TCVN 141: 2008

XI MNG POC LNG -

PHNG PHP

PHN TCH HA HC

TIU CHUN VIT NAM

TCVN 141: 2008

XI MNG POC LNG - PHNG PHP PHN TCH HA HC

Portland cement - Methods of chemical analysis

Li ni u

TCVN 141 : 2008 thay th cho TCVN 141 : 1998.

TCVN 141 : 2008 do Vin Vt liu xy dng - B Xy dng bin son, B Xy dng ngh, Tng cc Tiu chun, o lng, Cht lng thm nh, B Khoa hc v Cng ngh cng b.

XI MNG POC LNG - PHNG PHP PHN TCH HA HC

Portland cement - Methods of chemical analysis

1. Phm vi p dng

Tiu chun ny quy nh phng php phn tch ha hc cho cc loi xi mng poc lng, clanhke xi mng poc lng.

Tiu chun ny khng p dng cho clanhke v xi mng poc lng cha bari.

2. Ti liu vin dn

Cc ti liu vin dn sau y l cn thit khi p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b th p dng bn c nu. i vi cc ti liu vin dn khng ghi nm cng b th p dng phin bn mi nht, bao gm c phin bn sa i (nu c).

TCVN 4787 : 2001 Xi mng - Phng php ly mu v chun b mu.

TCVN 4851 : 1989 (ISO 3696 : 1987) Nc dng phn tch trong phng th nghim - Yu cu k thut v phng php th.

3. Quy nh chung

3.1. Ha cht dng trong phn tch c tinh khit khng thp hn "tinh khit phn tch" (TKPT).

Nc dng trong qu trnh phn tch theo TCVN 4851 : 1989 (ISO 3696 : 1987) hoc nc c tinh khit tng ng (sau y gi l "nc").

3.2. Ha cht pha long theo t l th tch c t trong ngoc n. V d HCl (1 + 3) l dung dch gm 1 th tch HCl m c vi 3 th tch nc.

3.3. Khi lng ring (d) ca thuc th m c c tnh bng gam trn mililit (g/ml).

3.4. Cc ch tiu phn tch c tin hnh trn mu th c gia cng theo mc 6 ca bn tiu chun ny.

3.5. Mi ch tiu phn tch c tin hnh song song trn hai lng cn ca mu th v mt th nghim trng (bao gm cc lng thuc th nh nu trong tiu chun, nhng khng c mu th) hiu chnh kt qu.

Chnh lch gia hai kt qu xc nh song song khng c vt gii hn cho php (c qui nh ring cho tng ch tiu th), nu vt gii hn cho php phi tin hnh phn tch li.

3.6. Vic xy dng li th chun (cho cc ch tiu th c s dng phng php trc quang, quang ph hp th nguyn t, quang k ngn la) tin hnh nh k theo khuyn co ca nh sn xut thit b theo cch lm nu trong tiu chun ny.

3.7. Biu th khi lng, th tch v kt qu.

- Khi lng tnh bng gam, chnh xc n 0,0001 g.

- Th tch buret tnh bng mililit, chnh xc n 0,05 ml.

- Kt qu th l gi tr trung bnh cng ca hai kt qu phn tch tin hnh song song tnh bng phn trm (%).

4. Ha cht, Thuc th

4.1. Ha cht rn

4.1.1. Natri cacbonat (Na2CO3) khan.

4.1.2. Kali cacbonat (K2CO3) khan.

4.1.3. Amoni clorua (NH4Cl) tinh th.

4.1.4. Kali peiodat (KIO4) tinh th hoc axit peiodic (HIO4) tinh th.

4.1.5. Kali pyrosunphat (K2S2O7) khan hoc kali hydrosunphat (KHSO4) khan.

4.1.6. Bari clorua (BaCl2) tinh th.

4.1.7. Phenolphtalein tinh th.

4.1.8. Axit benzoic (C6H5COOH) tinh th.

4.1.9. Km axetat ZN(CH3COO)2.2H2O.

4.1.10. Dikali hexafluorotitan (K2TiF6) khan.

4.1.11. Silic dioxit SiO2.

4.1.12. Kali clorua (KCl) tinh th.

4.1.13. Natri clorua (NaCl) tinh th.

4.1.14. Mangan oxit (MnO).

4.1.15. Hn hp nung chy: trn u Na2CO3 (4.1.1) vi K2CO3 (4.1.2) theo t l khi lng 1 : 1, bo qun trong bnh nha kn.

4.2. Ha cht lng, thuc th

4.2.1. Axit clohydric (HCl) m c, d = 1,19.

4.2.2. Axit clohydric (HCl), pha long (1 + 1).

4.2.3. Axit clohydric (HCl), pha long (1 + 2).

4.2.4. Axit clohydric (HCl), dung dch 5 %.

4.2.5. Axit clohydric (HCl), dung dch pH = 1,6 : Cho 2 n 3 git axit HCl m c vo 1 lt nc ng trong bnh nha. Kim tra gi tr pH bng my o pH.

4.2.6. Axit flohydric (HF) m c, d = 1,12.

4.2.7. Axit flohydric (HF) pha long (1 + 3).

4.2.8. Axit nitric (HNO3) m c, d = 1,40.

4.2.9. Axit nitric (HNO3), pha long (1 + 4).

4.2.10. Axit sunfuric (H2SO4) m c, d = 1,84.

4.2.11. Axit sunfuric (H2SO4), pha long (1 + 1).

4.2.12. Axit photphoric (H3PO4), pha long (1 + 1).

4.2.13. Axit axetic (CH3COOH) m c, d = 1,05 - 1,06.

4.2.14. Amoni hydroxit (NH4OH) m c, d = 0,88 - 0,91 (25 %).

4.2.15. Natri hydroxit (NaOH) dung dch 10 %, bo qun trong bnh nha polyetylen.

4.2.16. Natri hydroxit (NaOH) dung dch 30 %, bo qun trong bnh nha polyetylen.

4.2.17. Kali hydroxit (KOH) dung dch 25 %, bo qun trong bnh nha polyetylen.

4.2.18. Kali xyanua (KCN) dung dch 5 %, bo qun trong bnh nha polyetylen.

4.2.19. Natri florua (NaF) dung dch 3 %.

4.2.20. Bari clorua (BaCl2) dung dch 10 %.

4.2.21. Bc nitrat (AgNO3) dung dch 0,5 %, bo qun trong bnh thy tinh mu.

4.2.22. Amoni nitrat (NH4NO3) dung dch 2 %.

4.2.23. Natri cacbonat (Na2CO3) dung dch 5 %.

4.2.24. Axit boric (H3BO3) dung dch bo ha.

4.2.25. Axit xitric (C6H8O7H2O) dung dch 10 %.

4.2.26. Ru etylic (C2H5OH), tuyt i.

4.2.27. Glyxerin (CH2OH-CHOH-CH2OH).

4.2.28. Dung dch axit ascorbic (C6H8O6) 5 %, pha dng trong mt tun, bo qun trong chai thy tinh ti mu.

4.2.29. Dung dch kh: Ha tan lin tc vo nc 0,15 g C10H9NO4S (1-amino-2 hiroxynaphtalen-4 sunforic axit) + 0,7 g Na2SO3 khan + 9 g Na2S2O5 (natri metasunphit) thu c 100 ml dung dch. Dung dch ny s dng ti a trong mt tun.

4.2.30. Dung dch diantipyrinmetan 2 %:

Ha tan 20 g thuc th vo 300 ml nc c sn 25 ml axit sunfuric m c, thm tip 2 g n 3 g axit ascorbic, pha long thnh 1 lt. Bo qun trong chai thy tinh ti mu.

4.2.31. Amoni molipdat (NH4)6Mo7O24.24H2O dung dch 10 %.

4.2.32. Ch th fluorexon 1 %: Dng ci chy thy tinh nghin mn v trn u 0,1 g ch th mu fluorexon vi 10 g kali clorua; bo qun trong l thy tinh mu.

4.2.33. Ch th eriocrom T en (ETOO) dung dch 0,1 %: Ha tan 0,1 g ch th ETOO trong 100 ml cn 90 %, thm tip vo dung dch 3g Hydroxylamin hydroclorua; bo qun trong chai thy tinh ti mu.

4.2.34. Ch th amoni st III sunphat Fe(NH4)(SO4)2 dung dch bo ha.

4.2.35. Ch th xylenol da cam, dung dch 0,1 %: Ha tan 0,1 g thuc th trong 100 ml nc ct.

4.2.36. Ch th phenolphtalein, dung dch 0,1 %: Ha tan 0,1 g thuc th trong 100 ml cn 90 %.

4.2.37. Ch th metyl , dung dch 0,1 %: Ha tan 0,1 g thuc th trong 100 ml cn 90 %.

4.2.38. Axit sunfosalixylic (C6H4(OH)SO2H) dung dch 10 %: Ha tan thuc th trong nc ct.

4.2.39. Dung dch tiu chun bc nitrat (AgNO3) 0,1 N: Pha t ng chun (fixanal) AgNO3 0,1 N. Bo qun trong chai thy tinh ti mu.

4.2.40. Dung dch tiu chun amoni sunfoxyanua (NH4SCN) 0,1 N: Pha t ng chun (fixanal) NH4SCN 0,1 N.

4.2.41. Dung dch tiu chun EDTA 0,01 M: Pha t ng chun (fixanal).

4.2.42. Dung dch tiu chun km axetat (Zn(CH3COOH)2) 0,01 M.

Ha tan 2,26 g n 2,3 g Zn(CH3COO)2.2H2O vo 200 ml nc ct, cho thm 1 ml axit axetic c, un n tan trong, pha long thnh 1 lt.

* Xc nh h s K gia dung dch EDTA 0,01 M v dung dch km axetat 0,01 M:

Ly 20 ml dung dch EDTA 0,01 M (iu 4.2.41) vo cc thy tinh dung tch 250 ml, thm vo cc 100 ml nc v 20 ml dung dch pH = 5,5, thm 2 n 3 git ch th xylenol da cam 0,1 %. un ti nhit 70 oC n 80 oC, chun dung dch khi cn nng bng dung dch km axetat pha c n khi dung dch trong cc chuyn t mu vng sang hng, ghi th tch dung dch km axetat tiu th (VZn). T s nng K gia hai dung dch c tnh nh sau:

K = VEVZn

trong

VE l th tch dung dch EDTA ly chun , tnh bng mililit;

VZn l th tch dung dch km axetat tiu th khi chun , tnh bng mililit.

4.2.43. Dung dch m pH = 5,5: Ha tan 100 ml amoni hydroxit m c vo khong 400 ml nc, thm tip vo 100 ml axit axetic ri thm nc ct thnh 1 lt, khuy u.

4.2.44. Dung dch m pH = 10,5: Ha tan 54 g amoni clorua vo 500 ml nc ct, thm tip 350 ml amoni hydroxit m c, thm nc ct thnh 1 lt, khuy u.

4.2.45. Dung dch tiu chun gc titan dioxit (TiO2 = 0,1 mg/ml):

Cn 0,3005 g dikali hexafluorotitan (K2TiF6) sy kh vo chn bch kim, thm t 10 ml n 15 ml dung dch axit sunfuric (1 + 1), lm bay hi trn bp n kh, thm tip 5 ml axit na, tip tc lm bay hi n kh v ngng bc khi trng. Chuyn cc cht trong chn bch kim vo cc thy tinh bng dung dch axit sunfuric 5 %, thm vo cc 5 ml axit sunfuric (1 + 1) v un ti si.

Chuyn dung dch vo bnh nh mc dung tch 1000 ml, dng dung dch axit sunfuric 5 % thm n vch nh mc, lc u.

* Dung dch tiu chun lm vic (TiO2 = 0,05 mg/ml):

Ly 100 ml dung dch tiu chun gc vo bnh nh mc dung tch 200 ml, thm dung dch axit sunfuric 5 % ti vch nh mc, lc u.

4.2.46. Dung dch tiu chun gc silicon dioxit (SiO2 = 1 mg/ml)

Cn 0,200 g SiO2 c tinh khit 99,9 % cho vo chn bch kim, ri thm 2,0 g Na2CO3. Nung mu nhit 1000 oC 50 oC (nung ti thiu 15 pht) sau lm ngui ti nhit phng. Ly khi nng chy cho vo cc nha v ha tan trong nc, sau chuyn dung dch vo bnh nh mc 200 ml, thm nc ti vch nh mc, dung dch c bo qun trong bnh nha.

* Dung dch tiu chun lm vic (SiO2 = 0,02 mg/ml)

Ly 5 ml dung dch gc cho vo bnh nh mc 250 ml, thm nc n vch nh mc, lc u. Dung dch ny khng dng qu 7 ngy.

4.2.47. Dung dch tiu chun gc mangan oxit (MnO = 1 mg/ml).

Sy MnSO4.4H2O tinh khit n khi lng khng i nhit 250 oC 10 oC thu c

mangan sunfat khan. Cn 2,1287 g MnSO4 khan ( c loi nc trn), ha tan trong nc ct pha thnh 1000 ml.

* Dung dch tiu chun lm vic mangan oxit (MnO = 0,1 mg/ml)

Ht 100 ml dung dch tiu chun gc nh mc thnh 1 lt.

4.2.48. Xc nh chun T ca dung dch benzoic 0,1 N

* Glyxerin khng ngm nc: Cho 250 ml n 300 ml glyxerin vo cc 500 ml v un trong 3 gi nhit 160 oC n 170 oC, dng nhit kt nhng vo glyxerin kim tra nhit . Trong khi un, glyxerin c th tr thnh mu vng nht nhng khng tr ngi g. glyxerin loi nc vo bnh thy tinh 500 ml nt mi sy kh cn thn v y cht.

* Dung mi ru - glyxerin: Cho 200 ml glyxerin khng ngm nc vo cc 1000 ml, un nng ti 100 oC n 125 oC, thm 15 g bari clorua sy kh 130 oC v ha tan trong glyxerin. ngui dung dch, thm ru etylic tuyt i n 1 lt v khong 0,1 g phenolphtalein. Dng