毛细管气相色谱法测定谷类农产品中残留有机氯农药

用毛细管柱气相色谱法对谷类农产品中残留的2种有机氯农药,六六六和滴滴涕的8种异构体的含量作了测定.为了避免在样品预处理过程中出现乳化现象,采用了涡旋振荡和在4～6℃的冷却措施.用所提出的方法测定了6种谷物样品(黑豆、薏米、莲子、黄豆、芡实和蚕豆)中上述农药的残留量.方法的回收率在84.5%～103.2%之间,测定结果的相对标准偏差均小于5%.8种异构体的检出限为5μg·kg-1.     

偏振能量色散X射线荧光光谱法测定地质样品中18种元素

利用偏振能量色散X射线荧光光谱仪分析了硅酸盐基体样品. 选取岩石、土壤、水系沉积物等国家一级标准物质, 采用镶边粉末压片方法, 选择Al2O3偏振靶、 Mo、 Co二级靶, 在真空状态下对K、 Ca、 Ti、 Cr、 Mn、 Fe、 Ni、 Cu、 Zn、 Ga、 As、 Rb、 Sr、 Y、 Zr、 Nb、 Ba、 Pb等18种元素进行选择激发和探测, 所有元素的校正选用扩展的康普顿散射校正模型. 各元素的检出限为0.4～10.9 μg/g;除了As元素外, 均达到了1:25万多目标地球化学调查规范的要求. 根据60个地质调查多目标考核样品的分析结果, 采用Rousseau(2001)所提出的相对不确定度计算方法, 对所建立的方法进行了评估.     

气相色谱-质谱联用测定环境样品中三氯生

建立了气相色谱质谱联用(GC-MS)分析自然水体中三氯生的方法,采用C(18)固相萃取柱处理水样.利用N-甲基-N(三甲基硅)-三氟乙酰胺(MSTFA)对目标物进行衍生化.GC-MS分析中以菲-D10为内标,利用内标法对三氯生进行定量.河水海水中不同浓度加标的三氯生回收率为73%～101%,相对标准偏差(RSD)在4.5%～11.3%之间,方法检出限为0.2 ng/L.该方法适用于河水海水水体中三氯生的测定.     

ICP-MS测定土壤中铅同位素比值及地域差异性比较

建立用HNO_3-H_2O_2-HF体系微波消解前处理样品,利用电感耦合等离子体质谱测定土壤中铅同住素比值的方法,探讨并优化了影响测试结果的两种干扰因素.该方法中~(207)Pb/~(206)Pb和~(208)Pb/~(206)Pb的短期测量稳定性RSD分别达到0.12%和0.13%,长期测量的偏差分别在0.002和0.01以内,样品测量的最佳范围是10～40μg/L.采用标样-样品交叉法测定了湖南、湖北、云南、贵州、河南、福建、辽宁7个省的48个地区土壤中的铅同位素比值,结合聚类分析和主成分分析比较了各省土壤中同位素分布的差异,初步探讨了利用~(207)Pb/~(206)Pb和~(208)Pb/~(206)Pb比较烟叶产区的可能性.     

凝胶渗透色谱异常问题系列讲座(2)峰漂移

我们在使用凝胶色谱分析样品时,有时会发现色谱峰的出峰时间发生迁移.在这里,我将一些常见的出峰时间异常问题罗列如下.     

X射线荧光光谱法测定铝合金及纯铝中痕量元素

根据X射线荧光光谱法分析样品形状要求,按照待测物料形状,适合于X射线荧光光谱测量的棒状类样品用车床车割,块、片状类样品用锯、锉刀处理,屑类样品首先用液压机压成片状,再用锉刀处理成适合于X射线荧光光谱分析的待测样品.测试了铝合金和纯铝中铁、硅、铜、镓、镁、锰、锌、钛和铬的含量,对于测量不灵敏的镁,每次测试带全套标样,峰值计量,单独为组测量可保障其准确度.基体单纯、固定的样品,测量痕量元素含量时峰值强度计量优于扣除背景的净强度计量,可避免背景测量误差,测量结果与直读光谱法相符.9项元素的精密度均优于3%.     

Effect of Sorbents Added on Adsorption Capability of Soil for Nano-TiO2

The adsorption capability of loam soil for nano-TiO2 affected by the amount and intensity of leached water has been investigated by simulating the natural rainfall process under the leaching condition.The results show that the amount and the intensity of leached water are two important factors affecting the adsorption capability of loam soil for nano-TiO2.The results indicate that the depth of the loam soil containing a maximal amount of nano-TiO2 is proportional to the amount of leached water,while it is i...     

Effects of processing parameters on fatigue properties of LY2 Al alloy subjected to laser shock processing

We address the effects of processing parameters on residual stresses and fatigue properties of LY2 Al alloy by laser shock processing (LSP). Results show that compressive residual stresses are generated near the surface of samples due to LSP. The maximum compressive residual stress at the surface by two LSP impacts on one side is higher than that by one LSP impact. The maximum value of tensile residual stress is found at the mid-plane of samples subjected to two-sided LSP. Compared with fatigue lives of samples treated by single-sided LSP, lives of those treated by two-sided LSP are lower. However, these are higher than untreated ones.     

Accurate analysis of ellipsometric data for thick transparent films

Using e-beam evaporation, the ellipsometric parameters of thick transparent films are studied with the modified analysis method for the SiO 2 film samples deposited onto the Si substrate. The ellipsometric parameters are measured at the incidence angles changing from 50 to 70 and in the 3–4.5 eV photon energy range. The error in the conventional method can be significantly reduced by the modified ellipsometric method considering the spatial effect to show good agreement between the theoretical and experimental results. The new method presented in this letter can be applied to other optical measurement of the periodic or non-periodic film structures.     

Scintillating properties of LiYSiO_4:Ce

LiYSiO₄:Ce is a promising scintillator and some of its properties have been reported in previous papers. In this paper, samples doped with different concentrations of Ce are prepared and studied. First, the relative light yields of the samples are measured as 28.1%-37.1% compared with a standard anthracene crystal being irradiated by α particles and as ～ 27.2% compared with NaI being irradiated by X-rays. Second, the effects of sample thicknesses on light yields are presented. Finally the timing behaviors of samples with different doped concentrations being irradiated with alpha particles and X-rays are discussed. The result shows that LiYSiO₄:Ce is a kind of fast scintillator ( ～ 30 ns) with a moderate light yield that can be used for neutron detection.