16 Marzo 2020

EMERGENZA SANITARIA CORONAVIRUS

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 SPETTOSCOPIA ATOMICA
Fiamma
ASSORBIMENTO Fornetto di grafite
SPETTOSCOPIA ATOMICA
EMISSIONE ICP ICP/MS

Determinazione di metalli ed elementi (ICP – ICP/MS)

Da considerare:
pretrattamento - concentrazioni - costo strumento e/o analisi

Stefano Materazzi - Chimica Analitica Forense 2

Spettroscopia Atomica in Fiamma

Fornetto di grafite

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ICP - Inductively coupled plasma

Hg - vapori freddi Hg++ + SnCl2 -> Hg0 aria -> assorbimento

Generazione di idruri As, Bi, Sb, Pb, Ge, Se, Sn + agente riducente -> MeH 3
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 Esempi di applicazioni forensi

A fast ultrasound-assisted extraction procedure for trace elements determination

in hair samples by ICP-MS for forensic analysis 

Forensic Science International, Volume 192, Issues 1-3, 20 November 2009, Pages 88-93

Bruno Lemos Batista, Jairo Lisboa Rodrigues, Vanessa Cristina de Oliveira Souza, Fernando Barbosa Jr.

An ultrasound-assisted extraction method is proposed for the determination of trace elements in hair samples
by inductively coupled plasma-mass spectrometry (ICP-MS) for forensic investigation. Prior to analysis, 25 mg of
hair samples were accurately weighed into (15 mL) conical tubes. Then, 2 mL of 20% HNO3 is added to the
samples, sonicated at 2 min (50 W, 100% amplitude), and then further diluted to 10 mL with Milli-Q water.
Resulted diluted slurries are centrifuged and the analytes are directly determined in the supernatant.
Calibrations against aqueous solutions were carried out with rhodium as internal standard. The method was
successfully applied for the extraction of Al, As, Ba, Be, Cd, Co, Cr, Cu, Mn, Pb, Tl, U, V and Zn with a method
detection limit (3 s, n = 20) of 0.1, 0.4, 0.2, 0.09, 0.08, 0.04, 0.1, 2.9, 1.0, 0.9, 0.04, 0.05, 0.1 and 4.2 ng/g,
respectively. Method accuracy is traceable to Certified Reference Materials (CRMs) 85 and 86 human hair from
the International Atomic Energy Agency (IAEA). Additional validation data are provided based on the analysis of
hair samples from the trace elements intercomparison program operated by the Institut National de Sante’
Publique du Quebec, Canada. The proposed method is very simple and can be applied for forensic purposes with
the elimination of sample digestion step prior to analysis. Then, a considerable improvement in the sample
throughput is achived with the use of the proposed method.

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 Laser Ablation
ICP/MS

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 Application of laser ablation (LA-ICP-SF-MS) for the elemental analysis of bone
and teeth samples for discrimination purposes 

Forensic Science International, Volume 195, Issues 1-3, 25 February 2010, Pages 17-27

Waleska Castro, Jurian Hoogewerff, Christopher Latkoczy, José R. Almirall

Human bone and teeth fragments can be useful evidence when found in crime scenes and/or mass burials sites.
The elemental and isotopic composition of these samples can provide information about environmental
exposure events and could also be used to distinguish different individuals. The development and application of
robust analytical methods for the quantification of trace elements in these biological matrices may lead to a
better understanding of the potential utility of these measurements in forensic analyses The developed method
requires micrograms amount of sample (vs. milligrams required for solution-based analysis) while also reducing
the analysis time and resulting in good accuracy (typically <10% bias) and precision (<15% RSD). Additionally,
laser ablation allowed using spatial resolution analysis to assess the biogenic elemental composition in buried
bone samples.
Elemental analysis of bone samples from 12 different individuals provided better discrimination between the
individuals when the femur and humerus bones were considered separately (42.7% correct classification with all
bones vs. 75.2% and 63.1% for femur bones and humerus bones, respectively). Separation of individuals was
achieved by elemental composition of whole teeth samples from 14 individuals, except one case where not all
the teeth from the same individual were associated together. Separation of individuals was improved when
using elemental composition of the enamel and dentine + cementum layers separately in a set of samples from
7 individuals. These are promising results for the use of elemental analysis by laser ablation ICP-MS for
discrimination purposes.

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 Determination of arsenic in blood and stomach contents by inductively coupled
plasma/mass spectrometry (ICP/MS) 

Forensic Science International, Volume 81, Issue 1, 31 July 1996, Pages 43-50

Toshiko Tanaka, Kyoko Hara, Akihide Tanimoto, Kentaro Kasai, Toshiro Kita, Noriyuki Tanaka, Tatsunori Takayasu

Inductively coupled plasma/mass spectrometry (ICP/MS) was used and evaluated for the practical analysis of the
arsenic content of body fluid samples without ashing. The calibration curve for arsenic in blood solution was shown
to have good sensitivity, linearity and reproducibility. Blood obtained from normal volunteers was determined by
ICP/MS, and compared with that determined by atomic absorption spectrometry (AAS). The arsenic contents
determined by ICP/MS showed a linear correlation with that determined by AAS. Furthermore, arsenic was
determined in the blood and supernatant of stomach contents obtained from a suicide autopsy case resulting from
ingestion of an arsenic compound. It was therefore concluded that ICP/MS could be used rapidly and conveniently
in the field of forensic toxicology in acute metal poisoning cases.

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Applicazioni forensi della Spettroscopia atomica in fiamma
Applicazioni forensi della spettroscopia ICP (ottico o MS)
Laser Ablation ICP/MS

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