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Atmospheric Pressure Chemical Ionization Tandem Mass Spectrometry (APGC/MS/MS) an Alternative to High Resolution Mass Spectrometry (HRGC/HRMS) for the Determination of Dioxins

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(4) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. '!". GHI?JKL7IGJH,,. '#". J=74=6" 740" C_WI" S2:?2,Q" jL11011Q067" :<" WV=17=6?" 5,S,3=7@" ,6>" 5,S,3=7@" NH=;>=6?". '$". _00>1" 7:" L6,;@`0" I^I1" =6" U0D0;:S=6?" 5:H672=01k" 10D02,;" ,37=D=7=01" E020" H6>027,e06". '%". >H2=6?" 740" S02=:>" <2:Q" #++'" 7:" #+!+F".4=1" S2:?2,Q" =1" <:3H10>":6" 740" >0D0;:SQ067":<"". '&". ,6,;@7=3,;" 3,S,3=7@" <:2" 740" I^I1" H6>02" 740" 97:3e4:;Q" 5:6D067=:6" =63;H>=6?" 10D02,;". ''". S017=3=>01" KUU.8" 34;:2>,608" 7:V,S4060M" ,6>" =6>H172=,;" KB@MYS2:>H371" K>=:V=618" I5N1MF". '(". /03067;@"B2:Q=6,70>"<;,Q0"207,2>,671"KINUWM",6>",6":2?,6=3"<;H:2"3:QS:H6>"KI[^9M". ')". E020",>>0>"7:"740"3:6D067=:6F"^60":<"740"3:63;H1=:61":<"740"S2:?2,Q"E,1"74,7"=7"=1"aH=70". '*". ,"34,;;06?0"7:",6,;@`0",;;"I^I1"=6"740"1,QS;0"7@S01"S2:S:10>"<:2"740"?;:B,;"Q:6=7:2=6?". (+". S2:?2,Q" KZ-IM!8#F" .4=1" =1" 01S03=,;;@" 72H0" <:2" >0D0;:S=6?" 3:H672=01F" ^60" :<" 740". (!". >=<<=3H;7=01" 7:" >0D0;:S" ," H6=D021,;" Q074:>" <:2" 740" 97:3e4:;Q" 3:6D067=:6" I^I1" =1" 74,7". (#". B:74" T5" ,6>" Z5" 4,D0" 7:" B0" H10>" <:2" 10S,2,7=:6F" L;74:H?4" ,Q:6?" 740" 60E;@" ,>>0>". ($". 3:QS:H6>1" 7:" 740" 97:3e4:;Q" 3:6D067=:68" I[^9" =1" 2:H7=60;@" ,6,;@`0>" B@" T5O-98" 740". (%". Q:17"S2:B;0Q,7=3"3:QS:H6>1":6"740"97:3e4:;Q"3:6D067=:6"7:"B0",6,;@`0>",20">=:V=61F". (&". .:" ,34=0D0" 06:H?4" 1061=7=D=7@" ,6>" 10;037=D=7@" >=:V=61" ,20" 2:H7=60;@" ,6,;@`0>" B@" H1=6?". ('". 4=?4" 201:;H7=:6" Z5" 3:HS;0>" 7:" 4=?4" 201:;H7=:6" -98" =6172HQ067,7=:6" E4=34" =1" B:74". ((". 0VS061=D0",6>"3:QS;0V"0;,B:2,70"7:"Q,=67,=6F". ()". U=:V=61" ,6,;@1=1" =1" Q:17" 3:QQ:6;@" 3,22=0>" :H7" H1=6?" 4=?4" 201:;H7=:6" Z5O-9" H1=6?". (*". Q,?607=3"1037:2"-9"=6172HQ067,7=:6":S02,70>"=6"WGl"Q:>0F".4=1"70346=aH08"0D06"E406". )+". H10>",7";:E02"=:6=`,7=:6"0602?=01"Km$&0\M"201H;71"=6"1=?6=<=3,67"<2,?Q067,7=:6"20>H3=6?". )!". 740" =67061=7@" :<" 740" Q:;03H;,2" =:6" K-nlMF" .@S=3,;" 340Q=3,;" =:6=`,7=:6" K5GM" S2:>H301". )#". 1:<702" =:6=`,7=:68" E=74" ,6" 0602?@" 72,61<02" 74,7" ?0602,;;@" =1" ;:E02" ,6>" >:01" 6:7" 0V300>". )$". &0\F" _:2Q,;;@" 5G" Q,11" 1S0372," 0V4=B=7" ;011" <2,?Q067" =:61" 74,6" =6" WGF" 5G" =1" 7@S=3,;;@". )%". S2:>H30>"H6>02"D,3HHQ"3:6>=7=:61"H1=6?",6"=:6=`,7=:6"?,1"E4=34"<=;;1"740"=:6"1:H230F"G7" %" ". ACS Paragon Plus Environment. Page 4 of 27.

(5) Page 5 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. )&". =1" 20172=370>" 7:" 1S03=<=3" 340Q=3,;" 3;,1101$8%8&" 1=630" =7" =1" 6:7" ,1" ,6" H6=D021,;" =:6=`,7=:6". )'". Q034,6=1Q" ,1" WG" =<" 6:" 0V720Q0" 20,?0671" ,20" H10>F" J406" H1=6?" 5G" 3:6>=7=:61" <:2" 740". )(". =:6=`,7=:6":<">=:V=61":<706"0;0372:6"3,S7H20"340Q=3,;"=:6=`,7=:6"K_5GM":33H218"201H;7=6?". ))". =6";:11":<"=67061=7@":<"740"Q:;03H;,2"=:6F".40"=QS:27,630":<",6",BH6>,67"Q:;03H;,2"Q,11". )*". S0,e" :<" 740" ,6,;@70" =1" 01S03=,;;@" =QS:27,67" <:2" 740" >0D0;:SQ067" :<" -9O-9" B,10>". *+". Q074:>1F".40"10;037=:6":<",>0aH,70"S203H21:2"=:61",6>"740"1HB10aH067",SS;=3,7=:6":<"740". *!". -/-"Q:>0"064,630"10;037=D=7@",6>"1061=7=D=7@8"Q=6=Q=`=6?":2"0D06"0;=Q=6,7=6?"Q,72=V". *#". =6702<0206301F"J406"740"Q:;03H;,2"=:6"=1",B1067":2"=7"4,1"D02@";:E",BH6>,6308"=7"Q=?47". *$". B0"603011,2@"7:"10;037","K,BH6>,67M"<2,?Q067"=:6",1"S203H21:2"=:68"E=74";:E02"QO`",6>"=6". *%". Q:17"3,101";011"3:QS:H6>"34,2,3702=17=3F".4H18"=6",>>=7=:6"7:"740";:11":<"1061=7=D=7@8"740". *&". 1S03=<=3=7@" :<" 740" Q074:>" 3,6" ,;1:" B0" ,<<0370>" ,6>" ;:1=6?" 740" S:7067=,;" ,>D,67,?01" :<". *'". 7,6>0Q" -9F" L" 1:<7" ,6>" H6=D021,;" =:6=`,7=:6" 70346=aH0" ,B;0" 7:" S2:D=>0" ,BH6>,67". *(". Q:;03H;,2"=:61"7:"B0"H10>",1"S203H21:2"=:61"=6"QH;7="201=>H0"Z5o-9",6,;@1=1"E:H;>"B0". *)". ," 170S" <:2E,2>" E406" H1=6?" -9O-9F" G6" 74=1" E,@8" 740" ;:EY0602?@" K1:<7M" =:6=`,7=:6". **". Q034,6=1Q" :33H22=6?" =6" 740" LIZ5" 1:H230" ?0602,701" 1S0372,;" >,7," 7@S=3,;;@" 2=34" =6". !++". Q:;03H;,2" :2" S2:7:6,70>" Q:;03H;0" =:6" =6<:2Q,7=:6'F" N03,H10" :<" 740" 20>H30>". !+!". <2,?Q067,7=:6" E406" H1=6?" LI5G8" 740" 10;037=:6" :<" 740" S203H21:2" =:6" =1" 6:" ;:6?02" ,". !+#". 3:QS2:Q=10" B07E006" 10;037=D=7@" ,6>" 1061=7=D=7@" E406" >0D0;:S=6?" ," -9O-9" B,10>". !+$". Q074:>F". !+%". L7Q:1S402=3" S2011H20" =:6=`,7=:6" =6" Z5o-9" E,1" <=217"=672:>H30>" B@" b:26=6?" 07" ,;F(" =6". !+&". 740" 0,2;@" !*(+" H1=6?" ," '$_=" 3:2:6," >=134,2?0" 600>;0" 7:" <:2Q" =:61" :<" 740" 7,2?07". !+'". 3:QS:H6>1":2">=<<02067"20,?0671)F"/0;,7=D0;@"1::6",<7028"74=1"70346=aH0"E,1"H10>"<:2"740". !+(". LI5G" ,6,;@1=1" :<" >=:V=61" B@" b:26=6?" 07" ,;F*8" 9=0?0;" ,6>" -3]0:E6!+" ,6>" -=734HQ" 07". !+)". ,;F!!"E4:" ,;;" H10>" 740" '$_=" 1:H230" 7:" =:6=`0" #8$8(8)Y.05UU" ,7" ,7Q:1S402=3"3:6>=7=:61F". !+*". L;1:8"H1=6?"740"'$_="1:H2308"-=734HQ",6>"97,;;=6?!#"E020",B;0"7:",6,;@`0",;;"##"=1:Q02=3" &" ". ACS Paragon Plus Environment.

(6) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. !!+". 7072,Y>=:V=61F" .40" >07037=:6" ;=Q=71" 4:E0D02" E020" 20;,7=D0;@" 4=?4" D,2@=6?" <2:Q" '+Y$++". !!!". SS7" ,6>" ,;74:H?4" 1:Q0" 10;037=D=7@" E,1" ,34=0D0>" B@" H1=6?" >=<<02067" 20,?06718" LI5G" ,7". !!#". 74,7" 7=Q0" E,1" B@" <,2" ;011" 10;037=D0" ,6>" ;011" 1061=7=D0" 74,6" 4=?4" 201:;H7=:6" Z5O-9". !!$". 1@170Q1" E4=34" B03,Q0" 740" S20<0220>" Q074:>:;:?@" <:2" >=:V=6" ,6,;@1=1!$F" 9HB10aH067". !!%". Q:>=<=3,7=:61"E020">0132=B0>"=6"740")+1!%8!&8"BH7"740"70346=aH0"E,1"60D02"=QS;0Q0670>". !!&". <:2"3:QQ:6"2:H7=60",6,;@1=1F". !!'". /03067;@8" LI5G" 4,1" Q,>0" ," 20D=D,;" E406" ," 60E" 1:H230" H1=6?" 6=72:?06" SH2?0" ?,1" E,1". !!(". >0D0;:S0>" ,6>" 3:QQ023=,;=`0>!'8!(8!)F" L;74:H?4" 6:7" E=>0;@" ,SS;=0>8" =7" :<<021" ,772,37=D0". !!)". ,6,;@7=3,;" 3,S,B=;=7=01" <:2" Z5o-9O-9" ,6,;@1=1" ,6>" 4,1" B006" H10>" =6" >=<<02067" <=0;>18". !!*". =63;H>=6?" S017=3=>0" 201=>H0" ,6,;@1=1!*8" S4,2Q,30H7=3,;1" >0D0;:SQ067#+8" S2:<=;=6?" :<". !#+". S406:;=3"3:QS:H6>1"=6":=;#!",6>"Q07,B:;=3"S2:<=;=6?##F"LIZ5"E,1"203067;@"1H33011<H;;@". !#!". H10>" <:2" 740" ,6,;@1=1" :<" Q:20" 74,6" !++" >=<<02067" S017=3=>0" 201=>H01" B@" I:27:;01" 07" ,;F'". !##". H1=6?",6"=QS2:D0>"3:2:6,"600>;0">=134,2?0"1:H230F"LIZ5"Q,11"1S0372,"<:2"10D02,;":<". !#$". 740" I^I1" :6" 740" 97:3e4:;Q" 3:6D067=:6" 14:E0>" :6;@" ;=Q=70>" :2" 6:" <2,?Q067,7=:6". !#%". 1=?6=<=3,67;@"064,63=6?"740">07037=:6";=Q=71"<:2"3:QS:H6>1"1H34",1",;>2=68">=0;>2=6",6>". !#&". 06>:1H;<,6" E406" 3:QS,20>" 7:" 0;0372:6" =:6=`,7=:6" KWGM" E4020" 3:61=>02,B;0". !#'". <2,?Q067,7=:6" :33H220>" ,6>" 10;037=:6" :<" =:61" <:2" aH,67=<=3,7=:6" =6" 740" 9/-" Q:>0" =1". !#(". >=<<=3H;7F" W1S03=,;;@" <:2" I^I" -9O-9" ,SS;=3,7=:61" =7" =1" =QS:27,67" 7:" ?0602,70" ,1" QH34". !#)". Q:;03H;,2" =:6" :<" 740" Q:17" ,BH6>,67" =:61" :<" 740" 34;:2=60" 3;H1702" <:2" 1HB10aH067". !#*". <2,?Q067,7=:6F" [:2" =1:7:S0" >=;H7=:6" aH,67=<=3,7=:6" H1=6?" !$5" ;,B0;0>" 17,6>,2>18" 74=1" =1". !$+". S20<02,B;@"740"Q:;03H;,2"=:6F". !$!". .4=1" 14:E1" 74,7" 740" H10" :<" LIZ5" =1" ," S:11=B;0" E,@" <:2E,2>" =6" 740" >0D0;:SQ067" :<" ,". !$#". H6=D021,;" >07037=:6" 1@170Q" <:2" ,;;" 97:3e4:;Q" 3:6D067=:6" I^I1" B,10>" :6" Q,11". !$$". 1S0372:Q072@F"[:2">=:V=618"E4020"4=?4"201:;H7=:6"Z5O-9"1@170Q1",20":<706"20aH=20>"7:". !$%". ,D:=>" =6<0206301" ,6>" 7:" ,34=0D0" 740" 0V720Q0" ;:E" ;=Q=7" :<" >07037=:6" KT^UM" 600>0>" <:2" '" " ACS Paragon Plus Environment. Page 6 of 27.

(7) Page 7 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. !$&". <::>" ,6>" <00>#$8" ,=2" :2" 4HQ,6" 1,QS;018" LIZ5" 3:H;>" S:7067=,;;@" B0" ," D02@" ,772,37=D0". !$'". ,;7026,7=D08" :S06=6?" 740" E,@" <:2" ," H6=D021,;" Q,11" >07037:2" <:2" ,;;" I^I1" :6" 740". !$(". 97:3e4:;Q"3:6D067=:6"=63;H>=6?">=:V=61F"". !$)". .40" ,=Q" :<" 74=1" S,S02" =1" 7:" >0Q:6172,70" 740" 3,S,B=;=7=01" :<" LIZ5O-9O-9" K7,6>0Q". !$*". aH,>2HS:;0M"H1=6?","LI5G"B,10>"=:6"1:H230"<:2"740">0702Q=6,7=:6":<">=:V=61"=6","D,2=07@". !%+". :<"1,QS;01"=63;H>=6?"06D=2:6Q067,;8",=28"4HQ,6",6>"<::>"1,QS;0"0V72,371F". !%!". 9!IM?G!N,!HK,9MI>JK:,. !%#". 57KK8O,%".02.)2%,.02,:.#&/(%,,. !%$". WILY!'!$IL/",6>" .[Y.5UUY-pN" 17,6>,2>1" 1:;H7=:61"3:67,=6=6?" >=<<02067" Q=V7H201". !%%". :<" 6,7=D0" I5UUO[" 3:6?060218" WILY!'!$T59" ,6>" WILY!'!$G99" !$5Y;,B0;0>" I5UUO[". !%&". 17,6>,2>1" <:2" 1,QS;0" S20S,2,7=:68" ,1" E0;;" ,1" 3,;=B2,7=:6" 17,6>,2>1" " !'!$YWIL59T" 7:". !%'". !'!$YWIL59&8" E=74" B:74" 6,7=D0" ,6>" !$5Y;,B0;0>" I5UUO[" ,6>" .5UU" 1:;H7=:6" .[Y. !%(". .5UUY-pN8" E020" ,;;" :B7,=60>" <2:Q" J0;;=6?7:6" T,B:2,7:2=01" KZH0;S48" ^67,2=:8". !%)". 5,6,>,MF" 5027=<=0>" 20<020630" Q,702=,;1" N5/Y'+(" K6,7H2,;" Q=;e" S:E>02M8" N5/Y'((". !%*". K10E,?0"1;H>?0M8"N5/Y%*+",6>"N5/Y'!&"K<;@",14M"E020",3aH=20>"<2:Q"740"G617=7H70"<:2". !&+". /0<020630"-,702=,;1",6>"-0,1H20Q0671"KG/--M8"WH2:S0,6"5:QQ=11=:6YP:=67"/010,234". !&!". 506720"KZ00;8"N0;?=HQMF"G67026,;"20<020630"Q,702=,;1"K1S=e0>"<00>"1,QS;018"4HQ,6"B;::>". !&#". ,6>" 6,7H2,;;@" 3:67,Q=6,70>" <::>" ,6>" <00>" 1,QS;01M" <:2" 2:H7=60" aH,;=7@" 3:672:;OaH,;=7@". !&$". ,11H2,630" KhLOh5M" =6" 740" ;,B:2,7:2=01" ,6>" >=<<02067" Q,72=301" <2:Q" =67026,7=:6,;" =6702Y. !&%". ;,B:2,7:2@" 3:QS,2=1:6" 17H>=01" K<=14" 1,QS;0" <2:Q" 740" G6702;,B:2,7:2@" 5:QS,2=1:6" :6". !&&". I^I1"=6"[::>"#+!#"K!$74"/:H6>M8"_:2E0?=,6"G617=7H70":<"IHB;=3"b0,;74"K^1;:8"_:2E,@M". !&'". ,6>" I." 7017" 1,QS;01" <2:Q" S2:<=3=063@" 70171" :2?,6=`0>" B@" 740" WCY/T" <:2" U=:V=61" ,6>". !&(". I5N1"=6"[00>",6>"[::>M"E020",;1:"H10>"7:"3:QS,20"740"201H;71":6">=<<02067"=6172HQ0671F". !&)". L>>=7=:6,;;@8"10D02,;"S2:30>H2,;"B;,6e1"4,D0"B006",6,;@`0>"B:74"B@"b/-9",6>"LIZ5" (" ". ACS Paragon Plus Environment.

(8) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. !&*". <:2" ,;;" 1,QS;0" 7@S01F" L;;" B;,6e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qM":2"?0;"S02Q0,7=:6"342:Q,7:?2,S4@F"[H27402"1,QS;0"SH2=<=3,7=:6"E,1". !')". S02<:2Q0>"B@",6",H7:Q,70>"1@170Q"KI:E02"I20Sr8"[-9"G63F8"J,;74,Q8"-L8"C9LM8":2". !'*". ," Q,6H,;" 3;0,6" HS" H1=6?" ,6" ,;HQ=6," :V=>0" 3:;HQ6" 0;H70>" E=74" 40V,60" ,6>" ,". !(+". 40V,60O>=34;:2:Q074,60" Q=V7H20" :2" <;:2=1=;" 3:;HQ6" 0;H70>" E=74" 6Y40S7,60" ,6>" 7:;H060". !(!". <:;;:E0>" B@" ," 3,2B:6" 3:;HQ6" 0;H70>" E=74" 40V,60" ,6>"7:;H060F" .40" <=6,;"0V72,371" E020". !(#". 0=7402"<=6,;;@",6,;@`0>"B@"LIZ5O-9O-9":2"B:74"B@"LIZ5O-9O-9",6>"b/Z5Ob/-9F". !($". ,. !(%". G0%")-#(0"./,!0./3%*%,. !(&". F>.2T;CT;C%9?(B-$-?(<!. !('". [:H2" >=<<02067" LIZ5O-9O-9" 1@170Q1" E020" H10>" =6" 74=1" 17H>@" =6" <:H2" >=<<02067". !((". ;,B:2,7:2=01" ,7" J,70218" -,634017028" Z20,7" N2=7,=6i" GCIL8" 5,170;;:68" 9S,=6i" WC/T" <:2". !()". U=:V=61",6>"I5N18"[20=BH2?8"Z02Q,6@",6>"-.-8"A20B2:8"9E0>06F".40"B,1=3"107"HS":<". !(*". 740"=6172HQ067"E,1"1=Q=;,2"=6",;;"3,101F".40"Z5"1@170Q"3:61=170>":<",6"L?=;067"()*+L". !)+". KL?=;0678"I,;:"L;7:8"5L8"C9LM"0aH=SS0>"E=74",6",H7:"1,QS;02"KL?=;067"('*$MF".40"Z5". !)!". E,1" 3:HS;0>" 7:" ," aH,>2HS:;0" Q,11" 1S0372:Q0702" Kp0D:" .hY98" J,7021" 5:2S:2,7=:68". !)#". -,634017028" C]M8" 0aH=SS0>" E=74" ,6" LIZ5" =:6=`,7=:6" 1:H230F" [:2" >=:V=6" ,6,;@1=1" 740" )" ". ACS Paragon Plus Environment. Page 8 of 27.

(9) Page 9 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. !)$". Z5"E,1"0aH=SS0>"E=74"0=7402","1=;=3,"UNY&-9"KCGM"3,S=;;,2@"3:;HQ6"K'+"Q"s"+F#&"QQ". !)%". =>F"s"<=;Q"74=3e6011"+F#&"dQM"KPtJ"93=067=<=38"[:;1:Q8"5L8"C9LM":2","NIpY&"3,S=;;,2@". !)&". 3:;HQ6"K$+"Q"s"+F#&"QQ"=F>F8V"+F#&"QM"K9ZW"L6,;@7=3,;"93=06308"\=37:2=,8"LC9MF".40". !)'". =6c037:2"E,1":S02,70>"=6"1S;=7;011"Q:>08"=6c037=6?"!"dT",7"#)+"u5",7",;;"=6172HQ0671"B@". !)(". SH;10>" 1S;=7;011" =6c037=:6" H1=6?" ,6" =6=7=,;" S2011H20" :<" #%+" eI," :2" =6c037=6?" &" H;" =6" 740". !))". I.\"1:;D067"D067"Q:>0"KWC/T8"[20=BH2?MF"".40"=6702<,30"70QS02,7H20"E,1"107"7:"#)+Y. !)*". $'+" u5" H1=6?" _#" K<2:Q" ?,1" 3@;=6>028" aH,;=7@" v" **F***+qM" ,1" Q,e0YHS" ?,1" ,7" !&+Y$(+". !*+". QTOQ=6" =6" 740" 3:617,67" <;:E" Q:>0" >0S06>=6?" :6" 740" =6172HQ067F" L1" ,HV=;=,2@" ?,1" _#". !*!". K<2:Q";=aH=>"_#8" 6=72:?06"?0602,7:2":2"?,1"3@;=6>02M"E,1"H10>",7"#&+Y$++"TO4"E=74"7HB0". !*#". 7:" E,170" :2" #++" TO4" E=74:H7" 7HB0" 7:" E,170F" .40" 3:60" ?,1" E,1" H10>" 7:" :S7=Q=`0" 740". !*$". =:6=`,7=:68" ,6>" 107" ,7" !(+Y#++" TO4" E406" 740" 3:QS,2=1:6" E,1" Q,>0" B07E006" ,;;" <:H2". !*%". =6172HQ0671F".40"LI5G"3:2:6,"S=6"E,1":S02,70>"B07E006"!F)",6>"#F!"dLF".40"=:6=`,7=:6". !*&". S2:3011" :33H220>" E=74=6" ," 3;:10>" =:6" D:;HQ08" E4=34" 06,B;0>" 3:672:;" :D02" 740". !*'". S2:7:6,7=:6O34,2?0"72,61<02"S2:301101F"". !*(". hH,67=7,7=D0",6,;@1=1"E,1"S02<:2Q0>"=6"740"QH;7=S;0"20,37=:6"Q:6=7:2=6?"Q:>0"K-/-M". !*)". B@" Q:6=7:2=6?" 7E:" 72,61=7=:61" <:2" 0,34" :<" 740" 6,7=D0" I5UUO[" 3:6?06021" ,6>" 740=2". !**". 3:2201S:6>=6?" !$5Y;,B0;0>" ,6,;:?H01F" .40"Q:;03H;,2" =:6" w-nlx"E,1" ,;E,@1" 10;0370>" ,1". #++". S203H21:2" =:6" <:2" ,;;" 3:QS:H6>1" K3:6?06021" ,6>" !$5" ,6,;:?H01M" ,6>" <2,?Q0670>" B@". #+!". 3:;;=1=:6"=6"740".YE,D0"3:;;=1=:6"30;;F".40">,7,"E020"S2:30110>"H1=6?"740"aH,67=<=3,7=:6". #+#". ,SS;=3,7=:6" Q,6,?02" .,2?07T@6V.-" E4=34" ,H7:Q,701" >,7," ,3aH=1=7=:68" S2:3011=6?" ,6>". #+$". 20S:27=6?" <:2" aH,67=7,7=D0" 201H;71F" G7" =63:2S:2,701" ," 2,6?0" :<" 3:6<=2Q,7:2@" 3403e1" 74,7". #+%". =>067=<@"1,QS;01"74,7"<,;;":H71=>0"H102Y1S03=<=0>":2"20?H;,7:2@"742014:;>1F"L"1HQQ,2@":<". #+&". 740" 0VS02=Q067,;" 3:6>=7=:61" =6" 740" >=<<02067" ;,B:2,7:2=01" =1" ?=D06" =6" I.C/(, PF" .40". #+'". -9O-9"3:6>=7=:61" E020"7,e06" <2:Q" 740" ;=702,7H20#'8#(" ,6>" :S7=Q=`0>"E406" 600>0>",6>". #+(". ,20"?=D06"=6"I.C/(,QF". #+)". *" ". ACS Paragon Plus Environment.

(10) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. #+*". ?M:LNI:,!HK,KG:7L::GJH,. #!+". G$0*1."*$0,$&"*#*1."*$0,. #!!". .40" =:6=`,7=:6" =6" 740" LIZ5" Q:>0" E,1" :S7=Q=`0>" B@" H1=6?" 4=?4" 3:630672,7=:6". #!#". I5UUOI5U[" 17,6>,2>1" K59&8" #++" 6?OQT" <:2" .5UUM" E4=34" E020" =6c0370>" H6>02" <H;;". #!$". 13,6" 3:6>=7=:61F" .40" =:6=`,7=:6" H1=6?" LI5G" H6>02" 34,2?0Y72,61<02" 3:6>=7=:61" K6:" b#^". #!%". E,1" ,>>0>" 7:" 740" 1:H230M" 20D0,;0>" ,6" ,BH6>,67" S2010630" :<" 740" Q:;03H;,2" =:6" <:2" ,;;". #!&". 10D067006" #8$8(8)" 34;:2=60" 1HB17=7H70>" >=:V=61" ,6>" <H2,61F" .4=1" =1" =6" ?::>" ,?200Q067". #!'". E=74"203067"SHB;=3,7=:61'" 0VS;,=6=6?"740"=:6=`,7=:6"Q034,6=1Q"<:2"LI5GF"".40"6=72:?06". #!(". S;,1Q,"K_#l",6>"_%lM"320,70>"B@"740"3:2:6,">=134,2?0"600>;0"=:6=`01"Q:;03H;01"@=0;>=6?". #!)". 7@S=3,;;@"-nlF".40"S2:7:6,70>"Q:;03H;0"w-lbxl"3,6"B0",;1:"S201067"=6"740"1S0372HQ">H0". #!*". 7:"740"S2010630":<"E,702"D,S:2"72,301"=6"740"1:H2308"74=1"3:QS07=6?"Q034,6=1Q"20>H301". ##+". 740"=67061=7@":<"740"Q:;03H;,2"=:6F".40"=:6=`,7=:6"H6>02"S2:7:6Y72,61<02"3:6>=7=:61"E,1". ##!". 70170>" B@" =672:>H3=6?" E,702" ,1" Q:>=<=02" =6" 740" LI5G" 1:H230" K,6" H63,SS0>" D=,;" E=74". ###". E,702" E,1" S;,30>" =6" ," 1S03=,;;@" >01=?60>" 4:;>02" S;,30>" =6" 740" 1:H230" >::2MF"b:E0D028". ##$". 6:60":<"740"7072,Y"7:":37,Y34;:2=6,70>">=:V=61":2"<H2,61"14:E0>"QH34"S2:7:6,7=:68"74=1"=1". ##%". 0V0QS;=<=0>" =6" O*=-)(, P" E4=34" 14:E1" 740" =:6=`,7=:6" B04,D=:2" :<" ^5U[" E=74" ,6>". ##&". E=74:H7"E,702",>>0>"7:"740"1:H230F"G7"3,6"3;0,2;@"B0"1006"74,7"=:6=`,7=:6"E4=34"=1"3,22=0>". ##'". :H7":6;@"E=74"_#" K34,2?0"72,61<02M"=1"Q:20"0<<037=D0"K=6"702Q1":<"201S:610M",6>"740"QO`". ##(". %%%"S203H21:2"201H;70>"=6"4=?402"1S0372,;",BH6>,630"E=74:H7"H1=6?"E,702",1"Q:>=<=02",6>". ##)". 20>H3=6?"S2:7:6"72,61<02",1"QH34",1"S:11=B;0F"[:2"740"3:67=6H,7=:6":<"740">0D0;:SQ067". ##*". :<" ," Q074:>" <:2" I5UUOU[1" ,6,;@1=1" 34,2?0" 72,61<02" 3:6>=7=:61" E020" H10>F" L" 1=QS;0". #$+". 3403e" 7:" 100" =<" S2:7:6,7=:6" :33H21" =1" 740" ,6,;@1=1" :<" S406,6742060" ,6>" 3:QS,2=6?" 740". #$!". ,BH6>,630" :<" QO`" !()" K34,2?0" 72,61<02M" ,6>" QO`" !(*" KS2:7:6,7=:6M8" <:2" 74=1" 20;,7=D0;@". #$#". 0,1@"S2:7:6,70>"3:QS:H6>"740"S2:7:6,70>"=:6"14:H;>"6:7"0V300>"$+qF". #$$". " !+" ". ACS Paragon Plus Environment. Page 10 of 27.

(11) Page 11 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. #$%". J&"*#*1."*$0,$@,"'(,+$0(,<$/".=(,. #$&". .40" 3:60" D:;7,?0" E,1" :S7=Q=`0>" <:2" 0,34" I5UUO[" B@" 7017=6?" D,;H01" B07E006" #+" ,6>". #$'". (+\" =6" :2>02" 7:" :B7,=6" 740" B017" 1061=7=D=7@F" L;74:H?4" 6:" 1=?6=<=3,67" >=<<0206301" E020". #$(". :B102D0>8" 1;=?47;@" 4=?402" 201S:610" <,37:21" E020" :B7,=60>" ,7" $+\" K01S03=,;;@" 3:QS,20>". #$)". E=74"(+\M",6>"74H1","3:60"D:;7,?0":<"$+\"E,1"H10>"<:2"Q:17":<"740"0VS02=Q0671"34:106F". #$*". .40":S7=Q=`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`,7=:6"740">=<<02067"?,1"<;:E1"=67:"740". #%(". 1:H230F". #%)". ". #%*". 9?9,#("'$2". #&+". [=217;@8" S2:>H37" =:6" 13,6" 0VS02=Q0671" E020" S02<:2Q0>" =6" :2>02" 7:" <=6>" 10;037=D0". #&!". 72,61=7=:61"B,10>":6"740"H10":<"-nl",1"S203H21:2"=:6F"U=<<02067"3:;;=1=:6"0602?=01"K!+8"#+8". #&#". $+8"%+",6>"&+"0\M"E020"70170>",6>"740"Q:17"1061=7=D0"72,61=7=:61"E020"10;0370>"<:2"740". #&$". >0D0;:SQ067" :<" 740" 1HB10aH067" -/-" Q074:>F" 5:;;=1=:6" 0602?=01" :<" $+" 0\" E020". #&%". 10;0370>" <:2" ,;;" 740" .5UU1" ,6>" D,;H01" :<" %+" 0\" E020" 10;0370>" <:2" 740" .5U[1F" T:E02". #&&". 0602?=01" ;0>" 7:" 60,2;@" ,B10630" :<" S2:>H37" =:61" ,6>" 7::" 4=?4" 0602?=01" ;0>" 7:" 0V3011". #&'". <2,?Q067,7=:6",6>"74020<:20";:E02"1061=7=D=7@"L7";:E"3:;;=1=:6"0602?=01"740"S2:>H37"=:6". #&(". 1S0372HQ"=1">:Q=6,70>"B@"740" $&5;";:118"BH7",7"740"<=6,;":S7=QHQ"3:;;=1=:6"0602?=01"740". #&)". 72,61=7=:61"10;0370>"3:2201S:6>0>"7:"740";:11":<"w5^$&5;x"KO*=-)(,:PMF".4=1"<2,?Q067"=1" !!" ". ACS Paragon Plus Environment.

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(16) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. $&*". !7DHJVNMK6M9MHI,. $'+". .40" ,H74:21" ,;1:" ,3e6:E;0>?0" 740" <=6,63=,;" 1HSS:27" :<" Z0602,;=7,7" \,;063=,6,8" ,1". $'!". 2010,234" ?2:HS" :<" 0V30;;0630" I/^-W.W^O#++*O+&%" ,6>" ,;1:" 740" 902D0=1" 50672,;1". $'#". >kG6172HQ067,3=R"5=067~<=3,"K95G5M":<"740"C6=D021=7@"P,HQ0"G"<:2"740"H10":<"Z5YKLI5GY. $'$". hahMY-9O-9F"U,E0="Z06?"=1"1HSS:270>"B@"740"54=6,"934:;,214=S"5:H63=;"KZ2,67"_:F". $'%". #+!#+'%++++$MF. !'" ". ACS Paragon Plus Environment. Page 16 of 27.

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(20) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. $))". ?(@()(0+(%, """""""""""""""""""""""""""""""""""""""" """""""". !. "\,6"T00HE068"9FIFPFi"07",;F"=#F2"QXPRY"]^*"!*)Y#+'S". ". #. "T01;=08"bFLFi"07",;F"=#F2"QXPRY"]^*")&Y*F". ". $. "LQ06>:;,8"TFi"07",;F"F(')S%23-6S%F9$'"QXXQ"8%'!8"*(Y!+)F". ". %. "94068"5Fi"07",;F8"=')'($'"QXPPY")%8"!%!Y!%(F". ". &. "ZH:8"hFi"07",;F"5S%F\F2%P($F"QXPX8"*$8"#*&Y$+&F". ". '. "I:27:;018".Fi"07",;F"5S%;'<<%CW"9$#?6F"QXPX8"%&8"*#'Y*$'F". ". (. "b:26=6?8"WF"5Fi"07",;F"F(')S%23"6F8"PZ[R8"%&8"*$'Y*%$F". ". ). "U`=>=38"GFi"07",;F"F(')S%23"6F"PZ[UY,%)8,!('$Y!(')F" "" ! "b:26=6?8"WF"5Fi"5,22:;;8"UF"GFi"U`=>=38"GF"2)-(S%23"6F"PZ[[8"#$8"!$Y#!F" " !+ "9=0?0;8"-F"JFi"-3]0:E68"-F"5F"5S%23#?6'$?/#F"PZ[U8"!##8"*(Y%!$F" " !! "-=734HQ8"/F"]Fi"-:;028"ZF"[Fi"]:2<Q,3402"JF"LF"F(')S%23"6F"PZ\X8"&#8"##()Y##)#F" " !# F-=734HQ8"/F"]Fi"07",;F"F(')S%23"6F"PZ\Q"8"&%8"(!*o(##F" " !$ "CF9F"W6D=2:6Q067,;"I2:7037=:6"L?063@F",,,S"W'S/?&"PZZS"!Y)*" ! !% "]:2<Q,34028"JF"LFi"07",;F"LH2%_%22F"PZ\[8"!+8"'%!Y'%'F" " !&" ]:2<Q,34028"JF"LFi"07",;F"LH2%_%22F"PZ\[Y,!+Y,%$Y%&F" " !' "934=0E0e8"/F"-Fi"07",;F"F(')S%!-?'(')S%23"6F"QXX\8"$*#8")(Y*'F" " !( "-3WE068"5F_F"G67F"PF"-,11"9S0372:QF"QXX[8"#&*8"&(Y'%F" " !) "-3WE068"5F_Fi"-3],@8"/F"ZF"5S%F6S%C?9S%;'<<%CW"9$#?6F"QXXTY,!'Y"!($+Y!($)F" " !* "54027,8"TFi"07",;F"5%23#?6'$?/#F"F"QXPR8"!$!%8"##%Y#%+F" " #+ "N2=17:E8".Fi"b,22=1:68"-Fi"9=Q18"-F"H'W-B%2?661(S%;'<<%CW"9$#?6F"QXPX8"#%8,"!'($Y!')!F" " #! "Z,23=,Y\=;;,;B,8"/Fi"07",;F8"5S%23#?6'$?/#S%FF"QXPP8"!#!)8"*&*Y*(!F" " ## "5,22,13:YI,63:2B:8"LFi"07",;F"F(')S%23"6F")!"QXXZ8")!8"!++(!Y!++(*F" " #$ "]:7`8"LFi"07",;8"LF"^2?,6:"b,;:?06"5:QSF"(%"QXPQ"!&'Y!&*F" " #% "LB,>8"WFi"9,H;R8"PFi"5,=V,348"PFi""/=D02,8"PFF"5%23#?6'$?/#S%F"QXXXY")*$8"$)$Y$*!F" " #& "W_"!'#!&f#+!#"WH2:S0,6"97,6>,2>"W_"!'#!&8"WH2:S0,6"3:QQ=7700"<:2"17,6>,2>=`,7=:68"LS2=;"#+!#" KEEEF306F0HMF" " #' "[:3,67"PFY[Fi"I=2,2>"5Fi"WSS0"ZFi"U0"I,HE"WF"5S%23#?6'$?/#F"L"QXXT"!+'(8"#'&Y#(&F" ". " #+" ". ACS Paragon Plus Environment. Page 20 of 27.

(21) Page 21 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. """""""""""""""""""""""""""""""""""""""" """""""""""""""""""""""""""""""""""""""" """""""""""""""""""""""""""""""""""""""" """""""""""""""""""""" ". #(. "JH"PFYPFi"4,6?"NFi"U:6?"9FYPFi"406?"-FYbF"54=6F"5S%F(')S%23"6F"QXPP,RZY,!#*(Y!$+!B,. ". #). "D,6">06"N02?8"-i"N=26B,HQ8"Ti"N:1D0;>8"L.i"07",;F"E(&-#?(%L"')$3%>"#<W"9$"PZZ\,PXU"((&Ä(*#F"". ". #*. "UF"[2,=1108"^F"I,=1108"TF"_?H@06"b:6?8",6>"-F"[F"Z:66:2>F"R#"<"(-1<%5%F(')%23"6"PZZS"$%)f!&%Y!&)". #!" ". ACS Paragon Plus Environment.

(22) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Page 22 of 27. !! !. ! !"#$%&'()'*+,-.%"/+0'+1'23&'"+0"4.2"+0'53.%.52&%"/2"5/'+1'6*7!'"0'23&'89:*'/+$%5&';"23'<&03.05"0#' -%+2+0.2"+0='.0>';"23+$2';.2&%'<&03.05"0#'53.%#&'2%.0/1&%='"0'23&'/+$%5&)'' ?@AB(CD,,'<CE'B'CE'79F=''. ! !. ACS Paragon Plus Environment.

(23) Page 23 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. !! !. !. ! !. !"#$%&'()'*&+,-.+&'+$%/01&',2-3'+4-5".#'0$6"2"0%7'#0+'89:%;<='>&%+$+'1-.&'#0+'89:%;<='-,3"?"@03"-.'/-%' A&BCC)'' (DE6<FG??'8HF'6'HF'CAI=''. ACS Paragon Plus Environment.

(24) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Page 24 of 27. !! !. ! !"#$%&'()'*+,&-."/+'/0'1'$2'/0'3'14'0#5$2'6/2$."/+'/0'7899'/+'3':;<=>'(4?'<'4)@>'??A'4)@>'B?'-/2$?+'$6"+#' .C&'D;E8'-/+F"."/+6'"+'73G2&'@)'' @(1<1@H??'IJK'<'JK'9;*L''. ! !. ACS Paragon Plus Environment.

(25) Page 25 of 27. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Analytical Chemistry. !! !. ! !"#$%&'()'*&+,"-"."-/'-&,-'01-&%'"+2&3-"4+'41'5'$6'41'0'-&,-',46$-"4+'34+-0"+"+#'78599':#;$6'41'<"11&%&+-'=>??' ",4@&%,'4+'0'A9'@'?B8CD*'346$@+'E9)7C'@@'"<'F'9)7C'$@G)'' 7C(F5H9@@'EHA'F'HA'?IJG''. ! !. ACS Paragon Plus Environment.

(26) Analytical Chemistry. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60. Page 26 of 27. !! !. ! !"#$%&'()'*&+,,'-./'*&+,!'-0'12'3#4'5&+,,4'5&+,!4'67+,!4'67+,,4'68+,,4'-./'68+,!''-0'(23#'-./' 9+,,'-./'9+,!'-0'122'3#4'1$:'".;&<0&/'=&&'*->:&'?'3@%'ABA'<@./"0"@.=)'' ?(C71D2EE'FDG'7'DG',5HI''. ! !. ACS Paragon Plus Environment.

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