摘要
建立了一种测定高纯氟化盐试剂中杂质阴离子的离子色谱柱切换技术分析方法。在纯水流动相下,采用IonPac ICE-AS6离子排斥柱将待测杂质Cl^-,SO_4^(2-),NO_4^-及PO_4^(3-)从高浓度的氟化盐溶液中分离出来,分离出的待测组分富集于IonPac TAC ULP1浓缩柱上。以4.5 mmol/L Na_2CO_3-0.8 mmol/L NaHCO_3为淋洗液,流速1.2 mL/min,经过柱切换,将待测离子从浓缩柱上洗脱下来,通过IonPac AG23(50 mm×4 mm)和IonPacAS23(250 mm×4 mm)色谱柱进行分离,抑制电导检测器检测。本方法在线性范围内,Cl^-,NO_3^-,PO_4^(3-)和SO_4^(2-)的相关系数分别为0.9996,0.9999,0.9998和0.9997;加标回收率为92.0%～103.5%;相对标准偏差RSD(n=7)均小于3.0%;检出限(S/N=3)分别为0.2,0.6,3.0和0.5 mg/kg。
A method was developed for the determination of trace anions（Cl^-,NO_3^-,PO_4^（3-） and SO_4^（2-） ） in high pure fluoride reagents by ion chromatography（IC） with column-switching.Ion excluding column IonPac ICE-AS6 was used in the first step to separate the trace anion analytes from the high concentrated fluoride using deionized water as the mobile phase,separated analytes were enriched in the pre-concentration column IonPac TAC-ULP1 at the same time.By using a mixture of 4.5 mmol/L Na_2CO_3-0.8 mmol/L NaHCO_3 as the eluent at a flow rate of 1.2 mL/min,the analytes were eluted from the pre-concentrated column after switching the pre-concentrated column into the analytical system.The separation of the analytes was performed with IonPac AG23（50 mm×4 mm） as guard column and IonPac AS23（250 mm×4 mm） as analytical column,and the detection was performed by suppressed conductivity detector.As a result,the linear ranges of the method for Cl^-,NO_3^-,PO_4^（3-）and SO_4^（2-） were 0.02-5.0 mg/L（r= 0.9996）,0.02 - 5.0 mg/L（r=0.9999）,0.05- 10.0 mg/L（r = 0.9998）, 0.02—5.0 mg/L（r = 0.9997） respectively.The average recoveries were 92.0%—103.5%with the relative standard deviations（RSD,n = 7） less than 3.0%.The detection limits（S/N = 3） were 0.2, 0.6,3.0 and 0.5 mg/kg for Cl^-,NO_3^-,PO_4^（3-）and SO_4^（2-）,respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2012年第11期1703-1708,共6页
Chinese Journal of Analytical Chemistry
基金
浙江大学国家重点实验室开放基金项目(No.2011KF07)
安徽省教育厅高校科研项目(No.KJ2011B211)资助
关键词
离子色谱
柱切换
氟化盐
高纯试剂
阴离子
Ion chromatography
Column switching
Fluoride
High pure reagent
Anions
