CC PHNG PHP QUAN TRC CHT LNG NC TRONG AO NUI THY SN Nguyn nh Trung I. LY V BO QUN MU NC 1.

1 Nguyn tc Cc nguyn tc ch yu cn c m bo khi ly mu nc l: Mu nc ly phi i din c cho ton b nc a im nghin cu. Th tch ca mu nc cn phi phn tch cc thnh phn cn thit bng cc phng php c la chn trc. Vic ly v bo qun, vn chuyn mu cn c thc hin nh th no khng lm thay i hm lng ca cc cu t cn xc nh hoc cc tnh cht ca nc. 1.2 Chn ch ly mu Ch ly mu nc cn c la chn ph hp vi mc ch ca vic phn tch nc. Ngoi ra cn phi ch n tt c nhng yu t c th gy nh hng n thnh phn ca mu. 1.3 Cc loi mu C hai loi mu chnh: a. Mu n gin: L mu c ly mt ln mt a im v thi gian nht nh. b. Mu trn: c nhn bng cch trn nhng mu n gin c ly ng thi nhng ch khc nhau nhng thi im xc nh. Khng nn dng mu trn xc nh hm lng ca nhng ch tiu ca nc d b thay i nh pH, cc kh ha tan. 1.4 Dng c v cch ly mu Mu nc thng c thu bng dng c chuyn dng gi l batomet hoc c th ly mu nc thng vo cc bnh ng. 1.5 Bo qun mu Quy nh v bo qun mu nc cho cc mc ch phn tch khc nhau c nu trong Bng 1. Bo qun mu nc l nhm gi gn cc yu t, ng thi duy tr tnh cht v tnh trng mu nc trong mt khong thi gian ngn trc khi em phn tch. Bng 1: Dng c cha mu, v iu kin bo qun mu nc iu kin bo qun Lnh 4o C Khng Lnh 4o C C nh ti ch (Winkler) Lnh 4o C Lnh 4o C 1 Thi gian bo qun ti a 4 gi 6 gi 24 gi 6 gi 4 gi 24 gi

TT 1 2 3 4 5 6 TSS pH

Phn tch

Chai ng PE PE PE TT PE PE

kim Oxy ha tan (DO) BOD COD

7 8 9

NH 3 NO3PO43-

PE PE TT

Lnh 4o C 2mL H2SO4 c/L mu Lnh 4o C Lnh 4o C

24 gi 24 gi 24 gi

Ghi ch: PE: Chai polyethylen TT: Chai thu tinh PHNG PHP NH LNG MT S THNG S NH GI CHT LNG NC 2..1. Cht rn (Solids) Cc cht rn l mt phn ca mu nc khng b mt i do qu trnh bay hi. Cht rn trong nc bao gm cc dng l lng v dng ho tan. Cht rn tng cng (Total Solids TS): l lng cht cn li trong cc sau khi lm bay hi nc trong mu v lm kh trong t sy nhit xc nh. Cht rn tng cng bao gm tng hm lng cc cht rn l lng (Total Suspended Solids) l phn tng cht rn cn li trn giy lc v hm lng cht rn ho tan (Total Dissolved Solids ) l phn cht rn ha tan i qua giy lc. Mu khuy trn u c lm bay hi trong cc cn v lm kh n khi lng khng i trong t sy nhit 103 -105o C. tng khi lng cc chnh l khi lng cht rn tng cng. Tng cht rn ho tan = cht rn tng cng tng cht rn l lng 2..2. TDS (Total Dissolved Solids) L tng lng vt cht hu c v v c ha tan trong nc (c kch thc nh hn 1nm =10 9 m). Phng php xc nh: TDS (mg/l) = k x EC ( S / cm) Trong : k: h s dn in = 0,50 0,85 (ty vng) EC: dn in ring, l gi tr nghch o ca in tr ring ca dung dch. n v tnh: S/ cm (microsiemen/cm) 2.3. TSS (Total Suspended Solids) L tng lng vt cht hu c v v c l lng (ph sa, mn b hu c, to) l lng trong nc (c kch thc 10 5 - 10 6 m). Mt phn cc cht l lng c kch thc ln hn 10 5 m s lng xung y. Hm lng cht rn l lng tng hoc hm lng cht rn c kh nng lng t l ch tiu nh gi mc nhim ca nc thi t cc c s nui thy sn. Phng php xc nh: TSS c xc nh theo phng php khi lng. Tin hnh nh lng: 1. Sy giy lc nhit 105oC trong 8 gi 2. Cn giy lc va sy xong (m1<mg>) 2

3. Lc 100mL mu nc qua giy lc xc nh khi lng 4. ro 5. Dng kp (khng dng tay) a ming giy lc vo sy nhit 105oC trong 8 gi. 6. Lm ngui, ri cn giy lc (m2, <mg>)
( m 2 m1) x1000 v

TSS (mg/L) =

Trong : m1 m2 v 1000 2.4. pH

= = = =

Khi lng ban u ca giy lc (mg) Khi lng sau ca ming giy lc v phn vt cht lc c (mg) Th tch mu nc em lc (mL) h s i thnh 1L

c hng dn ca nh sn xut trc khi s dng my o pH. Trc khi tin hnh xc nh pH ca mu nc, hiu chnh my o vi dung dch pH chun = 7. Nu cc mu cn o c tnh axt, hiu chnh my vi dung dch pH chun = 5. Nu cc mu cn o c tnh kim, hiu chnh my vi dung dch pH chun = 9. o mu nc, c kt qu trn my. 2.5. mn mn ca nc l tng hm lng cc ion ho tan trong nc. Biu din bng n v tnh: g/L hoc phn nghn o/oo hoc ppt (1g/L= 1ppt). Trong nc l, mn, mn c th c xc nh bng phng php ho hc bng cch chun mu nc nghin cu vi dung dch Ag NO3 ch th K2CrO4. T trng ca nc tng khi mn tng. V th t trng k c ci tin c th o c mn thay v o t trng nc. mn ca nc cn c o bng khc x k. 2.6. kim Trong s cc thnh phn to nn kim chung ca nc l v nc mn c ngha chnh nht l cc anion HCO3- v CO32- ca axt H2CO3. Bi vy kim ca nc l s o tng ca cc ion HCO3- v CO32- trong nc. Phng php xc nh: Chun trc tip mu nc bin bng dung dch HCl, phn ng xy ra nh sau: RHCO3 + HCl RCl + CO2 + H2O im kt thc phn ng c nhn bit rng s i mu ca ch th metyl da cam (hoc ch th mu hn hp) cho vo. kim ca nc c biu th bng mili ng lng gam (meq) ca axt HCl khi chun . i vi nc t nhin kim tng cng (total alkalinity) thc t trng vi cng cacbonnat, bi vy trong tnh ton ngi ta thng biu th n v tnh kim t s mili ng lng gam/lt thnh mg CaCO3 /L , theo h s chuyn i: 1meq/L = 50mg CaCO3 /L 3

 Trnh t tin hnh Ly 100mL nc nghin cu cho vo bnh nn, thm 4 git ch th metyl da cam (hoc ch th mu hn hp), dung dch chuyn sang mu vng (hoc mu xanh), chun bng dung dch HCl 0,1N cho n khi chuyn sang mu hng (hoc mu xm) th dng li. Lm 2 ln ly kt qu trung bnh. Tnh ton kt qu: kim = Trong : A N V 1,04 1000 50
A.N .1,04 X 1000 V

= meq /L x 50 = mg CaCO3 /L : s mL dung dch HCl tiu tn khi chun : nng dung dch HCl (0,1N) : th tch mu nc ly phn tch : h s hiu chnh do nh hng ca CO2 : h s i thnh lt : h s chuyn i t meq thnh mg CaCO3

2.7. xy ho tan (DO) Phng php Winkler: 2.7.1. Nguyn tc phng php Phng php ny kh n gin, d thc hin v cho php t chnh xc cao khi hon thnh cn thn tt c khu khi tin hnh nh lng. Phng php da trn c s phn ng m Mn ho tr 2 trong mi trng kim (dung dch c cho vo trong mu nc trong cng hn hp vi dung dch KI) b O2 trong mu nc xy ho n hp cht Mn ho tr 4, s ng lng ca hp cht Mn ho tr 2 lc c kt hp vi tt c O2 ho tan. MnCl2 + 2NaOH = 2NaCl + Mn(OH)2 Trng Mn(OH)2 + O2 = 2MnO(OH)2 Vng nu S ng lng ca Mn ho tr 4 c to thnh dng kt ta mu vng nu bng s ng lng xy ho tan trong nc. Khi thm axit H2SO4 vo trong mu, hp cht Mn ho tr 4 hay ni khc i l s ng lng ca O2 ho tan, chnh bng s ng lng I2 c trong mu nc. MnO(OH)2 + 2H2SO4 + KI = MnSO4 + K2SO4 + 3H2O + I2 I2 t do c tch ra, d dng nh lng dung dch chun Na2S2O3. I2 +2 Na2S2O3 = 2Nal + Na2S4O6 Bit th tch v nng Na2S2O3 khi chun ta d dng tnh c hm lng xy ho tan trong mu nc. V th khi xc nh O2 ho tan trong nc c thc hin trong 3 giai on: Giai on I: C nh O2 ha tan trong mu (c nh mu) Giai on II: Tch I2 bng mi trng axt (axt ha, x l mu) Giai on III: Chun I2 bng Na2S2O3 (phn tch mu) Hn ch ca phng php: phng php Winkler xc nh O 2 ha tan trong nc khng p dng vi nhng mu nc c cht xy ho (vng nc b nhim bn nc thi cng nghip) c kh nng xy ho anion I- , hoc cc cht kh (dihydrosunfua H2S) kh I2 t do. 4

2.7.2. Trnh t tin hnh a. C nh mu nc Thu nc mu bng batomet chuyn sang chai 125mL mt mi, cho vi cao st y chai nc trn ra ht khong 1/3 th tch cha lc u. Lp tc cho vo 1mL MnCl 2 , 1mL dung dch KI/NaOH. y nt chai li khng cho c bt kh. o u t trn xung di. Trong mu nc xut hin kt ta mu trng ri chuyn sang mu vng nu. b. X l mu yn chai ng mu nc c nh ch mt trong 1 gi. Sau thm vo 1mL H 2SO4 c, kt ta mu vng nu tan ht. Trong mu nc xut hin mu vng ca I2. Trng hp phi mu lu, th ngm trong chu nc lnh bo qun mu. c. Phn tch mu Chuyn 25mL nc mu x l vo bnh nn, chun bng Na2S2O3 0,01N n khi c mu vng nht th thm vo 3 git h tinh bt, dung dch c mu xanh tm, ri nh tng git Na 2S2O3 0,01N n khi ht mu xanh tm. Ghi th tch Na2S2O3 0,01N chun ht. Lm t 2-3 ln ly kt qu trung bnh. 27.3. Cng thc tnh ton Hm lng O2 ho tan trong nc c tnh theo cng thc: mg O2/ L =
V .N .8.1000 V o

Trong : V : S mL dung dch Na2S2O3 0,01N dng ht N :Nng dung dch chun Na2S2O3 V0 :Th tch mu nc x l phn tch 8 :ng lng ca O2 1000 :H s i thnh lt Ch : Trong giai on c nh, chng ta thm 2mL ho cht (1mL MnCl2 + 1mL KI/NaOH) vo trong chai mu 125mL, nn lng nc thc t c nh lng (tr phn ho cht cho vo) l: 25 x
125 2 = 24,6 (mL) 125

V nh vy hm lng O2 ha tan trong nc chnh xc l: mg O2/ L =

V .N .8.1 0 00 2 ,6 4

2.7.4. C s thit lp cng thc Trong qu trnh xc nh hm lng O2 ha tan nc theo phng php Winkler, chng ta thc hin nhng bc sau: Giai on c nh mu: S ng lng O2 = s ng lng MnO(OH)2 5

Giai on x l v phn tch mu: S ng lng MnO(OH)2 = s ng lng I2 = s ng lng Na2S2O3

Nh vy cui cng ta c: S ng lng O2 = s ng lng Na2S2O3 VO2 . NO2 = VNa2S2O3 . N Na2S2O3 VO2 :c th xem nh l V mu nc c x l: VO2 = H2O do :

NO2 = Na2S2O3 . N Na2S2O3

V H2O i N nng ng lng ra miligam. S mg = ng lng x s ng lng x 1000 = x N x 1000 S mg O2/l = O2 . NO2 . 1000 M O2 = M/n Vi M : Phn t lng n : S e- trao i khi tham gia phn ng Trong trng hp ny: O2 + 4 e- = 2 O2- vy O2 = 32/4 = 8

mg O2 / L =

VNa2S2O3 . N Na2S2O3 . 8 . 1000 V H2O

2.7.5. Ha cht cn thit a. Dung dch MnCl2 Ha tan 250g MnCl2.4H2O trong 620mL nc ct ng vo l trng. b. Dung KI/NaOH Ho tan 150g KI trong 200mL nc ct, ho tan 500g NaOH trong 500mL nc ct (khi ho tan va khuy va lm lnh). Trn 2 dung dch ny vi nhau v thm nc ct n 1L. ng vo l nu, nt cao su. c. Dung dch tinh bt Cch pha th 1: Ha tan 0,5g tinh bt d tan vi 1L nc ct, ri thm 100mL nc ct v khuy, un n si. C th thm 3git CCl4 hoc CHCl3 dit vi khun. Cch pha th 2: Cho 2g tinh bt d tan vo trong 1L nc ct. Dng NaOH 20% va cho va khuy vo dung dch tinh bt (ht khong 30mL dung dch kim) cho ti khi c mt dung dch trong sut, hi snh. yn trong 1 gi, dng dung dch HCl 20% va cho va khuy trung ha kim, cho n khi phn ng axt yu (th o giy o pH = 6 l c). Thm hn hp 1mL axt axetic 99% bo qun. Dung dch mt nm mi hng. d. Dung dch nguyn chun K2Cr2O7 0,1 N 6

Cn 4,903g tinh th ha tan v nh mc n 1L bng nc ct hoc l dng phecxanal K2Cr2O7 N/10. e. H2SO4 c f. Dung dch H2SO4 25% Trn mt th tch H2SO4 c vi th tch nc ct. Ch : Khi pha phi axt vo nc, khng lm ngc li. ong lng axt trong ng ong m khng dng pipet. g. Dung dch KI 1M Ha tan 8,3g KI vo trong 500mL nc ct. Trn u ri cho vo l nu. h. Dung dch Na2S2O3 0,1 N Ha tan 25g tinh th Na2S2O3 . 5H2O trong 1L nc ct, un si ngui ( ui ht CO2). Thm 6 ht NaOH rn ri cho vo l hoc dng phecxanal Na2S2O3 N/10. Dung dch va pha khng c nng chnh xc v vy cn phi xc nh li nng . L do l trong tinh th Na2S2O3 thng ln Na2S, Na2CO3, Na2SO3 ... v Na2S2O3 d b vi khun phn gii, b xy trong khng kh xy ho. Cch lm nh sau: Np dung dch mi pha ln burnet. Cho vo bnh nn 10mL dung dch H2SO4 25%, 10mL KI 1M, 10mL K2Cr2O7. Lc u yn 5 pht, chun bng Na2S2O3 0,1 N cho n mu vng nht, ri cho 3 git h tinh bt. Tip tc nh tng git Na2S2O3 cho n ht mu xanh tm (ch n mt mu xanh tm ca dung dch tinh bt ch khng th mt mu ca Cr + c). Ghi th tch Na2S2O3, tiu tn Vm. Nng dung dch Na2S2O3 c tnh theo cng thc: N = Tng qut: N=
1 x 0,1 0 V

V K2Cr2O7 . N K2Cr2O7 V

T dung dch Na2S2O3 bit chnh xc nng , ta pha dung dch Na2S2O3 0,01 N l dung dch chun xc nh O2 ha tan. 2.8. Nhu cu xy sinh ha (Biochemical Oxygen Demand BOD) BOD l lng xy cn thit vi sinh vt tiu th trong qu trnh phn hy cc cht hu c trong nc trong iu kin hiu kh. Phn ng xy ra nh sau: Cht hu c + O2 VSV CO2 + H2O xy s dng trong qu trnh ny l xy ha tan trong nc.

2.8.1. Phng php xc nh Thu mu nc: Chuyn mu vo hai chai thy tinh nt mi 125mL. Chai th nht xc nh ngay hm lng O2 ban u. Chai th hai ti, nhit 20o C, thi gian 5 ngy (hoc 3 ngy nhit 30o C). nh lng hm lng O2 trong chai th hai. BOD 5 = O2 u - O2 cui (mg/L) Trng hp nc c hm lng cht hu c cao, cn pha long nc nghin cu bng dung dch pha long Chun b dung dch pha long: nc pha long c chun b chai to, ming rng, bng cch thi khng kh sch 20o C vo nc ct v lc nhiu ln cho bo ha xy, sau thm, 1mL dung dch m phtpht, 1mL dung dch MgSO4, 1mL FeCl3, nh mc n 1L bng nc ct. 7

Sau khi pha long xong, chuyn mu nc vo hai chai thy tinh nt mi. Xc nh BOD5 nh trnh by. pha long khuyn ngh xc nh BOD5 BOD5 d on (mg/L) H s pha long 3.6 gia 1 v 2 4.12 2 10.30 5 20.60 10 40.120 20 Lng BOD5 c tnh theo cng thc: BOD5 = (O2 u - O2 cui ) x k

k: h s pha long 2.8.2. Ha cht cn thit Cc loi ho cht nh lng O2 ho tan. Dung dch m phtpht: ha tan 8,5g KH2PO4 , 21,75g K2HPO4 , 33,4g Na2HPO4 , 1,7g NH4Cl trong 500mL nc ct v nh mc thnh 1L. Dung dch Mg SO4 : ha tan 22,5g Mg SO4.7 H2O trong 1L nc ct. Dung dch CaCl2 : ha tan 27,5g CaCl2 trong nc, nh mc thnh 1L. Dung dch FeCl3:ha tan 0,25g FeCl3.6H2O trong nc, nh mc thnh 1L. 2.9. Nhu cu xy ho hc (Chemical Oxygen Demand -COD) COD l lng xy cn thit cho qu trnh xy ho ho hc cc cht hu c trong nc thnh CO2 v H2O. i a s cc cht hu c c trong nc u mang c trng kh nn COD c trng cho kh nng tiu th xy ho tan trong qu trnh xy ho cht hu c. Vi ngha , COD c gi l xy ho ca nc. 2.9.1. Phng php xc nh a. Xc nh xy ho ca nc theo Phng php permangannat Phng php Permangannat l phng php ph bin rng ri xc nh oxy ha ca nc Kalipermangannat KMnO4 l tc nhn xy ho c th xy ho trong mi trng axit v mi trng kim. Phn hu ca KMnO4 xy ra khc nhau trong hai mi trng ny v s lng O2 c gii phng ra cng khc nhau. Trong mi trng axit : 2 KMnO4 H+ K2O + 2MnO + 5O (1)

Cc xt c to nn b ha tan trong H2SO4 3 H2SO4 + K2O + 2MnO K2SO4 + 2MnSO4 + 3H2O (2)

Nng ng lng ca KMnO4 trong phn ng ny: mol/ 5 [(1)+(2)] Trong mi trng kim: 8

2 KMnO4

K2O + 2MnO2 + 3O

Nng ng lng ca KMnO4 trong phn ng ny: mol/ 3 S xy ho c tin hnh trong mi trng axt khi hm lng ion Cl- trong nc nghin cu nh. Khi hm lng Cl- ln hn 300mg Cl- /L th tn hnh trong mi trng kim. V trong mi trng axt xy ra phn ng: 10Cl- + 2 KMnO4 + 8H+ = 5Cl 2 + Mn2+ + 2K+ + 4 H2O Thc t ion Cl- khng b xy ho bi O2 nn khng b tiu hao O2, phn ng xy ho kh ny gia Cl- v KMnO4 xy ra chm nhng c phn ng xy ho kh gia cc cht hu c vi KMnO4 xy ra cng mt lc trong mu nc lm tng tc . N.A.Silop (1904) gi trng hp ny l phn ng lin hp. V vy khi xc nh xy ho ca nc bng phng php Peramngannat trong mi trng axt khng chnh xc. Xc nh oxy ho ca nc trong mi trng kim theo phng php Permangannat It Thiosuphat Nguyn tc phng php Trong mi trng kim KMnO4 tin hnh xy ho cc cht kh theo phng trnh: 2KMnO4 K2O + 2MnO2 + 3O Lng KMnO4 cn tha li sau phn ng li b kh tip bng mt lng xc nh KI trong mi trng axt H2SO4 : 2KMnO4 + 10KI + 8 H2SO4 = 5I2 + 2MnSO4 + 6K2SO4 + 8H2O Lng I2 c gii phng ra, c chun bng Na2S2O3 ch th h tinh bt: I2 + 2Na2S2O3 = Na2S4O6 + 2NaI Trnh t tin hnh Mu tht: Cho vo bnh nn 50mL nc nghin cu, 1mL NaOH 20%; 10mL KMnO4 0,01N. un cch thy 10 pht. Ly ra ngui n nhit phng (c th nhng bnh nn vo chu nc lnh, ri thm 2mL H2SO4 25%, 2mL KI 10% lc u, yn ch ti 5 pht. Sau chun bng dung dch Na2S2O3 0,01N ch th h tinh bt. Ghi th tch Na2S2O3 (B mL). Trong bc ny ta thc hin c: S mili ng lng cht kh trong mu nc + cht kh ln trong thuc th v s t hu ca KMnO4 l: VKMnO2 + N KMnO4 VNa2S2O3 x NNa2S2O3 b.

Khi nng ca KMnO4 v Na2S2O3 u l 0,01N ta c: 10 . 0.01 - V Na2S2O3 . 0,01 hay 10. 0,01 B .0.01 Mu trng: Cho vo bnh nn 50mL nc ct, 1mL NaOH 20%, 10mL KMnO4 0,01N v tip tc lm nh mu tht. Ghi th tch Na2S2O3 tiu tn l A mL. Trong bc ny ta thc hin c: S mL ng lng cht kh c trong thuc th v lng t hu ca KMnO4 l: 0,01 . 10 A . 0,01 Vy s ml ng lng cht kh c trong mu nc l: (0,01 . 10 -B . 0,01) (0,01.10 - A . 0,01) = (A - B) . 0,01 S mili ng lng c trong 1L nc l: 9

( A B ). 0,01 x1000 50

Gi tr ny bngs mili ng lng O2 cn thit xy ho cht kh trong 1L nc. Vy s O2 cn thit xy ho kh trong 1L nc l:

( A B ). 0,01 .1000 .8 50

8: S miligam O2 tng ng vi 1 mili ng lng. Ha cht cn thit: Dung dch KMnO4 0,01N: cn 0,526g KMnO4 tinh khit ho hc ho tan trong 1L nc ct, chuyn vo bnh nh mc 1L ri thm nc ct n vch. Dung dch NaOH 20%: Ha tan 20g NaOH trong 100mL nc ct. Dung dch KI 10% :Ha tan 10g KI trong 100mL nc ct. Dung dch H2SO4 25%. Dung dch Na2S3O3 0,01N. Dung dch h tinh bt. 2.10. Ammonia NH4 + S c mt ca ammonia NH4 + bt ngun t s phn hy prtin trong thc n, trong cht thi vt nui v bi sn phm bi tit ca vt nui. Mt trong nhng phng php xc nh hm lng NH4+ l phng php Indophenol hoc cn c gi l phng php Phnat. 2.10.1. Nguyn tc Ammonia trong mu nc tc dng vi hypoclohrite v phenol di s xc tc mui Mn 2 + to ra phc cht mu xanh m c hp th cc i bc sng 630 nm. 2 Phenol + NH3 + 3OClindophenol + 2H2O + OH- + 3Cl(mu xanh)

Phng php ny gip xc nh hm lng ammonia tng s, v trong mi trng kim mnh ammonia ion ho (NH4+) s chuyn thnh ammonia khng ion ho (NH3). 2.10.2. Tin hnh Chun b mu - Cho 10mL nc mu vo bnh nn, thm 1 git MnSO 4, lc u, thm 0,5mL dung dch hypochlorous axit v 0,6mL dung dch thuc th phenat. Lc u. - Phc mu xut hin sau 10 pht v bn t nht 24 gi. o bc sng 630 nm. - o hp ph ca cc mu cn phn tch v mu chun bit trc hm lng ammonia. S dng cng thc sau tnh hm lng mamonia tng cng c trong cc mu nc phn tch: C1 A1 = C2 A2 = C2 = A 2 x C1 10 (9.1)

A1 Trong : C1 : hm lng ammonia trong mu chun. C2 : hm lng ammonia tng cng trong mu nc. A1 : hp th ca mu chun. A2 : hp th ca mu nc. 2.10.3. Ha cht - Dung dch hypochlorous axt: dng 10mL dung dch NaOCl 5% v 40mL nc ct, chnh pH khong 6,5 7 bng HCl. Dung dch ny bn trong mt tun. - Dung dch MnSO4 0,003M: Ha tan 50mg MnSO4.4 H2O trong 100mL nc ct. - Dung dch thuc th Phenate; ha tan 2,5g NaOH v 10g phenol trong 100mL nc ct. Dung dch dng trong mt tun. - Dung dch lu tr NH3: (1mL = 1mgN-NH3 = 1000 g N-NH3 ). Ha tan 3,819g NH4Cl ( sy kh 100oC), thm nc ct va 1L (1mL = 1mg N = 1,22mg NH3). - Dung dch chun N-NH3: (1mL = 10 g N-NH3) pha long 10mL dung dch lu tr vi nc ct va 1L (1mL = 0,010 mg N = 0,0122 mg NH3). - Hoc c th dng b test kit NH4 + / NH3 thay th cc ho cht cn pha trong phng php phn tch. 2.11. Nitrate NO3 : Nitrate l sn phm ca giai on xy ho cao nht trong chu trnh ca nit, ng thi cng l giai on cui cng trong tin trnh xy sinh hc cc hp cht hu c c cha nit. Mt trong nhng phng php xc nh nitrate l phng php Griees-Ilosvay. 2.11.1. Nguyn tc Trong phng php ny, ton b NO3- s b kh thnh NO2- nh bt Cadmi. NO2- phn ng vi sulfanilamide v N (1 naphthyl) ethylene diamine to ra mt cht nhum v c c mu hng m. Nh m hm lng ca n c th o c bng phng php o mu. Cng mu c hp ph cc i bc sng 410 nm. 2.11.2. Tin hnh - Chun b mu: cho 10mL nc mu vo bnh nn (do kh khn v ct kh Cd, nn c th dng b test kit NO3- to mu phn ng vi NO3- trong nc mu). - o bc sng 410nm. - o hp ph ca cc mu cn phn tch v mu chun bit trc hm lng nitrate. - S dng cng thc (9.1) tnh ton hm lng nitrate trong mu nc cn phn tch. 2.11.3. Ha cht - Dung dch N-NO3 lu tr (1mL = 0,1 mg N-NO3): ha tan 0,7218g KNO3 trong nc ct, nh mc thnh 1L. - Dung dch N-NO3 chun (1mL = 0,002 mg = 2 Mg N-NO3 ): pha long 2mL dung dch lu tr thnh 100mL c 1L dung dch chun = 2 g N-NO3 - S dng b test kit NO3 lm thuc th. 2.12. Pht phat PO4 3Trong thin nhin phtphat c xem l sn phm ca qu trnh ln ho, thng gp nng rt thp trong nc t nhin. 2.12.1. Nguyn tc 11

 nhit cao, trong mi trng axt, cc dng ca phtphat c chuyn v dng orthophtphat v s phn ng vi anionium molybdate phng thch axt molybdophosphoric, sau axt ny s kh bi SnCl2 cho molybdenum mu xanh dng. PO43- + 12 (NH4)2M0O4 + 24 H+ (NH4)3PO4. 12M0O3 + 21 NH4+ + 12 H2O (NH4)3PO4. 12M0O3 + Sn2+ Molybdenum + Sn4+ (xanh dng) 2.12.2. Tin hnh - Cho 20mL mu nc vo bnh nn, thm 0,5mL hn hp dung dch (NH 4)2M0O4/H2SO4, lc u. - Thm 3 git SnCl2 long, lc u. Mu xanh dng ca Molybdenum xut hin. o bc sng 882nm. - o hp th mu ca cc mu cn phn tch v mu chun bit trc nng phtpht. - S dng cng thc (9.1) tnh ton hm lng phtpht cn phn tch. 2.12.3. Ha cht - Dung dch H2SO4 9N: ha tan 50mL H2SO4 m c trong 200mL nc ct, va khuy va lm lnh. - Dung dch (NH4)2M0O4 10%: cn 10g (NH4)2M0O4 pha trong 100mL nc ct un nng. - Hn hp dung dch (NH4)2M0O4/H2SO4: trn 1 th tch (NH4)2M0O4 10% vi 3 th tch H2SO4 9N. - Dung dch SnCl2: ha tan 4,3g SnCl2.4H2O trong 10mL HCl c, thm nc ct n 100mL. - Dung dch SnCl2 long: ht 5mL dung dch SnCl2 va pha trn trong 20mL HCl 5%, sau mt t phn tch b i v pha li. - Dung dch phtpht lu tr: ha tan 219,5mg KH2PO4 khan (sy kh 105oC trong 1 gi) trong nc ct v nh mc thnh 1L (1mL = 50 g P-PO43-). - Dung dch phtpht chun: ht 5mL dung dch lu tr pha long thnh 100mL. Dung dch ny c nng 1mL = 2,5 g P-PO43-.

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