Organic palladium and palladium-magnesium chemical modifiers in direct determination of lead in fractions from distillation of crude oil by electrothermal atomic absorption analysis

Kowalewska, Zofia; Bulska, Ewa; Hulanicki, Adam

doi:10.1016/s0584-8547(99)00049-x

Cited by 38 publications

(12 citation statements)

References 18 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Platform atomization, matrix modification, integrated absorbance and powerful background correction techniques together with ETAAS have been used to overcome these problems. Different permanent modifiers (W-Rh, W-Ir and W-Ru) (Lima et al, 2002a, b) and other suitable modifiers, such as Sc + Pd + NH 4 NO 3 (Acar, 2005), Sc + Ru + (NH 4 ) 2 HPO 4 (Acar, 2004) and organic palladium and palladiummagnesium chemical modifiers (Kowalewska et al, 1999) have been used for the determination of Cd, Cu and Pb in various samples in order to stabilize the analytes to higher permissible pyrolysis temperatures and to reduce such interferences in a sample matrix prior to the atomization steps. An Sc + Ir + NH 4 H 2 PO 4 modifier mixture has not been used in previous studies.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Acar¹

2012

Grasas y Aceites

View full text Add to dashboard Cite

RESUMENEvaluación de cadmio, plomo, cobre, hierro y zinc en aceites vegetales y aceitunas de la dieta turca mediante espectrometría electrotérmica y absorción atómica de llama.Se han determinado los metales Cd, Cu, Pb, Fe y Zn en aceites vegetales comestibles (soja, girasol, flores, nueces, maíz y aceite de oliva) y aceitunas (aceitunas-1, negra, verde, negra machacadas con semillas y verde machacadas con semillas) mediante espectrometría de absorción atómica electrotérmica (ETAAS) utilizando como modificador químico la mezcla Sc + Ir + NH 4 H 2 PO 4 y mediante espectrometría de absorción atómica de llama (FAAS) tras digestión con microondas. Se estudiaron las temperaturas de pirólisis y atomización para Cd, Pb y Cu en disolución con y sin modificador. Los límites de detección (LOD) fueron: 0.1, 0.6, 0.9, 15.0 y 12.0 mg L -1 para Cd, Cu, Pb, Fe y Zn, respectivamente. La precisión del procedimiento propuesto se confirmó mediante el análisis de materiales estándar de referencia (SRM) 1577b de hígado de bovino y mediante una solución de muestra sembrada. Los resultados se compararon con los valores certificados. Las desviaciones estándar fueron inferiores al 7% y el rango de las recuperaciones obtenidas de 96 a 101%. La mezcla propuesta Sc + Ir + NH 4 H 2 PO 4 se aplica a la determinación de Cd, Pb y Cu en los aceites y en aceitunas. Los resultados encontrados en las muestras se compararon con los recogidos en las reglamentaciones internacionales y nacionales de calidad de los alimentos, así como con los valores encontrados en la bibliografía. PALABRAS CLAVE: Aceites y aceitunas -ETAAS y Faas -Metales -Modificador Químico. SUMMARY Evaluation of cadmium, lead, copper, iron and zinc determinations in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometryThe Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH 4 H 2 PO 4 chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 µg L -1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH 4 H 2 PO 4 mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compar...

show abstract

Section: Introductionmentioning

confidence: 99%

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Acar¹

2012

Grasas y Aceites

View full text Add to dashboard Cite

show abstract

“…In the simplest sample preparation procedure, when only dilution with an organic solvent is made (direct method), calibration standards in an appropriate organic form are required to assure good accuracy of analysis [23,24]. The pumping of oil samples diluted with an organic solvent requires a solvent resistant pump-tube that is not always available [23].…”

Section: Introductionmentioning

confidence: 99%

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

Kowalewska¹,

Ruszczyńska²,

Bulska³

2005

Spectrochimica Acta Part B: Atomic Spectroscopy

Self Cite

View full text Add to dashboard Cite

“…Apart from Pd, the application of air in the pyrolysis stage turned out to be crucial for the determination of Ni [48] and V porphyrins [35] and in the determination of V in residues and heavy fractions from petroleum distillation [35]. In some other analyses, for example in the determination of Pb in the form of Pb cyclohexanebutyrate [46] or the determination of V or Ni in forms containing O-bound metal (e.g. S21, VC, VA3 and VA4) [35,52], the pretreatment with iodine dissolved in toluene, followed by a treatment with MTOACl was indispensable.…”

Section: Experiments With Air Ashing and I 2 þ Mtoacl Pretreatmentmentioning

confidence: 99%

“…In some of our earlier work, devoted to the determination of other elements in xylene solution of petroleum products, Mg acetylacetonate (MgA) was successfully applied as part of a modifier system. MgA, added to Pd acetylacetonate (PdA) solution, significantly increased the integrated absorbance of Pb in S21 multielement Conostan oil standard, Pb in 1634b oil and tetraethyllead [46], and it also added to thermal stabilization of the analyte. The addition of MgA to the PdA modifier turned out to be indispensable for the quantitative determination of S in a polysulfide form using graphite furnace molecular absorption spectrometry [47].…”

Section: Introductionmentioning

confidence: 99%

Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry

Kowalewska

Welz

Castilho

et al. 2013

Talanta

Self Cite

View full text Add to dashboard Cite

The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is recommended to check the effect of Mg using recovery tests of V in a form that is affected by MgA.

show abstract

Organic palladium and palladium-magnesium chemical modifiers in direct determination of lead in fractions from distillation of crude oil by electrothermal atomic absorption analysis

Cited by 38 publications

References 18 publications

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry

Contact Info

Product

Resources

About