Qun l cht lng nc nui trng thy sn

Phn tch cht lng nc

CHNG 7 nh (7g) t 44.000 lt nc khong gn ni Bad Nauheim, Germany. S khm ph PHN TCH NC ny l nn tng cho s khm ph tip CHT theo vLNG s hp thu v pht x ca hp thu phn t. Nm 1879 Marie Alfred Cornu thy rng, nhng tia c bc sng ngn ca bc x 1 NG DNG THUYT PHN T UV-VIS TRONG PHN TCH CC YU T mt tri CHT trn b mt tri t b hp th bi kh quyn. Mt nm sau , Walther LNG NC Noel 1.1 S lc lch s nghin cu v quang ph Hartley m t rt t m v s hp th UV ca O vi di bc sng 200 v 300 nm Quang ph hc l mt mn hc chnh yu3 trong thin vn hc, n c ng dng v n tr nn r rng hn khi h pht hin ra rng O cha y trong bu kh 3 tinh chng ta. thnh cng nghin cu v kh quyn trong hnh quyn. Cch y 200 nm, Joseph Fraunhofer (1787-1826) ln (400-840nm). u tin sn xut loi my In 1880, J. Chappuis khm ph ravon s hp thu trong vng kh kin Nm o quang ph m tnh nng khng cquang g snh ph kp lc byrt gi. ng y khm ph ra 1925 Dobson pht trin mt my mi n nh s dng nhiu cc ng ti trong quang ph ca nh sng mt tri. lng rt knh bng thch anh. ng y c th xc nh chnh xc di bc sng ca nhiu "Fraunhofer lines" 1.2 i cng quang (vch) v v thut ng ph ny ngy nay vn c dng. Tuy nhin, trong thi gian ny ng khng hiu c c s vt(nh l v ngha nhng vn m ng y khm Trongy quang ph hc, nhnhng sng nhn thy sng kh v kin), tia hng ngoi, tia t ra. ngoi,ph tia Rnghen, sng radio... u c gi chung mt thut ng l bc x. Theo thuyt sng, cc dng bc x ny l dao ng sng ca cng in trng v cng t trng, nn bc x cn c gi l bc x in t. Sau thuyt sng, thuyt ht cho thy bc x gm cc "ht nng lng" gi l photon 8 chuyn ng vi tc nh sng (c = 3.10 m/s). Cc dng bc x khc nhau th khc nhau v nng lng h ca cc photon. y, nng lng ca bc x c lng - J.s = : hng s bc Planck. t ha,h ngha l nng lng ca x khng phi lin tc m cc lng t nng 34 6,625.10 lng t l vi tn sca ng in tc theo thc Louis de Broglie a dao ra thuyt thng nht khi h nim sngPlanck. v khi nim ht ca =h sng nh sng. nh sng va c tnh cht sng va c tnh cht ht. Tng qut hn l bc x khi c bn cht m sng ht. Ni dung nh tc sau: Ht c lng chuyn ng vi vn v c bc sng i i vi n l cho bi h thc: Hnh 7-1. Thit b Spektralapparat thit k bi Gustav R. Kirchhoff v Robert = h =h W. mv p Bunsen (1823) Trong tu p = quan mv ltrng ng k lng Thnh tip ca v "Fraunhofer lines" l qu trnh tm ra nguyn l vt ht : l ca s hp thu v pht x vo nm 1859 vi s cng tc ca nhiu nh vt l ni l bc sng (de ting nhBroglie) Gustav R. Kirchhoff (1824-1887), Robert W. Bunsen (1811-1899) ti h = 6,625.10 -34 J.s l hng s Heidelberg. Thit b m h s dng l 'Spektralapparat', h ghi nhn c qu trnh Planck. pht x rt c bit ca nhiu nguyn t khc nhau. Vi phng php ny h 14 tip tc khm ph ra 2 nguyn t mi l Csium v Rubidium, h chit c mt lng rt 0 13 9

Phn tch cht lng nc 1.2.1 Cc i lng o bc x in t Bc sng : L qung ng m bc x i c sau mi dao ng y . n v: m, cm, m, nm, o . (1cm = 8 o = 107 m =10 4 m) A 10 Tn s : L s dao ng trong mt nAv thi gian (giy) c Trong 1 giy bc x i c c cm v bc sng cm, vy: = 8 Lu : Bc x truyn trong chn khng vi vn tc c = 2,9979.10 m/s (thng ly 8 trn 3.10 m/s) 3 6 n v: CPS ( VNG DY), Hz, KHz, MHz. (1CPS=1Hz; 1MHz=10 KHz=10 Hz) Nng lng bc x: Cc dao ng t (phn t chng hn) ch c th pht ra hoc hp th nng lng tng n v gin on, tng lng nh nguyn vn gi l lng t nng lng: = h = hc = hc n v: Jun (J), Calo (Cal), electron von (eV). 1.2.2 Cc dng bc x Bc x in t bao gm 1 dy cc sng in t c bc sng bin i trong khong m) tia Rnghen hoc nh hn o -10 rt rng: t c mt sng raio n na. c A (10 Ton b dy sng c chia thnh cc vng ph khc nhau.

Hnh 7-2. Cc ph ca sng in t

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Qun l cht lng nc nui trng thy sn Mt ngi ch cm nhn c mt vng ph in t rt nh gi l vng nhn thy (kh kin) bao gm cc bc x c bc sng t 396-760 nm. Hai vng tip gip vi vng nhn thy l vng hng ngoi v vng t ngoi. 1.2.3 S tng tc gia vt cht v bc x in t iu kin bnh thng, in t ca phn t nm trng thi lin kt, nn phn t c mc nng lng thp, gi l trng thi c bn Khi chiu mt bc x in t vo mt mi trng vt cht, s xy ra hin tng cc phn t vt cht hp th hoc pht x nng lng, hay c gi l trng thi kch thch . Nng lng m phn t pht ra hay hp th vo l: E = E - E = h 2 1 Trong , E v E l mc nng lng ca phn t trng thi u v trng thi cui 1 2 (hay cn gi l trng thi kch thch) l tn s ca bc x in t b hp th hay pht x ra. Nu E > 0 th xy ra s hp th bc x in t. Nu E < 0 th xy ra s pht x nng lng. Theo thuyt lng t, cc phn t v cc bc x in t trao i nng lng vi nhau khng phi bt k v lin tc m c tnh cht gin on. Phn t ch hp th hoc pht x 0, 1, 2, 3,n ln lng t h m thi. Khi phn t hp th hoc pht x s lm thay i cng ca bc x nhng khng lm thay i nng lng ca n, bi v cng bc x in t xc nh bng mt cc ht phton c trong chm tia, cn nng lng bc x in t li ph thuc tn s ca bc x. V th khi chiu mt chm bc x in t vi mt tn s duy nht i qua mi trng vt cht th sau khi i qua nng lng ca bc x khng h thay i m ch c cng bc x thay i. Cc phn t khi hp th nng lng ca bc x s dn n thay i cc qu trnh trong phn t (quay, dao ng, kch thch electron ) hoc trong nguyn t (cng hng spin electron, cng hng t ht nhn) Mi mt qu trnh nh vy i hi mt nng lng c trng cho n, ngha l i hi bc x in t c tn s hay chiu di sng nht nh kch thch. Do s hp th chn lc ny m khi chiu chm bc x in t vi mt di tn s khc nhau i qua mi trng vt cht th sau khi i qua chm bc x ny s b mt i mt s bc x c tn s xc nh, ngha l cc tia ny b phn t hp th. 14 2

Phn tch cht lng nc 1.2.4 S hp th bc x v mu sc ca cc cht nh sng nhn thy bao gm tt c di bc x c bc sng t 396-760 nm c mu trng (nh sng tng hp). Khi cho nh sng trng (nh sng mt tri) chiu qua mt lng knh, n s b phn tch thnh mt s tia mu (, da cam, vng, lc, lam, chm, tm). Mi tia mu ng vi mt khong bc sng hp hn (xem Bng 7-1). Cm gic cc mu sc l mt chui cc qu trnh sinh l v tm l phc tp khi bc x trong vng kh kin chiu vo vng mc ca mt. Mt tia mu vi mt khong bc sng xc nh. Chng hn bc x vi bc sng 400-430 nm gy cho ta cm gic mu tm, tia sng vi bc sng 560 nm cho ta cm gic mu lc vng. nh sng chiu vo mt cht no n i qua hon ton th i vi mt ta cht khng mu. Th d, thy tinh thng hp th cc bc x vi bc sng nh hn 360 nm nn n trong sut vi cc bc x kh kin. Thy tinh thch anh hp th bc x vi bc sng nh hn 160 nm, n trong sut i vi bc x kh kin v c bc x t ngoi gn. Mt cht hp th hon ton tt c cc tia nh sng th ta thy cht c mu en. Nu s hp th ch xy ra mt khong no ca vng kh kin th cc bc x khong cn li khi n mt ta s gy cho ta cm gic v mt mu no . Chng hn mt cht hp th tia mu ( = 610-730 m) th nh sng cn li gy cho ta cm gic mu lc (ta thy cht c mu lc). Ngc li, nu cht hp th tia mu lc th i vi mt ta n s c mu . Ngi ta gi mu v mu lc l hai mu ph nhau. Trn hai mu ph nhau li ta s c mu trng. Ni cch khc, hai tia ph nhau khi trn vo nhau s to ra nh sng trng. Quan h gia mu ca tia b hp th v mu ca cht hp th (cc mu ph nhau) c ghi bng sau: Bng 7-1. Quan h gia mu ca tia b hp th v mu cht hp th Mu ca cht hp (nm) Mu th 400 - 430 Tm (mu ca tia cn li) 430 - 490 Xanh Vng lc 490 - 510 Lc xanh Vng da cam 510 - 530 Lc 530 - 560 Lc vng ta 560 - 590 Vng Tm 590 - 610 Da cam Xanh 610 - 750 Xanh lc Lc Lu : Gia cc tia mu cnh nhau khng c mt ranh gii tht r rt. Vic phn chia nh sng trng thnh 7, 8 hay 9 tia mu cn ty thuc vo lng knh v s tinh t ca mt ngi quan st. Tia b hp th

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Qun l cht lng nc nui trng thy sn Mt cht c mu, th d nh mu chng hn l do n hp th chn lc trong vng kh kin theo mt trong cc kiu sau: - Cht hp th tia ph ca tia (tc l hp th tia mu lc) - Cht hp th cc tia tr tia mu . - Cht hp th hai vng khc nhau ca nh sng trng sao cho cc tia cn li cho mt ta cm gic mu . mt hp cht c mu, khng nht thit ca n phi nm vng kh kin m max ch cn cng hp th vng kh kin ln. Ni mt cch khc tuy gi tr cc i ca vn hp th nm ngoi vng kh kin nhng do vn hp th tri rng sang vng kh kin nn hp cht vn c mu. Tt nhin c c s hp th thy c vng kh kin th ca cht cng phi gn vi ranh gii ca vng kh kin. max Tng ng vi mt bc chuyn in t, ta thu c ph hp thu c dng: Hai i lng c trng ca ph hp thu l v tr v cng - V tr cc i hp thu, gi tr ty thuc vo E m hp cht ny hp max thu cc vng ph khc nhau. Bn chiu rng ca vn ph in t dao ng kh rng khong 50-60m. - Cng th hin qua din tch hoc chiu cao ca nh biu (peak). Cng vn ph ph thuc vo xc xut chuyn mc nng lng ca in t. Xc sut ln cho cng vn ph ln. Mt hp cht mu c ph hp thu tt khi nh biu (peak) cao v bn chiu rng vn ph hp. Peak A () Bn chiu rng vn ph

max Hnh 7-3. nh v bn chiu rng vn ph Khi bn chiu rng vn ph hp, th khi thay i nh th hp thu A thay i ln. iu ny rt c ngha trong phn tch nh lng. Gi s hp cht X c A max 500nm. Khi chng ta o bc sng 510nm... th hp thu o c s khc rt xa i vi bc sng 500nm. T ta thy rng mi hp cht mu c mt gi tr max 144 nht nh v n phn nh nhy ca phng php.

Phn tch cht lng nc Mt khc, mt hp cht i hi nh biu cao ngha l khi ta o bc sng th ta c hp th quang cc i, khong lm vic rng. max 1.2.5 nh lut Lambert - Beer Khi chiu mt chm tia sng n sc i qua mt mi trng vt cht th cng ca tia sng ban u ( I ) s b gim i ch cn l I o II T s 0 100 = T c gi l truyn qua. 00 I I 100 T s 0 00 = A c gi l hp th. I Nguyn tc ca phng php biu din theo s :

Hnh 7-4. S m t s hp th nh sng ca mt dung dch Trong : Io: Cng nh ban sng u ca ngun : Cng b hp thu sng bi dung dch I A I: Cng nh sng sau khi qua dung dch. I : Cng nh sng phn x bi thnh cuvette v dung dch, gi tr ny c loi b bng cch lp li 2 ln o. R Gia I , I, dy truyn nh sng (l) v nng (C) lin h qua quy lut Lambert Beer lA nh lut hp nht ca Bouguer: Lambert (1766) lg Beer (1852) : lg Io =Kl I 1 Io I = K1C

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Qun l cht lng nc nui trng thy sn truyn quang (T) hay hp th (A) ph thuc vo bn cht ca vt cht, dy truyn nh sng l v nng C ca dung dch. C th vit: I I nh lut Lambert - Beer : 0 A = lg( ) = *C *l

Trong : l h s hp thu phn t, C nng dung dch (mol/L), l dy truyn nh sng (cm), A l hp th quang. (Lu phng trnh trn ch ng i vi tia sng n sc). Trong phn tch nh lng bng phng php trc quang ngi ta chn mt bc sng nht nh, chiu dy cuvet l nht nh v lp phng trnh ph thuc ca hp th quang A vo nng C. Kho st khong tun theo nh lut Lambert - Beer : Khi biu din nh lut Lambert - Beer trn th ty theo cch thc hin php o, ta thng gp ng biu din s ph thuc hp thu A vo cng C ca dung dch c dng: y = ax + b H s gc a cho bit nhy ca phng php, trong phng php trc quang ngi ta ch o dung dch trong khong tun theo nh lut Lambert - Beer tc l khong nng m gi tr khng thay i. H s gc a cng ln v khong tun theo nh lut Beer cng rng l iu kin thun li cho php xc nh. S lch khi nh lut Beer: S lch khi nh lut Beer c biu din bng s sau: A LOL

C Hnh 7-5. Gii hn ca nh lut Beer v s hp th quang Khong tuyn tnh LOL (Limit of Linear Response) l khong nng tun theo nh lut Beer (A = *l *C) ngha l khi nng tng th hp th quang A tng. Ngoi gii hn LOL l s lch khi nh lut Beer, ngha l khi nng tng th hp th 146

Phn tch cht lng nc quang A hu nh khng tng na. Nguyn nhn ca qu trnh ny l do nng dung dch qu ln. Ngoi ra, khong tuyn tnh LOL cn b nh hng ca mc n sc ca nh sng s dng, pH ca dung dch, lc ion, s pha long... ngha ca cc i lng: - H s hp thu mol : ph thuc bn cht mi cht, bc sng , nhit , chit sut (theo nng ). Gi tr tnh l thuyt ca mt b c chuyn c php cho 5 -1 1 electron l = 10-1 mol .cm . = A (l.mol- lC cm ) 1 1 cao cho ta bit c nhy ca phn ng, l thc o nhy ca phng php. Trong phn tch trc quang, = 103-10 mol 5 . cm l nhy dng -1vo chit -1sut m chit sut li ph cho phng php trc quang, ph thuc thuc vo nng . Khi chit sut tng ln th gim v khng thay i th -2 phi thc hin C 10 mol/L. - hp th quang A: L i lng khng c n v, c tnh cht quan trng l tnh cng hp th quang. v C , hp thu ti bc sng l: A B A A=A +A = l *( C B + C ) A B A B Nu mt cht tan X no c hp th quang l A , dung mi c hp X th quang l A , ta c: dm A=A +A x dm o c chnh xc A th A = 0, c ngha l phi chn ca dung mi x dm max khc xa vi cht tan. Nhng cht c chn lm dung mi thng c max hp thu min ranh gii t ngoi chn khng. Bng7-2. thng s dng trongDung vng mi UV-VIS Bc sng gii DungCc midung mi Bc sng gii hn hn s dng (nm) s dng (nm) Nc ct Benzen 190 280 HCl Cloroform 190 245 Etanol, Tetra Clorocarbon 210 265 Metanol Dietyl Eter 210 218 n- Butanol Aceton 210 330 n- Hexan 1,4 Dioxan 210 215 Cyclohexan 14 7 Gi s 2 cht A v B c nng C

Qun l cht lng nc nui trng thy sn Trong hn hp c nhiu cu t khng lm thay i tng tc, khng phn ng ha hc, khng dch chuyn cn bng, th c th xc nh hn hp cc cu t theo h thc sau: A= lC + lC + ....... + i lC i + ...... + 1 1 2 2 n lCn - truyn quangIT: I0 T m A = lg( ) do A = = I lgT I V Totnh theo % nn: A = 2 lgT Nu T = 100% th A = 0 (ngha l khng hp th nh sng (I = I Nu T = 1% th A = 2 Nu T = 0 % th A = (hp thu hon ton nh sng) 1.2.6 Nguyn l cu to ca my quang ph Ngun sng Ngun sng cho my quang ph l chm bc x pht ra r n. My quang ph dng n hydro hay n Deuterium cho ph pht x lin tc trong vng UV t 200-380m (nhng thng s dng 200-340 m) v n tungsten halogen o vng 380-1000 m. lm vic cho c hai vng th phi c 2 loi n trn. Mt yu cu i vi ngun sng l phi n nh, tui th cao v pht bc x lin tc trong vng ph cn o. n Deuterium: cu to sm mt si t ph xit v mt cc kim loi t trong mt bng thu tinh cha kh Deuteri hoc hydro c ca s bng thch anh bc x t ngoi i ra v n khng truyn qua c thy tinh. Khi si t c t nng, electron cc phn + E ra kch * Dthch D' + D+ ht kh Deuteri (hoc hidro) bin thnh nguyn t D sinh e 2 v pht ra phton theo phn ng: 2 D'' =E * =E + E + h D D' y E l enng2lng electron kch thch, bc x pht ra l mt ph c bc sng t 160 nm n vng kh kin. B n sc B n sc c chc nng tch bc x a sc thnh bc x n sc, bao gm knh lc, lng knh hay cch t. Cch t l mt bng nhm hay cc kim loi Cu, Ag. Au... c vch thnh nhng rnh hnh tam gic song song. Khi chiu nh sng qua cch t, phn cn li c tc 148 o )

Phn tch cht lng nc dng to nn vn nhiu x c bc sng khc nhau, khi quay cch t s to ra ph nhiu x ging nh trng hp nh sng qua lng knh. u im l cho phn gii tt, tn sc tuyn tnh, rng ca di n nh, chn bc sng n gin, gn nh, d ch to nn hin nay s dng cch t to nh sng n sc c a chung. Cch t dng cho UV-Vis c 1200 vch/mm (thng dao ng t 300-3600 vch/mm, s vch cng nhiu th nng sut phn gii cng cao.

Detector Hnh 7-6. S cu to ca my quang ph 0 Lng knh ca my quang ph dng lng knh littrow (lng knh 30 ) bng thch anh, c c im nh sng i qua lng knh hai ln do phn x mt sau. Detector Detector l b phn o tn hiu nh sng trc v sau khi i qua dung dnh (ng trong cuvet). Cc tn hiu sau khi i ra Detector s c s c khuch i, lu gi v x l trn my tnh. Cuvet ng mu Cuvet phi lm bng cht liu cho bc x vng cn o i qua. Cuvet thy tinh khng thch hp cho vng UV. Cuvet thch anh cho bc x i qua t 1901000 nm. Cuvet nha ch dng trong vng Vis v ch s dng c 1 vi ln. 1.3 S dng phng php trc quang trong nh lng ha hc 4 l phi bn, t phn ly, n nh, khng thay i Yu cu v cc hp cht 3 cn xc nh -1 -1 thnh phn trong khong thi gian nht nh thc hin php o (10-20 pht). H s ln c gi tr t 10 -5.10 L.mol cm , c th thc hin phn ng to mu vi cc thuc th v c v hu c. 14 9

Qun l cht lng nc nui trng thy sn Nng cc cht xc nh theo nh lut Lambert - Beer. Khong xc nh -2 nng -6 - 10 mole. Gii hn pht hin ca phng php 7 10 mole. theo phng php l 10 Cc hp cht l phc cn o phi c khc xa vi ca thuc th trong cng max max iu kin tc l >2 ln na bn chiu rng ca vn ph (khong 80 -100 m). Th 2+ d, khi phn tch Fe bng phng php O-Phenanthroline. Sau khi thm thuc th ta c phc mu vng cam ( =510 m), trong khi thuc th max 1,10Orthophenanthroline c = 250 m. max 1.3.1 Phng php so snh So snh cng mu ca dung dch cn xc nh vi cng mu ca dung dch chun bit nng . iu kin: c hai dung dch trn phi c nng nm trong khong tun theo nh lut Beer. C x ---------------------- Ax A *C Ta cn nh C C x Atct C xc tc ---------------------: = x c x Khi s dng 2 dung dch chun: A tc C C = C 2 * (A x x C A ) + 1 1 hp thu v nng ca dung dch chun tng ng sao Vi A 1 , A , C , C l 1 2 A1 2 2 cho A 1 A1 < A x < A 2 c ngha C 1 < C x < C2 1.3.2 Phng php thm chun Phm vi ng dng l xc nh cc cht c hm lng vi lng hoc siu vi lng, loi b nh hng ca cht l. C 2 phng php l phng php s dng cng thc v phng php th. A dng cng thc - Phng php s C = x A A xx x C Trong a A :+ hp thu ca dung dch xc nh tng ng vi th x tch : V . a : Ax+ hp thu ca dung dch c thm chun. x a C : Nng cht chun thm vo. a 15 0

Phn tch cht lng nc ng cht cn xc nh trong N th c tch V Cng thc thit lp A = lC x x t: x A = l(C + C x (x+ C c biu din theo n v ca ) C . x a a) a Cch thc hin: C :x Ly 3 ln ca dung dch cn xc nh nng cho vo 3 bnh nh mc c th tch VmL. Bnh 1: Thm thuc th v cc cht to mi trng pH cho dung dch, dung dch gi l dung dch xc nh C , hp thu quang tng ng l A . x x Bnh 2: Thm mt lng chnh xc dung dch tiu chun bit chnh xc nng , tin hnh phn ng to mu ging nh bnh 1. Dung dch c hp thu tng C ng a l A . (x+a) Bnh 3: ch thm cc cht to pH cho dung dch, ly dung dch ny lm dung dch so snh. A . T C c trong th tch V (mL) c th qui p dng cng thc: C = x x x A A xx x v C C a + th tch ban u ca mu V Co (mg / a V L) = (mL): x o o V x 4 ln ca dung dch cn xc nh nng C t nht 3 dung dch thm chun. Ly t nht - Phng php s dng th cho vo 4 bnh nh mc V(mL). Sau thm chnh xc mt lng V , V , V 1 2 3 mL dung dch tiu chun c nng tng ng C , C , C vo 3 bnh nh mc trn. a1 a2 a3 Tin hnh phn ng to mu. Bnh cn li lm dung dch so snh, cng chun b ging nh phng php cng thc. hp thu ca cc dung dch thm so vi dung dch so snh.

15 1

Qun l cht lng nc nui trng thy sn A A + x a3 A + x a2 + AAa1 x x

Ca1

Ca2

Ca3

Hnh 7-7. Biu xc nh phng trnh hi quy tng quan ca phng php thm chun s dng th. C th c kt qu trn th hoc s dng phng trnh hi qui c dng: A A= =aC b +b x = b/a 1.3.3 Phng php C ng chun x u im l chnh xc, thc hin c nhiu ln. - Chun b t 6 dung dch chun (trong khong tun theo nh lut Beer). - Thc hin phn ng mu vi thuc th. - o hp th quang A ca dung dch so vi cc dung dch so snh max c chun b ging nh dung dch tiu chun nhng khng cha ion cn xc nh. - Biu din s ph thuc A theo C trn th hoc tnh theo phng trnh hi qui A=aC + b (a v b l h s cn tm ca phng trnh hi quy - tng quan) (xem Bng 7-3) - Dung dch xc nh: chun b v phn ng to mu vi thuc th ging nh mu chun. Dung dch chun C (mg/L) A Bng 7-3:1Dung dch chun dng xy dng ng chun 0,00 0,010 2 0,05 0,480 3 0,10 0,930 4 0,15 1,370 5 0,20 1,830 6 0,25 2,281 15 2 (hi quy tuyn tnh y = ax + b)

Phn tch cht lng nc Sau khi o c gi tr hp th quang ca cc dung dch chun, chng ta c th tin hnh xy dng ng chun v tm ra phng trnh hi quy tng quan: 2.500 2.000 1.500 1.000 0.500 0.000 0.00 y = 9.0543x + 0.0184 2 = 0.9999 R

A hu t p h s H

Qun l cht lng nc nui trng thy sn chnh xc trong phng php ny ph thuc vo hng lot nguyn nhn khc nhau rt phc tp bao gm sai s ngu nhin v sai s h thng, trong sai s quan trng nht l sai s ca tn hiu trong qu trnh o hp thu quang hc. 1.5 Mt s v d p dng phng php nh lng trc quang V d 1 -4 hp th quang A ca dung dch anilin 2.10 M trong nc o bc sng =280nm l 0,252. Chiu di nh sng i qua cuvet l 1cm. Tnh truyn quang ca anilin 1,03.10-3M khi o cng di bc sng nhng dng cuvet 0,5cm. Gii: I I 0 ) = *C *l vi dung dch 1 ta c: p dng cng thc A = lg( 0.05 0.10 - -0.15 0.20 0.25 0.30 3 = 0.252/(2.10 *1) = 1,26.10 l.mol cm . Nng 4 1 1 I p dng cng thc A = lg( ) = phng *C *l vi dung ta c:quan ca phng php Hnh 7-7. Biu xc nh trnh hi dch quy 2 tng ng 3 * 0,5 0 - = 0.649 A = 1,26.10 1,03.10 chun. * I 3 M: Sau khi thit lp ra: ng chun, dngdo phng A= -lgT suy lgT = -A ta =c -0,649, Ttrnh = y = ax + b vi y l hp 0,224 = 22,4% th quang, xquang l thu nng i vi dung dch xc nh, ta tin hnh phn ng v o c h s hp ca mu (A Vy truyn T. = 22,4% m = y), ta c th tnh c nng ca mu cn xc nh theo phng trnh: u V d 2: y b x quang = hp th a A o c t cc mu chun v mu nc thu t ao nui c cha ion PO43 nh sau: S tng quan gia hp th quang nng 0,15 C khi l = const l ni dung ca Nng mu chun 0,00 0,05 A v0,10 0,20 0,25 nh lut Beer. Khong tha mn1,370 nh lut ny khi2,281 r > 0,999. (mg/L) 0,010nng 0,480 0,930 1,830 hp th quang A 2 hp th ca rmu ao ca 3 ln lp H s quang tng A quan binnc i trong khong -1 rli 1 l: (R 1,256; = 0-1)1,245; 1,264. Tnh 3 nng trong mu nc ao. - - Khi r 1 c s tng quan cht ch gia x v y theo t l thun. PO - 4Khi r -1 c s tng quan cht ch gia x v y theo t l thun. Gii: - Khi r 0 hai i v lng nyth khng cn tng quan. T cc nng mu chun hp quang A. T kt qu thit lp phng trnh y = 9,0543 + phng 1.4 xc x trong hi qui ta c: chnh (r2 = php trc quang: 0,0184 Trong phn tch trc quang0,9999). cng nh bt k phng php no khc c th chia sai s T kt qu ca 3 ln phn tch lp li ta A = y= 1,255 thnh 2 nhm: c 0,0184 1 ,255 - Sai s do y tin hnh= phn ng ha = hc (ha cht, T ta c 0,137 mg / thao tc, dng c...) 0,0184 9 ,0543 - Sai s ca tn hiu o hp L thu ca dung dch (do h thng x= 9 ,0543 o). PO43- trong mu nc ao l 0,137 mg/L. Vy nng 154 15 3

Phn tch cht lng nc V d 3: xc nh hng s phn ly ca Methyl da cam (k hiu HIn), ngi ta o hp th quang A ca 3 dung dch cng nng Methyl da cam cc pH khc nhau: - Dung dch 1 trong HCl 0,1M; A = 0,475. 1 - Dung dch 2 trong NaOH 0,1 M; = 0,130. A - Dung dch 3 c pH = 4,34; 2 = 0,175 Cho bit o bc sng = 510nm v chiu di A nh sng i qua cuvet l 1cm. Tnh 3 hng s phn ly K ca Metyl da cam? Gii: hp th quang ca dung dch 3: [ In ] *l + [HIn]*l (7.1) A = I H I - ] = x; [HIn] 3 Vi [In = y ta HIn = C (7.2) nc: x + y = n C A In (7.3) = 2 v ton b cht ch th dng I C *l n Hin A v ton b cht ch th dng HIn (7.4) 1 = C *l Thay (7.3) v (7.4) vo (7.1) ta c: x y (7.5) A =A +A C C 3 . . x y 2 1 Qui c: = ; = (1 ) 0,175 = 0,130 + 0,475 (1-) C C = 0,869 Hng s phn ly ca HIn: K HIn H+ + In ; a + [H ] K= pK = pH In = pH lg [In ] 1 HIn HIn lg -4 pK = 4,34 - 0 ,869 1 0,689 = 7.34 0,82 = 3,52 K = 3,02.10 . lg Vy hng s phn ly ca methyl da cam l K = 3,02.104.

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Qun l cht lng nc nui trng thy sn 2 PHNG PHP THU V BO QUN MU 2.1 Chun b thu mu 2.1.1 Nhn nh s thay i cht lng nc Cht lng nc ti mi tri lun b thay i theo thi gian (ph thuc vo lu lng v mc tc ng ca cc ngun nhim), do vy cn o cc gi tr cc i, cc tiu v trung bnh ca cc thng s theo thi gian c th phn nh gn ng gi tr thc. S mu thu thp cn ln v nhp thu mu cn cao lm c iu ny . Tuy nhin, vic tng cao s mu v nhp thu s gy tn km nhiu v kinh ph v nhn lc. Cho nn cn tnh sao cho va tin cy va khng qu nhiu chi ph Theo GEMS (H thng quan trc mi trng ton cu) nhp thu mu cho nc nui thy sn nh mu sng thi gian thu mu cn tin hnh khi lu lng thp, ao h cn xem xt chu trnh sinh hc v cn tng nhp thu mu thi im c nng sut sinh hc cao. 2.1.2 Cc iu cn lu khi thu mu La chn v ra k chai, l ng mu. Dng tay cm chai, l nhng vo khong gia dng nc cch b mt nc 30-40cm. Hng ming chai, l ly mu hng v pha dng nc ti. Th tch nc ph thuc vo thng s cn kho st. y kn ming chai, l, ghi r l lch mu thu.

Bo qun mu ng qui nh nu bng 1. 2.2 Cc bo qun mu 2.2.1 Mu nc Ty theo ch tiu cht lng nc m cch ly mu v bo mu khc nhau, cch bo qun mu c trnh by Bng 7-4. 2.2.2 Mu t Mu t sau khi thu, phn tch cng sm cng tt. Nu mun bo qun lu cn lm nh sau: Tri mu cng mng cng tt trn bao nilon v phi kh trong iu kin nhit o phng. Sau nghin mn, ri cho vo cc snh, em sy nhit 105 C trong 24 gi. ngui mu trong bnh ht m, lc ny sn sng phn tch.

15 6

Phn tch cht lng nc Bng 7-4: Dng c thu mu v cch bo qun mu theo ch tiu phn tch STT Ch tiu Dng c Th tch Bo qun bo qun (mL) o 1 Alkalinity P;G 200 4C 2 Hardness P;G 100 o 4 C 3 DO P;G 100 1mL MnSO4, 1mL KI4 P;G 100 CO2 NaOH 5 P;G 100 COD 0,5 mL o CHCl 6 ChlorophyllP;G 500 3 2mL H SO 4M 7 a G 100 2 l nu 4 Lc, 4 C, 8 P;G 500 SiO2 HCl 1:1 9 P;G 100 TAN o 10 Nitrate P;G 100 Nitrite 4C o 11 NO - v P;G 200 4 C 12 NO 2 P;G 100 o 33 4C 13 PO4 P;G 500 o TN,TP P: Plastic bottle G: Glass bottle 4C o 2.3 Phng php thu mu 4C o Phng php thu mu chnh xc s gp phn tng tnh chnh xc4ca C kt qu phn tch. Ty mc ch nghin cu m vic thu mu mang tnh cht c bit hay i din cho ao c p dng ph bin hn. thu mu hn hp i din cho ao, c th thc hin cc bc sau: 2.3.1 Nguyn tc chung Thu nhiu im trong ao (3-5 im hoc hn), sau trn mu li (cng nhiu cng tt), ri ly mt mu i din loi mu cn phn t ch (ch tiu nc hoc bn y). mi im, cn thu ng thi 3 v tr, ri cho vo 3 x (mi mu/ x), tip tc lm nh th cho cc im khc trong ao. Sau khi thu mu s c 3 x hn hp mu i din cho ao, tng ng 3 ln lp li. 2.3.2 Dng c thu mu v cch thu - Nn s dng ng PVC (ng knh 10 cm, di 1 - 1,2m) thu mu nc hoc bn y ao. - i vi mu nc, chiu cao ct nc cn thu ty theo ao nng hay su, trnh khuy ng nn y ao khi thu mu nc. Trong trng hp y ao b khuy ng trong khi ang thu mu nc, th nn b mu thu mu khc gn ni . - i vi mu bn y, nn thu nh nhng trnh vt cht dinh dng trong bn b thi ra Sau khi thu mu cn loi b rc, si, ... Cn trn mu hn hp cho tht u ri cho vo chai nha 200mL mang v phng phn tch. 15 7

Qun l cht lng nc nui trng thy sn 3 PHNG PHP PHN TCH MT S CH TIU MI TRNG NC 3.1 Nhit xc nh nhit ca nc, ngi ta thng dng nhit k thy ngn c chia o C). Mun xc nh nhit ca nc tng mt, ta c bu t 0-50oC (ti a l 100 thy ngn ca nhit k vo trong nc su 15-20 cm, cho n khi nhit trong nhit k khng i (khong 5 pht), sau nghing nhit k v c nhit ca nc xong mi ly nhit k ln khi mt nc. Mun xc nh nhit ca nc tng gia hay tng y ca thy vc, ta cm nhit k vo np bnh thu mu nc, th bnh xung ng v tr cn xc nh nhit , cho nc vo y bnh, yn 5 pht sau ko ln v c ngay nhit nc tng . Chng ta cng c th o nhit bng my, hin nay mt s my o pH hay DO c ch to c th o c c ch tiu nhit . 3.2 pH 3.2.1 Bng hp giy so mu Giy c tm dung dch ch th mu thch hp, sy kh cho vo hp s dng. Khi c thm t giy s hin mu. Ty thuc pH ca nc, giy s hin mu khc nhau. Sau em so mu vi bng mu tiu chun km theo trn np hp, ta s bit c pH ca nc. 3.2.2 Phng php in th-my o pH + Ion H hot ng (pH) c xc nh trc tip bng php o in th. Sc in ng + E ca t bo Galvanic c lin quan n hot ng ca ion H trong dung dch theo + phng trnh Nernt. in th sinh ra t t bo t l vi nng ion H trong mu nc, in th ny c o bng mt in th k v c thit b c bit dch sang tr s pH hin trn mn nh ca my. T bo Galvanic bao gm 1 in cc thy tinh, v 1 in cc Calomel tip xc vi - in cc. Khi tip xc vi mu nc, in mu nc bng 2 mt tia Aming cui cc Calomel s xy ra phn ng: Hg Cl + 2e 2Hg + 2Cl in + cc thy tinh gm 1 in cc Ag-AgCl + ngm trong dung dch HCl 0,1M v + c bao bc bi 1 mng thy tinh c nhy cm rt cao vi ion H . in th ny + ca in cc s xut hin khi ion H c mng thy tinh hp th. S hp th 1 ion H trn mng thy tinh s phng thch 1 ion Li t mng thy tinh vo dung dch in cc. Theo Peters (1975) th t bo Galvanic i vi vic xc nh pH c th c vit nh sau: Ag / AgCl, HCl (0.1M) / mng thy tinh / mu nc / Hg Cl , KCl / Hg. 2 2 158

Phn tch cht lng Tt c in th trong t bo Galvanic u khng thay i, tr in thnc gia mng thy tinh - mu nc v gia mu nc - dung dch KCl trong in cc Calomel. 3.3 trong (Transparency), c (Turbidity) C nhiu cch xc nh trong v c ca nc, nhng k thut ph bin nht cho vic nui thy sn l s dng a secchi o trong. c c th c o chnh xc bng cch s dng my o c theo phng php Nephelometric. Ngoi ra c th xc nh lng vt cht l lng trong nc thng qua lng cht rn ho tan (TDS) v tng lng cht rn l lng (TSS) 3.3.1 o trong bng a Secchi a secchi dng hnh trn lm bng vt liu khng thm nc (inox, thic, tole...) chia a lm 4 phn u nhau, sn hai mu en v trng xen k nhau. a c treo trn mt que hay trn mt si dy c nh du khong cch mi khong chia l 5 hoc 10cm. Khi o, cm u dy th t t cho a ngp nc v ghi nhn ln 1 khong cch t mt nc n a khi khng cn phn bit c hai mu en trng trn mt a. Sau cho a secchi su hn v tr va ri v ko ln n khi va phn bit c hai mu en trng, ghi nhn khong cch ln 2 trong ca nc ao o bng a secchi l trung bnh ca hai ln ghi nhn khong cch. 3.3.2 o c bng phng php Nephelometric o Thit b o c c cc b phn d nh sng c t v tr vung gc (90 ) so vi chm tia ti c gi l my o nh sng khuch tn. Phng php ny c da trn vic so snh cng nh sng tn sc ca mu (trong iu kin xc nh) vi cng nh sng khuch tn ca mu chun i chng trong iu kin tng t. Cng nh sng khuch tn cng cao th c cng cao. Formazin polymer c s dng lm cht l lng trong mu chun. c ca nng cht l lng bng formazin c xc nh n 4000 NTU. Ngoi ra, mt s thit b o c c thit k xc nh c theo n v mg/L (Model QWC-22A-TOA, Nht). Cht l lng tiu chun c s dng lm dung dch i chng l Kaolin tinh ch (theo h thng cng nghip Nht bn-JIS). C th o c d dng bng cc my o nu trn. 3.4 Tng cht rn ha tan (TDS) v tng cht rn l lng (TSS) Cht rn hin din trong nc bao gm vt cht ha tan v khng ho tan. 15 o c tng lng cht rn ho tan (TDS). Mu cn c lc loi b vt cht khng 9 ho tan, v nc c lc cho bc hi v phn cn li c cn tnh hm lng cht

Qun l cht lng nc nui trng thy sn rn ha tan. Tng lng cht rn ha tan bao gm vt cht hu c v v c ho tan, biu th bng mg/L. Tng lng cht rn l lng (TSS) c tnh bng cch cn trng lng nhng cht cn li trn giy lc c s dng khi lc nc phn tch cht rn ho tan. TSS biu th lng vt cht khng ha tan l lng trong nc v c biu th l mg/L. Vt liu v dng c dng phn tch tng cht rn ha tan v tng cht rn l lng o gm: Giy lc si thy tinh, t nung 550 C, bnh lm ngui ht m, h thng lc chn khng, cn phn tch. 3.4.1 Tng cht rn ha tan TDS (Total Dissolved Solid) o Thu mu vo bnh 1 lt v y kn. Bo qun lnh 4 C Ngm giy lc thy tinh trong 24 gi, sau sy kh o Nung cc s (a snh) nhit 550 C trong 30 pht, sau lm ngui trong bnh ht m v cn khi lng ca cc s (W ) 1 Lc nc bng h thng lc chn khng. Ly 100mL c lc cho vo cc s c chun b sn. o o t cc s vo t sy nhit 95 C. Sau gia tng nhit ln 105 C trong 1gi. Lm ngui a v cn trng lng 2 (W ) 2 Tng lng cht rn ha tan c tnh theo cng thc sau: (W W TDS (mg / L) 2 x1000 ) = 1 Trong : W2: Trng lng a ln 2 (mg) V W1: Trng lng a ban u (mg) V: Th tch mu nc 3.4.2 Tng cht rn l lng - TSS (Total Suspended Solid) o Thu mu vo bnh 1 lt v y kn. Bo qun lnh 4 C Lc mu bng giy lc c cu to bng cht liu si thy tinh ng knh 47 mm, c lc 0,22-0,45 m. nh s mu trn giy lc. o Sy giy lc 105 C trong 2-3 gi. Cn v ghi khi lng giy lc (W ) o Lc u mu nc trc khi lc. 160

Phn tch cht lng nc Lc mu nc, ghi th tch mu nc lc (V mL) oC trong 2-3 gi, ht m 30 pht trong bnh ht m, cn khi lng (W ) Sy 105 1 o Nung 550 C trong 2-3 gi, ht m 30 pht trong bnh ht m, cn khi lng (W ) 2 Cc ch tiu v vt cht l lng c tnh theo cng thc sau: (W W TSS (mg / L) 1 x1000 ) = 0 x1000 OSS (mg / L) V = W ISS (mg / L) =(W TSS OSS ) 1 2 V V: th tch mu nc lc (mL) W: khi lng (mg) TSS: tng vt cht l lng (mg/L) OSS: vt cht hu c l lng (mg/L) (OSS = Organic Suspended Solid) ISS: vt cht v c l lng (mg/L) (ISS = Inorganic Suspended Solid) 3.5 dn in (EC) dn in l kh nng mang mt dng in ca dung dch. Kh nng ny ty thuc vo s hin din ca cc ion, tng nng , tnh linh ng, ha tr ca cc ion v nhit lc o c. Cc dung dch ca hu ht cc hp cht v c l cc cht dn tt nhng ngc li i vi cc phn t hu c c tnh dn in km. n v o dn in l micromho/cm ( mho/cm) hoc theo h thng n v o lng quc t (SI) l millisiemens/m (mS/m); 1 mS/m=10 mho/cm v 1 mho/cm=1 S/cm. Trong nc ngt, dn in thng t 50 n 1.500 mho/cm (Theo Hip hi sc khe cng ng ngi M-APHA, 1989; Arce v Boyd, 1980), mi trng nc l v mn th dn in cao hn nhiu. dn in v nng mui c lin quan rt cht v nng cc ion trong mi trng, dn in tng cng vi s tng nng mui. Vic o c chnh xc dn in thng khng c i hi cao i vi nui trng thy sn, m thay vo vic o nng mui ca nc thng c s dng hn. My o n in thng c s dng c tnh nhanh mc khong ha ca nc thin nhin v mc nhim ngun nc thi cng nghip. 3.6 Nng mui Thut ng nng mui ch tng nng cc ion h a tan trong nc. n v tnh l mg/L hoc phn ngn (). c tnh nng mui ca nc mt cch tt nht th 16 1

Qun l cht lng nc nui trng thy sn cn tnh tng nng 7 ion quan trng trong mi trng lm cho nc thin nhin c + , K ,+Ca , Mn 2+ , Cl , SO , v HCO nng mui l: Na 4 3 v cc ion ny thng 2+ s cc - ion ha 2-tan trong nc. chim hn 95% trong tng o nng mui chng ta c th s dng t trng k, nhng mc chnh xc ca dng c o ny khng cao. Trong lnh vc thy sn, thit b o nng mui c s dng ph bin nht l khc x k v my o nng mui. 3.7 Oxy ha tan (DO) 3.7.1 Phng php Winkler Nguyn tc Trong mi trng baz mnh, oxy ha tan trong nc s oxy ha ion2 thnh + Mn 4+ 2 ta nu. Mn c kt 2 2 2 + MnMnO + 2OH + 1/ 2O MnO 2H Om c. Trong mi trng acid, MnO Sau c ha tan=bng H + SO 2 2- 4 2 cht oxy ha mnh, c kh nng oxy ha I thnh I bng ng vi lng I c trong 2 2 l mu nc lc ban u: - + 4H + = Mn 2 + I + 2H O MnO2 + 2I 2 2 + I c gii phng ra s ha tan trong nc v c xc nh bng phng php 2 chun vi dung dch Na S O . H tinh bt c s dng lm cht ch th xc 2 2 3 nh im tng ng trong qu trnh chun ny: Khi I c mt trong dung dch, 2 n s kt hp vi tinh bt hnh thnh mt phc cht c mu xanh. Khi tt c I trong 2 dung dch c chun ht vi Na S O , dung dch s tr nn khng mu. 2 2 3 Thu mu Thu mu nc vo l nt mi nu 125 mL, cho ha cht c nh bng 1 mL MnSO 4 kt v 1mL dung dch KI-NaOH, y np l li, lc u, trong l xut hin ta. Ch , khi thu mu v sau khi c nh khng bt kh xut hin trong chai khi thu mu nc. Thuc th - Dung dch MnSO : Ha tan 50 g MnSO .5H O hay 41 g MnCl .4H 2O vi nc 4 2 2 ct thnh 100 mL.4 - Dung dch KI-NaOH: Ha tan 50 g NaOH v 15 g KI (hay 14 g NaI) vi nc ct thnh 100 mL. - 1000mL H SO nc (d=1,84) hay H PO c (d= 1,88). ct 2 4 3 4 - Dung dch Na S O tiu chun 0,1N: Pha mt ng Na S 2O 3 tiu chun 0,1N trong 2 2 3 2 16 2

Phn tch cht lng nc - Dung dch Na S O 0,01N: S dng cng thc N V 1 = N 2V 2 pha 2 2 3 1 dung dch c th nh sau: Ly 50 mL dung dch Na S O 0,1N pha long vi nc ct o thnh 2 2 3 2 2 500 mL. C - Ch th h tinh bt 1%: Ha tan 0,49 g3K S O trong 100 mL nc m (t 80-90 ) khuy u cho n khi dung dch mu trong sut, cho vo 0,5 mL formaline nguyn cht s dng c lu. Tin hnh - Sau khi c nh bng ha cht, yn cho kt ta lng. Tip tc lc u mt ln na kt ta hon ton, sau yn 5 pht i vi nc ngt, 10 pht i mu nc l mn. - Cho tip 2 mL H SO hay H PO m c (vn khng cho bt kh 2 4 3 4 xut hin trong l) - Lc u cho n khi kt ta ha tan. Dung dch c mu vng nu - ong 50 mL dung dch va c acid ha trn, cho vo bnh tam gic 100 mL. - Chun bng dung dch Na S O 0,01N cho n khi dung dch c mu 2 2 3 vng nht, cho 3 git ch th h tinh bt, lc u dung dch c mu xanh, tip tc chun cho n khi dung dch chuyn t mu xanh sang khng mu th dng li. . - Ghi th tch (V mL) dung dch Na S O 0,01N s dng chun mu. 1 Na S O 0,01N 2 2 3 Tnh V trung bnh ca dng Lm tng t 2 hoc 3 ln, ghi 3 th tch dung dch Na S O 0,01N dng chun 2 2 chun 2 2 3 V = (V +V +V ) / 3 TB 2 3 Tnh kt qu 1 TB x 8 x N x1000 V M Trong : V : l th tch trung bnh dung dch Na S O 0,01N (mL) trong cc T 2 2 3 chun . ln B N : l nng ng lng gam ca dung dch Na S O s 2 2 3 dng. = 8 : L ng lng gam ca oxy. V : l th tch (mL) mu nc em chun . 1000: l h s chuyn i thnh lt M 3.7.2 Phng php in cc oxy ha tan) - my o oxy Theo phng php ny th p sut ring phn ca oxy ha tan c o trc tip. Sau p sut ring phn c chuyn i thnh nng (mg/L). My o oxy tnh ton DO(mg / L) V

16 3

Qun l cht lng nc nui trng thy sn cc gi tr ny da trn mi quan h gia nhit , ha tan ca oxy v p sut khng kh. u d oxy bao gm 1 in cc dng (anode) c lm t Ag/AgCl, 1 in cc m (cathode) c lm t kim loi qu nh platinum, vng, tungsten hoc rhodium v dung dch in cc KCl bo ha ngn cch vi mi trng ngoi bi mng cm ng polyethylene, teflon, polypropylene hoc vt liu tng t c dy thng 25 m hoc mng hn (c kh nng thm oxy). Cc in cc trong h thng ny c 1 hiu in th gia chng thng khong 0,7 volts. Khi oxy trong mu nc tip xc vi mn cm ng, mn c kh nng thm oxy v t l m oxy i qua mng cm ng c lin quan n p lc ca oxy trong mu nc. Khi cung cp mt hiu in th cho u d th oxy phn t thm thu qua mng, phn ng vi cc cathode v b kh2 thnh 2 hydroxide vi t l 4 moles OH /mole oxy theo phng trnh sau: O +2H O + 4e 4OH Sau 1 dng in chy qua cc anode (in cc bng bc) v OH phn ng vi bc 0 bc theo - phng trnh sau: to thnh dng oxit 2 2 2Ag + 2OH = Ag O + H O + 2e . Do , s chnh s khc bit v p lc oxy gia trong v ngoi mng cm ng lm cho oxy thm thu qua mng. V vy, nu p lc oxy bn ngoi mng cm ng thp th dng in gia 2 in cc s t hn so vi khi p lc oxy bn ngoi cao. o o Ngoi ra, tnh thm ca mng cm ng b nh hng rt ln bi nhit (Mancy v Jaffe, 1966) (Trch dn bi Boyd & Tucker, 1992). Th d, dng in to ra 10 mg/L oxy ha tan 10 C ch bng 1/ 4 so vi vic to ra 10 mg/l 30 C. Bn cnh , nhit cn nh hng i vi dng in gia 2 in cc thng qua mi quan h v nhit v p lc oxy. Do , hu ht cc my o oxy ha tan trong nc thng c thit k c b phn hiu chnh nhit t ng trnh sai s do s nh hng ca nhit ln s liu o c. Hm lng oxy ha tan trong nc cng b nh hng bi nng mui. Hm lng oxy ha tan trong nc mc bo ha gim khi gim p sut khng kh v tng nng mui. V vy, hu ht cc my o oxy thng c thit k c s hiu chnh p sut v nng mui tng chnh xc trong o c. 3.8 Carbon dioxide (CO ) 2 3.8.1 CO Nguyn + tc NaOH = (7.6) 2 CO t do trong nc c xc nh bng phng php trung ha vi dung dch 16 2 NaHCO3 NaOH tiu chun v phenolphthalein lm cht ch th xc nh im tng ng 4

Phn tch cht lng nc Khi phn ng (7.6) t im tng ng, mt git d dung dch NaOH s lm cho mi trng c tnh kim yu (pH 8-10) phenolphthalein s chuyn t khng mu sang mu hng. Mun c kt qu chnh xc ta phi dng dung dch m c pH tiu chun bng 8,3 theo di s chuyn mu ca phenolphthalein m xc nh chnh xc im tng ng ca phn ng 3.8.2 Phng php thu v bo qun mu Thu mu trong chai nt mi trng 125 mL, c nh mu bng 0,5mL Chloroform 3.8.3 Chun b ha cht - Dung dch NaOH tiu chun 0,1N: Ha tan ng chun NaOH 0,1N vi nc ct thnh 1000mL - Dung dch NaOH 0,01N: Ha tan 100mL dung dch NaOH 0,1N vi nc ct thnh 1000mL. - Dung dch m pH= 8,3: Dung dch Na B O 0,05M: Ha 2 4 7 tan 1,91g Na B O .10H O vi nc ct thnh 100mL. 2 4 7 2 - Dung dch H BO 0,2M: Ha tan 1,24 g H BO vi nc ct thnh 100mL. 3 3 3 3 - Ly 20mL dung dch Na B O 0,05M cho vo 30mL dung dch H BO 3 0,2M. 2 4 7 3 Ta s c dung dch m c pH=8,3. - Dung dch ch th phenolphthalein 1%: Ha tan 1g ch th phenolphthalein 0 (C H O ) trong 100mL cn 60 . 20 14 4 3.8.4 Tin hnh Bnh 1 Bnh 2 Dng bnh tam gic 100mL, ln lt cho vo bnh cc ha cht nh sau (Bng 7.5): 1. 50mL dung dch mphn1. 50mL mu nc. Bng 7.5. Cc bc tin hnh tch hm lng CO 2 pH= 8,3 2. 3 git ch th phenolphthlein, lc u, 2. 3 git ch th phenolphthlein, dung dch khng mu. lc u, dung dch c mu hng nht. 3. Dung dch NaOH 0,01N chun t t cho n khi dung dch trong bnh c mu hng nht ging nh bnh 1 th dng li ( mu hng ch bn trong 1 pht). Ghi th tch V (mL) dung 1 dch NaOH 0,01N s dng. 4. Lm li cc bc 1 n 4 mt ln na ghi th tch V (mL) dung dch NaOH 0,01N s dng. 2 5. Tnh V = (V + V )/2. TB 1 2 16 5

Qun l cht lng nc nui trng thy sn 3.8.5 Tnh kt qu L) = - V CO TB x 44 2 x N x1000 : l th tch50 trung bnh dung dch NaOH 0,01N ca c ln chun . (mg / V

tb - N: l nng ng lng ca dung dch NaOH s dng. - 44: ng lng g ca CO . 2 - 50: th tch nc em chun . 3.9 Tiu hao oxy ha hc (Chemical Oxygen Demand - COD) 3.9.1 Phng php oxy bng KMnO trong mi trng kim 4 Thu v bo qun mu

Thu mu trong chai nt mi trng 125 mL, c nh mu bng 2 mL H SO 4M 2 4 Nguyn tc Vic xc nh hm lng COD c da trn nguyn tc cc hp cht hu c trong nc c th b oxy ha thnh CO v H O bi cc cht oxy ha mnh (KMnO ) 2 2 4 trong mi trng kim. 4 Trong mi trng baz, ion tc dng vi ion OH nh gc (OH) t do. - + OHMnO4 =MnO 2 s + (OH) MnO 4 hy cho ra oxy nguyn t. Gc (OH) ny khng bn n s phn 2(OH) = [O] + H O 2 Oxy nguyn t trng thi mi sinh l cht oxy ha mnh, c kh nng oxy ha hon ton cc hp cht hu c thnh CO + y/2H O 2 2 Sau mi trng c acid ha bng dung dch H SO . Trong mi trng acid, 2 4 vi 4 cn li s b kh hon ton thnh s hin din ca mt lng tha I , lng MnO 2 Mn v mt phn I b oxy ha thnh 2 I. + 10KI + 2KMnO + 8H SO = 5I + 2MnSO 4 + 6K 2SO 4 +8H 2O 4 2 4 2 I c to thnh c xc nh bnh phng php chun vi dung dch Na S O 2 chun ging nh phng php xc nh Oxy ha tan trong nc theo phng 2 2 3 tiu php Winkler. T lng I c to thnh trong mu tht v mu trng ta tnh c 2 lng oxy cn thit oxy ha hon ton cc hp cht hu c trong mu nc thnh CO v H O. 2 2 Thuc th 16 6 v H O. 2 2 CxHyOz + (2x + y/2 - z) [O] = xCO

Phn tch cht lng nc 0,1N: Ha tan 1 ng KMnO 0,1N trong mt t nc ct, 4 4 sau pha long thnh 1.000mL. iu chnh nng chnh xc bng dung o 4 15mL H SO 4 1:4 lc u em dch chun H chuyn O tiu chun 0,1N v C C dch n khi dung un nng 2 2 4 t khng mu sang mu hng 2 nht th dng li, ghi nhtch 80 . Sau KMnO dng dung dch KMnO phali trn ln t t cho th dung dch s dng (V va ). Lm nh chun trn mt na 4 1 ly gi tr trung bnh. Nng dung dch KMnO c iu chnh chnh xc 4 bo qun trong chai nu. bng cng thc: V N = V N . Dung dch c 1 1 2 2 - Dung dch KMnO 0,05N tnh kim: Ha tan 500mL dung dch KMnO trong 4 500mL nc ct c4ha tan 8g NaOH, cho vo bnh mu nu s dng. - Dung dch H KI 10%: 10g KI vi nc thnh 100mL. SO Ha 4M:tan Ha tan 22,2mL H ct SO m c vi nc ct 2 4 2 4 thnh 100mL. - Dung dch Na S O 0,1N: Ly 1 ng Na S 2O 3 0,1N chun pha long vi 2 2 3 2 nc ct thnh 1.000mL. - Dung dch Na S O 0,05N: Ly 500mL dung dch Na S 2O 3 0,1N dng 2 2 3 2 nc o ct opha long thnh 1.000mL. - 7. Ch th h tinh bt 1%: Ho tan 1 gam tinh bt trong 100mL nc m (t 80 C-90 C) khuy u cho n khi dung dch tr nn trong sut, cho vo 0,5mL formaline nguyn cht s dng c lu. - Dung dch NaOH 0.4N: Ly 40mL dung dch NaOH 10N, dng nc ct pha long thnh 1.000mL Tin hnh Dng 2 cp bnh tam gic 100mL, ln lt cho vo tng cp bnh cc ha cht sau (Bng 7.6): - Dung dch KMnO

16 7

Qun l cht lng nc nui trng thy sn Bng 7.6. Cc bc tin hnh phn tch COD Bnh 2 Bnh 1 1. 50mL nc ct. 1. 50mL mu nc. 2. 5mL dung dch NaOH 0,4N. 2. 5mL dung dch NaOH 0,4N. 3. 5mL dung dch KMnO 0,05N. 4 3. 5mL dung dch KMnO 0,05N. 4. em un cch thy im 4 4. em un cch thy im si si ng ng gi, ra KI 10% ngui 5. Tip tc vo 5mL KI 10% v 5mL dung mt 5. Tip tcly vo 5mL v 10 mt gi, ly4M, ra ngui 10 pht. 5mL dch H SO lc u dung dung dch H SO 4M, lc u 2 4 2 4 pht. dch c dung 6. Dng dch nu. Na S 0,05N mu vng nu. dch c dch mu vng 2 chun cho n khi dung dch O 6. Dng dch dch Na S O 0,05N c 2 3 2 2 3 chun cho n khi dung dch c mu vng mu vng nht, cho v 3 git ch th nht, cho v 3 git ch th h tinh bt h tinh bt 1%, lc u dung 1%, lc u dung dch c mu xanh, dch c tip tc chun t t cho n mu xanh, tip tc chun t t khi dung cho n khi dung dch tr nn khng dch tr nn khng mu th dng li ghi mu th dng li ghi th tch (V ) 2 th tch (V ) dung dch Na S O dung dch Na S O 0,05N 1 2 2 3 s 0,05N 2 2 3 dng. s dng. Tnh kt qu 7. Ly bnh cn li chun tng t nh7. Ly bnh cn li chun tng t nh bnh trn ly ga tr trung bnh. bnh trn ly gi tr (V trung V bnh. ) COD(mg / L) 2 1 x8 = x1000 xN - N: nng dung V dch Na S O chun 2 2 3 M - V : th tch dung dch Na S O chun mu nc cn phn tch. 1 2 2 3 - V : th tch dung dch Na S O chun mu nc ct. 2 phn 2 tch. 3 - V 2 : th tch mu nc em M 3.9.2 Phng php Dichromate Nguyn tc Trong phng php ny cc hp cht hu c trong nc b oxy ha thnh CO v 2 H O bi cht oxy ha mnh (K Cr O ) trong mi trng acid. Mt lng bit trc 2 2 2 7 K Cr O c thm vo mu nc s b acid ha vi H SO 4. Mu nc ny sau 2 un 2 7 c nng v cc cht hu c b oxy ha thnh 2 CO v H O, trong khi 2 2 2 +trnh 3 2Cr + CO + H Dichromate b kh theo sau: Cht hu c + Cr phng 2 + O 2 7 +H O 16 2 8

Phn tch cht lng nc Lng tha dichromate c th xc nh c bng cch chun vi ferrous ammonium sulfate - Fe(NH ( SO ) 2.6H 2O. 4 2) 4 2 + 14H+ 6Fe 3+ 2Cr 3 + 7H 6Fe2 + Cr O 2 + + + Lng dichromate 7 tiu O th cho vic oxy ha cc cht hu c c th c tnh ton t 2 mN (mili ng lng) ca K Cr O thm vo mu tr mN 2 2 7 ca Fe(NH (SO ) 2.6H 2O s dng trong vic chun kh lng K 2Cr 2O 7 tha. 4 2) 4 3.10 Nng sut sinh hc s cp C nhiu cch xc nh xc nh nng sut sinh hc s cp ca thy vc nh: phng 14 php bnh ti- bnh sng, phng php ng v phng x C , phng phc xc nh hm lng cc sc t quang hp trong nc, phng php xc nh sinh khi thc vt ni, phng php xc nh theo hm lng oxy trong nc. Phng php bnh ti - bnh sng c s dng ph bin hn c. Hm lng oxy t do trong nc c xc nh theo phng php Winkler 3.10.1 Nguyn tc Phng php bnh ti - sng da trn nguyn tc trong c th thc vt lun lun xy ra hai qu trnh ngc nhau, qu trnh to thnh v qu trnh phn hy cc vt cht hu c. Qu trnh to thnh cc hp cht hu c bng con ng quang hp s b dng li khi khng c nh sng, do s hp thu CO t mi trng v 2 lng O 2 c thi ra cng b dng li. Qu trnh h hp hp th O v thi ra CO tin hnh 2 2 vi tc ngang nhau trong ti v ngoi sng. Do da trn hm lng O ha tan trong bnh ti v bnh sng ta c th tnh c cng quang hp ca thc 2 vt ph du trong nc. Trong thc t i khi cng quang hp ca thc vt c coi l - Thy vcs ngho P1(1960), t 1-2 mg/L O xut / ngy, nng sut sinh hc cp. dinh Theodng: Winberg sc sn ca m thy vc theo nng 2 sut sinh - hc s cp (P) c trnh by bng sau: Thy vc dinh dng trung bnh: P1 t 2-5 mg/L O / ngy, 2 - m Thy rt giu 3.10.2 Dng c vc v ha cht dinh dng: P1 t 15-20 mg/L O / ngy, 2 m Dng c - H thng bnh sng- bnh ti: Cc bnh ti c chun b nh sau: dng hc n bi en ton b thnh bnh v y bnh. - a secchi: xem phn xc nh trong ca nc. Ha cht - Thy vc giu dinh dng: P1 t 5-15 mg/L O 2/ ngy, m

16 9

Qun l cht lng nc nui trng thy sn - Ton b ha cht xc nh ha tan theo phng php Winkler (xem mc 3.7.1). 3.10.3 Tin hnh Dng a secchi o trong ca nc, nhn trong vi 2 xc nh tng sng. Nu thy vc tng sng nh th ch cn thu mu v t bnh v tr gia ao v cch mt nc khong 20-30cm. Nu thy vc c tng sng ln (su), khi thu mu nc cn t bnh gc ao, gia ao, tng mt v tng y. mi v tr dng 6 bnh BOD 125mL (4 bnh sng v 2 bnh ti), thu y mu nc v tr theo nng sut sinh hc s cp. Ly 2 bnh sng phn tch O ban u u 2 (DO ), 4 bnh cn li dng gi t ng v tr cn thu mu nuc trn, yn trong ly ln phn tch hm lng O ha tan trong mi bnh v DO 24 gi 2 (DO ). CS CT 3.10.4 Tnh kt qu P (mg O /L/ngy) = DO - DO 2 CS CT R (mg O /L/ngy) = DO - DO 2 sinh hc (tng CT lng P : Nng sut oxy c to ta t qu trnh quang hp) P' (mg O /L/ngy) = DO - DO 2 ca thy sinh vt CS(tng R: H hp lng oxy tiu hao do qu trnh h hp) P': Nng sut sinh hc thc (s chnh lch gia oxy sinh ra t quang hp v oxy tiu hao do h hp. P' l s dng (+) khi thc vt c gia tng sinh khi, P' l s m (-) khi thc vt gim sinh khi. DO DO CS : Hm lng oxy cui (C) bnh sng (S), c o sau 24 gi

: Hm lng oxy cui (C) bnh ti (T), c o sau 24 gi CT DO : Hm lng oxy u (), c o lc bt u 3.11 Chlorophyll-a 3.11.1 Nguyn tc Phng php chit sut bi Ethanol 90% (Nusch, 1980). Cc sc t trong nc sau khi c lc qua mng lc ng knh 47mm, kch thc lc 0,22-0,45 m. Chng c chit sut bi ethanol. Sau c o bc sng 665 nm v 750 nm cc pheophytin c o cng bc sng sau khi x l acid. Phng php chit sut bi acetone Phng php ny c b sung bi Lalli (1984). Trong phng php ny, chloropyll c chit xut trong acetone v o mc hp thu quang ph 4 bc sng. 170

Phn tch cht lng nc 3.11.2 Tin hnh Ho cht Dung dch acetone nguyn cht Tin hnh - Ct nh giy lc mu cho vo ng nghin, - Thm 10mL acetone 100% v nghin trong mt pht - Lc qua giy lc GFF 25mm-0,2 m, ng thi thu mu dch chit sut vo chai, l 10mL nu. - Bo qun lnh v ti cho n khi o mu - o mu cc bc sng 630, 647, 664 v 750 nm. Tnh kt qu Chl-a = [11,85(E -E ) - 1,54(E -E ) - 0,08(E 630-E 750)]/[(1/d) x 664 750 647 750 (V 1*1000)/V 2] ( g/L) V : th tch acetone (10 mL) 1 : th tch nc mu c lc d: V di truyn quang (cuvet 1cm). 3.12 2 Hydrogen sulfide (H S) 2 3.12.1 Phng php Iodine Nguyn tc H S trong mu nc c cha H S s b kt ta CdS khi phn ng vi CdCl . 2 2 2 CdCl + H S = CdS + 2HCl 2 2 Sau CdS c ha tan bng mt lng tha I chun, trong mi trng acid. 2 CdS + I + 2HCl = S + CdCl + 2HI. 2 2 Lng tha I c xc nh bng phng php chun vi dung dch Na S O 2 2 2 3 tiu chun v h tinh bt c dng lm cht ch th xc nh im tng ng, ging nh qu trnh xc nh oxy ha tan trong nc bng phng php Winkler. I + I tinh bt + 2Na S O = Na 2S 4O 6 + 2NaI 2 2 2 3 xanh) (khng 2 + (mu tinh bt. mu) Thu v bo qun mu Tin hnh thu mu trong chai nt mi nu, c nh mu bng 1mL CdCl Thuc th - Dung dch CdCl 2%: Ha tan 2 g CdCl vi nc ct thnh 2 2 100mL. 17 1 2

Qun l cht lng nc nui trng thy sn - Dung dch HCl 4M: Cho 25mL HCl c (12M) vo v pha long thnh 100mL vi nc ct. dch I 0,1N: Ha tan 80 g KI trong 500mL nc ct khng, tip tc cho - Dung 2 vo12,7 g I khuy u cho tan ht, sau pha thnh 1.000mL. Dung ny sau 2 khi pha xong phi xc nh li nng chnh xc bng dung dch Na S O 2 2 3 0,1N tiu chun. cch tin hnh nh sau: Dng bnh tam gic 100mL, cho vo 20mL dung dch I va pha trn (dng buret xc nh th tch I , khng 2 dung dch Na S O 0,1N tiu chun, chun 2cho n dng ng ht), dng 2 2 3 khi dung dch c mu vng, tip tc chun cho n khi dung dch c mu vng nht, cho 3 git h tinh bt, lc u dung dch c mu xanh, tip tc chun cho n khi dung dch chuyn t mu xanh sang khng mu th dng li, ghi th tch dung dch Na S O 0,1N s dng. Lm li nh trn mt ln na - Dung dch I 0,01N:2 ly 2 50mL 3 I 0,1N dng nc ct pha long thnh 2 2 chnh nng dung dch I cho ly gi tr V trung bnh. Sau hiu 2 500mL. chnh xc - bng Dungbiu dchthc: Na S N V O = tiu N chun V 0,1N: Pha mt ng Na S 2O 3 tiu chun 0,1N 2 1 2 1 3 2 2 2 trong 1000mL nc ct - 500mL. Dung dch Na S O 0,01N: S dng cng thc N V 1 = N 2V 2 pha 3 Ho tan 0,49 g K S O trong 1 100mL nc m (t dd cth th - Ch h tinh 2 bt 2 1%: 2 2 3 nh sau: Ly u 50mL dung dch S dch O mu 0,1N pha sut, longcho vi vo nc ct 900C) khuy cho n khi Na dung trong 0,5mL 2 2 3 80thnh formaline nguyn cht s dng c lu. Tin hnh Thu mu nc vo 2 l nt mi 125mL, sau m np l ra, cho ln lt vo mi l 1mL dung dch CdCl 2%, y np l li lc u mt ln na, yn 24 gi (nu c 2 H S s c kt ta mu vng di y bnh). 2 M np l ra dng ng cao su ht b phn nc trong trn kt ta (ch : khi ht cn ng cao su gn mt nc ch khng c cm su vo y bnh v cho nc chy nh ra ngoi, nu nc chy mnh kt ta b vn ln v cun tri ra ngoi, lm kt qu khng chnh xc ). Ha tan kt ta bng 5mL HCl 4M v 5mL dung dch I 0,01N. Chuyn dung dch t 2 30mL nc ct, nc ct l nt mi sang bnh tam gic 100mL, trng l nt mi bng ny cng cho vo bnh tam gic. Dng dung dch Na S O 0,01N chun cho n khi dung dch mu vng nht, cho 2 bt, 3 lc u dung dch c mu xanh sau tip tc chun vo 3 git ch th h2tinh t t cho n khi dung dch chuyn t mu xanh sang khng mu th dng li, ghi tng th tch V 17 2 1 (mL) dch Na 2 S 2 O 3 0,01N s dng.

Phn tch cht lng nc Lm tng t nh trn cho l cn li, ghi th tch V (mL) dch Na S O 0,1N 2 2 2 3 s dng. Tnh VTB = (V +V )/2. 1 2 Bnh chun: Dng 2 bnh tam gic 100mL, ln lt cho vo tng bnh cc ha cht nh sau: 30mL nc ct, 5mL HCl 4M v 5mL dung dch I 0,01N, lc u dung dch c mu 2 vng nu . Dng dung dch Na S O 0,01N chun cho n khi dung dch tr nn mu vng 2 h 2 tinh 3 bt vo, lc u dung dch c mu xanh, tip tc chun nht, cho 3 git ch th cho n khi dung dch chuyn t mu xanh sang khng mu th dng li ghi th tch V Na S O 0,01N s dng. Lm tng t nh trn cho bnh cn li 0 2 2 3 ly th tch V trung bnh. 0 (V V Tnh kt x17 x1000 H qu S (mg / L) 0 )xN = TBtrung bnh dung dch Na S O s dng trong 2 ln phn - V 2 : Th tch TB 2 2 3 125 tch mu nc - V : th tch trung bnh ca dung dch Na S O trong 2 ln phn tch mu 0 2 2 3 trng - N: Nng ng lng ca dung dch Na S O s dng. 2 2 3 - 17: ng lng g ca H S. 2 3.12.2 Phng php Methylene blue Nguyn tc 2Nguyn tc ca phng php ny da trn phn ng ca sulfide (S ), ferric chloride v dimethyl-p-phenylenediamine to nn methylene blue. Ammonium phosphate 2c thm vo sau khi hin mu kh mu ca ferric chloride. Sau nng S c xc nh bi my so mu quang ph bc sng 664 nm. Thu mu v bo qun o Tin hnh thu mu trong chai nt mi nu, bo qun lnh 4 C Thuc th Dung dch PRE 1: 500mL HCl 37% pha thnh 1000mL vi nc ct. H Cl N trong PRE 1 thnh 1000mL. 8 14 2 2 Dung dch B: Ha tan 16g FeCl .6H O trong PRE 1 thnh 1000mL. 3 2 Dung dch chun 17 3 Dung dch A: Ha tan 4g C

Qun l cht lng nc nui trng thy sn - Dung dch Na S.9H O 100mg/L: ha tan 0,750g Na S.9H O trong 2 2 2 2 1000mL nc ct khng oxy (nc ct khng oxy: un nc ct ln si khong 10 pht em khi bp bt kn ngay ). ct thnh Dung dch Na S.9H O 5mg/L: ha tan 5mL dd Na S.9H O 100mg/l vi 100mL 2 2 2 2 nc Thit lp mu chun Bng 7.7. Cc bc thit lp mu chun phn tch H S theo phng 2 Methylene blue php Nng STT Th tch dung dch chun Th tch nc ct (mL) Na S.9H O 5mg/L mu 2 2 100,0 1 chun (mg/L) (mL) 2 99,6 0,0 0,00 99,2 3 0,4 0,02 4 98,8 0,8 0,04 5 98,4 1,2 0,06 98,0 6 1,6 0,08 2,0 0,10 Tin hnh - ong 20mL mu nc. - Ln lt cho thuc th vo 1mL thuc th A, 1mL thuc th B - Ch 5 pht khi mu xanh xut hin chng ta em o hp th quang bc sng 665nm. Tnh kt qu tng ng vi nng C ca mu chun ta c hp th quang A. Da vo s tng quan ny chng ta c th lp phng trnh tng quan dng A = aC + b Trong : A: hp th quang C : nng cht chun (mg/L) Sau khi thit lp phng trnh, chng ta o hp th quang ca mu cn phn tch 2v th vo A phng trnh chng ta s tnh c nng ca S c trong mu nc. b C= a tnh hm lng H S khi thu mu nc chng ta phi o pH v nhit . Da vo 2 bng tra (xem Chng 3, Mc 5, Bng 3.5) xc nh t l phn trm ca H S 2 cha trong tng sulfide, t tnh ra hm lng H S. 2 17 4

Phn tch cht lng nc 3.13 cng tng cng Vic xc nh cng tng cng ca nc c thc hin theo phng php chun Complexon. 3.13.1 Nguyn tc 2+ v Mg s kt hp vi thuc th EDTA (Ethylene Trong mi trng pH=10 ion Ca 2+ - K hiu Na H Y ) hnh thnh phc cht bn DiamineTetra-acetic Acid) (EDTA 2 diamine 2 vng, khng mu Calcium hay Magnesium ethylene tetraacetate. Eriochrome black T (C c s dng lm cht ch th xc nh 20 H13O 7N SNa) 3 2+ im tng ng. Eriochrome black T kt hp vi ion Ca v Mg hnh thnh phc 2+ cht khng bn vng c mu hng ca ru vang. Khi dng EDTA chun , cc ion 2+ Ca2 v Mg s kt hp vi EDTA hnh thnh phc cht bn vng, khng mu, v +c Eriochrome khi black T t do, dung dch c mu xanh Trong qu trnh chun ion Ca v Mg bng Na H Y lun gii phng ra 2 ion H , l2. + + +no M-Eriochrome black T + Na = trong Na + trnh 2H Eriochrome black T dung phn lm acid ha mi trng, doY qu chun phi cho 2 H 2 MY + dch 2 (Mu hng ru (mu xanh M m vo mi trng pH ca mi trng khng i trong , vang) l)sut qu trnh chun 2 + 2 2 dung dch m thng l NH 2 OH, NH + Cl. + 4 4 Nu trong mu nc c cha mt lng ng k ion Fe , Cu , Ni ,... th s chuyn mu ca cht ch th s khng r rng, nn cn phi che nhng ion ny trc khi chun bng cch dng cc ion CN hoc S che cc cation . 3+ 2+ 2+ 3.13.2 Thu v bo qun mu o Thu mu trong chai nha v bo qun lnh 4 C 23.13.3 Thuc th - Dung dch Na H Y (EDTA) tiu chun 0,1N: 2 2 Cch 1:Ha tan 18,612 g EDTA (C H O N Na .2H O) (sau sy 80 C, ngui trong bnh ht m) trong 400mL nc ct sau pha long o thnh 10 14 8 2 1000mL. 2 2 Nu khng c mui C H O N Na 2.2H 2O ta c th pha t acid 10 14 8 2 t do C H O N , cch pha nh sau: Ha tan 14,6 g C 10H 14O 8N 2 v 4,5 g NaOH 10 14 8 2 trong khong 400 mL nc ct khuy u cho cc ha cht ha tan hon ton, ngui ti nhit phng, sau dng nc ct pha long thnh 1000mL, dung dch ny sau khi pha long xong phi chun li bng dung dch NaCO tiu chun 0,1ppm bit nng chnh xc ca dung dch. Cch tin 3 hnh nh sau: Dng buret 10mL dung dch CaCO tiu chun 0,1ppm, cho vo 3 175

Qun l cht lng nc nui trng thy sn bnh tam gc 250mL tip tc cho vo 90 mL nc ct (2 ln ct) v 2mL dung dch m pH=10 lc u, dung dch c mu hng ru vang, dng dung dch Na H Y mi pha trn chun trn t cho n khi dung dch chuyn t mu 2 2 hng ru vang sang mu xanh l th dng li, ghi th tch dung dch Na H Y 2 2 s dng. iu chnh nng dung dch Na H Y cho chnh xc bng 2 2

biu

thc: V N = V N 2. 1 1 2 Cch 2: Pha long 1 ng Na H Y (EDTA) 0,1N vi nc ct thnh 1000mL. 2 2 - Dung dch Na H Y 0,01N: ly 50mL dung dch Na H 2Y 0,1N dng nc ct 2 500mL. 2 2 pha long thng - Dung dch pH=10: Ha tan 6,7g NH Cl trong 57mL NH OH m c 4 4 (d=0,91) sau dng nc ct pha long thnh 100mL tip tc cho tip 1mL dung dch MgSO 0,05N v 0,5mL dung dch Na H Y 0,1N lc u. 4 CaCO tiu chun 0,1N: Ha 2 tan 25 gam CaCO trong vi git dung - Dung dch 3 5-10 pht, dng dch HCl 1:1, pha 3long vi nc ct thnh 200mL, un si dung dch NH OH iu chnh pH ca mi trng v bng 7 sau pha long 4 1000mL. vi nc ct thnh - Dung dch MgSO 0,05N: Ha tan 1,232g MgSO .7H O trong mt t nc ct, 4 thnh 100mL. 4 2 sau pha long - Ch th Eriochrome black T: Ly 100g NaCl tinh khit phn tch em rang hoc o sy kh 110 C, ngui nghin mn bng ci chi thy tinh sch. Cn 0,5g ch th Eriochrome black T cho vo 100g NaCl trn trn u v nghin mn, cho vo l nu y np kn. 3.13.4 Tin hnh Trc khi tin hnh cn iu chnh pH ca mu nc v bng 7-8, sau tin hnh phn tch theo cc bc sau: - Dng 2+ ng ong 100mL, ong 100mL mu nc iu chnh v 7-8 cho vo 2+ bnh tam gic 250mL, tip tc cho vo 2mL dung dch m pH=10, v mt lng nh ch th Eriochrome black T (mt nhm bng ht u), lc u nu c ion Ca , Mg trong mu nc s c mu hng ru vang. - Dng dung dch Na H Y 0,01N chun t t cho n khi dung dch 2 2 chuyn 3+ t mu hng ru vang sang mu xang l th dng li, ghi th tch 2+ dung dch Na H Y 0,01N s dng V. Lm li nh trn ln na ly gi tr V trung 2 2 bnh. Nu s chuyn mu khng r, tc l trong dung dch c cc ion cn nh: Fe , Cu th cn tin hnh chun li vi mu nc khc v cch tin hnh nh sau: Sau khi cho 2mL dung dch m pH=10 vo mu nc ta cn thm vo 1mL dung dch KCN 5% che cc ion cn, sau mi thm cht ch th vo v tin hnh chun nh 17 trn. 6

Phn tch cht lng nc 3.13.5 Tnh kt qu VxN cng tng cng (mg x 50 V CaCO /L) M x1000 3 - V l th tch dung dch Na H Y (mL) dng chun . 2 2 - N l ng lng ca dung dch Na H Y s dng. 2 2 - V : th tch mu nc em chun M 3.14 kim tng cng Trong nc thin nhin kim c gy ra do s hin din ca cc mui acid yu, tn ti di cc dng bicarbonate nh: KHCO , NaHCO , Ca(HCO ) , Mg(HCO 3) 3 3 3 2 2... cc cht ny c to thnh trong t do tc dng ca CO vi nhng cht khong c 2 trong t nh CO + CaCO + H O Ca(HCO )2 2 3 2 3 Mt s trng hp, kim trong nc c gy ra do ion carbonate, bicarbonate, 2 cht hu c bin i trong nc. Tuy nhin, silicates, phosphates, ammonium v hp 3 2 4,5 th trong cc ion ng quan tm l HCO -, CO -, OH-. Khi pH nc ln hn 3 3 nc tn ti ion bicarbonate, khi pH ln hn 8,34 thi trong nc c ion- CO . Phng php xc nh kim l phng php chun acid. 3.14.1 kim carbonate hay kim phenolphthalein Cho2phenolphthalein vo mu nc, mu hng xut hin nu mu nc c cha ion 3 2 4 CO 2-. Chun bng H SO 0,01N cho n khi mt mu (pH =8,34), khi ion 3 CO - c trung ha. V vy kim phenoltalein cn c gi l kim 2 CO3 + H+ = HCO 3 carbonate. 3.14.2 kim tng cng Cho ch th methyl orange vo mu nc dung dch c mu vng cam. Chun bng dung dch H SO 0.01N cho n khi dung dch tr thnh mu cam (mi trng 2 4 4,5). Khi tt c + , acid, pH khong cc ion 2OH , CO , HCO , NH 3PO ... c 3 3 4 4 trung ha hon ton. V vy, phn tch vi ch th methyl orange chng ta c kim tng cng + HCO 3 + H HO 2 + CO 2 Thu v bo qun mu Thu mu trong chai nha v bo qun lnh Thuc th Dung dch PRE 1: ha tan 27mL H SO 98% vi nc ct thnh 2 4 1000mL 17 7

Qun l cht lng nc nui trng thy sn Phenolphtalein 1%: ha tan 1g Phenolphtalein trong 100mL C H OH 2 5

Dung dch H SO 0,1N: ha tan 100mL PRE 1 vi nc ct thnh 1000mL 2 4 hay pha long 1 ng H SO 0,1N chun vi nc ct thnh 1000mL. 2 4 Dung dch methyl orange 0,1%: ha tan 0,1g methyl orange vi nc ct thnh 100mL Dung dch chun - thnh Dung dch KHCO 1N: ha tan 10,011g KHCO vi nc ct thnh 100mL 3 3 - Dung dch KHCO 0,1N: ha tan 10mL dung dch KHCO 1N vi nc ct 100mL. 3 3 Tin hnh ong 100mL mu nc cn phn tch vo bnh tam gic 250mL Thm vo 3 git dung dch Phenophthalein, dung dch c mu hng nht. Chun bng dung dch H SO 0,01N n khng mu, ghi th tch (V mL) H SO 4 001N 2 4 1 2 s dng chun . Sau thm tip 3 git dung dch methyl orange, dung dch c mu vng cam. Tip tc chun bng dung dch H SO 0,01N n pH bng 4,5 dung dch 2 4 t mu vng cam chuyn sang mu cam, ghi th tch (V mL) H SO 0.01N. 2 2 4 Lm tng t nh mu nc i vi mu chun KHCO i chng. 3 Tnh kt qu kim tng cng (mg/ V x N x 50 M x1000 CaCO /L) 3 - V = (V + V ) : tng th tch dung M dch H 2SO 4 0,01N cho c 2 ln 1 2 chun - N: nng ng lng dung dch H SO 2 4 - V : th tch mu ong em chun M 3.15 acid (Acidity) + acid biu th kh nng phng thch ion H trong nc, do s c mt ca cc loi acid nh: acid carbonic, acid tanic, acid humic bt ngun t s phn hy cht hu c, mt khc do s thy phn cc mui t cc acid mnh nh Sulfat nhm, st to thnh. 2 Khi b cc acid v c thm nhp vo, nc s c pH rt thp 3 3 Trong nc thin nhin lun duy tr mt th cn bng ngia cc ion HCO , CO , kh CO ha tan, do nc thng ng thi mang hai tnh cht i nhau: tnh acid v 2 tnh kim. 17 8

Phn tch cht lng nc Trong thc nghim, hai khong pH chun c s dng biu th s khc bit trn tng ng vi hai lai cht ch th l methyl orange (pH = 4,2-4,5) v phenolphthalein (pH = 8,2-8,4) 3.15.1 Nguyn tc Dng dung dch kim mnh nh phn acid ca c acid v c mnh cng nh acid hu c hoc acid carbonic yu. Lng acid v c mnh khi nh phn thng vi ch th methyl orange, chun t mu chuyn thnh mu da cam v c gi l acid methyl Sau tip tc nh phn xc nh acid tng c ng vi ch th phenolphthalein, dung dch t khng mu chuyn sang mu hng (tm)nht, c gi l acid tng cng 3.15.2 Dng c v thit b - Bnh tam gic 250mL - ng ong 100mL - Burett 3.15.3 Chun b ha cht - Dung dch NaOH tiu chun 0,1N: ha tan 1 ng chun NaOH 0,1N vi nc ct thnh 1000mL - Dung dch NaOH 0,02N: Ly 200mL dung dch NaOH 0,1N ha tan cng vi nc ct thnh 1000mL - Ch th Phenolphthalein 0,5%: cn 0,5g phenolphthalein ha tan trong 50mL Ethanol 98%, cho nc ct vo thnh 100mL - Ch th Methyl orange 0,05%: cn 0,05g methyl orange ha tan trong nc ct thnh 100mL 3.15.4 Tin hnh phn tch Nu mu nc l nc ung, nc - cp sinh hot, trc khi chun nn thm 1 git 2 2 Na S O 0,1N loi b lng Cl cn d. 3 Nu pH nc < 4,5 - ong 100mL nc mu cho vo bnh tam gic, sau cho vo 3 git methyl orange. Dung dch c mu . - Dng NaOH 0,02N chun cho n khi xut hin mu da cam. Ghi nhn th tch dung dch NaOH (V mL) dng tnh acid methyl hay cn 1 gi l acid khong. - Tip tc thc hin bc xc nh acid tng cng. Nu pH nc >4,5 - ong 100mL nc mu cho vo bnh tam gic, cho vo 3 git ch th phenolphthalein. Dung dch khng mu 17 9

Qun l cht lng nc nui trng thy sn - Dng NaOH 0,02N chun cho n khi dung dch chuyn t khng mu sang mu hng (tm) nht. Mu phi bn t nht 5 pht. Ghi th tch V mL dung 2 dch NaOH 0,02N dng tnh acid tng cng 3.15.5 Tnh kt qu V acid khong (mg 1 V CaCO /L) x1000 M 3 (V V ) acid tng cng (mg 1 2 CaCO /L) x1000 3mu nc ln hn 4,5 th V V= 0) (Khi pH 1M 2+ 3.16 St tng s (Fe v Fe ) 3+ 3.16.1 Phng php so mu Thiocianate Nguyn tc Cc mui ha tan ca st trong nc thng c xc nh bng phng php so mu 2+ Thiocianate.3 Phng php ny da trn nguyn tc trong mi trng acid, Fe 3 3 b oxy bng mt tc nhn oxy ha thch hp. Fe ha thnh Fe+ Fe c + mi to thnh v + sn trong s kt hp vi SCN hnh thnh mt chtmu c mu mu, 3 phc cng mu m nc hay nht ph thuc vo hm lng ion Fe c trong nc ban + u. 3 10Fe2+ + 10H + K 2S 2O 7 = 10Fe + K 2S + 5H + + - = Fe(SCN) (Mu K2 SO + 3SCN mu) O O 2 3 2 8 2 7 Thuc th - Dung dch Thiocianate ammonium hay potassium: Ha tan 50g NH SCN hay 4 KSCN trong mt t nc ct sau pha long thnh 100mL. - Dung dch Potassium persulfate: Ha tan 1,7g K S O trong mt t nc 2 2 8 ct sau pha long thnh 100mL. - Dung HCl c 3 1,18 dch d= Fe tiu chun 0,2mg/mL: Cho 20mL H SO m c vo 50mL 4 dung dch ny. Cho nc ct, ha+tan 1,4g Fe(NH ( SO ) .6H 2 2O vo 4 2) 4 2 tng git KMnO 0,1N cho n khi dung dch tr nn mu hng nht 3 vo 3 th dng li. - Sau Dung dch Fe tiu chun 4 pha long thnh 0,1mg/mL: 1.000mL. Ly 50mL dung dch Fe tiu chun + long thnh 100mL. + 0,2mg/mL pha Tin hnh - Xc nh st tng s Ly 2 bnh tam gic 100mL, cng kch thc ln lt mi bnh cc ha cht sau: 180

Phn tch cht lng nc Bng 7. 8. Tin trnh phn tch hm lng Fe tng s trong nc Bnh 1 Bnh 2 1. 50mL mu nc 1. 50mL nc ct. 2. 1,5 mL HCl c lc 2. 1,5 mL HCl c lc u u. 4. 1,5 mL lc u 3. dung 4. lc u dung 3. 2,5mL K SKSCN, O , lc 2,5mL K 1,5 S mL O , KSCN, lc 2 2 8 2 2 8 u u. 3 dch khng dch c mu mu. mu. Dng dung dch +Fe tiu chun 0,1mg/mL chun t t cho n khi dung 3 dch c mu mu ging bnh 1 th+ dng li ghi th tch V dung dch 1 Fe tiu chun s dng. Lm li nh trn mt ln na ly gi tr V trung 1 bnh. - Xc nh2 tam gic 100mL, cng kch thc, ln lt cho vo mi bnh cc Fe Ly 2 bnh + ha cht nh sau: 2+ Bng 7.9. Tin trnh phn tch hm lng Fe trong nc Bnh 1 Bnh 2 1. 50mL mu nc. 1. 50mL nc ct. 2. 1,5 mL HCl c lc 2. 1,5 mL HCl c lc u 3. 1,5 mL KSCN, lc u u dung 3. 1,5 mL KSCN, lc u 3 dung dch dch c mu mu. khng mu. Dng dung dch +Fe tiu chun 0,1mg/mL chun t t cho n 3 c mu mu 2 khi dung dch + ging bnh 1 th dng li, ghi th tch V dung dch Fe tiu chun s dng. Lm li nh trn mt ln na Tnh kt qu ly gi tr V trung bnh. 2 0 1,x Fe tng s (mg/L) = x1000 V 50 0 1,x 3+ x1000 Fe (mg/L) V2 = 50 0 1,x ( V Fe tng s (mg/L) = 1x1000 V ) 2 50 18 1

Qun l cht lng nc nui trng thy sn 3.16.2 Phng php o-phenantroline Nguyn tc 2+ St b kh thnh dng Fe bng cch un si vi acid v hydroxylamine v c x l vi 1, 10 phenanthroline pH 3,2 - 3,3. 3 phn t phenanthroline to hp cht cng 2 thnh dng phc cht c mu -cam. Sau c cua vi mi mt nguyn t Fe + xc nh bi my so mu quang ph bc sng 510nm. Thuc th - Dung dch A - HCl m c - Dung dch B - Dung dch Hydroxylamine 10%: ha tan 10g NH OH.HCl vi 2 nc ct thnh 100mL. - Dung dch C - Dung dch m pH = 5: h a tan 250g CH COONH trong 3 4 nc ct sau thm 700mL CH COOH m c. 150mL 3 - Dung dch D - Thuc th o-phenanthroline: ha tan 0,1g o-phenanthroline 0 trong 100mL nc ct lm nng 80 C. 2 200mg/l: ho tan 1,4g Fe(NH ) (SO ) .6H O vi 20mL H SO Dung - dch Dungchun dch Fe 4 2 4 2 4 m c vi + 50mL nc ct. Dau thm vi git KMnO 0,1N dung dch s 2 2 4 c mu hng nht, pha long thnh 2 100mg/l: ong 50mL dung2 200mg/l pha long - 1000mL. Dung dch Fe + dch Fe + thnh 100mL Thit lp mu chun Chn 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.10. Cc bc thit lp mu chun phn tch Fe tng s bng phng php o-phenantroline. STT Nng mu Th tch dung dch Th tch nc ct hay nc 2+ chun Fe 100mg/l (mL) bin lc c S%o = S%o vi nc mu (mL) (mg/l) 100,0 1 0,0 99,6 2 0,0 0,4 99,2 3 0,4 0,8 98,8 4 0,8 1,2 98,4 5 1,2 1,6 98,0 6 1,6 2,0 2,0 Tin hnh - Ln lt ong 25mL ca 06 mu chun vo 06 bnh tam gic - ong 25mL mu nc cn phn tch vo bnh tam gic, - Thm vo: (cng cch lm cho mu chun v mu nc )

18 2

Phn tch cht lng nc 1mL dung dch A 1mL dung dch B - Sau , em un trn bp cho cn cn khong 10-15mL, em ngui. - nh mc li vi nc ct thnh 25mL, - Tip tc thm vo 5mL dung dch C v 0,5mL dung dch D, - Lc u, - em so mu bc sng 510nm Ch , nu mu dung dch qu m ta nn lm li bng cch pha long, sau khi ghi kt qu t my ta x l l vi h s pha long s cho kt qu nng ca mu m ta cn o. 3.17 Silicate (SiO ) 2 3.17.1 Nguyn tc SiO v cc dn xut ca n trong nc thng xc nh bng phng php so mu 2 Molybdosilicate. Phng php ny da trn nguyn tc trong mi trng pH t 3-4 SiO v cc dn xut ca n s tn ti di dng H SiO (acid Silicic), acid Silicic 2 3 s 2 kt hp vi Molybdate ammonium hnh thnh phc cht Molybdosilicic acid c mu vng, cng m hay nht ph thuc vo hm lng H SiO c trong mi trng. 2 3 H SiO + 12(NH ) MoO 4 + 24HCl = H 8Si(Mo 2O 7) 6 + 24NH 2 2O 3 4 2 4Cl + 9H 3.17.2 Thu mu v bo qun Thu mu trong chai nt mi trng 125mL, c nh mu bng 1 mL HCl 50% 3.17.3 Chun b thuc th - 1. Dung dch Molybdate ammonium 10%: Ha tan 10g (NH MoO 4 2) 4 hay (NH Mo O .4H 2O trong mt t nc ct nng pha long thnh 100mL, 4 6) 7 24 cho vo bnh polyethylene s dng. - 2. Dung dch HCl 50%: Ha tan 50mL dung dch HCl trong 50mL nc ct. - 3. Dung dch H C lo O .2H O 10%: Ha tan 10g H 2C 2O 4.2H 2O trong 2 2 ng 4 thnh 2 mt t ct, nc sau pha ct, sau K pha long thng 100mL. - 1000mL. 5. Dung dch 0,63%: Ha tan 0,63g K CrO trong mt t nc ct, 2 4 sau pha lo ng thnh -CrO 4. Dung dch Na B O .H O 1%: Ha tan 10g Na 2B 4O 7.H 2O trong 2 4 7 2 mt 100mL. 2t nc 4 3.17.4 Tin tam hnh Ly 2 bnh gic 100mL, cng kch thc ln lt cho vo mi bnh cc ha cht nh sau:

18 3

Qun l cht lng nc nui trng thy sn Bng 7.11. Cc bc tin hnh phn tch SiO Bnh 2 2 1. 50mL mu Bnh nc 1 1. 25mL dung dch Na B O .H O 1%, v 7 dch 2 khng 2. 1mL HCl 50% v 2mL 29,5mL nc ct, lc2u4dung mu. (NH Mo O .4H 2O 4 6) lc u. 7 24 Dng dung dch K CrO 0,63% chun yn 10 pht, sau tip tc cho 2. 2 4 t t cho n khi dung dch c mu vng vo 1,5mL H C O .2H O 2 2 4 2 10%, ging nh bnh 1 th dng li, ghi th tch lc u, dung dch c mu vng. dung dch K CrO 0,63% s dng. 2 4 3.17.5 Tnh kt qu V SiO ( mg / L ) = 2 50 x1000

Vi V l th tch dung dch K CrO 0,63% s dng. 2 4 + ) 3.18 Ammonia (NH ) v Ammonium (NH 3 4 Health Association, 1989) 3.18.1 Phng php Nessler (American Public Nguyn tc + Trong mi trng baz mnh NH s bin thnh NH 3 . NH 3 mi hnh thnh v 3 NH c trong mu nc s tc dng sn vi phc cht Indo mercurate kalium (K HgI ), 4 2 4 hnh thnh phc cht c mu vng nu, cng mu m hay nht ty thuc vo hm lng NH c trong mu nc. 3 2 K HgI + NH + 3KOH = Hg(HgIONH ) + 7KI + 2 H 2O 2 4 3 2 (mu vng) K HgI + NH + KOH = Hg(HgI NH 2) + 5KI + H 2O 2 4 3 (mu nu) 3 Nhng trong nc thin nhin thng cha cc ion 2+ Ca , (nc cng), 2+ Mg trng baz mnh cc ion ny s to thnh cc hydroxide trong mi dng keo, lm cho dung dch b vn c cn tr qu trnh so mu. khc phc hin tng trn, phi 2+ cc mui ny kt (KNaC hp vi cc vEDTA Mg hnh thnhcho cc vo hpmu cht nc ha tan, dng mui Seignett H ion O Ca ), hay (EDTA) phn tch, 4 4 6 2+ khng mu trong dung dch. + + = Na MI + 2H M + Na2H I6 2 2 2 + M 18 4 2 + KNa C H O = K + + Na + +MCHO 4 4 4 4 6

Phn tch cht lng nc Thuc th: + 1mg/mL: Ha tan 0,3822g NH Cl trong - Dung dch NH Cl tiu chun N-NH 4 4 o C trong 2 gi), sau 4 mt t nc ct khng m (un nng 100 pha long thnh 100mL. + + - Dung dch N-NH 4 tiu chun 0,01mg/mL: Ly 1mL dung dch N-NH4 1mg/mL, dng nc ct khng m pha long thnh - 100mL. Nc ct khng m: Cho 20mL H SO c vo 1 lt nc ct, lc u ri em 2 4 ct li mt ln na. - Dung dch Seignett: Ha tan 50 g KNaC H O .4H O trong mt t nc 4 4 6 2 ct khng m, sau pha long thnh 100mL. - Dung dch EDTA: Ha tan 50g EDTA trong 60mL nc ct khng m, sau cho vo 10g NaOH khuy u cho ha tan v pha long thnh 100mL. - Dung dch Nessler: Ha tan 15g HgI v 10g KI trong 500mL nc ct khng 2 u cho NaOH ha tan hon ton, m, sau cho vo 40g NaOH, Khuy lng vi ngy v gn ly phn nc trong cho vo bnh nu s dng. Nu khng c sn HgI th pha nh sau: Ha tan 9g HgCl v 15,5 g KI trong 5mL 2 sau cho vo 40g NaOH, khuy 2 nc ct khng m, u cho NaOH ha tan hon ton lng vi ngy, gn ly nc trong cho vo bnh nu s dng. Tin hnh: Chn 11 ng nghim c dung tch 25mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.12. Cc bc thit lp mu chun phn tch TAN bng phng php Nessler ng nghim 1 2 3 4 5 6 7 8 9 10 11 Dung dch N-NH+ 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1,0 0 4 0,01N mg/mL Nc ct khng 9,9 9,8 9,7 9,6 9,5 9,4 9,3 9,2 9,1 9,0 0 m (mL) 0 0 0 0 0 0 0 0 0 0 10 Mu nc Dung dch Seignett 0,2 0,2 0,2 0,2 0,2 0,2 0,2 0,2 0,2 0,2 hay trion B (mL) 0,2 Dung dch Nessler (mL) 1,0 1,0 1,0 1,0 1,0 1,0 1,0 1,0 1,0 1,0 1,0 Nng N-NH 3 tng Ly ng nghim th 11 (mu nc) em so mu vi 10 ng cn li. Mu trong ng 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1,0 ? s nghim th 11 trng vi mu ng nghim no th nng TAN (tng m amn) bng vi nng TAN trong ng . Khi so mu cn cc ng nghim trn nn mu trng, v nhn kt qu t trn xung di phn bit mu r rng. Phng php 18 5

Qun l cht lng nc nui trng thy sn ny so mu bng mt thng nn rt n gin v d thc hin nhng chnh xc khng cao, t c chnh xc cao chng ta c th p dng so mu quang ph. Ch , kt qu thu c t phng php ny l hm lng tng m amn (TAN), + + 4 . tnh c hm lng N-NH 3 v N-NH 4 khi thu mu TAN = N-NH3 + N-NH nc chng ta phi o pH v nhit , da vo tra (xem phn l thuyt Chng 3, Mc 7.1) xc nh t l NH cha trong TAN, t tnh ra kt qu: 3 Tnh kt qu Hm lng N-NH (mg/L) TAN x I = 3+ 100 Hm lng N-NH 4 (mg/L) = TAN - N- 3 NH - I l t l phn trm ca N-NH cha trong TAN 3 3.18.2 Phng php Indophenol Blue Nguyn tc Phn ng Berthelot da trn s th hin mu xanh ca dung dch khi ammonia phn ng vi phenol v alkaline hypochlorite v c gi l phng php Indophenol hoc phng php Phenate. Phng php ny c p dng cho phn tch mu nc thi vi cng tng cng nh hn 400mg/L v nng nitrite nh hn 5mg/L (Scheiner, 1976) Trong phng php Indophenol, phenol v Hypochlorite phn ng trong mi trng kim hnh thnh phenylquinone-monoimine, ri tr li phn ng vi ammonia to -OH + 2 Indophenol - -O +c NH + xanh, 3O - minh -N O + 2Htrnh O+ thnh c ha qua=phng sau: 3 mu 2 ClO = Indophenol (mu 3Cl xanh) Phenol Cng mu ty thuc vo nng hin din ca ammonia, v sodium nitroprusside c thm vo lm tng cng hin mu trong dung dch. Nng + ca tng m amn - TAN (NH 3 v NH 4 ) s c xc nh bi my so mu quang ph bc sng 630 nm (i vi nc ngt) v 640 nm (nc l- mn) Tin trnh phn tch nc mn, l Thu mu vo chai nha 125mL, bo qun lnh cho n khi phn tch mu xong Thuc th - Dung dch A: ha tan 4g phenol vi dung dch ethanol 95% thnh 500mL. - Dung dch B: ha tan 0,375 g sodium nitroprusside (sodium nitroferricyanide) vi nc ct thnh 500mL. 186

Phn tch cht lng nc - Dung dch C: ha tan 7,5 g trisodium citrate v 0,8g NaOH vi nc ct thnh 500mL. - Dung dch D: dung dch oxy ho: Ly 2 mL sodium hypochlorite (NaOCl, 5%) pha vi dung dch C thnh 100mL (chun b ngay trc khi s dng). Dung dch chun - Dung dch (NH SO 500mg/l: ho tan 0,2358g (NH ) 2SO 4 ) vi 4 2) 4 4 nc ct khng m thnh 100mL. - khng Dung dch SO 5mg/l: pha 1mL dd (NH ) 2SO 4 500mg/l) vi m (NH thnh 4 2) 4 4 nc ct 100mL. Thit lp mu chun Chn 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.13. Cc bc thit lp mu chun phn tch TAN bng phng php indophenol mu mn. Th tch nc bin lc c Nng blue cho STT Th tchnc dungl, dch S = S ca mu nc mu (NH SO 5mg/L 4(mL) 2) 4 (mL) chun (mg/l) 100 0 1 96 2 4 0 92 3 8 0,2 88 4 12 0,4 84 5 16 0,6 80 6 20 0,8 Tin hnh phn1,0 tch Dng pipete ht 3 mL mu nc v mu chun cho vo cc ng nghim khc nhau. - Thm 1 mL dd A, trn u. - Thm 1 mL dd B (nitroprusside), trn u. - Thm 2 mL dd D (dd oxy ho), trn u. - trong ti nhit phng khong 1-2 gi cho phn ng xy ra hon ton (mu th hin r). Phn tch bc sng 640 m i vi cuvet 1 cm di truyn quang. Mu Zero l nc bin lc c S = S ca mu nc Tin trnh phn tch nc ngt Thu mu vo bnh 1lt, bo qun lnh cho n khi phn tch mu xong Thuc th - Dung dch PRE 1: nc ct khng m - Dung dch PRE 2: phenole stock solution: ho tan 312,5g phenol trong methanol thnh 500mL. - Dung dch PRE 3: sodium hypochlorite 5% 18 7

Qun l cht lng nc nui trng thy sn - Dung dch PRE 4: dung dch NaOH 67.5%: ha tan 67,5g NaOH thng 100mL nc ct khng m. - Dung dch A- Ha tan 150g Na PO .12H O v 150g C 6H 5O 7.2H 3 4 2 2O trong 1000mL nc ct khng m. - Dung dch B- Ha tan 75mL PRE 2 vi 0.1g Na [Fe(CN) NO].2H O 2 5 2 trong 100mL nc ct khng m. - Dung dch C- Ha tan 75mL PRE 3 vi PRE 4 thnh 100mL. Dung dch chun: - Dung dch (NH SO 500mg/L: ha tan 0,2358g (NH 4) 2SO 4 trong 4 2) 4 100mL nc ct khng m. 100mL vi nc ct khng m. - Dung dch (NH SO 5mg/L: pha 1mL dung dch (NH 4) 2SO 4 4 2) 4 500mg/L thnh Thit mu chun: Chn lp 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.14. Cc bc thit lp mu chun phn tch TAN bng phng php indophenol blue cho mu ngt.dch mu STT Nng Th nc tch dung Th tch nc ct khng m (mL) chun (NH SO 5mg/l (mL) 4 2) 4 1 100 (mg/l) 0 2 96 0 4 3 92 0,2 8 4 88 0,4 12 5 84 0,6 16 6 80 0,8 20 1,0 Tin hnh Ln lt ong 25mL mu nc v 25 mL tng nng mu chun cho vo bnh tam gic 50mL. Sau , cho vo tng bnh cc dung dch sau: - 1mL thuc th A - 1mL thuc th B - 1mL thuc th C Ch 20-25 pht, xut hin mu xanh (mu s n nh sau 25 pht n 24 gi) em o hp th quang bc sng 630 m. Ch , nu mu xanh qu m ta nn lm li bng cch pha long, sau khi ghi kt qu t my ta x l l vi h s pha long s cho kt qu nng ca mu m ta cn o. Tnh kt qu Cc mu chun thit lp c em o hp th quang, tng ng vi nng C ca mu chun ta c hp th quang A. Da vo s tng quan ny chng ta c th lp phng trnh tng quan dng A = aC + b 188

Phn tch cht lng nc Trong : A: hp th quang C : nng ca mu (mg/L) Sau khi thit l phng trnh, chng ta o hp th quang ca mu cn phn tch v th vo phng trnh chng ta s tnh c nng ca TAN c trong mu nc. C= A b a

3.19 Nitrite (NO 2 ) 3.19.1 Nguyn tc Nitrite (NO- ) trong mi trng acid mnh s hnh thnh HNO , HNO mi hnh 2 2 2 thnh s kt hp vi acid sulfanilique cho ra mui Diazonium sulfanilique. H 2O NaNO 2 + 2HCl + HSO -C H -NH 2 = HSO 3-C 6H 4-N=N-Cl+ NaCl + 3 6 4

Sau mui diazonium sulfanilique s kt hp vi thuc th . napthylammine cho ra . Napthylammine diazonium sulfanilique. HSO -C H -N=N-Cl + C H 9NH 2 = HSO 3-C 6H 4-N=N-C 10H 8NH 3 6 4 10 2 + HCl 2 . napthylammine diazonium sulfanilique l mt hp cht c mu hng, cng m hay nht ty thuc vo hm lng NO c trong mu nc lc ban u. Nng c xc nh bi my so mu quang ph bc sng 543 m. Phng php ny c gi l phng php Griess llosvay, Diazonium. 3.19.2 Cc bc phn tch Thu mu v bo qun Thu mu vo chai nha 125mL, bo qun mu lnh cho n khi phn tch mu xong. Thuc th - PRE 1: Cn 5g sulfanilic acid v 250g natri acetate ha tan vi nc ct thnh 500mL. - PRE 2: ha tan 0,5g 1-naphthylamine v 25mL acetic acid vi nc ct thnh 500mL. - Dung dch A: Ha tan 100mL PRE 1 vi 100mL PRE 2. - Dung dch B: Dung dch acetic acid nguyn cht. Dung dch chun 100mL. - Dung dch NaNO 500mg/l: ha tan 0,2463g NaNO trong 100mL nc ct. 2 Thit mu chun - lp Dung dch NaNO 2 5mg/l: ha tan 1mL dd NaNO 500mg/l vi nc ct thnh 2 2 18 9

Qun l cht lng nc nui trng thy sn Chn 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.15. Cc bc thit lp mu chun phn tch nitrite bng phng php Griess llosvay, Diazonium. Mu Nng ngt STT nc Th tch dung dch Th tch nc ct (mL) mu NaNO 5mg/L 100 1 chun (mg/L) (mL) 2 98 2 0 0 96 3 0,1 2 94 4 0,2 4 92 5 0,3 6 90 6 0,4 8 Mu nc l, 0,5 10 Th tch nc bin lc c S%o Nng STT mn = S%o ca mu (mL) mu Th tch dung dch 100 1 chun (mg/L) NaNO 5mg/L 2 98 2 0 (mL) 96 3 0,1 0 94 4 0,2 2 92 5 0,3 4 90 6 0,4 6 8 Tin hnh 0,5 10 - Lm ng chun: ong ln lt 20mL tng nng chun cho vo 6 bnh tam gic c k hiu nng chun b. - ong 20mL mu nc cn o vo bnh tam gic khc. - Ln lt cho thuc th vo: 1mL thuc th A v 5mL thuc th B - Ch 40 pht dd s c mu hng nu c nitrite (mu s n nh sau 40 pht n 4 gi ), ta em so mu bc sng 530 m. - Mu Zero l nc bin lc c nng mui tng ng vi nng mui ca mu nu phn tch mu nc l. Ch , nu mu hng qu m ta nn lm li bng cch pha long, sau khi ghi kt qu t my ta x l l vi h s pha long s cho kt qu nng ca mu m ta cn o. Qu trnh tnh ton kt qu tng t nh phng php Indophenol blue o TAN hay phng php Methylen blue o H S. 2 -) 3.20 Nitrate (NO 3 3.20.1 Phng php kh Cadmium Nitrate (NO ) trong nc s b kh ton b thnh nitrite (NO 3 2 ) bi ct Cadmium c x l bi CuSO 4 . NO mi hnh thnh v NO 2 sn c trong nc s c xc nh bi phng php 2 diazonium. 190

Phn tch cht lng nc 3.20.2 Phng php phenoldisulfonic acid Nguyn tc Nitrate (NO ) c trong nc tc dng vi phenol disulfonic acid to thnh phc cht 3 khng mu nitrophenol disulfonic. mi trng baze - mnh, phc cht ny c mu 3 vng. Cng mu vng cng m th nng NO cng cao OH OH HSO NO HSO 3 + NO+H (1) 2 3 3 O 2 SO H SO H 3 3 Phenol dissulfonic acid OH HSO NO 2 3 SO Nitrophenol dissulfonic (phc cht khng O mu) HSO N3 OK SO H 3

+ 3KOH

+ 3H 2 O

(2)

H 3 phc cht mu Thuc th vng - Dung dch acid Phenoldisulfonic: Ha tan 3g phenol trong 20mL H SO c 2 4 trong mt cc thy tinh chu nhit, ngui cho vo l nu s dng. - Dung dch NH OH nguyn cht (khong 25%). Nu khng c, c th thay bng 68 g KOH 4 ha tan thnh 100mL vi nc ct. 2 3 - Dung dch Nitrate tiu chun N-NO 0,01 mg/mL: Ha tan 0,722g KNO (sau o khi sy kh 105 C v ngui trong bnh ht m) trong mt t nc ct, sau pha long thnh 100mL. Ly 1mL dung dch va pha long trn pha long thnh 100mL, ta s c dung dch N-NO tiu chun 0,01mg/mL. 3 Tin hnh Chn 12 ng nghim cng kch thc, c dung tch 25mL, ln lt cho vo mi ng nghim cc ha cht sau:

19 1

Qun l cht lng nc nui trng thy sn Bng 7.16. Cc bc thit lp mu chun phn tch nitrate bng phng php phenoldisulfonic acid. ng nghim 1 2 3 4 5 6 7 8 9 10 11 Dung dch N-NO0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8 2,0 3 0,01 mg/mL 2,2 (mL) Nc ct (mL) 9,8 9,4 9,2 0 9,0 0 8,8 08,6 0 8,4 0 8,2 0 8,010 0 9,6 0 0 0 7,8 Mu nc (mL) Dung dch acid 1 1 1 1 1 1 1 1 1 1 1 Phenoldisulfonic (mL) 1 1 1 1 1 1 1 1 1 1 1 NH OH Nng c N- 4 0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8 2,0 NO (mL) 2,2 3 (ppm) Ly 10mL mu nc, cho vo chn s em un cch thy cho n kh. Nu c NO 3 th trong chn s c kt ta. Ha tan kt ta bng 1 mL dung dch acid phenoldisulfonic, khuy u cho kt ta ha tan, cho dung dch trong chn s vo mt ng nghim th 12, sau ra sch chn bng 10mL nc ct, nc ra ny cng cho vo ng nghim, tip tc cho vo ng nghim 1mL NH OH c lc u, em so mu 4 vi cc ng nghim trong gam mu ging nh phng php xc nh TAN bng phng php Nessler. c kt qu chnh xc chng ta c th p dng phng php so mu quang ph. 3.20.3 Phng php salycilate Thu mu v bo qun Thu mu vo bnh 1 lt, bo qun mu lnh cho n khi phn tch mu xong. Thuc th - Dung dch A - Ha tan 5g natri salicylate thnh 1000mL vi nc ct. - Dung dch B - Dung dch H SO 98% 2 4 - Dung dc C - Ha tan 100g C H KNaO .4H O thnh 1000mL vi nc ct. 4 10N: 4 ha tan 6 400g 2 NaOH thnh 1000mL vi - Dung dch D - Dung dch NaOH nc ct. Dung dch chun - Dung dch KNO 500mg/l: ha tan 0,3609g KNO trong 100mL nc ct. 3 3 - nc Dungct. dch KNO 50mg/l : ha tan 10mL dd KNO 500mg/l thnh 100mL vi 3 Thit lp mu chun 3 192

Phn tch cht lng nc Chn 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: Bng 7.17. Cc bc thit lp mu chun phn tch nitrate bng phng php Salicilate. Mu ngt Nng mu STT nc Th tch dung dch Th tch nc ct (mL) chun KNO 50mg/l 3 (mg/L) 100 1 (mL) 0,0 96 2 0 2,0 92 3 4 4,0 88 4 8 6,0 84 5 12 8,0 80 6 16 20 Mu nc l 10,0 mn Th tch nc bin lc c STT Nng mu chun Th tch dung dch S%o = S%o ca mu (mL) (mg/l) 100 1 KNO 50mg/L 3 0,0 98 2 (mL) 0,1 96 3 0 0,2 94 4 2 0,3 92 5 4 0,4 90 6 6 0,5 8 Tin hnh 10 thuc th A - Ly 10 mL mu nc, cho vo 1mL 0 - em sy 105 C cho n cn - ngui. - Cho vo 1mL thuc th B - Ch 10 pht - Cho tip 20mL thuc th C - V 5mL thuc th D, dd s c mu vng anh nu c nitrate. - Ch 15 pht xut hin mu vng anh (mu n nh sau 15 pht n 6 gi), sau o hp th quang bc sng 410m. Ch , nu mu vng anh qu m ta nn lm li bng cch pha long, sau khi ghi kt qu t my ta x l l vi h s pha long s cho kt qu nng ca mu m ta cn o. Ghi kt qu hp th quang A v da vo phng trnh hi qui tnh ra nng ca mu 19 3

Qun l cht lng nc nui trng thy sn 3Orthophosphate (PO ) 4 3.21.1 Phng php xanh molybden Nguyn tc 3.21 Ln ha tan trongacid, ncion c 3 lc qua mng lc 0,45 m. Cc mui orthophosphate trong mi trng 4 s cho mt phc cht mu vng chanh vi thuc th PO Molybdate ammonium. + PO 3 + 12(NH MoO ++ 24H = (NH ) 2PO 4.12MoO 3+ 4 2) 2 4 4 21NH 4 + 12H 2O + cht kh nh SnCl , Dng -phospho molybdate NH4+, trong s hin din ca (-phospho molybdate NHcc ) 2 4 + v.v..d b kh thnh dng - phospho molybdate NH4 c mu xanh. Cng mu m hay nht ph thuc vo hm lng ion 43 c trong mu nc lc ban u. PO 2 + 16H + = (NH ) PO .(4MoO .2MoO ) +4 (NH4) PO .12MoO + Sn Sn +28H O 3 43 4 2 32 + + 4 xc nh bi my so mu quang ph bc sng 690 m. V c Ha cht - Dung dch Amonium molybdate Mo O .4H 2O ha tan trong 175 mL nc ct 4 6) 7 24 ong 280mL H SO m c pha vi 400mL nc ct, ngui 2 4 Trn ln hai dung dch li ri pha long vi nc ct thnh 1000mL - Dung dch SnCl Bo Cn 2,5g SnCl .H O ha tan trong 100mL Glycerin (Cung cp nhit). 2 2 qun dung dch t lnh 3 - Dung dch chun P-PO Dung dch KH PO 500mg/l: ha tan 0,2197g KH PO trong 100mL 4 2 4 2 4 nc ct Dung dch KH PO 5mg/l: ha tan 1mL dd KH PO 500mg/l thnh 2 4 2 4 100mL vi nc ct Thit lp mu chun Chn 6 bnh tam gic c dung tch 100mL, cng kch thc, khng mu ln lt cho vo cc ha cht sau: 2 Cn 25 g (NH

19 4

Phn tch cht lng nc Bng 7.18. Cc bc thit lp mu chun phn tch orthophosphate bng phng php xanh molypden . Nng mu Th tch dung dch Th tch nc ct STT KH PO 5mg/l (mL) chun 1 (mL) 100 (mg/l) 2 4 2 96 0 0 92 3 0,2 4 4 88 0,4 8 84 5 0,6 12 80 6 0,8 16 1,0 20 Tin trnh phn tch - Ly ln lt 50mL nc mu c lc loi b vt cht l lng c trong nc vo bnh tam gic, cng vi 50mL tng nng chun cho vo 6 bnh tam gic c k hiu sn nng . - Cho vo 2mL dd amonium molybdate, lc u - Cho vo 5 git SnCl , lc u 2 - o hp th quang bc sng 690m Tnh kt qu 3 Tnh nng P4 hin din trong mu da trn vic phng trnh hi qui tng - quang v nng cht tan cn phn tch tng t nh cc cc PO gia hp th quan phng php Methylen blue (phn tch H S), Indophenol blue (phn tch 2 TAN), 3 Salicilate (Phn tch NO )... 3.21.2 Phng php Acid ascorbic (4500-P E: Standard methods, 1998) Nguyn tc Ammonium molybdate v potassium antimonyl tartrate trong acid trung tnh phn ng vi orthophosphate to thnh 1 dng acid d a (heteropolyacid) acidphosphomolybdate b kh thnh dng c mu xanh tp trung molybde bi acid ascorbic. Nng ca P-3 s c xc nh bi my so mu quang ph bc sng 880 PO 4 m. Thuc th - H SO 5N: Pha 70 mL H SO m c vi nc ct thnh 500 2 4 2 4 0,12 g mL. K(SbO)C H O .1/2H O trong 400 mL nc ct. sau pha long thnh - Dung dch 4 4Potassium 6 2 antimonyl tartrate: Ha tan 500 mL. mL nc ct. - Dung dch ammonium molybdate: ha tan 20 g (NH Mo O .4H 2O 4 6) 7 24 trong 500 19 5

Qun l cht lng nc nui trng thy sn - Acid Ascorbic 0,1M: ha tan 1,76 g trong 100 mL nc ct. Dung dch n nh o khong 1 tun 4 C. - Thuc th kt hp (combined reagent): Trn cc thuc th trn li vi nhau theo t l sau c 100 mL thuc th kt: 50 mL H SO 5N 2 4 5 mL potassium antimonyl tartrate 15 mL ammonium molybdate 30 mL acid ascorbic. Trn u mi khi cho vo tng loi thuc th theo th t nu trn. Cho php cc thuc th trn nhit phng trc khi phi hp. Nu c xut hin trong thuc th hn hp th lc u ri yn cho n khi c khng cn xut hin. Thuc th ny n nh trong 4 gi. - Dung dch m (stock phosphate solution): Ha tan 219,5 mg KH PO trong 2 hay 4 1000mL nc ct c dung dch c nng cht chun l 50 g/mL 50 mg/L - Dung dch chun (Standard phosphate solotion): Ha tan 50 mL dung dch m vi 1000 mL nc ct c c dung dch chun c nng 2,5 g/mL hay 2,5 mg/L Tin trnh phn tch - Ly 50 mL mu nc v mu chun cho vo bnh tam gic 125 mL sch v kh. - Thm 0,05 mL ch th mu phenolphthalein. Nu xut hin mu th thm tng git dd H SO 5N cho n khi dung dch va mt mu. 2 th 4 kt hp (combined reagent) ri khuy u. - Thm 8 mL thuc - Sau 10 pht nhng khng qu 30 pht, o hp th quang tng mu bc sng 880 m, s dng mu trng lm dung dch i chng. - Khc phc mu b c hay nhiu mu: Nu cc mu sau khi cho vo cc thuc th m c mu hoc c th phi chun b mu trng bng cch thm tt c cc thuc th vo ngoi tr acid ascorbic v antimonyl potassium tartrate. Ly hp th quang ca tng mu chun v mu nc tr i cho hp th quang ca mu trng loi tr sau s do nhiu mu Qu trnh thit lp mu chun, xy dng ng chun v tnh kt qu (xc nh nng cht tan cn phn tch) tng t nh phng php xanh molypden. 3.22 Tng m (TN) v tng ln (TP) 3.22.1 Phng php Kjeldahl Nguyn tc 19 6

Phn tch cht lng nc Cc dng m hu c b oxy ha bi acid H SO m c vi xc tc K 2 o 4 2 2 SO 4 v + 2 4 4 3 CuSO hoc H O trong iu kin nhit cao (375-385 C) s chuyn ha hon ton thnh m ammonium (NH ). Ammonia (NH ) cng chuyn thnh ammonium. Sau khi thm vo dung dch baz, ammonia c ha tan trong mi trng kim v b hp thu bi acid boric hay acis sulfuric, ammonia c th c xc inh bng phng php so mu quang ph Indophenol blue. Cc dng ln hu c cng b oxy ha (trong iu kin tng t nh m hu c) s chuyn ha thnh orthophosphate. Orthophosphate c th c xc nh bng phng php so mu quang ph ascorbic acid hay xanh molypden. Do , phn tch tng m (TN) v tng ln (TP) chng ta c th thc hin cng ph trn cng mt mu, sau mi tin hnh phn tch hai ch tiu trn theo cc phng php dng phn tch cc dng mui m v ln v c ha tan. Thit b thc hin qu trnh v c ha m, ln hu c chng ta cn dng my cng ph mu (digestion apparatus). Hin nay trn th trng c bn nhiu loi my cng ph mu, th d nh BD-26 (BD-26 Block Digestor), c th ci t chng trnh iu khin trong nh ph mu. i. nhit Chun b cc mu qu nctr (V = cng 50 hoc 100 mL) cho vo cc ng cng ph; s dng 2-3 ng mu trng (nc ct); thm 2-3 vin si loi chuyn dng cho Tin trnh cng ph mu nc qu trnh cng ph (chng nc b bn ra ngoi khi si) vo mi ng. thm mi ng mu nc v mu trng 10 mL H SO m c, trn u, i 2 4 n khi mu ngui li.

ii .

Sau khi ngui, thm 10 mL H O m c (c th dng 6,7 g K SO v 2 2 2 4 0,365 iii. g CuSO ), mu qua m trc khi cng ph. 4 iv. t cc ng mu v gi ln my cng ph. v. M my cng ph v my ht (qu trnh cng ph nc bc hi nn phi dng my ht). Ci t chng trnh iu khin nhit : o Temp1 = 110 C, gi nhit ny trong vng 20 pht (khng k thi gian o o tng o t nhit phng ln 110 C). nhit o Temp2 = 200 C, gi trong vng 20 pht (khng k thi gian nhit tng t 110 C ln 200 C). o Temp3 = 300 C, gi nhit ny n khi mu cng ph c mu trng o 19 cng cao Ch , c th tng nhit cng ph ln n 375 C. Nhit th 7

Qun l cht lng nc nui trng thy sn thi gian cng ph cng ngn. Tng thi gian cng ph 3 bc trn c tnh khong 90 pht. vi. Sau khi qu trnh cng ph hon thnh, tt my, ngui. vii. Khi cc mu c cng ph v ngui hon ton, pha long phn acid sulphuric cn li trong ng vi 25 mL nc ct khng m ri ton b phn nc ny vo ng ong (V = 250 mL). Trung ha dung dch bng cch nh NaOH 40% (10 M) c s hin din ca cht ch th para-nitro-phenol (4nitro-phenol), sau chun li mi trng acid bng vi git dung dch dung H SO 20%; Dung dch sau cng c thm 1 git H SO 20% gi 2 4 2 4 dch c mi trng pH di 7,0 (5,0-7,0).

Xc nh hm lng tng m (TN) v tng ln (TP) 3Indophenol blue v Orthophosphate (P-PO ) bng phng php Xanh molypden hay Xc nh hm lng m TAN ca mu nc di dng N-NH bng phng php 4 4 Acid ascorbic. Ch , vi phng php cng ph Kjeldahl, kt qu hm lng m m thu c c gi l tng m Kjeldahl (Total Kjeldahl Nitrogen - TKN). TKN bao gm hm lng m hu c v TAN c trong mu nc (TKN = N-Hu c + TAN). Trong trng hp ny nu mun tnh c tng m (TN) chng ta phi xc nh thm hm lng m nitrite v nitrate TP = TKN + N-NO 2 + N-NO 3 Nu trc khi cng ph mu chng ta loi b TAN bng cch nng pH ca mu nc ln 9,5, khi NH+ 4 s chuyn hon ton thnh NH . un nh mu, NH s 3 3 thot ra khng kh sau mi cng ph mu. Trong trng hp ny kt qu hm lng m thu c chnh l m hu c (TKN = N-Hu c). Hm lng ln thu c t phng php cng ph Kjeldahl l tng ln (TP). Tin cng bn y i. trnh Mu bn ph thu mu v kh trong iu kin nhit phng, k n sy kh nhit 105oC. Mu sau khi sy c nghin mn, ry qua li v gi trong l kn n khi phn tch. Cn 0,15-0,25g mu bn cho vo ng cng ph, thm 2-3 vin nh (loi chuyn dng cho my cng ph) vo mi ng, tip tc thm 50 mL nc ct khng m 10 mL H SO , lc u, 2 4 ngui hon ton. Sau khi ngui, thm10 mL H O m c, mu qua m trc khi cng 2 2 ph.

ii . 19 8

Phn tch cht lng nc iii. t cc ng mu v gi ln my cng ph. iv. M my cng ph v my ht (qu trnh cng ph nc bc hi nn phi dng my ht). v. Ci t chng trnh iu khin nhit : o Temp1 = 110 C, gi nhit ny trong vng 30 pht (khng k thi gian o nhit tng t nhit phng ln 110 C). o Temp2 = 200 C, gi trong vng 30 pht (khng k thi gian nhit tng t o 110oC ln 200 C). o Temp3 = 375 C, gi nhit ny n khi mu cng ph c mu trng vi. Tng thi gian cng ph 3 bc trn c tnh khong 90 pht. vii. Khi cc mu c cng ph v lm lnh hon ton, pha long phn acid Sau khi qu trnh cng ng ph hon thnh, tt my, sulphuric cn li trong mt cch cn thn vi 25ngui. mL nc ct khng m ri ton b phn nc ny vo ng ong (V = 250 mL). Trung ha dung dch bng cch nh NaOH 40% (10 M) c s hin din ca cht ch th paranitro-phenol (4-nitro-phenol), sau chun li mi trng acid bng vi git dung dd H SO 20%; Dung dch sau cng, thm 1 git dd H SO 20% gi 2 4 2 4 dch c pH di 7,0 (5,0-7,0).

Xc nh hm lng tng m (TN) v tng ln (TP) Xc nh hm lng m TAN ca mu nc di dng N-NH bng phng php 4 3Indophenol blue v Orthophosphate (P-PO ) bng phng php Xanh molypden hay 4 Acid ascorbic. i vi mu bn y, kt qu hm lng m thu c l tng m (TKN = TN). Kt qu hm lng ln thu c l tng ln (TP) 3.22.2 Phng php cng ph persulfate Nguyn tc o 2 trng 2 3 C, m hu c v m v c b oxy Trong mi kim iu kin nhit 110 8S O s chuyn ha thnh nitrate (NO ). Ln hu c cng b oxy ha thnh ha bi K orthophosphate. Cc thuc th - NaOH 1 M: ha tan 40 g NaOH trong 800 mL nc ct, ngui ri pha thnh 1000 mL - Thuc th Oxy ho (OR): ha tan 50 g potassium peroxodisulphate (K S O ) v 2 ct. 2 Bo 8 30g acid boric trong 350 mL NaOH 1 M ri pha thnh 1000 mL vi nc qun trong chai, l mu nu trnh nh sng. 19 9

Qun l cht lng nc nui trng thy sn Tin trnh - Dng l nha 30 mL, cho vo 25 mL mu nc v cc mu chun ri thm vo 3,3 mL thuc th oxy ho (B). Trn u. o - y np l nha ri cho vo ni autoclave khong 20 pht 121 C v p sut 15 psi. Cho php lm lnh 1 gi. - Thc hin t nht 3 mu trng bng nc ct trong sut. Xc nh hm lng tng m (TN) v tng ln (TP) Hm lng tng m c th xc nh c bng cc phng php xc nh bng cc phng php phn tch nitrate (Phenoldisulfunic acid, Salycilate hay kh Carmidium). Ln hu c cng b oxy ha thnh orthophosphate v c xc nh hm lng bng phng php Xanh molypden hay Ascorbic acid. Kt qu hm lng m thu c khi phn tch bng phng php cng ph persulfate l tng m - TN (bao gm NHu c, TAN, N-NO- v N-NO 3 ) v hm lng ln thu c l tng ln - TP. 2

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