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Search = Home ‘Technology Education More Topics For Uploaders Get Started © Tips & TricksDAI HQC QUOC GIA HA NOI ‘TRUONG DAI HQC KHOA HOC TU NHIEN es Nguyén Vin Ri Ta thj thio Thue tap phan tich Hoa hoc PHAN 1 PHAN TICH DINH LUQNG HOA HQC Ha ngi — 2006Bai3 Churomg 2 MUC LUC Phin 1 Phin tich dinh lugmg hod hoe eo bin ‘Chuong 1 Bail Phuong php ehusin d@ axit-bazer ‘Chuiin d6 dom axit, don baz Hiigu chinh thé tich buret Thye hinh cfn nue edt Ve duémg cong higu chinh thé tich buret Pha ché dung dich chuan axit oxalie dé xe dinh baz Xae inh cfc nding dd dom axit da baza ‘Thiét lip: ndng 40 ‘NaOH theo dung dich géc H,C,0, dic dinh néng 9 HCL ‘Xie dinh néng 46 CH;COOH Xéie dinh nng do NH; Xde dinh ham lrong NH,’ theo phuong php foocmalin ‘Chuiin d6 da axit Dung dich chun Pha ché dung dich tir fixanal Thiét lip nong 4 HCI theo nati tetraborat ‘Xie dinh néng 49 da axit va mudi eta nd Xéie dinh nong d6 dung dich HsPOs bang dung dich chun NaOH Xéic dinh nong 6 HCI va HPO, trong eding hin hop, Xie dinh nong d KH:PO, vi KzHPO, trong cing hon hop ‘Chudin d6 da baze Cée dung dich chun Thiét lip nong d} HCI theo Na;COs Thiét ip nng d} NaOH theo HCI da ebuén Xe dinh da bazo bing axit manh Xsie dinh ndng a6 NazCOs va NaHCO trong hén hop Xie dinh him lrong Na,COs trong NaOH dng nghiép ‘Xdic dinh d6 cimg tam thi cia nuke miy ‘Cu hoi on tip phin ede phan img axit-baze Phuong php ehuxin d} complexon ‘Chuan 46 tnye tiép xc dinh cae ion kim loai Pha dung dich chuiin EDTA Xéic dink céeion kim loai Xie dinh Zn**, Mg"*, Pb, chat chi thi ETOO & pH 10 Xe dinh Ni2*, Cu, Ca, chi thi Murexit ‘Xie dinh Fe", chi thi axit sunfosalixilie H2SSal Xde dinh Cu chi thi PAN, pl Cae ky thudt chun d6 complexon ‘Chuiin dd phin doan xc dinh Bi”, Pb* ‘Chuan 46 nguge xc dinh Pb**biing Zn* va EDTA, 10 10 10 ul 12 13 13 13 1B 15 15 16 16 16 B 433 53.1 53.2 61d 612 62 62.1 62.2 63 Bai7 7 72 73 Chuomg 3 Bais 10.1 10.2 103 103.1 103.2 104 104.1 1042 Bai ll Wa 12 121 ‘Chuan 46 thay thé Xde dinh Pb? ‘Xéic dinh Ba°* khi e6 mit Mg”* hoyle Mg’ ‘Xtic dinh Ni?* v6i he chi thi CuY? PAN ‘Cac ky thugit chudin 46 complexon (tiép) Xde dinh him rong PO,” Neguyén tic (Quy trinh phan tich Xéic dinh Hg", Zn trong bin hop Neguyén tie (Quy trinh phan tich Xiic dinh d6 cimg toan phin cia nude may Xéie dinh hon hop AP", Ca°*, Mg* (bai kiém tra) Neuyén tie (Quy tinh phan tich (Cau hoi on tap Phuong phap chudn d@ két tia tao phire Xzie dinh ede halogenua, SCN Phuong php Mobr xéc dinh CI. Br Phuong php Fajans xe dinh Cl, Br, 1, SCN Phuong php Volhard xie dinh CI, Br, T, SCN Xéic dinh CI bing He(NOs)2 ‘Cu hoi on tap ‘Cée phumg php oxi hos - khir Phuong phip pemanganat Xde dinh nong dd dung dich pemanganat Xie dinh ndng d9 HO, céng nghiép Xd dinh ndng do NOz Xd dinh ndng d6 Fe", Fe™ trong hén hop Xéic dink him rong Ca"? Phuong php dicromat Pha dung dich K,Cr,0, Xd dinh nong dd Na,S,0; Xd dinh Pb bing phurong phip diromat Nguyen tie Quy tinh phan tich Xai dink him hong erom trong miu nue thai Neguyén te (Quy trinh phan tich Phuong php chuan d9 iot-thiosunfat Die diém cia phuemg phip Pha dung dich chun Pha dung dich Na;S:05 7 7 7 18 19 19 19 19 20 20 26 26 27 21 21 27 28 28 29 30 30 30 31 31 32 32 32 33 33 4 4 31Pha dung dich I> Xie dinh nong a6 dung dich Cur Xéic dinh néng d6 dung dich natrisunfit tic dinh néng d6 dung dich natriasenit ‘Xtc dinh him rong elo hogt dng trong nue javen Phuong phip chun 4 bromat, iodat Nguyén tie eta phyong phip Xie dinh néng d6 dung dich Sb™ bing phép do bromat Xaic dinh ham lurgng AI" trong miu bang phép do bromat ‘Xéic dinh néng d9 H" bing phép do iodat Phuong phép trong hemg Phuong phap phan tich trong lugng xe dinh Mg” Ky thuit loc Gily toe khong tin ‘Cach gap gidy loc va ky thuit loc Xie dink Mg theo phyomg phip trong lremg Nguyén tie xe dinh (Quy tinh phan tich Phuong php phan tich trong lung xe dinh Fe Nguyén te Xe dinh ham rong Fe trong phén sit 35 36 37 38 38 38 39 40 4 4 4 4 4 42 42 43 44, 44, 44 Xsie dinh SO,* bing phuomg php trong lung va complexon “5 Xéie dinh SO,? bing phuong phép trong long Nguyén te xe dinh (Quy trinh phan tich Xde dinh SO, bing phuong php complexon Nguyén tie xe dinh (Quy trinh phan tich (Cau hoi on tap Phan ich mau thye té Phan ich hop kim Xde dinh him hrong Mn trong gang Neguyén tic xie dinh Quy tinh phin ich Tinh todin két quit Hos ct Phan tich Al, Cu, Zn trong hop kim Devada Nguyén tie xe dinh (Quy trinh phan tich Xde dinh Fe, Cr, Ni tong gp kim inox Neguyén tie xe dinh (Quy trinh phan tich Tinh ton két qui 50 50 50 52Bai 20 Hoa chit . Xéic dinh Cu, Sn, Pb, Zn trong ding thaw Nguyén te xe dinh (Quy tinh phin tich Xéic dinh Sn Xéie dinh Cu, Pb, Sn trong dung dich nurée loc Tinh tod két qui Hoa chit Xie dinh ham lung Cu, Fe, Al, Zn trong hop kim nhm Nguyén tie xe dinh Quy trinh phan tich ‘Tinh tod két qui Hoi ct Phan tich cde sin phim e6ng nghigp Xie dinh him rang Al,0,, Fe,0,, CaO, MgO trong xi ming poocling Chuan bi miu Phan huy miu Neguyén tie xe dinh Quy trinh phn tich (theo TCVN 139 1991) Xéic dinh ham long FeO; Xsic dinh ham omg ALOs Xéic dink him lrgng CaO Tinh ton két qui Hoi chit ‘Xaie din him long P;Os trong phan bén NPK Nguyén tic xe dinh photpho (quy vé P,Q.) (Quy tinh phan tich Tinh toan két qua Hoa c ‘Xaic dinh Mn trong quiing piroluzit Nguyén tie xie dinh (Quy trinh phan tich Tinh tosin két qui Hoa chat Phan tich moi tring Xzic dinh mot sé chi tigu hod hoe etta nude va nude thai Xe dinh him rong oxi hod tan (DO) trong nude Neguyén tie xe dinh (Quy trinh phan tich Xtic dinh nhu ciu oxi hod hye trong nue (COD) Nguyen tic Lay miu va bio quan 37 37 37 37 58. 38 58. 39 39 60 60 61 61 61 62 62 62 62 62 63 63 63 64 64 64 65 38 8Quy tinh phan tich 65 Tinh tosn két qui 65 Hod c 65 Phan tich m@t sé chi 66 ‘Xiic dinh him lirong SO,” 66 Xe dinh him lromg Hs 66 Xie dinh ham omg Cl (phurong php Mohr) 66 Xdedinh d9 axit 7 Xe dinh 46 kim 67 Xéie dinh do etmg 7 Xéic dink him rong Ca°* 69 ‘Tinh todn két qui 69 Hoi ct 69 Phan tich thue phim 0 Phan tich mt s6 chi tiéu eta nude mim 70 Chuin bi miu 70 Quy trinh phan tich (theo TCVN- 1520-74) 70 Xie dinh d6 axit trong nurée mim (tinh theo CH;COOH) 70 Xie dinh ham lirgng mudi NaCl 70 Xe dinh him hromg N-fooemon trong nue mim n Xde dinh N toan phin cia nuée mim a Tinh ton két qui R Hoa chit va dung eu R Bai 27 Phan tich him lung edc loa dhrémg trong sita de e6 dutmg 74 211 Nguyén tée phurong php phan tich m4 212 Chui bi miu m4 273 Quy tinh phan tich 15 273.1 Dinh hom duimg lactoza 5 273.2 inh long duimg sacaroza 24 ‘Tinh todn két qui 15 265 Hod chat . . 15 Bai 28 Phan tich mot sé chi tigu hos hoe eta ebit béo 16 Xdie dinh chi s6 axit 16 Neguyén tie 76 (Céeh tién hin 16 ‘Xie dinh chi s6 xa phong. 16 Nguyen tie 16 (Céich tién hinh, 16 Xie dinh chi s6 este n Xée dinh chi s6 iot n Xée dinh chi sb peoxit n Nguyén tie 8 Quy trinh phan tich 828.6 28.7 Bai 29 29.1 29.2 292.1 292.2 293 2931 29.3.2 204 294.1 294.2 295 29.6 Bai 30 30.1 30.1.1 30.12 30.2 30.2.1 302 303 303.1 3032 304 305 Chuomg 10 Phu luc 1 PLL P12 Phu luc 2 P2.1 P23 P24 Phy luc 3 P31 P32 P33 Phu lue 4 Phu lue 5 Tinh Hoa chit ‘Xiic dinh mot sé chi tigu hod hoc cia nrgu ubng Xiic dinh 46 axit toan phin tic dink him lung axit xianhidrie Nguyen tie (Cah tién hin Xde dinh him rong andebit Neguyén tic (Céeh tién hin Xdic dinh him hong este Neguyén tie xe dinh (Cah tién hin Trinh tos két quit Hos chit Xie dinh him lirgng foocmandehit, phenol trong nuécuéng Xe dinh ham long KIO, trong mudi iot Xie dinh him omg andebitfooemic Neguyén tic xic dink (Cach tién hin Dinh hong phenol Neguyén tie (Céeh tién hinh Dinh lrgng KIO, trong mudi iot (theo TCVN 1998) Neguyén tie ‘Cach tién hanh Tinh ton két qui Hod chat ‘Cae phy Iue Bo trong luong (Cae loai ean Quy tae sir dung edn phan tich Do thé tich (Cée dung eu do thé tich thong thuimg Lam sach dung eu thuy tinh Higu chinh dung eu do thé tich Xaic dink dung tich pipet (Cée thiét bi sir dung trong phan tich trong Iuong Ti sly La nung Chén nung . Neguyén tr khéi cua mt sé nguyén t6 thring gp Cae hing sé phan ly axit 6 25°C két qua, 18 18 79 79 9 79 80 80 80 80 81 81 81 81 81 82 82 82 82 82 82 83 83 83 83 83 83 84 84 84 86 87 87 87 88 89 90 90 90 92 4 4Phu luc 6 Phu luc 7 Phu luc 8 Phu lye 9 Phu tue 10, Phu tue 11 Phu luc 12 Phu luc 13 Phu luc 14 MOt sé chi thi axit-bazo quan trong: Mot sé chi thi sirdung trong chuin 4 complexon_ M6t so chi thi oxi hoa khit Cac gid tri ryan dé phite complexonat kim loai {go thin hoain toan Hiing s6 ben ciia eae complexonat kim loai Hing s6 tgo thinh cua mat so phire 25°C Tich s6 tan eiia mot s6 hop chat kh6 tan 6 25° C Méts6 thé dign eye tidu chusin Nong d6 cia mot 6 axit-bazo die ban trén thi trudng: 95 96 96 96 7 7 100 101 104LOINOLDAU Phan tich dinh long durge diing dé xe dinh quan hé dinh Iugng gitta eée think phin cita chit nghién ciru, trong dé chit phin tich dong vai tré la trung tam. ‘Tuy thude vao yéu cdu va dic trung ky thuat sir dung dé xac dinh thanh phin cia chit phin tich, ede phuomg phip phin tich dinh hrong duge chia thanh 3 nhém: ede phurong phép phin tich héa hoc, vat ly va hod ly con goi Li phuong phip phan tich cong ‘Cée phuong phip phin tich hod hoc gim phuomg phip phan tich trong lung va phan tich thé tich (gdm phuemg php chun d6 thé tich, phuromg phip thé tich khi, phurong, phap thé tich King dong). Cac phurong php chun d6 thé tich dra trén 4 loai phan img co bin gdm phan img axit- bazo, phan tng go phite, phin img két tia va phan img oxi hod khir, ‘Cée phuomg phép phan tich cong cu xe dinh ede chat phin tich dy vao ede tinh chit hod ly cia chiing, thi dy tinh chit din dién, tinh chat hip thy quang.v.v, lién quan true tiép t6i ndng 46 cae chit phin tich. Diém khic bigt co ban gita phuong phip phan tich hod hoe va phuong php phan tich cong cu érchd dé xie dinh chit, phuong phép phan tich hod hoc dra vio ede phan ting hod hoe e6 thurée do Li khdi rong chit, thé tich dung dich, cin cée phuong phap phan tich edng cu c6 thude do la tin higu duge ghi lai dud dang mot vach phd, mOt xung dign v.v Trang bj ciia mt phing thi nghiém phin tich hod hoc bao gim cde dung ew thuy tinh, nlur buret, pipet, ng dong, thiét bi nung, siy, cn, edie dung cu kém theo dé két tita chat, Loc rita két ta v.v Trang bi cia mot phéng thi nghiém phan tich céng cy gdm cdc thiét bi hién dai hon, it tién hon, duge chia kim 3 nhom: inh dinh mire .v.v, dé phan tich trong lugng can c6 cic + Nhém ede thiét bi phiin tich quang hoc bao gdm: cde méy do phé hap thy phan tir UV- VIS, may do phé hap thy nguyén tir va miy do phé phat xa nguyén ti. + Nhém cdc thiét bi phan tich dign hod gdm: céic may do thé va do dong dign lid ‘quan ti ndng 6 cia chat phin tich trong dung dich, do li cde miy cue phd voi hé dién ‘cue khiée nhau, cde miy do thé v.v + Nhom cdc thiét bi tich, bao gim tach sic ky va tich chiét. Téich 1d mot ky thudt phan chia riéng biét cdc chat tir mot hn hop. Két hyp voi phiin nhén biét bing quang hoc hoge dign hod, c6 thé dinh Iugng chit phin tich & giéi han phat hign thip ct phan ti (ppm), phin ty (ppb), 461 khi ti phiin nghin ty (ppt)Mot phng thi nghiém phan tich tuy theo nhiém vy mi trang bi ede thiét bi cho phi hop, tuy nhién phai dim bio tinh phé théng, trang bi céc thiét bj thong thudmg dé chudn bj miu va phan tich cdc chat da lugng, vira dim bao tinh hign dai, c6 cdc thiét bi ti hin tich duge cc chat co him lugng thip, vét va siéu vét. Sy két hop ca phin phan tich hod hoe va phan tich cng cu la khong thé thiéu. Trong xu thé cita hoi nhap khu vue va toan cdu, ching ta ngay cing phai nding cao chit lugng ciia moi logi hinh sin phim trong dé khong it ede sin phim c6 déng gop cia ‘chuyén nginh Hod hoc Phan ich. Dé la phan tich nguyén ligu va sin phim ea qui trinh sin xudt trong néng nghiép cling nhu trong néng nghiép, phan tich céc miu trong nghién ‘iru khoa hoe, phan tich lim sing, phan tich ede miu phye vu cho qua trinh diéu tra phi an, v.v. M6t khéi Iugng khéng 16 cdc miu phin tich nu vay khéng it mau lién quan trye tigp t6i surthanh bai eda mot doanh nghiép, sire khot, va dic bigt ld sinh mang chinh tr ‘cla con ngudi. Digu dé néi lén nhu cdu thye té ddi hoi tinh chinh xdc va tinh ding din celta ede két qua phan tich Dé gilp sinh vign c6 nhimg kién thite co ban vé thye hinh Hod phan tich, dip img cho cong vige khi ra truvimg, ching 161 43 bién sogn lai cudn "Thye tp phan tich dink lrgng, phin 1 edie phurong phiip phan tich hos hge" nhiim trang bi cho sinh vign nhimg kién thie va nhing ky ning co ban vé phin tich dinh Luong. ‘Cudn sich gdm hai phin: Phin 1 1a cdc bai thye hanh phan tich dinh long co ban, Trade hét, ede ky thuilt kim vige v6i ede dung cu ding trong phan tich dink luomg nur en phan tich, dung cy thuy tinh v.v., sao cho dip img duge cic nhu cu 46 chinh xde cla phuong phip. Bén phan img co ban li axit-bazo, tao phife, két ta va oxi hod khirda durge ‘cu thé hod thanh ede bai xde dinh néng 46 cde chit. Sau mdi phiin c6 cdc bai kiém tra diinh gid ky ning thye hinh ciia sinh vién bing cdc miu cia phing thi nghiém, Phin 2 18 cde bai phan tich ee miu thue té, bao gbm cde quy trinh di duge kiém nghiém diroe dp dung phin tich cée miu thye nhur miu thye phim, miu nude, hop kim, én duge trang bj cdc kién thite lién quan dén miu tién phan bon v.v. Trong phn nay, sinh thyc té, cde tinh hudng phai xir ly dé thu durge két qua phan tich chinh xéc. Dé co duye cudn sich nay, ching t6i di durge sy gop ¥ rit quy biu cita cée Thi C6 cia b} mon Hod phn tich, khoa Hoi hoc, Trumg Dai hoc Khoa hoe Ty nhién cing, nhur cia nhiéu ding nghiép khée. Nhan dip nay, ching t6i xin chin thainh cim on cde Thay, C6 va cdc ban déng nghigp. Do théi gian c6 han, cudn sich khong khéi c6 nhing thiéu s6t, rit mong durge su gop ¥ cita de gid dé cudn sich ngay cing hoan thién hon.Cae te gid PHAN 1 PHAN TICH DINH LUQNG HOA HQC CO BAN CHUONG 1 PHUONG PHAP CHUAN DO AXiT - BAZO BAI 1: CHUAN DO DON AXiT, DON BAZO. 1.1 HIBU CHINH THE TICH BURET LAL Thwe hanh can meie cit (Cac logi edn phan tich va cach sir dung d& tinh bay 6 phy lye 1 tang 87-88) Nguyén tic: Thanh trong ciia buret thutmg kh6ng thing déu, nhung khi san xuat ngudi ta thug dinh du thé tich theo khong cach, digit 46 din ti sai léch thé tich eta timg doan cedng nhu eta cd buret. Can nude edt dé tim ra thé tieh thye cua timg doan sau d6 biéu dign sursai léch vao d6 thi va digu chinh trong qua trinh phan tich sau nay. ‘hinh: Ria sach buret, tring nude cat hai lain, khong cdn sly khd, ly nude cdt vaio buret dén ach “0”. Mt céc can c6 nip day dat 6 dudi buret, cin thé tich cita timg doan, méi dogn Smil, cho ti hét thé tich buret (50m! hojic 25 ml), sau do lap bang sé ligu theo miu bing 1 va vé d6 thi biéu dign sai Igch thé tich, gid thiét phép do duge thye hign 6 30°C (hinh 1), Bang 1: Bang sé ligu higu chinh thé tich buret. STT] Thétich | Khoi luong | Nnigtdg, | Thétich thye Avml cede doan nue SC | gHL0/ (250/100) | (Vay-Varnn) I 05 30 X; 10,99492 - 5 | % 30, Xs 10,99492 ¥ 6 |X 30, Xp 10,99492 ¥ 8 im 30, Xx 10,99492 ¥ 109 40-45 | Xo 30 Xo 10,9492 ~ 10 4550 | Xo 30 Xi0 /0,99492 1.1.2 Ve dueimg cong higu chinh thé tich buret Ay, ml +005 - 0,05 Hinh 1: Butmg eong higu chinh thé tich buret 1.2 PHA CHE DUNG DICH CHUAN AXIT OXALIC DE XAC DINH BAZO Neuyén tie: Ngu’vi ta céin mot lurgng xée dinh chat géc trén cén phan tich ¢6 a9 chinh xe 0.0001 hose 0,00001 g, hod tan dinh Iugng lrong edn trong binh dink mire e6 dung tich thich hgp ri pha loang bing mrée t6i vach, Tién hinh ; Cin, pha dung dich chudn H,C,0, 0,025 M (M=126,066) Cin chinh xéc 0.7879 gam H,C,O,.2H,0 c6 49 tinh khiét phan tich trong céc edn, chuyén axit qua phéu vao binh dinh mirc 250m! (hinh 2). Tring cdc can 3 Lin biing nudge ct vao binh dinh mirc. Thém khoang 150ml nude cét nita va Ide ki cho tan hét sau 46. thém nude cit dén vach mite, lic ki dé ton déu, ta c6 dung dich chudn axit oxalic 0,025M. A SY Hinh 2 Pha dung dich axit oxalic 1.3 XAC INH NONG BO CAC DUNG DICH BON AXIT, BON BAZO ul1.3.1 Thiét lap néng dé dung dich NaOH theo dung dich gc H,C:0, Neuyén tic: phurong phap c6 co sé la phan img trung hod H,C,0, + 2NaOH > Na,C,0, +20 Axit oxalic e6 pK1=1,25; pK2 = 4,27. Do bude nhay thir nhit ngin, phai chuan 46 dén mudi trung hoa. Tai diém tuong duong thir hai, dung dich chi co mudi bazar NasC,0., 6 pH = 9, lim déi mau chi thi phenolphtalein, nén phép chusin 4 két thie khi xuat hign miu hdng bén trong 30 gidy cita chit chi thi, ‘Tién hank: Ding pipet lay chinh xée Vil (10ml) dung dich axit oxalic chuin vio binh non co 250ml. Thém 2-3 gigt dung dich chat chi thi phenolphtalein 0,1% trong edn, lic du. Tir buret, vita nho tir tir dung dich NaOH cdin xée dinh nding a8 vao binh nén, vita lie déu dén khi dung dich xuit hign miu héng thi ngimg chudin 49. Ghi s6 ml NaOH da chudin 49 - Vo ml, Lam 3 Lin va lay két qua trung binh, Néng dd mol/l dung dich NaOH duge tinh theo cdng thire 1.3.2 Xée dinh nong dé dung dich HCL Nouyén tie: Co si eta phucrng php dua vio phin ting trung bos: HC1+ NaOH = NaCl+H,0 Tai diém tong duong, dung dich mudi NaCl ld mudi tring tinh, pl duimg cong chuin 46 ¢6 bube nhiiy pH lin (4-10), e6 thé ding ede chit chi thi 1a phenolphtalein hog metyl da cam, metyl d6 v.v. Tién hanh: Lay chinh xée Vl (10ml) dung dich HCI can xéc dinh ning 6 vao binh non ef 250ml, thém 2-3 giot dung dich chit chi thi. Tir buret, nho dung dich NaOH da biét ndng d@ vao va lic déu binh nén cho ti khi dung dich cé miu hing bén trong Khoiing 30 gidy thi dimg chudin d. Ghi sé ml dung dich NaOH 4a chuin d6 - Vom. Lam 3 Kin rdi lay két qua trung binh va tién hinh thi nghiém véi hai chit chi thi va so sénh két qua, giai thich (khi ding chat chi thi metyl da cam thi mau cla dung dich chuyén tir 46. sang ving). Nong d@ mol/l eta HCI duge xe dink nbur sau: hon ita1.3.3 Xée dinh néng dé dung dich CH;COOH Neuyén tie: Cosé cia phuong phaip dya vio phan img trung hoa: CH,COOH + NaOH > CH,COONa + 1.0 Twong ty nhu phép chuin d6 axit oxalic, tai diém wong duong chi cé mudi NaCH;COO, cé pH = 9 nén sir dung chat chi thi phenolphtalein hanh: Ly chinh xe Vinl (10ml) dung dich axit axetic vio binh nn e& 250ml thém 2-3 giot chit chi thi phenolphtalein, Tir buret, nhd dung dich NaOH da biét néng 46 vao, tic déu cho t6i khi dung dich cé miu hang bén trong khodng 30 gify thi dimg lai. Ghi sé ml NaOH di chudin d@ - Vol. Lim 3 lin C ty két qua trung binh, Y, Vv, C Tién hanh tuong ty vos chit chi thi metyl da cam, so sinh cic két qua va gidi thich. 1.3.4 Xée dink ning dé dung dich NH; Nguyén tie: Cosé cia phuong phap dya vio phan img trung hoa: NH + HCl NHC +H.0 ‘Tai diém wrong duong, mudi NH,Cl, c6 pH = hinh: Ding pipet ldy chinh xéc Vml (10ml) dung dich NH, can xde dinh néng 46 vio binh nén e&+250ml. Thém 2-3 giot dung dich chit chi thi metyl dé rditién hinh chun 9 biing dung dich HCI da biét ning 4. Khi dung dich chuyén tir miu ving sang miu dd thi dig chuin 4. Ghi sé ml HCI di chudn dQ - Voml. Lam 3 Lin va ly két qua trung binh. Nong d@ mol/l cia NH, durge tinh nhur sau: = SucrVo wa, = NHS nén sirdung chat chi thi: metyl do. én hanh rong ty véi chat chi thi phenolphtalein, so sinh cdc két qua va gidi thich. 1.3.5, Xée din ham turgng mudi amoni theo phiong phép focmalin Nguyén tic: Muéi amoni tic dung voi HCHO trong mde ( HCHO.H;0) tgo ra hong axit turong img duge xde dinh bing NaOH. ANH,’ +6CH:0-— (CH:),N.+4H"+ 61,0Tién hinh: Ding éng dong liy 5 ml dung dich focmalin vao binh nén 250 ml, pha loang bing nude cdt dén 20 ml, thém 2-3 giot chi thi phenolphtalein va trung hod luong HCOOH 6 trong focmalin bing dung dich chuin NaOH dén mau hing, (Can tn edn phan tich a g NH,CI (khong 0,2-0.3 g), dé vao dung dich focmatin da trung, hod & trén, Lie edn than hn hop, dé yén 3-5 phiit va chudin 6 lugng axit giai phong ra thing dung dich chuin NaOH. Ghi s6 ml NaOH tigu t6n_cho qua trinh chudn 49, Ham lurgng N-NH,* trong mudi NH,C! duge tinh theo cng thite: Crwon-Vrcou-M yy X yy. (= 100 a 10004 BAI 2. CHUAN DQ DA AXIT 2.1. DUNG DICH CHUAN 2.1.1. Pha ché dung dich chudn tie fixanal Neuyén tic: Ding nhimg lugng chit chit rin hay nhimg thé tich chit long tinh khiét hod hoe da duye ean, do chinh xée dung trong éng fixanal (hinh 3)Mé pha ede dung dich 66 49 chuiin xe dinh, Fixanal 1a éng bing thuy tinh cé céu tao dc biét: c6 hai vi tri rit mong gidp ngudi phin tich c6 thé d& ding ding dia thuy tinh dé choe thing, sau dé chuyén toan bo chat & trong fixanal vio binb dinh mie bing tia nude eft sau d6 hod tan vi dinh mic Hinh 3: Fixanal chia chit chun (Cée diém 1,2 trén hinh vé la cde diém edn phai duge choc thing bing dia thuy tinh & chuyén vio binh dinh mite) Trén méi éng Fixanal ngudi sn xuit di ghi r dung tich can pha dé thu duge ndng do nhit dinh, Thi dy: Fixanal dung Na;B,0;.10H:0 trén d6 6 ghi“N/10" nhu vay, nguis ta i cn 19,0685gam NasB,O;.10H,0 dé pha thanh Hit dung dich e6 ning 6 0,1N hay 005M. 421.2 Thiét lap néng dé dung dich HCI theo nati tetraborat Muéi natri tetraborat két tinh (NazB,0;.10H;O) 6 khéi Iuong phan tir lon 1,37), 06 thé ding lm chat gc. Trong dung dich long, ion tetraborat phin ting v6i H’ tgo thin axit boric: BO; + 2H" +5 1,0 4 1B0; Axit boric la da axit yéu, pK, 3 pK=12,74 ; pKy = 13,8. Do K, > Ky, Ky 6 thé xem nhur don axit yéu e6 pKx= pK, Khi chudin d6 dung dich natri tetraborat bing dung dich HCI, tai diém tuong durong, hinh thinh axit boric, do d6 tinh pH tai diém trong, durong nhur mét axit yéu: pHy = U2pK, - W2IgC, = 462 +05 = 512 éi vi pH nay e6 thé ding metyl d6 dé Lim cht chi thi. ‘én hinh: Can chinh xe 2.3835 Na;B,O>.10H,O cho vio binh dinh mize 250 ml, thém Khoding 150 ml nude céit néng, lic k¥ cho tan hét, dé ngudi dén nhiét dd phong thém nube cit i vach mire, dao ky, ta c6 dung dich néng 46 0,025M. Lay V, ml (10 ml) dung dich natritetraborat c6 néng 4} C, via diéu ché vao binh non 250 ml, thém vio mBi binh 2-3 giot dung dich metyl do (c6 khong di miu 4.4 - 6,2) dung dich e6 miu ving. Tir buret nbd timg giot dung dich HCI cho t6i Khi dung dich cchuyén tir miu ving sang miu da eam, hét V ml HCL Dé phép chuin d6 duge chinh xie din ding dung dich d6i chimg 1a dung dich 100 ml axit boric loding ci 1 % trong dém ¢6 pH =5,1-5.2 cé thém 2-3 ml NaCl 1 M va 2-3 giot dung dich chit chi thi metyl dé, dung dich co miu da cam. Tién hinh chudn 46 ba Lin, dy két qua trung binh, Nong 46 mol/l HCI duge xée dinh nbur sau pq = 2M Vv 2.2. XAC BINH NONG BO BA AXiT VA MUOI CUA NO 2.2.1. Xée dinh néng dé dung dich H,PO, bing dung dich chun NaOH Nguyén tie: Cosé cita phuong phap dya vio phan img trung hod HPO, theo hai nie: Nae 1 : HsPO, + NaOH + NaHPO; + HO HyPO,€6 pK, § pK: = 7.21, pk = 12.36; Tai diém tuong duwmg 1 pH = 1/2pK, + 1/2pk2 hodic metyl d6 c6 p’ tam chit chi thi, 4,665, ding metyl da cam e6 pT = 4 15Nie 2 : NaH:PO, + NaOH + Na:HPO, + H:0; Tai diém tung duong 2, pH = 12pK, + 12pK, = 9.785, ding phenolphtalein c6 ‘pT9 lam chat chi thi 14 phi hgp. hinh: Ding pipet lay chinh xe Vl (10ml) dung dich HPO, cho vio binh nén et 250ml. Thém 2-3 giot dung dich chit chi thi metyl da cam, dung dich e6 miu dd. Ding dung dich chuin NaOH chuiin 49 t6i khi dung dich tir miu d6 chuyén sang miu ving thi ding lai. Ghi s6 ml NaOH da chudin d6 - Vm. Thém vio dung dich chun 49 2-3 giot chit chi thi phenolphtalein, tiép tye chudn d6 (ndc thir hai cla axit HsPO,) bing NaOH ccho ti Khi dung dich e6 miu hing bén trong 30 gidy thi dimg Iai, ghi sé ml NaOH da chudin 49 ~ Voml. Lim 3 lin ly két qué trung binh, 22.2, Xée dinh néng dg HCI vi HyPO, trong ciing hin hop Neuyén tie: Ding dung dich NaOH dé chudn 46 HCI va HsPO, voi hai chat chi thi la metyl da eam va phenolphtalein, Khi metyl da cam déi miu (pT4), todin bG HCI da due chudn d6 cling véi nde 1 cua axit H,PO,. Khi phenolphualein adi mau (pT=9), nde thir hai cia HPO, duge chuan 49, sé mol NaOH ding cho nic niy chinh li sé mol H;PO,. S6- mol NaOH chénh Ich cia hai Kin chudin 49 chinh La sé mol HCL hinh: Lay chinh xde 10m! dung dich hn hop HCI vi H:PO, edn phin tich cho vio binh nén c& 250ml; thém 2-3 giot dung dich metyl da cam, lie déu vi chudin 4 bing dung dich NaOH c6 néng 4} C ti khi dung dich chuyén sang mau ving. Ghi sé ml NaOH di chun d6 (V;). Thém vio 3 giot dung dich phenolphtalein va tiép tue chulin 49 ti khi dung dich chuyén sang mau héng. Ghi sé ml NaOH da chun 49 Hin 2 (V2). Lam 3 Hin rbi ly két qua trung binh. Nong 49 mol/l cla axit photphoric duge tinh nhur sau: (V-V,).C 10 2.2.3. Xée dinh néng dé KH;,PO, va K3HPO, trong cing hon hop Nguyén te : C6 2 cdich xe dinh hén hop trén - Ciich 1: Chuin d@ bing KOH cho téi déi miu chat chi thi phenolphtalein dé xéc dinh KH:PO,, sau d6 ding HCI dé chuiin 46 dung dich via nhin duge ti chuyén miu Ciro, 10 ‘HC 16metyldacam (liic nay ca hai mudi déu phin img) sé milimol HCI chinh a tang milimol ‘cit hai logi. Higu sé milimol ea HCl vi KOH a sé milimol cla KzHPOs. - Cach 2: Chuin 46 bing HCI cho t6i déi miu chit chi thi metyl da cam dé xde dinb K:HPO,, sau dé ding KOH chudin 49 dung dich vita nhiin duge cho tai chuyén mau phenolphtalein dé xc dinh tong sé. Higu sé milimol cla KOH va HCI chinh la sé milimol et KH:PO.. hin :(1im theo eich 1) Ly vio binh nén 10 mi dung dich miu phan tich, thém 2 ‘ot dung dich chit chi thi phenolphtalein. Ding ding dich NaOH c6 ning 4 C, chu‘in 49 t6i xudt hign mau héng, hét Viml. Thém vao dung dich vira chun dO 3 giot dung dic metyl da cam, ding dung dich HCI e6 ning 4 C; chun d@ cho ti khi dung dich xuit hign mau do, hét V,, ‘Tinh két qua: Ning d6 KH.PO, vi néng d9 KsHPO, due tinh theo e6ng thie Cy, BAI 3 CHUAN DQ DABAZO 3.1. CAC DUNG DICH CHUAN 3.11. Thiét lap néng dé dung dich HCl theo NaxCO; Natri cacbonat khan cé .99, 1a mudi trung hod cla axit cacbonic (H,CO,). Mudi Na,CO, tinh khiét, khan cing durge diing Lim chat gée duge chuin bi bing cach nung Na;CO; loai tinh khiét phan tich t6i khéi lugng khong adi 6 270°C trong tu sdy 1 it Phan img gitta HCI vl NazCO; 0,1M c6 hai nic nhur sau: Na,CO, + HCI > NaHCO, + H:0 NaHCO; + HCI —>H,CO; + NaCl Axit cacbonie c6 K, = 4,3.107; K, = 5.61.10" hay pK, va pK, eta nd tuong img li 6,35 va 10,32, Tai diém tuong duong thir nhit ta c6: 7_ pK, + pk, _ 637 + 1025 2 2 Voi pH nay, ta ding phenolphtalein lam chat chi thi Tai diém tuong duremg thir hai, hinh thinh H,COs la da axit yéu, my nhién Kj>>K, IM (bo qua pha loding), pH due tinh nhur sau: pH, = 821 nén xem nhu mot don axit yéu, C= pit = pk, Ling Ca=3385 +05 3688 Nhu vay sir dung chit chi thi metyl da cam lim chat chi thi la phi hop. hanh : Can chink xe trén cn phan tich a gam Na;COs khan, p.a (khodng 0,102), cho vio binh nén 250ml, thém nue cat, lic déu dén tan hét. Thém 2 gigt dung phenolphtalein, chun 4 bing HCI cho dén khi dung dich mit mau hdng, hét Vml. Thém tiép vai giot dung dich metyl da eam (hoe bromocresol xanh) va chuin 46 tiép bhing HCI cho t6i khi dung dich e6 mau da eam (hoje miu xanh ld ey), dun s6i dé dudi H,COs, dé ngudi, lie ny dung dich e6 pH-8.3. Tiép tue chuiin 46 t6i khi dung dich chuyén sang mau da cam hoje mau xanh li cay, hét tng cOng Vom. Nang 46 mol/l HC! duge tinh nhur sau: 3.1.2 Thiét lap néng dé NaOH theo HCl dé chudn (Xie kip ndng d6 NaOH theo HCI duge tién hinh giéng myc 1.4.2 trong bai 1) 3.2. XAC BINH DA BAZG BANG AXiTMANH 3.2.1. Xéc dinh néng dé Na;CO, va NaHCO; trong hén hop Vige xie dinh NaxCO, va NaHCO; trong hén hop durge thye hign theo 2 edch: Céch 1: Chuin 4 hén hop bing HCI véi chat chi thi phenolphtalein. Khi d6 1 née NasCO, bi trung hoa thinh NaHCO, sau 46 tigp te chun 49 téng NaHCO, bing dung dich chudn HCI véi chat chi thi metyl da cam, Két hop 2 giai dogn chuan 46 sé tinh duge ham rong NaxCO, va NaHCO; (sinh vién ty thiét ip qui trinh thi nghiém va cing thire tinh him huong timg chat) 18Céch 2: Chuan &9 hin bop NasCO, vi NaHCO; bing HCI khi c6 chit chi thi metyl da ‘eam. Sau d6 thém mt lugng dr chinh xe dung dich kiém vio miu Khe ¢6 dung dich hin hgp 2 mudi dé chuyén ching thinh mudi cacbonat va thém tiép hrong du BaCl, dé tao két tia BaCO,. Khong cén loc két tita, chudn 46 hrgng kiém dur khi c6 mit chat chi thi phenolphtalein HCO; +OH +CO#+H,O ; Ba +CO,* > BaCo; ‘Caich nay cho két qui tét hon khi hén hop can phan tich chia NaHCO; it hon Na;COs. hinh (theo céich 2): Hut 10 ml hén hgp cdn chudn 49, thém 2-3 giot dung dich chit chi thj metyl da cam va chudin d6 dén khi dung dich cé mau da cam, hét V, ml, Ly 10 ml dung dich miu phan tich méi, thém vaio 4625 mi dung djch chin NaOH, 10 mi dung dich BaCl; IM va 2-3 gigt dung dich phenolphtalein, Chuan 46 luromg kiém dur dén mat miu phenolphtalein, hét V2 ml. Him lrgng Na,CQ, va NaHCO, duge tinh theo eng thie sau: 3.2.2. Xée dinh hime lieong Na;CO; trong NaOH cing nghiép Nguyén tic: Phan img gitta Na,CO, véi HCI 6 2 nic. Tai diém tung duong thir nhit, dung dich sé e6 pH khoing 8,21 (xem mye 3.1.1 bai 3) nén ding chit chi thi phenolphtalein Li phi: hop. Mat khiic khi chuan 4} bazo manh bing axit manh, duimg_ cong chudin 46 c6 buée nhay & pH 4-10, khi két thic voi chat chi thi phenolphtalein, toan bd NaOH cing phan img hét yéi HCl, ede phin img nhur sau: NaOH +HCI—>NaCl+H,0 ; NaCO;+HC > NaHCO, + H.0 Nh vay s6 milimol HCI cing chinh 1a sé milimol téng cita NaOH va NazCO; khi phenolphtalein mit mau héng. Chuin 46 tiép bing HCI t6i twong duong 2 sé phan img: NaHCO; + HCI > NaCl-+ H;CO; Tai diém tuomg duong 2, dung dich H,CO, ¢6 pH ~ 4, lim di miu metyl da eam tt ving sang d6, sé milimol HCI phan img & diy 14 sé milimol Na;COs. Higu sé ciia sé milimol HC! téng sé va sé milimol HCI cia phin img sau la sé milimol cba NaOH. 19Tién hanh: Can chinh xée a gam miu (khoing 1,0-1,5 gam) cin kiém tra cho vio binh dinh mie 250ml. Tring eéc can ba lin bing mrée edt vao binh dinh mirc, thém khoang: 100m! nue, lic déu cho tan hét rdi thém nude ct dén vach mire, tron déu, day nit ngay. Nurée cit ding 4 pha xt cin dun sdi ki rude dé dudi hét CO, hod tan trrée khi dem dang. Ding pipet huit chinh xe Vl (10ml) dung dich vira pha vao binh nén 250ml. Them 2-3 giot dung dich phenolphtalein (dung dich c6 miu héng). Tir buret nhé timg giot dung dich chun HCI cho dén khi mit mau héng thi ngimg chun a9. Ghi sé ml HCL - Vim. Thém vio dung dich 2-3 giot dung dich metyl da cam (dung dich e6 miu ving) vi ehuin 4 tiép bing HCI. Khi dung dich chuyén sang miu do thi ngirng chudn 49. Ghi sé ml HCI i chun d6 (V2 ml). Lam ba Lin r6i ly két qua trung binh, Cyaan = Cee = Va) €na,co; = GNa,CO, = CUueV2106 250 199 1000.a ‘10° 42.3, Xée dinh d@ ciong tam thai cita muréc méy Neuyén tic: DO cimg tam théi cua nude 1a do sur co mat ciia cae hidro cacbonat cla Ca, Mg doi Khi cd et Fe. Dé cig nay e6 thé duge logi bo bing ech dun s6i mde. Khi d6 ‘cic mudi hidro cacbonat bi phan huy thanh mudi cacbonat, oxicacbonat va hidroxit khng_ tan trong nude Ca(HCO,). > CaCO, + H,0 + CO, Mg(HCO;) > MgCO3 + H,0 + CO2 2 Mg(HCO;): > Mgx(OH):CO; + H,0 + 3CO> Fe(HCO;): > Fe(OH)2 +2 CO. Khi chuan 46 miu nude bing dung dich chudin HCI c6 mit chat chi thi metyl dacam, s® xy ra phan img sau. Ca(HCOs)2 + 2H" > Ca? +2 HO +2.CO, hanh: Ding dng dong Liy 100 ml miu nude cdn phin tich vio binh nén 250 ml, thém 2-3 giot dung dich mety! dacam rdi chudn 46 bing dung dich chudin HCI dén khi xudt_ mau da cam. 20Sinh vign ty Kip edng thire tinh 46 cimg theo s6 mili gam CaCO, trong 1 lit mide (xem nhur trong nue chi e6 Ca). 3.3. CAUHOL ON TAP PHAN CAC PHAN UNG AXIT-BAZO. 1. Néu ede trang bj co ban eta mot phing thi nghiém Hod Phan tic. 2. Nguyén tie sir dung edn phan tich Li gi? khi mao thi sir dung 3. Neu edch kiém tra dung tich thye eta dung cu do thé tich, 4, Tinh pH cia dung dich axit yéu, bazeryéu, da axit, da bazer, mudi cha da axit da bazo, cede dung dich dm, Tai sao ede chit chun ding trong phuong php chuin d axit-bazo thuimg ding ede ‘axit manh bazo manh chir khOng phai la axit yéu, bazo yéu ? Nguyén tic chon chit chi thi trong phuong phap chudn 49 axit - bazo la gi ? pH thay di nburthé nao dé mau cua chi thi 6 diém eubi thay déi rd ring? Tai sao ? hich tai sao khi dun sOi dung dich tgi gin diém cubi cud phép chun a eacbonat bing HCI sé Lim cho sir chuyén miu ciia chit chi thi 19 rét hon? 9. pK cit axit yéu thip dén mite nao dé cé thé chuiin 46 duge trong dung dich nuée. 10.D9 manh cia 2 axit c’in phai khéc nhau dén mite ndo dé c6 thé chudin d riéng bigt cchiing trong mt dung dich, tai sao? 11.Tinh pH eiia dung dich, vé duémg cong chun d6 khi thém: 0,0 ; 5.0 ; 15,0; 25,0; 40.0 545.0; 49,0 ; 50,0 ; 51,0; 55,0 ; 60,0 ml dung dich NaOH 0,1 M vio a. 50mlHNO> 0,1 M,Ka=4.10* bb. Piridin cforua 0,1 M; Piridin ¢6 Kb = 1,7.10° 10. Tinh pH ciia dung dich va vé duimg cong chun 4 khi thém: 0,0; 5,0 ; 15,0; 25,0 ; 40,0 ; 45,0 ; 49,0 ; 50,0 ; 51,0 ; 55,0 ; 60,0 ml dung dich HCI 0,1 M vio SO ml dung, dich NH; 0,1 M; Kb = 1.10%" ; $0 ml dung dich NaCN 0,1 M; Ka=7,2.10" (CHUONG 2 PHUONG PHAP CHUAN DQ COMPLEXON BAI4 CHUAN DO TRUC TIEP XAC DINH CAC ION KIM LOAL 4.1. CAN PHA DUNG DICH CHUAN EDTA 0,01 MMudi EDTA (NasH.Y. 2H,0 ¢6 Mepra= 372,24) diing dé pha dung dich chun 1a loai tinh khiét phin tich, e6 46 dm 0,3 - 0,5 %. Trude khi cin pha cdn phai dé mudi trong bat Khong cé nip va dé trong desicator khoang 1 ngay dém dé loai hoi dm bim trén bé mat tinh thé. Quy trinh: Cin trrde thuyén can (céc can) dé biét trong lrong, thém 0,9306g EDTA vao_ thuyén can, digu chinh Iugng can cho t6i khi dat vi tri thing bing, Khoa cin, chuyén toin bp long EDTA vio phéu dit trén binh dinh mite 250ml, diing binh edu tia chuyén todn b EDTA vio binh dinh mite (hinh 2, trang 3), tring lai phéu ba Lin, sau dé thém nude edt dén khoding 100 ml, lic kicho tan hét EDTA. Pha loding biing nuise cat dén vach mite, ta ¢6 dung dich EDTA 0,01M. 4.2. XAC DINH CAC ION KIMLOAL 42.1. Xée dinh néng dé Zn, Mg’*, Pb**, chét chi thi ETOO 6 pH=10 a/ Xie din Zn*, Mg* guyén tie Co sércita phuong phap la phan img tgo phite bén cla Zn, Mg™ voi EDTA 6 pH=10. Zo™ + HY? > ZnY? + 2H" ‘Chit chi thi ET-O0 6 miu xanb khi ér dang tyrdo, e6 miu d6 ho khi é dang phite Sit diém tuong duomg, EDTA phin img véi phire Znlnd chuyén ching tr lai dang ty do ¢6 mau xanb, Zand (46 nho) + HY" — ZnY* + Halnd (xanh) 1 hinh: Dizng pipet léy chinh xée Vnl (10ml) dung dich Zn* hose Mg’ edn xe dink vio binh nén e& 250ml, Thém 20m! nude edt nia, thém Sml dung dich dém amoniae va mt it chat chi thi (dung dich c mau dé nho). Lic déu va tién hinh chudn 49 bing dung dich EDTA da biét ndng 46. Khi dung dich co mau xanh biée thi ngimg chuin 40. Ghi 6 ml EDTA da chudn d@ -Voml. Lam ba lin rdi lay két qua trung binh. Nong 46 mol/l ciia Za va Mg duge tinh by Xie dinh_Pb* Nouyén tie: Sir dung EDTA dé xc dinh rit dinh lugng do Pb* tao phire bén wi EDTA mdi trudng trung tinh hole kiém. Pb" + HAY? > PbY? + 2H"Tuy nhién Pb* cing rit dé thuy phan nén khi chudn 49 v6i chi thi ET-OO & pH=10, truée khi ting pH cin cho thém tartrat hode trietanolamin dé tao phire phy kém bén sé tranh duge hign tong trén. hinh: Ding pipet lay chinh xéc Vil (10ml) dung dich Pb** cin xic dinh vao binh non cd 250ml, Thém 20m! nude eft, Sm! dung dich KNaC,H.O, 1M, bic déu, thém Sml dung dich dém amoniac va mét it chit chi thi ET-OO. Dun ndng nhe dén khoding 50°C va. tién hanh chudn 49 Pb** biing dung dich EDTA da biét nng d6 cho dén khi dung dich chuyén tir mau do sang miu xanh, Ghi sé ml EDTA di chun d@ - Voml. Lam ba Lin liy két qua trung binh. 42.2. Xéc dink NF*, Cu’, Ca°*, chi thi murexit al Xie dinh Cu?*, Ni?* voi chat chi thi murexit & pH 8 Neuyén ti: Dya trén phan img tao phire bén ciia Cu™ (N Cu’ + HY? > CuY? + 2H" Phan img duge tién hanh eo pH-8, chat chi thj 1 murexit 1% trong NaCl. (CuHnd’ (ving nhgt) + HEY? — Cu? + Hund’ (tim) hnh: Ding pipet lay chinh xde Vil (10ml) dung dich Cu* (Ni**) vio binh nén c& 250ml, thém mot it chit chi thi murexit, ding dung dich NH, IN dé digu chinh pH = 8 (thém it dung dich NH, cho t6i khi dung dich c6 mau ving nhgt thong due), Chun a Cu?* bing dung dich EDTA da biét néng d cho dén khi dung dich chuyén sang mau tim. Ghi s6 ml EDTA da tiéu tén (Voml). Lam ba lan ri lay két qua trung binh. Y, c,=Conts Vv ) voi EDTA: ty Xie din Ca?* Neuyén tie: Phuong phip dya trén phan img tao phite bén cia Ca” voi EDTA pH 213, sir dung ‘murexit lam chat chi thi cat + CaHdnd +H. Py cay? + 2H > Ca¥? + Hylnd(ao) (tim) hinh: Ding pipet lay chinh xd Vl (10ml) dung dich Ca’ cin xdc dinh vao binh chi thi murrexit (1% trong NaCl). Lic déu, dung dich c6 miu do. Chun 4 bing dung dich EDTA di biét néng 4 cho t6i khi dung dich chuyén sang mau tim. Ghi sé ml EDTA da cchudin 49 - Vom, Lim ba Kin roi Lay két qua trung binh, Ti non e@ 250ml. Thém 20ml nude edt nia, thém 2m! dung dich NaOH 2N va mot it cl ~ Cra Coa = v 42.3. Xée dink Fe, chi thi axit sunfesalixylic -HSSal Neuyén tie: Fe** tao phite bén voi EDTA trong méi trudng pH Fe" + HAY" > FeY +2H" FesSal’ + HY? — FeY + H,SSal do tim ving khémg mau Tién hinh: Dimg pipet lay chinh xc Vil (10ml) dung dich Fe** cin xic dinh vao binh non co 250ml. Thém 10 gigt dung dich chat chi thi, lic du. Néu dung dich chua ¢6 mau 4 tim thi thém tir tir timg giot dung dich dung dich NaCH,COO 5% lic déu cho toi khi xudt hién miu do tim, Dun néng dung dich ti 60-70°C, tién hinh chun 46 bing dung dich chuin EDTA cho t6i khi dung dich tir miu 0 tim chuyén sang miu vang bgt. Ghi s6 ml EDTA chudn 4 - Val. Lam ba kin 10i ly két qui trung binh. CevmVo v 4.2.4. Xée dinh Cit* vi chit chi thi PAN, pH=5 Jon Cu(ld) phan img. véi EDTA & pH 5 chim, tuy nhién phin img xy ra hon todn trong diéu kign néng > cuy? + 2H > CuY? + Hind tim dam ving tuoi hanh: Dung pipet ly chinh xic Vl (10m) dung dich Cu** can phn tich vio bin rnin c@ 250 mi, thém 10 ml dung dich dém acetat pH!= 5 hoge khong 2 gam urotropin va 3 giot dung dich chit chi thi PAN. Dun s6i dung dich va chudn d biing dung dich chunEDTA cho dén khi dung dich chuyén tir mau tim dim sang mau vang lye, hét V, ml, nong 49 mol cia ion Cu?* duge tinh nhur sau: ViCeors Comm = 10 BAI 5 CAC KY THUAT CHUAN DQ COPLEXON Ngoai ky thuat chun d9 true tiép dé xée dinh ning d6 cée ion kim logi, phuong phip complexon cdn str dung ede ky thugit chun dd phan don, chusin d9 ngurge, chun 4 thay thé 5.1. CHUAN DO PHAN DOAN, XAC BINH Bi* VA Pb"? euyén tie Phin img to phite cia Bi* voi EDTA e6 thé thue hign 6 pH =1-3 trong khi Pb?* phan img voi EDTA pH=5-6, ding théi cdc ion nay déu tgo phire mau véi chat chi thi xilenol da cam pH tuong img. Vi vay xc dinh Bi** & pH 1-3 sau dé diéu chinh pH ti 5-6 rbi tigp tue chudin d6 Pb, Bi + HY? 9BIY 42H (pH= 1-3) Pb? + HY? > PbY? +2H" (pH=5-6) ‘Chat chi thi xilenol da cam 1% trong KNO, (dang mudi) hog trong cin etylic. hin Ding pipet ly chinh xe Vil (10ml) dung dich phan tich vio binh nén ed 250ml. Chinh pH vé 2-3 bing dung dich NH, 5N (theo gidy cng go dé), Thém mgt it chit chi thi, lic déu, dung dich c6 miu do. Ding dung dich EDTA di biét ndng 49 chudn 4 Bi** cho ti khi dung dich chuyén sang mau ving. Ghi sé ml EDTA tigu tén - Vymi. Thém khoang 1g urotropin vio dung dich lie déu, dung dich tré lai miu do. Chuan dO tiép biing dung. EDTA t6i khi dung dich chuyén sang miu ving Ghi sé ml dung dich EDTA chudn d - ‘Vom. Lim 3 Lin dé Ly két qua trung binh, tie dung véi mot luong durchinh xac EDTA da biét ndng d} & pH =10 sau 46. chudin d@ lugng dr EDTA bing Zn? da biét ndng d6 voi chat chi thi ETOO.Po} = + HAY? > Phy? + 2H" (du) + Zn > Zny? + 2H" Zo* +HeInd (xanh) > Znlind (do nho) + 2H" ‘Tign hah: Ding pipet lay chinh xc Vml (10ml) dung dich Pb* cn xéc dinh vao binh non ci 250ml. Thém chinh xée mot lugng du EDTA (V,ml) da biét ndng d6. Thém tiép 10ml dung dich dém amoniac va mgt it chit chi thi ET-OO, lic déu, dung dich co mau xanh, ‘Chuan d@ bing dung dich chuiin Zn?* cho ti khi dung dich chuyén sang mau d6 no. G s6 ml Zn** da chun 46 - V.mil, Lam ba lan rdi léy két qua trung binh, Cams ~ Col, v ¢, 53.CHUAN BO THAY THE S31. Xée dink Pb?* Phire PbY? va MgY* 6 logarit hing s6 bén Lin lugt i 18 va 8,7 cho nén trong moi truimg dém amoniac, Pb™ sé diy Mg™ ra khoi MgY* mot cach dinh lung. Chuiin 46 Mg" sxe dinh due Pb. Pb?* + MgY? > PbY” + Mg”* MgInd(dé nho) + HY" > Mg hnh: Lay 20m! dung dich Mg”* vao binh non cé 250ml, cdc bude chuan d6 tiép theo nhu khi xic dinh néng dG Mg”* trong bai trude (myc 6.3.1), ta co dung dich complexonat magic. Lay chinh xc Vil (10ml) dung dich Pb°* can xde dinh cho can than vio dung complexonat vita méi diéu ché xong, lie ki, dung dich tir miu xanh lai chuyén vé miu dd nho. Chun lugng Mg™ giai phong ra bing dung dich EDTA da biét néng 9 cho dén khi dung dich chuyén sang mau xanh. Ghi sé ml EDTA da chudin 49. Lam 3 lin roi lay két ‘qui trung binb, Hind(xanh) prs Vers Cy Vv 5.3.2. Xée dinh Ba khi cé mat Mg* hoe Mg Neuyén tie:‘Cac ion kim logi Ba va Mg” déu tgo phite voi complexon IIL, ¢6 hing s6 bén xdp xi nhau, tuy nhién Ba** ¢6 kha nding tgo phite mau véi chit chi thi ET-OO kém hon Mg”. Khi chuin 49 hén hop niy é pH =10, tai sit diém wong durong, Mg” s& phin img véi chit chi thi tét hon nén phic Mglnd cdn lai sau cling trate Khi phin img voi EDTA dé cchuyén thin bi thi tye do, sy thay di miu rd et kim cho phép chun 9 chinh xe hom. Khi xa trongduong: Ba + — Bay? + 2H" Mg + > Mgy + 2H Tai diém trong duong: Mgind + HY? > MgY? + Hilnd (do nho) (xanh) ‘Tnréng hop thém MgY”, ty phire cla BaY? kém bén hon MgY?, nhung tai sit diém twomg dong ¢6 su thay déi phic, hinh think Mgind e6 mau da, Band + MgY? > BaY? + Mglnd pk 2 8.69 176 7 Nhin vao biéu thie trén ta thay tng pK cia vé phi lon hon vé tri nhidu cho nén phuong trinh phan ting din ra kha thufin loi. Tai diém trong duong phire Mglnd cing, phin ting voi EDTA Lim thay déi miu cua dung dich. Mgind +H:Y? —> MgY? + Hind (do nho) (xanh) hin Lay vio binh nén 10 mil dung dich Ba**, thém chinh xée Sml dung dich Mg”* 6 ning d6 yas (néu cho complexonat magie thi khong cin do thé tich chinh xée), thém 10m! dung, dich dém amoniae + amoni clonia, pH=10 vi mot it chit chi thi ET-OO, dung dich e6 miu do nho. Chuin a6 bing dung dich EDTA di biét nong 46 cho ti khi dung dich chuyén sang miu xanh. Ghi sé ml EDTA da chuin 46 - Voml. Lam song song dé ty két ‘qua trung binh, Néng 46 mol/l cia Ba** duge tinh nhur sau: Coo Vers ~ Cus Vane 5.4 XAC BINH Ni*, CHAT CHI THI CuY-PAN Neuyén tic: ‘Vi phite cia Cu* voi PAN bén hon rit nhiéu so véi phire cla chit chi thi nay voi cde kim loai khic nén c6 thé sit dung hg CuY- PAN. Lim chat chi thi diém trong duong trong phép chuin 46 tryc tiép phin lin céic kim loai khdc, 7hank: Hit 10 ml dung dich Cu?* vao binh nén 250 mi va tién hanh chudn 49 Cu? bing EDTA v6i chit chi thi PAN nhu é phan 6.3.4 dén diém tuong duong. Sau dé thém tiép vio dung dich niy 10 ml dung dich miu Ni?*, dun si dung dich va tiép tue chudn 6 bing dung, dich EDTA cho ti khi dung dich chuyén tir mau xanb tim sang miu ving ue. Ghi thé tich EDTA tiéu tn cho qui trinh chudin a6 Ni* (V, ml). Nong d6 Ni** durge tinh nhur sau: C, Cm =O 10 BAI6 CAC KY THUAT CHUAN DQ COMPLEXON (tiép) 6.1. XAC BINH HAM LUQNG PO,’ 61.1 Nguyén tic Trong méi truimg kiém yéu, két tia PO,* & dang MgNH,PO, .6H,0 ; Mg"* +(NHy:HPO, + 6H,0+NH, = MgNH,P0,.6H,0 + 2NH? Phan ting bi ngiin cin boi sw e6 mat cia Fe", Bi"*, AI, Ti'*, phai che bing EDTA née khi két ta. DE trinh sy tao thanh Mg(OH);, phan img cing cn duge thye hién khi mit mudi amor i, ty nhién khong ding luumg dur mudi amoni qui Kim. Cin cho them KCN vi ascorbic truée khi chudin dd, idu kign tién hanh phan ing: © Tid hinh két tia & pH >7 ~ Phai loai bé Li va cde cation khic cé thé tao két tia véi ion photphat (thém. EDTA dé to phite, truomg hop Ca e6 thé thém axit xitrie) (Chi thém mot Iuong due NH,’ vita phi 28Bun néng dén 70- 100°C Co dia thuy tinh vio thinh dng nghigm dé tao digu kign két tha, trinh hign trong, {qui bio hoa. Két tia MgNH,PO, bi thuy phin mot phan khi rim bing nude: MgNH.PO, + H;0 —> MgHPO, + NH,OH é trinh thuy phn, ngudi ta rim két tha biing dung dich amoniac loang. Loe, rira két ta, hod tan bling HCI 1M sau d6 tién hanh chudn 4 Mg** & pH=10 vir chi thj ET-OO. Tir lung Mg” da phin img, tinh duge long PO,” trong miu. 6.1.2 Quy trinh phan tich Lay miu chira PO,* trong céc thuy tinh 250 ml chiu nhiét sao cho Iugng PO,” khong qué 250 mg. Thém 10 ml dung dich MgSO, 0.5M, thém 5 ml HCI 6M, 2 giot dung dich chit chi thi métyl d0. Pha loding bing nurée cat ti thé tich 100 ml sau dé thém cham timg gigt dung dich amoniac dic, via thém vita khudy va co dia thuy tinh vao thinh cbc cho dén khi chit chi thi chuyén tir mau d6 sang miu vang. Thém 5 ml dung dich EDTA (0,02 M, thém tiép 5 ml NH, dic nia, day nip va dé yén 1 dén vai git. Trude khi loc, cin thir xem dai két tha hodn to’in chua. Loc két tia qua gidy loc béing xanh va rim bing dung dich amoniae 2,5%. Khi cin xée dinh magié that chinh xe duéi dang amoni-magi photphat, cin két tia lai két tha d6 Lin thir hai, vi dung dich phan tich luén luén chira long lin mubi amon, két tia e6 edng thie khéng that sir li MgNH,PO,.6H0. Kiém tra d6 sach cia két tia biing mét giot dung dich AgNO; + HNO, vao Iml dung dich nude rita khong cb két tha tring cla AgCL. ‘Chuyén ca gidy loc chia két tia vdo céc 250 ml, thém 10 ml dung dich HCl 1M, thém 30 ml nue, dun sdi dung dich. Loc dung dich qua giddy loc bing dd, rim gidy loc bing nude cat vao binh nén 100 ml. Thém dur chinh xc Vl dung dich EDTA (khong 10-20 ml) digu chinh pH cia dung dich bing dung dich NaOH dén déi mau gidy céng g6 dd. Thém 10 ml dung dich dém pH=10, thém 5 mI KCN 5 % va m@t lung nhd axit ascorbic, mot it chit chi thi ET- (00. Chuiin d9 ngoe EDTA bing dung dich Mg ti Khi dung dich chuyén mu tir xanh sang do.Lugng PO; duge tinh theo céng thite: mgPO,” = (Cem Vane ~ Cue Visg 95 6.2. XAC DINH NONG BO Hg** VA Zn** TRONG HON HOP. 62.1. Neuyén the a) Xae dinh tng s6 Hg™ va Zn™* Cho chit tao phite EDTA dur dé tie dung véi Hg?* va Zn’* sau dé chun 49 lung EDTA dur biing Cu** voi chit chi thi PAN & pH=S (ding dé Phuong trinh phan tmg cla Hg’ vaZn* voi EDTA nbursau: uurotrropin) Hg” +H.Y* —» HgY*+2H" ; Zn" +HzY” —» ZnY"+2H" ; rong EDTA dur dire chudn 6: HY? (du) + Cu? > Cuy? + 2H" by Xde dinh rigng Hg Cho lupng dir KI vio chin hin hop complexonat H Hg" thinh Hgl gid’ phong m hrong EDTA twong img etia Hg” vi chun dO Iuong EDTA nay bing dung dich chun Cu” & pH=S véi chit chi thi PAN. (Cée phan img nbur sau: * va Zn” & trén dé tao phite voi HgY" +41 +2 HY Hel? + HY? (du) + Cu’? > Cuy? + 2H" 62.2 Quy trinh phan tich Ding pipet liy chinh xe Vil (10ml) dung dich hn hyp Hg?* va Zn** cin xée dinh vio binh nén e@ 250ml, Thém chinh xée mot lung EDTA (Vim), da biét ning 46 (Co). Thém tiép 1 gam urotropin va mot it chit chi thi PAN, lic déu, dung dich c6 mau vang. Dun sdi dung dich va ding dung dich chun Cu** chun d6 cho ti khi dung dich chuyén sang miu tim, ml Cu?* da chusin d@ - Vom ‘Thém tiép vao dung dich vita chuin 46 & trén 5 mi dung dich KI 5%, khi dé dung dich c6 miu ving. Bun s6i lai ding dich va chudn d9 luong EDTA duge gidi phong ra bing dung dich chun Cu** hét V; (ml). Lam ba Kin ri Lay két qua trung binh, Nong 46 Hg?" va Zn’ duge tinh theo céng thie sau: 306.3 XAC BINH BQ CUNG TOAN PHAN CUA NUGC MAY Cé nhidu cich dinh gid vé d> cimg toin phin cia nude miy: Theo tigu chuén “GOST” cia Nga thi 9 cimg toan phin cla nude durge dinh nghia li s6 mili dong long: gametia Ca?* va Mg** trong mot lit nue. Theo Nguyén tie: Chuin dé ting sé Ca”* va Mg™ biing dung dich chuin EDTA & pH = 10, chuan chit chi thi E7-00 rdi tinh d6 cimg cia mrde. én hinh: Tréing binh dinh mire 100ml bing nude méy, binh nén 250ml biing nude ccdt, sau d6 ly made may vao binh dinh mic dén vach mite, 46 vao binh nén. Thém 10 ml dung dich dém pH=10, thém 5 ml KCD 5% (dé loai anh hung ciia ede kim logi ning chi thi ET-00. Tir burét, nhd timg giot dung dich EDTA vio binh nén cho ti khi dung dich chuyén tir mau d@ nho sang miu néu 6) va mot rong nho bing hat du xanh chai xanh, Sinh vien ty lip cdng thire tinh d9 cimg toan phan cita nude./. BAL 7 (Bai kiém tra) XAC DINH HON HOP Al, Ca, Mg Mue dich bai niy kiém tra tng hyp ede kj ning déi visi phurong php emplexon bao gim: chuiin d) ngurge, chun d6 lign iép, ky thusit che, ky thud Lich, 7.1 NGUYEN TAC Bude 1 - ich hn hop: Téich Al khoi hén hop bing ech dun néng dung dich véi NHy 6 mit NH,’ dé chuyén AI vé dang AIH). Loc, hoa tan két tiia bing HCI hofic H,SQ,, durge dung dich Al”, phin nude loc li dung dich Ca®* va Mg™. 31Bude 2 - Chuan d xée dinh ede chit: ~ Xéedinh Ak Chuan 4} nguge lugng EDTA dur & pH=S bing Zn”, chi thi PAN - Xie dinh tng Ca, Mg: Chuan d6 tye tiép hn hop bling EDTA 6 pH = 10, chi thi ET-00. ~ Xde dinh Ca: Che Mg** bing NaOH pH=13, chudn 46 Ca voi chi thi Murexit. 7.2 QUY TRINH PHAN TICH Lay ede chia miu phan tich cua phing thi nghiém, thém nude cat dén khodng 50 ml. Dun néng dén 70-80°C, thém Sml dung dich NH,CI 1 M, thém 10 ml NH; 6M, tiép tye dun néng 30 phit. Bé ngudi, loc két tia qua gify loe bang ving vio binh nén 250 ml (nue loc 1), Hoa tan két tia tri lai vao cdc ban dau bing 20 ml HCl 6M néng. Két ta lai ‘Al nhur di thye hign & trén (Sml NH,Cl + NH,, dun néng). Loc, nira két tia $ lan, mdi Lin 5 ml dung dich NH; 1% vao binh dinh mie 250m! di c6 nude loc 1. Thém murée ct dén vach, duge dung dich A chia Ca, Mg. Lay két tua, hod tan két tia ngay trén gidy loc bing dung dich H,SO, vio binh dinh mite vio binh 100 ml, duge dung dich B. Xie dinh ting Ca, Mg- Lay 10 ml dung dich A, thém 10 ml dung dich dém NH;+ NH,CI, thém me long nho chit chi thi ET-OO, chuin bing dung dich EDTA cho ti khi dung dich chuyén tir mau do sang xanh, hét V, ml. Xée dink Ca Lay 10 ml dung dich A khdc, thém 2 ml NaOH 2M, lic kY, thém mot it chi thi Murexit, dung dich c6 dé. Chuiin bing dung dich EDTA cho dén khi chuyén tir mau do sang tim, hét V2 mi Xie dinh Al: Lay 10 ml dung dich B vao binh nén 250 ml, thém mt miu gidy chi thi cong g6 do, diing dung dich NH; 6M diéu chinh cho ti khi gidy cong g6 chuyén sang miu hong, 32thém 30 ml dung dich EDTA 0,02 M, thém 5 ml dung dich dém CH;COOH + CH,COONa (pH=4). Dun s6i dung dich 10 phi, them mt it urotropin, lie ky, tiép tue dun nong dén 70°C, thém mt it chi thi PAN, chun 46 bing dung dich EDTA cho dén khi dung dich chuyén tir miu vang sang mau hdng, hét V, ml. (Sinh vién gr lip e6ng thire tinh kong Al, Ca, Mg trong miu) 7.3 CAU HOLON TAP 1. Néu nhing khai niém co bin vé phire chat (dinh nghia, phiin logi, danh phip) 2. Neu ning die diém corbin cua phite complexonat kim logi? 3. Hiing sé bén va hing sé bén diéu kign cla phite chit. Tinh hiing sé bén didu kién cia phite EDTA-Fe(IIl) cde pH : 15253; 455;5657;859; 10; 11 biét ring phite EDTA-Fe(II1) 06 hing sé 10°; Ka BFeY = 10°", HY c6 cdc hing s6 phan ly li Ky = 1 4107; Ke = 1,1. 10" Za sir FeCl) khong e6 phan ting phy khiée ngoai phan img voi EDTA. 4. Chait chi thi kim logi trong chun d} complexon ? dn hurdmg cia pH dén chi thi kim loai nhu thé no? 241108: Ky = 5. Néu ede ky thudt chudn d9 comlexon va pham vi img dung? Cho thi du minh hoa. 6. Tinh pSr va vé durimg cong chun d6 khi thém 0,0 ; 10,0 ; 24,0; 249 ; 25.0 26,0 ; 30,0 ml chat chun EDTA c6 ning d6 0,02 M vao 25 ml dung dich S* néng: 49 0,02 Mo pH=11 CHUONG 3 PHUONG PHAP CHUAN DQ KET TUA, TAO PHUC BAI & CHUANDOKET TUA TAO PHUCXACDINH CACHALOGENUA VA SCN 8.1. PHUONG PHAP MOHR XAC BINH CT, BrNeuyén tie: Phin img két tia gitra ion Ag* voi Cl hay Br xay ra nhanh, hon toan cé thé ding trong phan tich (TAgCI = 1.8.10", TAgBr = 6.10, Tagl = 1.1.10"). Khi qué dim tong durong, Iugng dur nho cha Ag* tgo két tia mau do vii CrO, sé la chat chi thi cho sue chuin do: Ag’ +Cl > AgCH tring ‘Chat chi thi: dung dich K,CrO, 5% 2 Ag + CrO,? > Ag.CrOw do Phan img thyc hién trong méi tnrémg trung tinh (6,5= pH < 10), & pH thip, CrO” bi gm do tao thinh HCrO, edn & pH ea Ag,O to think edn tn phin img. Phrong php ‘khdng xe dinh I va SCN’ vi: Agl c6 miu do khé nhjn biét diém trong duong, mit khiic, Agl va AgSCN hip phy kha 13 gay sai sé. hank: Ding pipet lay chinh xdc Vnl (10m) dung dich halogenua can xc dinh vao binh non e& 250ml. Thém 10 giot dung dich chat chi thi, lic déu va tién hinh chudn dO biing dung dich AgNO, da biét ndng 4 cho dén khi dung dich chuyén tir mau vang nhat sang mau do niu. Ghi sé ml AgNO; chuin 4 -V.ml. Lam ba lin rdi ly két qua trang binh. wo, Vo v D4i voi anion Br cing tién hinh tuong ty nhurtrén. 8.2. PHUONG PHAP FAJANS XAC INH Cl, Br, I’, SCN Neuyén tie: Phan img két tia giita ion CI’, Br, I, SCN’ v6i Ag’ tgo thiinh hop ebdt kho tan abu a trinh bay & trén. Chat chi thi cho diém trong duong la chat hip phy, fluorescein hay cosin 1% trong rugu etylic. Tnrde diém trong duung, hat két tha mang dign tich am do hip phy anion halogenua cho nén khdng thé hip phy chat chi thi. Khi qua diém tuong dirong, két tia sé hip phy ion Ag* dir tao thanh nhing hat mang dign tich durong va lién két veri anion chat chi thi tao nén nhirng khdi két tia mang mau (doi mau dung dich) ([(AgC)g. Ag} NOs, + Ind’ ([(AgCD,]Ag} “Indy Mmau tring miu hong (vi fluorexein) va tim (eosin) D6i voi chat chi thi Fluorescein (viét tit 1a HFI), phin img tién hinh trong mdi truimg trung tinh vi HIFL Ia mot axit yéu, pK =10°. Trong moi trrdng trung tinh HPI phan ly thanh FY 1a ion dm, lién két voi hat keo mang dign tich ducmg (khi da dur mét luong nh Ag’) bién thanh mau hdng. Dé ting cudng kha ning hip phy, dura thém hé tinh bét, miu dung dich sé bién di 13 hon, tat 1 HE, c6 thé phan ly & Li mdi trudng thugin loi cho phin img. Khi ding chat chi thi nay, khong xe dinh Oi véi chat chi thi cosin, 1a mt axit manh hon, vi CT viE hip phy manh, day Cl ra khdi két tia AgCl lam sai Iéch diém trong dong. Tién hink Ding pipet ly chinh xc Vl (10m!) dung dich Cl cdn xéc dinh yao binh non ci 250ml, thém 3-5 giot dung dich chat chi thi fluorescein, Im! hé tinh bot, lic déu va tién hinh chuiin d6 bing dung dich AgNO, di biét ning 46. Khi khdi mau hing thi ngimg chudn 4. Ghi sé ml dung dich AgNO, chuan 46 - Vaml, Lim lip lai lung dich chuyén sang 3 Lin rbi by két qua trang binh. Déi voi Br , TF va SCN’ ciing tén hinh tuong ty. Khi ding eosin, (khong xdc dinh Cl ) tién hin tuomg tur nur trén nhumg thém 5 ml H,SO, 4N dé tao moi trudng axit, 8.3. PHUONG PHAP VOLHARD XAC DINH Br, I, SCN’ VA CI Neuyén tic: Cho mot lugng dur chinh xée Ag* tic dung véi ede halogenua va SCN’ 0X)" sau d6 chun 4} Ag*dur biing SCN’ di biét néng 46, sir dung phén sit (Fe™*) lim chat chi thi. Khi vita dur SCN’ thi dung dich s@ c6 miu hdng. Iva Br 6 thé chudin 46 khi 6 mat AgX nhung d6i véi Cl thi phai loc bo két tha true khi chudin 46 vi Tasc>Tagscn. Ag’ +X’ AgXx (dur Ag’) Ag’ + SCN’ > AgSCN 35SCN’ +Fe'* — FeSCN** (miu hong) Phan img tién hanh trong méi trréng axit tranh Fe** bi thuy phin. hin Dinng pipet liy chinh xe Vl (10ml) dung dich halogenua edn xée dinh vao binh niin c& 250ml. Thém 3ml HNO; 6N, thém chinh xe mt thé tich dung dich AgNOs - Viml - ¢6 10 giot dung dich phén sit(IIl) 0.2 M, tic déu va tién hinh chuan 49 bing dung dich SCN’ da biét ndng 46 cho wi Kkhi dung dich chuyén sang mau hdng. Ghi sé ml dung dich SCN’ chudn d6 - Vzml. Lam 3 Lin rdi lay két qua trung binh. GM = CoonV X =I, Br .SCN’ bode Cr Neuyén tie: ‘Trong méi trrimg axit, phin img gitta Cl voi Hg” tao hop chit HgCl, it phin ly (K=6.10"). Tai diém trong duong, mt hygng dur nho Hg™ tic dung véi chat chi thi 5) than phire diphenyleacbazon (6 pH=1,5- 2,0) hoe diphenyleacbazit (6 pH ~ hin Ding pipet lay mot thé tich ehinh xe Vil (10ml) dung dich CI edn xe dink vio binh n6n cé 250ml, pha loing gip déi biing nue ct, Thém 2 ml HNO, 0,5M, 5 giot dung dich diphenyleacbazon 0.1% trong cén etylic. Tién hanh chudn 46 biing dung dich Hg(NOs)> cho dén khi dung dich chuyén sang mau tim thi ngimg chun 9, hét V, ml. Lam 3 Lin réi ly két qua trung binh. 0s, c= ‘er Vv 8.5 CAUHOION TAP 1. Néu didu kign hinh thanh két tia va quy ludt tich sé tan? Cae yéu 16 anh hurémg 161 46 tan, cho thi dy minh hog, 3. Néu die diém va pham vi ap dung cua ede phurong phip Mohr, Fajans, Volhard, 364. Co ché di miu cua chit chi thi trong phuong phip chudin 4 Ct bing He* CHUONG 4 CAC PHUONG PHAP OXI HOA - KHU’ BAI 9: PHUONG PHAP CHUAN DO PEMANGANAT 9.1. XAC BINH NONG BQ DUNG DICH KMNO; Neuyén tie: H,C,0, 1a mot chat gdc e6 tinh khir ding dé xe dinh ndng 46 KMnO,. Phin tng ign ra trong mi trudmg axit véi chit chi thi ld mau hdng eta lugng dir KMnO, trong dung dich chun do. SH,C,0, + 2KMnO, + 3H,S0, ~> 2MnSO, + 10CO; + 280, + 8H,0 hin Ding pipet lay chinh xe Vom! (10ml) dung dich chun HsC:0, vio binh nén ed 250ml; thém Sml H,SO, 2M lic déu, dun nong dén khoang 70°C (khéng dirge dun s6i). , nho timg gigt dung dich KMnO, chi dén khi dung dich c6 mau héng bén trong: Khodng 30 giay. sé ml KMnO, di chuin 46 - Vl. Lam ba lin rdi lay két qua trang binh, Nong 46 mol/l cita KMnO, 1a: Tir bur S 9.2. XAC DINH HAM LUQNG H.0: CONG NGHIEP iguyen t Phuong phip dinh lung dua trén phiin img SH:0; +2MnO, +6H' > SO; + 2Mn”* + 8H:0 Trén thi trudng, H,O, bin ra c6 néng do khong 30%, dé xac dinh néng d6 ciia no phai pha lodng t6i ning d6 khoding 0,01M. hnh: Lay V, ml dung dich H,O, ban trén thi trrémg pha loding dén thé tich V2 (Sinh vién tur tinh dé €6 gid tri V, va V2 phii hop cho phép chun 46). Lity 10 ml dung aa pha lodng vio binh nén dung tich 250 ml, thém 5 ml dung dich H2SO, 2M, chun bing 37dung dich KMnO, cé ning d6 C, tsi khi xudt hién mau hong, hét V, ml. Nong 4} mol 1,02 duge tinh: 9,3. XAC DINH NONG DQ NOs iguyén tic: Phan img oxi hos Khir gitta MnO, vi NOs din ra trong moi rung axit: 5.NOy +2MnO, +6 HY > 5 NO; +2 Mni* +3H,0 Tuy nhign, trong mdi trumg axit ion NOs’ bi phan huy thinh NO vi NO; theo phuong trish: NO; +H*-+HNO, NO +NO; + H:0 do d6 cin dio nguye thir tyr phin img (nhd tir tir dung dich NO; vao dung dich MnO, trong moi trémg axit. hin Hut 25 ml dung dich chuin MnO, vio binh nn 250 ml, thém 10 ml dung dich H,SO, 2M, pha loding véi khong 20 ml nude edt, dun nhe dung dich vi nh tir tir NOs tir buret xudng dén kh imdt mau hdng. Ghi thé tich NO, tiéu tén. Néng dd NOy trong dung dich chun d9 duge tinh theo edng thite: 5.25.C, M04 Cvo. 9.4. XAC DINH NONG DO Fe™ VA Fe" TRONG HON HOP Neuyén te: Xde dinh Fe(1l) bing cach chuan 46 trye tiép bing dung dich chudn KMnO, cho ti khi mbt gigt dung dich du KMnO, lim xudt hin miu héng. MnO, +5Fe* + 8H" —> Mn®* + SFe'* +4H,0 - Xie dinh téng him lugng Fe(II), Fe(Ill): khir toan bo Fe vé Fe™* bing SnCl, (lugng du SnCl, duge logi bing HgCl,), logi trir anh huémg cua CI bing hn hgp bio vé va chudin 46 long Fe** trong dung dich giéng nhu trén, 2 Fe + SnCh -> 2 Fe** + Sn“ + 2Cr SnCl, + 2HgCl, + Hg,Cl, + Sn + 4Cl 38‘anh Xe dinh ham lugng Fe** Ding pipet liy chinh xée Vm (10m!) dung dich miu vio binh nén e& 250ml, them 5 ml H;SO, 2M, thém 10 ml hén hop bao vé. Tir buret nko tr tir dung dich KMnO, c6 nong d6 C, cho tikhi xuat hién miu hong, hét Vm. Xe dinb tng him lugng Fe** va Fe™* Ding pipet léy 10 ml dung dich milu khie vdo binh nén c& 250ml. Thém Sml HCL 4M, dun nhe dén khoding 70°C, cho timg giot dung dich dung dich SnCl; 5% vio va lic nh cho t6i khi dung dich mat miu vang cla FeCl; thi thém 1 giot dung dich nia va Lic déu. Pha lodng dung dich bing nude cat dén khoang 100ml. Thém nhanh Im! dung dich HgCl, 5%, lic déu (néu dung dich c6 miu den thi phai lim lai). Thém 10m! hén hop bio vé va tién hanh chun d6 biing dung dich KMnO, c6 néng 46 C,. Khi dung dich c6 miu hang bén trong khoang 15 gidy thi ngimg chun 6. Ghi sé ml KMnO, chudn 46 1a V; mi. Lam 3 lin ly két qua tung binh. Nong 46 mol Fe(1) va Fe(II) durge xe dink nhur sau: 56, _5C,AV,-¥)) aay ym) > 9.5. XAC DINH LUQNG Ca TRONG MAU Neuyén tie: Két tia Ca” bling C,0,” sau 46 hoa tan két tia trongdung dich H,SO, ri chudn do H,C,O, sinh ra biing dung dich chuin KMnO,, Ca¥ + C07 > CaCO, CaCO, + H2S0, > CaSO, + HsC.05 2KMnO, + 5 HsC,0, + 3H:S0,—> 2 MnSO, + KzS0, +10 CO +8H;0 hin: Lay Vml miu phin tich chia Ca’ edn xe dinh véo céc thuy tinh chiu nhigt co 250ml, Thém S ml HCI 4M, 10ml dung dich (NH,):C:0, 4%, khully déu, Dun nhe dng, dich dén khoang 70°C, thém 2-3 giot dung dich mety! da cam va cho tir tir timg giot dung. dich dung dich NH, SM vao dung dich, khudy déu dén khi dung dich chuyén mau ving. thi dimg lai. Dun néng dung dich tré lai va dé yén 60 phat. Loc lay két tha trén gidy loc 39bing xanh, rim két tia 4-5 kin bing dung dich (NH,),C,0, 0,1%, sau d6 nira 2-3 Lan bing nurée ct. Hod tan két tia ngay trén phéu bing 20m! dung dich gidy loc biing nude néng vio binh nén cH 250ml. Toan b dung dich bao gdm nude loc va nurée rita, dun néng dén 70°C va chudn 49 H,C,0, bing dung dich KMnO, da biét nding 4, Khi dung dich e6 mau hong tong khoding 30 gify thi ngimg chun d6. Ghi sé mi dung, dich KMnO, chuan 46 - Vom, Lim 3 lin va lay két qua trung binh. Lugng Ca trong dung. dich phan tich tinh theo mg nhur sau \, 2M néng, ting ky M8 cu BAI 10 PHUONG PHAP CHUAN BQ DICROMAT 10.1. CAN PHA DUNG DICH K,Cr,0;0,002M_——_ (Mx.cxo, = 294,18) (Can chinh xe khosing 0,2942g K,Cr,O, loai tinh khiét hod phan tich, pha trong binh inh mire 500ml, ta ¢6 dung dich 0,002M 13.3. Xde dinh ndng a9 Fe** bing K.Cry Neuyén tic: Dua trén phan img oxi hod - khir gitta Cr:0;? va Fe: (CO; +6 Fe + 4H > 2Cr"* +6 Fe" + THO; (Chat chi thi: DiphenylaminE” = 0,76V 6 H,PO, hole phenylantranilie E" = +1,08V hinh: Ding pipet ly chinh xic Vil (10ml) dung dich edn xc dinh Fe™* yao binh non ed 250ml, Thém 2ml HsPOs 4M, 10ml HC14M va 3-4 giot dung dich chat chi thi, lie déu rdi tién hanh chudin dO bing dung dich K,Cr,0, da biét ndng dd. Khi dung dich cd 34 ml K>Cr.0, chuiin 46 - Voml. Lam ba lin roi Lay mu xanh tim thi dimg ebusin d9. G két qua trung binh, Néng d6 moll cita Fe** duge tinh nhur sau: 6Lx,cn0, “ Vv 10.2, XACDINH NONG DQ Na,S.05 C 40Yguyén tie: Ding mot lung xe dinh K.Cr,0, dé oxibod lrgng dir KI thanh Iva chudn d6 1; sinh ra bing dung dich Na,S,O, véi chat chi thj hé tinh bot, Tirndng 46 va thé tich ca KCr,0; ¢6 thé xée dinh duge néng dé cita dung dich thiosunfat. (Ch07 +61 + 14H > 2.Cr4 3b +70 1, +2520; +26 + S« hinh: Ding pipet lay chinh xéc Vinl (10ml) dung dich K3Cr,0; 06 nng do da biét vio binh non ed 250ml, Thém Sml H.SO, 3M, 10ml dung dich KI 5%, lie nhe cho déu, diy miéng binh bing kinh ding hé va dé yén trong bong t6i 10 phat. Sau dé chudn 46 long |, giai phong ra bing dung dich Na,S,O, cho ti khi dung dich cé mau ving rom, thém Iml hé tinh bt 1%, le déu va chuiin 46 tigp t6i khi mét niu xanh thi dimg lai. Gl s6 ml dung dich NazS2O; chudn 46 - Vomnl. Lam 3 tan va lay két qua trung binh. Nong d moll etta Nas$:05 duge tinh nb sau: Cres.0, = 10.3 XACDINH Pb BANG PHUONG PHAP DICROMAT 10.31 Nguyén tic xée dink - Tach Pb"* dudi dang PbSO, it tan bing H,SO.: Pb* + S02 > Ppsod - Hoa tan PbSO, biing dung dich dém CH,COONH, + CH;COOH 1M: PbSO, + 4NH,CH,COO > Pb(CH,COO),(NH,)3 + (NH);SO, ~ Két tia PbCrO, bing K,Cr,0;: 2Pb(CHsCOO)(NH,)2 + K.Cr0; + H,0 > 2PbCrO, + 2KCH,COO + 4NH.CH,COO +2CH,COOH ~ Hod tan PbCrO, daria sach ion CrO,” dur bing hin hp clorua sau dé cho tic dung: voi Kidu: (hdn hop clorua durge ni, du ché nhu sau: 320 gam NaCl + 100 ml HC! dae pha thinh 2PbCrO, + 4HCI — 2POCL, + HCO, + H.0 H,Cr0;+ 6 KI + 12HCI > 2CrCl, + OKC! +7H20 + 3 ~ Chuéin lirong 1, thodt ra bing Na,$,O, c6 néng 46 C, wi chi thi hé tinh bot: 41, + 2NaS.0, —> 2Nal + NaS.O, + 2Nal 10.32 Quy trinh phar tich Lay miu chia mot rong Pb** xic dinh (khong 10 mg), thém 50 ml nude cat. Thém 2 ml H,S0, die, dun néng dung dich t6i khong 80°C va dé yén 30 phi. Loc bing gifiy Joc bing xanh va rita két tia biing 4 lain biing H2SO, 1%. Hoa tan két tua biing 20 ml hin hop CH;COONH, + CH;COOH ning, nira gidy loc va thu toan bd dung dich vio céc 250 mil, thém 10 ml dung dich K.Cr.0; 5%, dun néng ri gin si, dé yén 30 phuit. Loc két tia trén gidy loc bing xanh, nia két tia bing nude loc nong cho t6i khi mrde na khong edn miu ving. Hod tan két tia trén gidy loc biing 20-25 ml hén hop NaCl +HCI. Rita, tring gify loe bing murde néng, dé ngudi, thém 10 ml dung dich KI 5%, lic nhe va dé yén 10 phut trong ché ti. Ding dung dich Na;S,0; ¢6 ning d6 C; chun 46 cho t6i khi e6 mau ving rom, thém Iml dung dich hé tinh bot va chudn tiép cho t6i khi dung dich mat miu xanh tim, hét V, eT mgPbO=C.V, 10.4. XAC DINH HAM LUQNG CROM TRONG MAU NUGC THAL 10.4.1 Nguyén tic xéie dink Crom cé trong nurée thai cla qué trinh thude da, ma dign, sim xudt cic mudi crém... No ¢6 thé t6n tai 6 dang C(I) cing nhur & dang Cx V1). Xe dinh ham lugng crém ting sé trudc hét edn oxihod to’n bd Cr(lil) Lén Cr(VI) bing persunphat trong méi trubng axit, c6 judi hét chat oxihod dur, Cr(VI) duge chun 49 bing dung dich Fe(Il). Bé chit chi thi cho sir oxihod hoain ton erdm, ngubi ta thém vio dung dich mot lugng nho Mai); va dé kim 10 sy chuyén miu tgi diém tuong dong ngudi ta cho thém vio dung dich mt luemg H,PO, trude khi chun dd (xem myc 19.4) 2Cr* + 38:07 +7H0 > Cr07 + 6502 + 14H CnO? + 6 Re + HY > 2cr* + ORY + THO 10.42 Quy tinh phan tich Ag* ding lam xte tc, Sau klLy chinh xe mt thé tich nude chia erém sao cho Iugng erém Khong ahd hon Img (thong thuimg khoding 10ml) cho vao binh nén dung tich 250ml, thém 5 ml dung dich H,SO, 3 M, 5 ml HsPO. 2 M, 5 git dung dich AgNO, 1%, 1-2 giot dung dich dung dich MnSO, 1%. Pha lo’ing dung dich bing nude ct t6i khong 100 ml, Dun nhe trén bép ign, cho timg lugng nho mudi persunphat vao, lic dio dung dich thu’mg xuyén, khi dung. dich ¢6 miu do héng (mau eiia Cr50;7 + MnO, ) thi dimg cho pesunphat. Tip tue dun s6i ky cho persunphat phéin huy hét (khong cdn bot nho Ii ti thodt ra tir dung dich). ‘Thém timg giot ding dich dung dich HCI 6M vio dung dich cho ti khi dung dich mit miu hing va chuyén sang mau ving da cam thi ngimg lai. Dun tiép 5 phat nita dé dudi hét Cls khoi dung dich. B& ngudi, thim Sml HsPO, 2 M, 3-4 giot dung dich chit chi thi (diphenylamin hose phenylantranilic axit), ding dung dich Fe(II) di biét trude néng 46 cchuiin 49 ti Khi dung djch chuyén tir mau tim sang mau xanb nat thi ngimg chudn d6. Ghi sé ml Fe(II) da chuan 49. Lam 3 lan va ly két qua trung binh. ‘Tinh, him lugng Cr trong Lit dung dich mu (mgt): Cy Vp.-1000 51,996 V, 3 mgCr/1 (Chi ¥ = NOs’ ngiin can phép xée dinh, trong truimg hop miu e6 NOs’, edn loai ching bing eich e6 can dung dich trong méi trudmg H»S0s ).BAI 11 PHUONG PHAP CHUAN DQ IOT-THIOSUNFAT 11.1 DAC DIEM CUA PHUONG PHAP IOT-THIOSUNFAT Phuong php dua trén phan img oxyhod - khir chuyén hos I thin T vai nguge bai L +2 Hé 1,/ 21 6 thé oxy hod khir vira phi, I” c6 thé la chat khir d6i véi nhiéu chit oxy ‘hod nhumg 1, cing 6 thé ki chit oxy hod déi voi mét sé chit, Thé Ox-Kh tiéu chudn ca cp Ly2P wong déi nho, bing 0,54 V cho nén c6 thé xem T ta mot chat khirrdt tt dé xe dinh nhiéu chit oxy hoa. MO6t dic diém cain lu ¥ 14 phan img xe dinh cdc chat oxy hod nay khong xe dinh dduoe diém tuong dirong do I, sinh ra ngay tir déu d kim xuit hign miu xank ei ehait chi thi hd tinh bot. DE khde phye hign tung nay, nguei ta sir dung phuong phip xdc dink iin tigp thong qua mot chit khir, thuémg ding natrithiosunfat Na,S;Os, vi vay phuong, phip nay edn goi li Phuemg php iot-thiosunfat. Nhu vay, khi cdn xic dinh chit oxy hod, nguivi ta cho no tic dung véi lugng di KI trong méi trudng axit hinh thinh mt lugng 1; wrong duong voi chit oxy hod vé duong turong. Tiép theo chun d@ lugng 12 thodt ra béing natri thiosunfat v6i chit chi thi hé tinh bat. ow nOx +mKI > m2L + oKh+ mK* 2NaS:0; + Iz > NaSiOq + 2Nal ‘Tir cdc hé s6 ca phan img, tinh lung chit oxy hod ban dau. So dé trén diing dé xtc dinh cdc chat oxy hod nh : KzCr;0;, KMnO,, KCIOs, Clz, Br, NO; Fe™*, Cu”, iu kign ctia phan img: ~ Phin img durge tién hinh trong moi tnrimg axit yéu dén kiém yéu, khong diroe tién hiinh phan img trong moi truémg kiém manh vi tgo thin 10 I, + 2NaOH — Nal + Nal +10 10 1a chit oxy hod manh, cé thé oxy hod duge thiosunfat dén sunfat nén im sai léch duong long cia phan tng. Mit khde cing khong tién hinh trong méi tnrdng axit manh néng 4 cao do H’ la m6t ion rit linh dong, lim ting qué trinh hoa tan oxy, sai lech phin img. ‘Chuin a9 ngudi vi iot ti chit d8 bay hoi, mit Khée hd tinh bot s@ kém phan img Véi it khi dun ndng, diéu d5 din dén gidm 49 nhay. 44Sir dung luomg KI du. = Phai dé yén dung dich trong ch t6i khong 10 phat cho phin tmg hoiin oan. Mic diu thé oxy hod Khir cia hé 12/21 nho nhung n6 vain cao hon mot sé cdip kha cho nén I; tré thinh chat oxy hod. Mt sé chat khir thutng gap la: SO,”, S*, Sn”* va dic bigt 1a AsO; Thé oxy hod khir tiéu chudin cua cip AsO;"/ AsO;° 1a 0,57 v cho nén néu nhin vao diy ta thy phan img chay theo chiéu nguoe lai. Nhung thie ra chinh 1 oxy hod durge asenit nhér thye hign phan img trong mdi trudmg kiém yéu, pHF8. Chiing ta sé xét ky ‘ede phan img may & phn sau. 11.2. CHUAN BI DUNG DICH CHUAN Na.8.0, Cac pha dung dich Na,S,0, Dung dich duge chudn bi biing céch hoa tan mOt rong mudi NazS.0;.5H,0 trong nurde ct sao cho e6 néng 46 0,01M. Can mét lugng céin mudi natrithiosunfat chinh xde trén cn phiin tich dé pha dung dich chudin 1a v6 nghia do mudi nay cé thanh phin khong hodin toin ding véi edng thire. T6t hon ed 1A edn tén can ky thudt, dé pha mot dung dich ning dé nio d6, sau dé dé yén va bao quin n6 trong lo ndu, edch li voi moi truémg khong khi mgt vai ngiy, loc dung dich, chudin d6 lai theo cde chat chun bén vig trude khi dem sir dung. Dung dich natrithiosunfat khong bén, sau khi pha xong, dung dich c6 néng 46 hoi cao hon nhung din din ching giam di do cde nguyén nhin oxy hod cia oxy khong hi va do vi Khudin, BE bio quin dung dich duge t6t, ngudi ta cho thém vio khong 0,1 g Ait Na;COs va khong 10 mg Hele /l dé logi trir vi khudn. * Xac dinh ndng 46 chinh xdc cita natrithiosunfat theo K,CrO; nhu mye 13.4 11.2, CHUAN BI DUNG DICH 10T Dung dich iot durgc chuan bi béing céich ho’ tan iot trong KI dé tgo phire K1s, luong KI phai gp 3 lin 1, Dung dich durge chudn bi nhur sau: C’in khoang 3-4 g KI bing can ky thudt, cho vao lo thuy tinh e6 nit nhdm, thém khoang 2 ml nusie. Khuily ky va dé cho nd tro vé nhigt 46 phong roi cén trén cin phin tich, c6 G,. Thém khoang 1,269 g 1, va day niit lai, le k¥, can trén cn phin tich kin thir 2, ta 6 G2, Vay Gi-G2 la hong 1, a Lay. Chuyén ton b9 dung dich vio binh dinh mite 0,5 lit va thém nude eft ti vach mite, Iie 45kj, ta 66 dung dich chudin ls ndngd6 khoding 0,01M. C6 thé xée dinh lai ndng 46 eiia dung dich iot theo dung dich natrithiosunfat vira chun bi é trén, 113. XAC DINH NONG DO DUNG DICH Cu* Neuyén tic: Cu** phan img voi I gil phong |, mét cdch dinh lugng, chuin 4} hrong Ly ‘giai phong ra bling dung dich chudn NazS2O, véi chit chi thi hé tinh bot. 2Cu" +41 > 2Cul +1, 1; +2Nay$:0;—> NayS.Og+2 Nal ‘Cul hip phu Ip nén ngudi ta thutmg thm CNS vio dé tao thinh CuCNS ngin chin hign tuyng hap phy nay, déng thdi lam ting thé oxihod - khir cia cp Cue*/Cu* do CUCNS c6 tich s6 tan nhd hon, Cul + CNS > CuCNS + I ‘Tién hinh: Ding pipet lay chinh x4c Vil (10ml) dung dich Cu?* cdin xde dinh vao binh non co 250ml. Thém Sml H,SO, 3Mva 10ml hén hgp KI + KCNS (déu 1a 5%), lic nhe déu rdi day migng binh lai bing nip kinh déng hé va dé yén trong béng tdi 10 phit. Sau 40 chuan d6 1, bing dung dich Na,S,O, 43 biét ning d6 cho t6i khi dung dich cé miu ving rom thi thém Iml dung dich hé tinh bot 1% (dung dich chuyén sang mau xan tim), ‘Chun 46 tiép cho dén khi dung dich mit miu xanh thi dimg Iai. Ghi sé ml Na;S,0; chudn 46 - Vom. Lam ba lin ri Lay két qua trung binh. Nong 49 mol cua Cu duge tinh hur sau: C, ca = 11.4. XAC DINH NONG DO DUNG DICH NATRI SUNFIT Nguyén tie : Oxy hod natri sunfit bing mt lurong duriot I; + NaxSO; + HO + NaSO, + 2HI ‘Chuan 46 lurong iot dur bling Na,S,0, vi chat chi thi hé tinh bot, tir dé xde dinh him rong NasSO,, 46I, +2 Na,S:03 > Na.S,04 +2 Nal (Chi: Truée diém tromg duromg khi edn dir SO, phan img xy ra khong theo ty 1¢ hop. thie doeé phin imgphy 2807-421 HO, +15 Ngoai ra do néng d6 H’ ting nén c6 kha ning bay hoi SO, va oxi hod H,SO, bing. ‘oxi khdng khi, do dé céin thém 1, dur dé loai sai sé nay va phai thém thudc thir theo thir tu: 6 dung dich SO,? vio dung dich Is du hinh: Can chiah xe gam Na;SOs.7H:0 (khong 0,63 gam) pha trong binh dink mie 250 ml, ta duge dung dich A (ndng 49 khosing 0.01 M). Ding buret thém chinh xe Viml (khoiing 35 ml) dung dich 1 c6 néng 49 C, vao binh nén 250ml, hit dich A hém tiép vao binh non. Dé yén &ché tdi vai phut sau dé dem chun 46 bing dung dich chudn natri thiosunfat ndng 46 C; (0,01 M), hét Vom. Him Iugng Na;SO duge tinh theo eéng thi: 5 ml dung QV,.C, -V.C,).252 250 100 %Na,S0,.7 1,0 aS ° ° 2.1000 25 a 11.5. XAC BINH NONG DO DUNG DICH Na,AsOs, (Cha y : Cac hop chat cia asen rit dc, phi edn thin khi sinh ki asin-AsH, phai tién hinh trong th hit hoi dc) Neuyén tic : Oxy hod asenit bing 1, trong mdi trudng kiém yéu. NasAsOs + 1, + HO > NasAsO, + 2 HI Mie dit thé oxy hod khir tiéu chuan cia cp AsO,"/AsO5° (0,57v) lin hon edip 1/20 (0,54v) nhung 1, vin oxy hod duge asenit Li do khi lay sin phim tao thinh ra khoi ving. hanh thi nghiém. Phin img phan img, Trong digu kign c6 du NaHCO, , pH cita dung dich bing 8, axit go thinh durge lay di cho nén thé biéu kién cla cp AsO,*/AsO;* gidm di: 0,059 Ey = 0,57 + log 10*)* =0,11V ‘Thé nay thap hon so voi thé cia cp 1,21, edn bing chay vé bén phai. Mot diém cin chi ¥ khiic nita 18 bao gis ta eting chudn bi dung dich asenit bing eich hod tan oxyt asen trong mdi tnrdng kiém dur AsOs + 6NaQH + 2NasAsO; + 3H,0 ‘cho nn phai trung hod kiém dur tnréc khi chudin do. 47‘hanh: Lay can than V ml (10 ml) dung di dung dich phenolphtalein, dung dich cb mau hing. Thém ting giot dung dich HS, 2M cho dén khi mat miu hing. Cho tiép vao binh chuiin 4 khosing 1 gam NaHCO,, lie déu (néu dung dich lai c6 mau hdng thi thém tiép H;SO, 2M cho ti khi mit mau. Thém 1-2 mi hd tinh b6t, chudin 46 miu via chun bi bing dung dich iot e6 néng dO Cy (kho’ng 0,01 M) cho toi khi xudt hign miu xanh nhgt, hét V, ml. Lam ba Lin rbi ly két qua tung: tink, asenit vo binh nén 250 ml. Thém 2 gigt Néng d mol cia dung dich asenit duge tinh nhur sau av, Vv 11.6. XAC DINH HAM LUONG CLO HOAT DONG TRONG NUGCJAVEN Neuyén tie: Trong mdi trudng axit, clo hoat dong trong nuve javen cd thé tie dung mot cach dinh luong v6i iédua gidi phong ra i6t nguyén t6 (trong méi trudng kiém phan img. xy ra khOng hoain todin). Chuan d@ Iuong idt gidi phéng ra bling dung dich natri thiosunfat di biét ndng d6 sé tinh duge him lung clo hoat dng trong dung dich. Khi hod tan clo trong muse, xay ra phan img: Ch + #0 > HCO +HCI iy La phin ting thudn nghich, cho nén HCIO hinh than c6 thé tai phdn huy thanh Ch. Nh vay trong dung dich tin tai ed hai logi, dung dich thutmg 6 miu ving nbat Chimg nao dung dich hét mau vang nhat chimg t tng cia hai loai én di hét. Dé tién dinh gid him lugng clo hoat ding trong nude, ta quy vé Cl, (xem ring toin bo CIO” da chuyén thinh Cl). Him lugng clo duge tinh bing sé gam clo nguyén t6 trong mot lit nude. Ch + 2KI > 2KCl + & 1, +2NazS:0;—> Na,S,0, +2 Nal hin: Lay dung dich nude javen cho vao binh dinh mire dung tich 100ml; thém nue ccdit dén vach mire va lie déu, dure dung dich A. Ly Lin lugt 3 ml dung dich H»SO, 6N, 10ml dung dich KI 10% sau d6 cho chinh xe V, ml (10ml ) dung dich A vita pha vao binh non 250ml, lic nhe cho déu, dé yén trong 48.bong t6i 5 phiit ri dem chudn 49 bing dung dich natrithiosulphat (Na:S,Qs) 0,01M toi hi dung dich e6 mau ving rom, Thém 1 ml dung dich hé tinh bot 1%, dung dich chuyén sang miu xanh tim. Tiép tye chun dO t6i khi dung dich mit mau xanh. Ghi sé ml dung dich natrithiosunfat chudin 46; Lim 3 lan iy két qua trung bin, Xie dinh miu tring: Cng tién hinh tong tw nbur trén, thém Lin lugt ede hos chit clin thiét nhung khéng cho: murde javen, thay vao 46 ta cho 10 ml nude edt ding dé pha long muréc javen, roi chuin d@ nhu trén, hét V; ml Na;S,O; 0,01 M Tinh s6 gam clo hogt dng trong 1 lit miu (g/l): mg [t= BEG. 1000 “ 1000” 100 355 BAI12 PHUONG PHAP CHUAN DO BROMAT, IODAT 12.1 NGUYEN TAC CUA PHUONG PHAP Phuong phéip dua trén co siy phan tmg oxi hod cia BrOs BrOy +6H"+6e— Br+3H,0. Eoociny = tASVSES, ,,, = +L087V Chit chi thi sir dung trong phuong phip la ede phim nhudm hiru co nhur metyl do, metyl da cam, Sau diém nrong duomg BrOy dir s@ oxi hod Br= BrOs +5 Br +6H" > 3Br+3H.0. Br, sinh ra c6 tac dung oxi hod chit chi thj fim cho nd mat mau dé phat hign chink ade diém twong dong. tuy abi ‘cdi cha ¥ ~ Nhiing chit chi thi nay khong phai chat chi thi oxi hod khir vi su oxi hoa khir nay fi bat thudin nghich, do d6 cn trinh dé thude thir dur timg ving. ~ Mit khde, chat chi thi mit miu trude diém tong durong (dic biét khi KBrO, duge thém yao nhanh) do do cin thém vai giot dung dich chat chi thi truée diém tuomg duong vi cn chuin 46 lip lai sau khi di e6 thé tich KBrO, gin ditm tuong durong. 49- Téc 49 phin img oxi hod khir khong 1én do d6 cdin phai chun dd trong dung dich ning vi e6 d axit cao. 12.2, XAC DINH NONG BO DUNG DICH Sb"* BANG PHEP DO BROMAT Nguyén tie: Trong méi trrimg axit, thé oxi hod khir tiéu chudn cla cp BrO;/Br (0,61 V), cao hom nhiéu so véi cdp SbOs/ SbO> ( -0.43 V), cho nén phan img oxi hod khir din ma thudn loi. Tuy nhién, antimon rit dé thuy phan tao két tia Sb(OH)s. vay edn phai dura thém mudi cia axit tartric, KHC.H,O, dé chuyén mudi Sb thinh ion phire K(SbO)C.H.O, rdi chun bing BOs cé ning 49 xic dinh trong moi truimg axit, voi chit chi thi 1a metyl da cam hogie metyl dd. BrO, +3Sb"+6H'— Br +38b"+3H.0 hay 3K(SHO)CJH.O, + KBrO, +1SHCI > 3SbCI, + KBr + 3KHC,H.O, + 6 Khi toan b9 Sb°* bi oxihod lén Sb thi mot giot dung dich dir BrOs sé tic dung véi Br to Br, lam mit mau chat chi thi, BiOy + Br’ + 6H” 93Br2 + 3430 hank: Lay Vl (10m) dung dich Sb can xic dinh vao binh non e@ 250 ml, thém 25ml HCI 6N + Sml KHC,H,O, 5%, thém 3 giot dung dich metyl da cam. Dun néng dén 70°C, tir buret nhé timg giot dung dich KBrO, c6 ndng 46 C, wi khi mit miu cht chi thi (khong Hy két qua nay). Lay 10 ml dung dich miu khic, cing kim tuong ty nhur trén nhung chua cho chat chi thi metyl da cam ngay. Tir buret nho timg gigt dung dich KBrO xudng t6i khi gin hét sé ml KBrO; Lin du thi thém 3 giot dung dich metyl da cam va tiép tuc nhd KBrO, xudng, lic déu cho ti khi mat miu cua dung dich. Ghi sé ml KBrO; di ‘ding (lam hai lan va ly két qua trung binh) hét V, ml. 3G, “10” 123. XACDINH HAM LUQNGAL” TRONGMAU BANG PHEP BOBROMAT Neuyén tie: Phin tmg két tia Al’ bing &-hydroxyquinolin durge thye hign trong moi tudmg dém acetat, pH = 5 . Luong thude thir 8-hydroxyquinolin chi nén dr khoang 4% vi néu cao, qua, n6 s& cng két visi nh6m-oxyquynolinat gay sai s6. Cac ion kim logi Cu?*, Zn?” Fe™*, Ca*, Ti*, Mo", Ca**, Co™, Mg", Ag’, Bi, Sn®*, Mn?" v.v cain tré phiin tmg, khi ¢6 mit 50cdc ion trén phai tién hinh che. Mt s6 anion cing can tr: PO,*, F, AsO,*v.v. Dung dich sau khi két tia e6 miu vang nhat. BHCSH.NO + AB > AI(CsH,NO)s + 3H" hay: 3 +a a3 +3Ht OH o AUS Hoa tan két tua nhém oxyquynolinat di rira sach bing HCl, sau d6 cho oxyquynolin phan img vii mot Iugng du KBrO, trong Br. Tiép theo, chuin Iugng dir KBrO; bing phuong phip iot - thiosunfat. Qué trinh nay e6 thé biéu dim nbur sau: 2B10; + 10Br + 2H" — 6Br,+6H,0 3 + Br, = 3 + 6H + 6Br Br OH OH BiOy +61 + 6H" > Br + 3h +3H,0 3h + 6 NaxS.0; —> 3 NayS.O,+ 6 Nal hanh Ding pipet liy 20m! dung dich Al** can xe dinh vao cdc c& 250ml pha loing bing nude cat wi gin SOml, dun néng im 10ml 8-hydroxyquinolin 5% trong CH,COOH IM va thm NH,CH\COO 2M 16i thong dye thi cho thém 10ml NH,CH,COO 2M nita va dun néng 10 phat. Loc nong trén gidy loc bing do. Rira két tia bing nude néng cho t6i khi nude rira khéng cén miu ving. Hoa tan két tha di rita sach bing 25-30ml HCl 2 M hosc H,SO, 1M. Rita tring gidy loc 3 kin, mdi Lin 3-Sml HCI2M. hoc H)SO, IM. Thém vio Iml KBr 5% + 2-3 giot dung dich metyl da cam. Cho tir tir dung dich KBrO; c6 néng 49 xic dinh ti khi dung dich mét mau chat chi thi + Sml KBr0, nila, toin bd KBrO; 0,001M 1a V, ml (khoang 25-30ml). Thém 5 ml KI 5% lic nhe va dé yén 5 phit. Tir buret nho din timg giot dung dich dung dich NasS.0, e6 néng 40 C. t6i khi dung dich cé miu ying nhat thi thém Imi hé tinh bt rdi tigp tue nho- iNa,S,0, xudng, lic déu cho dén khi dung dich mat mau xanh tim. Ghi s6 ml Na,S,O, di ding, hét V2 mt mgAl = (CV, aT 2 12.4. XAC INH NONG BO H" BANG PHEP BO IODAT Nouyén tie: Dua trén co siy eta phin ting 10; +514 6H" > 3h+3H,0 a ‘Chudin lugng Iz thoat ra bing NaS.0; di biét ndng 49 voi chat chi thi 1, +6NaS.0,-> 3Na,S,0,+6Nal tinh bot ‘Chi J: phan ting (1) sé ngimg khi trong dung dich thue té khdng edn axit Tién hinh: Ding pipet lay 10ml dung dich H* edn xde dinh yao binh nén ec 250ml, thém 15 ml dung dich KIO; e6 ndng 4} C, (0,001M) va Smi KI 5%, Dé yén 5-10 phiit Tir buret nho timg giot dung dich dung dich Na,S.0;c6 ndng dd C2 t6i khi dung dich e6 mau ving rom thi thém Iml hd tinh b6t va tiép me mhd NazS,0; xudng, bic déu t6i khi dung dich mit mau xanh tim. Ghi s6 mililit Na;S,O, da ding hét V2 ml. Lim 2 lain va ly két qua trung binh, Tinh néng 46 cita H*, iongam/. trong miu: CHUONG 5 PHUONG PHAP PHAN TiCH TRONG LUQNG Trong chug nay, trinh bay cic KY thudit phn tich trong luemng bao gor két tha, loc dé loi cle tap chit thu duroe dang két tia sach mude Khi- sy vi nung, dura chit phiin tich vé dang cin. KF thuft ar dung ld nung vi chén nung doe tinh bay phn pu lye 4 tang 93-96BAL 13 PHAN TICH TRONG LUQNG XAC BINH Mg” 13.1. KY THUAT LOC 13.1.1 Gidy loc khong tin Trong phin tich trong luong, nguiri ta loc két tha bing gidy loc khong tin. Gidy loc khdng tin 1a loai gidy khi dét chiy, khdi lugng con Iai tir 0,00003-0,00008g tro tuy theo timg logi. Thue té trong long ny khong Jinh huimg ti két qua phiin tich (40 chinh xe ‘cu cin 18 0,0001g) Newi ta digu ché gidy loc khong tin bing céch ché bién gidy loc bing HCI va HF. Sau khi sin xudt chiing dirge dong g6i thinh timg tip 100 ta. Trén mai hop gidy nguéi ta ghi kich thude gidy loc va trong long tro cia mot to. Cie logi gify Ipc sir dung c6 d min khée nhau, ching duge ky higu bing ede mau Kha nhau trén tip gidy: Bang mau xanh 1a logi gidy loc min, 4 xép nho nhit, thug sir dung dé loc cde két tia tinh thé nho nhur BaSO,, PbSO,v.v. Gidy loc bing miu tring, bing miu ving li loai gidy loc c6 d6 xép trung binh, ding dé loc cdc két tia hydroxit kim loai. Gidy loc bing do li loai gidy loc c6 46 xép lem nhit, ding dé loc cde két tia tinh thé lin. Nhuge diém cia ily loc 1 khong c6 kich thude 16 1% ring. Ngay nay nhiéu phong thi nghiém da sir dung ming loe polyme e6 keh thurée 16 chinh xe hon. Kich the gidy loc e6 cae 739511; 125 ; Bem. Néu khéi lugng tro >0,00001g thi khi tinh toan phai tinh dén ca khéi hrong tro. 13.1.2 Cich gap gidy Lge via k§ thut loc iy loc khdng tan qua nhiéu céng doan nén gid thinh wrong déi cao, chi nén sit dung gidy khong tan trong nhimg trudng hop can thiét. Sir dung gidy loc ding loai va kich thude cing Li mét yéu cu durge dit ra. Tuy thude vao Logi két tia, khdi hromg két ta, ma chon loai gidiy loc thich hop. KY thuat gip gidy loc cing phy thuge vio digu kign phan tich cdn lay két tia hay éu gip nhiéu nép dé cho toan bd gidy @ nhanh hon. Con néu ly két tha, nurée loc. N éu iy née loc, ta gap gidy loc theo loc tiép xtc iri dung dich nude cdi, khi d6 tbe 46 loc thi gap gidy loc theo kiéu phiing dé d@ thu hdi két tha. ip gidy loc theo kiéu nhiéu nép tién hanh nhur sau: Gap te gidy loc dé c6 hinh 1/4 to gidy sau dé mo tré lai va tir mt bén nia hinh tron ta gdp timg phin nho hinh tam gide cbchiéu rong khoaing lem, tiép we gip di gip lai cho dén khi hét nita t gidly loc, mi ra ta 06 tir gidy loc gap nhiéu nép. Gap gidy loc kiéu phiing don gian hon, ta gap doi te gidy loc, tiép tue gip doi mot lan nita, mi mot phiin nho cita t6 gidy sao cho c6 hinh nén dé nguge. Tuy theo hinh dang cia phéu ta gip dé cho ty gidy tiép xite voi phéu sao cho & phia tren tigp xe nhiéu hon 6 phia cudng phéu. C) Q \ ®& Y Y Hinh 4: Gap giy loc va ky thuat loc Dé loc tt, chon té gidy loc c6 kich thurée phi hop, mép tar gidy loc dich mép phu khoding 0,Sem. Sau khi dit gidy loc vao phéu, ding binh nude cat thim wot déu te gidy sau 6 dé day nude cit vio phéu cho chay. Néu gidy loc dit ding, cudng phéu sé duge lip diy nude tién hah loc ngay khi cuéng phéu van con day nude. Chinh c6t murée nay lam gidm dp sudt thuy tinh & phdn cuéng phéu va vi vay ting nhanh qué trinh loc. 13.2, XAC DINH Mg THEO PHUGNG PHAP TRONG LUGNG 13.2.1 Nguyén tic xée dinh Bude 1: Tién hinh két tia ion magie duéi dang MgNH.PO,.6H20: Mg* + (NH);HPO, + NH, + 6H,O — MgNH,PO,6H,0 | + 2NH, 34Bude 2: Nung két tia MgNH,PO,.6H.0 6 100°C tao thinh magie pirophotphat, tirdd tinh ra lugng Mg trong: miu: 2 MgNH.PO,6H;0 — Mg:P,0, + 2NH, + 7H,0% Dé trinh hinh thinh Mg(OH),, phan img két tia (NH,),HPO, cn duge thye hign khi mit mudi amoni. Tuy nhién khong ding long dir mudi amoni qué lén vi din ti tao thanh két tia e6 thanh phin Mg(NH,).(PO,)2, ma két tua nay sau khi nung mét phan tg0 thank P.O; Mg(NH,)(POs): > Mg(POs) + NHs + 2H,07 2Mg(PO,). > Mg;P,0; + P:0; Két tia MgNH,PO, bi thuy phan mot phin khi ri bing nube: MgNH.PO, + H;0 > MgHPO, + NH,OH é trinh thuy phan, can nita két tha biing dung dich amoniac lodng. idu kign tién hanh phan ing: = Tidn hinh két ta 6: pH >7 Phi logi bo Li va ede cation cin kha e6 thé tq0 két ta véi ion photphat (truimg hop (Ca e6 thé thém axit xitrie) (Chi thém mt lung due NH," vita pha = Bun néng dén 70-100°C ‘Co dita thuy tinh vio thinh éng nghiém dé tao diéu kign két tha, 13.2.2 Quy trinh phan tich Lay mot lung miu mudi Magie chita khoang 10 mg Mg trong nude, thém 5 ml HCI 6M, 2 giot dung dich chit chi thi métyl d0 va 6 ml dung dich (NH.)sHPO, 0,1M, pha lodng bing nue edt wi thé tich 100 ml, Sau dé thém chim timg gigt dung dich amoniac dic, vira thém vira khudy va co diia thuy tinh vao théinh cde cho dén khi chit chi thi chuyén tir miu do sang mau ving. Thém tiép 5 ml nita, day néip va dé vao ti Lam vi cho dén budi thi nghiém tiép theo. Trrde khi loc, cdn thir xem di két tia hodn ton chua. Loc két tia qua gidy loc bing xanh va ria biing dung dich amoniac 2,5%. Khi cin xic dinh magié that chinh xc duéi dang amoni-magié photphat, cin két tia lai két tia dé Lin thir hai, vi dung dich phin tich lun luén chira long lon mudi amoni, két tia cd cong thie khong that sy li MgNH,PO,.6H0. Kiém tra d6 sach cita két tia bing mot giot dung dich AgNO; + HNO, vio Iml dung dich nude ria khong cé két tha tring cla AgCl. 55‘Chuyén to’n bé gi loc va két tha vao chén nung da biét khéi lung (chén nung dt durge nung 60 phit & 900°C sau d6 dé ngudi trong mdi tru’mg khd va céin). Say kho két ta va gidy loc, mung 60 phiit 4 900°C. (Can lai chén nung lan thir hai, va tinh him lung Mg e6 trong miu. BAI14 — PHUONG PHAP PHAN TiCH TRONGLUQNG XAC DINH Fe 14.1. NGUYEN TAC Két tiia Fe duroi dang Fe(OH), bling NH; sau dé loc, nira va nung dé c6 dang can cudi cling Fe,0y Fe’ 4 3NH.OH > Fe(OH), + 3NH* Fe(OH), > FeO; + H,0 (nung) Digu kign két tia: Két tia Fe(OH); thudng kéo theo cdc tap chat dic biét trong trrimg hop ding thude thir NaOH dé két tia. Vi vay cdn dp dung cdc bién phap sau: ~ Sir dung NH, dé loai trirdurge nhiéu tap chat do tao phire amiacat; ~ Két tia tir dung dich khéng qué die c6 chia HNO, vi sau dé hinh think NH.NO, g6p phn day cdc tap chat khdi cdc trung tim hap phy va phi céic keo Fe(OH)s ; ~ Kéttia trong dung dich néng; ~ Loc néng vai rira két tia biing dung dich néng c6 thém NH.NO, 2% - Két tia ffp ndu trong dung dich 06 nhiu ede tap cht 14.2. XAC DINH HAM LUQNG Fe TRONG PHEN SAT Cin chinh xie khodng 1g NH,Fe(SO,):.12H,0 vao eéc 250 ml, thm 5 ml HNO; 4M vi 100 ml nude et Hoa tan va dun néng dén nhigt d6 60°C -70°C . Them NH,OH dic cho dén két ta hoan toan, thém dur 2 ml (tat cd hét 20 ml). Tiép we dun dén gin dung dich , dé yén dung dich 5 phut rdi loc néng qua gidy loc khong tin bing dd, Dun nong dung dich ria NH,NO, 2% rim khoang 8-10 lan, mdi Lin 5 ml dung dich nira cho én khi hét SO,? (thir bing dung dich BaCl, 5%). Sdy gidy loc va két tha & 100°C-200°C dén khd, chuyén. vao chén nung da chuin bi va biét trong long, G). Nung két tla & 900°C 40 phut, dé ngudi dén nhigt 46 khoang200°C réi chuyén vio binh hiit Am, dé ngudi tiép dén nhiét d6 phong, edn, e6 trong long G ‘Tinh ham lugng FeO, trong phen. BALIIS XACDINH SO,” BANG PHUONG PHAP TRONG LUQNG VA COMPLEXON 15.1 XAC DINH S07 BANG PHUONG PHAP TRONG LUQNG. 15.1.1 Nguyén tic xdée dinh Ding mot lung du chinh xé¢ Ba”* dé két tia ton bd SO,”. Loe, rira két tha qua gidly loc khdng tin bang xanh. Nung két tha & 850°C dén trong luong khong doi, tir Iugng céin cchén nung vi chén nung ¢6 két tia, xe dinh duge lung SO, trong miu. Nude loe dug ding dé xc dinh Ba** dur trong phn sau. Phuong php gip mét sé trér ngai do céc tap chit nhu Al, Fe va Sr, cing nhu mot sé tap chit khong tan anh huréng. Vi vay dé phiin tich cde miu thye té, mOt quy trinh loai tap chit duge dé ra. Trong diéu kign SO? da c6 sin, quy trinh phan tich nhur sau: 415.12 Quy trinh phara tich 1. Nung chén dén 850°C va git 1 gid dé ngudi tr tir cho t6i nbigt d Khosing 200°C, dura chén vao binh hit 4m (desicator) va tiép tue dé ngudi dén nhigt 46 phong. 2. Cin chén mung va ghi trong lugng eita chén, Gy g 3. Lay miu $O,? (chtta khoang 50-100mg) vao ce 250 ml, thém 5 ml HCIAN. Vira dun nong, vira thém mot long dung dich BaCl, 0,025M cho t6i khi két tia hoin toan, cho tigp thém 10 ml BaCl, nia (mét lrong chinh xic tit cd Khoang 40 ml). Tiép te dun néng dén 90°C sau d6 dé yén dung dich khong 1 gids. Loc gan két tia ba lan qua gidy loc khong tin bing xanh vio binh dinh mie 100 mi, sau dé chuyén ton bp két tia Len gidy loc va tip tuc nim ky kéttia 5 kin, mdi lin bing 5 ml murée néng. Todn bd mrée loc duge dinh mite thinh 100 ml cho phin sau (dung dich B). 4. Chuyén gily loc c6 két tia vao chén nung, sdy kho. ‘Chuyén chén nung cé gidy loc va két tha vao ld nung, dit nhiét 49 850°C, bat cng tic dp dign cho lo nung, Khi nhiét 46 dat t6i 850°C, gitt 1 gier. 376. Dé ngudi lb nung t6i < 200°C, chuyén chén nung vio desicator, tiép tue dé ngudi ti 0 phing. 7. Cain chén nung cé két tia, durge trong lugng G2, g, Trong lurgng cla BaSO, 1a G»-G,. 8. Tinh trong long SO: mSO, = (G:-G,). 9623333 g 15.2. XACDINH SO.? BANG PHUONG PHAP COMPLEXON 15.2.1 Nguyén tic xdée dinh Sir dung m@t lugng ehinh xée Ba?*, dir dé két tin SO? sau d6 chin a6 rong Ba” ‘dr 6 pH = 10 kh e6 mit cia MgY” véi chi thi fi ET-00 Phuong phap complexon c6 thé xc dinh Bari c6 trong két tia BaSO,,: rita sach bari dur, hoa tan trong méi tru’mg NH; 9M voi long dir EDTA roi chudin 49 EDTA dur bing: dung dich Zn?* ; 6 day ta lam theo edch thir nhit, lay dung dich B 6 phin trén. Phan img két tha BaSOx Ba” + SO,” = BaSO, (dur Ba"*) ; Phin két tia BaSO, 43 duge nung & phan trén, phan nurdc loc e6 Ba™* dur, cho thém Mg™ sau dé chuiin d@ bing EDTA ? 42H IY? + 2H" ‘Tai diém trong dug: Mgind (miu do nho) + H;Y* —» MgY” + Hyzlnd (mau xanh) Hing s6 bén ciia BaY? va MgY® tung 44i gin nhau, tuy nhién, ching cao hon hing sé bén cla Mgind. Mat khdc, hing sé bén cia Mgind cao hon Balnd rit nhiéu (10" so voi 10°) nén tai diém twong duong, phire Mgind (do nho) edn lai sau cing tarde khi chuyén sang Hind”(xanh). 45.2.2 Quy trinh phar tich Lay miu chita khoang 50-70 mg SQ, vao ede 250ml. Thém 4ml HCIAN, lie déu roi ccho tir tir dung dich BaCl, e6 ning 46 C, (0,025M) vio cho ti Khi két ta hoan todn, thém khoing 10m! BaCl, nia. Ghi sé ml BaCl chinh xic di cho vio eée - Vjml (chinh xic khoang 40 ml), Dun néng két tha dén khang 90°C (khéng dé s6i Lim bin mat dung dich), Dé yén 60 phat, loc gan qua gidy loc bing xanh; rim két tia 5 Kin, méi lan bing: khoiing 3m! nurée néng vio binh dinh mie 100 mi, urge dung dich B, Ly 20 ml dung dich B vao binh nén 250 ml, Trung hot dung dich B bing dung dich NaOH 2N t6i trung tinh (thir bing gidy quy). Thém chinh xc V. ml (Sm) dung dich Mg” c6 ndng 4} C; (néu cho complexonat magie thi khéng cin do thé tich chinh xc), thém Sml dung dich dém amoniac + amoni clorua vi mét it chi thi ET-OO khi d6 dang 58dich SB c6 miu d nho. Chuan 49 bing dung dich EDTA e6 néng 49 C, cho t6i Khi dung, dich chuyén sang miu xanh thi dimg li ml EDTA di chuin d6 - Voml. Lam song song dé iy két qua trung binh. $6 mg SO,” trong miu phin tich theo céng thite: ZI 100 15.3 CAU HOLON TAP 1, Neu diém kie biét cin bin gitt phuong phip phin tfch trong lung va phiin tich thé tich, cho thi du minh hoa? 2. Néu ce loai lo nung, chén nung trong phan tich trong lugng? Nhimg diéu cin tri ki Lim vige vi 1d nung, ehén nung? 3. Yéu edu eta dang két ta, dang cn? lim thé ndo dé dap img ede yéu cdu 46? 4. Cac ky thudt co ban khi tich cde chit biing phuong phap két tia? Cho thi du minh hoa. PHAN 2 PHAN TICH MAU THUC TE Mue dich cia phin nay 1a gidp cho hoc sinh lam quen voi cde miu thye té bing cdc phin tich mt sé miu c6 trong thi trutng, duge chia lim bin logi chinh, dé 1a cde md hyp kim, ede miu sin phim edng nghigp hod chat (xi ming pooe - King va phan bon NPK va quing piroluzit), cic miu méi tnrimg va cudi cing 1d céc miu thye phim. Hiu hét cae bai thy té, hoc sinh phai pha miu, loai tap chit tre khi phan tich va cudi cing, sinh vién ty lap cde cong thite tinh lurgng chit cé trong miu. CHUONG 6 PHAN TICH HOP KIM BAL16: XAC DINH HAM LUQNG Mn TRONG GANG 16.1, NGUYEN TAC XAC BINH Mn @ trong gang thug ton tai dutri dang MnS, Mn,C, MnO;, him lirgng cita n6 tir 0.2.3 %. Khi hoa tan mau gang chira Mn bing hén hop H2SO; + HPO, e6 mit HNOs phan ting xy ra nbur sau: MnS + H:SO, > MnSO, + HST 3MnS +14 HNO, > 3Mn(NO3)+ 8NO + 3 H:SO, +410Mn;C +8HNO; > —3Mn(NOs),+C + 2NO +410 Néu eb MnO,: 3MnO,+4HPO, > Mn\(PO,), +6 H;0 Khi c6 Fe** nd bi HNO; oxi hod thanh Fe™ va tao phite khong miu véri HsPO,. Mat khiic, HPO, cén e6 tie dung lam ting d@ bén cia HMnO,, trinh bi phan huy thinh MnO(OH)> va 0p). ~ Loe bd ba than chi, oxi hod Mn** thinh MnO, bing (NH). SO., c6 mit HsPO,, chit xtc tela ion Ag’. 2 MnSO,+ 5 (NH,)2 $:05+8 HO —> 2HMnO, + 5(NH,): SO; + 7H2SOs Shudn 4 MnO, sinh ra biing dung dich chudn Na;AsQ; (hosc Fe™) dén khi dung. {Os trong moi truimg dich mat mau tim. 2HMnO.+ 5 AsO;" +4H" > 2Mn™ +5 AsO," +310 Chi ¥: Khi him luong Co va Cr> 2% sé can tri phép xdc dinh vi Co* c6 mau hang va Ce* bi oxi hod thinh Cy0;? kim cho miu hing chuyén thinh miu ving é diém tong, duomg. 16.2 QUY TRINH PHAN TiCH - Can chinh xc trén cn phan tich a gam (khoang 0,25 gam) miu gang vao cde chiu ahigt 3 250 ml, Thém 10ml hén hyp H»SO., HsPO, va HNO, (pha 6 phin 21.4), dun nhe. Khi ki NO; khOng cdn thost ra (thutmg khoiing sau 10-15 phit dun néng), pha Jodng dung dich v6i 20 ml muse néng, loc bo ba than chi qua gidy loc bing ving vio binh dinh mie 100 ml. Rita gidy loc 3 Lin bing nude cit néng, dinh mie dén yach duge dung. dich A. - Ding pipet ly 25,0 ml dung dich A cho vao cdc chiu nhigt c6 250 ml, thém nuée edt dén khoing 70 ml, thém | ml dung dich AgNO, 1%. Dun néng dung dich, thém ting long nho tinh thé (NH,)28,0, cho dén khi xuat hién miu hong én dinh (khong cho dr nhiéu (NH,))S,O, vi anh hutmg ti phan img chudin 46). Lic déu, dun s6i thém 30 - 40 gidy dé loai chat oxi hoa du. Lay céc ra khoi bép, dé yén dung dich 3- 4 phut cho phan img xy ra hod toan réi kim ngudi ngay dudi voi nude chay. ~ Chuin 46 ngudi dung dich HMnO, thu duge bing dung dich chuin Na,AsO; (hoge Fe**) co ndng 49 C, (M) dén mat miu hofe chuyén sang mau ving (néu miu © Cp), hét V, ml, Can chudin 46 nhanh vi (NH,)28.0; ¢6 mt trong dung dich sé tig hod Mn** sau chun d@ thinh MnO, (mie dit énhit €9 thuimg phan ting xy ra chim), 16.3. TINH TOAN KET QUA tue oxi 60Sinh vién ty thiét lp cng thife tinh Iugng Mn (mg) trong miu trong gang cho tnrée. 164. HOA CHAT - Miu phin tich: miu gang dang phoi bio (di céin true khdi krong), mdi sinh vién mot miu. ~ Hén hop axit dé hod tan miu: Thém edn thin 125 ml H,SO. dc (d= 1,84 g/ml) vio 500 ml nude edt, im ngudi. Sau 6, thém tir tir vao hn hop trén 100 ml HsPO, dle (421,75 g/mmal) vA275 ml HINOs die, lie déu, ~ Dung dich chudin NaAsO,: cn 5,1-52 gam Na,CO, hod tan trong 100 ml nude cit. Thém vio dung dich 1,7 gam As;Os, dun néng. Dinh mie thinh 5 lit, Sinh vién ty cchuiin d9 lai ndng d6 ca dung dich nay theo phong php idt- thiosuntat. ~ Dung dich chuiin K3Cr0; 6 nding d6 chinh xéc, ede dung dich I>, NayS;Oy chu c6 ndng dé (sinh vién ty chuan dé Iai ndng 49 dé diing Lim dung dich chuiin), chit chi thi hi tinh bot -Cée dung dich edin thiét khde, sinh vién ty pha tir ede hex chdt sau: HNOs de, HCL di, tinh thé (NH,)2S.0s, NaHCOs, BAI17 XAC DINHALCu,Zn TRONG HOP KIM DEVADA 17.1. NGUYEN TAC XAC DINH Hoa tan hop kim trong hén hop HCI H.0, thanh dang dung dieb. - Xe dinh téng sé milimol Al, Zn, Cu trong miu biing phuong php chudn 46 complexon ‘@pH=S voi chit chi thi xylenol da cam: APY +HRY? > AIY 42H" Zot" + HY? > Za? 42H" Cu + HY? > CuY? 42H - Thém NaF va dun sOi ky, khi d6 nhém to phe véi florua gidi phong ra AD 4 6F 42H" HAY? + AIR, Ding Zn®* chudin 49 lugng HsY° duge gi phong, xée din duge Al" e6 trong miu, ~ Xéedinh him Iuong Cur theo phuemg phip i0t- thiosunfat. ‘Tirlugng Al’ va Cu” va téng sé mmol ba nguyén t6, xi¢ dinh duge Zn trong miu. 17.2. QUY TRINH PHAN TICH Can chinh xéc khoang 0,2 gam miu Devada da nghién no trén edn phan tich, chuyén vio ede chiu nbigt 250ml, dura vaio th hut, thém khodng 10m! HCI 6M, dun néng va thém 61timg giot dung dich HO. cho t6i khi tan hoain todn, sau d6 dun s6i ky dé dudi hét H502 dur, Chuyén toin b6 miu vao binh dinh mire 100ml, tring ede 3 lan biing nude cat vio. binh dinh mite, thém nude cat wi vach mire va lie déu, durge dung dich A. Lay 10m! dung dich A vao binh nn 250ml, thém mt mau gidy conggo do, nho timg ot dung dich CHsCOONa 5 % cho dén di miu gidy tirxang sang dé. Thém lai | giot dung dich HCl 6M, thém tiép 30 ml dung dich EDTA néng 46 C, (0,05 M), dun dén soi , thém tiép bing hat ng6 urotropin va tiép tuc dun Oi 3 phut. Dé ngudi dén khoding 60-70°C vi thém vai giot dung dich chit chi thi PAN, dung dich e6 miu ving xanb, Ding dung dich Zn** c6 ndng 4} C2 chun d6 ti khi dung dich chuyén sang miu d6 nho, hét V;ml Zn". Gitt nguyén dung dich nay, them vio khoang 0,5g NaF, lie ki, dun sOi sau d6 thém khoang 0,5g urotropin, kc ki, dung dich lai chuyén sang mau ving. Tiép tye chudin 46 bhing Zn** cho wi khi dung dich lai chuyén sang dd Kin 2, ghi thé tich Zn* da chun d6 - Vom Lay 10ml dung dich A, cho vio binh nén 250ml, dun si ki, thém khong 10m! nue thém tiép 10ml KL +KSCN 5%, dé vao ché t6i 10 phit. Ding dung dich NaS,0, c6 ning 4 Cs, chudin 4) cho t6i khi dung dich chuyén sang mau ving rom thi thém Im hd tinh b6t, dung dich sé 6 miu xanh tim. Chuan tiép biing Na,S,O, cho t6i hét miu xanh tim, hét Vs mb nh vién tur lap cOng thie tinh him hrong Cu, Al, Zn (mg) trong mau phin tich &6 long ean eho trrée. / BAL 18 XAC DINH HAM LUQNG Fe, Cr, Ni TRONG HQP KIM INOX 18,1, NGUYEN TAC XAC DINH ~ Hod tan mu inox bing hin hyp axit H.SO, 25 % va H,PO, 10% (trong truimg hop ‘cdi thiét c6 thé thém HNO) duge dung dich chira Fe"*,Cr” va Ni*. - Xée dinh Fe’: LAy dung dich hin hop sau khi hod tan mu, oxihod Cr+ thank Cr,0,7 bing (NH,),S20, c6 chat xtc tke AgNO, va Mn* Lim chit chi thi cho qué trinh ‘oxi hod hoan toan, Sau d6, logi MnO, bing HCI dur, két tha Fe(OH); trong méi truémg. NH,, hoa tan két ta nay béing HCI va chun d6 theo phuong phip complexon.- Xée dinh CP*: xi hod Ce* thanh Cr,0;* bing dung dich KMnO, dun néng, loai lugng dur KMnO, bing dung dich HCI loang, thém vao dung dich lrong du chinh xée Fe** va chun d6 Iuong Fe* dur bing dung dich chun KMnO,, - Xie dinh Ni**: Két tha Ni* biing dimetylglioxim trong mdi trrong NH, (khi di che Fe™* bling amoni xitrat va oxi hod Cr thnah Cr,0;*), loc My két tha va hoa tan tong: HCI 1:1 sau dé thém luong dur chinh xe EDTA va chuin lugng EDTA dur bing dung dich chudn Z1°* & pH =11 véi chit chi thi ETOO. CH. -OH Ni* +2 CHy C=N-OH CH; -C=N-0 18.2. QUY TRINH PHAN TiCH Can chinh xc trén can phan tich a gam (0.4- 0,5 gam) miu inox dang phoi bio, cho vao cdc chiu nhiét co 250 ml, thém vao dé tir 20 dén 40 ml hin hop axit HQ, 25 % va HPO, 10%, day ede bing nip kinh déng hd, Dun nong tir tir trén bép dign (t6t nhat La ding bép cach cat) dén khi miu hoa tan hét. Néu miu khéng tan hét (trrdng hop ¢6 nhiéu_ cacbua) thi thém tiép yao cdc 4-6 ml dung dich HNO, 1:1, dun tiép dén tan, sau d6 mo nip kinh déng ho va iép tuc dun cho dén khi béc khoi tring SOs, Dé cde ngudi, cn thin thém vio céc khoang 30 ml nude ct, loc, nt phan en khong tan qua gidy loc bang tring (néu cain) va chuyén yao binh dinh mie 100 ml, dinh mite dén vach, lic déu durge dung dich A. Xie dinh Fe Hit chinh xc 10,0 ml dung dich A vio e6e chju nhigt c& 250 mi, thém 1 giot dung dich MnSO, 2 %, 3-4 gigt dung dich dung dich AgNO, 1%, dun dén bit diu s6i \ém tir tir timg lurong nhé tinh thé (NH,)2S.0, dén khi dung dich c6 mau hdng én dinh, thém tiép timg giot dung dich HCI 1:1 dé logi KMnO, dén khi dung dich e6 miu ving. Thém vio dé khoang 0,5 gam NH,Cl, tig giot dung dich dung dich NH, 6 M dén mii khai dé két ta hoan toan Fe(QH)s. Loc gan, néng két tia qua gidy loc bing do, rira két tia 5 lin 63hinh két tia lai Fe(OH); lan thir hai, Hoa tan két ta bing dung dich HC! 1:1, nia gidy loc biing mude cat, thém 10 giot dung dich chat chi thi axit sunfosalyxilic va timg gigt dung dich CH;COONa 5 % (néu cin) dén khi dung. dich c6 miu tim va chudn 46 Fe** bing dung dich chuin EDTA dén déi mau chit chi thi, Xie dinh Cr Hat chinh xée 10,0 ml dung dich A vao binh nén dung tich 250 mi, thém khong 10 ml nue cit, 2ml H,SO, 4 M, dun dung dich dén s6i va thém tir tir dung dich KMnO, 2 bing dung dich NH.NOs 2%, sau d6 ti % dén khi xudt hign mau tim bén ving, tiép tue dun khoding 5 phuit, thém rit tir tir (than trong dé khdi thira) dung dich HCl foang (1:10) dén khi dung dich chic mau vang da cam cla H,Cr,07. Dé ngudi dung dich, thém vao 4 mgt Iuong chinh xéc dung dich chun Fe** (khoang 25 ml, ndng 46 0,02 M), 10 ml hén hop bio vé va chuiin 46 rong, Fe** dir bing dung dich chuin KMnO,, ch trong miu. Trong trrémg hop khong ¢6 vanadi va vonfram thi e6 thé chuin trye tiép bing dung dich FeSO, voi céc chit chi thi thong thu’mg nhur axit phenylanthranilic, ‘Cich lam nay loai trir anh huréng cia vanadi vi vonfram néu ching cd diphenylamin, ‘Xa dinh Ni* Hit chinh xée 10,0 ml dung dich A vio ede chiu nhigt e@ 250 mi, thém khodng 5 ml rurée cit, 1_ gam amoni xitrat (dé logi trir nh huémg cha Fe™), thém vai gigt dung dich HO, dic, 10m! dung dich NH, 6M (1:1) dén xudt hign khi mii khai, dun nong dén 50°C, thém tigp 10 ml dimetyl glioxim 1%, Dun néng dung dich dén khodng 90°C, tim mui két tia trong 60 phit va loc két tha qua gidy loc bing xanh, rita két tia bing dung dich NH; 2,5% tir 4-5 in dén khi nude loc khong cdn mau ving. Hoa tan két tia thu dirge bing Iuong vita di HCI 1:1, néng vao binh nén dung tich 250 mi, rim két tia béing nude nong, thém luong dur chinh xéc dung dich chuin EDTA (khoang 25 ml, néng 46 0,02 M), 1 mau gidy qui tim va tring hod HCI dur bing NHy 1:1 én di mau chit chi thi, sau d, thém10 ml dim NH,CI/ NH; (pH=10), vi chun 46, hat chi thi ETOO dén khi chat chi thi long EDTA dur bing dung dich chudn Zn” v cchuyén tir miu xanh sang d6 nho. 64.18.3, TINH TOAN KET QUA Sinh vign ty thidt lap cdng thire tinh Iugng (mg) Fe, Cr, Ni trong hgp kim inox trong miu inox da edn trade khéi lung. 184, HOA CHAT - Miu phin tich: miu inox dang phoi bio (da cn trac kh6i Iugng), mdi sinh vién mpt miu. - Hin hop H.SO. 25 % va HsPO, 10%: Thém edn thin 160 ml H,SOs die (d= 1,84 ‘gim)) vio 760 mi mrdc et, Lim ngudi. Sau dé, thém tir tir vio hdn bop trén 80 ml HPO. dic (=1,75 gimml) va lie déu. -Dung dich dimetyl glioxim 1%, dung dich NH 1/1, dung dich KMnO, chura 6 ning d@ chinh xic ding dé chun do. ‘Cac hod chit cdn thiét khéc sinh vién ty chudn bi gom: HCI die, 1:1 va 1:10 HNO, de vi. 1:1 NH; die, 1:1 va 2,5% ~ CH,COONa 5% ~ Tinh thé amon xitrat, Tinh thé (NH.):Fe(SO,)2, KMn0,, HAC,0,,.21,0, - NH.NOs, - KNO, BAI 19 XAC DINH HAMLUQNG Cu, Sn, Pb, Zn TRONG DONG THAU 19.1, NGUYEN TAC XAC BINH 65Hod tan miu déng thau dang phoi bio bing dung dich HNO; de, dun ndng va e dung, dich miu dén gin kh6, Sn‘* bi thuy phin thinh H,SnO, khong tn. Loc nia két ta H,SnOs, nude loc chia Cu", Zn, Pb’. Phin nude Ige: + Két tia Pb™ bing K,Cr,0; trong mdi truimg dém axetat (pH = 5-6) didi dang PbCrO,. Loe, rita sach két ta va hoa tan két tia bing hn hop NaCl + HCI va chudin 46 H, "20; sinh ra theo phuong phép iot ~ thiosuntat 2PbCrO, + 4NaCl + 4HC] —> 2NasPbCl, + HCr.0; + H. + Cu” durge xe dinh tnye tiép theo phuong phip iot — thiosunfat. + Téng ham Iuong Cu", Pb, Zn* duge xic dinh theo phuomg php chuin a} complexon ding chit chit chi thi PAN & pH = 5-6, tir d6 xae dinh duge him lurong Zn. Phiin két tia: Xée dinh Sn bing cich hod tan két tha H:SnO; trong HCI 1:1 sau d6, khir Sn thank Sn** bling H moi sinh (Zn trong moi trudmg axit) va chudin 46 Sn** sinh ra bing dung dich chuain I; véi chat chi thi hé tinh bét. H,Sn0;+4HCI > SnCl, +4H.0 ; Sn‘*+2H — Sn’ It Sn* > 20+ Sn** 19.2. QUY TRINH PHAN TICH ‘Cn chinh xde trén cn phan tich a gam (khong 1 gam) phoi ding thau vao ede chiu nhiét cd 250 mi, diy céc bing kinh ding hd, thém 10 ml HNO; die va 10 ml nude qua mo ec. dun néng trén bép cach edt. Sau khi hop kim tan hét, kim bay hoi dung dich & 80- 90 °C dén thé tich 5- 8 ml, Dé ngudi bist, thém khoang $ ml nude cit va tiép tuc ¢6 miu gin khé (cn lam bay hoi chim khoing 1 gid). Lay cdc ra, thém mrde néng, khudy ky va loe, nia két tia bling dung dich HNO; lofing, néng (1:20) qua gidiy oe bing xanh vio binh dinh mie 250 ml durge dung dich A. 19.2.1. XAC BINH Sn Hoa tan két ta trén gidy loc biing 10 ml dung dich HCI 1/1, rira sach gidy loc bing muréc ct, thu nude loc va nude nira vio binh nén dung tich 250 ml, Thém 2 gam hén hop Al+Zn va Iml dung dich FeCl; 1% vao binh nin dung tich. Bun nbe trén bép dign cho én khi dung dich hét_ miu ving. Dé ngudi, loc bo Al va Zn dur (qua gidy loc bing tring) va chun 9 dung dich thu duge bing dung dich chuin 1; voi chat chi thi hé tinh bot dén khi xudt ign miu xanb, 19.2.2. XAC INH Cu, Pb, Zn TRONG DUNG DICH NUGC LOC 42H"; 664) Xie dinh Cu?* theo phuemg phip iot-thiosuntat Lay 10 ml dung dich A vio binb nén 250 mi, thm 2 ml HsSO, 2M va dun nbe dén khi ‘¢6 kh6i tring SO; (cé thé c6 két ta tring PbSO,, dé loai trirhét NOs, edn bée SOs hai Lain ). Dé ngudi, thém 30 ml nude edt, dun sOi 1-2 phut, dé ngudi va thém timg giot dung dich NH, 10 % dé digu chinh pH dén moi trudmg trung tinh, sau d6 axit hod nhe bing S ml dung dich HPO, 5 %. Thém 10 ml dung dich KI 5% trong KSCN va chusin d > sinh ra. bing dung dich chun NazS,0; ning 4 C, (M/1) voi chit chi thi hé tinh bot, hét V, ml, b) Xéc dinh Pb™* bing phurong phip bicromat Ly 50,0 ml dung dich A cho vio ede chiu mbigt e& 250 ml, thém 10 ml amoni xitrat 5%, trung hod bing NaOH 5% khi dung dich chuyén sang miu xanh dim, thém CH;COOH 2 % dén tan két tia tring (pH ~5-6). Thém tiép vao dung dich 5 ml dung dich dm CH,COOH -CH;COONa pH-S va cho tir tir 10 ml KCr,O; 10% khudy ky, dun néng: dén bit dau sdi, My ra dé ling 1 gid. Loc, nira két tua trén gidy loc bang xanh biing nude cit dén hét CrO,?. Hod tan két tha trén gidy loc biing 15 ml hn hop HCl+ NaC! dun nong_ (pha & phan 19.4), rira gidy loc biing nude ct néng vao binh nén 250 ml, ~ Pha long dung dich thu duge & trén, thém 10 ml dung dich KI 5%, dé chd t6i 5 phuit vi chuiin dy sinh ra bing dung dich chuiin Na;S;O, t6i mu ving rom ri thém ebat chi thi hé tinh bot va tigp tuc chun dO bling dung dich chuin Na,S,O, c6 néng dO C, dén mit mau xanh, hét Vz ml ©) Xéc dinh tng him lugng Zn, Pb*, Cu?* Lay 10,0 ml dung dich A cho yao binh nn dung tich 250 mi, diéu chin méi trutng chuan 46 vé pH = 4 bing dung dich NH, 2M voi chit chi thi congo do, thém 2 g urotropin (hoe 10 ml dung dich dém acetat pH=5) vi chun d@ bing dung dich ebuin EDTA c6 néng d6 C2 (M/) voi chit chi thi PAN (dun si dung dich) dén khi dung dich cchuyén tir miu tim sang mau xanh ld cay, hét Vs mu 19.3,TINH TOAN KET QUA Sinh vien ty thiét lip cing thite tinh him luemg (mg) Cu, Zn, Pb, Sn trong miu phn tich | 19.4, HOA CHAT - Hn hop HCI va NaCl: edn 320 g NaCl hoa tan trong khong 200 ml nude, thém tigp 100 ml HCI die vai pha vita di thinh 1 lit; dung dich K.Cr:0, 5 % -Céie dung dich 12, Na2S.s, EDTA chur ¢6 néng d} chinh xie ding dé chuin 46, dung dich chuin K,C,O, ¢6 ndng 46 cho truise,chit chi thi PAN. ~ Cae hod chit khde sinh vién nr pha tir: HNO, dic, HCI dic, tinh thé amoni xitrat, urotropin tinh thé KI, KMnO,, Hi ). NH.NOs, KNOs, CH;COONa, K:Cr.0;, urotropin/. 67BAL 20 XAC DINH HAM LUQNG Fe, Cu, Al, Zn TRONG HOP KIM NHOM 20.1. NGUYEN TAC XAC BINH ~ Hoi tan miu hop kim nhém bing dung dich kiém dic, néng. ~ Phan cin khong tan chira Cu, Fe durge hod tan trong HNOs, Fe duge tich loai & dang Fe(OH); bing dung dich NH; dic, sau d6 hoa tan két tua, khir Fe ** xudng Fe™ va. xée dinh theo phuomg php pemanganat, con Cu’ trong nude koe & dang phite Cu(NH,).* duge xie dinh bing phurong phip complexon, ~ Nude pe 6 ehita AIOs va ZnO duge xée dinh theo phyong phip chuin d6 nguge vi EDTA, diing NaF dé che Al" va xée dinh duge Zn (xem bai xie dinh Al, Cu, Zn trong hop kim devada), 20.2. QUY TRINH PHAN TICH - Can chinh xc trén cn phan tich a gam (khong 0,5 gam) miu nhom dang phoi bio mong vio cde chiu nhiét c& 250 ml. Thém vao céc 20 ml NaOH 33 %, dun ndng trén ién cho tan. Lay cdc ra, dé ngugi bét va thém 20 ml nurde edt, loc, rira phn khong tan qua gidy loc bing tring vio binh dinh mire 100 ml. Nude loc duge dinh mite dén vach bing nue ct due dung dich A (ding dé xc dinh Al va Zn). ~ Chuyén giy loe chia phin khéng tan trong NaOH vio cdc chiu nhigt cd 250 ml, thém yao cdc 15 ml dung dich HNO, 1:1 dun s6i hén hop trén bép dign dén khi tan boan ton, thém vai giot dung dich H,SO, die va tiép tue dun néng dén khi_ khong cOn khi mau nau thodt ra. Lay ede ra, dé ngudi bot va loc qua gidy loc bing tring vio binh din mire 100 mi, din mire dén-vach duge dung dich B. Xie dinh Alva Zn: Ly 5,0 mi dung dich A vio binh nén dung tich 250 mi, thém 1 mau gidy céng g6 ‘dung dich HCI 2M dén khi chi thi di sang miu hoi xm, thém tiép 1 gam urotropin, thém dur chinh xéic V,ml dung dich chuan EDTA néng } C, (khoang 25 ml, ning d6 0,02 M) va dun sOi dung dich 3 phit. Ly ra dé ngudi va chun 49 rong EDTA dur biing dung dich chudn Zn** ndng 46 C, voi chat chi thi xilenol da cam dén khi chit chi thi déi tir mau vang sang mau do tim thi dimg lai, hét Vim. Gi 6, thém tir tir timg giot dung 68.nguyén dung dich nay, thém khoding 0,52 NaF, lic ki, dun séi sau d6 thém khoang 0.5g. ich urotropin, lic ki, dung dich lai chuyén sang mau ving, Tiép tye chudin 46 bing dung cchuiin Zn** cho t6i khi dung dich Iai chuyén sang dé tim. Ghi thé tich dung dich Zn°* teu tn, hét Vm, Xie dinh Fe va Cu Lay10,0 ml dung dich B vao eéc chiu nhiét co 250 ml, thém 10 ml nude . dun ning trén bép dign dén khosing 90°C va thém timg giot dung dich NH, 6 M dén khi e6 mii NH; (dé két tia hoin toin Fe). Dun s6i 5 phat, loc gan, néng dung dich, sau d6 chuyén két tia vio gidy loc bing dé, rita két tha 5 Lin bling nude néng. Lap lai qué trinh két ta 2 Hin. Toan bd muse loc ding dé xe dinh Cu”, - Hoa tan két tia vao mot binh nén dung tich sach bing dung dich HCI 6 M (khoang 15-20 ml), na gidy loc bing nude cit, dun nhe dén khong 70°C, thém vao dung dich 2- 3 miu nbd Zn va vai gigt dung dich CuSO, 5%. Dun néng dung dich dé phan ting Khir xiy ra hodn todn, dung dich e mau xanh rit nhat. Rita gan dung dich sang mot binh nén dung tich 250ml khic qua phéu c6 chira m6t it bong & cudng phéu dé loai nhimg miu kém dd, tring rita phéu. Thém tiép 2-3 ml dung dich HsPO, 4M va 3-4 giot dung dich chit chi thi diphenylamin hoe phenylanthranylic 0,2% vao dung dich dinh phan. Chuin 46 bing dung dich chudn K,Cr,0, nding dC, cho dén xuit hién mau xanh tim, bén khoang 1 phat, hét Vsml. ~ Phin nurse loc (sau khi tich Fe) chita Cu* & dang phite Cu(NHs)2* duge axit hod bing dung dich CH,COOH 2% ti khi déi mau qui tim, thém khodng 1 gam urotropin, mot it chat chi thi murexit va chudn 6 bing dung dich chuan EDTA dén khi dung dich chuyén tir mau vang luc sang mau tim, hét Vl, 20.3. TINH TOAN KET QUA Sinh vién ty thiét lip cOng thie tinh Iugng (mg) Al, Zn, Fe, Cu e6 trong mau phan tich cho trrde. 20.4. HOA CHAT ~ Miu nhém di can chinh xc khdi lugng, mdi sinh vién 1 miu, ~ Dung dich EDTA, Na2S,Qj . I ding dé chun 49 chura cé ning d6 chinh xa. 69~ Dung dich cde chit chi thi axit sufosalixylic, xilenol da cam, - ede hod chit cin thiét khiic, sinh vién ty pha tir NHs de, HCI die, HNO; die; NaOH rin, urotropin. CHUONG7 PHAN TICH MOT SO SAN PHAM CONG NGHIEP HOA CHAT. ‘Cac sin phim céng nghiép hod chat rit da dang, tay nhién sin phim cé tinh phd bién dién hinh 14 xi ming va phan bén, Trong chuomg nity, hoe sinh Lim quen véi pha miu xi mmiing vi phan tich mét s6 chi tiéu trong 6, tiép theo La phan tich phan bin NPK vi cudi cing ld quing mangan. BAI21 XAC DINH HAMLUQNG ALO, Fe,03, CaO, MgO TRONG XI MANG POOCLANG. 21.1. CHUAN BI MAU Lay 150- 250 g xi mang (cich lay theo tiéu chudn Viét Nam 4787-089) cho vao lo thuy tinh day kin, Miu duge dua vé phong thi nghiém, 4 trén ts gidy king, tril thinh 1 lop mong. Ding nam cham dé hit sit kim logi ln trong xi ming, Sau 45, ding phuong php chia tu dé Liy khoding 25 g, nghién nh miu thu durge trong c6i mi niio thanh bot min dé Lim miu phan tich. Phin cén lai gitr trong lo thuy tinh day kin. Sdy mu & 105° C dén khdi lugng khong di, trn déu trrde khi ein dé tién hanh phan tich, 21.2. PHAN HUY MAU Cn chinh xdc a gam (khoang 0,5 -0,7 g) miu vao cée chiu nhiét c& 250 ml, tim uot miu bing nude ct, ding dita thuy tinh dam tan hét cue, thém 1 gam NH,Cl. Diy ede bing m§t kinh dng hé va cho tir tir 10 ml HCI die qua mé cée, le déu, dun trén bép cdich thuy khoing 60 phut (vita dun vira khuiy). Néu miu bée gin khé thi liy ra thém tiép 5 ml 70HCI dje nda, dun tiép cho dén khi duge bia tring. Lay ede ra, thém 25 ml nude edt dun soi, khudy déu, dé Ling va loc gan qua gidy loc bing tring vao binh dinh mire 100 ml. Ding dung dich HCI 5 % mira két tia va thanh céc, loc gan 3 lan sau d6 chuyén két tia vio gidy loc, rira lai két tha bing murde ct dun soi dén hét ion Cl (thir bing dung dich AgNO 5% trong HNOs) sau do thém nuve cit dén vach mire, lic déu, due dung dich A 21.3. NGUYEN TAC BINH Chun 49 Fe(ID) trong dung dich A bing dung dich chun EDTA & moi trutmg pH = 15-1,8 voi chat chi thi axit sunfosalixylic. Két thic chudn d6 khi mau dung dich dink phan chuyén tirtim d6 sang mau vang nbgt Chuin 49 nguye dé xie dinh tng ham lugng Al(LM) va Fe(II) trong dung dich A bing eich cho lung dur chinh xe EDTA, digu chinh mdi truémg pH = 5, dun soi dung dich sau 46 chuin 6 Iuong EDTA dir bing dung dich chun Zn”*, vi chit chi thi CuY- PAN. Két thie chudin d) khi miu cua dung dich chuyén tir vang sang miu xanh tim, Két hop voi két qui xde dinh Fe(II) 6 trén dé tim ra Luong nhom c6 trong miu. Canxi vai magie durge tich khOi sit, nhom bing amonihydroxit. Chuin d9 canxi bing dung dich chuin EDTA & pH = 12 voi chit chi thi murexit. Tai diém tuong duong, dung dich chuyén tir mau db hing sang mau tim, ‘Chuin d9 xée dinh téng long canxi va magie trong miu bing dung dich chudin EDTA voi chit chi thi ET-OO & pH = 10. Xéc dinh him lurgng magie theo higu sé thé tich EDTA tiéu thy qua hai phép chuin 49, tir d6 xée dinh riéng canxi va mage. 21.4. QUY TRINH PHAN TICH (THEO TCVN 139-1991) 2141. Xéec dink him lugng Fe,0, Hit chinh xée 10,0 ml dung dich A vaio binh nén dung tich 250 mi, thém 30 ml nude cit, 5 giot dung dich dung dich H,0, 30%, dun nhe sau d6 dun ky dé loai hét H.0, dur, thém 1 ml dung dich axit sufosalixylic 10%, thém nude edt dén Khodng 100 ml. Ding dung dich CH,COONa 10% dé diéu chinh pH dén 1,5-1,8 (dung dich chuyén sang miu tim sim), Dun néng dung dich dén 50°C-60°C réi chuiin 46 béing dung dich chuin EDTA ning d@ Co (M) dén khi dung dich chuyén tir mau do tim sang mau ving nhat, hét V, ml. 242 Xée dink him legng ALO, 1Hit chinh xée 10 m1 dung dich A vao binh non dung tich 250 ml, thém mot miu nho gidy chi thi cong g6 dé va nho tir tir dung dich CH;COONa 10% cho ti khi gidy chit chi thi bit dau chuyén sang miu hdng, sau dé thém 1 gigt dung dich HCI 1:1. Thém tiép vio binh chun d6 25 ml dung dich chuin EDTA néng 45 Co, dun s6i dung dich, thém 0,5 gam urotropin va tip tye dun s6i dung dich 2 phit. Dé ngudi dén con 60-70"C, thém 2 siot dung dich chit chi thi CuY- PAN , dung dich c6 miu vang (c6 thé ding xylenol da cam). Chuan 46 lugng EDTA dur biing dung dich chudin Zn™ (ndng a9 C,) cho dén khi dung dich c6 mau xanh tim, hét V2 ml, 21.4.4Xée dink ham hegng CaO. 1a) Téich logi Ca va Mg ra khdi Fe va Al Ding pipet lay 10 ml dung dich A yao cdc chiu nhigt c% 250 ml, thém vio ede 1 g NH,Cl, dun néng dung dich dén 60°C-70"C va nho tir tir dung dich NH; 6 M dén khi két tia hodn todn (dung dich c6 mii amoniac), thém dtr vai giot dung dich NH 6 M nia. Dun soi dung dich trong this gian $ phit dé két tha déng ty va logi NH, dur. Loc dung dich edn ning qua gify loc bing do vio binh dinh mie 100 ml, Ding dung dich NHJNO, 2% néng ira két tia 5 Lin, méi Kin khoang 5 ml. Chuyén phéu cé gidiy loc va két tia sang cde 250 mil. Nho tir ti timg git dung dich HCI 1:1 (khoang 10 ml) vao két tia dé hoa tan két tia ngay trén gidy loc vio céc 250 ml (khdng cn choe thing gidy loc). Rira gidy loc bing nuréc néng va tién han két tia Iai Fe(OH); nhu lan 1, Loc va nim két ta 5 lin, mdi lin bhing 5 ml dung dich NH.NO; 2% ndng vio binh dinh mire 100 mi 6 trén va thém nue dit dén vach mite, lic ky, duye dung dich B. b) Xie dinh Ca”*: Ly vao binh nén dung tich 250 ml gém 10 ml dung dich B, thém nurée edt dén khodng 100 ml, thém tiép 5 ml dung dich KOH 2M, dun néng dung dich cho én hét mii amoniae, dé ngudi va thém chat chi thi murexit, Chudin d6 long Ca?* trong miu biing dung dich chun EDTA dén khi dung dich chuyén mau tir dé hong sang mau tim, hét Vs mb ¢) Xe dinh ting ham lrgng Ca”* va Mg™: Lay 10,0 ml dung dich B vao binh nén ‘dung tich 250 mi, thm 10 ml dung dich dm pH = 10 vii mot it chit chi thi ET-OO. Ding dung dich chuin EDTA ning dd Cy chuin d dén khi dung dich chuyén tir miu dé nho sang miu xanh, hét V; ml. 21.5. TINH TOAN KET QUA:Sinh vign ty thiét lip eng thite tinh ham lung (%) AlOs, FeO), CaO va MgO trong miu cho truée (a gam). 21.6. HOA CHAT - Miu xi ming Bat son da duge sy khé c6 khéi Iugng chinh xic, mdi sinh vién mot miu. - Dung dich EDTA (ning d6 khong 0,02M), dung dich Cu”*, dung dich Zn?* ding é chuin d6 (sinh vién wrxde dinh nding 49), ~ Chit chi thi PAN, axit sufosalyxilic 10%, murexit, ETOO. Dung dich dém pH=10, urotropin, dung dich AgNO, 5%. - Cée hod chit edn thiét khée sinh vién ur pha tir dung dich HCI dic, HO, 30%, dung dich NH, 6M, KOH rin, tinh thé NH,CI, tinh thé MgSO,.7H,0, CH,COONa r tinh thé NHWNO, BAI22 XAC DINH HAM LUQNG P,O; TRONG PHAN BON NPK NPK la phiin bon da luong can thiét cho qué trinh sinh trang va phat trién cita cay trdng durge pha ché tir améphot (gm NH,H;PO, va (NH,)sHPO, ¢6 12 % N va 47- % POs); di améphot (gim 6 (NH,);HPO, chita 18-21 % N vas % PO.) e6 tron thém K,S0,va KCL Nitrophot K la logi phan bén hén hop eiia améphdt vi KNOs chia 12-16 % N, 12-16 % KO va 12-16 % % POs Ngoai ra, tuy theo logi cy trong nguti ta c6 thé thay doi thanh phan N, P, K trong thinh phin phn bin phe hop. Kali a kim logi kiém, kh e6 phan ting phan tich thé tich phi hop; dé phan tich 13, mot phuomg php thich hop Li phan tich quang ké ngon lira, chiing ta sé khong dé cap trong gido trinh nay. Nito cing li nguyén t6 da lugng, phan tich durge bit dau voi vie v6 co hod miu bing H.SO, c6 chit xtie tie cu”*dé chuyén cde dang cla phan nito vé NH," tiép theo Li kiém hod dung dich va cét dinh lugng bing 16i cuén hoi nude vio mot dung dich axit dé BOi sau 6 chun dO axit — bazo. Chiing ta s@ gip phép phiin tich nay trong phan phan tich nurée miim & bai 26 trang72-75. 22.1. NGUYEN TAC XAC INH PHOTPHO (TINH THEO P:0s) “Hod tan miu: mu phan bon Nitrophot K duge hoa fan hodn ton trong nude thinh dung dich PO,* Xie dinh tng him long PO,” theo phuomg phi axit — azo. ~ Kéttia PO,” bing hén hop nitromolipdic ( NH.);MoO, + HNO; H,PO,+21 (NH,):MoO, +21HNOs — (NH,)s[P(Mo;0)e] + 2INH,NOs+12 H:0 ~ Loe, ria két tia dén sach HNO, va hod tan két tla trong lung du, chinh xée NaOH va chuin 4} lvgng NaOH dir bing dung dich chuin HCI véi chit chi thi phenolphtalein, (NH), P{Mo,O,o):] + 23 NOH —> NaNHHPO, + (NH);MoO, +1NaMoO, + 11 H,0 Néu hod tan két tia bing NaOH thutsng mit thém mét lung NaOH do cé phan img: NH,’ + OH > NH,+ 1,0 Do dé, dé trinh sai sé ny ngubi ta thém andehit foemic tude Khi hod tan két tha bing NaOH, khi do HCHO sé két hop visi NH," wo thanh urotroppin (CH.).N« 4(NH,),{P(Mo,0 ,»),] + 104 NaOH + 18 HCHO —> 4 Na,HPO, + 48Na,MoO, + 3 (CH).N, +74 1.0. QUY TRINH PHAN TICH (Can chinh xéc trén edn phan tich a gam (khoang 1 gam) phin bon NPK (miu phan bén nitrophotska ) vio cdc chiu nhiét c& 250 mil, hod tan biing 50 ml nude edt, loc bo phan khéng tan qua gidy loc béing ving vio binh dinh mic 100 ml, dinh mire dén vach, lic déu duroe dung dich A. Hut chinh xée 10 ml dung dich A vio eée chiu nhigt e& 250 ml, thém 10 ml NH,NO, 5%, dun nong t6i khoang 60 °C . Lay cée ma, vila khudy via thém timg gigt dung. dich dung dich nitromolipdic 0,5 M dén hét 20 ml. Lam mudi két tia 60 phut. Ria gan két tua biing dung dich KNO; 5% khoing 10 ln vao gidy loc bing xanh, sau 46 chuyén hét két tia 1én phéu. Tiép tue rita trén phéu dén hét phan img axit (ly Khoding 1 ml nude rita, thém 1 git dung dich phenolphtalein vi 1 gigt dung dich NaOH 0,1 M, néu dung dich c mau hong li duge). 4‘Chuyén két tua va gidy loc vio cdc, thém vao 46 10 ml dung dich andehit focmic (43 diéu chinh moi trudmg trung tinh véi phenolphtalein). Thém chinh xe mde lung dung, dich chun NaOH 0,25M t6i khi tan hét két tia, dung dich cé mau hing, thém tiép 5 ml nia dé NaOH dur (ghi téng thé tich NaOH da cho vao). Tir buret chusin 46 luomg NaOH ir biing dung dich chun HCI (ndng 4 0,05M) véi chat chi thi phenolphtalein dén Khi dung dich mit miu héng, hét V ml. 22.3.TINH TOAN KET QUA Sinh vién ty thiét lp céng thire tinh him Iugng phan trim P,Q; trong phan bon NPK. vai biio cao két quai 22.4, HOA CHAT ~ Miu phi tich: phan bon nitrophotska: mdi sinh vién niin mot miu phan tich, (e6 thé sinh vien ty edin du), - Dung dich hén hop nitromolipdic, HCI 6N, NHs 25 %. ~ KINO) tinh thé, chat gde Hy ~ Dung dich NaOH, HCI dé chuzin 46 chua c6 ning 49 chinh xc. ~ Chat chi thi phenolphtalein, metyl vang BAI 23. XAC DINH HAM LUQNG Mn TRONG QUANG PYROLUZIT. 23.1. NGUYEN TAC XAC DINH Dua trén sur khir MnO, khi dun néng: MnO; +2 CI +4H*— Mn +2H.0+Ch Kihi clo ty do téch ma dupe thu vio dung dich KI, phin ting nay lam gidi phong ra long iot tung duong. ‘Sau khi két thie phan img ngurdi ta cho lrgng fot tgo thin vio binh dinh mire, pha loding dén vach mite, lic déu va hit thé tich xc dinh i6t dé chudin 46 bing dung dich chun Nas 23.2. QUY TRINH PHAN TICH 03 Tir dé tinh durge ham lugng MnO; trong piroluzit, 15Can trén edn phin tich khodng 0,5 - 0.6 g piroluzit cho vio binh vurx, cbn éng din khi nhiing vio dung dich clo va cho dung dich KI vao binh hip thy, & c6 binh edu c6 lip phéu chiét cudng dii dén gin day binh cdu, cho vio phéu 50 ml HCI 30%, ‘Cho HC! qua phéu binh céu, dun nhe binh trén bép cach edt, sau d6 dun manh dén_ Khi toin bp long edn piroluzit tan trong HCI (é dy binh edu e6 thé cdn tap chit SiO: khong tan ). ‘Sau khi két thie qué trinh tich clo, théo binh hip thy, rita éng din khi bing nue cat va cho mréc nira vao binh hap thy. Lam lanh binh hip thy, sau do chuyén dinh rong véo binh dinh mire 250 ml. Rira binh hap thy vai lan biing nurée edit vi cho vao dinh mire trén, Dinh mite dén vach béing nue edt, ie déu. Hit 25 ml dung dich vao binh nén dung tich 50 ml va chudn 46 iot sinh ra bing dung dich chudn Na;S.O; ndng d6 C, voi chi thi ho tinh bot hét V ml. 23.3. TINH TOAN KET QUA Sinh vign ty thiét kip cng thite tinh him long MnO; (*)trong piroluzit. 23.4. HOA CHAT ~ Miu phan tich: sinh vien ty ein - Dung dich Na;$05 ding dé chun d6 chu e6 ndng a xée dinh. - Cae dung dich HCl 30 %, KI, chi thi hé tinh bot, CHUONG 8 PHAN TICH MOI TRUONG (C6 rt nbiéu chi tiéu cn phin tich trong méi trading, d6 la cdc kim loai ma dic biét li cdc kim logi e6 tinh de cao nhu thuy ngin, asen, chi, eadimi ede chat hitu co efing e6 tinh «de cao nhur phenol, edie hop chit co-elo, ede thude bio vé thye vat ..., ngodi ma ede chi tiéu vé nhu edu t6i thiéu cita méi tru’mg sng nhu oxi trong nube, murde thai, ce chat a hai trong khéng khi .. .ciing duge quan tim. Trong chuong nay, ching ta dé céip wi phan tich mt vai chi tu trong nucée va nude thai bing phan tich thé tik, 16BAI 24 PHAN TICH MOTSOCHI TIEU HOA HQC. CUA NUOC VA NUOC THAL 24.1. XAC DINH HAM LUQNG OXY HOA TAN (DO) TRONG NUGC MAY Tit cd cde sinh vit quy hiéu khi déu cdn oxi cho qué trinh hé hap dé séng. Céc sinh vat trén can sir dung oxy khong khi, cin cde sinh vat sing trong murée lay oxi tir oxi hod tan trong nuée. Oxy tan trong mirée rit it, 4 bao hod cia oxi trong née sach & 0" C khoang 14-15 ppm. Nhiét 6 cing ting dé tan cia oxi vido nude eding giim. Trong mrée e6 ede foal thye vat séng, do qué trinh quang hop gid phong ra oxi thi 6 nhimg ving dé rong oxi trong nurée nigu trén mite bo hoa e6 thé t6i 200% edn goi ld siéu bao hoa. * DO trong nude duvge diéu chinh bi Swrtrao déi gitta khong khi vi nude. - Oxi duge gidi phéng do qué trinh quang hop ca cdc the vat sng trong mrde (Hai qua trinh nay Kim cho d9 hod tan eit oxi dat bao hoa va siéu bao hoa). ~ Do dng vat, thye vét va ede sinh vat phin huy tigu thy qua tinh niy lim gdm DO trong nue * Gid tri DO bién déi theo nbip digu ngay va dém: eye dai vio gitta rua va eye tiéu vio ban dém, * Gid wi DO bién déi theo chiéu sau cita mrée, oxy thudmg hod tan nhiéu & lop nude mit (ting quang hop). Cin cir vao gid tri DO cé thé bién mite 46 6 nhiém cua ngudn nude, trong nude thai c6 chia nhiéu hop chit hu co thi DO giim ding ké. Ham lugng oxi trong nurée sach vio khoang 5-6 mg/l, thip hon gid tri nay 1a nude bi 6 nhiém. 24.1.1. Nguyén tie xde dinh Dé xi dinh DO ngudi w thrimg ding phuong phip Winkler edn goi la phuong, phip iot. Phuong phip nay dya trén nguyén tic oxi tan trong nude oxi hod dinh bron, Mail) thanh MnO; trong méi tnrdmg kiém. Mn™ + 20H’ + 1/20; MnO; 4+ H.0 (24.1) MnO; tgo ra sé oxi hod I” gidi phéng ra 1; rong moi trrgmg axit MnO, + 4H" + 20 —> Mn®* +1, +2H,0 (242) (COng hai phuong trinh (24.1) va 24.2) ta duge 120; +20 +2H' 1) +H,0 1Luong I thodt ra tung duong véi lugng oxi hod tan trong nuéc. Chusin d lung I> thoat ra biing dung dich chudn Na,S,O, v6i chit chi thi hé tinh bot ta sé tinh dirge Luong Do 1, +2 NazS;0; > Na.S,0, +2Nal Dé dim bio dé chinh xc két qua phin tich, cdn chi ¥ may diém sau: ~ Trinh hap thy thém khéng khi vao nude trong qué trinh ly miu va bio quin mau, ~ Cin 6 dinh hrgng DO cé trong nude, trinh mat oxi trong qué trinh vin chuyén do Khuyéch tin va su thay déi nhiét 46 cing nhu sy di dong cia cde vi khuin hiéu khi co trong nude, bing cich cir 300 ml miu thém vao 0,7 ml H,SO, dic, 1 ml NaNO, va git o noti 161 voi nhigt d6 tir 0-5°C, ~ Trrée khi phan tich edn xir Ii miu dé loai trir anh huréng cla ede chit oxi hot (Fe™*, NO, ...) ¢6 kh niing oxi hod thinh I, Kim cho két qui phan tich eao hon gid tri thye va edie chat khir (Fe™, S*, SOs ...) c6 kha nding khir 1, thinh T lim cho két qua phin tich thip hom gif tri thye 24.1.2. Quy trinh phian tich Miu nude duge ly cdn thin that diy vao chai chuyén dung (goi ki chai BDD) © ‘dung tich 300 ml. Bé yén, thém ngay 1 ml dung dich MnSO, (chuan bi bing edch hod tan 100 gam MnSO,.4H,0 trong 200 ml mrde cat dun da s6i dé dudi hét oxy hod tan, néu dung dich vin van due thi loc) va 1 ml dung dich KI trong KOH (chun bi bing eich hod tan 100g KOH va S0g KI trong 200 mi mrde edt dé dun sOi). Khi thém nén ding pipet dé dda thude thir vio lop nuée stu trong chai Chai chia miu sau khi c6 dinh, nit chit va déc nguge xudi nhiéu Kin dé tron déu. é yén ti khi két ta MnO, King xuéng khodng nira chai. Thém Iml H2SO, dic va. 1 ml HaPO; dic (dé che Fe(II) ), day nit va dio tron vai lin wi khi két tia tan hét, Ly 100,0 ml dung dich cho vio binh nén dung tich 250 mi, thém khoing 5 giot dung dich chat chi thi hd tinh b6t, chun 49 bing dung dich chudn natri thiosunfat NazS:O,, ndng 46 C; (0,01 M) ti khi dung dich chuyén mau, hét V ml, 24.2. XACDINHNHUCAU OXY HOA HOC (COD- CHEMICAL OXYGEN DEMAND) 24.2.1.Nguyén tie Cie chit v6 co va hut co trong miu duge oxy hot bing K:CrO, trong dung dich H,SO, 50fe, ¢6 xtic tic Ag:SO, khi dun boi lu miu nue. Anh hung cua Cl duge loai wir biing HgSO,. Luong dur K-Cr.0; durge chun 46 bing dung dich chudin amoni sit (11) 78sunfat, sir dung ehi thi feroin (phite Fe(1)-0. phenantrotin) hoje chi thi diphenyl amoni sunfonat (dung dich chuyén tirtim dé sang xanh tim), Két qua COD kh6ng mé ta quan hé voi BOD (nhu cau oxy sinh hod) cla nude thai hoje véri ting him Iugng ede bon hit eo (TOC), Phuong phip nay c6 thé img dung xée dinh COD trong miu nude thai cdng nghigp vi my phim cé ham lugng cde bon hitu co én hon 50 mg/l. Déi voi nhing mu c6 ham lurong cde bon thip nhur nhiing miu nude thai bé mat edn sir dung phuong phap phin tich COD ning dé thip. 24.2.2. Léy miu vie bio quin Miu duge lay vo chai thuy tinh (trudng hop khong c6 chat hiru co 66 thé chai nhya) sau d6 axit hod miu bing axit sunfuric dén pH <2 va gitt 64°C dén khi phiin tick, 24.2.3. Quy trinh pha tich Lay 50,0 ml miu can phan tich (hoc rong miu it hon thi pha loding dén 50 ml bing nude cat) vao binh céu 1 cd dung tich 250 ml dé dun hdi luu, thém 1 g HgSO,, vai vién da bot. Thém 5 ml H,SO, dic, lic manh dén khi HgSO, tan hét. Dat binh ciu vio bit c6 da va thém chim (déng thé lic manh) 25 ml K,Cr,0; ndng 46 C, (0,005 M). Sau do thém 5 ml dung dich Ag,SO, 5 % pha trong H2SO, vio binh edu 43 duge lim lanh, lic déu. Lip sinh hin hdi uu va dun hdi lun trong 2h (voi mt sé miu nude thai 6 thé rit ‘ngdin thei gian). é ngudi binh cdu va ira sinh hin biing 25 ml nude cdt, Néu ding binh cdu day trén cdin chuyén dung dich vao binh nén 250 ml, nira binh cdu 3-4 Lin bing mrde edt va dé ngudi dung dich dén nbigt db phng. Thém 8-10 giot dung dich chi thi ferroin vio dung dich va chuain dO K,Cr.0, dur bing dung dich chudn Fe(II) 0,025 M dén khi dung dich chuyén tirmau xanh li edy sang hoi dé hét Vm Cin tién hanh phép phan tich wi miu tréing wrong ty nhur tén. 24.3. TINH TOAN KET QUA Sinh vign ty thiét lip cdng thie tinh him Ivgng DO, COD trong miu phan tich (mg/l) 24.4. HOA CHAT ~ Dung dich feroin: Hod tan 1,48g 1,10 phenantrolin v6i 0,70 g FeSO,.7 H.0 trong 100 ml H.0 + H3S0, loing miu vio 79~ Dung dich NasS.05, I; Fe(ID), K.Cr.0, ding dé chudn a chua e6 néng d6 chinh xe; dung dich chat chi thi hé tinh bét. - Clic hod chit céin thiét khdc, sinh vién ty pha tir tinh thé MnSO,.4H,0, KOH, KI, SO, dic, HyPO, dic, AgsSO,, HgSO. BAI 25. PHAN TICH MOT SO CHi TIEU HOA HOC CUA NUOC BE MAT. 25.1, XAC DINH HAM LUQNG SO,” Nguyén tie: Trong mi trudng cd pH= 5-6, tién hinh két tila SO,” dudi dang BaSO,. Loe ria két tia va hod tan két tia bing lugng dur chinh x4e dung dich chun EDTA trong mdi trudmg NH, (pH=11) sau dé chun d9 lung EDTA dur bing dung dich chun MgC véi chit chi thi ETOO, Cach tién hank: Liy 50 ml miu nude cin phan tich (43 duge loc trong) vao ede chiu nhigt e& 250 ml, thém 4-5 gigt dung dich HCI 1:5 dé dung dich e6 pH =5-6. Bat ede len bép dign, dun nong 80-90 °C (trinh s6i), thém 10-15 ml dung dich BaCl, 10%, khudy déu dung dich trong khoding 5 phit dé phan img két tia xy ma hon ton, BE yén 45 phi dé lam mudi két ta. Loc gan két tia qua gidy loc bing xanh, rita két tia bing nude edt nong én hét ion Cl. Chuyén két tia vio cde 250 ml, thém 10 ml NH; dic, 25 ml dung dich chuin EDTA néng dC, (khoing 0,02M), 10 mi dém_amoni! amoniac pH=10, mot it chit chi thi ETOO, dung dich cé miu xanh biée. Chuin d6- EDTA du bing dung dich chun Zn’ (C,) dén khi dung dich c6 mau dé nho, hét Vml. 25.2, XAC DINH HAM LUONG HS. Nguyén tiie: Cho lugng dur Ly dé oxi hod HbS, sau d6 ding dung dich chuiin Na;S;05 dé cchudin d9 luong Is du HS + bh > S + 2HI 2NayS:Os + Ip > 2Nal_ + NasS.Ox ‘Cach tién hanh: Lay 50 ml miu nude can phin tich cho vao binh nén dung tich 250 mil. Thém chinh xée 10 ml dung dich chun I> (ndng 4 khodng 0,025M) vio binh nén, diy kin, lic déu. Dé yén vai phit, lay ra chuain 46 bing dung dich chuin Na,S,0, ning a6 C; dén khi cO miu ving nhgt, thém 1 mi hé tinh bot, dung dich 6 miu xanh va tiép tuc chudin dO bing dung dich chudin Na,$,, dén khi mit miu xanh va tré lai miu sic cia miu nude ban di, hét V2 ml. 25.3, XAC DINH HAM LUONG CI’ (THEO PHUONG PHAP MOHR) 80Nguyén tie: Ding dung dich chun AgNO, chuin 49 Cle trong miu véi chit chi thi K,CrO, dén khi két tia chuyén tir tring sang dé ndu. Lung Kin S* c6 trong miu can tro phép xde dinh sé durge loai tir bing dung dich Zn™* Ag’ + Cl AgCl 2Ag’ + CrO," > Ag.CrO, Cich tiém hnh: Hit 50,0 ml miu nude edn phan tich vio binh nén dung tich 250 ml, thém 2 giot dung dich chat chi thi phenolphtalein, néu thay dung dich c6 mau dé thi thém vai giot dung dich H;SO, 10 % dén khi mit miu. Néu miu phan tich khong c6 miu thi thém NaOH dén khi co miu hoi hdng réi méi cho H2SO, nh trén. Nhu vay, dung dich co pH=6-7. Thém 5 ml dung dich Zn(NO,); 5 % va loc bo két tia ZnS. Rita sach két tha bing nurée néng, thém 1-2 ml dung dich K3CrO, 5% va ding dung dich chun AgNO; (Cy) chudn 49 dén khi dung dich xuat hign két tia do gach, hét Vom. 25.4. XACDINH DQ AXIT D6 axit lA Luong axit trong nude cé phan img trung hoa voi bazo theo chit chi thi phenolphtalein, duge tinh bing sé mili duong lugng H* c6 trong 1 lit made. - Ly 50 mi miu nurée vio binh non dung tich 250 mil, thém 2-3 giot dung dich chit chi thi phenolphtalein 0,1 % va chudn 46 biing dung dich chun NaOH nong 49 C. én khi xuat hién miu hong nhat, hét Vaml. 25.5. XAC BINH BQ KIEM DO kiém ca nube ding dé chi tng him lugng cae ion OH’, CO;?, HCOy va cde Joai mudi cia axit yéu c6 trong nude. Tuy nhién, trong nue théng thuimg chu yéu chi cb HCO; va CO; nén téng s6 mili duong lugng 2 chit nay goi Li dé kiém, Ding HCI dé chuiin d6 cae ion trén voi hai chit chi thi phenolphtalein va metyldacam ta tim duge sé miliduong long ting e@ng. - Lay 50 ml miu. nude can phan tich vao binh nén dung tich 250 mi, thém 2-3 gigt dung dich chat chi thi phenolphtalein 0,1 %. Néu dung dich e6 miu dé thi ding dung dich chun HCI cé ndng 46 C; dé chun d6 dén khi dung dich mit mau. Sau khi chudn 4 xong_ lin 1 hodc nhd phenolphtalein ma dung dich khong c6 mau thi nhé tiép 3 giot dung di metyl da cam va chudin d6 lin thir hai dén khi dung dich chuyén sang miu dd, hét V5 ml 25.6. XAC BINH DO CUNG Nurée tur nhién c6 chita cic loai mudi HCOs’, CI, $0.2 eita cdc kim logi canxi va magié. Nude c6 chira it mudi canxi va magié goi 1a mde mém, nude chia nhiéu m canxi vi magié goi la nube cimg. Cé miy loai 46 cimg sau: 81= cimg tam thi: phy thude vio him long cde mudi Ca(HCO,)> va Mg(HCO,), tan trong nurée. Khi dun si, hai mudi nay chuyén thinh CaCO, va MgCO, vi gil phng CO,, khi dé nuée mit hin d eimg tam thi. - Dé cig vinh citu: tuy thude vao lugng cde mudi sunfat va clorua cia canxi va magi. D9 cuing niy khong thay dai khi dun néng. - Dé cing todn phan la tong 49 cimg tam thdi va dO cimg vinh ciru. Khi phan ich nude, 49 cimg toan phin va dO cimg tam thoi duge xde dinh mre tiép bing thi nghiém, sau d6 suy ra dO cig vinh ciru. DS eimg toin phin va dO cig tam thoi dupe tinh bing sé mg CaCO, ¢6 trong 1 lit mrée. Miu nue dé phan tich 46 cig phai tho min ede yéu cdu sau + Khong cé mau va chit lo limg (néu ¢6, phai loc va pha lofing) + Khdng o6 phiin img kiém voi phenolphtalein (néu c6 phai tung hoa bing HCl) + Khong c6 ion sit. Xée dinh 49 cig ton phan (theo phurong phap complexon) Nguyén tie: Phuong phip dia trén sy tao phire cla Ca** va Mg"* voi EDTA trong mdi tru’ng dém amoniac ¢6 pH = 11, sir dung chat chi thi ETOO. Néu him lirong Mg”* trong miu nhd edn thém vio miu lrong nhy MgY? odie pha nd vio dung dich dém. Cée ion Fe™*, Cu, Ni**... can tro phép chuiin 49 vi ching tgo phire bén voi EDTA va ETOO nén phai duye che truée khi chudn d@ bing CN hoiic S® Cach tién hinh : Lay 50,0 ml miu nude, thém 10 ml dung dich dém NH,"-NH, ¢6 pH=10 (néu d6 kiém cia miu nude lon, cin thém HCI 0,1 M dé diéu chinh vé pH = 7-8 sau db mdi thém dung dich dém), thém chat chi thi ETOO, dung dich c6 miu dé nho. Diing dung dich chuin EDTA e6 néng d9 C, dé chun d6 dén khi dung dich chuyén sang miu xanh biéc, hét Vor. ‘Cha J: Néu sir chuyén miu khOng rd ring, tie 14 tong dung dich e6 mit ede ion tién hinh chudn dé lai miu nude khdc biing cach thém vai gigt dung dich dung %, sau do thém chat chi thi va tién anh chudin dg nhur trén, Xie dinh 49 cdg tam thai: Nguyén tiie: Ding dung dich HCI chuiin d} HCOs, sau d6 dun s6i lung murée Khe trong thoi gian nat dinh dé logi bo d6 eting tam thoi vi chun dO lai dung dich di loe va tinh todin so sinh dé tim dp eimg tam this Chi ¥: Cach lam nay logi bd anh hutmg cia mudi hidro cdcbonat cla Fe, Na. K.. dén dd cig tam thd,Cieh tién hanh: ~ Truimg hyp 1: Nude e6 pH < 84 (nbd phenolphtalein vio duge dung dich khong mau) Hit 50,0 mi mau vao binh nén dung tich 250 mi, thém 2-3 giot dung dich chat chi thj metyl dacam. Ding dung dich chuin HCI ning d@ C; dé chuiin 46 dén khi dung dich ‘6 miu hng hét V; ml. Hat 100,0 ml miu nude khée vio cbc chiu nhigt e& 250 ml, dun s6i 30-60 phat. Trong qui tinh dun phi them nude edt dé git' thé tich dung dich khong déi. Bé ngudi va loc qua gidy loc dinh tinh Kho (bo di 15-20 ml diu tién) vio binh nén dung tich 250 ml Hit 100 ml dung dich da lpe vio binh nén dung tich 250 ml va nho vai giot dung metyl dacam, ding HCL néng dé C; chudn a6 dén khi c6 miu ving, hét Vs ml = Truimg hop 2: Nuve e6 pH > 8,4 (nho phenolphtalein vao, dung dich e6 miu 40), khi 6 miu phin tich c6 mudi cacbonat cua kim loai kiém. Hit 50,0 ml mau vao binh nén dung tich 250 mi, thém 2-3 giot dung dich chat chi thi phenolphtalein, Ding dung dich chuin HCI (Cs) dé chudn 46 dén khi dung dich mit mau hing, hét Vo ml. Thém tiép 3 giot dung dich metyl da cam va tiép me chuin dé bing HCI dén khi cé miu do ving, hét V,q ml, - Trutmg hop 3: (Nhd phenolphtalein vio, nude chura dun s6i da e6 miu dd, eng dun cing dé thim), khi dé dung dich cé chia ca mudi CO,? va HCOs, cach tién hinh nhur sau: - Lim thi nghigm nbutrutmg hop 2 dé xie dinh Vs va Vio - Lim thi nghigm nhurtruing hop 4 dé xie dinh V, va V, ~ Truimg hop 4 : (Nho phenolphtalein vdo, dun sOi 5-7 phat, dung dich mi c6 miu d6, Tarimg hop nay dung dich e6 NaHCO, va KHCO,...) Hit 50,0 ml miu vio binh nén dung tich 250 ml, thém 2-3 gigt dung dich chit chi thi metyl dacam. Ding dung dich chun HCI (Cs) dé chuin 46 dén khi dung dich e6 miu hdng, hét V,, ml. Hit 50,0 ml mu khée vao binh nén dung tich 250 mi va cho mot lung NaOH 0,05 M biing Iugng HC! da tiéu tn 6 trén, dun dung dich vira dén s6i thi loc nhanh, thém 3 giot dung dich metyl dacam vio nurée Ie va chudin 46 bing HCI dén mau a6 vang, hét Vom 7. XAC DINH HAM LUQNG Ca? ach tién hank: Lay 100 ml miu nude cho vio céc chiu nhiét c& 250 ml, thém 3 giot metyl da cam, Ding dita thuy tinh khudy déu, cho tir tr HCI (1:10) dén khi dung dich ©miu d6. Bun gin s6i dung dich va thém 10 ml NH,CI 10 % va iép tue khudy déu, Sau dé, thém 15 ml (NH,)C;O, 5 % vio dung dich va dé yén 15 phut. Thém vai giot dung dich NH; 25 % dén khi cé miu ving. Liy cdc ma khoi bép dé yén 1 gids dé kim mudi két tha. Loe két tia qua gidy loc bing xanh. Rima két tha biing (NH.)2C20, bio hoa sau 46 ria lai bing nuve edt dén sach ion C0," (thir lai bing dung dich AgNO). Ding 25 ml H)SO, (1:5) dé hoa tan két tia trén gily loc vao binh nbn dung tich 250. ml. Dun néng dén 80°C va chun d6 Iuong H.C.0, sinh ra bing dung dich chuin KMnO, (Co) dén khi xuat hign miu héng, hét V5 ml. 25.8. TINH TOAN KET QUA Sinh vién ty thiét lip cong thie tinh him long (mg/l) cae dai lugng cain xc dinh trong bi 25.9. HOA CHAT ~ Miu nude song ding dé thi nghiém, méi mot miu 500 ml - Cae dung dich ding dé chuan 49 chura c6 ning d6 chinh xéc: Mg”*, Zn™, Na;S203, 1, AgNOs, HCL ~ Cée chit chi thi ETOO, phenolphtalein, metyl da eam, K:CrO,, hé tinh bot. - Cae hod chit cén thiét khéc, sinh vién ty pha tir dung dich NH, dic, tinh thé NH,Cl, NaHY .2H,O, NaOH vign, KCN riin/, CHUONG 9 PHAN TICH THUC PHAM Phan tich thye phim c6 die diém rigng la ede miu it e6 tinh de hai cao nhur ede mmdlu phin ich moi trurmg va eng nghigp inrée day, my nhién, ede miu thuimg phite tap, can phai xir ly miu cing nhiéu qua giai dogn. Ching ta sé dé cp trong chuong, niy cic miu nude mim, dung, rugu va mudi iot...Céic eng vige cia phép phan tich bao gdm: pha miu, tach loai tap chat va cudi cing 1a phin tich thé tich, nén BAI 26 PHAN H MOT SO CHi TIEU HOA HOC CUANUOC MAM * Nude mim li sain phim cita sy thuy phén ty nhién thit cia cd boi cde men. chit dam proteaza cla cd va cde vi sinh vat c6 trong cd trong mdi tu’ng mudi dim dic. u hod 84Dua trén qui trinh san xudt nude mim, thit cia c4 06 thé thuy phin thinh nude mim t6t chira cdc chit dam hod tan hogic nude mim hong chira cde chit dam xdu, NH,... do dd in kiém ngbiém: «Hm hong axit qui v8 axit exec; - Him lurgng mudi NaCl; ~ Ham lurgng N tedin phiin va - Ham lurgng N-foemon. 26.1, CHUAN BI MAU Lic ky chai nue mim, loc qua gidy loc véo binh sach, kh. Hit chink xéc V ml (khoang 10 ml) nude mim di loc va chuyén vao binh dung mite 100 ml. Thém nude cat én vach, lie déu, durge dung dich A. 26.2. QUI TRINH PHAN TICH (THEO TCVN 1520-74) 26.2.1. Xée dinh d axit trong nwitc mim (tinh theo CH;COOH) Ly 10,0 mi dung dich A vio binh nén dung tich 250 ml , thém nude cit dén thé tich gip doi, thém 3 giot dung dich dung dich chit chi thi phenolphtalein vi chuan 46 bing. dung dich chuin NaOH ndng 46 C; (0,02M) dén xuit hign mau hing hét V, ml. (26.2.2. Xée dinh him legng mudi NaCt Ly chinh xée 1,0 ml dung dich A vao binh nén dung tich 250 ml, thém khodng 20 ml nurdc cat, 5 giot dung dich phenolphtalein. Néu dung dich khong co miu héng thi ding NaHCO, 5% thém timg giot dung dich cho tsi khi xuit hign miu hing, sau d6 thém timg gigt dung dich CH,COOH 5% diéu chinh cho t6i khi mit mau hing. Thém vio binh non dung tich 10 giot dung dich chat chi thi K;CrO, 10% va chudn 49 bing dung dich chudn AgNO; c6 ndng 46 C; t6i khi xuat hién mau dé nau, hét V2 ml, 26.2.3. Xée dinh him legng N-focmon trong nwitc mim (Cac axit amin c6 moi trudng gin nhu trung tinh. Khi giip focmon, nhom— NH; két hyp v6i focmon thanh nhém metylenic -N=CH; lim mit tinh chit kiém va hop chét khi 46 c6 tinh axit, do dé c6 thé dinh Ingng bing dung dich chun NaOH véi chat chi thi phenolphtalein R-CH-COOH +HCHO +R-CH-COOH +H,0 NH: N=CH; 85(Chi y: - Cée mudi amoni khi e6 mit foemon c6 phan img thinh hexametylen tetramin vi HCI, do d6 him lrgng N xée dinh theo phuong phip nay N- amin axit vi NHL. 4NH,CI+ 6 CHO — (CH2),Ni +4 HCI +6 HO - Diém tuong dirong qui trinh chudn d6 két thie 6 pH 46 dén khi phenolphtalein c6 mau d6 tuoi, ~ Néu trong miu c6 mudi photphat hoc cacbonat thi trong qué trinh chudin 49. nhiing mu6i nay tgo thainh dung dich dém va pH khé ting én dén 9 dé chuyén miu. Do 46 cn loai trirchting biing cach két tia voi BaCl, va Ba(OH); Céich tién hanh: Lay chinh xiie 25,0 ml dung dich A vio binh dinh muie 100 mi, thém 10 ml dung dich BaCl, 30%, 1 ml NaOH 6 M, thém nude edt dén vach va lie déu. Dé yén 15 phit rdi loc qua gidy loc bing xanh vio binh nén dung tich khd sach duge dung dich B. Hit chinh xe 10.0 ml dung dich B vira loc vio binh nén dung tich 250 ml khie, thém 10 giot dung dich chat chi thi hén hop (bromthimol xanh- phenolphtalein), ding dung dich HCL 0,05 M trung hod dén khi dung dich chuyén tir miu tim sang miu xanh ‘nhur miu eta dung dich tiéu chun pl Thém vio binh nén via chudn 49 6 trén 10 ml dung dich fooemon trung tinh, dung dich lai c6 miu ving, lic déu va dé yén 5 phit. Ding dung dich chuin NaOH 6 ning 4 C (0,02 M) chudin 46 cho ti khi dung dich chuyén tir miu yang sang mau xanh rdi xanh tim giéng mau cla dung dich chudn c6 pH =9,2,, hét V5 ml, 26.2.4, Xée dinh ham heong N toan phin “*Nguyén tic: VO co hod miu mrée mim biing H2SO, dic dé chuyén cde dang ton tai iia N thanh (NH,)SQ«, thay doi mdi tnrdmg dé giai phong NH bing phuong phap cat dam Idi cuén hoi nue. Hip thy khi NH; sinh ra bing trong dur chinh xc dung dich chudn H,SO, va chudn a6 lugng axit durbiing NaOH. Céich tién hanh: ~ Hat chinh xae 2 ml miu nude mim edn phan tich vio binh Kendan dung tich 100 mi, thém vao 46 3-4 g hin hyp xtic tic CuSOy- K2SO, (theo ty 1é khdi lurgng 1:3). Rot tir tir theo thanh binh Kendan dén hét 5 ml H:SO, dic, lic déu dé thim déu miu (trdnh dé miu dinh lén thinh binh), day binh bing phéu thuy tinh va Kip binh vao gid d& sao cho binh nghiéng 45 °, Dat binh trén bép dign vi dun néng dé v6 co hod miu dén khi dung -9,5 do db phai chun 86dich trong binh trong va c6 miu hoi xanh Li duoe (nguoe Iai, edn Hy ra khOi ngugi, thém vai gigt HO, die va tiép tye v6 co hod miu cho dat yéu ciu), ~ Sau khi v6 cor ho’, chuyén dung dich trong binh Kendal vio binh dinh mire 100 ml, thém nude edt dén vach mite, lie déu. Lay chinh xe 10,0 ml vita dinh mite vao binh edu cat bp oft Kendal, thém vai giot dung dich chit chi thi phenolpbtalein, Bay nit eb phéu tich, éng lam lanh thu hdi va dng thuy tinh dé sue hoi vao binh cdu. Bat phia cudi ng im lanh cée thu hdi dumg 30 ml H,SO; 0,05 M c6 vai giot dung dich chit chi thi metyl do. Kiém tra d6 kin cia hé théng va rot dung dich NaOH 33% qua phéu tich cia binh cit NH; dén khi dung dich cé mau hing, thém du 10 ml nifa. ‘Cho nuée lanh chay vao dng sinh hin va tién hanh edt 16i cuén trong 30 phuit ké tir khi nude bit dau sdi, sau d6, ha cbc himg xudng, cho dich cat chay lén gidy qui do, néu gidy qui khong chuyén mau thi xem nhur qué trinh cat da xong. ~ Ding binh cu tia rim dau dng sinh han, ldy céc himg ra, thém vai gigt dung dich chit chi thi metyl 40 va chuin d@ axit dur biing dung dich chudin NaOH c6 néng dC, dén khi chat chi thj déi miu tir do sang vang, hét V, ml, 26.3. TINH TOAN KET QUA Sinh vign ty thiét Ip céng thie tinh 49 chua, him lrgng NaCl, N- focmon, N- ton phan (g/) c6 trong miu nude mim ban div. 26.4. HOA CHAT VA DUNG CU. ~ Miu phan tich :méi sinh mot chai mau nude mim 250 ml, ~ Dung dich dém natri tetraborat 0, OSM, pH = 9,2: Can 12,367 g natri tetraborat, cho vio binh dung tich 1 lit, thém tiép vao 46 100 ml NaOH 0,1 M, dé nude cat dén vach lie dé. - Dung dich dgm photphat ( KH,PO, + NasHPO, ), pH = 7: Ten 60 ml dung dich NaHPO, 1/15 M véi 40 ml dung dich KH3PO, 1/15 M. - Dung dich AgNO, dung dich HCI, dung dich NaOH ding dé chudn d. Sinh vign ty xe dinh nding a6. ~ Hin hop chit chi thi: thn 5 thé tich bromthimol xanh 0,05 % trong etanol 60 % \v5i 4 thé tich phenolphtalein 0,5 % trong etanol 60%, - Chit chi thi K,CrO, 10% , phenolphtalein 0,1% trong etanol 60%. ~ Hin hop xie tée: cho 1 gam CuSO,5H.0 vio e6i str, thém 3 gam K,SOg, tron eu. ép, dé 87~ Cae hod chit cdn thiét khic, sinh vin ty pha ti tinh thé NaHCO, NaOH, dung dich H,SO, die -May fit dam theo phong phdp 10i cuén hoi nude nhu hinh dudi. 1 Binh cat hoi murée 5. Phéu nap miu 2- Khoa phéu nap nurée edit 6- Khod nap miu 3- Binh chia dung dich xa 7. Sinh han 4- Khoa xi nue nia 8- Binh chim miu phan tich Hinh 5 May cit dam ‘Vin hinh may edt dam nhur sau: un s6i nude trong binh tao hoi nude (1), mer nude vao dng sinh han (7). Sau d6 cho 10 ml miu da vo co hoa qua phéu (5) va khodi (6)vao binh cat (8), them NaOH (sau khi da dong cae khod (2,4); trang phéu bing nude cat, dong khod (6) lai Hoi nude tir binh (1) sue qua binh (8) va kéo theo NH sang sinh hain (7), diy NH durge ngung ty va chay sang cde hip thy (9). Qué trinh edt két thic trong khoang 15 phitt Sau khi di Lay cde hip thu (9) 4é chuan 46 lugng axit con dur, dong khod phéu (2, 6) ding thoi mé khod (4), dung dich sé chuyén tir binh ct (8) sang binh xa (3) thodt ra got. Thi nghigm xong phai rim sach my edt dam mét lin bing dung dich HCI lodng vi nhiéu lin bing nube. C6 thé ding dau nhon cia qua bop cao su lip vao cuéng phéu 5, mér khod (6) va (4), dong khod (2) sau d6 nhe ning ding khong khi day nhe dung dich tir binh 8 ra ngoai 88BAI 27: PHAN TICH HAM LUQNG CAC LOAI DUONG TRONG SUA DAC CO DUGNG 27.1, NGUYEN TAC PHUONG PHAP PHAN TICH * Neuyén tic phan tich gluxit 7 Gluxit 1a nhimg hop chat hiru co trong phin tir cd C, H, O két hop voi nhau trong d6 e6 nhiéu nhém OH vi 1 nhim CHO hay C=O. J ‘Vé phurong dign héa hoe, gluxit c6 thé chia thinh 2 nhém: ~ Nhém ‘oza’ (duéng khit) gdm cic loai during trye tigp khir oxy do cé nhom andehit hay xeton tyr do trong phin tir nhur glucoza, fructoza, lactoza. - Nhom ‘ozit’, khong khir tnrc tiép oxy vi cde nhom andehit va xéton 6 dang két hyp i cde nhOm chite khiéc, khi thay phan cho nhiéu oza nbur tink bot, sacaraza, Dinh Iurong lactoza va sacaroza trong sta die ¢6 duimg: Lactaza la dutmg tre tiép khir oxy nén dinh lugng trye tiép bing phuong phép iot, cbn duimg sacaroza phai thuy phan thinh glucoza vi fructoza trong mdi tug HCL IM & nhiét dd 68-70 ° C trong thi gian tdi da 7 phuit. Do dé bing ciich dinh long dung true vi sau khi thuy phan s® tim duge him lurgng lactoza vii sacaroza, ~ Thém vio miu sita chia lactoza hoje dung dich sau khi thuy phan sacearoza: dung, dich Felling A (CuSO.) va Felling B (kali natri tatrat trong m6i tnréng kiém), dun nong_ nhe: (CuSO, + 2 NaOH —> Cu(OH)s + NasSO, HO - CH ~COONa 0.CH-COONa WOH), + | sat | HO ~ CH. COOK (0 CHCOOK }CH.COONa HO -CH-COONa Rco+a Z| RCO CHOH2HOF — | ‘0-CH-COONa HO-CH-COoK Thém vio dung dich con néng lung dir HCI loding dé hod tan Cu,O, sau 4 loai HCI dur biing NaHCO, va chuan 4 mudi Cu(1) sinh ra bing 1, Cu,0 + 2HCI—> Cu,Cl, + H,0 1,+2Cu' 21+ Cur Luong I; dur durge chudn 46 bing dung dich chuin Na,$.O, voi chit chi thi hé tinh bot. 8927.2, CHUAN BI MAU Can 10 gam sita de 6 duémg trong chén edn va hod tan vio mot it nude néng, 8 vio binh dinh mite 100 ml. Ria chén vi mt ft nuée néng, mrée rim din tit e& vio) binh din mie. Cho nurée cit ngudi dén khodng ba phan tr binh, lic déu, thém 5 ml dung dich kali feroxianua K,{Fe(CN)q] 15%, $ ml dung dich kém axetat Zn(CHsCOO): 30 % dé khir tap chat, lc manh déu, kim ngudi binh dudi voi nude chiy va din mic thanh 100. mi. Lic déu va loc qua gidly loc bang do vao binh nén dung tich khd, sach. Hit chinh xic 10 ml_ nude loc cho vio binh dinh mite 100 ml va dinh mie dén vach duge dung dich A, 27.3, QUY TRINH PHAN TICH 27.3.1. Dinh licong dwing lactoza Hat 25,0 ml dung dich A, thém 10 ml dung dich Felling A, 10 ml Felling B, dung dich c6 mau xanh thim, Bun trén ngon hit nhe ¢6 luéri amiang nhumg sau 3 phit phai s6i, gidt dung dich si nhe trong 2 phi, khi d6 trong binh phan img c6 xuat hién két tia dé gach. Lay dung dich ra, thém ngay 10 ml HCI 10% (dur) dé hod tan CuO, dung dich e6 miu ving, BO vio dung dich mau gidy qui tim, thém tir tir ting gigt dung dich NaHCO, 5 % dén khi qui tim c6 mau xanh nhat. Bé ngudi, thém luong dur chinh xde dung dich chun 1, (khoaing 25 ml, néng 46 0,02 M), ban dau c6 két tiia tring sau d6 tan thinh dung dich mau do nau. Dé yén 5 phiit va chudin dé 1, dur biing dung dich chuiin Na;S,O; én khi dung dich c6 miu ving rom, thém tip chit chi thi hd tinh bt va tiép me chudn 49 dén khi dung dich c huyén tir miu xanh thim sang mau xanh nbgt 27.3.2, Dinh long ducing sacaroza iy 10,0 ml dung dich A vio binh nén dung tich 250 ml c6 nit, thém 5 ml dung dich HCl 4M. Dit binh vio ndi cdch thuy (nude di dun néng dén 75 °C), sau 2 phiit dung dich dem thuy phin phii dat 68 °C, gitr & nbigt dO ndy trong 5 phil, Lam ngudi nhanh ching dudi vdi nude chiy. Trung hod dung dich, truée tién bing NaQH 20 %, sau 46, bing NaOH 2 %, véi chit chi thi 1a phenolphtalein. Lim ngu@i dén nhiét phong, thém dung dich Felling A, B va tién hanh tuong ty nhu qui trinh én, Néu him lugng sacaraza ign thi phai tng lung 12 dén du. 27.4. TINH TOAN KET QUA Sinh vién ty thiét lip cng thire tinh him lugng 2 logi dug (g/kg) trong miu sia ic e6 dutmg cho tnrée. 27.5. HOA CHAT ~ Miu sita die 06 during, 90- Dung dich Felling A: 68,28 g CuSO,.5H,0 pha thinh 1000 mi - Dung dich Felling B: 346 g Kali Natri tatrat, 100 g NaOH vién va pha thanh 1000 ml biing nude edt, ~ Dung dich chudn cha cé néng dO chinh xdc: Na,S,0. Chit chi thi phenolphtalein ~ Cie hod chit edn Khde, sinh vién ty pha tir tinh thé K,[Fe(CN)«l. Za(CHsCOO)> , CuSOg .5H3O, kali natritatrat, NaOH vién, NaHCO, BAI28 PHAN TICH MOT SO CHI TIEU HOA HQC CUA CHAT BEO 28.1. XAC DINH CHI SO AXIT Chi sé axit 1a sé mg KOH edn dé trang hoa cde axit béo ty do e6 trong 1 gam chit béo. 28.1.1 Nguyén ti ‘Trung hoa axit ty do cé trong cht béo bing dung dich chuin KOH: RCOOH + KOH > RCOOK + H,0 28.1.2 Cich tién hiinh Ly vio binh nén sach, khd, dung tich 250 mi lung chinh xe khoding 1-2 gam chit béo (miu dau thye vat). Thém vao 46 20- 20 ml hon hyp éte- rugu (ty 18 1:1) dé hoa tan chit béo. Liie can than, néu chit béo vin chua tan hét, e6 thé dun nhe trén ndi eéich thuy, lic déu. Lam ngudi va chun 49 hén hop biing dung dich chudn KOH trong rugu co ning 49 C, (MII) (khoding 0,05 M), voi chat chi thi phenolphtalein dén khi xuat hién- miu hing. Ghi thé tich dung dich chudn KOH tiéu tn, V, ml. (Chay: Khong pha KOH trong nue dé trinh phan img x4 phong hod chit béo. 28.2. XAC DINH CH SO XA PHONG (Chi sé x phong 1 lung mg KOH edn dé trung hoa ede axit béo ty do eding nhur lién két c6 trong 1 gam chat béo, hay ndi cdch khdc, la lugng KOH can dé xa phong hod cde glixerit cing nhur edn dé trung hod cdc axit béo ty do trong 1 gam chit béo. 28.2.1. Nguyén tie ‘Dun s6i chit béo. voi lugng dur dung dich chun KOH thi chat béo bi thuy phin: CH,OCOR, qikoH GHOCOR: +310 + CHOH +R,OOH+R:COOH + R,COOH CH,OCOR, CHO Cac axit béo durge gid phing ra phan img voi KOH: oORCOOH + KOH > RCOOK + #0 Luong kiém dur khong phan img véi cde axit béo duge chudin a6 bing dung dich cchuin HCI 28.2.2 Cich tién inh Lay vao binh cdu 1 cé dung tich 250 ml, mét lugng chinh xdc kho’ing 0,5-1 gam chit béo. Ding pipet hode buret thém vao binh cdu 25 ml KOH (ndng dd khoang 0,05 M), diy binh bing nét cé Sng sinh han khi va dun cach thuy trong khoding 1 gio. Sau khi xa phong hod xong, Lim ngudi hdn bgp, thém chit chi thi phenolphtalein va chudin 46 rong, KOH dur bing dung dich chuin HCl c6 ning d6 C, (MII) (khoaing 0,05M), hét V2 ml. Cin tién hanh lam thi nghiém tring bing mot long nude cdt tuong img dé higu chinh két qua. 28.3. XAC DINH CHI SO ESTE Chi sé este 1 sé mg KOH edn dé x phong hod cée glixerit c6 trong 1 gam chit béo. Né Li higu sé gitta chi sé xa phong va chi sé axit, 28.4. XAC DINH CHI SO 10T Chi sé idt fi sé gam idt két hop voi 100 gam chat béo (do céc lién két ddi chura thio hot ciia ede axit béo khong no cé kha niing phin img dng hyp véi I> hog ede halogen kbc), C63 phong phip xc dinh chi sé idt: - Phuong phap: Wijs ding thudc thir 1a ménoclorua idt ~ Phuong phap: Hanus ding thuée thir 1a bromua idt. - Phuong phap Hubl ding thud thirla idt véi chit xtc téc li HeCh. Neguyén tic chung cita 3 phuong phép nay 1a cho chat béo hoa tan trong dung mdi khong nude tiép xtc véi thude thir 6 ché t6i trong mt thdi gian can thiét, Phin thude thir thita (phi bing nima long cho vio) sé két hop véi KI va gidi phong ra 1, tyr do, sau do duge chun 46 bing dung dich chudn Na,S.0,, * Ciich tién hanh : (theo phurong phip Wijs) {dt cloria duye tao thinh theo phan img: 2 KI+KIO, + 6HCI> 3 CIL+3KC1+3 0 Cl.e6 phin ting cOng hop vio ede lién két doi chua no eta axit béo, Lugng Cll dur duge xc dinh bing dung dich chudn Na;S2Os, Ly chinh xée vio binh nn nit mai dung tich 250 ml, khong 0,5 gam (3-7 got diu thye vat), Thém 5 ml éte etylic vao binh dé hoa tan chat béo, sau dé thém tiép 25 ml dung dich clorua iét trong HC10,2 M. Lic déu, day kin binh va dé yén 15 phit Tiép 46,thém 10 ml dung dich KI 10 %, 50 ml nue eft. Chuan d6 lung Is gia phing ma bing dung dich chun Na,S,0, 0,05 M dén khi xudt hién miu vang rom. Sau dé, thém 1 ml dung dich chit chi thi hé tinh bot 1 %, 3 ml cloroform (dé giai phong 12 hap thy én chit béo) va chuin 49 tiép dén khi dung dich bj mit mau hoan toan, hét V, ml. Lam thi nghiém trong ty véi mau tring. 28.5. XAC DINH CHI SO PEOXIT Chi sé peoxit 14 sé gam 1; cé thé phan img véi hidro hoat dng cla cde peoxit cd chira trong 100 gam chat béo, ndi eich khée, chi s6 peoxit li sé gam i6t duge giai phing, ra khi cho dung dich KI tic dung véi 100 gam chit béo nhi tic dung cia cde peoxit co trong chit béo. 28.5.1. Nguyén tie : ‘Cae peoxit (tao thinh trong qui trinh di cla chit béo) trong méi tnrémg axit c kha ning phan img v6i KI gidi phing ra Is theo phan tmg sau: RCH CH: Ry CHS CHR, 0-0 +2KI+2CHCOOH> — “0 +2.CH,COOK +H,0 +1, 1, tao thinh durge chun d6 bing dung dich chusin Na,S2Os 2 NayS:0, +h; > 2 Nal + NayS,O, 28.5.2. Quy trinh phan tich Lay vao binh nén dung tich 250 mil lurgng chinh xéc 2-3 gam dau thye vat. Thém 5-8 ml clorofocm dé hod tan chit béo va sau d6 thém 10-20 ml CH:COOH bing (hin hop axit axetic bing va clorofocm 2:1), 1 ml dung dich KI bao hod méi pha (hoje mot it in thé KD). Lie ein thin hén hop trong 5- 10 phat Thém vio hén hop 25 ml mude edt va dinh phin i6t tgo thanh bing dung dich Na;S,O; 0,01 M voi chit chi thj hd tinh bot, hét Vuml. Cin tién hanh thi nghiém kiém ching dé higu chinh két qua. 28.6.TINH TOAN KET QUA Sinh vién uy thiét lp cOng thire tinh chi sé axit, chi sé xa phing, chi sé este, chi s6 idt va chi sé peoxit trong miu dau thye vat. 28.7. HOA CHAT - KOH 0,05 M pha trong rugu: dun nong KOH trong nrgu cé lip éng sinh hin di lum, dung dich dé yén 1 ngdy dém, sau dé loc va bio quin trong binh miu niu. ~ Dung dich i6t clorua trong HCI 0,2 M: cho vio binh nit mai 11,1 gam KI; 7,0gam KIO, 50 ml nude eat, 50 ml dung dich HCI dim dic, lic cho tan hoan toan it, sau 46 thém 20 ml clorofocm. Vira lic tht manh via cho thém timg git KIO, 1 % cho dén khi miu tim cia clorofem bién mat, Chuyén dung dich sang phéu chiét, dé yén, bo lop nurée di va dung dich cén lai chuyén sang binh dinh mite rdi thém nude cat t6i 1 lit. Bao quan thude thir trong binh thuy tinh & ch BAI29 PHAN TICH MOT SO CHi TIEU HOA HQC CUA RUQU UONG. *Rugu 1a thire udng c6 chia cén etylic, 1a sin phim eta sur chumg cdt hofic khong chung edt ngi cde khoai, ci, hoa qua...chira gluxit, én men nrgu. Cé thé phan loai cdc rargu bur sau: ~ Rurgu lén men khdng qua chung cat tirngd cde: rugu vang, ruqu tio, nrgu bia. ~ Rugu qua chumg cat tir ngii cde: nugu tring, rugu lia méi, nrgu votca (Nga), = Rurout pha ché tir ole etylic tinh ché voi mréc: rugu nmi, nagu cam quit. Qui trinh ché bién: ~ Lén men nrgu: ‘en ACH _03), nC Ft, 2 2nCH,,0, 229 4m GH,OH2N CO, = Chimg oft rupu: + Phin déu cia qué trinh chung cét (rugu diu) gdm mot phin cdn etylic va cdc tap ‘chit c6 khéi ugng mol phan tir thip nhu CH,OH, CH;CHO, cae axit va este c6 nhigt 46 ‘sbi thip. + Rupu gitta gin odn etylic + Rugu cudi gdm fufurol, cde este va cde loai cn c6 phiin tir lugng va nhiét 40 si cao hon edn etylic. 4.29.1, DINH LUONG BQ AXIT TOAN PHAN ~ Cée axit trong eén, rugu chit yéu 1a cdc axit hitu co dé bay hoi nhur axit focmic, axit butyric...11rgu siin c6 thé chira HCN. - Ham lugng axit trong nrgu dure xe dinh bing ech chun d voi NaOH — chi thi phenolphtalein, - Ly 50 mi miu rugu vao binh nén dung tich 250 ml, thém chi thi phenolphtalein va chuin 49 bing dung dich chuin NaOH néng d6 C,dén khi xudt hién- miu hong nhat Vi ml - Két qua duge biéu thi bing axit axetic (mg) trong 1 lit nrgu qui vé 49 cén 100° va so sinh véi tigu chuiin (khng lon hon 15 mei), 29.2. XAC DINH HAM LUONG AXIT XIAN HIDRIC 29.2.1. Nguyén tic HCN phan img véi AgNO, trong mdi trudng NH; thinh mudi tan trong nude: axit axeti 2HCN + AgNO; —““-> AgCN.NH.CN + HNO, ‘Sau khi hét HCN, mét giot AgNO, cur sé phan mg véi Kl (im chi thi) tao thanh két tia Ag! miu ving khéng tan trong NH. 29.2.2, Cich tién hin Lay 200 ml nrgu vao binh non dung tich 250 ml, thém 10 ml NH; dic, 0,5 g KI, lie cho tan va chun d@ véi dung dich AgNO, ndng 49 C, dén khi xuiit hign két tha ving nhat hét V2 ml Lam tuong ty nhur trén nhumg vi miu tring dé higu chinh két qua sai do hoa chat. * Baio cdo két qua: ham lugng HCN (mg) trong 1 lit nugu qui vé 4} rugu 100° 29.3, XAC DINH HAM LUONG ANDEHIT Andehit I nguyén nhan gay ra vj xéc (chodng) cita rugu, kim cho b may tuin hoin, tiéu hod hogt déng manh, huyét dp cao, gay nhie dau. Trong niu, CHyCHO hinh think do sir oxi hoi C3H.OH. 29.3.1. Nguyén tic ~ Phuong phap thé tich sir dung phép do iét ‘Cac andéhit va xeton cé phin img véi_ bisunfit tao thinh a- oxisunfonic bén voi chat oxi hod. OH 95NaHSO,+ _-C=0 > ,C om ZN SO;Na Lugng dur NaHSO, tir phin img tein duge cho tée dung véi dung dich ehudin I, saw 46 chun 46 Iugng dur Ap bing dung dich chusin NasS.0, véi chi thi hb tinh bot NaHSO; +1, +H,0 > HI+Nal + Na:SOx 1, + 2Na,S,0, > 2 Nal + Na,S,0, - Ngodi ma eding e6 thé xe dinh him Iugng lim ede andebit theo phuomg phip thé tich bing eaich oxi hod nd boi hydroxylamin vi chun d6 dung dich thu duye bing NaOH Véi chi thi metyl da eam NH,OH- HCI + CH,CHO > CH,CHNOH + H,0 + HCL HCl + NaOH — NaCI +H,0 ~ Lugng nho ee andehit duge dink rong phuong phip so miu dya trén phin img, ‘cia andehit v6i fuchsin vi NaHSO; trong mdi trréng H.SO, tao ra hop chat mau hing, 29.3.2 Cich tién hiinh Ly vio 2 binh dinh mie 50 ml, mdi binh 25 ml dung dich chuin NaHSO,, thém vao m6t binh 25 ml rugu cin phén tich (binh cdn lai la mau tring), Dinh mie dén vach bing nue cat, tic déu va dé yén 30- 60 phut & nhigt 49 phng. Lay vao 2 binh nén dung tich 250 ml, mdi binh 25 ml dung dich chuin 1; néng 46 C, vita khuay déu vi thém 10 ml dung dich 6 binh dink mire. Dé phin img xay ra trong bong tdi 5 phat va chun d6 long 1; edn dur bing dung dich chudin NazS.0, ning 46: Vi chi thi hd tinh bOt, hét V5 mL Lam twong te nhur trén véi binh dinh mite chia mau tring * Béo cdo két qua: him lung andehit qui vé andéhit axetic trong 1 lit rugu 100° tinh hing mg 29.4. XAC DINH HAM LUQNG ESTE Cie este c6 trong nrgu 1a do cde axit cacboxilic hod hgp voi rugu etylic va mot sé nrgu khdc. Trong céc este thi lugng este etyl axetat 14 nhiéu nhit, Do dé két qua thu’ng durge bidu thi bing long etyl axetat, 29.4.1. Nguyén tie xde dinh Xa phing hod cdc este bing lung du, chinh xe dung dich NaOH. Sau khi xi phong hoa, thém mt krong axit cling néng 4 va thé tich voi NaOH 6 wen. Nhu vay phan 96(NaOH), dur 43 duge phan émg voi HCl, phin HCI edn lai chinh ki (NaOH), 43 phin img vor este RCOOR’ + (NaOH); > RCOONa + ROH HCI + (NaOH), > NaCl + H,0 HC, + NaOH -> NaCl + H,0 29.42, Cich tién hiinh ‘Cho vio binh cu day trdn cia may cét dung tich 200 ml gdm 50 ml nrgu (di didu chinh vé 50° cOn, vai vién da bot va 5 gigt chi thi phenolphtalein. Trung hoa axit hitu co trong miu thir bling NaOH 0,05 M. Thém 10 ml NaOH 0,05M, lip dng sinh hanh hoi liu va dun & ndi cach thuy séi trong ding 1 gid. Dé ngudi, thém 20 ml H;SO, 0,025 M. Lic déu va chudin d6 H,SQ, dur bing dung dich chudn NaOH 0,05 M. $6 ml NaOH nay la s6- ml NaOH diing 2 xa phing hod este. “*Cich khie: Dé ngugi va chuin d NaOH durbiing dung dich chun HCL *Baio cao két qua : him lugng este biéu thi bing mg etyl axetat trong 1 1 nugu thir qui vé 100". 29.5, HOA CHAT ~ Miu phan tich : Méi sinh vign mt miu nrgu tring 250 ml ~ Dung dich chudin K;Cr,0, cé ndng 49 chinh xe. ~ Cae dung dich dé chudn 46 chura c6 nding d6 chinh xic : AgNOs, NaHSOs, bh. ~ Cae hod chat cin thiét khdc, sinh vién nr pha ché tir NaOH vién, dung dich NH, ic, KI tink thé 30: XACDINH HAM LUQNG FOCMANDEHIT, PHENOL TRONG THUC PHAM, XAC DINH HAM LUQNG KIO, TRONG MUOLIOT. 30.1. BINH LUGNG ANDEHIT FOCMIC 30.1.1. Nguyén tic phuong phip Phuong phip sunfit HCHO phin ting v6i dung dich Na;SO, gidi phéng m long NaOH duce xie dink bling cach chudn 4 véi dung dich chudin HCI khi cé chit chit chi thi phenolphtalin. NaSOs+ HO <> NaHSO; + NaOH 7— OH H > CHY = s05Na NaOH +HC1 > NaCl +130 *Phuemg php iot Trong mdi trrémg kitm, iot oxi hod HCHO thinh HCOOH. Lurgng I, dir duge chun 6 bing dung dich chusin Na,S,O, sau khi da axit hod dung dich, chi thi hé tinh bét. (14n) I; + (2+ 2n)KOH — (n1)KI+ (n41)KIO + (nt 1H (n41) KIO + HCHO + KOH > KI+HCOOK +n KIO-+ 0 axit hod dung dich, khi dé: n KI + (n+1) KIO +2n H" > 2n K* +n HO +KI +n; 1, +2Na,8,0; > 2Nal + NazS,O, 30.1.2. Céch tién hank (theo phwong phap idt) Miu chita foemalin di duge chun bj trong binh dink mite 100. ml (da e6 sin 10 ml KOH 0.05 M) va dinh mite dén vach bing nude cit, Lic déu durge dung dich A. Ly vio. binh nén dung tich 250 ml, 10 ml dung dich A, thém tiép 25 ml dung dich 1, 0,05 M va 10 ml KOH 4 M, dung dich sé c6 mau ving nhat (néu c6 mau hung cin thém KOH). Dé yén 10-15 phiit cho phin img xay ra hodin ton, sau d6 thém 10 ml H.SOs 2M dé axit hod dung dich vi chudn d9 Iugng 1 trong dung dich bing ding dich chun ‘Naz; ¢6 ning 46 C3 voi chat chi thi hd tinh b6t dén hét mu xanh, hét V5 ml. 309.2. BINH LUQNG PHENOL 30.2.1. Nguyen tic Cho vio milu phenol da durge hod tan trong kiém mot thé tich chinh xe dung dich chuin KBrO; + KBr trong mdi tnrémg axit. Lung Br: dur duge xe dinh theo phuomg, phip chudin d6 13 ~ thiosunfat KBrO, + SKBr+6HCI > 3Br: + 6KC1+3H,0 OH OH lL pr =A: Br Qese, Ding < 1 Br Bry gy +2 KI 1, +2KBr :1; +NayS:0; — 2Nal + NasS.Og 98,30.2, 2. Ciich tién hanh Miu phenol di duge chuin bi (chit khoding 0,3 gam) hoa tan mu bing S ml NaOH 10% vi chuyén vo binh dinh mite 250 ml, tring rita va dinh mute dén vach Hiit 10 ml dung dich miu vio binh nbn dung tich 250 ml, thém 10 ml dung dich KBr 5% va 10 ml dung dich chudn KBrO, ndng d@ C., 15 ml H;SO, 4 M, day nét kc 10 phat. Thém 15 ml KI 5% lie déu va dé yén trong bing t6i 10 phiit. Chun 49 lugng I> sinh ra bing dung dich chudin Na,S,O, c6 néng dO C; t6i mau ving nat. Thém chi thi hé tinh bot va tiép tue chudn d6 biing Na,S,O; t6i mit mau xanh tim, hét 'V¢ ml, 30.3. DINH LUONG KIO; TRONG MUOLIOT (THEO TCVN 1998) 30.3.1. Nguyén tie Mu6i idt duge ché bién tir mudi dn co bé sung KIO duge hod tan trong nude, thém luong dir KI trong moi tnring axit va chudin 6 lugng I> giai phong ma bing dung dich cchusin Na;S;O; véi chit chit chi thi hé tinh bot. 30.3.2 Ciich tién hinh Can 10 gam miu mudi idt, véi 4 chinh xéc dén 0,01 gam cho vao binh nén dung: tich dung tich 250 ml, thém 30 ml nude cat va bic cho tan hét mu, Thém nude cat dén khoang 50 ml vithém 1 ml H,SO, 1M, 10 ml ding dich KI 5%. Bay nat va dé yén chd t6i 10 phat. Tir buret ho tir tir timg gigt dung dich dung dich chuin Na,S,0, c6 ning 4} C; chuin 46 cho dén khi c6 mau ving nhgt. Thém 1 ml chi thi hé tinh bot va tiép tuc cchudin 46 cho dén khi mat mau xanb thm, hét Vs ml, 30.4, TINH TOAN KET QUA Sinh vién ty thiét lip céng thire tinh néng 46 phan tim HCHO trong focmalin, ham lrgng phénol trong mau dang dung dich cho trade va tinh him lugng I (ppm) e6 trong rnd bot eanh iot. 30.5. HOA CHAT ~ Miu phan tich: Miu focmalin dic (P) cia TQ. + Dung dich miu phenol, méi sinh vién 1 mu trong ede 250 ml. + Miu mudi iét, méi sinh vién | miu. Dung dich chuan KCr,0; 6 ning d6 chinh xdc, cde dung dich 1), Na,S,0;, KBrO,chua c6 ndng 46 ding dé chudin 46, chit chi thi hé tinh bot. - Cac hod chat can thiét khac, sinh vién ty pha ché tir. KOH rin, HSO, die, KBr rin, KI tinh tha CHUONG 10 CAC PHU LUC PHU LUC 1 DO TRONG LUGNG 99Trong phan tich, dé dinh gid d6 chinh xéc, 49 ding cua mot phép do nhit thiét phai thong qua cde dung cu do trong lugng, dé la chige edn. No duge diing dé cin chat chuiin, ‘edn mu phan tich, edn hod chat phan img, cén sin phim v.v. Tuy nhién, ngudi phin ti dn biét_nguyén tic co ban cita phép can , can gi va cdin nhur thé nio? Phép cn phan tich duge thye hign dé cn cc vat cn la chat géc, cde chit ¢6 thanh phan xde dinh ding dé pha ce dung dich chudn; cin cdc sin phim cla mot qui trinh bién dei nguyén tic nhat dinh sao cho phép cfin vira chinh xie vira 06 ¥ nghia. ‘M6t phép cn ding phai bao gim ca hai yéu t6 tén; chinh xc nhung phai c6 ¥ nghia, Cé nhimg chat nhit thiét phai cn bing cén phén tich nhung cing c6 nhing chit diéu 46. khong cn thiét; hon nia e6 nhiéu chit néu can trén can phan tich 1 hodn toin v6 ngbfa. Thi dy mOt hod chat rt ho nude nhu NaOH, hay FeCl; v.v. sé thay déi trong lugng ngay trong qué trinh can; mot hod chat di qua han sir dung 4 bi bién chat hoe ¢6 hoi Am bim trén bé mit thm chi i chiy nude thi sir dung edn phan tich trong tnrimg hyp d6 1 khong cdin thiét. Mue dich sir dung eding quyét dink loai edn cho phi hop: chi cn pha mt dung dich

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• Wuthering Heights (Seasons Edition -- Winter)

  

  From Everand

  Wuthering Heights (Seasons Edition -- Winter)

  Emily Bronte

  Rating: 4 out of 5 stars

  4/5 (9975)