GC and SFC - Advanced Analytical Chemistry - Lecture Slides, Slides of Analytical Chemistry

Download GC and SFC - Advanced Analytical Chemistry - Lecture Slides and more Slides Analytical Chemistry in PDF only on Docsity! Gas and Supercritical Fluid e Outline e Reading (Skoog et al.) — Chapter 27, Gas Chromatography — Chapter 29, Supercritical Fluid Chromatography — Chapter 23, Gas Chromatography — Chapter 24, Supercritical Fluid Chromatography     !"# !"$%&  '(%)'!'&*)%*+)%,$%*%&"!'#-&./'&)"'% '%&' !'/'%(%)%& !%&!)")'#.% '&')"!!)%()'!$&*0%'$!($1223&*0%4526!!'$''!7!)8$&%&) $!'$()'9:$!'%%)8)$%* !"# !"$%& $!'%%)8)$%*'(%)'!'&*)%*+)%,$%*%&"!'#-&:;./'&)"'')6'*%&'$!'%%)8)$%*#:;.%!!)%()'$0%*'& '8)'$)' docsity.com      !" #$ %" !   &# !"'$ (  " ! ('& )*!" " !"   docsity.com GC Instrumen e Basic layout of a GC: Barra  GC Instrument e Atypical modern GC — the Agilent Dacre one lca conor oO cocr its  Columns for e@ Two major types of columns used in GC e Open columns work better at Packed column H, HEPT (mn) 40 20 30 Average linear carrier gas velocity (cm s~') Fig. 25.10 Van Deemter plots comparing the efficiencies for packed and open tubular columns. The minimum in the plot for an open tubular column is about half the value for a packed column and for fan open tubular column the linear (right-hand) portion of the curve has a smaller slope. As the curves imply, at the higher carrier gas velocities used in practice, open tubular column performance proves about three or four times better than packed column performance.  Columns fo © Open tubular columns: capillary IOS eC RCT SCARE en ry ctiTy contain packing, like HPLC columns typical particle sizes 100-600 um Cum elAle) 1000-3000 plates/m difficult to overload N up to 12000     !" #$%&$"" '()! " !! '*  !" #$%& $" '(+*,-./ ". $.'"0 !'12.%$ $'! .'$$" '&- ! -,34 !'(,34&(/ ". $.'"0)"" '%$. ". '"./ -"."0.5$%*34&($$ " ". $.'"0)"" '%$. ". '$$ "&" !. ."()6 .$"%"",34734&*($  %. $.'"078. !' docsity.com        ! "  #$%&'( "#"$ ( %)   # &!  # "   & *"&+ ,$&-& .,$!#$&- /0 1 2345 .*#$ *$!#$&- /0 1 2637( 2345 .**$ *$!#$&- /0 1 2436284( 2345 ."$**$ *$!#$&- /0 1 243629( 2345 .*$#$ $" 2# . "!&( "$"!-& :";' &"  *$!#$&- /,<=>5 3? ? ?30 >0 0 ? >00 ? >00 0 &"  *$#$ $" /,@A5 docsity.com       !"#$ % &''()*"!+,!"-#./010''2 !3+3!#! 4"5*./6162"3!57   8 89   : "3;# )  "<+= >4<1()5 )  ",! "# !3+3!#! 4" ?@0*:AB' B6' C"! #" " !#D3+ E "#*# +#*;)/#62"3! !3+3!#! 4" ?@B*:A6F B6' G3+3!##*!%! +#*+#*! "+  "+#6'2"3! !3+3!#! 4" ?@0H F6' .#*# +#*#+#*!3 !#6'2I!   3! !3+3!#! 4" ?@F0' F'' )! "+ #*"  #*!%3!#E#+E"J"# !33!"!3 ! )E $4F'> F6' G+#*!  !#*#*##"! !#*!3 !#6'23"  3! !3+3!#! 4" ?@FH6 F&' ; !3"#+I3+#* #"+#*I+#*!  !# docsity.com         !  " # $ %&  %&'% (  ) * + % +&  #&% (+  (& $   ) ,( - ( + %%. %!%%  ( / /% %) docsity.com     !"#$%&%$'"$$ ()*+,! !-.$%&"$$ %/$01*2. /! 3!.$/$ $($ $+ 4 $3%567 /.8'"$$%!9$!9.%!$ !"#$%&%$'(. $.:%;%$+ ;9. !$%!%!9!!'$628 #$<===>?.!.%$%&$!01*6@ !-".$#$%& docsity.com       !"#$%&  %'#()%)  #*+,-."  / %' %#  !' (012 *)3$ '   /$ %+.$   /  4$#."$%#'#+5'#! 6  "+)%)7('  !*898:8; docsity.com GC Detectors: e Atomic emission detector: a systems (like ICP, but tal analysis e Sulfur chemiluminescence detectc reaction an FID-like process e Thermionic detector: optimized and emp (600-800 C) s to large ion currents for ective detector that is 00x as sensitive as specialized form of UV emission from flame products UV irradiation used to ionize analytes, detected by an ion current.            ! " #$ "%"&'   " "  " (   "    " %( )*   !  ("   " "+ ),  ! "   -./0123.  ) 4&4 5     ! $   " $ 674 8" " " 9"" ) :; " "< =>? ) #   % ) " "< !   " " !    %"& )> @ ABBC =C "  # ! # "  ? )8" " "< DEFGHG EEI JKLJL MMN O PO PQGQG QGRG EE EEQS JTUVLJTUVL JTUVLJTUVLWXXWXX W MYM MYMZN Z docsity.com Purge and Trap GC for Volatile e Invented 30 years ago by T.A. Be e Principle: sous sample above sample, through to a trap is heated to desorb the nto a GC — ppb detection of VOC's like benzene, decane, halomethanes, etc... in water samples eSB Coen oe Cae Pee oe ROE CE MEU Cen amu eons ce nM eT Kee              !"# $ %#& '#!(& %#)*$ !' (+ %$* ),!$ -. /01 $&2 3$$ 45& ,(!$ )&(  &#+(!# 3$$ 46& $*#& !' (+7 $*#& # &$  &!* ! "# (#+ -87 #$!92 & +#&3$:$ ! "# #; &#+ <#&3$:$= !*#'! &#!$-2 $*$ '+,  $#  $*$ $  ##& $ # &$# & +#$#!$ >+3$)#= 4 %#& 8?< -!&## #$3$2 4 $":# *#$@#$3# !' (+ 4 3+ $)   !(#+ " @!(' &#!$ -!&"7 '7 '2 4 ' &3# $*# # &$ , !#@&#$#+ '#!(# <+3$)#= 4A#B(&# &()  &#!$7 %$*  $ !' #;$# docsity.com          !"# $%"& '%  % $% % ( %  )%$   * ! $! )%$ % +,- . ! %  !) / )!! 0' )%$  !1 %2  %( %2 !3 ! " $%" +, $ !1 (  %( $ ( !3 ! 0'   )! * " ")  %  % 4!% )!$* %  +, 5% 67 % '73 )89 /:!( )%$  ; ! < !!%# +% )%$$% $  ;!"% % % ! $! ! !4 5+,-9 docsity.com            !    "# $  %#  &  $ "'(     )   $* (      "  ""$+ docsity.com         ! " # $%" &'$  (" $"  ) &$" $  $**""$ %$$ +!  $  $$, docsity.com         ! "# $"%"  &' () #* (#(+,#! (' -#'"!. ,#! (!."/ 0#'* 1%2  -"2(#!3 " 4546 #* 7+786 %(  ' "# 2!, #! !9 ,#! %#-,#('/ "2 ,%"%! *!' %(  ' 1(#" "2" :;<  %"4 (' %##4= &2! : (' ,("(  *!-- !3 >?? >@ A BCDEFGHI?J KLMNO PQRS@J TUV WXXY Z[\\]̂@ docsity.com          !   "  # $$ # $$  % & !'" $$( &!)*++,-,./0123456-7809:4;<=>?@ABCBDEDCFGHG?DIJKEBFCEDLMNOBDMCD@GAPFMIOBFCEDCA=Q0R+8S:8R2=*R:4+23T=,U=VWXY- docsity.com             !"#$%! & '(") * + ,&($($%! '!,-  ,- %  )".! &% / %(-0%(  "(0 )!%( " 12 docsity.com