求助,HJ 703-2014土壤21种酚类化合物怎么做才能全部出峰?
最近按照HJ 703-2014 土壤和沉积物 酚类化合物的测定 气相色谱法 这个标准做标准物质(Accustandard,货号M-8041,21种酚类混合 1mg/mL),发现只出了15个峰。如下图1(50ppm和100ppm)
仪器参数完全按照标准,进样口温度260℃,10:1分流进样,FID280℃,HP-1ms(30m*0.25mm*0.25um),柱流速1.0mL/min。程序升温下图2
图1
[img=,421,256]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141223302695_6623_2428659_3.png!w421x256.jpg[/img]
图2
[img=,690,253]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141223448804_1586_2428659_3.png!w690x253.jpg[/img]
方法有提及到用中等极性柱做,我就将HP-1MS柱更换成HP-5ms柱,稍微更改了下柱温箱的升温程序(图3),21种酚类化合物(50ppm和100ppm)的谱图出峰如下图4
图3
[img=,438,212]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141223581794_9571_2428659_3.png!w438x212.jpg[/img]
图4
[img=,690,227]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141224276074_9375_2428659_3.png!w690x227.jpg[/img]
另附标物证书图5
[img=,464,589]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141225181155_1274_2428659_3.png!w464x589.jpg[/img][img=,465,623]https://ng1.17img.cn/bbsfiles/images/2018/05/201805141225184585_463_2428659_3.png!w465x623.jpg[/img]