Phng php 6 - Xc nh pht thi sulfur dioxide 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 chiu t cc phng php khc trong phn ny. V vy, c c kt qu ng tin cy, ngi s dng phng php ny cn phi c mt kin thc ton din ca cc 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 SO2 CAS No. 7449-09-5 Sensitivity( nhy)

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 sulfur dioxide (SO2) t cc ngun tnh. 1,3 Mc tiu cht lng d liu. Vic tun th cc yu cu ca phng php ny s nng cao cht lng ca cc d liu thu c t phng php ly mu cht 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 v trixt lu hunh, bao gm c nhng phn s trong bt k sng m axit lu hunh, c tch ra. Cc phn SO2 c o bng phng php chun bariThorin. 3,0 Cc nh ngha. [Thuc v] 4,0 nhiu. 4.1 min Amoniac. t do amoniac can thip vi phng php ny bng cch phn ng vi SO2 to thnh ht sulfite v phn ng vi ch th. Nu ammonia t do (iu ny c th c xc nh bi kin thc v qu trnh v / hoc nhn thy vn ht trng trong thm d v isopropanol bot xa bng), phng php thay th, 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

mt b lc si len thu tinh v mt bot xa bng isopropanol, do , h khng nh hng 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 cao hiu qu phi c s dng ti ch ca cc plug si len thu tinh (tc l, mt trong 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, hot ng, v thit b. Phng php th nghim ny khng th gii quyt tt c cc vn an ton lin quan vi vic s dng ca n.y l trch nhim ca ngi s dng thit lp an ton thch hp v thc hnh sc khe t v xc nh kh nng p dng ca php l hn ch trc khi thc hin phng php ny th nghim. 5,2 thuc th n mn. Cc thuc th sau y l nguy him. Trang thit b bo h c 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 15 pht. Ci b qun o c tm v lm sch. iu tr bng ha hc cn li l bng nhit. 5.2.1 Hydrogen Peroxide (H2O2). D ng cho mt, da, mi v phi. 30% H2O2 l mt tc nhn oxy ha rt mnh.Trnh tip xc vi da, mt, v cc vt liu d chy. Mang gng tay khi x l. 5.2.2 Sodium Hydroxide (NaOH). Gy thit hi nghim trng cho mt v da. Ht phi gy kch ng mi, hng v phi.Phn ng to nhit vi mt lng gii hn ca 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 t vong 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/m3 trong 8 gi ng h s gy ra thit hi phi, hoc nng cao hn, ci cht.Cung cp thng hi hn ch ht phi.Phn ng d di vi cc kim loi v 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 trong Hnh 6-1.Thit b ly mu c m t trong Phng php 8 c th c thay th v tr ca thit b ln impinger Phng php 6. Tuy nhin, o to Phng php 8 phi c sa i bao gm mt b lc lm nng gia u d d v isopropanol impinger, v hot ng ca on tu ly mu v phn tch mu phi c mc lu lng 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

bng cch hoc l (1) thay th nc trong h thng Phng php mt 5 impinger vi mt gii php H2O2 3%, hoc (2) thay th h thng impinger Phng php 5 nc vi mt phng php isopropanol 8 b lc h thng H2O2. Vic phn tch i vi SO2 phi ph hp vi cc th tc Phng php o 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 xy dng 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 nngofstack) loi b cc ht vt cht, bao gm c sng m axit sulfuric. Mt plug si len thu tinh l mt b lc tha ng. 6.1.1.2 bot xa bng v Impingers. Mt ln bot xa bng vi nguyn liu nu thy tinh trung th v borosilicate hoc thch anh len thy tinh ng gi trong u (xem Hnh 6-1) ngn chn acid sulfuric sng m mang sang, v ba hinh rt nho 30-ml impingers. Bot xa bng kh rt nho v ln impingers phi kt ni trong lot vi cc u ni thy tinh r r. M Silicone c th c s dng, nu cn thit, ngn chn r r. Impinger kh rt nho c th c s dng v tr ca kh rt nho bot xa bng.

Ch : b gim thu gom v tc dng chy c th

c s dng, ty thuc vo s chp thun ca qun tr, nhng hiu qu thu gom phi c th hin c t nht 99 phn 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 mt hng lot ba bi kim tra, ti liu khng phi l yu cu. tin hnh th nghim hiu qu, hp th thm phi c thm vo v phn tch mt cch ring bit. iu ny hp th thm khng 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, heatstable m silicone c th c s dng, nu cn thit. 6.1.1.5 Nhit cm bin. quay nhit k, hoc tng 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 li cho thy loi silica gel, hoc tng ng, kh kh mu v bo v ng h v my bm. Nu silica gel c s dng, kh 177 EC (350 EF) trong 2 gi. New silica gel c th c s dng nh nhn c. Ngoi ra, khc cc loi cht lm kh (tng ng hoc tt hn) c th c s dng,

ty thuc vo s chp thun ca qun tr. 6.1.1.7 Van. Kim van, iu ho kh mu tc dng chy. 6.1.1.8 bm. Bm mng b r r, hoc tng ng, ko kh thng qua o to. Ci t mt nh b iu p gia my bm v ng h tc ph nhn xung 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% ca la 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 trong 2%, hiu chnh tc dng chy chn v iu kin thc t gp phi trong qu trnh ly mu, v c trang b mt cm bin nhit (nhit k quay s, hoc tng ng) c kh nng o nhit chnh xc trong vng 3 EC (5,4 EF). Mt l quan trng c th c s dng trong ni DGM quy nh trong phn ny vi iu kin c chn, nh c, v s dng theo quy nh ti Mc 16. 6.1.2 kh p k. Thy ngn, bng st , hoc khc p k c kh nng o p sut kh quyn trong 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 thit cho mu phc hi: 6.2.1 Chai Ra. Hai polyethylene hoc thy tinh chai 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 y cn thit cho phn tch mu: 6.3.1 Pipet. Th tch loi, 5 ml, 20 ml (mt cn thit cho mi mu), v kch c 25 ml. 6.3.2 lng th tch bnh. Kch c 100 ml (mt cho mi mu) 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 mi mu, trng, v tiu chun). 6.3.5 nh git Chai. Kch thc 125-ml, thm

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 phi ph hp vi cc chi tit k thut c thnh lp ca U ban Cc 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 phm tt nht c sn lp. 7,1 Thu Thp mu. Vic cht phn ng sau y cn 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 KMnO4 cht hu c c th c b qua khi nng cao ca cht hu c khng c d kin s c mt. 7.1.2 isopropanol, 80 phn trm theo th tch. Trn 80 ml isopropanol vi 20 ml nc. 7.1.2.1 Kim tra tng l ca isopropanol i vi peroxide cc tp cht nh sau: Lc 10 ml isopropanol 10 ml 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 khi 1 pht, c hp th 352 nm quang ph s dng chiu di ng dn 1-cm. Nu hp th vt qu 0,1, t chi ung ru s dng. 7.1.2.2 peroxit c th c g b t isopropanol redistilling hoc bng cch thng qua thng qua mt ct kch hot nhm, tuy nhin, thuc th lp isopropanol vi ph hp cc mc peroxide thp c th c ly t ngun thng mi. T chi rt nhiu nhim c th, do , l mt hiu 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 b ti hng ngy. 7.1.4 Gii php Kali Iodide, 10 phn trm khi lng theo Khi lng (w / v). Ha tan 10,0 g KI trong nc, v pha long 100 ml. Chun b khi cn thit. 7,2 mu Thu hi. Vic cht phn ng sau y cn thit thu hi mu:

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 trong Mc 7.1.2. 7,3 Phn tch mu. Vic thuc th sau y v tiu 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 tan 1,95 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 bari trihydrate. 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 c trc y c tiu chun ha i vi axit kali phthalate (tiu chun cp tiu hc). 7.3.6 m bo cht lng kim ton mu. khi tun th cc quyt nh, cc mu kim ton, nu c phi thu c t Vn phng khu vc thch hp EPA hoc t cc c quan thc thi trch nhim v phn tch trong kt hp vi cc mu lnh vc. Lu : Vic c quan thc thi chu trch nhim nn c thng bo t nht 30 ngy trc ngy thi cho php c 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 ml 80% isopropanol vo bot xa bng kh rt nho v 15 ca ml 3% H2O2 vo nhau ca hai impingers kh rt nho u tin. li impinger kh rt nho cui cng kh. Lp rp cc o to nh th hin trong Hnh 6-1. iu chnh my si thm d mt nhit ngn chn s ngng t nc. ni nghin nc v nc xung quanh impingers. 8,2 ly mu Train r r-Kim tra th tc. Mt leakcheck trc khi chy ly mu c ngh, nhng khng yu cu. Mt kim tra r r sau khi chy ly mu l bt buc. Th tc kim tra r r nh sau

8.2.1 Tm thi nh km ph hp (v d, 0 - n 40 ml / pht) rotameter vo cm ca DGM, v mt ni chn khng nh gi ti hoc gn u vo u d. Cm u d u vo, ko ra mt chn khng ca t nht 250 mm Hg (10. Hg), v lu tc dng chy nh c ch ra bi rotameter. Mt r r t l vt qu 2% t l ly mu trung bnh l khng th chp nhn. Ch : Cn thn (v d, t t) pht hnh thm d cm u vo trc khi tt my bm. 8.2.2 l ngh (khng bt buc) m my bm c r r kim tra mt cch ring bit, hoc l trc hoc sau khi ly 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 sy hoc my bm, ko mt chn khng 250 mm Hg (10. Hg), cm pinch cc ca hng ca c o lu lng, v sau tt my bm. Chn khng nn duy tr n nh cho t nht 30 giy. Nu thc hin trc khi chy ly mu, leakcheck bm c u tin kim tra s r r ca on tu ly mu m t ngay lp tc trn, nu thc hin sau khi ly mu chy, my bm b r r kim tra c thc hin theo on tu ly mu kim 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 p p lc. bt u ly mu, v tr nh ca vt o ti im ly mu, kt ni u d bot xa bng, v bt u bm. iu chnh lu lng mu cho mt t l khng i khong 1,0 lt / pht nh c ch ra bi t l mt. Duy tr t l ny khng i ( 10%) trong chy ly mu ton b 8.3.2 Hy c (DGM khi lng, nhit ti DGM v ti impinger cm, v tc ng h o tc dng chy) t nht mi 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 The bm, loi b cc u d t ngn xp, v ghi li trn chung kt c. 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

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 li mt phn ca tu bng cch v khng kh trong sch mi trng xung quanh thng qua cc h thng cho 15 pht t l ly mu. Lm sch mi trng xung quanh khng kh c th c cung cp bng cch khng kh thng qua mt b lc than hoc thng qua mt impinger kh rt nho thm c cha 15 ml dung dch 3 % H2O2. Ngoi ra, khng kh xung quanh khng thanh lc c th c s dng. 8,4 mu Thu hi. Ngt kt ni cc impingers sau khi purging. Loi b cc ni dung ca bot xa bng kh rt nho. Rt cc ni dung ca ln impingers vo mt s r r min ph polyethylene chai cho l hng. Ra sch ln ba impingers 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 7.1.2 8.2, 10.1-10.4 10.5 11.2.3 11.3 Quality Control Measure Isopropanol check Sampling equipmen leak-check and calibration Effect

Ensure acceptable level of peroxide impurities in isopropanol Ensure accurate measurement of stack gas flow rate, sample volume

Barium standard Ensure precision( chnh xc) of Solution normality determination standardization Replicate titrations Ensure precision of titration determinations 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, leakcheck h thng o (sy ng, kim van, bm, t l mt, v DGM) nh sau: t mt thc o chn khng u vo ng sy v ko mt chn khng 250 mm Hg

(10. Hg). Cm hoc bm cm ca dng chy ng h o, v sau tt my bm. Chn khng phi duy tr n nh cho t nht 30 giy. Cn thn th cc my o chn khng trc khi pht hnh vo cui lu lng k. 10.1.1.2 G b ng sy, v hiu chnh h thng o (tc dng chy ly mu theo quy nh ca phng php) nh sau: Kt ni mt cch thch hp kch thc t kim tra ng h o (v d, 1 lt cho mi vng) u vo ca kim 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 nghim hiu chun khi lng chia cho khi lng DGM, c khi lng iu chnh nhit tham kho v p sut) cho mi ln chy, v trung bnh cc kt qu ( Yi). Nu bt k gi tr Y lch bi hn 2% so vi ( Yi), o h thng l khng th chp nhn c s dng. Nu h thng o lng chp nhn c, s dng ( Yi) l nhn t hiu chun sau th nghim chy. 10.1.2 Sau th nghim Hiu chun Kim tra. Sau khi tng lnh vc hng lot th nghim, tin hnh kim tra hiu chun bng cch s dng th tc nu ti mc 10.1.1.2, ngoi tr ba hoc nhng cuc cch mng ca DGM c th c s dng, v ch c hai chy c lp cn c thc hin. Nu trung bnh ca hai th nghim hiu chnh cc yu t sau khng i chch hn 5% t Yi, sau Yi c chp nhn nh DGM yu 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 li o h thng nh trong mc 10.1.1, v xc nh mt posttest hiu chnh yu t ( YF). So snh Yi v YF , nh hn ca hai yu t c chp nhn nh l vic chun DGM 597 yu t. Nu hiu chun li ch ra rng h thng o lng l khng th chp nhn c s dng, hoc lm mt hiu lc chy th nghim hoc s dng phng php, ty thuc vo s chp thun ca qun tr, xc nh mt gi tr chp nhn c i vi cc mu thu thp c m lng 10.1.3 DGM nh l mt tiu chun hiu chun. Mt DGM c th c c s dng nh mt tiu chun hiu chun cho cc php o khi lng trong ni ca ng h t kim tra quy nh ti mc 10.1.1.2, rng l hiu chun ban u v recalibrated nh k theo cc th tc nu trong

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 mt cng sut 1 lt / rev (0,035 ft3/rev) hoc 3 lt / rev (0,1 ft3/rev) v c kh nng o lng khi lng trong 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 mu o to c hiu chnh cng mt tc dng chy. 10,2 Cm bin nhit . Hiu chnh chng li mercuryin thy tinh nhit k. 10,3 T l o. ng h o tc khng cn phi c hiu chun, nhng cn c lm sch v duy tr theo hng dn ca nh sn xut. 10,4 p k. Hiu chnh i vi mt hm lng thy ngn p k. 10,5Gii php chun Bari. Chun ha Bari perchlorate hoc gii php clorua so vi 25 ml tiu 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 bn phn tch cc chun ng trong vng 1% hoc 0,2 ml, ty theo iu kin no l ln hn. 11,0 Th tc phn tch. 11.1 Mu Mt Kim tra. Lu mc cht lng trong container v xc nhn xem mu no b mt trong qu trnh l hng; lu pht hin ny trn bng d liu phn tch. Nu mt s lng ng ch ca r r xy ra, hoc v hiu mu hoc s dng cc phng php, ty thuc vo s chp thun ca Qun 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 tr bnh nh mc 100 ml, pha long n chnh xc 100 ml nc, v pha trn cc mu pha long. 11.2.2 Pipet mt s chia ht mt s 20 ml dung dch mu pha long vo 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 hng bng cch s dng gii php 0,0100 N Bari tiu chun. 11.2.3 Lp li cc th tc trong mc 11.2.2, v trung bnh khi lng chun . Chy mt khong trng vi mi lot cc mu.

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 bari t 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 mu chng minh s ph hp vi quy nh ngun pht thi, mt mu kim ton, nu c, phi c phn tch. 11.3.2 ng thi phn tch mu kim ton v cc mu ph hp trong cng mt cch thc nh gi k 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, v h thng phn tch phi c s dng cho cc mu tun th v cc mu kim ton. Nu iu kin ny c p ng, trng lp kim 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. mt kim ton thit lp mu c th khng c s dng xc nhn cc b khc nhau cc mu ph hp thuc thm quyn ca ring c quan thi hnh, tr khi sp xp trc khi c c thc hin vi c hai c quan thc thi. 11,4 Kt qu mu kim ton. 11.4.1 Tnh ton nng mu kim ton v gi kt qu bng cch s dng cc hng dn c cung cp vi kim ton mu. 11.4.2 Bo co kt qu ca cc mu kim ton v vic xc nh tun th cc mu cng vi h m s, v tn ca nh phn tch. thm quyn chu trch nhim thi hnh. Bao gm thng tin ny vi cc bo co ca bt k phn tch ph hp tip theo cho cng thc thi thm quyn trong thi gian 30 ngy. 11.4.3 Cc nng ca cc mu kim ton thu c t nh phn tch phi ng trong vng 5% thc t tp trung. Nu 5% c im k thut khng phi l c p ng, reanalyze tun th v kim ton mu, v bao gm gi 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 th hoc tnh trng khng tun th ca c s b nh hng, Qun tr vin c th b yu cu ti phn tch, tip tc kim ton, hoc thi li v chp nhn kt qu vic thc hin

th nghim. Trong khi cc bc ang c thc hin gii quyt phn tch kim ton vn , 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 ph con s c ngha vt ra ngoi cc d liu thu c. vng tt 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 ton mu, mg / dscm. CSO2 = Nng SO2, kh c s, sa cha tiu 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 cha vi iu kin tiu chun, dscm (dscf). Vsoln = Tng khi lng ca gii php, trong SO2 mu c cha, 100 ml. Vt = Th tch ca cht th chun tiu chun bari c s dng cho mu (trung bnh ca chun ti to), ml VTB = Th tch ca cht th chun tiu chun bari c s dng cho trng, ml. Y = DGM hiu chnh yu t. 12,2 Th tch mu kh kh, hiu chnh chun iu kin ny. Cng thc trang 602 epa6

13,0 Phng php Performance. 13,1 Phm vi. Gii hn pht hin ti thiu ca phng php c xc nh l 3,4 mg SO2/m3 (2,12 x 10-7 lb/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 nho impingers, c cha 15 ml dung dch 3% H2O2. da trn cc tnh ton l thuyt, gii hn nng trn mu 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 bi m lng. Ma = Trng lng phn t ca khng kh xung quanh bo ha impinger nhit , g / g-nt rui (lb / lb-nt rui). Ms = Trng lng phn t ca kh mu bo ha impinger nhit , g / g-nt rui (lb / lb-nt rui). Pc = Inlet chn khng c c trong hiu chun chy, mm Hg (. Hg). Psr = Inlet chn khng c c trong ly 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 tra chy 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 phng ng h o, m3 (ft3). VSB (tiu chun) = Th tch ca kh c o bng bong bng x phng ng 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 sut Cc php o. Mt l quan trng c th c s dng thay cho DGM quy nh ti mc 6.1.1.10, vi iu kin l n l

la chn, nh c, v s dng nh sau: 16.2.1 Chun b ca tu ly mu. Lp rp cc o to ly mu c th hin trong hnh 6-2. Cc ng h o tc v b 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 mt Phng php o to ly mu 6 loi nh sau: Insert loi tay o, nt chai l huyt thanh vo hai cng on gim. a kim 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 dng kim 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 dng cung 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 trong phn. Chn mt l quan trng c kch thc hot ng tc dng chy mong mun. Kch thc v ng kim di th hin trong Bng 6-1 cho gn ng sau y dng chy t l. 16.2.2.2 Xc nh s ph hp v chn khng thch hp hot ng ca l quan trng nh sau: Nu c th, tm thi nh km mt ng h o tc v b iu p u ra ca o to ly mu, nu ni thit b khng c mt (xem Phn 16.2.1). Bt my bm v iu chnh cc van cung cp cho mt cm chn khng c tng ng vi khong mt na p sut kh quyn. Quan st cc ng h o tc c. Dn dn tng cc chn khng cho n khi mt c n nh l thu c trn ng h tc . Ghi li chn khng quan trng, l chn khng cm khi cc 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 khi chy ly mu c ngh, nhng khng cn thit. cc r r kim tra th tc nh sau: Tm thi nh km mt ph hp (v d, 00-40 ml / pht) rotameter v b tng, hoc mt ng 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 250 mm Hg (10. Hg), v lu tc dng chy nh c ch ra bi rotameter hoc ng h o bong bng. Mt t l r r vt qu 2% t l ly mu trung bnh (Q tiu chun) l khng chp nhn c. Cn thn th d tm trc khi cm u vo tt my bm.

16.2.3.2 Xc nh m. Ti ly mu v tr, trc khi th nghim, xc nh m% ca khng kh mi trng xung quanh bng cch s dng nhit bu t v kh hoc, nu thch hp, mt ng h o m tng i. 16.2.3.3 quan trng l chai Calibration. ti v tr ly mu, trc khi th nghim, hiu chnh ton b ly mu o to (tc l, xc nh tc dng chy ca ly 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. ghi cc thng tin c lit k trong hnh 6-4. Tnh ton tiu chun khi lng khng kh c o bng ng h bong bng x phng v t 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)

16.2.3.4 ly mu. 16.2.3.4.1 Hot ng o to ly mu mu thu chn khng c s dng trong qu trnh hiu chun chy. Bt u xem v my bm cng mt lc. Hy c (nhit , ng h tc , chn khng u vo v u ra chn 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 cch s dng cc th tc hiu chun c nu trong mc 16.2.3.3. Nu Qstd thu c trc v sau khi th nghim khc nhau bi nhiu hn 5%, lm mt hiu lc chy th nghim, nu khng, tnh ton khi lng ca kh c o vi l quan trng bng cch s dng phng trnh 6-6 nh sau: Vm(std)
=

Eq. 6-5

Qstd .s (1 - Bwa) (Pbar+ Psr)/(Pbar+ Pc)

Eq. 6-6

16.2.3.4.3 Nu% s khc bit gia trng lng phn t ca khng kh xung quanh iu kin bo ha v kh mu l 3%, sau cc trng lng phn t ca mu kh phi c xem xt trong tnh ton bng cch s dng phng trnh sau y:

(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 v Cc bi kim tra kt qu hiu chun chy s cho bit liu c r r bt k. 16.2.3.4.4 X bn tm nc , v ty ly mu o to s dng cc th tc c m t ti mc 8.3.4. 16,3 xo b nhiu Amoniac. cc theo th tc thay th phi c s dng b sung nhng quy nh c th trong phng php ly mu ti ngun c 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-stack b lc (si thy tinh) loi b cc ht vt cht. cc vt 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 trong Tham kho 10 ti Mc 17,0 Phng php 5 l mt v d v mt b lc c chng minh lm vic. Trng hp c tnh kim ht vt cht v m ngng t c mt trong dng kh, b lc c un nng trn m im sng nhng di y 225EC (437EF). 16.3.2 Thu hi mu. Khi phc cc mu theo Mc 8.4 tr loi b cc ni dung ca kh rt nho bot xa bng. Thm ni dung bot xa bng, bao gm c rinsings ca bot xa bng vi nc, ring polyethylene chai t phn cn li ca mu. Theo kim tra iu kin bnh thng trixt lu hunh s khng c hin din ng k, cc th nghim c th la chn xa cc kh rt nho bot xa bng t o to ly mu. Nu mt xp x nng trixt lu hunh l mong mun, chuyn nhng cc ni dung ca cc bot xa bng kh rt nho ring polyethylene chai. 16.3.3 Phn tch mu. Thc hin theo cc th tc Mc 11.1 v 11.2, ngoi tr thm 0,5 ml dung dch HCl 0,1 N bnh Erlenmeyer v trn trc khi thm ch s. Cc th tc phn tch sau y c th c s dng cho mt xp x ca nng trixt lu hunh. Cc chnh xc nng tnh ton s ph thuc vo ammonia SO2 t l v mc ca hin ti oxy trong dng kh. Mt phn nh ca SO2 s c tnh l trixt lu hunh nh amoniac SO2 t l v mu Lng oxy tng ln. Ni chung, khi t l ny l 1 hoc t hn v lng oxy trong khong 5%,

t hn 10% ca SO2 s c tnh l trixt lu hunh. Phn tch cc mu peroxide v isopropanol phn ring bit. Phn tch phn peroxide nh m t trn. Trixt lu hunh c xc nh bi s khc bit bng cch s dng chun tun t ca isopropanol phn ca mu. Chuyn cc ni dung ca isopropanol lu tr container bnh nh mc 100 ml, v pha long chnh xc 100 ml nc. Pipet mt ml 20 s 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, v 2-4 git ch th Thorin. Chun vi mt mu hng thit b u cui s dng 0,0100 N Bari perchlorate. Lp li v trung bnh khi lng chun ng trong vng 1% hoc 0,2 ml, ty theo iu kin no l ln hn. S dng khi lng trong phng trnh 6-2 xc nh nng trixt lu hunh. T bnh cha phn cn li ca isopropanol mu, xc nh cc phn ca SO2 c thu thp trong bot 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, v chun nh trc. T khi lng chun ny, tr cht th chun khi lng xc nh cho trixt lu hunh, v thm khi lng cht th chun xc nh cho phn peroxide. iu ny khi lng cui cng to nn Vt, cc khi lng bari perchlorate c s dng cho cc mu SO2. 17,0 Ti liu tham kho. 1. Pht thi kh quyn t axit sulfuric Sn 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 trong L kh. Tp ch ca Vin nhin liu. 24:237-243. Nm 1961. 3. Matty, R.E., v E.K. Diehl. o thi-kh SO2 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. Air Hip hi Kim sot nhim. 13:162. Nm 1963. 5. Rom, J.J. Bo tr, hiu chun, v hot ng Thit b ly mu Ngun Isokinetic. Vn phng ca Air Cc chng trnh, C quan Bo v Mi trng Hoa K. Nghin cu Triangle Park, NC. APTD-0576. Thng 3 nm 1972. 6. Hamil, H.F., v D.E. Camann. hp tc nghin cu Phng php Xc nh pht thi Dioxide lu hunh

Ngun Vn phng phm (hi t nhin liu ha thch My pht in). C quan Bo v Mi trng Hoa K, nghin cu Triangle 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 v Vt liu. Philadelphia, PA. Nm 1974. trang 40-42. 8.Knoll, J.E., v M. R. Midgett. p dng cc EPA Phng php 6 Nng Dioxide lu hunh cao. M C 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 kh Tiu chun hiu chun. nh gi Hi ngun Bn 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 ngun Bn tin. 5 (1) :24-28. Thng 2 nm 1980. 11.Lodge, J.P., Jr, et al. Vic s dng ca tim di da Kim nh l quan trng trong ly mu khng kh. J. Air Hip hi Kim sot nhim. 16:197-200. Nm 1966. 12. Shigehara, R.T., v C. B. Sorrell. S dng L quan trng nh Phng php 5 CalibrationStandards. ngun Bn tin Hip hi nh gi. 10:4-15. Thng Tm nm 1985. 13. Curtis, F., Phn tch Phng php 6 mu trong S 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 nhau
Tip theo trang 615 cua epa6