TRNG I HC CNG NGHIP TP.

HCM KHOA CNG NGH HA HC

TIU LUN MN:

PHN TCH CNG NGHIP

XC NH HCl V CLO T DO, Fe TRONG HCl TRONG CNG NGHIP

GVGD: Trn Nguyn An Sa SVTH: V Th Dng MSSV: 09168221 LP: 210408701

NI DUNG

2
.

Gii thiu chung v HCl k thut

.

Yu cu k thut

Phng php th

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1.Gii thiu chung v HCl k thut

1.1 Tiu chun
Thuc th TCVN 2298-78 C hiu lc t 1-7-1979

AXIT CLOHIDRIC
Reagents.

HCl: l dung dch ca hydro clorua trong nc.khng mu, trong sut, bc khi trong khng kh. Cng thc : HCl

2.1

Khi lng phn t : 36,46.

1.Gii thiu chung v HCl k thut

1.2 Quy nh chung Thuc th s dng phi c tinh khit cao. Nc ct dng phi ph hp vi TCVN 2117-77 ng so mu c kch thc bng nhau, khng mu, y phng, cng tnh cht quang hc v c nt mi. Dung dch so snh v dung dch th chun b trong cng iu kin.

Quy nh tiu chun

Khi so mu, Vth = Vso snh.

Dung dch so snh trong cc ng so mu quy c theo th t.

2. Yu cu k thut
2.1 iu kin dHCl=1,17-1,19 g/cm3 200C

2.2 Yu cu
Tn ch tiu TKHH 1.Dng bn ngoi 2. Hm lng hidro clorua ( HCl) tnh bng % 3.Hm lng cn sau khi nung tnh bng % khng c ln hn. 4. Hm lng axit sunfur, tnh bng %, khng c ln hn.. 5. Hm lng sunfat (SO4), tnh bng %, khng ln hn 6. Hm lng Clo t do ( Cl2 ) 7. Hm lng mui amoni ( NH4) tnh bng %,khng c ln hn 8.Hm lng st (Fe) tnh bng %, khng c ln hn 9 Hm lng kim loi nng tnh theo ch (Pb) tnh bng %, khng c ln hn mc 3.2 35-38 0,001 0,0005 0,0002 Mc 3.7 0,0003 0,00005 0,0001 35-38 0,002 0,001 0,0005 Mc 3.7 0,0006 0,0001 0,0002 35-38 0,005 0,001 0,001 Mc 3.7 0,0006 0,0005 0,0005

Mc
TKPH Tinh khit

3. Phng php th
Ly mu Xc nh hm lng hidro clorua ( HCl) trong mu HCl k thut Phn tch clo t do trong HCl cng nghip Hm lng st (Fe) trong cng nghip

3.1

3.2

3.3

4.4

3.1 Ly mu
Thuc th HCl da trn c s phn tch mu ly c tng l hng.

L hng l sn phm c cng ch tiu, cng loi bao gi, giao

nhn cng thi gian v c giy chng nhn cht lng. Ly mu theo cch chn ngu nhin n gin. Tin hnh ly mu vi1lng sao cho m(g)muTB >= 750 g.

Dng c ly mu phi kh, sch, ly mu nhng v tr tu

trong bao gi v khng nh hng n cht lng ca thuc

th. Cho php dng pipet c chnh xc n 1 %.

3.2 Xc nh hm lng HCl trong mu HCl thut

Chun HCl bng NaOH vi ch th MO, PP Ch th MO, im tng ng khi dung dch t cam vng cam.

Nguyn tc

Ch th PP, im tng ng khi dung dch sang mu hng nht.

Nc ct
Metyl , dung dch 0,1 % trong etanola Metyl da cam, dung dch 0,1 % trong nc

Dung dch v thuc th

Natri hydroxit, dung dch 1 N

Etanola, tinh ch, tinh khit cao

3.2 Xc nh hm lng HCl trong mu HCl k thut

3.2.1Tm tt quy trnh
2ml mu
20 ml nc

Cng thc tnh: (%)HCl= V x 0,00365 x 100/m

Lp li 3 ln

Dung dch
3 git MO

Chun bng NaOH

Kt qu c mu vng

Trong : V: th tch dung dch NaOH 1N tiu tn 1ml. 0,0365: lng acid HCl tng ng vi 1ml NaOH 1N, g.

3.2 Xc nh hm lng HCl trong mu HCl k thut

Cc ng dng ca phng php

Chun ha nng ca dung dch chun trong chun

acid bazo. L nhng acid bazo nguyn cht, bn, khng b phn hy khi bo qun, d tinh ch d kim tra tinh khit. Cc cht dng chun acid thng dng: borat,

natricacbonat...

3.3.Phn tch clo t do trong HCl cng nghip

Nguyn tc Chun iod to thnh khi cho dung dch KI vo dung dch mu bng Na2S2O3 vi ch th h tinh bt. im tng ng nhn c khi dung dch mt mu xanh. Dung dch v thuc th: Kali iotdua, dung dch 10%.

H3PO4 m c
Dung dich Na2S2O3 0.01N Iot, dung dch 0,01 N;

3.3.Phn tch clo t do trong HCl cng nghip

Tm tt quy trnh
20g mu
100ml nc H3PO4+ KI10%

Cng thc tnh

V V .C (%) Cl
1 2

Na 2 S 2O3

.D

Cl 2

1000

100 . m

Dung dch
Na2SO3 0.01N

Trong : V1: th tch dung dch Na2S2O3

Lp li 2 ln

Chun
5 git htb

0.01N tiu tn chun mu,ml

V2: th tch dung dch Na2S2O3 0.01N tiu tn chun trng, ml

Dung dch c mu xanh

3.3.Phn tch clo t do trong HCl cng nghip

3.3.1 3.3.2

Xc nh tng st vi thuc th 1-10 phenantrolin Phng php chun so mu sunfocianur Phng php so mu vi acid sulfosalicylic

3.3.3
4 5 3

3.3.1 Xc nh tng st vi thuc th 1-10 phenantrolin

Nguyn tc Ion Fe2+ pH = 29 to phc vi thuc th hu c 1-10 phenantrolin to phc mu , cng mu ca phc t

l vi nng ca ion st trong khong nng tuyn tnh

0,135ppm. Xy dng ng chun ca Fe2+.

Xc nh tng st bao gm Fe2+ v Fe3+ th kh Fe3+ v Fe2+

3.3.1 Xc nh tng st vi thuc th 1-10 phenantrolin Tin trnh

Lp th chun: Ly dung dch tiu chun Fe2+ 50 mg/l xy dng ng chun, thm vo mi bnh 5ml m axetat pH =5, 1ml hydroxylamin, 1ml dumg dch 1,10- phenantrolin. Dung dch so snh c tin hnh tng t nhng khng c st chun. * Chun b dung dch xc nh: Ly chnh xc 25ml mu th

vo 2 bnh nh mc, cho thm vo mi bnh 5ml m axetat pH

=5, ch cho 1ml hydroxylamin vo 1 bnh, 1ml dumg dch 1,10phenantrolin.

3.3.2 Phng php chun so mu sunfocianur

Nguyn tc Trong mi trng acid ion Fe3+ to phc vi ion SCN phc mu tm: Fe3+ + 3SCN- --> Fe(SCN)3 iu kin xc nh Thuc th SCN- ch hin mu trong mi trng acid vi Trong mu nc phi loi tr cc ion PO43-, F-. Mt s ng.

lng thuc th d thch hp.

cation nh ng, bitmut, coban cng nh hng n phn

3.3.2 Phng php chun so mu sunfocianur

Tin trnh
Lp th chun: Ly dung dch tiu chun Fe3+ 50 mg/l xy dng ng chun, cho thm vo mi bnh. ng dng ca phng php Vi mt ng chun cho php phn tch hng lot mu.

Dung dch cng khng i hi phi tun theo nh lut

Beer mt cch nghim ngt.

3.3.3 Phng php so mu vi acid sulfosalicylic

Nguyn tc Ion Fe3+ trong mu s to c cc phc c mu vi acid sulfosalicylic cc pH khc nhau. pH = 1,8 2,5 to phc mu tm . pH = 4 8 to phc mu cam. pH = 9 11 to phc mu vng. Khong nng tun theo nh lut Lamber Beer l 0,2 10ppm. Ta xc nh st III di dng phc mu vng o hp thu quang bc sng 410nm. em so mu vi dy chun, ta tnh c hm lng st. mg/lFe = * 100 a : l s mg Fe tnh c t ng chun.

3.3.3 Phng php so mu vi acid sulfosalicylic

iu kin xc nh Thuc th H2SSal hin mu vi Fe3+ v th mun quy hm lng st v st III ht th cn oxy ha Fe2+ v Fe3+ bng

H2O2.

Cn un si k dung dch vi pht.

Fe2+ + H2O2 --> Fe3+ + H2O Fe2+ + S2O82- --> Fe3+ + SO42- + SO2 + H2O

Cn cho thuc th H2SSal trc ri iu chnh mi trng

bng NH3.Sau khi hin mu 10 pht tin hnh o quang.

3.3.3 Phng php so mu vi acid sulfosalicylic

Tm tt quy trnh
25ml mu
Thn NH3

Chun b dy chun: tin hnh tng t nh mu thay mu bng dung dch chun.

Dung dch pH= 1,8-2,5

5 ml sulfo

Dung dch c mu tm
Thm d NH3

Dung dch c mu vng

o quang