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TRNG I HC S PHM
NGUYN TH HN
LUN VN THC S HO HC
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I HC THI NGUYN
TRNG I HC S PHM
NGUYN TH HN
LUN VN THC S HO HC
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LI CM N
Li u tin ca lun vn ny ti xin chn thnh cm n PGS.TS Nguyn
ng c. Thy tn tnh hng dn v gip ti trong qu trnh thc hin
lun vn.
Ti xin chn thnh cm n cc thy c trong Khoa Ha hc, Trng i hc
S phm, i hc Thi Nguyn; cc thy c, anh ch v cc bn trong b mn Ha
hc, Trng i Hc Khoa Hc, i hc Thi Nguyn gip to iu kin cho
ti trong sut qu trnh lm lun vn.
D c nhiu c gng, song do nng lc cn hn ch nn trong lun vn ca
ti chc chn khng th trnh khi thiu st. Ti rt mong nhn c kin ng
gp ca cc thy c v cc bn lun vn ny c hon chnh hn.
Thi Nguyn, thng 8 nm 2010
Hc vin
Nguyn Th Hn
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DANH MC CC CH VIT TT
Vit tt
Ting Anh
Ting Vit
Abs
Absorbance
hp th
AAS
Atomic Absorption
Php o quang ph hp th
Spectrometry
nguyn t
Php o quang ph hp th
Spectrometry
nguyn t ngn la
HCL
n catt rng
ppm
Mt phn triu
F- AAS
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MC LC
Trang
M U ..................................................................................................................1
CHNG 1: TNG QUAN ...................................................................................3
1.1. Gii thiu chung v rau xanh ..........................................................................3
1.1.1. Vai tr ca rau ..........................................................................................3
1.1.2. Th no l rau sch ...................................................................................3
1.1.3. Cng dng ca mt s loi rau ..................................................................4
1.1.4. Mt s tiu ch rau an ton ........................................................................6
1.1.4.1. nh ngha .........................................................................................6
1.1.4.2. Cc yu t gy nhim cho rau ..........................................................7
1.1.4.3. V cht lng ca rau an ton ............................................................9
1.2. Tnh cht ca Cd v Pb [14,22,23] ..................................................................9
1.2.1. Tnh cht vt l .........................................................................................9
1.2.2. Tnh cht ha hc. .................................................................................. 11
1.2.3. Cc hp cht ca Cd v Pb .....................................................................12
1.2.3.1. Cc xt............................................................................................ 12
1.2.3.2. Cc hyroxit..................................................................................... 13
1.2.3.3. Cc mui .......................................................................................... 13
1.3. Vai tr, chc nng v s nhim c Cd, Pb [5,17] ......................................... 14
1.3.1. Vai tr, chc nng v s nhim c Cd................................................... 14
1.3.2. Vai tr, chc nng v s nhim c Pb [10] ............................................ 16
1.4. Cc phng php xc nh Cd, Pb.................................................................17
1.4.1. Phng php phn tch ho hc [13] ....................................................... 17
1.4.1.1. Phng php phn tch khi lng ................................................... 17
1.4.1.2. Phng php phn tch th tch ........................................................ 18
1.4.2. Phng php phn tch cng c .............................................................. 19
1.4.2.1. Phng php in ho [7,13]............................................................ 19
1.4.2.2. Phng php quang ph ...................................................................21
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DANH MC BNG
Trang
Bng 1.1: Hng s vt l ca Cd ............................................................................ 10
Bng 1.2: Hng s vt l ca Pb ............................................................................ 10
Bng 3.1: Kt qu kho st vch ph ca cadimi ................................................... 32
Bng 3.2: Kt qu kho st vch ph ca ch ......................................................... 33
Bng 3.3: Kho st cng dng n vi nguyn t Cd ...................................... 33
Bng 3.4: Kt qu kho st cng dng n vi nguyn t Pb .......................... 34
Bng 3.5 : Kt qu kho st khe o vi nguyn t Cd ........................................... 34
Bng 3.6 : Kt qu kho st khe o vi nguyn t Pb ........................................... 35
Bng 3.7: Kt qu kho st chiu cao n nguyn t ho mu ca Cd ................... 36
Bng 3.8: Kt qu kho st chiu cao n nguyn t ho mu ca Pb .................... 36
Bng 3.9: Kt qu kho st thnh phn kh chy C2H2 i vi Cd.......................... 37
Bng 3.10: Kt qu kho st thnh phn kh chy C2H2 i vi Pb ........................ 37
Bng 3.11: nh hng ca cc loi axit v nng axit ti php o Cd................ 39
Bng 3.12: nh hng ca cc loi axit v nng axit ti php o Pb ................ 39
Bng 3.13: Kho st nh hng ca thnh phn nn .............................................. 41
Bng 3.14: Kt qu kho st nng LaCl3 ........................................................... 41
Bng 3.15: nh hng ca nhm cation kim loi kim ......................................... 42
Bng 3.16: nh hng ca nhm cation kim loi kim th.................................... 43
Bng 3.17: nh hng ca nhm cation kim loi nng ho tr II ........................... 43
Bng 3.18: nh hng ca nhm cation kim loi ho tr III .................................. 43
Bng 3.19 : nh hng tng ca cation ................................................................. 44
Bng 3.20: Kho st nh hng ca anion SO42- ,H2PO4-, F-, I- .............................. 45
Bng 3.21: Kho st nh hng ca tng cc anion ............................................... 45
Bng 3.22 : nh hng ca tng cc cation v anion ............................................. 46
Bng 3.23: Kt qu kho st khong nng tuyn tnh ca Cd ............................ 47
Bng 3.24: Kt qu kho st khong nng tuyn tnh ca Pb ............................ 48
Bng 3.25: Kt qu sai s v lp ca php o cadimi ........................................ 54
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DANH MC HNH
Trang
Hnh 2.1 : S cu to my ph hp th nguyn t .............................................. 29
Hnh 3.1: th kho st khong nng tuyn tnh ca Cd.................................. 48
Hnh 3.2: th kho st khong nng tuyn tnh ca Pb .................................. 49
Hnh 3.3: th ng chun ca cadimi ............................................................... 50
Hnh 3.4: th ng chun ca ch .................................................................... 52
Hnh 3.5: th hm lng Cd qua kt qu phn tch rau mt s x
ca huyn i T tnh Thi Nguyn ....................................................... 64
Hnh 3.6: th hm lng Pb qua kt qu phn tch rau mt s x ca
huyn i T tnh Thi Nguyn ............................................................. 65
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M U
Ngy nay vic bo v mi trng v an ton thc phm l vn quan trng
i vi mi quc gia. Trong i sng, rau xanh lun l ngun thc phm cn thit
v quan trng. Hin nay do nhiu nguyn nhn khc nhau m ch yu l vic s
dng phn bn ho hc, thuc bo v thc vt, thuc tr su, dit c, cht thi ca
cc nh my, khu cng nghip dn n s nhim ngun t, ngun nc v bu
kh quyn. Do rau xanh c th b nhim mt s kim loi nng nh Sn, Pb, Hg,
Mn, Zn... v cc vi sinh vt gy bnh. Nu con ngi s dng phi s b ng c c
th gy ra nhng cn bnh him ngho nh ung th s dn n t vong.
Vn ang c t ra Thi Nguyn ni ring v c nc ni chung l
lm th no c c rau xanh an ton (rau sch)?
Nh vy vic iu tra, nh gi cht lng rau sch tr nn v cng cp thit.
Mt trong cc ch tiu dng nh gi an ton thc phm ni chung v rau sch
ni ring l hm lng cc kim loi nng. Do , vic phn tch tm ra hm lng
cc kim loi nng trong rau xanh trn a bn huyn i T - tnh Thi Nguyn s
gp phn kim sot c cht lng rau sch theo tiu chun rau sch ang c p
dng Vit Nam. C nhiu phng php xc nh hm lng cc kim loi, ty
thuc vo hm lng cht phn tch m c th s dng cc phng php khc nhau:
phng php phn tch th tch, phng php phn tch trng lng, phng php
in ha, phng php phn tch cng c (phng php quang ph, phng php ph
pht x nguyn t AES, phng php ph hp th nguyn t AAS) trong phng
php ph hp th nguyn t ngn la F- AAS l phng php c nhy, chn
lc cao, ph hp vi vic xc nh lng vt cc kim loi nng trong thc phm.
Xut pht t nhng l do trn chng ti chn ti: "Xc nh hm lng Cadimi
v Ch trong mt s loi rau xanh ti huyn i T- tnh Thi Nguyn bng
phng php ph hp th nguyn t ngn la (F-AAS)".
Mc ch: Xc nh c hm lng Cadimi v Ch gy nhim trong rau
xanh v nh gi hin trng nhim bi hai kim loi ny trong rau xanh mt s
x ca huyn i T tnh Thi nguyn.
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nhiu tnh nng v tc dng trong vic phng v cha bnh nh: thanh nhit gii
c ma h, lng huyt, cm mu, cha tm phin, chy mu mi, li ru
vng, kht nc mt, tai chng mt; au u trong trng hp huyt p cao; au
d dy, nng rut, chua, ming kh ng; say sn, ng c sn; gii cc cht c
trong thc n; cc chng bnh chy mu nh chy mu cam, ho nn ra mu; tiu
tiu ra mu, tr, l; sn ph kh sinh; kh h bch i; ph thng ton thn do thn,
b tiu tin; i tho ng; quai b; chng n trong ming hoc l khe ming
tr em; l nga, lot ngoi da, zona, ong cn; rm sy, mn nga; si, thy u tr
em Rau mung cung cp nhiu cht x, c vitamin C, vitamin A v mt s thnh
phn tt cho sc khe, l thc n tt cho mi ngi.
Ci bp c v ngt, tnh hn, khng c, c tc dng ho huyt thanh nhit,
thanh ph, tr m thp, mt d dy, gim c li tiu. Ci bp cng chng suy
nhc thn kinh, gim au nhc, phng chng cc bnh ung th, tim mch v nhiu
loi bnh khc.Theo ty y, ci bp c dng cha bnh thng thng nh:
mn nht, su b t, giun, au d dy. Mt s tc dng cha bnh chnh ca ci
bp c bit n phng bnh ung th v ph n, cha lot d dy, hnh t
trng, phng trnh ung th ng tiu ho
Rau ci xoong trong rau ci xoong cha hm lng vitamin C cao, li c
vitamin A, B1, B2 nn gip bo v sc kho, chng oxi ho, chng c, lm tng
sc khng, chng hin tng lo ho bnh l, gi gn nt ti tr. Rau ci xoong
gip ta n ngon ming li ty c, li tiu, c nhiu cht x nn tc dng tt i vi
d dy, c tc dng thng gan mt v gp phn lm gim bnh mu.
Rau gip c l mt loi rau gia v rt quan trng trong ba n hng ngy ca
gia nh. Ngoi vic d trng, v thm ngon rau gip c cn c nhiu cng dng
cha bnh. Theo ng y gip c c v chua, mi tanh, tnh mt c tc dng thanh
nhit gii c, li tiu, st trng, cha vim phi, th huyt, l lot c t cung, vim
khp, to bn, kit l do vi khun cp tnh... Y hc hin i cng chng minh rau
gip c c tc dng chng nhim khun, chng vi khun, nng cao sc khng v
li tiu. Theo nghin cu ca y hc hin i, trong rau gip c c cht decanoyl-
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10
Cadimi c 8 ng v, trong
112
113
Cd c thit
Cd
[Kr]4d105s2
Cu hnh electron
Nng lng ion ho th nht (eV)
8,99
1,56
Th in cc chun (V)
- 0,402
112,411
321,07
Nhit si (0C)
767
Cu trc tinh th
Lc gic b cht
* Tnh cht vt l ca Pb :
Ch l kim loi mu xm thm, rt mm, d lt mng, c cu trc kiu lp
phng tm din, s th t l 82 trong bng h thng tun hon.
Bng 1.2: Hng s vt l ca Pb
Hng s vt l
Cu hnh electron
Pb
[Xe]4f145d106s26p2
7,42
1,75
Th in cc chun (V)
-0,126
207,21
327,4
Nhit si (oC)
1740
Cu trc tinh th
Lp phng tm din
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11
2PbO
CdX2 (X = halogen)
Pb + X2
PbX2
CdO + H2
2Pb + O2 + 2H2O
2Pb(OH)2
* Cadimi tc dng d dng vi axit khng phi l cht oxi ha, gii phng
kh hiro. V d:
Cd + 2HCl
CdCl2 + H2
2[Cd(H2O)2]2+ + H2
H2PbCl4
PbSO4 + H2SO4
3Pb + 8HNO3 (long)
Pb(HSO4)2
3Pb(NO3)2 + 2NO + 4H2O
2Pb(CH3COO)2 + 2H2O
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12
K2[Pb(OH)4] + H2
1.2.3. Cc hp cht ca Cd v Pb
1.2.3.1. Cc oxit
a. Cadimi oxit:
- CdO c mu t vng n nu gn nh en ty thuc vo qu trnh ch ho
nhit , nng chy 1813oC, c th thng hoa, khng phn hy khi un nng, hi
CdO rt c.
- CdO khng tan trong nc ch tan trong axit v kim nng chy:
CdO + 2KOH(nng chy)
K2CdO2 + H2O
2CdO
Cd(OH)2
CdO + H2O
CdCO3
CdO + CO2
b. Ch oxit :
- Ch c hai xit l PbO, PbO2 v hai oxit hn hp l ch meta planbat Pb2O3
(hay PbO.PbO2), ch orthoplanbat Pb3O4 (2PbO.PbO2)
- Monooxit PbO l cht rn c hai dng : PbO - mu v PbO mu
vng , PbO tan cht t trong nc nn Pb c th tng tc vi nc khi c mt oxi .
PbO tan trong axit v tan trong kim mnh , khi un nng trong khng kh b xi
ha thnh Pb3O4
- ioxit PbO2 l cht rn mu nu en , c tnh lng tnh nhng tan trong
kim d hn trong axit . Khi un nng PbO2 mt dn oxi bin thnh cc oxit trong
ch c s oxy ha thp hn :
PbO2
290 320oC
(Nu en)
530 550o C
()
PbO
(Vng)
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13
2KI
K2[PbI4]
2HCl
H2[PbCl4]
PbCl2 +
1.2.3.2. Cc hyroxit
Cd(OH)2 l kt tu nhy t tan trong nc v c mu trng, cn Pb(OH) 2 l
cht kt ta mu trng khng tan trong nc. Khi un nng chng d mt nc bin
thnh oxit.
Cd(OH)2 khng th hin r tnh lng tnh, tan trong dung dch axit, khng
tan trong dung dch kim m ch tan trong kim nng chy, cn Pb(OH) 2 l cht
lng tnh.
Khi tan trong axit, n to thnh mui ca cation Cd2+, Pb2+ :
Cd(OH)2 + 2HCl
CdCl2 + 2H2O
Pb(OH)2 + 2HCl
PbCl2 + 2H2O
Cd ch tan trong kim nng chy, cn Pb tan trong dung dch kim mnh, n
to thnh mui hiroxoplombit:
Pb(OH)2+ 2KOH
K2[Pb(OH)4]
[Cd(NH3)4](OH)2
1.2.3.3. Cc mui
a. Cc mui ca Cadimi
a s cc mui Cadimi(II) u khng mu. Cc mui sunfat v nitrat ca
cadimi u tan ch c mui sunfua, ccbonat ca chng l t tan trong nc
S ha bi Trung tm Hc liu i hc Thi Nguyn
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14
K2[PbI4]
H2[PbCl4]
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15
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17
Liu lng ti a ch (Pb) c th chp nhn hng ngy cho ngi, do thc n
cung cp, c tm thi quy nh l 0,005mg/kg th trng. Ng c cp tnh do ch
thng t gp. Ng c trng din l do n phi thc n c cha mt lng ch, tuy
t nhng lin tc hng ngy. Ch cn hng ngy c th hp th t 1 mg ch tr ln, sau
mt vi nm, s c nhng triu chng c hiu: hi th thi, sng li vi vin en
li, da vng, au bng d di, to bn, au khp xng, bi lit chi trn (tay b bin
dng), mch yu, nc tiu t, trong nc tiu c poephyrin, ph n d b sy thai.
Ch c nhiu nh hng c hi n cc c quan, t chc trong c th con
ngi. c bit khi xm nhp vo c th, ch c th ph v mt cch mnh lit cc
chc nng chnh ca c th v t y dn n cc bin chng rng, t nn ma n
ri lon thn kinh hay t vong.
1.4. Cc phng php xc nh Cd, Pb
Hin nay, c nhiu phng php khc nhau xc nh cadimi v ch nh
phng php phn tch khi lng, phn tch th tch, in ho, ph phn t UVVIS, sc k lng hiu nng cao (HLPC), ph pht x nguyn t (AES), ph hp th
nguyn t ngn la (F-AAS) v khng ngn la (GF-AAS) Sau y l mt s
phng php xc nh Cadimi v Ch.
1.4.1. Phng php phn tch ho hc [13]
Nhm cc phng php ny dng xc nh hm lng ln (a dng) ca
cc cht, thng thng ln hn 0,05%, tc l mc miligam. Cc thit b v dng
c cho cc phng php ny n gin v khng t tin.
1.4.1.1. Phng php phn tch khi lng
* Nguyn tc: y l phng php da trn s kt ta cht cn phn tch
vi thuc th ph hp, sau lc, ra, sy hoc nung ri cn chnh xc sn phm
v t xc nh c hm lng cht phn tch.
* Cch tin hnh: Vi Cd, ngi ta thng cho kt ta di dng CdS trong
mi trng axit yu.Cn ch kt ta di dng PbSO4, PbCrO4 hay PbMoO4.
Phng php ny n gin khng i hi my mc hin i, t tin, c
chnh xc cao, tuy nhin i hi nhiu thi gian, thao tc phc tp v ch phn tch
hm lng ln, nn khng dng phn tch lng vt.
S ha bi Trung tm Hc liu i hc Thi Nguyn
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PbY2- + 2H+
Tuy nhin, ch rt d thu phn nn trc khi tng pH phi cho Pb 2+ to phc
km bn vi tactrat hoc tritanolamin.
- Cch 2: Chun ngc Pb2+ bng Zn2+. Cho Pb2+ tc dng vi mt lng
d chnh xc EDTA bit nng pH = 10. Sau chun EDTA d bng
Zn2+ vi ch th l ET 00.
Pb2+ + H2Y2-
PbY2- + 2H+
ZnY2- + 2H+
ZnInd + H2Y2-
ZnY2- + HInd
( nho)
(xanh)
PbY2- + Zn2+
ZnY2- + HInd
(xanh)
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Detector
B phn ch th
H thng
- nebulizzer v burner
Dung dch mu
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32
326,1nm
Ln 1
0,3540
0,3350
Ln 2
0,3540
0,3340
Ln 3
0,3540
0,3350
Trung bnh
0,3540
0,3350
%RSD
0,1123
0,2312
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33
Vch o (nm)
217,0 nm
283,3 nm
Ln 1
0,0885
0,0357
Ln 2
0,0887
0,0362
Ln 3
0,0889
0,0358
Trung bnh
0,0887
0,0359
%RSD
0,3429
0,7348
Abs-Cd
60
65
75
83
Ln 1
0,3040
0,2965
0,2882
0,2909
Ln 2
0,3042
0,2967
0,2885
0,2910
Ln 3
0,3044
0,2969
0,2888
0,2909
Trung bnh
0,3042
0,2967
0,2885
0,2909
%RSD
0,5089
0,2613
0,1400
0,2145
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60
70
73
80
Ln 1
0,0890
0,0895
0,0795
0,0853
Ln 2
0,0889
0,0897
0,0794
0,0853
Ln 3
0,0890
0,0893
0,0795
0,0852
Trung bnh
0,0890
0,0895
0,0795
0,0853
%RSD
0,2243
0,5107
0,9325
0,8829
Abs-Pb
0,1
0,2
0,5
1,0
Ln 1
0,3132
0,3130
0,3157
0,3125
Ln 1
0,3134
0,3132
0,3157
0,3124
Ln 1
0,3135
0,3134
0,3157
0,3123
Trung bnh
0,3134
0,3132
0,3157
0,3123
Abs
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35
0,1
0,2
0,5
Ln 1
0,0871
0,0868
0,0875
0,0872
Ln 2
0,0870
0,0869
0,0875
0,0871
Ln 3
0,0869
0,0870
0,0875
0,0873
Trung bnh
0,0870
0,0869
0,0875
0,0872
Abs
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Abs- Cd
Ln 1
0,3127
0,3128
0,3131
0,3131
0,3026
Ln 2
0,3129
0,3128
0,3129
0,3131
0,3028
Ln 3
0,3123
0,3127
0,3130
0,3131
0,3027
Trung bnh
0,3126
0,3128
0,3130
0,3131
0,3027
Abs- Pb
Ln 1
0,0856
0,0848
0,0852
0,0858
0,0845
Ln 2
0,0857
0,0849
0,0850
0,0858
0,0846
Ln 3
0,0857
0,0848
0,0851
0,0858
0,0845
Trung bnh
0,0857
0,0848
0,0851
0,0858
0,0845
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Abs-Cd
0,9
1,0
1,1
1,2
1,3
Ln 1
0,3125
0,3023
0,3127
0,3129
0,3124
Ln 2
0,3125
0,3022
0,3126
0,3129
0,3123
Ln 3
0,3124
0,3022
0,3126
0,3129
0,3122
Trung bnh
0,3125
0,3022
0,3126
0,3129
0,3123
0,9
1,0
1,1
1,2
1,3
Ln 1
0,0867
0,0870
0,0869
0,0871
0,0868
Ln 2
0,0866
0,0869
0,0870
0,0871
0,0866
Ln 3
0,0867
0,0869
0,0870
0,0871
0,0862
Trung bnh
0,0867
0,0869
0,0870
0,0871
0,0865
Abs - Pb
http://www.lrc-tnu.edu.vn
38
http://www.lrc-tnu.edu.vn
39
HNO3
Ln 1
0,3045
0,3051
0,3052
0,3042
Ln 2
0,3047
0,3058
0,3053
0,3046
Ln 3
0,3043
0,3050
0,3053
0,3047
Trung bnh
0,3045
0,3053
0,3053
0,3045
0,1240
0,5498
0,1860
0,3415
Ln 1
0,3045
0,3009
0,2992
0,2968
Ln 2
0,3047
0,3008
0,2990
0,2968
Ln 3
0,3043
0,3009
0,2985
0,2969
Trung bnh
0,3045
0,3009
0,2989
0,2968
0,1240
0,2328
0,2960
0,2007
%RSD
HCl
%RSD
Ln 1
0,0679
0,0749
0,0760
0,0775
Ln 2
0,0683
0,0749
0,0763
0,0776
Ln 3
0,0678
0,0748
0,0763
0,0776
Trung bnh
0,0680
0,0749
0,0762
0,0776
Sai s (%RSD)
0,9040
0,2605
0,2571
0,7329
Ln 1
0,0679
0,0709
0,0723
0,0738
Ln 2
0,0683
0,0710
0,0722
0,0739
Ln 3
0,0678
0,0710
0,0723
0,0739
Trung bnh
0,0680
0,0710
0,0723
0,0739
0,9040
0,9859
0,2370
0,2045
HNO3
HCl
Sai s (%RSD)
http://www.lrc-tnu.edu.vn
40
http://www.lrc-tnu.edu.vn
41
Cd2+ 1ppm
Pb2+ 2ppm
Abs
% RSD
Abs
% RSD
0,3147
0,2985
0,3147
0,2985
NH4Ac 1%
0,3201
0,2175
0,0725
0,1535
NH4Ac 2%
0,3143
0,4015
0,0716
0,8745
NH4Ac3%
0,3249
0,0936
0,0721
0,4659
NaAc 1%
0,3072
0,3798
0,0719
0,3424
NaAc 2%
0,3056
0,3005
0,0720
0,8570
NaAc 3%
0,3027
0,3423
0,0718
1,0187
Cd
Pb
(%)
Abs
%RSD
Abs
%RSD
0,3105
0,2715
0,0785
0,6985
0,5
0,3200
0,2341
0,0802
0,1723
1,0
0,3225
0,2507
0,0829
0,2753
1,5
0,3212
0,4618
0,0811
0,3703
http://www.lrc-tnu.edu.vn
42
C0
C1
C2
C3
C4
200
300
400
800
Na+ (ppm)
100
200
400
500
Abs-Cd
0,3056
0,3049
0,3048
0,3054
0,3058
Abs-Pb
0,0709
0,0714
0,0726
0,0706
0,0722
Ion
K+(ppm)
http://www.lrc-tnu.edu.vn
43
C0
C5
C6
C7
C8
Mg2+ (ppm)
50
100
150
200
Ca2+ (ppm)
50
100
150
200
Ba2+ (ppm)
10
20
30
40
Sr2+ (ppm)
10
20
30
40
Abs-Cd
0,3056
0,3036
0,3062
0,3059
0,3064
Abs-Pb
0,0709
0,0714
0,0707
0,0716
0,0700
Ion
C0
C9
C10
C11
C12
Cu2+ (ppm)
20
30
40
50
Ni2+ (ppm)
20
30
40
50
Zn2+ (ppm)
20
30
40
50
Mn2+(ppm)
20
30
40
50
Abs-Cd
0,3056
0,3040
0,3041
0,3043
0,3045
Abs-Pb
0,0709
0,0702
0,0718
0,0725
0,0723
Ion
C0
C13
C14
C15
C16
Al3+ (ppm)
20
60
80
100
Fe3+(ppm)
20
60
80
100
Cr3+(ppm)
10
Abs-Cd
0,3056
0,3051
0,3069
0,3063
0,3060
Abs-Pb
0,0709
0,0716
0,0718
0,0709
0,0705
Ion
http://www.lrc-tnu.edu.vn
44
C0
C17
C18
C19
C20
K+(ppm)
200
300
400
800
Na+ (ppm)
100
200
400
500
Mg2+(ppm)
50
100
150
200
Ca2+ (ppm)
50
100
150
200
Ba2+ (ppm)
10
20
30
40
Sr2+ (ppm)
10
20
30
40
Cu2+(ppm)
20
30
40
50
Ni2+ (ppm)
20
30
40
50
Zn2+ (ppm)
20
30
40
50
Mn2+(ppm)
20
30
40
50
Al3+ (ppm)
20
60
80
100
Fe3+(ppm)
20
60
80
100
Cr3+(ppm)
10
Abs-Cd
0,3056
0,3056
0,3049
0,3063
0,3060
Abs-Pb
0,0709
0,0700
0,0727
0,0728
0,0708
http://www.lrc-tnu.edu.vn
45
C0
C1
C2
C3
C4
SO24 (ppm)
50
100
150
200
H2PO4- (ppm)
50
100
150
200
F-(ppm)
50
100
150
200
I-(ppm)
50
100
150
200
Abs-Cd
0,3056
0,3049
0,3050
0,3057
0,3062
Abs-Pb
0,0709
0,0730
0,0742
0,0726
0,0720
Ion
C0
C1
C2
C3
C4
NO3-(%)
Cl- (%)
SO24 (ppm)
50
100
150
200
H2PO4- (ppm)
50
100
150
200
F- (ppm)
50
100
150
200
I- (ppm)
50
100
150
200
Abs-Cd
0,3056
0,3052
0,3055
0,3060
0,3059
Abs-Pb
0,0709
0,0730
0,0720
0,0719
0,0715
http://www.lrc-tnu.edu.vn
46
C0
C1
C2
C3
C4
K+(ppm)
200
300
400
800
Na+ (ppm)
100
200
400
500
Mg2+(ppm)
50
100
150
200
Ca2+ (ppm)
50
100
150
200
Ba2+ (ppm)
10
20
30
40
Sr2+ (ppm)
10
20
30
40
Cu2+(ppm)
20
30
40
50
Ni2+ (ppm)
20
30
40
50
Zn2+ (ppm)
20
30
40
50
Mn2+(ppm)
20
30
40
50
Al3+ (ppm)
20
60
80
100
Fe3+(ppm)
20
60
80
100
Cr3+(ppm)
10
NO3-(%)
Cl- (%)
SO24 (ppm)
50
100
150
200
H2PO4- (ppm)
50
100
150
200
F- (ppm)
50
100
150
200
I- (ppm)
50
100
150
200
Abs-Cd
0,3056
0,3056
0,3052
0,3058
0,3060
Abs-Pb
0,0709
0,0710
0,0721
0,0725
0,0712
Nhn xt: T bng s liu trn chng t rng cc ion trong vng kho st
khng nh hng n php xc nh Cd v Pb. Hn na trong cc mu thc t th
hm lng cc ion trn nh hn hm lng kho st rt nhiu nn c th khng nh
rng cc ion ny khng gy nh hng n php o. y cng chnh l mt u
im ni bt ca php o F-AAS so vi phng php khc.
http://www.lrc-tnu.edu.vn
47
Ln 1
Ln 2
Ln 3
Trung bnh
0,0260
0,0270
0,0260
0,0260
0.5
0,0330
0,0340
0,0330
0,0330
0,0660
0,0670
0,0670
0,0670
0,1290
0,1290
0,1290
0,1290
0,1910
0,1920
0,1910
0,1910
0,2470
0,2470
0,2470
0,2470
0,2980
0,2990
0,2990
0,2990
0,3420
0,3420
0,3420
0,3420
0,4000
0,4000
0,4000
0,4000
Nng (ppm)
0.25
http://www.lrc-tnu.edu.vn
48
Abs-Cd
6
7
8
Conc-Cd(ppm)
Trung
Ln 1
Ln 2
Ln 3
0,1
0,0324
0,0325
0,0325
0,0325
0,25
0,0486
0,0485
0,0484
0,0485
0,0610
0,0610
0,0609
0,0610
0,0794
0,0795
0,0793
0,0794
0,0960
0,0960
0,096
0,0960
0,1126
0,1127
0,1127
0,1127
0,1445
0,1444
0,1446
0,1445
0,1603
0,1605
0,1606
0,1605
0,1741
0,1742
0,1742
0,1742
0,1814
0,1816
0,1815
0,1815
10
0,2119
0,2120
0,2120
0,2120
Nng (ppm)
bnh
http://www.lrc-tnu.edu.vn
49
Abs - Pb
0.20
0.18
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
10
CPb
X Axis Title
http://www.lrc-tnu.edu.vn
Abs-Cd
50
0.30
Y=A+B.X
0.25
0.20
0.15
0.10
0.05
0.00
0
Conc-Cd(ppm)
Hnh 3.3: th ng chun ca cadimi
Phng trnh ng chun Data1_B:
Y=A+B*X
Thng s
gi tr
sai s
-----------------------------------------------------------A
0.00904
0.00274
0.05897
9,74.10-4
------------------------------------------------------------
SD
-----------------------------------------------------------0.99932
0.0043
< 0.0001
------------------------------------------------------------
http://www.lrc-tnu.edu.vn
51
LOD
3.S y
B
3.0,004
0,2( ppm)
0,059
LOQ
10.S y
B
10.0,004
0,678( ppm)
0,059
3.3.2.2. ng chun ca ch
T kt qu thu c bng 3.24 chng ti dng phn mm Origin 6.0 xc
nh ng chun ca ch v thu c kt qu nh sau:
http://www.lrc-tnu.edu.vn
52
0.18
Abs - Pb
Y Axis Title
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0
X Axis Title
8
CPb
Parameter
Value Error
---------------------------------------------------A
0.04672
0.00113
0.01617
2.23629E-4
-----------------------------------------------------
SD
-----------------------------------------------------0.99952
0.00144
<0.0001
-------------------------------------
http://www.lrc-tnu.edu.vn
53
3* S y
B
3.0,00144
= 0,267 (ppm)
0,0162
10 * S y
B
10 * 0,00144
= 0,889 (ppm)
0,0162
( At Ai )
*100%
At
Trong :
+ %X : Sai s phn trm tng i .
+ Ai : Gi tr cng hp th o c (Abs)
+ At : Gi tr cng hp th tm c theo ng chun (Abs)
lp li ca php o c xc nh theo cc i lng S2 v %RSD.
Cc i lng c tnh theo cng thc :
http://www.lrc-tnu.edu.vn
54
S =
( A A )
t
Suy ra : S =
n 1
S2
% RSD = S *100%
Atb
0, 25
0,0255
0,1287
0,2989
Ln o
Ai
%X
Ai
%X
Ai
%X
0,0245
3,92
0,1278
0,70
0,2958
1,04
0,0250
1,96
0,1262
1,94
0,2960
0,97
0,0253
0,78
0,1275
0,93
0,2945
1,47
0,0242
5,09
0,1270
1,32
0,2915
2,48
0,0247
3,14
0,1265
1,71
0,2912
2,58
0,0239
6,27
0,1263
1,86
0,2909
2,68
0,0249
2,35
0,1259
2,18
0,2923
2,21
0,0240
5,88
0,1272
1,17
0,2902
2,91
0,0252
1,18
0,1269
1,40
0,2905
2,81
10
0,0248
2,75
0,1268
1,48
0,2938
1,71
Atb
0,0247
3,33
0,1268
1,47
0,2927
2,09
0,001
0,002
0,007
%RSD
4,05
1,58
2,39
http://www.lrc-tnu.edu.vn
55
CPb (ppm)
At (Abs)
0,0610
0,1127
0,1742
Ln o
Ai
X%
Ai
X%
Ai
X%
0,0590
3,28
0,1120
0,62
0,1720
1,26
0,0585
4,09
0,1115
1,06
0,1715
1,55
0,0583
4,43
0,1106
1,86
0,1705
2,12
0,0595
2,46
0,1117
0,89
0,1710
1,84
0,0580
4,92
0,1102
2,22
0,1700
2,41
0,0576
5,57
0,1098
2,57
0,1707
2,01
0,0588
3,61
0,1100
2,39
0,1705
2,12
0,0579
5,08
0,1095
2,84
0,1709
1,89
0,0597
2,13
0,1109
1,60
0,1701
2,35
10
0,0599
1,80
0,1113
1,24
0,1695
2,70
Atb
0,0587
3,74
0,1108
1,73
0,1707
2,03
0,0025
0,0022
0,0038
% RSD
4,26
1,99
2,23
http://www.lrc-tnu.edu.vn
56
Pb
228,8
217
0,5
0,5
65 %
70 %
1,2
1,2
nn
Nguyn t
0,2
0,267
0,678
0,889
0,25-5
0,25- 8
Cc yu t
Khe o (nm)
Cng dng n (%Imax)
Lu lng kh C2H2 (ml/pht)
phn
Thnh
Thng s my o
Vch ph hp th (nm)
http://www.lrc-tnu.edu.vn
57
Loi rau
Bp ci (BC)
Ci xoong (CX)
Ci canh (CC)
Ngi cu (NC)
X lch (XL)
Mung nc (MN)
Ci tha (CT)
Mng ti (MT)
Dn (DD)
10 Gip c (GC)
a im ly mu
Thi gian ly mu
http://www.lrc-tnu.edu.vn
58
Phn trm kh
khi sy (g)
(%)
Bp ci (BC)
35,67/1000
3,567 %
M2
Ci xoong (CX)
41,54/1000
4,154 %
M3
Ci canh (CC)
53,37/1000
5,337 %
M4
Ngi cu (NC)
89,48/1000
8,948 %
M5
X lch (XL)
37,78/1000
3,778 %
M6
Mung nc (MN)
44,54/1000
4,454 %
M7
Ci tha (CT)
86,78/1000
8,678 %
M8
Mng ti (MT)
67,94/1000
6,794 %
M9
Dn (DD)
83,56/1000
8,356 %
10
M10
Gip c (GC)
110,47/1000
11,047 %
STT
Mu
Loi rau
M1
http://www.lrc-tnu.edu.vn
59
STT
Mu rau
10
11
12
13
14
15
Bp ci (BC)
Ci xoong (CX)
Ci canh (CC)
Ngi cu (NC)
X lch (XL)
Mung nc (MN)
Ci tha (CT)
Mng ti (MT)
Dn (DD)
10
Gip c (GC)
http://www.lrc-tnu.edu.vn
60
CX V
m
Trong :
X: hm lng cadimi, ch trong th tch mu em o (mg).
C X : Nng cht phn tch trong mu o ph tm c theo ng
chun (mg/l).
V: Th tch dung dch mu (10 ml).
m: Lng mu phn tch x l v nh mc thnh th tch (5 gam).
T kt qu trn ta xc nh c hm lng cadimi, ch trong 1000 gam mu
ti theo cng thc sau:
X = X.% kh
X : hm lng Cd, Pb trong 1000 gam mu ti).
3.7.2. Kt qu xc nh hm lng cadimi, ch trong cc mu rau
Chng ti tin hnh x l 10 mu rau nh cp phn 3.6.2. Chun b
dung dch o v tin hnh o mu cc iu kin ti u nh cp phn 3.5.
Cc kt qu thu c l trung bnh ca cc ln o v tr i mu trng.
Mu rau ma xun bao gm: Bp ci (BC); Ci xoong (CX); Ci canh (CC);
X lch (XL). Rau ma h bao gm : Ngi cu (NC); Mung nc (MN); Ci tha
(CT); Mng ti (MT); Dn (DD); Gip c (GC).
http://www.lrc-tnu.edu.vn
61
STT
Mu
Nng tnh
theo ng
Abs- Cd
chun
(ppm)
0,0302
0,3260
Hm lng
trong mu
rau ti
(mg/kg)
0,0233
Bp ci (BC)
Ci xoong (CX)
0,0294
0,3125
0,0260
Ci canh (CC)
0,0285
0,2969
0,0317
Ngi cu (NC)
0,0288
0,3025
0,0541
X lch (XL)
0,0255
0,2455
0,0185
0,2735
0,0244
Ci tha (CT)
0,0519
0,6990
0,1213
Mng ti (MT)
0,0518
0,6982
0,0949
Dn (DD)
0,0355
0,4173
0,0697
10 Gip c (GC)
0,0299
0,3218
0,0711
Gii hn cho
php 46/2007
Q BYT
(mg/kg )[19]
0,2
STT
Mu
Bp ci (BC)
Ci xoong (CX)
0,0516
0,4320
0,0359
Ci canh (CC)
0,0507
0,3580
0,0382
Ngi cu (NC)
0,0532
0,5323
0,0953
X lch (XL)
0,0550
0,6457
0,0488
0,7854
0,0699
Ci tha (CT)
0,0600
0,9530
0,1654
Mng ti (MT)
0,0534
0,5423
0,0737
Dn (DD)
0,0514
0,4210
0,0704
10 Gip c (GC)
0,0585
0,8578
0,1895
0,3
http://www.lrc-tnu.edu.vn
62
(Ci Ctb )2
S
S S2
n 1
2
% RSD
S
.100%
Ctb
t.S
n
http://www.lrc-tnu.edu.vn
63
C1
C2
C3
Ctb
%RSD
Bp ci (BC)
Ci xoong (CX)
Ci canh (CC)
Ngi cu (NC)
X lch (XL)
Mng ti (MT)
Dn (DD)
Gip c (GC)
Mu
theo ng chun
(ppm)
Hm lng trong
mu rau ti (mg/kg)
Bp ci (BC)
0,3260 0,0022
0,0233 0,0022
Ci xoong (CX)
0,3125 0,0007
0,0260 0,0007
Ci canh (CC)
0,2969 0,0010
0,0317 0,0010
Ngi cu (NC)
0,3025 0,0010
0,0541 0,0010
X lch (XL)
0,2455 0,0005
0,0185 0,0005
Mung nc (MN)
0,2735 0,0002
0,0244 0,0002
Ci tha(CT)
0,6990 0,0010
0,1213 0,0010
Mng ti (MT)
0,6982 0,0010
0,0949 0,0010
Dn (DD)
0,4173 0,0005
0,0697 0,0005
10
Gip c (GC)
0,3218 0,0007
0,0711 0,0007
http://www.lrc-tnu.edu.vn
64
gkg
800
600
400
200
54.4
23.3 26.0 31.7
18.5 24.4
M1
M2
M3
M4
M5
M6
121.3 94.9
69.7 71.1
M7
M8
M9
M10
Mu
C1
C2
C3
Ctb
%RSD
Bp ci (BC)
0,0312
0,0002
Ci xoong (CX)
0,0694
0,0007
Ci canh (CC)
0,1117
0,0010
Ngi cu (NC)
0,1315
0,0017
X lch (XL)
0,0310
0,0005
0,0382
0,0007
Ci tha (CT)
0,9530 0,0003
0,0315
0,0007
Mng ti (MT)
0,0369
0,0005
Dn (DD)
0,1425
0,0015
Gip c (GC)
0,0233
0,0005
http://www.lrc-tnu.edu.vn
65
Ta c kt qu chnh xc ca cc mu nh sau:
Bng 3.36: Hm lng chnh xc Pb trong rau
Mu
STT
Hm lng trong
mu rau ti (mg/kg)
Bp ci (BC)
0,3210 0,0002
0,0229 0,0002
Ci xoong (CX)
0,4320 0,0007
0,0359 0,0007
Ci canh (CC)
0,3580 0,0010
0,0382 0,0010
Ngi cu (NC)
0,5323 0,0017
0,0953 0,0017
X lch (XL)
0,6457 0,0005
0,0488 0,0005
Mung nc (MN)
0,7854 0,0007
0,0699 0,0007
Ci tha (CT)
0,9530 0,0007
0,1654 0,0007
Mng ti (MT)
0,5423 0,0005
0,0737 0,0005
Dn (DD)
0,4210 0,0015
0,0704 0,0015
10
Gip c (GC)
0,8578 0,0005
0,1895 0,0005
g / kg
1200
1000
800
600
400
200
189.5
16.54
22.9
M1
35.9
38.2
M2
M3
95.3
M4
73.7 7.04
48.8 69.9
M5
M6
M7
M8
M9
M10
Mu
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Mu rau
NC
Thnh phn
Mu rau ngi cu khng thm cht phn tch Cd,Pb
NC + t1
NC + t2
Mu NC + 2ppm Cd + 4 ppm Pb
NC + t3
Mu NC + 5 ppm Cd + 8 ppm Pb
BC
BC + t1
BC + t2
Mu BC + 2 ppm Cd + 4 ppm Pb
BC + t3
Mu BC + 5 ppm Cd + 8 ppm Pb
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Kim loi Cd
Nng mu Nng chun Nng thm Hiu sut
thu c
(ppm)
NC
1
thm vo
(ppm)
vo thu c
(ppm)
thu c Sai s
(%)
0,3025
NC + t1
0,5732
0,25
0,2305
92,20
7,80
NC + t2
0,8309
2,00
1,8856
94,28
5,72
NC + t3
1,2512
5,00
4,6570
93,14
6,86
BC
0,3260
BC + t1
0,4267
0,25
0,2315
92,60
7,40
BC + t2
0,9235
2,00
1,8875
94,38
5,63
BC + t3
1,3685
5,00
4,6752
93,50
6,49
Nng
Nng
mu thu c
chun thm
vo thu c
(ppm)
vo (ppm)
(ppm)
(%)
thu c Sai s
NC
0,5323
NC + t1
0,7145
0,25
0,2367
94,68
5,32
NC + t2
0,9231
4,00
3,8560
96,40
3,60
NC + t3
2,3570
8,00
7,7015
96,27
3,73
BC
0,3210
BC + t1
0,8120
0,25
0,2341
93,64
6,36
BC + t2
1,005
4,00
3,8425
96,06
3,94
BC + t3
2,5324
8,00
7,6792
95,99
4,01
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Nhn xt: Qua kt qu thu c cho thy hiu sut thu hi Cd, Pb u ln
hn 90% v sai s u nh hn 10%. C th sai s i vi nhng mu thm u
ng chun v cui ng chun l ln hn sai s i vi mu thm gia ng
chun, nh vy kt qu ny hon ton ph hp vi l thuyt phn b sai s Gauss.
Vy c th s dng mt trong hai phng php ng chun hoc thm
chun xc nh hm lng Cd, Pb trong rau xanh.
Trn y l kt qu p dng phng php ph hp th nguyn t ngn la F
AAS xc nh hm lng cc kim loi nng vo thc t. V thi gian nghin
cu c hn nn mun c kt qu phn tch chnh xc hn th cn phi ly mu hng
ngy vo cc thi im khc nhau trong ngy, trong nhiu thng vo cc ma khc
nhau em phn tch, ly kt qu nh gi, so snh vi kt qu phn tch bng cc
phng php khc na th kt qu thu c mi m bo chnh xc v c tnh
thuyt phc hn.
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KT LUN
Trn c s nghin cu phng php xc nh cadimi v ch trong rau bng
phng php ph hp th nguyn t F-AAS chng ti thu c cc kt qu nh sau:
1. a ra cc iu kin ph hp o ph F-AAS ca cadimi v ch.
2. Xc nh c khong tuyn tnh v lp ng chun ca cadimi v ch.
3. Xc nh c gii hn pht hin v gii hn nh lng ca php o.
4. nh gi c sai s v lp li ca php o.
5. Chn c cc iu kin ph hp ly mu x l mu rau.
6. Kim tra c kt qu x l mu bng mu lp, mu thm chun v cho kt
qu tt (sai s u nh hn 10 %).
7. Phn tch c hm lng Cd v Pb trong cc mu rau xanh x H Thng,
M Yn, Yn Lng, Ph Cng vo ma xun v ma h thuc huyn i T tnh Thi
Nguyn.
Tuy cc mu nghin cu v phn tch hm lng kim loi nng u di
mc cho php theo TCVN, nhng chng ta cng nn ch n cc mu c hm
lng kim loi vt hn cc mu bnh thng.
- Hm lng Cd theo TCVN: Mc cho php trong rau l 0,2 ppm th ng biu
din trong cc hnh huyn i T tnh Thi Nguyn u di mc cho php, mu c
hm lng Cd cao hn cc mu khc nh M7 (121,30 g/kg) .
- Hm lng Pb theo TCVN: Mc cho php trong rau l 1 ppm th ng biu
din trong cc hnh huyn i T tnh Thi Nguyn u di mc cho php, mu
c hm lng Pb cao hn cc mu khc nh M10 (189,50 g/kg) .
Chnh lng kim loi nng hin din trong cc rau xanh canh tc theo h
thng dy chuyn: t -> cy rau hp th -> con ngi dinh dng, hp th v tch
lu trong c th qua chui thc n -> nh hng n sc kho cng ng
Nh vy, phng php ph hp th nguyn t c th xc nh c hm
lng cc kim loi nng trong rau. Qua thc nghim, cho thy mt s loi rau ti
mt s khu vc ca huyn i T tnh Thi Nguyn theo cc kt qu phn tch cho
thy hm lng cadimi v ch nm trong gii hn cho php ca B Y t.
S ha bi Trung tm Hc liu i hc Thi Nguyn
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70
Do thi gian lm lun vn khng di nn chng ti cha tin hnh phn tch
c nhiu loi rau v mi tng quan ca chng vi iu kin sng. Chng ti
mong rng s sm c mt ti nghin cu ton din v vn ny v kt lun
chnh xc v tnh hnh rau hin nay.
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