![Page 1: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/1.jpg)
CHIMICA ANALITICA II CON LABORATORIO
(AA 2016-17)8 C.F.U. - Laurea triennale in Chimica
21
![Page 2: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/2.jpg)
2
![Page 3: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/3.jpg)
Il processo di misura chimico o Chemical Measurement Process
• Il campionamento (fattori limitanti, approcci, tipi di campione,
errori, metodi);
• La preparazione del campione
• La misura e la trasduzione del segnale analitico
• L’acquisizione del segnale e l’elaborazione dei dati
• Le operazioni di calibrazione (di strumenti e apparati, metodi)
(capitolo 4: Kellner, 2004)3
![Page 4: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/4.jpg)
PASSI PRINCIPALI DI UN Processo di Misura Chimico CMPDAL CAMPIONE AI RISULTATI
Tecnica / Metodo (Procedura) 4
![Page 5: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/5.jpg)
Il CAMPIONAMENTO può essere definito in modi
complementari
1.La procedura pratica impiegata per selezionare una
singola porzione (aliquota) o più porzioni da un materiale
(oggetto) studiato;
2.Il legame tra l’oggetto e gli altri passi del processo
analitico;
3.Il modo in cui si consegue la rappresentatività dei risultati
analitici rispetto a uno specifico insieme di aspetti/parametri
(features) dell’oggetto da caratterizzare, tenendo conto sia
delle caratteristiche dell’oggetto che dell’informazione
richiesta su di esso 5
![Page 6: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/6.jpg)
Oldies and goldies…Sampling for chemical analysis Byron Kratochvil, John K. Taylor
Anal. Chem., 1981, 53 (8), pp 924A–938A DOI: 10.1021/ac00231a001
• http://pubs.acs.org/doi/pdf/10.1021/ac00231a001
applicazioni
• http://pubs.acs.org/doi/pdf/10.1021/ac00269a010
ASTM E300 - 03(2009) Standard Practice for Sampling Industrial Chemicals
Representative samples of industrial chemicals are required for the determination of chemical
and physical properties which are used to establish standard volumes, prices, and compliance
with commercial and regulatory specifications.
The objective of sampling is to obtain a small portion (spot sample) of material from a selected
area within a container which is representative of the material in the area or, in the case of
running or all-level samples, a sample whose composition is representative of the total material in
the container. A series of spot samples may be combined to create a representative sample
6
![Page 7: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/7.jpg)
“COLLI DI BOTTIGLIA” NELLE PROCEDURE DI CAMPIONAMENTO
1. Il campionamento (fattori limitanti)
7
![Page 8: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/8.jpg)
Sample
preservation
and
transport:
es. bags per
VOCs
Tedlar=Polivinilfluoruro
Teflon=Politetrafluoro-
Etilene
Nalophan=Polyethylene-terephthalate8
![Page 9: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/9.jpg)
Protocollo di campionamento deve rispondere a:
• Dove?
• Quando?
• Quanti?
• Che quantità?
• Come?
9
![Page 10: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/10.jpg)
APPROCCI AL CAMPIONAMENTO1. Il campionamento (approcci)
10
![Page 11: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/11.jpg)
es. variabilità spazialeI pallini son punti di campionamento
es. variabilità temporaleLe frecce son momenti di campionamento
Mancanza di uniformità spaziale o temporale dell’oggetto da fescrivere
11
![Page 12: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/12.jpg)
(1)
12
![Page 13: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/13.jpg)
Andamento IPAIPA totali
0
50
100
150
200
250
gen-
06fe
b-06
apr-0
6giu
-06
lug-0
6se
t-06
nov-
06dic
-06
feb-
07ap
r-07
mag
-07
ug/k
g
Mytilus galloprovincialis
fluorene
fenantrene
antracene
fluorantene
pirene
benzo[a]antracene
crisene
benzo[b]fluorantene
benzo[k]fluorantene
benzo[a]pirene
indeno(1,2,3-cd)pirene
benzo[g,h,i]perilene
10 ppb -RegolamentoEuropeo1881/2006
13
![Page 14: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/14.jpg)
VALORE DI RIFERIMENTOper il benzene
nell’aria ambiente, MEDIA ANNUA 5
ug/m3
I pallini blu e fucsia indicano dati orari per due siti diversi
14
![Page 15: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/15.jpg)
Tipi di campione1. Il campionamento
(tipi di campione)
15
![Page 16: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/16.jpg)
Esempi di riduzione della quantità di campione
16
![Page 17: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/17.jpg)
IL SITO ACQUARIO
20071998
Terrapieno di colmata (fascia a mare a valle della strada Provinciale n.14 Muggia-Lazzaretto).Superficie 28.094 m2 = 24.583 m2 di terrapieno + 3.511 m2 di scogliera.Estensione lungo-costa di circa 1.000 m - larghezza media di circa 30 m.Considerando uno spessore medio del terreno di riporto di circa 4 m, il volume totaledel terrapieno risulta di circa 100.000 m3. 17
![Page 18: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/18.jpg)
Ubicazione sondaggi e sedime marino
18 18
![Page 19: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/19.jpg)
19
DATABASE PER ANALISI DATI E PIANIFICAZIONE INTERVENTI
19
![Page 20: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/20.jpg)
20
Nuovo MODELLO CONCETTUALE PRELIMINARE
SORGENTE ⇒ TRASPORTO ⇒ BERSAGLI
SORGENTE FORZANTI PERCORSI RICETTORI
VOLUMI Q FALDA Q O UT-ATMMARE
(colonna d'acqua, sed., biota)
MATRICI Q PIO GG IA Q O UT-SUOLO SUOLO
ETEROGENEITA' (zonazione)
Q MARE Q O UT-MARE (diretto) ATMOSFERA
CONCENTRAZIONI Q O UT-MARE (sed im enti)
20
![Page 21: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/21.jpg)
ANALISI CHIMICHE su suoli e acque
•UNITS - DISGAM (Referente Covelli) granulometria, Umidità, Carbonio Organico, Mercurio
•UNITS - DSCh (Referente Barbieri) IPA, PCB, OT
•UNITS - DSCh (Referente Adami) Metalli
•EnviroLab d.o.o.(referente Addobbati) Amianto e C>12
•Ambiente Analisi srl (referente Sancandi) speciazione C>12 per analisi di rischio, IPA (HPLC-FD)
21
![Page 22: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/22.jpg)
Errori sistematici di campionamento(dovuti a strumentazione o conservazione del campione (H2O, CO2, O2, metabolismo di microorganismi))Possono aver segno positivo o negativo
Errori casuali/random di campionamentogli errori casuali in genere diminuiscono con l’aumentare della quantità di campione e con il numero dei campioni
Il campionamento (errori)
22
![Page 23: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/23.jpg)
Errore relativo in relazione alla massa di campioneIl campionamento (errori)
“Ingamells has shown that the relationWR2 = Ks (2)is valid in many situations. In Equation 2, W represents the weight of sample analyzed, R is the relative standard deviation (in percent) of sample composition, and K. is the sampling constant, corresponding to the weight of sample required to limit the sampling uncertainty to 1% with 68% confidence. The magnitude of Ks may he determined by estimating ss from a series of measurements of samples of weight W” Kratochvil , An.Chem. 1981
23
![Page 24: CHIMICA ANALITICA II - units.it · 2016. 10. 9. · ASTM E300 -03(2009) Standard Practice for Sampling Industrial Chemicals Representative samples of industrial chemicals are required](https://reader035.vdocument.in/reader035/viewer/2022071416/611379d382fd096091162f68/html5/thumbnails/24.jpg)
24