摘要
开发了以次磷酸钠为抗氧化剂的亚硫酸根样品预处理方式,与用甲醛稳定SO32-相比,二者在前80小时内稳定效果处于同一水平,且SO32-保存度皆在90%以上;90 h后甲醛稳定效果下降明显,而次磷酸钠稳定效果下降缓慢,水平占优。最终建立以次磷酸钠为前处理稳定剂的亚硫酸根样品离子色谱检测方法。色谱柱为盛瀚SH-AC-18,淋洗液为3.6mM Na2CO3+4.5mM NaHCO3,流速1 mL·min^-1,进样量25μL。亚硫酸根在0~12 mg·L-1线性关系良好,相关系数0.999,检出限(S/N=3)0.024 mg·L^-1。在土壤浸出液中添加0.056、0.125、2.000 mg·g^-1三种水平的标准样品,其加标回收率为89%~105%,平行测试的相对标准偏差小于0.25%,精密度和准确度良好,符合标准要求。
New pretreatment method of sulfite sample was developed with antioxidant sodium hypophosphate.Compared with the application of formaldehyde for the stabilization of SO32-,both showed outstanding performance at the same level with above 90%preserved of SO32- during the former 80 hours.But after 90 hours,the stabilization effect of formaldehyde descended apparently while the effect of sodium hypophosphate only declined slowly.Finally,Method of sulfite sample determination by ion chromatography was established with the assistance of stabilizer sodium hypophosphate.Sulfite was separated on SH-AC-18 column using solution of(3.6mM Na2CO3 +4.5mM NaHCO3)as eluent with 1.0 mL·min-1 flow rate and 25μL injection volume.Range with good linearity for sulfite was 0~12 mg·L-1 with the correlation coefficient of 0.999 and detection limit was 0.024 mg·L-1.With three levels of standard sample(0.056,0.125,2.000 mg·g-1)added to soil extract,recoveries varied from 89%to 105%with relative standard deviations below 0.25%for each level,representing good precision and accuracy within GB requirements.
作者
邵光印
张锦梅
崔成来
SHAO Guang-yin;ZHANG Jin-mei;CUI Cheng-lai(Shenhan Chromatography Technology Co.Ltd.,Qingdao 266100,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2020年第2期221-226,共6页
Chemical Research and Application
