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煙花爆竹中苦味酸測試的方法的研究

時間:2019-04-20 16:22來源:畢業論文
建立了煙花爆竹中苦味酸成分進行定性和定量分析的方法。分別采用國標法-《煙花爆竹禁限用藥劑檢測方法》(GB/T21242-2007)、紫外分光光度分析法和高效液相色譜法,對煙花爆竹中禁限用

摘要:建立了煙花爆竹中苦味酸成分進行定性和定量分析的方法。分別采用國標法-《煙花爆竹禁限用藥劑檢測方法》(GB/T21242-2007)、紫外分光光度分析法和高效液相色譜法,對煙花爆竹中禁限用藥劑苦味酸進行測試。國標法以顯色反應的方式測定樣品中苦味酸;紫外可見光分光光度法,檢測波長在357.1nm處,苦味酸有較好的峰型,苦味酸的質量濃度在0~100mg/L時,繪制標準曲線線性良好,相關系數為0.999,對煙火藥劑樣品進行3個不同濃度水平的添加回收,相對標準偏差在1.87%~3.23%之間,加標回收率在94.5%~107.4之間;高效液相色譜法,采用Zorbax EclipseXDB–C18柱(4.6×250 mm,5µ m)分離,V(甲醇):V(0.1%冰醋酸水溶液)=55:45,等梯度洗脫,流速0.8mL/min;測定溫度為40℃;本實驗中使用紫外可見檢測器進行光譜檢測,檢測波長在357.1nm處。苦味酸的質量濃度在0.5-20mg/L時與色譜峰面積之間線性關系良好(r=0.9998);在低、中、高三個添加水平,苦味酸的加標回收率為85.3%-93.2%,相對標準偏差(RSD)為1.5%-6.4%。通過優化煙火藥劑中中苦味酸測定的條件,滿足不同人群對煙火藥劑中苦味酸測定的要求。34741
畢業論文關鍵詞:苦味酸;煙火藥劑;紫外分光光譜法;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%.
源¥自%六:維;論-文'網=www.aftnzs.live

Keywords:Picric acid;Pyrotechnic composition;UV qualitative analysis;HPLC
目錄
1    緒論 1
1.1    煙花爆竹用煙火藥劑概述 1
1.1.1     氧化劑 2
1.1.2     可燃劑 2
1.1.3     粘合劑 3
1.2    煙火效應的產生 3
1.3    苦味酸4
2    國標法 5
2.1    樣品與試劑5
2.2    試驗方法5
2.2.1    反應方程式及實驗現象 5
2.2.2    樣品檢測 6
2.2.3    對照實驗 6
2.3    實驗內容討論6
2.3.1     化學方法定性檢測苦味酸 6
2.3.2     萃取劑的選擇 7
2.3.3     影響因素7
3    紫外可見光譜法7
3.1    儀器與試劑7
3.2    檢測波長的確定 7
3.3    溶液配制8
3.3.1     標準溶液配制 8
3.3.2     樣品溶液配制 8
3.3.3     標準曲線繪制 8 煙花爆竹中苦味酸測試的方法的研究:http://www.aftnzs.live/huaxue/20190420/32360.html
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