2016/12/19 09:09
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分享:方案摘要:
产品配置单:
液相色谱-原子荧光联用
型号: AFS1101N (1)
产地: 江苏
品牌:
¥5万 - 10万
参考报价
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方案详情:
水产品中一甲基砷、二甲基砷、砷酸根和亚砷酸根的测定
高效液相色谱-原子荧光光谱法
本方法检测限:一甲基砷为2μg/kg,二甲基砷为3μg/kg,砷酸根为2μg/kg,亚砷酸根为5μg/kg。
仪器与设备
高效液相泵。
原子荧光光谱仪,配有砷空心阴极灯。
提取与净化
称取经粉碎、混合均匀的样品5g(精确至0.001g)于50mL的离心管中,加10mL50%甲醇溶液,涡旋震荡均匀之后,70℃超声萃取15min,3000r/min离心15min,取其上清液于25mL的比色管中,将其沉淀重复上次萃取1次,合并两次上清液,用50%甲醇定容至25mL,取其上清液用滤纸过滤,取滤液5mL,于70℃下吹氮浓缩至约1.5mL,冷却后用流动相定容至2.5mL,再用过滤膜过2次膜,过C小柱,收集洗脱液待测。同时做试剂空白。
测定参考条件
色谱柱:阴离子交换柱色谱(长250mm,内径4.1mm,粒径10μm)或相当者
流速:1mL/min;
进样体积:100μL;
还原剂:1.5%KBH和0.5%KOH;
载流:7%HCl;
蠕动泵速:70r/min;
原子荧光条件:灯电流:100mA;
负高压:270V;
载气流量:300mL/min;
屏蔽气流量:600mL/min;
辅阴极电流:30mA。
图A1为亚砷酸根(AsⅢ)、二甲基砷(DMA)、一甲基砷(MMA)、砷酸根(AsV)四种砷标准样品色谱图
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