Phương pháp 6 xác định SO2 ống khói( BẢNG DỊCH)

7/28/2019 Phng php 6 xc nh SO2 ng khi( BNG DCH)

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Phng php 6 - Xc nh pht thi sulfurdioxide t ngun tnh

Ch :Phng php ny khng bao gm tt c cc chi tit k thut (v d, thit b, vt

t) v cc th tc (v d nh, ly mu v phn tch) cn thit hiu qu ca n.Mt s vt liu c kt hp bng cch tham chiut cc phng php khc trong phn ny. V vy, c c kt qu ng tincy, ngi s dng phng php ny cn phi c mt kin thc ton din cacc phng php kim tra b sung sau y: Phng php 1, phng php 2,phng php 3, phng php 5, v png php 8.

1.0 Phm vi v ng dng.

1,1 cht phn tch.

Analyte CAS No. Sensitivity( nh y)

SO2 7449-09-5 3.4 mg SO2/m3

(2.12 x 10-7 lb/ft3)

1,2 p dng. Phng php ny p dng i vi cc php o lng kh thi sulfurdioxide (SO2) t cc ngun tnh.

1,3 Mc tiu cht lng d liu. Vic tun th cc yu cu ca phng phpny s nng cao cht lng ca cc d liu thu c t phng php ly mucht gy nhim khng kh.

2.0 Tm tt Phng php.

2.1 Mt mu kh c tch ra t im ly mu trong ngn xp. Cc SO2 vtrixt lu hunh, bao gm c nhng phn s trong bt k sng m axit luhunh, c tch ra. Cc phn SO2 c o bng phng php chun bari-Thorin.

3,0 Cc nh ngha. [Thuc v]

4,0 nhiu.

4.1 min Amoniac. t do amoniac can thip vi phng php ny bng cchphn ng vi SO2 to thnh ht sulfite v phn ng vi ch th. Nu ammoniat do(iu ny c th c xc nh bi kin thc v qu trnh v / hoc nhn thyvn ht trng trong thm d v isopropanol bt xa bng ), phng php thayth, ty thuc vo s chp thun ca qun tr l bt buc. Mt gii php thay th c ph duyt c lit k trong Ti liu tham kho 13 ca Mc 17,0.4,2 Nc-cation ha tan v mui fluor. Cc cation v mui fluor c loi b bi


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mt b lc si len thu tinh v mt bt xa bng isopropanol, do , h khng nhhng n phn tch SO2. Khi mu c thu thp t mt dng kh vi nng cao ca kh kim loi (v d, bnh xt cation rt tt), mt b lc si thy tinh caohiu qu phi c s dng ti ch ca cc plug si len thu tinh (tc l, mttrong thm d) loi b s nhiu cation.

5.0 Safety.

5,1 T chi. Phng php ny c th lin quan n vt liu nguy him, hotng, v thit b. Phng php th nghim ny khng th gii quyt tt c ccvn an ton lin quan vi vic s dng ca n.y l trch nhim ca ngis dng thit lp an ton thch hp v thc hnh sc khe t v xc nh khnng p dng ca php l hn ch trc khi thc hin phng php ny thnghim.

5,2 thuc th n mn. Cc thuc th sau y l nguy him. Trang thit b bo hc nhn v cc th tc an ton rt hu ch trong vic ngn chn bn ha cht.Nu lin h xy ra, ngay lp tc ra bng s lng nhiu nc trong t nht 15pht. Ci b qun o c tm v lm sch. iu tr bng ha hc cn li lbng nhit.

5.2.1 Hydrogen Peroxide (H2O2). D ng cho mt, da, mi v phi. 30% H2O2 lmt tc nhn oxy ha rt mnh.Trnh tip xc vi da, mt, v cc vt liu dchy. Mang gng tay khi x l.

5.2.2 Sodium Hydroxide (NaOH). Gy thit hi nghim trng cho mt v da. Htphi gy kch ng mi, hng v phi.Phn ng to nhit vi mt lng gii hnca nc.

5.2.3 axit sulfuric (H2SO4). Nhanh chng ph hy m c th. S gy ra bng th ba.Eye thit hi c th dn n m la. Qua ng h hp c th gy tvong co tht. Qua ng h hp c th gy t vong do co tht thanh qun,thng l trong vng 30 pht.C th gy tn thng m phi vi ph.1 mg/m3trong 8 gi ng h s gy ra thit hi phi, hoc nng cao hn, cicht.Cung cp thng hi hn ch ht phi.Phn ng d di vi cc kim loiv hu c.

6,0 Thit b v Vt t.6,1 Thu Thp mu.Cc hng mc sau y c yu cu cho thu thp mu:

6.1.1 Ly mu Train.Mt s mch ca o to ly mu c th hin trongHnh 6-1.Thit b ly mu c m t trong Phng php 8 c th c thay th v tr cathit b ln impinger Phng php 6. Tuy nhin, o to Phng php 8 phic sa i bao gm mt b lc lm nng gia u d d v isopropanolimpinger, v hot ng ca on tu ly mu v phn tch mu phi c mc lulng v khi lng dung dch php quy nh trong Phng php 8. Ngoi ra,SO2 c th c xc nh ng thi vi cc ht vt cht v xc nh m


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bng cch hoc l (1) thay th nc trong h thng Phng php mt 5impinger vi mt gii php H2O2 3%, hoc (2) thay th h thng impingerPhng php 5 nc vi mt phng php isopropanol 8 b lc h thngH2O2. Vic phn tch i vi SO2 phi ph hp vi cc th tc Phng phpo to ly mu 8.TheMethod 6 bao gm cc thnh phn sau:

6.1.1.1 u d.Borosilicate thy tinh hoc thp khng g (cc vt liu khc xydng c th c s dng, ty thuc vo s chp thun ca qun tr vin),khong dy 6 mm (0,25 in.) Bn trong c ng knh, vi mt h thng si m ngn chn s ngng t nc v mt b lc (hoc-stackhoc un nng-ofstack) loi b cc ht vt cht, bao gm c sng m axit sulfuric. Mt plug si lenthu tinh l mt b lc tha ng.

6.1.1.2 bt xa bng v Impingers. Mt ln bt xa bng vi nguyn liu nu thy tinh trung th v borosilicate hoc thch anhlen thy tinh ng gi trong u (xem Hnh 6-1) ngn chn

acid sulfuric sng m mang sang, v ba hinh rt nh 30-mlimpingers. Bt xa bng kh rt nh v ln impingers phikt ni trong lot vi cc u ni thy tinh r r.M Silicone c th c s dng, nu cn thit, ngn chnr r. Impinger kh rt nh c th c s dng v tr cakh rt nh bt xa bng .

Ch : b gim thu gom v tc dng chy c thc s dng, ty thuc vo s chp thun ca qun tr, nhnghiu qu thu gom phi c th hin c t nht 99phn trm cho mi bi kim tra chy v phi c ghi chp trong

bo co. Nu hiu qu c tm thy c th chp nhn c sau khi mthng lot ba bi kim tra, ti liu khng phi lyu cu. tin hnh th nghim hiu qu, hp th thmphi c thm vo v phn tch mt cch ring bit. iu ny hp th thmkhng c c hn 1% ca tng s SO2.

6.1.1.3 len thy tinh. Borosilicate hoc thch anh.6.1.1.4 voi khoa nc Grease. Acetone-khng ha tan, heatstablem silicone c th c s dng, nu cn thit.6.1.1.5 Nhit cm bin. quay nhit k, hoctng ng, o nhit ca kh li impinger

o to trong vng 1 EC (2 EF).

6.1.1.6 sy ng. ng ng gi sn gi vi 6 - 16 licho thy loi silica gel, hoc tng ng, kh khmu v bo v ng h v my bm. Nu silica gel c s dng, kh 177 EC (350 EF) trong 2 gi. Newsilica gel c th c s dng nh nhn c. Ngoi ra, khccc loi cht lm kh (tng ng hoc tt hn) c th c s dng,


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ty thuc vo s chp thun ca qun tr.6.1.1.7 Van. Kim van, iu ho kh mutc dng chy.

6.1.1.8 bm. Bm mng b r r, hoctng ng, ko kh thng qua o to. Ci t mt nhb iu p gia my bm v ng h tc ph nhnxung ng hiu ng ca my bm mng chn trn ng h tc

6.1.1.9 T l Meter. Rotameter, hoc tng ng,c kh nng o tc dng chy trong vng 2% cala chn tc dng chy khong 1 lt / pht (0,035 cfm).

6.1.1.10 Khi lng Meter. Kh kh mt (DGM), chnh xc o lng khi lng mu trong2%, hiu chnh tc dng chy chn viu kin thc t gp phi trong qu trnh ly mu, v

c trang b mt cm bin nhit (nhit k quay s, hoctng ng) c kh nng o nhit chnh xctrong vng 3 EC (5,4 EF). Mt l quan trng c th c s dng trongni DGM quy nh trong phn ny vi iu kinc chn, nh c, v s dng theo quy nh ti Mc 16.

6.1.2 kh p k. Thy ngn, bng st , hoc khcp k c kh nng o p sut kh quyntrong vng 2,5 mm Hg (0,1. Hg). Xem Ch trong Phng php 5,Mc 6.1.2.6.1.3 My o chn khng v Rotameter. t nht 760-mm Hg

(30 trong Hg) nh gi v 0 - 40-ml/min rotameter, c s dng kim tra r r ca o to ly mu.

6,2 mu Thu hi. Cc hng mc sau y l cn thitcho mu phc hi:6.2.1 Chai Ra. Hai polyethylene hoc thy tinhchai 500 ml.6.2.2 Chai lu tr. Polyethylene chai 100 ml, lu tr impinger mu (mt cho mi mu).6,3 Phn tch mu. Cc thit b sau ycn thit cho phn tch mu:

6.3.1 Pipet. Th tch loi, 5 ml, 20 ml (mtcn thit cho mi mu), v kch c 25 ml.6.3.2 lng th tch bnh. Kch c 100 ml (mt cho mimu) v kch c 1000-ml.6.3.3 Burettes. Kch thc 5 - 50 ml.6.3.4 Erlenmeyer bnh. Kch c 250 ml (mt cho mimu, trng, v tiu chun).6.3.5 nh git Chai. Kch thc 125-ml, thm


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ch th.6.3.6 Tt nghip xi lanh. Kch thc 100-ml.6.3.7 quang ph. o hp th 352 nm.

7,0 Ho cht v tiu chun.Ch : Tr khi c ch nh khc, tt c cc thuc th phiph hp vi cc chi tit k thut c thnh lp ca U banCc thuc th phn tch ca Hip hi Ha hc M.Trong trng hp thng s k thut nh vy khng c sn, s dng sn phmtt nhtc sn lp.

7,1 Thu Thp mu. Vic cht phn ng sau ycn thit cho thu gom mu:7.1.1 nc. Kh Ion ha ct ph hp tiu chun ASTM

c im k thut D 1193-77 hoc 91 Loi 3 (kt hp bi

ti liu tham kho - 60,17). Cc th nghim i vi oxy ha KMnO4cht hu c c th c b qua khi nng cao cacht hu c khng c d kin s c mt.

7.1.2 isopropanol, 80 phn trm theo th tch. Trn 80 mlisopropanol vi 20 ml nc.7.1.2.1 Kim tra tng l ca isopropanol i vi peroxidecc tp cht nh sau: Lc 10 ml isopropanol 10ml dung dch mi chun b 10% dung dch ioua kali.Chun b mt trng bng cch tng t nh iu tr 10 ml nc. sau khi1 pht, c hp th 352 nm

quang ph s dng chiu di ng dn 1-cm. Nu hp thvt qu 0,1, t chi ung ru s dng.

7.1.2.2 peroxit c th c g b t isopropanolredistilling hoc bng cch thng qua thng qua mt ct kch hotnhm, tuy nhin, thuc th lp isopropanol vi ph hpcc mc peroxide thp c th c ly t ngun thng mi.T chi rt nhiu nhim c th, do , l mthiu qu th tc.

7.1.3 Hydrogen Peroxide (H2O2), 3 phn trm theo th tch.

Thm 10 ml dung dch 30% H2O2 90 ml nc. Chun bti hng ngy.7.1.4 Gii php Kali Iodide, 10 phn trm khi lng theoKhi lng (w / v). Ha tan 10,0 g KI trong nc, v pha long100 ml. Chun b khi cn thit.7,2 mu Thu hi. Vic cht phn ng sau ycn thit thu hi mu:


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7.2.1 nc. Tng t nh trong mc 7.1.1.required thu hi mu:

7.2.2 isopropanol, 80 phn trm theo th tch. Tng t nh trongMc 7.1.2.7,3 Phn tch mu. Vic thuc th sau y vtiu chun c yu cu cho phn tch mu:7.3.1 nc. Tng t nh trong mc 7.1.1.7.3.2 isopropanol, 100 phn trm.7.3.3 Ch s Thorin. 1 - (o-arsonophenylazo) -2 -naphtol-3,6-disulfonic acid, disodium mui, hoc tng ng.Ha tan 0,20 g trong 100 ml nc.

7.3.4 Tiu chun Gii php Bari, 0,0100 N. Ha tan1,95 g trihydrate perchlorate bari [Ba (ClO4) 2 3H2O]200 ml nc v pha long n 1 lt vi isopropanol.Ngoi ra, 1.22 g dihydrate bari clorua[BaCl2 2H2O] c th c s dng thay v perchlorate baritrihydrate. Chun ha nh mc 10,5.

7.3.5 Tiu chun axit sulfuric, 0,0100 Mua N.chun ha n 0,0002 N so vi 0,0100 N NaOH ctrc y c tiu chun ha i vi axit kaliphthalate (tiu chun cp tiu hc).7.3.6 m bo cht lng kim ton mu. khitun th cc quyt nh, cc mu kim ton, nu c phithu c t Vn phng khu vc thch hp EPA hoc tcc c quan thc thi trch nhim v phn tch trongkt hp vi cc mu lnh vc.

Lu : Vic c quan thc thi chu trch nhim nn cthng bo t nht 30 ngy trc ngy thi cho phpc thi gian giao hng mu.

8,0 Thu Thp mu, bo qun, lu tr thng vn ti.8.1 Chun b Train ly mu. o 15 ml80% isopropanol vo bt xa bng kh rt nh v 15 ca ml3% H2O2 vo nhau ca hai impingers kh rt nh u tin.

li impinger kh rt nh cui cng kh. Lp rp cc o to nhth hin trong Hnh 6-1. iu chnh my si thm d mt

nhit ngn chn s ngng t nc. ninghin nc v nc xung quanh impingers.

8,2 ly mu Train r r-Kim tra th tc. Mt leakchecktrc khi chy ly mu c ngh, nhng khngyu cu. Mt kim tra r r sau khi chy ly mu l bt buc.Th tc kim tra r r nh sau


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8.2.1 Tm thi nh km ph hp (v d, 0 - n 40 -ml / pht) rotameter vo cm ca DGM, v mt nichn khng nh gi ti hoc gn u vo u d. Cm u du vo, ko ra mt chn khng ca t nht 250 mm Hg (10. Hg), vlu tc dng chy nh c ch ra bi rotameter. Mt r r

t l vt qu 2% t l ly mu trung bnh lkhng th chp nhn.Ch : Cn thn (v d, t t) pht hnh thm dcm u vo trc khi tt my bm.

8.2.2 l ngh (khng bt buc) m my bmc r r kim tra mt cch ring bit, hoc l trc hoc sau khily mu chy. kim tra r r bm, tin hnh nh sau:Ngt kt ni cc ng lm kh t lp rp u d-impinger.

t mt thc o chn khng u vo hoc ng syhoc my bm, ko mt chn khng 250 mm Hg (10. Hg), cmpinch cc ca hng ca c o lu lng, v sau ttmy bm. Chn khng nn duy tr n nh cho t nht 30giy.Nu thc hin trc khi chy ly mu, leakcheck bmc u tin kim tra s r r ca on tu ly mum t ngay lp tc trn, nu thc hin sau khi ly muchy, my bm b r r kim tra c thc hin theo on tu ly mukim tra r r.

8.2.3 Cc th tc kim tra r r c th c s dng,ty thuc vo s chp thun ca qun tr.8,3 Thu Thp mu.

8.3.1 Ghi li c DGM ban u v kh pp lc. bt u ly mu, v tr nh ca vt oti im ly mu, kt ni u d bt xa bng , vbt u bm. iu chnh lu lng mu cho mt t l khng ikhong 1,0 lt / pht nh c ch ra bi t lmt. Duy tr t l ny khng i ( 10%) trongchy ly mu ton b

8.3.2 Hy c (DGM khi lng, nhit ti DGMv ti impinger cm, v tc ng h o tc dng chy) t nhtmi 5 pht. Thm nhiu hn trong thi gian chy gi

nhit ca kh ri khi impinger cui cng ti 20 EC(68 EF) hoc t hn.

8.3.3 Theo kt lun ca mi ln chy, tt Thebm, loi b cc u d t ngn xp, v ghi li trn chung ktc. Tin hnh mt r r-kim tra nh m t ti mc 8.2.(Kim tra r r ny l bt buc.) Nu r r c pht hin, void


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chy th hoc s dng cc th tc chp nhn c.Qun tr vin iu chnh m lng mu cho cc r r.

8.3.4 X bn tm nc , v thanh trng cn limt phn ca tu bng cch v khng kh trong sch mi trng xung quanhthng qua cch thng cho 15 pht t l ly mu. Lm sch mi trng xung quanhkhng kh c th c cung cp bng cch khng kh thng qua mt b lc thanhoc thng qua mt impinger kh rt nh thm c cha 15 ml dung dch 3% H2O2. Ngoi ra, khng kh xung quanh khngthanh lc c th c s dng.

8,4 mu Thu hi. Ngt kt ni cc impingers sau khipurging. Loi b cc ni dung ca bt xa bng kh rt nh . Rtcc ni dung ca ln impingers vo mt s r r min phpolyethylene chai cho l hng. Ra sch ln baimpingers v ng kt ni vi nc, v thm

ra sch cng mt bnh d tr. nh du mc cht lng.Con du v xc nh cc thng cha mu.

9.0 Quality Control.

Section Quality Control Measure Effect

7.1.2 Isopropanol check Ensure acceptable level

of peroxide impurities in

isopropanol

8.2, Sampling equipmen Ensure accurate

10.1-10.4 leak-check and measurement of stack gascalibration flow rate, sample volume

10.5 Barium standard Ensure precision( chnh xc) of

Solution normality determination

standardization

11.2.3 Replicate titrations Ensure precision of

titration determinations

11.3 Audit sample Evaluate analyst's

Analysis technique and standards

preparation

10,0 hiu chun v Tiu chun.10,1 Th tch H o .10.1.1 Hiu chun ban u.10.1.1.1 Trc khi s dng ban u ca n trong lnh vc, leakcheckh thng o (sy ng, kim van, bm,t l mt, v DGM) nh sau: t mt thc o chn khngu vo ng sy v ko mt chn khng 250 mm Hg


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(10. Hg). Cm hoc bm cm ca dng chyng h o, v sau tt my bm. Chn khng phi duy trn nh cho t nht 30 giy. Cn thn th ccmy o chn khng trc khi pht hnh vo cui lu lng k.

10.1.1.2 G b ng sy, v hiu chnhh thng o (tc dng chy ly mu theo quy nh ca phng php) nhsau: Kt ni mt cch thch hp kch thc t kim trang h o (v d, 1 lt cho mi vng) u vo cakim van. Lm cho ba chy hiu chnh c lp,s dng t nht nm vng ca DGM mi ln chy.Tnh ton hiu chnh yu t Y (ng h o t xt nghimhiu chun khi lng chia cho khi lng DGM, c khi lngiu chnh nhit tham kho v p sut) chomi ln chy, v trung bnh cc kt qu ( Yi). Nu bt k gi tr Ylch bi hn 2% so vi ( Yi), o

h thng l khng th chp nhn c s dng. Nu h thng o lngchp nhn c, s dng ( Yi) l nhn t hiu chunsau th nghim chy.

10.1.2 Sau th nghim Hiu chun Kim tra. Sau khi tng lnh vchng lot th nghim, tin hnh kim tra hiu chun bng cch s dngth tc nu ti mc 10.1.1.2, ngoi tr bahoc nhng cuc cch mng ca DGM c th c s dng, v ch c haichy c lp cn c thc hin. Nu trung bnh ca haith nghim hiu chnh cc yu t sau khng i chch hn5% t Yi, sau Yi c chp nhn nh DGMyu t hiu chun (Y), c s dng trong phng trnh 6-1 tnh ton khi lng mu c thu thp (xem Phn 12,2). Nu lch l hn 5%, xc nh lio h thng nh trong mc 10.1.1, v xc nh mt posttesthiu chnh yu t ( YF). So snh Yi v YF , nh hnca hai yu t c chp nhn nh l vic chun DGM597yu t. Nu hiu chun li ch ra rng h thng o lngl khng th chp nhn c s dng, hoc lm mt hiu lc chy thnghim hoc s dngphng php, ty thuc vo s chp thun ca qun tr,xc nh mt gi tr chp nhn c i vi cc mu thu thp cm lng

10.1.3 DGM nh l mt tiu chun hiu chun. Mt DGM c th cc s dng nh mt tiu chun hiu chun cho cc php o khi lng trongni ca ng h t kim tra quy nh ti mc 10.1.1.2,rng l hiu chun ban u v recalibratednh k theo cc th tc nu trong


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Phng php 5, mc 10.3 vi cc trng hp ngoi l sau y: (a)DGM l hiu chnh i vi mt ng h o t xt nghim c mtcng sut 1 lt / rev (0,035 ft3/rev) hoc 3 lt / rev (0,1ft3/rev) v c kh nng o lng khi lngtrong vng 1%, (b) DGM c hiu chnh mc 1 lt / pht

(0,035 cfm) v (c) hp ng h o ca 6 Phng php ly muo to c hiu chnh cng mt tc dng chy.

10,2 Cm bin nhit . Hiu chnh chng li mercuryinthy tinh nhit k.10,3 T l o. ng h o tc khng cn phi chiu chun, nhng cn c lm sch v duy tr theohng dn ca nh sn xut.10,4 p k. Hiu chnh i vi mt hm lng thy ngnp k.

10,5Gii php chun Bari. Chun haBari perchlorate hoc gii php clorua so vi 25 mltiu chun acid sulfuric 100 ml 100%isopropanol c thm vo. Khi trng lp phn tch.Tnh bnh thng bng cch s dng trung bnh ca nhn bnphn tch cc chun ng trong vng 1% hoc 0,2ml, ty theo iu kin no l ln hn.

11,0 Th tc phn tch.11.1 Mu Mt Kim tra. Lu mc cht lng trongcontainer v xc nhn xem mu no b mt trong qu trnhl hng; lu pht hin ny trn bng d liu phn tch.Nu mt s lng ng ch ca r r xy ra, hoc v hiumu hoc s dng cc phng php, ty thuc vo s chp thun caQun tr vin, chnh xc kt qu cui cng.11,2 Phn tch mu.

11.2.1 Chuyn giao cc ni dung ca cc container lu trbnh nh mc 100 ml, pha long n chnh xc 100 mlnc, v pha trn cc mu pha long.11.2.2 Pipet mt s chia ht mt s 20 ml dung dch mu pha longvo mt bnh Erlenmeyer 250-ml v thm 80 ml 100%isopropanol cng vi 2-4 git Thorin ch s.Trong khi khuy ng cc gii php, chun mt im cui mu hngbng cch s dng gii php 0,0100 N Bari tiu chun.

11.2.3 Lp li cc th tc trong mc 11.2.2, vtrung bnh khi lng chun . Chy mt khong trng vi mi lot cc mu.


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Chun ti to phi ng trong vng 1% hoc 0,2 ml, ty theo iu kin no l ln hn.

Ch : Bo v 0,0100 N gii php tiu chun barit bc hi tt c cc ln.

11,3 Kim ton mu phn tch.11.3.1 Khi phng php ny l s dng phn tch muchng minh s ph hp vi quy nh ngun pht thi, mtmu kim ton, nu c, phi c phn tch.11.3.2 ng thi phn tch mu kim ton v ccmu ph hp trong cng mt cch thc nh gik thut ca cc nh phn tch v chun b cc tiu chun.11.3.3 Cc cng mt nh phn tch, thuc th phn tch, vh thng phn tch phi c s dng cho cc mu tun thv cc mu kim ton. Nu iu kin ny c p ng, trng lpkim ton ca cc phn tch ph hp tip theo cho cng mt

c quan thi hnh trong mt khong thi gian 30 ngy c min. mtkim ton thit lp mu c th khng c s dng xc nhn cc b khcnhaucc mu ph hp thuc thm quyn ca ringc quan thi hnh, tr khi sp xp trc khi c cthc hin vi c hai c quan thc thi.

11,4 Kt qu mu kim ton.11.4.1 Tnh ton nng mu kim ton vgi kt qu bng cch s dng cc hng dn c cung cp vikim ton mu.

11.4.2 Bo co kt qu ca cc mu kim ton vvic xc nh tun th cc mu cng vi hm s, v tn ca nh phn tch.thm quyn chu trch nhim thi hnh. Bao gm thng tin nyvi cc bo co ca bt k phn tch ph hp tip theo chocng thc thi thm quyn trong thi gian 30 ngy.11.4.3 Cc nng ca cc mu kim tonthu c t nh phn tch phi ng trong vng 5%thc t tp trung. Nu 5% c im k thut khng phi lc p ng, reanalyze tun th v kim ton mu, v bao gmgi tr ban u v ti phn tch trong bo co th nghim.

11.4.4 Khng p ng cc c im k thut 5%c th yu cu thi li cho n khi cc vn kim ton c gii quyt.Tuy nhin, nu kt qu kim ton khng nh hng n vic tun thhoc tnh trng khng tun th ca c s b nh hng,Qun tr vin c th b yu cu ti phn tch, tip tckim ton, hoc thi li v chp nhn kt qu vic thc hin


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th nghim. Trong khi cc bc ang c thc hin gii quyt phn tchkim tonvn , ngi qun tr cng c th chn s dng d liu xc nh tnh trng tun th hoc khng tun th.nh hng n c s

12,0 Phn tch d liu v tnh ton.Thc hin tnh ton, gi li t nht mt trong nhng phcon s c ngha vt ra ngoi cc d liu thu c. vngtt s liu sau khi tnh ton cui cng.

12,1 Danh mc.CA = thc t nng SO2 trong mu kim ton,mg / dscm.Cd = Xc nh nng SO2 trong kim tonmu, mg / dscm.

CSO2 = Nng SO2, kh c s, sa chatiu chun iu kin, mg / dscm (lb / dscf).N = Bnh thng ca cht th chun Bari tiu chun, meq / ml.Pbar = Barometric p lc, mm Hg (. Hg).Pstd = chun tuyt i p lc, 760 mm Hg (29,92. Hg).RE = li tng i ca phn tch mu kim ton bo m cht lng,%Tm = DGM trung bnh nhit tuyt i, EK (ER).Tstd = chun tuyt i nhit , 293 EK(528 ER).Va = Khi lng s chia ht mt s mu chun , ml.Vm = khi lng kh kh c o bi DGM,DCM (DCF).Vm (tiu chun) = khi lng kh kh c o bi DGM, sa chavi iu kin tiu chun, dscm (dscf).Vsoln = Tng khi lng ca gii php, trong SO2mu c cha, 100 ml.Vt = Th tch ca cht th chun tiu chun bari c s dng chomu (trung bnh ca chun ti to), mlVTB = Th tch ca cht th chun tiu chun bari c s dng chotrng, ml.Y = DGM hiu chnh yu t.

12,2 Th tch mu kh kh, hiu chnh chuniu kin ny.

Cng thc trang 602 epa6


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13,0 Phng php Performance.13,1 Phm vi. Gii hn pht hin ti thiu caphng php c xc nh l 3,4 mg SO2/m3 (2,12 x 10-7lb/ft3). Mc d khng c gii hn trn c thnh lp,th nghim ch ra rng nng cao 80.000 mg/m3

(0.005 lb/ft3) ca SO2 c th c thu thp mt cch hiu qu vi tc 1,0 lt / pht (0,035 cfm) trong 20 pht trong hai kh rt nhimpingers, c cha 15 ml dung dch 3% H2O2. datrn cc tnh ton l thuyt, gii hn nng trnmu trong 20 lt (0,7 ft3) l khong 93.300 mg/m3(0,00583 lb/ft3).

14,0 Phng chng nhim. [Thuc v]15,0 Qun l cht thi. [Thuc v]16,0 Th tc thay th.16,1 Danh mc. Tng t nh mc 12.1, vi

sau khi b sung:BWA = Hi nc trong khng kh xung quanh, t l bim lng.Ma = Trng lng phn t ca khng kh xung quanh bo haimpinger nhit , g / g-nt rui(lb / lb-nt rui).Ms = Trng lng phn t ca kh mu bo haimpinger nhit , g / g-nt rui(lb / lb-nt rui).Pc = Inlet chn khng c c tronghiu chun chy, mm Hg (. Hg).Psr = Inlet chn khng c c trongly mu chy, mm Hg (. Hg).Qstd = th tch lu lng thng qua l quan trng,SCM / pht (SCF / pht).

_Qstd = Lu lng trung bnh t l kim tra trc v sau kim trachy hiu chun, SCM / pht (SCF / pht).Tamb = xung quanh nhit tuyt i ca khng kh, EK (ER).VSB = Th tch ca kh c o bng bong bng x phngng h o, m3 (ft3).VSB (tiu chun) = Th tch ca kh c o bng bong bng x phngng h o, sa cha vi iu kin tiu chun,SCM (SCF).2 = x phng bong bng du hnh thi gian, min.2 = Thi gian, min.16,2 l quan trng cho Th tch lng v li sutCc php o. Mt l quan trng c th c s dng thay choDGM quy nh ti mc 6.1.1.10, vi iu kin l n l


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la chn, nh c, v s dng nh sau:16.2.1 Chun b ca tu ly mu. Lp rp cco to ly mu c th hin trong hnh 6-2. Cc ng h o tc vb iu p l khng bt buc nhng c khuyn co pht hin nhng thay i trong tc dng chy.

Ch : Cc l quan trng c th c thch nghi vi mtPhng php o to ly mu 6 loi nh sau: Insert loi tay o,nt chai l huyt thanh vo hai cng on gim. akim vo nt chai c hin th trong hnh 6-3.16.2.2 La chn cc l quan trng.16.2.2.1 Cc th tc sau y m t vic s dngkim tim di da v tubings kim thp khng g, c tm thy ph hp s dng nh l quan trng.Cc nguyn vt liu v thit k khc l quan trng c th c s dngcung cp cc hnh ng l l l tht s quan trng, (tc l,

mt chn khng quan trng c th thu c) nh m t trongphn. Chn mt l quan trng c kch thc hot ngtc dng chy mong mun. Kch thc v ng kim di th hin trong Bng 6-1 cho gn ng sau ydng chy t l.16.2.2.2 Xc nh s ph hp vchn khng thch hp hot ng ca l quan trng nhsau: Nu c th, tm thi nh km mt ng h o tc vb iu p u ra ca o to ly mu, nu nithit b khng c mt (xem Phn 16.2.1). Btmy bm v iu chnh cc van cung cp cho mt cm chn khng ctng ng vi khong mt na p sut kh quyn.Quan st cc ng h o tc c. Dn dn tng cc chn khngcho n khi mt c n nh l thu c trn ng h tc .Ghi li chn khng quan trng, l chn khng cm khicc ng h o tc u tin t n mt gi tr n nh. l khng t c mt gi tr quan trng khng phi c s dng.

16.2.3 Th tc trng.16.2.3.1 r r-Kim tra th tc. R r kim tra trc khichy ly mu c ngh, nhng khng cn thit. ccr r kim tra th tc nh sau: Tm thi nh km mtph hp (v d, 00-40 ml / pht) rotameter v b tng, hoc mtng h o bong bng x phng v xe tng tng vo cm ca my bm.Cm u vo thm d, ko mt chn ra ca t nht 250mm Hg (10. Hg), v lu tc dng chy nh c ch ra birotameter hoc ng h o bong bng. Mt t l r r vt qu2% t l ly mu trung bnh (Q tiu chun) l khngchp nhn c. Cn thn th d tm trc khi cm u vott my bm.


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16.2.3.2 Xc nh m. Ti ly muv tr, trc khi th nghim, xc nh m%ca khng kh mi trng xung quanh bng cch s dng nhit bu t vkhhoc, nu thch hp, mt ng h o m tng i.

16.2.3.3 quan trng l chai Calibration. tiv tr ly mu, trc khi th nghim, hiu chnh ton bly mu o to (tc l, xc nh tc dng chy caly mu tu khi hot ng iu kin quan trng).

nh km mt ng h o 500 ml bong bng x phng u vo ca thm d,v hot ng o to ly mu ti mt chn khng ra ca 25 50 mm Hg (1-2.Hg) trn chn khng quan trng. ghicc thng tin c lit k trong hnh 6-4. Tnh tontiu chun khi lng khng kh c o bng ng h bong bng x phng vt l lu lng th tch bng cch s dng cc phng trnh di y:

Vsb(std) = Vsb (Tstd/Tamb)(Pbar/Pstd) Eq. 6-4

Qstd = Vsb(std) Eq. 6-5

16.2.3.4 ly mu.16.2.3.4.1 Hot ng o to ly mu muthu chn khng c s dng trong qu trnh hiu chunchy. Bt u xem v my bm cng mt lc. Hyc (nhit , ng h tc , chn khng u vo v u rachn khng) t nht mi 5 pht. Vo cui ca

ly mu chy, dng li xem v my bm cng mt lc

16.2.3.4.2 Thc hin mt hot ng hiu chun sau khi th nghim bng cchs dngcc th tc hiu chun c nu trong mc 16.2.3.3. NuQstd thu c trc v sau khi th nghim khc nhau bi nhiuhn 5%, lm mt hiu lc chy th nghim, nu khng, tnh tonkhi lng ca kh c o vi l quan trng bng cch s dngphng trnh6-6 nh sau:

Vm(std) = Qstd .s (1 - Bwa) (Pbar+ Psr)/(Pbar+ Pc) Eq. 6-6

16.2.3.4.3 Nu% s khc bit giatrng lng phn t ca khng kh xung quanh iu kin bo hav kh mu l 3%, sau cctrng lng phn t ca mu kh phi c xem xt trongtnh ton bng cch s dng phng trnh sau y:


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(std)= Qstd .s (1 - Bwa) (Pbar+ Psr).(Ma/Ms)1/(Pbar+ Pc) Eq. 6-7

Ch : kim tra r r sau khi xt nghim khng cn thit vCc bi kim tra kt qu hiu chun chy s cho bit liuc r r bt k.

16.2.3.4.4 X bn tm nc , v ty ly muo to s dng cc th tc c m t ti mc 8.3.4.16,3 xo b nhiu Amoniac. cctheo th tc thay th phi c s dng b sungnhng quy nh c th trong phng php ly mu ti ngunc lng kh thi ammonia.

16.3.1 Ly mu. Thm d phi c duy tr 275EC (527EF) v c trang b vi mt hiu qu cao-trong-stackb lc (si thy tinh) loi b cc ht vt cht. ccvt liu lc c khng phn ng SO2. ng ta la ai 934AH(trc y l Reeve Thin thn 934AH) cc b lc x l nh m t trongTham kho 10 ti Mc 17,0 Phng php 5 l mt v d v mtb lc c chng minh lm vic. Trng hp c tnh kimht vt cht v m ngng t c mt trong dng kh, b lc c un nng trn mim sng nhng di y 225EC (437EF).

16.3.2 Thu hi mu. Khi phc cc mu theoMc 8.4 tr loi b cc ni dung cakh rt nh bt xa bng . Thm ni dung bt xa bng , bao gm crinsings ca bt xa bng vi nc, ring

polyethylene chai t phn cn li ca mu. Theokim tra iu kin bnh thng trixt lu hunh s khng chin din ng k, cc th nghim c th la chn xa cckh rt nh bt xa bng t o to ly mu. Nu mt xp xnng trixt lu hunh l mong mun, chuyn nhngcc ni dung ca cc bt xa bng kh rt nh ringpolyethylene chai.

16.3.3 Phn tch mu. Thc hin theo cc th tcMc 11.1 v 11.2, ngoi tr thm 0,5 ml dung dch HCl 0,1 Nbnh Erlenmeyer v trn trc khi thm ch s.

Cc th tc phn tch sau y c th c s dng cho mtxp x ca nng trixt lu hunh. Cc chnh xc nng tnh ton s ph thuc voammonia SO2 t l v mc ca hin ti oxy trongdng kh. Mt phn nh ca SO2 s c tnh ltrixt lu hunh nh amoniac SO2 t l v muLng oxy tng ln. Ni chung, khi t l ny l 1hoc t hn v lng oxy trong khong 5%,


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t hn 10% ca SO2 s c tnh l trixt lu hunh. Phn tch cc muperoxide v isopropanolphn ring bit. Phn tch phn peroxide nhm t trn. Trixt lu hunh c xc nh bis khc bit bng cch s dng chun tun t ca isopropanol

phn ca mu. Chuyn cc ni dung caisopropanol lu tr container bnh nh mc 100 ml,v pha long chnh xc 100 ml nc. Pipet mt ml 20s chia ht mt s ca gii php ny vo mt bnh Erlenmeyer 250 ml, thm 0,5 ml 0,1 N HCl, 80 ml ca 100% isopropanol, v2-4 git ch th Thorin. Chun vi mt mu hngthit b u cui s dng 0,0100 N Bari perchlorate. Lp li vtrung bnh khi lng chun ng trong vng 1% hoc 0,2 ml, ty theo iukin no l ln hn. S dng khi lng trong phng trnh6-2 xc nh nng trixt lu hunh. Tbnh cha phn cn li ca isopropanol

mu, xc nh cc phn ca SO2 c thu thp trongbt xa bng bi pipetting aliquots 20 ml vo 250 ml Erlenmeyer bnh. Thm 5 ml dung dch 3% H2O2, 100 ml 100%isopropanol, v 2-4 nh git ca Thorin ch s, vchun nh trc. T khi lng chun ny, trcht th chun khi lng xc nh cho trixt lu hunh, v thmkhi lng cht th chun xc nh cho phn peroxide. iu nykhi lng cui cng to nn Vt, cc khi lng bariperchlorate c s dng cho cc mu SO2.

17,0 Ti liu tham kho.

1. Pht thi kh quyn t axit sulfuricSn xut qu trnh. Hoa K DHEW, PHS, Phng Air nhim. Y t cng cng Dch v Xut bn s 999-AP-13.Cincinnati, OH. Nm 1965.2. Corbett, P.F. Xc nh ca SO2 v SO3 trongL kh. Tp ch ca Vin nhin liu. 24:237-243.Nm 1961.3. Matty, R.E., v E.K. Diehl. o thi-khSO2 v SO3. Power. 101:94-97. Thng 11 nm 1957.

4.Patton, W.F., v J.A. Thit b mi Brink, Jr.v k thut kh ha hc Quy trnh ly mu. J. AirHip hi Kim sot nhim. 13:162. Nm 1963.5. Rom, J.J. Bo tr, hiu chun, v hot ngThit b ly mu Ngun Isokinetic. Vn phng ca AirCc chng trnh, C quan Bo v Mi trng Hoa K. Nghin cuTriangle Park, NC. APTD-0576. Thng 3 nm 1972.6. Hamil, H.F., v D.E. Camann. hp tc nghin cuPhng php Xc nh pht thi Dioxide lu hunh


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Ngun Vn phng phm (hi t nhin liu ha thchMy pht in). C quan Bo v Mi trng Hoa K, nghin cuTriangle Park, NC. EPA-650/4-74-024. Thng 12 nm 1973.

7.Sch hng nm ca Tiu chun ASTM. Phn 31; nc,Kh quyn Phn tch. American Society cho th nghim vVt liu. Philadelphia, PA. Nm 1974. trang 40-42.

8.Knoll, J.E., v M. R. Midgett. p dng ccEPA Phng php 6 Nng Dioxide lu hunh cao. MC quan Bo v mi trng. Research Triangle Park,NC. EPA-600/4-76-038. Thng 7 nm 1976.9. Westlin, P. R., v R. T. Shigehara. Th tc

o c v s dng Mt Th tch kh khTiu chun hiu chun. nh gi Hi ngunBn tin. 3 (1) :17-30. Thng 2 nm 1978.10. Yu, K. K. nh gi ca Effect m kh

Hiu chun kh o. nh gi Hi ngunBn tin. 5 (1) :24-28. Thng 2 nm 1980.

11.Lodge, J.P., Jr, et al. Vic s dng ca tim di daKim nh l quan trng trong ly mu khng kh. J. AirHip hi Kim sot nhim. 16:197-200. Nm 1966.12. Shigehara, R.T., v C. B. Sorrell. S dngL quan trng nh Phng php 5 CalibrationStandards. ngunBn tin Hip hi nh gi. 10:4-15. Thng Tm nm 1985.13. Curtis, F., Phn tch Phng php 6 mu trongS c mt ca Amoniac. Bn tin Hip hi nh gi ngun.13 (1) :9-15 thng hai nm 1988.

18,0 bng, biu , s khi v d liu Xc Nhn.BNG 6-1. C LNG GI FLOW cho cc kch c KIM khc nhauTip theo trang 615 cua epa6

Phương pháp 6 xác định SO2 ống khói( BẢNG DỊCH)

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