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12 Analytical Instrumentation The easiest way to contact us leads@pin-pub.com Request information on products featured in this issue


Laboratory Fluorinated By-Products Analyser


The Hydrofluoric (HF) Alkylation process catalytically combines C3 – C5 olefins with isobutene to produce motor fuel alkylate. There is an increasing demand for alkylate because of its properties as a low-sulphur, highoctane blending component for unleaded and reformulated gasoline. The products of the process contain traces of HF and organofluoride by-product compounds. Elevated levels of residual fluorinated byproducts in process streams can cause serious problems in refinery operations including corrosion, catalyst poisoning, downtime, and lost production. Fluorinated by- products are removed by catalytic decomposition at 177 – 220 °C to HF and olefins. The HF released during this decomposition step is removed by adsorption on a bed of alumina forming aluminium fluoride. This step reduces total fluoride levels from approximately 100 – 400 ppm down to low ppm levels in the motor fuel alkylate.


OI Analytical’s (USA) FBA 5320 is a laboratory fluorinated by-products analyser (FBA) designed to detect and measure total fluorinated contaminants (HF and organofluoride compounds) in liquid propane, liquid butane, and motor fuel alkylate from the HF alkylation process. The analyser is based on an Agilent 7890 gas chromatograph equipped with an automated liquid sampling valve for sample introduction, a packed-inlet injection port, a stainless steel column, and a 5320 Electrolytic Conductivity Detector (ELCD) configured for fluoride detection. The FBA 5320 accurately detects total fluoride concentrations in the low parts-per-million (ppm) range. The FBA 5320 is typically calibrated with a calibration gas mixture (e.g. 3- fluoropropane in n-Butane) or using a sample from a C4 process stream analysed by the Wickbold Method (ASTM D 7284). The measurement range of the FBA 5320 is 0.02 to 100ppm-F.


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Although Analytical Services (AS) have many standards and calibration sets available as catalogue items, they can also provide custom sets based on your specific needs. AS specialise in the custom formulation of multi-element standards in difficult matrices. A complete line of consumables such as film, cups and pipets necessary for XRF analysis, is also offered. Their manufacturing facility is located just north of Houston, and they ship worldwide into almost every country. AS are fully certified in the shipment of dangerous goods and their customer service staff is prepared to assist with ordering, technical assistance and any questions you may have regarding their products and services. All standards are produced and certified in-house and are accompanied with a Certificate of Analysis indicating traceability to ASTM and NIST methods, validity term and degree of uncertainty.


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Calibration Standards for Acetaldehyde in Carbon Dioxide


Trace concentration calibration standards of acetaldehyde in carbon dioxide are dynamically blended using the FlexStream Automated Gas Standards Generator and TraceSource Permeation Tubes from Kin- Tek Laboratories (USA). Acetaldehyde emitted by the permeation tube is added directly to a controlled flow of purified or beverage grade carbon dioxide to form the mixture. Mixture concentration is adjusted by varying to carbon dioxide flow. Users may achieve concentrations from over 400 ppb down to 25 ppb using a single permeation tube. Lower concentrations, or variable concentration in constant flow, are available using optional secondary dilution. The standard additions technique is used to compensate for residual acetaldehyde in the carbon dioxide. Mixtures concentrations are traceable to NIST through physical standards.


Acetaldehyde is a key component causing ‘off taste’ and ‘off odour’ problems in carbonated beverages and is routinely monitored to ensure concentrations below 200ppb. Trace concentration mixtures are generally not stable in storage. The dynamic blending method using permeation tubes avoids that problem and insures reliable standards.


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