离子交换树脂分离-电感耦合等离子体质谱法测定卤水中溴碘

Determination of Bromine and Iodine in Brine by Ion Exchange Resin Separation and Inductively Coupled Plasma-Mass Spectrometry

  • 摘要: 天然卤水中蕴藏着丰富的溴(Br)、碘(I)等资源,但其高盐基体中存在大量钠(Na+)、钾(K+)、钙(Ca2+)、镁(Mg2+)等阳离子,对电感耦合等离子体质谱(ICP-MS)测定Br、I产生严重基体干扰,影响检测准确性。本文采用强酸性大容量阳离子交换树脂动态吸附去除卤水中的阳离子,建立了准确测定高盐卤水中Br、I的分析方法。系统研究了高盐基体对Br、I测定的干扰程度及稀释倍数对测定结果的影响。结果表明,当卤水溶解性总固体(TDS)≥3960 mg/L时,基体干扰显著;稀释方法虽可一定程度地降低干扰,但不同稀释倍数下测定值相对偏差大,精密度低。经离子交换树脂处理后,卤水中Na+等阳离子总去除率最高可达99.4%,TDS显著降低,有效消除了基体干扰。该方法对Br、I的检出限分别为0.36 μg/L和0.23 μg/L,相对标准偏差(RSD)均低于3.64%(n=7),加标回收率为82.7%~116.1%,符合DZ/T 0130—2006规范要求。本方法可用于分析TDS>60 g/L的高盐卤水,无需大倍数稀释(稀释倍数<30倍)即可实现Br、I的准确测定,具有前处理简便、基体去除率高、结果准确等优点,为高盐卤水资源中Br、I的评估提供可靠技术支撑,也为离子交换树脂在复杂卤水体系微痕量元素分析中的应用提供了实践依据。

     

    Abstract: Natural brine contains abundant resources, including bromine (Br) and iodine (I). However, the large number of cations such as sodium (Na+), potassium (K+), calcium (Ca2+) and magnesium (Mg2+) present in the high-salt matrix, which causes severe matrix interference in the determination of Br and I by inductively coupled plasma-mass spectrometry (ICP-MS) and affect the accuracy of detection. In this work, a novel method for the accurate determination of Br and I in high-salt brine was established by using strongly acidic and high-capacity ion exchange resin to dynamically adsorb and remove of cations from the brine. The interference degree of high-salt matrix on the determination of Br and I and the influence of dilution factor on the determination results were systematically studied. The results showed that, when the total dissolved solids (TDS) of the brine exceeded 3960 mg/L, significant matrix interference occurred. While the dilution method reduced interference to a certain extent, the relative deviation of the measured values under different dilution factors was significant, resulting in low precision. After ion exchange resin treatment, the total removal rate of cations such as Na+ in the brine was up to 99.4%, TDS was significantly reduced and matrix interference was effectively eliminated. The detection limits for bromide and iodine were 0.36 μg/L and 0.23 μg/L, respectively, with relative standard deviations (RSD) of less than 3.64% (n=7) for both. Spike recovery rates ranged from 82.7% to 116.1%, meeting the DZ/T 0130-2006 specification requirements. This method is suitable for high-salinity brine with a TDS higher than 60 g/L, enabling the accurate determination of bromide and iodine without large multiple dilution (dilution <30 times). Advantages include simple pretreatment, a high matrix removal rate and accurate results. This provides reliable technical support for evaluating Br and I in high-salinity brine resources, and also provides practical basis for the application of ion exchange resin in the analysis of trace elements in complex brine system.

     

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