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CHNG 6

PHNG PHP PHN TCH KHI LNG


GV: Trn T Phng Tho HBK 1

NI DUNG CHNH (2LT+1BT)


I. NGUYN TC II. CC GIAI ON CA PPKL TO TA III. NG DNG
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I. NGUYN TC
PPPTKL thuc nhm phng php phn tch ha hc. nh lng cu t X da trn php o khi lng.
GV: Trn T Phng Tho HBK

Phn bit PPHH v PPPT dng c


Ch tiu so snh Lng mu Tnh chn lc Thi gian chnh xc Dng c Ngi phn tch
GV: Trn T Phng Tho HBK 4

Phng php ha hc

Phng php dng c

I. NGUYN TC
u im: C chnh xc cao (0,01%), c dng lm phng php trng ti. n gin v nguyn tc, dng c phn tch thng thng p dng nhiu i tng, gii hn hm lng rng. ng v lp li tt (nu cn thn)
GV: Trn T Phng Tho HBK 5

I. NGUYN TC
Nhc im: Tn km thi gian (4-12-24 gi) do phi tri qua nhiu giai on. Thao tc phc tp. Phi c cn phn tch (chnh xc n 0,1mg) Hn ch s dng trong thc t.
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GV: Trn T Phng Tho HBK

I. NGUYN TC
SAI S TRONG PPPTKL: Sai s h thng: Sai s ngu nhin:

GV: Trn T Phng Tho HBK

I. NGUYN TC
Phn tch khi lng c th tin hnh nhiu phng php: 1. Phng php trc tip 2. Phng php gin tip 3. Phng php kt ta
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GV: Trn T Phng Tho HBK

1. Phng php trc tip


X c tch khi mu di dng n cht, hp cht bn, t tan, em cn. AX A + X (cn X) mX(g) mmu(g)

GV: Trn T Phng Tho HBK

1. Phng php trc tip

GV: Trn T Phng Tho HBK

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1. Phng php trc tip

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2. Phng php gin tip


X c tch khi mu di dng hp cht d bay hi. Cn mu trc v sau khi phn tch. AX mmu(g) + mcn li(g) A X

khi lng = mX
GV: Trn T Phng Tho HBK 12

2. Phng php gin tip

GV: Trn T Phng Tho HBK

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3. Phng php kt ta Ha tan mu chuyn X thnh ion trong dung dch. AX X + + Ammu(g) Dng thuc th C kt ta v tch X di dng hp cht t tan CX. C- + X+ CX mCX(g) Tch v em cn CX.

GV: Trn T Phng Tho HBK

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3. Phng php kt ta Phng php ny ng vai tr quan trng, s dng rng ri trong thc t. V d:

GV: Trn T Phng Tho HBK

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II. CC GIAI ON CA PPKL KT TA Giai on chun b: (bt buc) Chn mu i din. Cn lng mu thch hp sao cho nhn c lng cn thch hp ca sn phm sau khi nung l:
Ta tinh th: 0,200 0,500g Ta v nh hnh: 0,10 0,300g

Chuyn mu thnh dung dch phn tch: ph mu bng nc ct, axit, baz,
GV: Trn T Phng Tho HBK 16

II. CC GIAI ON CA PPKL KT TA

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II. CC GIAI ON CA PPKL KT TA

Cc giai on phn tch: 1. Chn thuc th C thch hp, to ta cu t di dng hp cht bn. 2. Lc, ra ta. 3. Chuyn dng ta sang dng cn. 4. Cn sn phm. 5. Tnh ton kt qu theo yu cu.
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GV: Trn T Phng Tho HBK

1. To ta
1.1. Yu cu i vi thuc th C 1.2. Yu cu ca dng ta, dng cn 1.3. iu kin to ta thch hp 1.3.1. nh hng ca dng ta 1.3.2. Cc nh hng khc
GV: Trn T Phng Tho HBK 19

1.1. Yu cu chn thuc th C


C tch chn lc cao: ch tc dng vi cu t kho st. Ta to thnh c tan cng nh cng tt.

GV: Trn T Phng Tho HBK

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1.1. Yu cu chn thuc th C Dng tha thuc th 10 30% phn ng hon ton, dng d 2 3 ln nu thuc th bay hi. Tuy dng tha nhng thuc th phi c loi b d dng khi lc, ra, nung, v khng b hp ph ln ta chnh.
GV: Trn T Phng Tho HBK 21

1.1. Yu cu chn thuc th C VD: Dng tha H2SO4 lm gim tan ca ta BaSO4 (TBaSO4 = 10-9,97)

GV: Trn T Phng Tho HBK

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1.1. Yu cu chn thuc th C


Lu cc trng hp nu d thuc th c th lm tan ta ( to phc tan).

GV: Trn T Phng Tho HBK

Thuc th c kh nng to thnh dng cn c hm lng X cng nh cng tt (h s chuyn nh) gim sai s do cn.
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1.1. Yu cu chn thuc th C

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1.2. Yu cu ca dng ta, dng cn V d: dng ta BaSO4 Al(OH)3 Fe(OH)3 MgNH4PO4,


GV: Trn T Phng Tho HBK

dng cn
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1.2. Yu cu ca dng ta, dng cn


Dng ta L dng hp cht t tan c c ngay khi cho thuc th vo (CX). C cng thc phn t xc nh, chuyn sang dng cn d dng. Bn, t tan, ta phi c tinh th ln (cng to cng tt) t tan, d lc ra v gim b mt hp th cht bn. Ta c tinh khit cao, t hp ph hay nhim bn.
GV: Trn T Phng Tho HBK 26

1.2. Yu cu ca dng ta, dng cn Dng cn L dng trc tip c cn khi phn tch xong. Dng cn phi c s tng ng gia thnh phn v cng thc ha hc xc nh bn, khng b hp ph kh, m, khng b oxy ha hay phn hy bi nhit
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GV: Trn T Phng Tho HBK

1.3. iu kin to ta thch hp 1.3.1. nh hng ca dng ta: Khi cho C + X n mt lc no . [C].[X] TCX dung dch qu bo ha, ta CX xut hin.
GV: Trn T Phng Tho HBK 28

1.3. iu kin to ta thch hp


Giai on u (To mm kt tinh): to nn khong 4 phn t nn kch thc rt nh trung tm cation v anion kt ta ln b mt. Giai on tip theo: mm pht trin thnh ht ta c hnh dng xc nh theo mng li tinh th 3 chiu kt ta tinh th.
GV: Trn T Phng Tho HBK 29

1.3. iu kin to ta thch hp


S lng mm sinh ra + kt ta ht to, nh ph thuc qu bo ha ca dung dch.

Q S qu bo ha (QBH) = S

Q: nng ca cc thuc th sau khi trn vo nhau (mol/lit). S: ha tan ta sau khi cn bng (mol/lit).
GV: Trn T Phng Tho HBK 30

1.3. iu kin to ta thch hp


Nu qu bo ha rt b to mm chm t mm vt cht tp trung kt ta trn b mt ht mm c sn ht to (do lng anion v lng cation trong mt dung dch l hng s) ion sp xp trn mng li tinh th ta c hnh dng xc nh tinh th. tan S ca ta rt ln th s to ta tinh th.
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GV: Trn T Phng Tho HBK

1.3. iu kin to ta thch hp


Nu qu bo ha rt ln to mm nhanh s mm nhiu khng pht trin thnh ht to rn chc m ch lin kt vi nhau bng lc yu cc ht sp xp hn n khng nh hng ta v nh hnh S rt nh qu bo ha rt ln ta v nh hnh
GV: Trn T Phng Tho HBK 32

1.3. iu kin to ta thch hp


Ngoi ra, nu qu bo ha rt ln to dung dch keo, cha ht rt nh v mang in tch cng du khng lng c bng cch ly tm, lt qua giy lc d (do kch thc ht rt nh so vi kch thc l xp giy lc). ph keo bng cch thm dung dch in ly v gia nhit.
GV: Trn T Phng Tho HBK 33

1.3. iu kin to ta thch hp


Trong thc t, ngoi bn cht ca kt ta, dng ta l tinh th hay v nh hnh ph thuc nhiu vo qu trnh to ta. V d: BaSO4 vi dung mi nc: ta tinh th BaSO4 vi dung mi nc etanol (30 60%) ta v nh hnh.
GV: Trn T Phng Tho HBK 34

KT TA DNG TINH TH
GV: Trn T Phng Tho HBK 35

Yu cu c ta tinh th ht to
qu bo ha gim S tng v Q gim. Tin hnh ta pH thp: iu kin ny ta tan nhiu nhng mm nh tan mm ln ln ln.

GV: Trn T Phng Tho HBK

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Yu cu c ta tinh th ht to
Tin hnh to ta t dung dch long, nng, rt t t, khuy u trnh bo ha cc b. Long trnh to nhiu mm kt tinh Nng nhng mm nh tan ra, bi p cho nhng mm ln ln ln v gim hp ph ion l gy bn kt ta, trnh ta dng keo.
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GV: Trn T Phng Tho HBK

Yu cu c ta tinh th ht to
Sau khi to ta xong: a v pH thch hp ta c tan S min yn t 20 30 pht hoc 1 6 gi lm mui ta (to cho ta ln ln) nhit cao, nhng trnh dung dch si (v nhit cao qu ta s tng tan). Giai on ny: tinh th nh tan ra tinh th ta ln ln ln.

GV: Trn T Phng Tho HBK

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Yu cu c ta tinh th ht to
Tuy nhin, ty tng trng hp m thi gian lm mui ta khc nhau, nu thi gian qu di cng kt hu ta. Nu cu t chnh qu lu trong dung dch cc cu t ph ta theo gim bng cch lc, ra ta ngay. VD: Zn2+ (s ta vi S- thnh ZnS) theo cc ta CuS, HgS
GV: Trn T Phng Tho HBK 39

Yu cu c ta tinh th ht to
Gim qu bo ha dd bng cch dng phng php kt ta ng th to thuc th t t trong dung dch qua ha cht trung gian thay v cho thuc th trc tip vo dung dch. V d: kt ta hydroxid kim loi khng tan (NH2)2CO + H2O 2NH3 + CO2
GV: Trn T Phng Tho HBK 40

Yu cu c ta tinh th ht to
u im ca PP kt ta ng th: To qu bo ha thp. Gip cu trc mng ca tinh th hon chnh hn.
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KT TA V NH HNH
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Nu thu c ta dng v nh hnh Lu :


Dung dch (C + X) m c, nng gim hp ph, ta xp, d lng. Thm nhanh C vo X, khuy u, ngn bm bn. Sau khi to ta thm ngay dung dch cht in ly mnh ph v lp in tch kp trn nhng ht keo ta d ng t.
GV: Trn T Phng Tho HBK 43

Nu thu c ta dng v nh hnh


Thm vo mt lng nc nng gim nng cu t l trong dung dch, tch ta khi dung dch. Lc ngay trnh phn ng ph nu ta tan nhit cao lm ngui nc lc.

GV: Trn T Phng Tho HBK

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Nguyn nhn lm bn ta
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Nguyn nhn lm bn ta
Trong qu trnh to ta: c xy ra s cng kt (mt s cht c mt trong dung dch cng ta theo) lm bn ta. C nhiu loi cng kt. a. Hp ph b mt b. Ni cng kt c. Cng kt hu ta
GV: Trn T Phng Tho HBK 46

Nguyn nhn lm bn ta
a/ Hp ph b mt: c tnh chn lc (u tin ion to ta chnh hay ion to ta khc cng bn knh ion to ta chnh). Loi bng cch: To ta tinh th to, gim Sbm. Nhit cao tng gii hp. Pha long dung dch, gim nng tp cht. Ra nhanh ta sau lc bng dung dch thch hp.
GV: Trn T Phng Tho HBK 47

Nguyn nhn lm bn ta
b/ Ni cng kt: l hin tng gy bn trong ht ta. Gm cc dng: Cng kt ng hnh: v tr ca C v X b thay i bng nhng ion c cng in tch, bn knh gn bng nhau khc phc: tin hnh ta li. Cng kt do to thnh hp cht ha hc.
GV: Trn T Phng Tho HBK 48

Nguyn nhn lm bn ta
Cng kt do to ta ph t mm tinh th ca ta chnh chuyn ion nh hng sang dng khc (dng phc hay ion c in tch khc). Cng kt do s hp lu: ta gi bn trong l bn, khi n ln ln tp tp trung vo khuyt tt tinh th ca ta phn b khng u.
GV: Trn T Phng Tho HBK 49

Nguyn nhn lm bn ta
VD: Nu cho Ba2+ kt ta nhanh Fe3+ cha b tch ra ht c ion l nm trong ta. C nh th ta ln dn ln. Gim bng cch: + To ta t dung dch long. + Rt thuc th t t. + Khuy u. + Kt ta trong mi trng ng th.
GV: Trn T Phng Tho HBK 50

Nguyn nhn lm bn ta
c/ Cng kt hu ta: Nu cu t chnh qu lu trong dung dch cc cu t ph ta theo gim bng cch lc, ra ta ngay. VD: Zn2+ (s ta vi S- thnh ZnS) theo cc ta CuS, HgS
GV: Trn T Phng Tho HBK

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1.3.2. Cc nh hng khc


Khi dung dch c mt nhiu ion l tan ca ta tng ln do: Ion l tham gia cn bng ph vi C, X hoc CX.

C + Z1
GV: Trn T Phng Tho HBK

X + Z2
spp2

CX + Z3
spp3
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spp1

1.3.2. Cc nh hng khc


S hin din ca nhiu ion lm tng lc ion trong dung dch dn n h s hot ca cc ion gim, lm S ta tng.
AB An+ S
+

BnS

TAB = [An+].[Bn-].fA.fB = S2

GV: Trn T Phng Tho HBK

TAB S= fA .fB

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1.3.2. Cc nh hng khc


Tng nng thuc th:

CX

TCX = [C+].[X-] = const [C+] tng [X-] gim: SCX gim


GV: Trn T Phng Tho HBK 54

1.3.2. Cc nh hng khc


Tuy nhin, [C+] tng s: Tng lng ion trong dung dch dn n tng S ta (tng lc ion). To phc vi ion ta lm tan ca ta tng ln. [C+] thm vo phi khng ch 10 50% d, khng ty tin.
GV: Trn T Phng Tho HBK 55

1.3.2. Cc nh hng khc


Cc ta phn cc d tan trong dung mi phn cc do i vi ta v c ha tan hon ton trong nc th gim tan bng cch thm ru etylic vo. tan t l nghch vi bn knh ht ta, ta cng mn cng tan nhiu do Stx b mt ln. Nhit tng lm ta tan nhiu hn (do phn ln qu trnh ha tan l thu nhit).
GV: Trn T Phng Tho HBK 56

LC V RA TA
GV: Trn T Phng Tho HBK 57

2. Lc v ra ta
2.1. Cc loi giy lc: PPKL s dng giy lc khng tro (lng tro rt nh): thnh phn giy ch yu l cellulose (rt t ph gia) - l xp mn: (bng xanh). - l xp trung bnh: (bng vng). - l xp ln: (bng ). Chn la sao cho ta khng chui qua l giy lc ng thi thi gian lc khng qu lu.
GV: Trn T Phng Tho HBK 58

2. Lc v ra ta
Nung ta nhit cao hn 2500C: dng phu thy tinh v giy lc. V nhit ny chy ht giy lc. Nu ta b kh (khng bn) nhit ln hn 2500C: dng phu thy tinh c hoc chung lc Gooch.
GV: Trn T Phng Tho HBK 59

2. Lc v ra ta
mn ca lp thy tinh c ph thuc kch thc ta. C 4 c phu: 1 (100 120m) 2 (40 - 50m) 3 (20 25m) 4 (< 10m)
GV: Trn T Phng Tho HBK 60

2. Lc v ra ta
2.2. Ra ta: Ra ta trong becher, ch gn phn nc trong qua giy lc. Khi no ta sch mi chuyn ht sang giy lc trnh rch giy Nn ra nhiu ln, mi ln t nc trnh tan ta. Dung dch ra nng (tng gii hp). Ch nhit cao s lm tng tan ca ta.
GV: Trn T Phng Tho HBK 61

2. Lc v ra ta
Cha ion chung so vi ta chnh (trnh tan ta). Cha lng nh axit hoc baz gim thu phn. Cha cht in ly gim hin tng peptit. (ta v nh hnh to dng keo sau khi ng t). Ch : cc cht v ion thm vo d tng khi lng khi nung, cn hn ch trnh sai khi lng ta.
GV: Trn T Phng Tho HBK 62

CHUYN DNG TA SANG DNG CN


GV: Trn T Phng Tho HBK 63

3. Chuyn dng ta sang dng cn (nung)


t chy ht giy lc bn ngoi trc khi chuyn vo l nung. Dng ta c sy, nung s chuyn thnh dng cn: loi nc hp ph + kt tinh. Chuyn dng ta hn hp sang dng cn c cng thc phn t xc nh v ng nht.
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GV: Trn T Phng Tho HBK

3. Chuyn dng ta sang dng cn (nung) Thi gian sy hoc nung: ti khi dng cn c khi lng khng i. Sau khi sy, nung cn ngui trong bnh ht m ri cn.
GV: Trn T Phng Tho HBK 65

3. Chuyn dng ta sang dng cn (nung) CuSO4.5H2O: < 2000C BaSO4 BaSO4: 700 8000C Fe(OH)3 Fe2O3: 9000C Al(OH)3 Al2O3: 1000 - 11000C CaC2O4 CaCO3 (6000C) CaO (1000 12000C)
GV: Trn T Phng Tho HBK 66

4. Cn
Dng cn phn tch (chnh xc 0,0001g) B: m0 (g) B + ta: m1 (g) khi lng ta mta(g) = m1 m0
GV: Trn T Phng Tho HBK 67

5. Tnh ton kt qu
5.1. Mu dng rn 5.2. Mu dng lng (C(g/l)

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
(thng tnh hm lng X%): a(g) mu PPKL m(g) kt ta dng cn A

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
VD: Xc nh hm lng st trong mu qung bng PPPTKL: Cn 0,3568g mu, ha tan v to ta vi OH-, lc v nung ta, cui cng thu c 0,1234g Fe2O3. Tnh %FeO v %Fe3O4 trong mu.
GV: Trn T Phng Tho HBK 70

5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
VD: Mt mu ch cha MgCO3 v SiO2 cn nng 0,500g c nung ui CO2. Lng mu cn li sau khi nung cn nng 0,400g. Tnh %ca CO2; MgCO3; SiO2 trong mu ban u

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn

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5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
VD: Mt mu qung cn nng 1,7890g c sy n khi lng khng i l 1,7180g. Cn 0,3980g mu qung ban u, ha tan v to ta, thu c 1,0780g BaSO4. Tnh %S trong mu ban u v mu sy kh.
GV: Trn T Phng Tho HBK 76

5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
a(g) mu V(ml) DD 1 VX(ml) dd 1 m(g) A (dng cn)

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
VD: xc nh hm lng NiSO4 v nc kt tnh trong mu NiSO4.xH2O dng PPPTKL: cn 2,7160g mu, ha tan thnh 100ml DD1; ly 20ml DD1 to ta bng DD Ba2+. Khi lng ta thu c 0,4511g. Tnh x v % NiSO4.
GV: Trn T Phng Tho HBK 80

5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
VD: Ha tan 4,090g hn hp ch gm CaCl2 v KCl thnh 1 lt DD. Lm kt ta ht ion Cl- c trong 50ml DD trn bng AgNO3 thu c 0,4230g AgCl. Tnh % CaCl2 v KCl trong mu.

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn
Gi a, b l s mol CaCl2 v KCl trong mu.

GV: Trn T Phng Tho HBK

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5.1. Mu dng rn

GV: Trn T Phng Tho HBK

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5.2. Mu dng lng (C(g/l)


VX(ml) mu PPKL m(g) A (dng cn)

GV: Trn T Phng Tho HBK

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5.2. Mu dng lng (C(g/l)


VD: nh lng ion Ba2+ trong DD bng PPPTKL: ht 5,00ml DD mu, to ta vi acid sulfuric, thu c 0,3258g ta. Tnh nng Ba trong nc di cc dng: C(g/l) Ba2+ C(g/l) BaCl2
GV: Trn T Phng Tho HBK 87

5.2. Mu dng lng (C(g/l)

GV: Trn T Phng Tho HBK

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5.2. Mu dng lng (C(g/l)

GV: Trn T Phng Tho HBK

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5.2. Mu dng lng (C(g/l)


V(ml) dd mu pha long V1(ml) dd long VX(ml) dd long m(g) A (dng cn)

GV: Trn T Phng Tho HBK

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III. NG DNG
1. nh m - nc kt tinh 2. nh tro 3. Xc nh lng mt khi nung 4. nh lng bng cch to ta
GV: Trn T Phng Tho HBK 91

1. nh m - nc kt tinh
m sy 100 - 110oC Nc kt tinh 120 - 200oC

GV: Trn T Phng Tho HBK

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1. nh m - nc kt tinh
Sy chn to sy mu (cho n khi lng khng i) cn mo(g) Cho mu vo chn (1-10g) cn m1(g) Sy chn c mu cn m2(g)

GV: Trn T Phng Tho HBK

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2. nh tro (600-800oC)
S g cht v c c trong 100g mu. Phi lu nhng cu t d bay hi khi nung nh: P, As, Hg, Cd, Fe, S.

GV: Trn T Phng Tho HBK

m1 = mo + mmu m2 = mo + mtro
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3. Xc nh lng mt khi nung (600-800oC)


S g cht mt khi nung nhit trn trong 100 g mu

m1 = mo + mmu m2 = mo + mtro
GV: Trn T Phng Tho HBK 95

4. nh lng bng cch to ta


Thuc th v c Thuc th hu c To anion trong mi trng ng tng (p111-112)
GV: Trn T Phng Tho HBK 96