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tiu chun vit nam

TCVN 7242 : 2003

L t cht thi rn y t Phng php xc nh nng cacbon monoxit (CO) trong kh thi
Health care solid waste incinerators Determination method of carbon monoxide (CO) concentration in fluegas

1 Phm vi p dng
Tiu chun ny quy nh phng php xc nh nng cacbon monoxit (CO) trong kh ng khi l t cht thi rn y t, quy v iu kin nhit v p sut tiu chun. Ch thch: Nhit v p sut tiu chun l nhit 0 oC v p sut 101,3 kPa. Sau khi ly mu, dung dch mu c phn tch bng mt trong hai phng php sau: - Phng php A: Xc nh CO bng phng php to mu vi kali iodua p dng trong trng hp nng CO cao. Gii hn xc nh ca phng php l 63 mg cacbon monoxit trong 1 m3 khng kh. - Phng php B: Xc nh CO bng phng php to mu vi thuc th Folin - Xiocant p dng trong trng hp nng CO thp. Gii hn xc nh ca phng php l 30 mg cacbon monoxit trong 1 m3 khng kh. Sai s cho php ca phng php l 5 %. Cn tr: Cc ion phn ng vi ion bc (nh Br , I , CN , S2, SO32, SCN) u nh hng vic xc nh. Cc cht cn tr ca phng php l anhydrit sunfur (SO2), hydro sunfua (H2S).

2 Tiu chun vin dn

TCVN 4851: 1989 (ISO 3696: 1987), Nc dng phn tch trong phng th nghim. Yu cu k thut v phng php th. 3

TCVN 7242 : 2003 3 Nguyn tc

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3.1 Nguyn tc chung cho c 2 phng php Cacbon monoxit tc dng vi paladi clorua d to thnh paladi kim loi CO + PdCl2 + H2O = CO2 + 2HCl + Pd 3.2 Phng php A (1)

Sau khi cacbon monoxit tc dng vi paladi clorua, to thnh paladi kim loi, nh lng lng paladi clorua d bng cch cho tc dng vi kali iodua s to thnh paladi iodua (PdI2) c mu PdCl2 + 2 KI = 2 KCl + PdI 2 (mu ) (2)

Xc nh nng cacbon monoxit trong kh ng khi bng cch s dng my o quang ph o hp th ca dung dch mu bc sng t 490 nm n 530 nm. 3.3 Phng php B

Sau khi cacbon monoxit tc dng vi paladi clorua, to thnh paladi kim loi. Thm thuc th folinxiocant (dung dch photphomolipdic), thuc th folinxiocant s tc dng vi paladi kim loi va to thnh v b kh, dung dch chuyn t mu vng sang mu xanh. Phn ng c thc hin trong mi trng kim (Na2CO3) 2H3PO4.10MoO3 + 4HCl + 2Pd = 2PdCl2 +2H2O + 2 [(MoO3)4.(MoO2). H3PO4] (3)

Xc nh nng cacbon monoxit trong kh ng khi bng cch s dng my o quang ph o hp th ca dung dch mu vng xanh bc sng t 650 nm n 680 nm.

4 Thuc th
Trong phn tch, tr khi c nhng quy nh khc, ch s dng cc thuc th c tinh khit c tha nhn v nc ct hoc nc loi khong hoc nc c tinh khit tng ng theo TCVN 4851 :1989. Cnh bo Khi dng cc thuc th phi tun theo cc quy nh thch hp v an ton sc kho. 4.1 Thuc th chung cho c hai phng php:

4.1 .1 Dung dch hp th paladi clorua (PdCl2 1 , HCl 4 ) Sy kh paladi clorua tinh khit 105 oC trong 1 h, ngui. Cn 0,5 g paladi clorua sy kh ri cho vo bnh nh mc dung tch 500 ml, thm 200 ml nc, 2 ml axit clohydric c (HCl = 1,18), lc cho tan ht. Cui cng thm nc va 500 ml T phng trnh (1), 1 ml dung dch paladi clorua 1 tng ng vi 0,157 mg CO. 4

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4.1.2 Dung dch natri cacbonat (Na2CO3 .10 H2O 20 %) Ho tan 20 g natri cacbonat (Na2CO3 .10 H2O) trong khong 30 ml n 50 ml nc trong bnh nh mc 100 ml, thm nc va n vch. Lc u 4.2 Thuc th cho phng php A: 4.2.1 Dung dch alumin sunfat [Al2(SO4)3 10 %] Cn 10 g alumin sunfat [Al2(SO4)], ho tan trong khong 30 ml n 50 ml nc trong bnh nh mc dung tch 100 ml, thm nc va 100 ml. 4.2.2 Dung dch kali iotdua (KI 20 %) Cn 20 g kali iodua (KI), ho tan trong khong 30 ml n 50 ml nc trong bnh nh mc dung tch 100 ml, thm nc va 100 ml. 4.3 Thuc th cho phng php B: 4.3.1 Dung dch Folinxiocant (dung dch photphomolipdic) Cho vo mt bnh nh mc 1500 ml: 100 g natri tungstat (Na2WO4.2H2O) 25 g natri molipdat (Na2MoO4) Lc cho tan hon ton, sau thm: 100 ml axit clohydric c ( = 1,18) 50 ml dung dch axit photphoric 85 % Lc u v un si trong 10 h trong mt bnh cu c lp ng sinh hn ngc (trnh bay hi). ngui n nhit phng, thm nc va 1000 ml. Bo qun trong chai mu nu, nt kn. 4.3.2 Axit Focmic c (H-COOH)

5 Thit b, dng c
Dng c thng thng phng th nghim, v cc thit b sau: 5.1 u d ly mu, lm bng vt liu khng b n mn nh borosilicat hoc thu tinh thch anh, mt u ni nhm hnh cu ng knh trong t 6 mm n 10 mm, c chiu di thch hp ti c cc im o trong mt phng o ca ng khi v c bc mt lp v to nhit c kh nng to ra nhit ti thiu l 200 oC. 5

TCVN 7242 : 2003

Ch thch:

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1. Lp v to nhit ny ng thi ng vai tr bo v cho ng ly mu kh, v vy ng ly mu kh lun c bc lp v to nhit; 2. Mt van ngt c t trc b hp th th nht ngn nga s tht thot cc tc nhn phn ng khi ly mu kh ng khi cc iu kin lc ht.

5.2 B lc bi, lc bi khi kh, lm bng borosilicat hoc thu tinh thch anh c cc u ni nhm hnh cu. B lc ny c th kt hp vi u d ly mu hoc ring, v c th trong hoc ngoi ng dn kh thi. Th d b lc lp ngoi c ch ra trn hnh 1. Dng bng thu tinh thch anh lm vt liu lc trung tnh t nng nu cn. 5.3 Thanh t nng, th d thanh t nng iu khin bng thyristor ( sy nng thit b ly mu bn ngoi ng khi). 5.4 ng hnh ch T, th d bng borosilicat hoc thu tinh thch anh, sy nng nu cn. 5.5 Bnh ly mu kh (bnh hp th), dng bnh dung tch 200 ml, 500 ml hoc 1000 ml (tu chn), c hai kho [xem hnh 2]. Dung tch bnh c xc nh bng phng php dng nc o th tch. Ch thch

Ngoi bnh ly mu c th tch bit chnh xc, c th dng bm tim (th tch 200 ml hoc

500 ml). Trng hp ny, hiu qu nh c th khng t c.

5.6

Bnh ra, loi hi axit (th d SO2, HCl) bo v bm ht. Bnh ny ch dng khi c nhiu hi

axit trong mu kh. 5.7 ng lm kh, bo v bm. Dng ht silica gel hoc canxi clorua lm cht ht m. 5.8 Bm ht Bm ny c kh nng ht kh vi lu lng t 0,3 l/min n 3 l/min trong khong thi gian ly mu vi p lc t -10 kPa n -30 kPa. 5.9 Thit b o p sut, o p sut trc v sau khi ly mu kh; thit b o p sut thu ngn hoc dng c o p sut tng ng. 5.10 ng sinh hn 5.11 Bnh nh mc, dung tch:1500 ml, 500 ml, 100 ml, 25 ml. 5.12 Van iu chnh Van kim c kh nng iu chnh lu lng kh ng khi t 0,02 m3/h n 0,2 m3/h. 6

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5.13 Thit b o lu lng khng kh Thit b o lu lng kh m (hoc thit b o lu lng kh kh vi mt ng lm kh u dng kh) c kh nng s dng mc lu lng kh ng khi trong khong t 0,02 m3/h n 0,2 m3/h. Gii hn sai s nh hn 2 %. Cn kim tra gii hn sai s hai ln trong mt nm bng mt dng c o dng bong bng x phng thch hp. 5.14 Nhit k Nhit k o c trong phm vi t 5 oC n + 50 oC, sai s ca php o nh hn 0,2 oC. 5.15 p k p k c kh nng o p sut kh quyn ni ly mu, sai s ca php o nh hn 1 %. 5.16 ng h bm giy 5.17 Vi ly mu, l mt ng thu tinh nh, c ng knh ngoi 6 mm ng knh trong 1 mm, v chiu di khong 60 mm, mt u c vut nhn. c im ca vi ly mu phi m bo sao cho khi ni vi bnh ly mu dung tch 1 l, s tng p sut u n s xy ra trong vng t 5 min n 12 min. th vi ly mu, mt kho ca bnh ly mu ni vi dng c o p sut, kho kia ni vi vi ly mu. Khi m cc kho, p sut s tng t t. 5.18 Nhit k, o nhit xung quanh khi ly mu kh. 5.19 My o quang ph, c kh nng o cc di bc sng t 490 nm n 530 nm v t 650 nm n 680 nm v cuvet c b dy t 1,0 cm n 5,0 cm. Ch thch - bo v da ngn tay khi b tc ng ca dung dch kim nn dng gng cao su mng. Gng
polyvinylclorua khng nn dng v chng d bm vo b mt thu tinh.

5.20

Bm tim (tu chn) nh m t trn hnh 3. Bm tim dng a dung dch hp th vo bnh

ly mu. 5.21 My lc

TCVN 7242 : 2003

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Kch thc tnh bng milimt

1 Bng thch anh, khong 0,5 g n 0,8 g, nhi y. 2 Tm c l hoc b lc bng gm.

Hnh 1 Th d v b lc bi lp ngoi ng dn kh thi

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2a

2b

Hnh 2 Th d v cc bnh ly mu kh hai kho

1 ng cao su silicon 2 Dung dch hp th

Hnh 3 Bm tim a dung dch hp th vo bnh ly mu

TCVN 7242 : 2003 6 K thut ly mu

6.1 Khi qut Lp t h thng thit b ly mu ph hp vi s trnh by hnh 4. Phi m bo khng c r r trong h thng thit b ly mu. Khi ly mu cn trnh khng bi vo bnh ly mu lm hng thuc th. 6.2 6.2.1 Ly mu kh bng phng php th ch th tch Ni bnh ly mu kh (6) vi thit b ly mu nh hnh 4. Khi ng bm ht (5), thi sch

ng ly mu v bnh n khi th tch kh i qua bng 10 ln th tch bnh ly mu. Sau ng hai kho ca bnh ly mu sao cho to ra s qu p nh trong bnh. Khi nhit cn bng (thng trong 3 min) bnh c di nc, o nhit v p sut khng kh bn ngoi v a dung dch hp th vo bng bm tim (xem 5.20). 6.2.2 Tho bnh ng kho ca bnh ly mu. Tho bnh ra khi thit b ly mu. 6.2.3 a dung dch hp th vo bnh Dng ng cao su silicon ni u kho ca bnh ly mu vi bm tim (5.20) cha sn dung dch hp th paladi clorua 1 (4.1.1): 3 ml (nu xc nh CO bng phng php A), 1 ml (nu xc nh CO bng phng php B). Sau m kho v a dung dch hp th vo bnh. ng kho bnh v tho bm tim khi bnh. tip xc t nht 4 h. 6.2.4 Lc bnh Lc mnh bnh, thnh thong ngng trong vng 3 min hoc sau khi lc mnh bnh 1 min ri t bnh vo my lc v lc thm 2 min.

10

TCVN 7242 : 2003

1 u d ly mu, lm nng nu cn 2 B lc bi, lm nng nu cn 3 ng ly mu (cng ngn cng tt) lm nng,nu cn 4 B phn ngng t 5 Bm ht 6 Bnh ly mu kh 7 Thit b o lu lng kh 8 Nhit k 9 p k

Hnh 4 - S h thng ly mu ngng t, bnh ly mu hai kho

7 Cch tin hnh

7.1 Phng php A : Xc nh CO bng cch to mu vi kali iodua 7.1.1 Phn tch Sau 4 h dung dch paladi trong chai b kh ht, dung dch s khng mu v c vng en trn b mt th cho thm paladi clorua ri tip tc thm 4 h na. Nu dung dch hp th trong chai c mu vng th chng t cn d paladi clorua, do khng cn cho thm. Chuyn ton b mu vo bnh nh mc dung tch 100 ml, trng bnh ly mu nhiu ln bng nc ri nhp nc ra ny vo dung dch mu, thm dung dch kali iodua v thm nc n vch, lc u. Dung dch s chuyn thnh mu . Song song lm ng thi mt mu trng. Sau 15 pht, xc nh nng cacbon monoxit trong kh ng khi bng cch dng my o quang ph o hp th ca dung dch mu bc sng t 490 nm n 530 nm. 11

TCVN 7242 : 2003

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7.1.2 Xy dng ng chun cacbon monoxit (CO) Ly nm bnh hp th, dung tch 500 ml ra v ngm bng dung dch sunfo cromic, trng ra k bng nc v nh s t 0 n 4. Dng pipt ht ln lt 0,0 ml; 0,4 ml; 0,8 ml; 1,2 ml v 1,6 ml dung dch hp th paladi clorua 1 (4.1.1) vo dy bnh trn. Thm vo mi bnh 5 ml dung dch kali iodua (4.2.2) v 50 ml nc. Sau 15 min, s dng my o quang ph o mt quang bc sng t 490 nm n 530 nm. Bng 1 - Hm lng CO tng ng trong cc bnh Bnh s 0 Thuc th (ml) Dung dch paladi clorua 1 (4.1.1) Hm lng CO (mg) 0,0 0 0,4 0,0628 0,8 0,1256 1,2 0,1884 1,6 0,2512 1 2 3 4

7.2 Phng php B: Xc nh CO bng phng php to mu vi thuc th Folin - Xiocant 7.2.1 Phn tch Chuyn ton b mu vo bnh nh mc dung tch 25 ml (th tch V1), trng bnh ly mu nhiu ln bng nc ri nhp nc ra ny vo dung dch mu v nh mc n vch, lc u. Song song lm ng thi mt mu trng. Ht 10 ml dung dch trn chuyn vo mt bnh khc. Thm 1,5 ml thuc th Folinxiocant 1 % (4.3.1), un cch thy 30 pht. Trn ming bnh t mt phu nh ( = 5 cm) gi cho dung dch khi b cn. Thnh thong lc cho tan kt ta. ngui. Chuyn dung dch sang bnh nh mc dung tch 25 ml, trng bnh cch thu bng nc. Thm 10 ml dung dch natri cacbonat (Na2CO3) 20 % (4.1.2) v thm nc n vch, lc u. Sau 15 pht, s dng my o quang ph o mt quang bc sng t 650 nm n 680 nm. 7.2.2 Xy dng ng chun cacbon monoxit (CO) Ly nm bnh hp th, dung tch 500 ml ra v ngm bng dung dch sunfo cromic, trng ra k bng nc v nh s t 0 n 4. Cho ln lt dung dch paladi clorua 1 (4.1.1) vo tng bnh theo th t: 0,0 ml; 0,2 ml; 0,6 ml; 0,8 ml v 1,0 ml. Sc mt lng kh CO d kh ht lng paladi clorua trong cc bnh. 12

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Bng 2 - Hm lng CO tng ng trong cc bnh Bnh s 0 Thuc th (ml) Dung dch paladi clorua 1 (4.1.1) Hm lng CO (mg) 0 0,0314 0,0942 0,1256 0,157 0,0 0,2 0,6 0,8 1,0 1 2 3 4

Kh CO c iu ch nh sau: H2SO4, to HCOOH CO + H2O y nt kn, tip xc t nht trong 4 h, thnh thong lc, cn thn trnh kt ta en dnh ln thnh bnh. un cch thu 30 pht. Bm khng kh sch ui ht cacbon monoxit (CO) d. Cho thm ln lt dung dch paladi clorua 1 (4.1.1) va 1 ml (1,0 ml; 0,9 ml; 0,8 ml; 0,7 ml; 0,6 ml; 0,5 ml). Cho tip vo mi bnh 1 ml thuc th Folinxiocant (4.3.1), lc u. un cch thu 30 pht, lc u. Sau chuyn ln lt cc dung dch trn sang cc ng ong dung tich 25 ml, ra, trng bng nc v nh mc n vch. Ht 10 ml dung dch trn chuyn vo bnh khc. Thm 1,5 ml thuc th Folinxiocant 1 % (4.3.1), un cch thy 30 pht. Trn ming bnh t mt phu con gi cho dung dch khi b cn. Thnh thong lc cho tan kt ta. ngui. Chuyn dung dch sang bnh nh mc dung tch 25 ml, trng bnh cch thu bng nc. Thm 10 ml dung dch natri cacbonat (Na2CO3) 20 % (4.1.2) v nh mc bng nc n vch, lc u. Sau 15 pht, o mt quang bc sng t 650 nm n 680 nm.

8 Tnh kt qu
8.1 Tnh lng mu kh ly Tnh lng mu kh ly, qui v iu kin nhit v p sut tiu chun (0 oC v 101,3 kPa) bng cng thc (4):

Vs =Va
trong

p 1 pw 1 p0 101, 3 273+ t 1 273+ t 0

273

(4)

Vs l lng mu kh ly, tnh bng lit; Va l dung tch bnh ly mu (5.5), tnh bng lit; p0 l p sut trong bnh trc khi ly mu, tnh bng kilopascan; p1 l p sut trong bnh sau khi ly mu, tnh bng kilopascan; 13

TCVN 7242 : 2003

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t0 nhit trong bnh trc khi ly mu, tnh bng Celsius ( C); t1 nhit trong bnh sau khi ly mu, tnh bng Celsius ( C); pw1 l p sut hi nc t1 (bng 0 nu kh kh), tnh bng kilopascan. t1 = t0 v cng thc (4) c gin lc thnh cng thc (5)

Vs = Va
Cc k hiu nh cng thc (4). 8.2 Tnh nng cacbon monoxit

273 101, 3

p 1 p w1 p 0 273 + t 1

(5)

Tnh nng cacbon monoxit trong mu kh thi theo cng thc:

c= f A
Trong

Vt 10 3 Vs

(6)

c l nng cacbon monoxit trong mu kh thi, tnh bng miligam trn mt khi; f l h s hiu chun, tnh bng miligam trn lt dung dch; Ch thch - Gi tr ca f phi ph hp vi b dy cuvet, nu thay cuvet phi dng li ng chun. A l hp th; Vt l th tch ca dung dch mu tng, tnh bng lit; Vs l th tch ca mu kh iu kin tiu chun nh tnh 8.1, tnh bng lit.

9 Bo co kt qu
Trong bo co kt qu, cn thit phi c cc thng tin sau: a) Vin dn tiu chun ny b) Nhn bit mu th; c) M t l t cht thi v qu trnh hot ng (cng ngh); d) iu kin vn hnh ca l t; e) V tr mt phng o; f) V tr im o trong mt phng o; g) Nhng thay i trong cc hot ng ca l t trong khi ly mu, chng hn nhng thay i b phn t nhin liu;

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TCVN 7242 : 2003

h) Nu ra bt k thao tc no khng c quy nh trong tiu chun ny hoc c coi l thao tc tu ; i) Kt qu phn tch; j) Ngy thng v thi gian ly mu.

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