主题:【讨论】卤素测试相关问题

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mattzhang
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原文由 fgx1008(fgx1008) 发表:
If you deal with the preparation well during combustion ofsample, the recovery rate is perfect. I have detected a lot of sample for determination of chloride and bromide ion, and the range of recovery rate is from 95.63% to 109.53%. It meets the requirement of EN 14582. Concerning to the test of halogen ion by combustion ways, the following content ought to be pay attention to carefully.
1)All vessels must be very clean, and they must be rinsed by ultrapure water;
2)All receiving solution must be used ultrapure water to dissolve or dilute, and the concertration of receiving solution ought to be accordant during test period.
3)The sample must be burnt completely.
4)The oxygen vessel must be cleaned for three times at least. and confrim it is very clean.
5)After the samples are burnt, the gas in oxygen vessel ought to be receipted in eluent solution.
6)The content of chloride or bromide ion must be at the middle of standard curve.
7)The CC of standard curve must be greater than 99.9%.
8)Operator or analyst must verify the standard curve everytime of test. it is possible, suggest you make the standard curve everytime.
9)The IC ought to be steadby about the single of detector before carrying out the test.


高手! 英语很棒!
mattzhang
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卤素测试本来回收率就低,主要是燃烧 和润洗的是否充分. 润洗很重要
silviakwok
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请问各位大虾,过程空白应该怎么做呢?
如果什么都不加的话是不能点燃的吧?
那么与样品相比就没有了燃烧的过程了呀
hpcjr8076
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关键是样品前处理,一定要燃烧充分,此外,水质要求要很高。
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84575763
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我之前做过各种实验,经常是当时回收率到了90%以上后,坚持了一段时间后发现回收率又降低了,现在我都不知道怎么去改进前处理方法了,有时候我都怀疑是不是仪器或色谱柱出现了问题,但从基线和标液的情况来看色谱柱应该是没问题的,好困惑啊!!!
steven_lly
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从样品\前处理\仪器逐个排查,实验出现了与一直之前做得有点不同了,会有点意思,不然就是不断的重复的完成工作任务了。
y820gm
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爆发吧,小宇宙
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淋洗液有没有问题,吸收不好就会回收低的,但是你的85%回收应该不错了。
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