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METHOD 1311

QUY TRNH TCH CHIT CHT THI NGUY HI


1.0 PH M VI V NG DNG 1.1 Phng php tch chit cht thi nguy hi (TCLP) c dng xc nh tnh lu ng ca c cht hu c v v c hin din trong cht lng, t, v cht thi hn hp. 1.2 Nu phn tch tng cht thi cho thy thnh phn phn tch ring l khng hin din trong cht thi, hoc n c mt, nhng nng thp hn mc cho php th TCLP khng c p dng. 1.3 Nu phn tch mt trong cc phn nh c trong cht lng, pp TCLP ch ra rng mt hp cht c quy nh l c nng cao, ngay c sau khi pha long t cc phn khc ca dung dch ngm chit m nng vn cao hn so vi mc cho php l cht thi nguy hi v vic phn tch cc thnh phn cn li l khng cn thit. 1.4 Nu phn tch dung dch chit thu c bng cch s dng bnh chit cho thy nng ca cht d bay hi cn phn tch vt qu so vi mc quy nh, th cht thi l cht thi nguy hi nguy hi v qu trnh ngm chit s dng thit b ZHE l khng cn thit. Tuy nhin, chit xut c th khng c s dng chng minh rng nng ca hp cht d bay hi di mc quy nh 2.0 TM TT PHNG PHP 2.1 Cht thi lng (c cha t hn 0,5% cht rn kh ), sau khi lc qua mng si thy tinh 0,6 n 0,8 lc, s c phn tch nh pp ngm chit TCLP. 2.2 i vi cht thi c cha 0,5% cht rn. Cht lng c tch ra t pha rn v c lu tr phn tch sau. Kch thc ht ca pha rn c gim (nu cn). Cc phn rn c trch ly vi mt lng dung dch chit bng 20 ln trng lng ca pha rn. Dung dch trch ly c s dng ng vai tr nh kim ca pha rn trong cht thi. Mt bnh chit c bit c s dng khi kim tra cc phn tch cht bay hi (xem bng 1. danh sch cc hp cht d bay hi), cht lng sau ngm chit c tch khi pha rn bng qu trnh lc qua mng lc si thy tinh 0,6 n 0,8. 2.3 Nu tng thch ( nhiu pha khng hnh thnh trong s kt hp), cht lng ban u ca cht thi c s thm vo phn dung dch sau chit, v c phn tch vi nhau. Nu khng tng thch, cc cht lng c phn

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tch mt cch ring bit v kt qu s c kt hp chnh xc tnh ton cho mt nng trung bnh th tch ca cht thi. 3.0 CN TR 3.1 Nhng cn tr tim n c th gp phi trong qu trnh phn tch c cp trong cc phng php phn tch t bit 4.0 THIT B V CHT LIU 4.1 Thit b xoay: Thit b xoay phi c kh nng xoay bnh ngm chit t trn xung di (xem hnh 1) 30 2 rpm. Thit b ph hp theo EPA c xc nh trong bng 2 4.2 Bnh ngm chit

4.2.1 Bnh ngm chit Zero-Headspace (ZHE). Thit b ny s dng ch khi cht thi c th nghim cho cc phn tch tnh linh ng ca cht d bay hi (danh sch c lit k trong bng 1). Bnh ZHE (m t trong hnh 2) cho php phn tch cht lng/rn trong thit b, v c hiu qu ngn cn khong cch. Loi bnh ny cho php phn tch cht lng/cht rn ban u, ngm chit, v lc phn c chit cui cng m khng cn m bnh (xem phn 4.3.1). Bnh c th tch bn trong l 500600ml v c trang b ph hp vi mt b lc 90-100mm. Cc thit b c cha Viton o-ring nn c thay th thng xuyn. Thit b ZHE ph hp c EPA s dng c trnh by trong bng 3. i vi bnh ZHE c th chp nhn cho vic s dng, cc piston trong bnh ZHE s c th c di chuyn vi khong 15 psi hoc t hn. Nu n ly nhiu p sut di chuyn cc piston, th o-rings trong thit b nn c thay th. Nu iu ny khng gii quyt c vn , th bnh ZHE khng c s dng cho vic phn tch theo pp TCLP v nn lin lc vi nh sn xut . Bnh ZHE cn c kim tra r r sau khi ngm chit. Nu thit b cha ng h o p sut, th sc p ln thit b n 50 psi, cho php n dng li khng s dng trong 1 gi v kim tra li p sut. Nu thit b khng tch hp sn trong my o p sut, iu chnh p sut cho cc thit b n 50psi, nhn chm trong nc, v kim tra s hin din ca bt kh thot ra trong bt k b phn no ca thit b. Nu p sut b mt, kim tra tt c c b phn v thay th o-rings nu cn thit. Kim tra li thit b. Nu vn r r c th khng c gii quyt, cnlin lc vi nh sn xut. Mt s bnh ZHE s dng p lc kh vn chuyn piston trong bnh, trong khi s khc s dng p lc c hc (xem bng 3). Trong khi , quy trnh phn tch cht bay

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hi (xem phn 7.3) cp n p sut ( psi), i vi piston k thut, p sut s dng c o trong torqueinchipounds. Hy tham kho hng dn ca sn xut chuyn i thch hp. 4.2.2 Bnh chit xut. Khi cht thi c nh gi s dng pp ngm chit cht thi khng bay hi, mt ci l vi th tch cha mu v dung dch ngm chit cn s dng. Khong trng trong bnh c cho php. Bnh ngm chit c th c lm t cc vt liu khc nhau, ty thuc vo pp phn tch v tnh cht ca cht thi (xem phn 4.3.3). l khuyn co rng cc chai thy tinh borosilicate c s dng thay v cc loi thy tinh khc, c bit l phn tch cac cht v c. Cc chai nha, ngoi tr polytetrafluoroethylence, khng c s dng nu phn tch cht hu c. Cc loi bnh u c sn ti cc ca hnh cung cp thit b phng th nghim. Khi loi bnh ngm chit ny c s dng, th thit b lc tho lun trong phn 4.3.2 c s dng tch cht lng / rn ban u v lc phn ngm chit cui cng. 4.3 Thit b lc: Phng php ny ngh rng tt c cc qu trnh lc c thc hin trong t hood. 4.3.1 Zero - Headspace chit xut mch (ZHE) khi cht thi c c lng cho cht bay hi khng - headspace chit xut mch c m t trong phn 4.2.1 c s dng lc cc thit b phi c kh nng h tr v lu gi trong cc b lc si thy tinh. v c th chu c p lc cn thit thc hin vic tch (50 psi) LU : Khi c nghi ng rng b lc si thy tinh b v.b lc si thy tinh c th c s dng lm vt liu lc bn trong Zhe 4.3.2 B lc cm tay: khi phn tch cht thi khc hn so vi phn tch cht d bay hi, b lc c kh nng h tr b lc si thy tinh v c kh nng chu c p lc thc hin vic tch .B lc ph hp vi cc n v chn khng n gin n cc h thng tng i phc tp c kh nng to p lc ln 50psi hoc nhiu hn. Kiu lc holder c s dng ph thuc vo tnh cht ca vt liu c lc (xem phn 4.3.3) cc thit b ny s c mt th tch ti thiu bn trong 300 ml v c trang b cha mt b lc kch thc ti thiu l 47 mm (b lc cm tay c cng sut 1.5L hoc cao hn v c trang b cha mt b lc ng knh 142 mm, c khuyn co lc chn khng ch c th c s dng i vi cht thi vi cht rn thp (<10%) thay cho cc dng ht ln. Cht thi lng c cha tt c cc loi khc cht thi c lc bng cch s dng lc p lc dng. Thch hp b lc ch c bit n EPA c th hin trong bng 4.

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4.3.3 Cht liu: chit xut mch v cc thit b lc c lm bng vt liu tr khng thm hoc hp th cc thnh phn cht thi . Thy tinh, polytetrafluoroethylene (PTEE), hoc loi 316 khng b bng thp c th c s dng khi nh gi tnh linh ng ca c hai thnh phn hu c v v c.Thit b lm polythylene mt cao (HDPE), polypropylence (PP) hoc choride polyvinyl (PVC) c th ch c s dng khi nh gi tnh di ng ca kim loi. Chai thy tinh borosilicate c ngh s dng trn kiu chai thy tinh c bit l khi cc cht phn tch quan tm l v c. 4.4 B lc: b lc c lm bng si thy tinh borosilicate, khng c vt liu cht kt dnh, v phi c mt kch thc l 0,6 n 0,8 m hoc tng ng. B lc ca EPA p ng c im k thut ny trong bng 5. Lc s b khng c s dng. Khi nh gi tnh linh ng ca kim loi, b lc c ra sch trc khi s dng bng cch ra bng axit nitric 1N, sau dng nc ct kh Ion ra 3 ln (ti thiu l 1 lt cho mi ln ra ). B lc si thy tinh rt mng manh v cn c s dng cn thn. 4.5 My o pH: o phi chnh xc n 0,05 n v 25oC. 4.6 Thit b thu dung dch sau ngm chit ZHE: TEDLAR ti hoc thy tinh, thp khng g hoc PTFE ng bm kn kh c s dng thu tpha lng ban u v dung dch ngm chit cui cng ca cht thi khi s dng thit b ZHE. Cc thit b c lit k c khuyn ngh cho s dng theo cc iu kin sau y: 4.6.1 Nu cht thi c cha pha lng hoc cht thi khng cha mt lng ng k cht lng (<1% tng cht thi), ti TEDLAR hoc syringe 600ml c s dng thu v kt hp cht lng ban u v phn rn c chit ra. 4.6.2 Nu cht thi c cha mt lng ng k ca cht lng trong pha lng ban u> 1% tng cht thi, syringe hoc ti TEDLAR c th c s dng cho c phn tch cht rn / cht lng ban u v phn chit ra cui cng. Tuy nhin, cc nh phn tch cn s dng mt loi trong 2 loi trn hoc loi khc hoc khng s dng c hai loi trn. 4.6.3 Nu cht thi khng c cha cht lng ban u (100% cht rn) hoc pha rn khng ng k (100% cht lng), th ti TEDLAR hoc ng bm c th c s dng. Nu ng bm c s dng, th loi b nhanh 5ml u tin ca cht lng khi thit b. Phn cn li c s dng phn tch. 4,7 Thit b chuyn i dung dch ngm chit ZHE: bt k thit b c kh nng chuyn dch chit v ZHE m khng thay i bn cht ca dch ngm

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chit c th chp nhn c (v d nh mt chuyn r rng hay bm nhu ng ng bm kh kn, p lc filtractionn v (xem phn 4.3.2) hoc cc thit b ZHE khc. 4,8 Cn phng th nghim : bt k cn phng th nghim chnh xc 0,01 gram c th c s dng (tt c cc o lng trng lng l c trong vng 0,1 gram) 4,9 Cc thy tinh hoc bnh thy tinh erlenmeyer, 500ml 4,9 Cc thy tinh hoc bnh thy tinh erlenmeyer, 500ml 4,11 Khuy t 5.0 THUC TH 5.1 Thuc th c s dng trong tt c cc bi kim tra. Tr khi c ch nh khc, tt c cc thuc th phi ph hp vi cc chi tit k thut ca y ban v hi thuc th phn tch ha hc Americal chi tit k thut nh vy. mt khc c th c s dng n l ln u tin c xc nh l thuc th c tinh khit cao cho php vic s dng ca n m khng lm gim tnh chnh xc ca vic xc nh 5.2 Thuc th nc nc tinh khit c nh ngha l nc, trong khng quan st thy trn gii hn pht hin ca phng php ca cc cht phn tch quan tm.cho nc khng bay hi ASTM loi II hoc tng ng p ng nh ngha ca nctinh khit.chit xut d bay hi, n l nc tinh khit c to ra bi bt k phng php sau y.nc tinh khit nn c theo di nh k cho cc tp cht 5.2.1 Thuc th nc cho chit xut d bay hi c th c to ra bng cch i qua nc my thng qua mt lp l carbon c cha khong 500 gram than hot tnh (Calgon corp, filtrasorb 300 hoc tng ng 5.2.2 Mt H thng lc nc (millipore siu-Q hoc tng ng) cng c th c s dng to ra nc tinh khit cho chit xut d bay hi 5.2.3 Thuc th nc cho chit xut d bay hi cng c th c chun b bng nc si trong 15 pht .V duy tr nhit nc 905 C, bt kh khng c cht gy nhim-kh tr (v d nh nit) thng qua nc trong 1 gi. trong khi vn cn nng chuyn nc n ming chai sit np chai dizero-headspace v con du vi mt teflon - lt vch ngn v np 5,3 Hyrochcoric axit HCl 1N c lm t loi thuc th ACS 5,4 Axit nitric 1N HNO3 c thc hin t lp thuc th ACS

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5.5 Xt NaOH 1N lm t loi thuc th ACS 5,6 Acid acetic 1N CH3CH2OOH t lp thuc th ACS 5,7 Dung dch ngm chit 5.7.1 Dung dch ngm chit s 1: cho 5,7 ml CH3COOH vo 500 mL ca nc tinh khit (xem phn 5,2), thm 64,3mL dd NaOH 1N, v pha long thnh 1L. Khi c pha chnh xc, pH ca dung dch ny s l 4,93 0,05. 5.7.2 Dung dch ngm chit s 2: Pha long 5,7 ml CH3COOH vi nc tinh khit (Xem Phn 5.2) thnh 1L. Khi pha chnh xc, pH ca dung dch ny s l 2,88 0,05. LU : Cc dung dch ngm chit nn c theo di thng xuyn i vi cc tp cht. pH phi c kim tra trc khi s dng m bo rng cc dung dch c pha chnh xc. Nu c tp cht hoc pH khng nm trong khong c bit trn, th dung dch phi c loi b v chun b li dch ngm chit. 5.8 Tiu chun phn tch phi c chun b ph hp vi phng php phn tch. 6.0 LY MU, BO QUN V X L 6,1 Tt c cc mu s c ly bng cch s dng mt chng trnh ly mu ph hp 6,2 TCLP c th t yu cu v kch thc ti thiu phm vi ca mu , ph thuc vo trng thi vt l hoc trng thi ca cc cht thi v phn tch quan tm. Cn nh gi s b, trong chit xut cht lng c s dng cho quy trnh chit xut cht phn tch khng bay hi.c th l cn thit thc s tin hnh vic chit xut khng bay hi(Xem mc 1.4 lin quan n vic s dng chit xut ny i vi cc cht hu c d bay hi). Nu hu c d bay hi c quan tm.Bin php kim sot cht lng c th yu cu thm. Hn na, kinh nghim thu mu ch trong trng hp h gp kh khn vi cc n lc ban u tin hnh cc kim tra 6,3 Cht bo qun khng c thm vo mu trc khi chit xut. 6.4 Mu c th c lm lnh, tr khi kt qu lm lnh thay i tnh vt l ca cht thi. Nu kt ta xy ra, ton b mu (bao gm kt ta) nn c ngm chit. 6,5 Khi cht thi phn tch cht d bay hi, thc hin cn thn gim thiu thit hi ca cht bay hi. Mu s c thu v lu tr ngn chn s mt mt ca cht

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d bay hi (mu v d nh phi c thu trong l Teflon lt vch ngn c np y v bo qun 4oC mu nn c m ngay khi trch xut) 6,6 PP ngm chit TCLP nn c chun b phn tch v phn tch ngay sau khi chit . Cht chit hoc phn chit phn tch kim loi phi c axit ha bng axit nitric pH <2, tr khi kt ta xy ra (xem phn 7.2.14 nu kt ta xy ra). Cht chit cn bo qun i vi cc cht phn tch khc theo hng dn c a ra trong cc phng php phn tch ring. Cht chit hoc cc phn ca cc cht chit phn tch hu c s khng c php tip xc vi khng kh (tc l khng c khong cch ) ngn chn tn tht.Xem phn 8,0 (bo m cht lng yu cu) 7.0 TIN HNH 7.1 nh gi s b Thc hin cc nh gi TCLP s b ti thiu l 100 gram cht thi. c th khng thc t tri qua chit xut TCLP. Nhng nh gi s b bao gm: 1: xc nh cc cht rn % (mc 7.1.1) 2 xc nh liu cht thi c cha cc cht rn khng ng k l trch xut ring ca n sau khi lc (mc7.1.2) 3 xc nh vic liu phn rn ca cht thi i hi phi gim kch thc ht (mc 7.1.3) v (4) xc nh ca dch chit xut c s dng tch TCLP khng bay hi ca cht thi (mc7.1.4) 7.1.1 Xc nh s b ca % cht rn: % cht rn c nh ngha nh phn nh ca mt mu cht thi (nh l mt t l phn trm ca tng s mu)m t cht lng khng c th b buc ra bi mt p lc p dng, theo m t di y 7.1.1.1 Nu cht thi r rng l khng c cht lng khi b lc p lc (v d nh l 100%t) tin hnh mc 7.1.3 7.1.1.2 Nu mu l cht lng, tch cht lng / rn multiphasic lm s b ca% cc cht rn l cn thit. iu ny lin quan n thit b lc c m t trong mc 4.3.2 v c trnh by trong mc 7.1.1.3 thng qua 7.1.1.9 7.1.1.3 Pre-Cn cc b lc v bnh cha s cha c dch lc. 7.1.1.4 Lp rp cc bnh cha b lc v b lc theo hng dn ca nh sn xut. t b bnh cha trn tm chn chng chc chn 7.1.1.5 Cn mu ph cht thi (100 gram ti thiu) v ghi li trng lng 7.1.1.6 Cho php cho php pha rn .Cht thi c th c ly tm trc khi lc nu s

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dng cht lng nn c chit ra bnh v lc tip theo l lc ca phn rn cht thi mc d cng bnh cha h thng lc 7.1.1.7 s lng chuyn cc mu cht thi n holder lc | (pha cht lng v rn). cc mu cht thi tri u trn b mt ca b lc. Nu lc cc cht thi ti 4oC lm gim s lng cht lng r rng. nhit phng sau cho php cc mu lm nng ln n nhit phng trong cc thit b lc trc LU : Nu thnh phn cht thi (> 1% trng lng muban u) r rng tun th thng cha, c s dng chuyn mu cho b my lc, xc nh trng lng cht thi ny v tr i trng lng mu c xc nh trong mc 7.1.1.5 xc nh trng lng ca mu cht thi s c lc. Tng bc p dng chn khng hoc p lc nh nhng 1-10psi, cho n khi khng kh c nn di chuyn qua cc b lc. Nu im ny l khng t di 10 psi, v nu khng c cht lng b sung c thng qua b lc trong bt k khong thi gian 2 pht, t t lm tng p lc trong10psi tng n ti a l 50 psi. Sau khi mi s tng thm l 10 psi, nu kh nn khng di chuyn ngha rng cc b lc, v khng c cht lng b sung qua b lc trong khong thi gian 2 pht ,tin hnh tng 10psi. Khi kh nn bt u di chuyn qua cc b lc, hoc khi dng chy cht lng ngng 50 psi (v d: lc khng kt qu trong bt k dch lc them trong bt k khong thi gian 2 pht) dng lc. LU : ng dng tc thi ca p sut cao c th lm suythoi cc b lc si thy tinh v c th gy ra smHnh ng hay qu trnh lm ngng dng nc, du hay kh chy vo hay ra mt thnh h thng qua l khoan hay ging xuyn qua thnh h . 7.1.1.8 Cc vt liu trong b lc ch c xc nh l pha rn ca cht thi, v lc c quy nh nh pha lng LU : Mt s cht thi, chng hn nh cht thi du v mt s cht thi sn, r rng s c mt s nguyn liu l mt loi cht lng. Ngay c sau khi p dng chn khng hoc lc p lc, nh nu ti mc 7.1.1.7 vt liu ny khng c th lc. Nu y l trng hp, cc vt liu trong thit b lc c xc nh l mt cht rn. Khng thay th cc b lc ban u vi mt b lc trong bt k trng hp no. S dng duy nht mt b lc.

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7.1.1.9 Xc nh trng lng ca pha cht lng bng cch tr i trng lng ca bnh ng cht lc(xem Phn 7.1.1.3) t tng trng lng ca bnh ng cht cha y dch lc.Xc nh trng lngca pha rn ca mu cht thi bng cch tr i trng lng ca pha cht lng t trng lng ca mucht thi tng s, c xc nh trong mc 7.1.1.5hoc 7.1.1.7 Ghi li trng lng ca pha lng v rn. Tnh% rn nh sau:
trng lng ca rn (phn 7.1.1.9)* 100

%t=

Tng trng lng ca cht thi (phn 7.1.1.5 hoc7.1.1.7

7.1.2. nu %cc cht rn xc nh trong phn 7.1.1.9 bng hoc ln hn 0,5%, sau tin hnh hoc mc 7.1.3 xc nh xem cc vt liu rn i hi gim kch thc ht hoc mc 7.1.2.1 Nu nhn thy rng mt lng nh ca dch lc l b cun theo s thm t ca b lc.Nu %cc cht rn xc nh trong mc 7.1.1.9 t hn 0,5%, sau tin hnh mc 7.2.9 nu TCLP khng bin i c thc hin phn 7,3 vi mt phn r rt cht thi nuTCLP d bay hi c thc hin 7.1.2.1. Loi b cc pha rn v b lc t b my lc 7.1.2.2 Lc kh v pha rn 100200C cho n 2 trng lng lin tip c gi tr nm trong thi hn 1% trng lng cui cng LU : Thn trng thc hin m bo rng cht rn i tng s khi nng . l l l sy cho thot ra mt hood hoc thit b thch hp khc 7.1.2.3 Tnh cht rn % kh nh sau

(WT. cht thi kh + lc) -Trng lng b wt. ca b lc * 100 % cht rn kh = cht thi Ban u wt. (mc 7.1.1.5 hoc 7.1.1.7) 7.1.2.4 Nu % cht rn kh l t hn 0.5% sau tin hnh phn 7.2.9 nu TCPL khng bay hi c thc hin, v phn 7.3 nu TCLP d bay hi c thc hin. Nu cc cht rn kh ln hn hoc bng 0.5%. v nu cc TCLP khng bay hi c thc hin , quay tr li bt u ca phn 7.1, vi mt phn r rt cht thi.Xc nh vic gim kch thc ht l cn thit ( phn 7.1.3) v xc nh dch chit thch hp ( mc 7.1.4) nu ch c TCLP d bay hi c thc hin , xem ghi ch trong mc 7.1.4 7.1.3 Xc nh vic cht thi i hi phi gim kch thc ht ( kch thc ht gim trong bc ny ) bng cch s dng phn cht rn ca cht thi , nh gi vng chc cho

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cc kch thc ht gim kch thc ht l cn thit tr khi cht rn c b mt mi gram ca vt liu bng hoc ln hn 3.1 cm2 hoc nh hn 1 cm trong khng gian hp ca n ( VD c kh nng i qua dy 9.5mm( 0.375 ich ) tiu chun kch thc . Nu din tch b mt nh hn hoc ht cho chit bng cch nghin, gim nghin cht thi din tch b mt hoc kch thc ht nh m t trn nu cc cht rn ang chun b cho chit cht bay hi hu c, cc bin php phng nga c bit phi thc hin ( xem mc 7.3.6) LU : Tiu chun din tch b mt c ngha l si ph liu ( VD nh giy, vi v tng t ) o c thc t din tch b mt l khng cn thit . i vi nguyn liu khng r rng p ng cc tiu ch , phng php mu c th s cn phi c thit lp v s dng o din tch b mt. Phng php nh l khng c sn 7.1.4 Xc nh phng php tch chit cht lng thch hp: nu thnh phn rn ca cht thi 0.5% v nu mu c tch chit cho cc thnh phn khng bay hi (phn 7.2) th xc nh phng php tch chit cc thnh phn khng bay hi nh sau: LU : ch ly mu cha thnh phn bay hi (phn 5.7.1). nu khng yu cu ly mu cha thnh phn khng bay hi th xem phn 7.3 7.1.4.1 Cn mt lng mu sao cho phn rn l rt nh, gim phn rn (nu cn thit) n ng knh ht khong 1mm hoc thp hn, chuyn 5g phn rn ca cht thi vo erlen 500ml. 7.4.4.2 Thm 96.5ml thuc th vo cc, y li v khuy mnh trong 5 pht bng my khuy t. o pH, nu pH < 5, dng cch tch chit mu #1. Tin hnh theo phn 7.2 7.1.4.3 Nu pH > 5, thm 3.5ml HCl 1N, trn u, y li v un n 500C v gi 500C trong 10 pht. 7.1.4.4 ngui n nhit phng v o pH. Nu pH < 5, dng cch ly mu #1. Nu pH > 5, dng cch tch chit mu #2. Tin hnh theo phn 7.2 7.1.5 Nu pha long mu cht thi nh gi s b (phn 7.1.1-7.1.4) v c xc nh bng 100% cht rn phn 7.1.1.1, th n c th c dng cho phn ly mu 7.2 (gi nh cn t nht 100g), v phn 7.3 (gi nh mu cn t nht 25g). Pha long mu theo phn 7.1.1.7, phng php tch chit cc thnh phn bay hi theo phn 7.3. Pha long mu theo phn 7.1.1.7 thch hp vi phng php tch chit phn 7.2 nu thu c ton b phn rn (xc nh mc 7.1.1.9). Lng cht rn cn thit ph thuc vo lng lng cht rn trong qu trnh tch chit nh hng n qu trnh

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phn tch.. Nu cn li lng cht rn, tin hnh theo phn 7.2.10 tch chit phn khng bay hi. 7.2 QUY TRNH PHN TCH KHNG BAO GM CHT BAY HI Khng nn dng lng mu t khong 100g (bao gm c phn rn v phn lng). Trong mt s trng hp, lng mu nhiu s tt hn, ph thuc vo thnh phn rn ca mu cht thi (phn trm thnh phn rn, xem phn 7.1.1), trong phn cht lng ban u ca cht thi s c trn ln vi phn cht lng tch chit ra khi phn rn, v trong phn v c, nhng cht hu c bn n nh, thuc tr su, thuc dit c l nhng cht cn phn tch. Cn phi tch chit lng cht rn p ng cho tt c cc ch tiu cn phn tch cn thit. Nu mt ln tch chit khng lng cht rn phn tch tt c cc ch tiu th c th thc hin tch chit nhiu ln v trn li phn tch. 7.2.1 Nu khng cn cht lng sau khi lc (100% cht rn, xem 7.1.1), cn t nht 100g cht thi v tin hnh theo phn 7.2.9 7.2.2 Nu mu lng hoc st th cn phi tch ring phn rn v phn lng. Cn phi c thit b lc nh m t trong phn 4.3.2 v phn gch di trong phn 7.2.3 ti 7.2.8. 7.2.3 Cn dng c s cha cht thi trc. 7.2.4 Lp rp thit b lc theo hng dn ca nh sn xut. t giy lc vo mng v vn cht. Ra thit b lc bng acid (xem phn 4.4) Ghi ch: Acid ra lc, c th s dng cho tch chit tt c cc thnh phn khng bay hi, thm ch nhng kim loi khng quan tm. 7.2.5 Cn t nht 100g cht thi. nu cht thi cha thnh phn rn kh <0.5% (phn 7.1.2), phn lng ca cht thi, sau khi lc, c xc nh khi tch chit TCLP. V vy, cn lng mu lng nc sau lc c th dng phn tch tt c cc ch tiu cn thit. i vi cht thi c lng rn kh > 0.5% (phn 7.1.1 n 7.1.2), s dng thng tin phn trm rn kh trong phn 7.1.1 xc nh lng mu ti u (t nht 100g) lc. 7.2.6 Nhng mu bn c th lng phn rn. Cht thi lng chm cn phi li tm trc khi lc. Ch s dng my li tm h tr cho qu trnh lc. Nu cht thi c li tm, phn cht lng cn c chit ra v lc qua thit b lc ca phn cht rn trong cht thi qua cng mt h thng lc. 7.2.7 Cho mu cht thi (phn lng v rn) vo thit b lc (xem phn 4.3.2). Tri u mu cht thi ln b mt thit b lc. Nu lc 40C lm gim lng cht lng so vi nhit phng th lm m mu n nhit phng trong thit b thch hp trc khi lc.

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Ghi ch: nu cht thi (>1% so vi khi lng ban u ca mu) bm vo thit b cha mu khi chuyn mu sang thit b lc, xc nh khi lng ca phn cn li ny v tr khi khi lng mu (xc nh trong phn 7.2.5), xc nh khi lng mu thc s lc. Ht chn khng t t hoc p sut khong 1-10psi, cho n khi khng kh khoc kh nn i qua thit b lc. Nu khng t di 10 psi, v nu cht lng khng qua c thit b lc trong 2 pht, tng t t p sut trong 10psi n ti a 50psi. Sau mi ln tng ln 10psi, nu kh nn v cht lng khng lc qua c trong 2 pht th tip tc tng ln 10psi na. Khi kh nn bt u qua lc hay khi dng cht lng ngng 50psi (khng lc thm c na trong 2 pht), dng qu trnh lc. Ghi ch: s gia tng p sut cao t ngt c th lm thoi ha giy lc si thy tinh v c th gy tt nghn sm. 7.2.8 Vt liu c gi li trong thit b lc l phn rn, phn nc sau lc l phn lng, cn phn nc sau lc. Phn cht lng ny c th mang i phn tch (xem phn 7.2.12) hoc tr 40C cho n khi phn tch. Ghi ch: vi loi cht thi nh cht thi c cha du v cht thi sn c cha mt s cht trong cht lng. Thm ch khi ht chn khng hay tng p sut th nhng cht ny c kh nng khng lc c. Trong trng hp ny, vt liu trong thit b lc xem nh phn rn v c trch ly nh cht rn. Ch s dng mt thit b lc duy nht. 7.2.9 Nu cht thi cha <0.5% cht rn kh (xem phn 7.1.2), tin hnh theo phn 7.2.13. Nu cht thi cha <0.5% cht rn kh (xem phn 7.1.1 hoc 7.1.2), v nu cn lm gim kch thc ht ca cht rn nh trong phn 7.1.3, tin hnh theo phn 7.2.10. Nu cht thi qua ry 9.5mm, chuyn lng vt liu rn vo bnh trch ly cng vi giy lc dng tch ring phn nc v phn rn, v tin hnh nh phn 7.2.11. 7.2.10 Chun b phn rn trch ly bng cch nghin, ct, hay tn nhuyn cht thi n mt din tch b mt (kch thc ht) nh m t trong phn 7.1.3. Khi din tch b mt (kch thc ht) ph hp, chuyn lng cht rn ny vo bnh trch ly. Bao gm phn giy lc dng tch ring phn lng v phn rn. Ghi ch: Thng thng khng cn ry cht thi. Yu cu din tch b mt cho cc vt liu dng si nh giy, vi.. v tng t nh vt liu thi. Thc t khng cn tnh n din tch b mt. Nu cn thit phi ry, nn dng lp ph Teflon (L tn thng mi cho cht plyme ca polytetrafluoroethylene c c tnh ha hc l tr chng cc loi thuc th ngoi tr kim loi kim nung chy. Mt loi nha thng dai, bn cha floruacacbon c c tnh chng nhit dng trong ng gi, chu lc, b lc, cht cch in, dng c nu n v hn ch) trnh nhim bn mu.

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7.2.11 Xc nh dung dch trch ly thm vo bnh trch ly nh sau: Khi lng ca dd trch ly =
20 %chatran (7.1.1) khoiluongc hatthaisau loc 100

Thm t t dung dch trch ly (7.1.4) vo bnh trch ly. Vn cht bnh trch ly (nn dng dy Teflon m bo bt kn), lp vo thit b quay, v quay 305 vng/pht trong 182 gi. Nhit mi trng gi 2320C trong sut thi gian trch ly. Ghi ch: trong qu trnh chuyn ng, i vi mt s loi cht thi nh vi hay CaCO3 cha cht sinh kh CO2, p sut c th tng ln trong bnh trch ly. m bo p sut trong sut qu trnh trch ly, nn m np bnh nh k 15 pht, 30 pht v 1 gi thng kh. 7.2.12 Trch ly 182 gi, tch thnh phn lng v rn trong bnh trch ly bng cch lc qua giy lc si thy tinh mi, xem phn gch di trong phn 7.2.7. Bc lc cui cng ca trch ly TCLP, giy lc si thy tinh c th i nu cn thit m bo qu trnh lc. Giy lc nn c ra acid (xem phn 4.4) nu phn tch kim loi. 7.2.13 Chun b trch ly TCLP nh sau: 7.2.13.1 Nu cht thi ban u khng cha cht lng th cht lng c c t phn 7.2.12 l dung dch trch ly. Tin hnh phn 7.2.14. 7.2.13.2 Nu ph hp (nhiu pha kt hp s khng c kt qu), kt hp cht lng sau lc t phn 7.2.12 vi phn cht lng ban u ca cht thi trong phn 7.2.7. Kt hp 2 cht lng ny c xem nh trch ly TCLP. Tin hnh theo phn 7.2.14. 7.2.13.3 Nu phn cht thi ban u ca cht thi (phn 7.2.7) khng tng thch vi phn cht lng sau lc (7.2.12) th khng kt hp hai loi cht lng ny. Phn tch phn cht lng, xc nh nh trch ly TCPL, v kt hp tnh ton kt qu theo phn 7.2.14 7.2.14 Nn o pH ca dung dch trch ly, pha long v tr dung dch phn tch. Phn tch kim loi th phi acid ha bng acid nitric n pH < 2. Nu quan st thy cn khi thm adic nitric th phn cn li ca dung dch ko cn acid ha phn tch kim loi v phn tch sm nht c th. Tt c nhng phn pha long khc ca dung dch phi c tr lnh 40C cho n khi phn tch. Trch ly TCLP phi c chun b v phn tch bng phng php thch hp. Trch ly TCLP phn tch kim loi cn c phn hy bng acid tr nhng trng hp s phn hy lm mt nhng kim loi cn phn tch. Nu phn tch dung dch sau trch ly cha phn hy cho thy nng kim loi phn tch vt qu mc kim loi n nh th cht thi l nguy hi v vic phn hy dung dch sau trch ly l khng cn

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thit. Tuy nhin, s liu phn tch dung dch sau trch ly khng phn hy khng th kt lun cht thi khng nguy hi. Nu nhng pha ring l c phn tch ring bit, xc nh nng ca cc pha ring bit ( n 0.5%), tin hnh phn tch thch hp, v kt hp kt qu bng trung bnh th tch khi lng. Nng phn tch cui cng = Trong : V1: Th tch ca pha u (l) C1: Nng ca ch tiu phn tch trong pha u (mg/l) V2: Th tch ca pha th hai (l) C2: Nng ca ch tiu phn tch trong pha th hai (mg/l) 7.2.15 So snh nng phn tch trong dung dch sau trch ly TCLP vi mc quy nh trong quy chun thch hp. Tham kho phn 8.0 m bo cht lng yu cu. 7.3 PHNG PHP PHN TCH CHT BAY HI Vic s dng bnh chit ZHE thu c dung dch chit TCLP ch p cng cho cc phn tch hp cht bay hi. Kt qu ngm chit t vic s dng bnh ZHE s khng c s dng nh gi tnh d bin i ca cc phn tch hp cht khng bay hi (nh: kim loi, thuc tr su ). Bnh chit ZHE c kh nng cha bn trong xp x 500 mL. V vy, bnh ZHE c th cha c ti a 25 g cht rn (c nh r rng phn nh mu khng c cht lng s chu p sut 50 psi), bi v cn thit thm vo mt lng dung dch ngm chit bng 20 ln khng lng ca cht rn. Cho mu vo bnh ZHE mt ln v khng m bnh cho n khi ngm chit kt thc (ca cht rn) c ly ra. mu vo bnh ZHE ln na thu c 25g cht rn l khng c php thc hin. Khng cho php cht thi, cht lng ban u, hoc dung dch ngm chit b phi trn vi khng kh bt k ln no l rt cn thit. Bt k thao tc thc hin vi mu nn c thc hin khi lm lnh (4oC) hn ch s bay hi. 7.3.1 Cn dng c cha mu trc (4.6). Nu s dng mt ti TEDLAR, chuyn nhanh tt c cht lng t bnh ZHE vo trong ti, hoc tch ring cht lng v cht rn ban u hoc tch ring cht lng v cht rn cui cng, v ly mt c s t cht lng trong ti cho vic phn tch. Mt s dng c cha lit k trong phn 4.6 c ngh s dng di cc iu kin c trnh by trong phn 4.6.1 4.6.3.
(V 1)( C1) + (V 2)( C 2) V 1 +V 2

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7.3.2 t pittong ca ZHE trong bnh ZHE (u tin n c th gip ch lm m s nhng 0-rings ca pittong bng dung dch ngm chit). iu chnh pittong nm cao trong bnh ZHE s gim ti thiu khong cch m pittong phi di chuyn n bnh ZHE c in vo bi mu (ph thuc vo yu cu kch thc mu xc nh trong phn 7.3, 7.1.1 hoc 7.1.2). Bo m kh vo hoc ra mp bnh pha trn ph hp vi hng dn ca nh sn xut. m bo mng lc si thy tinh nm gia tm chn h tr v cnh bn. cht lng vo hoc ra ti mp trn ca cnh bn. 7.3.3 Nu cht thi l 100% cht rn (xem 7.1.1), cn 1 mu cht thi ph (ti a 25 g), v thc hin nh phn 7.3.5. 7.3.4 Nu cht thi cha < 0,5% cht rn kh (phn 7.1.2), phn lng ca cht thi sau khi lc c xc nh c im bng pp ngm chit TCLP. Lc mu lng cht lng c lc s h tr cho tt c cc phn tch v hp cht bay hi c yu cu. i vi ch61t thi cha 0,5% cht rn kh (xem 7.1.1 hoc 7.1.2) s dng thng tin phn trm chn rn thu c trong phn 7.1.1 xc nh th tch mu vi iu kin tt nht np vo bnh ZHE. Th tch mu c ngh nh sau: 7.3.4.1 i vi cht thi cha < 5% cht rn (xem phn 7.1.1), cn 500 g mu ph v khi li khi lng. 7.3.4.2 i vi cht thi 5% cht rn (xem phn 7.1.1), xc nh lng cht thi np vo bnh ZHE nh sau: Khi lng cht thi np vo ZHE = * 100

Cn mu cht thi ph vi th tch ph hp v ghi li khi lng. 7.3.5 Nu gim th tch mu ca phn cht rn trong cht thi c yu cu trong phn 7.1.3, th thc hin theo phn 7.3.6. Nu gim th tch mu khng c yu cu trong phn 7.1.3, th thc hin theo phn 7.3.7. 7.3.6 Chun b mu cho vic ngm chit bng qu trnh nn p, ct gt, hoc nghin nt phn cht rn ca cht thi c din tch b mt v kch thc phn t nh c trnh by trong phn 7.1.3. Cht thi v thit b nn p thch hp nn c lm lnh, nu c th, 4oC trc khi gim kch thc phn t. iu ny c ngha ca vic gim kch thc phn t khng c sinh ra nhit trong chnh bn thn ca chng. Nu gim lng cht rn trong cht thi l cn thit, th ta cht thi tip xc vi khng kh nn trnh ti mt mc nht nh c th. LU : Vic sng cht thi khng c ngh bi v kh nng cht bay hi s b tht thot. S dng thc o c chia vch ph thp c ngh nh mt phng php khc

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c7 th chp nhn c. Yu cu v din tch b mt c ngha cho cht thi c dng si (nh: giy, vi) v nhng loi cht thi tng t. Vic o c thc t din tch b mt khng c ngh. Khi din tch b mt hoc kch thc phn t c thay i mt cch ph hp, thc hin phn 7.3.7. 7.3.7 Cht thi bn than (xi mng) khng c cho php cht rn lng tnh. Khng ly tm cht thi trc khi lc. 7.3.8 Chuyn ton b lng mu (cht lng v cht rn) nhanh chng vo bnh ZHE. m bo b lc v tm chn h tr trn nh mp thit b v m bo nh mp thit b n than bnh ZHE ph hp vi hng dn ca nh sn xut. Sit cht cc b phn ca thit b v t thit b ti v tr thng ng (mp dng kh vo hoc ra ti y bnh). Khng c gn thit b ngm chit vi tm bc trn nh. LU : Nu thnh phn cht thi ( > 1% khi lng mu ban u) bm vo thng cha c s dng chuyn mu sang bnh ZHE, th xc nh khi lng ca phn d ra v tr khi lng ca n ra trong khi lng mu c xc nh trong phn 7.3.4 xc nh khi lng mu cht thi s c lc. Gn ng dn kh vo van dn kh vo hoc ra (mp y bnh) v, vi van cht lng ra hoc vo (mp nh ca bnh) m, bt u s dng p sut thp t 1-10 psi (hoc nhiu hn nu cn thit) y tt c khong trng ra ngoi bnh ZHE t t trong mt ci np y. Ti ln xut hin u tin ca cht lng t van x cht long vo/ra, nhanh chng ng van li v ngng tng p sut. Nu qu trnh lc cht thi ti 4oC gim lng cht lng c nn p trn nhng g c th nn nhit phng, th cho php lm m mu nhit phng trong thit b trc khi lc. Nu cht thi l 100% cht rn (xem 7.1.1), tng t t p sut n gi tr ti a l 50 psi y hu ht khong trng ra ngoi thit b v thc hin phn 7.3.12. 7.3.9 Gn thng cha mu lc c cn trc vi van x cht lng vo/ra v m van. Bt u s dng p sut thp t 1-10 psi y cht lng ca mu vo thng cha mu lc. Nu khng thm cht lng i qua mng lc trong khong thi gian 2 pht, th tng t t lng p sut l 10 psi n ti a 50 psi. Sau mi lng tng p sut l 10 psi, nu khng thm cht lng i qua mng lc trong khong thi gian 2 pht, th thc hin tip 10 psi. Khi dng cht lng dng li th tip tc lc p sut ti 50 psi khng c kt qu trong bt k qu trnh lc thm no trong khong thi gian 2 pht, ngng qu trnh lc. ng van cht long vo/ra, ngng tng p pittong, v ngng kt ni v cn thng cha mu lc.

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LU : Vic tng p sut qu nhanh s lm nt mng lc si thy tinh v c th l nguyn nhn ca vic bt kn qu nhanh. 7.3.10 Cht liu trong bnh ZHE c xc nh r c tnh bi v cht rn ca cht thi v dung dch lc c xc nh trong pha lng. LU : Mt vi cht lng, nh cht thi du v mt vi cht thi sn, cha mt vi cht xut hin l cht lng. Thm ch sau qu trnh lc p sut, cht ny s khng c lc. Nu trong trng hp ny, cht trong thit b lc c xc nh nh mt cht rn v c thc hin qua pp ngm chit TCLP l cht lng. Nu cht thi ban u cha < 0,5% cht rn kh (xem phn 7.1.2), th qu trnh lc c xc nh bng pp ngm chit TCLP v c phn tch trc tip. Thc hin theo phn 7.3.15. 7.3.11 Cht lng c phn tch nhanh chng (xem phn 7.3.13 n 7.3.15) hoc c tr ti 4oC vi khong trng nh nht cho n thi gian phan tch. Xc nh khi lng dung dch ngm chit 1N b vo bnh ZHE nh sau: Khi lng dung dch ngm chit = 7.3.12 Nhng phn sau y th hin chi tit lm th no thm vo lng dung dch ngm chit ph hp cht rn c trong bnh ZHE v lc mnh bnh ZHE. Cht lng ngm chit #1 c s dng trong tt c cc trng hp (xem phn 5.7). 7.3.12.1 Bnh ZHE vi v tr thng ng, gn ng t b cha dung dch ngm chit n van x cht lng vo/ra. ng ng c s dng s cha dung dch ngm chit mi v cho thng vo trc vi dung dch kim tra ti kh trong ng dn. Loi b p sut kh trong pittong bnh ZHE (t van x kh vo/ra), m van x cht lng vo/ra, v bt u chuyn dung dch ngm chit (bng bm) vo trong bnh ZHE. Tip tc bm dung dch ngm chit vo trong bnh ZHE cho n khi lng dung dch thch hp c a vo bnh. 7.3.12.2 Sau khi thm vo dung dch ngm chit, nhanh chng ng van x cht lng vo/ra v ngng kt ni vi ng dn dung dch ngm chit. Kim tra bnh ZHE m bo rng tt c cc van c ng v tr. Xoay bnh bng tay t u u n y bnh t 2 n 3 ln. t li vi tr thng ng ca bnh ZHE vi van x cht lng vo/ra trn nh bnh. Cho p sut vo bnh ZHE t 5-10 psi (nu cn thit) v m chm van x cht lng vo/ra thot khong trng (trong mt ci np) c hng dn bi v thm vo dung dch ngm chit. Vic thot khong trng s c thc hin nhanh v c ngng li khi c s

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xut hin u tin ca cht lng trong van. To p sut ln na trong bnh ZHE vi 5-10 psi v kim tra tt c cc pittong trong bnh ZHE m bo rng chng c ng. 7.3.12.3 t bnh ZHE trong thit b xoay (nu c) v xoay vi tc 30 2 rpm trong 18 2 gi. Nhit xung quanh (nh: nhit phng khi ngm chit) s c duy tri ti 23 2oC trong sut qu trnh xoay. 7.3.13 Trong khong thi gian 18 2 gi xoay, kim tra p sut trong pittong ZHE bng cch m v ng nhanh van x kh vo/ra v ch s thot kh. Nu p sut khng c duy tr (nh: khng quan st s thot kh), th thit b ang b h. Kim tra cc khe h ca bnh ZHE c trnh by trong phn 4.2.1, v thc hin ngm chit ln na vi mu cht thi mi. Nu p sut trong thit b c duy tr, cht trong bnh ngm chit c tch ln na trong dung dch thnh hai phn lng v rn. Nu cht thi cha cht lng ban u, cht lng c lc trc tip bng thng cha mu lc (nh: ti TEDLAR) gi lng cht lng ban u ca cht thi. Thng cha dung dch lc ring bit c s dng nu s kt hp to ra nhiu pha, hoc ko th tch trong thng cha dung dch lc. Lc qua mng lc si thy tinh, s dng bnh ZHE v c trnh by trong phn 7.3.9. Tt c dung dch ngm chit s c lc v thu li nu ti TEDLAR c s dng, nu dung dch ngm chit c nhiu pha, hoc nu cht thi cha cht lng ban u (xem phn 4.6 v 7.3.1). LU : Mng lc si thy tinh 1 chiu c s dng lc cht thi trong bnh ZHE nu n b nghi ng rng mng la si thy tinh b nt v. 7.3.14 Nu cht thi ban u khng cha pha lng, cht lng c lc thu c t phn 7.3.13 c xc nh bng pp TCLP. Nu cht thi cha cht lng ban u, cht lng c lc thu c t phn 7.3.13 v cht lng ban u (phn 7.3.9) c xc nh bng pp TCLP. 7.3.15 Theo pp ngm chit TCLP, chun b nhanh chng dung dch ngm chit cho vic phn tch v lu tr vi khong trng nh nht ti 4oC ho n khi c phn tch. Phn tch pp ngm chit TCLP tng t nh cc phng php phn tch khc. Nu pha ring l c phn tch ring l (nh: khng th trn ln vi nhau), xc nh th tch ca pha ring l (n 0,5%), kim sot pp phn tch thch hp, v kt hp kt qu mt cch chnh xc bng vic s dng trung bnh th tch mu c cn: Nng phn tch cui cng = Trong : V1: Th tnh pha ban u (L) C1: nng phn tch pha bna u (mg/L) V2: Th tch pha th 2 (L)

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C2: nng phn tch ca pha th 2 (mg/L) 7.3.16 So snh cc nng phn tch trong pp ngm chit TCLP vi cc mc c xc nh trong khong quy nh thch hp. Tham kho phn 8.0 trnh by cc yu cu m bo v cht lng. 8.0 QUALITY ASSURANCE m bo cht lng 8.1 S dng mu trng vi th tch ti thiu (s dng dung dch ngm chit tng t nh s dng cho cc mu) phi c phn tch cho 20 ln ngm chit bng bnh ngm chit. 8.2 Mt nhm mu chnh s c th hin cho mi loi cht thi ( bn hot tnh x l nc thi, t b nhim ) tr khi kt qu vt qu mc quy nh v d liu u c s dng chng minh rng cht thi vt qu mc quy nh. Mt dng thi chnh ti thiu phi c phn tch cho mi ln phn tch mu. i vi lng ti thiu, phi theo hng dn thm v matrix spike c cung cp trong mi phng php phn tch. 8.2.1 Cc nhm mu chnh c thm vo sau giai on lc ca phng php ngm chit TCLP v trc khi bo qun mu. Cc nhm mu chnh khng nn thm vo trc khi ngm chit mu theo phng php TCLP. 8.2.2 Trong hu ht cc trng hp, cc nhm mu chnh nn c thm vo ti mt nng tng ng vi mc quy nh tng ng. Nu nng phn tch thp hn mt na mc quy nh, nng bit c th thp bng mt na nng phn tch, nhng khng thp hn 5 ln gii hn pht hin ca phng php. trnh s khc nhau trong cc nh hng ca nhm mu, cc nhm mu chnh phi c thm vo th tch khng ng k ca phng php ngm chit TCLP m c phn tch cho nhng mu cha bit. 8.2.3 Mc ch ca nhm mu chnh l kim vic thc hin cc phng php phn tch, v xc nh cc cn tr thuc matrix c tn ti hay khng. S dng cc phng php internal calibration methods, sa i cc phng php phn tch, hoc s dng cc phng php phn tch thng thng c th cn o chnh xc nng phn tch trong phng php ngm chit TCLP khi hon lu nhm mu chnh sau khi thc hin phng php phn tch c la chn. 8.2.4 Hon lu li nhm mu chnh c tnh ton bng cng thc sau: %R (% Hon lu) = 100.(Xs Xu)/K

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Trong : Xs = gi tr o ca mu bit; Xu = gi tr o ca mu cha bit; K = gi tr bit ca spike trong mu. 8.3 Tt c vic o lng kim sot cht lng m t trong cc phng php phn tch thch hp. 8.4 S dng phng php internal calibration quantitation methods c thc hin cho cht thi nhim kim loi nu: (1) thu hi cht nhim t pp ngm chit TCLP khng thp hn 50% v nng khng vt qu mc quy nh, v (2) nng ca cht nhim c o trong dung dch ngm chit bng 20% mc quy nh thch hp. 8.4.1 Phng php s dng dung dch chun nn thc hin nh phng php internal calibration quantitation methods cho tng loi cht thi nhim kim loi. 8.4.2 Phng php s dng dung dch chun yu cu chun b chun calibration trong mu chnh thay v cht phn ng hoc dung dch trng. N yu cu ly 4 c s ng nht ca dung dch v thm vo cc lng dung dch chun bit cho 3 c s. c s th 4 cha bit. Hn th na, phn thm vo u tin nn c chun b kt qu nng xp x 50% nng yu cu ca mu. Phn thm vo th 2 v th 3 nn chun b kt qu nng xp x 100% v 150% nng yu cu ca mu. Tt c 4 c s c duy tr ti th tch mu cui cng tng t nhau bng vic thm cht phn ng hoc dung dch trng, v cn iu chnh vic pha long duy tr du hiu trong dy tuyn tnh ca thit b k thut. Tt c 4 c s c phn tch. 8.4.3 Chun b mt k hoch hoc d liu c lin quan n s st gim tuyn tnh ca cc du hiu v thit b k thut hoc nng external-calibration-derived concentration l nng i lp (trc y) bin thin l thuc phn dung dch chun thm vo l nng bin thin khng ph thuc (trc x). gii hn s cn tr ca honh (nng bin thin khng ph thuc, trc x) l nng cha bit. 8.4.4 Bn cnh , tr i cc du hiu ca thit b k thut hoc nng externalcalibration-derived concentration ca mu cha bit (unspike) t cc du hiu ca thit b k thut hoc nng external-calibration-derived concentration ca phn dung dch chun thm vo. K hoch hoc d liu lin quan n s st gim tuyn tnh ca cc du hiu chnh xc ca thit b k thut hoc nng external-calibration-derived concentration l nng bin thin ph thuc i lp vi nng bin thin khng ph thuc. t c nng cha bit phi s dng ng biu din internal calibration curve nh th n l ng biu din external calibration curve. 8.5 Cc mu phi c thc hin pp ngm chit TCLP trong khong thi gian nh sau:

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Cht bay hi Cht bn bay 14 hi Thy ngn 28 Kim loi (ngoi tr 180 Thy ngn) NA = Khng p dng

THI GIAN Gi MU TI A (NGY) T: Ngm chit T: Chun b ngm T: Ly mu TCLP chit n: Ngm n: Chun b n: PP phn tch chit TCLP ngm chit c xc nh 14 NA 14 7 NA NA 40 28 180

Tng thi gian 28 61 56 360

Nu thi gian gi mu b vt qu, gi tr thu c s c xem nh nng thp. Vt qu thi gian gi mu khng th chp nhn chng t rng cht thi khng c vt qu mc cho php. Vt qu thi gian gi mu s khng lm v hiu c tnh nu cht thi vt mc cho php. 9.0 HIU QU CA PHNG PHP 9.1 Cn tr: 2 nghin cu cc cn tr c thc hin xc nh nh hng ca cc s chnh lch khc nhau trn cc yu t c bit trong quy nh ca pp TCLP. Vic kim tra cc cn tr xc nh nhy ca s bin thin nh thng gp c mong i xy ra trong qu trnh thc hin cc phn tch trong PTN. 9.1.1 Kim loi Cc iu kin di y c s dng khi ngm chit cht thi phn tch kim loi: iu kin khc nhau T l lng/rn 19:1 hoc 21:1 Thi gian ngm chit 16 gi hoc 18 gi Khong khng 20 % hoc 60 % Dung dch m axit 190 meq hoc 210 meq 2N B lc ra axit C hoc Khng Mng lc 0,7 m hoc 0,45 m hoc Kiu lc polycarbonat Kiu bnh/chai Borosilicate hoc Flint glass S bin thin ca 7 phng php c th nghim, axit ca dung dch ngm chit c tc ng ln nht n cc kt qu. 4 trong 13 kim loi trong pp APT tc bn t hn hp cht thi xi m (APT/EW) v 2 trong 3 kim loi t cht thi lng cha vi ammonia c ngm chit vi nng cao bng vic s dng nhiu dung dch m axit. Do nhy ca s

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thay i pH, phng php yu cu rng dung dch ngm chit c chun b gi tr pH cui cng nm trong khong l thuyt l 0,05. 9.1.2 Cc Hp Cht Hu C Bay hi Cc iu kin di y c thc hin khi phn tch VOC cho cht thi: iu kin khc nhau T l lng/rn 19:1 hoc 21:1 Khong khng 0 % hoc 5 % Dung dch m axit 1N 60 meq hoc 80 meq Phng php ngm chit Syringe hoc Tedlar bag c s C hoc Khng p sut sau piston 0 psi hoc 20 psi Khng mt thng s no c tc ng quan trng n kt qu ca cc kim tra s cn tr. 9.2 TNH CHNH XC Nhiu nghin cu v tnh chnh xc ca pp TCLP c thc hin v th hin tng qut rng tnh chnh xc ca pp TCLP c th so snh c hoc vt qu tnh chnh xc ca pp kim tra c tnh EP v tnh chnh xc ca pp ny l ph hp. Mt trong nhiu s ng gp quan trng n s xut hin ca tnh khng chnh xc l c m t tnh ng nht ca mu v s khc nhau trong cc phn tch trong PTN (do c tnh ca mu cht thi). 9.2.1 Kim loi Kt qu nghin cu nhiu th nghim c trnh by trong bng 6 v ch ra rng mt phn tch n l khng ph hp vi yu cu v s nhn bit v c tnh ca cht thi. 9.2.2 Hp cht hu c bay hi mt phn cc kt qu ca 2 nghin cu c trnh by trong bng 7 v 8. Tnh chnh xc ca phn tch n l ti u vi hn 90% kt qu trong RSD thp hn 25%. Trn 85% tt c cc hp cht n l trong nghin cu nhiu th nghim gim xung trong khong t 20 120%. C hai nghin cu kt lun rng pp TCLP cung cp tnh chnh xc ph hp. N cng xc nh rng nng acetat cao trong dung dch ngm chit khng xut hin cc vn (s st gim ct trong pp sc k kh) cho cc iu kin phn tnh c s dng. 9.2.3 Hp cht hu c bay hi hon ton 11 th nghim c thc hin trong mt nghin cu kt hp ca vic s dng ZHE vi 2 loi cht thi m c b sung thm hn hp VOCs. Kt qu ca nghin cu kt hp c trnh by trong bng 9. Kt qu v tnh chnh xc ca VOCs c hng xy ra ngoi khong c xem xt. Tuy nhin, khong gi tr ca RSD c so snh gn ging vi nhiu kt qu phn tch kim loi trong bng 6. Blackburn v Show kt lun rng ti mc 95% c ngha quan trng: (1) khi phc li cc phn tch tng t bng thng k, (2) vic

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khi phc khng thay i nhiu gia 2 loi cht thi, (3) mi ln phn tch th hin m hnh tng t cua vic khi phc tng mu trong 2 mu.

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