Talanta. 2013 Oct 15;115:681-7. doi: 10.1016/j.talanta.2013.06.039.
A new method has been described for generation of volatile species of Cd using vanadium(III) cyanide complex. Aqueous solutions of 0.04 mol L(-1) vanadium chloride (VCl3) and 0.12 mol L(-1) potassium cyanide (KCN) were reacted on-line yielding a suspension of vanadium hydroxide, V(OH)3. This suspension was dissolved along the stream of sample solution in dilute HCl to form heptacyanovanadate(III) complex, [V(CN)7]4-. Volatile Cd species were generated by reacting the stream of sample solution and cyanovanadate(III) complex with sodium borohydride (NaBH4). Feasibility of off-line and on-online approaches was investigated for quantitative determinations. Better precision and daily stability were achieved with on-line settings. Optimum signals were obtained from sample solutions within a range of 3 to 5% v/v HCl. A concentration of 2% m/v NaBH4 was adequate to achieve an enhancement of 20-fold in the presence of cyanovanadate(III) complex. The limits of detection were 5.0 and 4.5 ng L(-1) for 110Cd and 111Cd isotopes, respectively. Precision (%RSD) was better than 4.7% for six replicate measurements. The interferences of Cu(II) and Ni(II) were marginal (<10%) at 1.0 µg mL(-1). Depressive effects from Bi, Se and Sn were not significant below 0.1 µg mL(-1). The method was validated by determination of Cd using ICP-MS in certified reference materials of Nearshore seawater (CASS-4), Bone ash (SRM 1400), Dogfish liver (DOLT-4) and Mussel tissue (SRM 2976).
一种新的方法已被描述为使用三价钒氰化物配合物生成 Cd 的挥发性物种。0.04 mol L(-1) 三氯化钒 (VCl3) 和 0.12 mol L(-1) 氰化钾 (KCN) 的水溶液在线反应生成氢氧化钒悬浮液,V(OH)3。将该悬浮液溶解在稀盐酸中,与样品溶液一起沿流路反应,形成七氰合钒酸根 (III) 配合物,[V(CN)7]4-。通过将样品溶液和氰合钒酸根 (III) 配合物与硼氢化钠 (NaBH4) 反应,生成挥发性 Cd 物种。离线和在线方法的可行性进行了研究。在线设置可获得更好的精密度和日常稳定性。在 3 至 5% v/v HCl 的范围内,从样品溶液中获得最佳信号。在存在氰合钒酸根 (III) 配合物的情况下,2% m/v NaBH4 的浓度足以实现 20 倍的增强。110Cd 和 111Cd 同位素的检出限分别为 5.0 和 4.5 ng L(-1)。六个重复测量的精密度(%RSD)优于 4.7%。在 1.0 µg mL(-1) 时,Cu(II)和 Ni(II)的干扰小于 10%。低于 0.1 µg mL(-1)时,Bi、Se 和 Sn 的抑制作用不显著。该方法通过使用 ICP-MS 在近岸海水 (CASS-4)、骨灰 (SRM 1400)、鲨鱼肝 (DOLT-4) 和贻贝组织 (SRM 2976) 的认证参考材料中测定 Cd 进行了验证。