gc/ms ppt !#$%&' - agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122...
TRANSCRIPT
![Page 1: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/1.jpg)
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C. Kai Meng
Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610
USA
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![Page 2: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/2.jpg)
�� !"#$%&'
� 6890 GC��� !"#$%�PTV�[2,3]��
� 5973�� !"#$�MSD�
� 7683�� !"#$�ALS��� !"#$%
� HP-5MS�� !�30 m�0.25 mm�0.25 µm��
P/N 19091S-433
� G1701BA�� B.00.00 MSD ChemStation��
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� G1049A MSD RTL�� !"
�� ! �� ! ��
�� 25 L (50 L�� !" 1 L (10 L�� !"(�� ) �� 5183-0318) �� 9301-0713)
�� ! �� @ 100 L/min ���� @ 300 L/min�� @ 4500 L/min
�� !" 40(0.35)/600/320 280 �(3)/50/200�� !"
�� �� !� 0.29 min�� !� 150 mL/min�� !� 0.00 psi
�� 60 ml/min @ 2 min 60 ml/min @ 2 min
�� �� �� �� �� (P/N 5183-2037) (P/N 5183-2037)
�� !" �� CO2
�
� 1. GC�� !
�� 70(2)/25/150(0)/3/200(0)/8/280(10) = 41.87 min
�� PTV
�� !" 17.30 psi�� !"#$%&'( 16.593 min���� !
� 2. �� !
�� ! 3 min
�� ! Atune.u
�� 280 �
�� 150 �
�� 230 �
�� 150
�� # 2
�� ! 35-500 amu�� !"#�
40 � SIM ��SIM���
� 3. MS�� !
� 4. SIM�� !"#$%&
Extraction window � 0.100 minuteQualifier mode AbsoluteQualifier% 30Zero qualifiers LncludedSubtraction mode Average start/stopScreen database Rtlpest.SCD
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RTL[1]�� !
1. �� !"#$%&'()*
2. �� !"#$%&'()*
3. �� RTL�� !"#$%&��'(
4. �� !"#$%&�RT��� !"�#$
5. �� !"#SIM�� !"#$%&�RT���
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6. �� SIM�� !"#
�� !"#80�� !"#$%&'()*+,-
�� !"�� !"#$%5000 pg/µL��� !
���� !"#$%&'()�� !�� !��
�� !� 1�� !"#$%& 50�100� 500 pg
�� !"#$%&'�TIC��� !"#$��
�� !"#$%&'()1 - µL�� !"#$%&
�� !"#$%&'()*+,-./01500 pg�
2
![Page 3: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/3.jpg)
5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00
20000
60000
100000
140000
180000
220000
240000
50 pg on column
100 pg on column
500 pg on column
SIM ��
�� !"#$%�� SIM�� �� ! SIM �
�� !"#$�� !"#$%&'()*��RTL
�� !"#$%&'()*+, SIM�� ��
�� SIM�� !"#$%&
1. �ChemStation�� MSD RTL �� !"��
2�� !"#$%�� !"#$%&'"()*
2. �� !"#$%&'()*+,-./0
� 1 . 80�� !"#$ 50�100 � 500 pg�1 L�� !"#$%& '�TIC�
� 2. �� !"#$%&'()*�� !"#$%&'�� !"#�� !"�� !"#�� !"#$%
3
![Page 4: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/4.jpg)
#243542515576829298
102103104111113117120122124129
Compound Name2,6-DichlorobenzonitrileMevinphosProphamo-PhenylphenolPentachlorobenzenePropoxurDiphenylamineChlorprophamEthalfluralinBendiocarbTrifluralinBenfluralinPhorateBHC alpha isomerHexachlorobenzeneDicloranDemeton-SDimethoateSimazine
Group #1
23
4
5
6
7
Group RT3.00
7.758.35
9.60
10.76
11.41
Q1173192179169252152168213316126264264121219286176
6093
186
T171127
93170250110169127276151306292
75181284206
8887
201
MSD_RT6.757.607.918.788.95
10.3510.5211.0511.2811.5411.6411.7311.9612.0912.3812.5612.6312.6812.91
3. �� !"#$%"&'()*�� ! 3��
�Group#���
� �� !"#$%&'
� �� !"��#$%&'()*+�,0.2 min�
�� �� 42�51�� !!"#$0.2 min,
�� !"#$%&'()�� 51�55��
�� 0.2 min��� !"#$%
4. �� !"#$ !%&'()*+,-./0
SIM�� !"#(�� 3�� �Group RT�
��)��� �� 42�7.91 min�� 2����
�� 51�8.78 min�� 3 ���� !"#$%
8.35 min��� !"#$%&'3�� !"#$
���� !"#$%&'!()*+,-./01
�� !"#$%&'()*+,�MS SIM/Scan
�� �� !
5. �� !"#$%&'()*+'(�Q1�Q2�/
�Q3��� !"#ChemStation SIM�� ��
4���� ! SIM�� !"#$%&'() 3�
SIM�� !"#$%&'()*+,-./0#(
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� 5�� !"#$%&'() SIM�� 50 pg/µL
�� !"#�1- µL�� !"#$�� !"#$
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�� ! SIM�� !�� �S/N��� 100��
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�� !"#$%&'�� !"�S/N��
� 3. �� !"#$%&'()&'!"#*+,-./&00.2 min�� !SIM�� !"#$�� !"#$%"#&'()*� RT�� !"#$%&'()
� 4. MSD ChemStation�� !"#$%�� MS � SIM�� SIM ���� ID��� !"#$%&�� 3��
4
![Page 5: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/5.jpg)
5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00
1000
3000
5000
7000
9000
11000
13000
15000
17000
19000
21000
SIM
Scan
SIM�� !"#$%�� !"#$%&'()*
���� ! RTL��� !"#$%&'()*+
�RT��� ![4]��� !"#$%&'�� !
�� !"#$%"&'()�RT���� !"#$
�� !"#$%&'(�� !"#$%&'()*
�� !"#$�� !"�#$%#&'()��
�� !"#$%&'()*+�� !"#$%&
�� !"#
�� !"#SIM�� !"#$%&'()*��
�� !"#�� �� !"#$%&'()*+,
�� !"#$�� !"#$%&'"()$*+
��
�� !"�LVI�
�� !"#$%&'(�� !"�#$%&'(
�� !"#$%&'(�� �� !"#$��
�� !"#$%&'()*+,�� !"#$%
PTV�� !"�� !"#$%&'()!*+,
�� !"#$%� 6�� 25 µL�� !"#$
1 µL�� !"#�� !"#$%&� 50 pg ��
�� !"#$�� !"#$�� !"#$%&'
�� !"#$�� !"#$%&'(')*+,�
�� �� !"#$%�� !"#$%&'()*
���� !"#$%&'()*+,-./012
��
� 5. 50 pg/ L �� 1 L�� !"#$%&'() SIM�� !"
5
�� : 1 L�� : 50 pf/ LPTV ��: ��
![Page 6: GC/MS ppt !#$%&' - Agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122 124 129 Compound Name 2,6-Dichlorobenzonitrile Mevinphos Propham o-Phenylphenol Pentachlorobenzene](https://reader033.vdocument.in/reader033/viewer/2022041518/5e2cb1988d42783ff52e0fab/html5/thumbnails/6.jpg)
Tune voltage
Tune voltage + 400 V
(Magnified 10X)
6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00
-25000
-30000
-35000
-20000
-15000
-10000
-5000
0
5000
10000
15000
20000
25000
30000
35000
40000
Injection volume: 25 µLConcentration: 0.5 pg/µL
6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00
-4000
-5000
-3000
-2000
-1000
0
1000
2000
3000
4000
5000
6000
7000
Injection volume: 1 µLConcentration: 50 pg/µLPTV mode: Splitless
Injection volume: 25 µLConcentration: 2 pg/µLPTV mode: Solvent vent
SIM
�� !"#$ %�EMV�
�� !"���MS��� !"#�$�EMV��
�� !"#$%&'�7���� !"#$%&'
��10�� !25 µL�0.5 pg/µL�� !"#�$
�� �� !"#"$�� !"#�$%&'�$
�� 400 V�� !"�� !"�#�EMV���
400 V ���� !"#$ 10 ���� !"#$%
���� !"#$%&'10���� !"�S/N�
��
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� 7. 12.5 pg�� !"�� EMV�� !"#$ 400 V � SIM�� !
� 6. 50 pg�� !"�� ! 1 L�� !"# 25 L�� !"#$SIM�� !
6
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SIM
Scan
26.30 26.40 26.50 26.60 26.70 26.80 26.90 27.00 27.10 27.20 27.30
6000
12000
18000
24000
30000
p,p’-DDT
Endosulfan sulfate
160
190
220
250
280 Injection volume: 25 µLConcentration: 0.2 pg/µL (5 pg on column)
Injection volume: 1 µLConcentration: 500 pg/µL (500 pg on column)
�� !"�LVI�� SIM�� !"#
�� !LVI�SIM��8��9�� !"#$%&
�� 5 pg�� !"#$%&'� 8�� !"#$
0.2 pg/µL� 500 pg/µL�� �!"# p,p�-DDT �
�� !"#$�� 25 µL�� !"#SIM��
�� 1 µL�� !"#$%&'(�� ! LVI�
SIM��� !"#�� !"#$%& 2500���
500 pg/µL� 0.2 pg/µL���� !"#$%&'(
�S/N��
�� !"#$%&'100 µL��� !"#0.05 pg/
µL�� !"#$%&'�� 9�� �� !"#
�� 100 µL�� !"#$%&'()m/z 299�
m/z 301�� !"#$%�EIC���� !"100 µL
��SIM�� !"#$%&'()%&*+,-SIM
�� !"#$%&'()*$+&,-./0
� 8. �� 0.2 pg/ L � 500 pg/ L�� �!"# p,p'-DDT�� !"#$%�� !"#$% 25 L�� !"#$ /SIM�� �� !"#$% 1 L�� !" /�� !"
7
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0
200
400
600
800
1000
1200
1400
*
*
*
**SIM group start time
Ion 299
Ion 301
Ion 299
Ion 301Scan
SIM
0
18.6 18.8 19.0 19.2 19.4 19.6 19.8 20.0 20.2 20.4
200
400
600
800
1000
1200
1400
0
200
400
600
800
1000
0
18.6 19.0 19.2 19.4 19.6 19.8 20.0 20.2
200
400
600
800
1000
Concentration: 0.05 pg/µL
Concentration: 0.05 pg/µL
�� !"#$
�� ! RTL� G1049A MSD RTL�� !"#�
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�� !"#$%&'()*+ [5]��� !"#�
SIM�� !"#$%&'()*+,MSD Chem-
Station�� !30�� !"#$%&567�� !
�� !"#�10��0.5 pg/µL���SIM�� �
� 25 µL��� !�� !"�� !"#�� x �
����� !"#�� !"#$�� !"12.5 pg
�� �� !"#$%&'()*+,-./
� 9 .�� 100 L � 0.05 pg/ L�� !"#$%&'()�� !"#$%&'()&'*�� !" SIM�� !
8
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��
�� RTL�� !"#$%&�� !"#$��
�� !"#$�2�� !"#$%&' 80��
�� ! SIM�� �� !"#$%&'()*�
�� ! LVI � SIM�� !"#$%&'()*+
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�� !500 pg�� 5 pg��� !"#$%LVI�
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��
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�� !
1. Vince Giarrocco, Bruce Quimby, andMatthew S. Klee, Retention Time Locking:Concepts and Applications, AgilentTechnologies Application note, 5966-2469E,printed March 2000, www.agilent.com/chem
2. Bill Wilson, Philip L. Wylie, andMatthew S. Klee, Large Volume Injectionfor Gas Chromatography Using a PTV Inlet,Agilent Technologies Application note,5965-7770E, printed February 2000,www.agilent.com/chem
� 10. GC/MS�� !"#$%&'()�� !�� !"#�� x�� ��� !"#����� !�� !"�� !"#$%&'()*�+!"#$,-./�� !"#$%&�� !"#$%&'()*+,*-�� !"#$
9
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3. Philip L. Wylie, Trace Level PesticideAnalysis by GC/MS Using Large-VolumeInjection, Agilent Technologies Applicationnote, 5966-1214E, printed April 2000,www.agilent.com/chem
4. Prest, H. and p. Cormia, Retention TimeLocking: Advantages in GC/MS SIM Analysis,Agilent Technologies Application note,5968-3797E, printed December 1999,www.agilent.com/chem
5. Harry Prest, Philip L. Wylie, ken Weiner, andDoug Agnew, Efficient Screening for Pesticidesand Endocrine Disrupters Using the 6890/5973GC/MSD System, Agilent Technologies Applica-tion note, 5968-4884E, printed December 1999,www.agilent.com/chem
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