Fast GC-MS Analysis of Semi-Volatile Organic

Compounds: Migrating from Helium to Hydrogen
as a Carrier Gas in US EPA Method 8270
Jessie Butler, Alexander N. Semyonov, and Pat O’Brien
Thermo Fisher Scientific, Austin, TX, USA

Overview

Results

Purpose: Optimize US EPA Method 8270 with hydrogen carrier gas
Methods: Configure hydrogen carrier with smaller id column and installation of
hydrogen kit on mass spectrometer
Results: Improved peak shape, resolution, and run time

Introduction

The global helium shortage and price increase of this non-renewable noble gas cause
more and more laboratories to migrate to hydrogen as a carrier gas. This transition is
easy for the gas chromatography (GC) methods utilizing FID, TCD, ECD, and other
non-mass-selective detectors. However, for the gas chromatography- mass
spectrometry (GC-MS) methods, especially complex and regulated ones, migration to
hydrogen carrier gas presents significant challenges. In addition to the changes in
chromatographic conditions of the run due to the physical property differences of
hydrogen, its chemical reactivity brings about chemical reactions in the mass
spectrometer’s ion source that do not occur with helium.
The analysis of semi-volatile organic compounds (SVOCs) in wastewater by United
States Environmental Protection Agency (EPA) Method 82701 involves identification
and quantitation of more than 120 analytes of varying chemical structure, polarity and
volatility. The diversity of the analytes in this method presents particular challenges
when migrating from helium to hydrogen carrier.
GC-MS analysis of SVOCs was performed in accordance with EPA Method 8270 on
the Thermo Scientific™ TRACE™ 1310 GC coupled to a Thermo Scientific™ ISQ™
single quadrupole mass spectrometer using helium or hydrogen as carrier gases. Key
modifications to both GC and MS hardware and methods are necessary for
successfully switching to hydrogen. The final, optimized EPA Method 8270 was fully
migrated to hydrogen carrier gas with improved peak shape, resolution, and run time.

Methods

Stabilization Bake Out fo

When switching from heliu
required. If using a hydrog
be plumbed with pre-clean
used, grade UHP 5.0 or be
installed in the mass spect
out. The hydrogen carrier
during the bake out period
and the source temperatur
The hydrogen gas strips th
the gas lines, a m/z of 19 i
typical of chemical ionizati
2). Elevated levels of low m
spectrum (Figure 4). Thes

FIGURE 2. Air/water spectru
out
m/z 18
m/z 19

m/z
m/z 28

FIGURE 4. Cal gas (FC-43) s
before bake out

Sample Preparation
All standards were prepared in methylene chloride. A performance mix containing
pentachlorophenol, DFTPP, benzidine, and p,p’-DDT was made at a concentration of
50 ppm. A calibration curve was prepared from 1 to 200 ppm with internal standards
and surrogates at 40 ppm.
Gas Chromatography
An instant connect split/splitless injector module was used in the split mode. The
standard Thermo Scientific™ TraceGOLD™ TG-5MS capillary column (30 m x 0.25
mm x 0.5 µm) was replaced with a TraceGOLD TG-5MS column of smaller i.d. (20 m x
0.18 mm x 0.36 µm). A one microliter injection was made.
Mass Spectrometry

Due to the lower viscosity
head pressure is required
of the column, the pressure
reduction in the vapor volu

The ISQ mass spectrometer was equipped with the new hydrogen kit and
preconditioned by baking out with an elevated hydrogen carrier flow rate.
Data Analysis
Data was collected using Thermo Scientific™ Xcalibur™ 2.0 acquisition software, and
processing was performed using Thermo Scientific™ Target 4.14 software. Xcalibur
software was configured for direct target processing. A typical chromatogram of a 40
ppm standard is shown in Figure 1.
RT: 0.00 - 13.27

FIGURE 6. Comparison of
0.18 mm i.d. column

NL:
5.35E8
TIC MS
level8

6.83

100

Selecting the Appropriate

95
90
85

3.85

80

10.24

75

RT: 0.000 - 13.008
100

4.56
6.26

5.18

60
55

5.65 6.08

6.45

6.97

5.34

50
3.88

45

8.41
11.16

4.61

3.34

40

4.67
5.02

9.45

7.37
5.95

10.79

50
40
30

1.368

2

0
100

12.55

13 ps

90

30

80

25

9.97

3.31

70
60

20

50
40

15

2.25
1.80

10

2.98

30
20

2.51

10

5
0

60

10

11.72

8.84

70

20

11.44

9.76

7.01

4.26

35

80

11.19

8.06

8 ps

90

12.35

10.27

7.64

Relative Abundance

65
Relative Abundance

8.98 9.19

7.90

70

8.48
0

1

2

3

4

5

6

Time (min)

7

8

10.54
9

10

12.17
11

12

0

12.70
13

FIGURE 1. TIC of 40 ppm standard with hydrogen carrier gas

2 Fast GC-MS Analysis of Semi-Volatile Organic Compounds: Migrating from Helium to Hydrogen as a Carrier Gas in US EPA Method 8270

1.079 1.526
0

1

2

FIGURE 7. Methylene chl

Results

and installation of

newable noble gas cause
ier gas. This transition is
, TCD, ECD, and other
tography- mass
ulated ones, migration to
ition to the changes in
operty differences of
ions in the mass

Peak Shape and Resolution

Stabilization Bake Out for Hydrogen Carrier Gas
When switching from helium to hydrogen as a carrier gas, a brief stabilization period is
required. If using a hydrogen generator, no gas filters are necessary. Gas lines should
be plumbed with pre-cleaned 1/8” stainless steel tubing. If a cylinder of hydrogen is
used, grade UHP 5.0 or better is required with inline gas purifiers. The hydrogen kit is
installed in the mass spectrometer. The source temperature is set to 350 °C for bake
out. The hydrogen carrier is set to 4 mL/min. The filament is turned on for one hour
during the bake out period. After bake out, the hydrogen flow is reduced to 1 mL/min,
and the source temperature was set to 325 °C. Figures 2–5 show the effect of bake out.
The hydrogen gas strips the contamination off the entire flow path. If water is present in
the gas lines, a m/z of 19 is seen. This is due to protonation of water (M+1). Other ions
typical of chemical ionization and protonation are also seen, m/z 29 and m/z 41 (Figure
2). Elevated levels of low mass hydrocarbons are observed in the calibration gas
spectrum (Figure 4). These all are reduced after the one hour bake out.

The advantage of hydrogen carrier is that hig
without sacrificing resolution. With less reside
polynuclear aromatic hydrocarbons (PNAs) c
The critical separation of benzo[g&h]flouranth
RT: 11.87 - 13.34

12.29

100

H

12.50

90
80
70

Relative Abundance

rier gas

60
50
40
30
20
10
0
100

11.88

11.97 12.02

12.11 12.14

12.34

12.26

12.53 12.56 12.63
12.65

12.37

12.72 12.76 12.81

1

90

Helium

80
70
60
50
40
30
20
10
0

11.90 11.94

12.03 12.05 12.09 12.16 12.21 12.25 12.27

11.9

12.0

12.1

12.2

12.72

12.37 12.42 12.46 12.52 12.54

12.3

12.4

12.5

12.6
Time (min)

12.7

12.75 12.84
12.8

FIGURE 8. Improvement of Peak Shape
benzo[g,h,i]perylene (peak 2)
RT: 10.26 - 10.43
100

NL:
1.19E7
m/z=
251.50252.50
MS level5

10.36

10.33

95
90
85

FIGURE 2. Air/water spectrum before bake
out

FIGURE 3. Air/water spectrum after
bake out

60
55
50
45
40
35
30
25
20
15
10
5
0

m/z 18

10.42

10.26
10.26

10.27

10.28

10.29

10.30

10.31

10.32

10.33

10.34
10.35
Time (min)

10.36

10.37

10.38

10.39

10.40

10.41

10.42

Helium

m/z 18

FIGURE 9. Critical Separation of benzo[

m/z 28

m/z 19

th EPA Method 8270 on
ermo Scientific™ ISQ™
gen as carrier gases. Key
e necessary for
A Method 8270 was fully
resolution, and run time.

70
65
Relative Abundance

n wastewater by United
01 involves identification
cal structure, polarity and
ts particular challenges

80
75

Linearity

m/z 29

m/z 19

m/z 28

FIGURE 4. Cal gas (FC-43) spectrum
before bake out

m/z 29

A linearity study was performed in the range o
CH2Cl2. The results are shown in Figures 10
relative percent standard deviations (%RSD)
the method. A few compounds required the fi

FIGURE 5. Cal gas (FC-43) spectrum
after bake out

mance mix containing
ade at a concentration of
m with internal standards

the split mode. The
ry column (30 m x 0.25
umn of smaller i.d. (20 m x

FIGURE 10. Comparison of linearity wi
compounds on the insert required R2 f
Selecting the Appropriate Column Dimensions and Inlet Pressure
Due to the lower viscosity of hydrogen carrier gas as compared to helium, a lower
head pressure is required to obtain 1 mL/min of column flow rate. By reducing the i.d.
of the column, the pressure may be set to usable level (Figure 6). Also note the
reduction in the vapor volume of methylene chloride at higher pressures (Figure 7).

rogen kit and
ier flow rate.

acquisition software, and
4.14 software. Xcalibur
al chromatogram of a 40

FIGURE 6. Comparison of inlet pressure for helium and hydrogen for a 0.25 mm and
0.18 mm i.d. column

NL:
5.35E8
TIC MS
level8

10.24
RT: 0.000 - 13.008

7.031

100

80
Relative Abundance

11.19

11.16

NL:
2.12E8
TIC MS
level1

8.596

5.795

4.039

9.808

70
60
50

3.016

40
30

1.368

20

11.44

6

8 psi

90

12.35

10.27

10

11.72
10.79

2.002

0
100

12.55

6.358

4.698 5.057

7.075 7.874

8.953 9.423

10.099

11.114 11.520

12.801
NL:
1.55E8
TIC MS
1ng

8.309

80

9.97

3.281

13 psi

90

6.802

9.338

70

5.430

3.730

60
50
2.719

40
30
20
10

10.54
10

12.17
11

ier gas

12

0

12.70
13

1.079 1.526
0

1

2.681
2

3.000
3

4.367 4.721
4

5

6.035
6

6.849 7.633

Time (min)

7

9.036
8

9

10.411 10.742 11.648 12.000

9.577
10

11

12

13

FIGURE 7. Methylene chloride solvent tailing at low vs. high inlet pressures

FIGURE 11. Typical linearity plots with

Thermo Scientific Poster Note • PN10323_e 05/13S 3

as a carrier gas, a brief stabilization period is
o gas filters are necessary. Gas lines should
s steel tubing. If a cylinder of hydrogen is
with inline gas purifiers. The hydrogen kit is
ource temperature is set to 350 °C for bake
min. The filament is turned on for one hour
, the hydrogen flow is reduced to 1 mL/min,
5 °C. Figures 2–5 show the effect of bake out.
n off the entire flow path. If water is present in
due to protonation of water (M+1). Other ions
ion are also seen, m/z 29 and m/z 41 (Figure
ons are observed in the calibration gas
ed after the one hour bake out.

Sensitivity

The advantage of hydrogen carrier is that higher than helium linear velocities can be used
without sacrificing resolution. With less residence time in the stationary phase, the late eluting
polynuclear aromatic hydrocarbons (PNAs) come out with a narrower peak width (Figure 8).
The critical separation of benzo[g&h]flouranthene was easily achieved (Figure 9).

The sensitivity of the m
achieved with helium.
0.082 ppm and 0.15 pp
IDLs at around 0.1 ppm

RT: 11.87 - 13.34

12.29

100

80
70
60
50
40
30
20
10
0
100

11.88

11.97 12.02

12.11 12.14

12.34

12.26

12.53 12.56 12.63
12.65

12.37

12.72 12.76 12.81

12.87

12.93

13.01

13.06 13.12

13.17

13.26

NL:
7.26E6
m/z=
275.50276.50
MS level5

90
13.23

Helium

80
70
60
50
40
30
20
10
0

11.90 11.94

12.03 12.05 12.09 12.16 12.21 12.25 12.27

11.9

12.0

12.1

12.2

12.72

12.37 12.42 12.46 12.52 12.54

12.3

12.4

12.5

12.6
Time (min)

12.7

12.75 12.84 12.87 12.94 12.98 13.03
12.8

12.9

13.13

13.0

13.1

13.2

13.3

FIGURE 8. Improvement of Peak Shape for Indeno[1,2,3-cd]pyrene (peak1) &
benzo[g,h,i]perylene (peak 2)
RT: 10.26 - 10.43
100

NL:
1.19E7
m/z=
251.50252.50
MS level5

10.36

10.33

95
90

RT: 11.06 - 11.20

95
90

80

75

75

70

70
65

60
Relative Abundance

Relative Abundance

65

55
50
45
40
35

60
55

FIGURE 12. Instrume

50
45
40
35

30

30

25

25

20

20

15

15

10

10

5

5

0

11.11

85

80

FIGURE 3. Air/water spectrum after
bake out

NL:
6.19E6
m/z=
251.50252.50
MS level5

11.14

100

85

10.42

10.26
10.26

10.27

10.28

10.29

10.30

10.31

10.32

10.33

10.34
10.35
Time (min)

10.36

Helium

10.37

10.38

10.39

10.40

10.41

10.42

0
11.06

11.07
11.07

11.16

11.08
11.08

11.09

11.10

11.11

11.12

11.13
Time (min)

11.14

11.15

11.16

11.17
11.17

11.19
11.18

11.20

11.19

Hydrogen

Robustness and Ion Ra

FIGURE 9. Critical Separation of benzo[g&h]flouranthene

The stability of ion ratios
performance is shown in
of 5 % diesel samples in
the internal standards. T
plotted of the internal sta
of 10 diesel samples. Al

m/z 18
m/z 28

NL:
5.23E6
m/z=
275.50276.50
MS level5

Hydrogen

12.50

90

Relative Abundance

arrier Gas

Peak Shape and Resolution

Linearity
m/z 19

m/z 29

FIGURE 5. Cal gas (FC-43) spectrum
after bake out

A linearity study was performed in the range of concentration from 1 to 200 ppm in
CH2Cl2. The results are shown in Figures 10 and 11 below. Helium carrier gave lower
relative percent standard deviations (%RSD) than hydrogen but still met the criteria for
the method. A few compounds required the fit of least squares (R2 = > 0.99).
Compounds: R2 = >0.99
nitrophenols
nitroanilines
dinitrophenols
4,6-dinityrophenol-2-methylphenol
trichlorophenols
dinitrotoluenes
hexachlorocyclopentadiene
tribromophenol
pentachlorophenol
butylbenzylphthalate
di-n-octylphthalate
bis(2 ethylhexyl)phthalate

FIGURE 10. Comparison of linearity with helium and hydrogen carrier (the
compounds on the insert required R2 fit with hydrogen)

ensions and Inlet Pressure

FIGURE 13. Ion Ratio

rier gas as compared to helium, a lower
min of column flow rate. By reducing the i.d.
usable level (Figure 6). Also note the
e chloride at higher pressures (Figure 7).

RT: 0.00 - 13.26
100
95
90
85
80

for helium and hydrogen for a 0.25 mm and

75
70

Relative Abundance

65
60
55
50
45
40
35
30
25
20
15
10
5
0

1.70
0

1

1.96 2

2

FIGURE 14. TIC 5 % d
NL:
2.12E8
TIC MS
level1

8.596

9.808

8.953 9.423

10.099

11.114 11.520

12.801
NL:
1.55E8
TIC MS
1ng

8.309

9.338

9.036
9

10.411 10.742 11.648 12.000

9.577
10

11

12

13

ailing at low vs. high inlet pressures

FIGURE 11. Typical linearity plots with hydrogen carrier

4 Fast GC-MS Analysis of Semi-Volatile Organic Compounds: Migrating from Helium to Hydrogen as a Carrier Gas in US EPA Method 8270

FIGURE 15. Stability o

an helium linear velocities can be used
me in the stationary phase, the late eluting
out with a narrower peak width (Figure 8).
was easily achieved (Figure 9).

Sensitivity

Run Time

The sensitivity of the method using hydrogen carrier was within a factor of two to that
achieved with helium. The average Instrument Detection Limit (IDL) with helium was
0.082 ppm and 0.15 ppm with hydrogen. The chart in Figure 12 shows most of the
IDLs at around 0.1 ppm. Replicate injections of the standard were made at 1 ppm.

The run time was reduced by
0.36 µm) and hydrogen carrie
the TG-5MS 30 m x 0.25 mm
C:\chem\...\level8.d\level8

1

RT: 0.00 - 20.01

NL:
5.23E6
m/z=
275.50276.50
MS level5

100
90

3.85

80

13.17

13.26

NL:
7.26E6
m/z=
275.50276.50
MS level5

13.23

Butylbenzyl phthalate
Dichlorobenzidine
Di-n-octylphthlate

Bis-2-chloroisopropylether

Relative Abundance

12

5.18

60

5

50

3.34

40
30

3.88
4.26

4.61

3.31

20
1.80

10

2.25
2.98
2.51

0
100

13.13
13.2

4.56

70

13.3

deno[1,2,3-cd]pyrene (peak1) &

90
80
70
60

5.34

40

11.11

30

11.16

11.08
11.08

11.09

11.10

11.11

11.12

11.13
Time (min)

11.14

11.15

11.16

11.17
11.17

11.19
11.18

2.65
0

1

2

3.24
3

4.17
4

5

11.20

11.19

Hydrogen

louranthene

centration from 1 to 200 ppm in
1 below. Helium carrier gave lower
ydrogen but still met the criteria for
ast squares (R2 = > 0.99).

Robustness and Ion Ratio Stability
The stability of ion ratios for DFTPP was studied. The values were very stable. The
performance is shown in Figure 13. Next, a robustness study was run by injecting 30
of 5 % diesel samples in methylene chloride. The samples also contained 40 ppm of
the internal standards. The diesel sample TIC is shown in Figure 14. A chart was
plotted of the internal standards in Figure 15. A check standard was run after each set
of 10 diesel samples. All check standards met the QC criteria for the method.

FIGURE 16. Comparison

Conclusion

Compounds: R2 = >0.99
nitrophenols
nitroanilines
dinitrophenols
4,6-dinityrophenol-2-methylphenol
trichlorophenols
dinitrotoluenes
hexachlorocyclopentadiene
tribromophenol
pentachlorophenol
butylbenzylphthalate
di-n-octylphthalate
bis(2 ethylhexyl)phthalate

GC-MS analysis of SVOC
a TRACE 1310 GC couple
hydrogen as a carrier gas.
methods necessary for su
final, optimized EPA Metho
improved peak shape, res
maintained good ion ratio

ium and hydrogen carrier (the
h hydrogen)

gen carrier

2.82

10
0

11.07

3.84

20

FIGURE 12. Instrument Detection Limits (ppm) Average = 0.15 ppm

11.07

5.36

50

NL:
6.19E6
m/z=
251.50252.50
MS level5

11.14

FIGURE 13. Ion Ratios for DFTPP
RT: 0.00 - 13.26

NL:
6.22E8
TIC MS
diesel5

7.76

100

6.21

95

6.77

8.18
7.30

90

4.55

85

5.65

3.43

8.57

4.01

75
70

8.92

Relative Abundance

60
7.79

50
45
5.50
5.29

40
35

9.25

7.01

5.97

 

Sensitivity was withi

 

Ion ratio stability and

 

Run time was shorte

6.55
9.56

4.92

30

7.47

25

3.75

20

2.80

9.85

4.35

3.21

15

10.13

10

2.63

5
0

Linearity met the cri

1.  EPA Method 8270D
Mass Spectrometry

65

55

Resolution was goo

 

References

7.31

5.09

80

 

1.70
0

1

1.96 2.15
2

3.19

10.24

2.57

10.68
3

4

5

6

Time (min)

7

8

9

10

11.47
10.95
11

11.62 12.01 12.80 13.23
12

13

FIGURE 14. TIC 5 % diesel sample

FIGURE 15. Stability of internal standard areas during injection of 5% diesel

© 2013 Thermo Fisher Scientific Inc.
Scientific Inc and its subsidiaries. This
manner that might infringe the intellec

Thermo Scientific Poster Note • PN10323_e 05/13S 5

Run Time

rrier was within a factor of two to that
Detection Limit (IDL) with helium was
hart in Figure 12 shows most of the
the standard were made at 1 ppm.

The run time was reduced by using a smaller i.d. column (TG-5MS 20 m x 0.18 mm x
0.36 µm) and hydrogen carrier gas. The more commonly used column with helium is
the TG-5MS 30 m x 0.25 mm x 0.5 µm (Figure 16).
C:\chem\...\level8.d\level8

12/5/2012 2:04:03 PM

RT: 0.00 - 20.01

NL:
Hydrogen 1 mL/min
5.35E8
MS
(TG-5MS 20 m x 0.18 mm x 0.36µm) TIC
level8

6.83

100
90

3.85

80
Relative Abundance

Butylbenzyl phthalate
Dichlorobenzidine
Di-n-octylphthlate

7.90 8.98

4.56

70

6.26

5.18

60

6.97

5.65

50

3.34

40
30

3.88
4.26

4.61

10.24

9.19

10.27

7.64
8.06
8.41
9.76

7.01

12.35
11.19

11.16

11.44

10.79

8.84

12.55

3.31

20

2.25
2.98
1.80
2.51

10

12.70

0
100
6.63

90

8.06

6.14

80

8.80

7.58
7.46

9.44
10.65 10.71

8.59
9.01

9.56

10.89

12.13

12.43

13.21 13.84

13.15
11.27

15.37

9.61

70
60

5.34

50

18.08

7.22

5.36
6.04

NL:
1.12E8
TIC MS
03091102_
110309112
925

14.62

13.96

12.57

10.02

15.33

15.85

6.76
18.71

40
30
20

m) Average = 0.15 ppm

15.92

2.82

10
0

The values were very stable. The
stness study was run by injecting 30
e samples also contained 40 ppm of
shown in Figure 14. A chart was
heck standard was run after each set
e QC criteria for the method.

3.84

2.65
0

1

2

3.24
3

11.32

4.17
4

5

6

7

8

9

10
Time (min)

11

12

18.91

16.42 17.11
13

14

15

16

17

18

19

20

Helium 1 mL/min
(TG-5MS 30 m x 0.25 mm x 0.5µm)

FIGURE 16. Comparison of run time with hydrogen and helium at 1 mL/min

Conclusion
GC-MS analysis of SVOCs was performed in accordance with US EPA Method 8270 on
a TRACE 1310 GC coupled with an ISQ single quadrupole mass spectrometer utilizing
hydrogen as a carrier gas. Key modifications to both GC and MS hardware and
methods necessary for successful migration to hydrogen carrier were performed. The
final, optimized EPA Method 8270 fully was migrated to hydrogen carrier gas with
improved peak shape, resolution, and run time. The ISQ GC-MS was stable and
maintained good ion ratio stability after injecting 5% diesel samples.

NL:
6.22E8
TIC MS
diesel5

8

 

Resolution was good and peak shape was improved

 

Linearity met the criteria of the method

 

Sensitivity was within a factor of 2 of that obtained with helium carrier gas

 

Ion ratio stability and robustness were good

 

Run time was shortened

References

8.57

8.92

1.  EPA Method 8270D, Semi-volatile Organic Compounds by Gas Chromatography/
Mass Spectrometry (GC/MS) Rev. 4, 2007, Environmental Protection Agency.

9.25

9.56

9.85

10.13
10.24
10.68
9

10

11.47
10.95
11

11.62 12.01 12.80 13.23
12

13

as during injection of 5% diesel

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6 Fast GC-MS Analysis of Semi-Volatile Organic Compounds: Migrating from Helium to Hydrogen as a Carrier Gas in US EPA Method 8270

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