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CHNG 1

I CNG V HA PHN TCH

GV: Trn T Phng Tho HBK

NI DUNG CHNH (2LT)


I. Ni dung v yu cu ca ho phn tch II. Phn loi cc phng php phn tch III. Cc loi phn ng ho hc dng trong ho phn tch IV. Cc giai on ca mt phng php phn tch
GV: Trn T Phng Tho HBK 2

I. NI DUNG V YU CU CA HO PHN TCH 1. Gii thiu v Ha phn tch 2. Cc yu cu ca Ha phn tch


GV: Trn T Phng Tho HBK 3

1. Gii thiu v Ha phn tch


VD: Mu nc sinh hot c s dng nu n c hay khng? Ch tiu nc ung (Tieu chuan Quoc te): pH: 6,5 8,5 SO42- < 250ppm Tng Fe < 0,3ppm Cl- < 250ppm NO3- < 50ppm
GV: Trn T Phng Tho HBK 4

1. Gii thiu v Ha phn tch


Kim tra xem mu nc c t tiu chun khng? Mu nc c s hin din ca cc ion hay khng? Phn tch nh tnh Hm lng ca cc ion ny l bao nhiu? C vt ch mc cho php hay khng Phn tch nh lng
GV: Trn T Phng Tho HBK 5

1. Gii thiu v Ha phn tch


Ho hc phn tch l khoa hc nghin cu : Cc phng php phn tch nh tnh Cc phng php phn tch nh lng Cc phng php kim tra cc qu trnh ha l v k thut ho hc.
GV: Trn T Phng Tho HBK 6

Phn tch nh tnh


Nhn danh cu t trong mu phn tch. nh gi s b hm lng (a lng (> 0,01%), vi lng (vt)) BNG CCH: Chuyn cht phn tch v cht mi c c trng c th nhn bit c (mu, tinh th, trng thi vt l xc nh)
GV: Trn T Phng Tho HBK 7

NH4

Phn tch nh tnh o - t + OH NH3 + H2O co kh mui khai sinh ra lam xanh quy tm

Co ion NH4 trong dd

Pb

2+

+ CrO4

2-

PbCrO4 tua vang


8

GV: Trn T Phng Tho HBK

Test for Lead Pb(NO3)2


CrO42solution

Yellow PPT Solution of Pb2+ (5 -10 drops)


GV: Trn T Phng Tho HBK 9

Phn tch nh lng


Xc nh chnh xc hm lng trong mu da trn php o nhng c tnh: o mu sc khi lng, th tch Vai tr chnh trong HPT tuy nhin do phc tp ca mu trong thc t m ta cn phi nhn danh mu trc th mi c th tin hnh chn PPL ph hp.
GV: Trn T Phng Tho HBK 10

Cc phng php kim tra cc qu trnh ha l v k thut ho hc.


Kim tra quy trnh cng ngh ha hc Kim tra cht lng sn phm.. .
GV: Trn T Phng Tho HBK 11

2. Cc yu cu ca ha phn tch
Pht trin ngang tm vi cc ngnh KH khc C kin thc v cc mn khoa hc t nhin v tin hc nm vng nguyn tc ca phng php, pht trin pp mi trn cc cn bn c sn. C tnh cn thn, kin nhn, chnh xc, sch s, trung thc v kh nng phn on kt qu phn tch.
GV: Trn T Phng Tho HBK 12

II. PHN LOI CC PHNG PHP PHN TCH


1. Theo bn cht phng php 2. Theo lng mu phn tch hay k thut phn tch 3. Theo hm lng cht kho st 4. Theo trng thi cht kho st
GV: Trn T Phng Tho HBK 13

PHN LOI THEO BN CHT CA PP

PP ho hc Dng p/ ha hc chuyn cu t kho st thnh hp cht mi

PP vt l Pht hin v xc nh thnh phn cc cht da trn tnh cht vt l : quang, in, nhit, t...

PP ho l (PP PT dng c) Kt hp PP ha hc v vt l

PP vi sinh nh lng vt cu t da trn hiu ng ca chng vi tc pht trin ca VSV

PP phn tch ng hc PP phn tch da vo cc phn ng xc tc

PP khc - pp nghin - pp nh git - pp iu ch ngc borat hay phosphat - pp soi tinh th

PP phn tch dng c

GV: Trn T Phng Tho HBK

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PHN LOI THEO LNG MU PHN TCH HAY K THUT PHN TCH

Phn tch th 1 10 g hay 1-10 ml

Phn tch bn vi lng 10-3 1 g hay 10-1-1 ml

Phn tch vi lng 10-6 10-3 g hay 10-3-10-1ml

Phn tch siu vi lng < 10-6 g hay < 10-3 ml

GV: Trn T Phng Tho HBK

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PHN LOI THEO HM LNG CHT KHO ST

Phn tch a lng

Phn tch vi lng ( phn tch vt) < 0.01 %

Phn tch lng ln ( 0.1 100%)

Phn tch lng nh (0.01 0.1%)

GV: Trn T Phng Tho HBK

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1. Theo bn cht phng php


a. Phng php ho hc b. Phng php vt l c. Phng php ho l d. Cc pp khc PP soi tinh th di knh hin vi PP nghin iu ch ngc Borax (Na2B4O7) hay photphat PP nh git
GV: Trn T Phng Tho HBK

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a. Phng php ho hc
Cau t khao sat Phh

chat mi Co tnh chat ac trng e nhan danh

GV: Trn T Phng Tho HBK

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a. Phng php ho hc
CH3

O...... H
N
2+

HO N N OH + Ni H3C C C CH3 Dimetylglyoxim

2+

NH3

N Ni
N H...... O

CH3

C CH3

N O

CH3

(TUA O SON)

GV: Trn T Phng Tho HBK

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NH4OH

DMG

Test for Ni2+ (e.g NiSO4)

Solution of Ni2+ ( 5 10 drops)

Pink red PPT

GV: Trn T Phng Tho HBK

Blue solution

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b. Phng php vt l
Tnh cht vt l v thnh phn ho hc c mi lin quan vi nhau. PPVL khng dng phh PPVL s dng cc tnh cht vt l: quang, in, t, t trng.. nh tnh v nh lng cu t kho st.
GV: Trn T Phng Tho HBK 21

b. Phng php vt l
Xc nh t trng ca dd acid, baz, mui tra bng bit nng Xc nh chit sut ca tinh du nh gi s b thnh phn ha hc. Xc nh nhit nng chy, nhit si ca hp cht Da vo tnh tan, tnh hp ph nh tnh v nh lng: PP sc k
GV: Trn T Phng Tho HBK 22

c. Phng php ha l
Va kt hp PPHH v PPVL S dng dng c v thit b kh tinh vi, phc tp gi l PPPT dng c. Gm c: pp ph nghim, pp in ho, pp sc k v mt s pp khc.

GV: Trn T Phng Tho HBK

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c. Phng php ha l
Thc hin phh Kt hp my o quang ph thy c o cng mu ca phc Nng Fe cng nhiu th cng mu cng tng.

Fe

3+

+ nSCN

[Fe(SCN)n]

(3-n)+

GV: Trn T Phng Tho HBK

Phc o mau ( n=1:6 )


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Test for Iron (FeCl3)


NH4SCN solution

Solution of Fe3+ (5 -10 drops)


GV: Trn T Phng Tho HBK

Instense red solution

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c. Phng php ha l

Co

2+ +

nSCN

[Co(SCN)n]

(2-n)+

phc xanh am (n=1:4)

GV: Trn T Phng Tho HBK

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Test for Co2+ (e.g Co(NO3)2)


NH4SCN (crystal or concentrated solution

Blue solution
Solution of Co2+ (5 -10 drops) + Amyl Alcohol (2 - 3 drops)

GV: Trn T Phng Tho HBK

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NHN XT
PP VT L v PP HA L: khng cn ranh gii r rng. PPVL + PPHL: ghp chung thnh PP phn tch dng c.
GV: Trn T Phng Tho HBK 28

d. Cc phng php khc


PP soi tinh th di knh hin vi PP nghin PP iu ch ngc Borax (Na2B4O7) hay photphat PP nh git PP th nghim ngn la
GV: Trn T Phng Tho HBK 29

PP soi tinh th di knh hin vi


Tinh th ca cc vt cht khc nhau c cu trc khc nhau c trng Tinh th ca ion K+ v acid platinoclohidric l K2[PtCl6] c hnh bt din (cc mt khc x nh sng c mu vng chanh) + hnh lp phng. Phn bit CuSO4 v BaSO4
GV: Trn T Phng Tho HBK 30

PP nghin
Mu phn tch v thuc th rn c nghin trong ci s Nguyn t cn pht hin s to hp cht mi vi thuc th Hp cht mi c tnh cht c trng: mu, mi nhn din.

GV: Trn T Phng Tho HBK

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PP nghin
VD: Nghin mu vi vi KSCN, nu mu xut hin du hiu mu mu vi c cha st (III)

GV: Trn T Phng Tho HBK

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PP iu ch ngc Borax (Na2B4O7) hay photphat


Cr + borax Mn- Borax Cu borax
GV: Trn T Phng Tho HBK

to

Ngc bch xanh Mu tm Xanh


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PP nh git
Da vo hin tng mao dn v hp ph. P thc hin trn tm s, thy tinh, giy lc Giy lc: cht lng thm vo giy, sn phm mang mu to thnh b hp ph mt phn nh ca giy lm tng nhy ca p.
GV: Trn T Phng Tho HBK 34

PP nh git
Nhn bit [Fe(CN)6]4- v SCN- trong cng mt mu Giy lc tm FeCl3

Phc mu mu xung quanh


GV: Trn T Phng Tho HBK

Mu xanh ca phc Fe4[Fe(CN)6] gia

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PP th nghim ngn la
Mt s kim loi pht ra bc x c mu c trng khi t trn ngn la xanh ca n kh. Na: la vng K: la tm Ca: la gch Ba: la lc
GV: Trn T Phng Tho HBK 36

2. Phn loi theo lng mu phn tch hay k thut phn tch
PPPT Th Bn vi lng Cch thc hin
Tch rn khi lng bng lc ly tm

Lng mu
(1-10g) hoc 1-10ml (10-3-1g) hoc 10-1-1ml 10-6-10-3 g 10-3-10-1 ml <10-6g <10-3ml

Dng c
50-500ml <50ml <1ml

knh hin vi Vi lng hay phn ng git knh hin vi in t Siu v mi trng GV: Trn T Phng vi lng Tho c bit HBK

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3. Theo hm lng cht kho st


Phn tch a lng: phn tch lng ln (0,1 - 100%) phn tch lng nh (0,01 - 0,1%) Phn tch vi lng (vt): cht kho st c hm lng nh hn 0,01%
GV: Trn T Phng Tho HBK 38

4. Theo trng thi cht kho st Phn tch li t: mu dng dd Phn tch li kh: mu dng rn
GV: Trn T Phng Tho HBK 39

III. CC LOI PHH DNG TRONG HPT


1. Gii thiu phn ng ha hc 2. Phn loi phn ng ha hc 3. Yu cu ca phn ng ha hc
GV: Trn T Phng Tho HBK 40

1. Gii thiu phn ng ha hc


Phn ng phn tch l phn ng ho hc dng trong PTT v PTL:

C + X?

A+B
DD chun
41

C: thuc th dng xc nh X C: c nng xc nh


GV: Trn T Phng Tho HBK

1. Gii thiu phn ng ha hc


PHH l qu trnh to ra s thay i thnh phn ho hc, cu to ca cc cht. Nhim v PHH: Ho tan ho cht, mu Chuyn cht t dng oxy ho sang dng kh v ngc li Tch, che v gii che cc nguyn t
GV: Trn T Phng Tho HBK 42

2. Phn loi phn ng ha hc


P lm thay i s oxy ha ca mt s nguyn t: phn ng trao i in t (P oxy ha kh) Phn ng khng lm thay i s oxy ha ca cc nguyn t: phn ng trao i tiu phn: P acid baz P to phc P to ta
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GV: Trn T Phng Tho HBK

PHN NG HA HC DNG TRONG HA PHN TCH


CC LOI PHN NG HA HC DNG TRONG HPT

Phn ng oxy ha kh

Phn ng trao i tiu phn

Phn ng acid - baz

Phn ng to ta

Phn ng to phc

GV: Trn T Phng Tho HBK

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Phn ng oxy ha kh Ha tan mu:

3Cu + 8 HNO3

3Cu(NO3)2 + 2NO + 4H2O

GV: Trn T Phng Tho HBK

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Phn ng oxy ha kh Tch ion ra khi hn hp: Da vo th oxy ha chun


Eo(I2/2I-) = 0.54V, Eo(Cl2/2Cl-) = 1.36V, Eo(NO2-(H+)/NO) = 0.99V

tch I- ra khi hn hp (I- + Cl-)


GV: Trn T Phng Tho HBK 46

Phn ng oxy ha kh
nh tnh

2Fe

3+

+ 2I

2Fe + I2 lam xanh giay tam ho tinh bot


Mn
2+

2+

nh lng 2+ MnO4 + 5Fe +


GV: Trn T Phng Tho HBK

+ 8H

+ 5Fe + 4H2O

3+

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Phn ng acid - baz


Ho tan: CaCO3 + 2HCl CaCl2 + CO2 + H2O Ph hy phc: [Ag(NH3)2]Cl + 2H+ AgCl + 2NH4+
GV: Trn T Phng Tho HBK 48

Phn ng acid - baz


nh tnh: Xc nh tnh acid baz bng cch o pH nh lng: H2SO4 + 2NaOH Na2SO4 + 2H2O
GV: Trn T Phng Tho HBK 49

Phn ng to ta
nh tnh: AgCl (ta trng), PbCrO4 (ta vng), AgBr (vng nht), AgI (vng) Fe3+ + K4[Fe(CN)6] kalihexacianoferat (II) Fe2+ + K3[Fe(CN)6] kalihexacianoferat (III)
GV: Trn T Phng Tho HBK

Fe4[Fe(CN)6]3 xanh berlin Fe3[Fe(CN)6]2 xanh turbin


50

Phn ng to ta
nh lng: SO42- + BaCl2 BaSO4 + 2ClTch nhm: Vd: tch Ag+, Pb2+, Hg22+ ra khi hn hp dd ca chng vi Fe3+, Al3+, Zn2+ bng ion ClGV: Trn T Phng Tho HBK 51

Phn ng to phc
K hiu: [MLx]n+ M: thng l nguyn t kim loi chuyn tip (ph tng d cha lp y in t) Ligand L: nguyn t hoc nhm nguyn t c electron t do
GV: Trn T Phng Tho HBK 52

Mt s loi Ligand
CH2COOH

CH2COOH

CH2COOH
GV: Trn T Phng Tho HBK

COMPLEXON I

53

Mt s loi Ligand
CH2COOH N CH2COOH

H2 C

H2 C

N CH2COOH

CH2COOH

COMPLEXON II (EDTA)
GV: Trn T Phng Tho HBK

acid EtylenDiaminTetraAcetic)

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Mt s loi Ligand
CH2COONa N CH2COONa

H2 C

H2 C

N CH2COOH

CH2COOH

COMPLEXON III
GV: Trn T Phng Tho HBK

(TRILON B)

55

Phn ng to phc
Ho tan: AgCl + 2NH4OH [Ag(NH3)2]Cl + 2H2O Che cu t di dng phc bn: Vd: hn hp c Fe3+ v Co2+ u to phc vi SCN-, do nh tnh Co2+ phi che Fe3+ bng F- hoc C2O42- di dng phc FeF63- hoc Fe(C2O4)33GV: Trn T Phng Tho HBK 56

Phn ng to phc
nh tnh:

Fe

3+

+ nSCN

[Fe(SCN)n]

(3-n)+

Phc o mau ( n=1:6 )


nh lng:
Al3+ + H2Y2- AlY- + 2H+

Gii che:
GV: Trn T Phng Tho HBK

Hg2+ + [Fe(CN)6]4- Hg(CN)2 + Fe2+

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3. Yu cu ca phn ng HH
3.1. Yu cu ca P phn tch 3.2. Yu cu ca thuc th trong ho phn tch 3.3. Yu cu ca dd chun (thuc th c nng chnh xc)
GV: Trn T Phng Tho HBK 58

3.1. Yu cu ca P phn tch


Xy ra tc thi. Xy ra hon ton theo chiu mong mun C h s xc nh v cho sn phm c thnh phn xc nh. C du hiu c trng nhn bit phn ng chm dt.
GV: Trn T Phng Tho HBK 59

YU CU I VI CC THUC TH DNG TRONG HPT

tinh khit cao H/ cht k thut X 99% H/ cht tinh khit (P): 99,0% X 99,9% H/ cht tinh khit PT(PA):
99,90% X 99,990% X 99,99% 99,999%

H/cht tinh khit ha hc: H/cht tinh khit quang hc :


99,9990% X 99,9999%

nhy cao - Gii hn pht hin : lng ti thiu ca X (g / ml) cn pht hin c bi thuc th. - long gii hn : th tch dung mi ti a (ml) dng ha tan 1 g cu t X m vn cn pht hin c X

Tnh chn lc (c hiu) cao

GV: Trn T Phng Tho HBK

60

3.2. Yu cu ca thuc th trong ho phn tch


Tinh khit, tnh chn lc cao Tnh nhy cao: c kh nng pht hin X d hm lng thp Gii hn pht hin (g/ml) long gii hn (ml/g) Thi gian du hiu nhn bit xut hin
GV: Trn T Phng Tho HBK 61

3.2. Yu cu ca thuc th trong ho phn tch


Gii hn pht hin (g/ml): lng X ti thiu (ppm) m thuc th vn cn kh nng pht hin c. V d: Gii hn pht hin ca SCNi vi Fe3+ l 0,25 (g/ml)
GV: Trn T Phng Tho HBK 62

3.2. Yu cu ca thuc th trong ho phn tch


long gii hn (ml/g): th tch dung mi ti a ho tan 1g X m vn cn pht hin c X Thi gian du hiu nhn bit xut hin: V d: SCN- pht hin Fe3+ nhy hn NH4OH do ta nu xut hin chm hn phc mu.
GV: Trn T Phng Tho HBK 63

3.3. Yu cu ca dd chun C
Tr vi mi trng Dng bt mn c th cn chnh xc ti 0,1 - 1mg Phn t lng ln gim sai s khi cn
GV: Trn T Phng Tho HBK 64

IV. CC GIAI ON CA MT PHNG PHP PHN TCH


1. Giai on chn mu 2. Giai on chuyn mu thnh dd 3. Chn phng php thch hp v thc hin phn ng 4. Kim chng kt qu v x l kt qu phn tch
GV: Trn T Phng Tho HBK 65

1. Giai on chn mu
Phi c tnh cht i din cho ton l hng. Chn mu ring: chn ngu nhin cc v tr (n v) khc nhau ca l hng. Chn mu ban u: chn i din cc v tr (n v) khc nhau ca mu ring mu chung. Chn mu trung bnh: mu chung nghin ry trn

GV: Trn T Phng Tho HBK

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1. Giai on chn mu
Mu trung bnh th nghim chia lm 3 phn: Ni giao hng gi Ni nhn hng gi Ni phn tch gi
GV: Trn T Phng Tho HBK 67

1. Giai on chn mu

Nu mu chung qu ln
GV: Trn T Phng Tho HBK 68

2. Giai on chuyn mu thnh dd


Khng lm mt v bn mu. Phng php t: ho tan trong dung mi thch hp. Phng php kh: nu khng c dung mi ho tan thch hp nung kh vi rn (kim chy) trong chn Pt hay Ni 5001000oC ho tan bng dung mi thch hp.
69

GV: Trn T Phng Tho HBK

3. Chn phng php thch hp v thc hin phn ng


Yu cu pp: nhy, chn lc, tc phn tch cao v cho kt qu gn kt qu thc. Thc hin phn ng vi thuc th thch hp theo iu kin xc nh. Quan st du hiu c trng xut hin nh tnh. o th tch, cn khi lng hp cht to ra nh lng.
GV: Trn T Phng Tho HBK 70

4. Kim chng kt qu v x l kt qu phn tch PTT: kim tra bng phn ng c hiu khc.
PTL: tnh ton theo d liu ghi nhn, biu din kt qu theo yu cu ca pp thng k.
GV: Trn T Phng Tho HBK 71

VD v cc giai on ca 1 PPPT
Yu cu: nh lng st trong mt mu vi. 1. Chun b mu th nghim: chn mu i din: mu TB th nghim. 2. Cn chnh xc m(g) mu ha tan bng acid thch hp lc mu nh mc thnh V(ml) 3. St trong dd l Fe3+: ty hm lng Fe3+ c th dng:
GV: Trn T Phng Tho HBK 72

VD v cc giai on ca 1 PPPT
Nu [Fe3+] > 10-3M: dng PP ha hc. PP phn tch khi lng PP phn tch th tch (chun oxy ha kh, chun to to phc vi EDTA) Nu hm lng st (III) qu b: Dng PP so mu (PP quang ph hp thu thy c). 4. Tnh kt qu theo yu cu v x l kt qu phn tch theo PPTK
GV: Trn T Phng Tho HBK

73

VD: e xac nh ham lng SiO2; Al2O3, Fe2O3, CaO, MgO; K2O va Na2O trong mot mau cao lanh, ngi ta can 0,3000 g mau, chuyen vao chen Ni va them vao 3g KOH. Nung chay hon hp noi tren nhiet o thch hp, lam nguoi va hoa tan khoi ran thu c bang acid HCl. ?. Phng phap (PP) a c s dung e hoa tan mau?

GV: Trn T Phng Tho HBK

74

C cn 2 ln, lc ta SiO2; nung; cn v xc nh hm lng ca n trong mu. Dung EDTA e chuan o Al3+, Ca2+, Mg2+ ieu kien thch hp. Dung 1,10- phenanthroline tao phc o cam vi ion Fe (dang Fe2+ ) roi em o quang va so sanh vi cac dung dch cha Fe2+ a biet trc nong o. o cng pht x ca nguyn t K v Na trong mu ri so snh vi chun bit hm lng.
GV: Trn T Phng Tho HBK 75

??. Ten goi cua PP a c s dung e nh lng SiO2; Al2O3, Fe2O3, CaO, MgO; K2O va Na2O. Theo bn cht phng php Theo k thut phn tch Theo hm lng cht kho st (nu bit rng mu cha 55,19%SiO2; 24,4%Al2O3, 6,5%Fe2O3, 0,51%CaO, 1,07%MgO; 3,2%K2O & 0,10%Na2O).
GV: Trn T Phng Tho HBK 76

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