蜡笔中痕量铅的测定

用铋膜电极替代汞膜电极电位溶出法测定痕量重金属铅。研究了同位镀铋膜及测定条件。铅在以HAc- Na Ac为支持电解质的铋膜电极上可得到灵敏的电位溶出峰 ,线性方程为 :I=0 .0 6 0 9m 0 .0 0 0 3,相关系数 :r=0 .9986 ,检出限为 9.0× 1 0 -8g/ L,线性范围为 0 .1— 9× 1 0 -3 g/ L,RSD为 3.89%。采用加热和加速浸提法处理蜡笔 ,铋膜电极溶出法测定了蜡笔中铅的含量 ,该法简单快速 ,准确度和精密度均符合要求 ,回收率为 98.1 %— 1 0 1 %。     

铋膜电极溶出伏安法测定苍耳子中锌的含量

采用电位溶出法,用铋膜电极替代汞膜电极对中药苍耳子中微量元素锌的测定作了研究,考察了同位镀铋膜及测定微量元素锌的条件。实验结果表明：锌在以KSCN为支持电解质的铋膜电极上可得到灵敏的电位溶出峰,线性方程为：为I=2.0062C＋0.0069,相关系数为r=0.9967,检出限为6.0×10-8g/L线性范围为0.5×10-6—2.8×10-6mol/L,RSD=2.24%。该法简单快速,准确度和精密度均符合要求,回收率为89.5%—100.3%。     

铋膜电极差分脉冲溶出伏安法测定镉

用铋膜电极对水样中的Cd2+进行了差分脉冲溶出伏安法检测.观察并优化了采用同位镀铋法测定水样中的镉离子时的影响条件.结果显示:镉可以在铋膜电极上得到灵敏的电位溶出峰.加入1/15mol/L的NazHPO4-KH2PO4缓冲液(pH7.5),在1.1V电压下富集300s,镉的检测下限达到0.1μg/L,在1-120μg/L内呈现良好的线性关系.每次使用完可方便的将电极上残留的镉和铋溶出,从而使得各次检测具有良好的重现性.     

铋、氧化铋、硫化铋在硝酸-硫脲中的溶解性

研究了铋、氧化铋、硫化铋在硝酸-硫脲中的溶解性。三价铋离子与硫脲溶液可形成黄色络合物,在波长为460nm处,反应温度为25℃,反应时间为6min,硝酸浓度为1.0mol/L,硫脲浓度为0.5mol/L,振荡速率为160r/min条件下铋含量在0.059—4.57μg/mL范围内服从郎伯-比尔定律,检出限为m=0.04μg。铋矿物的溶解性顺序大小为Bi2O3>Bi>Bi₂S₃。本方法操作简便,可靠,实验结果满意,具有广泛的实用意义。     

ICP-MS测定中药煎制前后8种重金属元素的含量及溶出率

建立电感耦合等离子体-质谱法(ICP-MS)测定5种药材及其水煎液中8种重金属元素Pb、Cd、Cr、Cu、As、Hg、Sb、Sn含量的方法。使用微波消解处理样品,研究并优化了微波消解条件,对电感耦合等离子体-质谱仪的各项技术参数进行了选择。方法表明,8种元素的检出限小于等于0.003μg/L,精密度在1.3%—3.0%,药材加标回收率在93.6%—100.2%,药材水煎液加标回收率在94.2%—103.5%,煎煮前后药材重金属溶出率0%—33.33%,表明中药煎煮过程重金属元素不易溶出。     

铋膜电极差分脉冲溶出伏安法测定痕量镉

研究了用铋膜电极测定痕量重金属元素镉的差分脉冲溶出伏安法,并对实验条件进行了优化。结果表明：铋膜电极可以获得和汞膜电极类似的良好溶出峰,且电极重现性好。在优化的实验条件下,镉离子的氧化峰电流与镉离子的浓度在10—440μg.L-1的范围内呈线性关系,检出限为4.66μg.L-1。铋膜电极优异的电化学性能加上低毒性,使其可以用来测定环境和工业中的镉。     

氢化物原子荧光光度法测定水中硒方法的改进

考察适于本地区水中硒含量测定的方法。参考国家标准的生活饮用水检验方法(GB/T5750—2006),对本地区的水质进行了多次的检测。不加入掩蔽剂有良好的线性关系,r=0.9996,RSD=1.87%,DL=0.28μg/L,回收率为97.5%—103.8%。硒的含量在0—50μg/L之间。该方法简捷,易于掌握,灵敏度高,稳定,准确。     

分散液液微萃取-分光光度法测定环境水样中孔雀石绿

建立了简便、快速、有效的分散液液微萃取-分光光度法测定环境水样中孔雀石绿的分析方法。对萃取剂、分散剂的种类和体积、萃取时间、离心时间、盐浓度等影响萃取效率的因素进行了优化。在优化的萃取条件下,方法的线性范围为8—1000μg/L（r=0.9992）,相对标准偏差（RSD）为4.1%（C=100μg/L,n=6）,检出限为4.20μg/L。对3种实际水样中的孔雀石绿进行测定,加标回收率在74.7%—108.2%之间（n=5）。方法适用于环境水样中的痕量孔雀石绿的检测。     

原子荧光光谱法测定土壤中的砷

应用原子荧光光谱法测定砷的含量。以深层生土、地表熟土为样品,采用顺序注射氢化物发生-原子荧光光谱法进行测定。在最佳实验条件下,方法的线性范围在2—60μg/L以内,相关系数r=0.9993,检出限为0.16μg/L,测定标准溶液的RSD为1.6%(n=11),样品加标回收率为96.5%—103.5%,方法简单、快速,可测定土壤中的砷。     

浊点萃取-GFAAS测定水中铬的形态

在Triton X-114溶液中,当加热至其浊点温度时,溶液分为两相,Cr(Ⅵ)-DDTC络合物进入非离子表面活性剂相,从而实现与Cr(Ⅲ)的分离,利用石墨炉原子吸收光谱法测定了水中不同形态的铬.方法详细探讨了溶液pH、试剂浓度等实验条件对浊点萃取及测定灵敏度的影响.在最优实验条件下,Cr(Ⅵ)的检出限为0.081μg/L;相对标准偏差为2.57%(C=1.0μg/L,n=6).本方法具有简便、安全、低毒、高效等优点.     

Strain induced epitaxial relationships of Cr on Co/Pd(111)

The growth and structure of Co ultra-thin films on Pd(111) and Cr on Co/Pd(111) have been analyzed by grazing incidence X-ray diffraction and low energy electron diffraction. It is shown that the in-plane lattice constant of the epitaxial Co film depends on the growth temperature. Although the strain decreases as a function of the Co film thickness, it persists for 20 monolayer (ML) films or even thicker. When Cr is deposited at room temperature on a strained Co film (10 to 20 ML thick) a Kurdjumov–Sachs epitaxial relationship is observed, whereas when Cr is deposited on a Co(0001) single-crystal or on a very thick Co film on Pd(111), a Nishyama–Wassermann orientation is obtained.     

Test investigation on interfacial characteristics of Cr/Al nanofilms structure

The objective of this paper is to provide a systematic test for fabrication or evaluation of a bilayer film structure between Cr and Al in micro/nanoelectronic manufacturing. The Cr/Al bilayer film is fabricated by using the magnetron sputtering. To understand the basic mechanical properties of the Cr/Al bilayer films, the elastic modulus and the hardness of the sample are investigated by using a nanoindenter test. The test can show the changing trend of the Cr/Al sample structure. To investigate the integrating characteristics of the sample in progress, the effect of the thermal cycling loading and no-thermal cycling loading on the integrating force of the Cr/Al samples is tested by using nanoscratch. The interfacial binding force in the films can be obtained for understanding the integrating characteristics. It builds a basis for future work on progress investigation of physical property of Cr/Al bilayer film structure.     

涂层界面结合强度检测研究(Ⅰ):涂层结合界面应力的理论分析

利用激光划痕测试法和弯曲应力理论，建立了涂层结合界面应力的理论模型，推导出结合界面剪应力、正应力和剥离应力分布公式，分析了结合界面应力产生的机理.理论分析结果表明，界面正应力主要集中在界面中心区域内，而在界面边缘附近，正应力迅速下降，在界面边缘处其值降为0；剪应力和剥离应力主要集中在界面边缘区域内，在远离界面边缘区域，剪应力和剥离应力则迅速下降；涂层中正应力和涂层厚度、基体厚度以及杨氏模量无关，界面间剪应力以及剥离应力随涂层厚度增加而增加，并且由涂层与基体厚度以及杨氏模量所共同决定.     

Direct evidence for compositional fluctuation in sputtered Co-Cr thin films

Nano-scale concentration fluctuations in sputtered Co-23 at% Cr magnetic thin films were analyzed by atom probe field ion microscopy (APFIM). The atom probe concentration depth profile obtained from the film which was deposited on the W tip at 200°C clearly showed that the composition fluctuated significantly. The concentration of the Cr enriched region was in the range of 30–40 at% Cr, while that of the Cr depleted region was in the range of 5–10 at% Cr. This result proves that compositional fluctuations are present inside the grains of the Co-Cr sputtered film as suggested by the TEM observation of the chrysanthemum-like pattern (CP) structure.     

Study of the early stages of Cr/6H-SiC(0 0 0 1) interface formation

The early stages of the Cr/6H-SiC(0 0 0 1) interface formation at room temperature were investigated using XPS, LEED and work function (WF) measurements. Upon stepwise Cr evaporation in UHV up to a thickness of 5-10 monolayers (ML) at RT, the binding energy of the XPS Cr 2p_3/2 core level peak shifted from 576.1 eV, at submonolayer coverage, to 574.7 eV (corresponding to metallic Cr) for the final Cr deposit, while the binding energies of the substrate XPS core level peaks remained stable. The WF exhibited a steep decrease of about 0.5 eV from the initial SiC substrate value, upon submonolayer coverage, but then increased gradually to saturation at a value of about 4.8 eV (polycrystalline Cr film with some chemisorbed oxygen). The growth of the ultrathin film was via 3D-cluster formation. The height of the Schottky barrier for the Cr/6H-SiC(0 0 0 1) contact was found by XPS to be 0.5 ± 0.1 eV. The results, generally, indicate the absence of any extended interfacial silicide-like interaction at RT.     

Coexistence of two different Cr ions by self-doping in half-metallic CrO2 nanorods

We investigated the physical properties of Cr ions in half-metallic CrO(2) using 53Cr nuclear magnetic resonance (NMR). The 53Cr NMR spectra showed two peaks with a similar intensity instead of the single peak anticipated from a uniform single valence Cr(+4). Both Cr peaks exhibited a strong anisotropy in the hyperfine field and similar values in the enhancement factor and T2 relaxation time. These results suggest the coexistence of two different Cr ions (provisionally, Cr(+4 +/- 1/3)) by a self-doping effect, which is a likely origin of the metallic ferromagnetism in CrO(2).     

Effect of Cr and V dopants on the chemical stability of AZO thin film

The effect of the dopants of Cr and V on the optoelectronic properties of AZO thin film by pulsed DC magnetron sputtering has been investigated. We also use HCl and KOH solutions to conduct the chemical stability of AZO:Cr:V thin film. The experimental results show that the optimum AZO optoelectronic properties without Cr and V doping obtain the resistivity of 9.87 × 10⁻⁴ Ω cm, optical transmittance of 84% and surface roughness rms value of 2.6 nm. The chemical stability of AZO will increase after Cr and V doping. Under the added V = 0.19 wt.%, Cr = 0.56 wt.%, AZO:Cr:V thin film showed 52% increased chemical stability and 128% decrease in surface roughness after etching (the resistivity was 3.62 × 10⁻³ Ω cm and optical transmittance 81%). From the experimental results, the higher resistivity obtained after KOH etching compared with after HCl etching. The reason is that the Zn/Al ratio will reduce after etching and cause the AZO film carrier density to reduce as well. However, the optical transmittance obtained after KOH etching will be higher than that after HCl etching. This is because that a better surface roughness after KOH etching obtained than after HCl etching.     

Wave reflection and transmission from a thin film with one-dimensional disorder

This paper deals with a TE plane wave reflection and transmission from a thin film with one-dimensional disorder by means of the stochastic functional approach. The relative permittivity of the thin film is written by a Gaussian random field in the horizontal direction with infinite extent, and is uniform in the vertical direction with finite thickness. Arandomwavefield is obtained in terms of a Wiener-Hermite expansion representation with approximate expansion coefficients (Wiener kernels) under a small fluctuation case. For a SiC thin film and a glass thin film having one-dimensional disorder with Gaussian correlation or an exponential correlation, numerical examples of the first-order incoherent scattering cross section and the optical theorem are illustrated in the figures. It is then found that ripples and four major peaks appear in angular distributions of the incoherent scattering. Such four peaks may occur in the directions of forward scattering, specular reflection, backscattering and in the symmetrical direction of forward scattering with respect to the normal to surface of the thin film. Physical processes that yield such ripples and peaks are discussed.