【求助】四氯硝基苯

应助达人

看日本官方公布的单独法中包括这个项目.方法名称是:
六六六、林丹、滴滴涕、艾氏剂和狄氏剂、丁氟消草、氯唑灵、异狄氏剂、五氯硝基苯、氯丹、三氯杀螨醇、四氯硝基苯、四氯杀螨砜、七氟菊酯、氟乐灵、苄螨醚、甲氰菊酯、六氯苯、七氯、乙丁氟灵和甲氧滴滴涕检测方法（农产品）
找找看能不能找到.

应助达人

日本的一齐法GCMS就包括这个项目.
下面是一个可以看到方法的链接:
http://www.fsr.org.cn/method_file/law/BA30DAE.PDF
附表的93项目有它的定量粒子和参考粒子.

用GC-ECD应该可以

这种物质用ECD的灵敏度应该很好的。

我用硫酸磺化的方法， 用ECD检测， 可是回收率都在50-60%左右，我不知道怎么做才能提高回收率啊？难道测四氯硝基苯不能用磺化的方法么？谢谢！

你好！四氯硝基苯是否能用磺化方法来净化，您可以单独对磺化这一步骤进行回收率实验，看看回收率怎么样？

这里有一篇文献，您可以参考一下：
四氯硝基苯环境卫生标准的研究结果和建议
此外，您也可以检索一下外文的tetrachloronitrobenzene检测方法。

四氯硝基苯在旋蒸的时候要注意真空度不要太低了，真空度太低了回收率低！

High-Performance Liquid Chromatographic Determination of TCNB(tetrachloronitrobenzene) in Potatoes
R. J. Bushway, et al.;
Journal of Liquid Chromatography & Related Technologies, Volume 7, Issue 6 May 1984 , pages 1185 - 1193

Abstract:
A high-performance liquid chromatographic (HPLC) method was developed for the determination of TCNB (tetrachloronitrobenzene), a sprout inhibitor, in potato peels and flesh fortified at levels of 0.16 to 53.5 ppm. TCNB was analyzed on a u Bondapak C18 column with UV detection at 210 nm. The mobile phase was acetonitrile-methanol-water (35:35:30) at a flow rate of 1.0 ml/min. Retention time was approximately 10 min. TCNB was extracted by blending for 5 min in acetone. Samples at a level of 1 ppm or higher were directly injected whereas samples below 1 ppm were partitioned into hexane followed by passage through an alumina column. Average recoveries varied from 85.6 to 96.8% with coefficients of variation ranging from 2.18 to 11.68%. A study conducted to test 23 pesticides for possible interferences with TCNB demonstrated that none of them co-chromatographed. The lower limit of detection was 0.08 ppm.

http://www.informaworld.com/smpp/content~content=a767985356~db=all