analiza spectrala a materialelor metalice
TRANSCRIPT
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UNIVERSITATEA “DUNĂREA DE JOS” GALATIFACULTATEA DE INGINERIEM.S.I.M
PROIECT E T O D E T E N S I O E T R I C E
AUTOR, Ionuţ ŞUCHEA
ÎNDRUMĂTOR,
Po!. ". #n$. Ionel Chirica
http://www.im.ugal.ro/om/personal/Ionel%20Chirica/index.htmhttp://www.im.ugal.ro/om/personal/Ionel%20Chirica/index.htm
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INTRODUCERE
C%&%'(%( %)'% *o('% &%+ (# "#n(#& )%&'o "% (&'#-#'('%, )u*u) &%+o (# "u%&o*%'#'## )# *%(n%n' )u *%)#un%( )o+#'(#+o "% *#('(. In "uu+ "% +( #"%% +( (*+#&('#% /
&%&%'(%( %)'% *#u+ )%$%n', &%+ &(% ("0u"%&( )(u *#%"%, *%n'u &(% nu %1#)'( -#&%/&(*#on#.
Rolul stiintei si tehnologiei %)'% &on)#"%(' primordial #n ()#$u(%( un%# %&ono## (2('% *% &uno()'%%, &u o &%)'%% )u)'#nu'( )# )'(#+(, &(*(#+( )( $%n%%2% +o&u# "% un&(,&o%2#un% )o(+( )# %$#on(+(, )( )('#)!(&( n%-o#+% )o(+% )# )( ()#$u% )(n('('%( %"#u+u#.
Globalizarea, !%no%n &(% &((&'%#2%(2( #n *%2%n' %&ono#( on"#(+(, *%)u*un%#n'o"u&%%( (*#"( ( noilor tehnologii )# o'#n%%( "% noi produse *%n'u ( !# #n *%(n%n'3#n (&'u(+#'('%.
Coun#'('#+% u(n% )un' "%)&#)% )# %-(+u('% "% &%+% (# u+'% o# 4n !un&'#% "%&(*('('%( +o "% ( $()# #0+o(&% '%5n#&% *#n &(% )( )u*(-#%'u#()&(, )( )% adapteze&on"#'##+o "% %"#u )# )( progreseze *% *+(n %&ono#&, )o(+ )(u *o+#'#&. In &on'%1'u+!(&'o#+o &(% #n!+u%n'%(2( "#%&' ()u*( *o&%)u+u# "% *o"u&'#% '%u#% +u(' #n &on)#"%(%&(, metodele analitice aplicate #n'%-#n *% "#!%#'% %'(*% (+% &+u+u# "% -#('3 ( *o"u)%+o 6# (u&( o#%&'#- %+u"(%( ()*%&'%+o )*%!#&% !#%&3%# !(2% "#n lantul tehnologic.Po*#%'('#+% 6#
*%!o(nţ%+% &((&'%#)'#&% (+% unu# (nu#' '#* "% ('%#(+, &( !(&'o "#%&' "% &(% "%*#n"%)%&-%n'( '%5no+o$#&( ("o*'('3 *%n'u %(+#2(%( unu# o#%&' (nu%, &u *%!o(n'%&((&'%#)'#&% #*u)%, )un' %-#"%n'#('% *#n (*+#&(%( uno %'o"% )*%!#&% "% (n(+#2( )#on#'o#2(%.
S/( "o-%"#' &( 4n'%+%$%%( )# &uno()'%%( (# *o!un"(, *% (2( "('%+o o'#nu'% *#n(n(+#2%+% !#2#&o/&5##&%, ( !%no%n%+o "#n *(&'#&( ( "u) +( *%!%&'#on(%( &on'#nu( (
*%!o(n'%+o o$(n#2('##+o 7#n)'#'u'##+o $u-%n(%n'(+% )(u ( !#%+o *#-('%8, (+% *o"u)%+o, ('%#(+%+o )(u '%5no+o$##+o. D% (&%%(, instrumentelor analitice 7)(u (*(('%+o &u &(% )% %1%&u'( ()u('o#+%8 +# )/( ()#$u(' *% *+(n on"#(+ un loc important #n )'##n'3 )#'%5n#&(, +(o('o(% "% &##n(+#)'#&(, +(o('o(% &+#n#&%, #n #n"u)'#( )(u &o%'u+ &u *o"u)%)#"%u$#&% )# nu 4n u+'#u+ (n" #n "o%n#u+ on#'o#2(## *o+u(n'#+o %"#u+u#.Iun('('##+% (u !(&u' #n)'u%n'%+% (# &o*+%1%, "( (# )#*+u "% )'(*(n#', "% %$u+(()#)'('% "% un &(+&u+('o )(u un #&o*o&%)o.
Con"u&%%( )# $()#%( )o+u'##+o o*'#% (+% *o&%)%+o '%5no+o$#&% )% *o' !(&% 4n&on"#'## "%o)%#' "% un% "(&3 )% &ooo%(2( &u metode performante de investigare amaterialelor , (*+#&('% #n '%5no+o$##+% o"%n% )# &(% (u +( (2( u+'#%+% %(+#2(# #n"o%n##+% %)*%&'#-% (+% !#2##, %+%&'o'%5n##, %+%&'on##, &5##%# )# *o'%0(%( %"#u+u#.
“Obiectele materiale şi tehnologiile sunt expresii concrete şi materializări ale ideilor şi gândirii umane” ( V.G. Childe)
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1. ANALIZA SPECTRALA
1.1. SPECTROSCOPIA
Spectroscopia %)'% )'##n'( &(% )'u"#(2( #n'%(&'#un%( "#n'% ("#('##+% %+%&'o($n%'#&%&u ('%#(. S*%&'o)&o*#( %)'% 'o'o"('( o "%nu#% $%n%#& "('( un%# &+()% "% *o&%"%% )#'%5n# %1*%#%n'(+% *#n &(% )% u(%)'% )# )% &u(n'#!#&( %!%&'u+ %#)#%# )(u ()o'#%# "%%n%$#% "% &('% o *o( )o+#"(, +#&5#"( )(u $(2o()(, #n )&o*u+ (n(+#2%# &(+#'('#-% )#9)(u&(n'#'('#-% ( (&%)'%#(. P('%( )*%&'o)&o*#%# &% )% o&u*( &u +%$('u( "#n'% #n'%n)#'('%( ("#('##+o %+%&'o($n%'#&% &% #n'%(&'#on%(2( &u ('%#(+ (n(+#2('( )# &on&%n'('#( )*%#+o ('o#&% )(uo+%&u+( "#n ('%#( (n(+#2('( *o('( "%nu#%( "% spectrometrie.
Analiza spectrala %*%2#n'( %'o"% )# *o&%"%% "% #n-%)'#$(% ( )u)'(n'%+o &% )% (2%(2( *% &%&%'(%( )*%&'%+o (&%)'o(. Un )*%&'u o!%( #n!o('## *%)% "%)*% &o*o2#'#(&(+#'('#-( )# &(+#'('#-( ( ('%#%# (n(+#2('(.
Analiza spectroscopica calitativa )% (2%(2( *% "%*%n"%n' *%)( &% %1#)'( #n'%un (nu#' %+%%n', ("#&(+, $u*(% !un&'#on(+ )(u o+%&u+( )# +un$## "% un"(7!%&-%n'%8 )*%!#& +( &(% %#' )(u ()o ("#('#% %+%&'o($n%'#& )*%#+%&5##&%. O (nu#'( )*%% &5##&( *%2#n'( %#)#% )(u ()o'#% "% ("#('#%%+%&'o($n%'#& *% (# u+'% +un$## "% un"( )*%!#&. P%n'u #"%n'#!#&(% %)'%!o+o)#'( "% %$u+( +un$#%( "% un"( un"% ("#('#( (% #n'%n)#'('% (1#( "%%#)#% )(u ()o'#%. L( (%)'%&u# &o*+%1%, un"% %1#)'( +un$## "% un"(!o('% (*o*#('% +( "ou( )*%# "#!%#'%, &(% *o' "u&% +( %o(% "% #"%n'#!#&(%
*#n &on!un"(%, )% (*%+%(2( +( +un$## "% un"( )*%!#&% &u #n'%n)#'('%( ("#('#%#(# #&(.
Analiza spectroscopica cantitativa *o('( "%nu#%( "% spectrometrie )# )% (2%(2( *% "%*%n"%n' "#n'% #n'%n)#'('%( %#)##+o )(u ()o'##+o )*%&'(+)*%!#& %+%%n'%+o, ("#&(+#+o, $u*(#+o !un&'#on(+% )(u o+%&u+%+o "#n&o*u)# )#*+# )(u (%)'%&u# &o*+%1% "% &o*u)# )# &on&%n'('#( (&%)'o(. In)o*u+ %!%&'u(## (n(+#2%# &(n'#'('#-% %)'% ()u('( !o'o%+%&'# #n'%n)#'('%( ("#('#%#%+%&'o($n%'#&% %#)% )(u ()o#'% "% )u)'(n'( (n(+#2('(, &(% %)'% &on-%'#'(
*% (2( uno %+('## ('%('#&% )# ( uno &u% "% %'(+on(% #n -(+o# "%&on&%n'('#%.
1.2. METODE SPECTROSCOPICE UZUALE PENTRU ANALIZA
CANTITATIVA
D#!(&'#( &u (2% : S*%&'o)&o*#% "% !+uo%)&%n' &u (2% : S*%&'o)&o*#% "% ()o'#% )#9)(u %#)#% ('o#&( S*%&'o)&o*#% "% !+uo%)&%n' ('o#& S*%&'o)&o*#% "% ()o'#% o+%&u+( UV/VIS C(+o#%'#% S*%&'o)&o*#% "% !+uo%)&%n' o+%&u+( UU/VIS S*%&'o)&o*#% IR S*%&'o)&o*#% R((n S*%&'o)&o*#% "% ()( o$(n#&( S*%&'o)&o*#% "% ()( ; ICP
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S*%&'o)&o*#% "% ()( ; GC
D#!%#'%+% %'o"% )*%&'o)&o*#&% nu *%2#n'( (&%+%()# *%!o(n'% +( "%'%#n(%(&on&%n'('##+o #n "o%n#u+ u%+o &( +( "%'%#n(%( &on&%n'('##+o #n "o%n#u+ *o&%n'%+o )(u 2%+o "% *o&%n'%. In (&%)' )%n), )un' *%2%n'('% #n '(%+u+ n.
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• S*%&'o)&o(*% "% +(o('o• S*%&'o)&o(*% *o'(#+%.
2. DETER INAREA CHI ICA CANTITATIVA PRIN TEHNICI DE
SPECTROSCOPIE DE E ISIE OPTICA
2.1.ENERALITATI
An(+#2( )*%&'(+( ( ('%#(+%+o %'(+#&% )% %(+#2%(2( &u (0u'ou+ unu# (*((' &uno)&u')u "%nu#%( "% )*%&'o%'u. Sistemul spectrometru "%!#n%)'% )#)'%u+ (n(+#'#& &o*+%', #n '#*&% '%%nu+ spectrometru )% %!%( #n )*%(+ +( 'o('% &o*on%n'%+% &u %1&%*'#( &o*u'%u+u#,#*#(n'%# )# )o!'(%/u+u#.
F#%&(% #n)'u%n' %)'% &on!#$u(' )( )('#)!(&( &%#n'%+% )*%!#&% (+% u'#+#2('ou+u# 7%1.!(n'%+% )# !o'o#+'#*+#&('o## )un' )%+%&'('# *% (2( %+%%n'%+o &(% -o !# "%'%&'('%8. O -(#%'('%
"% %'%+% "% "#!(&'#% )# "% )u)% "% %1'(% )un' "#)*on##+% *%n'u ( ()#$u( !(*'u+ &(#n)'u%n'u+ )('#)!(&% &%#n'%+% )*%!#&%.
Co*u'%u+ *%)on(+ &oun#&( &u #&o&o*u'%u+ #/"#%&'#on(+. To('% &o%n2#+%)%+%&'('% "% u'#+#2('ou+ #n)'u%n'u+u# )un' #n'o"u)% *#n PC. In o" ()%(n('o, PC/u+
*o&%)%(2( "('%+% (n(+#'#&% )# *%$('%)'% (*o('%+% "% (n(+#2(. Mon#'ou+ &o*u'%u+u# (('()'(%( &on"#'##+o &#'#&% (+% #n)'u%n'u+u#, &u ( !# #n(+'( '%n)#un% 7HV8 )# -#"u+ #n !%%()'(
*%n'u Analize Probe, *%&u )# #n'/un nu( "% (+'% !%%)'%.
D(&( )'(%( *%2%n'( ( *((%'#+o %)'% )('#)!(&('o(%, o #n"#&('#% ("%&-('( (*(% *%un &(* -%"%, #n &(2 &on'( #n"#&('#( &+#*%)'% *% un &(* o)u. A&%)'% #n"#&('## )un'B VAC
*%n'u -#"u+ "#n *o+#&o('o si !V *%n'u #n(+'( '%n)#un% ( !o'ou+'#*+#&('ou+u#
An(+#2( un%# *o% *#n Spectrometria de Emisie Optica prin Arc Spar! "arcscanteie# #*+#&( '%# *o&%)% "#)&%'%B
I. E$citarea atomilor din proba *#n'/o "%)&(&(% "% %n%$#% #n(+'( '#* )&(n'%#%)(u (&
II. %asurarea intcnsitatii luminii &(% %)'% %#)( +( o +un$#% "% un"( )*%!#&(#n u( '(n2#'#%# "#n )'(%( %1'('(
III. &ompararea intensitatii emise &u &%( ( un%# *o% "% &on&%n'('#% &uno)&u'(.
Lun$##+% "% un"( &(% )un' %#)% )un' &((&'%#)'#&% %+%%n'%+o "#n *o(. In$%n%(+, un %+%%n' -( %#'% ("#('#% +( "#!%#'% +un$## "% un"( 7+inii 8. In'%n)#'('%( un%# +#n##"('% %)'% "#%&' *o*o'#on(+( &u &(n'#'('%( "% %+%%n' "#n *o( 7concentratia elementului 8.
In )*%&'o%'#( ('o#&( "% %#)#% "o# !(&'o## #*o'(n'# '%u#% +u('# #n &on)#"%(% )#(nu%, rezolutia si sensibilitatea:
R%2o+u'#( )% %!%( +( &(*('('%( "% ( ()u( )%n(+u+ un%# +#n## )*%&'(+% "% o
+un$#% "% un"( "('( !(( #n'%!%%n'% "% +( (+'% +un$## "% un"( %#)% "% *o(. S%n)##+#'('%( )% %!%( +( &(*('('%( "% ( "%'%&'( u% (+% n#-%+%+o "% &on&%n'('## (+%
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%+%%n'%+o "% #n'%%).
E)'% "% "o#' &( #n *o#%&'(%( )*%&'o%'u+u# (&%)'# "o# !(&'o# )( !#% &(' (# (#.E1#)'(, 'o'u)#, (nu#'% )#'u('## &(% #un('('%)& unu+ "#n !(&'o# %"u&(n"u/< *% &%+(+(+'.
Po#%&'(%( #n)'u%n'u+u# )% !(&% ()'!%+ #n&(' )( )% o'#n( o %2o+u'#% )# )%n)##+#'('# ("%&-('%.
2.2.DESCRIEREA PROCESULUI
'('()( E$citarea probei
C(n" o *o( %'(+#&( %)'% )u*u)( unu# *o'%n'#(+ %+%&'#& #"#&(' (*( u('o(%+% *o&%)%B
A'o## )un' #n"%*('('# 7%1'()#8 "% *% )u*(!('( *#n -(*o#2(% )(u "#)'#+(%. Un##
('o# )% *o' #on#2(.
Un %+%&'on "#n'/un ('o )(u #on -(*o#2(' -( !# *oo-(' *% o o#'( )u*%#o((%n%$%'#&. A&%()'( )'(% %)'% &uno)&u'( &( o )'(% %1'('( !('( "% )'(%( !un"(%n'(+ 7#n&(% %+%&'on## )% (!+( #n &on!#$u('#( "% &%( (# 0o()( %n%$#%8.
D%2(&'#-(%( )'(## %1'('% &on"u&% +( %#)#( un%# ("#('## #n UV9 -#2##+. Lun$#%( "%un"( %#)( %)'% &((&'%#)'#&( %+%%n'u+u#. In'%n)#'('%( un%# +#n## %)'% "%*%n"%n'( "%&on&%n'('#( %+%%n'u+u# #n *o(.
A&%)'% *o&%)% 7&(% )un' nu#'% ardere8 )% *o"u& #n )*('#u+ "#n'% "o# %+%&'o2#. Unu+
"#n %+%&'o2# %)'% &5#( *o(, &%+(+(+' %+%&'o" %)'% nu#' &on'(/%+%&'o" )(u (# )#*+u%+%&'o". C%+ (# o#)nu#' '#* "% %1'(% %)'% descarcarea tip scanteie.
O "%)&(&(% '#* )&(n'%#% %)'% #n o" no(+ !o+o)#'( *%n'u (n(+#2( *o%+o *+('% )(u( )(%+o. L( o "%)&(&(% '#* )&(n'%#% *o'%n'#(+u+ %)'% "% >> V 7'%n)#un% -(!8 +( > A7&u%n' -(!8 )# '%*%('u( +( )u*(!('( %'(+u+u# *o('% -(n( "% +( >>> +( >>>C. Cu)u)%+% "% )&(n'%#%% )% *o('% o'#n% un $(" !o('% #n(+' "% *%#% )# (&u('%'% 7(*o(*%&o*((#+( &u &%( o'#nu'( &u '%5n#+% )*%&'o)&o*#&% "% (2% :8. A'(' +#n##+% #on#&% &(' )#&%+% ('o#&% )un' o)%-('% #n )*%&'u.
O )&(n'%#%% "% %n%$#% #n(+'(, nu#'( de preardere %)'% !o+o)#'( *%n'u ( oo$%n#2( *o(.
'('('( Detectia spectroscopica
F#%&(% %+%%n' "#n *o( %#'% ("#('## (-(n" un nu( "% +un$## "% un"(&((&'%#)'#&% 7+#n##8. A&%)'% +#n## )un' )%*(('% "% )*%&'o%'u )# !o&(+#2('% *% o )%#% "%"%'%&'o# &(% &on-%'%)& ("#('#( o*'#&( #n %n%$#% %+%&'#&( &(% %)'% (*o# (*+#!#&('(.
'('('()(Spectrometrul
Lu#n( &(% %)'% %#)( "% *o( '%&% *#n'/o !(n'( "% #n'(% )# %)'% !o&(+#2('( "% o%'%( "% "#!(&'#% &on&(-(, &(% %)'% un "#)& "% &u(' &on&(- )!%#& &u o )%#% "% '()('u# *((+%+% )# %&5#"#)'(n'% *%n'u ( )%*(( +u#n( *o+#&o('#&( #n ("#('#% ono&o('#&( 7+#n##8.
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D#!%#'%+% +#n## '%& *#n'/o )%#% "% !(n'% "% #%)#% &(% "#%&'#on%(2( ("#('#( &u +un$#%( "%un"( "o#'( *% "%'%&'o## #n"#-#"u(+#.
'('('('( Reteaua de difractie
C(n" un !()&u+ "% ("#('#% ono&o('#&( &u o +un$#% "% un"( )*%!#&( &("% *%
%'%(u( "% "#!(&'#%, %( %)'% "#!(&'('( )u un un$5# )*%!#&, &u )% (('( #n !#$.
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R("#('#( "#!(&'('( %)'% "#%&'#on('( )*% *+(nu+ !o&(+ (# #n)'u%n'u+u#.R("#('#( "% o+un$#% "% un"( "('( #n'%)%&'%(2( *+(nu+ !o&(+ +( o *o2#'#% )*%!#&( "%o(%&% un$5#u+ "%%!+%1#% %)'% "#!%#' *%n'u !#%&(% +un$#% "% un"(. F(n'%+% )un' #n&o*o('% #n *+(nu+ !o&(+ +("#!%#'% *o2#'## *%n'u ( *%#'% ("#('#%# )*%!#&% +un$##+o "% un"( )( '%(&( )*% "%'%&'o#.
*nghiul de blaze 7#*()'#%%8 "#n !#$.< #n"#&( un$5#u+ +( &(% "#!(&'#( %'%+%# "%
"#!(&'#% %)'% (1#(. Lun$#%( "% un"( &(% &o%)*un"% (&%)'u# un$5# )% nu%)'% lungimede unda blaze(
D(&( +u#n( #n"%n'( *% '()('u# )% o)%-( +( un un$5# &(% %)'% %$(+ )# o*u) &%+u# (+("#('#%# #n"%n'%, ("#('#( 'u'uo +un$##+o "% un"( -( !# '(n)#)(. A&%()'( )#'u('#% %)'%nu#'( #($#n% &%n'(+( 7)(u %!#%&'('(8 )(u o"#nu+ 2%o.
P!TMULT1PLIERS
)i*+ra 2. Dia*ra,a o-ica a -olicro,aor+l+i
S*%&'o%'u+ "% %#)#% o*'#&( K(#" !o+o)%)'%, o*'#on(+, "ou( %'%+% "% "#!(&'#%"#!%#'%. A&o*%#%( "o%n#u+u# )*%&'(+ B
O"#nu+ #n'(# > A / > A 7(n)'on#8O"#nu+ "o# A/ A
Un %n%!#u (+ )#)'%u+u# &u doua ordine de difractie %)'% +%$('( "% un$5#u+7+un$#%( "% un"(8 +(2%. A&%)' un$5# %)'% !#1(' *#n )%+%&'#( un%# (nu% %'%+% )# %)'% (+%)
*%n'u ( o*'##2( *%!o(n'%+% #n)'u%n'u+u#, #n %$#un# )'(#+#'% (+% )*%&'u+u#. C( o%$u+( $%n%(+(, '(n)#'(n'( %'%+%# 7!(&'ou+ "% %!+%&'#-#'('%8 )&("% o "('( &u &%)'%%("#!%%n'%# "#n'% +un$#%( "% un"( o)%-('( )# +un$#%( "% un"( +(2%. A&%()'( -( &on"u&%+( o %"u&%% ( )%n)##+#'('## )#)'%u+u# +( (&%+% +un$## "% un"( &(% )un' )%n#!#&('#- "#!%#'%"& +un$#%( "% un"( +(2%. In'/un #n)'u%n' arcspar! '#*#&, un$5#u+ +(2% %)'% (+%) *%n'uo*'##2(%( )%n)##+#'('## #n %$#un%( "#n 0uu+ -(+on# "% >> n #n o"#nu+ #n'(#, !##n"
o*'##2('(, "% ()%%n%(, )%n)##+#'('%( #n 0uu+ -(+o## "% >> n #n o"#nu+ (+ "o#+%(. D(&(!o+o)# un )#n$u o"#n "% "#!(&'#%, "o( o )#n$u( +un$#% "% un"( +(2% -( !# *%2%n'(.
O (+'( "#!%%n'( )%n#!#&('#-( #n'% o"#nu+ #n'(# )# o"#nu+ (+ "o#+%( %)'% dispersiaretelei , &(% %)'% %1*#('( "% "#)'(n'( *% &u( !o&(+( &(% &o%)*un"% unu# < n #n
)OCAL
PLANE
CRATIN
SLIT
MONOC!ROMATICRADIATION
POLIC!ROMATIC
RADIATION
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)*%&'u. In *#u+ o"#n (% o "#)*%)#% %*o&( +#n#(( %"#% "% >. n9 , #n '#* &%#n (+ "o#+%( o"#n !un#2%(2( o "#)*%)#% +#n#(( %*o&( %"#% "% >. n9 . O "#)*%)#%+($( 7%"#( "#)*%)#%# +#n#(% %*o&% (# #&(8 &on"u&% +( o )&n)##+#'('% )# %2o+u'#% (#
un(. S%n)##+#'('%( %)'% &%)&u'( *%n'u &( !on"u+ %)'% %"#(' *% un "o%n#u (# +($ "%+un$## "% un"(, #n '#* &% %2o+u'#( &%)'% *%n'u &( )*%&'u+ %)'% %1*(n"(' *% o "#)'(n'((# (% #n *+(nu+ !o&(+ 7("#&( *o(#+#'('%( "% #n'%!%%n'( %)'% (# )&(2u'(8. R%'%(u( &(%
( !o)' )%+%&'('( *%n'u )#)'% o!%( ()'!%+ )%n)##+#'('% (% )# %2o+u'#% )*%&'(+( )u*%#o((,#n )*%(+ *%n'u %+%%n'%+% &(% )un' ()u('% #n o"#nu+ (+ "o#+%( 7(&%()'( #n&+u"% (*o(*%'o('% %+%%n'%+%8.
D#n *un&' "% -%"%% (n(+#'#&, !(*'u+ &( %'%(u( *o('% *%2%n'( "ou( +#n## "% "#!%#'%+un$## "% un"( *%n'u (&&%()# *o2#'#% *% &u( !o&(+( nu *%2#n'( un #n'%%) )%n#!#&('#-.D(&( o +#n#% "% +( un o"#n "#!%#' *o('% )( #n'%!%%2% &u +#n#( (n(+#'#&(, !#+'% o*'#&% )#9 )(u un!o'ou+'#*+#&('o &(% !un&'#on%(2( #n +##'% )*%!#&% "% +un$## "% un"( -o !# !o+o)#'%
*%n'u ( "#)&##n( +#n##+% &(% #n'%!%%(2(.
F(n'%+% "% #%)#% )un' +o&(+#2('% *% &u( !o&(+( ( )*%&'o%'u+u#. L#n##+% )*%&'(+%
)un' '%o%'#& o #($#n% ( !(n'%# "% #n'(%.F(n'%+% "% #%)#% )un', 'o'o"('(, (# +($# *%n'u ( *%#'% (nu#'% #)&(# (+% )*%&'u+u# !(( )( &%%2% %o# (n(+#'#&%. In o" no(+ !(n'%+%"% #%)#% u'#+#2('% )un' "% , >, )# u..
D(&( )% !o+o)%)'% o %'%( *%n'u "o%n#u+ /> n, !(n'( "% #n'(% -( !# "%
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%)'% (# oo$%n(, &( %2u+'(' (+ !(*'u+u# &( ( !o)' prelucrata 7(% o )'u&'u( (# !#n(8.E'(+o(n%+% "% )'(n"("#2(% '%u#% )( (#( &on&%n'('## %"## *%n'u &(' "% u+'% %+%%n'%%)'% *o)##+. P%n'u ( (&o*%# 'o('% %+%%n'%+%, "% &%+% (# u+'% o#, %)'% &%u' (# u+' "%un )#n$u %'(+on "% )'(n"("#2(%.
E'(+o(n%+% "% )'(n"("#2(% )un' ()u('% #n (&%+()# '#* &u &o+%&'(%( "('%+o "%
%'(+on(% *%n'u "%'%#n(%( curbei analitice. D('%+% (n(+#'#&% (+% %'(+o(n%+o "%)'(n"("#2(% )un' "% ()%%n%( #n%$#)'('%. In(#n'% "% ()u(%( *o%+o )un' (n(+#2('%%'(+o(n%+% "% )'(n"("#2(% "#n nou, *%n'u ( "%'%#n( o#&% o"#!#&(% ( %+('#%#&on&%n'('#%9 #n'%n)#'('%.
E'(+o(n%+% "% )'(n"("#2(% nu (u n%-o#% "% !#1(% *% &u( "% &(+#(%, n%!##n"n%&%)(( &uno()'%%( &on&%n'('#%# *%)% ( %+%%n'%+o. E)'% #*o'(n', 'o'u)#, )( )%&uno()&( "(&( (*o('%+% "% #n'%n)#'('# (+% %'(+o(n%+o "% )'(n"("#2(% )un' #n "o%n#u+ "%#n'%n)#'('# (+% &u%+o "% %'(+on(%.
'('(.( Etalonarea
E'(+on(%( )% !(&% &u ('%#(+% "% %!%#n'( *%n'u ( "%'%#n( !o( $%n%(+( (%+('#%# &on&%n'('#%9 #n'%n)#'('% *%n'u %+%%n'%+% "% #n'%%).
D% o#&%# )% !o+o)%)& ./)' probe &u n#-%+% "% &on&%n'('## "#!%#'%, *%n'u ( (&o*%# 'o'#n'%-(+u+ "% %'(+on('. F#%&(% ardere !un#2%(2( o -(+o(% ( (*o'u+u# "% #n'%n)#'('#, &(% %)'%(*o'u+ #n'% #n'%n)#'('%( %+%%n'u+u# (n(+#2(' )# #n'%n)#'('%( %+%%n'u+u# ('##. A&%)'%(*o('% (+% #n'%n)#'('#+o )un' (*o# !o+o)#'% *%n'u ( &(+&u+( &u( "% %'(+on(% 7&%( (# un(!#'(%8 !o+o)#n" metoda celor mai mici patrate. Con)'(n'%+% &u%# "% %'(+on(% )un' (*o#!o+o)#'% *%n'u ( &(+&u+( &on&%n'('#(. Cu (+'% &u-#n'%, rapoartele intensitatii sunt variabileindependente )# concentratiile calculate sunt variabile dependente.
'('(0(Standardizarea
S'(n"("#2(%( &o%&'%(2( o'#%( )(u '(n)+('#( &u%# "% &(+#(% #n !un&'#% "% '#*,"('o#'( )&5#(#+o "% '%*%('u( )(u o"#!#&(#+o # (+% &on"#'##+o "% %"#u 7%1.o"#!#&(# "% '%*%('u(8.
1recventa standardizarii "%*#n"% "% nu(u+ "% *o% &(% )un' ()u('% )##n'%-(+u+ #n &(% )un' (n(+#2('%. In $%n%(+, &u &(' #n)'u%n'u+ %$% (# u+' &u ('(' )&("%(# u+' !%&-%n'( )'(n"("#2(##.
'('(0()(Standardizarea intr/un singur punct
L( )'(n"("#2(%( #n'/un )#n$u *un&' nu(# un (*o' (+ #n'%n)#'('#+o !#%&(u#%+%%n' %)'% +u(' *%n'u ( )% &o%&'( !('( "% (*o('%+% #n#'#(+%, ()'!%+ nu(# un *un&' "%)'(n"("#2(% (0u)'%(2( *(n'( &u%# 7o#$#n%( ((n% n%o"#!#&('(8. S'(n"("#2(%( #n'/un)#n$u *un&' %$% #n% "(&( &on&%n'('##+% *o%+ "% )'(n"("#2(% )# *o%+% "% (n(+#2(')un' +( #0+o&u+ )(u #n 0u('('%( )u*%#o(( ( &u%# "% %'(+on(%. S'(n"("#2(%( #n'/un
)#n$u *un&' %)'% #n o" o#)nu#' !o+o)#'( ('un &(n" &u( "% %'(+on(% *%n'u un %+%%n'
%)'% *%n'u un domeniu ingust de concentratii .
'('('(0(Standardizarea in doua puncte
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L( )'(n"("#2(%( #n "ou( *un&'% "ou( (*o('% (+% #n'%n)#'('#+o, &o%)*un2('o(% un%#&on&%n'('## #n(+'% )# un%#( 0o()% *%n'u !#%&(% %+%%n', )un' !o+o)#'% *%n'u ( %)'(#+# *o2#'#(o#$#n(+( 7#n#'#(+(8 ( &u%# "% %'(+on(%. In (&%)' o" "% (o"(% *(n'( )# o#$#n%( &u%#)u!%( (0u)'(#.
O )'(n"("#2(%( #n "ou( *un&'% %)'% %&o(n"('( &(n" intervalul in concentratie (
probelor este mare )#9 )(u concentratia elementelor "% #n'%%) este aproape de limita dedetectie. O *o( *u( )(u (*o(*% *u( *o('% )%-# "%*' *o( "% )'(n"("#2(% *%n'u *un&'u+ "% #n#. In'%-(+u+ "#n'% &%( (# "% 0o) )# &%( (# "% )u) *o( "% )'(n"("#2(% ( '%u# )( !#% "%)'u+ "% (%, (+'!%+ )'(n"("#2(%( #n'/un )#n$u *un&' -( !# (# (*#"( )# (#(&u('(.
'('('(2( Standardizarea de tip
In )'(n"("#2(%( "% '#*, o *o( )*%!#&( %)'% !o+o)#'( *%n'u &o%&'(%( &u%+o "%%'(+on(%. A&%()'( '%5n#&( )% !o+o)%)'% *%n'u a3ustarea acuratetii curbelor de etalonare +( o
*o( reala &(% nu &o%)*un"% %1(&' &u ('#&%( %'(+o(n%+o u'#+#2('% +( )'(#+#%( &u%+o "%
%'(+on(%. E'(+onu+ "% '#* '%u#% )( !#% oo$%n. Co*o2#'#( %'(+onu+u# "% '#* '%u#% )( !#%"%'%#n('( *#n %'o"% &5##&% u%"%, ()o'#% ('o#&(, %'&. )(u *#n (+'% '%5n# (n(+#'#&%()o+u'%. 4u trebuie determinata &u un (+' )*%'o%'u "% %#)#% o*'#&(. Co%&'##+% )% !(& &u!(&'o# "% &o%&'#% u+'#*+#&('#-# )(u ("#'#-#.
2.3.STANDUL ANALITIC
Standul analitic %)'% %$#un%( #n)'u%n'u+u# un"% %)'% ()%2('( )# %1'('( *o(. In&%+% (# u+'% &(2u#, )*%&'o%'u+ !o+o)%)'% o )u)( &u )&(n'%#%% &(% %)'% on'('( *%
*('%( "% 0o) "#n )'(n$( #n)'u%n'u+u#, "u*( &u )% (('( #n fig(+. D(&( )% "o%)'%, )% *o'on'( "ou( )'(n"u# (n(+#'#&%. S'(n"u+ *o%# %)'% #n *('%( "%(*'( ( )#)'%u+u# "(&(
#n)'u%n'u+ %)'% &u un )#n$u )'(n".
Po( "% (n(+#2(' )% *un% *% )u*(!('( %)%# *o%#, &( #n fig( +. E1'(%( (% +o& #n#n'%#ou+ %)%# *o%#, #n &(%( "% %1'(%, &(% %)'% o &(-#'('% )*(+('( &u ($on. T%n)#un%(
*%n'u %1'(% )% (*+#&( #n'% *o( )# &on'(/%+%&'o"u+ &(% %)'% #n #n'%#ou+ +o&u+u#.R("#('#( %2u+'(n'( '%&% *#n +o&u+ "% on'(% ( )'(n"u+u# (n(+#'#& 7&(% +%($( )'(n"u+(n(+#'#& "% #n)'u%n'8 )# !%%()'( "% #n'(%, *%n'u ( #n'( #n &o*('#%n'u+ o*'#&.
R%$#un%( "#n ()( *o%# #n &(% (% +o& %1'(%( %)'% *u0('( &u ($on *%n'u (#n"%*('( (%u+ )# -(*o## "% (*(. A&%)'% $(2% ()o ("#('#( "#n "o%n#u+ UV %"u&(n")%n#!'&('#- #n'%n)#'('%( +#n##+o )*%&'(+%.
O !%%()'( "% #n'(% %)'% *+()('( #n'% )'(n"u+ (n(+#'#& )# &o*('#%n'u+ o*'#&.A&%()'( !%%()'( *o('% !# )&o()( *%n'u &u('(%.
)i*.3. San/+l analiic
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'(+()( Asezarea probei pe masa probei
Po( %)'% ()%2('( *%)'% o "%)&5#2('u( "% *% ()( *o%#, )# !#1('( &u (% ('%n'#% *%n'u ((&o*%# #n #n'%$#% &(%( "% ("%%. Po( '%u#% )( (#( o )u*(!('( *+(n( )# '%u#% )( (&o*%%"%)&5#2('u(. O#&% -(#('#% #n !+u1u+ "% ($on &(u2('( "% ()%2(%( n%&o%)*un2('o(% ( *o%#,!o+o)#%( un%# *o% &u )u*(!('( n%*+(n( )(u ( un%# *o% &(% &on'#n% $o+u#, $(u# )# &(*('u# -((!%&'( u+' "%)&(&(%( )# "% )# validitatea analizei
'(+('( Sistemul de gaz pentru pur3are
C(%( "% %1'(% "#n )'(n"u+ "% )&(n'%#%% %)'% )*(+('( &u ($on. A&%)' $(2 #n%' )%-%)'% +(
#n"%*('(%( (%u+u# )(u ( -(*o#+o "% (*( &(% ()o ("#('##+% &u +un$## "% un"( # )##&)o%(2( &(*(#+#'('%( #n)'u%n'u+u# "% ( ()u( %+%%n'%+% &(% %#' #n UV.
In'% ("%#, &(%( "% )&(n'%#%% %)'% )*(+('( &on'#nuu &u ($on. A&%()'( #&)o%(2( *%#o("("% '#* &%u'( *%n'u %+##n(%( o#&(o -(*o# "% (*(9 (% ('un &(n" o nou( *o( '%u#%(n(+#2('(.
P(nou+ "% &on'o+ (+ $(2u+u# %)'% ()%2(' #n *('%( "% 0o) ( #n)'u%n'u+u#. Cu (&%)' *(nou )%&on'o+%(2( "%#'%+% "% ($on +( o*'#&( "% #n'(%, #n )#)'%u+ "% !#1(% ( *o%# )# #n )'(n"u+ "%)&(n'%#%%. D%#'%'u+ "% *% !('( *(nou+u# #n"#&( "%#'u+ (&'u(+.S#)'%u+ '%u#% )( !#% )*(+(' "%o1#$%n )# (+'% $(2% #n(#n'% "% ( )% !(&% o ()u('o(% (n(+#'#&(.
C( *('% ( *o&%)u+u# "% #n'%'#n%% "% u'#n(, !%%()'( "% #n'(% '%u#% )( !#% &u('('(. Du*(&u('(%( !%%)'%# %)'% n%&%)( )( )% *u0%2% )#)'%u+ &o*+%' #n(#n'% "% ( #n&%&( o (n(+#2(. C%+ (#%!#&(&% o" "% *u0(% ( )#)'%u+u# %)'% "% ( )% ("% "% &('%-( o# o *o( .Du*( &% o *o( ( !o)' ()("% (# u+'% o#, )% ()%(2( *o( "% #n'%%) )# )% (&&%)%(2( o*'#un%( “("%%”.Du*( *#( ("%% (*(%(!#)('( &on&%n'('#( %+%%n'%+o "#n *o( )# #n !un&'#% "% &on'#nu'u+ (&%)'o( )% )'(#+%)'% &(+#'('%(('%#(+u+u# %)*%&'#-, &on!o )'(n"("u+u#.
. SPECTROMETRU CU EMISIE OPTICA SPECTROVAC DV-6 BAIRD
3.1.CARACTERISTICI TE!NICE
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S*%&'o%'u+ &u %#)#% o*'#&( KAIRD Mo"%+ DV/ %)'% *o#%&'(' *%n'u (n(+#2%&(n'#'('#-% (*#"% (+% %+%%n'%+o #n )o+#"%. E)'% u'#+#2(' #n +(o('o(%+% "% *% *+('!o(A&%+oM#''(+ G(+('# *%n'u "%'%#n(%( &o&%n'('#%# &5##&% ( *o%+o "#n o'%+ )# !on'(,
*#n %'o"% )*%&'o)&o*#&% "% %#)#% o*'#&( / (n(+#2( &(n'#'('#-( "% %#)#% &u %1'(% #n)&(n'%#%.
S#)'%u+ #n&+u"% u('o(%+% &o*on%n'%B
o )u)( *%n'u %1'(%( *o%#
un +o& *% &(% )'( *o(
un )*%&'o%'u &(% )( "#)*%)%2% ("#('#( "% %1'(% #n -#"
o )%#% "% "%'%&'o# &(% )( ()o(% #n'%n)#'('%( ("#('#%# %#)%
un &o*u'% "%"#&(' "%)'#n(' &on-%)#%# )%n(+%+o #n'/un !o(' *%n'u *o&%)(%( "('%+o *#n'/un &o*u'% *%)on(+ )# (*+#&('## )o!'(%
un )#)'% "% %'(+on(% un &o*u'% *%)on(+, (*+#&('## )o!'(% 7K(#" S*%&'o&o* A**+#&('#on
So!'(%8 )# o #*#(n'(.
P%n'u "%'%#n(%( &on&%n'('#%# "% %+%%n'% %1#)'( "#!%#'% *o$(% "% (n(+#2( &(%&u*#n" &u% "% %'(+on(% *%n'u !#%&(% %+%%n'.
Po$(% "% (n(+#2( u'#+#2('% B
SLAKALI, LAS < *%n'u o'%+ )+( (+#('INO: *%n'u o'%+ #n(+' (+#('
SILICIOS *%n'u o'%+ )#+#o)MANGANOS *%n'u o'%+ (n$(no)FONTA *%n'u !on'(ALSOL / *%n'u (+u#n#u )o+u#+
3.2.MODUL DE LUCRU
P%n'u %!%&'u(%( (n(+#2%# )% (+%$% *o$(u+ "o#' ()'!%+ B
S% (*()( ESC ENTER *% ROUTINE ANALIEENTER *% *o$(u+ "o#'
P%n'u *()'(%( (n(+#2%+o *% %&(n +( )&5#(%( *o$(u+u#, )% *o&%"%(2( ()'!%+ B
S% '()'%(2( ESC, )% ("u&% &u)ou+ *% OPTIONS, (*o# *% LOAD ALLO )# )% '()'%(2( ENTER.
L( #n&%*u'u+ +u&u+u# &u (*(('u+ )% -%#!#&( ($onu+ "(&( %)'% #n *((%'# 7*% (n(+#2( *+u'#'ou+ '%u#% )( !#%
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*o%# 7#%2u+8. Po( '%u#% *o2#'#on('( ()'!%+ #n&(' )( (&o*%% o#!#u+ 7#n &(% )% (!+(%+%&'o"u+8, "u*( &(% )% !#1%(2( &u )u*o'u+ )# )% #n&5#"% &(*(&u+.
S% )&(n'%#(2( *o(, '()'#n" F.
D(&( )un%'u+ )&(n'%## %)'% "%n('u(' )% #"#&( &(*(&u+ )(u )% '()'%(2( ESC, *%n'u
#n'%u*%%( )&(n'%##.
In &(2u+ unu# (*((' *%$('#' &on!o #n)'u&'#un#+o "% +u&u, u( "%)&(&(##7)&(n'%##8 *% )u*(!('( *o%# -( *%2%n'( un &%& #n'un%&(' #n 0uu+ (#%# )&(n'%#('%. D(&( 2on(&u+(( #n'un%&('( *%2#n'( )# un #n%+ +u#no), ('un *o( nu ( !o)' ('(&('( &o%&'. P%n'u o(n(+#2( &o%&'( )% -o !(&% #n#u "ou( "%'%#n(# "u*( &(% )% -( -%#!#&( )# *#n()u(%( unu# %'(+on.
P%n'u #*#(%( %2u+'('%+o )% !o+o)%)'% '()'( F,
P%n'u )'%$%%( un%# (n(+#2% )% !o+o)%)'% '()'( DELETE "% "ou( o# #( (*o# )%
'()'%(2( ESC.
P%n'u )'%$%%( 'u'uo (n(+#2%+o )% '()'%(2( F (*o# F.
C(n" nu )% +u&%(2( &u (*(('u+ )% -( #"#&( &(*(&u+ )'(n"u+u# #( o#!#u+ )% (&o*%(&u o *o( *%n'u ( nu *%#'% *('un"%%( (%u+u# #n )'(n".
P%n'u (nu+(%( un%# &o%n2# )% '()'%(2( ESC.
S% &u('( %+%&'o"u+ "u*( !#%&(% *o( (n(+#2('(
D%*' %2u+'(' -(+(#+ )% #( -(+o(%( "%'%#n(## %1%&u'('% &on!o *o&%"u## )#(-(n" #n -%"%% u('o(%+% B -%#!#&(%( %'o"%# "% "%'%#n(%, u'#+#2(n" un %'(+on )'(n"("&%'#!#&(' "% un In)'#'u' "% S'(n"("#2(%, *('#*(%( +(o('ou+u# +( &(*(n## "% &o+(o(%&u (+'% +(o('o(% "% (&%+()# *o!#+, #n &("u+ &(o( )% !(& "%'%#n(# (+% (&%+%#()# *o%7%'(+on8.
Po$(%+% (n(+#'#&% )# "o%n##+% "% &on&%n'('## &% *o' !# (n(+#2('% &u %&5#*(%n'u+SPECTROVAC DV/ )un' '%&u'% #n An%1( <
C(+&u+%+% )un' %!%&'u('% "% &('% un #&o*o&%)o, #( %2u+'('%+% )un' (!#)('% "#%&' #n&on&%n'('## *o&%n'u(+%. Sun' (&&%*'('% %o#+% (1#% ("#)% &u &(% +u&%(2( +(o('o(%+%&5##&% 7An%1( 8
D#!%%n'%+% ("#)% &on!o STAS/u#+o %n'#on('% #n An%1( *o' &on)'( #n %o#+%"% ()u( "('o('% %o## u(n%, %o# &(% #n'%-#n #n '#*u+ "%'%#n(## (n(+#2%+o &u ( !#B *%$('#%( *o%+o, %'(n)%#'('%( &(%%# "% %1'(%, *u0(%( n%&o%)*un2('o(% #n ($on (&(%%# "% %1'(%. A&%)'% %o# "% ()u( &on)'(u #n "#!%%n'% *o2#'#-% )(u n%$('#-%.
E1*#(%( %2u+'('%+o ()u('o#+o %)'% &o*+%'( nu(# #n)o'#'( "% #n&%'#'u"#n%("% ()u(%.
3.3 (RECALIRAREA "STANDARDIZAREA'
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S'(n"("#2(%( 7%&(+#(%(8 )% -( !(&% o# "% &('% o# %)'% n%&%)(. S'(n"("#2(%(&o%&'%(2( o'#%( )(u '(n)+('#( &u%# "% &(+#(% #n !un&'#% "% '#* "('o#'( )&5#(##&on"#'##+o "% +u&u 7'%*%('u(, ($on, &u('(%( +%n'#+%#)# ( )'(n"u+u# "% (n(+#2(8. A&%()'()&5#(% #n &u( "% %'(+on(% %)'% &o*%n)('( *#n ()u(%( &('o-( %'(+o(n% *%n'u ("%'%#n( no#+% -(+o# *%n'u *(n'( )# o"on('( +( o#$#n%. S% !o+o)%)'% )'(n"("#2(%( #n "ou(
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