售后分享之一：标准品进样不出峰，真乃怪事情！

上海安谱

2012/05/25

私聊

厂商论坛

真实案例：客户买了标准品，进样后不出峰，用自己配置的内标进样，居然出的好好的，真是怪事，问题出在哪里呢？考考你的慧眼

图1为39种混标1ppm的谱图，该溶液的配制方法为：在10mL棕色容量瓶中先加入少量正己烷，用微量进样针（0.1mL）移取0.2mL 39种PBDEs混标母液（50ppm）至容量瓶中，再用正己烷定容、摇匀。取1mL该溶液至棕色GC小瓶，用GC-MS测定。图1和图2均使用图3和图4的质谱色谱条件，色谱柱为DB-5ms。

图1 39种混标（1ppm）谱图

图2为 39种混标（2ppm）+BDE-77、BDE-118、BDE-128、BDE-181单标（2ppm）的谱图。配制方法：取1mL 2ppm内标溶液（BDE-118，128），2mL 1ppm替代物溶液（BDE-77，181），2mL 1ppm39种混标溶液，置于氮吹管中，用柔和氮气吹干后加入1mL正己烷，充分振荡、涡旋后移至棕色GC小瓶中。理论上，BDE-77、118和181的浓度为4ppm，其他单体为2ppm。

但在图2的谱图中只有4个明显的峰，根据质谱，从右到左分别是7溴、6溴、5溴和4溴代物，判断可能分别是BDE-181、128、118和77，即所添加的内标和替代物。

图2 39种混标（2ppm）+BDE-77、BDE-118、BDE-128、BDE-181单标（2ppm）的谱图

图3 质谱条件

相关话题

+关注

私聊

上海安谱

第1楼2012/05/25

标准品证书：

Product Detail Page

Catalog Number: BDE-AAP-A
Number Of Components: 39
Concentration: Varied conc in Isooctane
Description: PBDEs Standard Solution for Accuracy & Precision
Storage Condition: Ambient
Unit: 1 mL
Price: $195.00
Comments:

To add this product to your order, scroll down to the bottom of the page and select from the options available.

Component	CAS	Concentration (either)
Component	CAS	Units: ng/mL	Units,Weight:
2’,3,4-Tribromodiphenyl ether	147217-78-5	100
2-Bromodiphenyl ether	N/A	100
2,2',3,4,4',5',6-Heptabromodiphenyl ether	207122-16-5	250
2,2’,3,4,4’,5’-Hexabromodiphenyl ether	182677-30-1	200
2,2’,3,4,4’,5,6-Heptabromodiphenyl ether	189084-67-1	250
2,2’,3,4,4’-Pentabromodiphenyl ether	182346-21-0	150
2,2’,4,-Tribromodiphenyl ether	147217-75-2	100
2,2’,4,4’,5-Pentabromodiphenyl ether	60348-60-9	150
2,2’,4,4’,5,5’-Hexabromodiphenyl ether	68631-49-2	200
2,2’,4,4’,5,6’-Hexabromodiphenyl ether	207122-15-4	200
2,2’,4,4’,6-Pentabromodiphenyl ether	189084-64-8	150
2,2’,4,4’,6,6’-Hexabromodiphenyl ether	35854-94-5	200
2,2’,4,4’-Tetrabromodiphenyl ether	5436-43-1	100
2,2’,4,5’-Tetrabromodiphenyl ether	243982-82-3	100
2,3’,4’,6-Tetrabromodiphenyl ether	189084-62-6	100
2,3’,4-Tribromodiphenyl ether	147217-77-4	100
2,3’,4,4’,5-Pentabromodiphenyl ether	N/A	150
2,3’,4,4’,6-Pentabromodiphenyl ether	189084-66-0	150
2,3’,4,4’-Tetrabromodiphenyl ether	189084-61-5	100
2,3,3’,4,4’,5,6-Heptabromodiphenyl ether	189084-68-2	250
2,3,4,4’,5,6-Hexabromodiphenyl ether	189084-58-0	200
2,3,4,5,6-Pentabromodiphenyl ether	N/A	150
2,4’,6-Tribromodiphenyl ether	189084-60-4	100
2,4’-Dibromodiphenyl ether	N/A	100
2,4-Dibromodiphenyl ether	N/A	100
2,4,4’,6-Tetrabromodiphenyl ether	189084-63-7	100
2,4,4’-Tribromodiphenyl ether	41318-75-6	100
2,4,6-Tribromodiphenyl ether	N/A	100
2,6-Dibromodiphenyl ether	N/A	100
3-Bromodiphenyl ether	6876-00-2	100
3,3’,4-Tribromodiphenyl ether	147217-80-9	100
3,3’,4,4’,5-Pentabromodiphenyl ether	N/A	150
3,3’,4,4'-Tetrabromodiphenyl ether	93703-48-1	100
3,3’-Dibromodiphenyl ether	N/A	100
3,4’-Dibromodiphenyl ether	N/A	100
3,4-Dibromodiphenyl ether	N/A	100
3,4,4’-Tribromodiphenyl ether	147217-81-0	100
4-Bromodiphenyl ether	101-55-3	100
4,4’-Dibromodiphenyl ether	2050-47-7	100