Evaluation of Analytical Procedures in the Determination of Trace Metals in Heavy Crude Oils by Flame Atomic Absorption Spectrophotometry

In the present work, four trace metals, V, Ni, Cu and Fe, have been determined in five crude oil samples of Eastern Baghdad area, Iraq by flame atomic absorption spectrophotometry. The crude oils are characterized with API gravity values in the range, 25 - 15. The V/Ni ratios for the studied crudes were in the range 3.7 to 5.4 and indicated a typical of the sapropelic-type organic matter. The Ni and V contents were correlated with API gravity where an increase of metal contents with the decrease in the API values could be observed. The plots of V and Ni versus sulfur indicated linear correlation. This is attributed to the increase of porphyrinic structures of the metals. The method of direct dilution (DD) with organic solvent and the standard addition (SA) were evaluated as compared with standard dry ashing-acid dissolution (DA). In most cases the DD method gave V and Ni concentrations that are higher than DA and for the heavier crude oil (API = 15) the DD results were significantly smaller than those of the DA method. The SA method can be a good solution to determine the trace metals in heavy crude oils provided that the addition must not exceed the levels of the metal concentration in the diluted samples.

Concentration determination of gold nanoparticles by flame atomic absorption spectrophotometry

While engineered nanoparticles are widely used and maybe eventually released into the environment,natural nanoparticles are also commonly found in the Earth system.Nanoparticles may critically affect the geochemical migration of associated elements and pose potential threats to the ecological environment.It is necessary to establish an accurate and reliable method for measuring the concentration of nanoparticles.AAS is one of the most commonly used methods for the concentration determination of nanoparticles.However,till now,there has been no systematic report on how experimental variables affect AAS measurements.In this study,we used gold nanoparticles(AuNPs) as an example and studied the influences of a list of factors on the concentration determination of AuNPs by AAS,including digestion method,ionization interference,acidic medium,background correction method,and organic matter.We demonstrate that all these factors may have varying degrees of influence on the measured gold concentrations.When the gold colloid is digested at room temperature for more than 8 h or at 60℃ for more than 2 h,and the system contains a low concentration of organic matter,AAS can accurately measure the AuNP concentration at ppm-level.The deuterium lamp background deduction method is not recommended to use for samples with lower gold concentrations.

Use of Flame Atomic Absorption Spectroscopy and Multivariate Analysis for the Determination of Trace Elements in Human Scalp

The analysis of trace elements in human hair for use as biomarkers continues to generate considerable interest in environmental and bioanalytical studies, medical diagnostics, and forensic science. This study investigated the concentrations of essential and toxic elements (Fe, Mg, Ca, Cu, Zn, Cr, Cd, and Pb) using flame atomic absorption spectroscopy (FAAS) in human scalp hair obtained from subjects living in Forsyth County, North Carolina, USA. The influence of age, sex, race, and smoking habits on the levels of trace elements in the hair samples were also investigated. Additionally, analyses were subjected to a statistical, regression, and principal component analysis to evaluate inter-elemental association and possible pattern recognition in hair samples. Furthermore, Ca/Mg and Zn/Cu ratios, which are often used to evaluate the degree of Ca and Cu utilization in humans and as markers for various health related issues including, atherosclerosis, hypertension, insulin sensitivity, and pancreatic cancer, were calculated. The overall mean concentrations of Fe (25 μg/g), Ca (710 μg/g), Mg (120 μg/g), Zn (190 μg/g), Cu (12 μg/g), and Cr (0.20 μg/g) were found in hair samples. The trace element concentrations varied widely in hair samples as demonstrated by large range of concentrations obtained for each element. However, levels of Cd and Pb elements of <0.030 μg/g were detected in hair sample. In general, the levels of the trace elements in hair samples were poorly correlated. However, significant correlations were found between Ca and Mg (r = 0.840, p = 0.05). The levels of Fe, Ca, Mg, Zn, Cu, and Cr in hair samples and the calculated Ca/Mg and Zn/Cu ratios were found to be largely correlated with age, race, sex, and smoking habits.

Uncertainty Estimation for the Determination of Trace Heavy Metals in Human Hair by Flame and Electrothermal Atomic Absorption Spectrometry

Trace element analysis on hair samples has been widely used to assess wildlife and human exposure to different contaminants present in the environment or at the workplace. Pollutants due to the presence of toxic metals in environment not only enter the body by breading, water, and foodstuff accumulates in hair, but they could be adsorbed directly on the hair from environment. In order to remove adsorbed elements and thus determine the internally bound elements correctly, hair sample must be washed. In the present work, we propose uncertainty estimation for the analytical results that are obtained from determination of cadmium, lead, copper, iron, manganese and nickel in human hair by flame and electrothermal atomic absorption spectrometry （FAAS and ETAAS）. To estimate the uncertainty of analytical result obtained, two types of bias are calculated in the assessment of trueness： a proportional bias and a constant bias. Nested design was applied for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in human hair is： （1.019 ±0.026）, （0.918 ±0.014）, （1.073±0.016）, （1.0597± 0.017）, （1.073± 0.020） and （0.934± 0.117） for Cd, Pb, Mn, Ni, Fe and Cu respectively.

Application of Nanometer-Size Titanium Dioxide in Extreme-Trace V(Ⅴ) Analysis

The adsorption properties of nanometer-size TiO2 for V（Ⅴ ） were studied. The adsorption rate could reach above 99~ when the pH values were at the range of 4 10. The adsorption balance time was 10 min , the saturation capacity of adsorption of nanometer-size TiO2 to V（Ⅴ） was 6.43 mg per gram. Using 2 mL 1.5 mol · L^-1 NaOH as elution, we found the elution rate could reach 95%. A novel method of extreme-trace V（Ⅴ ） preconeentration with nanometer-size titanium dioxide and determination by graphite furnace atomic absorption spectroscopy （GFAAS） was advanced. The detection limit（3σ）of the method was 0.61μg ·L^-1 , and the relative standard deviation was 8.1% （n=6） of 2.5μg ·L-^1 V（Ⅴ）. Environmental samples experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 91.2% and 102.0%.

Trace and Macro Elements Concentrations in Selected Fresh Fruits, Vegetables, Herbs, and Processed Foods in North Carolina, USA

Fresh fruits, vegetables, herbs, and processed foods continue to be the major sources of essential trace elements in humans’ diet required for proper body development. However, food products can potentially be contaminated by toxic heavy metals (HMs) from environmental contamination or industrial food processing. The deleterious health implications of essential trace and macro elements’ deficiency and toxic consequences of HMs in humans necessitate proactive monitoring of the essential trace elements and HMs concentrations in the humans diet to ensure public health safety. Accordingly, this study investigated a comparative analysis of essential elements and potential toxic HMs concentration in food products in the Greensboro metropolis, North Carolina, USA. A total of 49 food samples comprising of 16 difference fresh fruits, 17 fresh vegetables, 4 herbs, and 12 processed foods were purchased from local grocery stores and analyzed for iron (Fe), calcium (Ca), magnesium (Mg), nickel (Ni), zinc (Zn), copper (Cu), lead (Pb), cadmium (Cd), and chromium (Cr) by the use of flame atomic absorption spectrometry (FAAS). The concentrations of elements were subjected to a regression analysis to further gain insight of the inter-element association in the food samples. The results of the study showed high variability in the concentrations of elements in the fresh fruits, vegetables, herbs, and processed foods. The overall average concentrations of Ca (1501 μg/g), Mg (186.5 μg/g), Fe (55.8 μg/g), Zn (22.2 μg/g), Pb (10.2 μg/g), Cu (5.8 μg/g), Cr (<0.1 μg/g), Cd (<0.1 μg/g), and Ni (<0.04 μg/g) were obtained in all food samples categories. The elements concentrations were generally poorly correlated in the food samples. However, a strong inter-element association between Cu and Fe concentration (R2 = 1.000) and a weak association between Ca and Fe (R2 = 0.5609) were found in the food samples. A survey questionnaire was administered to 396 participants in the Greensboro metropolis to evaluate the food consumption pattern and a daily/weekly dietary estimate intake of vegetables, fruits, herbs and processed foods. The results of the food survey analysis showed that the amount of vegetables, fruits, herbs, and processed foods dietary intake varied widely. In general, the participants consumed more processed foods than vegetables, fruits, and herb foods. The low dietary intake of vegetables, fruits, herbs suggests that most participants may be obtaining insufficient essential trace elements and other vital nutrients necessary for normal growth and body development in their diet.

原子吸收光谱法测定苦瓜中微量金属元素的含量

用微波消解法对苦瓜进行预处理,采用火焰原子吸收光谱法测定了苦瓜中钙、镁、铁、锌四种微量金属元素的含量。在最佳条件下测得苦瓜中各金属元素的含量分别为Ca:3843.50μg/g,Mg:2545.492μg/g,Fe:93.3415μg/g,Zn:77.685μg/g;RSD为0.19%~0.85%;检出限为0.0020μg·mL^(-1)~0.0703μg·mL^(-1);相关系数为0.9927~0.9997;加标回收率为94.60%~102.92%,此方法简单、快捷、经济、有效。

石墨炉原子吸收测定间接空冷机组循环水中的痕量铝

采用石墨炉原子吸收测定SCAL型间接空冷机组循环水中的痕量铝,从石墨炉工作参数、基体改进剂、试剂空白、水样前处理等方面进行了实验条件优选。实验结果表明:石墨炉灰化温度、原子化温度分别为700℃和2 700℃,不加基体改进剂条件下,铝离子标液质量浓度在0~20μg/L范围内标准曲线线性相关系数可达到0.999 8,相对标准偏差小于10%,检测下限为0.5μg/L。采用水样酸化静置1 h后直接测定并与标准加热消解法测定值进行了对比,相对误差小于5.0%,空白值小于0.5μg/L,有效解决了加热消解法空白值高的问题,提高了间接空冷机组循环水中小于10μg/L痕量铝测定的准确性。

火焰原子吸收分光光度法测定水中锰的不确定度分析

综合理论分析与实践调查,对火焰原子吸收法测定水中锰的不确定度展开分析。在简要概述测定实验中所需的材料与方法后,为其实际测定中不确定度评定建立数学模型,对其不确定度的分量来源加以归纳,并对各分量造成的不确定度加以计算。最后通过各分量的合成与拓展,得出水中锰测定中不确定度的具体数值。

水质中总铬含量测定方法对比及应用研究

从标准曲线、检出限、精密度、正确度等方面比较电感耦合等离子体质谱法(ICP-MS)、火焰原子吸收分光光度法(F-AAS)和紫外分光光度法(UV)测定水质总铬含量的情况。各方法标准曲线相关系数均能达到0.999,对有证标准物质的分析结果均在真值范围内;ICP-MS检出限2.7×10-5 mg/L,测定下限为1.08×10-4 mg/L,精密度1.3%~1.9%,正确度为97.9%~103.8%;F-AAS检出限0.0162 mg/L,测定下限0.0648 mg/L,精密度0.6%~4.1%,正确度为96.0%~104.0%;UV检出限0.0037 mg/L,测定下限0.0148 mg/L,精密度1.3%~6.6%,正确度为95.0%~102.0%。结果表明三个方法均能准确测定水中总铬含量,应根据实验室条件及样品含量选择合适的方法。

原子吸收分光光度法在岩石矿物分析中的应用

文章论述了原子吸收分光光度法在岩石矿物分析中的应用,而后提出原子吸收分光光度法分析在测定岩石矿物中的干扰因素及消除方法,可为我国原子吸收分光光度法在岩石矿物分析中的应用提供参考。

黄芪中微量元素的形态分析

按照传统煎煮法对中药黄芪中铜、锌、铁、镁、钙和铬6种元素进行提取;用微孔滤膜分离提取液中的可溶态与悬浮态;利用大孔吸附树脂柱对可溶态中的有机态与无机态进行分离;采用火焰原子吸收光谱法对各种形态中的6种元素进行测定.结果显示：黄芪中6种元素的总提取率在44.0%～74.4%,浸留比在79.4%～293.8%,悬浮态颗粒吸附率在10%左右,可溶态中铬的有机态与无机态的比例为114.6%,铜、锌、铁、镁、钙的有机态与无机态的比例在3.7%～43.5%.该法对各元素的加标回收率在96.8%～103.1%;相对标准偏差小于1.5%.

中老年糖尿病轻重度患者血清中的铁铬钴镍

对 12 8例中老年糖尿病患者进行了血清中微量元素铁、铬、钴、镍的含量测定 ,并与正常对照组进行了比较。结果表明 ,血糖正常组和高血糖组的糖尿病患者血清铁铬水平均低于正常对照组 ,且两病例组与对照组比较铬水平有非常显著差异 (P <0 0 1)。血清镍水平患病初期降低 ,后升至正常 ,高血糖组与对照组比较差异显著 (P <0 0 5 ) ,两病例组间差异非常显著 (P <0 0 1)。血清钴水平随病情加重而逐渐升高 ,但无统计学上的显著意义。

火焰原子吸收光谱法测定山药中多种微量元素

利用火焰原子吸收光谱法测定了山药中钾、钙、钠、镁、铜、锌、铁、锰、锶和镍的含量.其中前八种元素的RSD分别为0.43%,1.10%,4.41%,0.68%,1.44%,1.88%,1.29%和0.03%.回收率为90.0%～111.0%,该方法灵敏度高,结果准确,可用于山药等中草药中多种微量元素的同时测定.用该法对不同地区的中草药进行微量元素分析测定.文章还对不同产地中草药微量元素含量的变化及其分布的规律性进行了讨论,可以为探讨微量元素与中草药的质量关系提供一定的理论依据.

原子吸收光谱法测定血清中不同化学形态的铜、铁、锌

融合分子生物学技术与原子吸收光谱对血清中元素铜、铁和锌的化学形态进行研究。用60%乙醇低温(4℃)沉淀血清蛋白的方法将血清中的铜,铁,锌分为结合态和非结合态,原子吸收分光光度计分别测定血清中Cu,Fe和Zn三种元素的总量及非结合态含量,通过减差法求出血清中结合态元素含量,从而建立了Cu,Fe和Zn元素这两种化学形态的分离分析方法,并讨论了有关的实验条件。该方法铜、铁和锌的检出限分别为9·84×10-3μg·mL-1,2·76×10-2μg·mL-1,1·06×10-3μg·mL-1,相对标准偏差为0·30%～2·31%,回收率为95·0%～104·0%。该法已应用于SD大鼠血清中Cu,Fe和Zn三种元素不同化学形态的测量。

火焰原子吸收光谱法分析香青兰中微量元素的溶出特性及化学形态

结合香青兰的药用功效,对其铜、锌、锰、铁、镁、镍6种微量元素的含量和形态进行了分析.分别用0.45 μm滤膜、D101型大孔吸附树脂,将香青兰水煎液中铜、锌、锰、铁、镁、镍分为悬浮态和可溶态、有机态和无机态;并采取正辛醇-水分配体系模拟水煎液中铜、锌、锰、铁、镁、镍在人体胃肠中的分配情况,建立了上述6种元素的4种形态分离分析方法,用火焰原子吸收光谱法测定6种微量元素的含量、分布及其在不同溶剂中的溶出特性和化学形态.结果表明,方法的回收率在92%～106%范围内,相对标准偏差均在3.8%以下,铜、锌、锰、铁、镁、镍是各以某种形态为主的多种形态共存的混杂体系.

中药丹参及其近缘种中微量元素的主成分和聚类分析

采用原子吸收光谱法测定了不同产地的中药丹参及其近缘种植物白花丹参、雪山鼠尾草、云南鼠尾草、甘西鼠尾草、贵州鼠尾草、血盆草、粘毛鼠尾草、峨眉鼠尾草、黄鼠狼花、短唇鼠尾草和犬形鼠尾草中的Cu,Zn,Fe,Mg,Ca,Cr,Pb,Mo,Mn和Cd共10种微量元素的含量,应用主成分和聚类分析法对测定结果进行了研究。经过主成分分析得出3个主因子,其累计方差贡献率达79.3%。第一主因子的方差贡献率为49.6%,故所对应的Fe,Mn,Cu,Zn,Cd和Pb是丹参及其近缘种的特征元素。聚类分析将21个样品聚成2组,除浙江栽培丹参和白花丹参外,来自不同产地的9个丹参样品聚为一组;除贵州鼠尾草外,其他鼠尾草样品聚在一起,故此法可以将丹参和鼠尾草属其他植物区分开,总符合率达90%。因此利用原子吸收光谱法测定丹参及其近缘种中微量元素含量并对测定结果进行聚类分析是鉴别正品丹参的一种快速、准确的方法。

新资源食品中微量元素测定方法的研究

用硝酸-高氯酸消解样品,用火焰原子吸收光谱法测定新资源食品葛根、葛花、四叶参、仙人掌、菊花、小麦胚和蚕蛹中Cu,Zn和Fe元素的含量,并对其结果进行了分析。结果显示：在选定的实验条件下,测定方法的回收率为94.66%~105.24%,测定Cu,Zn和Fe的精密度RSD分别为1.79%,0.71%和4.78%。建立的原子吸收光谱法简便、快速、灵敏、准确。经F检验与SNK检验,河南省新资源食品葛根、葛花、四叶参、仙人掌、菊花、小麦胚和蚕蛹中微量元素Cu,Zn和Fe含量分别为：铜的分布量依次为：菊花≈蚕蛹〉葛花≈小麦胚≈四叶参≈葛根〉仙人掌,锌的分布量依次为：仙人掌〉蚕蛹≈葛花≈葛根≈小麦胚≈四叶参≈菊花;铁的分布量依次为：蚕蛹≈菊花≈葛根〉葛花≈小麦胚≈四叶参≈仙人掌。

速效救心丸中Ca,Mg,Fe,Cu,Zn的测定及Ca/Mg,Cu/Zn比值分析

本文采用火焰原子吸收分光光度法测定了速效救心丸中Ca ,Mg ,Fe,Cu ,Zn五种金属元素的含量 ,并对速效救心丸中Ca/Mg ,Cu/Zn含量比值进行了分析研究。结果表明 ,速效救心丸中含有丰富的Ca,Mg ,Fe ,Cu ,Zn元素 ,元素含量Ca>Fe >Mg >Zn >Cu ,它为探讨速效救心丸中Ca ,Mg ,Fe ,Cu ,Zn与治疗冠心病之间的关系提供了有用的数据。

原子吸收法测定中药黄芩中不同化学形态的Cu、Zn、Fe和Mn

研究用原子吸收光谱法(AAS)测定中药黄芩水煎液中Cu,Zn,Fe和Mn化学形态的分析方法。水煎液经0.45μm滤膜过滤后分为悬浮态和可溶态组分试样;对于可溶态组分试样,采用LSA-10大孔树脂将其分为有机态和无机态组分试样,并采用正辛醇-水分配体系,在模拟人体胃肠环境条件下,将水可溶态中待测元素分离为醇溶态和水溶态,然后用AAS测定上述各组分试样中待测元素的含量,即可给出比现有的仅测量中药黄芩中上述各待测元素总量为多的信息。该法待测元素Cu,Zn,Mn的检出限(3倍空白标准差)为0.01μg.mL-1,Fe为0.02μg.mL-1,精密度(RSD,n=11)为1.5%～3.6%,对可溶态和无机态组分试样进行加标测定的回收率为96.7%～105.0%。所得结果对黄芩的综合研究有重要的实际意义。