tiu chun vit nam

TCVN 5978: 1995

Cht l|ng khng kh - Xc nh nng khi l|ng l|u hunh dioxit trong khng kh xung quanh Ph|ng php trc quang dng thorin
Air quality - Determination of mass concentration of sulphur dioxide in ambient air - Thorin spectro photometric method
1. Lnh vc Tiu chun ny m t ph|ng php trc quang dng thorin (mui natri ca axit 4- [(2arsenophenyl)azolj 3-hydroxy 2,7-naphtalen- disunphonic), xc nh nng khi l|ng ca l|u hunh dioxit trong khng kh xung quanh. Phm vi p dng Ph|ng php ny |c dng xc nh nng khi l|ng ca l|u hunh dioxit trong khng kh xung quanh trong khong nng t 3,5 n 150Pg/m3 vi th tch mu l 2m3 v th tch dung dch mu l 50ml. Vi nhng nng cao hn th phi pha long mu tr|c khi xc nh. S c mt ca amnic v hydrosunfua vi nng rt cao trong mu c th gy cn tr php o. Trong lc ly mu phi loi b bi bng cch lc khng kh trnh nh h|ng (xem 8.3).
Ch thch: S pha long i khi l khng cn thit nu nh| vic ly mu khng kh trong thi gian quy nh |c gim xung bng cch chia ton b thi gian ly mu thnh tng khong thi gian ngn nh| nhau v nh| vy s ly mu cng gin on theo khong thi gian v bm ly mu b ngt.

2.

3.

4.

Tiu chun trch dn Tiu chun sau y |c p dng cng vi tiu chun ny: TCVN 5968: 1995 (ISO 4219: 1979) - Cht l|ng khng kh - Xc nh hp cht kh ca l|u hunh trong khng kh xung quanh. Thit b ly mu. Nguyn tc Cho mu khng kh i qua dung dch hydroperoxit axit ha c pH xc nh trong mt thi gian |c quy dnh. L|u hunh dioxit c trong mu s |c hp th v oxy ha to thnh axit sunfuric. Kt ta ion sunfat d|i dng bari sunfat bng bari perclorat d| v xc nh l|ng ion bari d| nh to phc mu vi thorin v o mu b|c sng 520nm.
Ch thch: Hiu s gia l|ng ion bari tr|c v sau phn ng t|ng ng vi nng ca ion sunfat trong dung dch hp th, ngha l t|ng ng vi l|ng l|u hunh dioxit b oxy ha. hp th t l nghch vi nng ion sunfat trong dung dch hp th.

5.

Thuc th Trong phn tch ch dng nhng thuc th c tnh khit phn tch |c chp nhn v ch dng n|c ct hai ln hoc n|c ct loi ion.
Ch thch: Phi cn thn khi dng nhng ha cht nguy him nh| dung dch axit percloric, dung dch bari perclorat, dioxan v thorin.

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5.1. 5.2.

TCVN 5978: 1995

5.3.

5.4. 5.5.

5.6.

Hydro peroxit dung dch 27 n 30% (mlm) Dung dch hp th Pha long 10ml dung dch hydro peroxit (5.l) vi n|c thnh l000ml. iu chnh pH ca dung dch gia 4 v 4,5 bng dung dch axit percloric (5.4) nn dng pH mt o dung dch ny trong t lnh v ch dng |c trong vng l thng k t lc pha. Axit percloric dung dch 0,lmol/l Cho 4,3ml dung dch axit percloric 72% (m/m) vo bnh nh mc 500ml, cho n|c n vch v lc trn u. Axit percloric dung dch khong 0,01mol/l: pha t dung dch 0,lmol/l (5.3). Bari peclorat dung dch. Ha tan 0,525g bari peclorat khan [Ba (ClO4)2] trong mt l|ng nh dung dch axit percloric 0,lmol/l (5.3) trong bnh nh mc 250ml, ri thm dung dch axit percloric 0,lmol/l n vch, lc u. Bari perclorat/dioxan dung dch Cho l0ml dung dch bari perclorat v 40ml n|c vo bnh nh mc l000ml, thm dioxan n vch, lc u.
Ch thch: 1) C th dng mt s dung mi hu c nh| dioxan, ieopropanol, axeton nh|ng dng dioxan lp |ng chun l tt nht. 2) Dung mi hu c tc dng lm gim tch s tan ca bari sunfat nh|ng iu ny vn cn c ngha trong vng nng nh, th|ng cho thm mt l|ng nh khng i ion sunfat vo dung dch trng, cc dung dch chun v phn ht ca mu.

5.7.

Thorin dung dch 2,5g/l. Ha tan 0,125g thorin trong 20ml dung dch sunfat tiu chun (5.8.2) v mt l|ng nh n|c trong mt bnh nh mc 50ml, thm n|c ti vch v lc trn u. Chun b dung dch ny dng trong ngy. 5.8. Dung dch sunfat tiu chun 5.8.1. Dung dch sunfat tiu chun cha 0,5 mol H2SO4 trong mt lt. nh chun dung dch ny mt cch chnh xc bng cch chun vi dung dch natri hydroxit chun v bn thn dung dch NaOH ny |c nh chun vi kali hydro phtalat (KC8H4O ), lml ca dung dch tiu chun ny t|ng ng vi 32mg SO2. 5.8.2. Dung dch sunfat tiu chun cha 0,00125mol H2SO4 trong l lt. iu ch t dung dch sunfat tiu chun (5.8.l) bng cch pha long nh| sau: a) Dng pipt ly 25ml dung dch sunfat tiu chun cho vo bnh nh mc l000ml, cho n|c ti vch, lc trn u, lml ca dung dch ny t|ng |ng vi 800Pg SO2; b) Dng pipt ly l0ml dung dch sunfat tiu chun thu |c t im a cho vo bnh nh mc l00ml, cho n|c ti vch v lc u, lml ca dung dch tiu chun ny t|ng |ng vi 80Pg SO2. 6. Thit b Nhng thit b ca phng th nghim thng th|ng l

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6.1.

TCVN 5978: 1995

Thit b ly mu |c quy nh trong TCVN 5168: 1995 (ISO 4219) t 5.l n 5.7 v b sung thm nh| quy nh trong 6.l.l d|i y. 6.1.1. Cc bnh hp th Dng nhng bnh thy tinh bosilicat kiu Drechsel c nhng ch ni bng thy tinh nhm c th thay th |c (xem hnh l). Bnh hp th c cc ch ni bnh cn thy tinh nhm nh| vy l rt thch hp bi v lm gim cc s c do cc cht lng ng ri xung dung dch hp th khi tho u ly mu ra. Dng bnh 125ml cho ly mu 24 gi v 250ml cho ly mu 48 gi. |ng knh ngoi ca ng vo v ng ra ca bnh hp th l l0 n 12mm. ng dn khng kh vo dung dch c |ng kinh t 6 n 8mm v cch y bnh t 5 n 10mm.

6.2.

Ph quang k loi l chm tia v loi 2 chm tia Nu dng ph quang k mt chm tia th phi iu chnh |c c|ng chm tia ti bng mn chn hoc rng khe o. Vi mt ph quang k mt chm tia th chnh xc cao nht c th t |c nu my c kh nng iu chnh sao cho "s c" ca dung tch c nht c th o |c n gi tr cng gn 0 cng tt. Tuy nhin vi cc my hin nay, kh nng tt nht ch l iu chnh c|ng chm sng t |c "s c" l 0,800 vi dung dch trng o trong cuvet l0mm hoc 20mm. Nu dng ph quang k hai chm tia th c th c trc tip s chnh lch ca hp th gia mu (hoc cc dung dch.chun) vi dung dch tr|ng.

tiu chun vit nam

TCVN 5978: 1995

Ch thch: "S c" l gi tr c |c trn mt ca ph quang k 1 chm tia; tn hiu o |c t l vi logarit ca c|ng .

6.3.

Cc cuvet thy tinh Cc cuvet thy tinh l0mm hoc 20mm. Nu dng hai hoc nhiu cuvet o, th cc cuvet phi ng nht v quang. 6.4. Cc pipt c dung tch 0,25ml hoc thit b pha long t ng. 7. Ly mu Lp cc thit b |c quy nh trong TCVN 5968: 1995 (ISO 4219) theo nhng yu cu ca TCVN 5968: 1995 (ISO 4219) v mi, yu cu c bit ca kh quyn ni ly mu. t ci lc bi (5.3 ca TCVN 5968) vo gi lc (5.3.2. ca TCVN 5968). Cho vo mt trong nhng bnh hp th (6.l.l) mt l|ng thch hp dung dch hp th (5.2), nh du mc dung dch v ni bnh vo my ly mu. Nu thi gian ly mu l 24 gi th th tch dung dch l 50ml, nu thi gian ly mu l 48 gi th th tch l 150ml.
Ch thch: 1) Nu nhit ca mu khng kh v|t qu 250C hoc nu khng kh rt kh th phi s dng th tch dung dch hp th ln hn. L|ng dung dch chnh xc cn thit hp th |c ton b l|u hunh dioxit c trong mu khng kh |c ly trong nhng khong thi gian ly mu n nh phi |c xc nh bng nhng th nghim tr|c .

2) C th dng thit b t ng thay i cc bnh hp th

Chnh nt iu chnh dng kh (5.6 ca TCVN 5968: 1995 - ISO 4219) |c tc dng khi l 90l/gi. Ghi li s ch trn l|u l|ng k (5.6 ca TCVN 5968), thi gian bt u hot ng ca bm ly mu (5.7 ca TCVN 5968); n cui giai on ly mu, tt bm ly mu, ghi li s ch trn l|u l|ng k v thi gian. Tho bnh hp th ra khi my v cho thm n|c vo cho bng mc ban u. trnh kh nng lm bn nhng phn ht ca mu dng phn tch, phi nt bnh tht cht, hoc nu khng th |c th chuyn dung dch sang mt bnh khc kh v sch v gi n phng th nghim phn tch. Thay th bnh |c ly i bng mt bnh th hai cha dung dch hp th mi v thay ci lc khc. 8. Quy trnh 8.1. Chun b |ng chun 8.1.1. Cc dung dch tiu chun iu ch cc dung dch tiu chun c nng sunfat t|ng ng vi nh|ng nng l|u hunh dioxit l 0,8 - l,6... 8,0 Pg/ml bng cch cho l,00 - 2,00... l0,00ml dung dch sunfat tiu chun (5.8.2) vo mt lot bnh nh mc l00ml, pha long n vch, lc trn u. 8.1.2. Dung dch trng iu ch dung dch trng bng cch trn cn thn 4,0ml n|c, l0ml baripeclorat/dioxan (5.6) v 0,25ml dung dch thorin (5.7), c th dng pipet hoc dng dng c t ng pha long (6.4).

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TCVN 5978: 1995

Cho dung dch thorin ngay tr|c khi o hp th ca dung dch. Ch rng dung dch trng n nh |c 30 pht nu trong ti. 8.1.3. Dy dung dch chun iu ch mt lot cc dung dch chun tr|ng ng vi mi dung dch tiu chun (8.l.l) bng cch trn ln 4,0ml ca mi dung dch vi cng mt l|ng thuc th nh| i vi dung dch trng (8.1.2). o hp th ca cc dung dch chun trong vng l0 pht. 8.1.4. o Kim tra ph quang k theo ch dn ca hng sn xut sau khi n nh, iu chnh v b|c sng 520nm (s iu chnh ph quang k phi |c kim tra th|ng xuyn bng dung dch trng mi pha). thu |c kt qu ng tin cy cn phi thc hin php o t nht 2 n 3 ln i vi mi dung dch. 8.1.4.1. Ph quang k mt chm tia Cho dung dch trng (8.1.2) vo y cuvet (6.3) t cuvet vo dng sng v iu chnh s c v vch 0,800. Thay th dung dch trng bng cc dung dch chun v ln l|t o hp th ca tng dung dch ny. 8.1.4.2. Ph quang k hai chm tia . Cho dung dch trng vo y 2 cuvet, t chng vo dng sng o so snh v iu chnh s chnh lch ca hp th v s 0. Thay th dung dch tr|ng trong cuvet dng sng so snh ln l|t bng cc dung dch chun v o chnh lch hp th ca mi dung dch. 8.1.5. |ng chun Lp |ng chun bng cch v th ca hp th ca dung dch chun (bao gm c dung dch trng nu dng ph quang k mt chm tia) theo nng ca l|u hunh dioxit ca cc dung dch tiu chun (8.l .l) hoc theo chnh lch hp th so vi dung dch trng (ph quang k hai chm tia) (xem hnh t 2 n 5). Phi lp |ng chun mi mi khi pha mi dung dch thorin v dung dch ban nerclorat/dioxan. 8.2. Xc nh nhit ca dung dch hp th cha mu th thu |c theo mc 7 bng nhit ca dung dch thuc th. m bo kt qu, cn phi xc nh nng l|u hunh dioxit trong dung dch mu t nht vi 2 n 3 phn ht. 8.2.1. Phn ht Dng pipet ly 4ml dung dch trong bnh hp th. 8.2.2. Dung dch o Trn phn ht (8.2.l) vi l0ml dung dch baripeclorat/dioxan l5.6) v 0,25ml dung dch thorin (0.7) nh| quy nh trong 8.1.2. 8.2.3. o Cho dung dch cn o (8.2.2) vo y cuvet v o hp th ca dung dch nh| quy nh trong 8.l.4 phi xong trong vng 10 pht. Xc nh nng ca l|u hunh dioxit trong phn ht bng cch so snh vi |ng chun thch hp (8.1.5).

tiu chun vit nam

TCVN 5978: 1995

Nng rt cao ca amoniac v hydrosunfua c th gy cn tr. Amoniac c th lm thay i pH ca dung dch mu ra ngoi gii hn cho php phn tch. Hydrosunfua c th b oxy ha thnh axit sunfuric trong bnh hp th. Nu pH ca dung dch hp th thp hn 3,5 hoc cao hn 9,8 th nng l|u hunh dioxit t|ng ng thu |c s qu cao hoc qu thp, pH ca dung dch hp th em phn tch c th thay i t 3,5 n 9,8 m khng gy nh h|ng. 9. Trnh by kt qu 9.1. Ph|ng php tnh ton Nng l|u hunh ioxit (SO2) trong mu khng kh |c tnh bng microgam trong 1m3 theo cng thc:

U SO2 

f u Ucal u

V1 V2

Trong : f - h s pha long (8.2.3); pcal - nng khi l|ng ca SO tnh bng microgam trong 1ml, xc nh theo V1 - th tch ban u (tnh bng ml) ca dung dch hp th; V2 th tch ca mu khng kh, tnh bng m3. Kt qu l trung bnh ca 2 hay 3 ln xc nh (xem 8.2) .

tiu chun vit nam

TCVN 5978: 1995

9.2. Gii nn pht hin 9.2.1. Dng pM quang k mt chm tia hp th ca dung dch trng ( hp th 0,800) c th xc nh chnh xc n r 0,003, l mc nhiu ca ph quang k. Gii hn pht hin |c quy nh i vi mt tn hiu c c|ng mnh gp 3 ln mc nhiu |ng nn tc l gi tr hp th 0,800 - (3 x 0,003) = 0,791, t|ng ng vi nng SO2 l 0,13Pg/ml. 9.2.2. Dng ph quang k hai chm tia Gii hn pht hin c cng c nh| ca ph quang k mt chm tia, tc l 0,l Pg/ml. 9.3. lp li 9.3.1. Ph quang k mt chm tia lp li |c nh gi bng lch chun (vi s mu n = l0) l nh| sau: - S dng pipet bng tay: r 0,07Pg/ml; - S dng my pha long: r 0,03Pg/ml. 9.3.2. Ph quang k hai chm tia Nhng php o dng cc dung dch kali sunfat trao i cation lm dung dch tiu chun cc nng SO2 t 0,3Pg/ml n 8Pg/ml c lch chun l r 0,06Pg/ml. 10. Bo kt qu Bo co kt qu phi bao gm nhng chi tit sau: a) Ton b cc thng tin nhn bit v mu kh; b) Theo tiu chun ny; c) Tham kho TCVN 5968 (ISO 4219); . d) Kt qu v ph|ng php trnh by kt qu dng; e) Nhng i bt th|ng xy ra trong lc xc nh; f) Nhng thao tc thc hin trong qu trnh xc nh m khng c quy nh trong tiu chun ny hoc c quy nh trong tiu chun tham kho khc, hoc |c coi nh| l t chn.