by 
mbdixon » Tue Jan 02, 2024 10:28 am
													
 
					
						I get the same thing with my Glycols analysis and would like to know why.
https://photos.app.goo.gl/soyBceYcpsisxDdz6
 
The above chromatogram has a broad peak for ethylene glycol at 6.2 mins and a nice sharp peak for diethylene glycol at 7.8 mins.
The matrix is water and the method is :
Sample Volume (uL):                        0.5
Mode                                         Pulsed Splitless
Heater                                       On    280 °C
Pressure                                     On    3.2572 psi
Total Flow                                   On    64.5 mL/min
Septum Purge Flow                            On    3 mL/min
Gas Saver                                    On    20 After 2 min mL/min
Injection Pulse Pressure                     20 psi Until 0.5 min
Purge Flow to Split Vent                     60 mL/min at 1 min
Liner                                       AG0-8173 Liner for Agilent (4 mm ID x 78.5 mm L x 6.3 mm OD), Split/Splitless, Dual Taper, 5/Pk 
Oven
Equilibration Time                           1 min
Max Temperature                              250 °C
Maximum Temperature Override                 Disabled
Slow Fan                                     Disabled
Temperature
Setpoint                                     On
(Initial)                                    40 °C
Hold Time                                    0 min
Post Run                                     240 °C
Program
#1 Rate                                      20 °C/min
#1 Value                                     210 °C
#1 Hold Time                                 0 min
Column Information                           Phenomenex 7HG-G013-11: 1135458
ZB-WAXplus                                   
Temperature Range                            -60 °C—250 °C (250 °C)
Dimensions                                   30 m x 250 μm x 0.25 μm
Column lock                                  Unlocked
In                                           Front SS Inlet H2
Out                                          MSD 
(Initial)                                    40 °C
Pressure                                     3.2572 psi
Flow                                         1.5 mL/min
Thermal Aux 2 (MSD Transfer Line)
Temperature
Setpoint                                     On
(Initial)                                    250 °C
Post Run                                     0 °C
[SIM Parameters]
Group 1               Group ID                  :  Glycols (227)
Resolution                : 1
Group Start Time          : 5
Number of Ions            : 6
Ions
Dwell In Group            

  Mass,  Dwell) (  Mass,  Dwell)  (  Mass,  Dwell) 
                           (  31.10,50  )  (  33.10,50  )  (  45.10,50  ) 
                           (  62.00,50  )  (  75.00,50  )  (  76.00,50  )