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TCVN 5293 : 1995

Cht lng khng kh - Phng php Indophenol xc nh hm lng amoniac


Air quality - Indophenol method for determination of ammoniac content
1. Phm vi p dng Tiu chun ny trnh by phng php so mu xc nh amoniac trong khng kh theo phn ng indophenol. 2. Bn cht ca phng php 2.1. Phng php c s dng xc nh hm lng amoniac trong khng kh tng ln v trung bnh ngy m trong khong t 0,1 n 1,0 mg/m3. 2.2. Phng php da trn c s tc dng ca amoniac vi hipoclorit v phenol c s tham gia ca cht n nh phn ng l natri nitropruxit. Tnh cht l ho ca amoniac c nu trong ph lc 1. 2.3. Cng nhum mu xanh ca dung dch indophenol ph thuc vo hm lng amoniac; 2.4. Cc amin thm v focmandehit gy cn tr trong vic xc nh nng amoniac. 3. Dng c v ho cht 3.1. Dng c a. My ht kh c lu lng k c vch chia n 0,005 lt/ pht; nhit k; p k v m k; b. Dng c hp th Ricte (xem ph lc 2) c vch o 6ml hoc dung dch hp th khc; c. Quang ph k hoc my so mu quang in vi knh lc c truyn quang ln nht bc sng 625 nm v cuvet c b dy 10 mm. d. ng nghim c nt mi dung dch 10ml; e. Phu Bucne. 3.2. Ho cht v Thuc th 3.2.1. Phi s dng cc ho cht loi "tinh khit ho hc" (TKHH) hoc tinh khit phn tch (TKPT). 3.2.2. tin hnh s dng cc thuc th sau: a. Natri hydroxit (NaOH) b. Kali iodua (Kl) dung dch 10%; c. Amoni clorua (NH4Cl); d. Natri cacbonat Na2CO3; e. axit sunfuric H2SO4 d = 1,18, dung dch 10% (theo th tch); f. Natri clorua (NaCl); g. axit salixilic [OH(C6H4)COOH]; h, Natri thiosunfat (Na2S2O3) 5H2O dung dch 0,05 mol/l;

i. axit oxalic (H2C2O4); j. Phenol (C6H5OH); k. Clorua vi (CaOCl2) l. Nc ct 2 ln, c ct vi axit sunfuric (0,5 ml axit sunfuric d = 1,8 trong 1 lt nc ct) hay nc kh ion hon ton. chun b dung dch v tin hnh phn tch s dng nc kh amoniac; 3.3. Chun b ho cht th a/ Dung dch hp th: Pha long 0,5ml axit sunfuric d = 1,84 trong 1 lt nc. Bo qun dung dch trong bnh hnh ng, c y kn bng nt c ng thu tinh cha y tinh th axit oxalic; b/ Thuc th phenol: Ha tan 5g phenol mi chng ct, 25mg natri nitropruxit trong 100ml nc. Bo qun thuc th khng qu 6 thng nhit 40C. c/ H tinh bt dung dch 0,5%. Trn u 0,25g tinh bt vi 10ml nc, cho thm 40ml nc nng 60 -700C un n si, dung dch sau 1 pht th lm lnh. d/ Thuc th hipoclorit: ho tan 10g natri hydroxit v 11,7g natriclorua trong 100ml nc bo ho clo (vi nng t 0,6 - 0,8 clo). Thuc th c bo qun khng qu 6 thng. Thuc th c th chun b t clorua vi : nghin nh 5g clorua vi cng vi 100ml nc. Dung dch c lc trong chn khng, ra cn bng nc. Gp dung dch lc vi nc ra cn, ri thm nc n th tch 1 lt. Tin hnh xc nh hm lng clo hot tnh trong hipoclorit nh sau: chuyn 20 m dung dch trong sut vo bnh cu c nt mi, sau cho thm 10ml dung dch axit sunfuric 10% v 10ml dung dch kali iodua 10%. y kn bnh cu v trong bng ti khong 10 pht. Sau chun iot bng dung dch natri thiosunfat 0,05mol/l n mu vng nht. Thm mt vi git h tinh bt chun tip bng natri thiosunfat cho n khi dung dch mt mu, 1ml dung dch natri thiosunfat 0,05mol/l tng ng vi 0,00354g clo. Thuc th phi cha t 0,6 - 0,8 g clo trong 100ml. Khi hm lng clo khng chun dung dch cn ly tng lng clorua vi ln hn (hoc lm bo ho nc bng clo); e/ Dung dch amoniac chun ban u c hm lng 100 g amoniac trong 1ml; ho tan 0,3141g NH4cht lng trong 1dm3 nc. Bo qun dung dch khng qa 2 thng. f/ Dung dch amoniac chun cng tc o hm lng 1 g amoniac trong 1ml; dung dch ny c chun b bng cch dng dung dch hp th pha long 100 ln dung dch chun ban u. Dung dch ny ch pha trc khi s dng. 4. Ly mu 4.1. xc nh hm lng tng ln amoniac, cho khng kh cn nghin cu i qua hai ng hp th mc ni tip vi nhau, mi ng c cha 5ml dung dch hp th vi lu lng 0,5lt/ pht lin tc trong thi gian t 10 n 30 pht.

4.2. xc nh hm lng amoniac trung bnh ngy m c th ly theo 2 cch: a. Ly mu nh 4.1 vi s ln khng t hn 6, cch u nhau trong mt ngy m; b. Cho khng kh cn nghin cu i qua dung dch hp th c cha 50ml dung dch hp th vi lu lng 0,2 lt/ pht lin tc trong 24 gi. Phi theo di trong qu trnh ly mu, nu dung dch b cn th cn b sung nc ct. 5. Tin hnh phn tch 5.1. Dng nc ct 2 ln a mc dung dch trong thit b hp th n 10ml; 5.2. Ht ng 2ml dung dch mu th, chuyn vo ng nghim c nt mi, thm 3ml dung dch hp th, 1ml thuc th phenol. Nu s lng mu nhiu hn 1 mu, thi gian cho cc thuc th vo tng mu khong 1 pht. Sau va lc cn thn ng nghim va cho thm 0,5ml thuc th hipoclorit. Khi nng amoniac ln, cho php ly lng dung dch mu th t hn. 5.3. Sau 2h tin hnh o mt o quang ca dung dch vi cuvt c dy 10mm bc sng 625nh my so vi nc. Thi gian cho thuc th cui cng n lc o mt quang ca dung dch i vi tt c cc mu phi nh nhau. 5.4. Chun b ng thi "mu trng" cng t dung dch hp th rt vo thit b hp th. 5.5. o mt quang ca 5ml dung dch hp th c iu ch thnh "mu trng". Gi tr mt quang ca "mu trng" khng c vt qu 0,02. Trong trng hp ngc li, cn kim tra sch ca nc, dng c cuvt v cht lng cc dung dch. 5.6. Lng amoniac trong mu th c xc nh bng ng chun theo hiu s gia gi tr mt quang ca mu em phn tch v mt quang ca "mu trng". 6. Lp ng chun 6.1. lp ng chun cn chun b mt dy dung dch chun trong bnh nh mc dung tch 50ml theo bng sau: Tn dung dch Chun cng tc, ml Hp th, ml Hm lng NH3 tng ng trong 5ml dung dch mu th, mg 1 0,1 S hiu ca dung dch chun 2 4 6 8 n 50ml trong mi bnh 0,2 0,4 0,6 0,8 10 1,0

6.2. chun b thang chia dung dch chun ly 5ml dung dch t mi bnh chuyn vo ng nghim v tin hnh nh ch ra mc 5.

6.3. ng chun ca mi lin h gia gi tr mt quang vi lng amoniac c lp da trn c s cc gi tr trung bnh tnh ton t kt qu o ca 3 hay 5 ln. 7. X l kt qu Hm lng amoniac (C) trong khng kh cn nghin cu, c tnh bng mg/m3, theo cng thc:
C=

Trong : a - lng amoniac trong dung dch mu ly phn tch, mg; B - tng th dung dch mu th, ml; Ba - th tch dung dch mu th ly phn tch, ml; Vo - th tch mu khng kh c a v iu kin chun, m3; Khi xc nh nng trung bnh ngy m, th tch khng kh khng cn a v iu kin chun. Ph lc A Tnh cht l ho ca amoniac Cht kh khng mu c mi kh chu, ngng gh tip nhn mi l 37mg/m3. T trng so vi khng kh l 0,59. nhit -33,40C amoniac b ho lng v nhit -77,80C ng c thnh mt khi tinh th khng mu. Amoniac d ho tan trong nc, ru. Dung dch nc bo ho amoniac c t trng 0,908 cha 25,65% amoniac theo khi lng. Trong 100ml ru 200C ho tan c 13,2% amoniac (theo th tch). Ph lc B Dng c hp th Ricte (kiu trung bnh)

a.B Ba .Vo

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