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Quantitative analysis of residual SiH in silicone surfactants

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Information about Quantitative analysis of residual SiH in silicone surfactants
Technology

Published on March 12, 2014

Author: ISXperts

Source: slideshare.net

Description

The chemical industry still applies methods and technology that, in our point-of-view, is outdated and extremely inefficient. The analysis of residual SiH in silicone
surfactants, for example, is still carried out by means of the ancient gasometric method in which residual SiH is converted to hydrogen after reaction with KOH/EtOH.
Needless to say, this procedure is extremely time consuming and highly susceptible to the experience and the personal interpretation of the operator. In the context of
a Lean reconversion project, we have translated the outdated gasometric method to a GC compatible procedure with on-line derivatization and integrated calibration.
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Add reagent Agitate Clean syringe Change syringe Inject Clean syringe Change SyringeChange syringe Change SyringeChange SyringeChange syringe Typical chromatogram EXPERT CHROMATOGRAPHY FOR EVERYONE ! Performance results Precision: 2.5% RSD (n = 10) Linearity (standards prepared by online digital dilution): R² = 0.9999 Bias: < 15% compared to the gasometric method Sensitivity: 0.005 mL hydrogen/g Stress test: 48 h continuous operation without technical/analytical outlier QUANTITATIVE ANALYSIS OF RESIDUAL SIH IN SILICONE SURFACTANTS The chemical industry still applies methods and technology that, in our point-of-view, is outdated and extremely inefficient. The analysis of residual SiH in silicone surfactants, for example, is still carried out by means of the ancient gasometric method in which residual SiH is converted to hydrogen after reaction with KOH/EtOH. Needless to say, this procedure is extremely time consuming and highly susceptible to the experience and the personal interpretation of the operator. In the context of a Lean reconversion project, we have translated the outdated gasometric method to a GC compatible procedure with on-line derivatizationand integrated calibration. The system is fully validated and being applied in various laboratories across The Netherlands and Belgium. Instrumentation Thermo Trace 1310 GC equipped with S/SL and µ-TCD and hyphenated to an online digital dilution unit. Typical hydrogen analyzer equipped with Q-BOND column for separation of CO2 from air, backflush to injector, and Molsieve 5A column. Total runtime: 5.00 min. Typical chromatogram ! Performance results Precision: 2.5% RSD (n = 10) Linearity (standards prepared by online digital dilution): R² = 0.9999 Bias: < 15% compared to the gasometric method Sensitivity: 0.005 mL hydrogen/g Stress test: 48 h continuous operation without technical/analytical outlier Sample prep procedure Carried out with a Triplus RTC sampler. ? www.the-uninspired-scientist.com “On-line Calibration Functionality guarantees System Suitability Run after Run” W. Liekens and J. Vercammen www.is-x.com More?j.vercammen@is-x.com

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