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胡忠阳, 叶明立, 潘广文, 等. 在线基体消除-离子色谱法测定墨水染料中的氯及硫酸盐[J]. 分析测试学报, 2012,31(5):580-583.
Determination of Inorganic Anions in Ink Dye by On-line Removing Matrix-Ion Chromatography[J]. 2012,31(5):580-583.
建立了一种在线基体消除的方法,采用离子色谱法测定了墨水染料中的氯和硫酸盐。样品经溶解、稀释后直接进样,在纯水的输送下依次经过DIONEX OnGuard Ⅱ P和IonPac NG1柱,在线实现了墨水样品中染料和疏水性干扰基体的去除,死时间流出的待测阴离子浓缩于阴离子交换柱IonPac AG11-HC。浓缩柱经阀切换进入离子色谱系统,以4.5 mmol/L Na2CO3-0.8 mmol/L NaHCO3作为淋洗液,流速1.2 mL/min,待测离子经IonPac AS23(4 mm×250 mm)分析柱分离,采用DIONEX DS6电导检测器检测,外标法定量。Cl-和SO2-4的线性范围分别为0.05~5.0、0.1~10.0 mg/L,相关系数分别为0.999 8和 0.999 7,加标回收率为94%~103%,相对标准偏差(n=11)小于1.0%,检出限(S/N=3)分别为0.02、0.05 mg/L。该方法用于墨水染料中氯和硫酸盐的测定,结果满意。
An on-line removing matrix method with pre-concentration of the analytes was developed for the simultaneous determination of impurity anions(e.g.chloride,sulfate) in ink dye by ion chromatography(IC).The sample was diluted with de-ionized water,filtrated by 0.22 μm nylon membrane and then injected into the IC system directly without any further pretreatment.The sample solution in the loop was delivered by de-ionized water,and then filtrated on line by DIONEX OnGuard II P column and IonPac NG1 column for pre-removing of dyestuff and hydrophobic components.The analytes flowing out in the dead time were concentrated in the high capacity anion-exchange guard column IonPac AG11-HC.The concentrator then stepped in the IC system when the valve switched to injection mode.The chloride and sulfate were separated on a DIONEX IonPac AS23(4 mm×250 mm) column by using 4.5 mmol/L Na2CO3 -0.8 mmol/L NaHCO3 as the eluent at a flow rate of 1.2 mL/min.The analytes were detected with a Dionex DS6 conductive detector and quantitively analyzed by the external standard method.The results indicated that the linear ranges of Cl-and SO2-4 were 0.05-5.0 mg/L(r=0.999 8) and 0.1-10 mg/L(r=0.999 7),respectively.The average recoveries were in the range of 94%-103% with relative standard deviations(RSDs) no more than 1.0%.The detection limits(S/N=3) were 0.02 mg/L for Cl- and 0.05 mg/L for SO2-4.The method was applied in the determination of chloride and sulfate in ink dye samples with satisfactory results.
离子色谱墨水染料氯离子硫酸盐在线基体消除
ion chromatographyink dyechloridesulfateon line removing matrix method
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