针对部分地质样品伴生稀有Li、Be、Rb、Cs、Nb、Ta含量变化范围大、高含量Nb和Ta易水解、传统分析方法流程复杂、不易实现同时测定的特点,采用体积比为10:5:1的HF-HNO3-H2SO4酸溶体系常压加热分解样品;以80 g/L酒石酸溶液微热提取,使Nb、Ta充分络合;再加入王水加热使Li、Be、Rb、Cs充分提取进入溶液;选择7Li、9Be、85Rb、93Nb、133Cs、181Ta作为分析同位素,电感耦合等离子体质谱法(ICP-MS)测定Li、Be、Rb、Nb、Cs、Ta;选择Li 670.784 nm{Ⅰ}、Be 234.861 nm{Ⅰ}、Rb 780.023 nm{Ⅰ}、Nb 316.340 nm{Ⅱ}、Ta 268.517 nm{Ⅱ}作为分析谱线,电感耦合等离子体原子发射光谱法(ICP-AES)测定Li、Be、Rb、Nb、Ta,建立了 ICP-MS和ICP-AES相结合测定地球化学样品中Li、Be、Rb、Cs、Nb、Ta的方法.Li、Be、Rb、Cs、Nb、Ta校准曲线线性相关系数为0.999 4~0.999 9,检出限和定量限(以ICP-MS计)分别为0.01~0.15 μg/g和0.012~0.807 μg/g.按照实验方法测定纳米比亚某伟晶岩矿实际样品和土壤、水系沉积物、钽矿石有证标准物质中Li、Be、Rb、Cs、Nb、Ta,测定结果的相对标准偏差(RSD,n=7)为0.78%~9.6%,测定值与认定值的对数差绝对值(|△lgC|,n=7)为0.000 2~0.020,标准物质的测定值与认定值基本一致,实际样品的加标回收率为93%~104%.
文章建立了直接测定半导体二级40%含量氢氟酸(CMOSⅡ40%-HF)多元素含量的方法。以膜去溶作为进样系统,电感耦合等离子体质谱仪(ICP-MS)作为分析仪器,分别采用热焰和冷焰模式分析,首先测定CMOSⅡ 40%-HF,然后测定以Be、Co、In和Bi作为加标的CMOSⅡ 40%-HF,加标样品测定加标回收率,同时测定Na、Mg、K、Ca和Fe的检出限。实验结果证明该方法具有进样速度快、精密度高等优点,冷焰模式降低了Na、Mg、K、Ca和Fe的检出限,同时降低了CMOSⅡ40%-HF的检出下限,提高了准确度。膜去溶与ICP-MS联用是快速分析高纯度HF中金属离子的有效方法,膜去溶的使用解决了使用玻璃雾化器和石英炬管时HF无法直接进样的问题,有效地减小了基体干扰,同时冷焰模式提高了碱金属元素的测量精度。
Silicone modified epoxy resin with excellent properties was synthesized when the hydrolysis temperature was 35~40 ℃,the hydrolysis time was 1~1.5 h,and the hydrolysis ratio was n(H2O)∶ n(Cl)=(6~7)∶ 1.IR indicates that the chemical reaction mainly occurred between hydroxyls of silicone and epoxy resin.The mechanical properties,heat-resistance and moisture resistance of modified and unmodified epoxy resin were respectively studied and compared.The results show that,for modified epoxy resin,when n(R)/n(Si) was 1.5,the tensile strength was 23.91 MPa,the bending strength was 29.24 MPa,the impact strenth was 10.02 kJ/m2 and the temperature of 50% weight loss was 431 ℃,higher than those of unmodified epoxy resin by 3.86 MPa,9.49 MPa,6.18 kJ/m2,30 ℃,respectively.At the same time,the moisture resistance of modified resin was increased.