h i g h l i g h t s " Galvanised and carbon steels have proven to be compatible with biodiesel. " Biodiesel properties were not affected for a storage time of 56 days. " Zinc release in non-stabilised biodiesel did not stimulate biodiesel deterioration. " TBHQ was rapidly consumed in the first days of the corrosion immersion test. " TBHQ acted as a corrosion inhibitor and enhanced storage stability of biodiesel.
a b s t r a c tThe storage stability and corrosive character of soybean biodiesel stabilised with tert-butylhydroquinone (TBHQ) was investigated through static immersion corrosion tests. Coupons of carbon steel and galvanised steel were immersed in soybean biodiesel with and without TBHQ for 12 weeks. Measurements of total acid number, peroxide value, oxidation stability (Rancimat induction period), metal release, and TBHQ consumption at different stages of corrosion were performed. After 12 weeks of the static immersion test with both steels, the non-stabilised biodiesels presented induction times below the EN 14214 limit (6 h); these results were in agreement with increase in the peroxide values. Zinc release was only detected in the non-stabilised biodiesel exposed to galvanised steel, whilst iron was not detected in any biodiesel samples exposed to carbon steel. The absence of zinc in the TBHQ-doped biodiesel exposed to galvanised steel indicates that TBHQ may have acted as a corrosion inhibitor. Additionally, TBHQ was rapidly consumed in the first 3 days of experiments, providing evidence of its activity. For a storage period of up to 56 days, both galvanised and carbon steels were shown to be compatible with biodiesel even in the absence of an antioxidant. The presence of zinc (>2 lg g À1 after 28 days of immersion) due to corrosion did not promote biodiesel deterioration.
Electroanalytical stripping techniques have been well-used for trace-metal determinations, because of their
remarkable sensitivity and selectivity. However, when these techniques are applied for organic materials, such
as crude oil and petroleum-based fuels, the samples must be decomposed. This paper evaluates the use of
different microwave ovens for the decomposition of crude oil and diesel fuel to determine the content of
copper, lead, mercury, and zinc in the digestates. A focused-microwave (FM) oven using H2SO4/HNO3/H2O2,
operated at atmospheric pressure, and a closed-vessel microwave (CVM) oven using HNO3/H2O2, operated
under pressure in a vessel, were evaluated. Square-wave stripping voltammetry (SWSV) and stripping
chronopotentiometry (SCP) at gold film electrodes were applied for copper, lead, and mercury. Potentiometric
stripping analysis (PSA) at mercury film electrodes was applied for copper, lead, and zinc. SWSV was more
affected by residual organic matter, especially for lead determination. SCP presented higher sensitivity for
copper and mercury at gold electrodes. PSA at mercury electrodes was preferred for lead and zinc determination.
Better detection limits were attained for FM-digested solutions, after 0.8−1.0 g of sample can be digested, in
contrast to the low quantities (0.10−0.25 g) used when pressurized vessels were explored. Nevertheless, the
loss of mercury was verified when samples were decomposed in the FM oven.
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