pre-concentration of Cd(II) ions

In this research,an eco-friendly magnetic adsorbent based on Fe_(3)O_(4)/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method.The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy,X-ray diffraction,and Fourier transform infrared spectroscopy.The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II)ions from synthetic solutions.Some experimental factors affecting the extraction efficiency were investigated and optimized.Following elution with acetic acid(pH 3.5),the pre-concentrated analyte was quantified by flame atomic absorption spectrometry.In optimal conditions,a linear calibration graph was achieved in the concentration range of 0.2–30 ng·mL^(−1) with a determination coefficient(R^(2))of 0.9953.The detection limit,the enhancement factor,inter-and intra-day relative standard deviations(for six consecutive extractions at the concentration level of 10 ng·mL^(−1))were 0.04 ng·mL^(−1),100,2.38%and 1.52%,respectively.To evaluate the accuracy of the method,a certified reference material(NIST SRM 1643e)was analyzed,and there was a good agreement between the certified and the measured values.It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8%and 103.2%.

Use of 2-(tert-butoxy)-N-(3-carbamothioylphenyl)acetamide and graphene oxide for separation and preconcentration of Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ) and Zn(Ⅱ) ions in different samples

A simple and selective method using a column packed with graphene oxide（GO） as a solid phase extractant has been developed for the multi-element preconcentration of Fe（Ⅲ）,Ni（Ⅱ）,Cu（Ⅱ） and Zn（Ⅱ）ions prior to flame atomic absorption spectrometric determinations.The method is based on the sorption of mentioned ions on synthesized GO using 2-（tert-butoxy）-N-（3-carbamothioylphenyl）acetamide as a chelating agent.Several parameters on the extraction and complex formation were optimized.Under the optimized conditions（pH 6,flow rate 9 mL/min）,metal ions were retained on the column,then quantitatively eluted by HNO3solution（5 mL,3.0 mol/L）.The preconcentration factor was calculated as250.The detection limits for the analyte ions of interest were found in the range of 0.11 ng/mL（Ni2＋） to0.63 ng/mL（Cu2＋）.The column packed with GO was adequate for metal ions separation in matrixes containing alkali,alkaline earth,transition and heavy metal ions.

Ultrasound-assisted emulsification solidified floating organic drop microextraction for the determination of trace amounts of copper in water samples

A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorption spectrometry,for the extraction and determination of trace copper in water samples.1-(2-Pyridylazo)-2-naphthol(PAN)was used as chelating agent.Microextraction efficiency factors(including extraction solvent type,extraction volume,time,temperature,and pH),the amount of the chelating agent,and salt effect were investigated and optimized.Under the optimum extraction conditions,figures of merit of the proposed method were evaluated.The calibration graph was linear in the range of 20–600 mg·L^(–1)with a detection limit of 0.76 mg·L^(–1).The relative standard deviation(R.S.D)for ten replicate measurements of 20 and 400 mg·L^(–1)of copper was 3.83%and 2.65%,respectively.Finally,the proposed method was applied to tap water,river water,and sea water,and accuracy was assessed through the analysis of certified reference water or recovery experiments.