悬浮液进样-石墨炉原子吸收光谱法测定生物样品中微量铬

提出了固体悬浮液进样石墨炉原子吸收光谱法直接测定铬的方法,并对各分析条件进行了优化.采用1.2 g·L-1琼脂溶液为悬浮剂,将样品均匀悬浮于其中,由自动进样器直接将样品悬浮液注入石墨炉中,加入基体改进剂,石墨炉原子吸收光谱法测定生物样品中铬.在优化的试验条件下,方法的检出限(3σ)为0.5 pg·L-1.铬的质量浓度在50 μg·L-1以内呈线性关系,回归方程为A=0.2521 C 0.0311,样品加标回收率为98.6%～103.2%.     

Hydrothermal Synthesis and Vacuum Ultraviolet-Excited Luminescence Properties of Novel Dy^3＋-doped GdPO4 White Light Phosphors

Novel Dy^3＋-doped GdPO4 white light phosphors with a monoclinic system are successfully synthesized by the hydrothermal method at 240℃. The strong absorption at around 147nm in the excitation spectrum is assigned to the host absorption. It is suggested that the vacuum ultraviolet excited energy is transferred from the host to the Dy^3＋ ions. The f - d transition of the Dy^3＋ ion is observed to be located at 182nm, which is consistent with the calculated value using Dorenbos＇s expression. Under 147nm excitation, Gd0.92PO4：0.08Dy^3＋ phosphor exhibits two emission bands located at 572 nm （yellow） and 478 nm （blue）, which correspond to the hypersensitive transitions ^4 F9/2-^6 H13/2 and ^4 F9/2-^6 H15/2. The two emission bands lead to the white light. Because of the strong absorption at about 147nm, Gd0.92PO4：0.08Dy^3＋ under vacuum ultraviolet excitation is an effective white light phosphor, and has promising applications to mercury-free lamps.     

流动注射在线离子交换柱富集-火焰原子吸收光谱法测定钨矿中的铜、锌和铅

建立了流动注射在线离子交换柱富集-火焰原子吸收光谱法测定钨矿中的铜、锌和铅的方法,样品经盐酸和硝酸分解后,加入5%宁可辛溶液使样品中大量的钨呈钨酸析出,样品中一般的伴生元素都可形成可溶性化合物与钨酸分离,之后采用流动注射在线富集与原子吸收联用技术,分别加入浓度依次递增的3种元素的标准溶液,用空气-乙炔火焰原子吸收连续测定Cu、Zn和Pb的含量。建立了优化的仪器工作条件,并对可能存在的元素进行干扰试验。方法检出限Cu为0.001μg/mL、Zn为0.001μg/mL、Pb为0.01μg/mL,相对标准偏差Cu为2.7%、Zn为3.6%、Pb为1.9%,加标回收率为96%—106%。     

碱性模式氢化物发生原子荧光光谱法测定铁矿石中砷

建立了碱性模式氢化物发生原子荧光光谱法测定铁矿石中砷的最佳仪器和实验条件。采用微波消解分解样品，在硫脲和L-半胱氨酸存在下将As（Ⅴ）还原为As（Ⅲ），以1mol／L KOH作为介质，以0．75mol／L H3PO4作为载流，原子荧光光谱法测定样品中的砷。方法检出限为0．35μg／L，RSD在2．0％。9．4％之间，加标回收率95％～103％。对标准样品进行分析验证，结果与标准值相符。应用于铁矿样品的测定，结果满意。     

薄层层析-光度法联用测定甲基对硫膦中o,o''''-二甲基-对硝基苯基硫代膦酸酯

应用薄层色谱法(TLC)使对硫膦中的主成分,o,o'-二甲基-对硝基苯基硫代膦酸酯(DMNPTP),与以杂质共存的二硝基与邻硝基衍生物分离.TLC法中用硅胶(G254)作吸附剂,用石油醚与乙酸乙酯(8 2)的混合物作为展开溶剂,经TCL分离后,用刀片将样品(含DMNPTP)的色谱带括下,经蒸发除去有机溶剂,用硝酸-高氯酸加热消化并蒸发至干后,用硝酸溶解残渣.此时,溶液中原来以DMNPTP存在的化合物已转化为正磷酸盐,随即用磷钒钼杂多酸光度法测定其磷含量,测定波长为其吸收峰450 nm,由测定值换算为DMNPTP的含量.     

Novel Dy^3＋-doped Gd（PO3）3 white-light phosphors under VUV excitation for Hg-free lamps application

Novel Dy3+-doped Gd(PO3)3 white light phosphors each with an orthorhombic system are successfully synthesized by solid-state reaction.The luminescence properties of white-light Gd1-x(PO3)3:xDy3+(0 x ≤ 0.25) under vacuum ultraviolet(VUV) excitation are investigated.The strong absorption at around 147 nm in excitation spectrum energy can be transferred to the energy levels of Dy3+ ion from the host absorption.Additionally,the white light phosphor is activated by a single Dy3+ ion.Therefore,the luminescence of Gd1-x(PO3)3:xDy(0 x ≤ 0.25) under VUV excitation is effective,and it has the promise of being applied to mercury-free lamps.     

薄层层析-光度法联用测定甲基对硫膦中o,o′-二甲基-对硝基苯基硫代膦酸酯

应用薄层色谱法(TLC)使对硫膦中的主成分,o,o′-二甲基-对硝基苯基硫代膦酸酯(DMNPTP),与以杂质共存的二硝基与邻硝基衍生物分离。TLC法中用硅胶(G254)作吸附剂,用石油醚与乙酸乙酯(8 2)的混合物作为展开溶剂,经TCL分离后,用刀片将样品(含DMNPTP)的色谱带括下,经蒸发除去有机溶剂,用硝酸-高氯酸加热消化并蒸发至干后,用硝酸溶解残渣。此时,溶液中原来以DMNPTP存在的化合物已转化为正磷酸盐,随即用磷钒钼杂多酸光度法测定其磷含量,测定波长为其吸收峰450 nm,由测定值换算为DMNPTP的含量。     

火焰原子吸收光谱法测定汽油中铅

汽油中最具代表性的组分是辛烷。辛烷值是[1]表示汽油在汽油机中燃烧时的抗震性的指标。它是将汽油样品与抗震性很好的异辛烷(辛烷值规定为100)和抗震性很小的正庚烷配合成的混合液在标准汽油机中进行比较而得。例如一种汽油样品的抗震性与95%异辛烷和5%正庚烷的混合液相等,该样品的辛烷值即为95,就称为95号汽油。直馏汽油的辛烷值在55~72之间。在每升汽油中加入0.6 g“铅”可以将辛烷值提高79~88。加入汽油中的铅主要含有约60%(质量分数)的四乙基铅Pb(C2H5)4或四甲基铅Pb(CH3)4和约40%的二溴乙烷(或二氯乙烷)的混合物。四乙基铅阻止提前…     

A novel Dy3+-doped GdPO4 white-light phosphors under vacuum ultraviolet excitation for Hg-free lamps application

Novel Dy3+-doped GdPO4 white light phosphors with monoclinic system were successfully synthesised by hydrothermal method at 240 ℃. This paper investigates the luminescence properties of white-light Gd1-xPO4 : xDy3+ under vacuum ultraviolet (VUV) excitation. The strong absorption at around 147 nm in excitation spectrum energy can be transferred to the energy levels of Dy3+ ion from the host absorption. Additionally, this white light phosphors are activated by a single Dy3+ ion and with a lower preparation temperature, which tend to decrease the consumption of rare earth resource and energy. Therefore, the luminescence of Gd1-xPO4 : xDy3+ under VUV excitation is effective, and proves to be promising in application to mercury-free lamp.