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问题:如何定量分析计算乳液聚合体系中过氧化氢异丙苯(CHP)的含量?
类型:求助 (悬赏分:3分)
提问:16802378
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版块:分析化学(wangsui,maqinghe,peiliang,)
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时间:2006-03-07 08:22:13  编辑    加入/取消收藏    订制/取消短消息    举报该贴    


各位大侠:

如何定量分析计算乳液聚合体系中过氧化氢异丙苯(CHP)的含量?

各位同行请赐教啊。

h16802378@126.com
回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 08:32:29   编辑 1楼
乳液聚合实验是您自己做的吗?还是想分析别人的样品?所加过氧化氢异丙苯的量的范围在乳液聚合的专著中有的.


回复人:16802378, (乳液聚合;聚合物增韧) 时间:2006-03-07 08:45:02   编辑 2楼
想没自己实验中的CHP残留量


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 10:08:45   编辑 3楼
想测定自己实验中的CHP残留量?建议使用GC法.



回复人:upstart, (药物设计及合成,感兴趣精细化工) 时间:2006-03-07 13:48:24   编辑 4楼
GC法不合适, 过氧化氢异丙苯受热分解. 而且乳液聚合生成高分子,根本不能进行溶液处理.

建议采用化学滴定法(碘/淀粉液)


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:14:10   编辑 5楼
Determination of dicumyl peroxide in workplace air.
Ann Occup Hyg. 2002 Oct;46(7):637-41.
Department of Chemical Environmental Science, Chalmers University of Technology, SE-412 96 Goteborg, Sweden.

A method for the determination of dicumyl peroxide in workplace air was developed and applied. Micro-impinger bottles and personal air sampling pumps were used for the sampling. Gas chromatography/mass spectrometry was used for the analytical separation and quantitative determination. The technique makes it possible to monitor peroxide concentrations down to 5 micro g/m(3) in air.
可参考文中的GC实验条件.


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:14:43   编辑 6楼
Dicumyl peroxide is an organic peroxide. The peroxide bond with its two oxygen atoms is easily broken up. For this reason, organic peroxides are often used as free radical sources in polymerizations and similar reactions. Dicumyl peroxide is among the less reactive of the organic peroxides. Large amounts of dicumyl peroxide are used as cross-linking agents in the polymer industry. Exposure of the workers to this compound may occasionally be high, for example when sacks of dicumyl peroxide are cut open and the peroxide is poured into hot melting tanks. This operation is sometimes performed without any protective equipment


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:18:15   编辑 7楼
Analytical conditions of the GC/MS method (an HP 5890 GC was used)
Analytical column 12 m x 0.20 mm i.d.; J&W
Stationary phase Methyl silicone, DB-1, 0.33 µm
Carrier gas flow 0.5 ml/min; He
Injector 100°C, 0.5 µl injected sample volume, splitless, split valve (1:20) opened after 1 min
Detector MS detector, HP 5970 (quadrupole)
Oven 90°C, 1 min, +50°C/min to 120°C, 25 min
Transfer line 120°C
Auto injector HP 7673A



回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:21:12   编辑 8楼
Fig. 1. Typical chromatogram (GC/MS, single ion monitoring, m/z = 119) from the analysis of dicumyl peroxide in workplace air. Complete mass spectrum of dicumyl peroxide.


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:41:54   编辑 9楼
Fig. 1. Typical chromatogram (GC/MS, single ion monitoring, m/z = 119) from the analysis of dicumyl peroxide in workplace air. Complete mass spectrum of dicumyl peroxide.

对不起由于dicumyl peroxide 的GC,GC-MS的图谱大于10K,上传不了.







回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:44:14   编辑 10楼
再次上传dicumyl peroxide 的GC,GC-MS的图谱


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:48:01   编辑 11楼
下面的文章可用,作者用GC法测定聚合物生产环境中dicumyl peroxide 的量.
http://annhyg.oxfordjournals.org/cgi/content/full/46/7/637
提供楼主参考,建议楼主选择你的样品处理方法.


回复人:celan,▲▲▲▲ (化学品成分和结构剖析服务:www.chemnmr.com) 时间:2006-03-07 15:49:57   编辑 12楼
Cumene Hydroperoxide (CHP) has been used in producing dicumyl hydroperoxide (DCDO) and phenol. In Taiwan, several severe fire and explosion incidents had occurred due to its thermal instability or reactive incompatibilities. In this study, the exothermic decomposition of CHP in cumene was characterized by the isothermal microcalorimeter, TAM (Thermal Activity Monitor). It could investigated the thermal hazards while storing CHP in chemical plant, and determined its thermokinetic data under isothermal condition, such as heat of decomposition, heat flow and time of reaction etc. In this study, thermogram that possessed an autocatalytic phenomenon on decomposition was novel discovered between 75℃ to 90℃. Heat of decomposition and kinetics of autocatalytic behaviors were measured and compared with previous studies.




回复人:upstart, (药物设计及合成,感兴趣精细化工) 时间:2006-03-07 16:34:59   编辑 13楼
Good articles. I learn something. Thanks


回复人:16802378, (乳液聚合;聚合物增韧) 时间:2006-03-09 19:47:49   编辑 14楼
非常感谢:celan and upstart

谢谢你们的知识和热情!



回复人:wangsui,▲▲▲ (我不思故我不在) 时间:2006-05-17 22:46:05   编辑 15楼
已经打分了。


得分人:celan-2,upstart-1,


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