原子吸收光谱法测定人体血清中的微量元素锌、铜、铁、钙和镁

本法不需要消解样品,样品经分离稀释后,直接用火焰原子吸收光谱法测定人体血清中的锌、铜、铁、钙和镁5种微量元素的含量。该方法简便,快速,精密度高,相对标准偏差(RSD≤8.52%)回收率在95%—100%之间。结果准确可靠。     

混合熔剂半熔ICP-AES测定天青石矿中的锶、钡、钙、镁和铁

在最佳仪器条件下,样品用混合熔剂半熔,于10%王水介质中测定天青石中的锶、钡、钙、镁、铁含量,其最终结果与现行国家标准方法测得结果一致。     

火焰原子吸收光谱法测定阳春砂仁中铜、锌、锰和铁

样品经灰化处理后,用火焰原子吸收光谱法测定样品中铜、锌、锰和铁的含量,平均加标回收率为85.5%-99.4%,相对标准偏差(RSD)为1.70%-2.70%.在给定范围内呈现良好的线性关系,相关系数大于0.998,方法简便,快速,结果可靠.     

土壤中铅、砷、铬、铜和锌含量的连续快速测定

建立了土壤中铅、砷、铬、铜和锌含量的连续快速测定方法。土壤样品经微波消解,用同一份消解液,分别连续测定土壤中的铅、砷、铬、铜和锌含量,铬、铜和锌采用火焰原子吸收光谱法,铅和砷采用氢化物发生-原子荧光光谱法。采用本方法,对环境土壤标准样品ESS-1黑钙土(GSBZ50011)和ESS-3红壤(GSBZ50013)进行多次测定,检测结果与标样的推荐值吻合。经统计计算,回收率为95.2%—103.6%,精密度RSD均小于7%。本法操作简单快速,光谱测定结果已成功地用于无公害水果和蔬菜生产基地的土壤环境质量评价。     

石墨炉原子吸收法测定大气降水中的铜、铅和镉

用石墨炉原子吸收法连续测定大气降水中的铜、铅、镉 3种重金属的含量。降水样品经酸化处理后 ,直接进行测定 ,Cu、Pb、Cd的检出限在 0 .18— 1.12 pg范围内 ,精密度 (RSD) <2 .5 % ,标准加入回收率在10 0 .8%— 10 6.0 % ,方法简便、快速、准确 ,已用于黄海与东海海域的大批降水样品的测定 ,结果令人满意     

黑龙江膜荚黄芪多糖及微量元素Fe、Zn、Cu和Mn的测定

采用水提醇沉法制备黄芪多糖提取物,苯酚-硫酸分光光度法测定多糖的含量,在0.00-0.14mg/mL线性范围内具有良好的线性关系,回收率在94.81%-103.50%.测定黄芪多糖含量为4.3%.采用校准曲线法,用空气-乙炔火焰原子吸收光谱法测定样品中Fe、Zn、Cu和Mn的含量,膜荚黄芪中微量元素含量较高.     

近红外光谱法非破坏性测定黄豆籽粒中蛋白质、脂肪含量

采用傅里叶近红外漫反射光谱非破坏性分析 ,能够提供完整籽粒黄豆样品成分的含量信息 ,结合偏最小二乘回归法 (PartialLeast Squares,PLS) ,以 39个不同品种的完整籽粒黄豆样品建立蛋白质和脂肪含量近红外定量分析模型 ,其中蛋白质、脂肪含量分析模型的测定系数R2 分别为 99 30 ,97 5 2 ,相对标准偏差RSD分别为 0 76 %和 1 3% ,检验集的化学值与模型预测值的相关系数r分别为 0 94 73,0 86 95。用所建模型对 2 6 4个不同品种的黄豆样品进行预测 ,并采用R error指标来估计分析结果的误差 ,其中蛋白质和脂肪模型预测的最小相对误差分别为 0 0 4 %和 2 4 6 % ,最大相对误差分别为 2 4 5 %和 4 2 5 %。该结果对育种过程中的早代筛选工作有重要意义     

微波消解-石墨炉原子吸收法测定汽油中的锰

用微波消解方法处理汽油样品,石墨炉原子吸收光谱法测定汽油中锰含量,建立了用微波消解-石墨炉原子吸收光谱法测定汽油中锰含量的新方法。用正交试验法考察了消解时间、温度、微波功率和酸度对消解效果的影响,确定了最佳微波消解条件。研究结果显示：测定汽油样品中锰含量时相对标准偏差（n=11）≤4.12%,加标回收率在96.5%—110.2%之间。方法具有测定精密度好、样品用量少、操作简单、环境友好等优点,可用于汽油样品中锰含量的测定。     

高氯酸萃取-连续流动法测定烟草中的淀粉含量

淀粉是烟草中较难测定的成分之一.为了快速准确地测定烟草中的淀粉含量,研究了高氯酸萃取-连续流动法测定烟样中淀粉含量的方法,即每0.1g烟草样品用1.0mL 50%的乙醇和1.2mL 72%高氯酸萃取烟草样品中的淀粉,通过自动化学分析仪(滤光片波长660nm)测定淀粉含量.采用本法测定了云南烤烟烟叶、杀青烟叶、白肋烟和香料烟的淀粉含量,平均回收率为96.71%,相对标准偏差在1.79%-5.58%之间.与传统的酸解法和酶解法比较,本法操作步骤简单、检测成本低、快速准确.     

分光光度法测定饲料用灌木中的淀粉含量

饲料用灌木中的淀粉用酶水解 ,水解产生的葡萄糖用蒽酮显色后分光光度法测定 ,由葡萄糖含量换算为淀粉含量。方法检出限为 2 μg/ m L,相对标准偏差为 1.4 %— 2 .2 % ,标准回收率在 97%— 10 3%之间。本方法用于几种灌木样品中淀粉含量的测定 ,结果令人满意。     

Interlaboratory comparison of tooth enamel dosimetry on Semipalatinsk region: Part 1, general view

For intercomparison of methods of dose determination using electron paramagnetic resonance (EPR) spectroscopy of tooth enamel, the same sets of enamel samples were analyzed in different laboratories using similar recording parameters. The sets of samples included calibration samples irradiated in known doses, test samples irradiated to doses unknown to the participants and accidental dose samples prepared from teeth of humans affected by radioactive fallout from nuclear tests in the Semipalatinsk Nuclear Test Site in Kazakhstan. The test samples were analyzed to determine the differences in the resulting doses using different spectrometers and different spectra processing methods. The accidental dose samples were analyzed in order to test the precision of doses determined by EPR spectroscopy and to obtain more accurate values by averaging the results from different laboratories.     

Comparison of Dry,Wet, and Microwave Ashing Methods for the Determination of Al,Zn, and Fe in Yogurt Samples by Atomic Absorption Spectrometry

Abstract

Digestion methods such as dry and wet ashing and microwave oven were examined at various conditions to determine a rapid, reliable, and simple digestion procedure for yogurt. Digestion by microwave oven was found to be an excellent method in comparison with dry and wet ashing methods when only Al and Zn in yogurt samples were determined. Iron in this matrix is not completely digested by the microwave oven method at the examined conditions. From the obtained results, yogurt can also be a good source of essential nutrients such as minerals in human diet, especially zinc. Aluminum concentrations in yogurt samples fermented in Al containers were found to be significantly higher than in plastic containers. Al concentrations of yogurt taken from the bottom of the container were found to be higher than from the center and top of Al containers. The determinations of metals were carried out via an atomic absorption spectrophotometer using calibration curve and standard additions methods. Aluminum concentrations in yogurt samples produced in big production centers were found to be significantly higher than the other yogurt samples produced in‐house when plastic containers were used.     

X射线荧光光谱理论α系数法测定古青铜钱币中的铅铜锡

本将Ｌａｃｈａｎｃｅ－ｔｒａｉｌｌ（Ｌ－Ｔ）方程理论α系数法应用于古青铜钱币中的Ｐｂ,Ｃｕ,Ｓｎ分析,并与基本参数法和标样法的结果进行了比较。由于本法和模拟标样法都是从基本参数法演变来的,使用的标样是一样的,三种方法计算结果数据比较接近。本法计算速度快,效率高,但对标样的依赖性较大。     

Synthesis,structural, optical and magnetic properties of Cu-doped ZnO nanorods prepared by a simple direct thermal decomposition route

Cu-doped ZnO nanorods (i.e. Cu = 1.75, 3.55, 5.17 and 6.39 at.%) have been successfully synthesized by simple, direct, thermal decomposition of zinc and copper acetates in air at 300 °C for 6 h. The prepared samples were characterized by X-ray diffraction (XRD) and transmission electron microscopy. The XRD results indicate that the 1.75 at.% Cu-doped ZnO sample has a pure phase with the ZnO wurtzite structure, while the impurity phases are detected with increasing Cu concentrations. It was found that the doping of Cu results in a reduction of the preparation temperature. The optical properties of the samples were also investigated by UV–visible spectroscopy and photoluminescence measurements. The results show that the Cu doping causes the change in energy-band structures and effectively adjusts the intensity of the luminescence properties of ZnO nanorods. X-ray photoelectron spectroscopy analysis implies that there are some oxygen vacancies in the samples and also indicates that all the doped samples are associated with the mixture of Cu ion states (Cu²⁺ and Cu¹⁺/Cu⁰). Magnetic measurements by vibrating sample magnetometry indicate that undoped ZnO is diamagnetic, whereas all of the Cu-doped ZnO samples exhibit room temperature ferromagnetic behavior. We suggest that Cu substitution and density of oxygen vacancies (V _o) may play a major role in the room temperature magnetism of the Cu-doped ZnO samples.     

ICP-AES测定工业碳酸锶中的钙、钡、钠和磷

试料经酸分解后,于王水介质中同时测定碳酸锶中的钙、钡、钠和磷的含量,操作简便、快速,最终结果与现行国家标准分析方法测得结果一致。     

原子吸收法连续测定氧化铝中微量钙钠铁锌

本文确定以硼酸－碳酸锂为混合溶剂，在铂坩埚中于１０００℃高温炉熔融氧化铝试样，用盐酸浸取，加释放剂，保护剂和消电离剂，用空气－乙炔火焰原子吸收法连续测定四种元素的氧化物含量。该法多次分析标样含量和准确值之差均小于规定的允差范围，测定样品与ＧＢ６６０９－８６法测定的数据安全吻合，已用于１００多批次进口氧化铝的测定，本法准确，可靠，而且简便，快速，有应用推广价值。     

非完全消解-火焰原子吸收光谱法测定虾皮中的铁、铜、锌和锰

用非完全消解法处理虾皮样品,即在低温下用浓硝酸-过氧化氢(3+1)混合酸消解样品,再用乳化剂OP溶解未消解的油脂而配制成无色透明的溶液,将此溶液用火焰原子吸收光谱法测定其中铁、铜、锌和锰元素的含量。建立了快速测定虾皮中微量元素的火焰原子吸收光谱法。对样品处理条件、混合酸中杂质及共存OP的干扰进行了实验,铁、铜、锌和锰的检出限(3S/k)分别为0.021、0.047、0.008、0.026m g.L-1。该法测定虾皮中铁、铜、锌和锰的含量,所得结果与灰化法测定结果一致。     

Characterization,spectroscopic investigation of defects by positron annihilation,and possible application of synthesized PbO nanoparticles

Nanocrystalline samples of highly pure lead oxide were prepared by the sol-gel route of synthesis.X-ray diffraction and transmission electron microscopic techniques confirmed the nanocrystallinity of the samples,and the average sizes of the crystallites were found within 20 nm to 35 nm.The nanocrystallites exhibited specific anomalous properties,among which a prominent one is the increased lattice parameters and unit cell volumes.The optical band gaps also increased when the nanocrystallites became smaller in size.The latter aspect is attributable to the onset of quantum confinement effects,as seen in a few other metal oxide nanoparticles.Positron annihilation was employed to study the vacancy type defects,which were abundant in the samples and played crucial roles in modulating their properties.The defect concentrations were significantly larger in the samples of smaller crystallite sizes.The results suggested the feasibility of tailoring the properties of lead oxide nanocrystallites for technological applications,such as using lead oxide nanoparticles in batteries for better performance in discharge rate and resistance.It also provided the physical insight into the structural build-up process when crystallites were formed with a finite number of atoms,whose distributions were governed by the site stabilization energy.     

Comparison of responses of CR-39, PM-355, and CN track detectors to energetic hydrogen-, helium-, nitrogen-, and oxygen-ions

Samples made of the CR-39 and PM-355 plastic nuclear track detectors (NTDs) as well as of the CN films were irradiated with quasi-monoenergetic beams of protons, alphas, N⁺-, and O⁺-ions produced by various accelerators. For different samples an energy value of the particle beams was changed from several hundreds keV to 3 or 4.5 MeV. After irradiation the detector samples were etched chemically under controlled conditions during periods lasting from 2 hrs to 20 hrs. Every 2 hrs track diameters were measured by means of an optical microscope. Differences in the crater diameters in the detectors etched in steps, and those etched continously, have been found to be smaller than 10 percent. The paper results detailed calibration diagrams showing a dependence of track diameters on the ion energy value for different etching times.