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490 

M

astovska

et al

.

:

J

ournal of

AOAC I

nternational

V

ol

. 98, N

o

. 2, 2015

separation for benzo[

b

]fluoranthene, benzo[

j

]fluoranthene,

and benzo[

k

]fluoranthene (concentration ratio of 1:1:1).

Note

:

Criteria for separation of chrysene and triphenylene (another

PAH critical pair) were not set for the collaborative study. For

accurate quantitation of chrysene, at least 50% valley separation

is recommended, which can be achieved using selective

stationary phases.

The maximum oven temperature program may not

exceed the maximum temperature limit for a given column.

Backbone-modified columns, such as Rxi-17Sil MS or

DB-17MS, are recommended for their better temperature

stability and also good selectivity for critical PAH pairs

or groups, including the anthracene/phenanthrene pair

or benzofluoranthenes. Conduct proper inlet and column

Table 2014.08G. (

continued

)

Laboratory No.

6

7

8

9

10

He flow/pressure program

1.5 mL/min (13 min),

10 mL/min

2

to 2 mL/min

1.5 mL/min (constant flow)

1 mL/min (constant flow)

1.3 mL/min (19.5 min),

50 mL/min

2

to 2 mL/min

2 mL/min (constant flow)

Injection mode

Hot splitless

Hot splitless

Pulsed splitless

Splitless

PTV solvent vent

Injection volume, µL

1

1

1

10

5

Inlet temperature (program)

300

°

C

280°C

320°C

60°C (2.25 min), 300°C/min

to 335°C (45 min)

50°C (0.5 min), 600°C/min 400°C

(15 min), 30°C/min 70°C

Liner

SGE, Focus liner

Agilent, single taper, glass

wool-packed, 4 mm id

Agilent, double taper, 4 mm id

Apex, ProSep taper liner,

2 mm id

Agilent, PTV multi-baffle,

2 mm id

PTV solvent vent time

NA

NA

NA

NA

0.5 min

PTV solvent vent flow

NA

NA

NA

NA

100 mL/min

PTV solvent vent pressure

NA

NA

NA

NA

50 kPa

Pressure pulse and duration

NA

NA

50 psi for 0.2 min

NA

NA

Split vent purge flow and start

50 mL/min, 1 min

50 mL/min, 1 min

50 mL/min, 1 min

50.0 mL/min, 2.30 min

100 mL/min, 3 min

Gas saver flow and start time

20 mL/min, 3 min

20 mL/min, 2 min

15 mL/min, 6 min

NA

15 mL/min, 6 min

MS transfer line temperature, °C

300

280

320

300

325

Figure 2014.08C. GC separation criteria: (

1

) A baseline separation of ben

benzo[

e

]pyrene (concentration ratio of 1:5), (

2

) at least 50% valley separ

phenanthrene and anthracene (concentration ratio 2.5:1; evaluated for

which is the second peak in the figure), and (

3

) at least 50% valley separ

benzo[

b

]fluoranthene, benzo[

j

]fluoranthene, and benzo[

k

]fluoranthene

of 1:1:1).

(3)

(2)

(1)

Figure 2014.08C. GC separation criteria: (1) A baseline separation

of benzo[

a

]pyrene and benzo[

e

]py ene (concentr tio ratio of 1:5),

(2) at least 50% valley s parati of phenanthrene and anthracene

(concentration ratio 2.5:1; evaluated for the anthracene peak,

which is the second peak in the figure), and (3) at least 50% valley

separation for benzo[

b

]fluoranthene, benzo[

j

]fluoranthene, and

benzo[

k

]fluoranthene (concentration r tio of 1:1:1).