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TCVN 6002 : 1995

ISO 6333: 1986

Cht l|ng n|c - Xc nh mangan Ph|ng php trc quang dng fomaldoxim
Water quality - Determination of manganese - Formaldoxime spectrometric method
M u Khi n|c c cha oxi, hu ht mangan tn ti d|i cc dng khng tan, th|ng lin kt vi cc vi sinh vt v to phc, th d vi axit humic. Nu n|c khng cha oxi hoc c mi tr|ng axit mnh, tt c mangan tn ti dng ha tan. Phm vi p dng Tiu chun ny |a ra ph|ng php trc quang dng fomaldoxim xc nh tng l|ng mangan (gm mangan ha tan, huyn ph v mangan lin kt vi cc cht hu c) trong n|c mt v n|c ung. Ph|ng php ny dng xc nh mangan trong khong nng t 0,01mg/l n 5mg/l. Nhng nng mangan ln hn 5mg/l cng c th xc nh |c sau khi pha long mu thch hp. Cc yu t cn tr |c nu mc 8.
Ch thch: Ph|ng php ny khng p dng cho cc loi n|c b nhim cao nh| n|c thi cng nghip.

1.

Nguyn tc Thm dung dch fomaldoxim vo mu th v o qang phc mu da cam b|c sng khong 450nm. Nu mangan tn ti d|i dng huyn ph hoc lin kt vi cc hp cht hu c, cn phi x l tr|c chuyn mangan thnh dng phn ng |c vi fomaldoxim. Phc cht mangan foinaldoxim bn pH gia 9,5 v l0,5 v c|ng mu t l vi l|ng mangan c trong dung dch. Quan h tuyn tnh gia nng hp th t ti nng mangan 5 mg/l. Hp th cc i khong 450mn (h s hp th mol l 11 x 103 l/mol.cm). 3. Thuc th Cnh bo - Cc thuc th nu 3.4, 3.5.l v 3.5.3. l nhng cht c hi c bit. Phi lm vic vi cc cht ny trong t ht rrnh n hoc ht phi hi ca chng v phi bo v mt, mt v tay cn thn. Phi dng gng tay v knh cc cht ny bm vo da, phi ra ngay v ra k. Ht phi hi fomaldehyt v fomaldoxim s gy kch thch mnh v ph n phn trn ca b my h hp. Trong phn tch, ch dng cc thuc th tinh khit phn tch, n|c qua trao i ion hoc n|c ct bng thit b thy tinh m l|ng vt mangan cng thp cng tt. 3.1. Cht oxi ha Dng kali pesunfat (K2S2O8) hoc natn pesunfat (Na2S208) 3.2. Natri sunfit khan (Na2SO3) 3.3. Dung dch EDTA 0,24 mol/l, dng mui tetranatri

2.

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TCVN 6002 : 1995

Ha tan 90g dinatri EDTA dihidrat (Na2EDTA.2H2O) v 19 g natri hidroxit (NaOH) trong n|c v pha long thnh 1000ml. Cch khc l ha tan l09g tetranatri EDTA tetrahidrat (Na4EDTA.4H2O) hoc tetra natn (C10H12N2NNa4O8.2H2O) trong n|c v pha long n 1000ml. 3.4. Dung dch fomaldoxim Ha tan 10g hidroxylamoni clorua (NH3OHCL) trong khong 50ml n|c. Thm 5ml dung dch metanal 35% (khi l|ng/khi l|ng) (HCHO) (fomandehyd) (d-1,08 g/ml) v pha long bng n|c n l00ml. Gi dung dch trong bnh ni ti v mt. Dung dch bn t nht mt thng. 3.5. Dung dch hidroxylamoni clorua/amoniac 3.5.1. Dung dch hidroxylamoni clorua (NH3oHc/), 6mol/l Ha tan 42g hidroxylamoni clorua trong n|c v pha long thnh l00ml. 3.5.2. Dung dch amoniac (NH3) 4,7 mol/l. Dng n|c pha long 70ml amoniac c (d = 0,91 g/ml) thnh 200ml. 3.5.3. Pha ch Trn hai th tch bng nhau ca (dung tch amoniac (3.5.2) v dung dch hidroxylamoni clorua (3.5.l). 3.6. Dung dch amoni st (II) sunfat hexahidrat [(NH4)2Fe (SO4).6H2O700 mg/l. 3.6.1. Axit sunfuric (H2SO4 3 mol/l. Thm t t 170ml axit sunfuric c (d = 1,84 g/ml) vo 750ml n|c. ngui ri pha long thnh l000ml. Dung dch ny c bn sn (H2SO4 d = l,19 g/ml). 3.6.2. Pha ch Ha ta 700mg amoni st (II) sunfat hexahidrat trong n|c, thm 1ml axit sunfric (3.6. l) v pha long thnh 1000ml: 3.7. Dung dch natri hidroxit (NaOH) - 4mol/l Ha tan 160g natri hidroxit trong n|c v pha lon thnh l000ml. 3.8. Dung dch chun mangan, t|ng |ng vi 100mg Mn/l. Ha tan 308mg mangan sunfat monohidrat (MnSO4.H2O) vo n|c trong bnh nh mc dung tch 1000ml. Thm l0ml axit sunfuric (3.6.1) ri nh mc bng n|c v lc u lml ca dung dch chun ny cha 0,lmg Mn. C th dng dung dch chun c bn sn. 4. Thit b, dng c Thit b thng th|ng trong phng th nghim, v cc thit b sau: 4.1. My trc quang, c b lc bin i lin tc (dng lng knh hoc cch t) hoc gin on (dng lc sng gii hp) o |c hp th khong 450nm, |c trang b cc cu-vt c chiu di truyn quang n l00mm ( o cc nng mangan nh hn 0,3 mg/l) v l0mm ( o cc nng mangan trn 0,3 mg/l). 4.2. Bnh thy tinh, dung tch l00ml, nt nhm c kp kim loi hoc nt vn bng cht do khng mu, thch hp cho quy trnh hp (autoclave). 4.3. Ni hp hoc ni p lc, c kh nng duy tr nhit 1200C v p lc 200kPa.

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TCVN 6002 : 1995

Ch thch: Mi dng c thy tinh, bnh ly mu cn |c ra bng axit clohidric khong 1 mol/l (HCb v dng n|c trng sch tr|c khi dng.

5.

Ly mu v mu Cnh bo - Cn ht sc cn thn khi axit ha mu, phng c th c kh c bay ra. Ly mu vo bnh polyetylen, polyvinyl clorua hoc thy tinh v axtt ha mu bng axit sunfuric (3.6.1) n pH khong 1, nh|ng khng nh hn l. Vic axit ha nhm gim s hp ph mangan ln thnh bnh ng thi to iu kin ha tan cc dng keo v kt ta ca mangan. 6. Cch tin hnh 6.1. Phn mu th Phn mu th l 50ml mu axit ha, cha t hn 0,25mg mangan (5 mg/l), hoc mt th tch mu nh hn v |c pha long thnh 50ml. 6.2. Chun b dung dch th Nu mangan tn ti dng huyn ph hoc lin kt vi cht hu c, thm 225 H 25mg cht oxi ha (3.1) vo phn mu th (6.1). Oxi ha c th thc hin bng mt trong hai cch: a) Hp hn hp ng trong bmh (4.2) trong 30 pht, ngui v thm khong 0,5g natri sunfit (3.2) kh cht oxi ha d|; b) un si hn hp trong bnh nn hoc cc dung tch l00ml khong 40 pht; ngui v chuyn hn hp vo blnh nh mc 50ml, thm n|c n vch v thm khong 0,5g natri sunfit (3.2) kh cht oxi ha d|. Nn hp nu mu cha axit humic. Nu khng th tin hnh phn tch nguy, mu va chun b c th qua m.
Ch thch: Mu v vn c b ph hy hon ton trong giai on x l tr|c. Nu thc t cho thy giai on x l tr|c l khng cn thit, nh| a s tr|ng hp mu n|c ung, th c th b qua.

6.3.

Mu trng Lm mt mu trng song song vi mu tht bng cch thay phn mu th bng 50ml n|c ct. Nu hp th ca mu trng khc nhiu so vi hp th ngoi suy ca thnh phn "khng" (6.4.4) th cn phi xem xt li l do ca s khc nhau . 6.4. Chun ha 6.4.1. Chun dy dung dch chun Dy A: 0 n 0,50 mg/l mangan. Pha long 20 H 0,2ml dung dch mangan tiu chun (3.8) thnh l000ml bng n|c trong bnh nh mc dung tch 1000ml. Ly 0; l0; 20; 30 v 40ml dung dch mangan va pha long vo 5 bnh nh mc dung tch 50ml ri thm n|c n vch. |c dy dung dch chun 0; 0,l; 0,2; 0,3 v 0,4 mg/l mangan. Dy B: 0 n 5 mg/l mangan. Pha long 200 H 2ml dung dch mangan tiu chun (3.8) thnh l000ml bng n|c trong bnh mc dung tch l000ml. Ly 0, l0, 20, 30 v 40ml dung dch va pha long vo 5 bnh nh mc dung tch 50m.l ri thm n|c n vch. |c dy dung dch chun 0, 1, 2, 3 v 4 mg/l mangan.

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6.4.2. Hin mu

TCVN 6002 : 1995

Thm 1ml dung dch amoni st (II) sunfat (3.6) v 2ml dung dch EDTA (3.8) vo tng dung dch chun va pha trn. Sau khi lc u, thm lml dung dch fomaldoxim (3.4) v lp tc thm 2ml dung dch natri hidroxit (3/7). Lc k cc dung dch v yn 5 n l0 pht, sau va lc thm 3ml dung dch hidroxylamoric clorua/amoniac (3.5) ri yn t nht l gi. 6.4.3. o quang Trong khong l n 4 gi sau khi hin mu, o hp th ca cc dung dch bng my trc quang 450nm, dng n|c lm so snh. Vi cc dung dch dy A dng cuvt l00mm (0 n 0,5 mg/l mangan), vi cc dung dch dy B dng cuvt l0mm (0 n 5 mg/l mangan). 6.4.4. V |ng chun Mi dy dung dch chun mt |ng chun, nng mangan tnh bng mg/l t trn trc honh, hp th t|ng ng t trn trc tung. |ng chun cn phi thng. H s chun ha l nghch o dc ca |ng chun. im |ng chun ct trc tung cho bit gi tr hp th ngoi suy ca thnh phn "khng" ca dy cc dung dch cn chun ha. H s chun ha cng c th |c tnh ton bng gii tch chui. 6.4.5. Kim tra |ng chun bo m lp li tt cn nh k kim tra |ng chun, nht l khi dng cc thuc th mi pha. 6.5. Xc nh 6.5.1. Hin mu Thc hin nh| mc 6.4.2 nh|ng dng phn mu th (6.2) thay v dng cc dung dch chun. Nu mu th |c x l tr|c (xem 6.2), tng l|ng natri hidroxit (3.7) t 2ml ln 2,5ml. 6.5.2. o quang Xem 6.4.3. 7. Tnh ton kt qu 7.1. Tnh ton Nng mangan, CMn tnh bng mg/l, |c tnh theo cng thc: CMn = f(A1 A0)g Trong : f l h s chun ha t|ng ng vi |ng chun chn v |c tnh nh| nu mc 6.4.4, mg/l; A1 l hp th ca dung dch mu cn phn tch (6.5.2); A0 l hp th ngoi suy ca thnh phn khng (6.4.4); g l mt h s |c tnh theo cng thc:

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V V

TCVN 6002 : 1995

g 

1 2

V1 l th tch ca phn mu th, ml ( y l 50ml); V2 l th tch phn mu ht ra, ri pha long thnh 50ml nu c.
Ch thch: Th tch axit thm vo mu (mc 5) cn |a vo tnh ton.

Bo kt qu: a) Nng mangan t 0,01 n l mg/l, ghi kt qu chnh xc n 0,01 mg/l. b) Nng mangan ln hn l mg/l, ghi kt qu chnh xc n 0,1 'mg/l. 7.2. chnh xc Xem bng. 8. Cc yu t cn tr 8.1. Ion st (II) to phc mu tm vi fomaldoxim v cn tr vic xc nh mangan. Thm EDTA (3.3) v hidroxylamoni clorua/amoiac (3.5) lm gim cn tr ny. Tuy nhin, cch tt nht loi tr nh h|ng ny l thm mt l|ng chnh xc, nh| nhau ion st (II) (dng amoni st (II) sunfat) vo cc dung dch chun, mu trng v mu th. Coban nng l mg/l gy kt qu t|ng |ng vi 402g Mn/l. Nng ion phophat trn 2 mg/l (tnh theo P) lm thp kt qu nu dung dch cha canxi. 8.4. Canxi v magie c mt ng thi vi tng nng trn 300 mg/l lm cao kt qu. 8.5. Nu dung dch b c sau khi .to thnh phc mu, c th li tm tr|c khi o quang (6.4.3). 9. Bo co kt qu Bo co kt qu gm nhng thng tin sau: a) Trch dn tiu chun ny; b) M t mu; c) Ph|ng php s dng; d) Ph|ng php v kt qu tr nh h|ng cn tr; e) Nhng hin t|ng bt th|ng trong qu trnh xc nh; f) Nhng thao tc khng c trong tiu chun ny, hoc |c xem nh| t chn. 8.2. 8.3.

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TCVN 6002 : 1995

Bng 1- lp li ca ph|ng php (S liu ly t kt qu lin quan phng th nghim, 1982) Nng mangan (mg/l)
0,050 0,100 0,100 0,500 1,000 1,000 2,000 2,000 4,000 4,000

Phng th nghim
B A B B A B A B A B

S cc kt qu
30 30 30 30 30 30 30 30 30 360

Gi tr trung bnh (mg/l)

0,049 0,12 0,099 0,497 1,01 1,001 1,99 2,055 4,02 4,198

lch chun (mg/l)

0,0035 0,025 0,0021 0,0085 0,04 0,0091 0,035 0,0111 0,047 0,1333