Envantage da vinci_lgi_gcc2011

Improving the analytical precision forthe analysis of contaminants in liquefied gases GCC 2011 Jay Grills – Envantage Lenny Kouwenhoven - Da Vinci Europe

phthalate esters Contaminants in liquefied gases • Oily residues in LPG • P-Tertiary-Butylcatechol in Butadiene • Elemental Sulfur in LPG • DIPA in LPG

Current methodsEN 589:2008 • EN 13757: Liquefied Petroleum gases -Determination of oily residues -High-temperature method • EN 15470: Liquefied petroleum gases - Determination of dissolved residues - High temperature Gas chromatographic method • EN 15471: Liquefied petroleum gases - Determination of dissolved residues - High-temperature gravimetric methodASTM D1835 • D2158:Standard Test Method for Residues in Liquefied Petroleum (LP) GasesASTM D1157: Total inhibitor content (TBC) of Light Hydrocarbons

LSV or GSV?• No deposit of high boilers before the column• Flash of the sample in the column• Injection under pressure in liquid phase

GC Injector based on GDI“Gasoline direct injector”

Gasoline Direct Injectordevelopment of Shell Global Solutions

Alternative based on GC a new type of GC injector1 2 3A Gasoline directinjector….. Injects liquefied gases directly on-column! Mounted on a slide and connected to a needle….

Pressure stationSamplecylinder the sample manager Sample in Sample out GDI Cool on column P rotameter GC vaporizer Waste

 COC inlet Application overview Retention Gap Solvent vent valve Retaining Pre- Column Solvent vent Cool on-column inlet Detector Column splitter Analytical Column FID Retention gap Retaining precolumn Analytical column

Problems of Oily Residue for the Automotive Industry Blisters containing oily residues Abrasion and disgregation of the material

Oily Residue analysisASTM D7756 in LPG • C10-C40; 174°C-522°C; °F-°F • 10-600 mg/kg • GC Configuration: COC – solvent vent – boiling point column FID • Injection volume: 25 ms ( 30µl)

N-Alkane standard C10 C20 C30 C40

Repeatability

Precision D2158

Precision D7756Residue GC method

Precision D 7756Residue GC methodConcentration Repeatability Relative(mg/kg) Standard deviation 10.3 1.2 4.0 % 51.3 5.3 3.8 % 103 8.3 2.9 % 302 14.5 2.4 % 602 14.4 3.1 %

P-TBC in Butadiene• Oxidation inhibitor• Butadiene is extremely flammable and a suspected human carcinogen• ASTM D1157: evaporation of 100ml measuring the absorbance using a photoelectric photometer after adding FeCL3

Overlay of6 chromatograms

Linearity of p-TBC by GC

Precision ASTM D1157

Precision p-TBC by GC pTBC Relative standard concentration in deviation mg/kg 36 2.4% 120 3.3% 241 3.0% 361 1.6% 482 3.3% 602 4.0%

diisopropanolamine (DIPA)Desulfurization

0,9 ppm Elemental S S8 Area: ~40.000

ConclusionImprovedprecision The Liquefied Gas Injector Faster is an alternative for theanalysis evaporative methods for high boiling components & in low boiling matrices Safe!

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Envantage da vinci_lgi_gcc2011

by clhellyer on Oct 25, 2011

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Envantage da vinci_lgi_gcc2011 — Presentation Transcript