火焰原子吸收光谱法分析中药中锰的形态

1　引　　言中药中锰具抗癌、益精生血、益肝明目及提高机体抵抗力等作用。正辛醇在结构上与人体内的碳水化合物和脂肪类似 ,药理学中药物鉴定用Ｋｏｗ参数 (Ｋｏｗ =Ｃｏ Ｃｗ ,Ｃｏ 和Ｃｗ 分别为该化合物在正辛醇相和水相中的平衡浓度 )评价药物亲脂性及生物活性。正辛醇醇溶态微量元素具较强的亲脂性和生物活性 ,如作为中药有效成分 ,醇溶态含量应与中药药性、药效密切相关。本实验按中药常用煎煮方式制水煮液 ,用正辛醇 水分配体系模拟水煎液中锰在人体胃肠中的分配情况。火焰原子吸收法 (ＦＡＡＳ)测药材、水煎液中锰含量及水溶态锰、…     

火焰原子吸收光谱法分析中药中锌的形态

采取正辛醇水分配体系模拟中药水煎液中锌在人体胃肠中的分配情况，用原子吸收光谱法测定了十二味中药药材及其水剪液中锌的含量，水煎液中水溶态锌、醇溶态锌的含量。实验结果表明，中药中锌的水煮溶出率较氏，中药中锌的形态与中药成分，配伍情况及作用靶位（胃肠）的酸度有关，酸度及配伍对中药中锌的溶出率及水煎液中锌的形态影响较大。     

火焰原子吸收光谱法测定某城区污泥中4种重金属元素

将采集的污泥样品晾干并碾碎至粒径为150μm的细粉,置于105℃温度条件下烘干4 h,称取烘干的样品,用硝酸-氢氟酸-高氯酸混合酸消解后,将溶液定容至250 mL容量瓶中。分取5.00 mL试液置于100 mL容量瓶中用硝酸(0.2+99.8)溶液定容至100 mL,用火焰原子吸收光谱法按所选仪器工作条件测定其中4种重金属元素锰、铜、镉及铅的含量。方法的检出限(2s)分别为0.006 5(锰),0.001 6(铜),0.001 9(镉)及0.020 7(铅)mg.L-1。用标准加入法做回收试验,测得回收率在92.3%~98.6%之间。     

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.     

火焰原子吸收光谱法测定氧化铝中杂质元素

普通氧化铝中杂质元素主要有钠、钾、硅、铁、钙、镁、锌、锰、铜、锂、钙等。在国家标准[1] 中 ,Ｎａ2 Ｏ、Ｋ2 Ｏ的分析采用火焰光度计法 ,Ｆｅ2 Ｏ3 的分析采用比色法 ,ＺｎＯ的分析采用原子吸收光谱法。国家标准中没有Ｌｉ2 Ｏ的分析方法 ,文献 [2 ]介绍了Ｌｉ2 Ｏ的分析方法。这些元素的测定采用了不同的溶样方法和测定方法 ,手续多 ,时间长 ,而且使用了三种分析仪器。本文采用ＨＣｌ溶样 ,加消电离剂 ,用空气 乙炔火焰连续测定氧化铝中五种元素的含量 ,取得了满意的结果。1　试验部分1.1　主要仪器与试剂岛津ＡＡ 6 80 0型原子吸收分…     

原子吸收光谱法测定烟叶中的重金属总量及形态分析

采用火焰原子吸收光谱法测定烟叶中Mn,Cu,Zn元素,石墨炉原子吸收光谱法测定Cd,Cr,Pb元素,以HNO3-H2O2微波消解法获取烟叶中的重金属总量,以超声水提取法获取水溶态重金属进行初级形态分析,以Tessier逐级提取法获取5种形态的重金属进行次级形态分析。实验结果表明,原子吸收光谱法检测6种重金属线性良好,相关系数(r2)不低于0.998 8,检出限为0.16~3.1μg·L-1。烟叶样品中Mn,Cu,Zn,Cd元素主要以可交换态和碳酸盐结合态的形式存在;Cr主要以残渣态的形式存在;而Pb主要以碳酸盐结合态和残渣态的形式存在。     

火焰原子吸收光谱法测定云母钛珠光颜料中6种重金属元素

采用硝酸+氢氟酸+盐酸混合酸消解样品,火焰原子吸收光谱法定云母钛珠光颜料中的Pb、Cd、Co、Cr、Cu、Ni 6种重金属元素的含量。各元素校正曲线的线性关系良好,相关系数均大于0.999,检出限在0.001 8～0.051 0mg/L。平行测定7次,各元素的相对标准偏差(RSD)均不大于1.3%。各元素在添加水平为0.5μg/mL时的回收率为88.9%～108%。方法获得了令人满意的测定效果,对云母钛珠光颜料中重金属含量的测定提供了可靠的分析方法。     

原子吸收光谱法测定植物叶中微量重金属

用浓硝酸与高氯酸混酸消解植物叶,其中铜、锌及锰含量较高,可直接用火焰原子吸收光谱法测定;铅、镉及铬含量较低,用石墨炉原子吸收光谱法测定;铅和镉含量甚微,受基体及共存元素干扰严重,用标准加入法消除干扰。     

火焰原子吸收光谱法测定高纯碳酸锂中多种杂质元素

采用火焰原子吸收光谱法测定了高纯碳酸锂中多种杂质元素（包括锌、钠、铅、钾、铁、钙及镁）的含量。结果表明：测定上述各元素的相对标准偏差（n=9）在1.9%～4.4%之间。各元素的工作曲线具有良好的线性关系,相关系数在0.9943至0.9998之间。用标准加入法做回收试验,测得平均回收率在98.3%至101.0%之间。     

离子交换预富集-火焰原子吸收光谱法测定地下水中重金属

建立了采用强酸性阳离子交换树脂富集与火焰原子吸收光谱法测定地下水中铜、钴、镍、镉、锌、铁、锰、铋、锑、铅等金属离子,讨论了洗脱剂类型、浓度、洗脱流速和阳离子交换树脂用量等对交换树脂富集效果的影响。结果表明,在交换柱内径为1.0cm,柱高为50cm,732#树脂用量为30ml,吸附速度为4.0ml·min-1时,用2.4mol·L-1盐酸以1.0ml·min-1的速度洗脱,可达到良好效果。该方法可同时测定地下水中痕量重金属元素,其加标回收率为97%～103%。     

原子吸收法对藏草药川木香中12种元素的初级形态分析

用原子吸收分光光度法,测定了产于青藏高原的藏草药川木香的全药材、水提液、醇提液中12种元素(Cr、Cu、Fe、Mn、Ni、Se、Zn、K、Ca、Mg、Cd、Pb)的含量,以及水提液中各元素可溶态、水溶态的含量,同时采取正辛醇-水分配体系模拟藏药水提液中各微量元素在人体胃肠中的分配情况,对藏药中微量元素的初级形态进行了分析,初步探讨了酸度变化(人体胃肠酸度)对微量元素的影响,结合藏药药效讨论其相关性,为进一步研究微量元素与藏药药性、药效的关系提供科学的依据和奠定基础.     

The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.     

火焰原子吸收光谱法测定软儿梨中微量元素

采用火焰原子吸收光谱法测定了软儿梨果肉和果汁中K、Mg、Fe、Ca、Mn、Cu、Zn的含量.样品以HNO3-HClO4消解,对消解和仪器测定条件进行了优化选择,建立了相应的原子吸收光谱测定方法.方法的RSD在1.0%～3.0%之间,加标回收率在90%～100%之间.     

火焰原子吸收法测定鸡尾木中无机元素的含量

鸡尾木(ExcoecariaVenenataS.LeeetF.N.Wei)属大戟科,海漆属,为民间药用珍贵植物,用于治疗牛皮癣、慢性湿疹等,疗效颇佳[1]。鸡尾木中无机元素,尤其是医学微量元素的测定对其药理效的研究有重要的参考价值。1　实验部分1 1　仪器及试剂TAS 986原子吸收分光光度计(北京普析通用仪器有限责任公司);空心阴极灯:Fe、Cu、Ni、Cr、Cd、Zn、Co、Ba、Ca(北京瑞利普光电器厂);Mg、Pb(北京真空电子技术总公司);Mn(北京市朝阳天宫电器厂);AdventurerTM电子天平(奥豪斯国际贸易〈上海〉有限公司)。标准储备液:配制Zn2+、Mg2+、Fe3+、Mn2…     

ICP-OES法与石墨炉原子吸收法测定饮用水中重金属元素比较

通过对比电感耦合等离子体发射光谱法(ICP-OES)与石墨炉原子吸收法(AAS)测定水中重金属的检出限、重复性、加标回收率等实验,验证两种方法的准确性,从而为饮用水中重金属的测定提供可靠的方法。结果表明,石墨炉原子吸收法测定饮用水中砷、镉、铬、铅、汞、硒检出限均低于ICP-OES法,但ICP-OES法测定线性范围宽,重复性和加标回收率均优于石墨炉原子吸收法,分析速度快,操作便捷,结果满意,是目前饮用水中重金属的测定非常可靠的方法。     

混凝土中重金属元素溶出量的质谱分析

利用带八极杆碰撞/反应池和屏蔽炬技术的电感耦合等离子体质谱直接测定混凝土中Cr,Mn,Ni,Cu,Zn,As,Cd,Sn,Sb,Pb等多种重金属元素的溶出量。通过向碰撞池中引入氢气和氦气消除多元素分子离子的干扰,以50μg/L的Ge,In,Tb为内标元素校正基体干扰和漂移。10种待测元素的检出限为0.001～0.033μg/L,相对标准偏差为0.85%～2.8%,样品的加标回收率在91.1%～103.9%之间。     

Determination of inorganic and methylmercury in fish by cold vapor atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry

Simple and rapid analytical procedures for the determination of Hg²⁺ and methylmercury in fish were proposed after careful optimization of chemical and instrumental parameters for Hg measurement by cold vapor (CV)/hydride generation (HG) atomic absorption spectrometry (AAS) and CV/HG inductively coupled plasma atomic emission spectrometry (ICP-AES). Quantitative extraction of Hg species avoiding any inter-species conversion was achieved by fast microwave assisted solubilization of fish tissue with relatively low amount of tetramethylammonium hydroxide (TMAH) or 6 mol L^− 1 HCl. After careful optimization of chemical parameters selective determination of Hg²⁺ in the presence of excess of methylmercury is attained by using continuous flow CV AAS, 1% m/V SnCl₂ as reductant and 0.1 mol L^− 1 HCl as reaction medium. Simple calibration curve prepared with aqueous standard of Hg²⁺ is recommended for its quantification. Both Hg²⁺ and methylmercury could be determined simultaneously with equal sensitivity by CV/HG ICP-AES directly in the diluted TMAH solution obtained after extraction with 1% m/V NaBH₄ as reductant. Quantification of the sum of Hg²⁺ and methylmercury against calibration curve prepared with aqueous standard of methylmercury is suggested. It should be mentioned that batch hydride generation system with quartz tube heated in air/acetylene flame could also be used for simultaneous determination of both Hg species in fish extracts, with standard additions calibration. The validity of the developed analytical procedures for selective determination of Hg²⁺ and methylmercury (by difference between the total Hg and Hg²⁺) is confirmed by the analyses of certified reference material DOLT-1 and reference material IMEP-20. Very close agreement between certified values and analytical results was found.     

原子吸收法对藏草药水母雪兔子和多刺绿绒蒿中12种元素的初步形态分析

用原子吸收光谱法,对产于青藏高原的藏草药水母雪兔子和多刺绿绒蒿,测定了全药材、水提液、醇提液中12种元素(Cr、Cu、Fe、Mn、Ni、Se、Zn、K、Ca、Mg、Cd、Pb)的含量,以及水提液中各元素可溶态、水溶态的含量,同时采取正辛醇-水分配体系模拟藏药水提液中各微量元素在人体胃肠中的分配情况,对藏药中微量元素的初级形态进行了分析,初步探讨了酸度变化(人体胃肠酸度)对微量元素的影响,结合藏药药效讨论其相关性,为进一步研究微量元素与藏药药性、药效的关系提供科学依据.     

Arsenic speciation in natural water samples by coprecipitation-hydride generation atomic absorption spectrometry combination

A speciation procedure for As(III) and As(V) ions in environmental samples has been presented. As(V) was quantitatively recovered on aluminum hydroxide precipitate. After oxidation of As(III) by using dilute KMnO₄, the developed coprecipitation was applied to determination of total arsenic. Arsenic(III) was calculated as the difference between the total arsenic content and As(V) content. The determination of arsenic levels was performed by hydride generation atomic absorption spectrometry (HG-AAS). The analytical conditions for the quantitative recoveries of As(V) including pH, amount of aluminum as carrier element and sample volume, etc. on the presented coprecipitation system were investigated. The effects of some alkaline, earth alkaline, metal ions and also some anions were also examined. Preconcentration factor was calculated as 25. The detection limits (LOD) based on three times sigma of the blank (N: 21) for As(V) was 0.012 μg L⁻¹. The satisfactory results for the analysis of arsenic in NIST SRM 2711 Montana soil and LGC 6010 Hard drinking water certified reference materials for the validation of the method was obtained. The presented procedure was successfully applied to real samples including natural waters for arsenic speciation.     

Speciation of chromium in river water samples contaminated with leather effluents by flame atomic absorption spectrometry after separation/preconcentration by cloud point extraction

In the present work, a cloud point extraction (CPE) system has been proposed for determination of species de chromium in the natural water samples, Cr(III) and Cr(VI). The procedure was based on the reaction of Cr(III) with 1-(2-pyridilazo)-2-naphtol (PAN) in a surfactant solution (Triton X-114) yielding a hydrophobic complex, which then is entrapped “in situ” in the surfactant micelles. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of Cr(III)-PAN entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Separation of the two phases was accomplished by centrifugation for 15 min at 2500 rpm. The Cr(VI) assay is based on its reduction to Cr(III) by ascorbic acid which subsequently reacts with PAN in a similar manner. The main factors affecting the cloud point extraction, such as complexation pH (7.7), buffer concentration (0.025 mol L^{− 1}) and microwave irradiation time (10 min) were optimized by response surface methodology (RSM) using Box–Behnken design. Under the optimized conditions, the preconcentration system (50 mL sample) permitted an enrichment factor of 48, linear range of 2.5–80 μg L^{− 1}, limit of detection and quantification of 0.7 and 2.5 μg L^{− 1}, respectively, and the relative standard deviation (n = 10) of 2.0% for 50 μg L^{− 1} Cr(III) solution and (n = 10) 5.5% for 10 μg L^{− 1}. The proposed procedure was applied to the speciation of chromium in river water samples. The procedure affords recoveries of 84–115% and a relative standard deviation lower than 4.2%. The analytical results of total chromium in the river water samples under study agreed well with those by electrothermal atomic absorption spectrometry (ET AAS). It is proved that the procedure can be successfully employed as an alternative to the commonly used preconcentration and speciation analytical techniques.