【讨论】卤素测试相关问题

,有点冷清...

答案：1.质控样要看你是什么样品，要是检测单位不可能买那么多质控样，
用EC681K是可以的。实在不行，你可以采用加标方法做回收率。
2.你可以采用优化实验，能够达到你的要求就行。
3.那也就是洗了，还有就是买个好点氧弹，实在你担心还可以用回收率


你的回收率低，很可能是没有燃烧完全，或者燃烧密封不好！~！

EC681K在燃烧之后，完全干净，我觉得应该是吸收问题，准备换个方式看看，采取慢慢导出放气吸收，虽然BS EN14582里面提及到，一般大于20mg/kg时才选择这种方式。

我们用的是氧氮燃烧，用5倍的淋洗液作为吸收液，氧氮燃烧的罐子会带来很大的污染，一定要清洗干净

呵呵，做测试过程，一定要注意污染问题,有一次我的同事，在过滤的时候不小心把一些自来水搞（很少量）到空白里面去，当时也没有怎么留意，一测氯离子的尝试为3.0ppm。

回收率一般不会低吧，我想，因为一般都有影响！~只会高才对嘛！~
我们做都是高点！~要不饶就是你们冲洗的时候掉了！~
或者没燃烧完全！~

因为卤素测试吸收一直是个问题，我还没有做过10%吸收，回收率也做不到超过100%！

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.

85%,不错了。

说你低的，俺略怀疑中。。。做的标品多吗？