微波消解-FAAS法测定鱼酱酸中八种微量元素

采用微波消解火焰原子吸收光谱法测定苗族、侗族同胞传统制作的原生态发酵型调味品鱼酱酸中的Fe,Zn,Cu,Mn,Cd,Ni,Cr,Pb含量,为原生态民族风情旅游地区黔东南发酵型调味品鱼酱酸的开发利用提供参考.     

火焰原子吸收分光光度法快速测定饮料中的铜

本法采用火焰原子吸收法测定饮料中的铜含量,并在此基础上用硝酸稀释法处理样品,经过比较,发现该法样品前处理简便、快捷,克服了消化法繁琐、耗时以及直接进样法的易堵塞燃烧头、基线漂移等缺点,测定结果准确。该方法样品加标回收率为92%～103%,相对标准偏差为0.58%,检出限为0.015mg/L。     

石墨炉原子吸收法测定碳酸饮料中的痕量铅

本文研究了在酸性条件下用吡咯烷二硫代甲酸铵和二乙氨基二硫代甲酸钠及甲基异丁酮(APDC+DDTC-MIBK)体系萃取富集碳酸饮料消化液中Pb2+,经硝酸反萃后用石墨炉原子吸收法测定Pb2+含量的检测方法.方法检出限为0.04μg/L,线性范围为O.1～1.125μg/L,相关系数为0.9981,加标回收率为94.04~100.28%,相对标准偏差为1.08～4.37%.     

火焰原子吸收法测定番荔枝中的几种微量元素

用火焰原子吸收光谱法测定了番荔枝果肉、果皮及种子中的K、Na、Ca、Mg、Cu、Zn、Mn、Fe、Ni、Pb、Cd等微量元素,各元素回收率在98%~117%之间。结果表明,番荔枝中富含人体必需的微量元素及宏量元素,有害元素Pb、Cd含量较低。     

超声波辅助提取-悬浮液进样-FAAS测定银杏叶中微量元素

将超声波辅助提取与悬浮液进样技术相结合,采用火焰原子吸收光谱法(FAAS)测定银杏叶中的微量元素的含量。在最佳仪器条件下对介质的影响、化学干扰、超声波时间、检测限及加标回收率进行考察。结果表明：相对标准偏差小于2.2%,回收率97.8%～104%。方法简便、快速,可用于银杏叶中批量微量元素的准确测定。     

火焰原子吸收光谱法连续测定黄酒中的金属离子

用微波消化罐消化样品,以火焰原子吸收光谱法在同一系列体系中测定黄酒中微量铜、锌、铁、锰的方法。考察了硝酸、过氧化氢的不同用量以及消化时间长短的影响和在同一体系中铜、锌、铁、锰的彼此干扰情况。结果：检出限铜为0．0048μg／mL,锌为0．0062μg／mL,铁为0．0045μg／mL,锰为0．0081μg／mL,相对标准偏差为2．0％～4．5％,回收率为99．6％-102．1％。     

氢化物发生原子吸收测定食盐制品和盐化产品中微量铅

方法采用铁氰化钾将盐溶液中的Pb2 氧化为Pb4 ,用NaBH4-HC l将Pb4 还原为铅烷(PbH4↑),进行原子吸收光谱测定。称样1.00g±0.02g于25m l比色管中,加无离子水约10m l溶解,加0.5m lHC l(4.2mol/l),0.5m l草酸(10g/l),1.0m l铁氰化钾(100g/l),用水定容至刻度,混匀后AAS测定,直读含量。方法检出限为0.012mg/kg,测定范围0~0.6mg/kg,相关系数为0.999X,回收率为95.6%~110%,平均为102%。RSD≤5.4%。方法简单易行,灵敏、快速、准确、环保、健康、更具人性化,特别适合食盐制品中微量铅的分析。     

Silica Gel Chemically Modified with Ionic Liquid as Novel Sorbent for Solid-Phase Extraction and Preconcentration of Lead from Beer and Tea Drink Samples Followed by Flame Atomic Absorption Spectrometric Determination

Lead is a harmful metal element that has aroused considerable concern; therefore, it is of great importance to develop sensitive and reliable analytical techniques for the precise monitoring of lead in various foodstuffs. In the present study, an enrichment and separation procedure for lead via its solid-phase extraction as dithizone chelate on an ionic liquid 1,3-di(n-butyl) imidazolium hexafluorophosphate [DnBIM][PF₆]-chemically modified silica gel has been established prior to its flame atomic absorption spectrometric determination. The parameters that affect the extraction recovery of lead was investigated, including sample pH, dithizone concentration, eluent type and volume, and flow rate of sample and eluent. The analytical performance of the method was evaluated. Under the optimized conditions (sample pH, 8.0; dithizone concentration, 0.0005 % (w/v); eluent, 2 mL of 1.0 mol/L HNO₃; sample flow rate, 3 mL/min; eluent flow rate, 0.5 mL/min), the limit of detection was 0.36 μg/L (3σ, n?=?7), and the relative standard deviation was 3.5 % (c?=?5.0 μg/L, n?=?7). The proposed method was successfully applied to the determination of trace lead in beer and tea drink, and the recoveries for the spiked samples were in the range of 97.3–102.5 %.     

螺旋藻预富集-FAAS测定干制品浸出液中的痕量铜

建立了螺旋藻预富集-火焰原子吸收光谱法测定干制品浸出液中的痕量铜的方法,讨论了螺旋藻的预处理方法、用量、颗粒大小、洗脱剂类型、洗脱剂浓度、洗脱流速、pH值等对干制品中痕量铜富集效果的影响。结果表明,在交换柱内径为0.8 cm、柱高为15 cm、螺旋藻用量为2 g、pH值6的条件下,干制品浸出液流速为10mL/min时,用0.6 mol/L HCl以6 mL/min的速度洗脱,可对Cu2+进行高效富集。用该方法测定几种干制品中的痕量铜,当n=6时,SD为0.000 02～0.000 09,RSD为2.5%～4.2%,特征浓度为0.059μg/L,加标回收率为97%～103%。     

云南文山雪莲果中微量元素的测定——应用火焰原子吸收法

采用干法灰化处理样品,用火焰原子吸收光谱法测定雪莲果中Zn、Fe、Cu、Mn、Ni、Cr、Cd、Co、Pb9种微量元素的含量;结果表明:RSD%值在0.66~3.25之间,回收率为99.8%~103.7%。对分析结果进行了对比分析,发现文山雪莲果中人体必需元素Fe、Zn含量均较高。     

The Mesoporous Porphyrinic Zirconium Metal-Organic Framework for Pipette-Tip Solid-Phase Extraction of Mercury from Fish Samples Followed by Cold Vapor Atomic Absorption Spectrometric Determination

In this study, the highly stable mesoporous porphyrinic zirconium metal-organic framework, namely PCN-222/MOF-545 (Zr-MOF), was prepared and used for pipette-tip solid-phase extraction of Hg(II). As a high-capacity sorbent, 4 mg of the Zr-MOF was placed into a conventional pipette tip and used, for the first time, for the fast extraction and preconcentration of mercury ions. For desorption, 50 μL of 10% HCl was used by 15 repeated aspirating/dispensing cycles, and Hg ions in elusion were measured by a cold vapor atomic absorption spectrometer. Affecting parameters on extraction efficiency were studied, and optimum conditions were established as amount of sorbent 2 mg, pH was adjusted to 5.0, the eluting volume was 15 μL, and extraction was performed on 1.8 mL of the sample. The optimal number of aspirating/dispensing cycles for extraction and desorption of analytes was found to be 10 and 15 cycles, respectively. The limit of detection of the method was found to be 20 ng L^?1 with a relative standard deviation of ≤3.1% (for seven replicate analyses of 20 μg L^?1 of mercury). Adsorption capacity and enrichment factor were 35.5 mg g^?1 and 120-fold, respectively. The proposed method was successfully applied for the determination of Hg(II) ions in fish samples.     

浊点萃取-热喷雾火焰炉原子吸收光谱法测定荔枝和桂圆肉中痕量Pb和Cd

为测定荔枝和桂圆肉中的Pb和Cd。采用浊点萃取-热喷雾火焰炉原子吸收光谱法对该样品进行分析,考查二乙基二硫代氨基甲酸钠(DDTC)浓度、溶液pH值、TritonX-100浓度、加热时间、水浴温度、干扰离子等实验条件对浊点萃取效率的影响。在最优试验条件下,即pH5.0、温度100℃、萃取时间15min、TritonX-100体积分数0.3%、DDTC质量浓度0.02g/100mL、进样速率0.3mL/min,该方法对Pb和Cd的富集倍数分别为30倍和26倍;方法的检出限对Pb和Cd分别为2ng/mL和0.1ng/mL,相对标准偏差分别为5.2%和3.6%。利用该方法对荔枝和桂圆中的铅和镉进行测定,结果令人满意。     

枣中微量硒的原子荧光光谱法分析

采用原子荧光光谱法对枣中硒的含量进行分析,确定最佳测定条件。结果表明：硒的检出限为0.57ng/ml,线性范围为1.0～32.0ng/ml,回收率为99.0%～106.3%,变异系数小于1.71%。     

石墨炉原子吸收法测定罐头食品中的锡

以密闭消解样品,石墨炉原子吸收法测定食品中微量锡。对影响测定灵敏度的条件进行优化,以氯化钯＋硝酸镁为基体改进剂,在灰化温度1000℃,原子化温度1800℃条件下,方法检出限为6.7μg/L,线性范围0.05～0.20mg/L,回收率99.2%～104.4%,相对标准偏差4.3%。本方法具有检出限低、灵敏度高、简便、准确等优点,可满足食品中准确测定较低含量锡的要求。     

在线双毛细管火焰原子吸收法测定海带中的微量锶

研究在线双毛细管快速测定海带中微量锶的方法,使用相同管径的双毛细管对酸度和干扰离子进行探讨。采用湿法溶样对样品进行前处理,通过在线加入十二烷基磺酸钠抑制干扰,采用10.0 L/min空气流量和1.2 L/min乙炔流量进行了实验,结果显示：海带中Sr含量在700 μg/g左右。方法检出限为0.1 μg/g,样品回收率在97.8%～107.4%,精密度小于5%。方法准确快速、成本低廉,适合样品中微量锶的测定。经实际样品验证获得较为满意的结果。     

Direct Determination of Trace Elements in Meat Samples via High-Resolution Graphite Furnace Atomic Absorption Spectrometry

This work presents a direct and straightforward approach for the determination of trace elements in fish muscle, oyster, and bovine liver via direct solid sample analysis (SS) using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The preliminary studies revealed the presence of spectral interferences at the analytical line of Ni at 231.096 nm, which could be corrected subtracting the spectrum of SiO and PO from the sample spectra using least-squares background correction. Moreover, all meat samples were proven homogeneous according to the homogeneity factor (H _e) (all values were <10 mg^½). Pyrolysis (Tp) and atomization (Ta) temperatures were studied and optimized as 800 °C (Tp) and 2500 °C (Ta) for Mn, 700 °C (Tp) and 2600 °C (Ta) for Ni, and 600 °C (Tp) and 2500 °C (Ta) for Rb. Calibration against aqueous standards was proven feasible for Mn determination, whereas Ni and Rb required calibration against solid standards for their quantification. The detection limits achieved were demonstrated adequate for application to food analysis (0.005 μg g^?1 for Mn, 0.002 μg g^?1 for Ni, and 0.1 μg g^?1 for Rb). The developed method was successfully applied for the elemental analysis of fish muscle, oyster, and bovine liver and three certified reference materials, demonstrating good agreement with the certified values and with the reference technique at a 95 % statistical confidence level.     

微波消解-火焰原子吸收光谱法测定油脂样品中的9种金属元素

为建立一种能对油脂样品中9种金属元素含量进行准确测定的方法,以5种食用油和2种地沟油为试材,采用微波消解法对样品进行前处理,利用火焰原子吸收光谱仪进行测定,并对微波消解油脂样品时的程序和条件进行了设计和优化,最终建立了包含5个步骤的微波消解新程序,其中最大消解压力为35 atm,最大温度为190 ℃,保持时间为20 min。方法性能考察表明:9种待测金属元素在各自的浓度范围内均具有良好的线性关系,决定系数为0.9982~0.9994,检出限为0.0013~0.0122 μg/mL,样品的加标回收率范围在98.94%~101.45%之间,RSD≤4%（n=6）。采用所建方法对7种油脂样品中的9种金属元素进行了含量测定,检测结果表明:5种食用油中含有丰富的营养元素,而Cr、Cd、Pb元素未检出,初步判断油脂的营养价值和安全性较高。而地沟油样品由于检出含有Cr、Cd、Pb,且Pb的含量远超国家标准限定值,已不适宜食用。实际应用表明:所建方法具有操作简便、准确度高等优点,能满足各类油脂中金属元素的检测需要。     

火焰原子吸收光谱法测定海螵蛸中15种微量元素含量

用火焰原子吸收光谱法测定海螵蛸中微量元素(Ca、Mg、K、Cu、Zn、Mn、Cr、Co、Ni、Fe、Si、Al、Pb、As和Cd)的含量,并对结果进行分析比较。该方法的加标回收率为96.5%～108.7%,RSD小于2.8%,具有良好的准确度和精密度。人体必需的重要微量元素Zn、Fe、Mn、Cu含量均较高。另外,样品中还检出微量有毒元素铅、砷和镉。