摘要
建立了工业硫酸中二氧化硫的高效液相色谱定量分析方法.首先在低温密闭条件下将工业硫酸稀释,并用氢氧化钠调节pH使二氧化硫转变为亚硫酸钠,随后采用高效液相色谱法测定工业硫酸中的二氧化硫含量.采用SB-AQ色谱柱(250 mm×4.6 mm,5μm),以浓度为50 mmol/L、pH为1.8的磷酸二氢钾与磷酸的缓冲溶液和乙腈作为流动相进行等度洗脱,流速为0.6mL/min,柱温为30℃,检测波长为195nm.方法的准确度高、精密度好、灵敏度高.在高浓度工业硫酸中,二氧化硫的加标回收率达到107.98%,方法的相对标准偏差(RSD)为0.55%,检出限低于1 mg/L.方法不仅可以快速准确的测定工业硫酸中的二氧化硫含量,而且对于样品的无损衍生处理和二氧化硫测试方法开发提供了新思路,具有应用价值.
A high performance liquid chromatography(HPLC)for the determination of sulfur dioxide in industrial sulfuric acid has been established.First,the industrial sulfuric acid sample was diluted under low-temperature closed conditions,and adjust the pH using sodium hydroxide,while sulfur dioxide was converted to sodium sulfite.Then the sulfur dioxide content in the industrial sulfuric acid was determined by HPLC.A SB-AQ column(250 mm×4.6 mm,5μm)was used,and the isocratic elution was carried out with a 50 mmol/L phosphate buffer solution(pH=1.8)and acetonitrile as mobile phase,under the following conditions:a flow rate of 0.6 mL/min,a column temperature of 30°C,and a detection wavelength of 195 nm.The method has high accuracy,good precision and high sensitivity.Under the high concentration conditions,the spiked recovery of sulfur dioxide reached 107.98%,the relative standard deviation(RSD)of was 0.55%,and the detection limit was less than 1 mg/L.It can not only quickly and accurately determine the sulfur dioxide content in industrial sulfuric acid,but also provide a new idea for the non-destructive derivatization of samples and the development of sulfur dioxide detection methods.
作者
梁初燕
王石慧
王慧敏
陈小锋
邓杭军
陈耀
LIANG Chuyan;WANG Shihui;WANG Huimin;CHEN Xiaofeng;DENG Hangjun;CHEN Yao(Zhejiang NHU Special Materials Co.Ltd.,Shaoxing 312300,Zhejiang China)
出处
《分析测试技术与仪器》
2025年第5期285-292,共8页
Analysis and Testing Technology and Instruments
关键词
高效液相色谱法
工业硫酸
二氧化硫
亚硫酸钠
high performance liquid chromatography
industrial sulfuric acid
sulfur dioxide
sodium sulfite
