Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

LI KHUYN CHUNG
V phi s dng nhng th tch dung dch kh nh, sinh vin cn phi lm: - K lng. - Sch s (ng ht no vo ng l ny, ng b giy ba bi trn mt bn). - Ly tm v ra tht k kt ta , khng ln cc cation ca cc nhm sau. I. CCH LM TA. a. Th acid trc khi thm thuc th. Th bng giy qu xem acid ca dung dch c ng nh trong sch dy hay khng. Nu phn ng phi c thc hin mi trng acid, giy qu phi . Trong trng hp mi trng c tnh baz, giy qu phi xanh. C rt nhiu trng hp ta khng ta c v acid khng ng nh trong li dn b. Thm thuc th tng git mt v theo ng s git dn trong sch. c. Lc mnh sau mi ln thm mt git thuc th cho dung dch v thuc th c trn u, xong t ta lng xung ri hy thm mt git thuc th mi (ngoi tr trng hp cn phn cch thuc th vi dung dch khng cho trn ln nhau, s c li dn ring). Nn lu ng thuc th dnh thnh ng nghim v vi phng php bn vi phn tch, s lng thuc th dnh nhiu khi rt ng k. d. Phi lm ta hon ton mt ion trc khi qua ion mt nhm khc. Mun vy sau khi thm thuc th, em ly tm ri thm mt git thuc th vo nc ly tm. Nu thy cn ta tc l ta cha cho thuc th. Khi y phi thm thuc th, em ly tm ri th tr li cho ti khi khng cn ta mi thi. II. CCH HT LY TM PHA TRN CHT TA. Ly mt ng ht, bp cht nt cao su, a u ng vo trong dung dch, cch mt cht ta vi mm, bung t t mc nc dng ln. Lm nh th hai ba ln cho n khi no ht ht nc ly tm mi thi. Nn trnh ng phi ta. Nc ly tm ny s c a qua mt ng nghim khc tm cc cation khc.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh III. CCH RA CHT TA. Thm mt t nc (5 10git) (hoc dung dch ra khi c li dn ring). Lc mnh cho ta tch khi y ng nghim v ho u trong nc. em ly tm, ht nc ly tm ra. Nc ny c th b i hoc gi li tm ion khc tu theo li dn. IV. CCH HO TAN CHT TA. Thm t t acid (hoc baz). Lc mnh sau mi git. BM (Bain Marie) nu cn. Thm t t nh th cho n khi tan ht cht ta mi thi. Nn nh ng nn dng d acid (hoc baz) c th c hi cho cc phn ng sau ny. V. CCH UN NG NGHIM. Phn ln cc phn ng cn un nng u c un cch thu (BM). Nh vy trnh c vic dung dch trong ng nghim c th bn ra ngoi nguy him. Nu cn un cn mt lng nh dung dch (5 - 15 git) c th trong ng nghim m un, khi un cch xa ngn la va un va lc. Nu cn un cn mt lng tng i nhiu dung dch (2 5ml) nn dng chn chung trn ngn la n gaz c li ngn, cng va un va lc hoc dng u quy trnh dung dch bn ra ngoi, nht l lc gn cn. Nn nh, khi ly chn chung hay ng nghim ra khi ngn la, chn chung hay ng nghim vn cn nng tip tc lm bay hi dung dch. Cn lu iu ny khi c li dn khng c un ti kh. s lng ng k dung dch dnh trn chn chung, phi trng cho sch. VI. CCH QUAN ST MU PHN NG. Quan st mu sc, nhn trn nn trng. Quan st mu trng hoc quan st mt dung dch c t ta, ch thy c: nhn trn nn en. Quan st mu ca kh bc ln: nhn theo trc ng t trn xung di, t ng nghim thng ng trn nn trng. Cn thn ly ra khi la trc khi quan st dung dch khi bn vo mt.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

CH V CCH DNG MY LY TM
My ly tm khi quay phi cha 2 ng nghim t trong 2 ng khng i xng, cc ng y phi c trng lng gn bng nhau my ccnng. Nu khng, my s rung mnh khi quay v rt mau h. V vy nu ch c mt ngi dng my th nh t thm mt ng nghim cha mt th tch nc bng th tch dung dch trong ng nghim phi ly tm. Tt nht l i mt ngi bn hai ngi dng my mt lt. Bt u quay t t. Nu thy my rung mnh, ngng quay tc khc, xem li coi hai ng nghim nm trong hai ng i xng c khi lng bng nhau hay khng. Khi ngng, bung tay cho my ngng quay t t. Ngng gp ng nghim c th bay ra ngoi. Trc khi quay cn kim sot cc con c gn my ly tm vo bn c lng khng, nu c, nh nhn vin trong phng sit cht li. Sinh vin phi lu quay theo chiu mi tn v trn my ly tm (chiu ca tay quay) trnh s ni lng con c s lm vng cc ng ra ngoi rt nguy him. Thng ch quay 30 40 vng l nc trn trong. Ring trng hp cc hidroxid v sunfur khi mi trm hin ln u (cha ra) i hi mt thi gian quay lu hn t 2 n 5 ln. Nn chu kh quay kh lu tt c trm hin lng xung di.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

Chng I GII THIU CHUNG V PHN TCH NH TNH

I. Mc ch. 1. Xc lp thnh phn. Ion, nguyn t, phn t ca cc cht tan trong dung dch. Trong c: - Bn cht v c hoc hu c ca cht cho. - Loi cht no: + Acid. + Mui. + Baz. + Acid Baz (lng tnh). + Phc cht. - Nu l cht hu c th thuc nhm no: + Ru, a ru, phenol. + Acid hu c. + Lng tnh. + Hp cht Diazo mang mu. 2. Pht hin. - Cc dng xc nh ca cation, anion t n gin n phc tp, phc cht bn v.v... - Cc nguyn t ho hc: + Nm trong bng h thng tun hon cc nguyn t. + Cha xut hin trong bng h thng tun hon. - Cc dng tiu phn khc nhau ca cng mt nguyn t: Fe3+, Fe2+, [Fe(H2O)6]3+, [Fe(CN)6]3-, [Fe(CN)6]4-, [Fe(SCN)6]3-, hoc cc dng oxy ho khc nhau ca lu hunh S2-, S22-, So, S2O32-, SO42-.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh 3. Tch hoc c lp cc cht nhm mc ch tinh ch. - Tch cc ion trong cng mt nhm phn tch. Th d: Ba2+, Sr2+, Ca2+, Mg2+. - Tch cc anion trong cng mt nhm phn tch. Th d: Cl-, Br-, I-. 4. Nhn bit v nh tnh. - Da vo cc biu hin vt l, ho hc, ho l c trng. - Da vo cc phn ng phn tch c trng (c s dng thuc th). II. iu kin tin hnh cc phn ng nh tnh. 1. Tnh c trng v nhy ca phn ng. - C rt nhiu phn ng c th thc hin (hng chc ngn), nhng ch c nhng phn ng c trng mi c ngha thc tin trong phn tch nh tnh. - Phn ng c trng: l phn ng m nh chng, trong nhng iu kin xc nh ca phng th nghim c th xc nh c liu duy nht trong dung dch, khi ang c s hin din ca nhng ion khc pht hin c nh vo: + Xut hin mu sc c trng. + C s kt ta. + C s gii phng kh. Th d: SCN- + Co2+ mu xanh sng ca cobalt. 3SCN- + Fe3+ Fe(SCN)3 mu mu. O CH3 C=NOH 2 CH3 C=NOH + Ni
2+

CH3 C N
+ HN O3

N C CH3 Ni O Ni C CH3

CH3 C N

+ H2O

Dimethyl Glyoxin 2. nhy ca phn ng:

Dimethyl Glyoximat Ni mu thm nh

t

2N

- L lng cht nh nht (ca cc ho cht) m ta c th: t + Pht hin c ion (nh tnh). + Pht hin c cht (nh lng). - Ngi ta biu th nhy ca phn ng bng mt s gi tr c lin quan n nhau l: + Cc tiu pht hin: l lng nh nht ca cht trong dung dch ta c th pht hin c n.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

cc tiu pht hin

Th d: 2K+ + [PtCl4]2- K2[PtCl4] kt ta vng quan st c. Th d: 2K+ + PtCl4 K2[PtCl4]

Dng git PtCl42- v 1 git K+

lng cht 0,01 0,03 ml

= 5Mg

+ Nng ti thiu: l nng nh nht ca dung dch m phn ng cn c th

nng K+ ti thiu

(1gK+/10lt) = 0,1g/lt

+ long gii hn: l gi tr nghch o ca nng ti thiu. xc nh long gii hn, ngi ta cho thc hin phn ng mt nng xc nh, sau dng dung mi pha long cho n khi no khng cn xc nh c phn ng na th l pha long gii hn. Phn ng phn tch cng nhy: nu cc tiu pht hin, nng ti thiu cng nh v pha long gii hn cng ln. Th d: phn ng pht hin 2K+ + Ag[Co(NO2)6]= K2Ag[Co(NO2)6] Tinh th mu vng * Cc tiu pht hin l 1Mg * Nng ti thiu (1N/50000) = 2.10-5 N/lt long gii hn l: 50000 ln nhy ca phn ng cn c xc nh bng khong thi gian m phn ng xy ra (phn ng ca cc ion c thi gian phn ng nhanh hn nhiu ln so vi thi gian phn ng ca cc nguyn t, phn t trung ho). Thi gian phn ng ph thuc vo mi trng phn ng. Th d: kt ta Mg2+ bng Na2HPO4 hoc MgHPO4 Na2CO3 Mg2(OH)2CO3
thi gian kt ta rt lu

nu cho NH4OH 1N (5 git) lm mi trng: Mg2+ + NH4OH + Na2HPO4 MgNH4PO4 3. nhy cc i ca thuc th (Reactive = R). Thuc th R (khng mu) + A (khng mu) = RA c mu (R c gi l thuc th so mu. Thuc th ny c kh nng lm xut hin mt phn ng phn tch). Thuc th R c trng vi cht A (m khng cn tp trung cht A trc bng cc bin php lm giu, khi nng cht [A] > 2.10-7 mol/lt hoc gr.ion/lt.
kt ta nhanh chng ngay tc th

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh Trn c s nghin cu v nhy cc i (c th t c) ca thuc th ngi ta thy rng: rt kh xc nh mt tp cht A, c cha trong thnh phn mt hn hp phn tch m khng cn tp trung chng li bng phng php lm giu chng (t nng 2.10-7 ln ~ 10-5). V vy: - Ngay c khi s dng nhng thuc th nhy nht cng cn s dng thuc th c nng ln hn cc tiu pht hin. - nhy cao nht ca thuc th khng mnh (lm php mu) gii quyt cc nhim v phn tch do vy: ngi ta cn phi bit cch s dng thm nhng th thut lm tng nhy ca phn ng phn tch (m nhng th thut ny lun c m hc vin cn hc thc hin c). 4. Phng php lm tng nhy ca phn ng phn tch: c nhiu yu t nh hng n nhy ca phn ng phn tch cho nn lm tng nhy c ngha rt ln n kt qu ca phn tch nh tnh. - V nhy ca phn ng lin quan n cc tiu pht hin, nng ti thiu v pha long gii hn tc l lin quan n nng cht cc tiu cho nn vic cn lm l tp trung, lm tng nng v nhiu khi phi c lp cht pht hin cho c. a. C th lm tng nhy ca phn ng bng cch: dng thuc th c tinh khit cao (tinh khit ho hc hoc tinh khit quang hc nhm loi ht cc tp cht gy nhiu n kt qu phn tch ngoi ra thc hin cc th tc che chn (dng mt n) che cc phn ng ngn cn lm cho phn ng phn tch thc hin c dt khot r rng (nhng vic che chn ny nhiu khi cng cha mnh tng nhy ca phn ng). b. S dng cc bin php tp trung lm giu cht: + Chng ct. + Chit ly. + Kt ta. + Hp ph. c. Tng nhy ca phn ng bng cch lm thay i iu kin ca phn ng phn tch: Th d: hn hp phn ng c I-, Br-, Cl- cn ln lt tch tng thnh phn mt ra khi hn hp. I- (pH = 5 - dng 5git NH4Cl 1N) I2 kh mu tm. kh mu nu. kh mu vng. Br- (pH = 3 - thm 5gi CH3COOH 1N) Br2 Cl- (pH = 1 - cho thm 5 git H2SO4 1N) Cl2 -7Lm tng nng cht cn tm Lm cho nng cht [A] nng cht ti thiu

KMnO4 1M +

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh 5. Che v gii che cc ion (dng mt n): Trong thc hin phn tch (dung dch l hn hp cht v ion) c cha nhiu tp cht gy nn nhng phn ng ph, ngn cn phn ng chnh l phn ng phn tch m ta cn thc hin, gy nhiu cho kt qu phn tch. Khi thuc th: + Tc dng vi c cht cn phn tch v c vi tp cht lm gim nhy ca phn ng phn tch. + Ho tan mt sn phm ca phn ng phn tch, lm mt mu c trng. + To phc cht bn nh hng n pht hin cht. + Xy ra oxy ho kh: lm thay i tnh trng ca cht cn phn tch. a. Che chn tc dng ca phn ng ph: + S dng mui Sianur (CN-), Thiosianur (SCN-), florua (F-), phosphat PO43-, Thiosulfat (S2O32-) ca kim loi kim v NH4+ lm cht che v c. + S dng Acid ascorbic, A.Tartric, acid oxalic, a. Salysilc hoc mui kim loi kim ca chng: Complexon, ThioUrea, Ethylendiamin, diethyldithioCarbamat, Uniton (2,3 di Mercapto Sulfonat Na) v.v... lm cht che hu c. - Phng php ny c s dng rng ri trong ho phn tch v ho hc ni chung. Th d: Khi cho Co2+ + 4SCN- [Co(SCN)4] mu xanh cobalt m. (1) Tp gy nhiu Fe3+ + 3SCN- Fe(SCN)3 mu mu. (2) (1), (2) mu kt hp nu sm ngn cn xc nh Co2+ ngn cn to mu Fe(SCN)3 cho Fe3+ tc dng trc vi + 6F- [FeF6]3+PO43- FePO4 + C2O4 2- Fe(C2O4)33 lm cho mu xanh cobalt [Co(SCN)4]2- th hin tht r rng. - Cng c th kh Fe3+ v Fe2+ Fe2+ + SCNTh d: Khi xc nh Ti4+ c mt Fe3+ gy nhiu cho xc nh Ti4+ - Cch thc hin cho Fe3+ + PO43- FePO4 v Ti4+ c d dng xc nh. Ti4+ + H2O2 TiO2 (trng) Fe3+ + H2O2 Fe(OH)3 vng nu Fe(SCN)2 khng mu khng gy nhiu cho xc nh Co2+.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh b. Gii che: Nhng ion c che c dng phn ng ho hc a v trng thi t do ng hn l trng thi solvat (Hydrat). - Cho ion b che tc dng vi thuc th. Thuc th ny to vi cc phi t (Ligand) ca phc cht che mt phc cht khc bn hn kt qu l mt ion c gii phng. Th d: Che Ni + 4CN- [Ni(CN)4]2- gii che 2Ag+ + [Ni(CN)4]2- 2[Ag(CN)2]- + Ni2+ t do. Che Fe2+ + 6CN- [Fe(CN)6]4- gii che 3Hg+ + [Fe(CN)6]4- 3[Hg(CN)2]- + Fe2+ t do. Che Be2+ + 4F- [BeF4]2- gii che [BeF4]2- + 2Ba2+ 2BaF2 + Be2+ t do. Che Ti4+ + 6F- [TiF6]2- gii che 2[TiF6]2- + 3Be2+ 3[BeF4]2- + 2Ti4+ t do. c. nh hng pH ca mi trng: gi tr pH quan trng trong phn tch nh tnh: + pH quyt nh lng phn ng. + pH quyt nh sn phm phn ng. Th d: - KMnO4 + I- (pH= 5) I 2 (kh mu tm) S dng m acetate: CH3COOH 1N + CH3COONa 1N [H]+ = 10-5 = Ka. 1N. VCH3COOH/1N. VCH3COONa = 10-4,75. VCH3COOH/VCH3COONa 1ml CH3COOH 1N + 1,8ml VCH3COONa 1N - KMnO4 + Br- (pH= 3) Br2 (kh mu ) [H]+ = 10-3 = 10-4,75. VCH3COOH/VCH3COONa 5,6ml CH3COOH + 0,1ml CH3COONa * pH l g? Nc phn ly yu: Nng nc: 2H2O H3O+ + OHK = [H3O+][OH-]/ [H2O]2 = 3,24.1O-18 [H2O] = 1000/18 = 55,555.... = 3,24.10-18.(55,555)2 10-14 ( 250C) Nm 1920 Sorensen a ra khi nim ch s Hydro: pH = -lg[H+] Nc trung ha c: [H+] = [OH-] = KH2O = 10-7 pH = 7 Tch s ion ca nc: KH2O = [H3O+][OH-] = K[H2O]2
2+

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh * m l g? C tnh cht: - Gi tr pH thay i t khi cho thm vo dung dch mt lng axit hoc baze mnh. - S dng m iu chnh pH ca dung dch. m Anderson: * iu chnh pH. - pH thun li, phn ng phn tch xy ra theo hng ng, ion m ta cn nhn bit cho ta phn ng c trng, d dng thun li cho vic pht hin. - nhng gi tr pH khc, phn ng xy ra khng theo hng ng, lm nh hng n kt qu xc nh v pht hin ion. - Th d: phn ng pht hin Fe3+ 4Fe3+ + 3K4[Fe(CN)6] Fe
3+

[H+] = Ka. [Axide]/ [Baze]

Fe4[Fe(CN)6]3 (xanh berlin) Fe(SCN)3 ( mu)

+ 3SCN

Cc phn ng ny xy ra thun li khi pH< 7, khi pH> 7 c 2 cho kt ta Fe(OH)3 nu khng thun li cho vic pht hin Fe3+. - iu chnh pH > 7: Nh t t tng git KOH, NaOH, NH4OH O.1N, Na2CO3 O.1N, CH3COONa 1N Sau dng m Anderson: tt nht l dng m NH4Cl 1N, NH4OH 1N [H+] = Ka. [NH4Cl]/ [NH4OH] - iu chnh pH < 7: Nh t t tng git HCl, HNO3 O.1N, CH3COOH 1N, NH4Cl 1N, NH4NO3 1N Sau dng m Anderson: tt nht l m acetate CH3COOH 1N, CH3COONa 1N [H+] = Ka. [CH3COOH]/ [CH3COONa] d. Thuc th: (Reactive). - Thuc th l cng c sc bn ca ngi lm th nghim ho hc: + xc nh nhn bit cc cht, thnh phn ho hc ca chng. + xc nh cu to ca cc hp cht cn phn tch. - Phn loi thuc th: K thut Tinh khit Tinh khit phn tch Tinh khit ho hc Tinh khit quang hc Tinh khit bn dn Technical Pure Analytical pure (PA) Chenical pure (CP) Speetrel pure SP Semi condutor P SCP - 10 Hm lng cht chnh 0,99 0,999 0,9999 0,99999 0,999999 0,999999999 Hm lng tp 0,01 (10-2) 0,001 (10-3) 0,0001 (10-4) 0,00001 (10-5) 10-6 10-9

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh Trong phn tch nh tnh, loi tr nh hng ca tp gy nhiu ch s dng ho cht tinh khit (P) hoc tinh khit phn tch PA. - Nn nh: Quy nh cc loi thuc th tinh khit phn tch, phn tch ho hc cng ch l tng i trong mt s trng hp, chng vn b nhiu bu (trong cng ngh sn xut, do bao gi, do ng v.v...) do vy nhiu khi chng vn khng p ng c nhu cu do phn tch t ra hoc p ng c mt s yu cu ny, nhng khng p ng c nhng nhu cu khc! - Trong phn tch vt liu bn dn: th c tinh khit ho hc v tinh khit quang hc cng khng dng c do vy ngi ta phi chuyn sang cc phng php vt l, ho l hoc s dng mt n che phn tch c mt s cc ch tiu c bn nht ca vt liu ny. - C mt s lnh vc phn tch i hi tinh khit rt cao ca thuc th ( ng cng bng dng c siu sch) trnh ho cht b nhim bn t mi trng v t ng. - Mt s thuc th c dng ( c thc tin phn tch cng nhn) c mang tn tc gi ca chng. Th d: thuc th Tsugaev vi Ni2+ l dimethyl Glyoxin. Thuc th Nestler l dung dch kim ca K2[HgI4]. Thuc th Streng - Magne Uranyl Acetat. - Thuc th chn lc: Phn ng vi mt s c hn cc ion ring bit, cc ion ny i khi khng cng mt nhm phn tch vi nhau. - Thuc th nhm: Phn ng vi tt c ion trong nhm phn tch. Dung mi chn lc: c th chit ly 1 loi ion khi c mt tt c ion khc trong nhm. e. Yu cu i vi thuc th: - Gi tr v ngha thc tin ca thuc th phn tch c xc nh bi mt lot yu cu: + tinh khit. + nhy. + Tnh c trng. Nu thuc th nhim bn (hoc cha nhng tp cht gy nhiu n vic xc nh nhng ion khc) s cho ra kt qu xc nh khng ng tin cy. Hm lng gii hn ca cc tp cht (cho php) c trong thuc th c quy nh theo nhng yu cu ca tiu chun nh nc hoc tiu chun k thut ca nghnh. Tuy nhin: thc hin cc phn ng phn tch, khng nht thit lc no cng i hi thuc th tinh khit phn tch (PA) hoc tinh khit ho hc (CP) trong thuc th gc ( nhim - 11 L nhng yu cu ch yu

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh bn) li thng khng c nhng tp cht gy nhiu cho kt qu phn tch, cho nn tp bn trong nhng trng hp ny c th b qua. f. Nng thuc th c s dng. Trong phng th nghim phn tch, cn chun b nhng thuc th c nng xc nh (pha mt khi lng thuc th theo tnh ton vo mt th tch dung mi ph hp) - Nu cht ho tan trong nc khi yn dung dch b vn c (do kt ta do thu phn cht tan), trong trng hp ny phi cho thm vo dung dch mt lng axt ph hp. - Cc cht khng ho tan c trong nc: phi trung ho chng trong axit. - Mt s thuc th hu c khng ho c trong nc phi s dng cc dung mi hu c (r u, aceton). - Nng thuc th c biu th bng: s ng lng gram/lt - Thng axit l 5N, baze l 2N. pha cc dung dch phn tch: dng mui nitrate (NO3-) hoc chlorid (Cl-) c nng mui g/lt hoc mg/lt - thng nng mui c s dng l: 0,01g/lt = 10mg/lt. g - K thut dng thuc th. C thuc th chung v ring. - B thuc th ring c t trong cc hp ng, B thuc th dng chung t trn cc gi ngang hoc t trong cc ngn t b ng. - Dung dch thuc th c t trong nhng chai ln ming hp bng thu tinh, c nt mi hoc nt vn. - Khi s dng thuc th: ly tng xut nh cho vo cc bnh nh git. Nhng thuc th rn (phi dng mn) c t trong nhng chai nt mi ming rng. Thuc th c th cc trng thi: rn, lng, kh - Cn tun th cc qui tc s dng thuc th: + Thuc th lng ly tng git, trnh ly lng ln khng lng ph. + S dng xong thuc th: xp chai ngay ngn vo ch c. + Dung dch thuc th ly ra khi l (d cha s dng) cng khng c tr li l ng trnh nhim bn ngu nhin. - Cn thn chu o l vic m ngi lm trong phng phn tch phi lun m bo: + Mi l thuc th s dng mt pipette ring, siphng ht ring. + Nt chai sau khi m t nga trn mt bn, trnh lm bn nt chai. + Sau khi s dng xong thuc th phi y ngay np bnh li v xp bnh tr v v tr c.

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh + Pipette phi t trn gi ring (cho tng chai) - khng pipette t nm trn bn (trnh nhi m bn). III. Cc nhm phn tch. - Trong phn tch nh tnh cc cht v c, ngi ta ch yu s dng cht dung dch mui, acid bazo ho tan trong dung mi l nc, trong trng thi in ly. Do vy: phn tch ho hc dung dch nc ca cc cht in ly c gii hn php xc nh cc ion ring bit (cation v anion) ch khng phi l xc nh nguyn t hoc cc hp cht ca chng. - S phn chia cc ion (cation v anion) thnh cc nhm phn tch da trn quan h ca nhng ion ny vi tc dng ca thuc th, thnh nhng nhm phn tch ring. Trong ti liu ny ngi ta sp xp ion thnh 6 nhm: Nhm 1: Ag+, Pb2+, Hg22+. Nhm 2: Ba2+, Ca2+. Nhm 3: Zn2+, Al3+. Nhm 4: Fe2+, Fe3+, Bi3+. Nhm 5: Mg2+, Cu2+, Hg2+. Nhm 6: K+, Na+, NH4+. Anion v c c chia thnh 3 nhm: Nhm 1: Cl-, Br-, I-, S2-, NO3-. Nhm 2: AsO43-, AsO32-, PO43-, HCO3-, CO32-. Nhm 3: SO32-, SO42-. S phn chia ion thnh cc nhm phn tch chng t c mi lin h gia s phn nhm cc ion vi tnh cht ca cc nguyn t trong h thng tun hon Mendeleev nhng y khng phi l nhng mi lin h trc tip m l mt mi lin h logic, h qu ca nhng hot ng thc tin ca loi ngi trong lnh vc ny.

- 13 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

Chng II PHN TCH NH TNH THEO NHM BI 1: CATION NHM I (Ag+, Pb2+, Hg22+...)
A. c tnh ca nhm phn tch th nht cc Cation. 1. Nhm I s dng thuc th. HCl 2N to kt ta v nhng ta ny c phn ng khc nhau vi dung dch NH4OH. 2. Phn ng nhm: thuc th nhm l: HCl 2N - Ag+ + HCl - Pb2+ + HCl - Hg22+ + HCl * Ion Ag+ - Ag+ - 2Ag+ - 2Ag+ + KI + K2CrO4 + Na2CO3 Ag2CO3 * Ion Pb2+ - Pb2+ + KI - Pb2+ + H2SO4 - Pb2+ + (NH4)2S - Pb2+ + H2S - Pb2+ + K2CrO4 PbI2 (ta vng) + 2K+ (ta tan khi un nng) PbSO4 (ta trng) + 2H+ PbS (ta en) + 2NH4+ PbS (ta en) + 2H+ PbCrO4 (ta vng) + 2K+ AgI (ta vng nht) Ag2CO3(ta trng) Ag (ta en) + CO2 + K+ + 2Na+ + O2 Ag2CrO4 (ta gch) + 2K+ AgCl (ta trng) + H+ PbCl2 (ta trng) + 2H+ Hg2Cl2(ta trng) + 2H+ Ta tan trong dd NH4OH Khng tan trong dd NH4OH C mu en trong dd NH4OH

3. Phn ng ca cc Cation vi thuc th - Cc thuc th c trng.

(pH = 8, NaHCO31N) (Ta tan trong HNO3 6N v NaOH 2N, khng tan trong CH3COOH 2N) * Ion Hg22+ - Hg22+ - Hg22+ - Hg22+ - Hg22+ + Hg2I2 + + + KI + KId NH4OH Na2CO3 K2CrO4 Hg2I2 (ta xanh lc) + 2K+ Hg + [HgI4]2- + 2K+ [XHgNH2 + Hg] (ta xm en) + NH4+ + Cl- + H2O HgCO3 (ta trng) + Hg (Xm en) + 2Na+ Hg2CrO4 (ta ) + 2K+ - 14 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. Trnh t thc hin phn tch ion nhm I. 1. Thc hin phn ng vi thuc th nhm. * Ion Ag+ - Nh 5 git dd Ag+ + 5gi thuc th HCl - Nh 5gi dd Hg22+ + 5gi HCl 2N Nh tng git dd: NH4OH 2N + Hg2Cl2 [Cl-Hg-NH2 + Hg] (ta xm en) + NH4+ + Cl- + H2O kt ta trng PbCl2. - Nh 5gi dd Pb2+ + 5gi thuc th HCl kt ta trng AgCl. Kt ta trng Hg2Cl2

Nh tng git dd NH4OH 2N kt ta AgCl tan.

Nh tng git dd NH4OH 2N kt ta PbCl2 khng tan. 2. Thc hin phn ng vi cc thuc th Cation. * Ion Ag+ - 5gi Ag+ + 5gi KI - 5gi 2Ag+ + 5gi K2CrO4 - 5gi 2Ag+ + 5gi Na2CO3 * Ion Pb2+ - 5gi Pb2+ + 5gi KI - 5gi Pb2+ + 5gi H2SO4 - 5gi Pb2+ + 5gi Na2CO3 - 5gi Pb2+ + 5gi K2CrO4 PbCrO4 + CH3COOH 2N PbCrO4 + NaOH 2N * Ion Hg22+ - 5gi Hg22+ + 5gi KI - 5gi Hg22+ + 5gi NH4OH 2N - 5gi Hg22+ + 5gi Na2CO3 - 5gi Hg22+ + 5gi K2CrO4 3. Thc hnh. C 7 dung dch mu, hc vin chn mt mu (c nh s) trong 7 mu . - Thc hin phn ng vi thuc th nhm. - Thc hin phn ng vi cc thuc th Cation. Pht hin ion trong nhm theo nhng phn ng c trng. - 15 Hg2I2 (ta xanh lc) + 2K+ XHgNH2 (ta xm en) + Hg + NH4X + H2O HgCO3 (ta trng) + Hg (Xm en) + 2Na+ Hg2CrO4 (ta ) + 2k+ PbI2 (ta vng) + 2K+ PbSO4 (ta trng) + 2H+ PbCO3 (ta trng) + 2Na+ PbCrO4 (ta vng) ta khng tan Na2PbO2 (tan) + H2CrO4 AgI (ta vng) + K+ Ag2CrO4 (ta ) + 2K+ Ag2CO3(ta trng) + 2Na+

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. S pht hin Cation nhm I Bi 1.

Dung dch mu (nh s theo kt qu bc thm).

Thuc th nhm HCl 2N nh tng git c kt ta trng.

Thuc th NH4OH 2N nh tng git.

Nu tan kt ta

Nu kt ta khng tan

Nu c kt ta en

Lm cc phn ng c trng pht hin Ag+

Lm cc phn ng c trng pht hin Pb2+

Lm cc phn ng c trng pht hin Hg22+

- 16 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh D. Bo co kt qu phn tch mu. * Phn th nghim chung: TT Kt qu cho im thc hin hoc - Khng thc hin pht hin ion - Khng pht hin Chun b tt dng c ho cht: HCl 2N, 01 NH4OH 2N, KI 2N, K2CrO4 0,5N; Na2CO3, CH3COOH 2N, NaOH 2N, H2SO4 2N Thc hin cc phn ng nhm vi tng cation. - Nh 5gi dd mu Ag+ + 5gi HCl 2N AgCl kt ta trng, sau nh t t NH4OH 2N vo n khi kt ta ho tan. - Nh 5gi dd mu Pb2+ + 5gi HCl 2N PbCl2 kt ta trng, sau nh t t NH4OH 2N vo, lc u, kt ta khng tan. - Nh 5gi dd mu Hg22+ + 5gi HCl 2N HgCl2 kt ta trng, sau nh t t NH4OH 2N vo, lc u, c kt ta xm en. 03 Phn ng c trng ca Ag+ + - Nh 5gi dd ion Ag vo ng nghim, thm 5gi kali iod, c ta vng nht. - Nh 5gi dd ion Ag+ vo ng nghim, thm 5gi kali cromat, c ta gch. - Nh 5gi dd Ag+ vo ng nghim, thm 5gi natri carbonat, c ta trng. 03 Phn ng c trng ca Pb2+ - Nh 5gi dd Pb2+ vo ng nghim, thm 5gi KI, c ta mu vng. Chia ta thnh hai ng: mt ng cho tng git A. acetic, ta khng tan, mt ng cho thm NaOH 2N ta tan. - Nh 5 git dd Pb2+ vo ng nghim, thm 5 git kali iod, c ta vng ti. - Nh 5gi dd Pb2+ vo ng nghim, thm 5gi acid sulfuric 2N, c ta trng. - Nh 5gi dd Pb2+ vo ng nghim, thm 5gi natri carbonat, c ta trng. Phn ng c trng ca Hg22+ 03 2+ - Nh 5gi dd Hg vo ng nghim, thm 5gi amoni hydorxyd, c ta xm en. - Nh 5gi dd Hg22+ + 5gi KI 2N kt ta mu xanh lc. - Nh 5gi Hg22+ + 5gi K2CrO4 0,5N kt ta . - Nh 5gi dd Hg22+ + 5gi Na2CO3 2N ta xm en. 10 Tng cng Phn thc hin

- 17 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh * Phn pht hin ion mu ring: C 4 mu th 1, 2, 3, 4. Chn 1 trong 4 mu: Kt qu cho im Thc hin ng Khng thc hin ng Pht hin c ion Khng pht hin c Thc hin phn ng vi Thuc 1 th nhm Thc hin phn ng c trng 3 pht hin Ag+ Thc hin phn ng c trng 3 pht hin Pb2+ Thc hin phn ng c trng 3 pht hin Hg22+ 10 Tng cng Phn thc hin

TT

1 2 3 4

- 18 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 2: CATION NHM II ( Ba2+, Ca2+)

A. c tnh ca nhm phn tch th hai cc cation. 1. Nhm II s dng thuc th nhm l H2SO4 2N to kt ta tinh th mu trng. 2. Phn ng nhm. 5gi Ba2+ + 5gi H2SO4 BaSO4 kt ta trng + 2H+ - Kt ta rt bn c s dng nh lng Ba2+ v SO42+ 5gi Ca2+ + 5gi H2SO4 CaSO4 + 2H+ - Kt ta khng bn, cho thm 3ml aceton hoc 3ml ru 70. Ethylic to ra kt ta keo mu trng. 3. phn ng ca cation vi cc thuc th c trng. * Ion Ba2+ Ba2+ + K2CrO4 BaCrO4 (vng) + 2K+ Kt ta ny khng tan trong NaOH 2N v CH3COOH 2N Phn ng Voler Ba + H2SO4 2N 5 git 5 git
2+ KMnO4 0,1N

BaSO4 (ngm KMnO4) + 2H+ kt ta mu hng

- Sau dng H2O2 kh KMnO4: mt mu tm KMnO4 + H2O2 + H2SO4 K2SO4 + MnSO4 + O2 + H2O - Nhng ta BaSO4 (ngm KMnO4) vn gi li mu hng. Ba2+ + Na2CO3(2N) BaCO3 + 2Na+ 5 git * Ion Ca2+ Ca2+ + (NH4)2C2O4 5 git 5 git 5 git 5 git Ca2+ + Na2CO3 CaC2O4 + 2NH4+ kt ta trng CaCO3 kt ta trng 5 git kt ta trng

- Kt ta bn khng tan trong CH3COOH 2N tan trong HNO3, HCl, H2SO4 2N. - c s dng lm phn ng nh lng Ca2+, C2O42-

- 19 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. Trnh t thc hin phn tch ion nhm II v hn hp ion nhm I, II. 1. Phn ng v thuc th nhm. 5gi Ba2+ + 5gi H2SO4 2N BaSO4 kt ta trng + 2H+ kt ta bn 5gi Ca2+ + 5gi H2SO4 2N khng c kt ta. Thm 1ml C2H5OH 70% c kt ta trng keo CaSO4 2. Phn ng vi thuc th c trng - 5gi Ba2+ + 5gi K2CrO4 0,1N BaCrO4 kt ta vng + 2K+ Thm 1ml dd CH3COOH 2N kt ta khng tan - 5 git Ba2+ + 1git KMnO4 0,1N + 5 git H2SO4 2N BaSO4 (ngm KMnO4) + 2H+ kt ta mu hng Sau dng H2O2 1N nh t t vo hn hp phn ng. - Trong dung dch H2O2 + KMnO4 + H2SO4 O2 + H2O + K2SO4 + MnSO4(khng mu) - Cn kt ta khng phn ng vi H2O2 vn cn mu hng. - 5gi Ba2+ + 5gi Na2CO3 2N BaCO3 kt ta trng + 2Na+ - 5gi Ca2+ + 5gi (NH4)2C2O4 2N CaC2O4 (kt ta trng, bn) + 2NH4+. Thm 1ml CH3COOH 2N, kt ta khng tan. - 5gi Ca2+ + 5gi Na2CO3 2N CaCO3 kt ta trng, bn + 2Na+

- 20 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. S pht hin cation nhm I v nhm II: C 9 mu dung dch phn tch c nh s 1, 2, 3, 4, 5, 6, 7, 8, 9. Sinh vin c chn 1 mu hn hp cation nhm I, II

10 gi mu hn hp nhm I, II

10 gi HCl 2N ta trng

NH4OH 2N

Kt ta en Kt ta khng tan

Pht hin Ag+ Pht hin Pb2+

NH4OH 2N
Khng ta Phn dung dch

NH4OH 2N Kt ta trng u

C kt ta en

Pht hin Hg22+

H2SO4 2N 10 git
Khng ta Trong dung dch

Pht hin Ba2+

Thm 2ml C2H5OH 70o kt ta keo trng

Pht hin Ca2+

- 21 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh D. Bo co kt qu phn tch mu hn hp Cation nhm I, II * Phn th nghim chung TT Phn thc hin Kt qu cho im thc hin. Khng thc hin. pht hin Khng pht hin ion. ion 1

Chun b tt ho cht: dung dch Ba2+, Ca2+, hn hp cation nhm I, II, HCl 2N, H2SO4 2N, Ethanol 70o, K2CrO4 0,1N; CH3COOH 2N, KMnO4 0,1N; H2O2 30%, Na2CO3 2N, (NH4)2C2O4 2N. Thc hin phn ng vi thuc th nhm II - Nh 5gi Ba2+, nh 5gi H2SO4 2N c kt ta trng BaSO4 kt ta + 2H+ - Nh 5gi Ca2+, nh 5gi H2SO4 2N + 1ml Ethanol 70 CaSO4 kt ta keo + 2H+ Thc hin phn ng c trng vi tng cation * Ion Ba2+ - Nh 5gi dd Ba2+ vo ng nghim, thm 5 gi kali cromat, c ta mu vng ti, sau thm CH3COOH, ta khng tan. - Nh 5gi dd Ba2+ vo ng nghim, thm 1gi KMnO4, 5gi H2SO4 2N, c kt ta, yn vi pht, sau thm t t tng git H2O2 n khi dd mt mu hng tm cn kt ta mu hng. - Nh 5gi dd Ba2+ vo ng nghim, thm 5 gi Na2CO3, c ta trng. * Ion Ca2+ - Nh 5gi dd ion Ca2+ vo ng nghim, thm 5 gi (NH4)2C2O4 c ta trng, sau thm CH3COOH, ta khng tan. - Nh 5gi dd Ca2+ vo ng nghim thm 5 gi Na2CO3, c ta trng. Tng cng

03

03

03

10

- 22 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh * Phn thc hin vi hn hp Cation nhm I, II. TT 1 Phn thc hin S dng thuc th HCl 2N (10gi mu + 10gi HCl) - Phn nm trong dung dch l cc cation nhm II. - Phn nm trong kt ta l cation nhm I. Nh tip 10gi NH4OH 2N vo kt ta pht hin Ag+ trong dung dch - Kt ta mu trng pht hin Pb2+ - Kt ta en xm pht hin Hg22+ Nh tip 10gi H2SO4 2N vo phn nm trong dung dch: - Kt ta trng, bn pht hin Ba2+ - Cho thm 2ml C2H5OH 70o vo dung dch trong xut hin kt ta keo trng pht hin Ca2+ Tng cng Kt qu cho im thc hin Khng thc hin 02

04

04

10

- 23 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 3: CATION NHM III ( Zn2+, Al3+)

A. c tnh ca cation nhm III. 1. Cation nhm III s dng thuc th nhm l NaOH 2N ly lng d. 2. Phn ng nhm. - Zn2+ 5 git - Al
3+

2NaOH 5 git

Zn(OH)2 + kt ta trng Al(OH)3 kt ta trng +

2Na+ 3Na+

+ 3NaOH 5 git

5 git

Khi ly d lng NaOH 2N - Zn(OH)2 + 2NaOHd - Al(OH)3 + NaOHd Na2ZnO2 (tan) + 2H2O 2H2O (2Na+ + ZnO22-) NaAlO2 (tan) +
+ 2-

(Na + AlO ) 3. Cc phn ng c trng. * Ion Zn2+ - Montequi: ion Zn2+ tc dng vi thuc th Montequi (A+B) cho kt ta mu tm. 5 git - Zn2+ 5git - Zn2+ 5 git * Ion Al3+ - Al3+ 5 git - Al3+ 5 git - Al3+ 5 git + + + Aluminon 5 git NH4Cl 2N + 5 git Na2CO3 2N 5 git NH4OH 2N 5 git Al(OH)3 kt ta trng. Al(OH)3 kt ta keo trng. kt ta bng Al(OH)3 (Aluminon) + + (NH4)2S 2N 5 git 5 git Na2CO3 2N ZnS + ZnCO3 + kt ta trng 2Na+ kt ta trng 5 git + 1 git CH3COOH 2N 2NH4+

- 24 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. Bo co kt qu phn tch mu Cation nhm III * Phn th nghim chung TT Phn thc hin Kt qu cho im thc hin Khng thc hin. hoc pht hin Khng pht hin ion. ion. 02

Chun b tt dng c ho cht. Mu Zn2+, Al3+, NaOH2N, CH3COOH 2N, Montequi A,B, (NH4)2S2N, Na2CO3 2N, Aluminon NH4Cl 1N, NH4OH 1N - Nh 5gi dd Zn2+, thm NaOH 2N tng git, c ta trng, nh tip NaOH 2N, ta tan. - Nh 5gi dd Al3+, thm NaOH 2N tng git, c ta trng, nh tip NaOH 2N, ta tan. Thc hin cc phn ng vi TT cation: Cc TT ca cation Zn2+ - Nh 2gi dd Zn2+ thm 1gi CH3COOH, 5gi Montequi A v 1gi Montequi B, c ta mu tm hoa c. - Nh 5gi dd Zn2+, thm 5gi (NH4)2S c ta trng. - Nh 5gi dd Zn2+, thm 5gi Na2CO3, c ta trng. Cc TT ca cation Al3+ - Nh 5gi dd Al3+, thm 5gi Aluminon, un nh c ta bng . - Nh 5gi dd Al3+, thm 5gi NH4Cl, 5gi NH4OH, c ta trng keo. Nh 5gi dd Al3+, thm 5gi Na2CO3 c ta trng. Tng cng

04

04

10

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 4: CATION NHM IV ( Fe2+, Bi3+, Fe3+)

A c tnh ca cation nhm IV. 1. Cation nhm IV s dng thuc th nhm l NH4OH 1N v H2O2 20%, NH4Cl 1N. 2. Phn ng nhm: - 5gi Fe2+ + 5gi H2O2 + 5gi NH4Cl 1N + 5gi NH4OH 1N Fe(OH)3 kt ta nu . - 5gi Fe3+ + 5gi NH4OH 1N + 5gi NH4Cl 1N Fe(OH)3 kt ta nu . - 5gi Bi3+ + 5gi NH4OH 1N + 5gi NH4Cl 1N Bi(OH)3 kt ta vng. 3. Phn ng c trng ca cation: * Ion Fe2+ - 5gi Fe2+ + 5gi K3[Fe(CN)6] 0,1N Fe3[Fe(CN)6]2 (xanh turbin) + 6K+ - 5gi Fe2+ + 5gi Na2CO3 2N 2Na+ + FeCO3 kt ta xanh nu * Ion Fe3+ - 5gi Fe3+ + 5gi K4[Fe(CN)6] 0,1N 12K+ + Fe4[Fe(CN)6]3 xanh Berlin. - 5gi Fe3+ + 5gi KSCN 1N 3K+ + Fe(SCN)3 mu mu. - 5gi Fe3+ + 5gi NH4OH 1N 3NH4+ + Fe(OH)3 kt ta nu . - 5gi Fe3+ + Na2CO3 2N 3Na+ + CO3= + Fe(OH)3 kt ta nu . * Ion Bi3+ - 5gi Bi3+ + 5gi KI 2N Bi3I kt ta en. Nh thm KI d + BiI3 K[BiI4] kt ta tan c mu vng m. - 5gi Bi3+ + 5gi (NH4)2S 2N Bi2S3 kt ta en + 6NH4+ - 5gi Bi3+ + 5gi Na2CO3 c kt ta trng Bi(OH)3 + CO2

- 26 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. S xc nh hn hp Cation nhm I, II, III, IV. C 4 mu phn tch nh s 1, 2, 3, 4 sinh vin chn mu.
ta en pht hin Hg22+ Mu hn hp Cation (1ml) + 5 git Na2CO3 2N ta xanh nu pht hin Fe2+ ta trng + CO2 pht hin Bi3+ ta tan pht hin Ag+ Mu hn hp Cation (2ml) + 5 git HCl 2N khng ta ta trng + 5 git NH4OH ta khng tan pht hin Pb2+

Phn nm trong + H2SO4 2N 5 git dung dch khng ta + Ethanol 70o

ta trng pht hin Ba2+

ta keo trng pht hin Ca2+ khng ta

Phn dung dch tch ra + NaOH (trung ho) ta trng + NaOH d

pht hin Zn2+ lm trc ta tan Pht hin Al3+ lm sau. pht hin Pb2+

Ch : dung dch c th c Fe3+ th lun phn ng c trng vi K4[Fe(CN)6].

- 27 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C Bo co kt qu phn tch mu. * Phn thc hin chung TT Phn thc hin Kt qu cho im thc hin, Khng thc hin. pht hin Khng pht hin ion. ion.

Chun b cc dng c ho cht Fe2+, Fe3+, Bi3+, H2O2 20%, NH4Cl 1N, NH4OH 1N, K3[Fe(CN)6] 0,1N, KSCN 1N, KI 2N, (NH4)2S2N, K4[Fe(CN)6] Thc hin cc phn ng ca cation nhm IV vi TT nhm - Nh 5gi dd ion Fe2+, thm 5gi H2O2, 5gi NH4Cl, 5gi NH4OH c kt ta nu . - Nh 5gi dd ion Fe3+, thm 5gi H2O2, 5gi NH4Cl, 5gi NH4OH, c kt ta nu . - Nh 5gi dd ion Bi3+, thm 5gi H2O2, 5gi NH4Cl, 5gi NH4OH, c kt ta vng ng. Thc hin cc phn ng vi TT cation Cc TT ca cation Fe2+ - Nh 5gi dd ion Fe2+, thm 5gi kali fericyanid, c kt ta keo mu xanh m. - Nh 5gi dd ion Fe2+, thm 5gi Na carbonat c kt ta mu vng nu. Cc TT ca cation Fe3+ -Nh 5gi dd ion Fe3+, thm 5gi kali ferocyanid, c kt ta keo mu xanh m. - Nh 5gi dd ion Fe3+, thm 5gi KSCN, dd c mu mu. - Nh 5gi dd ion Fe3+, thm 5gi Na2CO3 c kt ta nu . Cc TT ca cation Bi3+ - Nh 5gi dd ion Bi3+, thm 5gi KI c kt ta en, thm KI, ta tan, dung dch c mu vng da cam. - Nh 5gi dd ion Bi3+, thm 5gi (NH4)2S, c kt ta mu en. - Nh 5gi dd ion Bi3+, thm 5gi Na2CO3 c kt ta trng v kh bay ra. Tng cng

02

02

03

03

- 28 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 5: CATION NHM V ( Cu2+, Hg2+, Mg2+)

A. c tnh ca cation nhm V Cation nhm V cng c thuc th nhm tng t nh nhm IV l: NH4OH 1N, NH4Cl 1N v H2O2 20% 1. Cc cation nhm V tc dng vi thuc th nhm khng to ra kt ta - 5gi Mg 2+ + 5gi NH4OH 1N Mg(OH)2 + 2NH4+ Nhng Mg(OH)2 trong mi trng NH4Cl 1N (5git) + H2O2 20% (5git) c tch s tan rt ln nn hu nh ho tan hon ton trong dung dch. - 5gi Cu2+ + 5gi NH4Cl + 5gi H2O2 + 5gi NH4OH [Cu(NH3)4]2+ c mu xanh lam (phc tetra ammoni cuprat) 2+ - 5gi Hg2+ + 5gi NH4Cl + 5gi H2O2 [Hg(NH3)2]2+ phc cht tan khng mu (phc diammoni Prusat)2+ Vic tc dng vi thuc th nhm nhng khng to ra kt ta l khc bit ca cation nhm V vi cc catien nhm IV. 2. Phn ng vi thuc th c trng. * Ion Mg2+ - 5gi Mg2+ + 5gi NH4OH 1N + 5gi Na2HPO4 1N MgNH4PO4 + 2Na+ + H2O MgNH4PO4 l kt ta trng ca mui kp Magne Amoni Phosphat. - 5gi Mg2+ + 5gi NaOH 2N Mg(OH)2 (kt ta trng) + 2Na+ - 5gi Mg2+ + 5gi Na2CO3 2N MgCO3 kt ta trng + 2Na+ * Ion Cu2+ - 5gi Cu2+ + 5gi NH4OH 1N [Cu(NH3)4]2+ phc tan mu xanh lam + 4H2O - 5gi Cu2+ + 5gi K3[Fe(CN)6] 0,1N Cu3[Fe(CN)6]2 kt ta + 6K+ - 5gi Cu2 + 5gi (NH4)2S 2N CuS kt ta en + 2NH4+ * Ion Hg2+ - 5gi Hg2+ + 5gi H2O2 20% + 5gi NH4Cl 1N + 5gi NH4OH 1N [Hg(NH3)2]2+ (phc cht tan khng mu) - 5gi Hg + 5gi KI 2N HgI2 kt ta + 2K (2K+ + [HgI4]2-) - 5gi Hg2+ + 5gi NaOH 2N HgO (kt ta vng xm) + 2Na+ + H2O - 29 2+ +

- HgI2 + 2KId K2[HgI4] phc cht tan khng mu tetra Iodua Prusat 2-

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. S xc inh hn hp Cation nhm I, II, III, IV, V. C 6 mu xc nh nh s t 1 n 6: sinh vin chn 1 mu.

C mu xanh Blue Quan st mu Mu phn tch - Ly 2ml C mu vng c Mu en Kt ta + 5gi Na2CO32N Mu nu xanh Phn dd tch ra khi ta Mu trng c kh Mu nu

Pht hin Cu2+

Pht hin Fe3+ Pht hin Hg22+ Pht hin Hg2+ Pht hin Fe2+ Pht hin Bi3+ Kt ta tan Pht hin Ag+

Kt ta trng + 5gi HCl 2N Phn dd tch ra khi ta Kt ta trng + 5gi H2SO42N Pht hin Ba2+ Khng kt ta + Ethanol 700 nh tng git Kt ta keo trng Pht hin Ca2+ Phn dd tch ra khi ta Pht hin Zn2+ lm trc Tan kt ta NaOH 2N trung ho Kt ta trng + NaOH 2N d Pht hin Al3+ sau NH4OH 1N nh tng git Kt ta khng tan Pht hin Pb2+

Kt ta trng khng tan

+ 5gi H2O2 + 5gi NH4OH + 5gi NH4Cl

Tan kt ta

Pht hin Mg2+

- 30 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. Bo co kt qu phn tch mu. * Phn thc hin chung TT Phn thc hin Kt qu cho im thc hin. Khng thc hin. pht hin Khng pht hin ion. ion 1

2 3 4

7 8 9

10 11 12

Chun b dng c ho cht Mg2+, Cu2+, Hg2+, H2O2 20%, NH4Cl 1N, NH4OH 1N, K3[Fe(CN)6] 0,1N, NaOH2N, Na2CO32N, KI 2N, Na2HPO41N Thc hin cc phn ng ca cation nhm V vi TT nhm - Nh 5gi dd ion Cu2+, thm 5gi H2O2,5giNH4Cl, 5gi NH4OH, dd c mu xanh lam. - Nh 5gi dd ion Mg2+, thm 5gi H2O2, 5gi NH4Cl, 5gi NH4OH khng cho ta - Nh 5gi dd Hg2+ thm 5gi H2O2, 5gi NH4Cl, 1 2gi NH4OH, c kt ta ri thm NH4OH n khi ta tan ht, dd khng mu. thc hin cc phn ng vi TT cation Cc TT ca cation Cu2+ - Nh 5gi dd ion Cu2+ thm 1-2gi NH4OH c kt ta, thm tip NH4OH cho n khi ta tan, dung dch c mu xanh lam. - Nh 5gi dd ion Cu2+ thm 5gi kali ferocyanid, c ta . Cc TT ca cation Hg2+ - Nh 5gi ion Hg2+, thm tng git KI c ta thm tip KI ta tan dung dch khng mu - Nh 5gi ion Hg2+, thm 5gi NaOH 2N c ta vng. - Nh 5gi dd ion Hg2+, thm 5gi Na2CO3, c ta nu (vng nu). Cc TT ca cation Mg2+ - Nh 5gi dd Mg2+, thm 5gi NH4Cl, 5gi NH4OH, thm 5gi Na2HPO4 c ta trng. - Nh 5gi Mg2+ thm NaOH 2N c ta trng. - Nh 5gi dd Mg2+, thm 5gi Na2CO3 c ta trng. Tng cng

1 1 1

1 1 1

1 1 1 12

- 31 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 6: CATION NHM VI (NH4+, K+, Na+)

A. c tnh ca cation nhm VI 1. Cation nhm VI khng c thuc th nhm y l nhng cation ca kim loi kim v amoni, chng to ra cc hp cht baze NH4OH, KOH, NaOH v cc mui Haloganid, Sulfat, Carbonat u d tan trong nc, cho nn phi xc nh thng nhng ion ny theo phn ng c trng. 2. Phn ng c trng ca cation nhm VI * Ion NH4+ - 5gi NH4+ + 5gi NaOH 2N NH3 + H2O + Na+ NH3 bay ra lm phenolphthalein chuyn sang mu giy ch th tng hp chuyn sang mu xanh. - 5gi NH4+ + 5gi thuc th Nessler cho kt ta nu * Ion K+ - 5gi K+ + 5gi HClO4 1N H+ + KClO4 kt ta trng - 5gi K+ + 5gi H2C4H4O6 1N KHC4H4O6 kt ta trng + H+ Ion NH4+ cng c phn ng tng t cho nn chc n phi xc nh NH4+ trc hoc un nng dung dch cho NH3 bay hi ra ngoi. O O2N - 5gi K+ + NO2 Acid picric * Ion Na+ - 5gi Na+ + 5gi Magne Uranyl Acetat (thuc th Streng) kt ta mu vng t mui Na+ trn ngn la gas c mu vng. C OH NO2 5gi NO2 Picrat Kali c mu vng kim O2N COOK NO2

- 32 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. S xc nh hn hp Cation t nhm I, II, III, IV, V, VI.

xanh Blue c Cu2+ Mu hn hp Cation 2ml quan st mu nu c c Fe3+ Phn dung dch tch khi ta pht hin Na+ en pht hin Hg22+ nu pht hin Hg2+ xanh nu pht hin Fe2+ trng + thot kh pht hin Bismut Bi3+ kt ta tan pht hin Ag+ Kt ta trng Phn dung dch tch ra t kt ta + H2SO4 2N 5 git Kt ta trng Pht hin Ba2+ + NH4OH 1N nh t t kt ta khng tan pht hin Pb2+ pht hin NH4+ (un nng) pht hin K+

Phn kt ta Phn dung dch tch ra t kt ta + HCl 2N 5 git

ta c mu

- Khng chu kt ta + 1ml C2H5OH 70o kt ta keo trng pht hin Ca2+ Phn dung dch tch ra t kt ta pht hin Al3+ sau + NaOH 2N trung ho Kt ta trng + NaOH d tan kt ta (dung dch) pht hin Zn2+ lm trc

Kt ta trng khng tan

+ H2O2 + NH4Cl + NH4OH

Tan kt ta

Pht hin Mg2+

- 33 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. Bo co kt qu xc nh cation nhm VI TT Kt qu cho im thc hin. Cha thc hin. pht hin Cha pht hin ion ion. Chun b tt dng c ho cht, dung dch NH4+, K+, 02 Na+, NaOH 2N, Phenolphthalein 1%, Nessler, HClO4 1N, H2C4H4O6 1N, CH3COOH 6N, Garola (A+B), Streng Thc hin cc phn ng vi TT cation 03 Cc TT ca cation NH4+ - Nh 5gi dd ion NH4+, thm 5gi NaOH 2N, y ng nghim bng giy lc tm mt git dd phenolphtalein un nh, giy c mu hng. - Nh 5gi dd NH4+, thm 5gi TT Nessler, xut hin ta nu (vng nu). 04 Cc TT ca cation K+ - Nh 5gi dd ion K+, thm 5gi HClO4, c ta trng - nh 5gi dd K+, 5gi dung dch m, thm 5gi acid tartric c ta trng (nu cha c ta c nh thnh ng). - Nh 5gi dd ion K+, thm 5gi acid picric c ta vng. - Nh 5gi dd K+, thm 5gi TT Garola A, mt t bt Garola B, 5 10gi acid acetic 6M c ta vng. 01 Cc TT ca cation Na+ + Nh 5gi dinh dng Na , thm 5gi TT Streng, c ta vng mu l m. Tng cng Phn thc hin

- 34 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 7: ANION NHM I (Cl-, Br-, I-, S2-, NO3-)

A Cc c tnh ca anion nhm I 1. Tc dng vi AgNO3 0,1N to ra kt ta bn, nhng kt ta ny khng tan trong dung dch HNO3 2N. - 5gi Cl- + 2gi AgNO3 NO3- + AgCl kt ta trng - 5gi Br- + 2gi AgNO3 NO3- + AgBr kt ta vng nht - 5gi I- + 2gi AgNO3 NO3- + AgI kt ta vng - 5gi S2- + 2gi AgNO3 NO3- + Ag2S kt ta en NO3- khng to ta vi Ag+ 2. Cc phn ng chung ca Anion Halogenua XS dng KMnO4 0,1N l cht oxy ho mnh, KMnO4 ly in t ca X- v chuyn chng thnh kh Halogen X2 trong mi trng acid. Tm Mn7+ + 5e Mn2+ 2X- - 2e X2 Chlor sau khi bay ln: dng giy lc tm thuc th Vilier-Fayol: giy chuyn t trng sang mu xanh tm. Br2: dng giy lc tm Fluorescein: chuyn t mu vng sang hng. I2: dng giy lc du h tinh bt: chuyn t trng sang mu lam. 3. Cc phn ng ring ca Cl-, Br-, I-. * Ion Cl- 5gi Cl- + 5gi AgNO3 0,1N AgCl (trng) + NO3AgCl + 2NH4OH 2N nh t t [Ag(NH3)2]+ (tan) + Cl- + H2O * Ion Br - Thuc th ca Br- chnh l nc Chlor (nc c Cl2 ho tan) 1ml Cl2 + 5gi Br - Br2 + 2Cl- Br2 ho tan trong Chloroform lm cho dung dch c mu vng nu. Khng mu 2KMnO4 + 10X- + 8H2SO4 2MnSO4 + 5X2 + 8H2O + 5SO42-

- 35 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh * Ion I- 5gi I- + 5gi HgCl2 1N HgI2 + 2ClHgI2 + 2KI d [HgI4]2- + 2K+ (tan) 5gi I- + 5gi Pb(CH3COO)2 1N PbI2 vng + 2CH3COO* Ion S2- 5gi S2- + 5gi Pb(CH3COO)2 1N - 5gi S2- + 5gi H2SO4 2N * Ion NO3- s dng thuc th Griess. (Zn + 2CH3COOH Zn(CH3COO)2 + H2) 2NO3- + 2H2 mi sinh 2H+ + NO2- + H2O NO2- tc dng vi thuc th Griess A + B thnh hp cht Aso c mu hng 5gi NO3- + Diphenylamin hp cht c mu xanh Blue B. S xc nh anion nhm I PbS en + 2CH3COOH2S mi hi + SO42-

Dung dch mu 2ml + 5gi Ba(NO3)2 1N Khng kt ta

+ 5gi AgNO3 0,1N

Kt ta

en pht hin S2Vng nht pht hin

I - (trc) Br - (sau)

Trng pht hin Cl-

pht hin NO3-

- 36 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. Bo co kt qu xc nh Anion nhm I. Phn thc hin Kt qu cho im - thc hin. - Cha thc hin. - pht hin - Khng pht hin Ion Ion.

TT

3 4 5 6 7 8 9

10

11

12

13

14

Chun b dng c, ho cht: Cl-, Br-, I-, S2-, NO3Ba(NO3)2 1N, AgNO3 0,1N, KMnO4 0,1N, H2SO4 2N. Thuc th Vilier-Fayol, Fluorescein, h tinh bt, NH4OH 1N chlorofrom, Nc chlor, HgCl2 1N, Pb(CH3COO)2 1N, km ht Zn Griess A + B, diphenylamin Th anion nhm I vi TT s b - Nh 5gi dd ion Cl-, thm 5gi Ba(NO3)2, khng c ta. - Thao to tng t vi cc dung dch Br-, I-, S2-, NO3- Nh 5gi dd ion Cl-, thm 5gi AgNO3, c ta trng, thm HNO3 2N, ta khng tan. - Nh 5gi dd ion Br-, thm 5gi AgNO3, c ta vng nhat, thm HNO3 2N, ta khng tan. - Nh 5gi dd ion I-, thm 5gi AgNO3, c ta vng kem, thm HNO3 2N, ta khng tan. - Nh 5gi dd ion S2-, thm 5gi AgNO3, c ta en, thm HNO3 2N, ta khng tan. - Nh 5gi dd ion NO3-, thm AgNO3, khng c ta. Th phn ng chung xc nh X- Nh 5gi dd Cl-, thm 5gi KMnO4, 2 3gi H2SO4 m c, y ng nghim bng giy lc tm TT VilierFayol, sau vi pht giy c mu xanh tm. - Nh 5gi dd Br-, thm 5gi KMnO4, 5gi H2SO4 m c, y ng nghim bng giy lc tm TT Fluoressein, giy chuyn t mu vng sang hng. - Nh 5gi dd I-, thm 5gi KMnO4, 5gi H2SO4 m c, y ng nghim bng giy tm h tinh bt, giy c mu tm xanh. Th anion Cl-, Br-, I- vi c TT ring - Nh 5gi dd Cl-, thm 2-3gi AgNO3, c ta trng, thm NH4OH ta tan. - Nh 5gi dd Br-, thm 5gi nc clor, 5gi cloroform, lc nh, quan st lp cloroform thy c mu vng nu. - Nh 5gi dd I-, thm HgCl2, c ta , thm tip dd I-, ta tan, dung dch khng mu. - 37 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh 15 16 Th anion S- vi cc TT - Nh 5gi dd S2-, thm 5gi ch acetat, c ta en. Th anion NO3- vi cc TT - Nh 5gi dd NO3-, thm mt ht km, 5gi Griess A. 5gi Griess B, lc nh, dd c mu hng. - Nh 5gi dd NO3-, thm 1 2gi H2SO4 c, 5gi diphenylamin, dd c mu xanh l. Tng cng

17

BI 8: ANION NHM II (AsO43-, AsO33-, PO43-, HCO3-, CO32-)

A. Nhng c tnh ca Anion nhm II. 1. Phn ng vi Ba(NO3)2: cho ra nhng kt ta trng, tan trong HNO3 2N. - 5gi AsO33- + 5gi Ba(NO3)2 1N Ba3(AsO3)2 + 6NO3- 5gi AsO43- + 5gi Ba(NO3)2 1N Ba3(AsO4)2 + 6NO3- 5gi PO43- + 5gi Ba(NO3)2 1N Ba3(PO4)2 + 6NO3- 5gi CO32- + 5gi Ba(NO3)2 1N BaCO3 + 2NO3Ion HCO3- khng to ra kt ta bn vi Ba2+ nhng do tham gia vo cn bng phn ly HCO3- H+ + CO32Cho nn vn to nn BaCO3 2. Phn ng vi AgNO3 0,1N: Cc Anion nhm II phn ng vi AgNO3 u cho kt ta, cc kt ta ny u tan trong HNO3. - 5gi AsO33- + 5gi AgNO3 0,1N 3NO3- + Ag3AsO3 vng - 5gi AsO33- + 5gi AgNO3 0,1N 3NO3- + Ag3AsO4 nu - 5gi PO43- + 5gi AgNO3 0,1N 3NO3- + Ag3PO4 vng - 5gi HCO3- + 5gi AgNO3 0,1N AgHCO3 trng + NO3- 5gi CO32- + 5gi AgNO3 0,1N 2NO3- + Ag2CO3 trng (b nh sng phn hu Ag xm en) 3. Cc phn ng xc nh AsO33- v AsO43-. Phn ng gia km v H2SO4 2N to ra Hydro mi sinh. Zn + H2SO4 ZnSO4 + 2Ho 3H+ + AsO33- + 6Ho AsH3 + 3H2O 3H+ + AsO43- + 8Ho AsH3 + 4H2O AsH3 bay ln gp giy lc tm AgNO3 lm cho giy c mu en. - 38 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh 4. Phn ng c trng ca AsO43-. - 5gi AsO43- + 5gi NH4Cl 1N + 5gi NH4OH 1N + 5gi MgCl2 2N MgNH4AsO4 Kt ta trng mui kp Amoni Magne Asenat 5. Phn ng ca HCO3- v CO32-. - 5gi HCO3- + 5gi Hg(NO3)2 1N HgCO3 kt ta nu + H+ + 2NO3- 5gi CO32- + 5gi Hg(NO3)2 1N HgCO3 kt ta nu + 2NO3Tc dng vi Acid mnh HCO3- v CO32- b phn hu thnh CO2 - 5gi HCO3- + H+ CO2 + H2O - 5gi CO32- + 2H+ CO2 + H2O CO2 bay ra tc dng vi Ca(OH)2 to kt ta trng c: CO2 + Ca(OH)2 CaCO3 + H2O Phn ng phn bit HCO3- v CO32- dng Mg2+ ch tc dng vi CO32- to kt ta trng, cn vi HCO3- khng to ra kt ta: Mg2+ + CO32- MgCO3 kt ta trng 6. Phn ng ca PO43-. PO43- tc dng vi (NH4)2MoO4 to kt ta vng: 12(NH4)2MoO4 + PO43- + HNO3 (NH4)3H4 [P(Mo2O7)6] kt ta vng + H2O + NH4NO3 Cc ion AsO33- v AsO43-. Khi tc dng vi (NH4)2MoO4 cng cho phn ng tng t cho nn khng b lm phi xc nh AsO33- v AsO43- trc khi xc nh PO43-. PO43- tc dng vi hn hp MgCl2, NH4Cl, NH4OH to ra mui kp kt ta trng: PO43- + Mg2+ + NH4+ MgNH4PO4

- 39 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. S xc nh hn hp anion nhm I, II

ClMu phn tch + Ba(NO3)2 2N 2ml 5git dung dch sau + khi tch ta kt ta en S2kt ta trng AgNO3 0,1N 5 git kt ta trng kt ta vng Br-, I-

tan kt ta nu pht hin AsO43+ AgNO3 0,1N 5 git kt ta vng pht hin AsO33- sau PO43kt ta trng CO32C kh bc ln + CH3COOH 2N 5 git + MgCl2 2N 5 git khng kt ta HCO3-

- 40 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. Bo co kt qu xc nh anion nhm II. Phn thc hin Kt qu cho im - thc hin. - Cha thc hin. - pht hin - Cha pht hin ion. ion.

TT

3 4 5 6 7 8 9

10 11 12 13 14 15 16

17

Chun b dng c ho cht: AsO33-, AsS43-, PO42-, HCO3-, CO32-, Ba(NO3)2 2N, HNO3 2N, AgNO3 0,1N, Zn, H2SO4 2N, CH3COOH 2N, Hg(NO3)2 1N, MgCl2 2N, (NH4)2MoO4 1N, NH4Cl 1N, NH4OH 1N. Th anion nhm II vi TT s b - Nh 5gi dd AsO33-, thm 5gi Ba(NO3)2, c ta trng, HNO3 2N ta tan. - Thao tc nh trn vi dd AsO43-, PO43-, HCO3-, CO32-. - Nh 5gi dd AsO33-, thm 5gi AgNO3, c ta vng. - Nh 5gi dd PO43-, thm 5gi AgNO3, c ta vng. - Nh 5gi dd HCO3-, thm 5gi AgNO3 c ta nu. - Nh 5gi dd HCO3-, thm 5gi AgNO3 c ta trng - Nh 5gi dd CO32-, thm 5gi AgNO3, c ta trng hi xm. Phn ng chung xc nh AsO33-, AsO43- Nh 5gi dd AsO33-, thm 1 ht km, 5gi H2SO4 2N y ming ng bng giy tm AgNO3, giy chuyn sang mu en. - Thao tc nh trn vi dd AsO43-. Phn ng chung ca HCO3- v CO32- Nh 5gi dd HCO3-, thm CH3COOH tng git, quan st ng thy c kh bay ra. - Thao tc nh trn vi dd CO32-. - Nh 5gi dd HCO3- thm 5gi Hg(NO3)2, c ta nu hoc vng nu. - Thao tc nh trn vi dd CO32-. - Phn ng phn bit HCO3- v CO32Nh 5gi HCO3- + 5 gi MgCl 2N khng kt ta. Phn ng ca PO43- 5gi PO43- + 5gi (NH4)2MoO4 0,1N un nh, ta vng. - 5gi PO43- + 5gi NH4Cl 1N + 5gi NH4OH 1N + 5gi MgCl2 2N kt ta trng. Tng cng - 41 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 9: ANION NHM III (SO32-, SO42-)

A. c tnh ca anion nhm III. 1. Phn ng s b ca Anion nhm III. - 5gi SO42- + 5gi Ba(NO3)2 2N BaSO4 trng + 2NO3- + HNO3 2N nh t t khng tan. - 5gi SO32- + 5gi Ba(NO3)2 2N BaSO3 trng + 2NO3- + HNO3 2N nh t t, kt ta khng tan v BaSO3 b HNO3 oxy ho thnh BaSO4. - 5gi SO42- + 5gi AgNO3 0,1N khng c kt ta. - 5gi SO32- + 5gi AgNO3 0,1N Ag2SO3 trng + 2NO2(ta ny tan tr li trong dung dch SO32-). Ag2SO3 + 3SO32- 2[Ag(SO3)2]32. Phn ng c trng ca SO32-. - 5gi SO32- + 5gi BaCl2 2N BaSO3 kt ta trng + 2ClBaSO3 + 2HCl 2N BaCl2 + SO2 + H2O SO32- b cc acid mnh phn hu thnh SO2, SO2 lm mt mu KMnO4. H+ + SO32- SO2 + H2O SO2 + 2KMnO4 + H+ 2MnSO4 + K2SO4 + H2O 3. Phn ng c trng ca SO42-. - 5gi SO42- + 5gi BaCl2 2N BaSO4 kt ta trng + 2Cl* Phn ng Voler - 5gi BaNO3 2N + 5gi SO42- + 3gi KMnO4 0,1N BaSO4 + 2NO3Kt ta mi hnh thnh BaSO4 s hp ph KMnO4 t trng mu hng BaSO4 (KMnO4) + H2O2 20% nh t t n khi mt mu KMnO4 trong dung dch. 5H2O2 + 2KMnO4 + HCl 2KCl + MnCl2 + O2 +H2O Nhng KMnO4 trong lp hp ph ca BaSO4 vn cn nguyn, kt ta BaSO4 (KMnO4) vn c mu hng. - 5gi SO42- + 5gi Pb(CH3COO)2 2N PbSO4 kt ta trng + 2CH3COO-.

- 42 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh B. S xc nh hn hp Anion nhm I, II, III.

Mu phn tch + CH3COOH 2N 2ml

c thot kh + MgCl2 2N 5 git

ta trng pht hin CO32-

khng ta pht hin HCO3dung dch khng ta ta trng pht hin Cldch tch ta + Ba(NO3)2 2N 5 git AgNO3 0,1N 5 git ta vng pht hin Br-,Clta en pht hin S2ta trng Trong c nhiu NO3ta khng tan + AgNO3 ta tan khng ta pht hin SO42+ AgNO3 0,1N 5 git nu AsO42vng pht hin AsO33- trc, PO43- sau kt ta pht hin SO32-

- 43 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh C. Bo co kt qu xc nh Anion nhm III. Phn thc hin Kt qu cho im thc hin. Cha thc hin. pht hin Cha pht hin Ion Ion 1

TT

3 4 5 6

Chun b tt dng c, ho cht: SO32- SO42-. Ba(NO3)2 2N, HNO3 2N, AgNO3 0,1N, BaCl2 2N; HCl 2N, H2SO4 2N, KMnO4 0,1N, H2O2 20%. Th anion nhm III vi TT s b - Nh 5gi dd SO42-, thm 5gi Ba(NO3)2, c ta trng, thm HNO3 2N, ta khng tan. - Nh 5gi dd SO32-, thm 5gi Ba(NO3)2, c ta trng, thm HNO3 2N, ta khng tan. - Nh 5gi dd SO42-, thm 5gi AgNO3, khng c ta. - Nh 5gi dd SO32-, thm 5gi AgNO3, c ta trng. Th anion SO42- vi cc TT - Nh 5gi dd SO32-, thm 5gi BaCl2, c ta trng, thm HCl 2N, ta tan. - Nh 5gi dd SO32-, thm 5 6gi H2SO4 2N, y ng bng giy lc tm KMnO4 un nh, giy mt mu hng. Th anion SO42- vi cc TT - Nh 5gi dd SO42-, thm 5gi BaCl, c ta trng, thm HCl 2N, ta khng tan. - Nh 5gi dd SO42-, thm 1gi KMnO4, 5gi HNO3 2N. 5gi Ba(NO3)2, lc k, vo gi khong 5 6 pht, sau yn vi pht, thm tng git H2O2, dd mt mu tm hng, ta vn c mu hng. - Nh 5gi dd SO42-, thm 5gi ch acetat, c ta trng. Tng cng

1 1 1 1 1

10

1 10

- 44 -

Bi ging L thuyt v Thc hnh Ho phn tch nh tnh

BI 10 Xc nh hn hp Cation v Anion trong dung dch

Trong bi 10 trong phng th nghim chun b 10 mu phn tch c thnh phn l hn hp cc cation nhm I, nhm III v nhm VI v anion nhm I. - Sinh vin bc thm mu th nghim T a ra s phn tch v bo co kt qu phn tch da trn s a ra. - Nhng phn ng thc hin u phi c trnh by y , cchi tit, chnh xc km theo kt qu quan st nhng hin tng xy ra khi thc hin phn ng. - Nhng mc sinh vin thc hin ng (hoc tm c kt qu ng) s c cng thm 1 im. - Nhng mc cha thc hin (hoc thc hin nhng cho kt qu sai s c ghi nhn 0 im). - im chm cho bi bo co th nghim 10 cng l im kim tra gia k ca sinh vin v s c chuyn i ra thang im 10 khi chia s im thc t c chm vi im ti a sinh vin c th nhn c kh thc hin th nghim ny. * Phn thc hin Trnh t xc nh Bi 10. * Phn ng th u tin: s dng Na2CO3 2N. TT Hin tng 1 - 5gi mu phn tch + 5gi Na2CO3 2N c ta en. 2 - 5gi mu phn tch + 5gi Na2CO3 khng kt ta. 3 - 5gi mu phn tch + 5gi Na2CO3 2N c kt ta trng v bt kh. * Ch : 1. Dung dch mui bao gi cng cha cation v anion. 2. Vic xc nh cation v anion tin hnh c lp vi nhau. Nhng c mt s cation cn tr vic xc nh anion v ngc li. 3. xc nh ion khng gp tr ngi, gy nhm ln, cn thc hin theo trnh t sau: - Quan st mu phn tch, nu mu c mu th theo mu xc nh cation tng ng nu mu phn tch khng mu phi thc hin cc phn ng th. Hng phn tch ng Xc nh cation t nhm I V trc, xc nh anion sau. Xc nh cation trc, xc nh anion sau. Tm Bi3+ v cation trc anion sau. Sai

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Bi ging L thuyt v Thc hnh Ho phn tch nh tnh Th d: + Mu phn tch 5gi + 5gi Na2CO3 2N khng ta: xc nh anion trc (tr CO32-). Ri n cation nhm VI (NH4+, K+, Na+) sau. (Cation cc nhm khc khng c). + Mu phn tch 5gi + 5gi Na2CO3 2N c kt ta trng v kt ta mu xc nh cation 5 nhm u trc, cation nhm VI v anion sau. - Vic xut hng phn tch cho sinh vin thc hin, ghi vo tp v trnh by vi ging vin hng dn x l kin a ra nhng thay i v trnh t v hng thc hin tip. - Trong qu trnh lm bi 10, nu gp kh khn, sinh vin cn trnh by vi ging vin hng dn c gip v c th xc nh tt tt c cc ion c trong dung dch phn tch. - Cc thy c hng dn cn tch cc tr li cc cu hi, a ra nh hng phn tch cho sinh vin hon thin k nng ging dy ca mnh.

TI LIU THAM KHO

1. Ho hc phn tch Ti liu hun luyn ca b Trung hc Dc B y t nh xut bn Y hc 1980. 2. Bi ging k thut kim nghim thuc - Vin kim nghim v trng trung hc k thut dc TW 1988. 3. A P Kreskov C s Ho hc phn tch quyn I nh xut bn i hc v Trung hc chuyn nghip 1990. 4. Phm Hi Tng Phm Gia Hu Ho hc phn tch T sch b mn Ho phn tch H dc khoa H Ni NXB Y hc H Ni 1978. 5. Charlot S tay tra cu Ho phn tch NXB Ho Bnh Moscva 1970. 6. C Thnh Long - Nguyn Th Xun Mai - Nguyn Th Minh. Hng dn thc hnh phn tch nh tnh bng cc phng php ho hc. T sch Trng i hc khoa hc T Nhin 1999. 7. V Th Bch Hu. Ho phn tch - Tp I. Nh xut bn Gio dc. H Ni 2007.

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