Riflettanza Diffusa nell'IR (DRIFT) applicata all'adsorbimento di inquinanti atmosferici su TiO2
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(5) INDICE Introduzione Scopo. 1 2 PARTE I: TEORIA. 1 CLOROTRIFLUOROETILENE E TRIFLUOROETILENE 1.1 Generalità sulle molecole 1.2 Chimica atmosferica 1.3 Effetti sulla salute. 3 3 5 5. 2 ANIDRIDE SOLFOROSA 2.1 Generalità sulla molecola 2.2 Sorgenti di SO2 2.3 Chimica atmosferica 2.4 Effetti sulla salute. 7 7 8 8 9. 3 OSSIDO NITROSO 3.1 Generalità sulla molecola 3.2 Sorgenti di N2O 3.3 Chimica atmosferica 3.4 Effetti sulla salute. 12 12 13 13 14. 4 VIBRAZIONI MOLECOLARI 4.1 Approssimazione armonica 4.2 Anarmonicità 4.3 Risonanza di Fermi 4.4 Applicazioni alla catalisi eterogenea. 16 16 18 20 21. 5 ADSORBIMENTO GAS-SOLIDO 5.1 Superfici dei solidi 5.2 Adsorbimento 5.3 Biossido di Titanio TiO2 5.4 Chimica Superficiale 5.5 Applicazioni TiO2. 23 23 25 26 27 29. 6 SIMULAZIONE COMPUTAZIONALE 6.1 Equazione di Schrödinger 6.2 Approssimazione di Born-Oppenheimer 6.3 Teoria Hartree-Fock 6.4 Teoria del Funzionale di Densità 6.5 Sistemi Periodici 6.6 Basis Set 6.7 BSSE 6.8 Ottimizzazione Geometrica e Calcolo delle Frequenze 6.9 Approcci all’Adsorbimento. 33 33 34 35 39 43 46 47 47 49.
(6) PARTE II: LAVORO SPERIMENTALE 7 STRUMENTAZIONE E PROCEDURA SPERIMENTALE 7.1 Spettroscopia in Trasformata di Fourier (FTS) nell’infrarosso 7.2 Riflettanza Diffusa (DR) 7.3 Configurazione Strumentale 7.4 Procedura Sperimentale 7.5 Validazione metodo 7.6 Prodotti Utilizzati. 52 52 56 57 61 64 74. 8 ADSORBIMENTO C2F3Cl. 76. 9 ADSORBIMENTO C2F3H. 85. 10 ADSORBIMENTO SO2. 96. 11 ADSORBIMENTO N2O. 108. Conclusioni. 117.
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
(15) A01375661. B18=05. X&0:&(),/()$5+$Y;1**+?+1'&$9X;1+*<. !ZO"#S$[. X&0:&(),/()$5+$\/.+1'&$9X6/.<. !QQ"WS$[. X&0:&(),/()$G(+,+2)$9X 2<. NOQ"ON$[. Y',)*:+)$5+$61(0)?+1'&$.,)'5)(5$9] 6^T8).<. _!RZ"`N$ab$01*_#. X&0:&(),/()$)*$:/',+$,(+:*1$9X,(<. #RW"ZN$[. c(&..+1'&$)*$:/',1$,(+:*1$9c,(<. Q"Q#ZW$;)(. ?1@5881"!J$5),+$2@+0+21_6+.+2+$(+*&A)',+$:&($KL!$HO>NIU$. $!"!$$K1(8&',+$5+$KL$!$HSI 3=&0+..+1'& $ 5+ $ )'+5(+5& $ .1*61(1.) $ '&**=)0;+&',& $ :/F$ &..&(& $ 2*)..+6+2),) $ ./**) $ ;).& $ 5&* $ 8&'&(& $ 5+ &0+..+1'&J$)',(1:+2)$1$'),/()*&"$ 3& $.1(8&',+ $'),/()*+ $5+ $KL! $.1'1 $+$ 2)0+'+$ A/*2)'+2+>$+* $0),&(+)*& $1(8)'+21$+'$5&210:1.+?+1'& $& *=1..+5)?+1'& $ 5+ $ 5+0&,+*.1*6/(1 $ &0&..1 $ 5)**=12&)'1" $ K&;;&'& $ *& $ &(/?+1'+ $ A/*2)'+2@& $ '1' $ .+)'1 :)(,+21*)(0&',& $6(&V/&',+>$&..&$(+0)'81'1$/')$5&**&$61',+$'),/()*+$:(+'2+:)*+$5+$KL !"$c&($V/)',1 21'2&('& $ +* $ 0),&(+)*& $ 1(8)'+21> $ &..1 $ 7 $ /') $ .1(8&',& $ 5+ $ )'+5(+5& $ .1*61(1.) $ +'5+(&,,1J $ *) 5&210:1.+?+1'&$./*$,&((&'1$15$+'$0)(&$:1(,)$)*$(+*).2+1$5+$^ !K$2@&$51:1$:12@&$1(&$A+&'&$1..+5),1$& :1(,)$)**)$61(0)?+1'&$5+$KL!"$ 3&$.1(8&',+$)',(1:+2@&$21',(+;/+.21'1$)**=&0+..+1'&$,)',1$V/)',1$V/&**&$'),/()*+$&$.1'1$+5&',+6+2),& '&**)$210;/.,+1'&$5+$2)(;/()',+$61..+*+$ 9:&($+*$WS_`Sd$5&*$,1,)*&<>$'&*$(&6+'+'8$:&,(1*+6&(1$&$'&**& 6/.+1'+ $ $ 0&,)**/(8+2@&" $ K+ $ .,+0) $ 2@& $ +* $ ROd $ 5&**=&0+..+1'& $ )',(1:+2) $ 5+ $ KL ! $.+) $ 5) $ +0:/,)(& )**=&0+.6&(1$;1(&)*&". $!"O$$G@+0+2)$e,01.6&(+2)$HSI f1:1 $ 2@& $ *=)'+5(+5& $ .1*61(1.) $ 7 $ .,),) $ (+*).2+),) $ '&**=)0;+&',& $ A)(+ $ :(12&..+ $ :(&'51'1 $ :+&5&> :1(,)'51'& $ )**) $ 21'A&(.+1'& $ &g1 $ (+01?+1'& $ 5)**=),01.6&()J $ 1..+5)?+1'&> $ E&,_5(h $ 5&:1.+,+1' $ &5 )5.1(;+0&',1$5)$:)(,&$5&*$./1*1$&$5+$A&8&,)*+" $i$ .,),1$.,+0),1$2@&$+*$#Qd$5&*$8).$&0&..1$A+&'& (+01..1$:&($0&??1$5+$1..+5)?+1'&$)$.1*6),1$&5$)2+51$.1*61(+21>$0&',(&$+$0&22)'+.0+$:(&510+')',+ .1'1$*)$E&,$1$5(h$5&:1.+,+1'$&$*=)5.1(;+0&',1"$$ C*$:(12&..1$5+ $1..+5)?+1'&$:/F$)A&(&$*/181 $+'$0151$1018&'&1$+'$6).&$8)..1.)$&$*+V/+5)>$1::/(& &,&(18&'&)0&',&$./**)$./:&(6+2+&$5+$:)(,+21*),1>$,/,,)A+)$7$:1..+;+*&$/')$2100+.,+1'&$5+$V/&.,&$,(& 015)*+,-"$3=1..+5)?+1'&$+'$6).&$8)..1.)$:/F$)AA&'+(&$,()0+,&$,(&$5+A&(.+$0&22)'+.0+"$C*$:(+01$A&5& 21+'A1*,+ $ +',&(0&5+ $ (&),,+A+ $ 8&'&(),+ $ 61,12@+0+2)0&',&> $ +* $ :+j $ +0:1(,)',& $ 5&+ $ V/)*+ $ 7 $ +* $ ()5+2)*& +5(1..+*+21>$.&21'51$*)$.&8/&',&$(&)?+1'&J$ $$$. `.
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
(18) rCr3CL%se\Ce H#I$He5A)'2&5$C'1(8)'+2$G@&0+.,(h>$\"$e"$G1,,1'$&,$%"$t+*a+'.1'>$#RW!$OuY5>$b1@'$t+*&h$v$K1'.I H!I$Hb1/(')*$16$G@&0+2)*$c@h.+2.>$G"^"$^1*5&($&,$)*">$#R`#>$::$SO!O_SO!S>$WSI HOI"HlCKX$G@&0+.,(h$t&;r11a>"@,,:JggE&;;11a"'+.,"81Ag2@&0+.,(hg>$!Q#QI HNI$HK2@&5)$5+$K+2/(&??)$KCef>$@,,:JggEEE".+)5"210g512.w.+)5w+,)gkK##O":56>$!QQZI HSI$HK/*:@/($f+1x+5&J$&'A+(1'0&',)*$&66&2,.>$6),&$)'5$;&@)A+1/(> $$$$$$$@,,:Jgg&'A+(1'0&',"81A");"2)g+'61g*+;()(hgZZ#S":56I. ##.
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(20) A6-192..-. B-:062. ]&0;&(),/()$5+$^T1**+<+1'&$F]T1+*M. #B[$_. ]&0;&(),/()$5+$O/.+1'&$F]A/.M. $#B!$_. ]&0;&(),/()$E(+,+2)$F] 2M. !CJ$_. ^',)*;+)$5+$A1(0)<+1'&$.,)'5)(5$F` A\D>).M. B79C[$ab$01*Y#. (-?2::-"@@$5),+$2:+0+21YA+.+2+$(+*&H)',+$;&($678$KQ9[LX$. c5$&*&H),)$,&0;&(),/()$*)$01*&21*)$.+$5&210;1'&$+'$67$&5$87$$&$W/&.,)$(&)<+1'&$H+&'&$.A(/,,),)$'&**) .1H()*+0&',)<+1'&$2:+0+2)$5&+$01,1(+$)$.21;;+1"$34)(+)$=$21.,+,/+,)$5)*$7Cd$+'$;&.1$5+$1..+>&'19 0&',(& $ +* $ ;(1,1..+51 $ 5+ $ )<1,1 $ 5)* $ !Id@ $ *46 78 $ +00&..1$ '&* $ 01,1(& $ A1('+.2& $ +* $ #Id $ +' $ ;&.1 $ 5+ 1..+>&'1$+'$;+Z$;&($*)$210T/.,+1'&9$;1(,)'51$)5$/'$+'2(&0&',1$5+$2)H)**+$A+'1$)*$[CYICd"$e/&.,1 )221(>+0&',1$A/$&.21>+,),1$5/()',&$*)$.&21'5)$>/&(()$01'5+)*& $;&($+$01,1(+$5&>*+ $)&(1;*)'+$5) 210T),,+0&',1$KIL". $!"7$$P1(>&',+$5+$6$78$KfL 34&0+..+1'&$5+$678$'&**4),01.A&()$=$2*)..+A+2)T+*&$./**)$T).&$5&**)$./)$1(+>+'&9$)',(1;+2)$1$'),/()*&" S*$21',(+T/,1$)',(1;+21$)**41..+51$'+,(1.1$;(1H+&'&$5)$5+H&(.&$A1',+@$*)$210T/.,+1'&$5+$2)(T/()',+ A1..+*+ $ 5- $ 210& $ ;(151,,1 $ ;(1;(+1 $ W/&.,1 $ >).9 $ )'2:& $ .& $ +* $ H1*/0& $ &0&..1 $ 5+;&'5& $ 5)* $ ,+;1 $ 5+ 210T/.,+T+*& $21+'H1*,1X $*&$0)(0+,,&$2),)*+,+2:&$;1..1'1$;(10/1H&('&$*)$A1(0)<+1'&9 $0)$(&2&',+ .H+*/;;+$.,)''1$+'H&(,&'51$,)*&$,&'5&'<)"$341..+5)<+1'&$2),)*+,+2)$5+$6\!$'&**)$;(15/<+1'&$5+$)2+51 '+,(+21$5-$210&$.1,,1;(151,,1$6789$2:&$H+&'&$)**1',)'),1$&$(+*).2+),1X$+*$;(1,1..+51$54)<1,1$=$.2)(,1 )'2:&$5&**)$.+',&.+$5+$)2+51$)5+;+219$/,+*+<<),1$;&($;(15/((&$'g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d$5&**41..+51$'+,(1.1"$S*$(&.,)',&$7Cd$(&)>+.2&$21'$*48$;(151,,1@ $. #!.
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