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5210 D. RESPIROMETRIC PHNG PHP ( XUT) 1. Tho lun chung a.

Nguyn tc: Respirometric phng php cung cp trc tip o lng oxy tiu th bi vi sinh vt t khng kh hoc mi trng oxy lm giu trong mt bnh kn trong iu kin khng i nhit v kch ng. b. S dng: Respirometry bin php oxy hp thu nhiu hn hoc t hn lin tc theo thi gian. Respirometric phng php hu ch nh gi: phn hy sinh hc ca cc ha cht c th, treatability hu c cng nghip cht thi; nh hng ca lng c bit n ca cc hp cht c hi trn phn ng oxy hp thu ca mt nc thi th nghim hoc ha hc hu c, nng m ti mt cht gy nhim hoc nc thi o c c ch sinh hc suy thoi, hiu qu ca phng php iu tr khc nhau nh kh trng, b sung dinh dng v iu chnh pH trn t l qu trnh oxy ha, nhu cu oxy cho qu trnh oxy ha c bn y cc vn sinh hc oxy ha; nhu cu s dng ging thch ng trong cc php o hp thu oxy sinh ha khc, chng hn nh pha long BOD th nghim, v s n nh ca cn. D liu Respirometric thng s c s dng tng i, c ngha l, trong mt so snh trc tip gia oxy uptakes t hai mu th nghim hoc t mt mu th nghim v kim sot. Bi v s khc bit vn c gia cc s dng, gia cc nn vn ha ging, trong s cc ng dng ca cc kt qu, v gia cc cng c, mt th tc duy nht cho kim tra respirometric p dng i vi tt c cc trng hp khng th c xc nh. V vy, ch c bn khuyn ngh v hng dn cho cc thit lp v th tc kim tra ton b c a ra. Thc hin theo hng dn ca nh sn xut cho hot ng chi tit c th cho cc cng c thng mi. c. Cc loi respirometers: Bn chnh loi respirometers thng mi c sn. Manometric respirometers lin quan hp thu oxy thay i p sut do tiu th oxy trong khi duy tr mt khi lng khng i. Lng th tch respirometers bin php oxy hp thu trong thay i gia tng trong khi lng kh t trong khi vn duy tr mt p lc khng i thi im c c. Respirometers in gim st lng oxy c sn xut bi in phn nc duy tr mt p lc oxy lin tc trong phn ng tu. Trc tip-u vo respirometers cung cp oxy mu t mt ngun cung cp oxy tinh khit thng qua o theo yu cu nh pht hin bi s khc bit p lc pht. Hu ht cc respirometers c instrumented cho php thu thp d liu v x l bng my tnh. Phn ngtu ni dung c trn ln bng cch s dng t hoc c kh khuy thit b hoc si bt giai on kh trong bnh phn ng thng qua giai on lng. Tt c cc respirometers loi b carbon dioxide c sn xut trong qu trnh tng trng sinh hc bng cch nh ch mt tp trung vt liu hp ph (dng ht hay gii php) trong bung phn ng khp kn hoc bng cch tun hon kh giai on thng qua mt my ch sn bn ngoi. d. Nhiu: Evolution kh khc hn CO2 c th gii thiu sai st trong p lc, khi lng o lng, iu ny l khng ph bin trong s hin din ca oxy ha tan. Khng y CO2 hp th s gii thiu li nu cc khon tin thch hp v nng kim thm khng c s dng. Nhit bin ng hoc khng y trn s gii thiu li. S dao ng ca p sut kh quyn c th gy ra li vi mt s respirometers. Tr nn quen thuc vi cc gii hn ca cc nhc c c s dng. e. Pht hin nng ti thiu: respirometers Hu ht doanh nghip thng mi c th pht hin nhu cu oxy trong gia nh nh l 0,1 mg nhng kim tra chnh xc ph thuc vo tng lng oxy tiu th vo thi im c, chnh xc ca p lc hoc o lng khi lng v nh hng ca nhit v kh p p lc thay i. Gii hn trn ca tc s dng oxy c xc nh bi kh nng chuyn oxy vo gii php t pha kh, m thng lin quan n cng pha trn. Chuyn thng gii hn phm vi t t hn 10 mg O2/ L / h cho cng thp trn trn 100 mg O2/ L / h cho cng cao trn. f. Quan h vi pha long BOD: Nhng bin i trong thnh phn cht thi, nng cht nn, trn, v nng oxy t mt ngun nc thi khc thng ngn cn s dng ca mt v tng mi quan h gia s hp thu oxy bi respirometers v 5-d, 20C, BOD (5210B, trn). Mi tng quan hp l chnh xc c th c c th cho nc thi c th. Thi k bnh o respirometric khng cn phi c 5 d v mi tng quan gi tr ngang nhau c th c thc hin gia 5-d BOD v s hp thu oxy respirometric pha long bt k thi im no sau 2 d. 1,2 im pha long ph bin v BOD respirometric dng nh xy ra khong 2 n 3 d cho nc thi, thnh ph trc thuc Trung ng. Tng quan gia cc php o respirometric v BOD 5-d i vi cht thi cng nghip v ha cht c th t nht nh. o Respirometric cng c th cung cp mt du hiu ca oxy sinh ha cui cng nhu cu (UBOD) (xem Phn 5210C). Trong nhiu trng hp, n l hp l xem xt rng-28 to oxy 30-d hp thu ch yu l bng vi UBOD.3 Thng thng hn, respirometers c s dng nh mt cng c chn on. Readout oxy lin tc tiu th trong cc php o respirometric ch tt hu, c tnh, hoc bt k bt thng trong cc phn hy sinh hc phn ng. S thay i trong hnh dng bnh thng ca mt ng cong hp thu oxy trong vi gi u tin c th gip xc nh nh hng ca cc cht thi c hi hoc bt thng vo mt nh my x l trong thi gian sa cha iu hnh.

g. Quan h vi phng php th nghim v cc giao thc khc: Phng php ny h tr hu ht cc giao thc v hng dn thnh lp bi T chc Hp tc v Pht trin Kinh t chu u (OECD) yu cu o hp thu oxy. h. Ly mu v lu tr: 1) Ly mu-Nu phn tch c bt u trong vng 2 gi ca b su tp mu, kho lnh l khng cn thit. Nu khng, gi mu di 4C t thi im thu tin. Bt u phn tch ca b su tp trong vng 6 gi; khi iu ny l khng th, ca hng ti hoc di 4 di C v bo co v nhit lu tr. Bao gi bt u phn tch hn 24 gi sau khi thu thp mu ly. 2) mu composite-Gi mu ti hoc di 4 C trong hp. Gii hn thi gian hp 24 h. S dng cng mt tiu ch cho vic lu tr cc mu ly, bt u o thi gian gi t kt thc giai on hp. Nh nc lu tr thi gian v iu kin vi kt qu. 2. Thit b a. Respirometer h thng: S dng b my thng mi v kim tra hng dn ca nh sn xut c th yu cu h thng, loi tu phn ng v khi lng, v c im hot ng c. b. Vn m hoc nc tm: S dng lin tc nhit phng, lng p bung, hoc b nc kim sot nhit 1C. Loi tr tt c nh sng ngn chn s hnh thnh oxy thc hin bi to trong mu. S dng mu , actinic bc chai phn tch bn ngoi ca mt lng p ti. 3. Ho cht Cng thc ca thuc th cc gii php c a ra cho khi lng 1-L, nhng khi lng nh hn hoc ln hn c th c chun b theo nhu cu. Loi b bt k thuc th cho thy du hiu ca s tng trng sinh hc hoc ha hc lng ma. Cc gii php chng khon c th c kh trng bng ni hp cung cp cho cuc sng cn hn s dng. a. Nc ct: Ch s dng cht lng cao, nc chng ct t mt hp khi hoc knh tt c vn (xem Phn 1080). Nc kh ion c th c s dng nhng thng cha s lng vi khun cao. Nc phi cha t hn 0,01 mg kim loi nng/L v c min ph ca clo, chloramines, kim n da, vt liu hu c, hoc axit. Lm cho tt c cc thuc th vi nc ny. Khi cc vng nc khc c yu cu cho mc ch th nghim c bit, nh nc r rng ngun v cht lng. b. Phosphate dung dch m, 1.5N: Ha tan 207 g natri dihydrogen phosphate, NaH2PO4.H2O, trong nc. Trung ha pH = 7,2 vi 6N KOH ( 3g di y) v pha long thnh 1 lt. c. Gii php clorua amoni 0.71N: Ha tan 38,2 g amoni clorua, NH4Cl, trong nc. Trung ha pH 7.0 vi KOH. Pha long n 1,0 L; 1 ml = 10 mg N. d. Dung dch canxi clorua, 0.25N: Ha tan 27,7 g CaCl2 trong nc v pha long thnh 1 L, 1 mL = 10 mg Ca. e. Gii php Magnesium sulfate, 0.41N: Ha tan 101 g MgSO4.7H2O trong nc v pha long thnh 1 L, 1 mL = 10 mg Mg. f. Gii php Ferric chloride, 0.018N: Ha tan 4,84 g FeCl3 6H2O trong nc v pha long thnh 1 L, 1 mL = 1,0 mg Fe. g. Gii php potassium hydroxide, 6N: Ha tan 336 g KOH trong khong 700 mL nc v pha long thnh 1 lt. THN TRNG: Thm KOH vo nc t t v s dng lin tc trn ngn chn s tch t nhit qu mc. Cch khc, s dng cc gii php thng mi c cha 30 n 50% KOH theo trng lng. h. Gii php Acid, 1N: Thm 28 mL conc H2SO4 hoc 83 mL conc HCl khong 700 mL nc. Pha long n 1L. i. Dung dch Alkali, 1N: Thm 40 g NaOH n 700 mL nc. Pha long n 1 lt. j. Cht c ch qu trnh nitrat ha: cht phn ng cp 2-clo-6-(trichloromethyl) pyridin (TCMP) hoc tng ng. * # (4) k. Glucose-glutamic acid gii php: cp thuc th kh glucose v cp thuc th acid glutamic 103C trong 1 gi. Thm glucose 15,0 g v 15,0 g acid glutamic nc ct v pha long thnh 1 lt. Trung ha pH 7,0 bng cch s dng 6N KOH ( 3g). Gii php ny c th c lu tr ln n 1 tun 4C. l. Cht in gii php (i vi respirometers in): gii php c ngh s dng ca nh sn xut. m. Sodium sulfite gii php, 0.025N: Ha tan 1,575 g Na2SO3 vi khong 800 mL nc. Pha long n 1 lt ny gii php l khng n nh, chun b hng ngy hoc khi cn thit. n. Theo di gii php yu t: Ha tan 40 mg MnSO4.4H2O, 57 mg H3BO3, 43 mg ZnSO4.7H2O, 35 mg (NH2) Mo7O24, v 100 mg Fe-chelate (FeCl-EDTA) vi khong 800 mL nc. Pha long n 1 L. Kh trng ti 120C v kPa 200 (2 atm) p lc trong 20 pht.

o. Gii php chit nm men: Thm 15 mg phng th nghim hoc t chit xut dc phm cp men bia n 100mL nc. Thc hin gii php ny lnh ngay lp tc trc mi bi kim tra, trong n c s dng. p. Dung dch dinh dng: 3 Thm 2,5 mL dung dch m phosphate (3b), 0,65 ml amoni clorua (3c), 1,0 mL canxi clorua (3d), 0,22 ml magnesium sulfate gii php (3a), 0,1 ml st clorua gii php (3f), 1 mL du vt yu t gii php (3n), v men 1 ml chit xut gii php (3o) khong 900 mL nc. Pha long n 1 Gii php ny cht dinh dng L. v nhng ngi sn v o trn c c bit xy dng s dng vi phng php OECD. (Ch : 10:01 tp trung gii php dinh dng c th c thc hin v pha long cho ph hp.) 4. Th tc a. Dng c hot ng: Thc hin theo hng dn respirometer nh sn xut th nghim, lp rp, hiu chun, v hot ng ca cc nhc c. Ch : ti a quy nh ca nh sn xut v gii hn ti thiu o lng khng phi lc no cng ging nh cc gii hn u ra c. Hy chc chn rng cc iu kin kim tra trong gii hn o. b. Th tch mu: mu khi lng hoc nng ca ha cht hu c c thm vo mch th nghim l mt chc nng d kin ca cc c tnh hp thu oxy v kh nng chuyn oxy ca cc nhc c. Nho khi lng hoc nng thp c th c yu cu cht thi c bn cao. Khi lng ln c th c yu cu cho sc mnh v thp cht thi ci thin chnh xc. c. Ghi d liu khong thi gian: Thit lp cc cng c cung cp cho c d liu trong khong thi gian ph hp. Khong thi gian 15 pht n 6 gi thng c s dng. d. Chun b mu: ng nht Nu mu cha cht rn ln settleable hoc c th ni trn mt ncc, ng nht n vi mt my xay sinh t v chuyn nhng phn kim tra i din trong khi tt c cc cht rn b nh ch. Nu c mt mi quan tm cho vic thay i.Phng php tiu chun cho Kim tra nc v nc thi c im mu, b qua bc ny. 2) iu chnh PH-Trung ha mu pH 7,0 vi H2SO4 hoc NaOH sc mnh nh vy ( s 3h v 3i) rng s lng thuc th khng pha long mu hn 0,5%. 3) kh clo-Trnh phn tch mu c cha clo cn li bng cch thu thp cc mu trc cc quy trnh kh trng bng clo. Nu clo cn li l hin ti, thng kh nh c m t trong 5) di y hoc yn trong nh sng 1 n 2 h. Nu Clo d vn cn, thm Na2SO3 gii php. Xc nh khi lng yu cu ca Na2SO3 gii php bng cch thm 10 ml 1 + 1 axit axetic hoc 1 + 50 H2SO4 v 10 ml dung dch kali iodid (10 g/100 mL) i vi mt phn ca mu. Chun vi 0.025N Na2SO3 gii php cho cc im kt thc tinh bt-iodine (xem Mc 4500-Cl.B). Thm vo mu v hiu ha mt khi lng t l ca gii php Na2SO3 xc nh trn, pha trn, v sau 10 n 20 min kim tra Clo d. Re ht mu (xem di 4h). 4) Cc mu c cha cht c hi Mt s cht thi cng nghip c cha kim loi c hi hoc hu c hp cht ny. Ny thng i hi phi nghin cu c bit v treatment. 5) nng oxy ban u Nu mu cha nng oxy ha tan trn hay di mong mun tp trung, vn ng hoc thng kh vi khng kh nn sch v c lc cho khong 1 h ngay lp tc trc khi th nghim. Ti thiu v ti a nng DO thc t s khc nhau vi mc tiu th nghim. Trong mt s trng hp, oxy tinh khit c th c thm vo cho cc tu respirometer tng nng xy trn mi trng xung quanh. 6) Nhit iu chnh Mang mu v nc pha long th nghim nhit mong mun (1C) trc khi lm pha long hoc chuyn giao kim tra tu. e. Pha long mu: S dng nc ct hoc nc t cc ngun khc ph hp ca vt cht hu c. Trong mt s trng hp, tip nhn nc sui c th c s dng pha long. Thm khi lng mu phn cho cc tu th nghim bng cch s dng -tip rng th tch pipet hoc thy tinh th tch khc ph hp. Thm nc pha long mu khong 80% khi lng cui cng mong mun. Thm mt lng thch hp ca cc cht dinh dng, khong cht, nitrat ha, m cht c ch nu mun, v vn ha ging nh m t trong s 4 e v h di y. Pha long mu khi lng cui cng mong mun. S tu th nghim chun b cho mi pha long ph thuc vo mc tiu th nghim v s lng sao chp mong mun. f. Cht dinh dng, khong cht v m: Thm nit amoniac cung cp mt COD: N: P 100:5:1 hoc TOC: N: P 30:5:1. Thm 2 ml canxi, magi, st clorua, v du vt gii php khong sn cho mi lt ca mu pha long, tr khi s lng cc khong cht c mt trong cc ban u mu. Yu cu pht pho s c p ng bi cc b m phosphate nu n c s dng (1 mL/50 mg/L COD hoc BOD cui cng ca mu pha long thng l duy tr pH gia 6.8 v 7.2). Hy thn trng trong vic thm b m phosphate vi cc mu c cha mui kim loi bi v pht pht kim loi c th ta v cho thy t c hi hoc c li hiu qu hn khi phosphate l khng c mt. tng thch vi OECD- kim tra, thay th cc cht dinh dng, khong sn, v cc khon m c lit k trong trang 3 cho cc cht dinh dng trn / khong cht m / s lng.

g. c ch qu trnh nitrat ha: Nu c ch qu trnh nitrat ha l mong mun, thm 10 mg 2-chloro-6(trichloromethyl) pyridin (TCMP) / mu L trong tu th nghim. Mu m c th d dng tiu toan ha bao gm sinh hc iu tr nc thi, cc mu ht vi nc thi c x l sinh hc, v sng waters. h. Gieo ht: Xem 5210B.4d 1) chun b cho ht ging. S dng lng ht ging vn ha ngn chn chnh tr trong phn ng hp thu oxy, nhng khng qu nhiu s hp thu oxy ca ht ging vt qu khong 10% s hp thu oxy ca mu ht ging. Xc nh s hp thu oxy ca vt liu ging nh i vi bt k mu khc. y l s kim sot ht ging. Thng thng, khi lng ht ging trong s kim sot ht ging nn c 10 ln khi lng c s dng trong cc mu ht ging. i. bnh: mu 20 C hoc nhit thch hp khc 1,0C. Chm sc m khuy thit b khng lm tng nhit ca mu. 5. Tnh ton chuyn i cc bi c c hp thu oxy, hy tham kho cc th tc ca nh sn xut. ng s hp thu oxy cho ht ging v pha long bi phng trnh sau: C = [A B (SA / SB)] (1000/NA) Trong : C = sa cha oxy hp th ca mu, mg / L, A = o oxy hp thu trong mu ht ging, mg, B = o oxy hp thu trong kim sot ht ging, mg, SA = khi lng ht ging trong mu A, mL, SB = khi lng ht ging trong mu B, mL, v NA = khi lng mu khng pha long trong mt mu mL,. 6. Qun l cht lng nh k s dng cc th tc sau y kim tra cht lng nc ct, dng c cht lng, dng c chc nng, v k thut phn tch bng cch o hp thu oxy bng cch s dng mt hn hp ca glucose v glutamic acid nh l mt gii php kim tra tiu chun. iu chnh nc xy dng mu kim tra nhit v bo ha vi DO bng cch np ga vi sch, hu c min ph lc khng kh. Bo v cht lng nc bng cch s dng thy tinh, ng, v chai sch. Chun b mt gii php th nghim bng cch b sung thm 10 gii php mL axit glutamic glucose-( 3k); 6 mL m phosphat ( 3b), 2 ml amoni clorua ( 3c), magnesium sulfate ( 3e), canxi clorua (3d), st clorua ( 3 f), v gii php nguyn t vi lng ( 3n) khong 800 mL nc. Thm 10 nitrat ha mg cht c ch (TCMP) / L. Thm ht ging t mt ngun ph hp nh c m t trong 4h cho mt t thi gian tr hn 6 gi (thng l 25 mL ni t gii php gii quyt chnh kim tra nc thi / L l ). Pha long n 1 lt. iu chnh nhit 20 1 C. Chun b mt trng ht ging bng cch pha long 500 mL hoc nhiu hn ca gii php ging n 800 mL bng nc ct. Thm cng mt s lng b m, cht dinh dng v TCMP nh trong cc gii php kim tra, v pha long n 1 L. iu chnh nhit 20 1 C. Ni th nghim cc gii php v ht ging gii php trng trong tu phn ng ring bit ca respirometer v trong 5 d 20C. Chy t nht ba ln lp li mi. Ht ging s hp thu oxy sa cha sau khi d 5 l 260 30 mg / L. Nu gi tr ca kim tra l bn ngoi phm vi ny, lp li cc th nghim bng cch s dng mt nn vn ha ht ging ti v tm kim nguyn nhn ca vn . 7. chnh xc v Bias a. chnh xc: Tiu chun Khng c sn kim tra tnh chnh xc ca s hp thu oxy respirometric o lng. c c d liu chnh xc trong phng th nghim, s dng glucose-hn hp axit glutamic ( 6 trn) c mt c bit n l thuyt gi tr ti a s hp thu oxy. Cc th nghim vi iu ny v hn hp hp cht hu c tng t ch ra rng lch chun, th hin l h s bin i, Cv, l khong 5% mu c uptakes oxy% mg / L v 3 50 100 tp trung nhiu hn samples. C nhn c ny u c gii hn kh nng c khc nhau c th nh hng n chnh xc. Cc phn ng ti thiu hay nhy ca respirometers thng mi nht dao ng t 0,05 n 1 oxy mg. Kim tra thng s k thut ca nh sn xut cho nhy ca thit b tay. b. Kim sot gii hn: thit lp cc gii hn kim sot phng th nghim, thc hin ti thiu ca axit glucose-glutamic 25 kim tra trong khong thi gian vi tun hoc vi thng v tnh ton trung bnh v lch chun. Nu c o s hp thu oxy trong 5 d 20 C l phm vi bn ngoi 260 mg / L 30, nh gi li th tc xc nh ngun gc ca li. i vi nhng mu khc, s dng gi tr trung bnh 3 lch chun nh l gii hn kim sot. c. Lm vic gii hn phm vi v pht hin: Phm vi lm vic v gii hn pht hin c thit lp bi gii hn ca mi dng c thng mi. Tham kho thng s k thut ca nh sn xut.