络合掩蔽-离子色谱法测定氯亚钯酸中硝酸根

Determination of nitrate content in chloropalladous acid solution by complex masking–ion chromatography

建立了络合掩蔽-离子色谱法,测定氯亚钯酸(H_(2)PdCl_(4))溶液中的硝酸根含量。用乙二胺(en)将阴离子[PdCl_(4)]^(2-)转化为[Pd(en)_(2)]^(2+)阳离子,用银柱除氯,避免大量氯离子拖尾影响阴离子的测定。采用高容量阴离子色谱柱,以5-15-35-5 mmol/L KOH在线梯度淋洗,抑制电导检测氯亚钯酸中的硝酸根含量。结果表明,常见阴离子对测定结果无干扰,方法在0.05~4.0μg/mL浓度范围内有良好的线性关系,相对标准偏差为0.8%~3.4%,加标回收率为93%~110%,满足产品质量检测要求。

A method for the detection of nitrate in H_(2)PdCl_(4)by complex masking-ion chromatography was established.The anionic PdCl_(4)^(2-)was first converted to Pd(en)_(2)^(2+)cations with ethylenediamine(en).A silver column were used to eliminate chlorine,so as to avoid the trailing effect caused by a large amount of chloride ion.A high capacity anion chromatographic column was selected for the determination of nitrate in chloropalladium acid with 5-15-35-5 mmol/L KOH as on-line gradient elution.The results showed that the common anions did not interfere with the determination results,and the method had a good linear relationship in the concentration range of 0.05~4.0μg/mL.The relative standard deviation was 0.8%~3.4%while the spiked recovery ranged from 93%to 110%.The established method can meet the requirements of the quality testing for H_(2)PdCl_(4).