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coeus.vn a3.CHẤT-NHŨ-HÓA
coeus.vn a3.CHẤT-NHŨ-HÓA
H NI - 2011
QCVN 4-22:2011/BYT
Li ni u
QCVN 4-22:2011/BYT do Ban son tho quy chun k thut
quc gia v Ph gia thc phm v cht h tr ch bin bin
son, Cc An ton v sinh thc phm trnh duyt v c ban
hnh theo Thng t s 01/2011/TT-BYT ngy 13 thng 01 nm
2011 ca B trng B Y t.
QCVN 4-22:2011/BYT
I. QUY NH CHUNG
1. Phm vi iu chnh
Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc yu cu
k thut v qun l v cht lng, v sinh an ton i vi cc cht nh ha c s dng
vi mc ch lm ph gia thc phm.
2. i tng p dng
Quy chun ny p dng i vi:
2.1. T chc, c nhn nhp khu, xut khu, sn xut, bun bn v s dng cc
cht nh ha lm ph gia thc phm (sau y gi tt l t chc, c nhn).
2.2. C quan qun l nh nc c lin quan.
3. Gii thch t ng v ch vit tt:
3.1. Cht nh ha: l ph gia thc phm c b sung vo thc phm nhm
mc ch to ra hoc duy tr dng nh tng ng nht ca hai hay nhiu thnh
phn ca thc phm.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food additive specifications; Joint FAO/WHO expert committee on
food additives; Volume 4 - Analytical methods, test procedures and laboratory
solutions used by and referenced in the food additive specifications; FAO, 2006): Cc
yu cu k thut i vi ph gia thc phm, Tp 4 Cc phng php phn tch, quy
trnh th nghim, dung dch th nghim c s dng (hoc tham chiu) trong yu
cu k thut i vi ph gia thc phm; JECFA bin son; FAO ban hnh nm 2006.
3.3. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.4. TS (test solution): Dung dch thuc th.
3.5. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.6. MTDI
3.6. INS (International numbering system): H thng m s quc t v ph gia
thc phm.
QCVN 4-22:2011/BYT
II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht nh ha c quy
nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1.
Ph lc 1:
1.2.
Ph lc 2:
1.3.
Ph lc 3 :
1.4.
Ph lc 4:
1.5.
Ph lc 5:
1.6.
Ph lc 6:
1.7.
Ph lc 7:
1.8.
Ph lc 8:
1.9.
Ph lc 9:
1.10.
Ph lc 10:
1.11.
Ph lc 11:
1.12.
Ph lc 12:
1.13.
Ph lc 13:
1.14.
Ph lc 14:
1.15.
Ph lc 15:
1.16.
Ph lc 16:
1.17.
Ph lc 17:
1.18.
Ph lc 18:
QCVN 4-22:2011/BYT
1.19.
Ph lc 19:
1.20.
Ph lc 20:
1.21.
Ph lc 21:
1.22.
Ph lc 22:
QCVN 4-22:2011/BYT
2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht nh ha sau khi hon tt ng k bn cng b hp quy v bo m cht lng,
v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut.
V. T CHC THC HIN
1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chc
nng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny.
2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhim
kin ngh B Y t sa i, b sung Quy chun ny.
3. Trng hp hng dn ca quc t v phng php th v cc quy nh
ca php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th th
p dng theo vn bn mi.
QCVN 4-22:2011/BYT
Ph lc 1
YU CU K THUT V PHNG PHP TH
I VI MONO V DIGLYCERID CA CC ACID BO
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
3. Cm quan
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Hp th hng ngoi
Acid bo
Glycerol
QCVN 4-22:2011/BYT
Ch s acid
Khng c qu 6.
Glycerol t do
Khng c qu 7%
X phng
Ch
6. Phng php th
tinh khit
X phng
Ch
QCVN 4-22:2011/BYT
Ph lc 2
YU CU K THUT V PHNG PHP TH
I VI ESTER CA GLYCEROL VI ACID LACTIC V ACID BO
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
Cht rn dng sp
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Acid bo
Acid lactic
Glycerol
Ch
6. Phng php th
tinh khit
Ch
QCVN 4-22:2011/BYT
Ph lc 3
YU CU K THUT V PHNG PHP TH
I VI ESTER CA GLYCEROL VI ACID CITRIC V ACID BO
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Acid bo
Acid citric
Glycerol
Glycerol t do
Khng c qu 4%
Glycerol tng s
10
QCVN 4-22:2011/BYT
Acid bo tng s
Ch
6. Phng php th
tinh khit
Glycerol tng s
Nguyn tc:
Mu c x phng ho bng dung dch KOH trong alcol v
cc acid bo c tch ra bng trch ly. Acid citric c
chuyn thnh cc dn sut trimethylsilyl (TMS) v c
11
QCVN 4-22:2011/BYT
phn tch bng sc k kh lng.
X phng ho:
Cn chnh xc 1 g mu cho vo bnh y trn, thm 25 ml
dung dch KOH 0,5M trong ethanol v un si vi sinh hn
ngc trong 30 pht. Acid ho hn hp bng HCl v cho
bc hi bng my c quay hoc bng phng php thch
hp khc.
Trch ly:
Chuyn ton lng mu trong bnh vo mt bnh gn, s
dng khng qu 50 ml nc v trch ly bng 3 ln 50 ml
heptan, loi b phn dch chit heptan tch ra. Chuyn lp
dung dch nc vo bnh nh mc dung tch 100 ml, trung
ho, pha ti th tch 100 ml bng nc v lc u.
Dn xut ho:
Dng pipet ly 1 ml dung dch pha c trn, 1 ml dung
dch acid tartric (1 mg/ml trong nc) cho vo bnh y trn
c th y np dung tch 10 ml v c n kh. Thm 1 ml
pyridin, 0,2 ml dung dch trimethyl-chlorosilan (TMCS), 0,4
ml hexamethyl-disilazan (HMDS), 0,1 ml n-methyl-ntrimethylsilyl-trifluoroacetamid (MSTFA). y np cht v lc
cn thn c dung dch tan hon ton. Gia nhit bnh
trong t sy 600C trong 1 gi.
Sc k kh:
Bt k sc k kh thch hp c th c dng vi detector
ion ho ngn la v ct (thu tinh, chiu di 1,8 m v ng
knh trong 2 mm), c nhi bng DC-200 10% trn
chromosorb Q (80/100 mesh). Cc iu kin cho sc k kh:
nhit l ct 1650C, nhit bung tim 2400C, nhit
detector 2400C; tc dng kh mang nitrogen 24 ml/pht.
Cch tin hnh:
Bm 5 l mu cc dn xut TMS. Thi gian lu i vi acid
tartric khong 12 pht v thi gian lu tng i ca acid
citric/acid tartric khong2,3.
Lp li cch tin hnh c m t trn trong phn Dn
xut ho v Sc k kh s dng 1 ml dung dch i chng
acid citric (3 mg/ml trong nc) thay th 1 ml dung dch mu
th.
Tnh kt qu:
o din tch mi pic bng phng php thch hp.
Acid citric tng (%) =
Trong :
ACS: Din tch pic ca acid citric (dung dch mu)
ATS: Din tch pic ca acid tartric (dung dch mu)
ATR: Din tch pic ca acid tartric (dung dch i chng)
ACR: Din tch pic ca acid citric (dung dch i chng)
WCR: Khi lng (g) ca acid citric trong 1 ml dung dch i
chng
W: Khi lng (g) ca mu ester glycerol vi acid citric v
12
QCVN 4-22:2011/BYT
acid bo.
Acid bo tng s
13
QCVN 4-22:2011/BYT
Ph lc 4
YU CU K THUT V PHNG PHP TH
I VI ESTER CA GLYCEROL VI ACID DIACETYL TARTRIC
V ACID BO
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
Trong :
1) Mt hoc hai nhm R l ca acid bo
2) Nhm R khc l ca hoc
- acid diacetylat tartric
- acid monoacetylat tartric
- acid tartric
- acid acetic
- hydrogen
3. Cm quan
4. Chc nng
Cht nh ho
5. Yu cu k thut
14
QCVN 4-22:2011/BYT
5.1. nh tnh
tan
1, 2- diol
Acid bo
Acid acetic
Acid tartric
Glycerol
Tro sulfat
Acid bo t do
Glycerol tng s
Glycerol t do
Khng c qu 2,0%
Ch
6. Phng php th
6.1. nh tnh
1, 2- diol
15
QCVN 4-22:2011/BYT
Acid acetic tng s
Dng c:
Lp rp b dng c chng ct Hortvet Sellier ci tin nh
hnh v sau, s dng ng Sellier c kch thc bn trong
ln (khong 38-x 203 mm) v by chng ct dung tch ln.
Cch tin hnh:
Cn chnh xc 4 g mu v cho vo ng bn trong ca b
dng c v lp ng vo bnh ngoi c cha khong 300 ml
nc nng va un si. Thm 10 ml acid perchloric 4 N [35
ml (60 g) acid perchloric 70% trong 100 ml nc] vo mu
th, v ni ng bn trong vi sinh hn lm mt bng nc
qua by chng ct. Chng ct bng cch gia nhit bnh
pha ngoi sao cho thu c 100 ml dung dch ct trong
khong 20 - 25 pht. Tp hp cc phn dch ct c 100
ml v thm phenolphthalein TS vo mi phn, chun
bng dung dch NaOH 0,5 N. Tip tc chng ct cho n khi
phn 100 ml dung dch ct c cn khng qu 0,5 ml dung
dch NaOH 0,5N trung ho. (Ch : khng c chng
ct n cn kh). Tnh khi lng (mg) acid bay hi trong
mu theo cng thc V x e, trong V l tng th tch (ml)
ca dung dch NaOH 0,5N dng chun v e l h
s ng lng 30,03.
16
QCVN 4-22:2011/BYT
Acid tartric tng s
ng chun:
Chuyn 100 mg acid tartric tinh khit c cn chnh xc
vo bnh nh mc dung tch 100 ml, ho tan acid tartric
trong 90 ml nc v thm nc n th tch 100 ml, lc
u. Ly cc phn 3, 4, 5 v 6 ml cho vo cc cuvet ring
bit ph hp (kch thc 19 x 150 mm), thm lng nc
thch hp c dung dch th tch 10 ml. Cho vo mi
cuvet 4 ml dung dch natri metavanadat 5% va mi pha, 1
ml acid acetic. (Ch : s dng cc dung dch ny trong
vng 10 pht sau khi mu tng ln). Chun b mu trng
ging nh cch trn, s dng 10 ml nc thay th dung
dch acid tartric. t thit b v tr bng 0 i vi mu trng
v sau o hp th ca 4 dung dch acid tartric ti
bc sng 520 nm vi my quang ph thch hp hoc my
so mu quang in c trang b knh lc 520 nm. T s
liu thu c, xy dng ng chun trn h trc to
vung gc vi trc tung biu din hp th, trc honh
biu din lng acid tartric tng ng (mg).
Chun b mu th:
Cn chnh xc 4 g mu cho vo bnh Erlenmeyer dung tch
250 ml, thm vo 80 ml dung dch KOH 0,5N v 0,5 ml
phenolphthalein TS. Ni bnh vi mt sinh hn khng kh c
chiu di t nht 65 cm, gia nhit hn hp trn tm nhit
trong 2,5 gi. Thm vo hn hp nng khong 10% acid
phosphoric cho n khi hn hp c phn ng acid r vi
giy ch th Congo. Ni li bnh vi sinh hn khng kh v
gia nhit cho n khi acid bo c ho lng v trong. Lm
ngui v sau chuyn hn hp vo mt bnh gn dung
tch 250 ml vi s h tr ca cc phn nh nc v
chloroform. Chit cc acid bo c gii phng ra bng 3
ln 25 ml nc lin tip v cho phn nc ra vo bnh gn
c cha lp nc. Chuyn ton b hn hp trong bnh gn
u vo cc dung tch 250 ml, gia nhit trn ni cch thy
loi b cc vt ca chloroform, lc qua giy lc mn
c ra acid vo bnh nh mc dung tch 500 ml, v cui
cng pha ti th tch 500 ml bng nc (Dung dch I). Dng
pipet ly 25 ml dung dch ny cho vo bnh nh mc dung
tch 100 ml v pha ti th tch 100 ml bng nc (Dung dch
II). Gi phn cn li ca Dung dch I xc nh glycerol
tng s.
Cch tin hnh:
Cho 10 ml Dung dch II c chun b trong phn Chun
b mu th vo cuvet 19 x 150 mm v tip tc lm theo
hng dn trong phn ng chun, bt u vi cho vo
mi cuvet 4 ml dung dch metavanadat 5%. T ng
chun xc nh khi lng (mg) acid tartric trong pha long
cui cng, sau nhn vi 20 v chia kt qu cho khi
lng mu gc thu c % acid tartric.
Glycerol tng s
17
QCVN 4-22:2011/BYT
Acid tartric tng s vo trong bnh Erlenmeyer c np thu
tinh dung tch 250 ml hoc bnh iod. Thm vo bnh 15 ml
acid acetic bng v 25 ml dung dch acid periodic, c
chun b bng cch ho tan 2,7 g acid periodic (H5IO6) trong
50 ml nc, thm 950 ml acid acetic bng v lc mnh; bo
qun dung dch ny trnh nh sng. Lc u hn hp trong
1 hoc 2 pht, yn trong 15 pht, thm 15 ml dung dch
KI 15% v 15 ml nc, lc xoy, yn trong 1 pht v sau
chun iod c gii phng ra bng dung dch natri
thiosulfat 0,1N, dng tinh bt TS l cht ch th. Thc hin
chun mu trng s dng nc thay th mu th. Th
tch thc l s ml dung dch natri thiosulfat 0,1N dng
chun glycerol v acid tartric trong mu th c 5 ml Dung
dch I. T % xc nh c trong Phng php th Acid
tartric tnh th tch dung dch natri thiosulfat 0,1N dng
chun acid tartric. Chnh lch gia th tch thc v th
tch tnh ton c dng i vi acid tartric l s ml ca
dung dch natri thiosulfat 0,1N tiu th bi glycerol trong
mu. Mt ml dung dch natri thiosulfat 0,1N tng ng
vi 2,303 mg glycerol v 7,505 mg acid tartric.
18
QCVN 4-22:2011/BYT
Ph lc 5
YU CU K THUT V PHNG PHP TH I VI SUCROGLYCERID
1. Tn khc, ch s
2. nh ngha
INS 474
Sucroglycerid thu c nh phn ng gia sucrose vi
cht bo hoc du n c hoc khng c mt ca dung mi.
Sn phm gm c hn hp mono- v di-ester ca sucrose
v acid bo kt hp vi mono-, di- v triglycerid t cht
bo hoc du. Ch cc dung mi sau y c th c s
dng trong sn xut: dimethyl formamid, cyclohexan,
isobutanol, isopropanol v ethyl acetat.
3. Cm quan
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Acid bo
ng
Khng c qu 2%
Th 2 g mu (Phng php I)
Ch s acid
Khng c qu 6
Sucrose t do
Dimethylformamid
Cyclohexan v
isobutanol
Ethyl acetat v
isopropanol
Ch
5.3. Hm lng
6. Phng php th
6.1. nh tnh
Acid bo
QCVN 4-22:2011/BYT
du c hnh thnh, v c ho tan khi thm 3 ml
diethyl ether.
20
QCVN 4-22:2011/BYT
ng
QCVN 4-22:2011/BYT
RF x din tch ni chun x mg mu
22
QCVN 4-22:2011/BYT
Dimethylformamid
Xc nh bng sc k kh lng
Ho cht, thuc th:
- Dimethyl formamid
- Dimethylamin hydrochlorid
- Methanol
- Ethanol
- HCl
- NaOH
Dung dch chun:
Chun b dung dch gc dimethylaminhydroclorid trong
ethanol 4,47 mg/ml (tng ng vi 4,0 mg/ml dimethyl
formamid) v chun b mt lot cc dung dch chun tng
ng vi 4; 2 v 1 g/ml dimethylformamid bng cch pha
long dung dch gc vi dung dch NaOH 0,1% trong
ethanol.
Chun b mu:
B dng c thu phn c trnh by trong phn Ph lc.
Cn chnh xc 40 g mu cho vo bnh y trn dung tch
1.000 ml. Thm 500 ml dung dch NaOH 5% trong
methanol, v gn bnh vo b dng c thu phn. t bnh
ct Erlenmeyer cha 10 ml dung dch HCl 1% trong
methanol vo b dng c thu phn. Gia nhit bnh y
trn v chng ct vi sinh hn ngc c nc lm mt
trong 1 gi, sau ct ly 50 ml dch ct c th dng li.
C dch ct c cho n kh trong cch thy si. Ho tan
phn cn bng mt lng nh ethanol, thm 2,5 ml dung
dch NaOH 5% trong ethanol v pha long n th tch 25
ml bng ethanol chun b mt dung dch mu.
Cch tin hnh:
Bm 2 l dung dch mu vo thit b sc k kh lng vi
cc iu kin di y.
ng chun:
Chun b ng chun bng cch bm 2 l cc dung dch
chun vo thit b sc k kh.
Cc iu kin sc k:
Ct:
- Di: 2m
- ng knh trong: 2 mm
- Cht liu: thu tinh
- Ct nhi: 10% amin 220 v KOH 10% trn nn
chromosorb W yu 80/100 c ra acid yu
- Luyn ct: Gia nhit ti 1300C qua m vi tc dng
nitrogen 5 ml/pht
Kh mang: nitrogen
Tc dng: 17 ml/pht
23
QCVN 4-22:2011/BYT
Detector: FID
Nhit :
- Bung bm mu: 198 50C
- Ct: 600C.
Tnh kt qu:
Nng dimethylformamid (CDFA) tnh theo cng thc sau:
Trong :
C: Nng dimethylformamid pht hin c ( g/ml)
W: Khi lng mu (g)
24
QCVN 4-22:2011/BYT
Cyclohexan v
isobutanol
25
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Isopropanol v ethyl
acetat
26
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0
- Nhit syringe: 85 C
- Th tch mu dng hi: 0,4 ml
Kt qu: c tnh theo cng thc:
Trong :
Ci: Nng dung mi i (mg/kg);
Ai: Din tch pic dung mi i ( v.giy.);
Cfi: H s chuyn i dung mi i ( dc ca ng
chun) ( g/ v.giy).
27
QCVN 4-22:2011/BYT
Ch
6.2. nh lng
28
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29
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Ph lc 6
YU CU K THUT V PHNG PHP TH I VI ESTER CA
POLYGLYCEROL VI CC ACID BO
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Acid bo
Glycerol v polyglycerol
Polyglycerol
QCVN 4-22:2011/BYT
hoc cao hn heptaglycerol.
Ch
6. Phng php th
6.1. nh tnh
Glycerol v polyglycerol
31
QCVN 4-22:2011/BYT
Ph lc 7
YU CU K THUT V PHNG PHP TH I VI STEARYL CITRAT
1. Tn khc, ch s
INS 484
ADI = 0 - 50 mg/kg th trng, c thit lp ti k hp ln
th 17 ca JECFA (1973).
2. nh ngha
Cng thc cu to
Thnh phn gn ng
4. Chc nng
5. Tnh cht
5.1. nh tnh
tan
Cn stearylic
Citrat
Ch
6. Phng php th
6.1. nh tnh
Cn stearylic
QCVN 4-22:2011/BYT
du ha v cho bay hi trn a s hoc thy tinh. Phn
khng bay hi phi c khong nng chy t 43o n 58o.
Citrat
Ch
33
QCVN 4-22:2011/BYT
Ph lc 8
YU CU K THUT V PHNG PHP TH
I VI TRIKALI ortho-PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Ch s C.A.S.
7778-53-2
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Kali
Phosphat
ortho-phosphat
Khng c qu 0,2%.
Fluorid
Arsen
Ch
QCVN 4-22:2011/BYT
5.3. Hm lng K3PO4
6. Phng php th
6.1. nh tnh
Kali
Phosphat
Thm 1ml dung dch acid nitric v 5ml dung dch nhm
molybdat (TS) vo 5ml dung dch mu th (1/100) v un
nng. Trong dung dch phi xut hin kt qu vng nht.
ortho-phosphat
QCVN 4-22:2011/BYT
xy ra. Ghi li th tch dung dch natri fluorid (TS) s
dng.
Th tch dung dch natri fluorid (TS) s dng khng c
qu 1 ml.
Ch
6.3. nh lng
36
QCVN 4-22:2011/BYT
Ph lc 9
YU CU K THUT V PHNG PHP TH
I VI CC MUI AMONI CA ACID PHOSPHATIDIC
1. Tn khc, ch s
2. nh ngha
Cng thc cu to
(thnh phn gn ng)
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
Phosphat
Acid bo
Glyceryl
5.3. Hm lng
6. Phng php th
37
QCVN 4-22:2011/BYT
6.1. nh tnh
Phosphat
Acid bo
6.3. nh lng
Phosphor
QCVN 4-22:2011/BYT
nhng khng cho mu th v s dng cng th tch acid nh
dng v c ha t mu th (Dung dch trng phn
hy).
Cho vo cc bnh nh mc 100-ml ring, thm t buret:
(a) 25,0 ml dung dch chun lm vic phosphat (= 5,0 mg
P2O5),
(b) 30,0 ml dung dch chun lm vic phosphat (= 6,0 mg
P2O5),
(c) 25 ml dung dch th cha t 5 n 6 mg P2O5
Cho vo mi bnh cha phosphor chun, (a) v (b), mt
lng dung dch trng phn hy c cng th tch nh dung
dch cho vo (c), b i vi vt phosphor c th c do
thuc th phn hy acid m n c th c trong dung dch
th.
Cho vo mi bnh 25 ml thuc th vanadat-molybdat, lc
u, pha long bng nc ti gn 100 ml, lc u, iu
chnh nhit ca dung dch ti 20C, pha long ti vch
bng nc v lc u.
Sau 10 pht, o hp th ca c dung dch 6 mg P2O5 v
dung dch th, mu trng l dung dch cha 5 mg cht
chun. Dng cc o 1 cm v o bc sng 420 nm, hoc
knh lc Ilford 604 nu dng my so mu quang in.
Tnh ton
% phosphor
At
A 6mg
0,873
m
Trong :
At = hiu hp th gia chun 5 mg v dung dch th
A6 mg = hiu hp th gia chun 6 mg v 5 mg
m = khi lng mu th (g)
39
QCVN 4-22:2011/BYT
Xc nh nitrogen amoni
Thit b ct ko hi nc
Thit b gm mt bnh 2-L y nt cao su, lp xuyn qua nt
c mt ng thy tinh khong 7,5 cm, c lp sao cho u
di ca ng gn st y bnh, v mt on ng hnh ch L
ngn hn lp sao cho ng cha ngang khong 6 mm bn
di b mt ca nt, hot ng nh ng ra ca lung hi
nc. Bnh c thm nc ct acid ha nh bng acid
sulfuric long (TS) ti khong 2/3 th tch bnh v vi mnh
thy tinh xp trnh tro khi hn hp trong bnh si mnh.
Bnh ny dng lm ngun cung cp hi nc. C th lp mt
vi vo bnh nu mun d dng b sung nc vo bnh gia
cc ln xc nh.
ng ra ca hi c ni qua mt by ngng ti u vo ca
u ct hi, ni vo mt bnh cu y trn c ngn 1-L c
bnh c B34. u ct phi sao cho ng u vo ca hi gn
chm y bnh 1-L v u ra phi ni vi hai by trnh bn,
mt gn nh ca bnh 1-L v ci kia gn nh ca mt sinh
hn thng ng, ni c B19, ni vi u ct. Sinh hn thng
phi lp vi ng u ra ko di, chm ti y ca mt bnh
nn 500-ml.
Thuc th
Dung dch acid boric 2% (kl/tt) trong nc
Dung dch natri hydroxyd 40% (kl/tt) trong nc
Acid hydrocloric 0,02 N
Hn hp ch th: Trn 5,0 ml dung dch xanh lc bromocresol
0,1% (kl/tt) trong alcol v 2,0 ml dung dch methyl 0,1%
(kl/tt) trong alcol v pha long ti 30 ml bng alcol 95%.
Dch silicon 200/50 MS
Tin hnh
Lp v cho hi nc i qua thit b. Cn chnh xc khong
0,2 g mu th mui amoni ca acid phosphatidic trung tnh
vo trong mt l thy tinh nh (ng knh khong 18 mm,
su khong 12 mm). Chuyn l v mu th cn vo bnh
ct v thm khong 250 ml nc ct. Ni u ct v by
chng bn vi bnh ct v sinh hn ng, lp sinh hn sao
cho u ra ngp di b mt ca 10 ml acid boric 2% v 1
ml hn hp ch th ng trong bnh nn 500-ml.
Thm vo bnh ct qua phu gn bng mt ng cao su ngn
vo ng dn hi nc vo, 75 ml natri hydroxyd 40%, v ra
vo trong bng nc ct. B phu v ni ng vo ca hi vi
ngun cung cp hi. (C th cho natri hydroxyd vo bnh qua
phu c kha, lp vi bnh ct nu mun v ra pha trong
bng nc ct. Nu lm nh vy phi duy tr mt lp cht
lng trn phu trong sut qu trnh thm v ct). Ct ko
mnh bng hi nc hn hp trong bnh ct v thu ly 200
ml dch ct vo trong acid boric. Trong qu trnh ct khuy
nh bnh ct nu cn, trnh mu th b lng ng xung
quanh b mt pha trn ca bnh. Khi thu lng dch
ct theo yu cu, h thp bnh hng, ngng cung cp hi
nc v ra pha trong ca sinh hn v bn ngoi u pha
di vi mt lng nh nc ct, gp dch ra vo bnh
hng.
40
QCVN 4-22:2011/BYT
Chun hn hp trong bnh hng bng acid hydrocloric
0,02 N. Lm t nht mt mu trng tin hnh theo cng cch
nhng khng c mu th.
Trong qu trnh ct c th c bt xut hin ca hn hp trong
bnh ct. Nu c, thm 2 git dch silicon vo bnh ct ti thi
im cho mu th; v mt lng tng t c cho vo
mu trng.
Tnh ton
Mi ml HCl 0,02 N = 0,2802 mg nitrogen.
% Nitrogen
Vt V o
mt
28,02
Trong
Vt = th tch dung dch HCl 0,02 N dng chun mu th
(ml)
Vo = th tch dung dch HCl 0,02 N dng chun mu trng
(ml)
mt = khi lng mu th (mg).
41
QCVN 4-22:2011/BYT
Ph lc 10
YU CU K THUT V PHNG PHP TH
I VI SUCROSE ACETAT ISOBUTYRAT
1. Tn khc, ch s
SAIB
INS 444
2. nh ngha
Tn ha hc
Ch s C.A.S
Cng thc ha hc
Cng thc cu to
Trong
R1 = -CH2OCOCH3
R2 = -CH2OCOCH(CH3)2, hoc -OCOCH(CH3)2
Khi lng phn t
832 856
C40H62O19 = 846,9
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Ch s khc x
Hp th hng ngoi
Ch s x phng ha
QCVN 4-22:2011/BYT
Triacetin
Khng c qu 0,1%.
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng
C40H62O19
6. Phng php th
6.1. tinh khit
Triacetin
Ch
6.2. nh lng
S dng ch s x phng ha, tnh % C40H62O19 theo cng
thc:
Trong
SV = ch s x phng ha
Ph hng ngoi
43
QCVN 4-22:2011/BYT
44
QCVN 4-22:2011/BYT
Ph lc 11
YU CU K THUT V PHNG PHP TH
I VI ESTER CA GLYCEROL VI NHA CY
1. Tn khc, ch s
Ester gum;
INS 445
2. nh ngha
M s C.A.S.
8050-30-4
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Hp th hng ngoi
T trng
im nng chy
Ch s acid
39
Ch s hydroxyl
Ch
QCVN 4-22:2011/BYT
6. Phng php th
6.1. nh tnh
Alcol nha v
glycerol nha
QCVN 4-22:2011/BYT
n th tch 100 ml bng toluen v lc u.
- Dung dch thu phn: Thm t t 50 ml dung dch H2SO4
m c, tinh khit vo 200 ml nc ct ng thi khuy
trong chu nc . Lm ngui ti nhit phng.
- Dung dch phenolphthalein: 1% trong ethanol.
- Dung dch NaOH: Ho tan 16 g NaOH trong 70 80 ml
nc ct v lm ngui ti nhit phng. Pha ti 100 ml
bng nc ct v lc u. trong bnh polyethylen.
- 1, 4- Butandiol: 99%
- Glycerol: 99%
- Dung dch ni chun: Cn 0,1 g 1, 4- butandiol cho vo
bnh nh mc dung tch 100 ml. Pha ti th tch 100 ml
bng nc ct v lc u.
- Dung dch glycerol: Cn 0,1 g 1, 4- butandiol v 0,1 g
glycerol cho vo bnh nh mc dung tch 100 ml. Pha ti
th tch 100 ml bng nc ct v lc u.
iu kin chy sc k kh:
I (alcol nha)
Nhit :
- Ct: 1900C, ng nhit
- u vo: 2500C
- Detector: 2500C
Tc dng:
- Kh mang (He): 30 ml/pht ti 63 psi
- H2: 30 ml/pht
- Khng kh: 240 ml/pht
II (glycerol)
Nhit :
- Ct: t theo chng trnh, 120 2000C vi tc
60C/pht
- u vo: 2500C
- Detector: 2500C
Tc dng:
- Kh mang (He): 30 ml/pht ti 63 psi
- H2: 30 ml/pht
- Khng kh: 240 ml/pht
Cch tin hnh I (i vi nha):
Cn 250 300 mg mu cho vo bnh Erlenmeyer dung tch
25 ml c thanh khuy t. Dng pipet ly 5,0 ml toluen cho
vo bnh v khuy t cho n khi mu c ho tan. Ly
5,0 ml Natri VitrideTM cho vo bnh, y np bnh v khuy
trong 30 pht. M np ra ng thi khuy, dng pipet ly
3,0 ml dung dch thu phn cho vo bnh. Tip tc khuy
trong 3 pht. Chuyn hn hp trong bnh vo ng li tm,
47
QCVN 4-22:2011/BYT
y np v lc u. Cho thot kh v li tm vi tc 2.800
3.200 vng/pht trong 5 pht. Bm 0,5 l lp trn vo
thit b sc k kh vi cc iu kin k thut t v ghi
sc k . So snh vi cc sc k c biu th pha
di xc nhn th t thi gian lu ca cc alcol nha.
Cch tin hnh II (i vi glycerol)
Dung pipet hoc syringe hypodermic, loi b lp toluen v
mt phn dung dch nc v li khong 2 ml dung dch
nc trong ng li tm. Thm 1 git dung dch
phenolphthalein v trung ho bng dung dch NaOH. Cc
mui nhm s kt ta. Dng pipet ly 5 ml dung dch ni
chun cho vo ng, pha n 15 ml bng nc ct, y
np, lc v li tm vi tc 2.800 3.200 vng/pht trong
5 pht. Bm 1 l dch trong trn b mt vo thit b sc k
kh vi cc iu kin k thut t v ghi sc k . Bm
1 l dung dch glycerol v ghi sc k . o cc thi gian
lu ca bt k cc pic so vi 1,4- butandiol. So snh cc
thi gian lu vi thi gian lu ca glycerol.
6.2. tinh khit
Khng c nha du cao Khi cc hp cht hu c c cha lu hunh c gia nhit
(Lu hunh)
vi s c mt ca natri format, lu hunh chuyn ho
thnh hydrogen sulfid c pht hin bng cch s dng
giy ch acetat. Php th dng tnh cho thy vic s
dng nha du cao thay cho nha g.
Thit b, dng c:
- ng th: loi tiu chun, kch thc 10 x 70 mm, lm
bng thu tinh chu nhit.
- n Bunsen: Thng dng c nh dng ngn la nh
Ho cht, thuc th:
- Dung dch natri format: Ho tan 20 g natri format tinh khit
(NaOOCH) trong 100 ml nc ct.
- Giy th ch acetat: dng thng mi c sn ca hu ht
cc nh cung cp ho cht
Cch tin hnh:
Cn 40 50 mg mu cho vo ng th v thm 1 -2 git
dung dch natri format 20% (khi lng/th tch). di
giy th ch acetat trn ming ng th. Gia nhit ng th
bng ngn la cho n khi khi c hnh thnh v tip
xc vi giy th. Tip tc gia nhit trong 2 5 pht. Khng
c c m en ca ch sulfid hnh thnh, nu c m
en th chng t s c mt ca cc hp cht cha lu
hunh. (Gii hn pht hin: 50 mg/kg lu hunh).
48
QCVN 4-22:2011/BYT
im nng chy
QCVN 4-22:2011/BYT
My khuy:
S dng my khuy thch hp vi tc 500 700
vng/pht. m bo phn tn nhit u trong mi
trng nng, hng ca trc quay nn y dch lng ln
pha trn. (Xem Hnh 2d ).
Chun b mu:
Ly mu i din gm cc mnh va mi b v c b mt
cha b oxy ho. No lp trn b mt mu thu cc
mnh v ngay trc khi s dng, trnh bao gm cc bt
mn hoc bi. Lng mu ly thng t nht gp i lng
cn cho s chic nhn yu cu nhng khng c
nh hn 40 g. Ngay sau lm nng chy mu trong dng
c cha sch, s dng t sy, tm gia nhit hoc cch ct
hoc cch du ngn qu nhit cc b. Trnh hnh thnh
bt kh trong mu nng chy, khng c gia nhit trn
nhit cn thit mu d dng m khng bao gm
bt kh. Thi gian tnh t lc bt u gia nhit cho n lc
mu khng qu 15 pht. Ngay trc khi y cc
chic nhn, gia nhit mu trc n nhit ti mu
c rt. Trong khi rt, cc vng trn c gi trn tm
ng thau. Rt mu vo cc vng trn tha cho ngui.
Lm ngui t nht 30 pht v sau ct b phn mu tha
bng dao h nng hoc dao bay. S dng dng c
cha sch v mt mu mi nu php th c lp li.
Cch tin hnh:
Mu c im nng chy trn 800C: Rt glycerol vo bnh
thu tinh ti su khng c nh hn 4 inch (10,2 cm)
v khng c qu 4,25 inch (10,8 cm). Nhit ban u
ca chu l 320C. i vi nha thng (gm c nha g),
glycerol cn c lm ngui n nhit khng c nh
hn 450C di im nng chy d on trc nhng
khng c thp hn 350C. V tr trc ca trc khuy gn
thnh sau ca dng c cha, vi cc li dao khng chm
vo thnh v phn di ca cnh dao cch nh ca vng
0,75 in (18 mm). Tr khi c hng dn chnh tm cu
c s dng, lm lm nh trung tm ca mu bng
cch nhn qu cu hoc mt que trn c h nng
dng cho mu cng, vo mu ti thi im ny. Treo vng
trn c cha cc mu trong chu glycerol b mt di
ca vng trn y cch b mt ca tm ngang thp hn l
1,0 inch (25,4 mm) (xem Hnh 1d), t nht 0,5 inch (13 mm)
v khng qu 0,75 inch (18 mm) trn so vi y ca bnh
thu tinh, hoc 1,0 inch (25,4 mm) trn so vi y ca
dng c cha (xem Hnh 2e). t qu cu trong glycerol
nhng khng c t ln trn mu th. Treo nhit k
ASTM 16C trong glycerol sao cho y bu ca nhit k
cch y chic nhn khong 0,5 inch (13 mm) nhng
khng c chm vo chic nhn. Duy tr nhit ban u
ca glycerol trong 15 pht v sau dng kp thch hp
t qu cu vo trung tm b mt trn ca mu trong
chic nhn. Bt u khuy v tip tc khuy vi tc 500
50
QCVN 4-22:2011/BYT
700 vng/pht cho n khi hon tt vic xc nh. Gia
nhit theo tc tng nhit ca glycerol 50C/pht, trnh
nh hng ca cn bng cch s dng cc tm chn nu
cn thit.
[Ch : Tc tng nhit s khng i v s khng c
tnh theo gi tr trung bnh trong ton b qu trnh th. Loi
b tt c cc php th trong tc tng nhit vt qu
0.5C cho bt k qu trnh no sau 3 pht u].
Ghi li im nng chy, chnh l nhit trn nhit k ti
mu chm vo tm nm ngang pha di (xem Hnh
1d) hoc y ca dng c cha (xem Hnh 2e). Khng hiu
chnh thn nhit k.
Mu c im nng chy di 800C: thc hin theo cch
tin hnh trn, ngoi tr s dng nhit k ASTM 15C v s
dng nc va un si c lm mt ti 50C to mi
trng nhit. i vi nha thng (gm c nha g), s
dng nc c lm ngui n nhit khng c nh
hn 450C di im nng chy d on trc nhng
khng c thp hn 50C.
Ch s hydroxyl
QCVN 4-22:2011/BYT
0,12 g acid benzoic vo cc dung tch 150 ml. Cho thanh
khuy t v 80 ml hn hp toluen/methanol theo t l 1/1.
Khuy u dung dch trong khi chun vi dung dch
KOH trong methanol. Dung dch KOH cn phi cho xung
di b mt ca dung dch, cch xa in cc. Tnh ton
nng dung dich KOH trong methanol da theo phng
trnh tnh ton c biu th di y.
- Tetrahydrofuran (THF): sy qua m v cho qua ry phn
t 3
- p-Toluenesulfonyl isocyanat (p-TSI)
- Dung dch p-Toluenesulfonyl isocyanat: khong 0,22 M
hoc 4,5 mEq/20 ml dung dch. Dng pipet ly 15 ml pToluenesulfonyl isocyanat (p-TSI)
cho vo 500 ml
tetrahydrofuran (THF) kh v lc u.
Ch :
V isocyanat c bn cht rt c nn khi chun b v s
dng dung dch isocyanat phi c tin hnh trong t ht.
Cn phi eo gng tay khi cm vo isocyanat v dung dch
ca isocyanat trnh tip xc vi da.
- Dung dch ch th bromocresol ta: cho 0,1 g
bromocresol ta vo 18,5 ml dung dch NaOH 0,1 N v
pha ti th tch 250 ml bng nc ct.
Cch tin hnh:
Cn 1 - 1,5 g mu chnh xc n 0,0001 g cho vo bnh
Erlenmeyer kh dung tch 250 ml c ni vi khp ni
thu tinh hnh trn. Dng pipet ly 10 ml dung dch THF
kh cho vo bnh v ho tan mu. Dng pipet ly 20 ml
dung dch p TSI cho vo bnh v lc u. Cho vi ht
bt, ni vi sinh hn v bnh trn tm gia nhit. Gia
nhit n khi si vi sinh hn ngc trong 10 pht. Trong
qu trnh chng ct b sung thm nc thch hp qua sinh
hn:
Mu trng
Mu th
Chun vi ch th mu
2
2
Chun bng o th
1
1
Ly bnh v sinh hn ra khi tm gia nhit v ngui ti
nhit phng. Ra sinh hn bng 5 ml THF. Tho sinh
hn ra khi bnh v chuyn ton b phn dch trong bnh
vo cc dung tch 150 ml vi s tr gip ca 50 ml THF.
Cho thanh khuy t v nhng cc in cc vo hoc thm
20 git dung dch ch th. Va khuy va chun bng
thit b chun o th hoc chun vi ch th mu trc
52
QCVN 4-22:2011/BYT
quan vi dung dch KOH trong methanol. Dung dch KOH
cn phi cho xung di b mt ca dung dch cch xa
in cc. Xc nh th tch dung dch KOH dng
chun mu th v chun mu trng c thc hin
qua tt c cc bc tin hnh trn.
Tnh kt qu:
Nng ca dung dch KOH trong methanol (N):
Trong :
W: Khi lng acid benzoic
122,1: ng lng ca acid benzoic
KOH: S ml dung dch KOH trong methanol dng chun
Ch s hydroxyl trong mu:
Trong :
A: S ml dung dch KOH dng chun mu th
B: S ml dung dch KOH dng chun mu trng
N: Nng dung dch KOH trong alcol
56,1: S mg KOH/mEq
AV: Ch s acid
Asen
Ch
QCVN 4-22:2011/BYT
ngui. Thm cn thn 5 ml acid nitric, lm bay hi n kh
trn tm gia nhit, sau nung trong l nung 4800C
trong 15 pht, v lm ngui. Trch ly tro trong 10 ml nc
trong 2 ln, lc mi phn dch chit vo mt bnh gn. Lc
qua bt k cht khng tan trn dng c lc bng 6 ml dung
dch amoni citrat TS, 2 ml hydroxylamin hydrochlorid TS v
5 ml nc, thm nc ra c lc vo bnh gn. Tip
tc theo hng dn trong phn Cch tin hnh trong th
Gii hn, bt u vi Thm 2 git phenol TS .... vo
bnh gn, s dng 10 g ion ch (Pb) trong mu i
chng.
Ph hng ngoi
Sc k kh ca cc alcol
nha thng
54
QCVN 4-22:2011/BYT
Thit b, dng c - im
nng chy
Hnh 1
Hnh 2
55
QCVN 4-22:2011/BYT
Ph lc 12
YU CU K THUT V PHNG PHP TH
I VI DINATRI DIPHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Ch s C.A.S.
7758-16-9
Cng thc ha hc
221,94
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Phosphat
Khng c qu 1%.
Fluorid
Arsen
Ch
5.3. Hm lng
Na2H2P2O7
6. Phng php th
56
QCVN 4-22:2011/BYT
6.1. tinh khit
Cc cht khng tan trong
nc
6.2. nh lng
57
QCVN 4-22:2011/BYT
Ph lc 13
YU CU K THUT V PHNG PHP TH
I VI CALCI POLYPHOSPHAT
1. Tn khc, ch s
2. nh ngha
INS 452iv
MTDI=70mg/kg th trng tnh cho phospho t cc ngun
thc phm
Hn hp d th ca cc mui calci ca acid polyphosphoric
c cng thc chung l Hn+2PnOn+1.
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Phosphat
Calci
Phosphat vng
Fluorid
Arsen
Ch
6. Phng php th
6.1. nh tnh
Phosphat
QCVN 4-22:2011/BYT
Ch
6.3. nh lng
59
QCVN 4-22:2011/BYT
Ph lc 14
YU CU K THUT V PHNG PHP TH
I VI CC MUI CA CC ACID BO
1. Tn khc, ch s
2. nh ngha
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Cation
Khng c qu 3%
Cc cht khng x
phng ha
Khng c qu 2 %.
Ch
5.3. Hm lng
6. Phng php th
6.1. nh tnh
Cation
un nng 1 g mu th vi hn hp gm 25 ml nc v 5 ml
acid hydrocloric. Cc acid bo to thnh ni trn b mt
thnh mt lp rn hoc du, tan trong hexan. Sau khi lm
60
QCVN 4-22:2011/BYT
ngui, gn ly lp nc v cho bay hi n kh. Ha tan
cht rn cn li trong nc v th cc cation thch hp.
61
QCVN 4-22:2011/BYT
Thnh phn acid bo
Cc cht khng x
phng ha
QCVN 4-22:2011/BYT
Chuyn ton lng tng t mt dung dch ether qua cung
ca phu tch vo bnh cu kh v cn b khi lng
chnh xc n 0,0001 g.
Lm bay hi dung mi bng cch ct trong b cch thy.
Thm 5 ml aceton v loi b hon ton dung mi bay hi
bng cch thi khng kh nh, nghing bnh cu khi quay
trong b cch thy.
Sy kh phn cn cn li nhit 1032 C trong 15 pht,
t bnh cu theo phng gn nh nm ngang. Lm ngui
trong bnh ht m v cn (chnh xc n 0,0001 g). Lp li
qu trnh sy trong mi 15 pht lin tip cho n khi chnh
lch gia 2 ln cn lin tip nh hn 0,0015g.
Ch : Nu khng thu c khi lng khng i sau 3 ln
sy kh, cc cht khng x phng ha c th b nhim
bn.
Sau khi cn, ha tan phn cn trong 4 ml diethyl ether,
thm 20 ml ethanol c trung ha (dung dch c mu
hng khi thm ch th l dung dch phenolphthalein(TS).
Chun bng dung dch kali hydroxyd trong ethanol 0,1 N
chun ha (pha dung dch kali hydroxyd trong ethanol c
nng gn ng 1 N bng cch ha tan 60 g kali hydroxyd
trong 50 ml nc v pha long thnh 1 L bng ethanol; pha
long dung dch ny 1:10 bng ethanol) n khi dung dch c
mu pht hng.
Hiu chun khi lng cn cn li bng cch tr i hm
lng acid t do. Tnh hm lng cht khng x phng ha,
theo % (kl/kl) bng cng thc sau:
trong :
m = khi lng (g), ca phn mu th,
m1 = khi lng (g), ca cn cn li.
V = th tch dung dch kali hydroxyd chun ha nng
dng chun .
T = Nng chnh xc ca dung dch kali hydroxyd dng
chun .
63
QCVN 4-22:2011/BYT
Ch
6.2. nh lng
Nguyn tc:
X phng ha cc mui v ester ha cc acid bo bng
methanol, c mt bo trifluorid, methanol kim. Tin hnh sc
k lng kh cc ester methyl ca acid bo.
Phn A - Chun b cc ester methyl ca acid bo
Thit b
- Bnh y trn c nhm 50 v 100 ml.
- Sinh hn hi lu, chiu di hiu dng 20 to 30 cm, c khp
ni nhm tng thch vi bnh cu.
- Cc phu tch 250 ml.
- ng ng vo dn kh nitrogen.
- ng nghim c nt thy tinh nhm.
- Pipet chia , c th tch t nht l 10 ml, c gn qu bp
cao su, hoc pipet t ng.
Thuc th
- Heptan, dng cho sc k (Ch 2 v 4)
- Du nh c ct li (nhit si t 40-60 ), ch s
brom < 1, khng c cn, hoc hexan (Ch 2)
- Natri sulfat khan
- Dung dch Natri hydroxyd trong methanol ~ 0.5 N: Ha tan
2g natri hydroxyd trong 100 ml methanol cha khng qu
0.5% (kl/kl) nc. Nu gi dung dch tng i lu c th to
thnh mt lng nh kt ta mu trng ca natri. iu ny
khng nh hng n kt qu iu ch methyl ester.
- Dung dch bo trifluorid trong methanol, 12 n 25% (kl/kl) .
Ch phm thng mi sn c l dung dch 14 v 50% (ch
2)
Cnh bo: Bo trifluorid c. V vy th nghim vin khng
nn pha dung dch bo trifluorid trong methanol t methanol
v boron trifluorid. (ch 3).
- Dung dch bo ha natri clorid trong nc.
- Methyl , dung dch 1 g/l trong ethanol 60% (tt/tt)
- Nitrogen, c hm lng oxy < 5 mg/kg
Tin hnh
Do bo trifluorid c, cc th nghim sau tt nht nn tin
hnh trong t ht. Cc dng c thy tinh phi c ra bng
nc ngay sau khi s dng.
Sy kh mu nhit 105 C n khi lng khng i, c
2 gi th kim tra khi lng 1 ln. Cn khang 350mg
64
QCVN 4-22:2011/BYT
(chnh xc n mg) mu sy kh. C th ly lng mu
ln hoc nh hn 350 mg, tuy nhin, th tch ca bnh cu v
lng thuc th s dng phi ph hp vi s liu trong bng
sau:
Khi lng
NaOH 0.5 Dung dch BF3
Th tch bnh
mu
N
trong methanol
(mg)
(ml)
(ml)
(ml)
100-250
50
4
5
250-500
50
6
7
500-700
100
8
9
750-1000
100
10
12
Cho lng acid bo nh vo bnh cu ph hp. Thm vi
lng ph hp dung dch bo trifluorid trong methanol. un
si trong vng 2 pht.
Thm 2 n 5 ml heptan (ch 4) (lng chnh xc khng
nh hng n phn ng) qua u trn ca sinh hn vo
hn hp ang si v tip tc un si trong 1 pht.
Ngt ngun nhit, ly sinh hn ra. Thm lng nh dung
dch natri clorid bo ha v lc nh bnh bng cch quay trn
bnh vi ln.
Thm dung dch natri clorid bo ha vo bnh cu sao cho
mc cht lng ngang c bnh. yn cho hn hp tch lp
v chuyn khong 1 ml lp trn (lp heptan) vo ng nghim
c nhm v thm vo mt lng nh natri sulfat khan loi
ht nc. Nu lng mu ly l 350 mg, dung dch ny cha
khong 7-17% methyl ester v c th bm trc tip vo ct
sc k kh-lng. Nu khng th pha long dung dch bng
heptan t c nng methyl ester l 5-10% (ch 5).
thu hi ton b lng ester kh, chuyn dung dch mui
v lp heptan vo phu tch. Tch ring cc lp. Chit phn
dung dch mui 2 ln bng 50 ml du nh. Gp dch chit du
nh thu c vo phn dung dch heptan, ra bng 20 ml
nc n khi ht acid (th bng ch th methyl). Lm kh
bng natri sulfat khan, lc v cho bay hi dung mi trong b
cch thy v thi kh nitrogen (ch 6 v 7). Vi cc mu c
khi lng nh hn 500 mg phi gim th tch dung mi v
nc s dng theo t l tng ng.
Bn cnh phng php trn cn c mt s phng php
khc khng s dng n bo trifluorid. Nhn chung c th thay
cc thuc th methyl ha, dung dch natri hydroxyd 0,5N
trong methanol v dung dch bo trifluorid 12-25 %, trong
methanol bng cc cht sau:
- Kali hydroxyd 1 N trong methanol, (phn ng vi cht bo
khi c mt lng d methanol c hm lng nc nh);
- Dung dch natri methylat (iu ch bng cch ha tan 1 g
natri kim loi trong 100 ml methanol c hm lng nc
nh).
Ch
1. Nu cc cht khng x phng ha gy cn tr, pha long
65
QCVN 4-22:2011/BYT
dung dch x phng ha vi nc v loi b cc cht khng
x phng ha bng cch chit vi diethyl ether hoc hexan.
Acid ha dung dch nc x phng v tch ly cc acid bo.
iu ch cc methyl ester t cc acid bo theo hng dn.
2. Khi o sc k kh lng ca cc methyl ester, mt s thuc
th, c bit l bo trifluorid trong methanol c th to nn cc
peak ngu nhin trn sc (trong vng cc ester c mch
C20-C22 nu dng bo trifluorid trong methanol). Do vy cn
phi kim tra li mi t thuc th mi bng cch iu ch
cc methyl ester ca acid oleic tinh khit, v o sc k. Nu
xut hin peak ngu nhin, phi b khng dng thuc th.
Cc thuc th khc nhau khng c php cho peak gy
nhiu n cc peak ca cc methyl ester ca cc acid bo
trong qu trnh chy sc k.
Dung dch bo trifluorid trong methanol phi c bo qun
trong t lnh.
3. Nu bt buc phi iu ch dung dch bo trifluorid t bo
trifluorid kh, nn dng phng php sau: Cn khi lng ca
bnh cu 2 L cha 1 L methanol. Lm lnh trong b . Vn
gi nguyn bnh trong b , sc kh BF3 t chai kh
(cylinder) qua ng dn thy tinh vo dung dch methanol cho
n khi hp th c 125 g BF3. Tin hnh th nghim trong
t ht. Phi cho BF3 chy qua ng thy tinh trc khi t
ng vo v rt ng ra khi methanol trnh trng hp
cht lng b ht vo h thng van ca chai kh. Khng c
cho kh chy nhanh qu c hi kh trng ra khi bnh.
Thuc th pha theo cch ny bn trong 2 nm.
4. Nu cc acid bo cha 20 hoc nhiu hn 20 nguyn t
carbon khng c mt, nn thay heptan bng hexan (hn hp
ca cc ng phn C7 tinh khit c th c kim tra bng
sc k kh lng)
5. Nu khng c lng mu nh yu cu, c th ly 10
mg, thm ch t hn, min l lng thuc th v kch c ca
cc dng c thy tinh c gim theo t l tng ng.
6. Cc dung dch methyl ester nn c phn tch cng sm
cng tt. Nu cn, bo qun dung dch heptan cha cc
methyl ester trong mi trng kh tr trong t lnh. Nu cn
phi bo qun trong thi gian di, nn bo v cc methyl
ester khi s oxy ha bng cch thm vo dung dch cc
cht chng oxy ha nng khng nh hng n kt qu
phn tch, v d nh 0,05 g/L EHT (2,6-di-tertbutyl-4-methyl
phenol).
Trong trng hp cn thit, c th bo qun cc methyl ester
kh sch dung mi trong kh tr trong t lnh trong 24 gi,
hoc c th bo qun lu hn nu gi ng lnh su trong
ng kn trong chn khng.
7. Mt phn cc methyl ester d bay hi nht c th b mt
nu thi gian bay hi dung mi ko di, hoc nu dng kh
nitrogen qu mnh,
o ph hng ngoi, phi loi b dung mi cng trit
66
QCVN 4-22:2011/BYT
cng tt.
o sc k kh lng, loi b hon ton dung mi.
Phn B - Sc k kh lng ca cc ester methyl acid bo
Thit b
Thit b thng thng dng cho sc k kh lng, dng ct nhi
v detector ion ha ngn la (ch 1). Bt k mt thit b
no cho hiu qu v phn gii cao vi cht bo cn xc
nh u ph hp.
Sc k kh lng
H thng bm mu: H thng bm mu phi c khng gian
cht nh nht c th. Nu c, phi nng c nhit
cao hn nhit ct t 20 n 50 C.
L: L phi cung cp cho ct nhit t nht l 220o v phi
duy tr c nhit cn thit trong khong 1 C.
Nu dng chng trnh t nhit , nn dng thit b c ct
i.
Ct nhi:
- Ct: Ct phi c lm t lai vt liu tr vi cht cn phn
tch: thy tinh hoc nu khng th dng thp khng r (ch
2). Chiu di: 1 n 3 m, nn dng ct tng i ngn nu
c cc acid mach di (C20+). xc nh cc acid bo C4 v
C6, nn dng ct 2 m; ng knh trong t 2 n 4 mm.
Nhi ct
- Cht mang: Diatomid ra acid v c silan ha, hoc
cc cht mang tr ph hp khc c khong bin thin
ng knh hp (25 m) trong khong ng knh c ht t
125-200 m, c ht trung bnh phi tng quan vi ng
knh trong v chiu di ct.
- Pha tnh: Dng polyester ca mt cht lng phn cc (v d
diethylen glycol polysuccinat, butandiol polysuccinat, ethylen
glycol polyadipat ...) hoc bt k cht lng no khc (v d
cyanosilicon ...) tha mn cc iu kin di y. Pha tnh
phi chim 5 n 20 % khi lng nhi. C th dng mt
pha tnh khng phn cc, ty theo tng php tch c th.
- Luyn ct mi ch to: Tch ct ra khi detector. Nu c
th, t t nung l n 185 C v dn dng kh tr qua ct vi
tc 20-60 ml/pht trong t nht l 16 gi ti nhit ny,
v thm 2 gi na ti 195 C.
Detector: Cc vn hnh di y tng ng vi detector ion
ha ngn la (ch 1)
Syring: Syring, c dung tch ti a l 10 l, chia n 0.1 l.
My ghi:
Nu s dng ng ghi tnh thnh phn hn hp phn
tch, phi dng mt my ghi in t c chnh xc cao.
My ghi phi tng thch vi thit b o. Cc c trng ca
67
QCVN 4-22:2011/BYT
my ghi phi nh sau:
- Tc p ng di 1,5 giy, tt nht l di 1 giy (tc
p ng l thi gian cn bt ghi chy t 0 n 90 %
theo 100 % tn hiu)
- rng ca giy: ti thiu l 25 cm
- Tc giy: 25-100 cm/gi.
B tch phn Integrator hoc my tnh (ty chn)
C th tnh mt cch nhanh v chnh xc nu dng b tch
phn in t hoc my tnh. Trong trng hp ny phi to
c tn hiu tuyn tnh vi nhy ph hp, v phn hiu
chnh cho s lch ng nn phi tha ng.
Ha cht
- Kh mang: Kh tr (nitrogen, heli, argon ...) kh, v cha t
hn 10 mg/kg oxy.
- Kh ph tr: Hydrogen (tinh khit ti thiu 99.9%) khng c
cc tp cht hu c, khng kh hoc oxygen.
- Cc cht chun so snh: Hn hp ca cc methyl ester,
hoc cc methyl ester ca mt cht du bit trc thnh
phn, tt nht l tng t vi cht bo cn phn tch.
Tin hnh
iu kin th
Xc nh cc iu kin vn hnh ti u: Cc gi tr cho trong
bng 1 v 2 cho di y v nguyn tc c th cho cc kt
qu mong mun:
Bng 1
ng knh trong ca ct
Kh mang cung cp
2 mm
15-25 ml/pht
3 mm
20-40 ml/ pht
4 mm
40-60 ml/ pht
Bng 2
Nng ca pha tnh
Nhit
5%
175 o
10%
180 o
15%
180o
20%
185 o
Nu c, injector phi nhit khong 200oC v
detector phi nhit bng hoc cao hn nhit ct.
V nguyn tc dng kh hydrogen cung cp cho detector ion
ha ngn la phi c tc bng mt na tc kh mang,
v tc kh oxygen phi bng khong 5 n 10 ln tc
kh hydrogen.
Xc nh hiu sut v phn gii (ty chn)
Tin hnh phn tch mu chun methyl stearat. La chn c
mu, nhit ct tch v tc kh mang sao cho peak ca
methyl stearat xut hin 15 pht sau peak dung mi v cao
khong 3/4 tn hiu ton thang.
- Phn tch:
68
QCVN 4-22:2011/BYT
Dng mu kim tra l 0,1 n 2 l dung dch heptan ca
methyl esters, pha theo hng dn trong phn A. Trong
trng hp khng c cc ester trong dung dch, chun b
dung dch c nng khong 10% trong heptan v bm 0,1
n 1 l dung dch ny.
Cc iu kin tin hnh c cho di y. Tuy nhin, c
th lm vic vi nhit ct thp hn nu xc nh cc acid
c mch carbon di C12 hoc nhit cao hn nu xc
nh cc acid bo trn C20.
i khi c th s dng chng trnh t nhit cho c 2
trng hp trn. Nu mu c cha cc methyl ester ca cc
acid bo di C12, phi bm mu nhit 100 C (hoc
nhit t 50 - 60 C nu c acid butyric) v ngay lp tc
tng nhit vi tc tng nhit t 4 - 8 C/pht cho n
nhit ti u. Trong mt s trng hp c th gp c 2 qui
trnh li: sau khi tng nhit, tip tc ra gii ti nhit
khng i cho n khi tt c cc hp phn c ra gii ra.
Nu thit b khng vn hnh vi chng trnh nhit , lm
vic ti 2 nhit c nh trong khong t 100 n 195 C.
Biu th kt qu
Phn tch nh tnh
Phn tch hn hp cht chun so snh c thnh phn
bit trong cc iu kin s dng o mu th. o khong
cch lu (hoc thi gian lu) cho cc ester bo tng ng.
Dng giy bn logarit, v th biu din s ph thuc ca
logarit khong cch lu (hoc thi gian lu) vo s nguyn
t carbon ca cc acid; trong iu kin ng nhit th ca
cc ester mch thng c cng khng bo ha (no) phi l
cc ng thng. gn nh song song vi nhau.
Nhn dng cc peak ca mu th t cc th ny, nu cn
th dng php ni suy. Phi trnh cc iu kin o lm xut
hin cc peak b che ph (masked peaks), c ngha l
phn gii khng ln tch c 2 hp phn.
Phn tch nh lng
Xc nh thnh phn
Tr cc trng hp c bit, s dng phng php chun
ha din tch, c ngha l gi thit rng ton b cc hp phn
u c biu din trn sc , sao cho tng din tch cc
peak biu din 100 % cc hp phn (tng ra gii).
Bng mt qui trnh chun ha ph hp (dng hn hp chun
so snh hoc dng cht chun ni), xc nh tng khi lng
ca cc acid bo trong mu kh. Tnh hm lng mui ca
cc acid bo vi cc cation c trng trong mu. Tng hm
lng Mui Acid Bo khng c ln hn 95% khi lng
mu kh. Ngoi ra, nu c cc ch tiu cho hm lng ca
mi acid bo ghi trn nhn sn phm, mu phi tha mn
c cc ch tiu ny.
Ch
1. C th s dng my sc k kh - lng dng thit b o
69
QCVN 4-22:2011/BYT
dn nhit ca kh (catharometer) (lm vic trn nguyn tc
o s thay i dn nhit). Cc iu kin o khi c
thay i nh sau:
Ct
- chiu di: 2 n 4 m
- ng knh trong: 4 mm
- cht mang: ng knh ht trong khong 160 n 200 m
- pha tnh: 15 n 25%
Kh mang: heli, nu khng th dng hydrogen, c hm lng
oxygen cng nh cng tt. Khng dng kh ph tr
- Tc kh: thng trong khong t 60 n 80 ml/pht
Nhit
Injector: cao hn t 40o n 60oC so vi nhit ct
Ct: 180o to 200oC
Phn tch nh lng: phi hiu chnh theo cc h s thu
c khi phn tch hn hp so snh ca cc ester c thnh
phn bit trong cng iu kin o vi mu th.
2. Nu trong mu c cc thnh phn cha nhiu hn 3 ni
i, chng c th b phn hy trn ct thp khng r.
70
QCVN 4-22:2011/BYT
Ph lc 15
YU CU K THUT V PHNG PHP TH
I VI ESTER CA SUCROSE VI CC ACID BO
1. Tn khc, ch s
2. nh ngha
3. Cm quan
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Acid bo
ng
Khng c qu 2%
Th 1 g mu (Phng php I)
Ch s acid
Khng c qu 6
Sucrose t do
Dimethylformamid
Dimethyl sulfoxid
Ethyl acetat,
isopropanol v propylen
glycol
Isobutanol
Methanol
QCVN 4-22:2011/BYT
php th
72
QCVN 4-22:2011/BYT
Ch
5.3. Hm lng
6. Phng php th
6.1. nh tnh
Acid bo
ng
73
QCVN 4-22:2011/BYT
Sucrose t do
74
QCVN 4-22:2011/BYT
Dimethylformamid
Xc nh bng sc k kh lng
Dung dch chun:
Chun b dung dch gc cha 1 mg/ml dimethylformamid
trong tetrahydrofuran. Chun b mt lot cc dung dch
chun cha 0,05; 0,1 v 0,2 g/ml dimethylformamid bng
cch pha long dung dch gc vi tetrahydrofuran.
Cc iu kin sc k:
Ct: polyethylen glycol (di 30 m x 0,32 mm ng knh
trong vi dy lp phim mng 0,5 m)
Kh mang: heli
p sut: 150 kPa (p sut khng i)
Detector: detector nitrogen phosphor (NPD) [(tn khc:
Detector nhit ion ngn la (FTD)]
Nhit :
- Bung bm mu: 1800C
- Ct: gi 400C trong 2 pht sau tng t 40 n 1600C
vi tc 200C/pht, gi trong 2 pht 1600C.
- Detector: 3250C
Phng php tim mu: Tim khng chia dng 1,0 l mu
bng bm t ng, sau bt u lm sch sau 1 pht.
Thi gian lu ca dimethylformamid o c vi cc iu
kin trn xp x 6,4 pht.
Cch tin hnh:
Cn chnh xc 2 g mu cho vo bnh nh mc dung tch
20 ml, thm vo 10 ml tetrahydrofuran ho tan mu,
thm tetrahydrofuran vo bnh n th tch 20 ml v lc
u dung dch. Bm 1,0 l dung dch mu vo thit b sc
k.
ng chun:
Chun b hng ngy bng cch bm 1,0 l mi dung dch
chun vo thit b sc k.
Tnh nng dimethylformamid (CDFA) theo cng thc sau:
Trong :
C: Nng dimethylformamid pht hin c ( g/ml)
W: Khi lng mu (g)
Lu : Detector nitrogen phosphor khng nhy vi cc
thnh phn khng cha N hoc P. V th, ct mao qun c
th tc vi cc hp cht bay hi thp, mc d ng nn
ca sc k n nh. Do , ct phi c luyn thng
xuyn. Luyn qua m (dng kh mang theo hng ngc
1800C ) c thc hin sau khong mi t 15 mu.
75
QCVN 4-22:2011/BYT
Dimethyl sulfoxid
Xc nh bng sc k kh lng
Dung dch chun:
Chun b dung dch gc 0,25 mg/ml dimethyl sulfoxid trong
tetrahydrofuran. Chun b mt lot cc dung dch chun
cha 0,5; 1 v 5 g/ml dimethyl sulfoxid bng cch pha
long dung dch gc vi tetrahydrofuran.
Cc iu kin sc k:
Ct: 10% PEG 20M v 3% KOH trn Gas Chrom Z (chiu
di 2 m x 3 mm ng knh trong). Tng nhit l ti
1800C vi tc 100C/pht v n nh 24 48 gi vi
iu kin tc dng kh nitrogen 30 40 ml/pht luyn
ct.
Kh mang: nitrogen
Tc dng: 50 ml/pht
Detector: detector trc quang ngn la (s dng b lc lu
hunh 394 nm)
Nhit :
- Bung bm mu: 2100C
- Ct: 1600C.
Thi gian lu ca dimethyl sulfoxid o c vi cc iu
kin trn xp x 3,4 pht.
Cch tin hnh:
Cn chnh xc 5 g mu cho vo bnh nh mc dung tch
25 ml, thm vo 10 ml tetrahydrofuran ho tan mu,
thm tetrahydrofuran vo bnh n th tch 20 ml v lc
u dung dch. Bm 3 l dung dch mu vo thit b sc k.
ng chun:
Chun b hng ngy bng cch bm 3 l mi dung dch
chun vo thit b sc k.
Tnh nng dimethyl sulfoxid (CDMSO) theo cng thc sau:
Trong :
C: Nng dimethyl sulfoxid pht hin c ( g/ml)
W: Khi lng mu (g)
76
QCVN 4-22:2011/BYT
Propylen glycol
Xc nh bng sc k kh lng
Dung dch ni chun:
Chun b dung dch 500
pyridin
Dung dch chun:
Trong :
C: Nng propylen glycol pht hin c ( g/ml)
W: Khi lng mu (g)
Lu : Nht thit phi lm sch cng bm mu v luyn
ct 3000C sau mi t 20 mu phn tch, bi ct b
nhim bn.
77
QCVN 4-22:2011/BYT
Methanol, isopropanol,
isobutanol, ethyl acetat
v methyl ethyl keton
QCVN 4-22:2011/BYT
Ch
6.3. nh lng
79
QCVN 4-22:2011/BYT
Ph lc 16
YU CU K THUT V PHNG PHP TH
I VI DIOTYL NATRI SULFOSUCINAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
S C.A.S.
577-11-7
Cng thc ha hc
C20H37NaO7S
Cng thc cu to
444,56
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Ph hng ngoi
pH
Tro sulfat
QCVN 4-22:2011/BYT
(th theo hng dn ti JECFA monograph 1 - Vol.4;
Phng php I, cn 1 g mu)
81
QCVN 4-22:2011/BYT
Bis-(2-ethylhexyl)-maleat
Khng c qu 0,4 %.
Ch
5.3. Hm lng
6. Phng php th
6.1. tinh khit
Bis-(2-ethylhexyl)-maleat Thuc th
- Cht in gii h tr: Ha tan 21,2 g lithi perchlorat
(LiClO4) khan vo 175 ml nc trong cc 250 ml. iu
chnh pH ca dung dch ny n 3,0 bng cch thm tng
git acid acetic bng (khong 1 n 2 git l ), dng mt
my o pH ph hp. Chuyn ton lng dung dch vo
bnh nh mc 200 ml, pha long n vch bng nc, v
trn u.
- Dung dch chun: Chuyn 100 - 110 mg (cn chnh xc)
bis-(2-ethyl-hexyl)-maleat, (bis-(2-ethylhexyl)-maleat vi
tinh khit ph hp c tn khc l OT-35 ca Cng ty
American Cyanamid, Pine Chemicals Department, Pearl
River, New York 10965, USA), vo bnh 100 ml. Ghi li khi
lng chnh xc, chnh xc n 0,1 mg, Wa. Pha long n
vch bng nc, trn u.
- Dung dch mu th gc: Chuyn 12,5 g mu th,
c cn chnh xc, vo cc 150 ml. Ghi li khi lng
chnh xc, Ws, chnh xc n 10 mg. Thm 80-90 ml
isopropanol, khuy bng a thy tinh n khi mu tan
hon ton. Chuyn ton lng dung dch ny vo bnh nh
mc 250 ml bng isopropanol. Pha long n vch bng
isopropanol, trn u.
- Dung dch th A: Dng pipet ly 50.0 ml "Dung dch mu
th gc" v 20,0 ml "Dung dch in gii h tr " vo bnh
nh mc 100 ml. Pha long vi isopropanol n khong
di vch nh mc 15 mm, y nt, lc u v trong 2
pht. Pha long tip bng isopropanol n vch, y nt,
lc u. Phi thu c dung dch tuyt i trong.
- Dung dch th B: Dng pipet ly 50,0 ml "Dung dch mu
th gc", 10,0 ml "Dung dch chun", v 20,0 ml Dung
dch in gii h tr" vo bnh nh mc 100 ml, v tip tc
qui trnh nh miu t trong phn Dung dch th A
- Mu trng: Dng pipet ly 20,0 ml "Dung dch in gii h
tr" vo bnh nh mc 100-ml, pha long n vch bng
isopropanol, trn u.
Tin hnh
Ra bnh cc ph H-cell vi ln bng tng lng nh
Dung dch th A, sau y mt na bnh bng dung
dch ny, t mt mu giy thm ln ming bnh v cho
dng kh nitrogen chy t t qua dung dch trong 15 pht
(Ch : Trc ht phi bo ha nitrogen bng cch cho
chy qua bnh sc ph hp c cha isopropanol). Sau 15
82
QCVN 4-22:2011/BYT
pht, hng dng nitrogen ln b mt dung dch v ly giy
ra khi bnh. Vi mt cc ph k ph hp c hiu
chun trc (nh cc ph k Metrohm Polacord E-261,
hoc tng ng t mt th phn cc -1,3V. iu
chnh nhy dng ti thang thp nht (nhy nht) m ti
cc dao dng dng vn nm trong thang. Ghi li cc
ph ti nhy ny, qut th trong khong t -0,9 n 1,5 V, dng in cc so snh l in cc calomel bo ha.
Ghi li dao ng trung bnh A ti th -1,3 V, v dao ng
trung bnh B, ti th -1,0 V, theo mm. (Ch : nu s dng
cc ph k khng t ng, ghi li cc dao ng dng
khuch tn trung bnh ca dung dch tng ng ti -1,3 V
v -1,0V). Lp li ton b qu trnh vi dung dch th B, ghi
li gi tr dao ng dng khuch tn trung bnh, D, ti -1,3 V
v E, ti -1,0 V.
Lm tng t vi mu trng, ghi li gi tr dao ng dng
khuch tn trung bnh, G, ti -1,3V v H, ti -1 V.
Tnh ton:
Trc ht tnh cc ga tr sau (theo mA):
trong
C l cng dng khuch tn ca Dung dch th A v
S1 l nhy dng khi o "Dung dch th A"
trong
F l cng khuch tn ca Dung dch th B v
S2 l nhy dng khi o "Dung dch th B"
trong
I l cng dng khuch tn ca Mu trng v
S3 l nhy dng khi o "Mu trng"
trong
J l dng khuch tn gy ra do thm maleat t Dung dch
chun vo Dung dch th B.
trong
K dng khuch tn gy ra do maleat c trong Dung dch
th A.
Cui cng, tnh phn trm ca bis-(2-ethylhexyl)-maleat c
trong mu ban u theo cng thc sau:
83
QCVN 4-22:2011/BYT
Ch
6.2. nh lng
Cc dung dch
- Dung dch mu: Chuyn khong 3,8 g mu th, trc
c sy kh 105 C trong 2 gi v c cn
chnh xc, vo bnh nh mc 500 ml, ha tan trong
cloroform. Pha long n vch bng dung mi trn, trn
u.
- Dung dch tetra-n-butylamoni iodid: Chuyn 1,250 g tetran-butylamoni iodid vo bnh nh mc 500 ml, pha long
n vch bng nc, trn u.
- Dung dch mui: Ha tan 100 g natri sulfat khan v 10 g
natri carbonat vo mt lng nc va c c th
tch cui cng l 1000 ml.
Tin hnh
Dng pipet ly 10,0 ml "Dung dch mu" vo bnh nh mc
250 ml, thm vo 40 ml cloroform, 50 ml "Dung dch
mui", 10 git dunh dch xanh bromophenol (TS). Chun
bng "Dung dch tetra-n-butylamoni iodid" n khi bt
u xut hin mu xanh trong lp cloroform sau khi lc
mnh dung dch. Tnh hm lng (%) C20H37NaO7S theo
cng thc:
trong
V = th tch (ml) ca dung dch tetra-n-butylamoni iodid
dng chun .
444,6 = khi lng phn t ca dioctyl natri sulfosuccinat
W = khi lng (g) ca mu th
369,4 = khi lng phn t ca tetra-n-butylamoni iodid.
84
QCVN 4-22:2011/BYT
Ph lc 17
YU CU K THUT V PHNG PHP TH
I VI STEARYL TARTRAT
1. Tn khc, ch s
2. nh ngha
Tn ho hc
Cng thc ho hc
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, khng tan trong ethanol lnh, tan
trong ethanol nng.
67 770C
Ch s hydroxyl
200 220
Tartrat
Ch s acid
QCVN 4-22:2011/BYT
Ch
5.3. Hm lng
6. Phng php th
6.1. tinh khit
Acid tartric tng s
ng chun:
Cn 100 mg acid tartric tinh khit cho vo bnh nh mc
dung tch 100 ml, ho tan trong khong 90 ml nc, thm
nc vo cho n khi t th tch 100 ml v lc u.
Chuyn cc phn tch bit 3, 4, 5, 6 ml vo trong cc cuvet
ph hp 19 x 150 mm, thm lng nc va n 10
ml. Thm vo 4 ml dung dch natri metavanadat 5% va
chun b v 1 ml acid acetic vo mi cuvet. (Ch : s
dng cc dung dch ny trong 10 pht sau khi xut hin
mu). Chun b mu trng theo cch tng t, s dng 10
ml nc thay th dung dch acid tartric. t trn thit b
hp th bng 0 i vi mu trng, sau o hp th
ca 4 dung dch acid tartric bc sng 520 nm vi my
quang ph thch hp hoc my so mu quang in c
trang b knh lc 520 nm. T cc kt qu thu c, v
ng chun trn h to vung gc vi trc tung biu
din hp th v trc honh biu din hm lng acid
tartric (mg).
Chun b mu th:
Cn chnh xc 4 g mu cho vo bnh Erlenmeyer dung tch
250 ml v thm vo 80 ml dung dch KOH 0,5N v 0,5 ml
phenolphthalein TS. Ni bnh vi mt sinh hn khng kh
c chiu di t nht 65 cm v gia nhit hn hp trn tm
bn nng trong 2,5 gi. Thm vo hn hp nng acid
phosphoric 10% cho n khi c phn ng acid r rt pht
hin c bng giy th congo. Li kt ni sinh hn kh
v gia nhit cho n khi acid bo ho lng v trong. Lm
ngui v chuyn hn hp vo mt phu chit dung tch 250
ml bng cc phn nh nc v chloroform. Chit tch cc
acid bo c gii phng ra bng 3 ln lin tip 25 ml
nc v cho phn nc ra vo phu chit cha lp
nc. Chuyn cc thnh phn c trong phu chit th nht
vo cc 250 ml, gia nhit trn chu hi nc loi cc
vt chloroform, lc qua giy lc mn vo bnh nh mc
dung tch 500 ml v cui cng pha ti th tch 500 ml bng
nc (Dung dch I). Dng pipet ly 25 ml dung dch ny
cho vo bnh nh mc dung tch 100 ml v pha ti th tch
100 ml bng nc (Dung dch II).
Cch tin hnh:
Chuyn 10 ml Dung dch II c chun b trong phn
Chun b mu th vo cuvet 19 x 150. Thm vo 4 ml dung
dch natri metavanadat 5% va chun b v 1 ml acid
acetic. (Ch : s dng cc dung dch ny trong 10 pht
86
QCVN 4-22:2011/BYT
sau khi xut hin mu). Chun b mu trng theo cch
tng t, s dng 10 ml nc thay th dung dch acid
tartric. t trn thit b o hp th bng 0 i vi mu
trng, sau o hp th ca 4 dung dch acid tartric
bc sng 520 nm vi my quang ph thch hp hoc my
so mu quang in c trang b knh lc 520 nm. T
ng chun xc nh hm lng acid tartric (mg) trong
dung dch pha cui cng, nhn hm lng acid tartric xc
nh c vi 20 v chia cho trng lng mu ban u
thu c % acid tartric.
87
QCVN 4-22:2011/BYT
Cht khng x phng
ha
88
QCVN 4-22:2011/BYT
Ch s acid
Ch
6.2. nh lng
89
QCVN 4-22:2011/BYT
Ph lc 18
YU CU K THUT V PHNG PHP TH
I VI SORBITAL MONOSTEARAT
1. Tn khc, ch s
INS 491
ADI=0-25mg/kg th trng
2. nh ngha
Ch s C.A.S
1338-41-6
Cng thc cu to
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
o
Khong nhit ng c 50-52 C.
Hp th hng ngoi
Ch s acid
Ch s x phng ha
Ch s Hydroxyl
90
QCVN 4-22:2011/BYT
Ch
5.3. Hm lng
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng
91
QCVN 4-22:2011/BYT
Ph lc 19
YU CU K THUT V PHNG PHP TH
I VI SORBITAN TRISTEARAT
1. Tn khc, ch s
INS 492
ADI=0-25mg/kg th trng
2. nh ngha
Ch s C.A.S
26658-19-5
Cng thc cu to
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
o
Khong nhit ng c 47-50 C.
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 15.
Ch s x phng ha
Ch s Hydroxyl
Ch
QCVN 4-22:2011/BYT
5.3. Hm lng
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng
93
QCVN 4-22:2011/BYT
Ph lc 20
YU CU K THUT V PHNG PHP TH
I VI SORBITAN MONOLAURAT
1. Tn khc, ch s
INS 493
ADI=0-25mg/kg th trng
2. nh ngha
Ch s C.A.S
1338-39-2
Cng thc cu to
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 7.
Ch s x phng ha
Ch s Hydroxyl
Ch
5.3. Hm lng
QCVN 4-22:2011/BYT
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng
95
QCVN 4-22:2011/BYT
Ph lc 21
YU CU K THUT V PHNG PHP TH
I VI SORBITAN MONOOLEAT
1. Tn khc, ch s
INS 494
ADI=0-25mg/kg th trng
2. nh ngha
Ch s C.A.S
1338-43-8
Cng thc cu to
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Ch s iod
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 8.
Ch s x phng ha
Ch s Hydroxyl
QCVN 4-22:2011/BYT
Ch
5.3. Hm lng
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng
97
QCVN 4-22:2011/BYT
Ph lc 22
YU CU K THUT V PHNG PHP TH
I VI SORBITAN MONOPALMITAT
1. Tn khc, ch s
INS 495
2. nh ngha
Ch s C.A.S
26266-57-9
Cng thc cu to
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
ng c
45 - 470
Hp th hng ngoi
Ch s acid
Ch s x phng ha
Ch s Hydroxyl
Ch
5.3. Hm lng
QCVN 4-22:2011/BYT
trong hn hp sorbitol, 1,4-sorbitan v isosorbid.
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng
99