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摘要:建立了烟花爆竹中苦酸成分进行定性和定量分析的方法。分别采用国标法-《烟花爆竹禁限用药剂检测方法》(GB/T21242-2007)、紫外分光光度分析法和高效液相色谱法，对烟花爆竹中禁限用药剂苦酸进行测试。国标法以显色反应的方式测定样品中苦酸；紫外可见光分光光度法，检测波长在357.1nm处，苦酸有较好的峰型，苦酸的质量浓度在0～100mg/L时，绘制标准曲线线性良好，相关系数为0.999，对烟火药剂样品进行3个不同浓度水平的添加回收，相对标准偏差在1.87%～3.23%之间，加标回收率在94.5%～107.4之间；高效液相色谱法，采用Zorbax EclipseXDB–C18柱（4.6×250 mm，5µ m）分离，V（甲醇）:V(0.1%冰醋酸水溶液)=55:45，等梯度洗脱，流速0.8mL/min；测定温度为40℃；本实验中使用紫外可见检测器进行光谱检测，检测波长在357.1nm处。苦酸的质量浓度在0.5-20mg/L时与色谱峰面积之间线性关系良好（r=0.9998）；在低、中、高三个添加水平，苦酸的加标回收率为85.3%-93.2%，相对标准偏差（RSD）为1.5%-6.4%。通过优化烟火药剂中中苦酸测定的条件，满足不同人群对烟火药剂中苦酸测定的要求。34741
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毕业论文关键词：苦酸；烟火药剂；紫外分光光谱法；HPLC；
The Study on the Determination of Picric Acid in Pyrotechnics
Abstract: A method for the determination of picric acid in pyrotechnic composition byqualitative and quantitative analysis was developed. Using the national standard method (GB/T21242-2007. Restriction of pyrotechnic composition detection methods，UV qualitative analysis, high performance liquid chromatography to detectpicric acid. GB method determinated picric acid sample by the way of color reaction. The UV qualitative analysis’s detection wavelength was 357.1nm, picric acid have excellent peak shape. Standard curve was good linear relationships when the mass concentration in the range of 0.5-20mg/L(r=0.9998)，the recoveries were 94.5%-107.4% with the relative standard deviations of 1.87-3.23%. A high performance liquid chromatography (HPLC) method was developed for the determination of picric acid in Pyrotechnic composition. The HPLC separation was performed on a Zorbax Eclipse XDB-C18 column with a gradient elution program of methanol-0.1%acetic acid solution as the mobile phase at the flow rate of 1.0 mL/min and 25℃. The detection wavelength was 274 nm. There were good linear relationships between the mass concentrations and the peak areas of gallic acid in the range of 0.5-20.0 µg/mL(r=0.9999). The recoveries were 85.3-93.2% with the relative standard deviations of 1.5-6.4%.
Keywords：Picric acid；Pyrotechnic composition；UV qualitative analysis；HPLC
目录
1 绪论 1
1.1 烟花爆竹用烟火药剂概述 1
1.1.1 氧化剂 2
1.1.2 可燃剂 2
1.1.3 粘合剂 3
1.2 烟火效应的产生 3
1.3 苦酸4
2 国标法 5
2.1 样品与试剂5
2.2 试验方法5
2.2.1 反应方程式及实验现象 5
2.2.2 样品检测 6
2.2.3 对照实验 6
2.3 实验内容讨论6
2.3.1 化学方法定性检测苦酸 6
2.3.2 萃取剂的选择 7
2.3.3 影响因素7
3 紫外可见光谱法7
3.1 仪器与试剂7
3.2 检测波长的确定 7
3.3 溶液配制8
3.3.1 标准溶液配制 8
3.3.2 样品溶液配制 8
3.3.3 标准曲线绘制 8