摘要
建立了离子色谱测定砜中SO2的方法。为避免亚硫酸盐氧化成硫酸盐,需在标准溶液和样品溶液中加入甲醛水溶液,并采用D101大孔树脂和732阳离子交换树脂对样品溶液进行处理,除去有机化合物和阳离子。采用柱温25℃,检测器温度30℃,IonPac AS23(250 mm×40 mm)作阴离子分析柱,IonPac AG23(50mm×40 mm)作保护柱,以流速为1.0 mL·min-1的4.5 mmol·L-1 Na2CO3和0.8 mmol·L-1 Na HCO3的混合物作为流动相,进行外标法的定量分析。结果表明:当SO2的浓度在3.6~72mg·L-1时,响应面积与浓度呈线性关系,且相关系数大于0.999,此方法检出限为0.83 mg·L-1。3种浓度样品的平均回收率在97.3%~101.8%之间,相对标准偏差(n=7)为0.9%~1.8%。方法适用于砜中SO2含量测定。
A method for the determination of sulfur dioxide in sulfone was established by ion chromatography.The formaldehyde was added to standard solution and sample solution to avoid sulfite oxidizing to sulfate,and the sample solution was dealt with D101 macroporous resin and 732 cation exchange resin to remove organic compound and cations.The quantification was performed by external standard.IonPac AS23(250 mm×4.0 mm)anion analysis column and IonPac AG23(50 mm×4.0 mm)guard column were used,the mixture of 4.5 mmol·L-1 Na2 CO3 and 0.8 mmol·L-1 NaHCO3 was used as mobile phase at a flow rate of 1.0 mL·min-1.The column temperature was set at 25℃,the detection cell temperature was set at 30℃.The results indicated that the calibration curves were linear between the peak area and the concentration in the range of 3.6~72 mg·L-1 for sulfur dioxide,the correlation coefficient was greater than 0.999.The method detection limit(MDL)was 0.83 mg·L-1.The average recoveries spiked in sample at the three concentration levels ranged from 97.3%to 101.8%with the relative standard deviations(RSD)of 0.9%~1.8%.The method is suitable for the determination of sulfur dioxide in sulfone.
作者
金玉坤
刘思乐
陶洋
马奥博
JIN Yu-kun;LIU Si-le;TAO Yang;MA Ao-bo(Department of Chemical Engineering,Shenyang Institute of Science and Technology,Shenyang 110000,China;Chemical Safety Technology and Engineering Center,Shenyang Research Institute of Chemical Industry,Shenyang 110000,China)
出处
《当代化工》
CAS
2021年第1期249-252,共4页
Contemporary Chemical Industry
关键词
离子色谱法
二氧化硫
砜
甲醛
Ion chromatography
Sulfur dioxide
Sulfone
Formaldehyde
作者简介
金玉坤(1997-),男,甘肃武威人;通讯作者:刘思乐(1986-),女,副教授,硕士,研究方向:先进能源技术和资源综合利用等。E-mail:sl.0117@163.com。
