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    Tailieuxanh Thi Nghiem Phan Tich Dinh Luong 2 8545 Compressed-Đã-Nén-1

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    Anh Ngoc

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    BINH LUONG MGT 6 ON VA PHAN TU TRONG CUMG DICH Phan 3 BINH LUQNG MOT SO ION VA PHAN TU TRONG DUNG DICH 3.1. DINH LUGNG DUNG DICH ACID HAY DUNG DICH BAZ 8.1.1 Chudn do dung dich acid manh, baz manh Dinh lugng dung dich HCl (H,SO,) bang dung dich NaOH UXOH) hoae nguse lai. d. Nguyén tée a. Phéin ting ehudn dé Ht 40H" > HaO ‘Tai diém tuong ducng: [OW] = (H'] = pHs = 7 b. Dink diém euéi Daing chat chi thi Bute nhay etia dudng chuiin d6 kha dai (td pH = 4 dén 10 voi Cat = Cow ~ 0,1N) =2 66 thé chon cde chat eh thi c6 sy chuyén mau trong khodng pH nay: methyl dé (4,2 + 6,2); bromothymol xanh (6,0 + 7,6); phenolphthalein (8,2-+ 10)... Ding méy do pH Dign eye chi thi: thdy tinh ho&e hydro Dien eye chudn: calomel hoze AgC] 2. Thite nghiom a. Héachét ~ Dung dich chudn acid hay baz G = 0,050N hay C = 0,100 - Dung dich chi thi bromothymol xanh 0,1%letanol 20% - Dung dich chi thi methy! dé 0,1%etanol 60% ~ Dung dich chi thj phenolphthalein 0,1%etanol 60%. b. Céch titn hank Dang chit chi thi Buret (ng nhé gigt): dd baz (hay acid) chun. Krlen (binh tam gide): V (mi) dd seid (hay baz) + it nude efit tring thanh binh + vai giot chi thi, Mau cia dd tai diém cudi thay déi phy thude vao vj tri cua dd chun va vao chat chi thi duige sii dung. Néu dd NaOH duge chita trén buret vA chi thi 1a: - Bromothymol xanh; dd vang -> lve xanh (pT = 6,8) - Methyl dé: dd héng dé > vang (pT = 6,2) - Phenolphthalein: dd khong mau -» héng nhat (pT= 9,1) bén 1 phat, 4g PHAN Ding may do pH - Buret: dd baz (hay acid) chudn. - Cc thuy tinh 250mé: V (mf) dd acid (hay baz) + nude eat dén khodng 100m!, hing hai dign cue vao dd chudn 49, khuiy dd bling hé théng khudy tit hay khuay e¢. Doe tri s@ pH eda dd sau mdi ldn thém héa chét tir buret, Ngung chudn 6 khi da vugt qua diém tueng duce. 3. Két qua a- Xéo dink V;hoite Vig Dang chat chi thj: tinh V; tit 3 lan chudin a3. Ding méy do pH: ve dubng chudn 49 pli = (Ve) va tim Vis bang phuong phap hinh binh hAnh hod tim Vie bing phuong phép ndi suy tit sf ligu oda dutng vi phan bac 2. be Tinh nbng d6 ditong Ligng, néng db mol, nbng dé khdt Luong etter dil bhéo sét 3.1.2 Chuéin dé dung dich acid yéu bing baz manh Chuan d6 acid borie HyBO; bang dd NaOH, 1. Nguyen tde Acid borie HBO; dugc xem tuvng duong acid yéu HB (kus = 10°"), Khi duge chun 49 bing baz mgnh NaOH, edn bing chuéin 46 sé tang tinh dinh lung név them vao dd chudin 4 mot lung nhé mannitol (Ma) ¢6 kha ning tao véi B- thanh hai phil BMa (Bling, - 105) va B(Mae(B3Miqy, = 10°"). a Phan ting chuén do Trong méi truting cé mannitol (Ma): . K’ OU + HB == Ht + BO 4 Ma fn BMs,BA, Hing 86 can bing ditu kien K = Kx 01 peaq) VOl Gage) = 1 + 10 UMal + 10a Tei diém tuong duong: [OH] > (H"] => pHy> 7 b- Dinh diém cust Diing chét chi thi Thy néng 40 dung dich acid Ikhdo sét, tly lugng mannitol sit dung, tinh K’ va BH tuong dung tit 46 chon chat chi thi thich hp (thuéng ding phenolphthalein), Ding may do pH ~ Dien eye chi thi: thiy tinh hode hydro. BINH LUONG MGT SO OH VA PHAN TU TRONG OUNG OCH 45 2 Thite nghiém a. Hoa chat - Dung dich chudin NaOH 0,050N hay 0,100N. ~ Dung dich chi thi: phenolphthalein 0,1%/etanol 60%. - Mannitol dang bot. &- Cach tien hank Dang chit chi thi - Buret: Dung dich chufin NaOH. - Erlen: Vonl) dd mau HBO (+ m(g) mannitol) + it nvée ct trang thanh binh + vai gigt chi thi. Mau cla dd tai diém cudi; khong mau > héng nhat bén mét phat. Ding may do pH - Buret: Dung dich chudin NaOH. - C6 thiiy tinh 250m/: Vinl) dd mdu HyBOs + nue cat dén khodng 100ml (+ m(g) mannitol khudy tan). Nhing hai dign eye vao dd chuéin dd, khudly dd bing he théng khudy tu hay Ihufly ect. Poe tri 86 pH eda dd sau méi lin thém NaOH ti buret. Ngung chudin 46 sau khi vugt qua diém tuong duong. 3 Ret qué: a. Xée dink V; hoite Vir Diing chat chi thi: tinh V; tu 3 lin chudin d6 Ding méy do pH: = Vé dudng chudn do pH = Vox.) (6 va khOng cé mannitol). = Tim Vic biing PP hinh binh hanh hode PP néi ouy. b- Tink néng do duong lugng, néng dd mol, néng dd khot lugng etia HyBOs trong dung dich khao sét 3.1.3 Chudn do dung dich da acid bing baz manh Chuén a6 dd HsPO, bang dd NaOH. 1. Nguyén the @ Phan ting chudn d6 HsP0,+NaOH —* NaH»PO, +H:0 Ky = 107? NaH.PO,+NaOH = NaHPO,+H0 ky = 107 NasHPO, +NaOH =® NasPO,+H:0 kes = 10" Bue diém: ~ He > 4, nbung &ys < 10” nén trong diéu kign binh thudng, chi chudn do ha dude hai chive dau eta HPO, (chic 1 tuong duong don acid trung binh; chic 2 tueng duung don acid yéu). 46 mau tai diém cuéi PHAN _ Khi o6 mbt acid manh hoae trung binh bi in vio HyPO,, acid maah bods trung binh sé bi trung hda cing mét hie véi chife 1 ctia HePOx. ~ Khi bi lin yao mét acid yéu, acid yéu s@ bi trung hda cing mot hic véi chde 2 cia HPO. - 6 thé chudn 4d duge chic thi ba néu them vio dd chudin d@ mot it Ca” (Ca 88 tao phute hoae tao tia véi PO,* lam cho efin bing chudn d@ theo nae 3 sé c6 tinh dink ligne). b- Dinh diém cust Dieng chat cht thi pH tuong dung duge tinh gin ding shu sau: 2. PH g, ~ 5 (Pho + Phy) = 7 igo = (Phys + Bh) = 98 Xie dink diém cutii = Co thé ding chi thi bromocresol lye (3,8+5,4) hoje methyl da cam (3,1 + 4.4) 4é xée dinh Vier - Ding chi thi phenol phtalein (8,2+10,0) a8 xde djnh Vio. Dang mdy do pH - Dién oye chi thi: thiy tinh hoe hydro. - Dién eye chun: calomel hote AgCl 2. Thue nghi¢m a Héa chat - Dung dich chuda NaOH 0,050N hay 0,100N - Dung dich chi thi bromocresol Iye 0,1%/etano] 20% = Dung dich chi thi methyl da cam 0,1%inude - Dung dich chi thi phenolphthalein 0,1%/etanol 60%. b. Céch titn hanh Ding chat chi thi - Buret: Dung dich chun NaOH. - Erlen: Virnl) dé mau H3PO, + it nuGe c&t tring thanh binh + vai giot chi thi ‘Dramocresol luc + vai giot chi thi phenolphthalein. Mau cia dd tai diém cus -Thé nhat: vang -> lye xanh (pT = 4,6) - Tht hai: xanh —> xanh tim (pT = 9,1), Ghi ehii: Néu ding methyl da cam + phenolphthalein lam chi thi, sy chuyén - Tha nhét: héng cam -» vang (pT = 4,4) -Tha hai: vang -> vAng ndu (pT = 9,1). BIH LUGNG MOT SO iON VA PHAN Tl TRONG OUNG DICH 47 Ding may do pH - Buret: Dung dich chudin NaOH - Cée thay tinh 260md: Vind) dd mau HPO, + nude cét dén Ahoang 100m, Nhiing hai dign eye vao dd chudn 49, khudy dd bang hé thong khudy tiz hay Khudfy ed. Boc tri 86 pH cia dd sau mdi Min thém NaOH ti burst. Ngumg chudn 46 sau khi yugt qua diém titeng duong thi hai, 3 Két qua a Xe dink Via vd Vier (Vigo 1a thé tich OH’ ding dé chudn d@ hai chite ddu). Diing chat chi.thi: tinh Vier va Viao tit ba lan chudin ag. Dang may do pH: = Ve duting chutin 40 pH = AViacr) Tim Veer va Viao bing phuong php hinh binh hanh ho&e bling phuong phép noi suy. 8. Tit Via: va Vise eho ket ind vé sy hién dién cia ede acid trong dd mau. o: Tinh nding dé dung higng, néng dé mol, néng do khéi Ivgng ofa HPO, trong dung dich khdo sat 8.1.4 Chudn dé dung dich da haz bing acid manh Chun 49 dd Na,CO, bing dd HC! hay H.S0,. Je Nguyen tde @- Phan ting chudn do Na,CO, +HCL == NaHCO, + NaCl ky. = 10 NaHCO; + HC] = HyCOs + NaCl ky = 10° Bate dhiém: - Na;CO, la mudi ciia diacid yu H2CO; va baz manh NaOH nén thé hign tinh baz theo hai chite. - Pied va k, 2107 = chulin 49 duge time chite eta NaCO, (che 1 xem ba nhit baz trung binh yéu, ehife 2 1a baz yéu). - Khi cé mét baz manh hode trung binh bi 4n vao Na,COs, baz manh hote trung bin sé bj trung hda cing mot lic voi che 1 eda NazCOs. - Khi bj lin vao mét baz yéu (vi du NaHCO,) baz yeu sé bi trung hoa cing mét hic véi chic 2 cla NasCOs. & Dink diém cust Dang chat chi thi Gi tr} pH tai cde diém tuong duong: Pye, = (Phe, + Bhy,) = 8895 EY 48 PHAR pHao ~ 4 (tay thuge néng db HCO, trong dung dich) C6 thé xée dinh hai diém cudi bing hai chi thi: phenolphtalein (8,2 +10,0) va metyl da cam (3,1 + 4,4). Diag may do pH - Dién eye chi thi: thiy tinh hode hydro = Dién eye chun: calomel ho&e AgCl. 2. Thye nghigm a Hoa chét = Dung dich chun HCI 0,050N hay 0,100 ~ Dung dich chi thi phenolphthalein 0,1%/etanol 60% ~ Dung dich chi thi methyl da cam 0,1%nuée. b. Céeh tidn hank Ding chat cht thi Dung dich chuain HCl 2 Vind) dd mau NasCOs + it nude cit tréng thinh binh + vai gigt chi thj phenolphthalein. ‘Mau cia dd tai diém cudi thi mhat: héng > khong mau (pT = 8,2). ‘Them vai giot methyl da eam, chudn d6 tip, Mau eda dd tai diém cudi thit hai: vang -> cam (pT = 3,8). Ditng méy do pH ~ Buret: Dung dich chudn HCI. ~ O6e thiiy tinh 250ml: Vonl) dd m&u Na,CO; + nuée edit dén khodng 100ml. Nhiing hai dién cue vao dd chuén 46, khuiy dd bang hé thong khudy ti hay Khudly co. Dye tr} sO pH cia dd sau méi lan them HCI tir buret. Ngung chudn 4¢ sau chi vugt que dim tuong duong thit hai. 3: Két qua @ Xée dinh Viay va Vice (Wag la thé tich HCI ding dé chudn 49 ed hai che) Ditng chat cht thi: tinh Vea va Vias ti 8 lan chudn do. Ding’ may do pH: - Vé dudng chudn 4 pH = AVxci) - Tim Vier va Vise bang phuong phdp hinh binh hanh ho&e bang phuong phép ndi suy. & Te Viai ve Vice cho két lugn vb sy hitn dién ofia cdc baz trong dd mau. © Tinh néng dp duong long, ning d6 mol, néng dp khdi Ingng eta NasCOs trong dd khdo sat. BINH LUONG MOT SO ION VA PHAN TU! TRONG DUNG DICH 49 3.1.5 Dinh d6 kiém etia mét mau nude 1. Nanyan te _ Miu nutie duge goi Ia nutéc kiém khi chita ion OH", CO,” hotle HCO,” hoe hon hgp 2 trong 3 ion: (OH + CO;* ) ho&e (CO; + HCOr ). BO kiém cia mbt mau nude duge xAc dinh bing eéch chudn 4 mau nude kiém véi mOt acid manh, vi dy HCl hose H,80,. @ Dink diém cudi Ding chat chi thj Xéc dink hai diém cudi bang hai chi thj phenol phtalein va metyl da cam. Ding méy do pH - Bign eve chi thi: thiy tinh hose hydro 2. Thue nghigm a. Héachét ~ Dung dich chudin HC] 0,050N hay 0,100N - Dung dich chi thi phenolphthalein 0,1%/o6n 60% = Dang dich chi thi mothy da eam 0,1%/nv6e. b Céch tién hank Dang chat chi thi - Buret: Dung dich chudn HC] ~ Erlen: Vil) dd mau nue kiém + it nude eat trang thanh binh + vai git chi thi phenolphthalein. Mau eda dd tai diém cui thir nhi‘t: hdng —> khéng mau (WT = 8,2. ‘Them vai giot methyl da cam, chuén do hai: vang -> cam (pT = 3,8). Dang méy do pH - Buret: Dung dich chun HC] = C6c thiy tinh 250ml: Vie) dd mau nuéc kim + nude cit dén khodng 100ml. Nhing hai dign eve vao dd chuén 46, kchudy dd bling hé théng kkhudy ti hay Ichudy ca. Doc tri sé pH oiia dd sau méi ln thém HCI tii buret. Ngung chudn d6 sau hi vutt qua tat ca cdc diém tong duong. Mau cia dd tai diém cuéi thir = DO kiém p: do kiém ting véi ede ion hién dién khi duge chudn do bing dd acid vdi chi thj phenolphthalein (thé tich Vian, on duge ki higu 1a V;). - Do kiém m: d@ kidm ing véi cdc ion hién dign khi duge chudn do bing dd acid véi chi thi methyl da cam (thé tich Vin, con duge ki higu la Vy, tinh ti lve bat déu chudn do dén khi metyl da cam chuyén mau). Bon vj dinh d9 kiém: 1 d (My) = Img CaCOyl. 50 PHAN 3 a- Xdc dinh Vp 0G Vig Ding chét chi thi: tinh Ve va Viz ti 3 lan chudn dp. Ding my do pH: - Ve dutng chudn do pH = (Vic) - Tim Vp va Vr biing phuong phap hinh binh hanh hoie bing phuing php nai suy. b- Tie Ve va Vy cho két lugn vé sy hign didn eda cde ion kiém trong mau nuée: aapaaReae éttugn suhien cen ‘ThE tich de acid manh_ ina he : ei tom bem or cor Hs Ven Vu on Ve e 0 il Vv: Vet HOO 9 Oo Ww Vn =2¥e coe oO avy oO 2Ve < Vu HEDy + COs _o "| 2Ve Vu- 2p 25 Vw Of + COs” Ve —Vu Bia - Ve) o - c- Tinh d kiém do titng ion gay ra theo don oj de kiém M3 3.2 DINH LUGNG ION Ag* 3.2.1 Dinh lvgng ion Ag’ theo phuong phap khéi lugng I. Nguyan tée Ding dd Clr tao tia véi dd Ag* theo phan ting: Ag’ +Cr © AgCl Tye = 10° Die diém: - Tha AgCl luc diu d dang keo, duge lam dong tu bing cach dun nong va Jie dd chia tda that manh. ~ AgCl tan khong dang ké trong méi trugng HNO, loaing (khodng 1%). ~ AgCl thay vdi anh sing nén cin tao tia trong tsi hoac trong ede cée co mau sdm, - Clin loai &nh hudng cila céc ion 06 thé tao tia vai Ol (PH, Cut, Hew): + Oxy héa Co’, Hg¢** bing dd HNO; dd truée khi tao tia. + Loai anh huting cia Pb* bing cAch pha loding dd dé ham lugng Pb**< 1,252, seu d6 méi thém cham dd HCl dé tao tia AgCl. Cae ion bi thiy phan trong méi trudng acid loang (Bi, Sb) khOng duye phép hign din. 2 Thue nghiem @ Hoa chat - Dung dich HNO, 0,1M; ——_- Dung dich HNO, 0,01@ - Dung dich HCl 0,2; - Dung dich AgNO, i%/nuiée. DinH LUNG MOT SO 1ON VA PHAN TU TRONS DUNG O1CH st b- Cach tin hank Teo tia - Céc thiiy tinh 250m: hit Vol) dd mau (chita khoing 0,1g Ag) + dd FINO; (tao moi truding HNO, 1%). Dun dd déin ichoding 70°C. Thém chim dd HCI 0,2M, khudly déu. ‘Trinh khong tao tia noi qu sng va ding qua du HCl. Dun nong cho dén khi tia ket ‘yén lai, lam ngudi dén nbiét do phong. Thém vai gigt HC] dé kiém tra qua trinh tao ‘tia da hoan tokn chua, Dé yén tla trong béng tdi vai gié hose qua dém Loe, rita va sddy tha - Ege tia qua chung Ipc Gooch hose chung lee sit hay chung thiy tinh (da say kb6 VA ean trudc), Ria tha bang dd HNO; 0,1M va rita lai baing dd HNO; 0,01 cho dén khi dd qua Igc hét ion Cl (kiém tra bling dd AgNOs). - Say tua, du tien 6 100°C va sau d6 nang lén 130 + 150°C dén khi khdi lung tia khang edn thay Adi. BE ngudi trong binh hit dm va edn. a. Ket qué Tinh néng dé mol, néng 46 khdi luyng cia Ag’ trong dd khdo sét. 3.2.2 Chudn do dung dich Ag’ bing phuong php Volhard I- Nguyén ide Ding dd KSCN hay NH,SCN chudin 46 dd Ag” véi chit chi thi phan s&t ba. a- Phan ing chudn dé Ag’ +SON" =e b- Dinh diém cudi Dang chi thi tao phi phén s&t ba; vdi lugng nhd SCN™ ding thita: Fe +SCN” == FeSCN* Begiye. = 10°? Dae diém: + Méi trudng can 06 pH khd acid dé trénh tgo tia Fe(OH), nhung eGing khong duge qué acid vi sé anh hudng dén dd bén eda phite FeSCN* (pH thich hyp thudng tU 0,5 + 1,5 ), Tao moi trutng acid bang HNOs, + Phuc FeSCN™ ¢6 mau dé -diéu kign dé mau xudis hien 10 1a [FeSCN*]=7.10°M ya [SCN] > 3.10°M. Bé c6 su tao phite gin diém tvong duong, [Fe] ~ 0,2M Gai sd = 0,1%). - Dung dich khong duge chita HNO: vi s@ tao mau d6 vsi HSCN. - Chudin 46 6 nhiét 4 thutng vi nhiét 46 cao s@ lam mat mau aia chi thi. - Phusng phdp Volhard thutng duse sit dung dé xée djnh ham luyng cia Ag trong ede hgp kim. Céc kim loai ding hign dign m& mudi cia ching 6 mau (Co, Ni, Cu - néu ham lugng cia Cu trong h¢p kim > 40%) anh huéng dén két qud xée* dinh Ag’. Muéi eda céc kim loai khong mau kh6ng anh hudng dén két qué xe djnh ‘Ag? try Hg’*, Pd (vi dang thiocyanate cia ching khong tan). 2 PHAN + Co thé si dung phuong phap Volhard dé chudin do Cl, Br, | theo céch chudp 49 nguye (thém lugng thita chinh xé¢ Ag* vao dd CI, Br, 1; chudn 49 lai lugng Ag’ bing dd KSCN hay NH,SCN). - C6 thé thay chi thi phén st ba bing chi thi tartrazine 0,5%/nuéc. Sy hién dign cia chi thi tartazine sé 1am cho tlia AgSCN 06 mau vang nhat trong sudt qué trinh chudin 46 va dd bén irén tir khong mau sé chuyén thanh mau vang chanh tai diém eusi, 2 Tayo nghigm @- Hoa chét - Dung dich chugn KSCN hay NH,SCN 0,100 = Dung dich HNO, (1:1) ~ Dung dich phén sat ba Fe(NH,)(S0,)..12H,0 bao hda (~ 1M) b. Cach tign hank - Buret: Dung dich chuén KSCN hay NH,SCN. > Brien: Viml) dd Ag’ + it nuée oft trang thanh binh + v(mé) dd HNO, (1:1). ‘Them lugng thich hgp ehi thi phen st ba, Chudn do cham bling dd chuin KSCN hay NH.SCN. Mau cia dd tai diém cui: vang nhat ¢6 tila AgSCN trAng dye > mau cam nhat. 8 Ket qué -Xae dinh Vy tit 3 lan chun do. - Tinh néng 46 mol, néng 44 khdi lugng ea Ag* trong dd khdo sét, + Ong dung Xac dinh ham lugng Ag trong mau hop kim. Can chinh xie khodng 2g mau, chuyén vio arlen 250m. Thém Sml nude + 10mi HNO; dd. Day erlen bing m9t phéu nbd, Dun dén tan hoan toan hop kim. ‘Tham nuée va dun 6 phat dé dudi NO,, Lam ngu6i dd va dinh mde thanh 100,0mé. Mut 25,00mnt dd + 2mé dd HNO; (1:1) + Imd dd phen sit ba bao hda hoac 4 giot dd tartrazine 0,5%. Lic manh huyén phi va chudn d6 bing dd KSCN 0,100. ‘Tinh néng 49 phan tram eda Ag trong mau hgp kim. 3.2.8 Dinh lugng ion Ag’ theo phuong phap dién khéi higng I- Neuyén tie Bae duge xée dinh him lugng bling ech dién phan trong méi trusng NOs, NH hoge CN’, ‘Trong dd CN*, bac hién dién chit yeu & dang ion phite: [Ag(CN)ay =e Ag’ 4 20N- va {Ag(CN)} + le = Ag + 2CN™ INH LUONG MOT SO ION VA PHAN TH TRONG DUNG DICH 53 Déte dim: Bge duge téich Ichdi Cu, Pb nhung nhiéu kim logi khac o6 kha nang phéng dién cing véi hae. ~ Khhi phan tich eae mudi bac khong tan (AgCl, AgBr, Agl, AgC20x..), ¢6 thé hda tan trye tigp ede mudi nay trong dd KCN. 2. Thye nghigm ~ Cée thiy tinh dign gidi 600ml: hét Vim!) dd mau (chita khoding 0,2¢ Ag) hien dién du¢i dang nitrate. Thém KCN ran cho dén khi tia AgCN bi tan tiép trong KCN thanh phic [Ag(CN),] ~. Thém khodng 0,2g KCN. Pha loang dd thanh 100 + 120ml. - Nhing ede dign eye (cathode Pt; ancde calomel) vao dd dién phan. Bign phan dd @ diéu kign: I = 0,2 + 0,54; AE = 3,7 = 4,8V; t* = 20+ 30°C. Luong Ag phong thich O,1g trong 3 gi Hole dién phan véi dién cyo quay 6 didu kign: I = 0,5 + 1A; AE = 2,5 + 4,2V. Lafong Ag phéng thich 0,2¢ trong 20 + 25 phat. - Kidm tra qué trinh dign phén hoan ton chita bing ech Idy vai giot dd dién phan cho vao 6ng nghiém, acid hoa bing HNOs, dun duéi HCN (rat dc). Tao moi truding NH va thém vao dd vai giot (NH,)S. Khéng thay xudt hién tia néu AgS nghia lA Ag da hét. 8. Két qué: Tinh tuong ty nhu phwong phap khéi lugng. 3.3. DINH LUQNG ION AI* 8.3.1 Dinh Iigng ion Al” theo phuong phap khdi !vgng J. Nguyen tde Ding NH,OH tao tia vai dd Al* (rong ay hign dién ciia NEC) theo phan img: Al’ 4 30H” =® AMOH)) Taxon, = 10% Dee diém: - Téa AVOH)s ¢6 mau trang, 6 deng vo dink hink, ¢é tinh lugng tinh nén edn tao tia trong mbi trutmg 6 pH thich hgp (6,5 + 8,5) tay ndng d Al ban du trong dd 4é trénh ede sai sido: AIH) + 3H? == Alt + 3H0 hose AM(OH) + OH” _ Aly + 24,0 = Vide kiém soat pH tao tia duge thye hign bAng chi thi methyl 45 hoc bang cach tao moi truéng d@m voi NH,Cl. Ngoai kha nang tao dem, NH,Cl cdn €6 tac 54 PHAN dung lam dong ty tia AKOH); dang keo, han ché dén mde toi thigu ede qué tinh dang tao tla cila céc kim loai héa tri 2 (Ca”*, Mg”...). - Tau tia voi dd néng, 44m dae, thém nhanh NH,OH va chat dign ly 46 gidm hép phy. = Téa duge rita bing dd NH,CI hoge NH.NOs 2% (khéng duce rita bang nude néng vi tia AKOH), ¢6 thé trd Iai dang keo (qua trinh peptise héa). ~ Loc sau khi tao tia 5+ 10 phit, bing phéu thiy tinh va gidy loc bang dé Goai Khong tro, méng) va duge nung 8 800°C dé chuyén hoan toan sang dang cn Aly. Ba han ché qué trinh hut 4m cia dang edn, tét nhat la nén nung tie them 10+ 15 phut 4 1200°C. ~ Gn logi anh hudng cla cdc ion c6 thé tgo tia hydroxyd. Néu dd e6 Fe", chi xde dinh duge téng ham lugng Al va Fe" (dang e€n thu duge gém Al,O,+ Fe2Od). - CAn Ioe bd cain Io ling khong tan trong dd truge khi tgo tda. 2 Thue nyghiom @- H6a chat - Dung djeh NH,OH (1:1) - NH,CI rin - Dung dich NH,NOs 2%/nuée (duve trang hoa bang NH,OH voi chi thi methyl 48) + Dung dich cht thj methyl 43 0,2%/etanol 60% - Dung dich AgNO; 1%inude. b- Cach tin honk Teo tia + Céc thdy tinh 200ml: hut Vonl) dd mau chia khodng 0,1g Al” (da Toc bo cin khéng tan, néu can). Néu dd mau qué dam 4&c, thém lugng nude eft ti thiéu dé tang thé tich dd ung véi luong eda dang tia v6 dink hinh duce tao thanh. Thém 5g NH,Cl. - Dun vita sbi dd + vai giot chi thj methyl 46. Thém timg gigt (vita thém vita khuily déu) dd NH,OH (1:1) din khi mau dd chuyén tit 43 sang vang. Dun dd 1+2 phot. Loe, rita va nung tthe - Lge tia qua gidy loc méng, khéng tro (gidy bang 48). Rita tha bing dd NH.NO; 2% néng cho dén khi hét Cl’ (kiém tra bling dd AgNOs, sau khi acid hoa dd qua Ige bing HNO;). + Gdi tia cho yao chén sif hoe chén Pt (da nung truée # 800°C va can), Dét 6 ngoai bp dign cho ta gidly loc chéy thanh than, cho chén st vio Ib nung 800°C trong 30 phat. Nang nhiét 46 lén 1200°C trong 10 + 15 phat. Dé ngudi trong binh hit dm va can. 3 Kot qua + Tih néng d9 mol, néng 4 kh6i lugng ciia Al’* trong dd khao sat. - Tinh néng do phéin tram 6 dang hgp cht Al,O, trong mAu rin. BINH LUONG MOT SO ION VA PHAN TU TRONG DUNG DICH 85 3.8.2 Chudn d6 dung dich Af* bling EDTA (chuan d6 ngugc) 2: Nguyen tde a Phan ing chudn do ‘Trong méi tru’ing pH 5 +6, thém luong thita xée dinh EDTA vao dd Al*: FRY? + AI" s® AIY-+2H" Bi, = 10%" Chuan a9 lugng EDTA thita bang dd M*: M™4H.Y" © MY? 42H" ‘M® ¢6 thé Ia Zn™, Pb" hoac Cu* Dito diém: = Ding edch chudn 4@ nguac vi phic ALY bén J nhiét do Khodng 80°C (edn dun dé trude khi chun 49 ligng EDTA thita). - Dé trainh can biing phy: Al 4 30H” == AIOM)s Tyo, = 10 edn pha long dd AI™ bing lvong nude ea thich hyp trude khi chun 4. - Két qua chudn 49 chi ding khi dd cht chute Al (cao ion Fe, Cu”, Ni”, Pb", Ti*,2n*; Zr, Sn” du tao phic bén vdi EDTA ¢ diéu kign chudia dé Al), - Trong cdc mau thién abiéa, hién din ééng thei voi AI* thudng 1a Fe". 06 ‘thé Joai anh huéng eda Fo" bing each ding EDTA tao phite bén FeY" ¢ pH 25 (xem edch chun dj Fe" bing dd EDTA). - Néu M®* la Zn®, phan ting tao phtic ZnY” xdy ra nhanh ¢ abiét dO cao (nén ehudn do khi nhiet do dd khodng 60°C). - Dé tang tinh chon loc cho phan Ung chudin do Al* c6 thé thy hign tiép phep chudn @) thé: cho mét lugng KF (NaF hose NEF) vio dd sau khi chudn do nguve ‘AI xong, F° tao véi Al* than phite AIF” bén hon phite AIY rat nhiéu nén sé day YY" ra kchdi phife AIY”. Chufin do lugng Y* bi day ra bang dd M™ (Zn* hay Cu”), ‘Thé t{eh eda dd M® sif dung sé ding dé tinh cho him lung cia Al’ ¢6 trong mau. Khi chun €6 theo céch nay, ket qua sé chi edn bj anh hudng bai Ti*, Zr", Sn”, b- Dinh diém cust Dang chi thi phtic kim logi o6 dang téing quat HaInd. Can bang chi thi: M*4H,Ind 3= MInd"® + mH" - M™ 1a Zn® hay Pb: chi thi thutmg ding la xylenol da eam (Ind: ving; ZnInd hay PbInd: 4). --M? 1a Gu": chi thi thudng ding 1a P.A.N (ind: vang: Culnd: héng). Can loai anh hudng ciia ce ion ob kha nang tao phite bén véi chi thi. Dé dé nhin mau tai diém euti, e6 thé thém vao dd chudn dQ vai gigt bromocresol luc. 56 Pune 3 2- Thite nghig¢m @- Héa chat - Dung dich chudn EDTA 0,0100M - Dung dich chudn M** 0,0100M - Dung dich dém acetate (tao pH 5) - Hexamethylenetetramine (hexamine) ran (tao pH 6) + Dung dich NH.OH (1:1) - NaF (KF, hoac NH,F) rin - Dung dich chi thi xylenol da eam 0,1%/otanol - Dung dich chi thi P.A.N 0,1%/etanol = Dung dich chi thi bromocresol lye 0,1%6/etanol 20%. b- Cach tin hank Chudin d nguge - Buret: Dung dich M™* chudin ~ Erlen: hit Vonl) dd méu, loai Fe**. Thém nuée cét thich hgp. Thém chink xac lugng thita EDTA + vai gigt chi thi bromocresol Ie. Thém ting gist NHLAOH cho dén khi dd chayén tir vang sang lye xanh (pH 5) + 2md dd dém pH 5. Bun dd gin sdi (80°C), Thdm 2ml dd dém pH 6 + vai giot chi thi. Chudn dé (tic dd dang néng) bing dd M**, Mau cia dd tai diém cus + Vang lye —> cam tim néu ding xylenol da cam + Vang lye > tim néu ding P.AN, Chutin dp thé - Buret: Dung dich M™ chudin ~ Erlen: Sau khi chaén do nguge xong (xem phn érén), thém 0.1g NaF rén + 2ml dd dim pH 5. Dun néng 80°C, dd trd lai mau yang luc. Them vai giot chi thi P.A.N hode xylenol da cam + 2ml dd dom pH 5, chuéin dp bling dd M°* an khi dd cé mau (cam) tim. Ghi nhan thé tich dd M", Thém tigp 005g NaF rin + 2mi dd dém pH 5 va tiép tue qué trinh chudn do cho dén khi dd IhOng con tnd Agi mau vang luc sau khi them NaF. Ghi nh§n téng thé tich M® da sit dung. 3. Két qué -Xae dinh Vy tir 3 lan chudn a} + Tinh néng d6 mol, nng d6 khdi lung eda Al trong dd Ithdo eat - Tinh néng d9 phan tram 4 dang hyp chat ALO; trong mau rin. Ghé ehii: Con c6 thé chudn do Al" big EDTA theo edch chudin dd nguge & pH 7 +8 (nang pH bang dd NH,OH 1:1), st dung kim loai M® la Zn? voi chi thi Eriochrome Black T 0,2%/etanol, Thue hién tuong ty nhuf trén nhung khong ding ehi thj dom mau Bromoerosol luc. Mau eda da tai aiém cudi: xanh > dd. 3.8.3 Dinh lugng ion Al” theo phuong phap quang phé hip thu thy duge Al duge tao phute v6i ligand L, thuéing 1A Aluminon hoe Rriochrome Cyanide R thanh phée ¢6 mau. Bo 4 hap thu eiia méu va dinh lugng bling eéch lap dutng chuéin. BINH LUNG MOT SCION VA PHAN Tif TRONG DUNG DICH 57 A- PHUONG PHAP ERIOCHROME CYANIDE R 1 Nguyen tie Trong mdi trudng pH 5,9 + 6,1; Al’ tao voi Briochrome Cyanide R thanh phite e6 mau dé tim (rgye ¥ 585nm), hé 86 bap thu mo] 40.000mo!'cm™ 1. Date diém: ~ Phyong phép thung due ding xée dink ham higng AI* trong nuée sinh hoat va nue thai (mién néng d6 Al t0i uu tir 10+ 250ug/)). - Dp nhay eda phuong phdp khodng 3ygil khi khong ¢6 mat cla F va cée phtic chéit phosphate vi edc efiu tit nay gay sai sé am (loai nh hudng cia F bing cach lap chudn trén nén méu; orthophosphate duye dua vé néng dd < 10mgit dé khong gay anh hudng bang cdch trung hda bang dd NaOH loang ti pH 4,3 + 4,5). - Zn®*, Ni®*, Cd, Mn” gay anh hudng khong dang ké d&n két qua phan tich, nhung Cu va Fe phai ving mat. - Dé higu chinh anh hudng cia mau hoe dd duc cia mau, chudn bi mot mau tring bing cach thém EDTA vio mfu (48 tgo phite véi Al) va acid ascorbic (4 loai trit anh huéng cia Fe va Cu). 2 Thige nghigm a. Héa chat ~ Dung dich Al?’ zmgil (pha tis dd chudn gée 1000mg/) ~ Dung dich dém pl 6 (dem acid acetic - acetate) - Dung dich NaOH 0,2M va HCl 0,2M - Dung dich acid ascorbic 0,1%/nuthe (pha trusie Khi ding) = Dung dich chi thi Eriochrome Cyanide ft 0,4%inude b- Cach tién hanh Pha loat dd chugn va mau trong Binh dinh mite (BDM) 100,0m ad chun ‘i mis ] TN ee oe ee ee ee | Viz amatimy | ooo | oso | 00 | 500 | wo | ws | - g. Son 06") > | 1 | 4 | 100 | 200 | 250 2 v [vw [vw dd gem pit 6 ae = 3.00, 5.00 Enoohrome Cyanide R sng 9.4% (my) = (26 nipnu A (¢) Tham khong 40.<£0mI nue edt *) Bidu chin pH ola do dén xp x16 bang dd NaOH 0,2MIHCI 0,2M truce kni hem da dem inh mue ngay bing nude edt, Lac déu, dé yen 5~10 phat, do dP hdp thy & 52Sam tong cuvet eb b= tem. 58 Peat 3 Ret qua - Ve dutmg A = flCw) - Xée dinh néng 46 AF* trong dd do tiy 43 thi ho4c bing phuong phap binh phuong eve tiéu. + Tinh néng do Al’* trong mau long (mg/l) hode trong mau rain (mg/kg). B- PHUONG PHAP ALUMINON J+ Nguyén tac O pH 5, Al tao véi Aluminon thank phie 6 mau d8 tim (max © 525nm), hé 86 hap thu mol khodng 24.000mol em ‘i. Dac diém: - Phuong phap thutng duve ding xée dinh ham Ivong Al trong nude sinh hoat va nude thai. - Mién néng 46 Al** ti uu ti 100 + 600pgi2 + Be** gay sai this, F” gay sai thiéu lén két qua xée dinh Al*. 2 Thue nghigm @- Hoa chat ~ Dung dich AP* Sing (pha tirdd chudn gO 1000me/l) - Dung dich d@m pH 5 (dém acid acetic - acetate) ~ Dung dich NaOM 0,2M va HC) 02M - Dung dich chi thi Aluminon 0,14%/nu6e. b> Cach tin hank Pha loat dd chudn va mau trong binh dinh mite (BDM) 100,0ml dd chuén “| dd mau to phe . E = @[eleleale Mi ee Eys. feof) ° 300 200, 300. 400. 500 Somes 500 E00 Alumina 0.1% nt) 5.0 5.09 Bonin RIA [ L_] () Them oding 40+ 5Somi nude cat. Bu chinh pH clia dd Bn xp x15 bing dd NaOH O.2MHCI 0,2M (*) Binh mic ngay bing rub cAt Leu, a8 yon =10 pt, do-dB hp thu & E2Enm rong cuvet ob b= tom. 3- Két qua: Tinh tuong ty PP Eriochrome Cyanide R. DINH LUONG MOT SO ION VA PHAN TU TRONG DUNG DICH 3 3.4 BINH LUUNG ION Ba’ 8.4.1 Dinh ligng ion Ba” theo phudng phap khéi ligng 1- Nguyén tdée Ding dd SO," tao tia vai dd Ba* theo phan ting: Ba +S0,* = BaSO, Tyaso, = 10°°? Dae diém: - Tada BaSO,c6 mau tring duc, & dang tinh thé min. - SO? duge cung cap dudi dang H,S0, dé 48 loai b3 Iugng thita trong giai doan log, rita va nung. - Cae ion kim loai Ca’, Sr, Pb", Hg”, Sb**, Ag*, Bi** gay anh hudng dén Ieét qué xde dinh Ba® do cfing tao tha véi SOF. = Cin tao tia trong mdi truéng acid véi dd néng, loding, thém chiim thud thi, Khudy déu aé thu duge ta tinh thé to (se thuan Igi cho qua trinh loc va ra ‘tia cing nhu tang €Q chinh xc cia phusmg phép phan tich). - Sau khi tao tia, dun céch thy 15+ 30 phat (hoc hon nia, néu o6 didu lin) é tinh thé hat tha phét trién ln Jén. ~ Tia duge Iye bling phiu thay tinh va gidly loc bang xanh (loai khong tro, day) va duge nung 6 800'C trong méi truéng di oxy dé trénh cén bing phy do phan tmg khif cia C (gidy loc) anh hudng len dang can BaSOy BaSOQ,+4C —* BaS + 4CO 2 Thue nghiém a- Hoa chat - Dung dich H280, 0,2M@ &- Céch tién hanh Tao tia = Ce thiy tinh 100m/; hit Vind) dd mau (4a ge bé c&n khong tan) + nude eit én Khoing 7m. Dun dd vita sai. Thdm chm 10+20mi dd H.80, 0,2M néng (vita thém vita khudy déu). Dun ech thay 15+30 phat. Lge, rita vd nung tika « Loe tia qua gidy loe day Ikhéng tro (gidy bing xanh). Rita tia bling nude néng = Géi tha cho vao chén st (d& nung trude & 800°C va can). Dét & ngoai bép ign cho tY gidy loc chdy thank than, cho chén sit vao I nung & 800°C dén ‘khdi luong khéng déi. Dé ngudi trong bin hat 4m va can. & Két qua: Tinh ndng d9 khéi lugng cia Ba” trong mau léng hode phan tram khdi lugng & dang hyp chat trong mau ridin. 6 PHAN 3 3.4.2 Chudin dé dung dich Ba” bing EDTA (chun do thé) 1 Neuyén tée @ Phan ting chudn dé ‘Trong mdi trudng pH LO, vai sy hién dién ela MgY?: Ba +MgY" s= Mg?’ 4 Ba? Chuéin d@ lugng Ba” cdn Iai va higng Mg? HY? +Ba” == BaY* + 2H* HAY + Mg" == MgY* + 2H" Bac diém: ~ Dang PP chuiin d9 thé gitp xée dinh diém eudi thuan Joi hon ehuén a6 tna tiép. + Co", Ni, Cu, Ce”, Zn™, Hg"... tao phite bén voi EDTA d pH chun 49, can logi anh hung bing céch thém vao dd mot luyng hydroxylamine, hydrochlodrie NH,OH,HCI (dé khif cdc ion kim loai-vé hoa tri thé’p hun) hay KON (che duéi dang phite cyanide). ~ Mg”, Ga’, Pb**, Mn™, Sr", Ga* cling tao phite bén vi EDTA 6 pH 10 vi kchdng thé loai anh hudng bing NE,OH,HC! hay KON. + Lugng MgY* sit dung phai thich hgp {{Mg¥*] = 10-4 10M) dé sinh re Mg’ dit tao dang phute mau véi chi thi Phan ting tao phuc MgY* nhanh 6 nhiét d) khodng 60°C. &- Dink diém eubi Ding chi thj Briochrome Black T Can bing chi thi: HY? + Mgind == MgY* + Ind + 2H" (Ind: mau xanh; Mglnd: mau 48) Dae diém: cén loai anh huting ea eée ion e6 kha nding tao tia hydroxyd hote tao phic bén véi chi thi nhur AD, Fe, Céch logis ~ Tao tia hydroxyd 5 pH 7 (kiém tra pH bing chi thi methyl 48) va lge bé tia (khi Al®, Pe 06 néng 46 kha |én). ~ Che bing CN”hay triethanolamine TEA (khi Al, Fe® c6 néng d6 bé). 2. The nghigm a: Héa chat - Dung dich chudn EDTA 0,0100M - Dung dich MgY* 0,014 - Dung dich dém pH 10 + Dung dich NH,OH (1:1) ~ Dung dich NH,OH-HCI (1:1) - Dung dich KON 10% nude ~ Dung dich TEA (1:1) ~ Dung dich chi thi methyl 46 6,1%/etenol 60% ~ Dung dich chi thj Eriochrome Black T 0,2%/etanal. BINH LUOWG MGT SO iON VA PHAN TY TRONG OUNG DjCH ot b- Céch tién hank - Buret: Dung dich EDTA chudn ~ Cie thy tinh 100mL: hit Vimnl) dd mau + luong nude eft thich hop. Dé loni dah hudng cia lugng 1én sat va nhOm, dun néng va cho vao dd vai gigt chi thi methyl d6. Thém timg giot NH,OH cho én khi dd chuyén ty dé sang vang, Loc bé tha AKOH); + Fe(OH);, Hing dung dich vao erlen 300ml, ~ Thém vao dd 1nd NH;OH-HCI hay mi KCN houe TEA + 3ml dd dem pH 10+ u(mi) dd MgY* + vai gigt chi thi Briochrome Black T. Chudin d6 bing dd EDTA. Mau ofia da tai diém cudi tt cam —> lye. 3. Rét qua ~Xée dinh Vy ti 8 lin chudn 43 ~ Tinh néng d§ mol, néng 46 khéi lugng cia Ba” trong dd khao sdt - Tinh néng 4} phan tram é dang hgp chat trong mau rén. 3.5 BINH LUQNG ION Cat va My? 3.5.1 Dinh ligng Ca™ bang phuang ph4p kh6i lwyng 1 Nguyén tée Dang dd oxalate C,0,? tac tia voi dd Ca™ theo phan tng: Ca® + C.0,2 + HO == Ca0LthO Treo, = 10 Dite diém: - Téa CaC,0,.H.O 06 mau trang dye, 06 thé duge en & dang CaC,0,.H,0 sau Ichi sily ¢ 100+ 108°C (két qua thudng bi sai tha 0,5 + 1%), - Dang cfin cing ¢6 thé 1A CaCO, néu nung tia CaC,0,.H,0 6 475 + 626°C hoe CaO néu nung tia 6 1200°C. ‘ - Céc ion kim loai Ba®, Cd**, Pb”... gay Anh hudng dén két qua xc dinh Ca* do cing tgo tia bén véi C20, + Khong due tao tiia trong moi trvng acid dé tranh sy tan tila CaCO, (moi truéng thich hyp 06 pH 2 4). - Thude thit néng, lofing duige thém chim vio miu chia Ca (eing néng, loing), kchudly du dé thu duge tia tinh thé to. + Sau khi tao tua, dé yén dd tao diéu kién cho tinh thé hat tia phat trién lon len, - Tia duge lge va duge chuyén sang dang din véi phuong tién va cach thie phy thuge vo dang sé duge can. 2 Thye nghitm @- Héa chat - Dung dich (NH): C,0, 5%/nueéie - Dung dich (NH) C.0, 0,1%/nuée ~ Dung djch NH,OH (1:1) - Dung dich chi thj methyl d5 0,14G/ctancl 60% - Dung dich AgNO; 1%/nuée. 82 pudN a b- Céich tién hanh Tao tia Ce thay tinh 200ml: hut Vint) dd mau Ca” (da Joe bd can khong tan) + nutic c&t dén kchoang 70mJ. Thém vai gigt methyl 6, Dun dd va séi. Thém chm 10 + 20ml dd (NH.),C.0, 5% néng (vite thém vita khudy déu). Trung hoa dd bing tung git NH.OH (1:1) cho dén khi dd chuyén tir dé sang vang. Dé yén dd (khong dun) it shit 1 gid. Loe, rita vi nung ta - Néu tia duge ean 6 dang CaC,0,.H,0 hoc CaCO: lee ta qua chung loe Gooch hoje chung thily tinh ea. Rifa tia bang dd (NHi)e CoO. 0,1% néng ft nbat 5 ln cho dén Khi dd qua loc khong cdn Clr (thir bing AgNO, sau khi acid héa dd qua loc bing HNO,). Say é 100+ 105°C trong 1+ 2 gid. Dé ngudi trong bink’ pit Am, cén. dang CaC,0,.H,0. Hode chuyén chén ehifa tia vao 10 Muffle, nung 6 500 + 25°C trong 2 gid hoae cho dén Kkhi kh0i lugng khong déi. Dé ngudi trong binh hit dm va efn dang CaCO, (é dé phong tia 4a bi chuy@n mt phan thinh CaO, lam dm tia bling dd (NH.)xCOs bao hoa: CaQ + (NH)gCOs > CaCOs + 2 NHg + HzO. Say d 105°C va cn). Néu tila duge can ¢ dang CaO; loc tia qua gidy loc day, khong tro (gidy bang xanh), Rifa tia bing éd (NH.),C,0, 0,1% néng din khi hét Cl Géi téa cho vao chén Pt (aa nung truée 1200°C va cin). Dét & ngoai bép dign che #8 gidy loc chay thanh than, cho chén Pt vao 10 nung 6 1200°C dén khdi lugng khong déi. Day chén, dt trong bink hat m va cn ngay sau Kkhi ngudi. 3 Két qué: Tinh ndng 4 Khoi lugng eda Ca® trong mau léng hoge phan tréim Khoi lugng & dang hgp chat trong mau rén. ‘ 3.5.2 Chudn d6 dung dich Ca” bang EDTA (chudn 46 true tiép) J- Nguyén tée a. Phan ting chudn dé ‘Prong méi trugng pH 12,5: HY" + Ca == CaY? + 2H* Dae diém: - Dd cfin c6 [Ca] < 5.10 °M dé tranh can bang phy Ca* + 20H == Ca(OH) Toxon, = 10? - 6 diéu kign chudn 4§ Ca”, néu trong mau 06 ede nguyén tS kim logi véi ham higng tusng Ung tré len sé can trd viée xde dinh diém cudi: Cu (2mgil); Fe?! (20mgil); Fe** (20mg/l); Mn®*(10mg/); Sn** (Smg/l); Zn** (Small); Po™ (Smgil); Al’* (Smg/l). Se™ va Ba™ ciing gay can tré dén vige xic dinh diém cui, néu do cuing vudt qué 200mg CaCOwl. bin LUONG MOT SO JON VA PHAN TY TRONG ONG DICH 63 + Trong thue té, cac ion gay edn tré hién dién phé bign nhat trong méu la Fe™ va Al’. Dé loai cdc Anh hudng néi trén, c6 thé tao tha hydroxyd réi loc bé tia hoi che st va nhém duéi dang phite v6i CN hay Triethanolamin (TEA). - G pH 125, (Mg”*] ~ 102 nan khong anh hudng dén két qua xde dinh Ca*, b Dinh diém cust Ding chat chi thi phite kim logi: Fluorexone (Ind: héng cam; Calnd: vang Ive hujnh quang) Calcon (Ind: xanh; Calnd: héng) Murexide (Ind: fm; Calnd: 46). Dée diém: = Can loai anh hung cba ede ion 6 kha nting tgo tin hydroxyd hoie tuo phiic bén vdi chi thi nhu Al", Fe, Cu". ~ Murexide it duge ding vi khé quan sdt diém cudi (dé + tim), va rat kém bén (hi hang sau kbi pha mdt ngay). 2 Thye nghi¢m w Hoa chit ~ Dung dich chuda EDTA 0,0100A¢ = Ding dich KOH 10" ~ Dung dich NH,OH (1:2) - Dung dich NH,OH-HCI (1:1) ~ Dung dich KON 10%/auée - Dung dich TEA (1:1) - Dung dich chi thi methyl 4é 0,1%/etanel 60% + Dung dich chi thj Fluorexone 0,1%/nuge - Dung dich chi thj Murexide 0,2/nuée. b- Cach tién hank + Buret: Dung dich EDTA chudn - Erlen: hit Vini) dd mau + lugng nuée edt thich hgp. Logi anh hudng cia edu tit gay nhiéu (xem phén chudin dQ Ba’* bang dd EDTA), Thém dd KOH 10N (vita them vita 1c déu) cho dén khi dd c6 pH 12,5 (kiém bing gidy pH) + vai gipt chi thi. Chun 4 bing dd EDTA. Mau oda dd igi diém cuéi thay déi phy thuge vao ch&t chi thi duge sti dung: + Galeon: héng -> xanh + Fluorexone: vang luc huynh quang + héng cam (quan sét trén nén den), + Murexide: dé > tim 3 Kt qua + Xe dinh Vp tir 3 lin chudn do = Tinh néng do mol, ndng a9 khOi lugng cba Ca’* trong cd kkhao sat - Tah ndng dé phan trim & dang hgp chat trong mu rin. fe 64 PHAN 3 3.5.3 Chudh 6 dung dich Ca bing EDTA (chutin 46 thé) J+ Nguyen tde a. Phan ting chudn do ‘Trong mii truding pH 10, véi sy hién dién cia MgY* c6 phan ting thé: Ca’ 4MgY* =% Mg?" + CaY* Boas = 10; Bygya = 10° ‘Chudn dd lugng Ca” cbn lai va lugng Mg?” sinh ra baing EDTA: HAY*+Ca* == Ca¥? 49H" HAY? +Mg* == MgY* + 2H" Dae diém: - Dang PP chudn do nay hi khong e¢ chi thj cho Ca ma c¢ chat chi thi cho Mg” (dd khong duge chia Mg”; néu dd chita Mg”, thé tich EDTA 1a thé tich ding chudin a6 tng Ca’ + Mg’). - Luong MgY* sit dung phai thich hgp ((MgY*] = 10% - 107M) dé sinh ra Mg” dé tao dang phite mau véi chi thi. - Phan ting tao phulc Mg¥* nhanh é nhiét dé khoang 60°C. b- Dink diém eudi Ding chi thj Eriochrome Black 7 CAn bang chi thi: HRY? +Mgind == MgY” + Ind + 2H" 2. Thue nghigm @ Hoa chat - Dung dich chudin EDTA 0,0100M - Dung dich dém pH 10 - Dung dich Mg¥” 0,014 - Dung dich NH.OH (1:1) ~ Dung dich NH,OH-HCT (1:1) - Dung dich KCN 10%/nude - Dung dich TEA (1:1) - Dung dich chi thi methyl 48 0,1%/etanol 60% - Dung dich chi thi Eriochrome Black T 0,2%/etanol. b- Céch tidn hanh + Buret: Dung dich EDTA chudn ~ Erlen: huit Vind) dd mu + iuyng nuée eat thich hgp. Loai anh hudng cia cfu tit nhiéu, Thém Gm dd dm pH 10+ o(md) dd Mg¥® + vai gigt chi thi Eriochrome Black T. Chuan 46 bang dd EDTA. Mau cia dd tai diém cudi tiv dé -> xanh, 3- Két qua: Tinh ham lugng Ca” tutong tu pong phép chudn dé trite tiép. DINH LUONG MOT SO 10N VA PHAN TO TRONG DUNG DICH 65 3.5.4 h higng Mg** bing phung phap khéi ligng 1 Nguyén tdée _, Ding dd diammonium hydrogen phosphate HPO,” va dd NH tao tia vai dd Mg" ¢ nhiét 9 thudng, trong mai truang acid: Mg” + HPO?" 4 8H,0 + NH, + OH +* MgNH,PO,,6H,O 7 =10728 Néu nung tia MgNH,PO, 2 MgNH.PO, —* Mg:P.0;+ 2NHs + HO Dae diém: + Cae ion kim logi Zn’, Mn®, Ca”, Be", Co**, UO... gay Anh hiding dén két qué xiv dinh Mg” do cing tao thanh ta ammoni phosphate. ~ Khi tgo tin trong méi truémg thiia nhiéu NF‘, Na* hogo K’, tia MgNHLPO,,6H,0 sé bj nhiém bin do sf tgo thanh Mg(NH)\(PO.) (sé chuyén thanh Mg(PO))s sau Khi nung), NajNHPO, hote KeNHPO, Dé 06 két qui chinh xéc, odin phil tién ‘hanh tao tia lai Lin thi hai, - Tula MgNH,PO,,6H,0 c6 dd tan kha lén (65mgil 8 10°C), nhung 88 gid kong dang ké trong mOi trutng NH, loang nén duge ra bang dd NE loang. ~ Do 06 xu hung tgo thanh dd qua bao hda, dd st duge dé yén vai gitr trude Khi loc. - Tua dude loc va dude chuyén sang dang can véi phvong tién va cach thie phy thuge vao dang s8 duge cén: + Dang cén 1a MgNH.PO,, 6H,0 néu tia duge rita ddu tién bing etanol, sau 46 bing ether khan. Phuong phép nay thuting duge chon néu PTN khong ¢6 1d nung hoae dé tiét kiém thoi gian, + Dang can 1a Mg,P,0; néu tia duge nung & nhiét do cao (100°C + 100°C). Qué trink nung dé chuyén tir dang tia MgNH,PO,, 6H,O sang dang can Mg,P.0; phai duge thye hidn hét site edn trong. Gidy loc phai duge a6t chay ¢ nhidt 46 thap vi C cdn lai c6 thé khd tia phosphate & nhiét dé cao. Cang cdn lu y dén sy pha hay chén Pt oda P 8 nhiét 46 cao. Ngoai ra, khi gia nhigt qué nhanh, adn phim 8 06 miu sim chif khong phi 1A mu tréing. 2 The nghi¢m @ Hoa chat = Dung djch (NH), HPO, 20%/nude (vite mdi pha xong) ~ Dung dich NH,OH (1:1) - Dung djch NH,OH 0,8M@ - Dung dich HCl aa - Dung mdi etanol 95% - Dung méi ether khan = Dung dich chi thj methyl 43 0,19%/etanol 60% = Dung djch AgNO) 14/nuée. 2) a Co Pung b- Céch tidin hank Tao tia : + Cév thiy tinh 300ml: hit Vind) dd mau Mg” (trung tinh ho&e acid yéu) chia khoding O,lg Mg + Smad dd HCl dd + nuve céit dén khoaiog 150ml. Thém vai gigt methyl d3 4 o(ml) dd (NH,)-HPO, 20% (vita thém vita khudy du). Trung hda dd bing timg giot dd NH,OH (1:1) cho dén khi dd chuyén tur dé sang vang. Tranh cham dda Ikhudy vao thanh ede vi tia sé tao thanh va bém vao thanh ofc ngay 14] . Tiép tye Kkhuéy dd 5 phat, thém time giot dd NH.OH (1:1) @@ gitt cho dd ludn luén ¢@ mau vang. Dé yén dd (khong dun) it nhét 4 gigs (tt nhat Ia qua dam). Loc, rita vd nung tha + Néu bia duye cin ¢ dang MgNH,PO,,6H,0: loc téa qua chung loc Gooch hoxe chung thiy tinh ca. Rita tia bing ting higng nhé dd NH,OH 0,8M (1:19) cho dén Khi dé qua loc khong cdn Cl (tha bang AgNO, sau Kkhi acid héa dd qua loc bing HNO,). Tiép theo, rita tha 3 lén, mbi lan v6i 10mi etanol 95%. Tiép tuc nia tha 5 lan, méi lan ding 5m ether khan. Hat khéng khi qua chung Ioe 10 phat, chuyén chung loc vae binh hut &m. Sau 20 phiit, can tia dang MgNH,PO,, 6H,0. ~ Néu tia duge céin & dang MgzP,0;: loc ta qua chung stt (khong nén ding gidy Joc), rita tia bang dd NH,OH 0,8M dén khi hét Say chung Ie 4 100°C + 150°C trong 1 gid. Cho chung sit vao ld nung, gia nhiet cham dén 1000°C + 1100°C va duy tri nhigt 46 may cho dén Ichi khéi ligng khong 46i. Day chén, ait trong binh hat Am va can ngay sau khi ngudi Ghi chit: Néu dd m&u Mg* bj lin nbiéu tap chat, phai tién hanh tao tila lai lin thd hai. Sau khi tao tia Mn 1, tha duge chuyén hés qua gidy loc din luong (Whatman No 40 hoke No 540) bing dd NH,OH 0,8M. Hoa tan tia trén gidy loc véi Khosing 50m! dd HCI (1:10) va nia gidy b&ng dd HCl loang (1:100) néng. Hing dd qua loc vao ofc thiy tinh dé ding dé tgo tila ln 1, Pha lo&ng bang nue edt thanh Khodng 150ml, thém vai giot methyl 48 + 0,2g (NH,),HPO, + ting giot NH,OH dd (va thém vita ‘chudy déu) cho dén khi dd chuyén sang vang. Thom 5mi dd NH,OH thita, Dé yén 4 gid hose qua dém, & Két qua: Tinh néng d khéi lugng cle Mg” trong mdn Jéng hoae phan tram khéi lugng 8 dang hop chit trong mau rin. 3.5.5 Chudn do dung dich Mg” bing EDTA (chudn d6 tric tiép) J- Nguyen tde @ Phdn tng chuGin d6 ‘Trong moi trudng pH 10: H,Y* + Mg™ == Mgy? 4 2H* Dae diém: ~ Dung dich cén 6 [Mg”] = 107M dé tranh cén bing phy; Mg" + 20H == Mg(OHy Tygom, =10°? INH LUONG MOT 56 (ON VA PHAN TU TRONG DUNG OCH “ 7 - Logi anh huting eda ede ion kim loai gay cin tré (Al*, Fe®*, Co’, Cu, Ca”, Ni*, Zn) bing KCN, NaS hay NH-OH,HCI. ~ Ca”, Pb", Mn™, Sr, Ga’ cng tgo phite bén voi EDTA 6 pH 10 va khong (hoge kh) logi Anh hudng cia ching bing NH,OHHCI hay KCN. Chat gy cn wre itt ps SG | i Chit che EKG |__ Chit ohe Ti: WoxS | _ Chit he TI: NHOH a 2 20 20 oe i vs 5 : ‘oa = 7 z L cor > 20 3 _ (0) cat > 00 20 08 Fe™ > 30 5 20 rem 20 Nn - 1 i ne 220 os oO | s® i : 7 2n* caes wt aa: PO eee: Fetyphosphae | 10 * duce chuén 60 ging Mg"; (O) chal che khong 26 tae dung. : - Phiin ting nhanh é nhigt do 60°C. b- Dink diém cudi ‘Thuting ding chi thi Eriochrome Black T: Ind: mau xanh; Mgind: mau tim (C&n bang chi thi: H.Y* +Mgind += MgY* + Ind* + 2H" CAn loai anh hudng cia cde ion e6 kha ning tao tha hydroxyd hote tao phic bén véi chi thi nhu Al", Fe". 2 Thue nghigm a Hoa chat ~ Dung dich chudin EDTA 0,0100M ~ Dung dich dém pH 10 - Dung dich NH,OH (1:1) ~ Dung dich NH,OH-HCI (1:1) = Dung dich KCN 10%/nude - Dung dich NagS 2%/nude = Dung dich TEA (1:1) - Dung dich chi thi methyl dé 0,1%/etanol 60% + Dung dich chi thi Eriochrome Black T 0,2%/etanol. 68 PHANG b- Céch tin hanh - Buret: Dung dich EDTA chudn Erlon: hit Vind] dd mu + luyng nude eft thich hgp. Logi anh hudng cla cau ttt nhiéu (xem phan chudn dé Ba’) + 3m/ dd dém pH 10 4 vai giot chi thj Eriochrome Black T. Chudin dé being dd EDTA. Mau etia dd tai diém eubi: +Dé > xanh név [Mg*] = 10° +Dé + tim néu(Mg”) ~ 10° 3 Ket qua +Xde dinh Vy ti 3 lan chudn 46 - Tinh néng d@ mol, ndng 46 khéi luong cia Mg™ trong dd khdo sat - Tinh néng d6 phan tram 6 dang hop chat trong mau rn, 3.5.6 Dinh dé ting cha mau mise DO cing cla méu nude due x4e dinh do sy hién dién cha mot trong hai ion hay ca hai ion Ca™ va Mg”. Tay thude vao dang muéi cua hai nguyén té néi trén, nguéi ta phan biét: 6 citng téng e6ng: ing voi ting ham lugng ede mudi Ca va Mg 6 moi dang (sulphate, carbonate, bicarbonate, chlorur...). DO cing tam thoi: ting v6i ving ham lugng cée mudi Ca va Mg & dang bicarbonate. DO cdmg sé bj mat Ikhi nude duge dun s6i (bi logi dudi dang tha carbonate). D6 cting thubng true: ing voi tong ham lugng cdc mudi Ca va Mg 6 dang sulphate va chlorur, Dé cting nay cdn lai sau Ishi nutéc di duye dun s6i. DQ cing con duge phén biét theo sy hign dign eda ion tao nén no: DO citng do Ca: dng voi téng ham lugng mudi Ca trong mau. Nguoi ta quan tam nhiéu aén d6 cing do Ca gay ra, béi mot lvgng ohé calcium carbonat cing di tao nén mgt mang cing bam vao mit trong dudng éng, lam gidm kh ndng trac déi nhiét, dé gay nhitng tai nan nguy hiém. D6 cting do Mg: tng voi tng ham lugng mudi Mg trong méu, DO cing tng: ting vdi ting ham lvong mudi Mg va Ca trong mau Don vj dinh dé eting dutge quy dinh thy theo quée gia: My: 14d = Img CaCOg/kg (ppm CaCO;) Phép: 1 dd = 10mg CaCO,fit Anh: 1 4 = Igrain CaCOylit = 0,084¢/2 Die: 1 d6 = 10mg CaO/it Suy ra: 1° Phap = 0,56 Dc = 0,7° Anh BINH LUONG MOT SO ION VA PHAN TH TRONG DUNG O;CH 69. A. PHUGNG PHAP CHUAN 09 VGl EDTA Phuong phép thudng duge ding xée dinh 6 etmg eiia cde loai nude udng, nude sinh hogt, nuve mat, nudc bién... e6 ham lugng Ca®* va Mg" Icha In. 4 Nguyén tie Dimg dd EDTA chudn 9 mu nuse ecing & pH 10 va pH! 12,6 vai chi thi thich hyp. 2 Thue nghigm ‘Thye hién hai thé nghiém (TN): IN 1: chuan d9 truc tip Ca’* 6 pH 12,5, chi thi fluorexon, calcon hoac murexide. ‘Thé tich EDTA st dung due kf higu Id Vj, (xem phin chudin d5 Ca?" bling EDTA), IN 2: chuéin a9 trvc tiép Ca” + Mg” & pH 10, Brio - T— den. Thé tfeh EDTA sit dung duge ki higu la Vs (xem phn chudn do Mg” bing EDTA), Néu thé tich Vai, trong 2'TN bing nhau = thé tich EDTA ding chudin 46 Mgt la Ve - Vi. Ghi chi: N6u muGn xée dinh dO cig tng, chi cén thye hien 1 TN la chudn 43 dd & pH 10 véi chi thi Eriochrome Black T. Néu mau khéng chia Mg** hode chi chia Me™ voi luong qua it, sy chuyén mau ciia dd tai diém cud! st khong 78 do Calnd rét kém bén; Ide dé, Briochrome Black T thé hién vai tra 18 chi thj acid - baz manh hen vai trd chi thi tao phic. Bé khde phue nhuge diém nay, thém vao dd mot jugag MgY* tao phan tng thé Ca’* vao MgY*. Mau dd tai diém cudi s8 tir dé > xanh d8 nhan ra hen rat nhiéu. ‘3 Két qua a _ = Xdedinh Vin va Vigo tir 3 lan chudn dé. - Tinh do eting cia mau nude do Ca’ va Mg” gay ra theo don vi ppm CaCOs. B- PHUONG PHAP QUANG PHO HAP THU THAY DUOC Phuung phép thuting duye ding xc dinh d9 cdimg clia cée loal nude udng, nude sinh hot, nuée mt, nuée bién... e6 ham lugng thay déi trong pham vi tis 1,5 + 60mg CaCOyl. I Nguyén tée Cho. MgY* vaio méu nuée eng dé thute hin phan ting thé: Ca®* 4MgY? == Mg? + Cav? Mg” sinh ra va Mg” c6 san trong mau dude cho te dung véi Calmagite & pH 10 tao thank phife e6 mau dé tim. 2 The nghiom a Héa chat - Dung dich MgY* 0,01M = Dung dich dém pH 10: 67,6g NH,Cl 4 572m NH,OH + nuéc edit -» 1 lit. - Dung dich NH,OH 1M: 70ml dd NH,OH 4a + nuée cat > 1 it. 70 PHAN 3 - Dung dich chi thi Calmagite: 0,25g chi thi + 500m! aude cat (khudy 30 phit cho tan biing may khudly ti). = Dung dich CaCO, Imgiml: 1,000g CaCO: (aa sy kho & 105°C) + dd HCl, dun dén tan. Thém 200ml nuse edt, dé ngudi. Thém vai giot methyl dé, dang dd NH.OH 8M diéu chinh pH (dd chuyén tir dé sang vang) va dink mie thanh 1000ml. ~ Dung dich CaCO 0,lmgimi: 100,0mz dd CaCO; mg/mi pha loang think 1000md, duge dd cé néng 49 0,1mg CaCOymi. b- Cach titn hanh Pha loat dd chudin va méu trong BDM 100,0nd dd chudn ddmiu ‘Thariyigo phic —- ype fe ue. ae [elo [es [oe [we Tm [om Veacas %Amgimi(mi) | 0,00 | 1,00 | 500 | 100 | 300 | soo - Cerca ma | @ | to | so | wo | a | eo war | oe A v bv [x | pt 10 mp { 5.00 500 i da Mav 0.0314 (np 300 106 6 Gatnagie (i) 3.00 [ 00 DohMptheA I I I (71¥6 €6 nba mau (nu efn), Trung héa mau bang dd NH/OH 1M. (7) Binh mac bdng nude oft. Lhe déu, do 66 hap thu aba phil & 620m eau £,6 phil 3 Ket qua = Ve duang A = f\Gexeo,)- ~ Xée dinh d6 eting (mg CaCO,/) cia dd do ti dé thi hode bing phifong phap binh phuong eye tiéu. ~ Xée dinh d9 ecmng trong miu lng (mg CaCOy/). 3.6 DINH LUGNG ION Ga” 8.6.1 Chuan 46 dung dich Ca” bing EDTA (chudn dé tryc tiép) 1 Nguyén tée a- Phan ting chudn d6 ‘Trong moi trudng pH 5 +6: HY" +Cd* 3 CdY* + 2H" én uu ¥ dén céc ion tao phite bén véi EDTA 4 diéu kién chusin 46 nhu Fe, Al, Cu, Zn®, Ni®*, Pb. BINH LUONG MOT SC 10N VA PHAN TW TRONG DUNG DICH n b- Dinh diém cudi Dang chi thi phi kim Jogi, thutmg 1a aylenol da cam hay P.A.N (Ind: vang; Cdind: 43). Can loai Anh huéng cla cdc ion ¢6 kha nang tao phife hén véi chi thi. Dé dé nhin mau tai diém cudi, c6 thé thém vao dd chudin 46 vai giot bromocresol luc. 2- Thue aghi¢m a Hoa chat ~ Dung dich chudn EDTA 0,0100M - Dung dich dém acetate (tao pH 5) - Hexamethylenetetramine (aexamine) rén (tao pH 6) + Dung dich NHOH (1:1) - Dung dich chi thj xylenol da cam 0,14/etanol + Dung dich chi thj P.A.N 0,1%/etanol ~ Dung dich chi thi bromocresol luc 0,1 %/etanol 20% b- Gach tién hank - Buret: Dung dich EDTA chudn Erlen: hut Vimd) dd mu, thém nude ct thich hop + vai giot chi thi bromocresol Iue. Thém ting giot NH.OH cho dén tthi dd chuyén by vang sang luc xanh (pH 5) + 2ml dd dém pH 5 + vai giot chi thi xylenol da cam hoae PAN. Chudn dé baing dd 8 Ket qua - Xée dinh V; tir 3 1dn chudn a6 + Tinh néng d@ mol, néng 46 khdi lvgng eda Ca” trong dd Ikhéo sat - Tinh néng 4 ph4n trim eta Cd” dang hgp chat trong mAu riin. Ghi chi: Dé db nbin mau hon, nén chudn dp Ca" bing EDTA theo céch ehudn 46 nguge. Tién hanh tuong tf cach chugn do Al’. Mau cia dd tai diém cudi: yang lye — tim. Hoiic chuén dg Cd ¢ pH 10, chi thi Eriochrome Black 'T (tuong tif céch chudn 49 Mg”), Mau cia dd tai diém eudi: dé — xanh. TA. Mau cia dd tai diém cudi: tim — tim lye > vang lye. 3.6.2 Dinh lugng ion Cd™ trong dung dich theo phuong phap quang phé hap thu thay duge 1- Nguyen te Ca duge tao phute c6 mau véi dithizone va duge chiét sang dung moi CCL: Ca" 4 2HD == CaD/nude + 2H"%nube | cab /CCl, 2 PHAN Phite CaADJCCL, 6 mau db, duve tao trong mdi tring baz manh (pH = 12) trong sy hign dién cua citrate hoac tartrate. Phiic hip thu bie xa A = 520nm, 2 Thite nghiem a: Hoa chat - Dung dich Cd® chudin 5,0mg/t - Dung dich dithizone 0,005%/CCl, + Dung dich NH.OH 1M - Dung dich KOH 100f - Hén hgp NHy-ON™S* (@6ml dd NH,OH da + 8md KON 10% + nude thinh 100mi. Ha tan 0,5g NasS vao dd) - Na citrate rin - Dung mdi COly. (b- Catch tién hanh ‘Tién hanh tuong ty phan xée dinh Pb* va Cu” theo PP quang phé hap thu thay duge véi dithizor nhung 6 pH = 12 (diéu chinh bang dd KOH 10M) vai néng 46 cia day chun Ca” ti 02+ 1,0ma/l. 8: Két qué = V8 dusng A = Cou). - Xée dinh néng 46 Cd? trong dd do tit d5 thi ho&e biing phuong phap binh phuong eye ti " ~ Tinh néng d6 Cd trong mau rn (mg/kg). 3.7. BINH LUQNG ION CI, Br, F VA SCN" 3.7.1 Chudin 49 dung dich CI, Br, I, SCN’ theo phufong phap Mohr J- Nguyén tee Phuong phip Mohr Ja phuong php chudn do tryc tip ion X (CI, Bry SCN’) vdi chi thi tao tia. @ Phin tng chudn do Agh+X° == Agx) Taget = 10 Tygsen = 10°"; Type = 10779; Tapp = 10: Dae diém: - Méi truting c6 pH< 10 dé tran edn bing pho: 2Ag' + 20H —> 2AgOH == AgO 14 H,0 - Tia AgCl va AgSCN 6 mau tring, tila AgBr vA Agl ed mau ving, bén trong méi trubng acid, tan trong moi trugag NH,OH do can bang tao phiie: AgX\ + 2NH; =© [Ag(NHp):]" +X" => trong moi truéng o6 NH,OH, pH cia dd cdn < 8 dé trénh can bing phy n6i tren. in BINH LUONG MOT SO ION VA PHAN Ti TRONG DUNE DICH B = Tia AgX 1a tia keo nén dé hap phy ofc ion déng hinh (Ag’, X") lon bé mat hat tia =2 edn chudn d6 cham va lde manh erlen. + Phép chudn 40 thich hop voi néng do [X"] khosing 10 + 107M, - Phuong phép Mohr rit: thich hop cho vite xdc dinh CI hoi Br° nbung khong thich hgp lim ddi voi va SCN” do hign tung hap phy manb lén ‘tia cia ching va viée nhin mau tai diém cudi tuong déi kho khan. - Khi déng hign dign trong dd, té&t 4 cde X déu tao tie bén vdi Ag’. b- Dinh diém cust Ding chét chi thi tao tia K,Cr0, véi edn bling chi thi Dag’ + CHOP s* AgWCrOd Tyygcio, = 10” Dec diém: + Tia Ag.CrO, mau dé nau, tan & nhiét 6 cao. - Méi truéng can c6 pH > 6,5 dé tranh can bing phu: 2CrOf + 2H? =% 2HCrO” == Crs0;7 + 1,0 = Laigng chi thi edn ding thich hgp dé diém eudi gn véi diém tuong duong. Dé GB quan sat diém cudiz + Nong do CrO,> trong LAgsCrO, = 10° + Nong d@ Cr0,* ty do = 10: 5.1074. - Cain loai nhang ion tgo tia bén véi CrO,? nhut Ba**, Pb**. Két hop diéu kién eda can bing chudin 6 va edn bing chi NH,OH tot nhat nén chudn do 6 méi trudng cd pH 7 + 8 (tao diéu eich thém vao dd m@L lugng nhé NafiCO, hay Na,B,0,). thi, khi dd co ign nay bing 2 Thye nghiom u- Hoa chat - Dung dich chudin AgNO, 0,040N hay 0,050N - Dung dich chi thi KsCrO, 10%/nude + NaHCO; hay NasB,0; rin. b- Céch tin hanh ~ Buret: Dung dich chudn AgNOs - Erlen: Ding pipet hat Vind) dd mau + it nude edt trang thanh binh. Ding gidy pH kiém tra pH cia dd, Thém NaHCO; hay NayB,O; ran (néu edn) + ulmi). chi thi K;Cr0,10% (v = 0,25ml tide 5 giot ting voi ting thé tich dd trong erlen tiv 25 + 100ml dé (Cr. = 1,25.10 = 5.10°°M), Mau eda dd tai diém cui: ving tusi > vang dnb hong. 3. Ket qua a) Ghi nan V; va tinh V; tit 3 la chudn a¢. b) Tinh adng 46 duong lugag, nbng 44 mol, ‘néng dd Ichdi lugng cilia NaCl teong dd khdo sat: ©) Néu mdu mudi duge chudn bi bang cach hoa tan 0,5000g mAu thinh 500,0ne dd, tinh % NaCl trong mau ban dau. 24 PHAN 3 8.7.2 Chuéin a dung djch Cl, Br, I, SCN" theo phudng ph4p Fajans I: Nguyen tée Phuong phép Fajans 1A phong php chudin dQ trye tiép ion X (CI, Br’, I, SCN) bang dd AgNO; véi chi thi hap phu. @- Phan itng chudn db Ag’ +X s= Agxl Bygg =I0 8, 5 Dayscie 105 Thay = 10, Typo 10-2608 Dae diém: ‘Moi truéing chun d5 trung tinh hoe acid yu (ding acid acetic tgo méi trudng). b- Dink diém eudi Bang cach ding chit chi thj hé'p phy, Chi thi duge Iva chon cin ei vao cfu tit edn chun dé: Chudn a9 cr Ding fluorescein (HF1, kyr = 107) hode di-chlorofluorescein (HFIX, kip = 10°) Jam chi t] Chi thi HEL: Trong dd cé can bing: HF] == Ht sFr Trude diém tuong duong cd hi¢n tuong hp phy Cl’ lén hat tha nen hat tia c6 cfu tao: (LAgC1, Cr: Ag’) Neay sau diém tuong duong od hign tuyng hap phu Ag" lén hat tia: (VAgOl, Ag*: NO Cén bing trao déi gia NOs trén hat tia va FY trong dd lam tia AgCl chuy€n mau: LAgCl, Ag’: NOs + FI —> LAgCl, Agt: FI + NOs Dee diém: ~ Moi trudng cdn 6 pH > 7 dé c6 sy phan ly ca cht thi + Dé dB quan sat diém cudi, can tang dign tich bé mat eda AgCl bing eéch: + Tranh sy déng ty cia tia (gid dd 6 nhiét 46 thudng) + Loai sul c6 mat ciia ede ion da hoa tri nhu Al’, Fe"... + Thém chat keo bdo ve tua nhu dextrine, gelatine. ~ Phép chudin d6 thich hop véi 5.10" < [Cl lp < 2,5.10°M (sai so < 2%): +1CIIo > 5.10M 46 luong tia dil Ién cho qué trinh hé'p phy + (CII < 2,5.10°M dé tranh su dong ty tia. BINH LUONG MOT SC ION VA PHAN TH TRONG ONG DICH 5 Khi chudn d@ gén dén diém cudi, tia AgCI déng tu va co mau hdng cuc bd xudt hién tai vi tri giot AgNO, roi xudng. Tiép tue cho AgNO, roi that cham cho én khi tia ted nén of mau héng dot ngdt. Chi thi RIX: Dac diém: - Moi tring cin c6 pH > 4 dé 06 sw phan ly eda chi thi ~ Chudin d¢ duge ede dd Cl’ 06 ham lugng rét thaip, vi dy trong nude uéng - Ding chngn d6 ce dd khéng thé chudn 46 trye tiép bing phuomg phap ‘Mohr, vi du chudin 46 Cl trong dd cae mudi Cu, Ni, Mn, Zn, Al, Mg. Khi chudn do gan dén diém cudi, tia AgC] dong tu va cé mau tim xanh cue bo xudt hign tai vi tri giot AgNO, roi xuOng. Tiép tue cho AgNOs roi that chém cho én khi tia trd nén o6 mau tim xanh dot ngot. Chniin dp Br C6 thé dung fluorescein (tai cudi, tia 6 mau héng) nhung tét nhét 1a nén ding eosine (tai diém cudi, tha cé mau 26) lam chi thi. Chudn do C6 thé ding fluorescein (tia mau cam), eosine (tia mau 43) nhumg tét nhat 1a nén ding di-iododimethyifluorescein (tai diéra cub, ta cé méu 43 xanh) lam chi thi, Chudin dg SCN" C6 thé dung fluorescein (tia mau héng), eosine (tia mau dé) lam chi thj. 2. Thite nghiém a. Héachét - Dung dich chudn AgNO; 0,050 hay 0,100N" - Dung dich chi thi fluorescein 0,2%/etanol 70% = Dung djch chi thi di-chlorofluorescein 0,1%¢/etano! 70% - Dung dich chi thi eosin 0,1%/etanol 70% - Dung dich chi thi di-iododimethylfuorescoin 1%etanol 70% - Dung dich CH,COOH (1:1) = Dung dich HNO, (1:1) = Dung dich NH.OH (1:1) + Dextrine rn. Céich tin hanh - Buret: Dung dich chugn AgNOs, - Erlen: hit Vil) dd mau + it nude eat tring thénh binh. Kiém tra va diéu chinh pH cda dd (néu cd); thém 0,1g dextrine + vai giot chi thi. ‘Mau ela dd tei diém cu6i thay déi phy thuge vao ion duge chudin d9 va vao ehi thi duge st dung. & Két qué: Tiah gidng phuong phép Mohr fis 76 PHAN 3 4 Ung dung & Chuén 46 dung dich chita hon hop Cl.+ I + Chudn d6 téng (CI'+ Uivéi chi thi Quorescein (Vi); Chuan 46 riéng I véi chi thi di-iedodimethylfuorescein(V;). Hiéu cia (V; ~ V2) IA thé tich AgNO, tinh cho Cr, Néu dd chia lugng Ida Clr, kt qué xde dink Ir 06 thé bi sai 96 khodng 1%. - Chudn 49 téng (Cr+ I") v6i chi thi di-chlorotetraiodofluorescein (tai dim cudi tin 06 mau d3 xanh); chuiin dd riéng T véi chi thy di-iododimethylfuorescein. Két qua xée dinh I theo phuong phap nay khé chinh xac ngay cA Ichi dd chia iuong 1én CI. b- Chudin dé dung dich chita hin hop Br +I Chuan 49 téng (Br+ 1°) véi chi thi fluorescein hoe cosine; chuda dé riéng T- vi chi thi di-iododimethy!fluorescein, 3.7.8 Chudn do dung dich CI, Br’, C, SCN” theo PP Charpentier Volhard I Nguyen ide Phuong phapVolhard 1A phudng phap ding dd AgNO; chuén 46 ion X- (CI, Br’, I’) theo edch chudn do nguye. a- Phan ing chudn do ‘Tham ligng thita xée dinh d AgNO, vao dd chia X*: Agh+X° == Agkt Dinh luyng Ag” thifa bing dd chun KSCN hay NH,SCN: Ag’ 4 SCN” F® AgSCNS Pygsey ~ 10717 b- Dink diém cust Ding chi thi tao phite phan st ba; véi ligng nhd SCN ding thita: Fe® 4 SCN” = FeSCN® pS, = 103% Dec diém: Ngoai cac dic diém da trinh bay & phan chufin 49. dd Ag* bing phuong phép Volhard, edn luu y: + Khi X= CT, do Taysow < Tago) nén gin dim tucng duong c6 thé 6 edn bling phy: AgX see Agh + XT JAgSCN LAgSCN+Fe™ ~ Loai can bang phy nay bang mét trong ede bién phap: + Loc bd tia AgCl trude Ikhi chudn do. BINH LUONG MOT SO'ION VA PHAN 7U TRONG DUNG DICH 7m + Thém vao dd mot luyny dung moi khong tron lin v6) nude (nitrobenzene), lée that manh dd trvée khi chuda do dé bao hat tia + Thay chi thi phen sit ba bitag chi thi tartrazine (ey hién dign ota chi thi tarsazine sé lam cho tia AgSCN’ co mau vang nhat trong subt qué trinh ehudn dg va dd bén trén ti Iehéng mau sé chuyén thanh mau vang chanh tai diém eudi), Bign phap don gian nhat 1a chi edn lic that manh erlen (sau khi them HNOs, rude khi chudn 46) dé lam két von cae hat tla lai. 2 Thue nghiém @ Hoa chat + dd chun AgNO; + dd chun KSCN hay NH,SCN - dd HNO; (1:1) ~ dd phén sat ba Fe(NH.MS0.)2.12H,0 bio hda (= 1M) ~ dd tartrazine 0,5%o/ude. b. Cach tién hank = Buret: Dung dich chudin KSCN hay NH,SCN. + Erlen: hit Viml) dd mau + it nude edt trang thanh binh + 2ml dd HNO; (111) + lwgng xée dinh dd chu&n AgNO; (thita khoiing 60% so voi ly thuyev). Han ché sy tan cia AgCll bing céch ioe bd tia AgCl (hode thém vao dd 0,5ml nitrobenzene) léc that manh dd. Thém lvgng thich hgp chi thi phan st ba, Chuén d@ bing dd KSON hay NH,SON. ‘Mau eiia dd tgi diém eudi: ving nhat + miu eam nhat, 9. Két qué: Tinh ging phuong phdp Mokr | 874 Chudn d6 dung dich CI, Br’, I, SCN" theo PP chudin d6 dién thé 1- Nguyén tde a. Phan ing chudn dp Ag’ +X SE Agxl b- Dinh diém trtong ditang Dang may do thé cé: = Dign eye chi thi: Ag. ~ Dign eye chudn: calomel ho&e AgCl. Phan ting ign héa chi thi AgXl+e = Ag+X Eoscg = Ehoxing + es Ghi nhan sy thay ddi cha Ey, theo thé tich AgNO, sit dung. Xéc dinh diém tuong dung bing PP thich hgp. 7B PHAN 3 Dae diém: - Cé kh nfing chudn dé dude ting ion khi ti sé tich sé tan cla cdc tua cach nhav 10° lén tré lén => xAe dinh duge dé chita (I + Cl) hode (Br + I) dbng hign dién. - Cé hidn tagng h&p phy eda ion lén bé mat hat tia lam cho phan ting cham ya kho khan, Vi dy, chudin do dd chita (I+ Cl") ¢6 hign tugng CF bi halo phy Jén mat tia Agl. Giém hién tugng nay bing eéch thém vao dd mt lugng nhé chat dién ly, vi dy Ba(NO;)o. 2: The nghiem a Hoa chet - Dung dich chudn AgNO, 0,040N hay 0,050" + Ba(NO,)g ran. b- Cach tien hank - Buret: Dung dich chudn AgNO; + OBe thiy tinh 250ml: hét Vimi) dd mdu chite (I + Clr) + nude eft dén Khoang 100mi + 1g Ba(NOsh khudy tan. Nhiing hai dign eye vao dd chudn do, Khusly dd bang hé thong khudy tix hay khudy ev. Doc tr] sf E cia dd sau méi Jin thém AgNOs tr buret. Ngung chudn 40 khi chde chdn rang da vugt qua diém tuong duong. 3. Ket qua = Ve dung chun dd B= /Vagno,) - Tim cée Viz bang phusmg phép hinh binh hainh ho&e phuong phép néi suy tit 80 ligu eda dutmg vi phan bac 2. - Tinh néng d§ ducng lugng, ning d) mol, ndng d@ khéi lung cia NaCl va Nal trong dd khdo sit, 3.8 DINH LUQNG ION Co* 3.8.1 Chudn do dung dich Co® bing EDTA (chudn dQ true tiép) I- Nguyén tée a- Phan ting chudn do Trong méi truiing pH 6: HY?" + Co** == CoY? + 2H” Can loai anh hudag etia cde ion tao phite bén véi EDTA & didu kin chudn 4 nhu Fe", Cu”, Zn®; Ni’*, Pb**, Ca. be Dinh diém eudi Ding chi thj phite kim loai, thuting 14 xylenol da cam (Ind: vang; Colnd: 43) Cn loai Anh huéng eda ede ion 06 khé nang tgo tao phite ban véi chi thi. DE dé nhin mau tai diém cudi, c6 thé them vao dd chudn 6 vai gigt bromocresol luc, INH LUOWG MOT SC ION VA PHAN TH TRONG DUNG DICH 79 2. Thite nghiom a. Hoa chat ~ Dung dich chun EDTA 0,0100M - Hexamethylenetetramine (hexamine) rén (tao pH 6) ~ Dung dich H,SO, loang (1:19) Dung dich chi thi xylenol da cam 0,1%/etanol ~ Dung dich chi thi bromocresol lye 0.1%/etanol 20%. b- Oach tién heh - Buret: Dung dich EDTA chuén + Erlen: hit V(ml) dd mu, thém nude eift thich hgp + vai gigt chi thi xylenol da cam. Thém tiing git HpSO, cho ¢én khi dd chuyén tit dé sang vang. Thém hexamine, dd c6 mau dé tdi. Thém vai giot chi thi bromocresol luc va chudn 46 bing dd EDTA. Cén chudin do that cham khi gan dén diém ‘Mau eda dd chuyén ti tim — tim lye luc. 5+ Ket qua - Xée dinh Vy tir3 lan chudn do. - Tinh néng do mol, néng do khOi lvgng ea Co” trong dd khéo sat + Tinh néng dé phan tram cia Co’ dang hgp chat trong mAu rén. Ghi chai: 6 thé chudin a) Co’ bing EDTA theo ech chudn a) nguge. ‘Tién hanh tudng ty csich chudn d6 AI, Mau etia dd tei diém eudi: lye > tim, 3.8.2 Chudn d6 Co” gidn tiép theo phudng phap Volhard d- Nguyén tae ‘Them lugng thiia SCN” vao dd musi Co™ chéa mot it pyridine dé tao thanh hop chat bén [Co(CsH,N),(SCN)]. Loc bé tia néi trén va chudn dé lugng thita SCN bing dd AgNOs, @- Phan tng chudn d6 Ag’ +SCN” S® AgSONL Pygoy = 10717 b- Dinh diém cust ‘Ding chi thi tao phife phén sat ba: Fe + SCN" +® FeSCN™ pa, = 10° 2. Thite nghifm a. Hoa chat - Dung dich chudn AgNO; = Dung djeh chudn KSCN hay NELSON = Pyridine = Dung djch HNO, loaing (1:10) = Dung djch phén sft ba Fo(NH,)(S0,),.12H,0 bio hoa (= 1M ). Pm 20 PHAN 3 bs Cach titn hanh Xi 19 mdu vt tao tia Hoe tan mau (chia khoang 0,05 + 0,1g mudi Co") bing 150m! nude trong cbc 250m. Acid héa bing dd TINO; lodng + Bn! pyridine + lugng thira NH,SCN. Tia {Co(C-H_N}{SCN)3} 88 duge lge khdi dd rit dé dang. Dd qua Ige duge himg vao BDM 250,0m/ va dinh mie dén vach. Chudn de SCN” thie - Buret: Dung dich chun KSCN hay NH,SCN + Brlen: hut Vord dd miu + it mute eat tring thinh binh 4 2ml dd HNO, (1-1) + lugng tht ade djnh dd chudin AgNOg, Thém ligng thich hyp chi Uhj phén sét ba. Chudn d6 Ivong Ag* thia bing dd KSCN hay NH,SCN. Mau eda dd ti diém cui: Vang nat -> cam nhat. 3- Ket qué: Tinh ham lugng Co* 6 dang hop chat trong mau rén. 3.8.3 Dinh higng ion Co” theo phiténg phap quang phé h&p thu thay duge Cobalt 4 dang Co” duge tao phife véi ligand L, 05 thé 1A SCN, Arsenazo, Dithizone, mudi Nitrozo R. Hai chat tao phite duge sit dung kha phé bién IA mui Nitrozo R va SCN’. A- DUNG NaSCN (KSCN, NH.SCN) 1- Nguyén tec Cobalt dang Co™ duye tao phic véi SCN” trong sy hién dién cia acetone: Co +4SCN == [Co(SCN) Dae diém: ~ Phite (Co(SCN),]* trong méi trutng acetone o6 mau xanh, hé s6 hap thu mol Khodng 950 mol” \em 41 ~ Ding H,SO, 48 khit Co vé Co”. = Mién néng d6 Co” thich hop tit 10+ 40mg/l. ~ Néu e6 Fo® s6 tao thanh phic [Fe(SCN)] c6 mau dé mau. Loi anh hudng cia Fe bang huyén phit Zn(OH), 2. Thue nghiem @- Hoa chat ~ Dung dich Co” chuéin 100mgit - Dung dich NaSCN 40% /nude - Dung dich HeS05 méi diéu ché (cho $0, bao hda trong nuée) ~ Dung dich NH,OH (1-1) - Dung méi acetone. b- Céch tidn hanh Chudin. bj logt chudn va miu trong otic thiy tinh 100md vA sau 46 tao phite trong BDM 160,0mi. BINH LUQNG MOT SO ION VA PHAN TU TRONG DUNG DICH a T me 7 Thi wf goprae pee L. Bae [aie Te Teepe ™ [oe Jocrvcems mil} 000 | 500 | 190 | 200 | doe | a0 ea) | Voie (0 i ce a 20 (mg) a 200 200

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