gc/ms ppt !#$%&' - agilent · 24 35 42 51 55 76 82 92 98 102 103 104 111 113 117 120 122...

10
C. Kai Meng Agilent Technologies, Inc. 2850 Centerville Road Wilmington, DE 19808-1610 USA !"#$%&'()*+,-./ppm! !"#$%&/ !" !"#$ !"# !"#$%&'( ppb (pg/ L)!"# !"#$!"#$ ppt !"# !"567 !"#$%&'()*+,-. ! !"#$%&'()*+,-./012567 !" !"#$%&'()*+,-./01234%5 !"#$ 2 !"#$%&' 80 !" !"#$%&'(!"#$%&'() !"#$%&'()*+GC!"# ESD!"#$%&'()*+,- ppb !"#$%&'()!"#$% !"#$%& GC/MS ppt !"#$"%&' !"# !"#$%&'()*+,- !"#$%&'(MS!"#$ !"#$%&'()*+ !"GC/MS !"#$%&'()*"+,-! !"#$%&'()*+,-./01234 GC/ESD !"#$% / !"#$ !" MS !"# 2 3 !" !"#$%&' !MS!"#$%&'SIM !"LVI !"#$%&'#(EMV !"#$%&'( 567!"#$% RTL [1] !"#$%&'()*+ 567 !"#$%&'(!"#$ SIM !"#$ !"#$%&'()*+,$-./0,$1 Scan !"#$%& SIM ! !"#

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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

��

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

�� !"#$%&'

� 6890 GC��� !"#$%�PTV�[2,3]��

� 5973�� !"#$�MSD�

� 7683�� !"#$�ALS��� !"#$%

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�� 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

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RTL[1]�� !

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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

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 �

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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

#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��

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SIM�� !"#(�� 3�� �Group RT�

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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

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

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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

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�

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6

Page 7: 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

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�� !"#

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µL�� !"#$%&'�� 9�� �� !"#

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m/z 301�� !"#$%�EIC���� !"100 µL

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7

Page 8: 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

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

�� !"#$

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8

Page 9: 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

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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

Page 10: 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

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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