元素在石墨炉内石墨探针表面上的原子化机理研究 ⅩⅢ.钼的原子化机理

本文应用x-射线衍射(XRD)、X-射线光电子能谱(XPS)、俄歇电子能谱(AES)、扫描电子显微技术(SEM)研究了钼酸铵在石墨炉内石墨探针表面上的原子化机理。实验结果表明,在温度<1350K时,钼酸铵经历MoO_3和Mo_4O_(11)中间产物转变为MoO_2(s)。在更高温度下,MoO_2(s)首先还原为Mo_2C,而后进一步转变为MoC(s)。MoC再分解为Mo(s)。钼的原子化起源于Mo的升华。     

A metallic furnace atomizer in hydride generation atomic absorption spectrometry: Determination of bismuth and selenium

A flow injection hydride generation system with a metal furnace atomizer (Inconel 600® alloy) was employed for Bi and Se determination. The presented methods have linear ranges up to 200 and 500 μg L^− 1 for Bi and Se, respectively, with good linearities (r² = 0.9997 and 0.9974, respectively). The limits of quantification obtained according to IUPAC recommendations were 2.3 μg L^− 1 for Bi and 6 μg L^− 1 for Se, and the relative standard deviations (N = 6) based on Bi and Se analytical responses from real samples were 2.7% and 10%, respectively. Accuracy evaluations were based on certified materials such as SRM 361, SRM 363, and SRM 364 (steel alloys) for Bi, Mess-3 (marine sediment), SRM 397 (human hair), and Bio-Rad2 — 69042 (urine) for Se. Good agreements between the results were obtained at the 95% confidence level, according to the t-test.     

石墨炉原子吸收法测定土壤中铅、镉、钴、锑、铍

建立石墨炉原子吸收法测定土壤中铅、镉、钴、锑、铍含量的方法。优化了石墨炉原子吸收光谱法测定条件,在最佳实验条件下,采用硝酸-盐酸-氢氟酸-双氧水混合酸体系微波消解土壤样品,选用抗坏血酸-硝酸镁混合溶液为基体改进剂。铅、镉、钴、锑、铍的质量浓度在各自的范围内与吸光度成良好的线性关系,相关系数均大于0.999,各元素的检出限为0.008~0.06 μg/g。样品加标回收率为90.5%~104.0%,测定结果的相对标准偏差均小于2.5%(n=6)。该方法样品前处理简便,灵敏度高,检出限低,测定结果准确、可靠,可用于土壤中铅、镉、钴、锑、铍的测定。     

含油污泥的热解特性研究

利用热重 傅里叶变换红外光谱联用仪与管式电阻炉对含油污泥热解特性进行了研究,分析了热解过程及影响因素（污泥性质与升温速率）,并由气体析出特性研究了热解机理。结果表明,热解过程包括水分挥发、轻质油挥发、重质油热解、半焦炭化与矿物质分解五种反应,矿物油反应集中发生在220℃～480℃。污泥性质影响因素中,产生环节最为显著,罐底泥、污水污泥失重明显而落地油泥失重不明显,矿物质组分含量越高,挥发分转化率越低;而污泥的油源基属影响较小。升温速率越大,反应进行的越快,挥发分转化率降低。热解机理包括矿物油含氧官能团裂解,链烃及侧链上的断链,环化、芳构化以及缩合脱氢。     

电热蒸发进样—等离子体原子发射光谱中钒和钛的蒸发机理研究

自1974年Nixon报道钽丝电热蒸发作为ICP-AES进样技术以来,这一技术已引起了人们的极大兴趣,受到越来越广泛的重视。电热蒸发(ETV)-ICP-AES是一种将蒸发和激发分步进行的联用技术。石墨是目前普遍使用的蒸发器材料。然而,在高温下某些元素和石墨材料可以发生碳化反应,形成热稳定的碳化物,使分析物蒸发不完全或根本不蒸发,从而影响分析结果的灵敏度和准确性。为了解决这一问题,我们曾提出了以聚四氟乙烯(PTFE)悬浮体为氟化剂,氟化辅助ETV-ICP-AES直接测定粉煤标样中钒和钛的新方法,其检出限     

Determination of fluoride in complex liquid matrices by electrothermal atomic absorption spectrometry with in-furnace oxygen-assisted ashing

A new chemical method is reported for the determination of total fluoride in complex liquids and suspensions, such as fruit juices, urine, serum and blood. It is based on the formation of the A1F radical in a graphite furnace afterin situ oxygen-assisted ashing of the untreated sample. The absorbance of this radical is measured at 227.45 nm. The method is relatively easy to use and provides a low detection limit (14 ng/ml) and reasonable reproducibility (5–10%).     

Neutral oxygen atom density in the MESOX air plasma solar furnace facility

The density of neutral oxygen atoms in the MESOX set-up, one device of the PROMES-CNRS solar facilities, was determined by a fiber-optics catalytic probe (FOCP). Plasma was created in a flowing air within a quartz tube with the outer diameter of 5 cm by a 2.45 GHz microwave generator with the output power up to 1000 W. The flow of air was varied between 4 and 20 l/h. The O-atom density was found to increase monotonously with the increasing discharge power, and it decreased with the increasing flow rate. The degree of dissociation of oxygen molecules in the plasma column depended largely on the flow rate. At the air flow of 4 l/h it was about 80% but it decreased to about 20% at the flow of 20 l/h.     

析相微萃取-石墨炉原子吸收法测定地质样品中痕量金

以MIBK为络合剂和提取剂,乙醇为助溶剂,建立了析相微萃取-石墨炉原子吸收法测定地质样品中痕量金的分析方法。详细探讨了金的不同析相微萃取体系的特性及析相规律,优化了金-MIBK体系的最佳析相微萃取条件及石墨炉升温程序。所建立的方法线性范围为0.006~1.0μg/L,检出限为0.0013μg/L,相对标准偏差为1.5%(n=11),用于国家地质标准参考物质(GBW07289)的测定,分析结果与推荐值吻合。     

溶膜预富集-石墨炉原子吸收法测定痕量钯

强酸性条件下 ,钯 (Ⅱ )与 5 [( 5 氯 2 吡啶 )偶氮 ] 2 ,4 二氨基甲苯 ( 5 Cl PADAT)生成紫红色螯合物 ,该螯合物可与十二烷基苯磺酸钠 (SDBS)生成离子缔合物 ,离子缔合物经 0 .3μm孔径的硝化纤维微孔滤膜富集后 ,于小体积 ( 0 .5mL)的浓硫酸中溶膜 ,用石墨炉原子吸收法 (GFAAS)测定 ,富集倍数可达 2 0 0倍 ,钯含量在 4.69× 1 0 - 1 2 ～ 7.0 9× 1 0 - 9mol/L范围内线性良好 ,检出限为 1 .78×1 0 - 1 2 mol/L。方法用于海水中痕量钯的测定。     

石墨炉原子吸收法测定化妆品中的砷

在过氧化氢溶液及硝酸镍存在下，用石墨炉原子吸收法测定化妆品中砷的含量，砷的浓度在0-1mg/L时与吸光度线相关，线性方程为A=0.838c 0.003，相关系数为0.99994。对液体和固体化妆品中的砷进行测定，砷的加标回收率为98.3%-98.7%，测定结果的相对标准偏差为0.65%-1.50%。