안녕하세요,
저는 Agilent 6890 GC와 5973 MSD에서 Purge & Trap을 사용하여 VOC를 분석하고 있습니다.
최근에 보정이 틀린 것 같다는 생각이 들어서 문의드리고 싶습니다.
Vocarb 3000 트랩 교체, 라이너 교체, 소스 세척 등 다양한 솔루션을 시도했지만 3분 범위의 대상 화합물에 대한 교정은 여전히 비정상적인 것으로 보입니다.
잠재적인 문제점을 파악하는 데 도움을 주시겠습니까?
감사합니다.
추가 지원이 필요하면 언제든지 알려주세요!
INSTRUMENT CONTROL PARAMETERS: MSD
-------------------------------------
C:\MSDCHEM\1\METHODS\VOCS METHOD 2024 7~12\VOCS SIM17-20241217.M
Tue Dec 17 15:39:11 2024
Control Information
------- -----------
Sample Inlet : GC
Injection Source : External Device
Mass Spectrometer : Enabled
No Sample Prep method has been assigned to this method.
=============================================================================
6890 GC METHOD
=============================================================================
OVEN
Initial temp: 35 'C (On) Maximum temp: 320 'C
Initial time: 4.00 min Equilibration time: 0.50 min
Ramps:
# Rate Final temp Final time
1 10.00 120 0.00
2 40.00 220 0.00
3 0.0(Off)
Post temp: 0 'C
Post time: 0.00 min
Run time: 15.00 min
FRONT INLET (UNKNOWN) BACK INLET (SPLIT/SPLITLESS)
Mode: Split
Initial temp: 250 'C (On)
Pressure: 6.75 psi (On)
Split ratio: 40:1
Split flow: 39.9 mL/min
Total flow: 43.8 mL/min
Gas saver: Off
Gas type: Helium
COLUMN 1 COLUMN 2
(not installed) Capillary Column
Model Number: J&W 122-5532
DB-5ms
Max temperature: 325 'C
Nominal length: 30.0 m
Nominal diameter: 250.00 um
Nominal film thickness: 0.25 um
Mode: constant flow
Initial flow: 1.0 mL/min
Nominal init pressure: 6.76 psi
Average velocity: 36 cm/sec
Inlet: Back Inlet
Outlet: MSD
Outlet pressure: vacuum
FRONT DETECTOR (NO DET) BACK DETECTOR (NO DET)
SIGNAL 1 SIGNAL 2
Data rate: 20 Hz Data rate: 20 Hz
Type: test plot Type: test plot
Save Data: Off Save Data: Off
Zero: 0.0 (Off) Zero: 0.0 (Off)
Range: 0 Range: 0
Fast Peaks: Off Fast Peaks: Off
Attenuation: 0 Attenuation: 0
COLUMN COMP 1 COLUMN COMP 2
(No Detectors Installed) (No Detectors Installed)
THERMAL AUX 2
Use: MSD Transfer Line Heater
Description:
Initial temp: 280 'C (On)
Initial time: 0.00 min
# Rate Final temp Final time
1 0.0(Off)
POST RUN
Post Time: 0.00 min
TIME TABLE
Time Specifier Parameter & Setpoint
GC Injector
Front Injector:
No parameters specified
Back Injector:
No parameters specified
Column 1 Inventory Number :
Column 2 Inventory Number : DB-5ms
MS ACQUISITION PARAMETERS
General Information
------- -----------
Tune File : atune.u
Acquistion Mode : SIM
MS Information
-- -----------
Solvent Delay : 1.50 min
EMV Mode : Relative
Relative Voltage : 0
Resulting EM Voltage : 2259
[Sim Parameters]
GROUP 1
Group ID : 1
Resolution : Low
Plot 1 Ion : 49.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 49.00, 100) ( 61.00, 100) ( 84.00, 100)
( 86.00, 100) ( 96.00, 100) ( 98.00, 100)
GROUP 2
Group ID : 2
Resolution : Low
Group Start Time : 2.30
Plot 1 Ion : 47.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 47.00, 100) ( 83.00, 100) ( 85.00, 100)
GROUP 3
Group ID : 3
Resolution : Low
Group Start Time : 2.70
Plot 1 Ion : 61.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 61.00, 100) ( 77.00, 100) ( 78.00, 100)
( 97.00, 100) ( 99.00, 100) (117.00, 100)
(119.00, 100) (121.00, 100)
GROUP 4
Group ID : 4
Resolution : Low
Group Start Time : 3.60
Plot 1 Ion : 95.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 83.00, 100) ( 85.00, 100) ( 95.00, 100)
(127.00, 100) (130.00, 100) (132.00, 100)
GROUP 5
Group ID : 5
Resolution : Low
Group Start Time : 5.00
Plot 1 Ion : 91.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell)
( 91.00, 100) ( 92.00, 100)
GROUP 6
Group ID : 6
Resolution : Low
Group Start Time : 6.00
Plot 1 Ion : 127.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
(127.00, 100) (129.00, 100) (131.00, 100)
(166.00, 100) (168.00, 100)
GROUP 7
Group ID : 7
Resolution : Low
Group Start Time : 7.00
Plot 1 Ion : 77.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 77.00, 100) ( 91.00, 100) (106.00, 100)
(171.00, 100) (173.00, 100) (175.00, 100)
GROUP 8
Group ID : 8
Resolution : Low
Group Start Time : 10.00
Plot 1 Ion : 115.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
(115.00, 100) (150.00, 100) (152.00, 100)
GROUP 9
Group ID : 9
Resolution : Low
Group Start Time : 11.80
Plot 1 Ion : 157.00
Ions/Dwell In Group ( Mass, Dwell) ( Mass, Dwell) ( Mass, Dwell)
( 75.00, 100) (155.00, 100) (157.00, 100)
[MSZones]
MS Source : 230 C maximum 250 C
MS Quad : 150 C maximum 200 C
END OF MS ACQUISITION PARAMETERS
TUNE PARAMETERS for SN: US10481150
-----------------------------
Trace Ion Detection is OFF.
EMISSION : 34.610
ENERGY : 69.922
REPELLER : 32.971
IONFOCUS : 89.208
ENTRANCE_LE : 19.000
EMVOLTS : 2258.824
Actual EMV : 2258.82
GAIN FACTOR : 2.14
AMUGAIN : 2321.000
AMUOFFSET : 125.000
FILAMENT : 1.000
DCPOLARITY : 0.000
ENTLENSOFFS : 16.816
MASSGAIN : 292.000
MASSOFFSET : -9.000
END OF TUNE PARAMETERS
------------------------------------
END OF INSTRUMENT CONTROL PARAMETERS
------------------------------------
|
Compound |
R.T. |
QIon |
|
|
I.S |
1,2-Dichlorobenzene-d4 |
11.145 |
152 |
|
1 |
1,1-Dichloroethene |
1.852 |
61 |
|
2 |
Dichloromethane |
1.933 |
84 |
|
3 |
Chloroform |
2.562 |
83 |
|
4 |
1,1,1-Trichloroethane |
2.799 |
97 |
|
5 |
Carbon tetrachloride |
3.013 |
117 |
|
6 |
Benzene |
2.998 |
78 |
|
7 |
Trichloroethylene |
3.691 |
95 |
|
8 |
Bromodichloromethane |
3.99 |
83 |
|
9 |
Toluene |
5.322 |
91 |
|
10 |
Tetrachloroethylene |
6.284 |
166 |
|
11 |
Dibromochloromethane |
6.216 |
129 |
|
12 |
Ethylbenzene |
7.637 |
91 |
|
13 |
m,p-Xylene |
7.879 |
106 |
|
14 |
o-Xylene |
8.351 |
106 |
|
15 |
Bromoform |
8.351 |
173 |
|
16 |
1,2-Dibromo-3-Chloropr... |
12.184 |
157 |
