phân tích nitrate, nitrite
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SVTH :
Nguyn Vn ThiPhng Hng MnhNguyn Phng TngSn Th Thanh TuynTrn Th Bch ThnhNguyn Th Thu Tm
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Tng quan v Nit v cc hp cht ca Nit
Trong t nhin tn ti ch yu di dng N2 kh ph bin v chim trn 78% th tch khng
kh
trong phn t N2, nit lin kt bng 3 lin ktha tr
Nit l kh c tnh tr v mt ha hc Phn ln cc sinh vt khng hp thu nit trc
tip c
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Nitrate trong nc v thc phm
Nitrat v nitrit c t nhin trong thcphm v nc
Trong CNTP nitrit c s dng nhiunhm bo v cc loi thc phm
Nitrat v nitrit thng tn ti trong ncdo ngun nc ngm b nhim
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Nitrate trong nc v thc phm
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Tnh c hi
Nitrite c hi hn so vi cc hp chtcha Nit
Nitrite +hemoglobin methaemoglobin
(lm gim qu trnh vn chuyn oxi trong mu)
Khi nitrite vo d dy nitrite c chuynthnh axit nitr
axit nitr+ amin hoc amit nitroamin(nitroamin, y l hp cht dn n ung th.)
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c tnh ca Nitrit
iu kin xy raphn ng : -Nhit nu qu cao
-Khi phi kh v khi hung khi cc loi lng thc
-Khi p tht vi loi mui Nitrate
-Khi tiu ho cc loi lng thc c cha Nitrite
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c tnh ca Nitrit
C ch gy c: NO3
-NO2
- di tc dng ca men tiuha trong c th
Nitrite +hemoglobin methaemoglobin
4HbFe2++ 4 NO2-+ 2 H2O ----> 2 HbFe
3++ OH-+ 4 NO3-+ O2
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c tnh ca Nitrit
NO2-+ amin nitrosamine
(mt hp cht tin gy ung th)
amin bc hai +axit nitrhp cht nitroso
nitrosamine
amin bc hai thng xut hin trong qu trnhnu rn thc phm giu protein hay qu trnh lnmen
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QUY NH V HM LNG NITRATTRONG THC PHM
Theo Q chung ca th gii, c gil rau qu sch, ti phi c lng nitratethp va phi
Q T chc Y t th gii (WHO) : nitrate trong nc ung l 50 mg/l Nitrate trong l rau 300 mg/kg rau ti
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QUY NH V HM LNG NITRATTRONG THC PHM
Loicy Hm lngNO3 Loicy Hm lngNO3
Dahu 60 Hnh ty 80
Dab 90 C chua 150
Mpngt 200 Dachut 150
Mngty 200 Khoai ty 250
uqu 200 C rt 250
Ng rau 300 Hnh l 400
Cibp 500 Bub 400
Su ho 500 C tm 400
Su l 500 X lch 1500
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Phng php nghin: dch nghin c munh hng n php xc nh nitrat.
Phng php ngm chit: thi gian lu,ko di qu trnh phn tch.
Phng php chit dng nng lng visng: thi gian chit tng i nhanh,dch chit khng mu, hiu sut chitcao.
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Phng php phn tch th tch
Nguyn tc: Phn tch chun l o th tch cadung dch cht chun ( bit chnh xc nng ) vcht chun phn ng hon ton vi dung dch t
mu thc phm cn tch.
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Phng php phn tch th tch
Tin hnh : da trn phn ng kh NO3-v cc trng thi oxi ho thp hn bngcc cht kh thch hp
Chun ngc : Cc phn ng xy ra nh sau:
NO3-+ 3Fe2++ 4H+ NO + 3Fe3++ 2H2O2
Fe2++ Cr2O72++ 14H+ 6Fe3++ 2Cr3++ 7H2O
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Phng php o mu
Nguyn tc : Chuyn cht cn xc nh thnh mt hp
chtc mu. oshpthnh sng cadung dchmu
ny hocso snh cngmu cadung dchphn tch
vicngmu cadung dchbittrcnng.
My o mu
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Phng php o mu
Tin hnh :
Cc phng php so mu cng c dng xc nh NO3-da trn ba loi phn ng sau:
Nitrat ho cc hp cht phenolic. Oxi ho cc hp cht hu c c nhm mang
mu c trng.
kh NO3-
thnh NO2-
hoc NH3ri xc nhchng theo phng php thch hp. Trong phng php nitrat ho ch yu c
s dng xc nh NO3- vi thuc th thng
dung l axit phenol isunfonic
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Phng php o mu
Tin hnh :
Khi s dng thuc th axit phenol 2,4 isunfonic,ion NO3
- phn ng vi axit ny to thnh axit
nitro phenol isunfonic. Trong mi trng kim,axit nitro phenol isunfonic to thnh mt muic mu vng cho hp th quang cc i bc sng 410nm.
My o mu v dd chun
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Phng php o mu
Tin hnh :
xc nh nng ca cht nghin cu, phi omt quang D ca dung dch th v dung dchchun bit nng .
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Phng php o mu
Tin hnh :
Tnh ton kt qu: Cx= (Dx/Dch).Cch
Vi Dx/Dch: mt quang dung dch th / dungdch chun
Cx/Cch: nng dung dch th / dung dch
chun Lp ng chun, dng th vi trc tung Y l
mt quang D o c, trc honh X l nng C
T th s tnh c hm lng NO3-
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Phng php o mu
Phng php ny n gin v cho nhy kh cao(0,05ppm).
khi c mt cc cht hu c,clorua, NO2-, cc ion c mu
s gy nh hng n kt qu phn tch
S dng axit sunfamin, ur, hay thiur tchNO2-, Cl-c loi b bng cch cho phn ng vi Ag2SO4.
Loi tr nh hng ca cc hp cht hu c bng cchoxi hobng H2O2hay s dng than hot tnh.
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Phng php o kh
Phn ng xy ra : 2KNO2+ CO(NH2)2+ 2HCl 2N2+ CO2+ 3H2O + 2KCl
KNO2+ HSO3 N2+ KHSO4+ H2O
Sau , un nng dung dch v to mi trngaxit mnh th nitrate s phn ng to thnh kh
N2O 2KNO3 + CO(NH2)2+ 2HCl 2N2O + CO2+ 3H2O + 2KCl
2KNO3+ HSO3NH2 + HCl N2O + H2SO4+ H2O + KCl
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Phng php o kh
Kh N2v N2O c gi li trong trc mk bng dung dch KOH trn 50%.
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Mt s phng php xc nhnitrit
Phng php th tch : Phng php ny c th xc nh c nitrite da
trn c s oxi ho nitrite thnh nitrate khi dngthuc th KMnO
4 Phng trnh chun : 2MnO4
-+ 5NO2-+ 6H+ 2Mn2++ 5NO3
-+ 3H2O
Trong mi trng axit ion NO2-b phn hu thnh NO
v NO2theo phng trnh: NO2
-+ H++ HNO2 NO + NO2+ H2O
Phng php ny c nhy khng cao v tnh chnlc km v trong dung dch c nhiu ion c kh nng b
MnO4-oxi ho
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Phng php cc ph
Nitrite l anion c hot tnh cc ph.
xc nh nitrite bng cc ph dng nn LaCl3
2%v BaCl22% th nitrit cho sng cc ph 1,2V so vi anot thu ngn.
Nu dng nn l hn hp m xitrate 2M c pH= 2,5 th gii hn pht hin l 0,225 ppm NO2-
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Phng php cc ph
Khi xc nh NO2-trong mu ngi ta thm 5mldung dch nn
Dd nn gm :4,86g KSCN v 17,2ml HClO470% trong mt lt nc ctv 1,25mliphenylamin v 20ml mu
iu chnh pH t 1- 2 bng axit HClO4 nu cn
Th nh pic xut hin - 0,52V.
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Phng php sc k
Ion nitrite phn tch bng phng php sc k lngcao p vi pha ng l axit p - hyrobenroic 8mM vBis - Tris 3,2mM.
Hm lng nitrite c th xc nh c n 10e-8M
Ion nitrite cng c th xc nh c cng vi cc
ion khc bng phng php sc k ion.
Tuy nhin gii hn phng php ny ch xc nhc 0,1 mg NO2-/ lit.
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Phng php quang trc
s dng thuc th Griss u tin nitrite phn ng vi axit sunfanilic to
thnh mui iazo
Sau mui ny phn ng vi - naphtylaminto thnh hp cht azo c mu hng
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Phng php quang trc
Phng php c chn lc cao
khi c mt lng rt ln ca Cloramin, Clo ,
Thiosunfat , Natripolyphotphat v St (III) th sais ca phng php ny l 10%.
Ngoi ra ngi ta cn s dng dn xut ca Griss
v cng t c kt qu ng k
Vd: 4-amino benzene sunfona(NH2C6H4SO2NH2) vN-(1-Naphtyl)1,2- diamino etanhidroclorua(C10H7NH-CH2- CH2-NH2.HCl).
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Phng php quang trc
Quy trnh tm tt : a) Chun b thuc th : - Ho tan 0,6 g acid sunfanilic trong 100ml dung
dch nc - acid axetic - Ho tan 0,6 g a - Naphthilamin trong 100ml
dung dch nc - acid axetic
b)/ Chun b mu : Mu rau qu c la sch bng nc ct , ct
nh v nghin bng my nghin. Sau thm
nc v lc 30 pht . Lc bng dng c kh
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Phng php quang trc
c)Tin hnh xc nh:
Cho mu vo ng o, thm nc nvch.
-Thm 4 git thuc th A, lc u, yn1 pht.
-Thm 4 giot thuc th B, lc u. - yn 20 pht, so mu dung dch vi
bng mu chun.
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Phng php quang trc
Kt qu khi hm lng Nitrite nm trongkhong t 0,1 n 10 ppm th sai stng i l 5%
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xut
Trong nng nghip : V tr cc ngun nc ung (ging, h, ao,
sui...) phi trn vng cao, cch xa cc
chung nui sc vt Bo qun tht k cc bao phn ha hc v
cch xa ngun nc. Hng dn cho ngi dn s dng ng cch
v ng liu lng thuc thc vt Sau ht ph bin n ngi dn nim thm
canh phi phi hp vi lun canh
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xut
Trong qu trnh bo qun v ch bin :
Khng lm dng vic s dng ph gia. S dng ng ph gia cho php (theo quy nh
ca B Y t) Xem k nhn trc khi s dng
Cm quan trc khi cn, ong, o, m. S dng ng liu lng, ng k thut. Ma no loi rau ny, dng cc loi rau trng
ngoi vn.
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xut
Tr nh di 5 thng khng nn n rau bina,c ci
Nn b cc cng v cc l gi ca cc loi rau
c nhiu Nitrate.
- Nhng rau s qua nc si c th gimlng Nitrate t 30 n 50%.
- Khng nn hm nng cc mn rau (canh) cnhiu Nitrate, v khi hm li Nitrate c th b
bin i thnh Nitrite.
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Kt lun
Nitrat, nitrit rt d b nhim vo rau qu, ncngm, v mt s loi thc phm khc.
Hm lng cao nitrat, nitrit i vo c th trongthi gian di s gy ra nhiu nguy him cho sckhe ca con ngi.
V vy, kim tra ch tiu nitrat v nitrit trongthc phm l rt cn thit