The impacts of temperature shifts from 30 to 45 degreesC on the structural stability and surface charge of activated sludge floes were assessed in four sequencing batch reactors (SBRs) treating pulp and paper mill effluent. The improvement in floc stability was tested by sludge magnesium enrichment in one SBR and by operating another reactor at a high sludge retention time (SRT) of 33 days. Floc stability was characterized by dissociation constants with solutions of CaCl2, KCL urea, and ethylenediamine tetraacetate (EDTA). Surface charge was assessed by cationic-anionic titration and metals concentrations were also determined. The temperature shift consistently caused an increase in the negative sludge surface charge from approximately -0.180 to -0.300 meq/g MLSS. Magnesium enrichment and a high SRT of 33 days promoted less negatively charged sludge, dampened the increase in negative sludge surface charge, and yielded structurally stronger floes; however, sludge deflocculation still occurred. Manganese and iron appeared to be released by sludge under the temperature shift. It was concluded that the temperature shift deteriorates the flocculating physicochemical properties of the sludge and that better floc stability achieved by magnesium enrichment and a high SRT is not enough to stop deflocculation. Further research is required to clarify the origin of the increase in negative sludge surface charge, the role of metals, and the governing factors in sludge deflocculation under such temperature shifts. (C) 2004 Elsevier Inc. All rights reserved.