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