建筑材料中甲醛含量的柱内衍生HPLC法测定  

Determination of Formaldehyde in Architectural Material by In-column Derivatization Reaction High Performance Liquid Chromatography

作　　者：赵景婵[1] 郭治安[1] 张小辉[1] 梁小云[1] 

机构地区：[1]西北大学化学系,西安710069

出　　处：《应用化学》2007年第1期76-79,共4页Chinese Journal of Applied Chemistry

基　　金：陕西省教委基金项目(03JK075);陕西省自然科学基金(2005B018)

摘　　要：选用偏二甲肼作柱内衍生剂,利用甲醛与偏二甲肼能在适当的pH值条件下生成有较强紫外吸收的偏二甲腙的实验原理,建立了内墙涂料和胶牯剂中甲醛的柱内衍生高效液相色谱测定方法。实验讨论了甲醛与偏二甲肼反应的机理、pH值对亲核加成反应的影响,估算了流动相的pH值范围为2<pH<6。确定了色谱柱为Zorbax ODS柱(150 mm×4．6 mm i．d．,5μm)．流动相为甲醇与含12 mmol／L偏二甲肼的20 mmol／L醋酸盐缓冲溶液(pH=5．0)的体积比为15:85,流速0．8 mL／min,柱温40℃,测定波长为238 nm的最佳分析条件。全面考察了衍生分析方法的各项指标,其中甲醛衍生物测试的回归方程为:A=8 904X-49．27,相关系数r=0．999 9,线性范围30～300 mg／L,最低检出限为5 ng,样品测试的精密度RSD在1．02％～1．51％之间,加样回收率在95．90％～102．49％。对内墙涂料和胶粘剂中的甲醛进行了定量分析,各种待测物质的测定相对标准偏差小于2．0％。方法简便快速,重现性和准确度令人满意,可作为内墙涂料和胶粘剂中甲醛含量的有效方法。An in-column derivatization high performance liquid chromatographic method for the determination of formaldehyde in inner wall paints and adhesives was developed. The reaction mechanism of formaldehyde and unsymmetrical dimethyl hydrazine （UDMH）, and the effect of pH on nucleophilic addition were discussed. The optimal range was between 2 and 6, and chromatographic conditions were： the column： Zorbax ODS（ 150 mm ×4. 6 mm i. d. , 5 μm）, the mobile phase： mixture of methanol-20 mmol/L acetate buffer（pH ≈5.0） containing 12 mmol/L UDMH （15：85, volume ratio）, the flow rate： 0. 8 mL/min, the column temperature ： 40 ℃, the detection wavelength ： 238 um. The regression equation is A = 8 904X - 49. 27, and the correlation coefficient is 0. 999 9. The linear range and detectable limit were 30 - 300 mg/L and 5 ng, respectively. The recovery was 95.90% - 102. 50% and RSD was 1.02% - 1.51%. The method has proven to be fast, simple, sensitive, accurate and reproducible with respect to other chromatographic methods that have been reported. It can be used for the routine analysis of formaldehyde in inner wall paints and adhesives.

关 键 词：柱内衍生高效液相色谱法 内墙涂料和胶粘剂 甲醛 含量测定 

分 类 号：O658[理学—分析化学]