Analysis of 18 Polycyclic Aromatic Hydrocarbons using a Varian 920-LC Analytical

HPLC and Pursuit® 3 PAH Column

By Phuong TruongVarian Australia Pty Ltd

679 Springvale Rd Mulgrave VIC Australia

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Introduction

• PAH’s are carcinogenic contaminants produced as a by-product of combustion

– Found in drinking water, soils and sludges

• Can be analysed by GC, GC-MS• Compared to GC, HPLC offers

• Easier sample preparation

• Improved sensitivity with FLD

• Better selectivity

• PAH’s are difficult to analyse because of their structural similarity

• Results in long gradient runs of 25 to 30 minutes

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Instrumentation

• Varian 920-LC Analytical HPLC (part no 00100xxx00)• Quaternary gradient pump with 4 channel degasser

• 200 position autosampler with 100 L syringe

• Thermostated column compartment

• Diode Array detector

• Optional Fluorescence detector (part no 99100xxx00)• Varian Pursuit® 3 PAH 100 x 4.6 mm column with

3m packing material (part no A7001100X046)

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Instrument Conditions - Gradient Conditions

Time (min) Flow rate

(ml/min)

% Water % Acetonitrile

0.0 1.3 40 60

3.0 1.3 40 60

7.0 1.3 10 90

13.3 1.3 0 100

16.0 1.3 0 100

16.1 1.3 40 60

21.0 1.3 40 60

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Instrument Conditions - Fluorescence Detector Conditions

Time (min) Excitation

(nm)

Emission

(nm)

0.0 270 323

5.6 250 375

7.1 270 410

8.5 265 380

10.5 280 420

14.7 293 498

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Results

Component UV LOD

(g/L)

Fluoro LOD

(g/L)

USEPA LOD

(g/L)

Naphthalene 2 0.04

Acenaphthylene 5

1-Methylnaphthalene

5 0.05

2-Methylnaphthalene

5 0.06

Acenaphthene 8 0.03

Fluorene 2 0.003

Phenanthrene 0.5 0.04

Anthracene 0.5 0.06

Fluoranthene 1 0.14

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Results

Component UV LOD

(g/L)

Fluoro LOD

(g/L)

USEPA LOD

(g/L)

Pyrene 1 0.02

Benzo(a)anthracene 1 0.01

Chrysene 0.5 0.04

Benzo(b)fluoranthene 1 0.01

Benzo(k)fluoranthene 1 0.01

Benzo(a)pyrene 1 0.01

dibenzo(ah)anthracene

2 0.01

Benzo(ghi)perylene 2 0.01

Indenol(123-cd)pyrene 0.5 0.02

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18 PAH by Varian 920-LC & Pursuit 3 PAH

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16 PAH by Dionex HPLC

• Gradient separation at 1.5 ml/min with Fl Detection

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17 PAH by Grace Prevail C18 column

• Flow rate 1.5 ml/min

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Conclusion

• The Varian 920-LC and Pursuit 3 PAH column are capable of separating all 18 PAH’s in 15 minutes

• The reproducible gradient delivery and thermostated column compartment ensure excellent retention time reproducibility

• With the optional built-in fluorescence detector, detection limits exceed the requirements of USEPA method 8310

• Offers 30% improvements in throughput compared to alternative HPLC separations (Grace Vydac 201 TP 5 column)