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Xc nh hm lng As, Hg, Se, Sb c trong nc

SVTH: Phm Th Kim Trinh

TRNG I HC CNG NGHIP TP. HCM


VIN CNG NGH SINH HC THC PHM
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BI BO CO THC TP TT NGHIP
TI

GVHD:
SVTH:
Lp:
MSSV:

TP. H Ch Minh, thng 6, nm 2010


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Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

MC LC
MC LC................................................................................................................1
LI M U........................................................................................................... 3
LI CM N........................................................................................................... 4
NHN XT CA C QUAN THC TP............................................................5
NHN XT CA GIO VIN HNG DN.....................................................6
PHN MT: TNG QUAN L THUYT...........................................................7
CHNG 1: TNG QUAN V TRUNG TM 3..............................................7
1.1. GII THIU V TRUNG TM 3..............................................................7
1.2. GII THIU V PHNG MI TRNG.............................................18
CHNG 2: TNG QUAN V NC...............................................................20
2.1 GII THIU..............................................................................................20
2.2. CC TNH CHT HA L CA NC...............................................20
2.3. VAI TR CA NC I VI S SNG...........................................22
2.4. VAI TR CA NC I VI SC KHE CON NGI................23
CHNG 3: GII THIU V As, Hg, Se, Sb....................................................26
3.1. ASEN...........................................................................................................26
3.2. THY NGN.............................................................................................33
3.3. SELEN.......................................................................................................39
3.4. ANTIMON..................................................................................................45
PHN HAI: CC PHNG PHP S DNG..................................................50
CHNG 1: PHNG PHP LY MU, TIP NHN V TH NGHIM
MU........................................................................................................................ 50
1.1. GII THIU..............................................................................................50
1.2. PHNG THC LY MU...................................................................50
1.3. THC HIN TIP NHN V TH NGHIM MU...........................51
1.4. THC HIN M BO CHT LNG CHO TH NGHIM MU53
CHNG 2: PHNG PHP QUANG PH HP THU NGUYN T .......56
2.1. S XUT HIN CA PH HP THU NGUYN T................................56
2.2. NGUYN TC CA PHP O...............................................................58
2.3. U IM V NHC IM CA PHP O......................................59
2.4. I TNG V PHM VI NG DNG CA PHP O...................60
2.5. CC B PHN CA THIT B O PH HP THU NGUYN T. .61
2.6. MT S YU T NH HNG TRONG PHP O AAS.................81
2.7. K THUT HA HI NGUI XC NH THY NGN..................97
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SVTH: Phm Th Kim Trinh
2.8. K THUT TO HYDRIDE...................................................................98
CHNG 3: PHNG PHP X L S LIU.............................................103
3.1. XC NH HM LNG KIM LOI BNG PHNG PHP AAS103
3.2. NH TR PHNG PHP XC NH..............................................105
PHN BA: XC NH HM LNG ASEN, THY NGN, SELEN,
ANTIMON C TRONG NC.........................................................................109
CHNG 1: XC NH HM LNG ASEN C TRONG NC...........109
1.1. NGUYN L...........................................................................................109
1.2. TI LIU THAM KHO.......................................................................109
1.3. THIT B, HA CHT, CHT CHUN..............................................110
1.4. CHUN B DUNG DCH MU.............................................................111
1.5. BO CO KT QU TH NGHIM..................................................112
CHNG 2: XC NH HM LNG THY NGN C TRONG NC114
2.1. NGUYN L............................................................................................114
2.2. TI LIU THAM KHO.......................................................................114
2.3. THIT B, HA CHT, CHT CHUN..............................................114
2.4. CHUN B DUNG DCH MU.............................................................116
2.5. BO CO KT QU TH NGHIM..................................................117
CHNG 3: XC NH HM LNG SELEN C TRONG NC.........118
3.1. NGUYN L............................................................................................118
3.2. TI LIU THAM KHO.......................................................................118
3.3. THIT B, HA CHT, CHT CHUN..............................................118
3.4. CHUN B DUNG DCH MU.............................................................119
3.5. BO CO KT QU TH NGHIM..................................................120
3.6. XC NH LOD, LOQ, HIU SUT THU HI V CONTROL CHART
CA PHNG PHP XC NH SELEN......................................................121
CHNG 4: XC NH HM LNG ANTIMON TRONG NC.........125
4.1. NGUYN L...........................................................................................125
4.2. TI LIU THAM KHO.......................................................................125
4.3. THIT B, HA CHT, CHT CHUN.............................................. 125
4.4. CHUN B DUNG DCH MU.............................................................127
4.5. BO CO KT QU TH NGHIM..................................................128
KT LUN.......................................................Error: Reference source not found
TI LIU THAM KHO...............................Error: Reference source not found

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Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

LI M U

Nc l ti nguyn v cng qu bu ca loi ngi v sinh vt trn tri t.


Ngoi chc nng tham gia vo chu trnh sng trn, nc cn l cht mang nng lng
(hi triu, thu nng), cht mang vt liu v tc nhn iu ho kh hu, thc hin cc
chu trnh tun hon vt cht trong t nhin. C th ni s sng ca con ngi v mi
sinh vt trn tri t ph thuc vo nc.
Tuy nhin, vi tc th ha, cng nghip ha ngy cng cao nh hin nay,
tnh trng nhim nc ang ngy cng tr nn trm trng. V vy vic xc nh hm
lng cc kim loi c hi c trong nc, cc ch tiu kim tra nc l cn thit.
Trung tm k thut 3 l mt c quan kim tra cht lng uy tn hng u Vit
Nam. Em rt may mn c thc tp ti y, c tip cn vi cc thit b hin i,
v tc phong lm vic nhanh chng, cng nghip v cc k nng thc hnh, cng nh
l thuyt ca cc phng php phn tch m trng cn cha cung cp . Do cn
nhiu hn ch v k nng v kinh nghim nn bi bo co ny cn nhiu sai st, rt
mong qu thy c, anh ch c quan v bn c b qua v gp .

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SVTH: Phm Th Kim Trinh

LI CM N

Trc ht em xin chn thnh cm n nh trng, cm n Thy L Nht Tm


gii thiu em c thc tp phng Mi trng thuc Trung tm k tut 3. ng
thi vi s hng dn tn tnh ca thy gip em hon thnh tt bi bo co ny.
K n, em xin cm n s ch dn tn tnh ca mi ngi trung tm 3 ni
chung, phng th nghim mi trng ni ring gip em hon thnh tt chng
trnh thc tp. Vi tm lng chn tnh em xin gi li cm n n tt c mi ngi.
Cm n anh Phan Thnh Trung - trng phng th nghim mi trng c nhng
kin ch o trong sut qu trnh thc tp.V hn ht em xin cm n anh Nguyn Hu
Tn, anh Nguyn Cng Chnh v anh Nguyn Vn Thng trc tip hng dn cng
vic cho em ngay t ngy u b ng. Cm n cc anh ch trong phng nhit tnh
ng vin gip v hng dn thm cho em.
Vi thi gian thc tp l 4 tun ngn ngi, vi kin thc v kinh nghim cn
qu t i nn khng sao trnh khi nhng hn ch v thiu st, em rt mong nhn
c nhng kin ch dn t pha thy gio hng dn, cc thy c, anh ch c
quan thc tp v nhng kin ng gp nhit tnh t pha cc bn sinh vin bi
Bo co thc tp tt nghip ca chng em t kt qu tt.

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Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
CNG HA X HI CH NGHA VIT NAM
c lp - T do - Hnh phc

NHN XT CA C QUAN THC TP


Nh my (vin, trung tm): Trung Tm o Lng Cht Lng 3
Xc nhn anh (ch ): Phm Th Kim Trinh l sinh vin lp HTP2 thuc Vin
Cng Ngh Thc Phm Sinh Hc, Trng HCN thnh ph H Ch Minh
n nh my (x nghip) thc tp t ngy 3/05/2010 n ngy 31/05/2010
Ni dung nhn xt:
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Bin Ha, ngy..thng.. nm 2010
NGI NHN XT
( Ghi h tn, ng du)

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SVTH: Phm Th Kim Trinh

NHN XT CA GING VIN HNG DN


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Tp. H Ch Minh, ngy.. thng.. nm 2010
NGI HNG DN
(Ghi r h, tn)

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SVTH: Phm Th Kim Trinh

PHN I: TNG QUAN L THUYT


CHNG 1
TNG QUAN V TRUNG TM 3
1.1. GII THIU TRUNG TM 3
1.1.1. Lch s hnh thnh v pht trin Trung Tm
Trung Tm K thut 3 c tn y l Trung tm K thut Tiu chun o
lng Cht lng khu vc 3 thuc Tng cc Tiu chun o lng Cht lng - B
Khoa hc Cng ngh v Mi trng, c tn giao dch quc t l Quality Assurance
and Testing Centre 3 (QUATEST 3).
L n v s nghip khoa hc phc v cng tc qun l nh nc v tiu
chun, o lng, cht lng (TCLCL) v cc hot ng dch v khc theo yu cu
ca cc t chc, c nhn.
Trc y Trung tm c tn l Vin nh Chun c thnh lp vo nm 1967
min nam Vit Nam. n nm 1972 i tn thnh Vin nh Chun Quc Gia theo
b lut 007/72 c chnh quyn c ban hnh ngy 01/12/1972.
Sau khi gii phng min Nam cc hot ng ca Vin nh Chun c t
chc li v sp xp theo cp bc Nh nc.
Nm 1979 C quan Tiu chun Cht lng v o lng min Bc v Vin
Kim nh chun min Nam kt hp li thnh b phn nh Chun Cht Lng
o Lng Quc Gia. Chnh s sp xp ny to thnh cc nh chun cht lng
vo nm 1984 vi tn mi l Cc Tiu Chun o Lng.
Trung tm ta lc:

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SVTH: Phm Th Kim Trinh
- Vn phng chnh: 49 Pastuer, phng Nguyn Thi Bnh - Q1 - TP. HCM. Vi t
cch php nhn c ti khon ngoi t v ni t, c con du giao dch cng tc.
Email: info@quatest3.com.vn
Website: www.quatest3.com.vn
- B phn dch v phng th nghim s 62 L Hng Phong - Q5 - TP. HCM.
Email: dl-thietbi@quatest3.com.vn
- Xng thit b o lng s 79 Trng nh, Q3, TP. HCM.
- Khi th nghim Bin Ha c ti s 7, ng 1, khu cng nghip Bin Ha
1, ng Nai
Email: testing@quatest3.com.vn
Nhn s:
Vi i ng cn b cng nhn vin c o to chuyn ngnh v c kinh
nghim trong lnh vc th nghim. Cc phng th nghim c trang b cc thit b
th nghim v o lng hin i, c y ti liu v tiu chun, phng php th,
c kh nng p ng cc yu cu v th nghim phc v cng tc th nghim,
thm nh k thut th nghim sn phm, kim nh v hiu chun cc phng tin
o trong sn xut kinh doanh, qun l cht lng, nghin cu khoa hc v gio dc
o to.
Bn cnh i ng chuyn vin k thut v chuyn gia c nhiu k nng v
kinh nghim trong cc lnh vc chuyn ngnh, Trung tm K thut 3 cn c mng
li cng tc vin l cc chuyn gia, gio s c trnh chuyn mn su t cc
ngnh cng nghip, Vin nghin cu, Trng i hc...
Trung tm K thut 3 ng gp tch cc vo cng tc tiu chun o
lng cht lng phc v cng ng, hot ng sn xut kinh doanh ca doanh
nghip cng nh cc hot ng nghin cu khoa hc ca t chc, c nhn.
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SVTH: Phm Th Kim Trinh
Vi nhng n lc ca i ng cn b chuyn nghip v tm nhn pht
trin cc hot ng ca mnh thch nghi vi tc ng v ngng thch thc do
qu trnh hi nhp kinh t quc t, Trung tm K thut 3 tr thnh mt trong
nhng n v cung cp dch v hng u trong c nc trong lnh vc nh gi
s ph hp v cung cp cc gii php v cht lng.
Trong qu trnh pht trin ca mnh Trung tm c s h tr t
chng trnh pht trin Lin hip quc nh:
- VIET 76/013 Cng c khi nim o lng v th nghim ca Quatest
3 ti TP. H Ch Minh.
- VIET 81/006 Mng li tiu chun cht lng o lng nh chun
v thm nh Quc gia cho Quatest 1 v Quatest 3.
- VIET 85/009 Pht trin v bo tr thit b ca Quatest 3.
V cc ti trn c trin khai ng dng thnh cng.
Mt s danh hiu c cng nhn trong qu trnh hnh thnh v pht trin:
- c ch nh l phng th nghim chun thuc khu vc ASEAN
(ARL- Asean Reference Laboratory) trong lnh vc vi sinh .
- c cng nhn ph hp theo ISO 17025 t nm 2004 bi t chc
cng nhn VILAS.
- c nh gi cng nhn ph hp theo ISO 17025:2005 bi t chc
cng nhn Na Uy vo thng 04/2007.
- lm mi th tc c th c cng nhn theo ISO guide 43-1 cho
lnh vc t chc th nghim thnh tho.
- c B Y t cng nhn l phng th nghim ch nh kim tra v
thc phm nhp khu.
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SVTH: Phm Th Kim Trinh
- c B Y t cng nhn l phng th nghim chun cp quc gia
trong lnh vc th nghim GMO.
- ang hon tt h s c B nng nghip v pht trin nng thn
ch nh l phng th nghim kim tra vi sinh phn bn.H thng qun l ca
Trung tm 3 c chng nhn ph hp vi tiu chun ISO 9001 cho mi lnh vc
hot ng v c cng nhn ph hp vi cc tiu chun ISO/IEC 17025 cho lnh
vc th nghim, ISO/IEC 17020 cho lnh vc gim nh hng ha v ISO/IEC Guide
65 cho lnh vc chng nhn sn phm (bn th ba).
- Khi th nghim duy tr c h thng cht lng ph hp vi cc yu cu
ISO/IEC Guide 25 v cc chun mc v cng nhn phng th nghim NATA,
Australia.
1.1.2. S c cu t chc

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SVTH: Phm Th Kim Trinh

Gim c Trung Tm
Ph Gim c

Ph Gim c

Ph trch Cht lng


Th nghim

Cc Phng Chc Nng

Th nghim

o lng

P.Qun l Th nghim

PTN. C kh - NDT

P.K thut
Th Nghim

PTN. Hng tiu dng

PL. Khi lng

PTN. g gia dng

PL. C

PTN. Xy dng

PL. in nng

PTN. in

PL. Nhit

PTN. EMC

PL. Ha l

PTN. Ha hc

PL. di

PL. Dung tch


lu lng

PTN. Du kh
PTN. Mi trng
PTN. Thc phm
PTN. Vi sinh - GMO
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SVTH: Phm Th Kim Trinh
1.1.3. Nhim v, chc nng v quyn hn ca Trung Tm
Theo iu l v t chc v hot ng ca Trung tm K thut 3 (ban hnh theo
qui nh s 128 ngy 21/02/1995 ca B Khoa hc Cng ngh V Mi trng) s c
nhim v, chc nng v quyn hn nh sau:
1.1.3.1. Chc nng v nhim v
Trung tm K thut 3 thc hin chc nng v nhim v phc v cng tc qun
l Nh nc v tiu chun, o lng, cht lng v thc hin cc dch v khc theo
yu cu ca doanh nghip, t chc v c nhn.
- Kim tra, nh gi, thm nh cht lng, k thut, v sinh v an ton sn
phm, hng ha, dch v v cng trnh.
- Kim nh, hiu chun, kim tra v nh gi cc phng tin o, h thng o.
- Th nghim cht lng, v sinh, an ton ca sn phm, hng ha.
- Chng nhn cht lng v an ton ca sn phm.
- nh gi thc trng cng ngh v cc yu cu v mi trng.
- Nghin cu, ch to v cung cp cc chun o lng, mu chun v cc
phng tin o lng.
- T vn p dng cc h thng qun l, ci tin nng sut cht lng v
trang b phng th nghim.
- o to, bi dng nghip v chuyn mn k thut TCLCL.
a. Thm nh
Thm nh k thut, cht lng, an ton ca sn phm hng ha thuc cc lnh vc:
- C kh, luyn kim, thit b cng ngh.
- Hng tiu dng, du kh v mi trng.
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SVTH: Phm Th Kim Trinh
- Nng sn, thc phm, thy sn v ha cht.
- in, in t v vin thng.
- Xy dng v an ton cng nghip.
b. Th nghim
Th nghim, nh gi cht lng, v sinh, an ton ca cc sn phm, hng ha
theo cc lnh vc:
- C kh - Khng ph hy (NDT): Vt liu kim loi, sn phm c kh, ni

hi, th nghim khng ph hy - NDT (tia X, tia gamma, siu m, bt t).


- Hng tiu dng: Vi si, may mc, giy, cc loi bao b, cao su, cht do,

sn, vecni, mc in, dng c th thao, chi,...


- g gia dng :Cc loi bn, gh, ...
- Xy dng: Vt liu xy dng (t, ct, , ct liu, xi mng, b tng,

bitum, gch, ngi cc loi, gm s, cu kin, ...), cng trnh xy dng v giao thng,
th nghim khng ph hy.
- in: Dy v cp in, dy in t, pin v acquy, dng c in dn dng,

c cu ng ngt, my bin th, th cch in, cao p n 600V,...


- Tng thch in t (EMC): Thit b in gia dng.
- Ha: Ha cht v c v hu c, phn bn, thuc tr su, cht ty ra,

nha, cao su, resin, thy tinh, gm s ,...


- Mi trng: Nc ung, nc sinh hot, cht thi c hi, nc thi, kh

thi, cht thi rn, hot phng x , ...


- Du kh: Sn phm lc du (xng, du FO,...), nha ng, du bi trn,

du th, kh thin nhin.


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SVTH: Phm Th Kim Trinh
- Thc phm: Nng sn, thc phm, thy sn, sc sn, thc n gia sc.
- Vi sinh - sinh vt chuyn i gen (GMO): Nc, thc phm, nng sn,

thy sn, sc sn, phn tch sinh vt chuyn i gen.


c. Kim tra
Trung tm K thut 3 c ch nh l t chc kim tra k thut sn phm
thuc danh mc sn phm, hng ha phi kim tra v cht lng ban hnh km theo
quyt nh 50/2006/QD-TTg, ngy 07 thng 03 nm 2006 ca Th tng Chnh ph
i vi cc loi sn phm hng ha di y:
- Thy sn.
- Thuc bo v thc vt.
- Phn bn.
- Thc n chn nui.
- Xi mng cc loi, dm b tng ct thp ng lc trc PPB, blc b tng.
- M an ton cng nghip, gng tay v ng cch in, bn mt n lc bi v

khu trang chng bi, knh hn in.


- M bo v cho ngi i xe my , thp trn, thp ct b tng cn nng v

dy thp d ng lc dng trong xy dng, dy in bc nha PVC, dng c v thit


b in gia dng v chi dnh cho tr em di 36 thng tui.
d. Chng nhn sn phm
Trung tm K thut 3 l t chc chng nhn thuc bn th ba, iu hnh hot
ng chng nhn ph hp vi yu cu ca Tiu chun ISO/IEC Guide 65 : 1996.
Trung tm K thut 3 c i ng chuyn gia nh gi, chuyn gia k thut,
chuyn gia th nghim c trnh chuyn mn cao, giu kinh nghim v h thng

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SVTH: Phm Th Kim Trinh
phng th nghim c trang b hin i. Sn phm v dch v c Trung tm
chng nhn hp chun c ngi tiu dng trong v ngoi nc tn nhim.

e. o lng
Cc dch v o lng bao gm:
- Kim nh v hiu chun theo cc phng php LVN, OIML, TCVN,
ISO, ASTM hoc API cho cc lnh vc:
- o lng c: Lc, cng, ngu lc, p sut, ...
- o lng in: ng h o in, cng t in, mgm mt, in tr, tn s, ...
- o lng nhit: Nhit k, cp nhit in, l nung, ...
- o lng di: Thc kim loi, thc cun, thc cp, thc vn o

ngoi, ng h so, b cn mu,...


- o lng dung tch: Bnh chun dung tch, ng h o nc lnh, b ong, ...
- o lng khi lng: Cn k thut, citc t, bnh chun, ng h o lu

lng, ...
- o lng ha l: My o m, t trng k, pH k, nht k, my o n, ...

f. T vn
Dch v k thut th nghim: t vn trang b, lp t, vn hnh thit b o
lng v th nghim, thit k, ch to, cc chun lng.
T vn v o to cho cc t chc v doanh nghip xy dng v p dng:
- H thng qun l cht lng ISO 9001, ISO/TS 16949, ISO/TS 29001.
- H thng qun l mi trng ISO 14001.

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SVTH: Phm Th Kim Trinh
- H thng qun l trch nhim x hi SA 8000.
- H thng qun l sc khe v an ton ngh nghip OHSAS 18001.
- nh gi h thng qun l cht lng v mi trng ISO 19011.
- H thng qun l phng th nghim ISO/IEC 17025, GLP.
- H thng qun l an ninh thng tin ISO/IEC 27001.
- H thng qun l an ton thc phm ISO 22000.
- Thc hnh sn xut tt theo GMP - CODEX, WHO - GMP, GMP - ASEAN.
- H thng kim sot v sinh v an tan thc phm theo HACCP, SQF 2000.
- Cc cng c qun l cht lng nh k thut thng k (SPC, Seven tools),
trin khai chc nng cht lng (QFD), chi ph cht lng (COC) 5S.
- Ci tin nng sut.
- Cng tc tiu chun ha, o lng v qun l cht lng trong doanh nghip.
g. Hot ng o to
o to v cc h thng qun l : Cc h thng qun l cht lng ISO 9001,
ISO/TS 16949, ISO/TS 29001, h thng qun l mi trng ISO 14001, h thng
qun l an ninh thng tin ISO/IEC 17799, h thng qun l an ton v sc khe
ngh nghip OSHAS 18001, h thng qun l trch nhim x hi SA 8000, h thng
qun l an ton thc phm ISO 22000, h thng qun l cht lng phng th nghim
ISO/IEC 17025, GMP trong lnh vc thc phm v dc phm, nh gi ni b theo
tiu chun ISO 19011, cc cng c ci tin cht lng nh k thut thng k (Seven
Tools), k thut cng nghip (Industrial Engineering), QFD, TQM, Benchmarking,
Six Sigma, chi ph cht lng (COQ), ...

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SVTH: Phm Th Kim Trinh
o to v k thut th nghim: o to kim nh vin o lng cho cc lnh
vc khi lng, in, p sut, lc, nhit,...hiu chun phng tin o lng khoa hc,
o to th nghim, phn tch cc sn phm thuc lnh vc: C l, ha hc, vi sinh,
khng ph hy...
h. Hot ng thng tin tiu chun
Cung cp thng tin v tiu chun v ti liu:
- Cc quy nh k thut ca Vit Nam, nc ngoi v cc ti liu nghip v
v tiu chun, o lng v cht lng.
- Tiu chun quc gia nh TCVN, JIS, GOST, BS, IS, AS, DIN, NF,
AINSI, KS,
- Tiu chun quc t: ISO, IEC, CODEX, OIML,
- Tiu chun ca cc hip hi: ASTM, APHA, ASME, AWS, API, AOAC,
AOCS, CIPAC,
1.1.3.2. Quyn hn
Cp phiu kt phiu kt qu th nghim, giy chng nhn cht lng, chng
th gim nh v cht lng sn phm hng ha v giy chng nhn kim nh thit
b o lng theo quy nh.
K cc hp ng v kim nh, th nghim v cc dch v cng nh cc ni
dung khc theo quy nh i vi c s sn xut kinh doanh, cc t chc v c nhn.
Thu l ph kim tra, gim nh, kim nh, th nghim,theo quy nh ca
Nh nc.
Nng lc chng nhn ca Trung tm 3

- Trang 17 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Trung tm 3 thc hin chng nhn sn phm v dch v ph hp tiu chun v
cc qui chun k thut thuc cc lnh vc: in, in t, c kh, ha cht, thc phm,
vt liu xy dng, hng tiu dng, gia dng, sn phm du kh,
Li ch ca doanh nghip khi sn phm c chng nhn:
- Sn phm ca doanh nghip c ngi tiu dng chn la v tn nhim
do c bn th ba chng nhn.
- Nng cao kh nng tip th sn phm.
- To uy tn bn vng cho thng hiu ca doanh nghip.
- Ngi tiu dng nhn bit ngay sn phm bo m cht lng v an ton
khi mua hng.
- Gim chi ph kim tra, th nghim sn phm do c bn th ba nh gi
chng nhn v gim st.
- C li th khi tham gia u thu, k kt hp ng cung cp sn phm c
chng nhn.
Trung tm 3 cam kt lun tha mn ngy cng cao yu cu ca khch hng
thng qua vic thit lp, duy tr v p dng hiu qu h thng qun l cht lng
cung cp cc dch v tin cy, chuyn nghip v khng thin v theo phng chm:
Chnh xc, khch quan, kp thi v hiu qu.
1.2. GII THIU V PHNG MI TRNG
1.2.1. Gii thiu
Phng th nghim mi trng c tch ra t phng th nghim ha mi
trng v phng th nghim ha hu c vo thng 01/2004, chuyn v th nghim
cc loi mu thuc lnh vc mi trng nh:
-

Phn tch cc loi kh: O2, N2, CO2


- Trang 18 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
-

Cc thnh phn v tnh cht cc loi nc t nhin, nc ung, nc sinh

hot, nc thi, cht thi rn


-

Thnh phn vi lng kim loi trong nc v vt liu.

Mu Azo, PCP, phenol v dn xut ca phenol, PCBs, PAHs

D lng thuc tr su trong thc phm, nc, vt liu

D lng cc dung mi hu c d bay hi nh toluen, xylen

nh danh thnh phn hu c, thnh phn dung mi, n hng

1.2.2. S phng th nghim

TRNG N V
CN B
CHT LNG

NHM PT
VT LIU

CN B K
THUT

NHM NC
MI TRNG

NHM CC LOI
MU KHC

CC KIM NGHIM VIN

1.2.3. Cc thit b chnh trong phng


- My sc k vi cc u d MS, ECD, FPD, TCD.
- My sc k lng hiu nng cao HPLC, u d PAD, FD post columm.
- My quang ph hp ph nguyn t AAS.
- My sc k lng nng cao vi u d dn in.
- Trang 19 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- Cc thit b th nghim v nc nh: BOD, dn in, pH, c, Jaotest,
my so mu DR - 2010.

CHNG 2
TNG QUAN V NC
2.1. GII THIU [1]
Nc l mt hp cht ha hc ca xy v hir, c
cng thc ha hc l H2O. Vi cc tnh cht l ha c bit
(v d nh tnh lng cc, lin kt hir v tnh bt
thng ca khi lng ring), nc l mt cht rt quan
trng trong nhiu ngnh khoa hc v trong i sng. 70%
din tch ca Tri t c nc che ph nhng ch 0,3%
tng lng nc trn Tri t nm trong cc ngun c th
khai thc dng lm nc ung.
Bn cnh nc "thng thng" cn c nc nng v nc siu nng. cc
loi nc ny, cc nguyn t hir bnh thng c thay th bi cc ng v teri
v triti. Nc nng c tnh cht vt l (im nng chy cao hn, nhit si cao hn,
khi lng ring cao hn) v ha hc khc vi nc thng.
2.2. CC TNH CHT HA L CA NC [1]
- Trang 20 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Cu to ca phn t nc to nn cc lin kt hir gia cc phn t l c s
cho nhiu tnh cht ca nc. Cho n nay mt s tnh cht ca nc vn cn l cu
cho cc nh nghin cu mc d nc c nghin cu t lu.
Nhit nng chy v nhit si ca nc c Anders Celsius dng lm
hai im mc cho bch phn Celcius. C th, nhit nng chy ca nc l 0
Celcius, cn nhit si (760 mm Hg) bng 100 Celcius. Nc ng bng c
gi l nc . Nc ha hi c gi l hi nc. Nc c nhit si tng
i cao nh lin kt hir.
Di p sut bnh thng nc c khi lng ring (t trng) cao nht l
4 C: 1 g/cm l v nc vn tip tc gin n khi nhit gim xung di 4 C.
iu ny khng c quan st bt k mt cht no khc. iu ny c ngha l: Vi
nhit trn 4 C, nc c c tnh ging mi vt khc l nng n, lnh co; nhng
vi nhit di 4 C, nc li lnh n, nng co. Do hnh th c bit ca phn t
nc (vi gc lin kt 104,45), khi b lm lnh cc phn t phi di xa ra to lin
kt tinh th lc gic m. V vy m t trng ca nc nh hn nc th lng.

Khi ng lnh di 4 C, cc phn t nc phi di xa ra to lin kt

- Trang 21 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
tinh th lc gic m

Nc l mt dung mi tt nh vo tnh lng cc. Cc hp cht phn cc hoc


c tnh ion nh axt, ru v mui u d tan trong nc. Tnh ha tan ca nc ng
vai tr rt quan trng trong sinh hc v nhiu phn ng ha sinh ch xy ra trong dung
dch nc.
Nc tinh khit khng dn in. Mc d vy, do c tnh ha tan tt, nc hay
c tp cht pha ln, thng l cc mui, to ra cc ion t do trong dung dch nc cho
php dng in chy qua.
V mt ha hc, nc l mt cht lng tnh, c th phn ng nh mt axit
hay baz. pH =7 (trung tnh), hm lng cc ion hydroxyt (OH -) cn bng vi hm
lng ca hydronium (H3O+). Khi phn ng vi mt axit mnh hn th d nh HCl,
nc phn ng nh mt cht kim:
HCl + H2O H3O+ + ClVi amoniac nc li phn ng nh mt axit:
NH3 + H2O NH4+ + OH2.3. VAI TR CA NC I VI S SNG [2]
Nc l ti nguyn vt liu quan trng nht ca loi ngi v sinh vt trn tri
t. Con ngi mi ngy cn 250 lt nc cho sinh hot, 1.500 lt nc cho hot ng
cng nghip v 2.000 lt cho hot ng nng nghip. sn xut 1 tn giy cn 250
tn nc, 1 tn m cn 600 tn nc v 1 tn cht bt cn 1.000 tn nc.
Ngoi chc nng tham gia vo chu trnh sng trn, nc cn l cht mang nng
lng (hi triu, thu nng), cht mang vt liu v tc nhn iu ho kh hu, thc
hin cc chu trnh tun hon vt cht trong t nhin. C th ni s sng ca con ngi
v mi sinh vt trn tri t ph thuc vo nc.

- Trang 22 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Lng nc trn Tri t theo tnh ton hin nay l 1,39 t km 3, tp trung trong
thu quyn 97,2% (1,35 t km3), cn li trong kh quyn v thch quyn. 94% lng
nc l nc mn, 2% l nc ngt tp trung trong bng hai cc, 0,6% l nc
ngm, cn li l nc sng v h. Lng nc trong kh quyn khong 0,001%, trong
sinh quyn 0,002%, trong sng sui 0,00007% tng lng nc trn tri t. Lng
nc ngt con ngi s dng xut pht t nc ma (lng ma trn tri t
105.000km3/nm. Lng nc con ngi s dng trong mt nm khong 35.000 km3,
trong 8% cho sinh hot, 23% cho cng nghip v 63% cho hot ng nng
nghip).

2.4. VAI TR CA NC I VI SC KHE CON NGI [3]


Nc chim 74% trng lng tr s sinh, 55 n 60% c th nam trng
thnh, 50% c th n trng thnh. Nc cn thit cho s tng trng v duy tr c
th bi n lin quan n nhiu qu trnh sinh ho quan trng. Mun tiu ha, hp thu
s dng tt lng thc, thc phm ... u cn c nc.
Nhiu nghin cu trn th gii cho thy con ngi c th sng nhn n trong
nm tun, nhng nhn ung nc th khng qu nm ngy v nhn th khng qu nm
pht. Khi i trong mt thi gian di, c th s tiu th ht lng glycogen, ton b
m d tr, mt na lng protein duy tr s sng. Nhng nu c th ch cn mt
hn 10% nc l nguy him n tnh mng v mt 20- 22% nc s dn n t
vong.
PGS. TS Nguyn Th Lm, Ph Vin trng Dinh dng quc gia, cho bit:
Khong 80% thnh phn m no c cu to bi nc, vic thng xuyn thiu
nc lm gim st tinh thn, kh nng tp trung km v i khi mt tr nh. Nu thiu
nc, s chuyn ha protein v enzyme a cht dinh dng n cc b phn khc
- Trang 23 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
ca c th s gp kh khn. Ngoi ra, nc cn c nhim v thanh lc v gii phng
nhng c t xm nhp vo c th qua ng tiu ha v h hp mt cch hiu qu.
Nhiu nghin cu cng cho thy: Nc l thnh phn ch yu ca lp sn v cht
hot dch, khi b phn ny c cung cp nc, s va chm trc tip s gim i, t
gim nguy c vim khp; ung nc lm cho h thng bi tit c hot ng
thng xuyn, bi thi nhng c t trong c th, c th ngn nga s tn ng lu
di ca nhng c t gy bnh ung th. Ung nc nhiu hng ngy gip lm long
v gia tng lng nc tiu bi tit cng nh gp phn thc y s lu thng ton c
th, t ngn nga hnh thnh ca cc loi si: ng tit niu, bng quang, niu
qun... Nc cng l mt bin php gim cn hu hiu v n gin, nht l ung mt
ly nc y khi cm thy i hoc trc mi ba n. Cm gic y d dy do nc
(khng calorie, khng cht bo) s ngn cn s thm n v quan trng hn nc kch
ng qu trnh chuyn ha, t chy nhanh lng calorie va hp thu qua thc phm.
Nu mi ngy ung u n su ly nc th mt nm c th gim hai kg trng lng
c th.
Chnh v vy, vic b sung, cng nh
p ng nhu cu nc hng ngy ca c th con
ngi l ht sc quan trng. i vi tr nh,
nhng hm tri nng, cn cho tr ung thm
nc, khi tr st cao, st xut huyt... th nhu
cu nc cn cao hn nhiu. Khi nhit c
th tr tng thm 10C, nhu cu nc s tng
thm 12%, tr b tiu chy nng c th mt ti mt lt nc trong mt gi. Du hiu
sm nht bo hiu thiu nc l cm gic kht, khi thy kht, tc l c th mt t mt
n 2% nc. Khi mt n 5% nc bt u xut hin cc ri lon chuyn ha v cht
v nu mt 10 n 15% nc, c th s trong tnh trng nguy kch, c th t vong.
Mt nc bao gi cng ko theo vic mt mt lng ng k cc cht in gii (ch
- Trang 24 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
yu l kali, canxi, st, it) v mt s vitamin. Hu qu l chc phn sng ca c th b
nh hng, cc phn x c iu kin v phi hp ng tc b gim st, c th chng
mt mi, kh tp trung... Chnh v vy, ngoi lng nc do ba n em li qua thc
n nh canh, sp... cn cho tr ung nc u n, trong 60% t nc un si
ngui hoc nc tinh lc, 20% t cc loi sa, 20% t nc p tri cy. Nc p tri
cy, sa cc loi l thc ung c gi tr dinh dng cao c th cho tr ung hng ngy.
Khng nn cho tr ung nc (d gy h hi rng v vim hng) v cc loi nc
cha nhiu nng lng "rng" nh nc ngt cc loi, nc tng lc, nc hng tri
cy, nc cha cht kch thch (ch, c ph, bia) hay cc loi nc gii kht c ga.
i vi ngi cao tui, d mc cc bnh cm st do vim phi, nhim trng
ng tit niu, tiu chy hay vic lm dng thuc nhun trng trnh to bn... cho
nn dn n tnh trng mt nc nhiu hn. Nc cn c lin tc vo ra c th di
mt s c ch iu ha. Khi lung nc gim, khi lng mu gim theo, nng
natri hi tng cao gi nc nhng li lm c th b ph hoc tng huyt p. Tuy
vy, vi ngi ln cc bnh l v thn, i tho ng, suy tim li cn phi hn ch
ung nc.
Nh vy, nc c vai trng rt quan trng i vi s sng ca con ngi v
mi sinh vt trn Tri t nhng vi tc pht trin nh hin nay, ngun nc ngy
cng b nhim. nhim nc c nguyn nhn t cc loi cht thi v nc thi
cng nghip c thi ra lu vc cc con sng m cha qua x l ng mc; cc loi
phn bn ho hc v thuc tr su ngm vo ngun nc ngm v nc ao h; nc
thi sinh hot c thi ra t cc khu dn c ven sng. Cc n v c nhn s dng
nc ngm di hnh thc khoan ging, khi khng s dng na m khng bt kn cc
l khoan li lm cho nc bn chy ln vo lm nhim ngun nc ngm. Cc nh
my x nghip x khi bi cng nghip vo khng kh lm nhim khng kh, khi tri
ma, cc cht nhim ny s ln vo trong nc ma cng gp phn lm nhim
ngun nc.
- Trang 25 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Hu qu chung ca tnh trng nhim nc l t l ngi cht do cc bnh lin
quan n nhim nc nh vim mng kt, tiu chy, ung th ngy cng tng ln.
Ngoi ra, t l tr em t vong ti cc khu vc b nhim ngun nc l rt cao.

CHNG 3
TNG QUAN V ASEN, THY NGN, SELEN, ANTIMON
3.1. ASEN [4]
Asen (thch tn) l mt kim gy ng c kht
ting v c nhiu dng th hnh: mu vng (phn t phi
kim) v mt vi dng mu en v xm ( kim). Ba dng
c tnh kim loi ca asen vi cu trc tinh th khc
nhau cng c tm thy trong t nhin (cc khong
vt asen sensu stricto v him hn l asenolamprit cng
parasenolamprit), nhng ni chung n hay tn ti di
Mt mu ln cha asen
t nhin

dng cc hp cht asenua v asenat.

Trng thi oxi ha ph bin nht ca n l -3 (asenua: thng thng trong cc


hp cht lin kim loi tng t nh hp kim), +3 (asenat (III) hay asenit v phn ln
- Trang 26 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
cc hp cht asen hu c), +5 (asenat (V): phn ln cc hp cht v c cha xy ca
asen n nh). Asen cng d t lin kt vi chnh n, chng hn to thnh cc cp AsAs trong sulfua hng hong (-As4S4) v cc ion As43- vung trong khong coban
asenua c tn skutterudit. trng thi oxi ha +3, tnh cht ha hc lp th ca asen
chu nh hng bi s c mt ca cp electron khng lin kt.
Tng qut
Tn, K hiu, S

asen, As, 33

Phn loi

kim

Nhm, Chu k, Khi

15, 4, p

Khi lng ring, cng 5727 kg/m, 3,5


B ngoi

mu xm kim loi
Tnh cht nguyn t

Khi lng nguyn t

74,92160(2) .v.

Bn knh nguyn t (calc.) 115 (114) pm


Bn knh cng ho tr

119 pm

Bn knh van der Waals

185 pm

Cu hnh electron

[Ar]3d104s24p3

e- trn mc nng lng

2, 8, 18, 5

Trng thi xi ha (xt)

5, 3, 1[1], -3 (axt nh)

Cu trc tinh th

hp mt thoi
Tnh cht vt l

Trng thi vt cht

rn

im nng chy

1.090 K (1.503 F)

im si

th 887 K (1.137 F)

Nhit nng chy

(xm) 24,44 kJ/mol

p sut hi

100 k Pa ti 874 K
Thng tin khc

m in

2,18 (thang Pauling)

Nhit dung ring

328,88 J/(kgK)

dn in

3x106 /m

dn nhit

50,2 W/(mK)

- Trang 27 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Nng lng ion ha

1. 947,0 kJ/mol
2. 1.798,0 kJ/mol
3. 2.735,0 kJ/mol

c trng ng ch
Asen v tnh cht ha hc rt ging vi nguyn t ng trn n l phtpho.
Tng t nh phtpho, n to thnh cc oxit kt tinh, khng mu, khng mi nh
As2O3 v As2O5 l nhng cht ht m v d dng ha tan trong nc to thnh cc
dung dch c tnh axit. Axit asenic (H3AsO4), tng t nh axit phtphoric, l mt axt
yu. Tng t nh phtpho, asen to thnh hirua dng kh v khng n nh, l
arsin (AsH3). S tng t ln n mc asen s thay th phn no cho phtpho trong
cc phn ng ha sinh hc v v th n gy ra ng c. Tuy nhin, cc liu thp hn
mc gy ng c th cc hp cht asen ha tan li ng vai tr ca cc cht kch thch
v tng ph bin vi cc liu nh nh l cc loi thuc cha bnh cho con ngi
vo gia th k 18.
Khi b nung nng trong khng kh, n b oxi to ra trioixt asen; hi t phn
ng ny c mi nh mi ti. Asen (v mt s hp cht ca asen) thng hoa khi b
nung nng p sut tiu chun, chuyn ha trc tip thnh dng kh m khng
chuyn qua trng thi lng. Trng thi lng xut hin p sut 20 tmtphe tr ln,
iu ny gii thch ti sao im nng chy li cao hn im si. Asen nguyn t c
tm thy nhiu dng th hnh rn: dng mu vng th mm, do nh sp v khng n
nh, v n lm cho cc phn t dng t din As 4 tng t nh cc phn t ca
phtpho trng. Cc dng mu en, xm hay 'kim loi' hi c cu trc kt tinh thnh
lp vi cc lin kt tri rng khp tinh th. Chng l cc cht bn dn cng vi nh
kim.
Hp cht
- Trang 28 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Cc hp cht quan trng nht ca asen l oxit asen (III), As 2O3, ('asen trng'),
opiment sulfua vng (hay th hong) (As2S3) v hng hong (As4S4), lc Paris,
asenat canxi, asenat hir ch (PbHAsO4). Ba hp cht cui cng tng c s dng
trong nng nghip lm thuc tr su v thuc c. Th hong v hng hong trc
y c dng lm thuc mu trong hi ha, hin nay b b do c tnh v kh
nng phn ng ca chng. Ngoi cc dng v c nh ni trn, asen cng tn ti trong
nhiu dng hu c trong mi trng. Asen v c v cc hp cht ca n, khi i vo
chui thc n, c trao i tch cc thnh dng t c hn ca asen thng qua qu
trnh methyl ha.
ng dng
- Asenat hir ch tng c s dng nhiu trong th k 20 lm thuc tr
su cho cc loi cy n qu. Vic s dng n i khi to ra cc tn thng no i vi
nhng ngi phun thuc ny. na cui th k 20, asenat methyl mononatri
(MSMA), mt dng hp cht hu c t c hi hn ca asen thay th cho vai tr
ca asenat hir ch trong nng nghip.
- Lc Scheele hay asenat ng, c s dng trong th k 19 nh l tc nhn
to mu trong cc loi bnh ko ngt.
- ng dng c nhiu e ngi nht i vi cng ng c l l trong x l g bng
asenat ng crm ha, cn gi l CCA hay tanalith.. Vic hp th trc tip hay gin
tip tro do vic t chy g x l bng CCA c th gy ra t vong ng vt cng
nh gy ra ng c nghim trng ngi; liu gy t vong ngi l khong 20 gam
tro.
- Trong cc th k 18, 19 v 20, mt lng ln cc hp cht ca asen c
s dng nh l thuc cha bnh, nh arsphenamin (bi Paul Ehrlich, iu tr giang
mai v bnh trng mi khoan) v trioxit asen (bi Thomas Fowler, iu tr ung th).

- Trang 29 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Axetoasenit ng c s dng nh l thuc nhum mu xanh lc di nhiu
tn gi khc nhau, nh 'Lc Paris' hay 'lc ngc bo'. N gy ra nhiu dng ng c
asen.
Cc ng dng khc:

Nhiu loi thuc tr su, cht c trong nng nghip.

S dng trong nui dng ng vt, c th l ti Hoa K nh l phng

php ngn nga bnh v kch thch pht trin.

Asenua gali l mt vt liu bn dn quan trong, s dng trong cc mch

tch hp (IC). Cc mch tch hp ny nhanh hn (nhng cng t tin hn) so vi cc


mch dng silic. Khng ging nh silic, n l khe h nng lng trc tip, v v th
c th s dng trong cc it laze v LED trc tip chuyn ha in thnh nh
sng.

Cng c s dng trong k thut m ng v pho hoa.

c tnh
Asen l mt cht rt c. C th cht ngay nu ung mt lng bng na ht
ng (bp). Nu b ng c cp tnh bi asen s c biu hin: kht nc d di, au
bng, nn ma, tiu chy, mch p yu, mt nht nht ri thm tm, b tiu v t
vong nhanh. Nu b nhim c asen mc thp, mi ngy mt t vi liu lng d
nh nhng trong thi gian di s gy: mt mi, bun nn v nn, hng cu v bch
cu gim, da sm, rng tc, st cn, gim tr nh, mch mu b tn thng, ri lon
nhp tim, au mt, au tai, vim d dy v rut, lm kit sc, ung th...
Ngi ung nc nhim asen lu ngy s c cc m sm mu trn thn th
hay u cc chi, nim mc li hoc sng ho da, gy sm v mt sc t, bnh Bowen
(biu hin u tin l mt phn c th ng, sau b chy nc v l lot). Bnh
sng ho da thng xut hin tay, chn, lng bn tay, gan bn chn - phn c th c
- Trang 30 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
xt nhiu hoc tip xc nh sng nhiu lu ngy s to thnh cc inh cng mu trng
gy au n. Bnh en v rng mng chn c th dn n hoi t, rng dn tng t
ngn chn. Tnh trng nhim c asen lu ngy cn c th gy ung th (gan, phi,
bng quang v thn) hoc vim rng, khp, gy bnh tim mch, cao huyt p.
nh hng c hi ng lo ngi nht ca asen ti sc kho l kh nng gy t
bin gen, ung th, thiu mu, cc bnh tim mch (cao huyt p, ri lon tun hon
mu, vim tc mch ngoi vi, bnh mch vnh, thiu mu cc b c tim v no), cc
loi bnh ngoi da (bin i sc t, sm da, sng ho, ung th da...), tiu ng, bnh
gan v cc vn lin quan ti h tiu ho, cc ri lon h thn kinh - nga hoc
mt cm gic chi v kh nghe. Sau 15 - 20 nm k t khi pht hin, ngi nhim
c thch tn s chuyn sang ung th v cht.

(Hu qu t nc ngm nhim asen v kim loi nng


ngun http://www.arsenfree.com)
Asen c u?
Asen l mt nguyn t khng ch c trong nc m cn c trong khng kh,
t, thc phm v c th xm nhp vo c th con ngi. iu tra s b c th
- Trang 31 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
khng nh nguyn nhn ch yu khin nc ngm nhiu vng thuc nc ta nhim
asen l do cu to a cht.
Tuy nhin, cng khng loi tr nhim l do tc ng ca con ngi nh gn
cc nh my ho cht, nhng khu vc dn t ng o v lp ging khng ng tiu
chun k thut khin cht bn, c hi b thm thu xung mch nc.
Gii hn cho php ca Arsenic trong nc
Nc ung ng chai (TCVN 6096:2004)

0.01mg/L

Nc cp sinh hot (TCVN 5502:2003)

0.01mg/L
0.05mg/L (loi A)

Nc thi cng nghip (TCVN 5945 2005)

0.1mg/L (loi B)
0.5 mg/L (loi C)

Cc thit b kim tra v kh asen trong nc

- Trang 32 Test th nhanh nc nhim Asen c


gi khong 38.000

Mt bnh kh arsen v tit trng


trong nc

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

3.2. THY NGN [5]


Thy ngn l mt kim loi chuyn tip nng
c nh bc, c dng lng khi nhit thng. Thy
ngn c s dng trong cc nhit k, p k v cc
thit b khoa hc khc.

Thng tin chung


Tn, K hiu, S

Thy ngn, Hg, 80

Dy ha hc

Kim loi chuyn tip

Nhm, Chu k, Khi

12 (IIB), 6, d
lng 13.579 kg/m3

T trng, cng

rn 39 C
15.600 kg/m3
1,5 Mohs

Mu

Trng bc
Cc thuc tnh

- Trang 33 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Khi lng nguyn t

200,59 u

Bn knh nguyn t (calc.)

150 (171) pm

Bn knh cng ha tr

149 pm

Bn knh van der Waals

155 pm

Cu hnh electron

[Xe]4f14 5d10 6s2

e- trn mc nng lng

2, 8, 18, 32, 18, 2

Trng thi xi ha (xt)

2, 1 (baz nh)

Cu trc tinh th

Lng tr xin

Cc thuc tnh vt l
Trng thi

Lng (nghch t)

Nhit nng chy

234,32 K (37,89 F)

Nhit si

629,88 K (674,11 F)

Th tch phn t

14,09 cm3/mol

Nhit bay hi

59,229 kJ/mol

Nhit nng chy

2,295 kJ/mol

im ba trng thi

234,32 K, 0,2 mPa

Vn tc m thanh

1407 m/s 20 C
Linh tinh

in m

2,00 (thang Pauling)

Nhit dung ring

140 J/(kgK)

dn in

1,041x106/.m

dn nhit

8,34 W/(mK)

Nng lng ion ha th nht 1007.1 kJ/mol


Nng lng ion ha th hai 1810 kJ/mol
Nng lng ion ha th ba

3300 kJ/mol

Cc ng v n nh nht
iso

NA

Bn r

DM DE MeV DP

Hg194 {TH}

444 y

0,040

Au194

Hg195 {TH}

9,9 h

1,510

Au195

Hg196 0,15%

n nh vi 116 ntron

- Trang 34 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Hg197 {TH}

64,14 h

Hg198 9,97%

Bn vi 118 ntron

0.600

Au197

Hg199 16,87% Bn vi 119 ntron


Hg200 23,1%

Bn vi 120 ntron

Hg201 13,18% Bn vi 121 ntron


Hg202 29,86% Bn vi 122 ntron
Hg203 {TH}

46,612 ngy -

Hg204 6,87%

Bn vi 124 ntron

0,492

Tl203

Thuc tnh
Thy ngn c tnh dn nhit km nhng dn in tt. N to ra hp kim vi
phn ln cc kim loi, bao gm vng, nhm v bc, ng nhng khng to vi st. Do
, ngi ta c th cha thy ngn trong bnh bng st. Telua cng to ra hp kim,
nhng n phn ng rt chm to ra telurua thy ngn. Hp kim ca thy ngn c
gi l hn hng.
Kim loi ny hot ng ha hc km hn km v cadmium. Trng thi oxi ha
ph bin ca n l +1 v +2. Rt t hp cht trong thy ngn tn ti c ha tr +3.
ng dng
Thy ngn c s dng ch yu trong sn xut cc ha cht, trong k thut
in v in t. N cng c s dng trong mt s nhit k. Cc ng dng khc l:

My o huyt p cha thy ngn ( b cm mt s ni).

Thimerosal, mt hp cht hu c c s dng nh l cht kh trng trong

vaccin v mc xm (Thimerosal in vaccines).

Phong v k thy ngn, bm khuych tn, tch in k thy ngn v nhiu

thit b phng th nghim khc. L mt cht lng vi t trng rt cao, Hg c s


dng lm kn cc chi tit chuyn ng ca my khuy dng trong k thut ha hc.

- Trang 35 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

im ba trng thi ca thy ngn, -38,8344 C, l im c nh c s

dng nh nhit tiu chun cho thang o nhit quc t (ITS-90).

Trong mt s n in t.

Hi thy ngn c s dng trong n hi thy ngn v mt s n kiu

"n hunh quang" cho cc mc ch qung co. Mu sc ca cc loi n ny ph


thuc vo kh np vo bng.

Thy ngn c s dng tch vng v bc trong cc qung sa khong.

Thy ngn vn cn c s dng trong mt s nn vn ha cho cc mc

ch y hc dn tc v nghi l. Ngy xa, cha bnh tc rut, ngi ta cho bnh


nhn ung thy ngn lng (100-200 g). trng thi kim loi khng phn tn, thy
ngn khng c v c t trng ln nn s chy trong h thng tiu ha v gip thng
rut cho bnh nhn.
Cc s dng linh tinh khc: chuyn mach in bng thy ngn, in phn vi
cathode thy ngn sn xut NaOH v clo, cc in cc trong mt s dng thit b
in t, pin v cht xc tc, thuc dit c (ngng s dng nm 1995), thuc tr su,
hn hng nha khoa, pha ch thuc v knh thin vn gng lng.
Hp cht
Cc mui quan trng nht l:

Clorua thy ngn (I) (calomen v i khi vn c s dng trong y hc).

Clorua thy ngn (II) (l mt cht c tnh n mn mnh, thng hoa v l

cht c cc mnh).

Fulminat thy ngn, (ngi n s dng rng ri trong thuc n).

Sulfua thy ngn (II) (mu thn sa l cht mu cht lng cao).

Selenua thy ngn (II) cht bn dn.


- Trang 36 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Telurua thy ngn (II) cht bn dn.

Telurua cadmi thy ngn l nhng vt liu dng lm u d tia hng ngoi.

Cc hp cht hu c ca thy ngn cng l quan trng.


Vn mi trng
Thy ngn i vo mi trng nh mt cht gy nhim t cc ngnh cng
nghip khc nhau:

Cc x nghip s dng than lm nhin liu l ngun ln nht (40% trong

kh thi ca M nm 1999, tuy nhin gim khong 85%).

Cc cng ngh trong cng nghip:


o

Sn xut clo, thp, phtphat & vng.

Luyn kim.

Sn xut & sa cha cc thit b in t.

Vic t hay vi lp cc cht thi th.

Cc ng dng y hc, k c trong qu trnh sn xut v bo qun vacxin.


o

Nha khoa.

Cng nghip m phm.

Cc th nghim trong phng th nghim lin quan n cc hp cht ca thy

ngn v lu hunh.
Thy ngn cng i vo mi trng theo ng x l mt s sn phm no .
Cc sn phm c cha thy ngn bao gm: cc b phn ca t, pin, n hunh
quang, cc sn phm y t, nhit k v my iu nhit. V cc vn lin quan ti sc
khe, cc c gng gim s dng cc cht c l ct gim hoc loi b thy ngn trong
cc sn phm .
- Trang 37 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Cc hiu ng sc khe & mi trng
Thy ngn nguyn t lng l t c, nhng hi, cc hp cht v mui ca n l
rt c v l nguyn nhn gy ra cc tn thng no v gan khi con ngi tip xc,
ht th hay n phi vi triu chng run ry, kh khn trong din t, gim st tr
nh ... v nng hn na c th gy t lit, nghnh ngng, ni lp, thao cung. Nu
nhim c thy ngn qua ng n ung vi liu lng cao, mt thi gian sau (c th
t 10 - 20 nm) s gy t vong.
Nguy him chnh lin quan n thy ngn nguyn t l STP, thy ngn c
xu hng b oxi ha to ra oxit thy ngn - khi b rt xung hay b lm nhiu lon,
thy ngn s to thnh cc ht rt nh, lm tng din tch tip xc b mt mt cch
khng khip.
Thy ngn l cht c tch ly sinh hc rt d dng hp th qua da, cc c quan
h hp v tiu ha. Cc hp cht v c t c hn so vi hp cht hu c ca thy
ngn. Cho d t c hn so vi cc hp cht ca n nhng thy ngn vn to ra s
nhim ng k i vi mi trng v n to ra cc hp cht hu c trong cc c th
sinh vt.
Mt trong nhng hp cht c nht ca n l imtyl thy ngn, l c n
n mc ch vi micrlt ri vo da c th gy t vong. Mt trong nhng mc tiu
chnh ca cc cht c ny l enzym pyruvat dehirgenat (PDH). Enzym b c ch
hon ton bi mt vi hp cht ca thy ngn, thnh phn gc axt lipoic ca phc
hp a enzym lin kt vi cc hp cht rt bn v v th PDH b c ch.
Thng qua qu trnh tch ly sinh hc mtyl thy ngn nm trong chui thc
n, t n mc tch ly cao trong mt s loi nh c ng. S ng c thy ngn i
vi con ngi l kt qu ca vic tiu th lu di mt s loi lng thc, thc phm
no . Cc loi c ln nh c ng hay c kim thng thng cha nhiu thy ngn
hn cc loi c nh, do thy ngn tch ly tng dn theo chui thc n.
- Trang 38 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Cc ngun nc tch ly thy ngn thng qua qu trnh xi mn ca cc
khong cht hay trm tch t kh quyn. Thc vt hp th thy ngn khi m t nhng
c th thi ra trong khng kh kh. Thc vt v cc trm tch trong than c cc nng
thy ngn dao ng mnh.
tyl thy ngn l sn phm phn r t cht chng khun thimerosal v c hiu
ng tng t nhng khng ng nht vi mtyl thy ngn.
Gii hn cho php ca thy ngn trong nc
Nc ung ng chai (TCVN 6096:2004)

0.001mg/L

Nc cp sinh hot (TCVN 5502:2003)

0.001mg/L
0.005mg/L (loi A)

Nc thi cng nghip (TCVN 5945:2005)

0.01mg/L (loi B)
0.01 mg/L (loi C)

3.3. SELEN [6]


Selen l mt phi kim, v mt ha hc rt
ging vi lu hunh v telua, trong t nhin rt
him thy dng nguyn t. i vi sinh vt, n
l c hi khi liu lng ln, nhng khi liu
Selen nguyn t trong cc dng
th hnh khc nhau: en, xm, .

lng du vt th n l cn thit cho chc nng


ca t bo.

Selen c c lp tn ti di vi dng khc nhau, n nh nht trong s l


dng bn kim loi (bn dn) mu xm nh ta v nng, v mt cu trc l chui
polyme tam gic. N dn in di nh sng tt hn trong bng ti v c s dng
trong cc t bo quang in. Selen cng tn ti trong nhiu dng khng dn in: th
hnh mu en tng t nh thy tinh, cng nh mt vi dng kt tinh mu c
to ra t cc phn t vng 8 nguyn t, tng t nh lu hunh.

- Trang 39 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Selen c tm thy trong cc qung sulfua nh pyrit, trong n thay th
phn no cho lu hunh trong cht nn ca qung. Cc khong vt cha selenua hay
selenat cng c bit ti nhng chng kh him.

Tng qut
Tn, K hiu, S

selen, Se, 34

Phn loi

phi kim

Nhm, Chu k, Khi

16, 4, p

Khi lng ring, cng (xm) 4810 kg/m, 2,0


B ngoi

xm en nh kim

Tnh cht nguyn t


Khi lng nguyn t

78,96(3) .v.

Bn knh nguyn t (calc.) 115 (103) pm


Bn knh cng ho tr

116 pm

Bn knh van der Waals

190 pm

Cu hnh electron

[Ar]3d104s24p4

e- trn mc nng lng

2, 8, 18, 6

Trng thi xi ha (xt)

6, 4, 2, 1[1], -2 (axt mnh)

Cu trc tinh th

lc gic

Tnh cht vt l
Trng thi vt cht

rn

im nng chy

494 K (430 F)

im si

958 K (1.265 F)

Nhit bay hi

95,48 kJ/mol

Nhit nng chy

(xm) 6,69 kJ/mol

p sut hi

100 k Pa ti 958 K

Vn tc m thanh

3350 m/s ti 293 K

Thng tin khc


m in

2,55 (thang Pauling)

Nhit dung ring

321,20 J/(kgK)

dn nhit

0,519 W/(mK)

- Trang 40 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Nng lng ion ha

1. 941,0 kJ/mol
2. 2.045,0 kJ/mol
3. 2.973,7 kJ/mol

Ph bin
Selen c mt t nhin trong mt s dng hp cht v c, bao gm selenua,
selenat v selenit. Trong t, selen thng xut hin trong cc dng ha tan nh
selenat (tng t nh sulfat), v b thm thu rt d dng vo cc con sng do nc
chy.
Selen c vai tr sinh hc v c tm thy trong cc hp cht hu c nh
dimethyl selenua, selenomethionin, selenocystein v methylselenocystein. Trong cc
hp cht ny selen ng vai tr tng t nh lu hunh.
Selen c sn xut ph bin nht t selenua trong nhiu loi qung sulfua,
chng hn t cc khong vt ca ng, bc hay ch. N thu c nh l ph phm ca
qu trnh ch bin cc loi qung ny, t bn ant trong tinh lc ng v bn t cc
bung ch trong cc nh my sn xut axt sulfuric. Cc loi bn ny c th c x
l bng nhiu cch thu c selen t do.
Cc ngun t nhin cha selen bao gm cc loi t giu selen, v selen c
tch ly sinh hc bi mt s thc vt c c nh cc loi cy h u trong cc chi
Oxytropis hay Astragalus. Cc ngun cha selen do con ngi to ra c vic t chy
than cng nh khai thc v nung chy cc loi qung sulfua.

Selen v sc khe
Mc d c c khi dng liu lng ln, nhng selen li l cht vi dinh dng
thit yu cho ng vt. thc vt, n c nh l khong cht ng ngoi cuc, i khi
vi t l gy c trong c cho gia sc (mt s loi thc vt c th tch ly selen nh l
phng tin phng ng chng li vic ng vt n chng, nhng cc loi thc vt
- Trang 41 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
khc nh cc loi ni trn y li cn selen v s tng trng ca chng ch ra s hin
din ca selen trong t). N l thnh phn hp thnh ca cc axt amin bt thng
nh selenocystein v selenomethionin. ngi, selen l cht dinh dng du vt vi
chc nng ca ph phi t cho vic kh cc enzym chng xi ha nh cc glutathion
peroxidaza v mt vi dng nht nh ca thioredoxin reductaza tm thy ng vt
v mt s thc vt (enzym ny c trong mi sinh vt sng, nhng khng phi mi
dng ca n trong thc vt u cn selen).
Selen cng ng vai tr trong chc nng ca tuyn gip bng cch tham d
nh l ph phi t cho ba hoc mn tuyn gip bit l cc deiodinaza.
Selen cho dinh dng n t cc loi qu hch, ng cc, tht, c v trng. Qu
hch Brasil (Bertholletia excelsa) l ngun dinh dng thng thng giu selen nht
(mc d n ph thuc vo kiu t, do qu hch Brasil khng i hi nhiu selen cho
nhu cu ca chnh n). Cc hm lng cao c trong nhiu dng thc phm nh thn,
cua v tm hm, theo trt t nh cp.
c tnh
Mc d selen l cht vi dinh dng thit yu nhng n li c c tnh nu dng
thi qu. Vic s dng vt qu gii hn trn ca DRI l 400 microgam/ngy c th
dn ti ng c selen. Cc triu chng ng c selen bao gm mi hi ca ti trong
hi th, cc ri lon ng tiu ha, rng tc, bong, trc mng tay chn, mt mi,
kch thch v tn thng thn kinh. Cc trng hp nghim trng ca ng c selen
c th gy ra bnh x gan, ph phi v t vong.
Selen nguyn t v phn ln cc selenua kim loi c c tnh tng i thp do
hiu lc sinh hc thp ca chng. Ngc li, cc selenat v selenit li cc c hi, v
c cc tc ng tng t nh ca asen. Selenua hir l mt cht kh c tnh n mn
v cc k c hi. Selen cng c mt trong mt s hp cht hu c nh dimethyl
selenua, selenomethionin, selenocystein v methylselenocystein, tt c cc cht ny
- Trang 42 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
u c hiu lc sinh hc cao v c hi khi liu lng ln. Selen kch thc nano c
hiu lc tng ng, nhng c tnh thp hn nhiu.
Ng c selen t cc h thng cung cp nc c th xy ra khi cc dng chy
ca cc h thng ti tiu mi trong nng nghip chy qua cc vng t thng thng
l kh cn v km pht trin. Qu trnh ny lm thm thu cc hp cht selen t nhin
v ha tan trong nc (nh cc selenat) vo trong nc, chng sau c th tch ly
m c hn trong cc vng "t m t" mi khi nc bay hi i. Nng selen cao
sinh ra theo kiu ny c tm thy nh l nguyn nhn gy ra mt s ri lon bm
sinh nht nh chim sng trong cc vng t m t.
ng dng phi sinh hc
Ha hc
Selen l cht xc tc trong nhiu phn ng ha hc v c s dng rng ri
trong nhiu phn ng tng hp ha hc trong cng nghip ln trong phng th
nghim. N cng c s dng rng ri trong xc nh cu trc ca cc protein hay
axt nucleic bng tinh th hc tia X.
Sn xut v vt liu
ng dng ln nht ca selen trn ton th gii l sn xut thy tinh v vt liu
gm, trong n c dng to ra mu cho thy tinh, men thy tinh v men
gm cng nh loi b mu t thy tinh bng cch trung ha sc xanh lc do cc
tp cht st (II) to ra.
Selen c s dng cng bitmut trong hn ch cho ng thau thay th cho
ch c hi hn. N cng c dng trong vic ci thin sc khng mi mn ca cao
su lu ha.
Cng nghip in t

- Trang 43 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Do cc tnh cht quang voltaic v quang dn nn selen c s dng trong k
thut photocopy, cc t bo quang in, thit b o sng v t bo nng lng mt
tri. N tng c s dng rng ri trong cc b nn dng. Cc ng dng ny phn
ln b thay th bng cc thit b dng silic hay trong qu trnh b thay th. Ngoi l
ng ch nht l trong cc thit b bo v in, trong kh nng truyn ti dng
in cng ln ca cc b trit dng dng selen lm cho n ng gi hn so vi
cc in tr bin thin dng xt kim loi.
Nhip nh
Selen c dng trong k thut to sc thi trong nhip nh, v n c bn
nh l cht to sc thi bi nhiu nh sn xut giy nh nh Kodak v Fotospeed.
ng dng sinh hc
Y hc
SeS2, thc t l disulfua selen hay sulfua selen (IV), l thnh phn hot ha
trong mt vi loi du gi u chng gu. Hiu ng ca thnh phn hot ha l git
cht nm da u Malassezia. Thnh phn hot ha ny cng c dng trong m
phm dng cho da iu tr nm da Tinea do nhim cc loi nm chi Malassezia.
Dinh dng
Selen c s dng rng ri trong iu ch vitamin v cc cht b sung dinh
dng khc, vi liu nh (thng l t 50 ti 200 microgam trn ngy cho ngi ln).
Mt i loi c lm thc n cho gia sc cng c tng cng selen.

3.4. ANTIMON [7]


Antimon l mt kim, c 4 dng th hnh.
Dng n nh nht ca antimon l dng kim mu
trng-lam. Cc dng mu vng v en l cc phi kim
Mt ng ng antimon mu en

- Trang 44 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
khng n nh. Antimon c s dng trong mi lp chng chy, sn, gm, men, mt
lot cc hp kim, cng nghip in t, cao su.
Tng qut
Tn, K hiu, S

antimon, Sb, 51

Phn loi

kim

Nhm, Chu k, Khi

15, 5, p

Khi lng ring, cng 6.697 kg/m, 3,0


B ngoi

xm bng bc
Tnh cht nguyn t

Khi lng nguyn t

121,760(1) .v.

Bn knh nguyn t (calc.) 145 (133) pm


Bn knh cng ho tr

138 pm

Cu hnh electron

[Kr]4d105s25p3

e- trn mc nng lng

2, 8, 18, 18, 5

Trng thi xi ha (xt)

-3, 3, 5 ()

Cu trc tinh th

hp mt thoi
Tnh cht vt l

Trng thi vt cht

rn

im nng chy

903,78 K (1.167,13 F)

im si

1.860 K (2.889 F)

Trng thi trt t t

khng c s liu

Nhit bay hi

193,43 kJ/mol

Nhit nng chy

25,23 kJ/mol

p sut hi

100 k Pa ti 1.858 K

Vn tc m thanh

3.420 m/s ti 293 K

- Trang 45 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Thng tin khc
m in

2,05 (thang Pauling)

Nhit dung ring

207,21 J/(kgK)

dn in

2,40x106 /m

dn nhit

24,4 W/(mK)

Nng lng ion ha

1. 834,0 kJ/mol
2. 1.594,9 kJ/mol
3. 2.440,0 kJ/mol

Tnh cht
Antimon dng nguyn t l mt cht rn kt tinh d nng chy, cng mu
trng bc c tnh dn in v dn nhit km v bay hi nhit thp. L mt kim,
antimon tng t nh kim loi b ngoi v nhiu tnh cht c l, nhng khng phn
ng nh cc kim loi v mt ha hc. N cng b tn cng bi cc axt v cc halogen
theo phn ng oxi ha-kh. Antimon v mt s hp kim ca n l bt thng ch
chng gin n ra khi ngui i. Antimon v mt ha a l c phn loi nh l a
ng (chalcophile), thng xut hin cng lu hunh v cc kim loi nng nh ch,
ng v bc.
c tnh v ph bin ca antimon trong lp v Tri t nm trong khong
0,2-0,5 ppm.

ng dng
Antimon c s dng ngy cng gia tng trong cng nghip bn dn sn
xut cc it, cc thit b pht hin bng tia hng ngoi v cc thit b dng hiu ng
Hall. dng hp kim, n tng mnh cng v sc bn c hc ca ch. ng dng
quan trng nht ca antimon l tc nhn lm cng trong ch lm cc loi c quy.
Cc ng dng bao gm:
- Trang 46 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

c quy

Hp kim chng ma st

Hp kim c ch in

n cho cc v kh cm tay v n la

Lp bc cho si cp

Cc loi thuc phng tr sinh vt nguyn sinh k sinh

Hn ch

Hn thic mt vi loi thic hn "khng ch" cha 5% Sb

Cc vng bi chnh v ln trong ng c t trong (di dng hp kim)

tng c dng iu tr bnh sn mng (hay bnh Schistosoma, ngy

nay Praziquantel l loi thuc thay th c s dng rng khp)

c dng trong cc my in kiu lin

Cc hp cht ca antimon trong dng cc oxit, sulfua, antimonat natri, triclorua


antimon c dng lm cc vt liu chng chy, men gm, thy tinh, sn, s. Trioxit
antimon l hp cht quan trng nht ca antimon v s dng ch yu trong cc vt
liu ngn la. Cc ng dng ngn la bao gm cc th trng nh qun o v chi
tr em, cc lp bc gh ngi trong t v my bay. N cng c dng trong cng
nghip sn xut composit si thy tinh nh l ph gia cho nha polyeste cho cc mt
hng nh lp che bc ng c my bay hng nh. Nha ny s bt chy khi c la
nhng n s b dp tt ngay khi la b loi b. Sulfua antimon l mt trong cc thnh
phn ca dim an ton.
Trong thp nin 1950, cc ht nh hp kim ch-antimon c s dng lm cc
pht v cc thu cho cc tranzito bin hp kim kiu NPN.

- Trang 47 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Sulfua t nhin ca antimon, gi l stibnit, c bit n v s dng t thi
k c i nh l thuc v m phm. Stibnit vn cn c s dng mt vi quc gia
ang pht trin nh l thuc. Antimon tng c s dng iu tr bnh sn
mng. Antimon t gn n vi cc nguyn t lu hunh trong mt vi loi enzym nht
nh m c c th ngi ln sinh vt k sinh u cn. Mt lng nh c th git cht
sinh vt k sinh m khng gy ra cc thng tn cho bnh nhn. Antimon v cc hp
cht ca n c s dng trong mt vi loi thuc th y nh Anthiomalin hay
thiomalat antimon liti, c dng nh l tc nhn iu ha v lm mt lng ng
vt nhai li (tru, b). Antimon c hiu ng nui v iu ha cc m keratin (sng)
ha, t nht l ng vt. Thuc gy nn Tartar l mt loi thuc c cha antimon
c dng nh l thuc chng sn mng. Cc diu tr ch yu c s tham gia ca
antimon gi l thuc antimon.
Cc loi dc phm da trn antimon nh Allopurinol, Meglumin, cng c
coi l cc loi thuc cn dng iu tr st rui ct (do sinh vt nguyn sinh chi
Leishmania gy ra) gia sc. Khng may, mc d c ch dn iu tr thp, nhng
thuc ny thm thu km qua xng ng, ni m mt s sinh vt gy bnh
Leishmania sng, v v th vic cha tr bnh c bit khi ni tng l rt kh.
Phng nga
Antimon v nhiu hp cht ca n l c hi. V mt lm sng, ng c
antimon tng t nh ng c asen. cc liu lng nh, antimon gy ra au u,
hoa mt, trm cm. Cc liu lng ln gy ra bun nn nhiu v thng xuyn v c
th gy t vong sau vi ngy.
Mt nghin cu pht hin thy antimon c th thm thu t cc chai ng nc
bng PET, nhng mc thp hn cc ch dn dnh cho nc ung. Cc ch dn ph
bin l:

WHO, 20 g/l
- Trang 48 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Nht Bn, 15 g/l

EPA Hoa K, Yt Canada v B Mi trng Ontario, 6 g/l

B Mi trng Lin bang c, 5 g/l

Gii hn cho php ca antimon trong nc


Nc ung ng chai (TCVN 6096:2004)

0.005mg/L

Nc cp sinh hot (TCVN 5502:2003) 0.005mg/L


0.005mg/L (loi A)
Nc thi cng nghip (TCVN 5945:2005)

0.01mg/L (loi B)
0.01 mg/L (loi C)

PHN II: CC PHNG PHP S DNG

- Trang 49 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

CHNG 1
PHNG PHP LY MU, TIP NHN
V TH NGHIM MU
1.1. GII THIU
- Thc cht ca vic ly mu l thu thp mt phn vt cht trong mt th tch
va , x l, vn chuyn v phng th nghim kp lc khi cht lng mu cha thay
i. Kt qu sau cng khng ch ph thuc vo cng vic phn tch m cn ph thuc
ngay t thi im ly mu, cch bo qun mu khi chuyn ch v lu tr mu. Vic
ly mu phi thn trng m bo yu cu c bn, tiu biu c tnh ca nc ti
ni kho st.
1.2. PHNG THC LY MU
- Cc chai ly mu cn c dn nhn, ghi y cc chi tit nh: a im,
ngy gi, khong cch b, su, tn ngi ly mu, kt qu o c ti ch, nhn
xt s b, nhit , mu sc, mi v, hon cnh, v tr ly mu.
- Trong qu trnh ly mu, phng th nghim ly bin bn ly mu, ghi li cc
yu t kim sot mi trng theo quy nh v cc thng tin lin quan khc.
- Trc khi ly mu chai cn c sc k 2 n 3 ln vi nc mu trc khi
ng mu. iu cn ch l chai ly mu khng c s dng ng cc cht lng
khc.
- Nu ly mu t h thng phn phi nc ca cc thnh ph th cc vi nc
cn phi x trong mt thi gian ngn cht r st c loi b ht, nh th mi m
bo ly mu c tiu biu, trung thc cho phm cht nc cung cp t nh my m
khng b nh hng t ng ng hoc vi (nu c).

- Trang 50 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- Nu mu nc l nc ging, lng nc ban u c bm ln khng th
s dng phn tch m cn my bm chy mt thi gian ngn ri mi ly mu,
nhm loi b nc ban u cn ng trong cnh qut hay ng dn, nu c th cn
ghi li lu lng bm khi ly mu.
- Nu ly mu sng, h, knh, rch cn ghi chiu su, khong cch b,
khong cch ngun nc thi, lu lng ma Do ty vo mc ch th nghim
m ta chn mu nc hn hp hay nhiu mu ring bit. i vi mu hn hp, tt
nht nn chn v tr gia dng v nhiu mt su khc nhau, t trn mt thong
xung tn y; vi loi mu ring bit s ty vo mc ch th nghim m chn v tr
dc 2 ven b hay gia dng v c su trung bnh.
- i vi mu nc ao h cc mc ch th nghim s quyt nh phng thc
ly mu v nc ao h thay i lin tc theo ma, gi, su, lu lng, ngy m, v
tr v cc iu kin a phng khc.
- c bit vi nc thi, nng cht bn cn thay i theo gi sinh hot, gi
sn xut cao im ca nh my, sn phm, lu lng, mc pha long, kh nng t
sch ha ca dng nc, hiu nng ca h thng th nu c. Do mi mu tng hp
tt nht nh gi s nhim xung quanh vng, trng hp ny mu c th ly
khong 125ml, cng v tr nhng thi im khc nhau, cch khong 5-10 pht v
trn thnh mt mu duy nht. Cc xt nghim c bit, cn thm ha cht bo qun t
u.
1.3. THC HIN TIP NHN V TH NGHIM MU
1.3.1. Kim nghim vin c phn cng nhn mu:

Nhn mu t b phn giao dch khch hng, vic giao nhn mu c

ghi nhn bng vn bn.

Thc hin m t mu ngoi quan mu, so snh i chiu lng mu thc

t v phiu yu cu ca khch hng. Ghi nhn m t mu theo bng m t mu.


- Trang 51 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Cc trng hp mu h hng, thiu mu khng ph hp cho phn tch

th phn nh ngay vi b phn giao dch khch hng ng thi thng bo cho Ph
trch phng tip tc phi hp x l.

Chuyn mu cho Ph trch phng (hoc ngi c u quyn).

1.3.2. Ph trch phng (hoc ngi c u quyn):

nh gi, xem xt s ph hp gia mu nhn c v cc thng tin yu

cu th nghim ca khch hng, chuyn tr b phn giao dch khch hng cc mu


th, yu cu khng ph hp.

Trao i vi khch hng khi trong cc trng hp cn thit: phng php

th nghim, mc ch s dng kt qu th nghim.

Phn cng th nghim da trn nng lc ca Kim nghim vin.

1.3.3. Kim nghim vin

Thc hin th nghim theo hng dn cng vic hoc phng php th ph

X l kt qu v vit bo co th nghim, Kim nghim vin c trch

hp.

nhim t kim tra v k tn vo bn bo co xc nhn rng php th nghim


c thc hin theo ng yu cu quy nh.

Gi li mu sau khi th nghim.

1.3.4. Trng nhm (hoc ngi c u quyn)

Kim tra li tnh y v chnh xc ca kt qu (hon tr bo co th

nghim cho Kim nghim vin nu thy nghi ng hoc sai st hoc yu cu th
nghim li, s dng phng thc kim tra cho khi thy cn thit).

K tn xc nhn vo kt qu th nghim.

Chuyn cho ngi nh my.


- Trang 52 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
1.3.5. Ph trch phng (hoc ngi c u quyn)

Xem xt ton b kt qu th nghim (kt qu th nghim, m s hp

ng v yu cu th nghim li, s dng phng thc kim tra cho khi thy cn
thit).

Quyt nh vic lu mu hoc tr mu lu v cho B phn giao dch khch

hng nu c yu cu.

K kt qu v chuyn cho phng H tr k thut trnh k.

1.4. THC HIN M BO CHT LNG CHO TH NGHIM MU


1.4.1. X l mu:
Cc mu th nghim nu khng x l kp trong ngy th cc kim nghim vin
phi bo qun trong mi trng acid nitric (2ml/100ml mu), nhit mt c my
iu ha.
1.4.2. La chn phng php th:

Phng php th phi ph hp vi bn cht mu v mc ch s dng vi

ca khch hng (so snh vi qui chun)

iu kin thc t ti phng th nghim phi p ng yu cu ca phng

php th.

Cc thay i phng php th do khch hng yu cu phi do Ph trch

phng (hoc ngi c y quyn) trao i trc tip v c s ng thun ca


khch hng.
1.4.3. m bo cht lng th nghim:

Thit b o c dung dch/ mu chun km theo th phi c kim tra mi

ngy hoc mi khi s dng bng dung dch/ mu chun km theo (pH, cn ).

- Trang 53 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Tun th ng cc yu cu kim sot cht lng (nu c) trong hng dn

th nghim c lin quan.

S dng mu kim sot cht lng (QC) cho cc php th tri qua nhiu

giai on chun b nhm kim sot qu trnh trong tng l th nghim mu. Gi tr
nh gi thng qua hiu sut thu hi. Thng thng hiu sut thu hi cho phn tch
hm lng mg/kg trong khong 70 -120 %. Lp control chart sau khi p dng khong
20 mu (QC).

Cc thit b d b tri nn nh quang ph AAS, ICP phi c ci t kim

tra chun khong 20 mu phn tch nhm kim tra v ti lp iu kin phn tch
nh ban u.

Yu t mi trng phi c kim sot ti nhng v tr nhy cm (t

chun), cc phng cha thit b phn tch nu thit b khng c yu cu nghim v


nhit hoc t b nhit th khng cn kim sot nhit nhng phi c lp t my
iu ha to thng thong v nhit thp (<30oC).
1.4.4. Bo qun mu sau th nghim:

Thng thng tt c cc mu sau khi th nghim v ban hnh kt qu cho

khch hng nu khng c yu cu c bit s c chuyn xung kho bo qun mu.


Trng hp khch hng c yu cu bo qun trong thi gian di, mu kim tra nh
nc th Ph trch phng s c lu , nu khng thi gian bo qun ti kho tun th
cc qui nh ti TTTN 03, qui nh ca kho.

Cc phn mu c bo qun ti phng th nghim trong iu kin nh

trong qu trnh cho th nghim trong thi gian 15 ngy nu khng c yu cu th


nghim li ca khch hng. Thanh l mu c thc hin nh k hng thng hoc khi
t cha y sm.

Vic chuyn mu xung kho lu, do nhn vin h tr thc hin v c

thc hin thng xuyn vi tn xut 2 ln/ tun v c theo di bng vn bn.
- Trang 54 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

LU KIM SOT QU TRNH TH NGHIM MU


Kim nghim vin

Nhn mu t
B phn giao dch

Ph trch phng

Xem xt s ph hp
ca mu v s H,
lng mu, vo s

Ph trch phng/
Cn b cht lng

Phn cng thc hin

Kim nghim vin

Th nghim mu
Bo co kt qu th nghim

Trng nhm

Ph trch phng/
Cn b cht lng

Ph trch phng/
Cn b cht lng

Kim tra bo co
th nghim, kt qu

B phn giao dch


(P. H tr k thut)

Khng ph hp

Phng php th
Theo biu mu sn c

X l theo
M01 TT05
(nu cn thit)

Vit kt qu th nghim,
vo s v chuyn nh my

Kim tra ton b h s.


Quyt nh vic lu mu
K tn

- Trang 55 -

Tr mu lu (nu c)

X l theo
M01 TT05
(nu cn thit)

P. H tr k thut
Trnh k

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

CHNG 2
PHNG PHP QUANG PH HP THU NGUYN T AAS
2.1. S XUT HIN CA PH HP THU NGUYN T
Nh chng ta bit, vt cht c cu to bi nhng nguyn t l phn t
nh nht cn c gi c tnh cht ca nguyn t. Nguyn t li bao gm ht nhn
nguyn t v cc in t, chuyn ng xung quanh khng gian ca ht nhn. Trong
iu kin bnh thng nguyn t khng thu hay pht ra nng lng di dng cc bc
x. Lc ny nguyn t tn ti trng thi c bn. l trng thi bn vng v ngho
nng lng nht ca nguyn t. Nhng khi trng thi hi nguyn t t do, nu ta
chiu mt chm tia sng c nhng bc sng (tn s) xc nh vo m hi nguyn t
th cc nguyn t t do s hp th cc bc x c bc sng nht nh ng ng vi
nhng tia bc x m n c th pht ra c trong qu trnh pht x. Lc nguyn t
nhn nng lng di dng cc tia bc x v n chuyn ln cc trng thi kch
thch c nng lng cao hn trng thi c bn. l tnh cht c trng ca nguyn
t trng thi hi. Qu trnh c gi l qu trnh hp th nng lng ca nguyn
t. Ph sinh ra trong qu trnh ny c gi l ph hp th nguyn t.
Nu gi nng lng ca tia sng b nguyn t hp th l E th chng ta c
E = ( Em Eo) = h

Hay l E

h.c

(1.1)
(1.2)

Trong Eo v Em l nng lng ca nguyn t trng thi c bn v trng


thi kch thch m ; h l hng s plank; c l tc ca nh sng trong chn khng ; v
l d di sng ca vch ph hp th.

- Trang 56 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Nh vy ng vi mi gi tr nng lng Ei m nguyn t hp th ta s c
mt vch ph hp th vi di sng . Ngha l ph hp th ca nguyn t cng l
ph vch.
Nhng nguyn t khng hp th tt c cc bc x m n c th pht ra c
trong qu trnh pht x. Qu trnh hp th ch xy ra i vi cc vch ph nhy, cc
vch c trng ca cc nguyn t. Cho nn i cc vch ph qu trnh hp th v
pht x l hai qu trnh ngc nhau. Theo phng trnh (1.1), nu gi tr nng lng
E l dng ta c qu trnh pht x, ngc li gi tr E l m ta c qu trnh hp

th. Chnh v th m ty theo tng iu kin c th ca ngun nng lng dng


nguyn t ha mu m qu trnh no xy ra l chnh.
Trong php o ph hp th nguyn t, m hi nguyn t ca mu trong ngn
la hay trong cuvet graphite l mt trng hp th bc x (hp th nng lng). Phn
t hp th nng lng ca tia bc x l cc nguyn t t do v cc thnh phn khc
(cc phn t cha phn ly) trong m hi . Do mun c ph hp th trc ht
phi to ra c m hi nguyn t t do, v sau chiu vo mt chm tia sng c
nhng bc sng xc nh ng vi cc tia pht x nhit ca nguyn t cn nghin
cu. Khi cc nguyn t t do s hp th nng lng v to ra ph hp thu nguyn
t ca n.

- Trang 57 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Em

E0
Pht x

Hnh: Cc chuyn di nng lng


2.2. NGUYN TC CA PHP O
Phng php phn tch da trn c s o ph hp th nguyn t ca mt
nguyn t c gi l php o ph hp th nguyn t (php o ASS). C s l thuyt
ca php o ny l s hp th nng lng (bc x n sc) ca nguyn t t do
trong trng thi hi (kh) khi chiu chm tia bc x qua m hi ca nguyn t y
trong mi trng hp th. V th mun thc hin c php o ph hp th nguyn t
cn phi tun th cc nguyn tc sau:
a> Chn cc iu kin v mt lot trang b ph hp chuyn mu phn tch
t trng thi ban u (rn hay dung dch) thnh trng thi hi ca cc nguyn t t do.
l qu trnh nguyn t ha mu. Nhng trang b thc hin qu trnh ny c
gi l h thng nguyn t ha mu (dng c nguyn t ha mu). Nh chng ta
c c m hi ca cc nguyn t t do ca mu phn tch. m hi ny chnh l
mi trng hp th bc x v sinh ra ph hp th nguyn t.
- Trang 58 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
b> Chiu chm tia sng pht x ca nguyn t cn phn tch qua m hi
nguyn t va iu ch c trn. Cc nguyn t ca nguyn t cn xc nh trong
m hi s hp th nhng tia bc x nht nh v to ra ph hp th ca n. y,
phn cng ca chm tia sng b mt lot nguyn t hp th l ph thuc vo
nng ca n trong mi trng hp th. Ngun cung cp chm tia pht x ca
nguyn t cn nghin cu c gi l ngun pht bc x n sc hay bc x cng
hng.
c> Tip , nh mt h thng my quang ph ngi ta thu, phn ly v chn
vch ph hp th ca nguyn t cn nghin cu o cng ca n. Cng
chnh l tn hiu hp th ca vch ph hp th. Trong mt gii hn nht nh ca nng
, gi tr cng ny l ph thuc tuyn tnh vo nng C ca nguyn t trong
mu phn tch.
2.3. U IM V NHC IM CA PHP O
Cng nh cc phng php phn tch khc, phng php phn tch ph hp th
nguyn t cng c nhng u im v nhc im nht nh. Cc u im l:
-

Php o ph hp th nguyn t c nhy v chn lc cao.

Chnh v c nhy cao, nn phng php phn tch ny c s dng

rng ri trong nhiu lnh vc xc nh lng cc vt kim loi. c bit l trong


phn tch cc nguyn t vi lng trong cc i tng mu y hc, sinh hc, nng
nghip, kim tra cc cht c tinh khit cao.
-

ng thi cng do nhy cao nn trong nhiu trng hp khng phi lm

giu nguyn t cn xc nh trc khi phn tch. Do tn t nguyn liu mu, tn t


thi gian v khng phi dng nhiu ha cht tinh khit cao khi lm giu mu. Mc
khc cng trnh c s nhim bn mu khi x l qua cc giai on phc tp.
cng l mt u im ln ca php o ph hp th nguyn t.

- Trang 59 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- Cc ng tc thc hin nh nhng. Cc kt qu phn tch c th lu tr trn
my tnh. ng thi vi cc trang b hin nay ngi ta c th xc nh ng thi hay
lin tip nhiu nguyn t trong mt mu.Cc kt qu phn tch li rt n nh, sai s
nh. Trong nhiu trng hp sai s khng qu 15% vi vng nng c ppm.
Bn cnh nhng u im, php o ph hp th nguyn t cng c mt s hn
ch v nhc im nht nh:
-

iu hn ch trc ht l mun thc hin php o ny cn c h thng my

tng i t tin. Do nhiu c s nh khng iu kin xy dng phng th


nghim v mua sm my mc.
-

Mc khc cng chnh do php o c nhy cao nn s nhim bn nh

hng rt ln n kt qu phn tch, c bit hm lng vt. V th mi trng


khng kh trong phng th nghim phi khng c bi. Dng c phi sch s, ha cht
dng trong php o phi c tinh khit cao. cng l mt kh khn khi p dng
phng php phn tch ny. Ngoi ra, cng chnh v php o c nhy cao nn cc
trang thit b my mc l kh tinh vi v phc tp. Do cn phi c k s trnh
cao bo dng v chm sc. Nhng yu t ny c th khc phc c qua cng tc
chun b v o to cn b
-

Nhc im chnh ca phng php ny l ch cho ta bit thnh phn

nguyn t ca cht trong mu phn tch, m khng ch ra trng thi lin kt ca cc


nguyn t trong mu. V th n ch l phng php phn tch thnh phn nguyn t.
2.4. I TNG V PHM VI NG DNG CA PHP O
i tng chnh ca phng php phn tch theo ph hp th nguyn t l
phn tch lng nh (lng vt) cc kim loi trong cc loi mu khc nhau ca cc
cht v c v hu c. Vi cc trang b v k thut hin nay, bng phng php phn
tch ny c s dng xc nh cc kim loi (khong 65 nguyn t) v mt s
kim n gii hn nng c ppb (nanogram), vi sai s khng ln hn 15%. Trong
- Trang 60 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
khong 10 nm nay, phng php phn tch ny c s dng xc nh hm
lng kim loi trong qung, t, , nc khong, cc mu ca y hc, sinh hc, cc
sn phm nng nghip, rau qu, thc phm, nc ung, cc nguyn t vi lng trong
phn bn, trong thc n gia sc.
Bn cnh cc kim loi, mt vi kim nh Si, P, As, Se, Te cng c xc
nh bng phng php phn tch ny. Cc kim khc nh C, Cl, O, N khng xc
nh c bng phng php ny. V cc vch phn tch ca cc kim ny thng
nm ngoi vng ph ca cc my hp th nguyn t thng dng (190 900nm). V d
C 165,70; N 134,70; O 130,20; Cl 134,78, S 180,70nm. Do , mun phn
tch cc kim ny cn phi c cc b n sc c bit. V th, cho n nay i tng
chnh ca phng php phn tch theo ph hp th nguyn t vn l phn tch lng
nh v lng vt cc kim loi.
Trn i tng , hin nay php o AAS v ang pht trin rt nhanh. N
cng v ang s dng nh mt cng c phn tch c lc cho nhiu ngnh khoa
hc v kinh t. Nhiu phng th nghim v php o ph hp th nguyn t c
xy dng. Cc hng trn th gii ch to nhiu my mi c nhiu tnh nng u
vit. Cc vin nghin cu khoa hc quc gia, cc vin nghin cu nng nghip, vin
a cht, cc ngnh a cht, cng ngh luyn kim, cng nghip ha hc, cng nghip
ha du, cng nghip thc phm, ngnh y bnh vin, cc trng i hc u c cc
phng th nghim v php o ph hp th nguyn t. C th ni n nay, hu ht cc
lnh vc khoa hc k thut v kinh t u s dng phng php phn tch ph hp
th nguyn t.
2.5. CC B PHN CA THIT B O PH HP THU NGUYN T
Nhn chung mt thit b o AAS bao gm 5 phn chnh sau:
Ngun pht bc x n sc.
H thng nguyn t ha mu.
- Trang 61 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
H thng quang hc.
Detector.
B x l v c s liu.

Nguyn t
ha mu

Ngun sng

B ngt
tia

Ngn la
hoc l

o nh sng v x l tn hiu

B n sc

Detector H in t

My ghi

Hnh: S nguyn l my quang ph hp thu


nguyn t
2.5.1. Ngun pht bc x n sc
Mun thc hin c php o ph hp th nguyn t ngi ta cn phi c
ngun bc x n sc (tia pht x cng hng) ca nguyn t cn phn tch chiu
qua mi trng hp th. Ngun pht bc x n sc trong php o ph hp th
nguyn t thng l cc n catot rng, cc n phng in khng in cc v cc
n ph lin tc c bin iu ( c n sc ha). Nhng d l loi no, ngun pht
tia bc x n sc cng phi tha nhng yu cu ti thiu sau y mi c th chp
nhn c.
1. Ngun pht tia bc x n sc phi to ra c cc tia pht x nhy (cc
vch pht x nhy) ca nguyn t cn phn tch. Chm tia pht x phi c cng

- Trang 62 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
n nh, phi lp li c trong nhiu ln o khc nhau trong cng iu kin, phi
iu chnh c vi cng mong mun cho mi php o.
2. Ngun pht tia bc x phi cung cp c mt chm tia bc x thun khit
ch bao gm mt s vch nhy ca nguyn t phn tch. Ph nn ca n phi khng
ng k. C nh th mi hn ch c nhng nh hng v vt l v v ph cho php
o AAS.
3. Chm tia pht x n sc do ngun cung cp phi c cng cao.
Nhng li phi bn vng theo thi gian, v phi khng b cc yu t vt l khc nhiu
lon, khng b nh hng bi cc dao ng ca iu kin lm vic.
4. Ngun pht tia bc x n sc phi bn lu, khng qu t tin v khng
qu phc tp cho ngi s dng. Tt nhin trong 4 yu cu trn, th 3 yu cu u tin
l quan trng nht, v bt buc phi tha mn, cho php o t kt qu chnh xc,
n nh v tin tng. Ring yu cu th 4 l c th chm chc c trong nhng
trng hp c th nht nh.
Xut pht t nhng nhim v v cc yu cu phi tha mn, hin nay trong
php o ph hp th nguyn t, ngi ta thng dng ch yu 3 loi ngun pht ra tia
bc x n sc. l:
-

n catt rng (HCL Hollow Cathode Lamp).

n phng in khng in cc (EDL).

n pht ph lin tc b bin iu (D2 Lamp, W Lamp).

Trong ba loi , n HCL c dng nhiu nht. n pht ph lin tc mi


c pht trin v s dng trong vi nm, nhng li c nhiu u vit trong cc my
nhiu knh v qu trnh phn tch t ng lin tip nhiu nguyn t.

- Trang 63 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.5.1.1. n catt rng Hollow cathode lamp (HCL)
n pht tia bc x n sc c dng sm nht v
ph bin nht trong php o AAS l n catot rng. n
ny ch pht ra nhng tia bc x nhy ca nguyn t kim
loi lm catt rng. Cc vch pht x nhy ca mt
nguyn t thng l cc vch cng hng. V th n
catt rng cng c gi l ngun pht tia bc x cng
hng.
V cu to n catt rng gm c 3 phn:
-

Phn 1 l thn n v ca s.

Phn 2 l cc in cc catt v ant.

Phn 3 l kh cha trong n. l kh tr He, Ar, hay N2.


Thn n gm c v n, ca s v b cc in cc ant v catt. V n

bng thy tinh hay thch anh chu nhit. Mt u ca v n l ca s cho chm
sng pht x t catt i qua v chiu vo mi trng hp th. Ca s ca n c th l
thy tinh hay thch anh trong sut trong vng UV hay VIS l ty thuc vo loi n
ca tng nguyn t pht ra chm tia pht x nm trong vng ph no. Ngha l vch
pht x cng hng o ph hp th vng no th nguyn liu lm ca s phi
trong sut cng mc .
in cc ca n l catt v ant. Ant c ch to bng kim loi tr v
bn nhit nh W hay Pt. Catt c ch to c dng hnh xylanh hay hnh ng rng c
ng knh t 3 5 mm v bng chnh kim loi cn phn tch vi tinh khit cao (t
nht 99,99%). Dy dn ca catt cng l kim loi W hay Pt. C hai in cc c gn
cht trn b ca thn n v cc catt phi nm ng trc xuyn tm ca n. Ant
t bn cnh catt hay l mt vng bao quanh catt. Hai u ca hai in cc c
ni ra hai cc gn chc trn v n, cm vo ngun in nui cho n lm vic.
- Trang 64 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Hnh: Cu to n HCL
a. Catt rng; b. Ant;
c: mica cch ly; d: ngun
n; e: ca s thch anh
Kh cha trong n: Trong n phi ht ht khng kh v np thay vo l
mt kh tr vi p sut t 5

15 mHg. Kh tr l argn, heli hay nit, nhng phi

c sch cao hn 99,99%. Kh np vo n phi khng pht ra ph lm nh hng


n chm tia pht x ca n v khi n lm vic trong mt iu kin nht nh th t
s gia cc nguyn t b ion ha v cc nguyn t trung ha phi l khng i. C
nh th n lm vic mi n nh.
n c t nng pht ra chm tia pht x cng hng nh mt
ngun in mt chiu n nh. Th lm vic ca n HCL thng l t 250

450 V

ty thuc vo tng loi n ca tng hng ch to v ty thuc vo tng nguyn t


kim loi lm catt rng. Cng lm vic ca cc n catt rng thng l t 3

50 mA v cng thay i ty thuc vo tng loi n HCL ca mi nguyn t do mi


hng ch to ra n. Th v cng dng in lm vic ca n HCL l c lin quan
cht ch vi cng tch kim loi ra khi b mt catt rng to ra hi kim loi sinh ra
chm tia pht x ca n HCL.
Mi n HCL c mt cng dng thch hp hot ng ti u. Mi s
dao ng v dng in lm vic ca n u lm nh hng n cng ca chm
sng pht x. Ni chung, cng dng cng ln th cng pht x cng ln v
nhiu ng nn cng nh. Tuy nhin, khi tip tc tng cng dng, tui th ca
n s gim v c th xy ra hin tng don rng vch ph (spectral line broadening)
lm gim nhy v tuyn tnh. V nhng l do trn, cc nh sn xut kho st
v cung cp cho ngi s dng mt cng dng thch hp (recommended current)
m bo tui th v hiu qu hot ng ca n. Trong thc t phn tch, nu cn t
- Trang 65 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
l tn hiu / nhiu nh, ngi s dng c th tng cng dng ln nhng khng
c qu cng cc i; cn nu yu cu ca php phn tch khng qu khc khe,
ngi s dng c th gim cng dng ko di tui th ca n.
Khi n lm vic, catt c nung v catt xy ra s phng in lin tc.
Do s phng in mt s phn t kh b ion ha. Cc ion sinh ra tn cng vo catt
lm b mt catt nng v mt s nguyn t trn b mt catt b ha hi v n tr
thnh nhng nguyn t kim loi t do. Khi di tc dng ca nhit trong n
ang c t nng , cc nguyn t kim loi ny b kch thch v pht ra ph pht
x ca n. chnh l ph vch ca chnh kim loi lm catt rng. Nhng v trong
iu kin c bit ca mi trng kh tr c p sut thp nn ph pht x ch bao
gm cc vch nhy ca kim loi m thi. chnh l s pht x ca kim loi trong
mi trng kh km. Chm tia pht x ny l tia n sc chiu qua mi trng hp
th thc hin php o AAS.

Ar+
M0

Ar+
M0

M*

M*

M0 +

Hnh: Nguyn l hot ng ca nHCL


Cc n catt rng c cu to nh m t trn l nhng n HCL n mt
nguyn t. Ngha l mi n HCL ch phc v cho phn tch mt nguyn t. Ngy
nay ngoi cc n HCL n, ngi ta cng ch to c mt s n kp i, kp
ba hay kp su nguyn t. Cc n kp i l (Ca + Mg), (Cu + Mn), (Cu + Cr),
(Co + Ni), (K + Na), (Cu + Pb), cc n kp ba nh (Cu + Pb + Zn) v n kp 6 l
(Cu + Mn + Cr + Fe + Co + Ni). ch to cc n kp, catt ca n HCL phi l
hp kim ca cc nguyn t . Hp kim ny phi c thnh phn ph hp, sao cho
cng pht x ca cc nguyn t l gn tng ng nhau. Ngha l s pht x ca
- Trang 66 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
kim loi ny phi khng c ln t s pht x ca nguyn t kia. V d n HCL kp
su ca Cu, Mn, Fe, Co, Cr v Ni th hp kim lm catt rng phi cha 25% Cu, cc
nguyn t khc c thnh phn l 15%.
Xt v nhy, ni chung cc n kp c nhy km cc n n tng ng,
hay tt nht cng ch gn bng l cng. Mc khc v ch to li kh khn hn n
n. V th cng ch c mt s n kp m thi v cng ch c dng trong mt s
trng hp khi vic thay i n c nh hng n qu trnh phn tch v trong cc
my nhiu knh th n HCL kp l c u vic hn, u hn.
n HCL c tui th hn ch. Nguyn nhn chnh l do s hp ph cc nguyn
t kh ln mt trong ca n. Khi p sut kh gim, hiu sut ca qu trnh va p vi
catt v qu trnh kch thch cc nguyn t kim loi gim lm cho cng pht x
ca n cng gim. Do , tng tui th ca n, mt vi nh sn xut ch to loi
n c th tch bn trong ln hn.
Trong qu trnh va p, mt s nguyn t kim loi c th b nh bt ra khi
hc catt v bm li nhng ch khc, ng thi cc nguyn t kh cng c th b
catt gi li. n ca cc kim loi bay hi nh As, Se, Cd, d xy ra khuynh hng
th nht. Tuy nhin khuynh hng th nht khng nh hng lm n hot ng ca
n m khuynh hng th hai nh hng nhiu hn, nht l cc n hot ng vi
cng dng cao.
Mt s vt liu lm catt c th pht ra kh hydro khi nng ln. Nu nng
hydro tng ln s xy ra s pht x ph lin tc lm nh hng n ph vch ca
nguyn t, kt qu l gim nhy v tuyn tnh. loi b nh hng ca hydro,
ngi ta gn mt ci by bng tantalum ln ant hp ph hydro sinh ra khi n
hot ng.
2.5.1.2 n phng in khng in cc Elactrodeless Discharge Lamp
(EDL)
- Trang 67 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Ngun pht tia bc x n sc th hai c
dng trong php o ph hp th nguyn t l n
phng in khng in cc. Loi n ny cng
nh n HCL u c nhim v cung cp chm tia
pht x c trng ca nguyn t phn tch. Nhng
vi mt s nguyn t, c bit l cc kim, th
n EDL cho nhy cao hn n HCL.
Bng so snh nhy v gii hn pht hin ca hai loi ngun HCL v EDL
Nguyn t
(nm)
Sb 217,6
As 193,7
Bi 223,1
Cd 228,8
Pb 283,2
Hg 253,6
P 213,6
Se 196,0
Te 214,3
Tl 276,8
Sn 286,3
Zn 213,9

nhy( g/ml)
HCL
EDL
0,48
1,10
0,45
0,025
0,43
6,4
260,0
1,0
0,35
0,45
2,5
0,014

0,44
0,90
0,53
0,025
0,46
4,5
300,0
0,63
0,36
0,43
2,6
0,016

Gii hn pht hin ( g/ml)


HCL
EDL
0,076
0,980
0,071
0,0026
0,019
0,4
93,0
0,54
0,077
0,05
0,19
0,0012

0,040
0,340
0,028
0,0007
0,014
0,15
33,0
0,21
0,038
0,03
0,08
0,00095

V cu to thc cht l mt ng phng in trong mi trng kh c cha


nguyn t cn phn tch vi nng nht nh to ra c chm tia pht x ch bao
gm mt s vch ph nhy c trng ca nguyn t . n EDL l mt ng thch
anh chu nhit di 8 10 cm, ng knh 1

1,5 cm, trong cha vi mg kim loi

hay mui kim loi d bay hi ca nguyn t cn phn tch , sao cho p sut hi ca
kim loi trong n iu kin nhit t 200

4500C l khong t 1 1,5

mHg. Mt u ca n EDL cng c ca s trong sut nh n HCL chm sng


pht x i qua. Trong n EDL cng phi ht ht khng kh v np thay vo l mt
kh tr Ar, He hay Nit c p sut vi thor, khi u cho s lm vic ca n EDL.
- Trang 68 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Cun xung quanh ngoi ng thch anh l mt cun dy cao tn Hf c cng sut t 200

400 W ty loi n ca tng nguyn t, v c ni vi ngun nng lng cao tn


ph hp nui cho n EDL lm vic.

Cun dy cao tn
Ca s thch anh
n (cha nguyn t hoc mui ca nguyn t
cn phn tch trong kh Ar p sut rt thp)
Vng bng gm

Hnh: Cu to n EDL
Ngun nng lng cao tn nui n EDL lm vic c ch to theo hai tn
s: tn s sng ngn 2450 MHz v tn s sng radio 27,12 MHz. Do ngun nui l
hai loi nng lng cm ng in t vi hai loi tn s khc nhau , nn n EDL
cng chia thnh 2 loi:
-

n EDL sng ngn, ngun nui tn s 2450 MHz.

n EDL sng radio, ngun nui tn s sng radio 27,12MHz.

Khi n lm vic, di tc dng ca nng lng cao tn cm ng, n c


nung nng , kim loi hay mui kim loi trong n c ha hi v b nguyn t
ha. Cc nguyn t t do c sinh ra s b kch thch v pht ra ph pht x ca n
trong iu kin kh km. chnh l ph vch ca kim loi cha trong n EDL.
Ngoi u im v nhy v gii hn pht hin, n EDL thng c bn
cao hn n HCL. ng thi vng tuyn tnh ca php o mt nguyn t khi dng
n EDL cng thng rng hn so vi vic dng n HCL.

- Trang 69 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Ngy nay cc hng sn xut my o ph hp th nguyn t sn sut c


n 40 n EDL cho 40 nguyn t. Nhng tt v c dng nhiu ch c 12 nguyn t
l As, Bi, Cd, Hg, P, Pb, Sb, Se, Sn, Te, Tl v Zn. Cc n EDL ca cc nguyn t ny
u c bn theo cc my ca cc hng. Nhng n EDL ca cc nguyn t khc
cn li l t c s dng. V n khng u vit hn n HCL, m gi thnh li t
hn.
Ngoi n catt rng v n phng in khng in cc, ngi ta cng ch to
ra c nhiu loi n pht tia bc x n sc ca cc nguyn t. Nh n catt rng
cng cao (high intensity emission lamp HIEL), n gradient nhit
(controlled temperature gradient lamp CTGL), n phng in chi sng (glow
discharge lamp GDL). Cc loi n ny c u im hn n HCL mt cht v
nhy, v vng tuyn tnh, v gii hn pht hin. Nhng cc loi n ny li kh ch
to v t tin, mc khc li km bn vng. V th n t c dng v khng c bn
ngoi th trng. Ch yu dng trong nghin cu l thuyt.
2.5.1.3. n ph lin tc c bin iu
Trong khong vi nm li y, mt loi ngun pht x ph lin tc cng c dng
lm ngun pht bc x cng hng cho php o AAS. l n hydrogen nng (D 2
- Trang 70 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Lamp), cc n Se p sut cao, cc n halit ca kim loi W. l cc loi n pht
ph lin tc trong vng t ngoi v vng kh kin (UV VIS). Cc tc gi Fassel,
Ivanob, Gibson, Mc Gee, Winerfordner l nhng ngi u tin nghin cu v s
dng cc loi n lm ngun pht x cng hng cho php o AAS. n ny tuy
pht ra ph lin tc, nhng nh h thng bin iu v h lc giao thoa, nn chm sng
pht x b bin iu v lng t ha thnh chm sng khng lin tc c ph
dng rng ca. Trong ngun sng c t trc h thng bin iu v b lc giao
thoa. Chm sng ny khi i qua h thng bin iu v b lc giao thoa th n s b
bin iu theo nhng di sng nht nh vi bin nh nhau. Sau cng c
chiu vo mi trng hp th l ngn la hay cuvet graphit. Cc nguyn t t do
trong mi trng hp th s hp th mt phn nng lng ca chm sng ng vi mt
di bin iu ca vng ph. Phn cn li s i vo b n sc v detector pht
hin v o cng sau khi qua b khuych i bng sng theo dy ph ca n
nn li tn s. Tip cng vch ph hp th cng c c v ch th theo cc
cch bit, nh hin s digital pick trn recorder, hay dng printer in ln bng giy.
Ngun pht ph lin tc c u im l d ch to, r tin v c bn cao. V
ch cn c mt n c th thc hin c php o AAS i vi nhiu nguyn t.
Do n rt u vit i vi cc my ph hp th nhiu knh v xc nh ng thi
hay lin tip nhiu yu t trong cng mt mu phn tch. Vng tuyn tnh rng, li
khng c hin tng t hp th ring. Song v n sc v chn lc th trong
mt s trng hp cn km cc loi n HCL hoc EDL. Nhng li u vit v d
dng i vi qu trnh phn tch t ng hng lot trong cc my o ph hp th
nhiu knh. Chnh v th m trong khong nm nm li y cc loi n ph lin tc
c pht trin, ci tin v s dng rt nhiu trong php o AAS v nhiu h thng
my o ph hp th vi ngun pht ph lin tc c bn trn th trng th gii.

- Trang 71 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

2
4

Gii ph lin tc

Gii ph lin tc bin iu

Vch ph hp th

Gii ph sau khi qua


mi trng hp th

2.5.2. H thng nguyn t ha mu


H thng nguynt ha mu c nhim v to ra cc nguyn t t do trng
thi c bn cn thit cho s hp thu nguyn t. lm iu ny cn phi cung cp
mt nhit nng ln ph v cc lin kt ca nguyn t trong phn t. Cc k
thut phn tch thng c s dng gm:
- K thut FIAS: p dng cho cc ch tiu Hg, As, Se, Ab.
- Trang 72 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- K thut ngn la cao (C2H2 : N2O): p dng cho cc ch tiu kim loi Al, Sn,
Ba, ...
- K thut ngn la (C2H2: khng kh): p dng cho cc ch tiu kim loi nng
cn li.
- K thut graphite: p dng cho cc kim loi Pb, Cu, Cd, Mo, Ni, Cr, ... nhng
c yu cu gii hn pht hin thp.
Trong , k thut c p dng rng ri v thng xuyn nht l k thut
nguyn t ha bng ngn la, s dng h thng bung trn v u t.
2.5.2.1. K thut nguyn t ha mu bng ngn la:
Dung dch mu c ht vo thng qua mt ng phun sng to thnh cc ht
nh li ti vo bung trn. Ti y, cc ht sng mu c trn vi kh t (acetylene)
v kh oxi ha (khng kh nn hoc N2O) ri i ln u t, di tc dng ca nhit
ngn la s xy ra s nguyn t ha mu.

Hnh: My o ph hp thu nguyn t bng ngn la

- Trang 73 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

2.5.2.2. K thut FIAS:


T bo nguyn t ho c s dng rng ri nht cho k thut to hp cht
hidrua l ng thch anh gia nhit rng hnh ch T c ng knh chun 10mm v
chiu di t 100- 150mm.
ng rng thch anh c gia nhit bng in n 700-1000 oC cho php ti u
ho nhit nguyn t ho cho tng nguyn t.
ng c th c nhng im cui h hoc nhng im cui ny c bt bng
cc ca s thch anh c th di chuyn c v cc l trng cui ng thch anh l ni
kh thot ra ngoi.
Cu to ca ng gip lm tng thi gian c tr ca cc nguyn t trn ng i
ca nh sng v nh th s gip tng nhy.
Khi ng nguyn t ho thch anh c s dng nhiu ln m khng thay mi
th s mt i nhy v chnh xc. Nguyn nhn l do mt trong ca ng thch anh
b nhim bn do qu trnh tch t cc phn t v cc git cht lng nh b m thit b
tch pha kh- lng khng loi tr c trit .

My o ph hp thu nguyn t theo k


thut FIAS
- Trang 74 -

ng thch anh ch T

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

2.5.2.3. K thut graphite:


Trong k thut ny, mt ng graphite nh c dng nh b phn nguyn t
ha mu. Mt th tch nh dung dch mu c cho vo ng thng qua mt l tim
nh khot chnh gia ng. Sau , ng c gia nhit theo mt chng trnh nhit
cho n khi cht cn phn tch trong mu b phn hy thnh cc nguyn t v s
hp thu nguyn t xy ra.
2.5.3. H thng quang hc
Bao gm 2 phn: mt phn gi l photometer, mt phn gi l monochromator
(b n sc).
2.5.3.1. Photometer
Photometer l mt phn ca h thng quang hc c nhim v dn lung nh
sng pht ra t n i qua b phn nguyn t ha ri vo b n sc. Hin nay c 3
loi photometer c s dng trong my hp thu nguyn t: loi mt chm tia (single
beam), loi hai chm tia (double beam) v loi gi hai chm tia (pseudo double
beam).
2.5.3.1.1. Loi mt chm tia (single beam photometer):

Hnh: My hp thu nguyn t mt chm tia

- Trang 75 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Hnh trn m t s nguyn tc ca mt my ht nguyn t mt chm tia. N
c gi l mt chm tia bi v ton b cc php o da trn s thay i cng
ca mt chm tia sang duy nht.
u im ch yu ca loi mt chm tia l c cu to n gin, do n d ch
to v r hn cc loi khc. Vi kt cu mt ng nh sang duy nht v c t cc
phn t quang hc, h thng mt chm tia cung cp mt cng nh sng rt cao.
Hn ch chnh ca n l khng b tr c nhng bin ng ca thit b trong qu
trnh phn tch, v d nh s thay i cng sng ca n.
2.5.3.1.2. Loi hai chm tia (double beam photometer):

Hnh: My hp thu nguyn t hai chm tia


Hnh trn m t s nguyn tc ca mt my hp thu nguyn t hai chm tia,
n s dng thm cc phn t quang hc chia nh sng t n thnh hai chm tia:
chm tia mu (c chiu thng qua b nguyn t ha mu) v chm tia so snh
(c hng i vng pha sau b nguyn t ha mu).
Trong h thng hai chm tia, chm tia so snh c tc dng nh mt phng
tin gim st cng sng ca n v p ng ca mch in t. Do , tn hiu hp
thu c xc nh t t s cng ca chm tia mu v chm tia so snh, khng ph
thuc vo nhng nh hng do s thay i cng sng ca n v nhng bt
- Trang 76 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
thng ca mch in t v nhng nh hng ny tc ng tng t ln c hai chm
tia.
K thut hai chm tia cho php thay i n v bt u mt php phn tch m
khng cn hoc cn rt t thi gian si n, iu ny lm gim thi gian phn tch v
tit kim tui th ca n.
Mt hn ch ca h thng hai chm tia l cng ca chm tia mu s nh
hn so vi h thng mt chm tia, iu ny c th lm nh hng n gii hn pht
hin ca thit b. khc phc, trong cc my hp thu nguyn t hin i ngi ta
ch to b tch tia sao cho cng chm tia mu ln hn nhiu so vi cng
chm tia so snh, v d theo t l 75% v 25%.
2.5.3.1.3. Loi gi hai chm tia (pseudo double beam photometer):

Hnh: My hp thu nguyn t gi hai chum tia vi lung sng t n c hng


theo ng i qua b nguyn t ha

- Trang 77 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Hnh: My hp thu nguyn t gi hai chum tia vi lung sng t n c


hng theo ng so snh
Hnh trn m t s nguyn tc ca mt my hp thu nguyn t gi hai chm
tia. H thng ny s dng hai gng quay (iu chnh bng c kh) hng ton b
nh sng t n lun phin i theo ng qua b nguyn t ha hoc theo ng so
snh.
H thng gi hai chm tia cung cp mt cng nh sng cao nh h thng
mt chm tia. ng thi n cng b tr c nhng bin ng ca thit b tng t
nh h thng hai chm tia, cn ch l ch tng t ch khng ging ht. H thng
hai chm tia thc hin vic b tr hn 50 ln trong mt giy, trong khi h thng gi
hai chm tia thc hin t hn nhiu, thng ch mt ln trn mi ln c tn hiu. Tc
thc hin b tr chm ca h thng gi hai chm tia lm hn ch kh nng b tr
ca n i vi nhng bin i nhanh v nhiu cng sng ca n, nht l khi n
mi c bt sng.
2.5.3.2. B n sc
B n sc c nhim v thu, phn
tch bc sng v chn vch ph cn o
hng vo nhn quang in (detector)
pht hin tn hiu hp thu ca vch ph .
- Trang 78 Hnh: Cu to ca mt b n sc

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Lung nh sng sau khi qua b phn nguyn t ha i vo b n sc qua khe
vo (entrance slit). nh sng s c hi t ln cch t (grating), ti y xy ra s
phn tch bc sng. Cch t l mt b mt phn x c khc nhiu vch nh song
song rt gn nhau (khong 2000 vch/mm).
S phn x ti mt b mt nh vy gy ra hin tng nhiu x, trong cc
bc sng khc nhau s lch i theo cc gc khc nhau. Cc bc sng phn x ny
s c hng v pha khe ra (exit slit). Bng cch thay i gc quay ca cch t,
bc sng phn tch c th c cho php i qua khe truyn vo detector, trong khi
cc bc sng khc s b ngn li.
Mun h thng my quang ph hp th nguyn t cho c kt qu tt, th h
thng tn sc phi c bo m c mt s yu cu bt buc sau y:
1. N phi c tn sc ln c th tch v c lp c tt cc vch ph
cn o, trnh s quy ri, s chen ln ca cc vch ph khc bn cnh.
2. Phi khng gy ra bt k hin tng no lm mt nng lng ca chm
sng trong my, nh s hp thu, s tn x, s khuych tn ca cc b phn cu to
thnh my. c bit l cc h thng gng, cc thu knh, khe vo, khe ra ca chm
sng. Cc thu knh phi trong sut trong vng ph lm vic ca my.
3. Khe vo v khe ra ca my phi c m chnh xc v phi iu chnh
c cho ph hp vi tng vch ph v c lp li cao trong mi php o.
4. Detector pht hin cng vch ph phi c nhy cao. C nh th
mi pht hin c s thay i nh trong qu trnh hp th ca ph.
l cc iu kin ti thiu ca h quang hc trong my ph hp th nguyn
t. Vi s pht trin ca khoa hc v k thut, ngy nay ngi ta c th tha mn
c tt c cc yu cu . Chnh v th hin nay c rt nhiu my o ph hp th
nguyn t c cht lng cao c bn trn th trng quc t. l my o ph

- Trang 79 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
hp th nguyn t ca hng Perkin Elmer, Varian, Bercmans, Philips Pye Unicam,
Wet Zeiss, Shimadu, Instr, Lab, Alpha,
2.5.4. Detector
Detector l mt loi dng c quang hc dng thu nhn, pht hin tn hiu
quang hc theo hiu ng quang in ca n. Trc y thu nhn cng ca
chm sng ngi ta thng dng knh nh hay phim nh. Sau l t bo quang in.
l cc dng c c in c nhy km, nht l knh nh. Hin nay, detector thng
dng nht l ng nhn quang (photomultiplier tube PMT).

Hnh: S nguyn tc ca mt PMT


Bn trong PMT l mt cathode nhy sng v mt s dynode c in th dng
hn so vi cathode. Dynode cui cng c in th ln nht c gi l anode. Khi
mt photon p vo cathode s c mt s electron bt ra khi cathode v i n
dynode u tin, ti y, mi electron ban u s lm bt ra mt s electron i n
dynode th hai. Qu trnh c tip tc nh th cho n dynode cui cng (anode).
Bng cch s dng mt PMT 9 dynode, s electron sinh ra c th c khuch i v
tng ln n 108 ln.
nhy ca mt PMT ph thuc vo bc sng ca nh sng ti.
- Trang 80 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.5.5. B x l v hin th s liu
Trong cc thit b hp thu nguyn t hin i, b x l v hin th s liu bao
gm mch in t c tc x l nhanh v my vi tnh c phn mm iu khin thit
b. Chng c kh nng tnh gi tr trung bnh, lch chun, lch chun tng i
ca cc php o lp, dng ng chun, tnh ton nng t hp thu, lu tr cc
thng tin v mu v cc thng s ca php o, im u vit nht l chng gip t
ng ha thit b.

2.6. MT S YU T NH HNG TRONG PHP O AAS


2.6.1. Cc yu t nh hng c tnh cht ph
2.6.1.1. S hp th nn
Yu t ny c trng hp xut hin r rng. Nhng cng nhiu trng hp
khng xut hin. iu ny ph thuc vo vch ph c chn o nm trong vch
ph no. Ni chung trong vng kh kin th yu t ny thc hin r rng. Cn trong
vng t ngoi th nh hng ny t xut hin, v ph nn trong vng t ngoi l yu.
Hn na s hp th nn cn ph thuc rt nhiu vo thnh phn nn ca mu phn
tch, t bit l matrix ca mu, ngha l nguyn t c s ca mu. V d khi xc nh
Pb trong mu sinh hc bng php o ngn la th s hp th nn l khng ng k.
Nhng khi xc nh Pb trong nc bin (nn 2,9% NaCl) th nh hng ny l v
cng ln.
Do trong mi trng hp c th phi xem xt tm trng hp loi tr.
loi tr ph nn, ngy nay ngi ta lp thm vo my quang ph hp th nguyn t h
thng b chnh nn. Trong h thng ny ngi ta dng n hyr nng (D 2- lamp)
b chnh nn trong vng t ngoi v dng n W (W- habit lamp) cho vng kh kin.
Do , trong mi php o xc nh mt nguyn t chng ta c th thc hin b
- Trang 81 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
chnh nn hay khng l ph thuc vo yu t c nh hng hay khng. Hn na,
ngy nay ngi ta dng c hiu ng Zeeman b chnh nn. K thut ny khng
nhng b chnh c nn c hiu qu cao hn, nht l cc mu nng mui nn l
ln, m cn tng c nhy ca php o nhiu ln.V hiu ng Zeeman c tc
dng lm tng cng ca vch ph hp th nguyn t ca nguyn t. K thut b
chnh th ba l dng n HCL hot ng hai ch lin tip: ch dng thp (do
tn hiu hp th tng) v ch dng cao (ch o cng hp th nn). Hiu gia
hai ln o l tn hiu hp thu thc ca vch ph. Cch b chnh ny tuy c tin hn, v
ch cn n HCL nhng n HCL li chng hng do phi dng ch dng cao lin
tc trong qu trnh o ph.
2.6.1.2. S chen ln ca vch ph
Yu t ny thng thy khi cc nguyn t th ba trong mu phn tch c nng
ln v thng l nguyn t c s ca mu. Tuy nguyn t ny c cc vch ph
khng nhy, nhng do nng ln, nn cc vch ny vn xut hin vi rng ln,
nu n nm cnh cc vch phn tch th cc vch ph ny s chen ln cc vch phn
tch, lm cho cng vch ph phn tch rt kh khn v thiu chnh xc nht l i
vi cc my c phn gii khng cao. V th trong mi mc ch phn tch c th
cn phi nghin cu v chn nhng vch phn tch ph hp loi tr s chen ln
ca cc vch ph ca nguyn t khc. Nu bng cch ny m khng loi tr c nh
hng ny th bt buc phi tch bt nguyn t c vch ph chen ln ra khi mu
phn tch trong mt chng mc nht nh, cc vch chen ln khng xut hin na.
Tt nhin vic ny l hn hu.
2.6.1.3. S hp th ca cc ht rn
Trong mi trng hp th, t bit l trong ngn la n kh, nhiu khi cn
cha c cc ht rt nh li ti ca vt cht mu cha b ho hi v nguyn t ho, hay
cc ht mui cacbon ca nhin liu cha t chy hon ton. Cc ht loi ny thng
- Trang 82 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
c th c lp v ca ngn la. Cc ht ny hoc hp th hoc chn ng ng i
ca chm sng t n HCL chiu vo mi trng hp th. Yu t ny thng c
gi l s hp th gi. Do cng gy ra nhng sai s cho kt qu o cng vch
ph thc.Yu t ny th hin rt r khi chn khng ng chiu cao ca n nguyn t
ho mu v khi hn hp kh chy khng c t chy tt, hay do thnh phn ca hn
hp kh chy khng c chn ph hp ( thng l qu d acetylen).

Bng: S chen ln v s trng vch ca cc nguyn t


Nguyn t
Vch phn tch (nm)
Al - 308.215
Cu - 324.754
Fe - 271.903
Mn - 403.307
Zn - 213.856

Nguyn t c vch chen ln


Vch chen ln (nm)
Nng xut hin (ppm)
V - 308.211
800
Eu - 324.753
254
Pt - 271.904
054
Ga - 403.298
025
Fe - 213.850
200

2.6.2. Cc yu t vt l
Thuc v loi yu t vt l ny thng c:
2.6.2.1. nht v sc cng b mt ca dung dch mu
Tc dn mu (1 cp 1g/m.gy)
Trong php o Q
AAS, vi k thut nguyn t ho mu trong ngn la, yu t
ny nh hng nhiu n tc dn mu vo bung aerosol ho v hiu sut aerosol
ho ca mu v t m nh hng n kt qu phn tch. Ni chung, tc dn
mu l t l nghch vi nht ca dung dch mu.

nht

- Trang 83 1

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Hnh: nh hng ca nht n tc dn mu (1 cp 1g/m.gy)


Chnh s khc nhau v nng axit, loai axit, nng cht nn ca mu, thnh
phn ca cc cht c trong dung dch mu l nguyn nhn gy ra s khc nhau v
nht ca dung dch mu. V th trong mi qu trnh phn tch mt nguyn t nht thit
phi m bo sao cho mu phn tch v cc mu u lp ng chun phi c cng
nng axit, loi axit v thnh phn ho hc, vt l ca tt c cc nguyn t khc,
nht l cht nn ca mu. Yu t ny thng c th hin nhiu trong php o F AAS. loi tr nh hng ny chng ta c th dng cc bin php sau y:
- o v xc nh theo phng php thm chun.
- Pha long mu bng mt dung mi hay mt nn ph hp.
- Thm vo mu mt cht m c nng ln.
- Dng bm y mu vi mt tc xc nh m chng ta mong mun.
2.6.2.2. Hiu ng lu li
Yu t ny th hin r rng c bit trong php o khng ngn la v cng ln
khi mu phn tch c nng cng ln. ng thi cng ph thuc bn cht ca cc
nguyn t, hp cht n tn ti trong mu, cng nh loi cuvet graphite c dng
nguyn t ho mu. Ni chung cc nguyn t kh bay hi v d sinh ra hp cht bn
- Trang 84 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
nhit lun lun gy ra nh hng ny ln. Cc cuvet c ch to t graphite c
hot ho thng hn ch c hiu ng ny. Hn na b mt bn trong ca cuvet
cng l mt yu t ng gp vo hiu ng ny. Ngha l b mt cng mn th nh
hng cng nh, b mt cng xp th nh hng cng ln. Do tnh cht ny m khi
nguyn t ho mu o cng vch ph th mt lng nh ca nguyn t phn
tch khng b nguyn t ha, chng c lu li trn b mt cuvet v c th tch t li
qua mt s ln nguyn t ho mu. Nhng n mt lc no th n b nguyn t ho
mu theo v do to ra nguyn t t do ca nguyn t phn tch tng t ngt khng
theo nng ca n trong mu. Ngha l lm tng cng ca vch ph v dn n
lm sai lch kt qu phn tch. V th, loi tr nh hng ny chng ta c th lm
theo cc cch sau:
- Lm sch cuvet sau mi ln nguyn t ho mu, lm bay hi ht cc cht
cn li trong cuvet. Tt nhin phi thc hin nhit cao nhit nguyn t ho
nguyn t phn tch.
- Dng cc loi cuvet c ch to t cc loi graphite c hot ho ton
phn, c b mt chc v mn.
- Khi phn tch nn o cc mu c nng nh trc.
- Thm vo mu nhng cht m c nng d ph hp.
- Trng b mt trong ca cuvet graphite bng mt lp cc hp cht bn nhit.
Tt nhin y ch l nguyn tc chung. Cn trong thc t cng tu vo tng
trng hp c th m chn bin php ph hp nht.
2.6.2.3. S ion ha
y l yu t vt l th ba nh hng n kt qu phn tch. V qu trnh ion
ho thng lm gim s nguyn t t do ca nguyn t phn tch trong mi trng
hp th to ra ph. Do lm gim cng vch ph hp th, nu nguyn t b ion
- Trang 85 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
ha cng nhiu. Nhng mc ion ho ca mi nguyn t l khc nhau, v cn ph
thuc vo nhit ca mi trng hp th. Trong mt iu kin nht nh, ni chung
cc nguyn t c th ion ho cng thp th b ion ho cng nhiu. Vi mi nguyn t,
khi nhit ca mi trng hp th cng cao th nguyn t cng b ion ha nhiu
hn.
Bng: Mc ion ho ca mt nguyn t
Nguyn t

Th ion ho

Na
K
Rb
Cs
Ca
Ba

S % b ion ho ca nhit
2000 C
30000C
40000C
0

(eV)
5,21
4,32
4,16
3,87
6,11
5,31

00,30
02,10
09,00
28,00
00,20
0.,00

05,00
22,00
34,00
70,00
01,50
06,00

26,00
82,00
90,00
96,00
17,00
23,00

Thc t cho thy rng, qu trnh ion ha ch c ngha i vi cc kim loi


kim v sau l cc kim loi kim th, cn i vi cc nguyn t khc s ion ho l
khng ng k trong mi trng hp th ca php o ph hp th nguyn t. loi
tr s ion ho ca mt nguyn t phn tch chng ta c th dng cc bin php phn
tch sau y:
- Chn iu kin nguyn t ho c nhit thp, m trong iu kin nguyn
t phn tch hu nh khng b ion ho.
- Thm vo mu phn tch mt cht m cho s ion ho. l cc mui
halogen ca kim loi kim c th ion ho thp hn th ion ho ca nguyn t phn
tch vi mt nng ln ph hp. Nh vy trong iu kin nguyn t phn tch s
khng b ion ho na.
2.6.2.4. S kch thch ph pht x
Yu t ny xut hin thng lm gim nng ca cc nguyn t trung ho c
kh nng hp th bc x trong mi trng hp th. Ni chung cc nguyn t c th
- Trang 86 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
kch thch ph pht x thp thng b nh hng nhiu. ng thi mi trng hp th
c nhit cng cao th nh hng ny cng ln. Nhng trong nhit ca php o
AAS, th s kch thch ph pht x thng ch xy ra mnh ch yu i vi cc kim
loi kim v sau l cc kim th. V cc nguyn t ny c th kch thch ph pht
x tng i thp.Cn cc kim loi khc th s kch thch ph pht x l khng ng
k.
loi tr nh hng ca cc pht x ca nguyn t phn tch chng ta c th
dng cc bin php sau y:
- Chn nhit nguyn t ho mu thp ph hp m ti nhit s kch
thch ph pht x l khng ng k hoc khng xy ra i vi nguyn t phn tch.
- Thm vo mu cht m hn ch s pht x ca nguyn t phn tch. l
c mui halogen ca cc kim loi kim, c th kch thch ph pht x thp hn th
kch thch ph pht x ca nguyn t phn tch.
Trn y l mt s yu t vt l c th c xut hin trong php o AAS v c
th nh hng kt qu phn tch. Nhng mc xy ra l khc nhau trong mi trng
hp c th, c khi c, c khi khng. Mc ny xut hin ln hay nh l ph thuc
vo nhit ca mi trng hp th, tnh cht ca nguyn t phn tch, v thnh phn
ca mu phn tch. Do cn phi xem xt tm bin php loi tr khi chng xut
hin.
Bng: Mc b kch thch ph pht x ca cc nguyn t
cc nhit khc nhau
No - s nguyn t trung ho ban u
Ni - s nguyn t b kch thch ph pht x.
Nguyn t

T s Ni/ No nht (0C)

Th kch thch
2000

- Trang 87 -

3000

4000

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
(eV)
Cs -852,10

1.76

4,00.10-4

7,10.10-3

3,00.10-2

Na - 589,00

2,12

1,00.10-5

6,00.10+-4+

4,00.10-3

Ca - 422,70

2,95

1,10.10-7

4,10.10-5

6,00.10-4

Zn - 213,90

5,86

7,00.10-13

6,00.10-10

1,10.10-7

2.6.3. Cc yu t ho hc
Trong php o ph hp th nguyn t cc nh hng ho hc cng rt a dng
v phc tp. N xut hin cng rt khc nhau trong mi trng hp c th v cng c
nhiu trng hp khng xut hin. Cc nh hng ho hc thng c th dn n kt
qu theo bn hng sau y:
- Lm gim cng vch ph ca nguyn t phn tch, do s to thnh cc
hp cht bn nhit, kh ho hi v kh nguyn t ho. V d nh nh hng ca cc
ion silicat, sunfat, phosphat, florua.
- Lm tng cng ca vch ph, do s to thnh cc hp cht d ho hi v
d nguyn t ho, hay do s hn ch c nh hng bi s ion ho v s kch thch
ph pht x ca nguyn t phn tch. l tc dng ca mt s hp cht, ch yu l
halogen ca kim loi kim v kim th hay lanthanchlorua. S tng cng vch
ph khi nguyn t phn tch tn ti trong nn ca mu l nhng hp cht d ho hi.
Lc cc cht nn ny c tc dng nh l mt cht mang cho s ho hi ca nguyn
t phn tch v lm n ho hi vi hiu sut cao hn. S gim cng ca vch ph
khi nguyn t phn tch tn ti trong nn ca mu l nhng hp cht bn nhit, kh
ho hi. Lc ny cc nguyn t nn kim hm s ho hi ca nguyn t phn tch.
Cc cht nn ny thng l nhng hp cht bn nhit ca cc nguyn t nh nhm,
t him,...
- Trang 88 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
V th vic nghin cu cc nh hng ho hc c trnh by trong mc ny
c tnh cht khi qut chung tt c cc loi c th c chng ta lu khi ng dng
php o ph hp th nguyn t, vi mc ch bit v loi tr cc nh hng ho
hc c th c sp xp theo cc loi sau y:
2.6.3.1. Nng cc axit v loi axit trong dung dch mu
Ni chung nng axit trong dung dch mu lun lun c nh hng n
cng ca vch ph ca nguyn t phn tch. nh hng ny thng gn lin vi
loi anion ca axit. Cc axit cng kh bay hi thng cng lm gim nhiu cng
vch ph.
D

F -AAS
H2O
HCl
HNO3
H2SO4
H3PO4
HF
2

(%)

Hnh: Khi qut v nh hng ca nng axit v loi axit n


cng vch ph hp th
Da vo th trn ta thy cc axit d bay hi gy nh hng nh. iu ny c
th thy r rng khi xc nh Ca khi o vch ph Ca - 422,7 nm trong cc mi
trng ca cc axit HCLO4, CH3COOH, HCl, HNO3, H2SO4, H3PO4, HF vi cng mt
nng l 25.

- Trang 89 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

CH3COOH
H2O

HCl
HNO3
H2SO4
H3PO4

C (g/mL)

Hnh: nh hng ca loi axit n cng vch ph


Ca 422,7 nm trong php o F - AAS (khng kh + C2H2)
Ni chung cc axit lm gim cng ca vch ph theo th t: HClO 4< HCl
< HNO3 < H2SO4 < H3PO4 < HF. Ngha l axit HClO 4, HCl, HNO3 gy nh hng nh
nht trong vng nng nh. Chnh v th trong thc t phn tch ca php o ph
hp th nguyn t (AAS) ngi ta thng dng mi trng l axit HCl hay HNO 3 1
hay 2%. V nng ny nh hng ca hai axit ny l khng ng k (nh hn
5%).
2.6.3.2. nh hng ca cc cation
Dung dch mu phn tch, ngoi nguyn t cn xc nh thng cn cha cc
nguyn t khc. Cc nguyn t ny thng tn ti di dng cation hay anion tan
- Trang 90 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
trong dung dch mu. Cc ion ny c th lm tng, cng c th lm gim hoc cng c
th khng gy nh hng g n cng vch ph ca nguyn t cn phn tch. Khi
c nh hng th mc nh hng ca mi ion cng rt khc nhau trong tng
trng hp c th. Nhng mt cch tng qut th chng ta c th quy nh hng ca
cc cation theo by loi sau:
D

1
Khng c

2
4
7
6
5

C1

C2

C3

3
C4

C5

Nng nguyn t nh hng

Hnh: Khi qut v nh hng ca cation bao gm 7 loi:


Loi 1: Khi C>C2 khng c nh hng.
Loi 2. nh hng cc i C1.
Loi 3. Gim lin tc theo ng cong li.
Loi 4. Khi C< C2 th khng c nh hng.
Loi 5. Gim lin tc theo ng cong lm.
- Trang 91 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Loi 6. Khi C> C2 th khng nh hng na.
Loi 7. Gim lin tc tuyn tnh, khi C tng.
Vi loi 1: khi nng cc ion gy nh hng ln hn C 2 th n khng lm
tng cng vch ph ca nguyn t phn tch na. nh hng ny c s dng
tng nhy ca phng php phn tch mt nguyn t, khi thm vo mu nguyn
t nh hng c nng ln hn C2.
Trong loi 2: ti nng C1 ca nguyn t gy nh hng th cng vch
ph ca nguyn t phn tch t gi tr cc i. V th nh hng ny cng c dng
tng nhy ca phng php phn tch. Nhng phi gi (khng ch) nng ca
nguyn t gy nh hng gi tr khng i C1.
Vi trng hp ca loi 3: Trong trng hp ny cng vch ph gim lin
tc theo ng cong li, khi nng nguyn t nh hng tng dn u.
Trng hp ca loi 4: Cc cation ch gy nh hng n cng vch ph
ca nguyn t phn tch khi nng ca n ln hn gi tr C 2. Do vy nu nng
ca cc cation trong mu nh hn gi tri C 2 th khng phi quan tm tm bin
php loi tr.
Trong trng hp loi 5: Trong trng hp ny cng vch ph ca nguyn
t phn tch li b gim lin tc theo ng cong lm, khi nng cation gy nh
hng trong dung dch mu tng dn v y nht thit phi tm bin php loi tr
nh hng ny.
Vi nh hng ca loi 6: Khi nng cc cation khc trong mu ln hn gi
tr C2 th chng khng lm thay i cng vch ph ca ngun t phn tch. Do
nu khng tm c bin php loi tr ph hp, th chng ta thm vo mu cation gy
nh hng vi nng ln hn gi tr C2, a nh hng gim thnh mt gi tr
hng s cho tt c cc mu phn tch v mu chun. Nh th cng loi b c nh

- Trang 92 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
hng ny. Nhng tt nhin l ta lm gim nhy ca phng php phn tch i mt
t.
Cui cng l cc nh hng thuc loi 7: y cc cation l lm gim lin
tc cng vch ph ca nguyn t phn tch theo chiu tng dn nng ca n
mt cch tuyn tnh. Do cng tm bin php ph hp loi tr nh hng ny,
hoc gi cho cc cation l c nng nht nh v khng i trong tt c cc mu
chun v cc mu phn tch.
nh hng cc cation trong dung dch mu n cng vch ph ca nguyn
t phn tch trong php o ph hp th nguyn t vi k thut nguyn t ho trong
ngn la v khng ngn la cng rt khc nhau. V d ion La (III) trong php o F AAS l yu t loi tr nh hng ca cc ion l khi xc nh Ca, Mg, Mn, Al, Fe.
Nhng chnh La (III) li l ion lm gim cng vch ph ca chnh Ca, Mg, Al, Fe
rt ln trong php o ETA - AAS. iu ngha l mi cation trong tng trng hp
c th v trong mi php o li c tc dng khc nhau, m chnh n trong php o ny
th nh hng, nhng trong php o khc li khng gy nh hng.
loi tr nh hng ca cc cation n cng vch ph ca nguyn t
phn tch chng ta c th s dng mt s bin php sau y hoc ring bit hoc t
hp chng vi nhau:
- Chn iu kin x l mu ph hp loi cc nh hng ra khi dung dch
mu phn tch o ph.
- Chn cc thng s ca my o thch hp.
- Thm vo mu phn tch nhng cht ph gia ph hp loi tr cc nh
hng ca cc cation nh LaCl3, SrCl2, AlCl3 trong php o F - AAS v LiBO 2,
NH4NO3 hay hn hp (LiBO2+ NH4NO3) trong php o ETA - AAS hay nhng cht
ph gia khc. Tt nhin trong mi trng hp c th cn phi nghin cu chn
c loi cht v nng ph hp vi n.
- Trang 93 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.6.3.3. nh hng ca cc anion
Cng vi cc cation, cc anion cng nh hng n cng vch ph ca
nguyn t phn tch. nh hng ny v tnh cht cng tng t nh nh hng ca
cc loi axit. Ni chung anion ca cc axit d bay hi thng lm gim t n cng
o vch ph. Ch ring c hai anion ClO 4, CH3COO- l gy hiu ng dng (lm
tng). Tc l lm tng cng vch ph ca nguyn t phn tch trong mt s
trng hp mt vng nng nht nh. Cc anion khc thng gy hiu ng m
(lm gim) theo th t Cl-, NO32-, CO32-, SO42-, PO43-, SiO32-. Trong anion SiO32- c
nh hng ln nht, cn t nht l ion Cl-. ng thi khi nng ca cc anion tng
th tc dng nh hng cng tng theo. Do thc t nn trong mi php o phi gi
cho nng cc ion trong mu phn tch cng nh mu chun l nh nhau v mt
gi tr nht nh khng i. Mt khc cng khng nn chn axit H 2SO4 lm mi
trng ca mu cho php o AAS m ch nn dng axit HCl hay HNO 3 vi nng
di 2%.
2.6.4. Thnh phn nn ca mu
Yu t nh hng ny ngi ta quen goi l matrix effect. Nhng khng phi
lc no cng xut hin, m thng ch thy trong mt vi trng hp nht nh.
Thng thng l cc mu c cha cc nguyn t nn di dng cc hp cht bn
nhit, kh bay hi v kh nguyn t ho. V d khi xc nh cc tp cht lng vt
trong cc mu oxit t him, oxit kim loi km th, oxit nhm, oxit zircn, cc mu
mui NaCl, th cc nn ny s kh cng ca vch ph ca nguyn t phn tch.
Qua lm gim nhy ca phng php phn tch. Trong nhiu trng hp yu t
ny lm gim hng chc ln, thm ch hng trm ln cng ca vch ph. Nguyn
nhn chnh ca nh hng ny l s tn ti ca hp cht bn nhit trong mi trng
hp th . Cc hp cht ny lm kh khn, cn tr qu trnh ho hi v nguyn t ho
ca cc nguyn t phn tch.

- Trang 94 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Bng: nh hng cc thnh phn nn ca mu phn tch


Cng vch ph C = 30 ppb php o ETA Cht nn ca mu
1. Dung dch HCl 1%
2. Nh 1, thm 2% LaCL3
3. Nh 1, thm 0,5% LaCL3
4. Nh 2, thm 1%

AAS
Mg - 202,60 nm
0,220
0,020
0,050
0,210

Ca - 422,70nm
0,250
0,025
0,060
0,245

NH4NO3
loi tr nh hng ca thnh phn nn ngi ta c th dng nhiu bin
php khc nhau:
1. Tng nhit nguyn t ho mu .
2. Thm vo mu cc cht ph gia c nng ph hp ngn cn s xut
hin ca cc hp cht bn nhit.
3. Tch loi b nguyn t nn, khi hai nguyn t trn khng t kt qu. Tt
nhin bin php ny l hu hn.
Trong ba bin php trn, bin php th nht cng ch thc hin c trong
mt chng mc nht nh. V chng ta khng th tng nhit nguyn t ho ln
cao mi c, do s hn ch ca trang thit b, bn cht ca kh t, hn na khi
nhit nguyn t ho mu qu cao th li xut hin nh hng ca s ion ho v
s pht x. Cho nn bin php hai l thng dng nht. Cc cht ph gia thng
c dng trong php o F - AAS l LaCl3, SrCl2, LiCl, KCl, AlCl3. y LaCl3
c s dng rng ri nht, cc cht cn li ch cho mt s trng hp ring bit.
Ngc li trong php o ETA - AAS cht ph gia c dng nhiu nht l LiBO 2,
NH4NO3 hay hn hp ca hai cht ny trong mt nng ph hp.

- Trang 95 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.6.5. nh hng ca dung mi hu c
Trong php o ph hp th nguyn t, c bit l i vi k thut nguyn
t ho mu trong ngn la, s c mt ca dung mi hu c trn ln vi nc trong
dung dch mu phn tch, hay mu phn tch ho tan trong dung mi hu c
thng lm tng cng ca vch ph hp th nguyn t ca nhiu nguyn t
ln nhiu ln. y l mt phng php tng nhy ca phng php ny. V
th khi phn tch cc nguyn t c nng nh st gii hn di ca php o,
chng ta c th thm vo mu phn tch mt dung mi hu c c nng ph hp
th c th tng nhy ca phng php phn tch ln n hai hay i khi ba ln
so vi khi ch dng dung mi nc, v phi c tinh khit cao. Nu dung mi c
tinh khit khng cao th chng li lm nhim bn mu phn tch. Hoc dung
mi hu c khng tan trong nc, th chng ta c th chit nguyn t phn tch t
dung mi nc dng hp cht phc, v d cc phc Me - APDC vo trong dung
mi hu c. V d dung mi MIBK (metyl Izobutyl Ketone) l dung mi hu c
in hnh chit cc phc Me - APDC cho php o F - AAS. Me l cc ion kim
loi nng, APDC l Amonnium Pyrolydine Dithio - Carbamate. Cc phc Me APDC c chit tt vo MIPK, CHCl3, CCl4 trong mi trng pH t 2 - 6.
Bng: nh hng ca dung mi hu c n cng vch ph
S
TT
1
2
3
4
5
6
7
8
9

Dung mi hu c thm vo
Dung dch HCl 0,1 M
Dung dch nc c 40% CH3OH
Dung dch nc c 40% C2H5OH
Dung dch nc c 40% Aceton
Dung dch nc c 20% Izo butanol
Dung dch nc c 70 % Aceton
Dung dch nc c 50% EAK
Dung dch nc c 80% Ethyl Amine Ketone
(EAK)
Trong MIBK (methyl Izobutyl Ketone)
- Trang 96 -

Cng
Cu - 324,70nm
1,000
1,670
1,750
2,000
2,400
2,50
2,600
2,800
3,000

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.7. K THUT HA HI NGUI XC NH THY NGN (COLD VAPOR
MERCURY TECHNIQUE)
2.7.1. Gii thiu
- CV - AAS l phng php quang ph hp x nguyn t khng ngn la, s
nguyn t ho thu ngn (Hg) c thc hin ngay ti nhit thng v Hg l
nguyn t tn ti th lng v c th bay hi ti nhit phng. Nh c tnh ring
bit ny nn Hg l nguyn t duy nht thch hp cho vic xc nh m khng cn
nguyn t ho sau khi c kh ti trng thi c bn. V vy hu nh ton b hi
thu ngn u tham gia vo qu trnh hp th.
- H thng CV - AAS c b ho hi lnh Hg gm cc bnh phn ng v h
thng li cun hi thu ngn.
2.7.2. Nguyn tc
Trong k thut ha hi ngui, ion Hg 2+ trong dung dch mu c kh thnh
nguyn t t do bng cch cho phn ng vi mt cht kh mnh nh thic clorua
(SnCl2) hoc natri tetrahydroborate (NaBH4) trong mt h thng kn. Sau , hi thy
ngn t do c dn t bnh phn ng n b phn hp th bng cch sc mt dng
kh mang thch hp, tr vi Hg (khng kh, nit hoc argon) vo dung dch mu. i
khi b phn hp th c gia nhit cht t (khong 100oC) trnh ngng t hi
nc.
Nu cht kh l SnCl2 th Hg2+ b kh theo phng trnh:
Sn2+ + Hg2+ Hg0 + Sn4+
Nu cht kh l NaBH4 th Hg2+ b kh theo phng trnh:
Hg2+ + 2BH4- Hg0 + H2 + B2H6
u im
- Trang 97 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- nhy ca phng php CV- AAS l ln hn khi so vi kt qu thu
c t phng php F-AAS. C th hiu sut ly mu l 100% (so vi 10% ca k
thut ngn la). Ton b Hg trong dng dch mu t trong bnh phn ng u
c nguyn t ho v c vn chuyn n cell mu v o.
- nhy c th tng ln nh s dng cc mu c th tch ln hn v ton b
hi Hg cha trong mu c gii phng o. Khi tng th tch mu th c ngha l
c nhiu nguyn t Hg c hiu lc c chuyn di ti cell mu v o.
- Gii hn pht hin ca CV-AAS khong 0.02ug/L.
2.8. K THUT TO HYDRIDE (HYDRIDE GENERATION TECHNIQUE)
2.8.1. Nguyn tc
K thut to hydride c mt im ging k thut ha hi ngui l mu c
cho phn ng vi mt cht kh, sau , kh sinh ra c dn n b phn hp thu
o. Tuy nhin, khc vi k thut ha hi ngui, kh sinh ra khng phi l hi nguyn
t t do m l hi phn t ca cc hp cht hydride. Cc phn t ny khng gy ra
hp thu nguyn t nn cn phi cung cp nhit phn hy chng thnh cc nguyn
t t do. K thut hydride c th c s dng phn tch cc nguyn t As, Pb, Sn,
Bi, Sb, Te, Ge, Se.
Trc y s to thnh cc hp cht hidrua AsH 3, SbH3 v H2Se trong dung
dch thng c thc hin nhiu nht bng phn ng:
Zn + 2 HCl ZnCl2 + 2 [H]
Em+ +(m+n) [H] EHn + mH+
Trong : E l kim loi cn phn tch, m c th bng hoc khc n.

Nhng do phn ng trn c nhiu hn ch nh:


- Trang 98 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Xy ra chm.
Kh t ng ho.
Kt qu phn tch ph thuc nhiu vo tinh khit ca km.
Hiu qu phn ng b gii hn v phn ng xy ra khng hon ton v cc
hp cht hidrua d bay hi b hp ph hoc b by trong lp mt km.
V th, thay cho qui trnh trn ngi ta s dng mt cht kh c hiu qu hn
l NaBH4.
NaBH4 + 3 H2O + HCl H3BO3 +NaCl + 8 [H]
Em+ + [H] EHn + H2
V d:
Phn ng kh chuyn As (V) v As (III) trong qu trnh x l mu:
H3AsO4 + 3I- + 2H3O+ H3AsO3 + I3- + 3H2O
Phn ng vi cht kh NaBH4
H3AsO3 + BH4- + H+ AsH3 + H2 + H3BO3
Phng php ny c s dng nhiu hn hn so vi phng php Zn/HCl do
c th p dng vi nhiu nguyn t hn, do tc , hiu qu ca phn ng v gim
c tp cht.
Phn ng xy ra hon ton trong khong thi gian t 10- 30s.
Tc cht c thm vo dung dch mu c acid ho trong khong t 0.110%.
Cc nhn t trn y gip cho s t ng ho d dng hn v l yu t quan
trng to nn s thnh cng cho k thut to thnh cc hp cht hidrua.
- Trang 99 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Acid dng cho qui trnh nu trn l HCl, HNO3 v H2SO4 cng c s dng.
Nng ti u ca acid l mt thng s cho s ti u ho, n c th thay i
rt ln ph thuc vo nguyn t phn tch v cht nn.
Hn ch ca phn ng:
Tc cht khng phi hon ton khng ln tp cht, lm nh hng n
nhy gii hn pht hin.
Lng ln kh H2 c phng thch cng gy cn tr.
2.8.2. Cc qu trnh din ra trong t bo nguyn t ha
Cc hp cht kh hidrua trong t bo nguyn t ho c t nng b phn
ly thnh cc nguyn t t do. S phn ly cc hp cht hidrua to thnh cc nguyn
t t do ny ch yu l t phn ng vi cc gc hidro t do, tuy nhin cc gc oxi
cng c vai tr tng t.
Hin nay vi cc t bo nguyn t ho thng c s dng l cc ng thch
anh rng, cc phn ng bn trong ng nguyn t ho thch anh c th xy ra nh sau:
H + O2 OH + O
O + H2 OH + H
OH + H2 H2O + H
Nng ca cc gc hidro t do trong ng nguyn t ho cn phi ln hn
nhiu ln so vi nng gc hidroxyl t do. V th nu a mt hp cht hidrua kim
loi vo ng nguyn t ho thch anh th n s tip tc tri qua cc phn ng sau
cui cng gii phng nguyn t kim loi t do dng kh:
EHn + H EHn-1 + H2
EH + H E + H2
- Trang 100 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Ngoi qu trnh trn, s phn hu nhit cc hp cht hidrua cng c cho l
c xy ra, tuy nhin n ch xy ra khi ngun cung cp oxy cho ng nguyn t ho
khng .
u im: k thut hydride c nhy cao v loi b c nh hng ca nn
(matrix interference).
Nhc im:
- Hiu sut to hydride v nguyn t ha ph thuc mnh vo nhiu yu t bao
gm trng thi oxi ha ca nguyn t cn phn tch, thi gian phn ng, p sut kh,
nng axit v nhit ca b phn hp th.
- S to thnh hydride cng b nh hng bi cc cht trong thnh phn mu,
do , k thut ny vn b nh hng v mt ha hc (chemical interference).
2.8.3. Cn nhiu
Trong giai on to hp cht hidrua, s cn nhiu c to nn do s c mt
ca cc ion kim loi ngoi cht phn tch.
Cc nghin cu cho thy phng php phn tch bng k thut to hp cht
hidrua cng chu s cn nhiu c giai on to hp cht hidrua v giai on nguyn
t ho. S cn nhiu lm thay i tn hiu phn tch (thng l lm gim tn hiu).
Chng hn nh khi phn tch As v Se nu trong mu cn c cc ion kim loi
chuyn tip khc nh Cu(II), Co(II), Ni(II)... th hiu sut to thnh cc hp cht
hidrua vi cht phn tch s gim, ng thi cc tn hiu phn tch ca As v Se cng
b che i. l do hidrua ca cht phn tch phn ng vi cc sn phm to thnh t
phn ng ca cc kim loi vi NaBH4.
Tuy nhin cng c th gim nhiu bng cch thm NaBH 4 vo t t vi nng
thp.

- Trang 101 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Trong h thng tim theo dng lin tc th s cn nhiu cng c gim thiu,
do trong h thng ny hu nh khng c mt thi gian no m cht kh v sn phm
phn ng hin din vi nng qu cao.
Khi phn tch cc nguyn t trong cc mu sinh hc, acid nitric thng c
dng ph mu v acid ho mu trc khi thm cht kh NaBH 4 v iu ny gy
nn vn l c s hin din ca cc oxit nit trong by nhit thp dng thu
thp cc phn t cht hidrua lm gim hiu sut to hp cht hidrua.
khc phc hin tng ny ngi ta thm mt lng acid sunfamic khi ph
mu.
Trong giai on nguyn t ho, tn hiu phn tch thng b trit tiu do b mt
ng nguyn t ho thch anh khng b thu tinh ho, v hoc b nhim bn do s tch
t cc git cht lng nh b bm trn b mt ng.
Qu trnh nguyn t ho cng c th b dp tt nu c s hin din ca cc vt
dung mi hu c.
Ngoi ra, hiu sut nguyn t ho cn gim st do s hnh thnh cc phn t
bn nhit.
gim nhiu do nhng nguyn nhn trn, c th lm sch b mt ng nguyn
t ho thch anh bng HF, tng nhit nguyn t ho bng cch s dng cc h
thng nguyn t ho c nhit cao v tng nng cc gc hidro t do trong ng
thch anh.

- Trang 102 -

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SVTH: Phm Th Kim Trinh

CHNG 3
PHNG PHP X L S LIU
3.1. XC NH HM LNG KIM LOI BNG PHNG PHP AAS
nh sng vi bc sng c trng c cng ban u I 0 c hng i qua
m hi cc nguyn t t do trng thi c bn. Cng nh sng s b gim mt
lng xc nh ty thuc vo mt nguyn t trong ngn la. Sau , nh sng s
c hng i vo detector o cng cn li I. Lng nh sng b hp thu c
xc nh bng cch so snh I vi I0.

Hnh: Qu trnh o hp thu nguyn t


C nhiu thut ng c dng nh ngha lng nh sng b hp thu:
truyn qua (transmittance): l t s gia cng cn li v cng
ban u, n cho bit phn nh sng i xuyn qua khi ngn la vo detector.
T = I/I0
Phn trm truyn qua (percent transmission): l truyn qua biu din
theo phn trm.
%T = 100 * I/I0
Phn trm hp thu (percent absorption): l phn trm cng ban u b
hp thu trong ngn la.
%A = 100 - %T
- Trang 103 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
hp thu (absorbance)
A = log(I0/I)
i lng hp thu c s dng rng ri nht c trng cho s hp th
nh sng v n c quan h tuyn tnh vi nng theo nh lut Beer:
A = a.b.c
Trong :

A: hp thu
a: h s hp thu, l mt hng s c trng cho mi nguyn t v

ph thuc vo thit b.
b: di quang l.
c: nng ca cht hp thu.
nh lut ny c pht biu mt cch n gin l: Trong mt tnh trng

hp thu

thit b xc nh, hp thu t l thun vi nng cht hp thu.


.

Da vo nh lut ny, khi o hp thu ca cc dung


dch bit trc nng , ta c th dng mt ng
chun th hin s ph thuc ca hp thu vo nng
. Trong vng tun theo nh lut Beer, ng chun
l mt ng thng. Khi nng v hp thu tng
ln s c nhng yu t xy ra c th lm ng chun
Nng

khng cn thng na.

Hnh: ng chun
Sau khi dng c ng chun, ta o hp thu ca dung dch cha bit
nng v t ng chun suy ra nng ca cht cn phn tch.

- Trang 104 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
3.2. NH TR PHNG PHP XC NH
3.2.1. Mc ch ca vic nh tr:
- Xc lp gi tr cho phng php p dng trong tng phng th nghim c th.
- Kim tra cht lng trong phng th nghim (vit hng dn cng vic, kim
tra tay ngh, biu kim sot cht lng).
- L yu cy bt buc ca ISO/IEC 17025:2005 v tiu ch c bn cho cc t
chc cng nhn.
Cc thng s nh tr y :
1. chn lc ca phng php.
2. ng ca phng php.
3. chm ca phng php.
4. Khong lm vic.
5. Gii hn pht hin.
6. Gii hn nh lng.
7. n nh ca phng php.
8. khng m bo o ca phng php.
Bi bo co ny ch xin trnh by cch xc nh gii hn pht hin, gii hn
nh lng, hiu sut thu hi v biu kim sot cht lng.
3.2.2. Gii hn pht hin LOD v gii hn nh lng - LOQ
3.2.2.1. nh ngha:
- LOD l lng thp nht ca cht cn phn tch trong mu th c th cho kt
qu c phn bit c khi so vi mu trng.

- Trang 105 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
- LOQ l lng thp nht ca cht cn phn tch trong mu th c th xc nh
c vi ng v chnh xc chp nhn c.
3.2.2.2. Cch xc nh: S dng mu trng.
Tin hnh phn tch 20 mu trng c lp, mi mu o mt ln, sau , tnh
lch chun SD ca mu th.

(x
n

SD

x)2

(n 1)

LOD = X + 3*SD
LOQ = X + 10*SD
Trong :

X: gi tr trung bnh ca mu trng.


SD: lch chun ca cc ln th nghim mu.

3.2.3. Hiu sut thu hi


Cch tin hnh: thm chun vo nn mu khng c cht cn phn tch.
H%=

|gi tr c trn ng chun gi tr blank vo|*100


gi tr thm vo

3.2.4. Biu kim sot cht lng


Cch tin hnh:
Da vo hiu sut thu hi ca cc mu kim sot cht lng c phn tch
trong thi gian di, sau tnh gi tr trung bnh (X) v lch chun SD.
- Gii hn cnh bo (WL): = X 2SD
- Gii hn hnh ng khc phc (AL): = X 3SD

- Trang 106 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Hnh: v d v mt control chart


ngha ca biu :
- Phng php c kim sot tt khi:
+ Hiu sut thu hi ca cc mu kim sot nm trong khong gii hn cnh
bo.
+ Mt gi tr nm trong vng gia gii hn cnh bo v gii hn hnh ng
nhng c 2 gi tr lin tip trc nm trong khong gii hn cnh bo.
- Phng php hot ng trong tm kim sot nhng khng tha mn kim
sot v mt thng k:
+ C lin tc 7 gi tr nm trong khong gii hn cnh bo nhng xu hng
tng dn hoc gim dn.
+ C lin tc 10 trong 11 gi tr trong khong gii hn cnh bo nhng nm
mt bn ca trc gi tr.
- Trang 107 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
C sai s h thng.
- Phng php khng kim sot c khi:
+ Gi tr mu kim sot nm trong khong gii hn hnh ng khc phc.
+ Mt gi tr nm trong vng gia gii hn cnh bo v gii hn hnh ng
nhng c t nht 1 trong 2 gi tr lin tip trc nm trong khong gii hn cnh
bo v gii hn hnh ng khc phc.

- Trang 108 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

PHN III: XC NH HM LNG ASEN, THY NGN,


SELEN, ANTIMON C TRONG NC
PHM VI P DNG
Phng php ny dng xc nh hm lng cc kim loi thng thng trong
mu nc bng quang ph pht x plasma.
Cc nguyn t Asen (As), Selen (Se), Antimon (Sb) c xc nh bng k
thut ha hi hydride quang ph hp thu nguyn t (HG AAS).
Nguyn t Thy ngn (Hg) c xc nh bng k thut ha hi lnh quang
ph hp thu nguyn t (CV AAS).

CHNG I
XC NH HM LNG ASEN C TRONG NC
1.1. NGUYN L
Trong mi trng acid, NaBH4 chuyn As thnh dng hydride tng ng. Hi
hydride c kh mang Ar a n ng thch anh c nung nng bng nhit in
thc hin qu trnh nguyn t ha chuyn thnh hi nguyn t, t nh lng
tng nguyn t bng k thut ha hi hydride quang ph hp thu nguyn t (HG
AAS).
Trng hp c yu cu phn tch hm lng cao trong mu nc, c th xc
nh bng quang ph pht x Plasma.
1.2. TI LIU THAM KHO
APHA 3114B
- Trang 109 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
APHA 3030G
Flow Injection Mercury/Hydride Analyses Recommended Analytical
Conditions ang General Information.
1.3. THIT B, HA CHT, CHT CHUN
1.3.1. Thit b - dng c:
My ph pht x nguyn t Plasma v cc thit b kt ni cn thit khc.
My quang ph hp thu nguyn t - k thut ha hi hydride (HG-ASS).
Cc thit b cn thit khc: cn phn tch, bp in
Cc dng c thy tinh: bnh nh mc, phu, a, beaker, mt knh ng h,
1.3.2. Ha cht dung dch ha cht:
1.3.2.1. Ha cht:
Nc ct hai ln ( dn >18M ).
Hydrochloric acid m c (Merk).
Nitric acid m c (Merk).
Sulfuric acid m c (Merk)
Acid Ascorbic (Merk)
Potasium Iodate (KI) tinh khit ha hc
Khng kh nn c lm kh.
Kh Argon tinh khit 99,99%.
1.3.2.2. Dung dch ha cht:
Dung dch hn hp KI Acid Ascorbic: ha tan 5g KI v 5g Acid Ascorbic vi
nc ct, nh mc thnh 100mL.
- Trang 110 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

1.3.3. Cht chun:


Cc cht chun c giy chng nhn hm lng v cn hn s dng. Cc cht
chun c th dng n cht hay hn hp ty theo nhu cu phn tch.
a. Dung dch chun As: thm acid HCl m c v hn hp KI Acid
Ascorbic (5g KI va 5g Acid Ascorbic vi nc ct thnh 100mL) t nng 5%.
b. Dung dch Blank chun: Thay mu th bng nc ct, chun b Blank theo
ton b quy trnh chun b mu.
c. Mu kim sot cht lng: Dung dch ny mua t cc nh cung ng v c
giy chng nhn.
1.4. CHUN B DUNG DCH MU
1.4.1. Chun b mu cho phn tch nguyn t kim loi Asen APHA 3114 B
Rt chnh xc 50 ml mu th vo Erlen 250 ml.
Thm 5 ml acid HNO3 v t ln bp in, dung dch si nh v ha hi cn
khong 15 20 ml.
Lm ngui, thm 5 ml H2SO4, t Erlen tr li bp in. Cho dung dch ha hi
n khi khi trng SO3 xut hin.
ngui dung dch, thm mt vi ml acid HNO3 v cho ha hi trn bp in.
Lp li qu trnh ny n khi dung dch khng cn cht hu c (thng thng dung
dch tr nn trong hoc mu khng thay i).
Thm mt t nc ct v cho ha hi n khi cn 15 20 ml.
Thm acid HCl m c v hn hp KI Acid Ascobic t nng 5%. nh
mc bng nc ct v yn dung dch khong 30 60 pht nhit phng.
- Trang 111 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Dung dch c chuyn sang cho nhm Quang ph phn tch trn thit b
quang ph hp thu nguyn t - k thut ha hi hydride (HG AAS).
1.4.2. Chun b mu blank v mu kim sot cht lng
1.4.2.1. Mu blank: c chun b trong cng mt l mu, thc hin thm y
cc tc cht nhng khng c mu th.
1.4.2.2. Mu kim sot cht lng: thc hin trn mu chun bit trc hm
lng hoc thm dung dch chun vo mu. Thc hin thm dung dch chun vo mu
(c xc nh khng c cu t cn phn tch) sao cho hm lng trong dung dch
cui ca mu thm chun phi nm trong khong gia ng chun. Hm lng thm
cho tng cu t khc nhau c th thay i do nhy ca thit b p ng vi tng
cu t khc nhau.
1.5. BO CO KT QU TH NGHIM
Cng thc tnh:
Hm lng nguyn t (X) c trong mu th c tnh theo cng thc:
X (mg / L)

(C Cblank ) xVxF
m

Trong :
m: lng mu, mL.
V: th tch nh mc, mL.
F: h s pha long (nu c).
C: nng nguyn t trong mu th c t ng chun, mg/L.
C blank: nng nguyn t trong mu blank c t ng chun, mg/L.
Phng trnh ng chun ca Asen
Nng (g/L)

- Trang 112 -

10

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
hp thu

0.0533 0.1046 0.2301 0.4149

Ta o c hp thu ca dung dch mu l 0.0264 nn t phng trnh ng


chun trn Hm lng thy ngn c trong dung dch mu l 0.118 (g/L).

- Trang 113 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

CHNG II
XC NH HM LNG THY NGN C TRONG NC
2.1. NGUYN L
Cc dng thy ngn (ion) c NaBH4 chuyn v dng thy ngn t do, kh
mang Ar li ko dng t do ny n ng thch anh c nung nng bng nhit in
thc hin qu trnh nguyn t ha chuyn thnh hi nguyn t, t nh lng
trn thit b (CV AAS).
Trng hp c yu cu phn tch hm lng cao trong mu nc, c th xc
nh bng quang ph pht x Plasma.
2.2. TI LIU THAM KHO
APHA 3112B
APHA 3030G
Flow Injection Mercury/Hydride Analyses Recommended Analytical
Conditions ang General Information.
2.3. THIT B, HA CHT, CHT CHUN
2.3.1. Thit b - dng c:
My ph pht x nguyn t Plasma v cc thit b kt ni cn thit khc.
My quang ph hp thu nguyn t - k thut ha hi hydride (HG-ASS).
Cc thit b cn thit khc: cn phn tch, bp in
Cc dng c thy tinh: bnh nh mc, phu, a, beaker, mt knh ng h,
2.3.2. Ha cht dung dch ha cht:
- Trang 114 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
2.3.2.1. Ha cht:
Nc ct hai ln ( dn >18M ).
Hydrochloric acid m c (Merk).
Sulfuric acid m c (Merk)
Potasium persulfate (K2S2O8) tinh khit ha hc.
Potasium permanganate (KMnO4) tinh khit ha hc.
Hydroxyamine sulfate ((NH2OH)2H2SO4) tinh khit ha hc
Sodium chloride (NaCl)
Khng kh nn c lm kh.
Kh Argon tinh khit 99,99%.
2.3.2.2. Dung dch ha cht:
Dung dch KMnO4 5%: ha tan 50g KMnO4 vi nc ct, nh mc thnh 1L.
Dung dch K2S2O8: ha tan 50g K2S2O8 vi nc ct, nh mc thnh 1L.
Dung dch NaCl + (NH2OH)2H2SO4: ha tan 120g NaCl v 120g
(NH2OH)2H2SO4 vi nc ct, nh mc thnh 1L.
2.3.3. Cht chun:
Cc cht chun c giy chng nhn hm lng v cn hn s dng. Cc cht
chun c th dng n cht hay hn hp ty theo nhu cu phn tch.
a. Cc chun lm vic ca nguyn t thy ngn: pha t dung dch gc v cc
hm lng thp hn bng cch pha long trong dung dch Nitric acid 2% v thm acid
HCl t nng 5% trong dung dch cui.
b. Dung dch Blank chun: Thay mu th bng nc ct, chun b Blank theo
ton b quy trnh chun b mu.
- Trang 115 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
c. Mu kim sot cht lng: Dung dch ny mua t cc nh cung ng v c
giy chng nhn.

2.4. CHUN B DUNG DCH MU


2.4.1. Chun b mu cho phn tch nguyn t kim loi Thy ngn APHA 3112B
Rt chnh xc 50 ml mu th vo Erlen 250 ml.
Thm 5 ml acid H2SO4 m c, t ln bp cch thy 950C trong 30 pht.
ngui dung dch, thm khong 5 ml dung dch KMnO 4 5%, lc u v
yn khong 15 pht.
Thm 5 ml dung dch K2S2O8, t Erlen tr li bp cch thy trong 2h.
ngui dung dch, thm mt t dung dch KMnO 4 5%. Nu dung dch cn si
bt th cho Erlen tr li bp cch thy. Lp li vic cho thm KMnO 4 5% n khi
khng cn hin tng si bt lc cho KMnO4 vo.
dung dch mu ngui n nhit phng, thm 5 ml acid HCl m c.
Dng dung dch NaCl + (NH2OH)2H2SO4 kh ht lng KMnO4 cn li trong dung
dch mu.
nh mc dung dch thnh 50 ml bng nc ct.
Dung dch c chuyn sang cho nhm Quang ph phn tch trn thit b
quang ph hp thu nguyn t - k thut ha hi lnh (CV AAS).
2.4.2. Chun b mu blank v mu kim sot cht lng
2.4.2.1. Mu blank: c chun b trong cng mt l mu, thc hin thm y
cc tc cht nhng khng c mu th.
2.4.2.2. Mu kim sot cht lng: thc hin trn mu chun bit trc hm
lng hoc thm dung dch chun vo mu. Thc hin thm dung dch chun vo mu
- Trang 116 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
(c xc nh khng c cu t cn phn tch) sao cho hm lng trong dung dch
cui ca mu thm chun phi nm trong khong gia ng chun. Hm lng thm
cho tng cu t khc nhau c th thay i do nhy ca thit b p ng vi tng
cu t khc nhau.
2.5. BO CO KT QU TH NGHIM
Cng thc tnh:
Hm lng nguyn t (X) c trong mu th c tnh theo cng thc:
X (mg / L)

(C Cblank ) xVxF
m

Trong :
m: lng mu, mL.
V: th tch nh mc, mL.
F: h s pha long (nu c).
C: nng nguyn t trong mu th c t ng chun, mg/L.
C blank: nng nguyn t trong mu blank c t ng chun, mg/L.
Phng trnh ng chun ca Thy ngn
Nng (g/L)
hp thu

1
0.006

2
0.012

- Trang 117 -

5
10
0.0303 0.0594

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Ta o c hp thu ca dung dch mu l 0.0036 nn t phng trnh ng


chun trn Hm lng thy ngn c trong dung dch mu l 0.576 (g/L).

CHNG III
XC NH HM LNG SELEN C TRONG NC
3.1. NGUYN L
Trong mi trng acid, NaBH4 chuyn Se thnh dng hydride tng ng. Hi
hydride c kh mang Ar a n ng thch anh c nung nng bng nhit in
thc hin qu trnh nguyn t ha chuyn thnh hi nguyn t, t nh lng
tng nguyn t bng k thut ha hi hydride quang ph hp thu nguyn t (HG
AAS).
Trng hp c yu cu phn tch hm lng cao trong mu nc, c th xc
nh bng quang ph pht x Plasma.
3.2. TI LIU THAM KHO
APHA 3114B
APHA 3030G
- Trang 118 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
Flow Injection Mercury/Hydride Analyses Recommended Analytical
Conditions ang General Information.
3.3. THIT B, HA CHT, CHT CHUN
3.3.1. Thit b - dng c:
My ph pht x nguyn t Plasma v cc thit b kt ni cn thit khc.
My quang ph hp thu nguyn t - k thut ha hi hydride (HG-ASS).
Cc thit b cn thit khc: cn phn tch, bp in
Cc dng c thy tinh: bnh nh mc, phu, a, beaker, mt knh ng h,

3.3.2. Ha cht:
Nc ct hai ln ( dn >18M ).
Hydrochloric acid m c (Merk).
Sulfuric acid m c (Merk)
Nitric acid m c (Merk).
Khng kh nn c lm kh.
Kh Argon tinh khit 99,99%.
3.3.3. Cht chun:
Cc cht chun c giy chng nhn hm lng v cn hn s dng. Cc cht
chun c th dng n cht hay hn hp ty theo nhu cu phn tch.
a. Dung dch chun Se: thm acid HCl m c v hn hp KI Acid
Ascorbic (5g KI va 5g Acid Ascorbic vi nc ct thnh 100mL) t nng 5%.

- Trang 119 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
b. Dung dch Blank chun: Thay mu th bng nc ct, chun b Blank theo
ton b quy trnh chun b mu.
c. Mu kim sot cht lng: Dung dch ny mua t cc nh cung ng v c
giy chng nhn.
3.4. CHUN B DUNG DCH MU
3.4.1. Chun b mu cho phn tch nguyn t kim loi Selen APHA 3114 B
Rt chnh xc 50 ml mu th vo Erlen 250 ml.
Thm 5 ml acid HNO3 v t ln bp in, dung dch si nh v ha hi cn
khong 15 20 ml.
Lm ngui, thm 5 ml H2SO4, t Erlen tr li bp in. Cho dung dch ha hi
n khi khi trng SO3 xut hin.
ngui dung dch, thm mt vi ml acid HNO3 v cho ha hi trn bp in.
Lp li qu trnh ny n khi dung dch khng cn cht hu c (thng thng dung
dch tr nn trong hoc mu khng thay i).
Thm mt t nc ct v cho ha hi n khi cn 15 20 ml.
Thm acid HCl m c t nng 5%, un nng 900C trong 20 pht.
ngui, nh mc bng nc ct.
Dung dch c chuyn sang cho nhm Quang ph phn tch trn thit b
quang ph hp thu nguyn t - k thut ha hi hydride (HG AAS).
3.4.2. Chun b mu blank v mu kim sot cht lng
3.4.2.1. Mu blank: c chun b trong cng mt l mu, thc hin thm y
cc tc cht nhng khng c mu th.
3.4.2.2. Mu kim sot cht lng: thc hin trn mu chun bit trc hm
lng hoc thm dung dch chun vo mu. Thc hin thm dung dch chun vo mu
- Trang 120 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
(c xc nh khng c cu t cn phn tch) sao cho hm lng trong dung dch
cui ca mu thm chun phi nm trong khong gia ng chun. Hm lng thm
cho tng cu t khc nhau c th thay i do nhy ca thit b p ng vi tng
cu t khc nhau.
3.5. BO CO KT QU TH NGHIM
Cng thc tnh:
Hm lng nguyn t (X) c trong mu th c tnh theo cng thc:
X (mg / L)

(C Cblank ) xVxF
m

Trong :
m: lng mu, mL.
V: th tch nh mc, mL.
F: h s pha long (nu c).
C: nng nguyn t trong mu th c t ng chun, mg/L.
C blank: nng nguyn t trong mu blank c t ng chun, mg/L.
Phng trnh ng chun ca Selen
Nng (g/L)
hp thu

1
2
5
10
0.0137 0.0238 0.0637 0.1199

- Trang 121 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Dung dch mu c hp thu l 0.0052 nn t phng trnh ng chun trn


Hm lng Selen c trong dung dch mu l 0.294 (g/L).
3.6. XC NH LOD, LOQ, HIU SUT THU HI V CONTROL CHART
CA PHNG PHP XC NH SELEN
Xc nh LOD, LOQ ca phng php
STT
1
2
3
4
5
6
7
8
9
10
11
12
Gi tr trung bnh
lch chun
LOD
LOQ
- Trang 122 -

Blank(g/L)
-0.146
-0.044
0.174
0.019
0.01
-0.01
0.004
0.001
-0.004
0.038
-0.025
0.025
0.0035
0.0718
0.2188
0.7213

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Xc nh hiu sut thu hi v biu control chart ca phng php


- Hm lng chun thm vo: 3 g/L
Mu A
A1
A2
A3
A4
A5
A6
A7
A8
A9
A10
Blank

Hm lng ban u

Gi tr thc t

Hiu sut thu hi

(g/L)
3
3
3
3
3
3
3
3
3
3

(g/L)
3.241
3.258
3.249
3.247
3.368
3.16
3.245
3.325
3.151
3.078
0.0035

(%)
107.917
108.483
108.183
108.117
112.15
105.217
108.05
110.717
104.917
102.483

Trung bnh
lch chun

STT
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

H - 3SD
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366
96.366

H - 2SD
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887
99.887

106.93
3.521

H
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93
106.93

- Trang 123 -

H + 2SD
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973
113.973

H + 3SD
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494
117.494

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
16
17
18
19
20

96.366
96.366
96.366
96.366
96.366

99.887
99.887
99.887
99.887
99.887

106.93
106.93
106.93
106.93
106.93

113.973
113.973
113.973
113.973
113.973

117.494
117.494
117.494
117.494
117.494

* Control chart

- Hm lng chun thm vo: 8 g/L


Mu B
B1
B2
B3
B4
B5
B6
B7
B8
B9
B10
Blank

Hm lng ban u

Gi tr thc t

Hiu sut thu

(g/L)
8
8
8
8
8
8
8
8
8
8

(g/L)
7.679
8.178
8.022
7.944
8.246
8.402
8.122
8.659
8.28
8.362
0.0035

hi (%)
95.944
102.181
100.231
99.256
103.031
104.981
101.481
108.194
103.456
104.481

Trung bnh
- Trang 124 -

102.113

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
lch chun

3.288

CHNG IV
XC NH HM LNG ANTIMON C TRONG NC
4.1. NGUYN L
Trong mi trng acid, NaBH4 chuyn Sb thnh dng hydride tng ng. Hi
hydride c kh mang Ar a n ng thch anh c nung nng bng nhit in
thc hin qu trnh nguyn t ha chuyn thnh hi nguyn t, t nh lng
tng nguyn t bng k thut ha hi hydride quang ph hp thu nguyn t (HG
AAS).
Trng hp c yu cu phn tch hm lng cao trong mu nc, c th xc
nh bng quang ph pht x Plasma.
4.2. TI LIU THAM KHO
APHA 3114B
APHA 3030G
Flow Injection Mercury/Hydride Analyses Recommended Analytical
Conditions ang General Information.
4.3. THIT B, HA CHT, CHT CHUN
4.3.1. Thit b - dng c:
My ph pht x nguyn t Plasma v cc thit b kt ni cn thit khc.
My quang ph hp thu nguyn t - k thut ha hi hydride (HG-ASS).
Cc thit b cn thit khc: cn phn tch, bp in
Cc dng c thy tinh: bnh nh mc, phu, a, beaker, mt knh ng h,

- Trang 125 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

4.3.2. Ha cht dung dch ha cht:


4.3.2.1. Ha cht:
Nc ct hai ln ( dn >18M ).
Hydrochloric acid m c (Merk).
Sulfuric acid m c (Merk)
Nitric acid m c (Merk).
Acid Ascorbic (Merk)
Potasium Iodate (KI) tinh khit ha hc
Khng kh nn c lm kh.
Kh Argon tinh khit 99,99%.
4.3.2.2. Dung dch ha cht:
Dung dch hn hp KI Acid Ascorbic: ha tan 5g KI v 5g Acid Ascorbic vi
nc ct, nh mc thnh 100mL.
4.3.3 Cht chun:
Cc cht chun c giy chng nhn hm lng v cn hn s dng. Cc cht
chun c th dng n cht hay hn hp ty theo nhu cu phn tch.
a. Dung dch chun Sb: thm acid HCl m c v hn hp KI Acid
Ascorbic (5g KI va 5g Acid Ascorbic vi nc ct thnh 100mL) t nng 5%.
b. Dung dch Blank chun: Thay mu th bng nc ct, chun b Blank theo
ton b quy trnh chun b mu.
c. Mu kim sot cht lng: Dung dch ny mua t cc nh cung ng v c
giy chng nhn.
- Trang 126 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

4.4. CHUN B DUNG DCH MU


4.4.1. Chun b mu cho phn tch nguyn t kim loi Asen APHA 3114 B
Rt chnh xc 50 ml mu th vo Erlen 250 ml.
Thm 5 ml acid HNO3 v t ln bp in, dung dch si nh v ha hi cn
khong 15 20 ml.
Lm ngui, thm 5 ml H2SO4, t Erlen tr li bp in. Cho dung dch ha hi
n khi khi trng SO3 xut hin.
ngui dung dch, thm mt vi ml acid HNO3 v cho ha hi trn bp in.
Lp li qu trnh ny n khi dung dch khng cn cht hu c (thng thng dung
dch tr nn trong hoc mu khng thay i).
Thm mt t nc ct v cho ha hi n khi cn 15 20 ml.
Thm acid HCl m c v hn hp KI Acid Ascobic t nng 5%. nh
mc bng nc ct v yn dung dch khong 30 60 pht nhit phng.
Dung dch c chuyn sang cho nhm Quang ph phn tch trn thit b
quang ph hp thu nguyn t - k thut ha hi hydride (HG AAS).
4.4.2. Chun b mu blank v mu kim sot cht lng
4.4.2.1. Mu blank: c chun b trong cng mt l mu, thc hin thm y
cc tc cht nhng khng c mu th.
4.4.2.2. Mu kim sot cht lng: thc hin trn mu chun bit trc hm
lng hoc thm dung dch chun vo mu. Thc hin thm dung dch chun vo mu
(c xc nh khng c cu t cn phn tch) sao cho hm lng trong dung dch
cui ca mu thm chun phi nm trong khong gia ng chun. Hm lng thm

- Trang 127 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh
cho tng cu t khc nhau c th thay i do nhy ca thit b p ng vi tng
cu t khc nhau.

4.5. BO CO KT QU TH NGHIM
Cng thc tnh:
Hm lng nguyn t (X) c trong mu th c tnh theo cng thc:
X (mg / L)

(C Cblank ) xVxF
m

Trong :
m: lng mu, mL.
V: th tch nh mc, mL.
F: h s pha long (nu c).
C: nng nguyn t trong mu th c t ng chun, mg/L.
C blank: nng nguyn t trong mu blank c t ng chun, mg/L.
Phng trnh ng chun ca Antimon
Nng (g/L)
hp thu

1
2
5
10
0.0242 0.0485 0.1216 0.2246

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Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

Dung dch mu c hp thu l 0.0069 nn t phng trnh ng chun trn


Hm lng Selen c trong dung dch mu l 0.104 (g/L).

KT LUN
Vi tc pht trin nh hin nay th vn nhim mi trng m c bit
l nhim nc c ngha ht sc quan trng i vi s sng cn ca con ngi v
mi sinh vt trn Tri t. V th, tuy vic xc nh hm lng cc kim loi trong
nc ch l mt mng nh trong phn tch nc nhng n cng gp phn vo vic xc
nh cc ngun nc b nhim gip cc c quan chc nng pht hin v c bin
php x l kp thi khng nh hng n sc khe v hot ng sn xut ca con
ngi.
Qua thi gian hc tp trng v thi gian thc tp ti Trung tm k thut 3,
vi s gip ca cc thy c v cc anh ch, chng em xy dng cho mnh mt
s kin thc c bn v l thuyt cng nh kinh nghim thc t. l nhng hnh
trang v cng qu bu gip chng em bc u t lp. Em xin knh gi li cm n
trn trng n cc thy c v cc c ch, anh ch Trung tm k thut 3.

- Trang 129 -

Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

TI LIU THAM KHO

[1] http://vi.wikipedia.org/wiki/N%C6%B0%E1%BB%9Bc
[2]

http://tusach.thuvienkhoahoc.com/wiki/N%C6%B0%E1%BB%9Bc_

%C4%91%C3%B3ng_vai_tr%C3%B2_quan_tr%E1%BB%8Dng_nh%C6%B0_th
%E1%BA%BF_n%C3%A0o%3F
[3]http://vdcnews.socbay.com/vai_tro_cua_nuoc_voi_suc_khoe_con_nguoi285212672-603291094-1
[4] http://vi.wikipedia.org/wiki/Asen
[5] http://vi.wikipedia.org/wiki/Th%E1%BB%A7y_ng%C3%A2n
[6] http://vi.wikipedia.org/wiki/Selen
[7] http://vi.wikipedia.org/wiki/Antimon

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Xc nh hm lng As, Hg, Se, Sb c trong nc


SVTH: Phm Th Kim Trinh

- Trang 131 -

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