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MC LC1. Phng php ph hp thu nguyn t AAS........................................................................1

1.1 Gii thiu....................................................................................................................1

1.2 Phng php xc nh.................................................................................................1

1.3 u i! "# nh$c i!..............................................................................................2

2. Phng php %u&ng ph hp th' ph(n t )*+*,S............................................................3

2.1 Gii thiu....................................................................................................................3

2.2 -h& tc xc nh........................................................................................................3

3. Phng php !#u "i giy t(! th/y ng(n 0n,,c4u&...............................................5

3.1 Gii thiu6...................................................................................................................53.2 -h& tc xc nh6.......................................................................................................5

3.3 78t %u9......................................................................................................................1:

3.; Ghi ch?ng >@ 'ng c' GutBCit........................................................11

;.1 Dguyn tEc................................................................................................................11

;.2 Fi t$ng p 'ng.....................................................................................................11

;.3 -hi8t > "# 'ng c'....................................................................................................11;.; HI& chtJ thuc th...................................................................................................12

;.K Phng php ti8n h#nh..............................................................................................13

;.L Ghi ch

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CC PHNG PHP XC NH ASENIC (AS)

1. Phng php ph hp th ng!"n t# AAS

1.1 G$%$ th$&

Phng php AAS $c "i8t tEt tNphng php ph hp thu nguyn tAt!icA>=4ptin SpCct4pht!Ct4ic. Oc nguyn t t4Qng thi >Rnh thng thR chUc xQnVng $ng nhng Mhi chUc xQ !# ch

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`ly chukn $c chukn > t4ng >Rnh nh !Uc 1::! thC thU tW =&u6

Rnh nh !Uc -4Eng 2 3 ;

Ohukn A= :.1 !gf : 1: 2: ;:

DiDd32 2! 1: 1: 1: 1:

Dc ct 8n "Qch 1:: 1:: 1:: 1::

Dong @ A=!gf : 1: 2: ;:

-i! 1:! cc >Rnh "# "# ti8p t'c nh phmn =&u6

-i8n h#nh ph(n t^ch6 -4@n 1:! !au "i 1! DiDd32. -i! 1:! "# Qi nc 13:dO t4ng "ng L:=. Dung ch9y 5K:dO t4ng ;:= "# ti8p t'c nguyn t hI& 2K: dOt4ng 3:=. F @ hp thu >c =Ing 13. n!.

78t %u9 $c t^nh thC !gf. Oh< q c/& phng php n#y # 2 egf.

1.3 $+, -. nh/ $+,

$+,

Phrp ph hp thu nguyn t cI @ nhQy "# @ ch]n ]c tng i c&. Oh^nh "R cI@ nhQy c& nn phng php n#y $c = 'ng 4t 4@ng 4li t4ng nhiu snh "Wc xc nh"8t cc Mi! Qi. Fc >it # t4ng ph(n t^ch cc nguyn t "i $ng t4ng cc i t$ng !au yh]cJ =inh h]cJ nTng nghipJ th/y =9n Mi! t4& cc hI& cht cI @ tinh Mhi8t c&. Fong thicvng cI @ nhQy c& t4ng nhiu t4ng h$p MhTng ph9i #! gi#u nguyn t cmn xc nht4c ph(n t^ch.

Yt Mhc cvng t4nh $c =W nhiw! >kn !au Mhi x q %u& cc gi&i Qn phUc tQp.F@ng tc thWc hin nh nh#ng. Oc M8t %u9 ph(n t^ch Qi cI th ghi Qi t4n >Vng giy h&ygi9n o u Qi. Fong thi "i cc t4&ng thi8t > hin n&y ngi t& cI th xc nh ongthi h&y in ti8p nhiu nguyn t t4ng !@t !au. Oc M8t %u9 ph(n t^ch Qi 4t n nhJ =&i= nh

Nh/ $+,

2

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-uy nhinJ phng php n#y cmn ph9i cI h thng !y AAS Et tin "# cI @ nhQyc& nn =W nhiw! >kn 4t cI q nghs& i "i M8t %u9 ph(n t^ch h#! $ng "8t.

2. Phng php 01ng ph hp th2 ph3n t# 4565IS

2.1 G$%$ th$&Dc > !t Ing "&i t4 h8t =Uc %u&n t4]ng i "i =W pht t4in Minh t8 "# xl h@i c/&

cn ngiJ ch/ y8u t\p t4ung cc &J hoJ m!... Hin n&y t4n & >#n th#nh ph F#Dzng cI Mh9ng 3: hoJ m! thWc hin cc chUc nVng ch^nh # iu ti8t ncJ iu h& "iMh^ h\uJ tQ c9nh %u&n p "# x q nc th9i T th. *R "\y =W nhiw! >kn >i cc cht @chQi "# Mi! Qi nng t4ng nc > !t # iu MhTng th t4nh Mhi .

Fc >it A= # cht Mch @cJ cI th g(y ch8t ngi Mhi > nhiw! @c cp t^nh "# Mhi >nhiw! @c !ln t^nh cI th g(y 4& 1 Qi >nh Mhc nh&uJ t4ng I cI cc >nh n&n y nhung th &J phi... nh nhiw! @c !ln t^nh &=Cn # !@t t&i h]& !Ti t4ng i "i =Uc

MhC cn ngi. *R "\y ph(n t^ch nh gi h#! $ng A= t4ng cc nguon nc # "ic#! cp >ch "# # "n %u&n t(! h#ng mu c/& cc nh# Mh& h]c. ` "\yJ A=Cn t4ngnc > !t $c xc nh >?ng phng php %u&ng ph hp th' ph(n t )*+*,S. -4nc = phng php l x(y Wng p 'ng ph(n t^ch A= t4ng !@t = nguon nc !tt4n & >#n thu@c th#nh ph F# Dzng .

2.2 7h18 t ' *nh

2.2.1 7h$9t :*;

Yy %u&ng ph hp th' ph(n t )*+*,S {&=c& *+K3: c/& Dh\t 9n "i cu"rt thQch

&nh@ ct A=. Piprt chi& @ 8n :J:2!| :J1!| >Rnh nh !Uc cc Qi...

Oc hI& cht thu@c Qi tinh Mhi8t hI& h]c c/& PhpJ FUc6 `ung ch gc &=Cn1:::pp!J H2d2 3:j. Yui6 D&t4i `iCtyitic&c>&!&t D&+``OJ AgDd3J 7,JP>OH3Odd2J D&2SJ S>O3. Axit6 HO cJ HDd3cJ H2Sd; c. -hi8c hQtJ M}! hQt.Dc ct h&i mn.

2.2.2 L! ,? -. '# @ ,?B

Yau nc > !t $c y cc &J hoJ m! t4n & >#n th#nh ph F# Dzng thC %uyt4Rnh c/& -O*D t4ng thng Lf2::. Yau nc Wng ch&i nhW& pyCtyCn "# $c x q= >@ >?ng HDd3c.

2.2.3 Phng php ph3n th h=1 hD>

F ph(n t^ch h#! $ng A= t4ng nc > !tJ = 'ng phng php %u&ng ph hpth' ph(n t )*+*,S.

3

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2.2.; 9t 0F -. thF8 @n

Oc phng php xc nh A= 4t & QngJ tuy nhin ph~ h$p "i iu Min c/&phng th^ nghi! hin n&y thR cI phng php %u&ng ph hp th' ph(n t )*+*,S "ithuc th >Qc iCtyitic&c>&!&t Ag``O t4ng c44!. Dguyn tEc c/& phng

php n#y # t#n >@ $ng &=Cn cI t4ng !au =} chuyn " &=Cn&t >?ng ung ch 7, hcD&,J =&u I i tc 'ng c/& ng hi4 !i =inh ph9n Ung c/& 0n "i &xit HO&=Cn&t > Mh th#nh &=in A=H3. 7h^ &=in tQ th#nh i %u& ng hp th' chU& >QciCtyitic&c>&!&t t4ng ung ch pi4iin hc c44! tQ th#nh !@t phUc cht !#u.

Lp i ung ch hp th' "# !\t @ %u&ng Qt gi t4 c& nht.

Ong @ !#u c/& phUc A=``O gi9! mn thC thi gi&n nn ch c9n t4 >i H2S "# S>H3. H2S ph9n Ung "i thucth tQ th#nh h$p cht cI !#u tng tWJ S>H 3 cvng cI Mh9 nVng ph9n Ung tng tW nhA=H3tQ h$p cht !#u hong nhQt. ` "\y chTng th/y tinh tk! P>OH3Odd24oi =yMhT. On S>H3ch[ tQ !#u hong nhQt Mhi h#! $ng c/& S> 3c& hn :.1!gf !# t4ngnc thng thR nong @ S>3ch[ $ng "8t nn MhTng cmn ph9i Qi t4N.

Dh "\y %u& M8t %u9 Mh9 =t l ch]n $c iu Min ti u ch %u t4Rnh ph(n t^chh#! $ng A= nh =&u6

-h t^ch hp th' 6 L! -hi gi&n tQ phUc6 3: ph

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`W& t4n cc iu Min ti u l ch]n xc nh gii hQn nong @ pht hin A= 3 #:J::2!gf tUc 1:+;!g A=Cn "# Mh9ng nong @ tuy8n t^nh c/& A=Cn # :.::1+:.:1K!g.

-4n c = cc iu Min ti u l ch]nJ chi8n @ng nhJ chUng t @ p Qi tt.

9ng 3. Y@t = gi t4 nh gi =&i = thng M c/& phng php.

Oc Qi $ng c t4ng As3+0,08 ppm As3+0,12ppmPhng sai S2 3,48.10-7 8,48.10-7

F@ ch chukn S 5,89.10-4 9,21.10-4

H = >i8n ]ng O"j :J51 :J5KF@ =&i chukn Sx 2,63.10-4 4,12.10-4

in gii tin c\y 7,32.10-4 1,15.10-3

S&i = tng i j 1J:1 1J:L`W& t4n M8t %u9 l Mh9 =t t4nJ l x(y Wng %uy t4Rnh ph(n t^ch h#! $ng A= t4ngnc > !tJ = o $c t4Rnh >#y t4n hRnh 3.1

K

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9t @n

78t %u9 nghin cUu %u t4Rnh x(y Wng phng php ph(n t^ch h#! $ng A= t4ngnc > !t ch phrp & 4& nhXng M8t u\n =&u6

1. 7h9 =t $c cc iu Min ti u ch %uy t4Rnh ph(n t^ch tng h#! $ng A=Cn

t4ng nc6 th t^ch ung ch hp th' Ag``O t4ng OHO 3 # L!J thi gi&n ph9n Ung# 3: phn t4ng K ph?ng thuc

L

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th Ag``O # :.::1+:.:1K !g. Fnh gi =&i = thng M ch %uy t4Rnh ph(n t^ch ch thy$c !Uc @ ch^nh xc c/& phng php.

;. Dghin cUu x(y Wng th#nh cTng %uy t4Rnh ph(n t^ch &=Cn t4ng nc >?ng thucth Ag``O t4ng OHO3

K. p 'ng %uy t4Rnh l x(y Wng ph(n t^ch !@t = !au nc t4ng cc ho n thu@c& >#n -h#nh ph F# Dzng nh gi !Uc @ T nhiw! nc >i A=Cn. 78t %u9 ch thyh#! $ng A=Cn t4ng cc !au nc u n?! t4ng gii hQn ch phrp thC tiu chukn!Ti t4ng c/& *it D&!.

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3. Phng php 8 ,. -%$ g$! t3, th! ng3n Jn(II)@8K1

3.1 G$%$ th$&B

A=Cn cn g]i # thQch t^nJ cI tW nhin t4ng thWc phk!. Dhng cc h$p cht "T c c/&A=CnJ "i iu $ng c&J 4t @c. Dgi Vn ph9i Qi thWc phk! nhiw! A=Cn hc ti8px nhiw! @c . D8u nhiw! %u& !u thR @chn nhiw! %u& ng tiu hI&.

3.2 7h18 t ' *nhB

Phng php !#u "i giy t(! th/y ng(n 0n,,c4u&. Oc h$p cht chU& A=Cn >Mh >i H2 t# th#nh A=Cn Hic4u&. Oht n#y ph9n Ung "i th/y ng(n c4u& HgO2 tk!t4n giy ]c tQ th#nh h$p cht !#u n(u.

S =nh @ \! c/& giy n#y "i ly giy tk! HgO2tiu chuknJ =} t^nh $c $ngA=Cn t4ng !au th.

3.2.1 2ng 2 h=1 htB

ng ng 2K!

nung iu ch[nh $c nhit @ tN ;:::O+ K:::O

Rnh nh !Uc ung t^ch 1:::!;`ipCt 1::!J 2K!J K!

Giy ]cJ ct th#nh gi9i chX nh\t :JKx 1Kc!O&pxun ung t^ch 2K:! ;O(n M thu\t.

Rnh nIn ung t^ch 1::!;(n ph(n t^ch

8p in >8p cch ct

ng th/y tinh6 #i 3:c!| ng M^nh :Jc!J cI Z ng M^nh :J3c! cch mu ng22c!| ng $c cE! %u& Z c/& nOH3Odd2$c cu@n t4n Qi "# tph^& t4n Z.

Aci nit4ic (1J;);1ci chy4ic c 1J1

Y&giC xit Ygd;>@t7}! hQt MhTng chU& &=Cn

A=Cn > xitJ t^nh Mhi8t Qi ,.

-h/y ng(n ,,c4u&J tinh Mhi8t Qi ,J ung t^ch Kj

5

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OhR &cCt&t P>OH3Odd2

Giy tk! thu ng(n ,, c4u&6 nhOH3Odd2 ung ch3j "t 4& MhT cu@n t4n giy th#nh ng hRnh t4'J ch "# mu t4n ng th/y tinh.

3.2.2 Chn :* 8p in nung ch ti =Ti ung ch 8n Mhi p t4 t&n h8t. F ngu@iJ ]c ungch tN c&pxun "# >Rnh nh !Uc ung ch K:!J th! nc ct 8n "Qch !UcJ Ec M.

c nh6 ~ng pipCt hRnh nh !UcJ ch >Rnh nIn ungt^ch 1::!J th! "# K! nc ctJ ch "# >Rnh nIn 1:! HO cJ "# 3g M}! nh&nhchIng \y nRnh nh !Ucung ch 1:::!J th! "# >Rnh nh !Uc 1:! &ci =unu4ic c 1J5;J th! ncct 8n "Qch !UcJ Ec M.

`~ng pipCt hut& y 1:! ung ch l ph& t4nJ ch "# >Rnh nh !Uc ung t^ch1:::! MhcJ th! nc ct 8n "Qch !Uc Ec M 1! ung ch n#y chU& 1:g A=.

mn $c ch "# 1: >Rnh nIn ung ch 1::!| Rnh thU nht ;! ung ch t4n Ung"i ;:g A= . >Rnh thU h&iJ L! Ung "i L:g A=. S&u I th! nc ct "# !Zi >Rnh ch /3:! "# ch "# !Zi >Rnh 1:! ung ch &ci chy4ic c 1J1 3g M}! . F\y nRnh n

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$c ly !#u tiu chukn. -~y $ng A= tVng mn !# &y hiJ nn 'ngc' ~ng xc nh A=Cn ph9i M^nJ n8u MhTng =} gi9! M8t %u9 ph(n t^ch. D

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;. Phng php ' *nh A :Qng :R 9 =Qch t4c Mhi x ^ !auJ 'ng c' th/y tinhph9i $c t4ng HO lng 1:jJ =&u I MhT.

WR

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Rnh t&! gic cI nOH3Odd2.3H2d j-h/y ng(n 4!u& Hg42j

Hy4pC4xit H2d2 \! c 3:j7&i ,u& 7, jJ -hi8c O4u& SnO2j7}! hQt MhTng cI A4=Cn cI M^ch thc 2: + 3: !C=hA4=Cn xit A=2d3JOtJ Giy ct.

Chn :* h=1 ht; thV th# -. ht hn

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A'$t HC@ (ZBZ)B L! [\ ,@ HC@ , ] h8 t^ t^ -.8 [\ ,@ n% t> A'$t N$tK$ ,

]>

`ung ch OhR AxCt&t 6 H& t&n 1:g P>OH3Odd2.3H2d "i 1:: ! nc ct.

Ot tk! OhR AxCt&t 6 Oh ct "# ung ch OhR AxCt&t ng(! ^t nht 1 ti8ngJ "t 4& =yMhTJ cI th ~ng t4ng 1 tumn.

Tng th/y tinh tk! OhR AxCt&t 6 Oh >Tng th/y tinh "# ung ch OhR AxCt&t ng(! ^tnht 1 ti8ngJ "t 4& =y MhTJ cI th ~ng t4ng 1 tumn.

-h/y ng(n 4!u& 6 H& t&n 3 + Lg Hg42t4ng 1:: ! 4$u Ctyic Kj h&y 4$ui=p4pyic.

Giy ct tk! -h/y ng(n 4!u& 6 Oh giy "# ung ch -h/y ng(n 4!u& ^t nht1 ti8ngJ "t 4&J MhT t/ h giy t4c Mhi #!xrt nghi! A4=CnJ M8t %u9 nhQy nht.

`ung ch 7&i ,u& 7, 1Kj f" 6 H& t&n 1Kg 7, "# 1:: ! nc ctJ >9 %u9nt4ng ch&i n(u.

`ung ch -hi8c O4u& SnO 2 ;:j f"6 H& t&n -hi8c O4u& ;: g t4ng 1:: !HO \! c.

7}! hQt MhTng cI A4=Cn.

`ung ch chukn gc A4=Cn 1::: !g A=f1! 6 O(n ch^nh xc 1J32:g A= 2d3 h& t&n"i 1:: ! nc ct l ph& "i ;g D&dH. S&u I th! nc ct 8n "Qch 1 ^t.

u q6 `ung ch n#y 4t @c ckn th\n Mhi = 'ng.

`ung ch chukn t4ung gi&n A4=Cn 1: !g A=f1 !6 Hmu n8u # !au ng "#>Rnh 7Cn&n K:: !J th! K ! HDd3LKj "# 2 ! H2d23:jJ t t4ng t/ h&n mu un nhJ =&u un !Qnh tN tN chti Mhi ung ch t4ng =ut MhTng !#u hc !#u "#ng ch&nh nhQt.

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D8u =&u 2: ph@ ung chn#y xc nh hc chuyn "# >Rnh nh !Uc K: 1:: ! th! nc ct 8n "Qch.

;.K.2 7$9n h.nh '_t ngh$&,

Ohukn > ng hp thu6 ct "# >Tng th/y tinh l $c tk! OhR AxCt&t. Giy ct l $ctk! Hg42.

\p th&ng !#u chukn6 : !gJ 1 !gJ 2 !gJ K !gJ 1: !g ung ch chukn A4=CnJ th!nc ct th#nh 2K ! "# >Rnh ph9n Ung. Sng =ng y 2K ! !au =&u Mhi l "T c hI&"# >Rnh ph9n Ung.

Oh mn $t cc hI& cht =&u "# th&ng !#u chukn "# !au ph(n t^ch6

! HO 161J Ec u ngu@i.K ! 7, 1Kj.

; gi]t SnO2;:j.F yn 1K ph

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