39 PP lay mau.pdf

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    Trn Mai Lin PP ly mu v x l mu 2

    Gii thiu mn hc

    S tn ch: 2 (30 tit)

    Trnh : sinh vin nm th 3, ngnh ha phn tch

    Mc tiu: gip sinh vin hiu, nm vng cc phng php

    ly, x l mu trc khi phn tch trong nhiu i tng khcnhau

    M t hc phn: bao gm cc kin thc v cch ly mu,bo qun v x l mu phn tch

    Gio trnh:

    Phm Lun GT hng dn v nhng vn cscacc kthut xl mu phn tch HN 1999

    JOHN WILEY - Sample Preparation Techniques inAnalytical Chemistry Departmentof Chemistry and

    Environmental Science New Jersey Institute of Technology

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 3

    Gii thiu mn hc

    Chng 1. Mu phn tch, ly mu v qun l mu

    Chng 2. Nhng vn c s ca cc k thut x l

    mu

    Chng 3. X l mu xc nh cc kim loi v phi

    kim

    Chng 4. X l mu xc nh cc cht hu c

    Chng 5. X l mu phn tch mu mi trng

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    Trn Mai Lin PP ly mu v x l mu 4

    Chng 1. Mu phn tch, ly mu v qun l mu

    Ti sao phi ly v x l mu phn tch

    Ly mu phn tch

    X l s b khi ly mu

    Cc cch ly mu phn tch

    Ghi chp v lp h s ly mu

    Chuyn ch mu v kho hay phng th nghim Qun l, bo qun v iu kin bo qun mu

    Khi nim QA/QC trong ly mu phn tch

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    Trn Mai Lin PP ly mu v x l mu 5

    Ti sao phi ly v x l mu phn tch?

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    Trn Mai Lin PP ly mu v x l mu 6

    Ti sao phi ly v x l mu phn tch?

    Mc sai s trong cc bc ca mt qui trnh phn tch

    Ly mu

    Chun bmu pt

    C c, chng ct,tch

    Xc nh

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    Trn Mai Lin PP ly mu v x l mu 7

    Ti sao phi ly v x l mu phn tch?

    Vic ly mu v x l mu ty thuc vo

    i tng cn nghin cu pt

    Bn cht, s tn ti v hm lng ca cht cnxc nh

    Loi mu

    Phng php phn tch

    Cc k thut x l mu

    KT v c ha kh

    KT v c ha t KT s dng l vi sng

    KT chit lng lng, rn lng, rn kh

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    Trn Mai Lin PP ly mu v x l mu 8

    Ti sao phi ly v x l mu phn tch?

    KT thng hoa

    KT chng ct

    KT kt tinh

    KT in phn tch cht

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    Trn Mai Lin PP ly mu v x l mu 9

    Ly mu phn tch

    Mc ch

    Yu cu

    i din ng cho i tng cn nghin cu

    p ng ng yu cu cn pt

    Khng lm mt hay nhim bn thm cht pt

    Ph hp vi phng php chn pt C khi lng phn tch

    Mu c l lch, ghi cc iu kin r rng

    m bo thc hin ng QA/QC

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    Trn Mai Lin PP ly mu v x l mu 10

    Ly mu phn tch

    Trang b v dng c ly mu

    Yu cu sch

    Khng lm sai khc cc thnh phn trongmu

    Ph hp vi tng loi mu

    Cc loi dng c: phn loi theo tnh

    cht ca mu Mu rn v mu bt: giy, nilon, chai thy

    tinh, PE

    Mu lng: can, chai nha, chai l thy

    tinh Mu c cht phn tch d b phn hy:

    giy, chai c mu chng nh sng

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    Trn Mai Lin PP ly mu v x l mu 11

    Ly mu phn tch

    Tnh cht ca mt s dng c cha v ph mu

    Nung chy vi hydroxit kim loi kim v Na2O2.c

    s dng khi x l mu bng dd kim c. Khngdng vi HCl

    Ni

    Nhit c th ti 11000C, r hn thch anh, tngtc vi HF, H3PO4, dd kim

    S

    Trong sut, chu nhit tt (11000C), dn, gi thnhcao hn thy tinh, tng tc vi HF, H3PO4, dd kim

    Thch anh

    Trong sut, chu nhit tt, dn d v, tng tc viHF, H3PO4, dd kim. ng dng rng

    Thy tinh

    c tnh v ng dngCht liu

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    Trn Mai Lin PP ly mu v x l mu 12

    Ly mu phn tch

    Gi thnh r hn Pt, chu rt tt HCl, c th chuc HNO3, H2SO4 50%; H3PO4 60% 100

    0C; c

    th nung chy vi NaOH; khng nung vi NaNO3,HSO4

    -. Thng c ch to dng hp kim: 98%Zr, 1.5% Sn, vt Fe, Cr v Ni. Khng s dng vi KFhoc HF

    Zr

    Hu nh khng b nh hng bi cc axit (HNO3,HCl, HF, H2SO4). Gi thnh rt cao; c kh nng

    to hp kim vi cc kim loi: Hg, Pb, Sn, Au, Cu, Si,Zn, Cd, As, Al, Bi v Fe. (khi nng d hp th H2l tc nhn kh). Khng s dng nu nung mu viNa2CO3

    Pt

    c tnhCht liu

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    Trn Mai Lin PP ly mu v x l mu 13

    Ly mu phn tch

    Chs dng vi dd axit < 0,1M; dn d vPS

    Tr hu ht vi cc hp cht v c v hu c (tr F2). Ct l trng hn PE. S dng an ton di 2500C, b phnhy 3000C. Kh to hnh dng (gi thnh cao). Dn nhit

    km (i hi t di tng nhit mu)

    Teflon

    Thng s dng cha mu v thuc th. Tng tcvi HNO3 16M v axit axetic ng bng. Bt u mm vbin dng 600C. Tn ti nhng l trng c kh nng mt1% v th tch khi cha Br

    2, H

    2O, H

    2S, HNO

    3.

    PE

    Chu c axit v kim nng chy, tng tc vi bisunfatnng chy, dn d v. Thnh bnh phi dy.

    Al2O3

    c tnhCht liu

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    Trn Mai Lin PP ly mu v x l mu 14

    Ly mu phn tch

    Mu khng kh, bi - TCVN 5704 - 1993 V tr ly mu

    Phi t u ly mu cha b phn lc cao1,5m so vi sn nh khi ly mu ti ngun phtsinh.

    Phi t u ly mu cha b phn lc cao

    1,5m n 2m so vi sn nh nhng v tr khcnhau trong phn xng nh gi mc nhim chung

    Phi t u ly mu cha b phn lc ti vng

    th khi nh gi mc tip xc

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    Trn Mai Lin PP ly mu v x l mu 15

    Ly mu phn tch

    Thi gian ly mu

    Phi ly mu lin tc trong mt ca lm vic (480 pht) tnh gi tr trung bnh ca ca lm vic. Ni c nhiu

    bi c php ly mu gin on lm nhiu ln, miln t nht 30 pht, tng thi gian ly mu khngc t hn 240 pht sau tnh gi tr trung bnh

    Cho php ly mu ti ngun pht sinh v cch nh

    gi nhim mi trng chung cho tng ln, mi ln30 pht, t nht phi ly 3 mu tch gi tr trungbnh.

    Phi ly mu bi trong khong thi gian t 5 n 10pht khi xc nh hm lng bi cao nht trong mtca lm vic, phi ly t nht 5 mu sau tnh gi trtrung bnh

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    Trn Mai Lin PP ly mu v x l mu 16

    Ly mu phn tch

    Mu phn tch nc Vic ly mu ph thuc vo iu kin ly mu, i tng ly

    mu, v tr ly

    V d:

    Mu t h thng phn phi nc t thnh ph: vi nccn c x trong mt thi gian (3 5 pht), r st trongng c loi b

    Mu nc ngm: trng hp nc ging, nc mi bmln cn x t nht 10 pht. Lu lng bm ly mu cn stvi lu lng bm thc t

    Ngun nc sng, knh, rch: ly mu theo su, v trso vi b, khong cch vi ngun nc thi, iu kin thi

    tit vo thi im ly mu, lu lng dng chy, thy triu, Ngun nc ao, h: ch : cht lng nc thay i theo

    ma, lng ma, tc gi, su, thi gian trong ngy

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    Trn Mai Lin PP ly mu v x l mu 17

    X l s b khi ly mu

    Ti sao phi x l s b?

    Cc loi mu cn x l s b

    Cc phng php x l s b

    Phn tch kim loi v anion

    Phn tch cc cht hu c

    Cc i tng sinh hc

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    Trn Mai Lin PP ly mu v x l mu 18

    Cc cch ly mu phn tch

    Cc kiu ly mu

    Ly mu n

    Ly mu lp, mu song song

    Ly mu hn hp

    Ly mu c thm cht chun

    Cch ly mu Ly mu theo thi gian Chng trnh thi gian lin tc

    Theo nh k Theo xc sut

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    Trn Mai Lin PP ly mu v x l mu 19

    Cc cch ly mu phn tch

    Ly mu theo tng, lp Trung bnh cc im

    Cc im theo v tr trn b mt

    Theo su

    Ly theo vng, mt ct hay im cn quan st

    Ly theo hng gi

    Mt s v d Cch ly mu t

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    Trn Mai Lin PP ly mu v x l mu 20

    V d: ly mu t

    Ly mu

    Ty theo mc ch nghin cu v kho st lachn cc phng php ly mu khc nhau Mu c bit c ly mt v tr xc nh (theo

    tng phu din)

    Mu hn hp: c trn t nhiu mu ban u tothnh mu chung i din cho mt phm vi tc kho st

    Ty theo hnh dng v a hnh mnh t cn lyt nht 5 im phn b u trn ton din tch

    theo qui tc ng cho, ng vung gc hayng zigzac

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    Trn Mai Lin PP ly mu v x l mu 21

    V d: ly mu t

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    Trn Mai Lin PP ly mu v x l mu 22

    V d: ly mu t

    Cc mu ban u c gom li thnh mu hnhp chung c khi lng t nht 2kg

    T mu hn hp chung, chn thnh mu hn hptrung bnh bng cch bm nh t, trn u vloi bt theo nguyn tc ng cho gc. Muhn hp trung bnh c khi lng 1kg

    1

    4

    3

    2

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    Trn Mai Lin PP ly mu v x l mu 23

    V d: ly mu phn tch phn bn

    Mu ban u

    Cc mu c ly ngu nhin, i din cho cc vtr trn, di, gia Trnh ly cc mu c bit,

    c th (bao b rch, sn phm b m) S ln ly ti thiu l 5, khi lng mi ln ti

    thiu l 200g

    Mu chung: gp tt c cc mu ban u nhgi

    Mu trung bnh: c ly t mu chung

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    Trn Mai Lin PP ly mu v x l mu 24

    V d: ly mu phn tch cy trng

    Mu ban u:

    Ly t cc b phn ca cy hoc theo khm

    c ly cng mt thi im

    Cc mu nh gi mc dinh dng ca cythng c ly 1 b phn ti mt giai onsinh trng

    Mu chung

    Mu trung bnh: mu cn c ra, sy kh, nhanhchng x l v phn tch.

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    Trn Mai Lin PP ly mu v x l mu 25

    Ghi chp v lp h s ly mu

    a im

    V tr

    Thi gian

    iu kin thi tit

    Loi mu

    Cch ly

    Khi lng

    Ghi r cch x l s b (nu c)

    Ngi ly

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    Trn Mai Lin PP ly mu v x l mu 26

    Chuyn ch mu v PTN

    Yu cu phng tin chuyn ch m bo nhanh

    Khng gy h hng, xo trn

    m bo tt iu kin gi mu

    Sch, khng gy nhim bn mu

    Thc hin ng QA/QC trong vn chuyn mu

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    Trn Mai Lin PP ly mu v x l mu 27

    Bo qun mu phn tch

    Yu cu ring tng loi, l, nhm Mi trng thch hp Cht khng phn hy, sa lng Nhit m bo khng xy ra phn ng ph

    Cc phng php bo qun Trong iu kin thng, khng kh sch Trong t lnh

    Trong t m Trong tuyt cacbonic Trong mi trng kh tr

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    Trn Mai Lin PP ly mu v x l mu 28

    Khi nim QA/QC trong ly mu phn tch

    Quality Assurance (QA)

    Quality Control (QC)

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    Trn Mai Lin PP ly mu v x l mu 1

    Chng 2:

    Cc k thutx l mu phn tch

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    Trn Mai Lin PP ly mu v x l mu 2

    2.1 Yu cu chung ca k thut x l mu

    Yu cu chung Ly c hon ton, khng lm mt cht phn

    tch

    Khng lm nhim bn thm cht phn tch vomu

    Kt qu x l ph hp vi phng php phn tch

    chn Cc ha cht m bo tinh khit

    Khng a thm cc cht gy nh hng vo

    mu Tch, lm giu cht phn tch (nu c th)

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    Trn Mai Lin PP ly mu v x l mu 3

    QA/QC trong x l mu phn tch Khi nim v QA

    Khi nim v QC

    Ni dung QA/QC trong x l mu phn tch

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    Trn Mai Lin PP ly mu v x l mu 4

    2.2 Phn loi mu phn tch

    Phn loi theo ha hc phn tch Nhm mu c nn l v c Nhm mu c nn l cc cht hu c v sinh hc

    Phn loi theo trng thi tn ti Trng thi kh Trng thi rn v bn rn: kim loi, t, , cy

    Trng thi lng: nc, ru, bia, xng Phn loi theo nhm ngnh

    Mu nng nghip

    Mu cng nghip Mu sinh hot Mu t nhin

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    Trn Mai Lin PP ly mu v x l mu 5

    2.3 Trang b x l mu phn tch

    Yu cu ca trang b s dng Cc loi dng cn gin

    Cc loi trang b hon chnh

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    Trn Mai Lin PP ly mu v x l mu 6

    Extraction of peppermint leaves with hot water

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    Trn Mai Lin PP ly mu v x l mu 7

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    Trn Mai Lin PP ly mu v x l mu 8

    2.4 Khi qut v bn cht cc k thut x l mu

    XLM l qu trnh chuyn mu thnh dng c th

    phn tch c bng mt phng php thch hp

    Mt qu trnh x l mu c th c cc giai on Ph v cu trc

    t chy cht hu c

    To mui tan

    Kt tinh, thng hoa

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    Trn Mai Lin PP ly mu v x l mu 9

    2.4.1 K thut v c ha t (wet digestion)

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    Trn Mai Lin PP ly mu v x l mu 10

    2.4.1 K thut v c ha t (wet digestion)

    Sn phm sau khi x l bng phng php tro ha t

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    Trn Mai Lin PP ly mu v x l mu 11

    V c ha t s dng dung dch axit c

    Nguyn tc

    Cc loi axit thng dng

    Thi gian phn hy mu Cc qu trnh xy ra

    t chy cc hp cht hu c

    Cc phn ng oxy ha kh

    u nhc im ca phng php

    Kh nng ng dng

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    Trn Mai Lin PP ly mu v x l mu 12

    V c ha s dng dung dch kim c

    Nguyn tc

    Cc loi axit thng dng

    Thi gian phn hy mu u nhc im ca phng php

    Kh nng ng dng

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    Trn Mai Lin PP ly mu v x l mu 13

    K thut ph mu trong l vi sng

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    Trn Mai Lin PP ly mu v x l mu 14

    Cc v d

    V c ha t mu trong l vi sng xc nh mts cation (Al, Ba, Mg, Fe, Cu, Pb, As, Sb) trongcc i tng bn, trm tch, t hoc du

    Mt s lu : Thit b: l vi sng chuyn dng cho cc PTN Cc bnh phn hy mu: 0,25g thng s dng

    trong bnh 120ml, p sut c tht ti 7,5 0,7

    atm Cc acid c s dng phi c tinh khit cao

    (thng qua mu trng loi tr)

    Qu trnh ph mu Cn mt lng mu: khng qu 0.5g cho mu bn,

    t, trm tch; 0.25g cho mu du

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    Trn Mai Lin PP ly mu v x l mu 15

    Thm 10ml HNO3: nu mu cha nhng cht dbay hi hoc nhiu hp cht hu c th c thmu phn hy trc khi cho trong l vi sng (gimkhi lng mu)

    Nhng mu bit trc c hm lng cht hu c 5 10% thng c phn hy ngoi 15 pht

    S phn hy thng 175 1800C trong thi gian

    5 pht Sau thi gian phn hy, mu c ha tan trong

    dung dch axit long

    Mu c thc li tm, lc m bo ngnht trong mu

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    Trn Mai Lin PP ly mu v x l mu 16

    V d:

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    2 4 2 K th t h kh (d di ti )

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    Trn Mai Lin PP ly mu v x l mu 17

    2.4.2 K thut v c ha kh (dry digestion)

    K thut v c ha kh thc cht l k thut nung(c th c trn thm cc ph gia)

    K thut nung khng ph gia:

    Mu Dng d ha tanNhit cao

    S tro ha, t chycht mn, hu c

    Ph v cu trc tinh th

    Qa trnh oxy ha, bayhi

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    V d t h kh d h i

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    Trn Mai Lin PP ly mu v x l mu 18

    V d: tro ha mu khng dng ph gia

    Tro ha mu rau xc nh cc kim loi (Na, K,Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb)

    Mu

    (5g)Sy kh chm Nung 500 5300C

    Mu tro trng

    Ha tan mu = HCl

    Ch : mt s kim loi (Cd, Cu, Pb, Zn) d b mt(10 15%) do bay hi

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    2 4 2 K th t h kh (d di ti )

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    Trn Mai Lin PP ly mu v x l mu 19

    2.4.2 K thut v c ha kh (dry digestion)

    K thut nung c ph gia

    Mu Dng d ha tan

    Nhit cao +ph gia

    S tro ha, t chy

    cht mn, hu c Ph v cu trc tinh th

    Qa trnh oxy ha, bayhi

    S tng tc cht phgia

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    2 4 2 K th t h kh (d di ti )

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    Trn Mai Lin PP ly mu v x l mu 20

    2.4.2 K thut v c ha kh (dry digestion)

    Cht ph gia v bo v: Cc axit mnh

    Mui

    Peroxit Hn hp kim + peroxit

    Vai tr cht ph gia: gim nhit nung, thi giannung, ph mu trit , khng lm mt cht

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    K thut v c ha kh t kt hp

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    Trn Mai Lin PP ly mu v x l mu 21

    K thut v c ha kh t kt hp

    Mu

    + dd axit

    Nung Ha tan

    u im:

    - Lng axit s dng t hn (= hoc 1/3 lng axit

    dng trong s l t)- Thi gian nung gim

    - Gim thi gian ui axit d

    - Thch hp cho phn tch kim loi v cc anion Cl-,SO42-, Br-

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    Mt s v d

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    Trn Mai Lin PP ly mu v x l mu 22

    Mt s v d

    Mu sa

    + 10ml HNO3 ,5ml Mg(NO3) 5%,

    2ml H2SO4 Nung

    500 5500C Tro trng Ha tan tro

    Mu rau

    + 10ml HNO3,5ml Mg(NO3) 5% Nung

    500 5500CTro trng Ha tan tro

    http://hoahocsp.tk

    2 4 4 Cc k thut chit

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    Trn Mai Lin PP ly mu v x l mu 23

    2.4.4 Cc k thut chit

    L thuyt chung v k thut chit: da trn s phnb ca mt cht vo 2 pha khng trn ln

    H s phn b

    ( )

    ( )

    X

    Y

    C AK

    C B

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    Qui trnh chit

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    Trn Mai Lin PP ly mu v x l mu 24

    Qui trnh chit

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    Liquid-liquid extraction

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    Trn Mai Lin PP ly mu v x l mu 25

    Liquid-liquid extraction

    Mixing or contacting

    Phase separation

    Collection of separate phases

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    V d

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    Trn Mai Lin PP ly mu v x l mu 26

    V d

    Chit vitamin A t sa:

    10 ml sa mu

    + 20 ml ru etylic

    + 5 g Na2

    SO4

    khan

    + 10 ml n-hexan

    Hn hpLcTch lp

    Dd nc n-hexan + vitamin A Xc nh Vitamin A = pp HPLC

    http://hoahocsp.tk

    Chit pha rn - SOLID PHASE EXTRACTION

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    Trn Mai Lin PP ly mu v x l mu 27

    Chit pha rn SOLID PHASE EXTRACTION

    http://hoahocsp.tk

    Chit pha rn - SOLID PHASE EXTRACTION

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    Trn Mai Lin PP ly mu v x l mu 28

    Chit pha rn SOLID PHASE EXTRACTION

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 29

    Solid Phase Extraction cartridges

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 30

    Various sorption techniques:

    centrifuge

    positive pressure

    http://hoahocsp.tk

    Large volumes:

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    Trn Mai Lin PP ly mu v x l mu 31

    http://hoahocsp.tk

    C ch chit pha rn

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    Trn Mai Lin PP ly mu v x l mu 32

    p

    Chit theo c ch hp ph pha thng Pha tnh: silica trung tnh, b mt phn cc

    Mat OH + RX {Mat OH}.RX

    Dung mi ra gii cht pt thng l cc dungmi hu c khng phn cc, c kh nng ha tantt cht pt tch c hon ton cht pt khipha rn (gi l pha ng)

    Cht chit pha tnh Cht pt Cht pt b hp phln pha rn

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 33

    polar

    non-polar

    http://hoahocsp.tk

    V d: chit thuc tr su trong mu nc

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    Trn Mai Lin PP ly mu v x l mu 34

    g

    Ct chit c chacc ht LaSiOH

    Mu ( lc bcn) c diqua ct chit vitc 4 ml/pht

    Chthp phtrn htLaSiOH

    Gii chit bngdung mi

    diclometan

    Cht pt tantrong dung mi

    http://hoahocsp.tk

    C ch chit pha rn

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    Trn Mai Lin PP ly mu v x l mu 35

    Chit theo c ch hp ph pha ngc Pha tnh: silica c b mt khng phn cc

    Mat (CH2)17CH3

    Cht chit C18

    RX+ Mat (CH2)17CH3.RX

    Cht pt hp ph ln pha rn

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 36

    http://hoahocsp.tk

    C ch chit pha rn

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    Trn Mai Lin PP ly mu v x l mu 37

    --

    - --

    -

    +

    +++

    + +

    +

    +

    + + -

    -

    -

    -

    Cation

    exchange

    Anion

    exchange

    Adsorbents

    Bound

    molecules

    Chit theo c ch trao i ion

    http://hoahocsp.tk

    Cation exchange: Lysozyme separation

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    Trn Mai Lin PP ly mu v x l mu 38

    Egg white proteins

    Egg

    whiteproteins

    Cation

    exchangeadsorbent

    Adsorbent+

    lysozyme

    Other

    egg

    white

    proteins

    Lysozyme

    +

    NaCl

    Cation

    exchangeadsorbent

    + NaCl

    http://hoahocsp.tk

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    on exchange

    A v B

    Anionexchangeadsorbent

    BA+

    NaCl

    Anionexchangeadsorbent

    + NaCl

    A +adsorbent

    http://hoahocsp.tk

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    ch chit pha rn

    hit theo c ch sng v ry phn t

    Sau khi hp ph

    Ra giiIon c kchthc ln ratrc ri n

    cc ion c kchthc nh

    http://hoahocsp.tk

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    thut chit hp ph dng kh

    He towaste

    Dng khtr nng

    H thngphn tch GC

    kh He

    Cthpth

    http://hoahocsp.tk

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    c k thut chit

    n-exchange chromatography

    ration is based on exchange of ionseen surface and eluents.

    Part it ion chromatographySeparation is based on solute partitioningbetween two liquid phases.

    dsorpt ion chromatographyration is due to a series of adsorption/rption steps.

    Size-exclusion chromatographySeparation is based on molecular size.

    + +

    -

    -

    -

    http://hoahocsp.tk

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    it Soxhlet (Soxhlet extraction process)

    http://hoahocsp.tk

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    it soxhlet

    http://hoahocsp.tk

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    it soxhlet

    ui tc chn dung miDung mi khng phn cc (du, ete, hexan) s

    ha tan cc cht khng phn cc (cht bo)

    Dung mi phn cc (metanol, etanol, nc)ha tan cc cht phn cc (mui, ng)

    i lc ca cht tan trong dung mi hu c c th

    tng khi s dng mt hn hp cc dung mi

    http://hoahocsp.tk

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    n hp cc dung mi

    xample: solublizationf an aliphaticrboxylic acid inthanol, acetone andmixture of both.

    -R-C

    O------------H-O-CH2-CH3

    O-H

    In ethanol

    In acetone R-C

    O-H---------O=C

    O

    CH3

    CH3

    Hydrogen bond

    Hydrogen bond

    R-C

    OH

    O HO-C2H5

    O=C

    CH3

    CH3

    (ethanol)

    (acetone)

    In a mixture of acetone and ethanolhttp://hoahocsp.tk

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    thut chit siu m

    2

    1 1

    2

    ng siu m S phn b licht phn tch

    trong 2 dung mi

    K

    http://hoahocsp.tk

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    .5 K thut chng ct

    guyn tc: da theo im sic kiu chng ct

    Chng ct thng thng

    Chng ct li cun (hi nc)Chng ct di p sut thp

    Chng ct trong mi trng siu m

    http://hoahocsp.tk

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    http://hoahocsp.tk

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    ng ct thng thng

    http://hoahocsp.tk

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    http://hoahocsp.tk

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    http://hoahocsp.tk

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    http://hoahocsp.tk

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    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 1

    Chng 3. X l mu xc nh

    cc kim loi v phi kim

    http://hoahocsp.tk

    t vn

    i t h t h ki l i hi ki

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    Trn Mai Lin PP ly mu v x l mu 2

    i tng phn tch: cc kim loi v phi kim

    Cc k thut c th dng x l: Hu ht cc kthut hc

    Phn loi mu chn cch x l:

    Mu nn v c: hp kim, qung, t, cc snphm cng nghip

    Mu nn hu c: thc vt, ng vt, thc phm

    http://hoahocsp.tk

    3.1 X l mu v c

    M t h h t h

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    Trn Mai Lin PP ly mu v x l mu 3

    Mt s hng phn tch Xc nh cc ion kim loi di ng

    Xc nh tng hm lng ca mt s cht trong

    mu Xc nh mt s anion, kim

    http://hoahocsp.tk

    X l ly cc ion kim loi di ng (trao i)

    l h ti th h t i

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    Trn Mai Lin PP ly mu v x l mu 4

    y l ch tiu thng c xc nh trong itng: t, phn bn

    Cc ion kim loi ny d dng trao i s dng

    mt dung mi thch hp chit cc ion kim loivo dung dch

    http://hoahocsp.tk

    X l ly cc ion kim loi di ng (trao i)1. Di qua dd mu NH4+

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    Trn Mai Lin PP ly mu v x l mu 5

    Mu t bao gmcc cation trao iCa, Mg, Na, K, H, Al

    Mu c bp havi NH4+

    2.y NH4+ bng K+

    3. Thu v xc nh NH4+

    t + K+

    Hn hpcc ion

    NH4+

    http://hoahocsp.tk

    X l ly cc ion kim loi di ng (trao i)

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    Trn Mai Lin PP ly mu v x l mu 6

    Xc nh CEC: olng d (NH4

    +)

    Xc nh ion kim loitrao i: xc nh

    lng mui to thnhsau khi di qua mudung dch cation traoi

    Ct

    t + Ct

    Ct

    Bng

    Cation

    trao i

    http://hoahocsp.tk

    X l mu ly hm lng tng kim loi

    Nhn xt:

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    Trn Mai Lin PP ly mu v x l mu 7

    Nhn xt: Ch tiu phn tch: tng kim loi trong mt i

    tng

    Phng php x l thch hp: V c ha t

    Kt hp x l kh + t

    Chit Mt s v d (GT)

    http://hoahocsp.tk

    3.2 X l mu hu c

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    Trn Mai Lin PP ly mu v x l mu 8

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 1

    Chng 4. X l mu xc nh

    cc cht hu c

    http://hoahocsp.tk

    Ni dung

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    Trn Mai Lin PP ly mu v x l mu 2

    4.1 Khi nim v phn loi mu hu c

    4.2 Cc k thut x l mu xc nh cht hu c

    http://hoahocsp.tk

    4.1 Khi nim v phn loi mu hu c

    Mu hu c l mu m cht nn ca n l cc cht

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    Trn Mai Lin PP ly mu v x l mu 3

    Mu hu c l mu m cht nn ca n l cc chthu c

    Cht hu c rt a dng, d b phn hy hn cccht v c

    V vy ngoi nhng yu cu chung, cn c cc yucu ring cho vic x l phn tch cc cht hu c

    Kh tch cht ra khi mu u

    Khng bn d b mt do phn hy

    Phi c nhiu trang b

    Cn s dng nhiu dung mi Khng ch nghim ngt cc iu kin

    http://hoahocsp.tk

    4.2 Cc k thut x l mu xc nh cht hu c

    Nguyn tc chung

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    Trn Mai Lin PP ly mu v x l mu 4

    Nguyn tc chung Chuyn mu thnh dng thch hp phn tch

    Ly mt lng nht nh phn tch bng cc

    phng php: chng ct, chit Cc phng php, k thut x l

    K thut chng ct

    Chng ct thng Chng ct chn khng

    K thut chit

    Chit lng lng Chit dng lin tc

    http://hoahocsp.tk

    K thut sc k

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    Trn Mai Lin PP ly mu v x l mu 5

    K thut sc k V d

    http://hoahocsp.tk

    SINH VIN THUYT TRNH

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    Trn Mai Lin PP ly mu v x l mu 6

    http://hoahocsp.tk

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    Trn Mai Lin PP ly mu v x l mu 1

    Chng 5. X l v phn tch mu

    mi trng

    http://hoahocsp.tk

    Ni dung

    5 1 Khi nim v mu mi trng v phn loi

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    Trn Mai Lin PP ly mu v x l mu 2

    5.1 Khi nim v mu mi trng v phn loi5.2 Cc phng php x l mu v v d

    5.2.1 Nc, nc thi v phn tch chng5.2.2 X l cc loi mu b thi

    5.2.3 X l mu khng kh, khi v bi

    5.2.4 X l mu t bn v trm tch

    5.2.5 X l mu rong ru trong nc

    http://hoahocsp.tk

    5.1 Khi nim v mu mi trng v phn loi

    Thy quynKh

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    Trn Mai Lin PP ly mu v x l mu 3

    Thy quyn Kh quyn

    a quyn

    http://hoahocsp.tk

    Ly mu v bo qun mu nc

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    Trn Mai Lin PP ly mu v x l mu 4

    http://hoahocsp.tk

    GII THIU CHUNG

    Ly mu l thu thp mt phn vt cht trong mt th tch y x l v vn chuyn v phng th nghim kp lc khi cht

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    Trn Mai Lin PP ly mu v x l mu 5

    y p p g y, x l v vn chuyn v phng th nghim kp lc khi cht

    lng mu cha thay i.

    Ngi ly mu phi chu trch nhim v cht lng mu cho

    n khi mu c gi n phng th nghim phn tch.

    http://hoahocsp.tk

    NHNGIU CN LU

    Mu phi c bo qun trnh mi ngun nhim bnhoc s phn hy c th xy n trc khi a v

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    Trn Mai Lin PP ly mu v x l mu 6

    p q ghoc s phn hy c th xy n trc khi a v

    phng th nghim.

    Phi sc ra t nht hai n ba ln bnh ly mu bngchnh ngun nc trc khi ly mu, tr trng hp

    bnh c x l bng ha cht bo qun hay cc

    cht kh clo.

    http://hoahocsp.tk

    NHNGIU CN LU

    i vi nhng mu phi vn chuyn xa, khng nn lyqu y m cha li 1% dung tch bnh khong trng

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    Trn Mai Lin PP ly mu v x l mu 7

    qu y m cha li 1% dung tch bnh, khong trng

    ny phng h s dn n nhit. Tuy nhin iu ny

    ty thuc vo cc xt nghim cn lm. Mu tiu biu cho nhiu ngun c thc to t vic

    pha trn cc mu ly thi im khc nhau hoc tng

    a im khc nhau.

    http://hoahocsp.tk

    NHNGIU CN LU

    c cht l lng v cht khc, nhng thay i ha ldo thng thong hay xy ra trong qu trnh tn tr l nhng

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    Trn Mai Lin PP ly mu v x l mu 8

    do thng thong hay xy ra trong qu trnh tn tr l nhng

    yu t quan trng nh hng n kt qu

    Tt nht nn ghi r mu lc hay cha lc

    Phi ghi chp nhng chi tit lin quan n vic ly mu. Cn

    ghi chp y , r rng tn ngi ly mu, ngy gi, nhit

    nc v km nhng d liu khc nh thi tit, mc nc,

    dng chy, trm quan trc thi im gi mu

    http://hoahocsp.tk

    NHNGIU CN LU

    Chtha im ly mu r rt trn bn , tt nht nnnh du cc v tr bng cc phao hay m t cc c

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    Trn Mai Lin PP ly mu v x l mu 9

    nh du cc v tr bng cc, phao hay m t cc c

    im hay b ngi khc d nhn din li d dng lc

    cn m khng phi vn dng li tr nh hay ln tm quali hng dn.

    Nu mun ly mu t h thng phn phi, nn x vi

    chy t do trong mt thi gian ngn m bo mu thhin ng cht lng ngun.

    http://hoahocsp.tk

    NHNGIU CN LU

    Cch ly mu hn hp ty thuc vo tnh cht, lulng v ch thy lc ca dng chy Nu ch cn ly

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    Trn Mai Lin PP ly mu v x l mu 10

    lng v ch thy lc ca dng chy. Nu chcn ly

    mu bt k, nn ly mu su trung bnh ti v tr

    gia dng. i vi mu cc h v hm cha, khi ly mu phi lu

    n tc ng ca ma, lng nc chy trn b mt,

    gi, yu t phn tng theo ma tt cu c th gynh hng n cht lng nc.

    http://hoahocsp.tk

    NHNGIU CN LU

    Trnh cc vng xo trn mnh v d lm tht thot cccht d bay hi trong c c cht c. Thng thng,

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    Trn Mai Lin PP ly mu v x l mu 11

    y g g g,mu c ly vng tnh, di mt thong. Nu c yucu v mt hn hp, phi thn trng i vi cc thnh

    phn d tht thot khng phi do qu trnh ly mu mv vic x l khng ng cch.

    Chs dng cc mu thch ng vi cuc kho st (hoc

    nhng mu nm trong chng trnh ly mu), khi lymu nhng iu kin khc nn ghi chp li r rng vy chi tit.

    http://hoahocsp.tk

    BIN PHP AN TON

    V trong mu c th c nhng thnh phn c cht nn phip dng nhng bin php phng hu hiu trong sut qu

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    Trn Mai Lin PP ly mu v x l mu 12

    p g g p p p g g q

    trnh ly v x l mu.

    i vi cht hu c d chy, cn phi p dng cc bin php

    an ton thch nghi.

    Khi cha tin tng vo mc an ton, mi bin php

    phng u rt cn thit, phi quan tm n vn hun luyn

    v an ton lao ng. Ty ngun nhim bn m c bin php phng h y t ngh nghip khc nhau.

    http://hoahocsp.tk

    MU BT K (MU C BIT)

    Khi mu c ly ti mt thi im, mt v tr nht nh, nicho ng mu y chth hin c mt cht lng ngun

    thi i t t i thi i l h

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    Trn Mai Lin PP ly mu v x l mu 13

    nc vo thi im v v tr ti m thi.i lc phngphp ly mu bt k cng c p dng cho c trng hpnc thi.

    i vi ngun c bit r l cht lng lin tc c thayi theo thi gian, nhng mu c bit c ly trong tngkhong thi gian thch hp v phn tch ring s cho d liuv nhng bin i trong phm vi gii hn.

    i vi cht mn, bn v nc thi, bn ven b cn phi cnphi cn nhc khi chn phng php ly mu.

    http://hoahocsp.tk

    MU HN HP

    i vi nhiu trng hp, thut ng mu hn hpc dng din t s trn ln cc mu c bit ly

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    Trn Mai Lin PP ly mu v x l mu 14

    nhiu im khc nhau trn cng 1 v tr.

    Mu hn hp thch hp cho vic kho st cc hmlng trung bnh, th d nh trong cch tnh ti trng hayhiu qu ca cng trnh x l nc thi.

    nh gi nhng hiu qu, bin ng ring bit hay

    cc lu lng tht thng th cng chcn ly mu hnhp trong sut thi gian xy ra cng .

    http://hoahocsp.tk

    MU HN HP

    Mun xc nh thnh phn hay cc yu t chth nhngthay i thng gp trong hm cha th khng nn dng

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    Trn Mai Lin PP ly mu v x l mu 15

    y g gp g g g

    mu hn hp. Trong trng hp ny, cc mu ring l

    s ph hp hn. Tm li, loi mu ny thng c dng cho vic xc

    nh thnh phn t thay i trong iu kin ly mu v

    bo qun mu.

    http://hoahocsp.tk

    MU HN HP

    Vic trn mu c thc hin trong mt bnh ln cdung tch 2 3 lt phn tch cc thnh phn trong

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    Trn Mai Lin PP ly mu v x l mu 16

    nc cng, nc thi, hoc t ng thot nc.

    Khng nn s dng cc dng c ly mu tng tr khip dng c y cc phng php cch bo qun.Tt c dng c phi c ra sch hng ngy trnhs pht trin sinh hc v cc cht lng ng khc.

    Thnh thong cng cn phn tch trn mt mu ring lnu xt thy cn.

    http://hoahocsp.tk

    PHNG THC BO QUN

    Th

    i gian t

    n tr

    ti aPh

    ng th

    c boqunCh

    tiu phn tch

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    Trn Mai Lin PP ly mu v x l mu 17

    48 gi40CMu

    6 gi40CMi

    24 gi40C acid, kim

    28 gi40C dn in

    Khng cn thitFloride (F-)

    Khng cn thitChloride (Cl-)

    Khng cn thitCalci (Ca2+)

    Khng cn thit cng

    http://hoahocsp.tk

    PHNG THC BO QUN

    Thi gian

    tn tr ti a

    Phng thc

    bo qun

    Ch tiu

    phn tch

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    Trn Mai Lin PP ly mu v x l mu 18

    24H2SO4, pH < 2, 40CPhenol

    24NaOH, pH >12, 40CCyanide

    72 ml/l HCl, pH < 2Carbon hu c

    282 ml/lH2SO4, 40CDu v m

    72 ml/lH2SO4COD

    8(0,7 ml H2SO4 + 1 ml NaN3)/300ml; 10-200C

    DO72 mg/l zine acetateH2S

    28 ngy40C; pH < 8Sulphate

    http://hoahocsp.tk

    PHNG THC BO QUN

    Thi gian tn tr

    ti a

    Phng thc

    bo qun

    Ch tiu

    phn tch

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    Trn Mai Lin PP ly mu v x l mu 19

    6 thngHNO3, pH < 2, 40CFe, Mn

    48 gi40CPhosphate

    Phn tch ngayH2SO4, pH < 2, 40CN-NO2; N-NO3

    7 ngyH2SO4, pH < 2, 40CN-NH3

    bo qunphn tch

    Th

    i gian phn tch cng s

    m cng t

    t

    http://hoahocsp.tk

    MT S THIT BO TI HIN TRNG

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    Trn Mai Lin PP ly mu v x l mu 20

    http://hoahocsp.tk

    Phng php ly v bo qun mu kh Ly mu khng kh mc ch nhm xc nh mt cch chnh xc nng

    cc cht nhim sau:SO2, NO2, O3, bi l lng, ch bi . bi vt vicquan trc phi tin hnh nghim tc, chnh xc theo ng quy nh banhnh.

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    Trn Mai Lin PP ly mu v x l mu 21

    Nhn vin quan trc phi c trnh chuyn mn, tay ngh caov phi c kh nng s l cc tnh hung

    Chun b quan trc phi chu o bao gm cc cng vic sau: Pha ch dung dch hp th ti hin trng, chun b v cn cc phin

    lc thu mu bi. Chun b cc bnh cha dung dch, ng nghim ng mu, cc mu

    i chng.

    Cc my ly mu phi t yu cu k thut nh chun xc v nnh v lu lng. u thu mu, ng hp th, cc my quan trc thitit phi m bo cc yu cu t ra

    Cc bng biu, nht k cng tc Cc thit b bo qun vn chuyn mu

    Cc thit b ph tr: my pht in, pin

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    Phng php ly v bo qun mu kh

    Nguyn tc ly mu: Bm khng kh c cha cht nhim qua dng c cha dung dch hp th hocphin lc hoc ng hp th cht nhim b gi li

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    Trn Mai Lin PP ly mu v x l mu 22

    phin lc hoc ng hp th, cht nhim b gi licn khng kh th i qua.

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    Chun b ho cht, dng c v thit b ly mu: Pha ch, bo qun dung dch hp th hoc giy

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    Trn Mai Lin PP ly mu v x l mu 23

    lc bi theo cc phng php tng ng

    Kim chun thit b v tin cy, chnh xc v lch chun ca lu lng. i vi my ly khc thng l cc bm ht c lu lng nh 0,5-

    5lt/pht; Chun lu lng trong khong 0,5- 1lt/pht khi ht qua dung dch hp th. Cc myly bi tng s phi c lu lng ln 20- 30

    lt/pht; Chun lu lng theo chdn ca my.

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    Phng php ly v bo qun mu kh

    u ly mu: Cc my mua mi u km theocc u ly mu.

    Khi ly mu bi phi chn giy lc dng si thu

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    Trn Mai Lin PP ly mu v x l mu 24

    Khi ly mu bi phi chn giy lc dng si thutinh c kch thc trng vi kch thc u ly

    bi. Khi ly mu kh, ng hp th thng c dung tch

    10ml, 25ml hoc 100ml c hoc khng c mng

    xp phn tn dng kh. Nn dng loi nh vni tip hai ng c cha dung dch hp thm bo cht nhim c hp th ht.i viCO ly mu bng chai, chai ly mu phi m

    bo khng thot kh mu thot ra ngoi hockhng kh bn ngoi thm nhp vo.

    t u o cch mt t 1,2- 1,5m .

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    Phng php ly v bo qun mu kh

    S h thng ly

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    u ly mu

    Lu lng k

    Mng lc bo v

    ngni

    S h thng ly mu kh, bi

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    Phng php ly v bo qun mu kh Mu bi ng trong bao kp bng giy can k thut c th bo qun d

    dng v lu di nhit thng, nhng ni chung khng nn quba ngy.

    Cc mu kh ly song phi bo qun trong bnh lnh c nhit 5 C

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    Cc mu kh ly song phi bo qun trong bnh lnh c nhit 5 Cv vn chuyn nhanh v phmg th nghim. Mu O3 sau kh ly phi

    phn tch ngay ti ch cng nhanh cng tt. Kh ly mu bng ng hp th, ly mu xong rt mu vo l thu tinh c

    nt nhm hoc ng nghim c nt chc chn, t trong bnh lnh vvn chuyn ngay v, nu cha kp phn thch th t trong ngn mtca t lnh (phi phn tch ngay trong 24h).

    i vi chai ng kh mu CO, chai ng mu phi nt v gn kn gitrong cc thng g hoc tn c chn xp trnh v.

    Nu c mu lu, cc mu lu khong ba thng, nu khng c iu gnghi ngi th c th lp bin bn hu mu.

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    Phng php ly v bo qun mu t

    Ly mu

    Ty theo mc ch nghin cu v kho st lachn cc phng php ly mu khc nhau

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    Trn Mai Lin PP ly mu v x l mu 27

    chn cc phng php ly mu khc nhau Mu c bit c ly mt v tr xc nh (theo

    tng phu din) Mu hn hp: c trn t nhiu mu ban u to

    thnh mu chung i din cho mt phm vi tc kho st

    Ty theo hnh dng v a hnh mnh t cn lyt nht 5 im phn bu trn ton din tchtheo qui tc ng cho, ng vung gc hay

    ng dch dc

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    Phng php ly v bo qun mu t

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    Phng php ly v bo qun mu t

    Cc mu ban u c gom li thnh mu hnhp chung c khi lng t nht 2kg

    T mu hn hp chung chn thnh mu hn hp

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    Trn Mai Lin PP ly mu v x l mu 29

    T mu hn hp chung, chn thnh mu hn hptrung bnh bng cch bm nht, trn u v

    loi bt theo nguyn tc ng cho gc. Muhn hp trung bnh c khi lng 1kg

    1

    4

    3

    2

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    Phng php ly v bo qun mu t

    Nhng mu t xc nh dung trng, t trng v xp c gi nguyn trng thi v c lybng dng c ring

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    Trn Mai Lin PP ly mu v x l mu 30

    g g g

    Trnh ly mu nhng ni c th: ni bn

    phn, vi, v tr gn b, qu cao hoc qu trng Mu t c cho vo ti vi hoc nha, ghi k

    hiu mu ngy ly mu, su, a im

    Nhng mu phn tch cc chtiu d bin inh: NH4+, NO3

    -, Fe2+ cn phn tch mu tti, bo qun lnh, trong ti kn, phn tch ngay

    Nhng mu phn tch cc chtiu thng thngu c xc nh bng t kh

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    Phng php ly v bo qun mu t

    Hong kh t:

    Chuyn ton bt vo khay nha sch, khtrong khng kh ni thong mt sch khng c

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    Trn Mai Lin PP ly mu v x l mu 31

    trong khng kh ni thong mt, sch, khng ccc kh nh H2S, HCl, NH3 Khng phi trc tip

    ngoi nng Nhng cc t ln c p nh hoc ct thnh

    lt mng ri u ra khay

    t c hong kh trong khng kh gi l t khkhng kh

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