TRNG I HC CNG NGHIP TP.

HCM
KHOA CNG NGH HO HC

N HC PHN
KHO ST KH NNG KH CA CC TC NHN KH
ACID ASCORBIC V THIC CLORUA I VI PHC
GIA PHOTPHO V MOLIPDOVANADAT

Ging vin hng dn: Ths. TRN NGHUYN AN SA

Sinh vin thc hin:TRNG PHM BNG DNG
NGUYN NGC NHUNG
Lp:

DHPT6LT

Kho:

2010 - 2012

TP. H Ch Minh, thng 12 nm 2011

`TRNG I HC CNG NGHIP TP.HCM

CNG HO X HI CH NGHA VIT NAM

KHOA CNG NGH HA HC

c lp T do - Hnh phc

NHIM V N HC PHN

H v tn sinh vin:

MSSV
TRNG PHM BNG DNG

10335991

NGUYN NGC NHUNG

10335971

Lp: DHPT6LT
Chuyn ngnh: Ha Phn Tch
Tn n hc phn: Kho st phc gia photpho v molipdovanadat.
Nhim v ca n hc phn:
1.

Tng quan v photpho

2.

Tm hiu v cc phng php xc nh photpho

3.

Tm hiu v cc tc nhn kh thng dng trong xc nh phc gia

photpho v molipdovanadat

4.

cng thc nghim v d ton kinh ph thc nghim

Ngy giao n: ngy 6 thng 10 nm 2011

Ngy hon thnh n: ngy

thng

nm 2011

H tn gio vin hng dn: ThS. Trn Nguyn An Sa

Tp. H Ch Minh, ngy 24 thng10 nm 2011
Ch nhim b mn

Ging vin hng dn

LI CM N

Li u tin nhm chng em xin gi li cm n chn thnh v su sc n

thy c Khoa Cng Ngh Ha Hc to iu kin cho chng em thc hin n.
Chng em xin chn thnh cm n thy c trong ban gim hiu nh trng, qu thy
c trong kkhoa a truyn at cho chung em nhng kin thc quy bau trong sut thi
gian va qua va a tao iu kin tt nht cho chung em chung em co th hoan
thanh an nay mt cach tt nht.
ng thi chng em xin chn thnh cm n c Trn Nguyn An Sa nhit
tnh ch bo v hng dn, to mi iu kin thun li cho nhm chng em trong
sut thi gian thc hin n.
Trong qu trnh thc hin n ny chc chn chng em khng th trnh khi
nhng sai st. Knh mong qu thy c v cc bn nhit tnh ng gp ti ny
ngy cng hon thin hn.
Nhm chng em xin gi n qu thy c li chc sc khe.
Chng em xin chn thnh cm n!

ii

NHN XT CA GING VIN HNG DN

.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.........................................................................................................................................
Tp. H Ch Minh, ngy

thng

GING VIN HNG DN

iii

nm 2011

NHN XT CA GING VIN PHN BIN

.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.........................................................................................................................................

iv

MC LC

NHIM V N HC PHN ........................................................................................i

LI CM N........................................................................................................................ii
NHN XT CA GING VIN HNG DN...............................................................iii
NHN XT CA GING VIN PHN BIN..................................................................iv
MC LC..............................................................................................................................v
DANH MC BNG BIU, S , HNH V..................................................................vi
LI M U......................................................................................................................vii
CHNG

TNG QUAN V PHOSPHO V CC TC NHN KH..............................................1

1.1. Tng quan v phospho....................................................................................................1
nh ngha phospho...............................................................................................................1
Vng tun hon ca phospho.................................................................................................1
Ngun gc, vai tr v chc nng ca Phospho......................................................................6
Tnh cht ca phospho............................................................................................................8
Axit H3PO4 ca chnh qu trnh ( tch flo) c cho tc dng vi vi nghin trong my
nho lin tc. Bn sn phm c sy kh, sng v ng bao. Cc phn ht qu mn hoc
to c quay vng tr li ....................................................................................................12
CHNG

CC PHNG PHP XC NH PHOTPHO.................................................................13

. Phng php xc nh cc hp cht ca phospho..............................................................13
CHNG

CNG THC NGHIM............................................................................................20

TI LIU THAM KHO.....................................................................................................ix

DANH MC BNG BIU, S , HNH V

vi

LI M U

Nh chng ta bit phospho tham gia vo qu trnh cu to ca xng, n

c s dng sn xut ra nng lng v hot ha nhiu hot ng sinh thi, l
cht khong c nhiu nht trong c th sau calci
Trong c th phospho c khong 80% trong xng, 10% trong c, 10% trong
cc m mm khc. l mt phc hp nng lng sinh hc c nhim v cung cp
nng lng , l nguyn t thit yu cho cuc sng.
Nu hm lng phospho trong c th tha th dn n c th c nhng tc
dng m tnh, hm lng calci gim i th dn n hin tng long xng v th ta
nn chn lc nhng thc n t c hm lng phospho cho c th.
Ngoi ra cn c mt s hp cht ca phospho c th iu ch phn bn, dng
trong thuc nh rng....

vii

CHNG 1
TNG QUAN V PHOSPHO V CC TC NHN KH

1.1. Tng quan v phospho

nh ngha phospho
T ting Hy Lap: phos c ngha l nh sng v phoros ngha l ngi/vt
mang, l mt nguyn t ha hc trong bng h thng tun hon c k hiu P v s
nguyn t 15. L mt phi kim a ha tr trong nhm nito, Phospho ch yu tm
c trong cc loi phosphat v c v trong c th sng. Do hot ng cao,
nn khng bao gi tm thy n dng n cht trong t nhin. N pht x nh sng
nht khi b phi ra trc oxy v xut hin di mt s dng th hnh, l nguyn t
thit yu cho c th sng. S dng n quan trng nht trong thng mi l sn xut
phn bn v n cng c s dng rng ri nht trong vt liu n, dim, pho hoa,
thuc tr su, thuc nh rng, cht ty ra...
Vng tun hon ca phospho
Phospho l mt trong cc nguyn t rt cn thit cho s sng. Trong v tri
t phtpho l nguyn t ng v tr th hai. Ha hc mi trng ca phospho
khc vi cc nguyn t phi kim loi khc ch cc phn ng kh ng vai tr
khng n nh. Lin kt phospho t nhin (P2O5) cha nguyn t phospho ha tr
+5, y l dng lin kt bn vng vi oxy (E D > 500kj/mol) song v c tnh in t
v phn t lng ln m hp cht phospho t nhin c p sut hi rt nh. Do
trong kh quyn thnh phn phospho rt t c ngha. Nn tng ca lin kt phtpho
trong mi trng l axit phosphoric H3PO4 vi hng s phn ly pK1 = 2,15; pK2 =
7,20 v pK3 = 12,35 250C. N to thnh khng t hn 200 loi khong tn ti
trong t nhin, trc ht l vi cc cation nh Na+, Mg+2, Ca+2, Al+3, Pb+2, Fe+2, Fe+3,
Mn+4, Cu+2, Zn+2, Th+4, UO2+2 v nhng nguyn t h lantan, trong ch c mt s
canxi phosphate l c ngha nh l nguyn liu ca ngnh cng nghip phtpho
(Bng 1). Khong 95% ngun phospho trn th gii tn ti di dng cc

fluorapatit. Phn hy phtpho qua xy ha kt hp vi nc to thnh axit

ortohophtphoric (H3PO4) sau thnh cc mui ortohophosphate. Phosphate ny
l dn xut ca cc axit phtpho dng chung Hn+2PnO3n+1 (n = 2 iphospho axit, n =
3: triphosphoaxit) v cha cu lin kt P - - O - - P.
V d:

2HPO4-2

P2O7-4 + H2O.

Axit phospho c th lin kt vi cc hp cht hu c hydroxyl l nhng hp

cht c ngha nn tng trong tt c cc h thng sinh hc. V d v mt s hp
cht hu c phtpho nh adenosintriphosphate, hp cht uridintriphosphate v
cytidintriphosphate.
Vng tun hon phospho bao gm cc qu trnh trao i phospho gia cc
phtphate v c v hu c trong qu trnh sng ca sinh vt. Theo mt s tc gi th
vng tun hon sinh ha ca phtpho c th tch ra thnh hai phn ring: t cy
trng v nc cn lng v hai phn ny trao i cht vi nhau rt t. iu ng ch
l mt phn phtpho thng qua s dng sinh hc v dn dng c phn tn
mt cch chm chp v mt s c gi li trn b mt Tri t hoc lng di
bin.

Hnh 1. 1. Vng tun hon ca P trong t nhin

Cn bng H2O H3PO4 ph thuc vo pH, gi tr pH = 7 tn ti cn bng
sau: H2PO4- = HPO4-2 + H+
Trong a quyn v thy quyn, cc ion kim loi nh Ca+2, Fe+3, Al+3 c kh
nng lin kt d dng vi phtpho. S ph thuc ca ha tan ca cc phosphate
kim loi vo pH rt c ngha i vi qu trnh kt ta phtphate trong cc h nc
ngt c hin tng ph dng (eutrophication). Nng phosphate thc t cao hn
2

nhiu so vi nng trng thi cn bng tng ng. iu ny c th l do nh

hng ca mt s ion l c kh nng ha tan tt hoc l do qu trnh kt tinh hoc
lin kt xy ra chp chp.
Lin kt ca cc ion kim loi vi phosphate to thnh t bc qu ca cc
phn ng kt ta v phn ng b mt. Qu trnh hp th phosphate bng nhm
hydroxyt, st hydroxyt hoc cc oxit ngm nc tun theo c ch lin hp v t
cc t cc i gi tr pH m ti tn ti dng ion H 2PO4-. Bc qu chuyn
sang mi trng kim c tc dng nh l qu trnh kh hp ph. c trng tng
hp qu trnh chuyn pha ca phtphate t pha lng sang pha rn l t l gia kim
loi v phospho trong sn phm kt ta. T l ny thng ln hn 1, kt qu l mt
phn ln phosphate a vo t di dng phn bn khng chuyn ha c thnh
cht dinh dng. V vy ty theo tnh cht ca tng loi t m phn phosphate
theo phn bn c th b gi li, khng c tc dng tch cc.
Dung dch nc ca cc sn phm phn ly ca H3PO4 ph thuc nhiu vo gi
tr pH nhng hnh thi H3PO4 (O), H2PO4- (1), HPO4-2 (2), PO4-3 (3). Trc ht cc
gc thc vt s hp th H2PO4- v HPO4-2. pH 6 bt u c s c nh phosphate
vi lin kt Fe+3 v Al+3 ch yu dn ti kt ta cc phosphate kim ca Fe+3 v Al+3
(M(PO4)6(OH)3(1-X), vi M l nhm hoc st). Qu trnh hp ph trn b mt cc oxit
ngm nc hoc keo l nh cc sn phm thy phn. pH 7 bt u kt ta cc
caxiphosphate nh CaHPO4 hoc cc hdroxylapatit Ca10(PO4)6(OH)2. Do khi s
dng phosphate lm cht dinh dng cho thc vt th yu cu gi tr pH trong mt
gii hn hp, v nu iu kin khng thch hp cc phosphate s b gi li trong
t.
Cc phosphate trong ngun nc chy hoc ngun tnh thng l ngun gc
dn n hin tng ph dng. Nhng cht ny c th l cc cht ty ra hoc cht
lm mm nc cng i vo thy quyn, nh pentanatripolyphosphate (Na5P3O10).
Ngoi ra cn c mt s cht nh st phtphate t cc lp cn lng c th b ha tan
tr li khi trong cc ngun nc c cha nhiu cht dinh dng v cht nhim c
th tn ti cc iu kin kh hoc gi tr pH thp, qu trnh c th xy ra theo
3

phng trnh sau:

Fe(PO4)r + H+ + e- = Fe+2 (nc) + HPO4-2 (nc)
Cht kh c th l H2S hoc cc hp cht hu c trong nc.
Nc bin vi pH = 8,1 l mt iu kin tt kt ta PO4-3. Nng
phospho tnh ton theo l thuyt cn bng pha vo khong 1,1 g/l. Nhng thc t
th nng phtpho trong nc bin ln hn nhiu, l do qu trnh ha tan tr
li ca cc keo phospho hoc cc hp cht hu c phtpho. Nng phospho trong
nc bin tng dn theo chiu su ca bin so vi lp b mt. iu ny c th gii
thch rng cc sn phm sinh hc cha phtpho di lp nc su ca bin s b
hn ch do cc tia mt tri khng ti c tham gia qu trnh tng hp.
1.1.1 Cc hp cht ca Phospho.
1.1.3.1 Phospho
Phospho l mt dng th hnh ca phtpho nhng l cht tr, khng c cc
hot tnh c bit nh ca P trng. Phtpho c ch to t phospho trng v
c xem l an ton.
Trc y, trong qu trnh s dng P ngi ta thy n gy ra mt s tc hi
sc khe, nguyn nhn l do trong P c ln P trng, c xem l tp cht
nhim.
P ch yu c dng trong cng nghip dim, ch to pho hoa, pho lnh,

1.1.3.2 Phosphin (PH3).

L cht kh khng mu, tinh khit khng mi (mi ti khi to thnh t

phtphua). T trng 1,175; si -87,4 oC; nng chy -132,5 oC.
Rt t tan trong nc, tan nhiu trong cn v te. N c th ha lng v chy
vi ngn la mu xanh sng.
Rt c, tc dng ln h thn kinh trung ng gy hn m. Gy kch ng phn
da h, nim mc mt, ng h hp, gy xut huyt phi.
1.1.3.3 Axit Phtphoric (H3PO4)

Axit phosphoric (H3PO4) cn gi l axit orthophosphoric, l mt cht lng,

trong snh, tan trong nc v cn. Phn t lng : 98; t trng : 1,83; im nng
chy : 42,3 oC; im si : 213oC (mt H2O)
Axit phosphoric l mt axit tng i mnh, c dng nhiu trong cng
nghip phn bn superphosphate. N c dng lm sch b mt kim loi trc
khi sn, nu c ln tp cht c th sinh ra hidro, t c th to ra mt kh cc
c l PH3
Nu b axit bn vo da hoc mt th ngay tc khc phi ra vi nhiu nc ti
ngun gn nht trc khi a nn nhn i cp cu.
1.1.3.4 Phospho pentaoxit (P2O5)

Cn gi l anhirit phosphoric, phosphoric pentaoxit, l mt bt trng, chy ra

trong khng kh, tan trong H2SO4, phn hy mnh m trong nc. Phn t lng :
142; t trng 2,39; im nng chy 569oC
c dng trong tng hp hu c lm tc nhn kh nc. N c tc dng n
mn i vi mt, nim mc, da. Ht phi hi phospho pentaoxit c th b ph phi.
1.1.3.5 . Phospho pentaclorua (PCl5)

L mt khi kt tinh, bc khi, m hng cay, kh ngi. Phn hy trong nc,

tan trong CS2, CCl4. Phn t lng : 208,2; t trng 4,64
c dng trong tng hp hu c. Phtpho pentaclorua phn hy to thnh
axit clohirit v axit phtphoric
Phtpho pentaclorua tip xc vi khng kh to ra khi n mn, rt nguy him
vi mt, nim mc v da. Ht th phi khi c th gy ph phi. Khi tip xc vi
da cng lm bng da.
1.1.3.6 . Phospho oxiclorua (POCl3)

Cn gi l phosphoryl clorua, l cht lng mu vng nht, mi kh ngi. Phn

t lng: 153,4; t trng 1,67; im nng chy: 2oC; im si: 105,3oC
c dng lm tc nhn clo ha cho hp cht hu c. Tnh cht ca n nguy
him nh phospho pentaclorua
1.1.3.7. Phospho triclorua (PCl3)
5

L cht lng khng mu, bc khi, tan trong dung mi hu c. N phn hy

trong nc, gii phng nhiu nhit.
c dng sn xut phtpho pentaclorua (PCl5) l tc nhn clo ha
Phospho triclorua l mt cht cc k n mn khi m. Nu un nng s to
thnh PH3. Phn ng mnh vi kim. Phospho triclorua l mt cht gy chy, n.
Tnh cht nguy him nh PCl5 nn khi tip xc phi rt thn trng d phng.
1.1.3.8. Phospho sesquisunfua (P4S3)
Cn gi l tetraphospho trisunfua. L cht kt tinh mu vng, tan trong nc
lnh, phn hy trong nc nng, tan trong mt s dung mi hu c. Phn t lng:
220,26; t trng 2,03; im nng chy: 1,74oC; im si: 408oC
Hin nay cht ny c dng nhiu trong cng nghip dim, lm u que
dim hoc bn sn hp dim (ht qut) nh dim (qut)
Tuy l cht tng i t c, nhng ht phi hi ca P 4S3 cng gy kch ng
cc nim mc.

Ngun gc, vai tr v chc nng ca Phospho

1.2.1 Ngun gc
Cc vi sinh vt bin nhn mt lng ng k phtpho t cc ngun thc phm
hoc cc c th cht di dng phtpho kh ha tan hoc photphate v c ha tan.
Ch mt phn nh phtphate di t (5%) l c th c cy trng hp th v ch
c ihydrogenphotphate (H2PO4-) c th ha tan tt trong nc. Cc photphate v
c kh ha tan s tn ti trong t v sau ny c th b cc axit nh axit limonic,
axit sunfuric ha tan v i vo thnh phn ca nguyn sinh ng vt. Cc phospho
tn ti cc gc r cy trng, s t t thy phn dng cc khong vi sinh do qu
trnh phtphate ha.
Lng photphate trong h sinh thi nc v sinh vt trn cn khng cung
cp dinh dng cho cc thc vt (lng phtphate ny ch vo khong 0,5 5%
khi lng, cho nn phtpho thng c biu th nh l cht dinh dng hn nh.
S thiu ht ny c b sung bi cc hot ng nhn to nh vic sn xut cc
phn bn photphate t cc qung photphate (superphtphate, isuperphtphate,
6

NPK .). Lng phtpho d trong phn bn thm qua t, qua sng ra bin v
lng . Trong nc ma nng c t 10 100 mg/m 3 ( do bi, mui bin bc
hi, cc qu trnh c nhit cao v qu trnh chuyn ha phtpho trong kh
quyn).
Ngun pht sinh phospho bao gm: trong t nhin, sn xut bom, n, sn
xut ha cht, phn bn, thuc bo v thc vt, cht thi, cc cht bi tit ca ng
vt, trong bn thi ca h thng x l nc thi.
Ht cc, sa, bt c v bt tht c xng l ngun cung cp P rt tt, trong khi
c kh v rm r cha rt t P. Cm go cha nhiu P trong khi bt sn cha rt
t.
Phospho cng c vn kh quan trng v hiu sut s dng. Phn ln
phospho ht ng cc v nht l cm dng phytate l mui ca axit phyric.
So vi phosphat v c nh dicanxi phosphat tha mc s dng phytat canxi
g con l 10%, g 50%, ln 30% v nhai li gn 90%. B s dng c nhiu
phytat nh c phytaza ly t thc n thc vt.
1.2.2. Vai tr ca phospho.
Phospho tham gia vo qu trnh cu to xng. N c s dng sn xut
ra nng lng v hot ha nhiu hot ng sinh thi . Tuy nhin, nhiu phospho
trong thc phm c kh nng gy ra nhng tc dng m tnh.
Phospho l cht khong c nhiu nht trong c th, sau calci: ngi ln nng
70 kg, s c 700g phospho trong c 80% c trong b xng, 10% trong c, 10%
cc m mm khc, c bit di dng phc hp phosphoprotein, phospholipid.
l mt phc hp nng lng sinh hc c nhim v cung cp nng lng
ATP cho chng ta, cng nh tham gia vo qu trnh hot ha trong yu t dinh
dng s iu ha cc hot ng ny.
1.2.3. Chc nng ca phospho.
Phospho l cht khong c nhiu chc nng hn bt k cht khong no khc.
Phospho ngoi nhim v to xuong cn c nhim v khc nh tahm gia vo lin kt
7

cao nng ca ATP, trong qu trnh tng hp phospholipit ca mng t bo, ca t

chc thn kinh, trong RNA v DNA v trong qu trnh tng hp protein v di
truyn do RNA v DNA.
Triu chng thiu phospho: trong thc n thng thiu phospho hn l canxi.
Nguyn nhn chnh l do thiu P trong t nn hm lng P trong cy trng thp.
Trn th gii rt nhiu vng t thiu P c bit l nc nhit i .
Thiu phospho gy ra nhng triu chng hoc bnh tt ch yu sau y: gy
bnh mm xng v xp xng nh thiu canxi.
Triu chng kinh nin nh khp xng cng v tht nho.Gim sn lng sa,
gim t l th thai, sinh trng chm. Nhiu ti liu cho l b sung P lm tng t l
th thai ca b chn th
Triu chng thiu phospho th hin trn cu nhiu hn trn b v cu c thi
quen chn la khi n. Cu thng chn nhng phn thc vt non ang sinh trng
phn cha hm lng P thp hn.

Tnh cht ca phospho

1.2.2 Tnh cht vt l
Phtpho (P) l mt nguyn t c nhiu trong t nhin di dng qung. sinh
vt, Phospho c vai tr quan trng, c nhiu trong xng ng vt di dng canxi
phtphate, trong no, lng trng, di dng hp hu c.
Phtpho l mt kim, nguyn t lng 31, t trng 1.83, im nng chy 94 oC,
im si 278oC, khng tan trong nc, tan trong dung mi hu c. L mt cht rn,
d gy nhit thng, mm d un, c ba dng th hnh l trng (vng), v
phtpho pryromorphic.
Dng ph bin ca phospho l cht rn dng sp mu trng c mi c trng
kh ngi tng t nh ti. Dng tinh khit ca n khng mu trong sut. Phi kim
ny khng ha tan trong nc. Phospho tinh khit bt chy ngay trong khng kh v
to khi trng cha pentoxit phospho.
Phospho tn ti dui ba dng th hnh c bn: trng, v en. Cc dng th
8

hnh khc cng c th tn ti. Ph bin nht l phospho trng v phospho c hai
u cha cc nhm phn b kiu t din ca phospho trng to thnh cc nhm
ring. Cc t din ca phospho lin kt vi nhau thnh chui. Phospho trng
chy khi tip xc vi ngun nhit v nh sng.
Phospho cng tn ti trong cc dng a thch v mt ng hc v nhit ng
lc hc. Chng c tch ra nhit chuyn tip -3.8OC. mt dng c gi l
alpha dng kia c gi l beta. Phospho l tng i n nh v thng hoa
p sut 1atm v 170OC nhng chy do va chm hay do ma st. Th hnh phospho
en tn ti v c cu trc tng t nh graphit, cc nguyn t c sp xp trong
cc lp theo tm lc gic v c tnh dn in. Cc ng v phospho gm: p 32 : cht
to bc x bate (1.71 MeV) vi chu k bn r 14.3 ngy. N c dng trong cc
phng th nghim khoa hc nghin cu v s sng ch yu to cc mu ADN v
ARN nh du phng x, v d s dng trong cc phng php nh du
Northern hay nh du Southern. Do cc ht beta cao nng lng c to ra thm
nhp qua da v gic mc, v do bt k lng P32 no i vo c th theo cc ng
tiu ha, h hp hay hp th qua qua cc ng khc u kt hp li trong xng
v cc nuleic, yu cu l mi ngi lm vic tip xc vi P 32 bt buc phi dng
qun o bo h v gng tay bo h. Ngoi ra do nng lng cao ca cc ht beta ,
thng thng ngi ta hay s dng vt che chn (chng hn ch), nhng u ny
to ra bc x th cp tia X. V th tm che phi km theo vi vt liu nh nh,
plexiglas, acrylic, cht do, g hay nc.
P33: cht to bc x beta (0.25MeV) vi chu k bn r 25.4 ngy. N thng
dng trong phng th nghim khoa hc v s sng trong ng dng m bc x beta
thp nng lng l u th hn, v d sp xp chui ADN.
1.2.3 . Tnh cht ha hc.

nhit thng th P c tnh kh yu, nhit cao th tnh kh mnh

2P + 5/2O2 = P2O5
P c tnh oxi ha yu n ch tc dng vi kim loi nhm IA, IIA, IIIA
P + Na = Na3PO4
9

P trng c tnh oxi ha mnh hn v en.

1.3 ng dng.
1.3.1 . Trong nng nghip

Acid phosphoric m c, c th cha ti 70% - 75% P 2O5 l rt quan trng

vi ngnh nng nghip do n c dng sn xut phn bn. Nhu cu ton cu v
phn bn dn ti s tng trng ng k trong sn xut phn bn (PO 43-) trong
na sau th k 20..
1.3.2 Trong cng nghip
Tro xng, phosphat can xi c s dng trong sn xut s.
Tripolyphophat natri c sn xut t acid phosphoric c s dng trong bt git
mt s quc gia, nhng li b cm mt s quc gia khc.
Acid phosphoric c sn xut t Phospho, nguyn t c s dng trong cc
ng dng nh cc ung cha soda. Acid ny cng l im khi u ch to cc
phosphat cp thc phm. Cc ha cht ny bao gm phosphat monocanxi c
dng trong bt n v tripolyphosphat natri v cc phosphat khc ca natri. Trong s
cc ng dng khc , ha cht ny c dng ci thin c trng cho tht hay pho
mat ch bin. Ngi ta cn dng n trong kem nh rng. Phosphat natri c
dng trong cc cht lm sch lm mm nc v chng n mn cho dng ng,
ni hi.
Phospho c s dng rng ri sn xut mt s hp cht hu c cha
phospho, thng qua cht trung gian nh clorua phospho v sulfua phospho. Ngoi
ra, Phospho c nhiu ng dng khc, bao gm cht lm do, lm chm chy, thuc
tr su, cht chit v cc cht x l nc.
Nguyn t ny cng l thnh phn quan trng trong sn xut thp, trong sn
xut ng thau cha phospho v trong nhiu sn phm lin quan khc.
Phospho trng c s dng trong cc ng dng qun s trong bom la, to ra
cc mng khi nh trong cc bnh khi v bom khi, v trong n la.
Phospho c s dng sn xut cc bao dim an ton , pho hoa v nht
10

l metamphemin (C10H15N).
Vi lng nh, phospho c dng nh l cht thm vo cho cc loi bn dn
Phospho P32 v phospho P33 c dng nh l cht pht hin du vt phng x
trong cc phng th nghim ha sinh hc.
Cch s dng khc cn c: cc phosphat c dng trong sn xut, cc loi
thy tinh c bit c s dng trong cc loi thy tinh n hi natri
1.3.3 Trong chn nui
gim gi thnh sn xut thc n gia sc, ngi ta thng s dng xng v
cc ph thi khc ca gia sc lm ph gia cung cp phospho v canxi. Tuy nhin,
vic s dng cc ph thi ny c nguy c l lm nhim khun thc n v gy c
cho gia sc. Nhng lo ngi hin nay chu u v dch b in, m ngi ta qui cho
vic s dng ph thi ngnh git m lm thc n gia sc, khi li mi quan tm
v cc quy trnh sn xut nhng ph gia phtpho v c t qung phosphate t
nhin.
Phospho l thnh phn quan trng ca thc n gia sc, n rt cn thit cho s
pht trin khe mnh, tc cng ca xng v tc ng tt n cc qu trnh trao
i cht.
Hm lng phospho trong thc n t nhin ca gia sc (la, ng, u tng...)
tng i thp ch khong 0,2 - 0,5% (trong khi t l phtpho cn thit cho thc n
chn nui phi c 0,3 - 0,7%). V vy, ngi ta phi b sung phospho t cc ph gia
khc.
Thc n gia sc c sn xut t cc ph phm git m v bt c c hm
lng P khong 3,0 - 3,4%. Tuy nhin loi ny lun tim n nguy c nhim c v
truyn bnh. Ngc li, so vi cc dng thc n gia sc trn cc phtphate khong
cht c u im l c hm lng phtphate dinh dng cao hn nhiu, ngun
nguyn liu qung phtphate khng hn ch, ngoi ra hm lng canxi trong loi
sn phm ny cng cao.
Hm lng flo trong phosphate khong cht l mt yu t quan trng cn xem

11

xt. Theo tiu chun quc t, t l P/F trong thc n gia sc phi ln hn hoc bng
100. Ngoi ra, mt s kim loi nng nh Cd, As, Pb, Hg c th c mt trong qung
phtphate phi c khng ch, do cn phi phn tch v th nghim trc khi
quyt nh s dng loi qung no lm nguyn liu sn xut thc n gia sc.
Sn xut ph gia thc n gia sc t qung phtphate Qung phtphate c s
dng ph bin sn xut phn ln. Quy trnh sn xut cc ph gia phtphate cho
thc n gia sc c nhiu im tng t quy trnh sn xut phn ha hc. Mc ch
ca c 2 quy trnh u l chuyn phtpho dng khng hp th c cho cy trng
(hoc gia sc) thnh dng hp th c. Nhng khi sn xut ph gia thc n gia sc
th vic chuyn phtpho sang dng hp th c c ngha quan trng hn nhiu,
ngoi ra nhng nguyn t c hi cho sc khe gia sc (nh flo) phi c gim
xung di mc cho php.
Hai quy trnh chnh c p dng sn xut ph gia phosphate cho thc n
gia sc l:
- Sn xut phosphate tch flo (DFP).
- Sn xut monocanxi phosphate (MCP) v dicanxi phosphate (DCP)

Qu trnh sn xut phosphate tch flo gm cc bc chnh sau: Vic tch flo
c thc hin bng phng php nung nhit cao. Qu trnh ny cng chuyn
ha cc thnh phn phospho dng gia sc khng hp th c thnh dng tan
trong axit xitric v amoni xitrat, l dng c th c hp th sinh hc. Sn phm sau
khi nung c lm lnh v sng thu c c ht theo yu cu, sau c ng
bao.
Qu trnh sn xut MCP v DCP gm cc bc chnh sau: cc nh my c
nh v va, ngi ta c th s dng axit H3PO4 c sn xut t cc loi qung
phtphate khc nhau m vn m bo hm lng flo cn li mc quy nh. Cn
cc nh nly c ln (trn 40 tn/gi) th ngi ta p dng quy trnh tch lin tc.
Axit H3PO4 ca chnh qu trnh ( tch flo) c cho tc dng vi vi nghin
trong my nho lin tc. Bn sn phm c sy kh, sng v ng bao. Cc phn
ht qu mn hoc to c quay vng tr li
12

CHNG 2
CC PHNG PHP XC NH PHOTPHO

. Phng php xc nh cc hp cht ca phospho

2.1.1 Xc nh orthophosphat
Lng phospho tn ti di dng orthophosphate c th c o bng nhng
phng php trng lng, th tch, so mu.

Phng php trng lng c s dng khi hm lng phospho hin din ln,
nhng iu ny khng xy ra trong thc t.

Phng php th tch c s dng khi nng nng phosphat ln hn

50mg/L nhng nng ny rt him gp trong trng hp nc si hay
chuyn ha k kh nhng cht ni. Phng php ny gm: kt ta, lc, lm
sch kt ta v chun . Phng php ny tn nhiu thi gian.

Phng php so mu o nc v nc thi c th c tha mn vi mt

chnh xc cao.
C ba phng php so mu c s dng xc nh orthophosphat, chng

c cng bn cht vi nhng nguyn tc trn nhng khc nhau ch l n c thm

vo mt s nguyn t t nhin to mu. Yu t ha hc cn thit nh: ion
phosphat kt hp vi ammonium molypdat trong iu kin acid thnh
molypdophosphat
PO43- + 12 (NH4)2MoO4 + 24H+ (NH4)3PO4.12MoO3 + 21 NH4 + 12 H2O
Khi hin din mt lng phosphat ln, trng thi ca molypdophosphat s l
nhng kt ta mu vng c th lc v o bng phng php th tch.
nng phosphat thp hn, to thnh nhng ht keo mu vng s c xc
nh hm lng bng phng php so mu .
Vi nng phosphat di 30mg/ L, mu vng ca ht keo khng th nhn
bit r v iu ny c ngha l cn phi pht trin theo mt hng khc.
Mt cch khc ci thin l thm vanadium hnh thnh dng phc hp
13

vanadomolypdophosphoric acid c mu vng r, cho php phn tch phospho vi

hm lng di 1mg/L hoc nhng khong thp hn.
Lng molypdenum cha trong ammonium phosphomolypdate cng c
gim to nhng sn phm c mu xanh t l tng ng vi lng phosphate
hin din
Mt lng tha ammonium molypdate khng b gim i v do khng can
thip vo qu trnh. Ascorbic acid (C6H6O6) hay stannous chloride c th s dng
nh mt nhn t kh. Hp cht mu c to thnh l mu xanh molypdeum hay
xanh heteropoly. Thic clorua cng c s dng nh mt nhn t c th c m
t qua phng trnh:
(NH4)PO4 + 12MoO3 + Sn2+ molypdenum + Sn4+
2.1.2 . Xc nh polyphosphat.
Polyphosphat c th chuyn ha thnh orthophosphat bng cch un si mu
c acid ha ti thiu 90 pht. Lng acid tha thm vo xc tc tng tc
thy phn phi c trung ha trc khi tip tc thm dung dch ammonium
molypdate vo.
Lng orthophosphat xut pht t polyphost c tnh nh sau:
Tng hm lng phosphat v c orthophosphat = polyphosphat
2.1.3 Xc nh phosphat hu c.
phn tch phospho hu c c trong cht thi cng nghip v c trong bn
i hi cht hu c phi c ph hy sao cho phospho c gii phng.
Cht hu c c th b ph hy bi mt trong ba phng php oxy ha m hoc
phng php chuyn ha di dng ion phosphat. Cht oxy ha c s dng l
sulfuric hay persulpahat

Acid perchloric l cht oxy ha mnh nht, nhng n cng l cht c hi

nht.

trnh nguy him t nhng v n, loi m c bit phi c s dng trong

qu trnh chuyn ha v phi thm vo mt s ha cht.
Mt khi chuyn ha hon tt, vic o lng phospho gii phng c th
14

c lm bng bt k mt phng php o orthophosphat no. Tt c nhng dng

phospho (tng) c o t s xc nh phospho hu c. Do vy, lng phospho
hu c c tinh nh sau:
Tng phospho phosho v c = phospho hu c.
2.2 . Cc phng php xc nh photpho

2.2.1 Xc nh photpho bng phng php khi lng

Mu sau khi v c ho, loi tp cht (cht khng tan, keo silic) ho tan trong
acid chuyn v dng phosphat. Kt ta phosphat dng mui kp
NH4MgPO4.6H2O bng hn hp (Mg + NH4+). Lc ra, than ho, tro ho chuyn kt
ta v dng cn Mg2P2O7. Cn dng cn v tnh ra phn trm phosphat c trong
mu.
2.2.2 Xc nh hm lng photpho bng phng php th tch vi thuc th
molypat.
Trong mi trng acid HNO3, acid phosphoric to thnh vi amonimolypdat
kt ta dng mui phc a d amoni phospho molypdat.
PO43- + 3NH4+ 12MoO42- (NH4)3[P(Mo12O40)] + 12H2O
Kt ta khng tan trong mi trng HNO3, tan mt phn trong HCl v H2SO4,
tan ha ton trong kim.
Sau khi kt ta hon ton H3PO4, lc v ra ta, sau ha tan kt ta vi mt
th tch dung dch chun NaOH d v chun ngc lng d NaOH bng dung
dch acid chun.
2.2.3 Xc nh hm lng photpho bng phng php trc quang vi thuc
th molypdat
Trong mi trng axit, PO43- to thnh vi molypdat hp cht phc hetoro
polymolypdophosphoric mu vng
PO43- + 12 MoO42- +27 H+

H3[P(Mo12O40)] + 12H2O

Trong hp cht cha t l P:M c th l 1:3, 1:6, 1:9 hoc 1:12. Trong t l
1:12 l bn nht v thng dng trong nh lng.

15

Hp cht phc ny hm lng nh, l hp cht phc mu vng, hp thu

380 nm. Khi hm lng phospho ln, s to thnh kt ta mu vng v c th nh
lng bng phng php th tch.
Lng d thuc th nh hng n php o do hp thu bc sng tng t.
Thng thng gim nh hng c th nh hng o bc sng 400 - 420 nm.
2.2.4 Xc nh hm lng phospho bng phng php trc quang s dng tc
nhn kh l thic clorua
a. Nguyn tc

Thic clorua kh acid molybdophosphoric v to mu xanh molypden mt

cch mnh lit. Gii hn o xung n 7 gP/L bng cch tng di ng i nh
sng. Nu nng di 100 gP/L th tin cy tng v s cn tr gim.
b. Gii hn pht hin l khong 3 g P/L. nhy c h s hp th l 0.3010,

khong nng 10 gP/L c s thay i h s hp th l 0.009.

2.2.5 Xc nh hm lng phospho bng phng php trc quang s dng
acid ascorbic
Nguyn tc: Amoni molybdat v kali antimonyl tartrate phn ng trong mi
trng acid va vi orthophosphate hnh thnh acid heteropoly - acid
phosphomolybdic - b kh mnh bi ascorbic acid to mu xanh molypden.
Cn tr: Asen phn ng vi thuc th molybdat c mu xanh tng t nh
phosphat. Nng As thp 0,1 mg/L gy cn tr xc nh phosphate. Crom ha tr
su v NO2 nng 1 mg/L lm gim kt qu khong 3% v 10 n 15% nng
10 mg/L. Sulfide (Na2S) v silicat khng gy cn tr nng 1,0 v 10 mg/L.
Gii hn pht hin: xp x 10 gP/L.
2.2.6 Xc nh hm lng phospho bng phng php trc quang t ng s
dng acid ascorbic
2.2.6.1. Phm vi p dng:
Xc nh orthophosphat cc vng nc mt, nc ung v nc mn cng
nh nc thi cng nghip nng 0.001 n 10.0 mgP/L khi o trc quang
16

bc sng 650 n 660 hay 880 nm qua mt dng chy 15 mm hay 50mm. nng
cao hn phi pha long mu. Mc d phng php t ng ch p dng cho
othophotpat, cc hp cht photpho khc c th chuyn mu v dng ph hp
2.2.6.2. Nguyn tc:
Amoni molybdat v kali antimon tartrate phn ng vi orthophosphate trong
mi trng axit va to thnh phc antimon phosphomolybdate, trong , acid
ascorbic kh thnh mu xanh mnh lit ph hp cho o lng trc quang
2.2.7 Xc nh hm lng orthophosphat bng phng php tim theo dng
2.2.7.1. Phm vi p dng
p dng cho mu nc mt v nc ngm
2.2.7.2. Nguyn tc:
Poly photphat chuyn thnh dng othophotphat bng acid sulfuric nung v
persulfat nung chuyn photpho hu c v dng othophotphat. Khi o, mu c
bm vo ng, ion othophotphat (PO43-) s phn ng vi amoni molydat v kali
antimon tatrat trong mi trng acid thnh dng phc. Phc ny b kh bi acid
ascorbic thnh phc mu xanh dng hp thu bc sng 880 nm. hp thu t l
vi nng photpho trong mu.
2.3 . Cc tc nhn kh

2.3.1 Kh acid phosphomolybdic bng acid ascobic

2.3.1.1 Nguyn tc
Phc a d phosphomolybdate to thnh gia orthophosphate v molybdate c
tnh oxy ha yu s b acid ascobic kh to thnh phc mu xanh c bc sng hp
thu cc i 840 nm.
2.3.1.2 nhy v tnh chn lc
Phng php ny c nhy thp, thi gian n nh mu mu lu v cn phi
un nng dung dch phn ng.
2.3.2 Kh acid phosphomolybdic bng thic( II) clorua
2.3.2.1 Nguyn tc
17

Phc a d phosphomolybdate to thnh gia orthophosphate v molybdate c

tnh oxy ha yu s b acid ascobic kh to thnh phc mu xanh c bc sng hp
thu cc i 690 nm.
2.3.2.2 nhy v tnh chn lc
Phng php ny c nhy cao nhng mu xanh khng bn theo thi gian
nn t s dng.
2.3.3 Kh acid phosphomolybdic bng acid ascobic c xc tc antimon
2.3.3.1 Nguyn tc
Qu trnh hnh thnh phc phosphomolybdate vi s c mt ca Sb(III) nh l
xc tc v l thnh phn to phc. Tc ln mu khong 10 pht nhit
phng, phc PSbMo c hai bc sng hp thu cc i 880nm v 710nm tng
ng vi h s hp thu phn t l 22400L. mol-1. cm-1 v 17000L. mol-1.cm-1. Theo L
Drummond, W. Mater, c ch phn ng gia phosphate v molypdate vi cht xc
tc Sb(III) nh sau:
PO43- + 12 MoO42- PMo12O403- + 12O2PMo12O403- PSb2Mo10O4032.3.3.2 nhy v tnh chn lc
Phng php ny c nhy cao, t chu nh hng bi mn ca mu, cc
thuc th c trn chung vi nhau nn rt ngn thi gian n nh ca hn hp
thuc th rt ngn.
2.3.4 Kh acid phosphomolybdic bng acid ascobic c xc tc bismuth
2.3.4.1 Nguyn tc.
Bismuth cng vi phosphate v molybdate hnh thnh rt bn trong mi
trng acid trung tnh v tr thnh mu xanh bi cht kh ascorbic. Mu xanh ca
phc c th o bng phng php trc quang hoc phng php trc quang dng
chy
2.3.4.2 nhy v tnh chn lc
Phng php ny c nhy cao v thch hp xc nh hm lng vt
18

phosphate trong nc, phospho trong than v mui than nhng chu nh hng rt
nhiu bi mn nn cht xc tc bismuth khng thch hp cho i tng mu l
nc mn.
2.4 . Cc yu t cn tr khi xc nh Phospho

Silic: silic nng ti 5 mg Si/L khng gy nhiu. Nhng nng cao hn s

lm tng hp th.
Asenat: Asenat to mu tng t nh orthophosphat to ra. nh hng ny c
th loi tr bng cch kh asenat thnh asenic vi Na2S2O3.
Hydro sunfua: Hydro sunfua vi nng 2 mg/L s khng nh hng g.
Nng cao s lm s lm gim n mc cho php bng cch cho kh nito i qua
mu c acid ha.
Flo: Flo vi nng 70mg F/L khng gy nh hng ln. Nng cao hn
200mg/L s km hm s pht trin mu.
Cc kim loi chuyn tip:

St s nh hng ti mu, nhng vi nng 10mg/L nh hng ti 5%.

Vanadat lm tng mu theo quan h tuyn tnh 5% vi nng 10mV/L

Crom(III) v crom(VI) vi nng 10mg/L khng gy nh hng g nhng

nng 50mgCr/ L s lm tng hp thu ln 5%

Vi nng Cu ln ti 10mg Cu/L khng gy nh hng

Nitrit: Nng nitrit trn 1mgN/L s to nn s bc mu. Lng acid sulfuric

phn hy nitric l 100 mg acid s phn ng vi NO2 nng 10mgN/L .

19

CHNG 3
CNG THC NGHIM

3.1 Mc tu nghin cu ti
Phospho l nguyn t a lng, phospho tham gia vo qu trnh cu to ca
xng, n c s dng sn xut ra nng lng v hot ha nhiu hot ng
sinh thi, l cht khong c nhiu nht trong c th sau calci
Trong c th phospho c khong 80% trong xng, 10% trong c, 10% trong
cc m mm khc. l mt phc hp nng lng sinh hc c nhim v cung cp
nng lng , l nguyn t thit yu cho cuc sng.
Nu hm lng phospho trong c th tha th dn n c th c nhng tc
dng m tnh, hm lng calci gim i th dn n hin tng long xng v th ta
nn chn lc nhng thc n t c hm lng phospho cho c th.
Do , cc phng php phn tch c nhy, chn lc cao dng phn
tch phospho vn ang c quan tm. Hin nay c rt nhiu phng php
phn tch hm lng phospho nh: phng php th tch, phng php trong lng,
phng php trc quang,phng php trc quang theo dng. Tuy nhn, c kt
qu tng i nhanh v chnh xc nn nhm chng ti chn phng php trc
quang v s dng hai loi tc nhn kh l acid ascorbc v thc clorua xc nh
hm lng ca phospho. T chng ti c th nh gi l s dng tc nhn kh
no cho kt qu ti u hn.
3.2 . Ha cht, thit b, dng c

3.2.1. Ha cht
Acid HNO3
Acid H2SO4

Acid HCl
Amoni (NH4OH)

20

 Dung dch amoni monovanadat: Ha tan 0.5875g amoni monovanadat

(NH4VO3) trong 100ml nc nng. Khuy u, thm t t 33ml dung dch acid
nitrit 14M v pha long bng nc.nh mc bng nc ct n 250ml
Dung dich amoni heptanmolipdat: ha tan bng nc nng 25g amoni

heptanmolipdat tetrahydrat (NH4)6Mo24.4H2O. Thm 2.5ml dung dch amoni v pha

long thnh 250ml bng nc ct.
Thuc th molipdovanadat: trn 100ml dung dch amoni heptanmolipdat vi

100ml dung dch amoni monovanadat va 67.5ml HNO3 14M trong bnh nh mc
v nh mc thnh 500ml
Dung dich phospho tiu chun (1000ppm) : ha tan 4.394g kali dihydro

phosphate (KH2PO4) bng nc trong bnh nh mc vi dung tch 1L, phi lm

kh KH2PO4 trc khi cn, pha long bng nc ct ti vch
Dung dch ch th phenolphthalein
Dung dch acid mnh: t t thm 300 mL H2SO4 nc ct khong 600 mL.

ngui, thm 4,0 mL HNO3 v nh mc n 1 lt

Thuc th amoni molybdate I: ho tan 25g (NH4)6Mo7O24.4H2O trong 175

mL nc ct. Thm cn thn 280 mL H2SO4 c vo 400 mL nc ct. Lm lnh,

thm dung dch molybdate, thm nc ct cho n 1 L.
Thuc th thic clorua I: ho tan 25g SnCl2.2H2O trong 100 mL glycerol.

un cch thu v khuy bng a thu tinh tan ht. Thuc th ny n nh v

khng gi hay bo qun li.
Dung dch photphat chun: ha tan trong nc ct 219,5 mg khan KH 2PO4

v pha long n 1000 mL, 1.00 mL = 50.0 g PO433.2.2. Thit b v dng c

My quang ph UV/VIS
Cn phn tch hai s v bn s
Cuvet thy tinh loi 10 mm v 50 mm
T sy
Bnh ht m

21

 Giy lc
Chn platin dung tch 100 n 150 ml.
B nc nng
Cc dng c thy tinh trong phng th nghim, dng c phng th nghim lm

bng polypropylene, polyetylen hoc polytetrafloetylen.

3.3 .Kho st cc thng s ca qui trnh s dng tc nhn kh acid ascorbic
3.3.1 . Kho st ph hp thu gia Phospho v thuc th Molipdovanadat

xc nh hm lng phospho bng phng php trc quang, trc tin ta

phi kho st bc sng ti u nht (max) ca phc mu xanh gia phospho vi
molipdovanadat.
Chun b mt mu dung dch theo bng
Bng 3. 1.Kho st ph hp thu
VP tiu chun

10ml

Vmolipdovanadat

10ml

Vacid acorbic

1ml

VHNO3

10ml

Thi gian v nhit n nh

10 pht v 25OC

nh mc ti vch 100 ml
Lc u v em o quang.
Tin hnh kho st qut bc sng ca dung dch trn t 300- 900 nm.
3.3.2 .Kho st nh hng ca hm lng thuc th Molipdovanadat

Xc nh hm lng Phospho bng phng php trc quang, ta phi tin hnh
kho st lng thuc th molipdovanadat, bit lng thuc th thm phi m
bo cho qu trnh to phc gia phospho v molipdovanadat. Ta chun b mu nh
bng v sau o quang bc sng thch hp.
Bng 3. 2.Kho st nh hng ca thuc th
22

Bnh

V P tiu chun

5mL

V acid ascorbic

1mL

Vmolipdovanadat

VHNO3

12

15

10ml
10 pht v 25OC

Thi gian nhit

nh mc ti vch 100 ml
3.3.3 . Kho st nh hng ca hm lng tc nhn kh acid acorbic

Xc nh hm lng Phospho bng phng php trc quang, ta phi tin hnh
kho st lng tc nhn kh m bo cho qu trnh kh xy ra hon. Ta chun b
mu nh bng v sau o quang bc sng thch hp
Bng 3. 3. Kho st nh hng ca acid ascorbic
Bnh

VP tiu chun
Vacid acorbic

1.0

1.5

2.0

5ml
0.2

0.4

0.6

0.8

V molipdovanadat

10mL

VHNO3

10ml
10 pht v 25OC

Thi gian nhit

nh mc ti vch 100 ml
3.3.4 . Kho st nh hng ca pH

pH ca dung dch nh hng n cc dng tn ti ca cc hp cht tham gia

phn ng. Nu pH ca dung dch thay i c th s lm thay i tc ca phn
ng. V vy, vic kho st pH ti u trong h phn ng l cn thit. Ta chun b
mu nh bng v sau o quang bc sng thch hp.
Bng 3. 4.Kho st nh hng ca pH
23

Bnh
Vmolipdovanadat
VP tiu chun
Vacid acorbic
VHNO3

4
5
10ml
5ml
1ml
6
8
10
10 pht v 25OC

Thi gian nhit

12

14

nh mc ti vch 100 ml
3.3.5 . Kho st nh hng ca thi gian n kh nng bn mu

kho st hm lng phospho bng phng php trc quang, ta phi tin
hnh kho st phc bn mu gia phospho vi thuc th molipdovanadat c bn
thay i theo thi gian nn cn kho st thi gian m bo mt quang ca
phc bn. Ta chun b mu nh bng v sau o quang bc sng thch hp.
Bng 3. 5. Kho st nh hng ca thi gian
Bnh

VP tiu chun

5ml

Vacid acorbic

1mL

Vmolipdovanadat

10ml

VHNO3

10ml

Nhit

25OC

Thi gian( pht)

10

12

15

17

20

25

nh mc ti vch 100 ml

3.3.6 Kho st nh hng ca nhit .

Nhit l mt thng s nh hng trc tip n hng s tc phn ng.
Nhit c th thay i tnh cht ca cc cht tham gia phn ng dn ti thay i
hp thu. V vy, vic kho st nhit trong phn ng l cn thit. Ta chun b
24

mu nh bng v sau o quang bc sng thch hp.

Bng 3. 6. Kho st nh hng ca nhit .
Bnh

Vmolipdovanadat

10ml

VP tiu chun

5ml

Vacid acorbic

1ml

VHNO3

10ml

Thi gian (pht)

10

Nhit

10

15

20

25

30

40

nh mc ti vch 100 ml
3.3.7 . Kho st hm lng khong tuyn tnh

kho st khong tuyn tnh ca phspho ta tn hnh thay i nng ca

phospho t 1ppm n 40ppm sau ta thc hin nh bng v tin hnh o quang
bc sng thch hp
Bng 3. 7. Kho st khong tuyn tnh
Bnh

Vmolipdovanadat

10ml

VP tiu chun

5ml

Vacid acorbic

1ml

VHNO3

10ml

Thi gian (pht)

10

Nhit

25

nh mc ti vch 100 ml

3.3.8 . Gii hn nh lng (LOD) gii hn pht hin (LOQ)

LOD hay cn gi l gii hn pht hin, thng s LOD c dng nh gi
nhy ca phng php phn tch.
Gi tr gii hn pht hin ca thit b c xc nh da vo t l gia tn hiu/nhiu

25

nn (

S
) v c tnh theo cng thc:
N

LOD = 3

S
C min
N
= 3 C min
vi 10 > T = N 3
T
S

LOQ hay cn gi l gii hn nh lng, l hm lng nh nht c th nh

lng mt cch chnh xc theo phng php chn. Gii hn nh lng (LOQ)
ca thit b c xc nh theo cng thc:
LOQ = 10

S
C min
N
= 10 C min
vi 10 > T = N 3
T
S

Trong :
Cmin l nng ti thiu m my c th pht hin c
S l mt quang A ti nng Cmin
N l mt quang A trung bnh ca mu trng
kho st LOD v LOQ, chng ti tin hnh o mt quang A ca phc
phospho molypdovanadat lp li. Qu trnh o quang vi cc nng nh dn, khi
n nng nh nht m phng php c th php hin hoc nh lng c
chnh l gii hn ca phng php.
3.4 . Kho st cc thng s ca qui trnh s dng tc nhn kh thic clorua
3.4.1 . Kho st ph hp thu gia Phospho v thuc th Molipdovanadat

xc nh hm lng phospho bng phng php trc quang, trc tin ta

phi kho st bc sng ti u nht ( max) ca phc mu xanh gia phospho vi
molipdovanadat.
Chun b mt mu dung dch theo bng

26

Bng 3. 8. Kho st ph hp thu

VP tiu chun

10ml

Vmolipdovanadat

10ml

VSnCl2

1ml

VHNO3

10ml

Thi gian v nhit n nh

10 pht v 25OC

nh mc ti vch 100 ml
Lc u v em o quang.
Tin hnh kho st qut bc sng ca dung dch trn t 300- 900 nm.
3.4.2 . Kho st nh hng ca hm lng thuc th Molipdovanadat

Xc nh hm lng Phospho bng phng php trc quang, ta phi tin hnh
kho st lng thuc th molipdovanadat, bit lng thuc th thm phi m
bo cho qu trnh to phc gia phospho v molipdovanadat. Ta chun b mu nh
bng v sau o quang bc sng thch hp.
Bng 3. 9. Kho st nh hng ca thuc th
Bnh

V P tiu chun

12

15

1mL
1

VHNO3
Thi gian nhit

5mL

VSnCl2
Vmolipdovanadat

10ml
10 pht v 25OC
nh mc ti vch 100 ml

27

3.4.3 . Kho st nh hng ca hm lng tc nhn kh thic clorua

Xc nh hm lng Phospho bng phng php trc quang, ta phi tin hnh
kho st lng tc nhn kh m bo cho qu trnh kh xy ra hon. Ta chun b
mu nh bng v sau o quang bc sng thch hp
Bng 3. 10. Kho st nh hng ca acid ascorbic
Bnh

VP tiu chun
VSnCl2

1.0

1.5

2.0

5ml
0.2

0.4

0.6

0.8

V molipdovanadat

10mL

VHNO3

10ml
10 pht v 25OC

Thi gian nhit

nh mc ti vch 100 ml
3.4.4 . Kho st nh hng ca pH.

pH ca dung dch nh hng n cc dng tn ti ca cc hp cht tham gia

phn ng. Nu pH ca dung dch thay i c th s lm thay i tc ca phn
ng. V vy, vic kho st pH ti u trong h phn ng l cn thit. Ta chun b
mu nh bng v sau o quang bc sng thch hp.
Bng 3. 11.Kho st nh hng ca pH
Bnh

Vmolipdovanadat

10ml

VP tiu chun

5ml

VSnCl2

1ml

VHNO3

10

12

14

10 pht v 25OC

Thi gian nhit

28

nh mc ti vch 100 ml
3.4.5 Kho st nh hng ca thi gian n kh nng bn mu

kho st hm lng phospho bng phng php trc quang, ta phi tin
hnh kho st phc bn mu gia phospho vi thuc th molipdovanadat c bn
thay i theo thi gian nn cn kho st thi gian m bo mt quang ca
phc bn. Ta chun b mu nh bng v sau o quang bc sng thch hp.
Bng 3. 12. Kho st nh hng ca thi gian
Bnh

VP tiu chun

5ml

VSnCl2

1mL

Vmolipdovanadat

10ml

VHNO3

10ml

Nhit

25OC

Thi gian( pht)

10

12

15

17

20

25

nh mc ti vch 100 ml
3.4.6 Kho st nh hng ca nhit .
Nhit l mt thng s nh hng trc tip n hng s tc phn ng.
Nhit c th thay i tnh cht ca cc cht tham gia phn ng dn ti thay i
hp thu. V vy, vic kho st nhit trong phn ng l cn thit. Ta chun b
mu nh bng v sau o quang bc sng thch hp.

29

Bng 3. 13. Kho st nh hng ca nhit

Bnh

Vmolipdovanadat

10ml

VP tiu chun

5ml

VSnCl2

1ml

VHNO3

10ml

Thi gian (pht)

10
5

Nhit

10

15

20

25

30

40

nh mc ti vch 100 ml
3.4.7 . Kho st hm lng khong tuyn tnh

kho st khong tuyn tnh ca phspho ta tn hnh thay i nng ca

phospho t 1ppm n 40ppm sau ta thc hin nh bng v tin hnh o quang
bc sng thch hp
Bng 3. 14. Kho st khong tuyn tnh
Bnh

Vmolipdovanadat

10ml

VP tiu chun

5ml

VSnCl2

1ml

VHNO3

10ml

Thi gian (pht)

10

Nhit

25
nh mc ti vch 100 ml

30

3.4.8 Gii hn nh lng (LOD) gii hn pht hin (LOQ)

LOD hay cn gi l gii hn pht hin, thng s LOD c dng nh gi

nhy ca phng php phn tch.
Gi tr gii hn pht hin ca thit b c xc nh da vo t l gia tn
S
) v c tnh theo cng thc:
N

hiu/nhiu nn (

LOD = 3

S
C min
N
= 3 C min
vi 10 > T = N 3
T
S

LOQ hay cn gi l gii hn nh lng, l hm lng nh nht c th nh

lng mt cch chnh xc theo phng php chn. Gii hn nh lng (LOQ)
ca thit b c xc nh theo cng thc:
LOQ = 10

S
C min
N
= 10 C min
vi 10 > T = N 3
T
S

Trong :
Cmin l nng ti thiu m my c th pht hin c
S l mt quang A ti nng Cmin
N l mt quang A trung bnh ca mu trng
kho st LOD v LOQ, chng ti tin hnh o mt quang A ca phc
phospho molypdovanadat lp li. Qu trnh o quang vi cc nng nh dn, khi
n nng nh nht m phng php c th php hin hoc nh lng c
chnh l gii hn ca phng php.
3.5 . D ton kinh ph
Bng 3.14 - D ton kinh ph
STT
1
2
3

Tn ho cht

Xut x

Amoni monovanadat
(NH4VO3)
Amoni heptanmolipdat
((NH4)6Mo24.4H2O)
Phospho tiu chun
(KH2PO4)
31

Quy cch

n v
tnh

Gi thnh

4
5
6
7
8
9
10
11

Amoni heptanmolipdat
(NH4)6Mo7O24.4H2O
Thic clorua
(SnCl2.2H2O)
Glycerol
(C3H8O3)
Acid nitrit
(HNO3)
Acid sulfuric
(H2SO4)
Acid clohdric
(HCl)
Amoni
(NH4OH)
Axit ascorbic
(C6H8O6)

Trung
Quc

25g

chai

35.000

3.6 . nh hng pht trin n chuyn ngnh

Chng ti tm hiu l thuyt v kho st phc ca phospho v molypdate
bng hai loi loi thuc th l acid ascorbic v thic clorua. Mi quy trnh s c u
im v nhc im ring. M trong kh nng hn ch ca n khng th bit ht
c. V th chng ti mun pht trin thnh n chuyn ngnh c kho st
cc quy trnh bng thc rt ra kt lun thc t hn.

32

TI LIU THAM KHO

[1]. L Vn Ct (2007),.X l nc thi giu hp cht nit v phtpho, NXB Khoa

hc t nhin v Cng ngh, H Ni
[2]. Hong Vn Bnh, c cht hc cng nghip v d phng nhim c, NXB
Khoa hc v K thut.
[3]. Standard Methods for the Examination of Water and Wastewater 4500-P
phosphorus
[4]. TCVN 1525: 2001
[5]. TCVN 4779: 1999
[6]. TCVN 6202: 2008
[7]. TCVN 6271: 2007
[8]. http://vi.wikipedia.org/wiki/Photpho

ix