MCU14/0056 Response to SARA - Consulting Report

EN 858-1:2002 (E)

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A.3 Gas chromatography method

A.3.1 General

This instruction describes a simplified analytical method based on EN |SO 9377-2 to determine fuel oil {SO-F-DMA
in accordance with 8.3.3.1.2 in water by gas chromatography (GC). The method is suitable for determining fuel oil,
if the conceniration-is greater than 1 mg/1. This methad is not suitable for wastewater.

The samples are extracted in petroleum ether, then analysed by gas chromatography between C49 and Cyp.

A.3.2 Reagents

c) extraction solvent: petroleum ether, boiling range 40 °C to 60 °C;

d) sodium sulphate (Na,SO,), anhydrous;

e) fuel oil ISO-F-DMA in accordance with 8.3.3.1.2 to prepare standards; -

f) reference standards n-decane (CioHz2) and n-tetracontane (C4oHe2).

A.3.3 Interferences

If fuel oil [SO-F-DMA in accordance with 8.3.3.1.2 without additives is used, interferences are not be expected.

A.3.4 Procedure

The petroleum ether shall be spiked with n-decane and n-tetracontane prior to analysis to give a concentration of
approximately 2 mg/l to 10 mg/l. All solutions analysed with the gas chromatograph shall contain these two
chemicals.

The sample may be taken in a sample bottle or separating funnel. Weigh the sampling vessel. Put approximately
500 ml of water directly into the sample vessel then re-weigh to obtain the mass of sample. If the samples shall be’
transported to an external laboratory, they shall be taken in glass bottles and acidified to pH 2 then transported
at 4°C. Add the appropriate volume of petroleum either to the extraction vessel and shake for at least 10 min. To
analyse over the range 1 mg/l to 40 mgf{ oil in water use 10 m! of petroleum ether. For the analysis range 10 mg/l to
150 mg/l use 25 mi of petroleum ether. If extracted in a separating funnel, run off the aqueous phase then collect
the organic phase. If a glass bottle is used, then a separator device may be used to recover the organic phase. The
collected extract is dried using sodium sulphate.

NOTE Failure to dry the extract sufficiently may irreparably damage the GC column.

A.3.5 Gas chromatographic analysis

The gas chromatograph shall be equipped with a non-discriminating injection system and a flame ionisation
detector (FID). The GC column shall be fused silica with one of the following stationary phases:

Non-polar, immobilised 100 % dimethylpolysiloxane (CHa[(CH3)2SiO],Si(CHs)3), or 95 % dimethyl-/5 %
diphenylpolysiloxane (CH3[(CHgHs)2SiO]n Si(CHs3)3) or modified siloxane polymer (H3Si(OsiH2),OSiHg).

Typical dimensions:

— Length . 5m to 30m
— Internal diameter: 5 mm to 0,53 mm
— Film thickness: 25 ym to 1,2 um

This is a licensed reproduction produced by SAI Global Ltd, an authorized distributor of British Standards 37