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Lấy Mẫu Và Quản Lý Mẫu Phân Tích
Lấy Mẫu Và Quản Lý Mẫu Phân Tích
Lấy Mẫu Và Quản Lý Mẫu Phân Tích
Cht phn tch Vt liu lm bnh cha Cht bo v/iu kin Thi gian bo qun ti
bo qun a
Cl-, SO42- P, G Khng 30 ngy
CN- P, G 0.06g ascorbic acid/L 15 ngy
4 oC
Nitrite P, G 4 oC 48 gi
SO32- P, G 4 oC 28 ngy
H+ (pH) P, G Bnh thng 24 gi
Kim loi (II, III) P, G HNO3, pH<2 3 thng
Hg P, G HNO3, pH<2 20 ngy
Cr(VI) P, G 4 oC 24 gi
Kim loi kim P, G HNO3, pH<2 36 thng
H acronitril G, PTFE 0.008% Na2S2O3, pH 14 ngy
4-5, 4 oC
H benzidines G, PTFE 0.008% Na2S2O3, 4 oC 7 ngy
H clor hu c G, PTFE 0.008% Na2S2O3, 4 oC 7 ngy
H dioxim G, PTFE 0.008% Na2S2O3, 4 oC 45 ngy
Halo ether G, PTFE 0.008% Na2S2O3, 4 oC 40 ngy
Nitro-aromatic G, PTFE 0.008% Na2S2O3, 4 oC 40 ngy
Du, m G 0.008% Na2S2O3, 4 oC 28 ngy
Thuc tr su hu c G 5 mL HCl, 4 oC 28 ngy
v phosphor hu c
H PCBs v phthalates G, PTFE 4 oC 40 ngy
ethers
Chlor hu c G, PTFE H2SO4, pH < 2, 4 oC 28 ngy
Radiological test G, PTFE HNO3, pH < 2, normal 6 thng
ng thi theo cc khi nim nu trn, cng tc ly mu phn tch phi bao gm cc vn
sau y, bt u t lc chun b i ly mu cho n khi thu c mu em v v bo qun
chng.
- QA/QC i vi tt c ngi thc hin ly mu
- QA7QC trong k hoch ly mu
- QA/QC i vi cc phng php, trang b v dng c ly mu
- QA/QC i vi ha cht phc v ly mu
- QA/QC i vi cc loi dng c ng, cha v bao gi mu
- QA/QC i vi cc hot ng ly mu, ghi chp h s ly mu
- QA/QC i vi cng tc chuyn ch mu v phng th nghim
- QA/QC i vi cng tc bo qun v lu gi mu sau khi ly c
Lm tt tt c cc vn ny tc l chng ta ly c mu phn tch tha mn c tt c cc
yu cu ca ly mu. Ngha l trong mi hot ng ca cng tc ly mu phn tch t lc bt u
chun b n lc ly c mu mang v v bo qun chng, hay phn tch ngay ti hin trng khi
cn thit. Ton b mi quan h ca cc cng vic ny c th m phng theo s hnh sau:
Bng XX: cc phng php tiu chun ly mu phn tch
Xc nh mc tiu ly mu
Lp chng trnh ly mu
Bo qun v vn chuyn
v kho hay PTN
X l mu v phn tch
Nhn xt v nh gi
Chng II. CC K THUT X L MU PHN TCH
2.1. Yu cu chung ca k thut x l mu
2.1.1. Yu cu chung ca k thut x l mu phn tch
X l mu l giai on u tin nhng rt quan trng ca qu trnh phn tch. Mi sai st
trong giai on ny u l nguyn nhn to ra sai s cho kt qu phn tch, c khi sai s rt ln.V
th mi cch x l mu phn tch, cng vi vic tun th theo QA/QC, cn phi bo m c
cc yu cu c th sau:
- Ly c hon ton, khng lm mt cht phn tch
+ Khng lm nhim bn thm cht phn tch vo mu t bt k ngun no
+ Kt qu x l phi ph hp vi phng php phn tch chn
- Dng cc ha cht phi m bo sch ng yu cu, mc ch v mc phn tch
- Khng a thm cc cht c nh hng vo mu
- C th tch hay lm giu c cht phn tch cng tt
2.1.2. Vn QA/QC trong x l mu phn tch
Mc tiu chung ca QA/QC trong x l mu phn tch l cung cp hay m bo cc iu
kin, cc bin php ti thiu cn thit m bo x l c tt mu phn tch t ng cht lng
mong mun.
X l mu l khu th hai v rt quan trng ca qu trnh phn tch. Nu vic x l mu
khng m bo c trung thc, ng n v loi c mi sai st nh hng nh mt hay
nhim bn cht phn tch th cc cng vic sau d cho c lm cn thn v chnh xc n u i
na th s liu phn tch cng khng cho ta ng thc t ca cht phn tch c trong mu. V vy
m bo cho cng vic x l mu c tt th nht thit phi thc hin cng tc QA/QC. Vy
QA/QC trong x l mu phn tch l g?
2.1.2.1 Khi nim v QA
Nh chng ta bit, mc tiu chung ca QA l cung cp hay m bo cc iu kin v
bin php ti thiu cn thit c c mt sn phm ca lnh vc nghin cu hay sn xut t
ng cht lng mong mun. Do c th ni mt cch tm tt l trong cng tc x l mu phn
tch th QA l cc quy tc, bin php v cc iu kin cn thit c nghin cu, la chn v
bin son thnh mt quy trnh (h thng), phc v cho cng tc x l mu phn tch nhm mc
ch ly c dung dch mu phn tch trung thc, khng mt cht phn tch, khng b nhim bn
v i din ng cho i tng cn phn tch. V vy thc hin QA trong x l mu phn tch l
iu rt cn thit v ch c m bo c QA trong x l mu th chng ta mi c y iu kin
khng nh cc s liu phn tch l c c s khoa hc, ng n v phn nh ng thnh phn
ca cht phn tch c trong mu nghin cu.
2.1.2.2. Khi nim v QC
Mc tiu chung ca QC l cung cp cc iu kin v bin php k thut cn thit gim
st v kim sot cht lng ca mt qu trnh no trong sn xut hay nghin cu khoa hc
m bo cht lng cho sn phm, ng thi pht hin cc sai st v tm bin php khc phc cc
sai st m bo thu c sn phm c cht lng ng yu cu mong mun. V th trong cng
vic x l mu cng vi QA, cng cn phi thc hin c bin php QC. Vy QC trong x l mu
phn tch l g?
Trong cng tc x l mu phn tch, QC l bin php, cc iu kin k thut v hot ng
gim st v kim sot cht lng ca mi cng vic trong x l mu phn tch. N l cc quy tc,
bin php v cc iu kin k thut c la chn, xy dng, bin son thnh nhng quy trnh
phc v vic kim tra, gim st, kim chun qu trnh x l mu nhm m bo cho vic x l
mu phn tch c c tnh chnh xc, ng n v dung dch mu thu c sau x l phn nh v
i din ng cho i tng cn nghin cu phn tch. ng thi trnh hay hn ch ti a c cc
sai st v trang b, dng c, ha cht, s nhim bn hay mt mt cht phn tch khi tin hnh x l
mu v cc tc ng khc ca mi trng lm vic m chng ta khng mong mun.V th bt buc
phi thc hin cc mu QC (nh mu trng hin trng, mu trng trang thit b, mu trng phng
php, mu thm chun, mu chun thm nh).
2.1.2.3. Ni dung v quan h QA/QC trong x l mu
X l mu l mt hot ng c thc hin c hin trng v trong phng th nghim m
ch yu l trong phng th nghim. N l bc hot ng th hai ca ton b dy chuyn hay cng
tc phn tch mu c c s liu, thng tin tin cy v cc i tng cn quan st. V th mi sai
st trong x l mu u nh hng n kt qu phn tch. Do chng ta phi quan tm ng mc
n vic bo m cht lng cho cng tc hay mi hot ng x l mu phn tch c c
nhng la chn v trang thit b, phng php, cc iu kin cn thit v cch x l mu. chnh
l ni dung ca QA/QC trong x l mu phn tch. V vn ny cn c mt s quyt nh c th
thc hin theo cc ni dung chnh sau y:
- Nhn s: xem xt tay ngh v kh nng ca cn b phn tch
- La chn phng php x l mu cho i tng cn phn tch
- Xc nh khi lng mu cn ly x l v s lng cn x l kp
- Chn trang thit b, dng c v cc iu kin cn thit x l mu
- La chn cch kim tra phng php ng dng x l
- La chn cc ha cht v thuc th cn thit cho x l t yu cu
- Kim tra mi trng xung quanh trong qu trnh x l mu
- Cng tc kim chun trong x l mu, mu lp v mu trng cc loi
- Chn phng php bo qun mu thu c sau khi x l phn tch, nu cha tin
hnh phn tch ngay c
ng thi theo cc ni dung nu trn th hot ng QA/QC trong cng tc x l mu
phn tch phi bao gm cc vn sau y, bt u t lc chun b cho cng tc x l mu phn
tch cho n khi thu c kt qu ca chng v bo qun, ngha l phi thc hin cng tc QA/QC
- i vi tt c nhng ngi thc hin x l mu phn tch
- i vi cc trang b, my mc v dng c dng x l mu
- i vi cc cht chun, ha cht v thuc th cn dng cho x l mu
- i vi cc loi dng c ng, cha mu thu c sau x l
- i vi cc hot ng trong khi tin hnh x l v ghi chp h s x l
- i vi cng tc kim chun trong qu trnh x l mu
- i vi cng tc bo qun v lu mu phn tch
- i vi vic pht hin sai st v cc bin php khc phc sai st
l cc vn t ra cho ngi lm phn tch trong giai on x l mu. Lm tt tt c
cc vn ny tc l chng ta thc hin c QA/QC v hot ng x l mu l tha mn c
cc yu cu ca phn tch. Ngha l trong mi hot ng ca cng tc x l mu phn tch t lc bt
u chun b cho n lc x l xong ly c dung dch mu v bo qun chng phn tch
theo mt phng php c la chn.
2.2. Phn loi mu phn tch
2.2.1. Phn loi theo ha hc phn tch
Theo quan im ha hc phn tch, ngi ta thng chia cc loi mu phn tch thnh hai nhm
chnh, da trn thnh phn nn (matrix) ca mu l v c hay hu c
- Nhm cc loi mu c cht nn v c
- Nhm cc loi mu c cht nn hu c
Trong mi nhm c th phi xc nh (phn tch) c cht hu c v v c, ty tng trng hp v
theo cc yu cu phn tch c th khc nhau.
Trong cc k thut , mi k thut ch thch hp cho mt s cht hay mt nhm cht nht
nh v mi k thut cng c mt s u v nhc im ring v phm vi ng dng ca n. Ngha l
khng th c mt cch x l mu no l ph hp c cho mi loi mu, mi cht phn tch. V th
ty theo yu cu c th ca cng vic phn tch m ngi lm phn tch phi nghin cu, xem xt
v la chn mt k thut no cho thch hp trong c s ca mnh v m bo c kt qu phn
tch ng n v tin tng. Tc l phi thc hin QA/QC trong cng vic x l v trong cng vic
phn tch t ra.
Trong khi x l hay phn hy mu, c th c rt nhiu qu trnh vt l v cc phn ng ha
hc c th xy ra ng thi, ty thuc vo mi loi nn mu, thnh phn ca mu v cc cht c
cho vo dng thc hin x l mu. Ni chung mt cch tng th c th c cc qu trnh sau y
xy ra:
- S ph v mng li cu trc ca cht mu ban u, gii phng cc cht phn tch, a
chng v dng dung dch di dng cc mui tan ca cc ion.
- Qu trnh oxy ha kh lm thay i ha tr, chuyn i dng, lm tan v cu trc vt
cht mu ban u gii phng chat phn tch v dng hp cht tan trong dung dch.
- S t chy, ph hy cc hp cht hu c v mn, to ra kh CO2, NO2, SO2, nc v
gii phng cc kim loi trong cht mu hu c ban u, a chng v dng cc hp cht
hay mui d tan trong acid.
- S to ra cc hp cht phc bn, t phn ly lm tan cht mu, to ra cc phc dng tan
ca cc cht phn tch trong dung dch (dung mi) qua m ha tan cht mu.
- To ra hp cht d bay hi, lm mt i anion ca cht mu ban u lm mu b phn
hy to ra cc cht khc tan trong dung dch acid hay kim hay acid.
- S kt tinh hay kt ta cht phn tch di dng hp cht khc, lm cht phn tch c
tch ra khi mu ban u v chuyn sang hp cht mi m chng ta ly c chng ra
khi mu ban u.
Nh vy trong qu trnh x l v phn hy mu c th c cc qu trnh vt l, cc phn ng
ha hc xy ra nh phn ng oxy ha kh, phn ng thy phn, phn ng to phc, phn ng ha
tan, phn ng kt ta ca cc phn t cht mu vi dung dch acid phn h mu v cc phn t
cht c trong mu vi nhau.
l ni chung tt c cc kh nng c th c, song trong thc t, ty thuc vo thnh phn
v bn cht ca mi loi mu, loi cht phn tch, phng php phn tch, ha cht x l mu m c
nhng qu trnh xy ra vi loi mu khi x l. Sau y chng ta s xem xt mt s k thut x l
mu c v ang c dng.
2.4.1. K thut v c ha t (x l t)
2.4.1.1. Bng acid mnh, c v c tnh oxy ha
a. Nguyn tc v bn cht
Dng acid mnh HCl, H2SO4 hay cc acid mnh, c c tnh oxy ha mnh (HNO3, HClO4)
hay hn hp 2 acid (HNO3-H2SO4) hay 3 acid (HNO3-H2SO4-HClO4) phn hy mu trong iu
kin un nng trong bnh Kendan hay trong ng nghim. Lng acid thng gp 20-15 ln lng
mu, ty loi mu. Thi gian ha tan mu (x l) trong cc h h, bnh Kendan thng t vi gi
ti vi chc gi, cng ty loi mu, bn cht ca cc cht. Cn nu trong l vi song h kn (c p
sut) th ch cn 50-60 pht. Di tc dng ca acid c v nhit , y cng c cc qu trnh vt
l v ha hc sau y xy ra, v d:
- S ph v mng cu trc ca cht mu, gii phng cc cht phn tch a chng v dung
dch di dng cc mui tan.
- Qu trnh oxy ha kh lm thay i ha tr, chuyn i dng, lm tan v cc cht mu,
gii phng cht phn tch v dng mui tan trong dung dch.
- Nu x l mu hu c phn tch kim loi th c s t chy, ph hy cc hp cht hu
c v mn to ra kh CO2, nc v gii phng cc kim loi trong cht mu hu c v
dng mui v c tan trong dung dch.
- To ra hp cht d bay hi, lm mt i anion trong phn t cht mu lm mu b phn
hy to ra cc hp cht khc tan trong dung dch.
- Nh vy trong qu trnh x l mu y cng c th c cc phn ng ha hc xy ra
nh phn ng oxy ha kh, phn ng thy phn, phn ng to phc, phn ng ha tan,
phn ng kt ta ca cc phn t cht mu vi cc acid dng phn hy mu v cc
cht c trong mu vi nhau.
Sau y l mt vi v d th hin cc qu trnh trn, khi x l mu phn tch khc nhau:
- v d 1: ha tan qung mangan oxide bng HNO3 v H2O2.
+ MnO2 + HNO3 + H2O2 Mn(NO3)2 + H2O + NO2.
- V d 2: ha tan qung st bng vng thy
+ Fe2O2.Fe3O4 + HNO3 + HCl FeCl3 + NO2 + H2O
- v d 3: x l mu thc phm, rau qu
+ Nn mu + HNO3 + H2SO4 CO2 + H2O + mui kim loi ha tan
Cc dung dch acid dng ha tan v x l mu: trong x l t, ngi ta thng dng cc
loi dung dch acid c, song tt nhin chn loi no l ty thuc vo bn cht ca nn mu v cht
phn tch tn ti trong mu
- Cc n acid c HCl, H2SO4, HNO3, HClO4.
- Hn hp 2 acid: cng thy, HNO3-H2SO4, HF-H2 SO4
- Hn hp 3 acid: HCl-HNO3-H2SO4, HNO3-H2SO4 -HClO4.
- Hn hp 1 acid v 1 cht oxy ha: H2SO4-KMnO4, HNO3-H2O2,
- Hn hp 2 acid v 1 mui: HNO3-H2SO4-KMnO4,
Nhit khi x l mu l ph thuc vo nhit si ca acid dng phn hy mu. Khi
dng hn hp acid th nhit x l mu cn ty thuc thm vo thnh phn ca hn hp acid v
thng thng nhit ny nm trong gii hn gia nhit si ca acid d si nht v acid kh si
cht. i vi nhng mu kh phn hy, ta phi dng cc acid hoc hn hp cc acid c nhit si
cao v tnh oxy ha mnh.
Acid HCl HNO3 H2SO4 H3PO4 HClO4 HF
C (%) 36 65 98 78 72 40
o
Tsi ( C) 110 121 340 213 203 120
b. Cc loi hay kiu x l t
Vic x l mu theo phng php t c th c thc hin trn cc loi trang thit b khc
nhau, ty thuc vo kh nng phng th nghim v tnh cht ca mu
- Trong iu kin thng, thit b n gin
+ Trong cc thy tinh, un nng trn bp in hay un cch thy.
+ Trong bnh Kendan thng
+ Trong bnh Kendan c hi lu
- Trong ni p sut cao: mu v acid c t trong cc hp kn sau t trong
+ T sy, bp cch ct, l nung
+ Luc trong ni nc si hay du si
- Trong l vi song (gm h kn v h)
+ H n gin: h bnh h hay h kn nhng khng iu khin nhit , p sut
+ H nhiu bnh, t ng hon ton: h h (c gim st nhit ) v h kn (c gim st
nhit v p sut).
Trong cc kiu x l trn, k thut x l t vi acid c c tnh oxy ha mnh trong bnh
Kendan hay trong l vi sng h kn ang c s dng rng ri, ph bin. cc nc pht trin, l
vi sng h kn c s dng mt cch ph bin trong x l mu do n trit , nhanh, hn ch mt
cht phn tch v nhim bn v tiu tn t ha cht.
c. Mt s th d v x l mu theo cch tro ha t
- V d 1: Ha tan mu kim loi v hp kim Cu hay Al bng acid HNO3; ly 1 g mu
nghin nh (hay dng phoi bo) vo bnh Kendan, tm t bng vi git nc ct, thm 10 mL
HNO3 65%, 4 mL H2SO4 98%, lc u, cm phu nh vo bnh Kendan, un nh cho mu si v
phn hy cho n khi dung dch mu trong. S ha tan y lm thay i ha tr v trng thi
ca Ca, Al kim loi trong hp kim, chuyn chng thnh mui tan trong dung dch. Phn ng ha
hc chnh xy ra l:
Al + HNO3 Al(NO3)3 + NO2 + H2O
Cu + HNO3 Cu(NO3)2 + NO2 + H2O
- V d 2: ha tan mu thp chrome bng hn hp acid HNO3 v HCl hay HNO3 v H2SO4.
Ly 0.5 g mu nghin nh (hay dng phoi bo) vo bnh Kendan, tm t bng vi git nc ct,
thm 15 mL HNO3 65%, 4 mL H2SO4 98%, lc u v un nh cho mu si v phn hy, cho n
khi dung dch mu trong. Qu trnh ny c s oxy ha kh ca Cl v N sinh ra Cl mi sinh phc
v cho phn hy mu. Di tc ng ca hn hp acid c ny v c nhit , mng li kim loi
b ph v, cc kim loi chuyn vo dung dch di dng cc mui tan. Phn ng ha hc chnh xy
ra y l:
Ni-Cr-Fe + HNO3 + HCl Ni(NO3)2 + Fe(NO3)3 + Cr(NO3)3 + NO2 + H2O
- V d 3: ha tan qung Mn oxide bng hn hp HNO3-H2O2. xc nh Mn v cc tp
kim loi trong qung ny, qu trnh ha tan c s oxy ha kh, chuyn Mn(IV) v Mn(II) tan trong
dung dch. Ly 1 g mu qung nghin nh vo bnh Kendan, tm t bng vi git nc ct,
thm 15 mL HNO3 65%, 2 mL H2O2 30%, lc u v un nh cho mu si v phn hy cho n khi
dung dch mu trong. Phn ng ha hc xy ra l:
MnO2 + HNO3 + H2O2 Mn(NO3)2 + H2O + O2
- V d 4: X l mu rau qu bng hn hp hai acid HNO3-H2SO4, trong bnh Kendan,
xc nh cc kim loi nng, c hi, nh Cd, Cu, Fe, Mn, Ni, Pb, Zn. Ly 5 g mu nghin mn v
trn u vo bnh kendan, thm 60 mL HNO3 65%, 5 mL H2SO4 98%, lc u v un nh cho mu
si v phn hy, cho n khi dung dch mu trong khng mu (6-8h ty loi mu). Chuyn dung
dch mu vo cc un 250 mL, lm bay hi ht dung dch acid cho n khi cn mui m, ngui,
nh mc bng dung dch HCl 2% thnh 25 mL. Trong qu trnh x l ny, cc nguyn t kim loi
di dng cc hp cht c kim ca mu rau qu s b acid c oxy ha, t chy cc cht hu c,
a cc kim loi v cc mui v c tan trong dung dch nc. Qu trnh ha hc chnh:
Nn mu + HNO3 + H2SO4 Mex(NO3)x + Men(SO4)m + H2O + CO2 + NO2.
- V d 5: X l mu tht c ti sng bng hn hp 2 acid HNO3-H2SO4 trong bnh Kendan
xc nh cc kim loi c hi nh Cd, Cu, Fe, Mn, Ni, Pb, Zn. Ly 5 g mu nghin mn v
trn u vo bnh Kendan, thm 60 mL HNO3 65%, 8 mL H2SO4 98%, cm phu nh vo bnh
Kendan, lc u v un nh cho mu si v phn hy, cho n khi dung dch mu trong khng mu
(6-8h ty loi mu). Chuyn dung dch mu vo cc un 250 mL, lm bay hi ht dung dch acid
cho n khi cn mui m, ngui, thm 5 mL dung dch HCl 10%, nh mc bng nc ct thnh
25 mL. Trong qu trnh x l ny, cc nguyn t kim loi di dng cc hp cht c kim ca mu
rau qu s b acid c oxy ha, t chy cc cht hu c, a cc kim loi v cc mui v c tan
trong dung dch nc.
Tt c cc mu trong v d 1-3 c th x l trong l vi sng h kn v lng acid ch cn
dng l nhiu. Thi gian x l ch trong 50-60 pht l xong. Cn x l nh trn th phi mt t 6-
10 gi m li khng trit bng x l trong l vi sng.
d. u nhc im v phm vi ng dng
Cc u v nhc im chnh ca k thut ny l:
- Khng mt cc cht phn tch
- Nhng thi gian phn hy mu rt di, nu khng dng l vi sng
- Tn nhiu acid c nht l khi s dng cc h h
- D b nhim bn khi x l bng h h do mi trng hay acid dng nhiu
- Phi ui acid d nn d b nhim bn do bi, hay mt mu
ng dng ch yu ca k thut ny l x l mu phn tch v mt s anion v c nh
halides, arsenate, sulfate, phosphate... trong cc loi mu sinh hot, mu hu c, v c, mu mi
trng, mu t, nc, bi, khng kh, mu kim loi, hp kim... K thut ny khng dng c cho
vic x l tch cc cht hu c phn tch v trong cc iu kin ny, cc cht hu c b ph hy
ht.
2.4.1.2. X l mu bng dung dch kim mnh c nng.
a. Nguyn tc chung
Trong phng php ny ngi ta thng dng cc dung dch kim mnh (NaOH, KOH) c
hay hn hp kim mnh v mui kim loi kim (NaOH-NaHCO3) hay hn hp kim mnh v
peroxide (NaOH-Na2O2), nng ln (10-20%) phn hy mu trong iu kin un nng trong
bnh Kendan, trong hp kn hay trong l vi sng.
Trong qu trnh x l, di tc ng ca kim v nhit cao, c th xy ra:
- Ph v cu trc nn mu, chuyn cht phn tch v dng dung dch
- Cc cht ca mu tng tc vi kim to ra sn phm tan c
- C th sinh ra cc kh bay ra gip mu ha tan tt hn
- C th to ra cc hp cht bn, t phn ly v tan trong dung dch
- To ra cc sn phm kt ta vi nn mu
b. Cc cch ha tan v dung dch ha tan
Theo k thut x l ny, chng ta c th dng cc dung dch ca cc cht sau y x l
mu:
- Dung dch kim c nng (NaOH, KOH: 10-20%)
- Dung dch kim c nng c cht oxy ha mnh (NaOH-Na2O2)...
- Hn hp kim c nng c cht kh mnh.
- Hn hp kim mnh v mui ca n (NaOH-NaHCO3, NaOH-Na2CO3)
Qu trnh phn hy c thc hin khi un si dung dch mu, trong mt thi gian nht
nh, thng l t 6-10 gi trong bnh Kendan h. Cn nu trong l vi sng h kn (p sut cao) th
ch mt khong 40-60 pht.
Nhit si ca cc dung dch kim ty thuc vo thnh phn, nng ca dung dch kim
s dng x l mu. Ni chung trong khong t 115-230 oC v y l yu t thc y phn ng
xy ra nhanh.
c. Vi v d ng dng
- V d 1: ha tan oxid nhm bng dung dch naOH 10% nng. Ly 0.5 g mu dng bt vo
bnh Kendan, tm t bng vi git nc ct, thm 10 mL NaOH 10%, un si ha tan mu. C
ch y l chuyn trng thi tinh th rn oxid sang dng ion tan trong dung dch theo phn ng:
Al2O3 + NaOH NaAlO2 + H2O
- V d 2: Ha tan qung silicate bng dung dch NaOH 20% nng. Ly 0.5 g mu dng bt
vo bnh Kendan, tm t bng vi git nc ct, thm 15 mL NaOH 20%, un si ha tan mu.
C ch y l chuyn trng thi tinh th rn sang ion tan trong dung dch v bn dng mui
Na2SiO3 theo phn ng
SiO2.nX + NaOH Na2SiO3 + H2O + nX
d. u nhc im v phm vi ng dng
K thut tro ha t ny cng c u im l khng lm mt cc cht phn tch nht l cc
nguyn t v hp cht d bay hi. Nhng m c mt nhc im ln nht l tn nhiu kim tinh
khit cao, thng phi dng gp t 10-15 ln nhu cu cn thit mi c th x l c mu v v vy
kh nng nhim bn rt cao. Sau khi x l mu, phi loi b lng kim d bng cch trung ha vi
acid, song li lm long mu. y l mt phn vic kh khn v mt nhiu thi gi v cng hay l
nhim bn mu. V th cch ny ch c dng cho mt s trng hp khi khng c cch la chn
no khc. V d khi phn hy mu xc nh cc anion v c nh halides, nitrate, phosphate,
sulfate... trong cc di tng khng x l c bng phng php acid.
2.4.1.3. X l t trong l vi sng
a. Nguyn tc
K thut x l mu t trong l vi sng thc cht cng l phn hy mu khi un nng bng
dung dch acid mnh, c c tnh oxy ha hay bng dung dch kim c nng nh nu bn trn.
Tc nhn phn hy l cc acid v nng lng nhit cung cp cho mu do hin tng truyn nhit do
i lu t mt ngun nhit bn ngoi. i vi l vi sng, nng lng un nng mu c cung cp
bng bc x vi sng tn s cao, cc phn t mu u c nhn nng lng ng u v trc tip t
ngun vi sng, ph v cu trc nn mu t pha trong ra, v th qu trnh x l mu nhanh v trit
hn. Hn na, i vi h kn cn c p sut cao v nhit cao do hiu qu cao v rt nhanh
li tn t acid so vi phn hy iu kin thng trong bnh Kendan. Cc qu trnh vt l v ha
hc xy ra khi x l mu bng vi sng cng tng t nh cch x l mu t thng thng khc
nhng c tc nhanh hn v trit hn.
b. Trang thit b
Vic x l mu trong l vi sng c th thc hin trong h bnh h hay trong h bnh kn. Cc
thit b ny ngy nay hin din trn th trng vi nhiu loi, kch c khc nhau, phc v cho
tng mc ch nht nh. Cc thit b ny li c nhiu kiu rotor khc nhau c th thay i c
nh rotor phn hy mu, rotor lm bay hi dung mi v acid, rotor dng chit, rotor dng
sy mu, rotor dng nung mu (nh l nung cao tn)... v th rt thun tin cho cng vic x l
mu phn tch. K thut ny c s dng ph bin cc nc pht trin.
c. Cc v d ng dng
T cc v d trnh by trong mc 2.4.1.1.c v 2.4.1.2.c u c th thc hin trong cc h
h. Tuy vy nu c thc hin trong h kn th lng ha cht tiu hao ch khong v thi gian
rt ngn xung cn t 40-60 pht m hiu qu x l li trit hn, t mt cht phn tch hn.
2.4.2. K thut v c ha kh (x l kh)
2.4.2.1. Nguyn tc v qu trnh xy ra trong x l
K thut tro ha kho l k thut nung x l mu, song thc cht ch l bc u tin ca
qu trnh x l mu v sau khi nung, mu b cn li cn phi c ha tan (x l tip) bng dung
dch mui hay dung dch acid ph hp chuyn cht phn tch vo dung dch cho mt phng
php phn tch chn. Qu trnh nung x l mu c th khng thm cht ph gia, cht bo v hoc
c thm cc cht ny vo mu tr gip qu trnh x l c xy ra nhanh hn, tt hn v hn ch
mt mt cht phn tch.
Trong qu trnh nung x l mu, c th c cc qu trnh vt l v ha hc sau y xy ra ty
theo bn cht, thnh phn ca mi loi mu v ph gia thm vo, v d nh
- Lm bay hi nc hp ph v nc kt tinh trong mu
- S tro ha, t chy cht mn, cc cht hu c khc ca mu
- Ph v cu trc ban u ca nn mu, chuyn sang cc nn n gin hn
- Chuyn dng cc cht phn tch t phc to sang n gin
- Qu trnh oxy ha kh thay i s oxy ha ca cc nguyn t trong mu
- Gii phng mt s kh nh CO, CO2, SO2
- C mt s tng tc ha hc gia cc cht trong mu vi nhau v vi ph gia thm vo
to ra cc cht mi.
Tt c cc qu trnh gp phn l tan v mu ban u, ha tan cht phn tch vo dung
dch. Bng sau y l vi v d v s nung mt s mu phn tch trong iu kin c v khng c
cht ph gia
Bng 2.1: v d v cc qu trnh trong x l kh trong l nung
V d 1: tro ha mu rau qu xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn,
Ni, Pb, Zn) dng cht ph gia. Cn 5 g mu vo chn thch anh, thm 1 g KNO3, 5 mL HNO3 65%,
trn u v un nh cho mu si u v cho n kh en. Nung mu nhit 450oC trong 3 gi,
sau nng ln 500-530 oC, n khi ht than en, thu c mu tro trng. Ha tan tro thu c
trong 15 mL dung dch HCl 18%, un nh cho tan ht, nh mc thnh 25 mL bng nc ct.
V d 3: Tro ha mu sa xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni,
Pb, Zn), dng cht ph gia l 8 mL H2SO4 45% v 2 g KNO3 hay LiBO2. Ly 5 g mu vo chn
thch anh, thm cht ph gia, trn u, sy cn thn cho mu kh (mu d b si bt v bn ra
ngoi) v thnh than en sau nung nhit 450oC trong 3 gi, sau nng ln 500-530oC n
khi ht than en, thu c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl 18%,
un nh cho tan ht, tip tc un ui acid cho n khi cn mui m. nh mc thnh 25 mL bng
HCl 2%.
V d 4: X l mu xc nh As trong qung hay b thi rn. Ly 0.5 g mu qung vo chn
Zr, thm 4 g KOH, un nh cho hn hp chy lng, thm cn thn 5 g Na2O2, lc u v nung
700 oC trong 10 pht, ngui, ly chn cha mu ra, lau sch bn ngoi chn v b c chn vo
cc dung tch 400 mL cha sn 100 mL nc m 70 oC, lc k cho mu tan, ly chn Zr ra v trng
chn (trong v ngoi) 2 ln bng 20 mL nc ct. Thm vi mnh s xp nh vo cc, y knh
ng h v un si nh ui H2O2 (khong 15 pht), ngui. Lc dung dch qua giy bng ,
ra kt ta v giy lc 3 ln bng 20 mL dung dch KOH 0.05% nng. Gp nc lc v nc ra,
c cn cn khong 65 mL, thm 25 mL HCl 35%, lc u v nh mc 100 mL. y l dung dch
mu xc nh As bng k thut hydride ha. Cch x l ny thch hp cho cc mu rn nh
qung st, t , rc thi rn, bn, trm tch xc nh As, nhng hm lng Si trong cc mu
ny phi nh hn 10%.
2.4.2.5. u nhc im v phm vi s dng
- Thao tc v cch lm n gin
- Khng phi dng nhiu acid c
- X l mu c trit nht l cc mu c matrix hu c
- Khng lu nh phng php x l t thng thng
- Nhc im: c th mt mt s cht d bay hi nh Cd, Pb, Zn, Sb, Sn... nu khng
dng cht ph gia v bo v.
2.4.3. K thut v c ha tro-t kt hp
2.4.3.1. Nguyn tc chung
Nguyn tc ca k thut ny l mu c phn hy trong chn hay cc nung mu. Trc
tin ngi ta thc hin x l t s b trong cc hay chn nung bng mt lng nh acid v cht
ph gia ph v s b cu trc ban u ca matrix mu v to iu kin lu gi nhng cht d
bay hi khi nung. Sau em nung nhit thch hp. V th lng acid dng x l mu
thng ch bng hay 1/3 lng cn dng cho x l t. Qu trnh nung sau se nhanh hn v
trit hn, hn ch bt s mt mt cht phn tch so vi cc cch x l mu n (t hay kh)
Cc qu trnh vt l v ha hc xy ra khi x l mu kh-t kt hp cng tng t nh cc
qu trnh xy ra khi x l mu kh hay t, song y l s kt hp hai qu trnh k tip nhau. X
l t ban u l bo v mt s nguyn t cho x l kh k tip theo khng b mt mu. Cch
ny thch hp cho cc mu c matrix l cht hu c, x l xc nh kim loi v mt s anion.
2.4.3.2. Cc phng php v v d
V l x l kh-t kt hp, x l kh v t k tip nhau nn mi din bin s tng t
nh x l theo mt trong hai kiu ni trn. im khc bit ng k trong quy trnh x l mu ny so
vi kiu x l mu t l khng phi ui acid d. Sau y l vi v d.
- V d 1: X l mu rau qu xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn,
Ni, Pb, Zn), ly 5 g mu cho vo chn nung, thm 10 mL HNO3 65% v 5 mL Mg(NO3)2 5%, trn
u ri sy hay un trn bp in cho mu si nh v n kh thnh than en. em nung nhit
400-450 oC trong 3 gi, sau nng ln 500-530 oC n khi ht than en, thu c mu tro trng.
Ha tan tro thu c trong 20 mL dung dch HCl 1:1, un nh cho tan ht, tip tc un ui acid
cho n khi cn mui m. nh mc thnh 25 mL bng HCl 2%. Dung dch ny dng xc nh
cc nguyn t ni trn.
- V d 2:X l mu sa xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni,
Pb, Zn),. Ly 5 g mu vo chn nung, thm 15 mL HNO3, 2 mL H2SO4 98% v 5 mL Mg(NO3)2
5%, trn u. x l mu t s b: sy mu cn thn trn bp in hay trong t sy cho mu kh
(mu d b si bt v bn ra ngoi) v thnh than en sau nung nhit 400-450oC trong 3 gi,
sau nng ln 500-530oC n khi ht than en, thu c mu tro trng. Ha tan tro thu c trong
15 mL dung dch HCl 1:1, un nh cho tan ht, tip tc un ui acid cho n khi cn mui m.
nh mc thnh 25 mL bng HCl 2%.
- V d 3: X l mu tm, cua, c... xc nh cc kim loi (Na, K, Ca, Mg, Cd, Co, Cr,
Cu, Fe, Mn, Ni, Pb, Zn). Ly 5 g mu vo chn thch anh, thm 5 mL H2SO4 98% v 5 mL
Mg(NO3)2 5% trn u. x l mu t s b: sy mu cn thn trn bp in cho mu kh v
thnh than en sau nung nhit 400-450 oC trong 3 gi, sau nng ln 500-530oC n khi
ht than en, thu c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl 1:1, un nh
cho tan ht, tip tc un ui acid cho n khi cn mui m. nh mc thnh 25 mL bng HCl 2%.
y l dung dch mu dng xc nh cc kim loi nu trn bng phng php ph hp thu phn
t hay ph nguyn t
2.4.3.3. u nhc im v phm vi p dng
u im ca k thut ny l tn dng v kt hp cc u im ca phng php x l mu
ut v kh
- Hn ch s mt mt ca mt s cht phn tch
- S tro ha l trit , sau khi ha tan tro s c dung dch mu trong
- Khng phi dng nhiu acid tinh khit
- Thi gian x l mu nhanh hn tro ha t
- Khng phi ui nhiu acid d, hn ch nhim mi trng, nhim bn mu
- Ph hp cho nhiu loi mu khc nhau xc nh kim loi
- Khng cn trang thit b phc tp, hin i, t tin
Cch ny c ng dng ch yu x l mu cho phn tch cc nguyn t kim loi v mt
s anion v c nh Cl-, Br-, sulfate, phosphate... trong cc loi mu sinh hc, mi trng, mu hu
c, v c. Cch x l ny khng dng c cho xc nh cc cht hu c. Trong cc phng th
nghim bnh thng, khng c trang b l vi sng th cch x l ny vn l mt phng php
thch hp, n gin m vn m bo c c kt qu tt.
2.4.4. Cc k thut chit
2.4.4.1. C s, nguyn tc v iu kin ca s chit
a. Nguyn tc v c s ca s chit
Chit da trn c s s ha tan (hay phn b) khc nhau ca cht phn tch vo trong hai
dung mi khng trn ln vo nhau. Tc l cht phn tch tan tt trong dung mi ny nhng li
khng tan tt trong dung mi kia, ngha l s phn b ca cht trong hai dung mi l rt khc nhau
nh m chng ta ly c cht phn tch ra khi mu ban u, chuyn n vo dung mi chng ta
mong mun sau xc nh n trong dung mi chng ta va chit vo. Nh th yu t quyt nh
s tch v x l mu y l h s phn b ca cht phn tch trong cc phase v iu kin thc
hin chit tch.
b. H s phn b ca cht
H s phn b l mt hng s vt l (hng s nhit ng) c trng cho s chit. N cho ta
bit s phn b (hay ha tan) ca cc cht phn tch trong hai dung mi (hay 2 pha) khng trn ln
vo nhau theo t l hay mc no. Nu gi tr hng s ny cng ln th s phn b cng khc
nhau nhiu v vy cng thun li cho s chit tch cc cht. V d cht X c phn b vo hai
dung mi khng trn ln vo nhau (A v B) th h s phn b ny c xc nh theo biu thc sau
C X (A)
KD
C X (B)
Trong CX(A) v CX(B) l nng cht X trong hai dung mi A v B. Nu h s phn b
KD > 99/1 xem nh cht X chuyn hon ton vo dung mi A. l iu kin ca qu trnh chit
ly cht phn tch ra khi nn mu.
c. Cc iu kin ca s chit
c c kt qu chit tt, qu trnh chit phi c cc iu kin v t c cc yu cu
sau y
- Dung mi chit phi c tinh khit cao, m bo khng lm nhim bn cht phn tch
- Dung mi chit phi ha tan tt cht phn tch, nhung khng ha tan tt cc cht c
trong mu
- H s phn b chit phi ln s chit c trit
- Cn bng chit nhanh t, thun nghch gii chit c tt
- S phn lp khi chit phi r rng, nhanh v d tch ra ring bit
- Phi chn pH hay mi trng acid thch hp
- Chn nhit ph hp
- Phi thc hin lc mnh trong qu trnh chit
- Cho thm cht chng to bt khi cn c s phn lp tt
2.4.4.2. Cc phng php v k thut chit
2.4.4.2.1. Phng php chit lng-lng
a. Nguyn tc v iu kin
Nguyn tc: nguyn tc ca k thut chit ny l hai pha lng khng trn ln c vo nhau,
trong hai dung mi ny c th c mt dung mi cha cht phn tch c trong mt dng c
chit (phu chit). Khi lc chit, cht phn tch s c phn b vo hai dung mi theo tnh cht ca
chng t ti trng thi cn bng. V th h s nhit ng KD ca cn bng chit l yu t quyt
nh hiu qu ca s chit. Chit theo kiu ny c hai phng php l chit tnh v chit theo dng
chay lin tc. Trong phn tch, phng php chit tnh c s dng ph bin hn.
iu kin chit: qu trnh chit t hiu qu tt, phi c cc iu kin chit nh m t bn
trn.
b. Cc phng php, trang b v v d
- Phng php chit tnh: l phng pho chit rt n gin, ch cn mt s phu chit dung
tch 100-250 mL, c th tin hnh c mi phng th nghim. Vic lc chit c th thc hin
bng tay hay my lc nh. Tt nhin khi phi lm hng lot mu th s mt nhiu thi gian.
V d 1: Chit lng vt cc ion kim loi nng (Cd, Co, Cr, Cu, Fe, Ni, Pb, Zn) t nc bin
vo dung mi MIBK vi thuc th to phc APDC trong mi trng pH 3-4 xc nh cc
nguyn t ny bng phng php ph hp thu nguyn t. Ly 250 mL mu vo bnh chit, chnh pH
3-4 bng HCl 10%, thm 2 mL APDC 0.1% v 10 mL MIBK ri lc chit trong 5 pht. yn 5
pht cho phn lp, tch ly phn MIBK c cha phc kim loi Me-APDC. Sau xc nh cc kim
loi chit vo MIBK trc tip hay gin tip sau khi gii chit kim loi vo dung dch HNO3
2.5M. Phng php ny thng c s dng tch chit v lm giu lng vt cc kim loi
trong cc loi mu nc nht l nc thi v nc bin.
V d 2: Chit ly tng iodine-triiodide t nc bin vo dung mi benzene trong s hin
din ca cht oxy ha mnh v mi trng acid chuyn iodide v iodine c chit vo
benzene. Sau xc nh n bng chun th tch hay bng trc quang. 200 mL mu + chnh
pH=3 + 5 mL H2O2 + 10 mL benzene + lc chit 6 pht, yn 5 pht cho phn lp. Tch ly lp
benzene cha Iodine i xc nh.
+ Cc loi mu bt, rau qu, trng tht: nghin hay xay thnh bt, bo qun -15 oC. Ly 5 g
mu vo bnh x l, thm 15-20 g Na2SO4 khan, trn u, thm 20 mL ethanol tuyt i, lc
mnh 2 pht, thm tip 10 mL hexane, lc mnh 4 pht, t trong t lnh 4 pht cho phn lp,
lc ht chn khng, tch ly lp hexane c cha cc retinoid phn tch chng bng HPLC
hay MCEKC.
+ Mu huyt thanh: ly 100 L mu huyt thanh cho vo ng nghim, thm 0.2 mL dung dch
NaCl 0.9%, 2 mL ethanol tuyt i, lc mnh 2 pht, thm 0.5 mL dung mi n-hexane, lc
mnh, ly tm cho phn lp, tch ly lp hexane c cha retinoid phn tch chng bng HPLC
hay MCEKC.
V d 4: chit v catotene t cc loi rau qu, l cy
a. Nguyn tc: chit Soxhlet l mt k thut chit c bit c thc hin nh mt loi thit
b ring ca n. Kiu chit ny cng nh kiu chit lng-lng nn v bn cht ca s chit vn l
nh lut phn b ca mt cht trong hai pha khng trn ln vo nhau. Song y hai pha khng
trn ln vo nhau. C th pha mu trng thi lng, bt, dng mnh hay l. Dung mi chit (hu
c) trong thi lng. V d chit ly du Meiton t l cy bc h bng dung mi hu c n-hexane
hay benzene. Chit cc thuc tr su hay bo v thc vt trong mu rau qu, mu t bng n-
hexane. V th y l kiu chit ca h chit c th c ng th v d th. Trong thc t, h d th l
ph bin v cht phn tch nm trong matrix rn.
b. Cc trang thit b v v d.
Dung mi ra gii cht phn tch trong loi ny thng l cc dung mi hu c khng hay t
phn cc v k nc hoc hn hp ca chng theo t l thch hp. V d: n-hexane, n-heptane,
CCl4, CHCl3, CH2Cl2, benzene... Cc dung mi ny c gi l pha ng v phi ha tan tt cht
phn tch.
+ V d 2: chit x l mu xc nh nhm cc kim loi (Cd, Co, Cr, Cu, Fe, Ni, Pb, Zn)
trong nc: thm 1 mL thuc th Ultrex- 8-oxyquinolin vo 250 mL mu, chnh pH 8-9 bng NH3
1N, lc u ri di mu qua ct Baker-10 C18 SPE 5 mL vi tc 2-4 mL/pht. Ra ct bng 10
mL nc ct. Gii hp cc phc kim loi trn ct bng 10 mL MeOH, xc nh cc nguyn t trong
pha MeOH bng AAS. xc nh kim loi, nn tro ha t dch chit MeOH bng HNO3. C th
thay thuc th ny bng Na-diethyldithiocarbamate 0.1% trong EtOH.
+ Chit x l mu xc nh mt s thuc BVTV trong nc. Ly 250 mL mu nc,
chnh pH 5, lc b cn. Di dung dch qua ct chit loi LR C18 vi tc 4 mL/pht. Ra ct bng
10 mL nc ct, ht chn khng 5 pht. Ra gii cc cht BVTV trong ct bng 20 mL EtOAc. Ly
dch ra gii ny di qua ct th 2 cha Na2SO4 -...-than hot tnh, ra gii bng 10 mL EtOAc.
Lm bay hi dung dch thu c bng dng kh Nitrogen n khi dung dch snh, nh mc thnh 2
mL bng EtOAc. Xc nh cc ha cht BVTV bng GC hay GCMS.
- Chit theo c ch trao i ion v cp ion.
Nguyn tc: da trn c s ca qu trnh tng tc ca cht phn tch vi ion i (ca cht
trao i ion-pha tnh). Cht phn tch s b lu gi trn pha tnh v s c ra gii bng mt pha
ng thch hp.
Cht trao i ion ca kiu chit ny c th c hai loi sau
+ Trao i cation acid mnh (gc R-SO3Na) v acid yu (R-COONa).
+ Trao i anion baz mnh (gc R-NR3OH) v baz yu (R-NHOH)
C ch trao i loi cation
Support-SO3Na + Men+ support-(SO3)nMe + n Na+
C ch trao i loi anion
Support-NR3OH + Xn- support-(NR3)nX + nOH-
Trong qu trnh trao i, ty thuc vo mi loi cht phn tch v pha tnh m qu trnh c th c
thc hin tt trong mt khong pH nht nh no .
Cng vi s trao i anion v cation; trong s chit pha rn cn c c ch chit theo kiu cp ion
(ion-pair). N cng hon ton tng t nh sc k cp ion ca h pha o (RP-HPLC). Pha tnh
y l cht trao i pha ngc.
C ch trao i cp cation
+ V d 1: Theo c ch trao i cation. Chit tch cc kim loi nng (Cd, Co, Cr, Cu, Fe, Ni,
Pb, Zn) trong mu nc khong, nc m, nc thi Acid ha 250 mL mu nc n pH 4, lc
b cn. Np mu vo ct chit (chelex-100, dng H+) vi tc 3-4 mL/pht. Gii chit cc kim
loi trong ct bng 10 mL HNO3 2.5M. Xc nh chng bng AAS hay ICP.
+ V d 3: theo c ch to cp trao i cation. Chit tch ly cc ion kim loi nng trong
nc thi bng R-C18. Ly 250 mL mu nc, chnh pH 5, lc b cn, thm cht to cp ion ri di
dung dch mu qua ct chit loi Hypersil ODS 5 m, 6 mL, tc 2-4 mL/pht, sau ra gii
cht cn phn tch bng 10 mL dung dch HIBA 0.25%, pH 4-5 hay EDTA, pH =5.
- V d 2: Chng ct tch MeOH tinh khit t MeOH k thut (nguyn liu th) v thu ly
b cn li xc nh mt s tp cht c trong MeOH k thut. Ly 200 mL MeOH vo bnh chng
ct, lp h thng c quay chn khng v chng ct MeOH cho n khi dch lng trong bnh chng
ct cn khong 2 mL, ngui. Ly b ny ha tan trong 5 mL DCM, ly tm hay lc tch b cn.
Xc nh cc tp cht hu c trong dch lc bng GC, GCMS hay HPLC.
2.4.8.1. Nguyn tc chung: da trn c s tnh cht hay c im ca cht phn tch c kh nng
thng hoa trong mt iu kin nht nh khi x l mu tch n ra khi matrix. V d kim loi Hg,
Ga.. ra khi mu t , qung hay b thi rn.
Cn a g
Lm bay hi acid d
c th thm cc
nh mc, thm ph gia
C th chit lm giu, cht cn thit
tch nhm trc khi phn tch
Phn tch
AES
AAS
UV VIS
HPLC
Ion CA
ECA
Ly mu Nghin trn
Cn a g
X l
Phn hy
V c ha kh
c th thm
Ha tan tro b trong acid
cht bo v
Lm bay hi acid d
c th thm cc
nh mc, thm ph gia
C th chit lm giu, cht cn thit
tch nhm trc khi phn tch
Phn tch
AES
AAS
UV VIS
HPLC
Ion CA
ECA
Ly mu ng nht, trn u
Ly V mL
C th lc b cn
X l mu bng
- Cc cch chit tch
- Chng ct c th thm cc
- Sc k cht cn thit
- C c
....
AES
AAS
UV VIS
HPLC
Ion CA
ECA
Ly mu Nghin, trn u
Cn a g
X l mu bng
- Cc cch chit tch
- Chng ct c th thm cc
- Sc k cht cn thit
- C c
....
UV VIS
HPLC
GC
GCMS
HVCEC
Fluorescen ce
So snh kt qu tro ha t v kh
Ng CX Cch tro ha Ph gia bo v Nhit Recovery
t (oC) (%)
Pb 10 t:
HNO3+HClO4 97-100
HNO3+HClO4+H2SO4 93-98
HNO3+H2SO4 90-94
Kh Khng 450 97-100
550 93-95
650 71-83
H2SO4 450 97-99
550 95-97
650 90-96
HNO3 450 97-99
550 97-99
650 70-84
Mg(NO3)2 450 98-99
550 92-95
650 91-96
Mg(OAc)2 450 97-98
550 95-98
650 92-94
Hg 10 t:
HNO3+HClO4 78-80
HNO3+HClO4+H2SO4 90-94
HNO3+H2SO4+K2Cr2O7 92-94
Kh Khng 450 0
550 0
Zn 10 t:
HNO3+HClO4 97-100
HNO3+HClO4+H2SO4 94-102
HNO3+H2SO4 96-100
Kh Khng 550 87-96
HNO3 550 93-97
H2SO4 550 97-100
Mg(NO3)2 550 98-99
As 10 t:
HNO3+HClO4 96-98
HNO3+HClO4+H2SO4 97-99
HNO3+H2SO4 91-98
Kh Khng 550 80-88
HNO3 550 80-84
H2SO4 550 90-96
Mg(NO3)2 550 92-99
Cu 10 t:
HNO3+HClO4 99-100
HNO3+HClO4+H2SO4 99-101
HNO3+H2SO4 99-100
Kh Khng 550 86-92
HNO3 550 94-96
H2SO4 550 95-97
Mg(NO3)2 550 97-99
Co 10 t:
HNO3+HClO4 98-100
HNO3+HClO4+H2SO4 98-100
HNO3+H2SO4 97-99
Kh Khng 550 97-99
HNO3 550 90-96
H2SO4 550 96-99
Mg(NO3)2 550 97-100
Cd 10 t:
HNO3+HClO4 98-100
HNO3+HClO4+H2SO4 98-100
HNO3+H2SO4 97-100
Kh Khng 550 86-94
HNO3 550 82-91
H2SO4 550 93-97
Mg(NO3)2 550 94-97
Sb 10 t:
HNO3+HClO4 94-98
HNO3+HClO4+H2SO4 95-98
HNO3+H2SO4 97-99
Kh Khng 550 90-94
HNO3 550 92-96
H2SO4 550 94-98
Mg(NO3)2 550 96-97
Cr 10 t:
HNO3+HClO4 97-100
HNO3+HClO4+H2SO4 98-100
HNO3+H2SO4 98-100
Kh Khng 550 94-98
HNO3 550 95-98
H2SO4 550 97-99
Mg(NO3)2 550 95-98
Fe 10 t:
HNO3+HClO4 96-100
HNO3+HClO4+H2SO4 98-100
HNO3+H2SO4 97-100
Kh Khng 550 94-98
HNO3 550 96-99
H2SO4 550 97-100
Mg(NO3)2 550 98-100
Au 10 t:
HNO3+HClO4 95-98
HNO3+HClO4+H2SO4 97-99
HNO3+H2SO4 97-99
Kh Khng 550 93-99
HNO3 550 87-98
H2SO4 550 97-99
Mg(NO3)2 550 97-100
Phn loi v s chit pha rn, SPE
Trang 4
D.Vi v d ng dng.
+ V d 1: Phn tch t nng nghip. Chit cc ion kim loi di ng. Dng dung dch mui
NH4Ac 1M, pH=4.7 chit cc ion K, Na, Cu,Zntrong t trng trtv sau xcnh bng
phng php AES hay AAS. Ly 10g mu t nghin nh vo bnh chit thm 100mL dung dch
chit, lc chit 10 pht, yn 5 pht gn hay ly tm ly dch chit xc nh cc kim loi ni
trn.
+ V d 2: Phn tch t nng nghip. Chit cc ion kim loi di ng. Dng dung dch chit
(HCl 0.05 M+ H2SO4 0.025M) chit cc ion K, Na, Ca, Cu, Mg, Cd, Zn,Fe, Mn,Pb trong t
trng trtv sau xcnh bng phng php AES hay AAS. Ly 10g mu t nghin nh vo
bnh chit thm 100mL dung dch chit, lc chit 10 pht, yn 5 pht gn hay ly tm ly dch
chit xc nh cc kim loi ni trn.
+V d 3: Phn tch phn bn v c. Chit cc ion kim loi di ng. Dng dung dch mui
NH4Ac 1M, pH=4.7 chit cc nguyn t Cd, Co, Cu, Fe, Mn, Pb, Zn sau xcnh bng
phng php AAS. Ly 10g mu t nghin nh vo bnh chit thm 100mL dung dch chit, lc
chit 10 pht, yn 5 pht gn hay ly tm ly dch chit xc nh cc nguyn t kim loi ni
trn.
3.1.3.1 K thut x l t (v c ho t)
y l k thut dng cc acid mnh, c hay hn hp ca cc acid mnh c tnh cht cxi ha
mnh,hoc dung dch kim c ha tan, phn hy mu, nhit phng hay khi un si trong
bnh kendan, hay chng ct hi lu. Nh vy mu phn hy y nh c acid mnh v nhit
thch hp. Nhit si y l nhit ca acid dng x l mu. V th nu cn c nhit si
cao th dng acid c nhit si cao nh acid H2SO4. Nhit si ph thuc vo bn cht ca acid.
V d acid HCl c nhit 115oC V th ty yu cu ca mu m chn acid no hay thnh phn hn
hp no t c nhit si ca hn hp phn hy musao ph hp.
Trc khi x l cc mu qung, t cn nghin thnh bt. Cc mu kim loihp kim
cn phay thnh phoi bo mng, cc mu sinh hc, rau qu phi thi nh hay xay nhuyn v dng bt
nho ng nht. Sau c th s dng 1 acid c hay cc loi hn hp sau y phn hy mu.
V d:
- Dng 1 acid mnh nh: HNO3, H2SO4, HCl..
- Dng nc cng thy (HCl+ HNO3) v hn hp 2 acid c tnh oxi ha mnh nh HNO3
+ H2SO4), (HClO4+ H2SO4 )..
- Dng hn hp 3 acid mnh
- Dng mt acid mnh v 1 peroxid (HNO3+H2O2)
- Dng dung dch kim mnh nh: NaOH 20%, KOH 20%.
- Dng hn hp acid v cht to phc (HCl + tartaric cho Sb)
Sau y l mt vi v d x l mu xc nh mt s kim loi nh Cd, Co, Fe, Mn,Ni,Pb,
Zn.
V d 1: Phn hy hp kim nhm: ly 1,000g mu (dng phi bo) vo bnh kendan, thm
0,5mL nc ct, lc u thm 20mL HNO3 1/1, lc u cm vo bnh mt phu nh, un nh cho
mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh
ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%.
V d 2: Phn hy qung t him nhm nh: ly 2g qung dng bt vo bnh kendan, thm
1,0mL nc ct, lc u thm 40mL nc cng thy, lc u cm vo bnh mt phu nh, un nh
cho mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh
ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%.
V d 3: Phn hy qung st: ly 1g qung dng bt vo bnh kendan, thm 1mL nc ct,
lc u thm 20mL nc cng thy, lc u cm vo bnh mt phu nh, un nh cho mu phn
hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh ui ht
acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%. y l dung dch mu xc
nh cc nguyn t trong qung st v xc nh c st.
V d 6: Phn tch t trng trt. Xcnh hm lng ton phn ca cc ion kim loi (Na, K,
Ca, Mg, Cd, Cu, Fe, Mn, Mo, Pb, Zn) trong t. Cn ly 2,000g t c sy kh trong khng
kh v nghin mn vo chn Pt hay chn thch anh. Tm t bng 1mL nc ct thm 20mL acid
HCl 1/1(18%) lc mnh v un si cho mu phn hy trong vng 45 pht. Lc ly phn dung dch
(dd 1), chuyn phn b cn li sang chn Pt, thm 2mL HCl 35%, 5mL H2SO4 98% v 8mL HF sau
un cch ct cho mu si v bc khi. n khi xut hin khi trng SO2. Li thm 8mL c na
v tip tc bc khi v cho n khi cn b gn kh (mui m) l c. ngui ha tan b ny
bng 10mL HCl 18%, un nh cho tan. Gp ton b dung dch ny vo dung dch 1 trn v
chuyn sang cc, un si u v lm bay hi cho n khi cn mui m. Sau nh mc mui ny
thnh 50mL bng dung dch HCl 2%. y chnh l dung dch mu xcnh cc kim loi ni trn.
Nhiu loi mu c cu trc rt bn vng, khng phn hy c bng bt k dung dch acid
no, hoc cho hiu sut rt km. Nn phi x l nung s b trc, ct l ph v cu trc bn ban
u ca mu, cho vic vic x l hay phn hy tip c d dng v hon ton. Nguyn tc l
ly mt lng mu a gam nht nh vo chn nung (v d a=2 hay 5 gam ty theo yu cu phn
tch). Nung mu mt nhit thch hp(450-700o C, ty loi mu), vi cc cht ph gia hay cht
chy ph hp, ph v cc cu trc mng tinh th ca cc cht mu chuyn chng sang dng c
cu trc d ho tan hn.Sau ha tan b thu c sau khi un trong nc hay acid hay trong dung
dch kim long, ly ht cc cht cn phn tch vo dung dch v xc nh chng theo cch
chn. Chng ta c th:
1.X l khng dng cht ph gia v cht chy. Ch nung mu nhit thchhp ph v cu
trc mng li tinh th ban u, lm cho mu d ho tan. Nhng cch ny thng t hiu qu, ch
c dng cho 1 s trng hpnn t c dng. V d
Qung H: LnCO3 F.xH2O Ln2O3 + H2O + CO2 + HF + Men Om
Qung st: Ferit.xH2O FeO + Fe2O3 + SO2 + H2O + Men Om
Qung Cu: CuS. xH2O CuO + SO2 + H2O + Men Om
2. X l c dng cht ph gia v cht chy: trn mu vi 1 cht chy hay hn hp cht chy, sau
nung mu nhit thch hp. cch ny c dng nhiu cho cho cc loi mu kh phn hy. cc
cht ny c th l:
- loi cht chy acid nh: NaHSO3, NaHCO3, NaH2 PO4, pyrosunphate
- Loi cht chy kim nh: Na2CO3, KOH,NaOH, LiBO2, Na2O2, NaNO2
- Lai cht chy hu c nh C6H5SO3Na, SDS..
V d:
Qung H + NaHCO3 Ln2O3 + H2O + CO2 + HF + Men Om
t + LiBO2 + NaHCO3 Men Om + Na2SiO3 + H2O + Na2B2O7
HNH 3.3
Trong h ng kn: mu phi trong bnh knh v chu p cao. Sau cng phn hy bng
hn hp nh trn. Nhng v h kn p sut cao. Nn s phn hy nhanh v trit hn, v lng
acid cn t hn. cc h thng x l mu theo cch ny hin nay cc hng c cung cp y , t n
gin n hon chnh, c chng trnh iu khin v t ng tt c.
Cc trang b ca k thut chit ny l cc bnh chit hay phiu chit khc nhau(hnh 3,4).
N l cc dng c thy tinh ph thng ca phng th nghim nn khng mc tin. Sau y l mt s
v d v chit x l mu phc v phn tch cc cht.
V d 1: chit xc nh cc kim loi nng nng c hi(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn...)
trong mu nc thi ly 250mL mu vo cc, acid ha mu n pH=1 lc b cn, chuyn mu vo
phiu chit, thm 2mL thuc th APDC 0.1% trong ru, v 15mL CHCl3 chit 10 pht yn 5
pht tch ly pha hu c CHCl3 vo phiu chit khc v gii chit cc kim loi bng 20 mL dung
dch HNO3 2.5M. ly dung dich nc gii chit lm bay hi mui m, sau dnh mc thnh 10
mL bng dung dch HCl 1% . y l dung dch xc nh cc nguyn t nu.
V d 2: chit xc dnh cc kim loi nng c hi(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn...)
trong mu nc bin. Ly 250mL mu vo cc. Acid ha mu n pH=2, lc b cn, chuyn mu
vo phiu chit. Thm 2 mL thuc th APDC 0.1% v 10 mL MIBK lc chit 10 pht yn 5 pht
tch ly pha hu c MIBK, lp li s chit nh th mt ln na, th 2 ln MIBK vo phiu chit
khc, v gii chit cc kim loi bng 20 mL dung dch HNO3 2.5 M. Ly dung dch nc gii chit
lm bay hi cn mui m, sau dinh mc thnh 10 mL bng dung dch HCl 1% v xc nh cc
nguyn t bng phng php ph F-AAS
V d 3: chit tch xc nh cc kim loi nng(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn..) trong
ng vng hay ng th. Ha tan 10 gam dng vo 80 mL nc ct, lc cho tan ht, chnh c
pH=1 bng acid HCl 10% lc b cn (nu c). Chuyn mu vo phiu chit. Thm 2mL dung dch
APDC 0.1%, 10 mL CCl4 lc chit 5 pht, tch ly lp hu c vo cc cha lp li s chit nh th
mt ln na tch ly phn hu c v gp phn dung mi hu c ca c 2 ln chit vo 1 phiu lc
khc. Thm 30 mL HNO3 3M lc gii chit. Tch pha ly phn dung dich nc acid c cha cc
kim loi vo cc 250 mL. un si lm bay hi nc m v nh mc thnh 10 mL bng dung dich
HCl 2% y l mu xc nh cc kim loi trong ng bng phng php F-AAS hay phng
php UV-VIS hay ICP-AES
Hnh
V d 1: chit x l mu nc bin ly cc kim loi nng (Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn....)
Xem v d 2 trong mc 2.4.4, 2.4.2.2 chng 2 (trang ) v v d 1, v d 3 trong mc 2.4.4,
2.4.2.3 chng 2 (trang ).
V d 2: chit x l mu nc xc nh mt vi anion (Halogen, Nitrat, v Sunphat ). Xem v d 2
v 4 trong mc 2.4.4, 2.4.4.2 chng 2 (trang ).
V d 3: Chit x l mu nc xc nh cc cyanua (CN ) xem v d trong mc XX chng 2
(trang )
V d 4: chit tch xc dnh hm lng ion CNS trong nc thi cng nhip thc phm. Ly 250
mL mu vo cc, chnh pH v 3 bng dung dch HCl 5% lc b cn. Ly dung dch trong di qua
ct chit (loi LA-ROH 7m) vi tc 3-4 mL/pht (nh ht p sut thp). Sau khi mu chy ht,
ht kh ct trong 2 pht. Ri ra gii ct chit ly ion CNS bng 10 mL dung dch NaOH 0.5 M.
Thu dung dch ny xc nh CNS.
Nguyn tc ca k thut ny l xay mu thnh bt, sau ly mt lng nht nh, v ngm
chit trong dung dch acid long (3-5% ). Phng php ny l chit ly cc ion kim loi c trong
mu phn tch, khi mu c ngm trong acid th cc ion kim loi s chuyn vo dung dch, dng
mui tan. V d ngm chit mu bt go trong dung dch acid HCl 5% ly cc kim loi kim v
kim th ra khi bt go v xc nh chng bng phng php ph hp thu nguyn t. Cch chit
ny n gin d lm, khng cn my mc phc tp. Ch cn nghin mu thnh bt, hay th nho,
sau thm acid vo mu v ngm chit qua m.
ngm chit ngi ta thng dng cc dung dch acid long (5-7 % ) trong nc ca acid
HCl, HNO3, hay H2SO4... sau y l vi v d ng dng.
V d 1: Ngm chit tch ly mt s kim loi (Na, K, Cd, Cu, Pb, Zn,....) t bi, chanh hay
cam. Ly 10 gam mu c nghin nh hay xay thnh bt vo bnh nn 250 mL, thm 200 mL
dung dch acid HCl 5% ngm chit. Khuy u un si, ngm chit qua m. Sau lc k 2
pht. V lc ly dung dich chit vo cc 250 mL, un si k. Lm bay hi ti cn mui m. V
nh mc thnh 25 mL bng dung dch HCl 2% (nu c vn c, lc b vn c). y l dung dch
xc nh cc kim loi v c ion nitrat, sulfat.
V d 2: ngm chit tch ly mt s kim loi (Na, K, Cd, Cu, Pb, Zn,....) trong cc rau xu
ho bp ci. Ly 10 gam mu c nghin nh hay xay thnh bt nho vo bnh nn 250 mL,
thm 100mL dung dch acid 5% ngm chit. Khuy u, un si,, lc mnh 1 pht, ngm chit
qua m. Sau lc k 1 pht, v lc ly dung dch chit vo cc 250 mL. un si k,lm bay hi
n cn mui m v nh mc thnh 25mL bng dung dch HCl 2% (nu c vn c th lc b vn
c). y l dung dch xc nh cc kim loi v mt s anion nh NO3-, SO42-.....
B thi cng nghip v c cng c nhiu loi, rt phc tp, a dng. N ty thuc vo mi
loi cng nghip.c th gm c nh sau:
B thi cc nh my ha cht, x luyn kim, gang thp
B thi cc nh my in, than..
B thi cng nghip khai thc, tuyn v ch bin qung khong sn.....
B thi ca cng nghip nguyn liu xy dng (xi mng, gch.)
B thi ca cng nghip thy tinh, snh s.......
..........
Nh vy mi loi khc nhau s phi dng cch phn hy khc nhau, nhng u dng k
thut x l t bng cc acid khc nhau trong bnh kenddan iu kin thng hay trong l vi
sng.
V d 2: phn tch mt s kim loi Al, Ca, Cd, Cu, Co, Fe, Mg, Mn, Na, K, Zn,.. trong mu
thc phm, tm, c,..ly 5 gam mu vo chn nung, sy cho kh dn. Ri nung 8 gi u 450oC
sau 520oC n khi c tro khng cn en(ht than en). Sau ha tan tro cn li bng
15mL HCl 1/1 un nh cho tan ht v ui ht acid d n cn mui m v nh mc thnh 25 mL
bng dung dch HCl 2%. Nu dung dch c cn th nn ly tm hay lc b cn. Cch ny d b mt
cc nguyn t Cd, Pb, Zn (8-15%) khi tro ha. Nht l khi tro ha nhit trn 530 oC. V th
cch ny khng thch hp cho Cd, Cu, Pb, Zn.
V d 3: Phn tch mt s kim loi Al, Ca, Mg, Na, K...trong mu dc phm thuc v y
hc. V d xc nh cc nguyn t Al, Na, K, Fe, Mn, Ni,...trong cao h ct. Ly 1 gam mu cho
vo chn nung, sy cho kh dn. Sau em nung 3 gi u 450 oC, sau 530 oC n khi c
tro khng cn en(ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un nh
cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%.
Nu dung dch c cn th lc b cn ly phn trong xc nh cc cht. Trong v d ny cc
nguyn t Cd, Cu, Pb v Zn cng b mt nh v d 2.
Cc v d:
VD1: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,Cr.. trong mu rau qu (rau mung rau ci).
Ly 5 gam mu cho vo chen nung thm cht bo v l KNO3 10% 10mL H2SO4 98% trn u say
hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c tro khng
cn en(ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un nh cho tan
ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%. Gii thch
c ch.
VD2: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn, Cr.. trong mu thc phm (tm c tht).Ly 5 gam
mu cho vo chen nung thm cht bo v l 5mL Mg(NO3)2 10% + 10mL H2SO4 98% trn u sy
hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c tro khng
cn en (ht than en ). Sau ha tan tro cn li bng 15 mL dung dch HCl 1/1 un nh cho tan
ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%, lc u.
(nu c cn th lc b)
VD3: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,.. trong mu thc phm sa bt, sa c c ng.
Ly 5 gam mu cho vo chn nung thm cht bo v l 12mL H2SO4 778% 5mL Mg(NO3)2 10%
trn u sy hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c
tro khng cn en (ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un
nh cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl
2%, lc u.
VD4: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,...trong mu rc thi ca thnh ph Ly 5 gam mu
cho vo chn nung thm cht bo v l 5mL LiBO2 10% + 5mL Mg(NO3)2 10% v 5mL H2SO4
98% trn u sy hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi
c tro khng cn en (ht than en ). Sau ha tan tro cn li bng 15 mL dung dch HCl 1/1
un nh cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch
HCl 2%, lc u. (nu c cn th lc b).
Trong vic x l mu hu c ly cc kim loi th k thut ny c nhng u v nhc im l:
Tro ha trit c mu ht cc hp cht hu c.
n gin v d thc hin
Khng tn nhiu acid tinh khit cao v khng c acid d
Hn ch c s nhim bn do dng d thuc th
Qua mu x l khng lu, kh phng php t.
Mu dung dch, mu thu c s sch.
Nhng..: nu khng dng cht bo v.
V d 5: X l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn,... trong mu nc
ngt gii kht, v d Cocacola, Pepsi... Ly 50 mL mu vo cc un dung tch 250 mL, thm 5 ,mL
HCl 36%, un cho cn cn 1/3, chuyn mu vo bnh Kendan, thm 50 mL HNO3 65%, lc u,
cm vobnh mt phu lc nh, un nh cho mu phn hy trong 2h, thm 2 mL H2O2 30%, un
tip n khi no uc dung dch trong khng mu (khong 6-7h). Chuyn ht mu sang cc, lm
bay hi ht acid n cn mui m v nh mc thnh 25 mL bng HCl 2%, nh vy sau khi x l,
mu uc lm giu 10 ln. Mu ny dng xc nh c kim loi kim v kim th.
V d 6: l mu xc nh cc nguyn t Cu, Fe, Mn, Ni, Pb, Zn,... trong mu nc tiu. Ly 50 mL
mu vo cc un dung tch 250 mL, thm 5 ,mL HCl 36%, un cho cn cn 1/3, chuyn mu vo
bnh Kendan, thm 50 mL HNO3 65%, lc u, cm vo bnh mt phu lc nh, un nh cho mu
phn hy trong 2h, thm 2 mL H2O2 30%, un tip n khi no uc dung dch trong khng mu
(khong 6-7h). Chuyn ht mu sang cc, lm bay hi ht acid n cn mui m v nh mc thnh
25 mL bng HCl 2%, nh vy sau khi x l, mu uc lm giu 10 ln. Mu ny dng xc
nh kim loi kim v kim th.
u v nhuc im ca k thut ny l:
+ Khng mt mt s nguyn t kim loi nh Pb, Fe, Zn, Cu
+ Nhng thi gian phn hy lu, thng l t 10 18h
+ Tn nhiu acid tinh khit, acid d nhiu, phi ui sau khi x l rt lu.
+ D gy nhim bn, nu cc ha cht khng c sch cao
+ Phi ui acid d lu, c khi kh khn khng ht c.
+ V d 1: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn trong mu rau
qu v thc phm. Ly 5gam mu vo chn nung, thm cht bo v l 2mL Mg(NO3)2 10%, 10mL
HNO3 65%, trn u, sy hay un nh cho kh dn v thnh than en. Ri nung 5h u 450oC,
sau 530 oC n khi c tro khng cn en (ht than en). Sau ha tan tro cn li bng
15mL HCl 1:1, un nh cho tan ht, v ui ht acid d n cn mui m v nh mc thnh 25mL
bng dung dch HCl 2%, lc u, lc b cn nu c. Mu ny xc nh c c mt s kim loi
kim v kim th.
y cng l mt k thut (phng php) x l t. Nn cng phi dng mt acid c tnh oxy
ho mnh, hay hn hp cc acid c tnh oxy ha mnh phn hy ht cc cht hu c trong bnh
kn, chuyn cc kim loi v dng cc ion trong dung dch mui v c. Vic phn hy c th thc
hin trong hp kn nn c p sut cao, n tng t nh ni p sut. S phn hy nhanh v trit ,
v cn t acid hn k thut thng thng ni trn. Song y phi c hp x l mu c bit,
chu acid, chu nhit v p sut cao. Cc bnh x l thng bng Teflon v t trong v thp dy
bo v, chu c nhit v p sut cao.
+ V d 1: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn trong mu rau qu
ti sng. Ly 5gam mu vo hp x l, thm 30mL cng thy, trn u, y np cht. Ri cho
hp mu vo l vi sng trong 50 pht. ngui, ly ra v chuyn mu sang cc, lm bay hi
ui acid v n cn mui m. Sau ha tan mui m v nh mc thnh 25mL bng dung dch
HCl 2%. Sau c th xc nh cc kim loi trong dung dch mu ny bng php o ph hp thu
nguyn t, pht x nguyn t hay phng php in ha
Cch ny thch hp cho cc loi mu c nhiu Si (hm lng Si>10%) v khi hm lng SiO3
trong mu ln th ta phi thm HF nhiu, gp hai hay gp ba s lng ni trn mi .
Phng php ny l da trn c s s thng hoa ca cht phn tch trng thi rn, khi chng ta
un nng mu phn tch ti mt nhit nht nh. Cht phn tch khi thng hoa s c ng
li trn y bnh ngng lnh.
V d: Xc nh hm lng iod trong b thi rn hay loi mu tng t. Ly 5g mu nghin
mn u vo cc thng hoa, thm 5g tinh th Al2 O3 v 2g CaO khan, trn u. Lp bnh ngng
ln trn cc thng hoa (hnh 3.12). un nh cho cht phn tch (iod) thng hoa, khi thy mu
nng chy th dng. Ly bnh ngng t ra ngui v nhng vo cc c sn 50mL benzen
ha tan iod. Ly dung dch benzen xc nh iod.
Hnh 3.12: Dng c thng hoa mu ly cht phn tch
CHNG VI:
X L MU XC NH CC CHT HU C
4.1. khi nim v phn loi mu hu c
4.1.1. mu hu c, cc loi v c im ca n
Mu hu c l cc loi mu m cht nn (matrix) ca mu l cc cht hu c. V d cc mu thc
phm, go, bt, thc vt, rau qu, cy l, sa, du m v.v. cc loi mu ny c th tn ti trng
thi rn, lng, kh, hay huyn ph. Cc mu hu c cng c c cc cht v c, cc cht kim loi,
chng tn ti trong mu dng hp cht c kim hay c hu c. V th c c xc nh cc cht hu
c v xc nh cc cht v c, cc nguyn t kim loi trong mu hu c. V d nh xc nh cc
thuc tr su dit c trong mu t nng nghip, l xc nh cht hu c trong mu v c. Nhng
trong mc ny ch yu trnh by cc k thut x l mu ly cc cht hu c trong cc i tng
mu hu c v v c khc nhau xc nh chng. Cht hu c c rt nhiu, song ngi ta phn
chia thnh cc loi sau y:
1. Cc loi hp cht hydrocacbua mch thng v mch vng.
2. Cc loi hp cht carbonyl (acid v aldehyd).
3. Cc loi hp cht amino acid, cc amin v vitamin.
4. Cc loi hp cht hu c c Halogen (Cl, Br) c nit.
5. Cc loi hp chy c kim loi
6. Cc loi hp cht d vng, c phosphor v nit v.v.
V d 3:Xc nh h clo-phenols trong mu rn, bt(nh thc phm hay mu t).Trc ht cng
phi xy mu thnh bt nho, trn u. Cn 5g mu vo phu chit, thm 20mL nc ct trn u,
chnh pH n 2 bng acid HCl 4M, lc u, thm 20mL dung mi dietyl-ete, lc chit mnh trong 5
pht, lng yn trong 5 pht.Sau tch ly lp hu c. Lp li s chit nh th mt ln na. Gp
pha hu c trong 2 ln chit li, lm kh bng Na2SO4 khan, ri chuyn vo bnh nh mc 50mL,
v nh mc bng dung mi chit. y l dung dch mu xc nh cc clo-phenols bng GC. Vi
cc loi mu nc nh nc thi, nc sng hLy 250mL mu, chnh pH v lm tip tng t.
Nu nng nh th ly 500mL mu.
V d 4:Xc nh h hp cht clo-phenoxy trong mu rn, bt(nh thc phm, t, bn, rau
qu.[Method 3221A]. Trc ht cng phi xy mu thnh bt hay bt nho, trn u, cn 5g vo
phu chit, thm 10mL nc ct, trn u, chnh pH n 2 bng acid HCL 4M, lc u, thm 20mL
dung mi dietyl-ete, lc chit mnh trong 5 pht, lng yn trong 5 pht.Sau tch ly lp hu
c. Lp li s chit nh th mt ln na. Gp pha hu c trong 2 ln chit li, lm kh bng 20-25g
Na2SO4 khan.Lm bay hi dung mi chit nh dng kh nit hay ct quay chn khng cn 1mL,
ngui v ho tan b rn ny trong 5mL MeOH ri xc nh bng HPLC,GCVi cc loi mu
nc nh nc thi, nc sng h,..Ly 250mL mu, chnh pH v lm tip tng t, nu nng
nh th ly 500mL mu.
V d 5:Xc nh h hp cht Carbamate trong mu rn, bt (nh thc phm, t, bn, rau qu)
[Method 8321A].Trc ht cng phi xay mu thnh bt hay bt nho, trn u.Cn 5g mu vo
phu chit, thm 10mL nc ct, trn u, chnh pH n 4-5 bng acid HCl 4M, lc u, thm
20mL dung mi Diclo-metylen (CH2Cl2), lc chit mnh trong 5 pht, lng yn 5 pht. Sau
tch ly lp hu c. Lp li s chit nh th mt ln na. Gp pha hu c trong 2 ln chit li, lm
kh bng 20-25g Na2SO4 khan.Lm bay hi dung mi chit nh dng kh nit hay ct quay chn
khng cn 1mL, ngui v ho tan b rn ny trong 5mL MeOH ri xc nh bng
HPLC,GCVi cc loi mu nc nh nc thi, nc sng h,..Ly 250mL mu, chnh pH v
lm tip tng t, nu nng nh th ly 500mL mu
4.2.2.2.2.A.Nguyn tc chung
Qu trnh chit y ch chit cch chit thng thng l khi chit mt trong hai pha l
chuyn ng lin tc, hay c th c hai pha cng chuyn ng nguc chiu nhau. Trong nu pha
chit (dung mi chit) c t khi ln hn dung mi (pha) cha mu nhiu, th s chit cng thun
li hn. V th qu trnh chit xy ra nhanh v hiu qu cao hn chit thng thung. Trong thc t,
ngi ta thung gi yn pha cha mu trong bnh chit, cn pha ng chit (dung mi chit) th
uc duc bm lin tc tun hon sc vo bnh chit, m khng phi lc chit k thut chit ny
hay uc dng trong chit sn xut, quy trinh chit cng ngh.
H trang b thc hin kiu chit ny c ch ra trong hnh 4.26. trong cng c hnh kiu n
gin ( simplet soxhlet ) v kiu t ng ( auto soxhlet ). Cc trang b ny hin nay hin nay u c
bn trn th trng v c cc mc chit khc nhau.
thc hin cch chit ny th phi c h chit kn ( hnh 4.28 ). Ngun cp kh tr tinh khit (
Nit hay Ar 99,99% ) v khng ch c tc dng mong mun. Cc trang b ca h chit theo
kiu ny hin nay c sn xut bi nhiu hng ch to dng c th nghim phn tch v c bn
trn th trng. Cc ct chit hay a chit c cha silica gel xp loi pha thng v pha ngc
cng c ch to v bn sn trn th trng. Cc ct chit ny thng c dung tch cht chit t 6
10 ml.
V d 2:Chit tch cc hp cht cacbonyl(aldehid hay aceton) d bay hi trong khng kh [Method
0011 v 0100].Mu khng kh c dn vo ct chit silicagel(ct chit bng silicagel xp c
ch ho trc vi dung dch nc ca 2.4-dinitro-phenylhyrazin, pH=2)vi tc 3-4 l/pht.Trong
qu trnh ny aldehid c gi li trong ct chit theo tnh cht hp ph ca silicagel, v to ra cc
sn phm th ho ca cc aldehid.V d nh fodmandehyd dinitrophenyldazzone.Sau cht phn
tch trong ct chit c ra gii ra khi ct bng 10mL dung mi acetonitril hay diclomethane, v
xc nh cc cht trong dung dch ra ny bng phng php HPLC,GC, hay ph UV-VIS.
V d 2: Tch chit nhm Aflatoxins ( B1, B2, G1, G2) t ht u v lcly 5g mu v xay
thnh mnh nh, cho vo ct v thm 50 ml ca hn hp MeOH/ H2O ( 85/15 ), lc 10 pht, lc
ly dung dch thm 30g Na2SO4 khan, lc u chit tch b cc cht bo bng 50 ml n hexane.
Ly dung dch MeOH di qua ct chit vi tc 1ml/pht.Sau ra gii cht phn tch ra
khi ct chit bng 10 ml hn hp CHCl3/CH3CN ( 60/40 ). Ly dung dch ra gii ny xc
nh bng phng php HPLC hay GC.
V d 3: Chit tch xc nh mt s cht Polyciclio Aromatic trong cc loi mu nc [
methode 5501 ]. Ly 500 ml mu chnh pH = 3 5, lc b cn ri di qua ct chit vi tc 2
5 ml/ pht, sau ra gii cht phn tch ra khi ct bng Acetonitril.y l dung dch mu
chit cc cht thuc h Hydrocacbon thm a vng nh Acenaphthene,
Acenaphthylene,Antracen, benzo antracene,pyrene Cch ny cng p dng cho mu rn v
nho nhng trc ht phi chn 1 dung mi ph hp nh ha mu thnh th huyn ph, hay ha
tan thnh dung dch c th cng tt lm kh n bng Na2SO4 khan sau ly dung dch ny
di qua ct chit.
Thiu trang 24
K thut chuyn ha ha hc
4.2.2.4A. Nguyn tc chung:
Dng mt loi phn ng ha hc ca cht phn tch vi mt thuc th c tnh cht nh lng
trong mt iu kin thch hp, to ra mt sn phm l mt cht bn, tch cht phn tch ra
khi mu dng sn phm ca phn ng . Sau xc nh n trong sn phm . Cch ny
thng kt hp vi phng php sc k, m ch yu l tch ly mt s cht thuc h aldehid
mch thng. V bn cht y chnh l phng php th ha trong sc k tch v xc nh cc
cht khng c tnh cht sc k tt.
iu kin y l phn ng chuyn ha phi:
+ c tnh cht nh lng.
+ Thuc th c kh nng tng tc vi mt nhm, hay mt cht phn tch.
+ Qu trnh th ha hay chuyn ha ny thng xy ra trong ct sc k, hay trong vng phn
ng v phi nhanh.
Theo khi nim trn th mu mi trng l rt a dng v ngun sinh ra n cng rt khc
nhau. Song theo trng thi tn ti, ngun sinh ra ca n, ngi ta tm chia thnh cc loi
nh sau:
V th phi ly mu theo mt quy trnh chun nht nh (Quc gia hay Quc t). Cc vn
ny c trnh by cc mc trn khi ni v mu phn tch v mu mi trng. V trong
phn tch th mu mi trng cng ch l mt loi hay mt nhm ca cc mu phn tch m
thi.
2. Cc phng php x l mu v v d:
Mc ch ca x l mu ca i lng mi trng l :
1. Xc nh cc nguyn t kim loi, nht l kim loi c hi
2. Xc nh mt s kim (As, Se, Te) v anion (Cl, Br, I, NO2, SO2,)
3. Xc nh mt s cht hu c, nht l cc cht c hi
4. Xc nh mt s vi sinh v vi khun c hi
5. Xc nh cht rn l lng (trong nc v khng kh)
6. Xc nh cc sinh vt ph du (trong nc)
7. Xc nh mt s kh (CO2, SO2, NO2, NH3) trong nc v khng kh
8. Xc nh hm lng oxy (DO, COD, BOD trong nc)
Mu mi trng l rt a dng v khc nhau, nn cch x l cng c nhiu cch khc nhau, ty
thuc vo mi loi, v vic x l l theo mi mc ch phn tch c th ring. Sau y l mt vi v
d c th minh ha mt s cch hay phng php x l ang c ng dng. Cc k thut hay
phng php c dng x l cc mu phn tch, cng c ng dng cho mu mi trng
phn tch cc cht. l cc phng php c trnh by trong mc 2.4 chng II v sau y
ch l mt s ng dng
2. Trc tin l phn tch, pht hin, v nh gi thc cht cc th gy nhim cho nc
thi, nht l cc cht vi sinh, vi sinh vt, xem cc th c hi mc no, ri c khuyn
co phng v x l.
3. X l nc thi loi tr nhng cht hay vi sinh vt, vi khun c hi.
4. Phn tch kim tra li nc sau kh x l.
5. Thi vo sng h hay dung li sau khi kim tra t yu cu.
(Xem cc bng A8, B1, B2, B4, phn ph lc 2 v 3)
Vic kim tra nh gi cht lng ca mt ngun nc thng phi xem xt theo mt s thng s
v yu t sau y:
1. Mu sc ca nc.
2. c ca nc.
3. o pH.
4. Hm lng cht rn trong nc, gm:
Tng cht rn ( )
Cht rn trong dng huyn ph ( )
Cht rn dng ha tan ( )
Cht rn c th bay hi ( )
Cht rn c th lng ng c ( )
5. acid hay kim.
6. cng ca nc (tm thi, vnh cu)
7. mui, mn.
8. Hm lng cc kim loi tan trong nc, nht l kim loi c hi.
9. Hm lng mt s kim v anion kim loi c hi (As, Se, F, NO2, CN, )
10. Hm lng Oxy ha tan (DO)
11. Hm lng Oxy sinh ha (BOD)
12. Hm lng Oxy ha hc (COD)
13. Hm lng Nito (N, NH2, NH3, NO2)
14. Hm lng du m
15. Hm lng mt s cht hu c c hi cho sinh vt v ngi:
+ Nhm khun Coliform (chnh l E-Coli)
+ Nhm khun Streptocxx (chnh l Streptocicus fecalis )
+ Nhm khun Clorstridca (chnh l Clostridium Perfringents )
V d 1 : X l mu phn tch kim loi nng c hi ( Cd, Co, Cr, Cu, Fe,Mn, Ni, Pb, Zn..)
Cc kim loi nng c hi thng c hm lng nh v gii hn cho php ca n cng nh.
Cho nn khi x l mu ngi ta thng kt hp lm giu lun. V th chit l k thut c nhiu u
vit trong i tng ny.
a/ Phng php 1: Chit thng thng (chit lng-lng) ly hm lng tng cc kim loi
nng ra khi mu ban u.
Chit bng: (APDC + MIBK) hay (APDC + CCl4)
Chit bng: (Ditizon + CCl4) hay (Ditizon + CHCl3)
+ Nguyn tc: (Xem mc chit pha lng-lng trn)
Dng thuc th to phc: APDC v dung mi chit l: CCl4 hay CHCl3 hay MIBK.
+ Cch tin hnh:
Ly 250 mL nc thi vo phu chit, acid ha n pH = 4 bng HCl.10%, thm 2 mL APDC
0.1%, thm 25 mL CCl4, lc chit mnh trong 5 pht. lng yn 5 pht, gn tch ly phn
dung mi hu c CCl4 xc nh cc kim loi. H s lm giu F = 10. Cng c th gii chit
kim loi trong pha hu c ny vo pha nc bng acid HNO3 3M, hay v c ha pha hu c, ri
ha tan tro bng acid ly kim loi v phn tch chng trong pha nc.
b/ Phng php 2: Chit pha rn (Rn-lng)
+ Nguyn tc chung: (Xem mc chit pha rn trn)
y l mt dng ca k thut sc k rn-lng (S-L), m cht chit l dng ht Silicagel v
xp. N tng t nh cc cht pha tnh ca sc k HPLC.
+ Cch tin hnh:
Chit tch lng vt cc kim loi kim: tch chit lng vt cc kim loi kim (Li, Na,
K), y ngi ta dng cht nhi kiu hp ph trao i ln ca hng Baker (Baker-10-SPE-
Column, Cat-No.7020-3). Sau khi ct chit c lm sch bng nc ct (10 mL), cho chy qua 10
mL HNO3 1N, sau ra sch li ct bng 10 mL nc ct. Ly 200 mL mu, acid ha n pH = 5,
lc b bn v np dung dch ln ct chit va chun b vi tc 2-3 mL/pht. Sau ra ct bng
2 mL nc ct. Ht chn khng ct bng phu lc Busmer trong 3-4 pht. Ri ra gii cc ion kim
loi ra khi ct (pha rn) bng 15 mL dung dch NH4NO3 2.5M, pH = 5.5. Khi pha ng chy ht
di ln ct 2 mL nc ct. Thu ly dung dch ra ny, lm bay hi cn mui m, them cht nn,
cht m v nh mc bng acid HCl 2% thnh 10 mL. y l dung dch mu xc nh cc kim
loi kim bng php o AAS hay ICP-AAS.
Chit tch lng vt cc kim loi nng: tch chit lng vt cc kim loi nng (Cd, Co,
Cr, Ca, Fe, Zn, Ni, Pb) t mu nc, y ngi ta dng cht nhi u hp ph ra ngc C18 ca
hng Baker (Baker-10-SPE-Column, Cat-No.7020-3). Sau khi ct chit c lm sch bng nc
ct (10 mL), cho chy qua 10 mL HNO3 1N, sau ra sch li ct bng 10 mL nc ct. Ly 200
mL mu, acid ha n pH = 4.5, lc b cn, ly dung dch them 3 mL thuc th APDC 0.1%, lc
u v cho chy vo ct chit va chun b vi tc 2-3 mL/pht. Sau ra ct bng 2 mL nc
ct. Ri ra gii cc ion kim loi ra khi ct (pha rn) bng 15 mL dung dch NH4NO3 2.5M, pH =
5.5. Khi pha ng chy ht di ln ct 2 mL nc ct. Thu ly dung dch ra ny, lm bay hi cn
mui m, them cht nn, cht m v nh mc bng acid HCl 2% thnh 10 mL. y l dung dch
mu xc nh cc kim loi kim bng php o AAS hay ICP-AAS.
V d 2: X l mu xc nh hm lng tng ca thy ngn (Hg). Ly 100 mL nc vo
bnh dung nn tch 250 mL, thm cn thn tng git n 10 mL H2SO4 98%, 2.5 mL HNO3
65% v lc u. Sau thm 2 mL KMnO4 2% v 8 mL K2S2O3 5%. Lc k sau 15 pht, nu
thy mt mu hng tm nht th nh thm vi git KMnO4 2% n xut hin mu bn. un cch
thy trong 2 gi, ngui n nhit phng. Sau kh cht oxy ha cn d bng dung dch
hydroxylamin 10%, n ht mu tm v ht c MnO2, thm 2 git K2Cr2O7 2%. y chnh l
dung dch xc nh Hg theo phng php AAS bng k thut to Hydrua. Cch ny cng
dung c x l mu xc nh Hg trong cc mu nc ngt, bia, v mi loi nc thi.
V d 3: X l mu xc nh hm lng tng ca arsen (As).Ly 200 mL mu vo bnh
Kendan, thm 5 mL H2SO4 98%, 5 mL HNO3 33%, b vo vi mnh s xp nh, chm vo bnh
mt phu nh di chui. un trn bp in n khi thy xut hin khi trng, ri ngui.
Chuyn hon ton mu sang cc 400 mL, trng bnh Kendan 2 ln bng 20 mL nc ct. Thm
40 mL dung dch LaCl3 5%, thm tng git dung dch NH4OH 12% n pH = 9. Ha tan kt ta
trn giy lc bng 20-25 mL HCl 25% nng, trng ra giy lc 3 ln bng 15 mL HCl 5%, thu
ton b dung dch vo bnh 100 mL v thm 4 mL KI 20%, lc u, nh mc thnh 100 mL,
lc u, un cch thy 20 pht, ngui. y chnh l dung dch xc nh Hg theo phng
php AAS bng k thut to Hydrua. Cch ny cng dung c x l mu xc nh Hg trong
cc mu nc ngt, bia, v mi loi nc thi.
V d 4: X l mu xc nh hm lng tng ca Selen (Se).
Ly 200 mL mu vo bnh Kendan dung tch 400 mL, thm 10 mL HClO4 70%, 5 mL H2O2
30%, cm vo bnh mt phu nh, un nh cho mu si, n khi no thy khi trng dy c
xut hin th ly ra v ngui. Chuyn ton b mu sang cc un 400 mL, thm 4 mL LaCl3
10 %, khuy u v thm dung dch NH4OH 25%, n pH = 10, khuy k v un cch thy 10
pht, lc qua giy bng ly kt ta La(OH)3 c hp ph Selen, ra kt ta 2 ln bng dung
dch NH3 c pH = 9. Ha tan kt ta bng 25 mL HCl 1M nng, thu nc lc v nc ra giy
lc vo bnh nh mc 20 mL v nh mc bng nc ct. y l dung dch mu xc nh
Selen. Cch ny cng dng c x l cc loi mu nc, nc thi xc nh Telu (Te),
cng nh cc mu nc ngt, bia, ru v mi loi nc thi.
V d 5: X l mu xc nh cc kim loi trong trng thi l lng trong nc.
Cc nguyn t kim loi hay cc ion trng thi l lng trong nc tc l chng khng tan trong
nc, m kt ta hay bm theo cc ht nh tng, cc ht rn nh, tn ti trong nc, lm cho
nc khng trong. V th nc cng khng trong th lha3 nng c cc ion kim loi cng nhiu.
V th xc nh hm lng ca cc kim loi tn ti cng vi cc ht khng tan trong nc,
trc ht phi tch c cc ht l lng bng cch lc hay ly tm cng vi cht ng t. Ly
200 mL nc vo bnh x l, thm 0.5 g cht ng t, lc u mnh, yn 20 pht, v ly tm
hay lc ly phn cn. Ha tan cn ny bng dung dch acid HCl 1/1 (6M) nng, thu dung dch
nay xc nh cc kim loi bng phng php AAS hay ph phn t UV-VIS
Phng php 1: Chit pha lng lng thng thng, xc nh cc clo-phenol (v d: 2- clo-
phenol, 2,4- diclo-phenol, 2,6-diclo-phenol, 2,4,6- triclo-phenol, 2,4,5- triclo-phenol, 3,4-
diclophenol, 2,3,4,6- tetraclophenol, Pentaclophenol). Ly 250 mL mu nc, kim h n
pH = 14, lc b cc cn b, dng 50 mL n-Hexan chit b cc cht bo v du m. Ly phn
dung dch nc, v acid ha n pH = 2, chit ly cc clo-phenol bng 20 mL dung mi
Dietylete. Lm bay hi dung mi bng ct quay chn khng hay bng dng kh nito nng, cn
li b m mu, ha tan trong 5 mL propanol v xc nh cc Clophenol bng phng php
HPLC v GC.
Phng php 2: Chit tch 1 s cht hu c thuc h Pesticide trong mu nc[ methode
3550b]. Ly 250 ml mu vo bnh chit chnh pH =2, thm 40 ml dung mi chit ( CH2Cl2 n
hexane theo t l V/V = 2/1 ), trn u, y np v t vo bung siu m, ng cht my siu
m, chn v t cc thng s siu m thch hp tin hnh chit trong 40 pht. ngui lc
hn hp mu ra tch pha, ly dung dch pha hu c, lm bay hi dung mi bng phng php
chng ct quay chn khng n khi cn 1 ml, ngui ta c b t. Ha tan b ny trong
5 ml dung mi MeOH hay n hexane. y l dung dch mu xc nh cc nhm Pesticide
bng phng php GC, HPLC hay GC MS.
Phng php 3: Chit pha rn. Chit tch 1 s cht hu c thuc h Pesticide trong mu nc[
methode 3550b]. Ly 250 ml mu vo bnh chit chnh pH =2,lc b cn ri di ln ct chit
loi XAD 2, 5 m vi tc 2 4 ml/pht, cho n khi chy ht mu qua ct chit.Sau
gii chit cht phn tch ra khi ct chit bng 20 ml dung mi n hexane c 15% CH2Cl2. Thu
dung dch ra ui cho ht dung mi bng dng kh tr sch n cn b m, ha tan b ny
trong 5 ml dung mi MeOH.y l dung dch mu xc nh cc nhm Pesticide bng
phng php GC, HPLC hay GC MS.
V d 4 : xc nh Cd, Co, Cr, Cu, Fe, Mn, Zn, Pb, Nitrong mu b thi rau qu v thc
phm. Ly 10g mu vo chn nung thm cht bo v l 2 ml Mg( NO3 )2 10%, 10 ml HNO3 65%,
trn u sy hay un nh cho kh dn v thnh than en. Nung 3 gi u 450 oC, sau 530oC
n khi c tro khng cn en ( ht than en ). Sau ha tan tro cn li bng 15 ml HCl 1M
nng, chuyn mu ht sang cc v un nh cho tan ht v ui ht axit d cho n khi cn mui m
v nh mc bng 25 ml bng dung dch HCl 2% lc u. Mu ny c xc nh cho c kim loi
kim v kim th.
Theo sch cch c trinh by trong chng 2 muc 2.4 chng ta p dng cho x l mu
b thi phn tch cc cht hu c
1. cc cht v c:
Cc kh CO, CO2, SO2, NO, NO2, Cl2,Br2, H2S, HCN
Cc hi kim loi ( Hg, Pb, Cd, Mn, Cr ), hi mui kim loi
Cc bi silic, amiang, xi mng, bt thy tinh
2. cc loi hp cht hu c.
Mt s hydro cacbua dng kh, aldehyd, alcol, axetylen, aceton..
Cc hp cht c kim, c nguyn t ca Pb, Hg, Cd, Mn, c Halogen
Cc ht cht hu c l lng, cc ht bi rn nh mn.
3. cc loi khi v bi
y l nhm b thi ht mn nh c thi ra khng kh, chng c th sa lng, song cng c th l
lng theo gi i khp ni, lm nh hng n s h hp ca ngi v ng vt n bao gm:
- Ca sinh hot con ngi, un than ci du.
- Ca cc ngnh cng nghip thi ra, in than, in mazut.
- Ca cc phng tin giao thng thi ra.
- cc loi bi ca bom n, pho cc bi phng x
- Nn t rng, dn t rng lm ry
V d nh ly cht phn tch kim loi nng c hi, hay phn tch Hg, As ngi ta thng ht
khng kh chy qua giy lc hp ph Whatman No 42 tm t ca hng Whatman vi 1 tc
thch hp trong 1 tjo2i gian nht nhi qua giy lc thng thng l trong vng 250 1000 lt v
vi tc 2 4 l/ ph. Khi cc ion kim loi nng hay nguyn t kim loi c trong khng kh s b
hp th v gi li trn giy lc ny. Sau ha tan giy lc, x l t bng axit oxi ha mnh nh
HNO3 H2SO4 l chng ta c mu xc nh cc kim loi trong khng kh. Nhng xc nh
cc nhm kh thuc nhn NO3-, SO42-, CO2 th chng ta phi hp ph chng vo cc dung dch thch
hp. V d dung dich NaOHloa4ng c nng nht nh . Ni chung mi loi cht phi c quy
trnh c th ring cho n [ TCVN. V ISO].
V d 1: X l mu xc nh cc lim loi nng c hi ( As, Cd, Co, Cr,Cu, Fe, Hg, Mn, Ni, Pb,
Se, Zn).Dng my ht ly 500 lt khng kh cn phn tch qua phu c giy lc Whatman ( No
42E ) vi tc 2l/ph cc ion kim loi v cc ht bi gi li trn giy. B giy c hp ph vo
bnh kendan, them 20 ml HNO3 65%, lc u, cm vo bnh 1 phu nh di chui v un trn bp
in cho dung dch mu si, ha tan ton b mu v giy n khi no c dung dch trong l
c. Thm 2 ml H2O2 30%, un tip 5 pht ngui bt chuyn hon ton mu sang cc 250 ml,
trng bnh v phu 2 ln bng 15 ml nc ct. un si v lm bay hi n ht axit khi cn mui m.
Ha tan mui m ny bng 10 ml HCl 10%, nh mc thnh 25 ml. l dung dch mu xc
nh cc nguyn t ni trn v cc kim loi kim v kim th. Cch ny nu x l trong l vi song
th cng tt.
V d 1: chit tch cc hp cht carbonyl ( aldehyd v ceton ) bay hi trong khng kh. Mu
khng kh c dn chit vo ct chit silicagel xp c ch ha trc vi dung dch ca 2,4
dinitrophenylhydrazin , pH=2 vi tc 3 4 l/ph. Trong qu trnh ny cc aldehyd c gi li
ct chit tnh theo cht hp ph ca silicagel v to ra cc sn phm th ha ca aldehyd. V d nh
formaldehyde dinitrophenylhydrazone c gi li trn ct. Sau cht phn tch c ra gii
trn ct bng 10 ml acetonitril hay diclomethane v xc nh cc cht trong dch ra ny bng
HPLC, GC hay ph UV VIS.
V d 2: chit tch cac cht bo v thc vt trong khng kh nh my sn xut cc kh ny. Mu
khng kh.Mu khng kh c dn chit vo ct chit VDL silicagel vi tc 3 4 l/ph. Trong
qu trnh ny cc pesticide c gi li ct chit tnh theo cht hp ph ca silicagel ny. Sau
cht phn tch c ra gii trn ct bng 10 ml diclomethane c 20% n hexane v xc nh cc
cht trong dch ra ny bng HPLC, GC hay ph UV VIS.
2.5.4. X l mu xc nh mt s cht hu c