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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
- Trang 1 -
- Trang 2 -
LI M U
- Trang 3 -
LI CM N
- Trang 4 -
- Trang 5 -
- Trang 6 -
- Trang 7 -
- Trang 10 -
Gim c Trung Tm
Ph Gim c
Ph Gim c
Th nghim
o lng
P.Qun l Th nghim
PTN. C kh - NDT
P.K thut
Th Nghim
PL. C
PTN. Xy dng
PL. in nng
PTN. in
PL. Nhit
PTN. EMC
PL. Ha l
PTN. Ha hc
PL. di
PTN. Du kh
PTN. Mi trng
PTN. Thc phm
PTN. Vi sinh - GMO
- Trang 11 Hnh 1.1: S c cu t chc
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,
- Trang 14 -
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
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.
- Trang 15 -
- Trang 16 -
- Trang 17 -
TRNG N V
CN B
CHT LNG
NHM PT
VT LIU
CN B K
THUT
NHM NC
MI TRNG
NHM CC LOI
MU KHC
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 -
- Trang 21 -
- Trang 22 -
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
asen, As, 33
Phn loi
kim
15, 4, p
mu xm kim loi
Tnh cht nguyn t
74,92160(2) .v.
119 pm
185 pm
Cu hnh electron
[Ar]3d104s24p3
2, 8, 18, 5
Cu trc tinh th
hp mt thoi
Tnh cht vt l
rn
im nng chy
1.090 K (1.503 F)
im si
th 887 K (1.137 F)
p sut hi
100 k Pa ti 874 K
Thng tin khc
m in
328,88 J/(kgK)
dn in
3x106 /m
dn nhit
50,2 W/(mK)
- Trang 27 -
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 -
- Trang 29 -
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 -
0.01mg/L
0.01mg/L
0.05mg/L (loi A)
0.1mg/L (loi B)
0.5 mg/L (loi C)
Dy ha hc
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 -
200,59 u
150 (171) pm
Bn knh cng ha tr
149 pm
155 pm
Cu hnh electron
2, 1 (baz nh)
Cu trc tinh th
Lng tr xin
Cc thuc tnh vt l
Trng thi
Lng (nghch t)
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
2,295 kJ/mol
im ba trng thi
Vn tc m thanh
1407 m/s 20 C
Linh tinh
in m
140 J/(kgK)
dn in
1,041x106/.m
dn nhit
8,34 W/(mK)
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 -
64,14 h
Hg198 9,97%
Bn vi 118 ntron
0.600
Au197
Bn vi 120 ntron
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:
- Trang 35 -
Trong mt s n in t.
cht c cc mnh).
Sulfua thy ngn (II) (mu thn sa l cht mu cht lng cao).
Telurua cadmi thy ngn l nhng vt liu dng lm u d tia hng ngoi.
Luyn kim.
Nha khoa.
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 -
0.001mg/L
0.001mg/L
0.005mg/L (loi A)
0.01mg/L (loi B)
0.01 mg/L (loi C)
- Trang 39 -
Tng qut
Tn, K hiu, S
selen, Se, 34
Phn loi
phi kim
16, 4, p
xm en nh kim
78,96(3) .v.
116 pm
190 pm
Cu hnh electron
[Ar]3d104s24p4
2, 8, 18, 6
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
p sut hi
100 k Pa ti 958 K
Vn tc m thanh
321,20 J/(kgK)
dn nhit
0,519 W/(mK)
- Trang 40 -
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 -
- Trang 43 -
- Trang 44 -
antimon, Sb, 51
Phn loi
kim
15, 5, p
xm bng bc
Tnh cht nguyn t
121,760(1) .v.
138 pm
Cu hnh electron
[Kr]4d105s25p3
2, 8, 18, 18, 5
-3, 3, 5 ()
Cu trc tinh th
hp mt thoi
Tnh cht vt l
rn
im nng chy
903,78 K (1.167,13 F)
im si
1.860 K (2.889 F)
khng c s liu
Nhit bay hi
193,43 kJ/mol
25,23 kJ/mol
p sut hi
100 k Pa ti 1.858 K
Vn tc m thanh
- Trang 45 -
207,21 J/(kgK)
dn in
2,40x106 /m
dn nhit
24,4 W/(mK)
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 -
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
Hn ch
- Trang 47 -
WHO, 20 g/l
- Trang 48 -
0.005mg/L
0.01mg/L (loi B)
0.01 mg/L (loi C)
- Trang 49 -
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 -
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.
Thc hin th nghim theo hng dn cng vic hoc phng php th ph
hp.
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.
ng v yu cu th nghim li, s dng phng thc kim tra cho khi thy cn
thit).
hng nu c yu cu.
php th.
ngy hoc mi khi s dng bng dung dch/ mu chun km theo (pH, cn ).
- Trang 53 -
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).
tra chun khong 20 mu phn tch nhm kim tra v ti lp iu kin phn tch
nh ban u.
thc hin thng xuyn vi tn xut 2 ln/ tun v c theo di bng vn bn.
- Trang 54 -
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
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
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
- Trang 55 -
Tr mu lu (nu c)
X l theo
M01 TT05
(nu cn thit)
P. H tr k thut
Trnh k
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)
- Trang 56 -
- Trang 57 -
Em
E0
Pht x
- Trang 59 -
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
- Trang 62 -
- Trang 63 -
Phn 1 l thn n v ca s.
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 -
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
450 V
Ar+
M0
Ar+
M0
M*
M*
M0 +
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
0,040
0,340
0,028
0,0007
0,014
0,15
33,0
0,21
0,038
0,03
0,08
0,00095
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
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:
-
- Trang 69 -
- Trang 71 -
2
4
Gii ph lin tc
Vch ph hp th
- Trang 73 -
ng thch anh ch T
- Trang 75 -
- Trang 77 -
- Trang 79 -
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
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
Th kch thch
2000
- Trang 87 -
3000
4000
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 -
F -AAS
H2O
HCl
HNO3
H2SO4
H3PO4
HF
2
(%)
- Trang 89 -
CH3COOH
H2O
HCl
HNO3
H2SO4
H3PO4
C (g/mL)
1
Khng c
2
4
7
6
5
C1
C2
C3
3
C4
C5
- Trang 92 -
- Trang 94 -
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 -
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
- Trang 101 -
- Trang 102 -
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.
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
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 -
- Trang 105 -
(x
n
SD
x)2
(n 1)
LOD = X + 3*SD
LOQ = X + 10*SD
Trong :
- Trang 106 -
- Trang 108 -
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 -
(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
- Trang 113 -
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 -
(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
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 -
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 -
(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 -
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
Hm lng ban u
Gi tr thc t
(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
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 ban u
Gi tr thc t
(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
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 -
- Trang 127 -
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
- Trang 128 -
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 -
[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
- Trang 130 -
- Trang 131 -