The need to have a reliable method for the measurement of total chloride in petroleum crude is well recognized in the petroleum industry.  This method serves as a primary indication of potential impact in refining facilities during crude distillation operations tower overhead systems and ferrous alloys throughout a refinery. Refineries spent millions of dollars annually in corrosion mitigation.<br/>There are different standard methods as well as a portfolio of analytical techniques to quantify chloride in crude. As example, in ASTM D4929 – “Standard Test Methods for Determination of Organic Chloride Content in Crude Oil., the crude oil is distilled, and the naphtha fraction is analyzed for organic chloride with either sodium biphenyl reduction followed by potentiometric titration (Test Method A), or by combustion with micro coulometric detection (Test Method B).  However, this implies multiple sample preparation steps before the chloride can be measured. Additionally, organic chloride, if present in the crude, must be distilled at 400 °F to quantify using this test method. ASTM D7536, Standard Test Method for Chlorine in Aromatics by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry (MWDXRF), measurement of the chlorine content of aromatics with minimal sample preparation and analyst involvement.<br/>Additionally, total chloride can be measured by Combustion Ion chromatography (CIC), Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES), Inductively Coupled Plasma Atomic Mass Spectrometry (ICP-MS) as well as instrumental Neutron Activation Analysis (INAA).<br/>Our goal was to understand the challenges associated with the total quantitation of chloride in petroleum crude samples by evaluating different detection techniques such as Combustion Ion chromatography (CIC), Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry (MWDXRF), Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES), and Inductively Coupled Plasma Atomic Mass Spectrometry (ICP-MS, single quadrupole and triple quadrupole) on a Standard Reference Material such as NIST 1634c (Trace Elements in Fuel Oil) as well as a suite of selected crude oil samples having different characteristics. . We will present the figure of merit obtained from the analysis of the SRM material, the precision among techniques and potential difficulties associated analyzing this element due to varying sulfur content present in the selected samples<br/>

Chloride analysis in petroleum crude samples part 1: Evaluation of different detections techniques

255th National Meeting (2018)

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