title: Comparison of direct solid sampling and slurry sampling for the determination of cadmium in wheat flour by electrothermal atomic absorption spectrometry.
abstract: Two analytical methods for the determination of cadmium in wheat flour by electrothermal atomic absorption spectrometry without prior sample digestion have been compared: direct solid sampling analysis (SS) and slurry sampling (SlS). Besides the conventional modifier mixture of palladium and magnesium nitrates (10 microg Pd+3 microg Mg), 0.05% (v/v) Triton X-100 has been added to improve the penetration of the modifier solution into the solid sample, and 0.1% H(2)O(2) in order to promote an in situ digestion for SS. For SlS, 30 microg Pd, 12 microg Mg and 0.05% (v/v) Triton X-100 have been used as the modifier mixture. Under these conditions, and using a pyrolysis temperature of 800 degrees C, essentially no background absorption was observed with an atomization temperature of 1600 degrees C. About 2 mg of sample have been typically used for SS, although as much as 3-5 mg could have been introduced. In the case of SlS multiple injections had to be used to achieve the sensitivity required for this determination. Calibration against aqueous standards was feasible for both methods. The characteristic mass obtained with SS was 0.6 pg, and that with SlS was 1.0 pg. The limits of detection were 0.4 and 0.7 ng g(-1), the limits of quantification were 1.3 and 2.3 ng g(-1) and the relative standard deviation (n=5) was 6-16% and 9-23% for SS and SlS, respectively. The accuracy was confirmed by the analysis of certified reference materials. The two methods were applied for the determination of cadmium in six wheat flour samples acquired in supermarkets of different Brazilian cities. The cadmium content varied between 8.9+/-0.5 and 13+/-2 ng g(-1) (n=5). Direct SS gave results similar to those obtained with SlS using multi-injections; the values of both techniques showed no statistically significant difference at the 95% confidence level. Direct SS was finally adopted as the method of choice, due to its greater simplicity, the faster speed of analysis and the better figures of merit.
authors.affiliation: Universidade Federal da Bahia, Instituto de Química, Grupo de Pesquisa em Química Analítica, Campus Ondina, 40170-290 Salvador, BA, Brazil.
authors.forename: Rennan G O
authors.initials: RG
authors.lastname: Araujo
authors.forename: Nédio
authors.initials: N
authors.lastname: Oleszczuk
authors.forename: Roger T
authors.initials: RT
authors.lastname: Rampazzo
authors.forename: Pedro A
authors.initials: PA
authors.lastname: Costa
authors.forename: Márcia M
authors.initials: MM
authors.lastname: Silva
authors.forename: Maria Goreti R
authors.initials: MG
authors.lastname: Vale
authors.forename: Bernhard
authors.initials: B
authors.lastname: Welz
authors.forename: Sérgio L C
authors.initials: SL
authors.lastname: Ferreira
mesh_terms: D002104:Cadmium / Q000032:analysis*; D004583:Electrons; D005433:Flour / Q000032:analysis*; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013696:Temperature; D014908:Triticum / Q000737:chemistry*
chemical_list: D002104:Cadmium