Determination of microplastic content in seafood: An integrated approach combined with the determination of elemental contaminants.

A method for the determination of microplastic (MP) content in seafood is proposed based on the selective digestion of seafood without the degradation of MP. A simple approach was developed using diluted acid with microwave-assisted wet digestion. The following parameters were evaluated: nitric acid concentration (0.5 to 14.4 mol L-1), digestion temperature (180 to 220 °C), irradiation program holding time (10 to 30 min), MP particle size (0.3 to 5 mm), and the seafood mass (0.5 to 2 g). To develop a reliable method for the determination of MP amount, up to 2 g of an in natura seafood sample were spiked with a known amount of MP (100 mg of mixed MP). Suitable conditions were obtained using 1 mol L-1 HNO3 at 200 °C (10 min holding time). Digests were filtered and the plastic content was gravimetrically determined. The heating program was 20 min, which represents a significant reduction in the time normally reported in the literature for MP analysis (from few hours up to 3 days). The proposed method allowed gravimetric determination of eight plastic types (polyethylene terephthalate, polystyrene, expanded polystyrene, polypropylene, high and low density polyethylene, polycarbonate and polyvinyl chloride) with particle size ≥0.3 mm. Up to 2 g of an in natura seafood sample (shark species, acoupa weakfish, tuna fish, trahira, and pink shrimp) were efficiently digested, which opened the possibility of using the proposed digestion method for determining elemental contaminants (Al, As, Ca, Cd, Co, Cr, Cu, Fe, Hg, La, Mg, Mn, Mo, Ni, Pb, and Zn). Thus, as the main feature of the proposed digestion method is the possibility of determining MP and elemental contaminants using the same digestion protocol, saves time and reagents and provides accurate and precise information about different classes of marine pollutants (MP and elemental contaminants).

Sodium in different processed and packaged foods: Method validation and an estimative on the consumption.

Excessive sodium (Na) consumption can lead to serious health problems such as hypertension, and cardiovascular and renal diseases. Therefore, the food industry in worldwide has been trying to reduce sodium levels in processed products. The aim of this study was to validate a method and quantify sodium in processed and packaged foods and to estimate its ingestion in the consumption. In the first step, for choose the adequate analytical procedure different samples preparations (mineralization) were evaluated as wet and dry ash mineralization, as well as CsCl concentration to suppress chemical interferences for apply FAAS technique. The best performance conditions were applied for the analytical method validation: mineralization by wet digestion and adding 0.1% CsCl, which characterized the method as simple and low cost. The method was validated and was applied in 12 different processed food matrices (5 brands, 3 batches), including products of vegetable and animal origins, different majority components and interferences for Na evaluation. The results showed that sausage, hamburger, ham, bread, tomato sauce, ketchup, mustard, mayonnaise and mashed potato were classified as high-sodium foods, with mean values above 460 mg 100 g-1. It was verified that 68% of the samples were regarded as having high sodium content and the maximum value found was 2851 mg 100 g-1 for a sample of mashed potatoes. In addition, it was found that 38% of the samples presented differences in Na concentration when compared to content declared on the label. It is also observed that is possible different sodium ingestion according the combinations of processed and packaged foods in the same meal and, in this case, the sodium consumption is above than the daily value as recommended by the regulatory agencies. It was concluded that the majority of processed and packaged foods presented high sodium concentration even with efforts of the food industry to reduce the levels of this mineral and its remains an important public health problem.

Determination of inorganic contaminants in carbon nanotubes by plasma-based techniques: Overcoming the limitations of sample preparation.

In this work, sample preparation of carbon nanotubes (CNTs) for further determination of inorganic contaminants was investigated using a microwave-assisted wet digestion single reaction chamber system (MAWD-SRC). Analytes (Al, As, Ca, Cd, Co, Cr, Fe, La, Mg, Mo, Ni, Pb and Zn) were determined in CNTs by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS, except for Al, Ca, Fe and Mg). Method parameters were evaluated, as the mass of CNT (25-300 mg), the temperature (220-270 °C) and the time (35-75 min) of irradiation program. The accuracy was evaluated by using a certified reference material (CRM) of CNT and also by comparison of the results with those obtained using neutron activation analysis (NAA) and high resolution continuum source graphite furnace atomic absorption spectrometry with direct solid sampling (DSS-HR-CS-GF AAS). Quantitative recoveries for all elements were obtained using 275 mg of CNTs, 6 mL of 14.4 mol L-1 HNO3 and 0.5 mL of 30% H2O2 with an irradiation program of 65 min (35 min at 270 °C). No statistical difference was observed between the results obtained after the decomposition of CNTs by MAWD-SRC with those obtained by NAA and DSS-HR-CS-GF AAS. No difference was also observed for the results using the proposed method and the values for the CRM of CNT. The use of MAWD-SRC showed good performance for CNTs digestion using relatively high sample mass (up to 275 mg), contributing to low limits of quantification (LOQs) and overcoming the current limitations of sample preparation. To the best knowledge of the authors, this work reports the highest sample mass feasible to be decomposed using wet digestion for CNTs among the methods proposed in literature.

Determination of toxic elements in yerba mate by ICP-MS after diluted acid digestion under O2 pressure.

In this work, a procedure allowing effective digestion of a high mass of yerba mate (up to 1500 mg) using diluted HNO3, in a system pressurized with oxygen, is proposed. Digests were suitable for direct analysis by ICP-MS, virtually free of interferences. Digestion was performed using 7 mol l-1 HNO3 and 8 bar O2. The digestion efficiency was better than 92% and digests presented a relatively low acidity (<10 mmol HNO3). The limit of quantification was 4.0, 1.0 and 1.0 ng g-1 for As, Cd and Pb, respectively. Under optimized conditions up to 1500 mg of sample were digested and no interferences were observed during analyses by ICP-MS, making this approach suitable for routine determination of As, Cd and Pb in yerba mate and also in agreement with the quality control requirements.

Microwave-assisted ultraviolet digestion of petroleum coke for the simultaneous determination of nickel, vanadium and sulfur by ICP-OES.

A method for the simultaneous determination of Ni, V and S in petroleum coke by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted ultraviolet digestion (MW-UV) in closed vessels was proposed. Digestion was performed using electrodeless discharge lamps positioned inside quartz vessels and turned on by microwave radiation. The following parameters were evaluated: HNO3 concentration (15 mL of 1, 4, 7, 10 or 14.4 mol L(-1)), volume of H2O2 (30%, 1 or 3 mL), sample mass (100, 250 or 500 mg) and heating time (40 or 60 min) with or without the use of UV lamps. Digestion efficiency was evaluated by the determination of the residual carbon content (RCC) in digests. Using UV lamps lower RCC was obtained and the combination of 4 mol L(-1) HNO3 with 3 mL of H2O2 and 60 min of heating allowed a suitable digestion of up to 500 mg of petroleum coke (RCC< 21%). The agreement with the reference values for Ni, V and S (obtained by digestion of petroleum coke by microwave-induced combustion) and with a certified reference material of petroleum coke was between 96 and 101%. The proposed method was considered as advantageous when compared to American Society for Testing and Materials method because it allowed the simultaneous determination of Ni, V and S with lower limit of detection (0.22, 0.12 and 8.7 µg g(-1) for Ni, V and S, respectively) avoiding the use of concentrated nitric acid and providing digests suitable for routine analysis by ICP-OES.

Avaliação do método de perda de peso por ignição na análise de matéria orgânica em solos da Serra Gaúcha do Rio Grande do Sul

Soil organic matter evaluation in soil analysis laboratories is done using wet combustion methods. But, these methods contaminate the laboratories waste with chromium, so it is impacted find alternative methods to measure soil organic matter. The work was carried out in Embrapa Grape and Wine soil analysis laboratory to evaluate the loss-on-ignition as an alternative to wet combustion method to measure organic matter content in a group of soils from Rio Grande do Sul, in Southern Brazil. Nineteen soils not cultivated with clay content varying from 210 and 530g kg-1, were collected in layer 0-20cm. The soils were dried, 2mm sieved, grounded and prepared organic carbon analysis with loss-on-ignition, Walkley-Black and sulfochromic solution methods. The results showed that the loss-on-ignition method and Walkey-Black, in general, determined smaller percentage of organic matter than the sulfochromic solution method. Thus, the adoption at loss-on-ignition method, that doesn’t use the pollutant chromium, needs calibration to correct the differences, since the Walkey-Black method and sulfochromic solution are asked as reference methods and estimate with great precision the percentage of soil organic matter.

A matéria orgânica do solo nos laboratórios de rotina de análise de solo, em geral, é determinada por métodos de combustão úmida. Entretanto, esses métodos contaminam com cromo os efluentes laboratoriais. Assim, surge a necessidade de avaliar métodos alternativos de determinação da matéria orgânica do solo. O presente trabalho teve como objetivo avaliar o desempenho do método de perda de peso por ignição como método alternativo e que não possui o contaminante cromo na análise de matéria orgânica do solo, tendo sido realizado no Laboratório de Análise de Solo e Tecido Vegetal da Embrapa Uva e Vinho, no município de Bento Gonçalves, RS. Amostras de dezenove solos não-cultivados e cobertos com pastagem natural da região fisiográfica da Serra Gaúcha do RS, com argila variando de 210 a 530g kg-1 foram coletadas na camada de 0-20cm. Os solos foram secodos ao ar, passados em peneira com malha de 2mm, retirados, manualmente, resíduos de vegetais remanescentes no solo, macerados, novamente passados em peneira com malha de 1mm e preparados para a análise de C orgânico pelos métodos de perda de peso por ignição, Walkley-Black e solução sulfocrômica. Os dados mostraram que o método de perda de peso por ignição e o método de combustão úmida Walkey-Black, em geral, estimaram percentagens de matéria orgânica menores que os determinados pela solução sulfocrômica. Assim, a adoção do método de perda de peso por ignição, que não possui o contaminante cromo, necessita de calibração para as correções das diferenças, desde que se admita o método Walkey-Black e de solução sulfocrômica como métodos de referência e que estimem com maior precisão os teores de matéria orgânica em solos.

Avaliação do método de perda de peso por ignição na análise de matéria orgânica em solos da Serra Gaúcha do Rio Grande do Sul

Soil organic matter evaluation in soil analysis laboratories is done using wet combustion methods. But, these methods contaminate the laboratories waste with chromium, so it is impacted find alternative methods to measure soil organic matter. The work was carried out in Embrapa Grape and Wine soil analysis laboratory to evaluate the loss-on-ignition as an alternative to wet combustion method to measure organic matter content in a group of soils from Rio Grande do Sul, in Southern Brazil. Nineteen soils not cultivated with clay content varying from 210 and 530g kg-1, were collected in layer 0-20cm. The soils were dried, 2mm sieved, grounded and prepared organic carbon analysis with loss-on-ignition, Walkley-Black and sulfochromic solution methods. The results showed that the loss-on-ignition method and Walkey-Black, in general, determined smaller percentage of organic matter than the sulfochromic solution method. Thus, the adoption at loss-on-ignition method, that doesnt use the pollutant chromium, needs calibration to correct the differences, since the Walkey-Black method and sulfochromic solution are asked as reference methods and estimate with great precision the percentage of soil organic matter.

A matéria orgânica do solo nos laboratórios de rotina de análise de solo, em geral, é determinada por métodos de combustão úmida. Entretanto, esses métodos contaminam com cromo os efluentes laboratoriais. Assim, surge a necessidade de avaliar métodos alternativos de determinação da matéria orgânica do solo. O presente trabalho teve como objetivo avaliar o desempenho do método de perda de peso por ignição como método alternativo e que não possui o contaminante cromo na análise de matéria orgânica do solo, tendo sido realizado no Laboratório de Análise de Solo e Tecido Vegetal da Embrapa Uva e Vinho, no município de Bento Gonçalves, RS. Amostras de dezenove solos não-cultivados e cobertos com pastagem natural da região fisiográfica da Serra Gaúcha do RS, com argila variando de 210 a 530g kg-1 foram coletadas na camada de 0-20cm. Os solos foram secodos ao ar, passados em peneira com malha de 2mm, retirados, manualmente, resíduos de vegetais remanescentes no solo, macerados, novamente passados em peneira com malha de 1mm e preparados para a análise de C orgânico pelos métodos de perda de peso por ignição, Walkley-Black e solução sulfocrômica. Os dados mostraram que o método de perda de peso por ignição e o método de combustão úmida Walkey-Black, em geral, estimaram percentagens de matéria orgânica menores que os determinados pela solução sulfocrômica. Assim, a adoção do método de perda de peso por ignição, que não possui o contaminante cromo, necessita de calibração para as correções das diferenças, desde que se admita o método Walkey-Black e de solução sulfocrômica como métodos de referência e que estimem com maior precisão os teores de matéria orgânica em solos.