摘要
建立了在线流动/停流双渗析模式联用-离子色谱检测腈纶溶剂中Na_2SO_4和NaSCN的分析方法。样品用0.05mol/L NaOH+0.02%甲醛无氧水溶液稀释,保护SO2-3根不被氧化的同时,沉淀重金属离子;自编控制程序,采用在线流动/停流渗析模式去除不溶物、高聚物与部分色素,与离子色谱联用,一次稀释,依次获得了含量差异大的Na_2SO_4和NaSCN的含量;采用A Supp 5Guard+A Supp 5-150/4.0mm色谱柱,以3.2mmol/L Na_2CO_3+1.0mmol/L NaHCO_3+3.5%丙酮为淋洗液,流速为1.25mL/min,抑制电导依次检测腈纶溶剂中Na_2SO_4和NaSCN。方法的相对标准偏差≤6.29%,加标回收率为95.8%~103.1%。方法用于腈纶不同装置水溶液中的Na_2SO_4和NaSCN分析,结果满意。
Sequential determination of Na2SO4 and NaSCN in acrylic solvent has been realized by ion chromatography coupled with online stopped-flow/flow dialysis.The sample solution was diluted by 0.05 mol/L sodium hydroxide and 0.02%(V/V)formaldehyde aqueous solution,which protected SO3^2- and facilitated precipitation of heavy cations.The online stopped-flow/flow dialysis removed insoluble matter,high polymer and several types of pigments.The A Supp 5 Guard+A Supp 5-150/4.0 mm separation column was used to detect SO4^2- and SCN-with 3.2 mmol/L Na2CO3+1.0 mmol/L NaHCO3+3.5%(V/V)acetone solution as the eluent and the flow rate set at 1.25 mL/min.This suppressed conductivity detection and allowed for sequential determination.The relative standard deviation of this method was less than 6.29%.The recovery rate for both Na2SO4 and NaSCN was between 95.8%and 103.1%.The current method has been applied to the analysis of Na2SO4 and NaSCN in different kinds of acrylic solvent with satisfactory results.
作者
陆克平
刘浩
周剑平
LU Ke-ping;LIU Hao;ZHOU Jian-ping(Inspection Center, SINOPEC Anqing Company ,Anqing 246002;Wanxinan Product Quality Supervision and Testing Center,Anqing 246002)
出处
《分析科学学报》
CAS
CSCD
北大核心
2018年第3期362-366,共5页
Journal of Analytical Science
基金
中国石化安庆分公司技术开发项目(No.HF-1409)
皖西南产品质量监督检验中心合作项目(合同号32000000-14-ZC0607-0002)
关键词
流动渗析
停流渗析
离子色谱
腈纶溶剂
Flow dialysis
Stop-flow dialysis
Ion chromatography
Acrylic solvent