Professional Documents
Culture Documents
M U..........................................................................................................................23
1.Tnh cp thit ca ti..............................................................................................23
2. ngha khoa hc v thc tin ca ti ...................................................................23
CHNG 1: TNG QUAN TI LIU........................................................................24
1.1.Molipden v d lng ca n trong mi trng ...................................................24
1.1.1.Gii thiu v Molipden..........................................................................................24
1.1.2.Ngun gc xut hin ca Molipden trong sp l ................................................24
Vai tr quan 1.1.3.Vai tr ca Molipden..............................................................24
1.1.4.Tc hi ca Molipden............................................................................................24
1.2.Cc phng php v c ha mu ...........................................................................25
1.2.1.Phng php v c ha mu kh.........................................................................25
1.2.2.Phng php v c ha mu t .........................................................................25
1.2.3.Phng php v c mu kh t kt hp .........................................................25
1.3.Cc phng php xc nh vi lng Molipden......................................................26
1.3.1.Phng php quang ph pht x nguyn.............................................................26
1.3.2.Phng php quang ph hp th nguyn t (AAS)............................................26
1.3.3.Phng php trc quang phn t UV-VIS..........................................................26
1.4.Phng php quang ph hp th UV-VIS..............................................................27
1.4.1.Gii thiu phng php quang ph hp th phn t UV-VIS...........................27
C s l thuyt ca phng php trc quang phn t UV VIS....................27
-22.1.1.Dng c...................................................................................................................36
2.1.2.Thit b....................................................................................................................36
2.1.3.Ha cht .................................................................................................................36
2.2.Cch pha cc loi dung dch ....................................................................................36
2.2.1.Pha dung dch chun gc amonimolipdat (NH4)6Mo7O24.4H2O....................36
2.2.2.Pha cc dung dch khc ........................................................................................37
2.3.Ni dung nghin cu ........................................................................................38
-Chn cc phng php chnh xc , hin i c kh nng thc hin trong iu
kin phng th nghim nc ta............................................................................38
-Nghin cu cc iu kin ti u xc nh nguyn t Molipden...................38
-Nghin cu p dng thc tin trn mt s mu thc t ..................................38
-Xy dng mt quy trnh tng i hon chnh ,c kh nng thc hin trong iu
kin phng th nghim ...........................................................................................38
2.4.Thc nghim nghin cu iu kin v c ha mu ...........................................38
2.4.1.Dung mi v c ha mu ..............................................................................38
Ta tin hnh v c ha mu bng phng php kh t kt hp .Sau khi tro
ha xong ,trn c s nghin cu cc ti liu v c im ca mu sp l chng ti
chn dung mi HCl v nc ha tan hon ton tro............................................38
2.4.2.Kho st nhit v thi gian nung ti u.....................................................38
Sau khi chn c dung mi thch hp, chng ti tin hnh kho st thi gian
nung thu tro trng . em nung cc nhit khc nhau , chn nhit nung ti
u...........................................................................................................................38
C nh nhit v thay i thi gian chn thi gian nung ti u.............38
2.5.Thc nghim nghin cu iu kin ti u phn tch hm lng Molipden trong
sp l bng phng php trc quang phn t UV-VIS............................................38
2.5.1.Kho st chn vch o...................................................................................38
Cch tin hnh : Cho 5ml dung dch Mo6+ c nng 0.1mg/ml vo bnh
nh mc 50 ml . Sau thm ln lt 25ml NaCl 20% , 7 ml HCl (d=1,16) ,5ml
H2SO4(d=1,84), 1ml dung dich thioure 1% v 1ml dung dich amonithioxyanat
50% ,lc u to phc Molipdenthioxianat c mu da cam. em qut bc sng
trong khong t 400-800 nm..................................................................................39
-61.5.......................................................................................................................... 47
2............................................................................................................................. 47
2.5.......................................................................................................................... 47
3............................................................................................................................. 47
Hin tng ............................................................................................................. 47
-..............................................................................................................................47
+............................................................................................................................ 47
+............................................................................................................................ 47
+............................................................................................................................ 47
+............................................................................................................................ 47
D............................................................................................................................47
0.8962....................................................................................................................47
0.9375.................................................................................................................... 47
0.9436....................................................................................................................47
0.9324....................................................................................................................47
0.9285.................................................................................................................... 47
Bng 2.Kt qu kho st thi gian nung .................................................................47
(-) : Mu cha chuyn mu , ( +) : Mu ha tro trng ......................................47
Kt lun : Nung mu nhit 470 oC trong 2 gi ............................................47
3.2.Kt qu kho st iu kin xc nh Molipden...................................................47
3.2.1.Kt qu kho st chn vch o ....................................................................47
Bng 3: Kt qu kho st vch o ca Mo...............................................................47
Vch o (nm)..........................................................................................................47
Abs- ln1................................................................................................................47
Abs- ln2................................................................................................................47
Abs- ln 3............................................................................................................... 47
Trung bnh..............................................................................................................47
-7450.........................................................................................................................47
0.7891....................................................................................................................47
0.7956....................................................................................................................47
0.7965....................................................................................................................47
0.7937....................................................................................................................47
460......................................................................................................................... 47
0.8895.................................................................................................................... 47
0.8924....................................................................................................................47
0.8978....................................................................................................................47
0.8932....................................................................................................................47
470.........................................................................................................................47
0.7896....................................................................................................................47
0.7935.................................................................................................................... 47
0.7962....................................................................................................................47
0.7931....................................................................................................................47
Da vo bng s liu ta chn vch ph l 460 nm..................................................47
3.2.2.Kt qu kho st bn mu ca phc theo thi gian ..................................47
Ly 2 ml dung dch Amonimolipdat 0.1 mg/ml sau thm vo bnh ln lt
25ml NaCl 20% , 7 ml HCl (d=1,16) ,5ml H2SO4(d=1,4), 1ml dung dich thioure 1%
v 1ml dung dich amonithioxyanat 50% lc u to phc Molipdenthioxianat c
mu da cam .Tin hnh o mt quang D ti cc thi im khc nhau.Thi gian
c kho st ti bng sau.....................................................................................47
Bng 4:Kt qu kho st bn mu ca phc .....................................................49
Thi gian o (pht).................................................................................................49
o ngay ................................................................................................................. 49
Sau 5' .................................................................................................................... 49
Sau 10'................................................................................................................... 49
Sau 15'................................................................................................................... 49
Sau 20'................................................................................................................... 49
-8Sau 25'...................................................................................................................49
Sau 30'................................................................................................................... 49
D............................................................................................................................49
0.4438....................................................................................................................49
0.4554.................................................................................................................... 49
0.4913....................................................................................................................49
0.4955.................................................................................................................... 49
0.4978....................................................................................................................49
0.4954.................................................................................................................... 49
0.4948....................................................................................................................49
Thi gian o (pht).................................................................................................49
Sau 35' ..................................................................................................................49
Sau 40' ..................................................................................................................49
Sau 45' ..................................................................................................................49
Sau 50'...................................................................................................................49
Sau 55' ..................................................................................................................49
Sau 60'................................................................................................................... 49
D............................................................................................................................49
0.4944....................................................................................................................49
0.4936....................................................................................................................49
0.4929....................................................................................................................49
0.4921....................................................................................................................49
0.4919....................................................................................................................49
0.4915....................................................................................................................49
...............................................................................................................................49
Vy nn o mt quang sau khi phc to mu khong 20 pht dung dch mu
n nh ..................................................................................................................49
3.2.3.Kt qu kho st nh hng ca Cu2+ i vi vic xc nh Molipden .........49
-10.......................................................................................................................... 53
............................................................................................................................... 53
Da trn biu th ta nhn thy ng hu nh khng nh hng n Molipden 53
3.2.4.Kt qu kho st nh hng ca Fe3+ i vi vic xc nh Molipden ..........53
-Qu trnh tin hnh : chun b 6 bnh nh mc 50 ml....................................53
+Thm vo 2ml Mo6+ 0.1mg/ml ..............................................................53
+Cho vo mi bnh thm 25 ml NaCl 20% , 7 ml HCl ( d=1.18) , 5 ml H2SO4
( d=1.4) ,1 ml dung dch thioure 1% ......................................................................53
+ Cho 0 ml , 0.5 ml, 1 ml , 2ml ,5 ml ,10 ml Fe3+ 0.01 mg/ml...................53
+Thm vo 1 ml amonithiocianat 1% .Kt qu thu c bng sau....53
........................................................................................................................... 53
Bng 6: Kt qu kho st nh hng ca st
................................................54
-110,0010.................................................................................................................... 55
0,5879.................................................................................................................... 55
0,004...................................................................................................................... 56
0,0020....................................................................................................................56
0,6159....................................................................................................................56
............................................................................................................................... 57
Nh vy st nh hng ng k n vic xc nh Moliden...................................57
3.2.5.Loi tr nh hng ca Fe3+.........................................................................57
-Loi tr nh hng ca Fe3+ bng NaF.........................................................57
-Kt qu loi tr c th hin bng kt qu v s sau:............................57
Bng 7:Kt qu loi tr nh hng ca st.............................................................57
Nng Mo6+........................................................................................................58
(mg/ml).................................................................................................................. 58
Nng Fe3+ (mg/ml)...........................................................................................58
Th tch NaF 4%..................................................................................................... 58
(ml)........................................................................................................................ 58
Mt quang D...................................................................................................... 58
0.004...................................................................................................................... 58
0.000...................................................................................................................... 58
0............................................................................................................................. 58
0.4972.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
0............................................................................................................................. 58
0.5549.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
-121............................................................................................................................. 58
0.5503.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
2............................................................................................................................. 58
0.5467.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
3............................................................................................................................. 58
0.5356.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
4............................................................................................................................. 58
0.5224.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
5............................................................................................................................. 58
0.5025.................................................................................................................... 58
0.004...................................................................................................................... 58
0.001...................................................................................................................... 58
6............................................................................................................................. 58
0.5145.................................................................................................................... 58
0.004...................................................................................................................... 59
0.001...................................................................................................................... 59
7............................................................................................................................. 59
0.5257.................................................................................................................... 59
............................................................................................................................... 59
-140,020 .....................................................................................................................61
0.03........................................................................................................................61
D............................................................................................................................62
1.2536....................................................................................................................62
1.4231....................................................................................................................62
1.7341....................................................................................................................62
2.8124....................................................................................................................62
2.7751....................................................................................................................62
2.687...................................................................................................................... 62
...............................................................................................................................63
Vy khong nng thch hp tin hnh php o l t 0,001 mg/ml n 0,016
mg/ml..................................................................................................................... 63
3.5.Kt qu xy dng ng chun .......................................................................63
-Dy chun gm 6 bnh nh mc 50 ml .........................................................63
-Thm vo mi bnh ln lt 0.5ml, 1ml ,2ml, 3ml, 4ml ,5 ml Mo6+ 0.1 mg/ml
...............................................................................................................................63
- Cho vo mi bnh thm 25 ml NaCl 20% , 7 ml HCl ( d=1.18) , 5 ml H2SO4
( d=1.4) ,1 ml dung dch thioure 1% ......................................................................63
- Thm vo 1 ml amonithiocianat 1% ........................................................63
- nh mc bng nc ct n 50 ml v o D ti bc sng 460 nm .Kt qu thu
c bng sau.....................................................................................................63
Bng 9: Kt qu xy dng ng chun.................................................................63
Nng Mo6+(mg/ml)...........................................................................................64
D............................................................................................................................64
0.001...................................................................................................................... 64
0.2134....................................................................................................................64
0.002...................................................................................................................... 64
0.3115....................................................................................................................64
0.004...................................................................................................................... 64
-150.4921....................................................................................................................64
0.006...................................................................................................................... 64
0.7252.................................................................................................................... 64
0.008...................................................................................................................... 64
0.8854.................................................................................................................... 64
0.01........................................................................................................................65
1.105...................................................................................................................... 65
...............................................................................................................................66
th biu din s ph thuc gia mt quang ca phc Molipdenthioxyanat vo
hm lng Mo6+....................................................................................................66
3.6.Kt qu kho st hiu sut thu hi ca phng php........................................66
xc nh hiu sut thu hi ca phng php, chng ti tin hnh phn tch
hm lng Molipden trn 5 mu gi.Sau tin hnh nh cc iu kin ti u
chn cc mc trn.Kt qu th hin trn bng ....................................................66
Bng 10:Kt qu tnh hiu sut thu hi ca phng php.......................................66
Ln o.................................................................................................................... 67
Nng Mo6+ thc t (mg/ml)..............................................................................67
Nng Mo6+ o c (mg/ml).............................................................................67
Hiu sut thu hi (%)..............................................................................................67
1............................................................................................................................. 67
0.004...................................................................................................................... 67
0.00353..................................................................................................................67
88.25...................................................................................................................... 67
2............................................................................................................................. 67
0.004...................................................................................................................... 67
0.00347..................................................................................................................67
86.75...................................................................................................................... 67
3............................................................................................................................. 67
0.004...................................................................................................................... 67
-160.00355..................................................................................................................67
88.75...................................................................................................................... 67
4............................................................................................................................. 67
0.004...................................................................................................................... 67
0.00351..................................................................................................................67
87.75...................................................................................................................... 67
5............................................................................................................................. 67
0.004...................................................................................................................... 67
0.00350..................................................................................................................67
87.5........................................................................................................................67
H trung bnh...........................................................................................................68
87.8........................................................................................................................68
Hiu sut thu hi trung bnh l 87.8%, t yu cu ca phng php phn tch vi
lng......................................................................................................................69
3.7.Kt qu nh gi sai s thng k ca phng php .........................................69
Chun b hai mu gi: hai mu c nng khc nhau, tin hnh quy trnh phn tch
mu gi nh khi xc nh hiu sut thu hi , lm 5 ln th nghim. Kt qu thu c
th hin trn bng 1 v kt qu tnh mt s i lng c trng sai s thng k ca
phng php c th hin trn bng 2.................................................................69
Bng 11:Gi tr nng Mo6+ o c ca mu gi sau 5 ln o.........................69
Ln o.................................................................................................................... 70
1............................................................................................................................. 70
2............................................................................................................................. 70
3............................................................................................................................. 70
4............................................................................................................................. 70
5............................................................................................................................. 70
Nng Mo6+ (mg/ml)..........................................................................................70
0.004 .....................................................................................................................70
0.00342..................................................................................................................70
-170.00345..................................................................................................................70
0.00351..................................................................................................................70
0.00344..................................................................................................................70
0.00353..................................................................................................................70
0.006...................................................................................................................... 71
0.00532..................................................................................................................71
0.00546..................................................................................................................71
0.00535..................................................................................................................71
0.00534..................................................................................................................71
0.00541..................................................................................................................71
Bng 12: Mt s kt qu nh gi sai s thng k ca phng php......................72
Cc i lng c trng..........................................................................................73
Nng Mo6+ 0.004 (mg/ml).................................................................................73
Nng Mo6+ 0.006 (mg/ml).................................................................................73
Nng trung bnh ................................................................................................73
3.47x10-3............................................................................................................... 73
5.38x10-3............................................................................................................... 73
Phng sai S2.........................................................................................................73
2.25x10-9............................................................................................................... 73
3.35x10-9............................................................................................................... 73
lch chun ca php o S.................................................................................73
4.74x10-5............................................................................................................... 73
5.79x10-5............................................................................................................... 73
lch chun ca i lng trung bnh cng ........................................................73
2.12x10-5............................................................................................................... 73
2.59x10-5............................................................................................................... 73
H s bin ng Cv%..............................................................................................73
-181.36........................................................................................................................73
1.07........................................................................................................................73
Bin gii tin cy ................................................................................................... 73
5.88x10-5...............................................................................................73
7.18x10-5............................................................................................................... 73
Sai s tng i %................................................................................................74
1.69.......................................................................................................................74
1.33........................................................................................................................74
(vi = 0.95, k = 4, t,k = 2.776).........................................................................75
Kt qu cho thy, sai s tng i % nh chng t phng php c chnh xc
cao, h s bin ng nh chng t lp li tt.....................................................75
3.8.Quy trnh phn tch xc nh hm lng Molipden trong sp l ........................75
Trn c s kt qu kho st cc iu kin ca phng php phn tch hm lng
............................................................................................................................... 75
Molipden trong sp l t mc 3.1 n mc 3.7 chng ti tin hnh xc nh quy
trnh....................................................................................................................... 75
phn tch Molipden trong sp l .............................................................................75
Sp l sau khi mua v ra sch nhiu ln bng nc ct, sau xay nh bng
my xay sinh t .Cn chnh xc khi lng sp l trong khong t 20-50 g .Sau
thm vo mu 0.5 ml HClO4 c , 2ml HNO3 c ,1 ml H2SO4 c , 2ml H2O2 30
% , 2 ml KNO3 10 % lm cht bo v.Sau ta em nung trn bp in n tro en
, sau em nung trong l nung nhit 470oC trong 2 n tro trng .Sau ha
tan bng HCl 20% v nh mc ..............................................................................75
Thm vo bnh ln lt 25ml NaCl 20% , 7 ml HCl (d=1,16) ,5ml H2SO4(d=1,4),
1ml dung dich thioure 1% v 1ml dung dich amonithioxyanat 50% ,lc u to
phc Molipdenthioxianat c mu da cam. yn sau thi gian 20 pht phc n
nh mu ri em i o mt quang ca dung dch bc sng 460 nm ............75
Mu trng c chun b tng t nh trn nhng khng c mt ca Mo6+ ,
thc hin qu trnh v c ha mu trong mu nc................................................75
Hm lng Mo6+ c tnh theo cng thc sau: (mg/kg).................................75
Trong m: khi lng mu rau mung ly phn tch...............................75
x: hm lng Mo6+ tnh theo ng chun (mg)............................75
-204............................................................................................................................. 78
20/3/2012............................................................................................................... 78
Ch Ha Khnh.......................................................................................................78
Sp l trng ...........................................................................................................78
6.32........................................................................................................................78
5............................................................................................................................. 78
22/3/2012............................................................................................................... 78
Ch Ha Khnh.......................................................................................................78
Sp l xanh............................................................................................................ 78
5.67........................................................................................................................78
6............................................................................................................................. 78
25/3/2012...............................................................................................................78
Ch Ha Khnh.......................................................................................................78
Sp l trng ...........................................................................................................78
6.44........................................................................................................................78
7............................................................................................................................. 78
27/3/2012............................................................................................................... 78
Ch Ha Khnh.......................................................................................................78
Sp l trng ...........................................................................................................78
6.12........................................................................................................................78
8............................................................................................................................. 78
30/3/2012............................................................................................................... 78
Ch Ha Khnh.......................................................................................................78
Sp l trng ...........................................................................................................78
7.78........................................................................................................................78
9............................................................................................................................. 78
3/4/2012.................................................................................................................78
-21Ch Ha Khnh.......................................................................................................78
Sp l xanh............................................................................................................ 78
3.89........................................................................................................................78
10...........................................................................................................................78
5/4/2012.................................................................................................................78
Ch Ha Khnh.......................................................................................................78
Sp l trng ..........................................................................................................78
6.45........................................................................................................................78
BYT /867.................................................................................................................79
15.00...................................................................................................................... 79
Qua bng kt qu phn tch cho thy hu ht cc mu sp l u c cha hm
lng Molipden nhng cha vt qu gii hn cho php ca BYT. Trong hai loi sp
l th sp l trng c hm lng Molipden cao hn so vi sp l xanh.Tuy nhin , sp
l trng mua ch Sn c hm lng Molipden cao nht (7.78 mg/kg) . iu
ny cng ph hp vi cc cng trnh nghin cu trc y v hm lng Molipden
trong sp l nhiu a im ...............................................................................80
KT LUN...............................................................................................................81
Kho st c dung mi v c ha mu ,nhit v thi gian nung mu ,kho st
chn vch o , bn mu ca phc theo thi gian v kho st cc yu t nh
hng ....................................................................................................................81
2 . Xc nh c khong tuyn tnh v lp ng chun ca Mo ........................81
3. Xc nh c hiu sut thu hi l 87.8 %.........................................................81
4. nh gi c sai s v lp li ca php o..................................................81
5. xut thnh cng quy trnh phn tch Mo trong sp l ...................................81
6. Quy trnh xut phn tch cc mu sp l trn a bn cc ch thuc
thnh ph Nng ................................................................................................81
KIN NGH.............................................................................................................. 81
1 .Phn tch hm lng cc kim loi khc c bit l cc kim loi c hi ..............81
2.Phn tch Mo trong cc loi rau khc nhau t c c s , k hoch bn
phn v ci to t tng nng sut cy trng ...................................................81
TI LIU THAM KHO..............................................................................................82
-22[1]. Phm Th H (2008), Cc phng php phn tch quang hc, TP. Nng.......82
[2]. Tng Th Vit H (2009), Nghin cu xc nh hm lng asen trong nc b
mt bng phng php quang ph hp th phn t UV-VIS, TP. Nng...............82
[3]. L Th Mi (2007), Ha hc phn tch nh lng, TP. Nng.........................82
[4]. T Vng Nghi, Hunh Vn Trung, Trn T Hiu (1986), Phn tch nc, NXB
Khoa hc v k thut H Ni....................................................................................82
[5]. http://dantri.com.vn/c7/s7-148482/anh-huong-cua-asen-doi-voi-suc- khoe.htm 82
[6]. http://danang-upload.dng.vn/images/fr7tmesqkfxep23dj19l.jpg.......................82
-23M U
1.Tnh cp thit ca ti
Hin nay dn s gia tng nhanh trn th gii cng nh Vit Nam, ngi ta cn c
nhiu lng thc, thc phm, c th l cung cp trong cc ba n hng ngy. Rau cng l
ngun thc n b dng nui sng con ngi. Rau khng nhng cung cp mt lng ln
sinh t A, B, C, m cn cung cp mt phn cc nguyn t vi,lng rt cn thit trong cu
to t bo.
Rau cn l mt ngun dc liu qu gp phn bo v sc kho cho con ngi.
Nhng nu trong rau cha mt lng ln kim loi nng th s gy hi cho con ngi.
D lng cn li ca cc kim loi nng trong rau ,trong Molipden l nguyn
nhn gy ra nhiu cn bnh cho ngi v ng vt . gp phn nh gi hm lng
Molipden trong rau , chng ti thc hin ti :Nghin cu phn tch hm lng
Molipden trong sp l bng phng php trc quang phn t UV-VIS.
2. ngha khoa hc v thc tin ca ti
ti gp phn xy dng quy trnh phn tch hm lng Molipden trong sp l
ph hp vi iu kin ca phng th nghim Vit Nam. Trn c s p dng vo phn
tch mt s mu thc t, nh gi mc nhim kim loi Molipden trong sp l trn mt
s khu vc ch thuc thnh ph Nng .
A: hp th quang
K: hng s thc nghim
C: nng nguyn t phn tch
D = lg
I
= .C.l
I
0
-28-
Trong : 1. n Vnfram; 2. Knh lc sng; 3. Cuvet cha dung dch so snh; 4. Cuvet
cha dung dch phn tch; 5. T bo quang in vi hiu ng quang in ngoi. 6. Gng;
7.T bo quang in; 8. in k chun ha 100% T.
1.4.2.Cc iu kin ti u cho phng php phn tch
1.4.2.1.nh sng n sc
Do tnh cht c trng ca cc cht mu ch hp th nhng bc x n sc c bc
sng thch hp nn nh lut Lambert- Beer ch ng khi dng nh sng n sc nghin
cu.
1.4.2.2.Ph hp th
Ph hp th l ng cong biu din s ph thuc gia mt quang v bc sng
. ng vi gi tr bc sng max l mt quang cc i Dmax. Vi mi dung dch nghin
cu ta phi xc nh bc sng max trc khi tin hnh phn tch nh lng.
.100
Hoc % =
.100
X
-31
Trong : X =
X 1 + X 2 + X 3 + ... + X 4
n
= X-
1.5.2. Cc i lng nh gi sai s trong phn tch
Khi tin hnh nhiu php phn tch, tc l tin hnh lp li th nghim, ta thu c
mt dy cc d kin thc nghim. Cc khi nim sau y c trng cho phn tn cc d
kin .
1.5.2.1. Phng sai
Phng sai l trung bnh cng ca cc bnh phng nhng hiu gia cc gi tr ring
bit v gi tr trung bnh, tc l:
S2 =
( X i X ) 2
n 1
trong n l s ln th nghim
y l i lng rt quan trng c trng cho phn tn dng tnh sai s ngu
nhin.
1.5.2.2. lch chun v lch tiu chun tng i
lch chun c xc nh bng cn bc hai ca phng sai.
S=
( X i X ) 2
.
n 1
lch chun ca i lng trung bnh cng Sx c tnh theo cng thc
Sx =
S2
=
n
(X
X )2
n(n 1)
Cv =
S
100% .
X
-32
= x
t.S
n
trong =
hoc
t.S
n
= x
-33-
-34Hin nay, nn kinh t th gii ang pht trin vi tc cao nhm p ng nhu cu cu
nhu cu ngy cng tng ca con ngi v t mc tiu to mc cn bng mi vi s n
nh th trn trn ton cu. Cng vi s gia tng dn s, nhu cu cung cp rau xanh cho loi
ngi cng ngy cng gia tng mnh m. Tuy nhin, cng vi s pht trin kinh t ko theo
hng lot cc vn c lin quan n mi trng xung quanh gy cn tr cc qu trnh pht
trin cng nh sc khe con ngi. Do s pht trin mnh m ca th v cng nghip cng
nh s gia tng lng phn ho hc, thuc tr su trong sn xut nng nghip gy nhim
mi trng v nh hng n sc kho con ngi.Trong nhng nm gn y, cc t chc
quc t nh t chc Nng lng (FAO), t chc Y t th gii (WHO) v cc t chc khc v
vn mi trng a ra cc khuyn co, hn ch vic s dng ho cht nhn to vo nng
nghip, xy dng cc quy trnh sn xut theo cng ngh sch, cng ngh sinh hc, cng ngh
s dng ngun nng lng ti to . T chc Y t th gii c tnh rng mi nm c 3 %
nhn lc lao ng nng nghip cc nc ang pht trin b nhim c kim loi nng trong
rau qu .
c cht c th tn ti nhiu hnh thc khc nhau nh cht v c hay hu c, th hp
cht hay n cht, dng lng, rn hay kh. Chng c mt trong c ba mi trng t, nc v
khng kh lan truyn v nh hng n h sinh thi ni chng tn ti. Do , tm hiu v xc
nh cc cht c trong mi trng s gip ta c bin php khng ch v x l n.
Theo tham kho kin ca mt s cc chuyn gia cho thy lm c cng vic ny
phi tn rt nhiu thi gian, kinh ph v sc lc v t c nhiu loi khc nhau v kh nng t
lm sch ca t cng nh kh nng m ca t l rt ln nn phi a ra rt nhiu cc thng
s c lin quan trong mi trng t nh thc vt, ng vt, kh nng lan truyn v hnh vi
ca cc c cht trong mi trng t, kh nng t x l v hp thu ca sinh vt trong mi
trng t
1.6.2.Tnh hnh nghin cu v kim sot hm lng kim loi nng Vit Nam
Mt lng ln kim loi nh km, ng, cadmium tch t trong rau c th gy ung th
t bin,ng c h thn kinh,ri lon chc nng thn.
Mt s cht c li c nhiu trong nhng loi rau ph bin nh rau dip, cn ty, ci bp,
-35khoai ty... Trc thc trng ny, lin tip trong nhng ngy gn y, U ban Khoa hc
Cng ngh v Mi trng ca Quc hi v B NN & PTNT t chc hp bn v vn
ny.
Th trng B NN & PTNT Bi B Bng cho rng ch vi thc t 3% rau xanh c
hm lng thuc bo v thc vt vt tiu chun cho php, tng ng vi hn 2 triu
ngi hng ngy phi n rau khng m bo. Thc t, vic hng ngy n phi rau khng
m bo tiu chun l mm mng gy nn nhiu cn bnh nguy him nh ung th, ng c
thn kinh, ri lon chc nng thn
1.7.S lc vi nt v sp l
Sp l, hay su l, bp su l, hoa l (ting Php: Chou-fleur),ci hoa, ci bng trng,
l mt loi ci n c, thuc loiBrassica oleracea, h Ci, mc quanh nm, gieo ging
bng ht. Phn s dng lm thc phm ca sp l l ton b phn hoa cha n, phn ny
rt mm, xp nn khng chu c ma nng. Phn l v thn thng ch c s dng
lm thc n cho gia sc
Vit Nam, cc vng trng sp l ph bin l min c kh hu lnh nh min Bc
vo ma ng hay cc vng ni cao nh Ty Nguyn, nht l vng Lt Lm ng.
-36-
Nc ct 2 ln
-39Cch tin hnh : Cho 5ml dung dch Mo6+ c nng 0.1mg/ml vo bnh nh mc
50 ml . Sau thm ln lt 25ml NaCl 20% , 7 ml HCl (d=1,16) ,5ml
H2SO4(d=1,84), 1ml dung dich thioure 1% v 1ml dung dich amonithioxyanat 50% ,lc
u to phc Molipdenthioxianat c mu da cam. em qut bc sng trong
khong t 400-800 nm.
2.5.2.Kho st s bn mu ca phc gia Mo5+ vi thuc th theo thi gian
Ly 2 ml dung dch Amonimolipdat 0.1 mg/ml sau thm vo bnh ln lt 25ml
NaCl 20% , 7 ml HCl (d=1,16) ,5ml H2SO4(d=1,4), 1ml dung dich thioure 1% v 1ml
dung dich amonithioxyanat 50% lc u to phc Molipdenthioxianat c mu da
cam . o D ti max trong cc khong thi gian : o ngay , 5 pht , 10 pht ,15 pht ,
20 pht , 25 pht , 30 pht , 35 pht ,40 pht , 45 pht , 50 pht , 55 pht , 60 pht .
2.5.3.Kho st nh hng ca Cu2+
Qu trnh tin hnh : chun b 6 bnh nh mc 50 ml
+Thm vo 2 ml Mo6+ 0.1 mg/ml
+Cho vo mi bnh thm 25 ml NaCl 20% , 7 ml HCl ( d=1.18) , 5 ml H2SO4
( d=1.4) ,1 ml dung dch thioure 1%
+ Cho 0 ml , 0.5ml , 1.5ml ,3ml , 5ml ,10 ml Cu2+ 0.01 mg/ml
+Thm vo 1 ml amonithiocianat 1% .Sau em o D ti bc sng max.
2.5.3.Kho st nh hng ca Fe3+
-Qu trnh tin hnh : chun b 6 bnh nh mc 50 ml
+Thm vo 2ml Mo6+ 0.1mg/ml
+Cho vo mi bnh thm 25 ml NaCl 20% , 7 ml HCl ( d=1.18) , 5 ml H2SO4
( d=1.4) ,1 ml dung dch thioure 1%
-41 xc nh hiu sut thu hi ca phng php ta tin hnh phn tch trn 5 mu gi
vi nng ban u ca Mo6+ bit chnh xc. Tin hnh v c ha mu v to phc
Molipdenthioxianat. o mt quang ca phc Molipdenthioxianat bc sng max
t nh gi hiu sut thu hi ca phng php.
2.8.nh gi sai s thng k ca phng php
nh gi sai s thng k, chng ti tin hnh v c ha mu theo quy trnh phn
tch vi cc iu kin ti u chn mc 2.4 v 2.5 trn 5 mu gi, mi mu 5 ln
vi nng ban u ca Mo6+ bit chnh xc.
2.9.Quy trnh kho st
Trn c s nghin cu cc iu kin ti u ca phng php xc nh hm lng Molipden
xt trn, chng ti tin hnh xy dng quy trnh phn tch xc nh hm lng
Molipden trong sp l, t p dng xc nh cc mu sp l thc t trn a bn cc
ch thuc thnh ph Nng.
2.10.p dng phn tch mt s mu sp l thc t trn a bn cc ch thuc thnh
ph Nng .
2.10.1. Chun b mu sp l
Sp l c mua ti ch trn a bn thnh ph Nng trong khong t thng 3
n thng 4 nm 2012.Sp l c ra sch v ra li bng nc ct hai ln, ct nh
khong 1cm, v c bo qun lm mu phn tch. Cc mu c ct nh v c
xay nhuyn trong ci xay sinh t v trn u
2.10.2.Cc a im ly mu
Chng ti tp trung ly cc mu sp l a im ch Ha Khnh thuc thnh ph
Nng.
-42-
-44Nhit
450
460
470
480
490
500
nung
(0C)
Hin
tng
-45D
0.9157
0.9168
0.9475
0.9365
0.9245
0.9164
-47Thi gian
1.5
2.5
Hin tng
0.8962
0.9375
0.9436
0.9324
0.9285
( gi )
Abs- ln1
Abs- ln2
Abs- ln 3
Trung bnh
450
0.7891
0.7956
0.7965
0.7937
460
0.8895
0.8924
0.8978
0.8932
470
0.7896
0.7935
0.7962
0.7931
-48-
Sau 5'
Sau 10'
Sau 15'
Sau 20'
Sau 25'
Sau 30'
0.4438
0.4554
0.4913
0.4955
0.4978
0.4954
0.4948
Sau 40'
Sau 45'
Sau 50'
Sau 55'
Sau 60'
0.4936
0.4929
0.4921
0.4919
0.4915
0.4944
-50+ Cho 0 ml , 0.5ml , 1.5ml ,3ml , 5ml ,10 ml Cu2+ 0.01 mg/ml
+Thm vo 1 ml amonithiocianat 1% .Kt qu thu c bng sau:
Bng 5: Kt qu kho st nh hng ca ng
-51Nng
Mo
6+
(m
g/
Nng
Cu2+
(mg/ml
)
Mt
quan
gD
ml)
0,004
0,0000
0,4946
0,004
0,0001
0,4976
0,004
0,0003
0,5012
0,004
0,0006
0,5065
0,004
0,0010
0,5070
-520,004
0,0020
0,5107
-53-
0 ,5
Gi tr D o c
0 ,4
0 ,3
M u i ch ng
M u o c
0 ,2
0 ,1
0
1 2 3 4 5 6 7 8
T h t m u
-54-
-55Nng Mo6+
(mg/ml)
Nng Fe3+
(mg/ml)
Mt quang D
0,004
0,0000
0,4957
0,004
0,0001
0,5079
0,004
0,0002
0,5407
0,004
0,0004
0,5728
0,004
0,0010
0,5879
-560,004
0,0020
0,6159
Gi tr D o c
-57-
0
0
0
0
0
0
0
,7
,6
,5
,4
,3
,2
,1
0
M u i c h ng
M u o c
T h t m u
-58Nng Mo6+
(mg/ml)
Nng Fe3+
(mg/ml)
Th tch NaF 4%
Mt quang D
(ml)
0.004
0.000
0.4972
0.004
0.001
0.5549
0.004
0.001
0.5503
0.004
0.001
0.5467
0.004
0.001
0.5356
0.004
0.001
0.5224
0.004
0.001
0.5025
0.004
0.001
0.5145
-590.004
0.001
0.5257
0 ,6
0 ,5
G tr D o c
0 ,4
0 ,3
M u i ch ng
M u o c
0 ,2
0 ,1
0
1 2 3 4 5 6 7 8 9
T h t m u
-61CMo6+(mg/ml)
0,001
0,002
0,004
0,006
0,008
0,010
0.2132
0.312
0.4917
0.7248
0.908
1.102
CMo6+(mg/ml)
0.012
0,014
0,016
0,018
0,020
0.03
-62D
1.2536
1.4231
1.7341
2.8124
2.7751
2.687
-63-
Vy khong nng thch hp tin hnh php o l t 0,001 mg/ml n 0,016 mg/ml
3.5.Kt qu xy dng ng chun
-Dy chun
gm 6 bnh nh mc 50 ml
-Thm vo mi bnh ln lt 0.5ml, 1ml ,2ml, 3ml, 4ml ,5 ml Mo6+ 0.1 mg/ml
- Cho vo mi bnh thm 25 ml NaCl 20% , 7 ml HCl ( d=1.18) , 5 ml H2SO4 ( d=1.4) ,1
ml dung dch thioure 1%
- Thm vo 1 ml amonithiocianat 1% .
- nh mc bng nc ct n 50 ml v o D ti bc sng 460 nm .Kt qu thu c
bng sau
-64Nng
Mo6+
(mg/ml)
0.001
0.2134
0.002
0.3115
0.004
0.4921
0.006
0.7252
0.008
0.8854
-650.01
1.105
-66-
-67Nng Mo6+
Ln o
Nng Mo6+
thc t
o c
(mg/ml)
(mg/ml)
0.004
0.00353
88.25
0.004
0.00347
86.75
0.004
0.00355
88.75
0.004
0.00351
87.75
0.004
0.00350
87.5
87.8
-69-
Hiu sut thu hi trung bnh l 87.8%, t yu cu ca phng php phn tch vi lng.
3.7.Kt qu nh gi sai s thng k ca phng php
Chun b hai mu gi: hai mu c nng khc nhau, tin hnh quy trnh phn tch mu gi
nh khi xc nh hiu sut thu hi , lm 5 ln th nghim. Kt qu thu c th hin
trn bng 1 v kt qu tnh mt s i lng c trng sai s thng k ca phng
php c th hin trn bng 2.
Bng 11:Gi tr nng Mo6+ o c ca mu gi sau 5 ln o
-70Ln o
Nng
0.004
0.00342
0.00345
0.00351
0.00344 0.00353
-71Mo6+
(mg/
ml)
0.006
0.00532
0.00546
0.00535
0.00534 0.00541
(mg/ml)
(mg/ml)
3.47x10-3
5.38x10-3
Phng sai S2
2.25x10-9
3.35x10-9
4.74x10-5
5.79x10-5
2.12x10-5
2.59x10-5
1.36
1.07
sX
H s bin ng Cv%
Bin gii tin cy
5.88x10-5
7.18x10-5
-74Sai s tng i %
1.69
1.33
x
(mg/kg)
m
-76Ly chnh xc 30 g sp l
xay nhuyn
+ 0.5 ml HClO4 c , 2ml H2SO4 c
+ 4ml HNO3 c , 5ml H2O2 30%
+4ml KNO3 10%
Than en
-77T quy trnh phn tch xy dng, tin hnh phn tch hm lng Molipden trong sp l
cc ch thuc thnh ph Nng. Kt qu phn tch c thng k trong bng .
Bng 13: gi tr hm lng Molipden trong mt s mu sp l
-78Mu
s Ngy mua
p
mu
Hm lng Mo6+
a im ly mu
Loi mu sp l
(mg/kg)
l
1
9/3/2012
Ch Ha Khnh
Sp l xanh
4.22
12/3/2012
Ch Ha Khnh
Sp l xanh
5.45
16/3/2012
Ch Ha Khnh
Sp l xanh
4.45
20/3/2012
Ch Ha Khnh
Sp l trng
6.32
22/3/2012
Ch Ha Khnh
Sp l xanh
5.67
25/3/2012
Ch Ha Khnh
Sp l trng
6.44
27/3/2012
Ch Ha Khnh
Sp l trng
6.12
30/3/2012
Ch Ha Khnh
Sp l trng
7.78
3/4/2012
Ch Ha Khnh
Sp l xanh
3.89
10
5/4/2012
Ch Ha Khnh
Sp l trng
6.45
-79BYT /867
15.00
-81KT LUN
Kho st c dung mi v c ha mu ,nhit v thi gian nung mu ,kho st chn
vch o , bn mu ca phc theo thi gian v kho st cc yu t nh hng .
2 . Xc nh c khong tuyn tnh v lp ng chun ca Mo
3. Xc nh c hiu sut thu hi l 87.8 %.
4. nh gi c sai s v lp li ca php o.
5. xut thnh cng quy trnh phn tch Mo trong sp l .
6. Quy trnh xut phn tch cc mu sp l trn a bn cc ch
thuc thnh ph Nng .
KIN NGH
1 .Phn tch hm lng cc kim loi khc c bit l cc kim loi c hi
2.Phn tch Mo trong cc loi rau khc nhau t c c s , k hoch bn phn v
ci to t tng nng sut cy trng .
-83-