Sampling

定容样品(自动液体进样) 定容样品(自动液体稀释进样) 一般选择方法6022801

0.1g正己醇+4g酒精+1g样品,并标好标签(标签可于 Chemical Analytic Project 中找到), 原样品和分析样品都要写上项目编码。

EF >>>>> 洗涤
CF >>>>> 洗护
AF >>>>> 香水
FF >>>>> 香氛
BF >>>>> 膏霜
P  >>>>> 成品

加入完成后,将其定容到1ml置于小型样品瓶(可在GC-MS最右侧抽屉中找到)中, 并标好标签。

直接进样

直接进样指的是当样品通过稀释之后,发现样品比较浑浊,无法通过6022801的方法进样(浑浊液无法通过针头实现均衡取样)。这个时候,只能通过直接取样,然后使用602280的方法进行进样。

SPME(Solid-Phase MicroExtraction)

若怀疑针头比较脏,可以用色谱纯的甲醇进行清洗。

操作步骤:

  1. 将SAAA-SPME-05 探针装入SPME手动或自动手柄中;

  2. 老化:将SPME探针插入GC进样口260度老化20min(探针萃取头略微变黄);

  3. 萃取:将SPME探针针管穿透样品瓶隔垫, 插入样品瓶中。推动手柄杆,伸出探针萃取头,探针萃取头可以进入水溶液中(浸入方式)或置于样品上部空间(顶空方式)进行萃取,萃取时间为5-60min. 收回探针萃取头,并将探针抽出样品瓶;

  4. GC进样: 将SPME探针针管插入GC进样口,推动手柄杆,伸出探针萃取头,热脱附分析物使其进入色谱柱,脱附时间为1-5min. 收回探针萃取头, 并将探针抽出进样口。

点开运行序列,按下Prep Run, 待Ready红灯熄灭之后,将导向器放在进样口,将SPME插入,将针头旋出, 开始运行。

SPME配制样品: 1%样品+饱和食盐水,总共配制成5g, 一般采用双倍配制,即0.1克样品溶解在10g溶液中。

谱图分析

  1. 一个峰中出现离子碎片变化比较大;

  2. 有时电脑也会一种物质判定成两种进行积分;

  3. 定时拆分帮助文档;

  4. 手段积分:Alt+T+T+M;

  5. 修正面积误差 1%-2%。

Direct Extraction

If time is limited, you can use the direct extraction. Simply use 10g a mixture of pentane and dichloromethane with ratio of 1:1 as solvent to dissolve the product, and then use a glass flask as a container (do not use a plastic one since dichloromethane is a strong solvent and it might dissolve the polymer part of a plastic flask).

Manual Sampling

Carefully take off the metal needle from the injector and then absorb 2ul detergents to wash up the needle about 10 times (try not to bend down the needle). Then absorb 1ul detergents and pull out the needle of the vesper, absorb some air and inject the needle into the vesper again and absorb 1ul detergents and push out the liquid immediately. Next, moist the needle with the extractant.

Tne Quantity of Rejection

For highly concentrated solution, you only need to drop down 0.5 ul liquid into the little container and select the method 602280 for rejection. For solutions with low concentration, you need to drop down 1 ul liquid into the little container and select the method 6022801 for rejection, in which 1 stands for 1 ul. As to split ration, just choose the right one.