火焰和石墨炉原子吸收法联用改善试金分析的检出限

在泡沫吸附原子吸收法试金分析中,用火焰原子吸收法测定含量大于0.3μg/g的金量,用石墨炉原子吸收法测定含量为0.05~0.3μg/g的金量,通过加入基体改进剂和优化测定条件,使一次处理的样品能用于二者的分析,从而节省测试工作量。方法的准确度及精密度均能达到行业要求。     

Coprecipitation with Cu(II)‐4‐(2‐Pyridylazo)‐resorcinol for Separation and Preconcentration of Fe(III) and Ni(II) in Water and Food Samples

The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L^?1 for Fe(III) and 0.43 µg L^?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.     

Dispersive Liquid–Liquid Microextraction for Preconcentration and Determination of Nickel in Water

A method for the determination of nickel in water was developed. The procedure involves preconcentration of nickel by using dispersive liquid–liquid microextraction. The Ni(II) ions were extracted in chloroform in the form of complex with the reagent 2‐(2′‐benzothiazolylazo)‐p‐cresol. Ethanol was used as the disperser solvent. After injection of the extracting mixture in a solution of nickel, a cloudy mixture was observed. A quick centrifugation induces phase separation and thus the settling of rich phase. The nickel content in the rich phase is measured by flame atomic absorption spectrometry. Under optimal conditions, the limit of detection and quantification obtained were 1.4 and 4.7 µg L^?1, respectively. Some parameters used to characterize preconcentration systems, such as enrichment factor and consumption index were calculated and resulted in 29 and 0.34 mL, respectively. After optimization of variables and determination of analytical characteristics, the method was used for the analysis of certified reference materials (BCR‐713: wastewater, effluent and BCR‐414: plankton) and real water samples.     

导数-原子捕集联用火焰原子吸收法测定粉煤灰中镉

研究并提出了将测定信号变化率的导数技术和浓缩待测原子的原子捕集技术与火焰原子吸收相联用于测定痕量镉的新技术.通过测定标准粉煤灰GBW08401和82201中痕量镉含量验证了该技术的可行性.与常规法相比,新方法的灵敏度和检出限可分别改善2～3个数量级和1～2个数量级(1～3分钟捕集条件下).10次测定的相对偏差为6.26%～7.23%,回收率可达95%～104%.研究表明,此技术可成功地测定粉煤灰中的痕量镉.     

沉淀分离－火焰原子吸收光谱法连续测定锌精矿中杂质元素

利用Ｚｎ（ＯＨ）＿２的两性沉淀富集待测杂质元素，分离高含量Ｚｎ以排除干扰，用火焰原子吸收法测定其中的杂质元素含量。实验结果表明：分离后残留的Ｚｎ对Ｆｅ、Ｃｄ、Ｎｉ、Ｍｎ、Ａｇ的测定无干扰；各元素之间互不干扰。加标回收率为９３％～１０６％，对菱锌矿中几种杂质元素进行测定，结果与ＩＣＰ－ＡＥＳ法相符，各元素测定的相对标准偏差（ｎ＝１２）为４．１％～８．８％。     

火焰原子吸收光谱法测定南丰蜜桔叶片中的微量元素

采用火焰原子吸收光谱法对南丰蜜桔叶片中的Cu,Zn,Mn,Fe,Co等5种元素的含量进行了测定,其方法简便、精密度高和灵敏度高。详细的研究了消解酸的种类、HNO3和HF的比例、消解酸的体积及消解时间对测定结果的影响。测定结果表明,南丰蜜桔叶片中铁和锌的含量较高。     

流动注射在线置换吸附预富集与火焰原子吸收联用分析地质样品中痕量银

介绍了应用编结反应器为吸附介质,流动注射在线置换吸附预富集消除Fe、Ca、Mn、Pb等共存金属离子的影响,与火焰原子吸收联用分析痕量银的方法,Ag(Ⅰ)吸收信号峰高比直喷时增感26倍,检出限为0.60μg/g。方法用于国家一级地质标准物质中Ag的测定,结果与标准值相符,5次测定的RSD≤4.8%。     

磷酸三丁酯醋酸纤维富集－火焰原子吸收法测定地质样品中痕量金

在５％～４０％王水介质中，用磷酸三丁酯（ＴＢＰ）－醋酸纤维吸附富集Ａｕ，被吸附的Ａｕ用热硫脲溶液解脱，火焰原子吸收法测定。Ａｕ的回收率大于９８％，方法简便快速，经地质标样分析验证结果可靠。     

含油岩石的荧光特征研究

在紫外光照射下,很多有机物质和部分无机物质能够发出不同颜色和亮度的荧光。本文研究了含油岩芯中岩石矿物的荧光特征,指出采用氯仿（或乙烷）试剂浸泡岩样是区别岩石矿物荧光的有效方法。本文着重对含油岩芯中有机质组成以及有机组分与荧光颜色的关系进行了深入的探讨,指出依据含油岩芯的荧光颜色可以进行油气水层的荧光解释。     

C18键合硅胶柱在线富集/FIA-FAAS系统测定海水中痕量重金属

基于8-羟基喹啉金属螯合物在C_(18)键合硅胶上的吸附原理,在海水样品中加入少量8-羟基喹啉溶液,建立在线C_(18)键合硅胶柱富集,甲醇洗脱,洗脱液直接进入火焰的流动注射-火焰原子吸收光谱系统(FIA-FAAS)测定海水中痕量Cu,Ni,Cd和Zn的方法。富集倍数达80,进样频率为每小时30次。对Cu Ni,Cd和Zn测定的特征浓度分别为0.30,0.26,0.12和0.07μg/L;检出限(2σ)分别为0.07,0.05,0.02和0.01μg/L;相对标准偏差分别为2.7,2.1,2.8和2.5％;回收率分别为102,98,96和102％。本法快速简便,污染少,灵敏度高。