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Combining submerged membrane technology with anaerobic and ...

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Acetic Acid (mg·L -1 )Chapter 2VFA are determined by gas chromatography (HP, 5890A) equipped <strong>with</strong> a flameionization detector (FID) <strong>and</strong> an automatic injector (HP, 7673A). The determination isperformed in a glass column (3 m long <strong>and</strong> 2 mm of internal diameter) filled <strong>with</strong>chromosorb WAW (mesh 100/120) impregnated <strong>with</strong> NPGA (25%) <strong>and</strong> H 3PO 4 (2%). Thecolumn, injector <strong>and</strong> detector temperatures are 105, 260 <strong>and</strong> 280°C, respectively. Gas N 2,previously saturated <strong>with</strong> formic acid before entering into the injector, is used as carriergas <strong>with</strong> a flow of 24 mL·min -1 . Air <strong>and</strong> H 2 are used as auxiliary gases <strong>with</strong> flows of 400<strong>and</strong> 30 mL·min -1 , respectively. VFA, after being separated in the column according to theirmolecular weights, are burnt in a H 2-air flame <strong>and</strong> finally measured in the FID at 280°C.The quantification of the sample is made <strong>with</strong> a 6-8 point calibration curve for each acid inthe range of 0-1 g·L -1 , using pivalic acid as internal st<strong>and</strong>ard (figure 2.2). The detectionlimit of the equipment is 20 mg·L -1 .140012001000y = 6043x - 125R² = 0.99980060040020000.00 0.05 0.10 0.15 0.20 0.25Integrated area of the peakFigure 2.2. Example of a calibration curve for the acetic acid.2.1.2. Nitrogen compounds2.1.2.1. AmmoniumThe two major factors that influence the ammonia determination method are theconcentration <strong>and</strong> the presence of interferences, such as chlorine. For the determination oflow ammonia concentration <strong>with</strong>out the presence of interferents, a colorimetric method(Wheatherburn, 1967) is used. This method base on the reaction of NH 3 <strong>with</strong> HClO <strong>and</strong>phenol, forming a strong-blue compound (indophenol) which can be colorimetricallydetermined using a spectrophotometer (Cecil CE 7200) at 635 nm.66

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