原子吸收测定明胶胶囊中铬知识课件知识讲稿

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1、Slide title: Font: Myriad or Arial, 36ptSub title (Author):Font: Myriad or Arial,18ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings.岛津“毒胶囊”中重金属测定解决方案 岛津企业管理(中国)有限公司市场部 杨乐 Headline for slide: In case of one-line: Myriad or Arial 32

2、ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings 岛津-明胶空心胶囊中铬测定解决方案Headline for slide: In case of one-line: Myriad or Arial 32ptIn cas

3、e of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings2010版中国药典涉及重金属的种类根据样品的特点选择不同的原子化器冷原子法(CVAAS)氢化物法(HGAAS)火焰法(FAAS)石墨炉法(GFAAS)l Pb:5.0 ppm (石墨炉)

4、l Cd:0.3 ppm (石墨炉)l As:2 .0ppm (氢化物)l Cu:2 0 ppm (火焰 )l Hg:0.2 ppm (冷吸收)l Cr :2.0ppm (石墨炉)l Sn:0.1ppml Ba:3.0ppm 药用辅料:从72种 增加 到132种Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size:

5、Sizes can be adjusted depending on the text length. Characters should not be overlapped on global stringsHeadline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depe

6、nding on the text length. Characters should not be overlapped on global strings未来的明胶空心胶囊的标准火焰石墨炉氢化物冷汞HgAsCrCdl 重金属以铅计不得多百万分之四十PbHeadline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Siz

7、es can be adjusted depending on the text length. Characters should not be overlapped on global strings微波消解石墨炉原子吸收法测定明胶胶囊的铬含量剪碎精密称取0.5g+8mlHNO3 微波消解60min (0.5ml HF)赶酸2%硝酸定容测定AA-7000Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad o

8、r Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings前处理-微波消解l取样0.5g,加硝酸510mll浸泡过夜、消解、赶酸、缓缓浓缩至13ml,放冷, 用2%硝酸转入 50ml 量瓶中,并稀释至刻度。l严格遵守操作规程和安全使用守则l优点:效率高,可以消除环境对样品的污染 ,待测元素挥发损失小,由于酸用量很少,因此可大幅降低空白值。l药典规定

9、:Pb、Cd、As、Cu、Hg,Cr都适用.7目前,最先进的元素分析样品前处理方法,在2010版药典中作为首选方法。Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not

10、 be overlapped on global strings测定条件的选择 在进行原子吸收光谱测定时,为了获得灵敏、重现性好和准确的结果,应对测定条件进行优选。 l 吸收线的选择l 通带宽度选择 l 空心阴极灯的工作电流 l 原子化条件选择 Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes ca

11、n be adjusted depending on the text length. Characters should not be overlapped on global strings光谱条件的选择l分析线的选择 一般选择最灵敏线,但当测定高含量的元素或在最灵敏线处有干扰时可选择次灵敏线,注意,选择不同的分析线测定的稳定性会有差别。l狭缝宽的选择狭缝越大,光强度越大,信噪比越好,读数越稳定,但如果邻近有干扰线通过时会降低灵敏度,标准曲线弯曲。狭缝越小,光强度越弱,信噪比差,读数不稳定,但光的单色性好,测试的灵敏度较高狭缝的选择原则:有保证只有分析线通过的前提下,尽可能选择较宽的狭缝以

12、保证较好的信噪比和读数稳定性Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings分析条件的选择选择l灯电

13、流 灯电流大,能量读数稳定,对于常量和高含量分析可提高测定的精密度,但灯电流大会缩短灯的寿命 灯电流小,灯发射的谱线的多谱勒变宽和自吸收效应变小,吸收灵敏度增高,但读数不稳定,噪音较大 选用灯电流的一般原则是,在保证有足够强且稳定的光强输出条件下,尽量使用较低的工作电流。 Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont

14、size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings分析条件优化结果灯电流l 10mA狭缝:l 0.2nm灵敏度和稳定性波长357.9Headline for slide: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or

15、Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings原子化条件优化-石墨炉升温程序干燥灰化原子化清洁蒸发溶剂 组分分馏盐类挥发待测元素原子化 净化石墨管 防止溶液爆沸 测定元素不损失 测定元素形态一致 确保待测元素原子化充分 完全清除石墨管内残存物质 120-150400-1300 1200-2500 2000-2600 斜坡升温 斜坡升温、保持 快速升温 快速升温Headline for sli

16、de: In case of one-line: Myriad or Arial 32ptIn case of two-lines: Myriad or Arial 28ptSubhead: Myriad or Arial 28ptText: Myriad or Arial 20ptFont size: Sizes can be adjusted depending on the text length. Characters should not be overlapped on global strings升温程序的选择干燥阶段时间: 根据进样量,每微升2-3秒温度: 略高于溶剂沸点。水110130摄氏度。在溶剂蒸干之前,超过沸点的温度易导致沸腾迸溅,可采用斜坡升温或多个升温阶段避免。特别对于稀释后粘度高的样品,要采用温和的斜坡升温并延长干燥时间,以防迸溅。灰化阶段要求在不损失待测元素的前提下,尽量挥发干扰元素。选择灰化温度和时间的原则:在保证被测元素不损失的条件下尽量采用较高的温度和较长的灰化时间。如果待测元素熔点低,那么可以加基体改进剂。目的:与待测元素结合为低挥发性的化合物,

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