tcvn

tIu chun vIt nam

TCVN 6626 : 2000 ISo 11969 : 1996

cht lng nc xc nh asen phng php o ph hp th nguyn t (k thut hydrua)

Water quality Determination arsenic Atomic absorption spectrometric method (hydride technique)

H ni -2000

Li ni u
TCVN 6626 : 2000 hon ton tng ng vi ISO 11969 : 1996. TCVN 6626 : 2000 do Ban K thut Tiu chun TCVN/TC 147 Cht lng nc bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc, Cng ngh v Mi trng ban hnh.

TIu chun vIt nam

tcvn 6626 : 2000

Cht lng nc Xc nh asen Phng php o ph hp th nguyn t (k thut hydrua)

Water quality Determination of arsenic Atomic absorption spectrometric method (hydride technique)

Cnh bo Asen v hp cht asen rt c v coi l mt ngun gy ung th trn ngi. Trnh ht phi. Mi phng h c nhn cn lm tt khi tip xc vi asen v hp cht asen.

1 Phm vi p dng
Tiu chun ny qui nh phng php xc nh asen, gm c asen lin kt vi cc hp cht hu c trong nc ung, nc ngm v nc mt nng t 1 g/l n 10 g/l. Nu nng asen ln hn th dng cch pha long mu.

2 Tiu chun trch dn

ISO 5667-1:1980 Cht lng nc Ly mu Phn 1: Hng dn lp chng trnh ly mu.

TCVN 5992:1995 (ISO 5667-2:1991)Cht lng nc Ly mu Hng dn k thut ly mu. TCVN 5993: 1995 (ISO 5667-3:1991) Cht lng nc Ly mu Hng dn bo qun mu.

TCVN 6626: 2000 3 Nguyn tc

Phng php da trn o hp th nguyn t asen c sinh ra do phn hu nhit asen (III) hydrua. Trong iu kin ca phng php ny ch c As (III) c chuyn nh lng thnh hydrua. trnh sai s khi xc nh, mi trng thi oxy ha khc cn chuyn v As (III) trc khi xc nh. As (III) c kh thnh kh asen hidrua AsH 3 bng natri tetrahydroborat trong mi trng axit clohydric. hp th c o bc sng 193,7 nm.

4 Thuc th
Ch dng cc thuc th tinh khit phn tch. Hm lng asen trong cc thuc th v trong nc ct cn phi khng ng k so vi nng thp nht cn xc nh.

4.1 Axit sunfuric (H 2 SO 4 ) , = 1,84 g/ml.

4.2 Axit clohydric (HCl) , = 1,15 g/ml.

4.3 Hydro peroxyt (H 2 O 2 ) , w = 30 % (m/m).

4.4 Natri hydroxyt (NaOH).

4.5 Dung dch natri tetrahydroborat

Ha tan 1 g natri hydroxit NaOH (4.4) trong khong 20 ml nc. Thm 3 g natri tetrahydroborat NaBH 4 . Pha long n 100 ml bng nc. Dung dch ny pha dng trong ngy. Ch thch 1 i vi h dng chy, ngh theo hng dn ca hng sn xut. Dng mt dung dch NaBH 4 0,5
% v NaOH 0,5 % l thch hp. Dung dch ny bn t nht 1 tun l.

4.6 Dung dch kali iodua axit ascobic

Ha tan 3 g kali iodua KI v 5 g L (+) axit ascobic C 6 H 8 O 6 trong 100 ml nc.

TCVN 6626: 2000

Dung dch ny pha dng trong ngy. Ch thch 2 Khng cn dng axit ascobic nu dng dung dch kali iodua KI 20 %.

4.7 Dung dch asen gc , 1000 mg As trong 1 lit.

Cn 1,320 g asen (III) oxyt (As 2 O 3 ) v cho vo bnh nh mc 1000 ml. Thm 2 g natri hydroxit NaOH (4.4) v thm nc n vch. Dung dch ny bn t nht 1 nm. Dung dch asen gc c th mua ngoi th trng. Nu dung dch cha As (V) th phi c x l nh mu nc trong bc kh (8.3.2).

4.8 Dung dch tiu chun asen 1 , 10 mg As/l

Dng pipet ht 10 ml dung dch asen gc (4.7) cho vo bnh nh mc 1000 ml. Thm 20 ml axit clohydric HCl (4.2) v pha long bng nc n vch mc. Dung dch bn khong 1 thng. Nu dung dch gc l asen (V) th cn kh n asen (III) theo 8.3.2 trc khi pha long thnh 1000 ml.

4.9 Dung dch tiu chun asen 2, 0,1 mg As/l

Dng pipet ht 10 ml dung dch tiu chun asen 1 (4.8) cho vo bnh nh mc 1000 ml. Thm 20 ml axit clohyric HCl (4.2) v pha long bng nc n vch mc. Chun b dung dch dng trong ngy.

5 Thit b, dng c
Cc thit b, dng c thng thng trong phng th nghim v:

5.1

My o ph hp th nguyn t , ph hp vi h hydrua v c ngun sng xc nh asen,

th d n phng in hoc n catot rng vi thit b hiu chnh ng nn nu cn.

5.2 Cp kh , argon hoc nit.

TCVN 6626: 2000

5.3 Dng c thy tinh , cn c ra ngay trc khi dng bng axit nitric long [10 % (V/V)], m,

v trng bng nc.

6 Ly mu
Ly mu theo ISO 5667-1 v TCVN 5992: 1995 (ISO 5667-2) Ly mu vo bnh polyetylen hay thy tinh bosilicat ra trc bng axit nitric HNO 3 [th d 10 % (V/V)] v trng bng nc. Thm ngay 20 ml axit clohydric (4.2) vo 1000 ml mu nc. Nu pH ca mu vn ln hn 2 th thm axit clohyric na cho ti khi pH < 2. Lu gi mu theo TCVN 5993: 1995 (ISO 5667-3).

7 Cn tr
Hu ht cc cht hu c cn tr vic xc nh asen. Chng c loi tr trc khi phn tch bng cch phn hy mu theo 8.3.1. Nhng mu to bt, khi thm tetrahydroborat cn c x l trc (th d thm cht chng bt hoc bng cch phn hu hon ton). Khi thm cht chng bt th cn th c vo mu trng v cc dung dch hiu chun. Ph lc A cho chi tit v cc cht cn tr khi xc nh asen. Cc kt qu nhn c t phng th nghim Anh. Trong cc cht th ch c ng khi ln hn 2,0 mg/l, antimon ln hn 0,2 mg/l, selen ln hn 0,05 mg/l v nitrat ln hn 100 mg/l cn tr vic xc nh asen nng 1,0 g/l. Cc kim loi qu nh platin v paladi c th lm gim tn hiu ca asen (III) hydrua A s H 3 .

8 Cch tin hnh

8.1 Mu trng
Dng pipet ly 2 ml axit clohydric (4.2) vo bnh nh mc 100 ml ri pha nc n vch. X l mu trng ging nh mu tht.

8.2 Dung dch hiu chun

Chun b t nht 5 dung dch hiu chun t dung dch asen tiu chun 2 (4.9) v c nng tng ng vi khong d kin lm vic.

TCVN 6626: 2000

Th d cho khong 1 g/l n 10 g/l th dng pipet ht 1 ml, 3 ml, 5 ml, 8 ml v 10 ml dung dch tiu chun 2 vo mt dy bnh nh mc 100 ml. Thm vo mi bnh 2 ml axit clohydric (4.2) v thm nc n vch. Cc dung dch ny c nng 1 g/l, 3 g/l, 5 g/l, 8 g/l v 10 g/l. Chun b cc dung dch hiu chun khi dng n. X l cc dung dch hiu chun ging nh mu nc.

8.3 X l trc
Hu ht cc hp cht hu c lin kt vi asen c phn hy bng ph mu theo 8.3.1. Nu bit trc mu khng cha cc hp cht nh vy th ph mu nh 8.3.1 c th b qua v lm tip 8.3.2. Ly 50 ml mu (xem iu 6) vo bnh cu y trn (hnh 1).

8.3.1 Cch phn hy mu

Cnh bo Khi bc ln t axit sunfuric m c (H 2 SO 4 ) b un nng gy kch thch, bi vy cn lm vic ny trong t ht. Thm 5 ml axit sunfuric (4.1) v 5 ml hydro peroxit H2O2 (4.3) vo bnh cu trn y (xem 8.3). Thm vi ht bt v ni bnh vo my nh ch trn hnh 1. un n si v thu phn hng c vo bnh hng. Tip tc un cho n khi khi ca axit sunfuric xut hin. Quan st mu. Nu mu c v khng mu th thm 5 ml hydro peroxit H 2 O 2 (4.3) na v tip tc un nh trc. Khi mu khng mu v khng c th ngui bnh, phn hng c vo bnh cu y trn v lm tip nh 8.3.2. Cn thn khng mu b cn kh.

8.3.2 Kh As (V) n As (III)

Thm 20 ml axit clohydric (4.2) v 4 ml dung dch kali iodua (KI) - axit ascobic (4.6) vo bnh cu y trn cha mu ph (8.3.1) hoc mu khng ph (8.3). un nng nh 50 o C trong 15 min. ngui dung dch v chuyn hon ton vo bnh nh mc 100 ml. Thm nc n vch.

8.4 Hiu chun v xc nh

Ty theo h thng hydrua c dng, th tch c th ly ln hn hay nh hn th tch m t di y. Tuy nhin cn gi t l nh.

TCVN 6626: 2000

t mi thng s my o ph hp th nguyn t (5.1) theo hng dn ca hng sn xut ( di sng 193,7 nm) v t cuvet v tr thch hp nht thu c chm sng truyn qua cc i. Cho mt dng argon hoc nit (5.2) qua h thng v t im "khng" cho my. o hp th ca cc dung dch theo th t sau: dung dch mu trng; dung dch hiu chun; mu, chun b nh sau

Chuyn mt th tch mu thch hp (xem 8.3.2) vo bnh phn ng. Ni bnh phn ng vi h thng hydrua. Cho argon hoc nit qua dung dch cho n khi hp th ch trn my o ph hp th nguyn t tr v khng. Vi 20 ml dung dch mu (8.3.2) th thm 5 ml + 0,1 ml dung dch natri tetrahydroborat (4.5) v ghi tn hiu. Lp li vi mi dung dch. Dng kt qu trung bnh. Thit lp ng chun bng cc gi tr trung bnh ca mu trng v dung dch hiu chun. Ch thch
3 4 Cn thnh thong kim tra li ng chun. Vi cc mu l, nn thm mt th tch bit asen vo t nht mt mu xem tin cy ca phng php.

9 Tnh kt qu dng ng chun

Tnh nng asen trong mu bng cch da vo ng chun (8.4). Mi s pha long u cn tnh n.

10 Biu th kt qu
Kt qu tnh bng microgam trn lit vi 2 s c ngha v mt s l sau du phy.

TCVN 6626: 2000 11 chnh xc

Mt php th lin phng th nghim tin hnh nm 1982 bng phng php c cng nguyn tc, da trn mu nc ung c b sung bng nc bit nng asen, kt qu cho trong ph lc B.

12 Bo co kt qu
Bo co kt qu cn c nhng thng tin sau a) trch dn tiu chun ny;

b) nhn dng mu; c) d) biu th kt qu nh ch ra iu 10; mi chi tit khng nm trong tiu chun ny v cc yu t c th nh hng n kt qu.

Hnh 1 Th d v thit b phn hy mu

TCVN 6626: 2000 Ph lc A (tham kho) nh hng ca cc cht khc n s xc nh asen

Cht khc

Cht thm vo

Nng cht khc mg/l

nh hng ca cht khc(g/l) n s xc nh asen nng 0,0 g/l 1,0 g/l + 0,06 0,00 + 0,12 0,00 + 0,02 0,03 + 0,03 0,01 0,04 0,06 0,06 0,15 0,19 0,00 0,00 + 0,13 + 0,09 0,30 0,00 0,04 + 0,04 0,02 0,03 0,03 0,00 0,00 0,00 0,10 0,05 0,04 0,12 0,23 0,26

Bc Nhm Cadmi Crm ng ng ng ng ng ng St Thy ngn Mangan Niken Niken Niken Niken Ch Antimon Antimon Antimon Antimon

Ag + Al 3+ Cd 2+ Cr 3+ Cu 2+ Cu 2+ Cu 2+ Cu 2+ Cu 2+ Cu 2+ Fe 3+ Hg 2+ Mn 2+ Ni 2+ Ni 2+ Ni 2+ Ni 2+ Pb 2+ Sb 5+ Sb 5+ Sb 5+ Sb 5+

Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Perclorat Clorua Clorua Clorua Clorua

10,0 10,0 10,0 10,0 0,5 1,0 2,0 5,0 10,0 20,0 10,0 10,0 10,0 0,5 1,0 2,0 10,0 10,0 0,2 0,5 1,0 2,0

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TCVN 6626: 2000

Cht thm vo Sb 5+ Sb 5+ Se 4+ Se 4+ Se 4+ Se 4+ Se 4+ Se 4+ Sn 4+ Sn 4+ Sn 4+ Sn 4+ Sn 4+ Zn 2+ Clorua Clorua Nitrat Nitrat Nitrat Nitrat Nitrat Nitrat Clorua Clorua Clorua Clorua Clorua Clorua Axit nitric Axit nitric Axit nitric Axit nitric Axit percloric Kali dihydro Axit sunfuric Nng cht khc mg/l 5,0 10,0 0,01 0,02 0,05 0,1 0,2 0,5 0,5 1,0 2,0 5,0 10,0 10,0 10,0 50,0 100,0 250,0 10,0 10,0 250,0 0,00 + 0,09 0,00 + 0,04 + 0,09 + 0,04 0,00 + 0,24 nh hng ca cht (g/l) n s xc nh asen nng 0,0 g/l 1,0 g/l 0,28 0,57 + 0,03 + 0,01 0,07 0,28 0,42 0,81 0,00 0,05 0,04 0,05 0,08 + 0,01 0,04 0,00 0,09 0,21 0,07 + 0,02 + 0,01

Cht khc Antimon Antimon Selen Selen Selen Selen Selen Selen Thic Thic Thic Thic Thic Km Nitrat Nitrat Nitrat Nitrat Perclorat Phosphat Sunfat

NO -3 NO -3 NO -3 NO -3 ClO -4 PO 34 SO 24

1) Nu cc cht khc khng gy nh hng, hiu ng s l 0,00 g/l + 0,02 g/l v 0,00 g/l + 0,08 g/l nng asen tng ng l 0,0 g/l v 1,0 g/l.

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TCVN 6626: 2000 Ph lc B (tham kho) D liu v chnh xc

Mu

na
%

x
g/l 1,40 4,38 7,99

x theor
g/l 1,30 4,00 7,50 RR

RR % 108 109 107 tm thy

sr
g/l 0,084 0,172 0,572

VC r % 6,0 3,9 7,1

sR
g/l 0,268 0,509 0,919

VC R % 19 12 12

1 2 3

60 60 60

1 1

2 2 0

n o na

l gi tr o dng c l gi tr o loi b l phn trm loi b l gi tr trung bnh l gi tr l thuyt

sr
VC r

l lch chun lp li l h s lch lp li l lch chun ti lp l h s lch ti lp

x
x theor

sR
VC R

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