Ni dung c bn: iu 2 3 3.1 3.2 3.3 4 4.1 4.2 4.3 4.4 4.5 4.6 5 6 6.2 6.3 7 8 9 10 11 12 13 14 15 15.1 15.

2 16 16.1 16.2 17 17.1 17.2 18 19 20 Ni dung Ti liu vin dn lin quan S lng cc php th v sai lch cho php Phn tch trng ti Cc phn tch mang tnh tham kho Yu cu k thut cho cc php th nhanh Yu cu chung Sai lch v gii hn Thit b, dng c Thuc th Chun b mu Tin hnh Bo co kt qu th nghim Cc phng php Cn khng tan (CKT) Silic dioxit (SiO2) Xi mng c hm lng CKT <1% Xi mng c hm lng CKT >1% Nhm kt ta bng NH4OH St (III) Photpho pentoxit (P2O5) Titan dioxit (TiO2) Km oxit (ZnO) Nhm oxit (Al2O3) Canxi oxit (CaO) Magie oxit (MgO) Sunfua (S2-) Sunfua trioxit (SO3) Sunfit (SO32-) Mt khi nung (MKN) Xi mng pooc lng Xi mng x v xi mng pooc lng x l cao Natri oxit v kali oxit (Na2O v K2O) Tng hm lng alkali Hm lng alkali ho tan trong nc Mangan dioxit (MnO) Clorua (Cl-) Cc hp cht hu c ho tan trong cloruaform Cc phng php khc thay th Canxi oxit (CaO) Carbon dioxit (CO2) Magi oxit (MgO) Mt khi nung (MKN)

21 22 23 24

24.1 25 26 27 28

Xi mng x v xi mng pooc lng x l cao Titan dioxit (TiO2) Photpho pentoxit (P2O5) Mangan dioxit (MnO) Canxi t do (CaO t do)

3- S lng cc php th v sai lch cho php 3.1 Phn tch trng ti (Refree Analyses): theo iu t 5-20 ca tiu chun Biu din kt qu bng phn trm (%), chnh xc n 0,01% . (Ring i vi ch tiu hp cht hu c ho tan trong cloruaform l biu din chnh xc n 0.001%). S dng mu chun c chng nhn CRM) kim tra tay ngh ca nhn vin th nghim v iu kin th nghim. Sai lch kt qu khng c ln hn quy nh ti bng 1 v 2. Nu ln hn phi tm hiu, phn tch nguyn nhn, tin hnh th nghim li. 3.2 3.3 Cc phn tch mang tnh tham kho (Optional Analyses) phi Yu cu ca cc php th nhanh: Tun th y cc yu c tho thun v nu r trong kt qu th nghim. cu k thut (thit b, ho cht, tay ngh, kim chng trn mu CRM...) 4- Yu cu chung Xc nh cc ch tiu c bn trong dung dch sau khi phn hu mu bng HCl hoc nung chy bng hn hp nung chy. Ghi r cc thao tc khc vi tiu chun quy nh. Mt s lu khi xc nh tng hm lng sunfua. Sai lch v gii hn : Sai lch cho php khi cn phn tch lp li l 0.0002 g, chnh xc 0.0002 g; phn gii (cn hin th s) khng vt qu 0.0001 g. i vi cn n, nhy ti a l 0.0003g 4.2 Thit b, dng c: Yu cu v dng c thu tinh trong PTN; bnh ht m, giy lc cc loi, chn s, chn nung, l nung 4.3 Ho cht, thuc th, 4.3.1 Mc tinh khit ca ho cht 4.3.2 Ho cht thuc th tng ng khc 4.3.3 4.3.4 4.3.5 4.3.6 Ho cht m c Ho cht v k hiu ho cht pha long bng nc Dung dch tiu chun Dung dch khng tiu chun. 4.1

4.3.7 Dung dch ch th

4.3.7.1 Metyl : pha 2g/1000ml C2H5OH 95% 4.3.7.2 Phenolphtalein: pha 1g/1000ml C2H5OH 95% 4.4 Chun b mu : sng mu qua sng 850 m, loi b phn trn sng; rt gn mu n khi lng khng t hn 50 g theo phng php chia t (nu th nghim ch tiu alkali ho tan trong nc th khi lng mu ly khng t hn 100g); nghin nh mu n khi ton b mu lt qua sng 150 m; ng nht mu; sy mu, lm ngui trong bnh ht m, bo qun trong bnh kn lu mu. Bng 3 quy nh v s ch s lm trn trong kt qu th nghim. 4.5 Cc thao tc lin quan 0.0001g 4.5.2 Cn khi lng v cn chn: trong cng iu kin v nhit , m. 4.5.3 Khi lng khng i ca phn sau nung: nung kt ta theo quy nh, lm ngui trong bnh ht m n nhit phng v cn, ghi li khi lng. Tip tc nung chn 30 pht trong l nung ln na, ly ra, lm ngui trong bnh ht m, cn. Kh lng dng cn c coi l khng i nu sai khc gia 2 ln nung, cn khng vt qu 0.2mg. 4.5.4 Lm bay hi trong ch bch kim: Vi cc qu trnh lm bay hi trong chn bch kim c coi l trit khi cng vi mt dng chn c lm sch nu sau khi nung, lng cn trong chn khng vt qu 0.2mg so vi th nghim trng. 4.5.5 Tinh ton 4.5.6 Lm trn s 4.6 Cc ch tiu yu cu phn tch: Cc thnh phn Cc thnh phn hm lng Cc php xc nh nh Na2O K2O TiO2 P2O5 ZnO Mn2O3 Sunfua sunfit khc Cn khng tan CaO t do CO2 Alkali ho tan trong nc Hp cht hu c ho tan trong cloruaform c bn SiO2 Al2O3 Fe2O3 CaO MgO SO3 MKN 4.5.1 Cn: chnh xc trn cn phn tch c nhy n

5. Cc phng php th

5.1 Cn khng tan 5.1.1.Nguyn tc : x l mu bng axit HCl, lc, tip tc x l bng NaOH. Phn cn cn li em nung, cn. 5.1.2 Vi xi mng pha, khi x l bng HCl, phn clanke xi mng c coi l ho tan trit . X dng NH4NO3 ra kt ta 5.2 Thuc th: 5.2.1 NH4NO3 dung dch 20g/l 5.2.2 NaOH dung dch 10g/l 5.3 Tin hnh th: 5.3.1 Cn 1 g mu. Thm 25 ml nc ct, thm tip 5 ml HCl c, dng a thu tinh dm nt cc kt ta. Thm tip nc ct nng n th tch V=50ml. t cc ln bp, un gn si khong 15 min. Lc qua giy lc chy trung bnh, phn nc lc hng vo cc dung tch 400ml xc nh sunfat. Ra sch cc v giy lc bng nc ct nng. Chuyn giy lc c cha kt ta tr li cc c. Thm tip 100ml dung dch NaOH 1% (10g/l) c un nng (n gn si) v un cc c cha giy lc v kt ta khong 15 min di nhit si. Khu dm nt giy lc. Axit ho dung dch thu c bng HCl, s dng metyl lm ch th, thm d khong 4 n 5 git na. Lc qua giy lc chy trung bnh v ra phn cn, cc t nht 14 ln bng dung dch NH4NO3 (20g/l) nng. Chuyn giy lc c cha kt ta vo chn bch kim, nung nhit 90010000C, lm ngui trong bnh ht m v cn 5.3.2 Lm mu trng so snh 5.4 Tnh ton S : Mu +25ml H2O +5ml HCl +50ml H2O/t0C

Nc lc

Cn

Xc nh sunfat - H2O nng

Ra bng : -100ml NaOH 1%

- Axit ho bng HCl / ch th metyl - NH4NO3 2% nng

Nung cn nh lng

6. Xc nh SiO2 6.1 La chn phng php Nu hm lng CKT lm theo iu 5 nh hn 1%, thc hin theo iu 6.2. Nu hm lng CKT lm theo iu 5 ln hn 1%, thc hin theo iu 6.3 6.2 SiO2 trong xi mng pooc lng c hm lng CKT nh Tin hnh: cn 0,5g mu vo cc dung tch 50 ml, thm tip 0,5g NH 4Cl, trn u, y mt knh ng h v thm tip 5ml HCl m c. B mt knh ng h v thm vo 1-2git HNO3, dng a thu tinh khuy u hn hp. y mt knh li v t cc ln cch thu khong 30min. trong sut qu trnh ny cn khu k dung dch v dm tan phn cn phn hu hon ton xi mng. Chuyn ton b hn hp ln phu lc (trnh pha long). Ra cc v phu lc bng HCl (1+99), sau rar tip khong 10-12 ln bng nc nng. 6.2.3.2 Chuyn giy lc c cha kt ta vo chn bch kim, x l HF xc nh hm lng SiO2, phn cn cn li c cha 1 phn Fe2O3 v Al2O3 6.2.3.3 Nu phn cn sau khi x l bng HF vt qu 0.0020g, php xc nh SiO2 phi tin hnh phn tch li. 6.2.3.4 Nu khi tin hnh phn tch li, hm lng cn sau khi x l HF vn ln hn 0.0020g, c ngha l hoc xi mng b nhim bn hoc khng c kt luyn hon to trong qu trnh ch to. Khi , tuyt i khng nung phn cn cn li sau x l HF bng K2S2O7. Ghi li khi lng cn sau khi x l HF 6.2.3.5 Vi cc mu xi mng khng phi l xi mng pooclang, thng thng lng cn sau khi x l HF bao gi cng ln hn 0.0020g, cn thm vo khong 0.5g Na2S2O7 hoc K2S2O7 vo chn bch kim, nung n khi phn cn cn li tan trong v ho tan khi chy bng nc v gp vi phn nc lc ra tch loi SiO2 xc nh nhm b kt ta bi amonihydroxit. 6.2.3.6 Tin hnh th mu trng 6.2.4 Tnh ton 6.3 SiO2 trong xi mng pooc lng c cn khng tan ln hn 1%. 6.3.1 X l mu bng cch nung vi hn hp nng chy ri tch loi SiO2 bng lc, ra, x l HF. 6.3.2 Tin hnh: 6.3.2.1 Cn lng mu tng ng vi mu c loi b mt khi nung, theo cng thc: W = [0.5(100 I)]/100 trong : W l khi lng ca phn mu qua nung, tnh bng gam I l lng mt khi nung, tnh bng %.

Trn u Na2CO3 v phn mu cn. Lt y chn bch kim dung tch 20-30ml mt lp mng Na2CO3 v chuyn nh lng hn hp mu Na2CO3 vo chn, ph ln trn mt lng Na2CO3 na, nung chn nhit 11000C trong khong thi gian 45 min. Ly ra, lc trn v ngui. Chuyn chn c cha khi nung chy vo bt c mu, dung tch 300ml, c cha sn khong 100ml nc nng. un nh bt c ho tan khi chy. Dng HCl (1+3) ra sch chn v thnh bt, ly chn ra. Thm tip 20ml HCl m c, y mt knh ng h ln bt c 6.3.2.2 C mu trn bp cch thu n khi kh kit ( gim bt thi gian c, c th thm vo 1 t gelatin). Nhc bt c ra khi bp, thm tip 5-10 ml HCl c, yn khong 2min, thm nc. y mt knh ng h v un nng khong 10min. Thm nc ln na v lc ra kt ta (s dng giy lc bng trung), ra bng HCl (1+99) nng v nc nng. Gi li kt ta. 6.3.2.3 Lm bay hi phn nc lc ra n kh kit, c kh thm na nhit 105-1100C khong 1h na. Lm ngui, thm 10-15 ml HCl (1+1), un nng10 min. Thm nc, lc ra tch loi lng nh SiO2 b ho tan. Gp kt ta vi kt ta thu c ti iu 6.3.2.2 v nung. Phn nc lc ra gi li xc nh nhm b kt ta bi NH4OH. theo iu 7.1-7.3 6.3.2.4 Xc nh SiO2 theo nh iu 6.2.3.2 S 1: Mu

CKT>1% Nung mu vi Na2CO3

CKT>1% X l bng HCl (+NH4Cl; HNO3)

Ho tan khi chy, c tch SiO2

Lc, ra

Nc lc A

Cn X l HF

Nung Phn cn Phn bay hi

Nung K2S2O7

X %SiO2

Ho tan khi chy

7 . Nhm kt ta bi NH4OH 7.1 Nguyn tc: t dung dch tch loi SiO2, kt ta Al3+; Fe3+; Ti4+; v cc hp cht ca photpho bng NH4OH. Nung cc kt ta v nh lng cc oxit. 7.2 Tin hnh 7.2.1 T phn nc lc ra (6.2.3.1) ly 200ml dung dch, c th thm 1015 ml HCl c. Thm tip vi git metyl , un nh n si. Thm tng git NH4OH (1+1)cho n khi dung dch chuyn sang vng. Cho d thm 1 git na. un n si v si thm 50-60s. Lc, ra kt ta bng giy lc chy trung bnh, s dng dung dch NH4NO3 (20g/l) khong 2-4 ln. 7.2.2 Ho tan kt ta ra cc ban u bng HCl (1+2). Ra sch phu (nc ra khong 100ml). Lp li thao tc kt ta bng NH4OH. 7.2.3 Chuyn kt ta vo chn bch kim, t ri nung nhit 105011000C. Lm ngui v cn. 7.2.4 Mu trng 7.3 Tnh ton 8. St (III) oxit 8.1 Nguyn tc: Kh Fe3+ bng SnCl2. Chun oxi ho kh bng K2Cr2O7 8.2 Thuc th: 8.2.1 Bari Diphenylamin Sunfonat : 0.3% pha trong nc. 8.2.2 K2Cr2O7 chun 8.2.3 SnCl2: Ho tan 5 g SnCl.2H2O vo 10ml HCl , thm nc n th tch 100ml. un n tan trong. 8.3 Tin hnh i vi loi xi mng khng phi l xi mng pooc lng, hoc cha r v hm lng CKT, cn tin hnh xc nh CKT trc ri mi xc nh theo cc iu 8.3.1. hoc 8.3.2 di y. 8.3.1 Vi mu c hm lng CKT <1%, cn 1g mu vo cc dung tch 500ml. Thm 40ml nc, khu k, thm 40ml HCl c. Sau tin hnh theo 8.3.3 8.3.2 Vi mu c hm lng CKT>1%, cn 0.5g mu, trn u vi 1g LiBO2 v chuyn vo chn c lm sch ht carbon v lt y 0.1g LiBO2. Ph ln trn khong 0.1g LiBO2 na. Nung chn nhit 11000C khong 15min. Ly chn ra v quan st xem mu c phn hu ho ton cha, nu cha phn hu, nung thm 30 min na. Nu s phn hu vn cha hon ton, tin hnh nung li vi lng mu cn l 0.25g. Ly khi nung ra bng 10 ml HCl m c v 50ml nc. Ra sch chn, un khong 10min, khuy ho tan khi chy. Tip tc tn hnh theo 8.3.3.

8.3.3 un nng dung dch n si. Thm tng git SnCl 2 n khi dung dch mt mu. Thm d 1 git na v lm ngui nhanh n nhit phng bng cch thm nc ngui. thm tip 10ml HgCl. Khuy k dung dch khong 1min. Thm tip 10ml H3PO4 (1+1) v git ch th bari diphenylamin sunfonat. Thm nc n th tch khong 75- 100ml. Chun bng K2Cr2O7 tiu chun 8.3.4 Mu trng 8.4 Tnh ton theo cng thc v lm trn s theo quy nh ti bng 3

9. P2O5 Photpho pentoxit 9.1 Nguyn tc: so mu 9.2 Thit b: 9.2.1 My so mu 9.2.1.1 n 9.2.4: yu cu k thut ca thit b: - Lm vic ti bc sng 725nm - chnh xc o bc sng hot ng : 1nm hoc thp hn - Di hp th t 0.1 n 1.0, hin th v hp th 1% hoc thp hn - Cch o mu tun th theo cc iu 9.4.1 n 9.4.9 9.3 Thuc th 9.3.1 Amoni molipdat: Ly vo cc dung tch 1l khong 500ml H2SO4 10.6N (9.3.7). Ho tan 25g Amoni molipdat (NH4)6Mo2O24.4H2O vo khong 250ml nc m v chuyn vo cc dung tch 1l c cha H2SO4. Khu k. ngui v pha long bng nc n th tch 1l, bo qun trong chai thu tinh. 9.3.2 Axit ascobic: s dng dng bt mn ho tan. 9.3.3 HCl tiu chun, nng 6.5 0.1N: pha long 540ml HCl m c bng nc n th tch 1l. chun ho li bng dung dch chun NaOH (9.3.6) mi ln s dng. 9.3.4 Dung dch photphat tiu chun A: Ho tan 0.1917 KH2PO4 khan nc v nh mc thnh 1 lt 9.3.5 Dung dch photphat tiu chun B: Ly 50ml dung dch A v chuyn vo bnh nh mc dung tch 500ml, thm nc ti vch, lc u 9.3.6 Dung dch NaOH tiu chun 1N 9.3.7 Dung dch H2SO4 tiu chun (10.6 0.1)N: ho tan 300ml H2SO4 trong 600ml nc ct, lm ngui, nh mc thnh 1lit. Chun ho nng bng NaOH trc khi s dng. 9.4 Tin hnh 9.4.1 Chun b cc dung dch c hm lng P2O5 t 0 n 0.5%: Thm vo cc bnh nh mc dung tch 250ml ln lt cc th tch dung dch phot phat tiu chun B v 25ml HCl 6.5N. Thm nc n vch mc, lc u. 9.4.2 Chun b 1 mu trng (Ly mt bnh nh mc dung tch 250ml khc, thm vo 25 ml HCl tiu chun) 9.4.3 o mu cc dung dch (c hiu chnh bng mu trng) theo cc iu 9.4. n 9.4.8. 9.4.4 V th 9.4.5 Cn 0.25g mu vo cc dung tch 250ml, lm m bng 10ml nc. thm 25ml HCl tiu chun, un si nh cho n khi tan ho ton. Lc vo

bnh nh mc dung tch 250ml, ra giy lc v phn silic khng tan bng nc ct nng. Lm ngui dch lc v thm nc n vch mc. 9.4.6 Ly 50ml dung dch lc vo cc dung tch 250ml, thm 5ml dung dch amonimolipdat v 0.1g axit ascobic bt mn. Khuy k axi ascobic tan ht. un dung dch n gn si v si, m np y khong 1.5 0.5min. Lm ngui v thm nc n chuyn vo bnh nh mc, thm nc n vch 9.4.7 o mt quang ca dung dch ti bc sng 725nm. 9.4.8 Lm mu trng hiu chnh 9.4.9 S dng th ni suy hm lng P2O5 10. Titan dioxit (TiO2) 10.1 Nguyn tc: So mu, s dng thuc th tiron 10.2 Thit b: my o mu 10.3 Thuc th: 10.3.1 m: ho tan 68g NaC2H3O2.3H2O vo 380ml nc, thm tip 100ml CH3COOH 5.0N 10.3.2 EDTA dung dch 0.2M: ho tan 37.2 g EDTA vo 350 ml nc m, lc. thm tip vo phn dch lc 0.25g FeCl.6H2O v pha long thnh 500ml. 10.3.3 HCl (1+6) 10.3.4 Dung dch HCl tiu chun 6.5N: Pha long 540ml HCl thnh 1lit 10.3.5 Amonihydroxit (NH4OH 1+1) 10.3. 6 Kali pyrosunfat (K2S2O7) 10.3.7 Titan dioxit tiu chun, dung dch A: 0.0314g TiO2, y HF, nung K2S2O7, ho tan bng H2SO4 (1+1), nh mc 250ml. 10.3.7.1 Titan dioxit tiu chun, dung dch B: ly 50 ml dung dch tiu chun TiO2 trn vo bnh nh mc dung tch 500 ml, thm nc n vch mc, lc u. 1ml dung dch thu c cha 0.0125mg TiO2 hay tng ng vi hm lng 0.05%TiO2 khi o mu theo cch tin hnh t iu 10.4.4. n 10.4.6. 10.3.8 Axit sunfuaric (1+1) 10.3.9 Tiron (dinatri 1,2-dihydroxylbenzen-3,5diunfonat) 10.4 Cch tin hnh 10.4.1 Chun b mt dy cc dung dch c cha TiO2 trong khong hm lng t 0 n 0.1% trong bnh nh mc dung tch 50ml. 10.4.2Tin hnh to phc mu theo cch tin hnh ti iu 10.4.4 bt u t phn thm EDTA. o mu phc to thnh theo iu 10.4.5 10.4.3 V th tng quan 10.4.4 Ly 25 ml dung dch thu c ti iu 9.4.5 vo bnh nh mc dung tch 50ml. Thm 5ml tiron v 5ml EDTA, lc u, thm tng git dng NH4OH (1+1) n khi dung dch chuyn t mu vng sang mu

xanh l cy, xanh bic hoc mu rubi. Tip tc thm tng git HCl (1+6) chuyn dung dch v mu vng. thm 5ml m v thm nc n vch mc, lc u. 10.4.5 o hp th quang ca dung dch bc sng 410nm. 10.4.6 T hp th quang ca dung dich v th, ni suy %TiO2. Hiu chnh hm lng tht ca TiO2 trong mu theo cng thc: %TiO2 = %TiO2 theo php ni suy (0.01 x %Fe2O3). Kt qu xc nh lm trn theo quy nh ti bng 3 11. Km oxit 11.1 Cc phng php phn tch u c th c s dng min l tun th y cc yu cu c quy nh ti iu 3.3 v bng 1 11.2 Bo co kt qu th nghim lm trn s theo quy nh ti bng 3 12.Nhm oxit 12.1 Tnh ton 12.1.1 Hm lng nhm oxit c tnh ton t hiu s thu c t % khi lng cc xit b kt ta bi NH4OH tr i hm lng TiO2; Fe2O3 v P2O5. Tt c cc php xc nh u c da trn cc phng php trng ti c m t tng ng vi phng php xc nh ny. Bo co kt qu v lm trn s theo quy nh ti bng 3. i vi cc phn tch khng trng ti, hm lng Fe2O3, TiO2 v P2O5 cn cng b r rng bt k quy trnh xc nh c gi tr k thut. 13. Canxi oxit 13.1 Nguyn tc: 13.1.1 Tch loi SiO2. MnO v cc hp cht b kt ta bi NH4OH. Kt ta canxi di dng xalat. Lc ra kt ta, ho tan li oxalat v chun bng KMnO4 13.1.2 Stronti cng c xc nh ng thi cng 13.2 Thuc th 13.2.1 Amoni oxalat, dung dch 50g/l 13.2.2 KMnO4 dung dch tiu tiu chun (0.18N): chun b dung dch c cha 5.69g KMnO4/l. dung dch ti thiu 1tun nhit phng. Chun ho bng natri oxalat. 13.2.2.1 Tnh ton lng CaO ca dung dch theo t nng ca dung dch KMnO4 c hiu chnh t natri oxalat (1ml dung dch KMnO4 tiu chun 1N tng ng vi 0.06701g natri oxalat tinh khit) 13.3 Tin hnh 13.3.1 Axi ho phn nc lc sau khi tch loi cc nguyn t b kt ta bi NH4OH (7.2.2). Trung ho bng HCl n khi dung dch c mu (s dng metyl lm ch th). cho d thm khong 6 git na.

13.3.2 Tch loi mangan: lm bay hi dung dch n th tch khong 100ml. Thm 40ml dung dch nc brm vo dung dch ngay khi cn nng v dung dch c tnh kim r rt. Thm 10ml NH4OH l . Ly mt mu giy, din tch khong 1cm2 th xung y cc v dng a khu gia khng cho mu giy b ni v kt ta mangan oxit (MnO). un si dung dch khong 5 min, nhng vn phi duy tr kim ca dung dch. lng kt ta v lc qua giy lc chy trung bnh, ra kt ta bng nc nng. Nu kt ta khng xut hin, lng thm khong 1h ri mi tin hnh lc. Loi b ht mangan dioxit. Axit ho nc lc bng HCl, s dng HCl v giy qu v un si cho n khi phn hu ht brm (th bng giy c tm KI). 13.3.3 Thm 5 ml HCl, pha long bng nc n th tch khong 200ml, thm tip vi git metyl v 30ml dung dch amoni oxalat (50g/l) nng. un hn hp nhit khong 70-800C v thm tng git NH4OH (1+1) cho n khi dung dch chuyn t mu sang mu vng. yn dung dch ch m khong 60 5min (ch khng lu hn) v khuy lin tc trong 30 min u. 13.3.4 Lc, s dng giy lc mn v ra kt ta t 8-10 ln bng nc nng, tng th tch lc v ra khng vt qu 75ml. Axit ho nc lc ra bng HCl xc nh hm lng MgO. 13.3.5 t cc trc y dng kt ta vo v tr di phu lc, dng a thu tinh chc thng y phu v tia ra bng nc nng ton b kt ta tr li cc. Thm khong 10 git H2SO4 (1+1) vo phn cnh ca giy lc. Ra giy lc t nht 5 ln bng nc nng. Pha long n th tch 200 mlv thm vo 10ml H2SO4 (1+1). un nng dung dch n si v chun ngay lp tc bng dung dch KMnO4 tiu chun 0.18N cho n khi thu c mu hng bn vng trong khong 10s. Ly phn giy lc vo cc chun , thm t. Nu mu hng mt i, tip tc chun n khi xut hin mu hng bn vng trong 10s. 13.3.6 Mu trng 13.4 Tnh ton 13.4.1 Hm lng CaO 13.4.2 Hiu nh hm lng CaO nu c mt SrO 14. Magi oxit 14.1 Nguyn tc: Kt ta di dng magi amoni photphat, nung chuyn v dng cn magi pyrophotphat (Mg2P2O7) 14.2 Thuc th: Amoni phophat (NH4)2HPO4 (100g/l) 14.3 Tin hnh 14.3.1 Axit ho phn nc lc tch canxi (13.3.4) bng HCl v lm bay hi dung dch n th tch cn khong 250ml. Lm ngui dung dch n

nhit phng, thm 10ml amoniphophat (NH4)2HPO4 (100g/l) v 10 ml NH4OH. Khuy k dung dch khi thm NH4OH v tip tc khuy 10-15min na. yn dung dch t nht 8h ri lc. Ra kt ta 5-6ln bng NH4OH (1+20), chuyn kt ta vo chn bch kim hoc chn s, t, nung nhit 11000C trong khong 30-45 min. Cn khi lng dng cn Mg2P2O7. 14.3.2 Mu trng 14.4 Tnh ton 14.4.1 Hm lng MgO tnh chnh xc n 0.1% theo cng thc. Ch : tc nng nhit hn ch s hp th C vo kt ta trong qu trnh nung (khng nng nhit qu nhanh) 15. Sunfua 15.1 Sunfua trioxit 15.1.1 Nguyn tc: kt ta bng BaCl2, nung cn dng cn BaSO4. 15.1.2 Tin hnh 15.1.2.1 Cn 1g mu, thm 25ml nc lnh, khuy k, thm tip 5ml HCl. un trn bp, dm tan cc ht en m bo phn hu ht xi mng. Pha long bng nc n th tch 50ml v duy tr nhit gn si khong 15min. Lc dung dch qua giy lc chy trung bnh, ra k phn cn bng nc nng. Pha long phn nc lc n th tch khong 250 ml, un si. Thm chm 10ml BaCl2 (100g/l), va thm va khuy v tip tc un cho n khi xut hin kt ta. yn dung dch khong 12 n 24h ni m. Lc, t, nung kt ta nhit 800-9000C. 5.1.2.2 Mu trng 15.11.3 Tnh ton 15.2 Sunfit 15.2.1 Nguyn tc: sunfua sunfit c xc nh bng cch lm bay hi di dng H2S, sc trc tip vo dung dich amoniac km sunfat hoc cadimi clorua. Chun lng sunfua sunfit ny bng dung dch KIO3 tiu chun. Tt c cc dng sunfit, thiosunfat v cc dng hp cht trung gian gia sunfat v sunfua u b hp th v chun trong qu trnh ny. 15.2.2 Thit b 15.2.2.1 Bnh thu kh. (M t) 15.2.3 Thuc th: 15.2.3.1 Dung dch amoni cadimi clorua: ho tan 5g (CdCl2.2H2O) vo 150ml nc v 350 ml NH4OH. lng 24h v lc. 15.2.3.2 Dung dch amoni km sunfat: Ho tan 50g ZnSO4.7H2O vo 150ml nc v 350ml NH4OH. lng 24h v lc. 15.2.3.3 Dung dch KIO3 tiu chun 0.03N: lm kh KIO3 nhit 1800C n khi lng khng i. Cn chnh xc 1.0701 g KIO3 v 12g KI. Ho

tan v nh mc vo bnh nh mc dung tch 1l. 1ml dung dch ny, tng ng vi 0.0004809g sunfua. 15.2.3.4 Thic clorua: Cn 10g SnCl2.2H2O vo bnh nh, thm 7ml HCl (1+1), un nh ho tan, sau lm ngui dung dch, thm vo 95 ml nc. Ch pha trc khi dng do l mui d thu phn 15.2.3.5 Dung dch h tinh bt: Thm 5ml dung dch nc huyn ph c cha 1g h tinh bt vo 100 ml nc nng. Lm ngui hn hp. Thm 1 gNaOH vo 10ml nc, v 3 g KI, khuy k. 15.2.4 Tin hnh 15.2.4.1 Ly 15ml dung dch amoni ZnSO4 hoc CdCl2 v 285ml nc vo cc. Cho vo 5g mu v 10ml nc vo bnh phn ng, lc u n khi mu b phn tn u. Thao tc ny v thao tc thm SnCl2 cn phi tin hnh tht nhanh chng ng tng xi mng. Ni bnh vi phu v phn ng ni. Thm 25 ml SnCl2 bng cch rt qua phu v lc bnh. Thm 100 ml HCl (1+3) qua ming phu v li lc tip. Trong qu trnh lc, gi phu cht v lun ng ni sc vo dung dch ZnSO4 hoc CdCl2. Ni phu vi ngun khng kh nn, m ng v t t cho dng kh nn i qua v t t un nng bnh phn ng n si. Tip tc duy tr trng thi si nh khong 3-4min. H nhit v vn dng kh i qua thm hong 3-4min na. Ngt ng v tho khi h thng. Lm ngui dung dch trong cc n khong 20-300C, thm 2ml dung dch h tinh bt v 40ml HCl (1+1) v chun ngay bng dung dch KIO3 tiu chun 0.03N cho n khi dung dch c mu xanh. 15.2.4.2 Lm mu trng 15.2.5 Tnh ton 16. Mt khi nung 16.1 Xi mng pooc lng 16.1.1 Nguyn tc: loi CO2 v m tng s. Cch tin hnh t 16.2.1 n 16.2.3 16.1.2 Tin hnh 16.1.3 Tnh ton 16.2 Xi mng x v xi mng pooc lng x 16.2.1 Nguyn tc; nung, hiu nh kt qu qua kt qu sunfua sunfit c tin hnh phn tch ti 24.1.1 n 24.1.3.1 16.2.2 Tin hnh 16.2.2.1 Cn 1g mu vo chn bch kim bit trc khi lng, nung nhit 950 500C trong khong 15min. Lm ngui n nhit phng trong bnh ht m, cn. 16.2.2.2 Xc nh SO3 theo cch tin hnh t cc iu 15.1.1.1 n 15.1.3.1

16.2.3 Tnh ton: MKN =MKN thc t +0.8 x %SO3 17. Natri oxit v kali oxit 17.1 Tng hm lng alkali 17.1.1 Nguyn tc: Hp th nguyn t 17.1.2 Thit b 17.1.2.1 My hp th nguyn t 17.1..2.2 Yu cu k thut v chun ho iu kin, kim tra chun... 17.1.3 Yu cu cht lng thit b, nhy 17.1.4 Thuc th 17.1.4.1 Bnh cha: bng thu tinh bo- silic v polyetylen 17.1.4.2 Canxi cacbonat 17.1.4.3 KCl 17.1.4.4 NaCl 17.1.4.5 Mt s ho cht cp k thut c th s dng, min l tun th theo 17.1.5 17.1.5 Chun b cc dung dch 17.1.5. Dung dch CaCl2: Thm 300ml nc vo cc dung tch 1500ml c cha sn 112.5 g CaCO3. Thm t t 500 ml HCl, va thm va khuy u. Lm ngui hn hp n nhit phng, chuyn vo bnh nh mc dung tch 1l, thm nc n vch , lc u. Dung dch ny c cha 63000 ppm CaO. 17.1.5.2 Dung dch Natri Kali clorua: Ho tan 1.8858g NaCl v 1.583g KCl (u c lm kh nhit 105-1100Cvi gi) vo nc. Pha long bng nc v chuyn vo bnh nh mc dung tch 1l, thm nc n vch, lc u. Dung dch ny cha 1000 ppm Na2O v K2O. S dng dung dch ny thit lp ng chun trn thit b. 17.1.5.3 Cc dung dch tiu chun: pha long t dung dch chun gc trn 17.1.5.4 Cc dung dch pha long vi nhiu cp nng : c th s dng cc loi bnh nh mc vi dung tch khc nhau. 17.1.6 Chun ho thit b 17.1.7 Tin hnh 17.1.7.1 Chun b dung dch xi mng: Chun b theo cc quy trnh ca nh sn xut thit b khuyn co. Nu khng c quy trnh khuyn co ca nh sn xut thit b, tin hnh cc bc theo cc trnh t ti 17.1.7.1.1 hoc 17.1.7.1.2 17.1.7.1.1 Cn 1.000 0.001g xi mng vo cc dung tch 150ml, thm 20 ml nc, khuy u. Thm tip 5ml HCl. Pha long bng nc n th tch 50ml. Dng a dm nt phn xi mng vn cc. un nh trn bp in trong khong thi gian 15min, lc qua giy lc chy trung bnh vo

bnh nh mc dung tch 100ml. Ra cc v giy lc bng nc nng, lm ngui phn nc lc ra n nhit phng, thm nc n vch mc, lc u. Tin hnh tip tc theo 17.1.7.2 17.1.7.1.2 Chuyn nh lng 1.000 0.001g xi mng vo chn bch kim, tm t mu bng 10 ml nc, lc u hn hp. Thm tip 5 ml HCl. Dm nt cc phn xi mng b vn cc v lm bay hi n kh kit trn bp. Thm tip 2.5 ml HCl v khong 20 ml nc na t chn ln bp un khong 5-10min na v lc qua giy lc chy trung bnh vo bnh nh mc dung tch 100 ml. Ra k phn cn bng nc nng cho n khi th tch nc lc ra vo khong 80-95ml. Lm ngui n nhit phng, thm nc n vch mc, lc u. Nht thit phi tch loi SiO2 ra khi dung dch trc khi phn tch 17.1.7.2 Nu cn, c th pha long dung dch php o c chnh xc 17.1.7.3 Cch tin hnh o Na2O: Theo thit b m phng hoc theo hng dn ca thit b c th c s dng, ch th nghim o lp li. 17.1.7.4 Nu thang o vt chun, cn lp li php phn tch vi lng cn mu l 0.5g v lng HCl s dng l 2.5ml. 17.1.7.5 Ccch tin hnh o K2O: tng t 17.1.8 Tnh ton 17.2 Alkali ho tan 17.2.1 Tin hnh Cn 25g mu vo bnh tam gic dung tch 500ml, thm 250ml nc. y bnh bng nt cao su v lc u hn hp khong 10min nhit phng. Lc qua phu lc Buchner, s dng phu kh, giy lc kh vo bnh lc, s dng bm chn khng. Ch khng ra. 17.2.1.2 Ly 50 ml nc lc vo bnh nh mc dung tch 100 ml v axit ho bng HCl c. Thm tip 9ml dung dch CaCl2 chun (nng 63000ppm CaO) c chun b ti 17.1.5.4 vo bnh nh mc dung tch 100ml v thm nc n vch mc, lc u. Xc nh hm lng K2O v Na2O theo nh m t ti 17.1.7.3 v 17.1.7.5. ghi li s ppm ca tng alkali trong dung dich c trong bnh nh mc dung tch 100ml. 17.2.2 Tnh ton: Quy ra Na2O 18 Mangan Oxit 18.1 Nguyn tc: oxi ho hp cht mangan bng natri bismutat v chun bng natri asenic. 18.2 Thuc th 18.2.1 Dung dch natri asenit tiu chun (1ml =0.0003g Mn2O3): Ho tan 3g natri cacbonat (Na2CO3) vo 100ml nc v thm tip 0.90g asen trioxit (As2O3), un nng hn hp cho n si. Nu dung dch c, cn lc

dung dch. Lm ngui dung dch n nhit phng v chuyn vo bnh nh mc, dung tch 1l, thm nc n vch, lc u. 18.2.1.1 Ho tan 0.58g KMnO4 vo 1l nc v chun ho li nng dung dch bng natri oxalat tiu chun. Ly 30 ml dung dch KMnO4 vo bnh tam gic. Thm vo 60 ml HNO3 (1+4) v 10 ml dung dch natri nitrit (NaNO2, 50g/l). un si dung dch cho n khi HNO2 thot ra hon ton. Lm ngui dung dch, thm NaBiO3 v chun bng natri asenit (NaAsO2) c m t ti 18.3.2. Tnh ton lng Mn2O3 tng ng vi 1ml dung dch asenit. 18.2.2 Natri metabismut (NaBiO3) 8.2.3 Dung dch natri nitrit (50gNaNO2/l) 18.3 Tin hnh 18.3.1 Cn 1.0 n 3.0 g mu vo cc dung tch 250 ml v x l mu bng hn hp gm 5-10ml nc v khong 60-70ml HNO3 (1+4). un si k hn hp. Thm 10 ml dung dch NaNO2 (50g/l) v tip tc un si cho n khi HNO2 bay ra ht, ch khng un qu cn do c th to thnh kt ta SiO2. Khi , c th xut hin cn hoc nu, cn s dng tng thm lng dung dch natri nitrit (50g/l) phn hu hon ton, sau li tip tc un n khi ht HNO2. Lc dung dch qua giy lc chy trung bnh, nc lc hng vo bnh tam gic dung tch 250ml, ra giy lc bng nc. 18.3.2 Th tch dung dch cn khong mc t 100-125ml. Lm ngui dung dch n nhit phng. Thm vo tng lng nh NaBiO3 (tng s khong 0.5g), va thm, va lc u. Tip tc lc khong 5min na, sau thm tip 50 ml HNO3 (1+33) v un si ngay ui HNO2. Lc dung dch, s dng li lc amiang. Ra cn khong 4 ln bng HNO3 (1+33). Chun phn dung dch thu c ngay bng dung dch natri asenit tiu chun. 18.3.3 Mu trng 18.4 Tnh ton 19. Clorua 19.1 Nguyn tc: chun in th bng AgNO3 19.2 Thit b 19.2.1 in cc chn lc ion clorua 19.2.2 My o in th 19.2.3 Buret, vch chia 0.05ml, dung lng 10ml 19.3 Thuc th 19.3.1 Natri clorua, dung dch chun 19.3.2 Bc nitrat 19.3.3 Kali clorua

19.3.4 Nc thuc th 19.4 Chun b dung dch 19.4.1 Natri dung dch tiu chun, nng 0.05N: Sy kh NaCl nhit 105-1100C n khi lng khng i. Cn chnh xc 2.9222 g ho cht kh, ho tan vo nc v chuyn vo bnh nh mc dung tch 1l, thm nc n vch, lc u. Khng cn phi chun ho li nng dung dch ny. 19.4.2 Bc nitrat, nng 0.05N: Ho tan 8.4938 g AgNO3 vo nc, pha long thnh 1l trong bnh nh mc, lc u. Chun ho li nng dung dch bng dung dch natri clorua pha tai 19.4.1 19.4.3 Ch th metyl da cam: pha 2g/1l C2H5OH 19.5 Tin hnh 19.5.1 Cn 5.0g mu xi mng hoc 10.0 g mu b tng vo cc dung tch 250 ml. Lm t mu bng 75 ml nc. T t thm tip vo 25 ml HNO3 (1+1), dng a thu tinh dm nt cc ht en. Nu c mi hi ca H2S, thm vo 3 ml H2O2 (30%). Thm tip 3 git metyl da cam, khuy u. y cc bng mt knh ng h, yn khong 2min. Nu c mu vng hoc mu vng cam trn b mt cc ht kt ta, chng t lng axit phn hu cha . Cn thm tip HNO3 (1+1) cho n khi mu ca dung dch chuyn sang hng hoc . Thm d 10 git na. un nhanh dung dch trn bp n si. Nhc cc ra khi bp 19.5.2 Lc dung dch qua giy lc th, ra kt ta, tng th tch nc lc v nc ra khong 175 ml. Chuyn ton b dung dch sang cc dung tch 250ml. 19.5.3 Chun ho thit b o 19.5.4 Lm ngui dung dch thu c ti 19.5.2 n nhit phng, dng pipet thm vo 2ml dung dch NaCl tiu chun nng 0.05N. t cc c cha hn hp ln my khuy t. Tin hnh chun in th. 19.5.5 Ghi th tch dung dch AgNO3 thu c khi th ca dung dch t -60mV. 19.5.6 Chun d thm 0.2ml na v quan st th ca dung dch. 19.5.7 n 19.5.9: mu trng, hiu chnh kt qu 19.6 Tnh ton 20. Hp cht hu c ho tan trong cloroform 20.1 Nguyn tc: xc nh cc dng cht hu c c a vo trong qu trnh sn xut xi mng. Phng php p dung c cho nhiu loi xi mng khc vi xi mng pooc lng. 20.2 Thuc th 20.2.1 Cloroform: 20.2.2 Thic (II) clorua

20.3 Tin hnh 20.3.1 Ly 40 g xi mng vo phu chit dung tch 1l v thm vo 520ml nc- chia lm 2 ln. Vi mi ln thm nc, cn lc k. Nhanh chng thm tip vo 185ml HCl c cha sn 10 g SnCl2, lc cho tan ht. y np, s dng khuy t ph tan cc ht en xi mng. H m np thot bt kh ri y ngay li v lc tip. Lm ngui nhanh bnh n nhit phng di vi nc chy. 20.3.2 Thm 75ml cloroform vo bnh, y np v lc k trong khong 5min. Cho thm nc v cloroform v yn khong 15min phn lp. Tch ring phn cloroform c cha t vng v mt phn nc ra mt phu chit dung tch 125ml. Ch ly hn chn phn nc. Lc k, lng v tch ring phn cloroform vo bnh chit khcdung tch 250 v c cha sn 50ml nc v vi git HCl, ch vn gi phn vng trong bnh chit dung tch 125ml. Lc k phu chit dung tch 250ml , v tch ring cloroform vo mt ph chit dung tch 250 khc cng c cha sn 50 ml nc v vi git HCl. Lc k ging nh i vi phu chit dung tch 250 ml s dng lc trc. Phn cloroform phn tch c ly vo bnh y bng chun, kh. 20.3.3 Thm 25 ml dung dch cloroform vo phn dung dch gc c trong phu chit dung tch 1l v tin hnh cc thao tc nu trong cc iu 20.3.2, gi li phn nc ra gc trong phu chit dung tch 250 ml. Lp li cc thao tc trn vi th tch 25 ml cloroform khc. 20.3.4 Chng ct phn cloroform sau chit tch n th tch cn khong 10-15ml. Lc phn thu c qua giy lc chy trung bnh, ra cn bng cloroform, phn dch lc thu c hng vo cc dung tch 100ml hoc chn bch kim c bit trc khi lng. Lm bay hi dung dch nhit thp (khong 630C) n kh kit v gi nhit ny trong khong 3min. kh ngoi khng kh khong 15s na, lm ngui v cn. Lp li qu trnh un nng, cn, cho n khi thu c khi lng khng i, chnh lch gia 2 ln cn lin tip khng vt qu 0.0010g. Gi tr khi lng ln hn trong 2 ln cn cui c ly lm gi tr ng. 20.3.5 Mu trng: Lm t mu xi mng c nung nhit 95010000C. 20.4 Tnh ton Phng php thay th khc 21. Canxi oxit 21.1 Nguyn tc 21.1.1Phng php ny l phng php xc nh CaO bng phn tch khi lng, sau khi tch loi SiO2 v cc nguyn t b kt ta bi NH4OH, kt ta canxi di dng oxalat, nung, cn.

21.1.2 Sronti cng tham gia cc phn ng nh canxi, thu c kt qu ng, cn phi hiu nh. 21.2 Nguyn tc 21.2.1 Axit ho phn nc lc thu c trong php xc nh nhm cc nguyn t b kt ta bi NH4OH (7.1 n 7.3), lm bay hi n th tch khong 200ml. thm 5 ml HCl, vi git metyl v 30 ml dung dch amoni oxalat (50g/l) c un nng. un ton b hn hp dung dch n nhit khong 70-800C v thm NH4OH (1+1) t t tng git cho n khi mu ca dung dch chuyn t sang vng. dung dch ni m khong 1h, khuy lin tc dung dch trong khong 30 min u. Lc dung dch qua giy lc mn v ra bng dung dch amoni oxalat (1g/l) lnh. 21.2.2 Chuyn giy lc c cha kt ta tr li cc . Ho tan oxalat trong 50ml HCl (1+4) v dm nt giy lc. Pha long bng nc ct n th tch 200ml, thm vi git metyl v 20ml amoni oxalat, un hn hp n si, kt ta li canxi oxalat theo bng cch trung ha bng NH4OH theo nh m t ti iu 13.3.1. yn dung dch t 1-2h, lc ra. Gp phn nc lc, ra xc nh magi (14.3.1). 21.2.3 t chy giy lc c cha kt ta trong chn bch kim bit trc khi lng, nung chn c cha kt ta nhit 1100-12000C. Lm ngui trong bnh ht m v cn. 21.2.4 Mu trng 21.3 Tnh ton 21.3.1 Tnh ton trn lng mu phn tch 21.3.2 Hiu chnh hm lng t lng SrO. 22. Carbon dioxit 22.1 C th s dng mt s phng php ph hp vi 22.2 nu ti ph lc X2 22.2 Mu s dng trong qu trnh nh lng. 22.3 Tnh ton. 23. Magi oxit. 23.1 Nguyn tc: Xc nh magi bng phng php phn tch th tch, sau khi nh lng SiO2; Al2O3; Fe2O3; v CaO. 23.2 Phng php nhanh (chun magi oxyquynolat). 23.3 Thuc th. 23.3.1 Dung dch amoni nitrat (NH4NO3, 20g/l). 23.3.2 Amoni oxalat (50g/l) 23.3.3 Dung dch hydroxyquynolin: ho tan 8-hydroxyquynolin trong 60 ml dung dich acetic. Khi dung dch trong, thm tip 2l nc lnh. 1ml dung dch thu c tng ng vi 0.0016g MgO

23.3.4 Dung dch kali bromat- kali bromua tiu chun nng 0.2N: Ho tan 20g kali bromua (KBr) v 5.57 g kali bromat (KBrO3) vo 200ml nc v pha thnh 1 lit. So snh nng ca dung dch pha c vi dung dch Na2S2O3 0.1N (22.2.6) theo cch sau: T buret, ly 25ml dung dch KBrO3- KBr vo cc dung tch 500 ml, c cha sn 200ml nc. Thm 20ml HCl, khuy v thm tip 10ml KI (250g/l). Khuy trn k hn hp v chun bng dung dch Na2S2O3 cho n khi mt mu Thm 2 git dung dich h tinh bt v tip tc chun cho n khi dung dch chuyn sang mu xanh. Tnh ton t l nng ca dung dch KBrO3KBr so vi dung dch Na2S2O3 bng cch chia th tch dung dich Na2S2O3 cho th tch dung dch KBrO3-KBr s dng chun . 23.3.5 Dung dch KI (250g KI/l) 23.3.6 Dung dch natri thiosunfat tiu chun, nng 0.1N: Ho tan 25g natri thiosunfat (Na2S2O3.5H2O) vo 200ml nc v 0.1g Na2CO3, pha thnh 1l dung dch trong bnh nh mc. yn khong 1 tun. Chun ho li nng dung dch thu c bng K2Cr2O7. 1ml dung dch Na2S2O3 0.1N ng vi 0.000504g MgO. 23.3.7 Dung dch h tinh bt: Ho tan 25ml dung dch huyn ph cha 5 g h tinh bt vo 500ml nc si, lm ngui n nhit phng, thm vo 5 g NaOH, thm tip 15g KI, khuy k. 23.4 Tin hnh 23.4.1 Ho tan 0.5g mu vo cc dung tch 400ml c cha 10ml nc, khuy k. Va khuy va thm 10ml HCl. Pha long bng nc n th tch khong 100ml. un nh v dng a thu tinh dm nt cc ht en v phn hu hon ton mu, thm khong 2-3 git HNO3, un n si. 23.4.2 Thm 3 git metyl , thm t t tng git NH4OH cho n khi dung dch chuyn sang vng. un si hn hp khong 50-60s. Lc kt ta qua giy lc chy trung bnh, ra kt ta bng NH4NO3 (20g/l) nng, gi li nc lc ra. Chuyn giy lc c cha kt ta vo cc c, ho tan bng 10ml HCl. Dm nt giy lc. Pha long bng nc ct n th tch khong 100ml v un si. Lc ra cc kt ta. Gp phn nc lc ra ny vi phn nc lc ra trc, tng th tch khng vt qu 300ml. Thm 5ml HCl, vi git metyl v 30ml dung dch amoni oxalat nng (50g/l). un nng hn hp n nhit 70-800C ri thm t t tng git NH4OH (1+1) cho n khi dung dch chuyn t mu sang vng. un nng nh dung dch khong 15min. 23.4.3 Thm 10-25 ml dung dch 8-hydroxyquynolin v thm tip c 4ml NH4OH cho100ml dung dch. Khuy hn hp 15min v lng kt ta. Lc dung dich qua giy lc chy trung bnh, ra kt ta bng NH4OH (1+40). Ho tan kt ta bng 50-70ml HCl (1+9) trong cc dung tch

(1+9). Pha long bng nc n th tch khong 200ml v thm vo 15ml HCl. Lm ngui dung dch n khong 250C v thm tip chnh xc 1035ml KBrO3-KBr 0.2N. Khuy k dung dch v khong 30s brom ho. Thm tip 10ml KI (250g/l). Khuy k dung dch v chun bng Na2S2O3 0.1N cho n khi dung dch c mu vng nh. Thm 2ml dung dch h tinh bt v chun n khi dung dch mt mu xanh. (xem mt s gi v th tch cc dung dch cn s dng c lin quan n khong hm lng MgO) 23.4.4 Mu trng 23.4.5 Tnh ton 24. Mt khi nung 24.1 Xi mng x 24.1.1 Nguyn tc: nung mu, hiu chnh bng bng lng SO3 c trong mu 24.1.2. Tin hnh 24.1.2.1 Cn 1 g mu vo chn bch kim bit trc khi lng, nung nhit 950500C trong thi gian khong 15min. Lm ngui n nhit phng trong bnh ht m v cn. Sau khi cn, chuyn nh lng ton b lng mu cn li sau khi nung vo bnh un dung tch 500ml. lc nh trnh vn cc. 24.1.2.2 Xc nh hm lng sunfit sunfua c trong lng mu sau khi nung bng quy trnh c m t ti iu 15.2.1 n 15.2.5. S dng cng quy trnh v thit b tng t xc nh hm lng sunfit sunfua tron mu xi mng cha qua nung. 24.1.3 Tnh ton: tnh hm lng mt khi nung ca mu theo cch tin hnh ti 24.1.2.1 v cng thm 2ln gi tr hm lng sunfit sunfua thu c t mu xi mng nguyn bn c xc nh theo 24.1.2.2. 25 Titan dioxit 25. 1 Nguyn tc: so mu, s dng H2O2 25.2 nh hng: cc nguyn t gy nh hng: V; Mo; Cr. Nu cn, nung chy bng Na2CO3 v chit tch 25.3 Thit b 25.3.1 My o mu 25.4 Ho cht, thuc th 25.4.1 Amoni clorua (NH4Cl) 25.4.2 Amoni nitrat (20g/l) 25.4.3 Dung dch chun Fe3+, c th s dng FeSO4.7H2O pha: ho tan 17.4g vo trong nc cha sn 50 ml H2SO4, nh mc thnh 1l, lc u. 1ml dung dch ny ng vi hm lng 1%Fe2O3 trong 0.5g mu 25.4.4 Hydro peoxit (H2O2 30%)

25.4.5 Natri cacbonat (20g/l) 25.4.6 Natri hoc kali pyrosunfat. (Na2S2O7 hoc K2S2O7) 25.4.7 Titan sunfat, dung dch chun (1ml=0.0002g TiO2): S dung TiO2 gc, cn khong t 0.2 n 0.21g TiO2 ( c lm kh nhit 1051100C khong 2h) vo cc dung tch 125ml. Thm 5g(NH4)2SO4 v thm tip 10ml H2SO4 v y cc bng phu. un nh hn hp cho n gn si v lc nh. Tip tc un cho n khi ho tan hon ton v khng c cn bm trn thnh cc. Lm ngu v nhanh chng thm vo 200 ml nc lnh na, va thm va khuy k. Ra thnh cc v phu bng H2SO4 (1+19), khuy, v gi nguyn phn nc ra ln phn dung dch trong khong 24h. Lc vo bnh nh mc dung tch 1l, ra giy lc k bng H2SO4 (1+19), nh mc ti vch bng H2SO4(1+19)., lc u. 25.4.8 Tnh ton TiO2 tng ng Titan sunfat 25.5 Tin hnh 25.5.1 Trn u hn hp gm 0.5g mu v 0.5g NH4Cl trong cc dung tch 500ml, y cc bng mt knh ng h v thm tip 5ml HCl, ch dung dch axit chy dc t ming cc. Dng a thu tinh khuy k hn hp v cc ln bp cch thu trong khong 30min. trong sut qu trnh, khuy dung dch v dng a thu tinh dm nt cc cn en phn hu hon ton xi mng. Lc dung dch qua giy lc chy trung bnh v chuyn nh lng kt ta ln phu. Ra kt ta 2-3 ln bng HCl (1+99) nng v 10-12 ln bng nc nng. 25.5.2 Chuyn giy lc c cha kt ta vo chn bch kim, t v nung. X l SiO2 bng 0.5-ml nc, 10ml HF v 1git H2SO4, lm bay hi trn bp in n kh kit. 25.5.3 un nng phn dung dch lc thu c, thm NH4OH n khi dung dch c mi trng kim yu v c mi amoniac. Thm vo mt mu nh giy lc vo dung dch v un khong 50-60s. kt ta lng xung, lc qua giy lc chy trung bnh v ra kt ta vi ln bng NH 4NO3 nng (20g/l). Chuyn giy lc c cha kt ta vo chn bch kim x l SiO2 bng HF v t chy, nung cho chy ht giy lc. 25.5.4 Thm 5g Na2CO3 vo chn v nung trong l khong 10-15min (xem 24.2.1). Lm ngui, dng nc ho tan khi chy vo cc. Lc dung dch thu c, s dng giy lc chy trung bnh v ra vi ln bng dung dch Na2CO3 (20g/l). B phn nc lc. Chuyn kt ta vo chn bch kim, t chy trn bp in v nung cho chy ht giy lc. 25.5.5 Thm 3 g Na2S2O7 hoc K2S2O7 vo chn v nung n tan trong. Lm ngui, ho tan khi chy trong nc c cha 2.5ml H2SO4. Gim thiu th tch, lc dung dch vo bnh nh mc dung tch 100ml, s dng giy lc chy trung bnh, ra kt ta bng nc nng. Thm 5ml H3PO4, lm

ngui dung dch n nhit phng. Thm H2O2, thm nc n vch mc, lc u. 25.5.6 Ly cc lng cn thit ph hp ca dung dch chun Ti(SO4)2 vo cc bnh nh mc dung tch 100ml. Thm vo mi bnh 3g Na2S2O7 hoc K2S2O7 c ho tan trong nc v mt lng FeSO4 tng ng vi lng Fe2O3 c trong 0.5 g mu; 2.5 ml H2SO4 v 5ml H3PO4. yn dung dch nhit phng, thm H2O2 (1.0ml m c), thm nc n vch mc, lc u. 25.5.7 o mu cc dung dch. 25.5.8 n 25.6.2 cc phng php o v tnh kt qu. 26. Photpho pentoxit 26.1 Nguyn tc: chun th tch 26.2 Thuc th 26.2.2 Dung dich amoni molipdat: chun b dung dch theo 9.3.1 26.2.2 Amoni nitrat (NH4NO3) 26.2.3 Kali nitrat (10g/l): ho tan 10 g KNO3 vo 1l nc loi CO2. 26.2.4 Natri hydroxit, dung dch tiu chun (0.3N): ho tan 12g NaOH vo 1l nc loi CO2 v lm ngui. Thm 10 ml Ba(OH)2 c lc. Khuy k hn hp trong vi gi v lc li. Bo qun dung dch trnh hp thu CO2. Chun ho dung dch bng kali phtalat hoc axit benzoic. Tnh ton lng P2O5 tng ng. 26.2.5 Natri nitrit (50g/l) 26.2.6 Axit sunfuaric tiu chun (0.15N): Ho tan 4.0 ml H2SO4 vo 1l nc c un si, ngui. Chun ho li nng bng NaOH. 26.3 Tin hnh 26.3 Cn 1-3g mu v 10g NH4NO3 vo cc dung tch 150ml. Trn u hn hp, thm nhanh 10ml HNO3, khuy k cho n khi phn hu hon ton xi mng, dm tan ht keo SiO2. y cc bng mt knh ng h, t cc ln bp un cch thu nhit khong 1000C trong khong 1520min, khuy u trong sut thi gian un. Thm 20ml nc nng, khuy u. Nu mu c cha mangan s quan st thy kt ta nu , thm tip vi mililit NaNO2 (50g/l) phn hu kt ta. un hn hp trong cc n khi phn hu ht kh NO2. Cn thao tc tin hnh kkhng vt qu 5min, thm ngay nc chng bay hi. Lc, s dng giy lc chy trung bnh, nc lc hng vo cc dung tch 400ml. ra cn SiO2 bng nc ct nng, phn nc lc v nc ra cn c th tch khong 150ml. 26.3.2 un nng dung dch n khong nhit 69-710C. Ngay lp tc thm 50-100ml amoni molipdat. Khuy dung dch trong khong 5min, ra thnh cc bng dung dch KNO3 (10g/l) lnh, y mt knh ng h v

 lng khong 2h. Gn cht lc, hn ch khuy dung dch, ra kt ta bng KNO3, n sch axit. 26.3.3 Chuyn giy lc c cha kt ta vo cc c. Thm 20ml nc loi CO2, khuy k. Thm d chnh xc mt lng dung dch NaOH 0.3N cho n khi khng cn kt ta vng, thm tip 50ml nc loi CO2 na v vi git phenonphtalein. Chun bng H2SO4 tiu chun 0.15N cho n khi mt mu hng. 26.3.4 Mu trng 26.4 Tnh ton 27. Mangan dioxit 27.1 Nguyn tc: Chun th tch di dn pemanganat 27.2 Thuc th 27.2.1 Kali pemanganat, dung dich tiu chun (0.18N) 27.2.2 Bt km oxit (ZnO) 27.3 Tin hnh 27.3.1 Cn 2g mu vo cc dung tch 250ml, thm 50 ml nc. Khuy k, thm 15 ml HCl. un hn hp n khi phn hu hon ton. Thm tip 5 ml HNO3 v 50 ml nc, un n khi phn hu ht clo. Thm nc th tch vo khong 100ml. Dng un, thm bt ZnO vo cho n khi trung ho ht axit. Thm d khong 3-5g na v un si dung dch vi pht. 27.3.2 Khng lc dung dch, duy tr nhit khong 90-1000C v tin hnh chun nng bng KMnO4 tiu chun 0.18N cho n khi dung dch c mu hng. 27.3.3 Mu trng 27.4 Tnh ton 28. Canxi oxit t do 28.1 Nguyn tc: y l phng php nhanh dng xc nh canxi oxit t do trong clanke. C 2 phng php c c: Phng php A v phng php B 28.2 Phng php A 28.2.1 Thit b 28.2.1.1 H: gm bnh tam gic y bng, dung tch 250 ml. ng dn c chiu di ti thiu t 300mm. Bnh tam gic v ng dn c ghp ni vi nhau. ng dn c lp vi h hp th c cha cht lm kh nh silicagen v vt liu c kh nng hp thu CO2, h hp th phi c y kn bng nt y cao su v ni vi ng dn. 28.2.1.2 Buret: dung tch 10ml, chia 0.05ml 28.2.1.4 B lc ht 28.2.1.4 bt 28.2.2 Cc dung dch cn thit

28.2.2.1 Etyl Acetoacetat- Izobutyl: hn hp gm 3phn etyl acetoacetic v 20 phn izobutyl theo th tch 28.2.2.2 Ch th thymol xanh: ho tan 0.1g thymol xanh vo 100ml izobutyl 28.2.2.3 Axit pecloric, dung dch tiu chun 0.2N: Ho tan 22ml axit pecloric 70-72% vo 1lit izobutyl. Chun ho nng bng cch: nung 0.1000g CaCO3 cht gc vo chn bch kim nhit 900-10000C. Lm ngui chn trong bnh ht m v cn chnh xc n 0.0001g. Chuyn ton b lng CaO thu c vo bnh tam gic y bng. Tin hnh cc thao tc doc m t ti 28.2.3.1 bt u t thm 70ml hn hp etyl acetoacetat-izobutyl.... Tnh ton gi tri chun ca axit theo CaO. 28.2.3 Tin hnh 28.2.3.1 Cn 1.00000g mu v chuyn vo bnh tam gic dung tch 250ml kh v sch. Thm 4-5 vin bt. Thm tip 70ml hn hp etyl acetoacetat. Khuy lc phn tn lng mu c trong bnh. 28.2.3.2 Lp bnh vo ng dn, un n si v duy tr khong 15min. 28.2.3.3 Tho bnh khi h, y kn np, lm ngui nhanh n nhit phng 28.2.3.4 Lc dung dch bng bm ht chn khng. rar bnh v cn vi ln, mi ln khong 10-15ml izobutyl cho n khi dch lc v nc ra t th tch khong 50ml. 28.2.3.5 Thm 12 git thymol xanh vo phn dch lc ra, ngay lp tc chun bng axit pecloric tiu chun 0.2N cho n i mu r rt 28.2.4 Tnh ton 28.3 Phng php B 28.3.1 Thuc th: 28.3.1.1 Amoni acetat, dung dch tiu chun (1ml= 0.005gCaO): ho tan 16g Amoni acetat c lm kh vo 1l dung dch etanol trong cc c lm sch v sy kh. Chun ho li dung dch ny bng cch tin hnh theo 28.3.2.1 v theo cch m t sau: cn 0.1g CaCO3 vo chn bch kim, nung nhit 900-10000C, lm ngui trong bnh ht m, cn chnh xc n 0.0001g, trnh tip xc vi nc v CO2. Chuyn nh lng CaO thu c vo bnh tam gic c cha glycerin-etanol v Sr(NO3)2. Tip tc tin hnh theo 28.3.2.2. tnh ton chun theo CaO 28.3.1.2 Ch th phenolphtalein: ho tan 1.0g trong 100ml etanol 28.3.1.3 Glycerin- etanol (1+2): trn 1th tch glycerin vi 2th tch etanol. C 1lit hn hp, thm vo 2.0ml ch th phenolphtalein. 28.3.1.4 Sronti nitrat 28.3.2 Tin hnh

28.3.2.1 Chuyn 60ml hn hp glycerin etanol vo bnh sch, kh. Thm 2g Sr(NO3)2 khan nc, chuyn dung dch v mt trng kim bng cch thm vi git dung dchNaOH pha trong cn cho n khi dung dch c mu hng. Cn 1.000g mu vo bnh, y np v lc khuy v un trong h ngng t khong 20min. 28.3.2.2 Tho ri bnh khi h ngng t, lc ht bng bm chn khng. un si phn dch lc v ngay lp tc chun bng dung dch amoni acetat n khi mt mu 28.3.3 Tnh ton