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a13.CHẤT ĐIỀU CHỈNH ĐỘ ACID
a13.CHẤT ĐIỀU CHỈNH ĐỘ ACID
H NI - 2010
Li ni u
QCVN 4-11:2010/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 28/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.
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:
Ph lc 1
YU CU K THUT V PHNG PHP TH I VI KALI ACETAT
1. Tn khc, ch s
INS 261
ADI khng gii hn
2. nh ngha
Tn ha hc
Kali acetat
M s C.A.S.
127-08-2
Cng thc ha hc
C2H3KO2
Cng thc cu to
CH3-COOK
98,14
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Kali
Acetat
Tnh kim
Natri
m tnh.
Ch
5.3. Hm lng
CH3-COOK
6. Phng php th
6.1. tinh khit
Tnh kim
Ch
6.2. nh lng
Cn 200 mg mu th c lm kh trc, chnh xc n
mg, ho tan trong 25 ml dung dch acid acetic bng. Cho
thm 2 git dung dch tm tinh th (TS) v chun vi dung
dch acid percloric 0,1 N trong acid acetic bng. Tin hnh
xc nh mu trng v hiu chun kt qu chun nu
cn.
Mi ml dung dch acid percloric 0,1N tng ng vi 9,814
mg C2H3KO2.
Ph lc 2
YU CU K THUT V PHNG PHP TH I VI NATRI ACETAT
1. Tn khc, ch s
INS 262(i)
ADI khng gii hn
2. nh ngha
Tn ha hc
Natri acetat
M s C.A.S.
127-09-3
Cng thc ha hc
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Acetat
Nhit
Kali
m tnh.
Ch
5.3. Hm lng
C2H3NaO4
6. Phng php th
6.1 tinh khit
Tnh acid v tnh kim
Ch
6.2. nh lng
Ph lc 3
YU CU K THUT V PHNG PHP TH I VI NATRI DIACETAT
1. Tn khc, ch s
Sodium diacetate
INS 262(ii)
ADI= 0 - 15 mg/kg th trng
2. nh ngha
Tn ha hc
M s C.A.S.
Cng thc ha hc
C4H7NaO4 . xH2O
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Th nung
Acetat
Natri
pH
Acid formic v cc tp
cht c th oxy ha
Aldehyd
Ch
5.3. Hm lng
6. Phng php th
6.1 tinh khit
Acid formic v cc tp
cht c th oxy ha
Aldehyd
Ch
6.2. nh lng
Natri acetat:
Cn 0,5 g mu th, chnh xc n mg, ho tan vo 50 ml
acid acetic bng. Lm kh bn ngoi ca t hp in cc
calomel-thu tinh gn vi 1 pH k, nhng in cc vo trong
dung dch, t pH k v mc hiu chnh +mV, sau thm
acid percloric 0,1N, mi ln thm mt th tch tng i ln
cho n gn im tng ng (s dao ng ca kim c
th d nhn thy). Sau gim th tch acid percloric 0,1N
ca mi ln thm l 0,1 ml n khi sau mi ln thm dung
dch, in th gim r rt. Xy dng th biu din tng
quan gi th tch acid percloric 0,1N vi in th o c,
qua nh lng cht cn chun tng ng vi im
gia ca bc nhy th.
V x N x 0,1421
% Natri diacetat =
x 100
w
Trong :
V: th tch ca dung dch acid percloric, ml
N: chun chnh cc ca dung dch acid percloric
w: trng lng ca mu th, g
Acid acetic t do:
Cn 4 g mu th, chnh xc n mg, v ho tan trong 50 ml
dung dch nc ct pha long. Chun dung dch vi dung
dch natri hydroxyd N c s dng dung dch phenolphatalein
(TS) lm cht ch th.
V x N x 0,060
% Acid acetic t do=
x 100
w
Trong :
V: th tch ca dung dch natri hydroxyd, ml
N: chun chnh cc ca dung dch natri hydroxyd
w: trng lng ca mu th, g
Ph lc 4
YU CU K THUT V PHNG PHP TH I VI CALCI ACETAT
1. Tn khc, ch s
INS 263
ADI khng gii hn.
2. nh ngha
Tn ha hc
Calci acetat
M s C.A.S.
62-54-4
Cng thc ha hc
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Acetat
Calci
pH
Khng c qu 0,3%.
Acid formic v cc tp
cht c th oxy ha
Aldehyd
Ch
5.3. Hm lng
C4H6CaO4
6. Phng php th
6.1 tinh khit
Tp cht khng tan trong
nc
Acid formic v cc tp
cht c th oxy ha
Aldehyd
Ch
6.2. nh lng
1. Hm lng calci:
Cn 2,5 g mu th, chnh xc n mg, cho vo cc, ha tan
trong 5 ml dung dch acid hydrocloric long nng. ngui,
chuyn vo bnh nh mc 250 ml, pha long n vch
bng nc ct, lc u. Ly 50 ml dung dch ny vo cc
400 ml, thm 100 ml nc ct, 25 ml dung dch natri
hydroxyd (TS), 40 mg hn hp ch th murexid v 3 ml dung
dch xanh lc naphtol (TS) (c th s dng ch th thay th l
2,5g xanh lam hydroxynaphtol, trong trng hp ny khng
s dng dung dch xanh lc naphtol). Chun bng dung
dch dinatri ethylendiamin tetraacetat 0,05M n khi dung
dch c mu xanh m.
Mi ml dinatri ethylendiamin tetraacetat 0,05M tng ng
vi 7,909mg C4H6CaO4.
2. Hm lng acid:
Nhi n na ct sc k (ng knh 1,5 cm, cao 20cm)
bng nha trao i cation mnh (Amberlite IR120, Amberlite
IR100, Duolit C III, Dorvex 50, Lewatit KS, Ion exchanger I
Merck). Cho dung dch acid hydrocloric 0,1 N ln ct t trn
xung di, vi vi ct c kha n khi phn nha ngp
trong dung dch, yn 1-2 gi. Rt ht acid v ra ct
Ph lc 5
YU CU K THUT V PHNG PHP TH I VI ACID LACTIC
1. Tn khc, ch s
INS 270
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
C3H6O3
Cng thc cu to
O
H3C
OH
OH
90,08
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Acid
Lactat
Khng c qu 0,1%
(Phng php I, cn 2 g mu th. Gi li tro th st).
Clorid
Khng c qu 0,2%.
Sulfat
Khng c qu 0,25%
St
Cyanid
Cc ng
Cc hp cht d b than
ha
Ch
6. Phng php th
6.1 tinh khit
Clorid
Sulfat
St
Cc ng
Cc hp cht d b than
ha
Ch
6.2. nh lng
Cn (chnh xc n mg) lng mu th tng ng vi 3
g acid lactic, chuyn vo bnh 250 ml, thm 50 ml dung dch
natri hydroxyd 1 N, lc u v un si trong 20 pht. Thm
dung dch phenolphtalein (TS), khi dung dch cn nng,
chun lng kim d vi acid sulfuric 1 N, tin hnh
lm 1 mu trng song song.
Mi ml dung dch natri hydroxyd 1N tng ng vi 90,08
mg C3H6O3.
Ph lc 6
YU CU K THUT V PHNG PHP TH I VI ACID MALIC
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
6915-15-7
C4H6O5
Cng thc cu to
COOH
CHOH
CH2
COOH
134,1
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
127o - 132o.
Malat
Ch
6. Phng php th
6.1 tinh khit
Ch
6.2. nh lng
Cn khong 2 g (chnh xc n mg) mu th, ha tan trong
40 ml nc mi un si, ngui, thm 2 git dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 1 N n khi dung dch bt u c mu hng nht
bn trong 30 giy.
Mi ml dung dch natri hydroxyd 1 N tng ng vi
67,04 mg C4H6O5.
Ph lc 7
YU CU K THUT V PHNG PHP TH I VI ACID FUMARIC
1. Tn khc, ch s
INS 297
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
110-17-8
Cng thc ha hc
C4H4O4
Cng thc cu to
COOH
C
C
HOOC
116,07
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Lin kt i
Tro sulfat
Acid maleic
Khng c qu 0,1%.
Ch
6. Phng php th
6.1 nh tnh
Acid 1,2 dicarboxylic
Lin kt i
6.3. nh lng
Cn 1g mu th, chnh xc n mg, chuyn vo bnh nn
250 ml, thm 50 ml methanol, ho tan mu bng cch lm
m nh trn b cch thu. ngui, thm dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 0,5 N cho n khi xut hin mu hng bn trong
t nht 30 giy. Tin hnh xc nh mu trng v hiu
chun nu cn.
Mi ml dung dch natri hydroxyd 0,5 N tng ng vi
29,02 mg C4H4O4.
Ph lc 8
YU CU K THUT V PHNG PHP TH I VI NATRI LACTAT
1. Tn khc, ch s
INS 325
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
72-17-3
C3H5NaO3
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
Nung
Phn ng mu
Lactat
Natri
t yu cu
pH
Ch
5.3. Hm lng
C3H5NaO3
6. Phng php th
6.1 tinh khit
Tnh acid
Ch
6.2. nh lng
Cn 0,6 g (chnh xc n mg) mu cho vo mt cc nh v
cho bay hi n kh. Thm vo cn cn li 60 ml hn hp
anhydrid acetic/acid acetic bng (1/5), khuy u n khi
cn tan hon ton. Thm dung dch tm tinh th (TS) v
chun vi dung dch acid percloric 0,1 N n im kt
thc dung dch c mu xanh.
Mi ml dung dch acid percloric 0,1 N tng ng vi
11,21 mg C3H5NaO3.
Ph lc 9
YU CU K THUT V PHNG PHP TH I VI KALI LACTAT
1. Tn khc, ch s
INS 326
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
996-31-6
C3H5KO3
Cng thc cu to
O
CH3
O
OH
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
Nung
Phn ng mu
Lactat
Kali
Cc hp cht kh
Ch
6. Phng php th
6.1 tinh khit
Tnh acid
Ch
6.2. nh lng
Cn 0,6 g (chnh xc n mg) mu cho vo mt cc nh v
cho bay hi n kh. Thm vo cn cn li 60 ml hn hp
anhydrid acetic/acid acetic bng (1/5), khuy u n khi
cn tan hon ton. Thm dung dch tm tinh th (TS) v
chun vi dung dch acid percloric 0,1 N n im kt
thc dung dch c mu xanh. Tin hnh lm mu trng
song song v hiu chnh kt qu nu cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
12,82 mg C3H5KO3.
Ph lc 10
YU CU K THUT V PHNG PHP TH I VI ACID CITRIC
1. Tn khc, ch s
INS 330
ADI khng gii hn
2. nh ngha
Tn ha hc
Acid 2-hydroxy-1,2,3-propantricarboxylic
M s C.A.S.
Cng thc cu to
CH2
HO
C
CH2
COOH
COOH
CH2
HO
COOH
Dng khan
C
CH2
COOH
COOH
.HO
2
COOH
Dng monohydrat
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Citrat
Tro sulfat
Khng c qu 0,05%.
Oxalat
Sulfat
6. Phng php th
6.1 tinh khit
Oxalat
Th theo hng dn ti JECFA monograph 1 - Vol.4 chuyn lun th gii hn Oxalat dng 1 g mu th. o
hp th quang ti 520 nm, s dng cuvet 10 mm. hp
th quang ca dch th o c phi nh hn 0,023 n v
o hp th.
Sulfat
Th theo hng dn ti JECFA monograph 1 - Vol.4 chuyn lun th gii hn Sulfat: dng 20 g mu th v 6 ml
dung dch acid sulfuric lm chun.
6.2. nh lng
Cn khong 2,5 g (chnh xc n mg) mu th, cho vo
mt bnh cn b. Ha tan trong 40 ml nc v chun
vi dung dch natri hydroxyd 1 N, dng ch th l dung dch
phenolphtalein (TS).
Mi ml dung dch natri hydroxyd 1 N tng ng vi
64,04 mg C6H8O7.
Ph lc 11
YU CU K THUT V PHNG PHP TH I VI NATRI DIHYDROGEN
CITRAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
C6H7NaO7
Cng thc cu to
214,11
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Citrat
Natri
Oxalat
t yu cu.
Ch
5.3. Hm lng
C6H7NaO7
6. Phng php th
6.1 tinh khit
Ch
Ph lc 12
YU CU K THUT V PHNG PHP TH I VI TRINATRI CITRAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Trinatri citrat; Mui trinatri ca acid 2-hydroxy-1,2,3propantricarboxylic; Mui trinatri ca acid -hydroxy
tricarballynic.
M s C.A.S.
68-04-2
Cng thc cu to
CH2
COO
+
3Na
HO
COO
_
CH2
COO
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Citrat
Natri
Tnh kim
Oxalat
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng
C6H5Na3O7
6. Phng php th
6.1 nh tnh
Citrat
Natri
Oxalat
Ch
6.3 nh lng
Cn khong 350 mg (chnh xc n mg) mu th, cho vo
cc 250 ml. Thm 100 ml acid acetic bng, khuy n khi
tan hon ton v chun vi dung dch acid percloric 0,1
N, s dng ch th l dung dch tm tinh th (TS). Tin hnh
lm mt mu trng song song v hiu chnh kt qu nu
cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
8,602 mg C6H5Na3O7.
Ph lc 13
YU CU K THUT V PHNG PHP TH I VI TRIKALI CITRAT
1. Tn khc, ch s
Potasium citrate;
INS 332ii
ADI khng gii hn
2. nh ngha
Tn ha hc
Trikali citrat; Mui trikali ca acid 2-hydroxy-1,2,3propantricarboxylic; Mui trikali ca acid -hydroxy
tricarballynic.
M s C.A.S.
866-84-2
C6H5K3O7.H2O
Cng thc cu to
CH2
COO
COO
HO
3K
.HO
2
CH2
COO
324,42
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Citrat
Kali
Tnh kim
Oxalat
Ch
6. Phng php th
6.1 nh tnh
Citrat
Kali
Oxalat
Ch
6.3 nh lng
Cn khong 250 mg (chnh xc n mg) mu th c
lm kh. Thm 40 ml acid acetic bng, un nh ha
tan hon ton. ngui v nhit phng thm 2 git
dung dch tm tinh th (TS) v chun vi dung dch acid
percloric 0,1 N. Tin hnh lm mt mu trng song song
v hiu chnh kt qu nu cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
10,21 mg C6H5K3O7.
Ph lc 14
YU CU K THUT V PHNG PHP TH I VI ACID TARTRIC
1. Tn khc, ch s
L(+)-tartaric acid
INS 334
ADI = 0 - 30 mg/kg th trng
2. nh ngha
Tn ha hc
M s C.A.S.
C4H6O6
Cng thc cu to
COOH
H
OH
HO
COOH
150,09
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
quay cc ring
Tartrat
Tro sulfat
Khng c qu 0,1 %.
Sulfat
Khng c qu 0,05%.
Oxalat
Ch
6. Phng php th
6.1 tinh khit
Tro sulfat
Sulfat
Oxalat
Ch
6.2 nh lng
Cn khong 2 g (chnh xc n mg) mu th c lm
kh, ha tan trong 40 ml nc, thm dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 1 N n khi dung dch bt u c mu hng nht
bn trong 30 giy.
Mi ml dung dch natri hydroxyd 1 N tng ng vi
75,04 mg C4H6O6.
Ph lc 15
YU CU K THUT V PHNG PHP TH I VI DINATRI TARTRAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
C4H4Na2O6.2H2O
Cng thc cu to
COO
H
OH
HO
+
2 Na 2 H2O
COO
230,8
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Natri
Tartrat
pH
Oxalat
Ch
5.3. Hm lng
C4H4Na2O6
6. Phng php th
6.1 tinh khit
Oxalat
Ch
6.2. nh lng
Cn khong 1,5 g (chnh xc n mg) mu th c
sy kh vo mt chn nung bng s cn b. u tin
nung nh n khi ch phm b than ha hon ton, trnh
cho ch phn b than ha lun tip xc vi ngn la.
ngui , t chn nung vo mt cc thy tinh, dng a thy
tinh dm nh khi cn than ha. nguyn chn nung v
a trong cc, thm vo cc thy tinh 50 ml nc, 50 ml
dung dch acid sulfuric 0,5 N. y cc v un si trong 30
pht. Lc v ra cn bng nc nng n khi dch ra
trung tnh khi th bng qu, ngui. Gp dch lc v dch
ra. Thm dung dch da cam methyl (TS) v chun acid
d bng dung dch natri hydroxyd 0,5 N.
Mi ml dung dch acid sulfuric 0,5 N tng ng vi
0,0097 g C4H4Na2O6.
Ngoi ra c th tin hnh nh lng theo cch sau:
Cn 0,45 g (chnh xc n mg) mu th c lm kh
trc, cho vo cc 250 ml, thm 100 ml acid acetic bng v
khuy u hn hp bng my khuy t n khi mu tan
hon ton. Chun dung dch vi dung dch acid percloric
0,1 N trong acid acetic bng, xc nh im tng ng
bng o th, khi gn n im tng ng chun
chm li, mi ln ch thm 0,2 ml thuc th.
Mi ml dung dch natri acid percloric 0,1 N trong acid acetic
bng tng ng vi 0,0097 g C4H4Na2O6.
Ph lc 16
YU CU K THUT V PHNG PHP TH I VI KALI NATRI TARTRAT
1. Tn khc, ch s
Potassium sodium tartrate; Potassium sodium dextrotartrate; Mui Rochelle, Mui Seignette
INS 337
ADI = 0 - 30 mg/kg th trng
2. nh ngha
Tn ha hc
M s C.A.S.
C4H4NaKO6.4H2O
Cng thc cu to
COO K+
H
OH
HO
H
_
.4HO
2
COO Na
282,23
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kali
Natri
Tartrat
pH
Oxalat
Ch
5.3. Hm lng
C4H4NaKO6
6. Phng php th
6.1 tinh khit
Oxalat
Ch
6.2. nh lng
Cn khong 1,5 g (chnh xc n mg) mu th c
sy kh vo mt chn nung bng s cn b. u tin
nung nh n khi ch phm b than ha hon ton, trnh
cho ch phn b than ha lun tip xc vi ngn la. Nhit
cui cng khng c cao qu nhit nng .
ngui , t chn nung vo mt cc thy tinh, dng a thy
tinh dm nh khi cn than ha. nguyn chn nung v
a trong cc, thm vo cc thy tinh 50 ml nc, 50 ml
dung dch acid sulfuric 0,5 N. y cc v un si trong 30
pht. Lc v ra cn bng nc nng n khi dch ra
trung tnh khi th bng qu, ngui. Gp dch lc v dch
ra. Thm dung dch da cam methyl (TS) v chun acid
d bng dung dch natri hydroxyd 0,5 N.
Mi ml dung dch acid sulfuric 0,5 N tng ng vi
0,05254 g C4H4NaKO6.
Ph lc 17
YU CU K THUT V PHNG PHP TH
I VI ACID PHOSPHORIC
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
7664-38-20
Cng thc ha hc
H3PO4
98,00
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
C th trn vi nc v ethanol.
Acid
Phosphat
Cc acid d bay hi
Clorid
Sulfat
Khng c qu 0,15 %.
Florid
Arsen
Ch
6. Phng php th
6.1 nh tnh
Phosphat
Cc acid d bay hi
Clorid
Sulfat
Arsen
Ch
6.3. nh lng
Cn 1,00 g mu th cho vo bnh thu tinh nt mi, pha
long vi 100 ml nc ct, thm 0,5 ml dung dch
thymolphtalein (TS) v chun bng dung dch natri
hydroxyd 1 N.
Mi ml dung dch natri hydroxyd 1N tng ng vi 0,049
g H3PO4.
Ph lc 18
YU CU K THUT V PHNG PHP TH
I VI mono-NATRI ortho-PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
7558-80-7
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Phosphat
Orthophosphat
Acid t do v dinatri
Florid
Arsen
Ch
Ch
6.2. nh lng
Cn 0,7 g mu th sy kh, chnh xc n mg, cho vo
cc 250 ml, thm 50 ml dung dch acid hydrocloric 0,1 N v
khuy u n khi mu tan ht. Cho in cc ca pH k
thch hp vo dung dch v dng buret cho t t dung dch
natri hydroxyd 0,1 N vo, va thm va khuy u, cho ti
khi pH = 3,3. Tip tc cho thm 0,5ml hoc 1 ml dung dch
natri hydroxyd (ty theo chia vch ca buret). Lp bng
d liu thc nghim theo mu:
V (ml)
pH
pH
2 pH
(1)
(2)
(3)
(4)
Trong :
V (ml): Th tch dung dch natri hydroxyd 0,1N c trn
buret.
pH: Hiu s chnh lch pH gia 2 ln thm dung dch
natri hydroxyd 0,1N lin tip.
Ph lc 19
YU CU K THUT V PHNG PHP TH
I VI TRINATRI ortho-PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
7601-54-9
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Phosphat
Orthophosphat
Florid
Arsen
Ch
6. Phng php th
6.1 nh tnh
Natri
Phosphat
Orthophosphat
6.3. nh lng
Cn mu, chnh xc n mg, khi lng mu tng
ng vi khong 5,5 6 g Na3PO4, ha tan vo 40 ml
nc ct trong cc 400 ml, thm 100 ml dung dch acid
hydrocloric 1N. Sc dng khng kh kh carbon dioxyd
qua dung dch, chnh cho dng kh to bt nh, thi gian
sc khong 30 pht ui ht carbon dioxyd, y nh
ming cc ngn nga mt dch trong khi sc kh. Ra
np v thnh cc bng nc ct v cho in cc ca pH
k thch hp vo dung dch. Chun dung dch bng
dung dch natri hydroxyd 1 N n im un ti pH ~ 4, tnh
th tch (A) acid hydrocloric 1 N tiu th. Bo v dung
dch trnh hp th carbon dioxyd t khng kh v tip tc
chun vi dung dch natri hydroxyd 1 N n im un
ti pH ~ 8,8. Tnh th tch dung dch (B) natri hydroxyd 1 N
tiu tn khi chun .
Ph lc 20
YU CU K THUT V PHNG PHP TH
I VI DICALCI ortho-PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Calci
Phosphat
Florid
Arsen
Ch
6. Phng php th
6.1. nh lng
Ph lc 21
YU CU K THUT V PHNG PHP TH I VI CALCI MALAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
C4H4CaO5
Cng thc cu to
O
2+
HO
Ca
O
172,14
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Malat
Calci
Khng c qu 2,0%.
(Sy ti 110oC trong 3 gi).
Florid
Acid maleic
Khng c qu 0,05%.
Ch
5.3. Hm lng
C4H4CaO5
6. Phng php th
6.1. nh lng
Ph lc 22
YU CU K THUT V PHNG PHP TH I VI NATRI FUMARAT
1. Tn khc, ch s
Monosodium fumarate,
INS 365
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
7704-73-6
Cng thc ha hc
C4H3NaO4
Cng thc cu to
138,06
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Lin kt i
Natri
Sulfat
Khng c qu 0,01%.
Acid maleic
Khng c qu 0,05%.
Ch
6. Phng php th
6.1 nh tnh
Acid 1,2 dicarboxylic
Lin kt i
6.3. nh lng
Cn 0,3 g chnh xc n mg, mu th c lm kh,
ha tan trong 30 ml nc ct. Chun vi dung dch natri
hydroxyd 0,1N, s dng ch th l 2 git dung dch
phenolphtalein (TS).
Mi ml dung dch natri hydroxyd 0,1N tng ng vi 13,81
mg C4H3NaO4.
Ph lc 23
YU CU K THUT V PHNG PHP TH I VI MAGNESI CARBONAT
1. Tn khc, ch s
Magnesium carbonate
INS 504(i)
ADI Khng gii hn
2. nh ngha
Tn ha hc
Magnesi carbonat
M s C.A.S.
546-93-0
Cng thc ha hc
MgCO3
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Magnesi
Carbonat
Khng c qu 0,05%.
Khng c qu 1,0%.
Calci
Khng c qu 0,4%.
Ch
5.3. Hm lng Mg
6. Phng php th
6.1 tinh khit
Cc cht khng tan trong
acid
Calci
6.2. nh lng
Cn 1 g mu th, chnh xc n 0,1 mg, chuyn vo bnh
nn 250ml. Thm 50 ml acid sulfuric 1N, khuy cho tan
mu. Chun acid d bng dung dch natri hydroxyd 1N
dng ch th l dung dch da cam methyl (TS). Hiu gia th
tch acid sulfuric 1 N tiu tn tr i lng acid sulfuric 1 N
tng ng vi lng Ca c trong mu (20,04 mg Ca tng
ng vi 1 ml acid sulfuric 1 N) chnh l th tch acid sulfuric
1N tiu tn trung ha magnesi carbonat.
Mi ml acid sulfuric 1 N tng ng vi 12,16 mg Mg.
Ph lc 24
YU CU K THUT V PHNG PHP TH I VI NHM KALI SULFAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
Cng thc ha hc
3. Cm quan
Tinh th ln, trong sut, hoc mnh tinh th, hoc bt tinh
th khng mi.
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Nhm
Kali
Sulfat
Florid
Selen
Ch
6. Phng php th
6.1. tinh khit
Cc mui amoni
Florid
Huyn ph vi
Cho cn thn, t t khong 56 g calci oxyd (c hm lng
clorid thp - khong 2 mg/kg) vo 250 ml nc, thm t t
250 ml acid percloric 60% vo, khuy u. Thm vi vin bi
thy tinh, un nng n khi khi acid percloric bay ra nhiu,
lm mt, thm 200 ml nc v tip tc un. Lp li qu
trnh pha long ny thm 1 ln, ngui v lc nu c kt
ta silic dioxyd. Rt dch lc trong, va rt va khuy vo
1000 ml dung dch natri hydroxyd 1/10, kt ta lng
xung, gn b lp dch trong. Loi mui natri ra khi ta
bng cch ra 5 ln trong bnh ly tm ln, mi ln ra lc
mnh. Cui cng lc kt ta thnh huyn ph v pha long
n 2000 ml. Bo qun huyn ph trong chai c nt gn
parafin, trc khi dng cn lc u. 100 ml huyn ph ny
c xem nh mu trng (cha flor mc khng ng k)
khi c c trong a platin v x l theo hng dn trong
phn "Tin hnh th" bt u t giai on "Nung trong thi
gian ngn ti 600oC ...".
Thit b chng ct
Ni bnh cu ct 125 ml vi 1 sinh hn, ng thi ni vi
ng mao qun v nhit k sao cho u ng mao qun v
nhit k ngp vo dung dch trong bnh. Ni ng mao qun
vi mt phu nh git hoc b phn sinh hi nc.
gim thiu nn trng do florid thi t thy tinh, thit b ct
c x l trc nh sau: X l tt c cc dng c thy
tinh cn s dng vi dung dch natri hydroxyd 10% nng,
tip theo xi qua vi nc v trng bng nc ct. Ti
thiu 1 ln/ngy, x l thm bng cch un si 15-20 ml
dung dch acid sulfuric 1/2 trong h thng ct n khi h
thng y khi acid, ngui, b acid, ti x l vi dung
dch natri hydroxyd 10%, trng ra ton b h thng ct.
Tin hnh th
Cn 1,67 g (chnh xc n mg) mu, cho vo bnh cu ct,
thm 25 ml dung dch acid sulfuric 1/2. Ct n khi t nhit
160o, sau duy tr nhit ti 160o n 165o bng
cch thm nc t phu nh git vo bnh, thu ly 300 ml
dch ct. Oxy ha dch ct bng cch thm 2-3 ml dung dch
hydrogen peroxyd 30% khng c florid ( c loi b
sulfit), yn hn hp vi pht, cho bay hi trn a platin
c sn lng d huyn ph vi.
Nung trong thi gian ngn ti 600o, sau lm mt v tm
t tro vi khong 10 ml nc. y a platin bng mt
knh ng h, cn thn thm vo lng acid percloric 60%
ha tan tro. Cho dch trn a platin qua phu nh
Ph lc 25
YU CU K THUT V PHNG PHP TH I VI NATRI HYDROXYD
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Natri hydroxyd
M s C.A.S.
1310-73-2
Cng thc ha hc
NaOH
40,00
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kim
Natri
Carbonat
Ch
6. Phng php th
6.1 tinh khit
Cc hp cht khng tan
trong nc
6.2. nh lng
Cn 1,5 g mu th, chnh xc n mg, ho tan trong 40 ml
nc va mi un si ngui, lm ngui n 150C, cho
thm dung dch phenolphtalein (TS) v chun vi dung
dch acid sulfuric 1N. Khi dung dch mt mu hng, ghi li
th tch acid nu cn, cho thm dung dch da cam methyl
(TS) v tip tc chun cho n khi c mu hng. Ghi
chp li tng th tch dung dch acid chun .
Mi ml dung dch acid sulfuric 0,1 N tng ng vi 40,0
mg tng lng kim, tnh theo NaOH.
Ph lc 26
YU CU K THUT V PHNG PHP TH I VI KALI HYDROXYD
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Kali hydroxyd
M s C.A.S.
1310-58-3
Cng thc ha hc
KOH
56,11
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kim
Kali
Carbonat
Ch
6. Phng php th
6.1. nh lng
Ph lc 27
YU CU K THUT V PHNG PHP TH I VI CALCI HYDROXYD
1. Tn khc, ch s
Calcium hydroxyde; vi ti
INS 526
ADI=khng gii hn
2. nh ngha
Tn ha hc
Calci hydroxyd
M s C.A.S.
1305-62-0
Cng thc ha hc
Ca(OH)2
74,09
3. Cm quan
Bt trng.
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kim
Calci
Khng c qu 0,03%.
Magnesi v cc mui
kim
Khng c qu 6,0%.
Khng c qu 1,0%.
Florid
Ch
6. Phng php th
6.1 tinh khit
Bari
0,3 ml dung dch bari chun (1,779g bari clorid trong 1000
ml nc ct) thm nc ct cho 20 ml, thm 2 g natri
acetat, 1 ml acid acetic long (TS) v 0,5 ml dung dch kali
cromat (TS), yn 15 pht.
Magnesi v cc mui
kim
Ha tan 500 mg mu th vo hn hp gm 30 ml nc ct
v 10 ml acid hydrocloric long (TS) v un si trong 1
pht. Thm nhanh 40 ml dung dch acid oxalic (TS), khuy
mnh n khi kt tu hon ton. Thm ngay 2 git dung
dch methyl (TS), sau thm tng git dung dch
amoniac (TS) n khi hn hp va c tnh kim, ngui.
Chuyn dung dch vo ng ong 100 ml, pha long dung
dch n 100 ml bng nc ct, yn trong 4 gi hoc
qua m, sau lc gn phn nc trong pha trn qua
giy lc kh. Ly 50 ml dch lc trong vo mt bt platin,
thm 0,5 ml acid sulfuric v cho hn hp bay hi cch thy
n gn cn. Cho bay hi t t phn cn li trn ngn la
n kh, tip tc un cho n khi cc mui amoni phn hy
v bay hi hon ton. Cui cng nung phn cn cn li n
khi lng khng i. Khi lng cn khng c qu 15
mg.
6.2. nh lng
Cn 1,5 g mu th, chnh xc n mg, cho vo cc thy
tinh, thm 30 ml acid hydrocloric long (TS). Khi mu tan
hon ton, chuyn dung dch vo bnh nh mc 500 ml,
trng sch cc thy tinh v gp nc ra cc vo bnh nh
mc, nh mc n vch bng nc ct, lc u. Ht ly
50 ml dung dch ny vo bnh nn c dung tch thch hp
v thm 50 ml nc ct, 15 ml ung dch natri hydroxyd
(TS), 40 mg hn hp ch th murexid (amoni purpurat) v 3
ml dung dch xanh lc naphtol (TS). Chun vi dung
dch dinatri ethylendiamintetraacetat 0,05M n khi dung
dch c mu xanh da tri m.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05M
tng ng vi 3,075 mg Ca(OH)2.
Ph lc 28
YU CU K THUT V PHNG PHP TH I VI CALCI OXYD
1. Tn khc, ch s
Calcium oxyde; vi
INS 529
ADI=0-6mg/kg th trng
2. nh ngha
Tn ha hc
Calci oxyd
M s C.A.S.
1305-78-8
Cng thc ha hc
CaO
56,08
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Phn ng vi nc
Kim
Calci
Bari
Khng c qu 0,03%.
Magnesi v cc mui
kim
Khng c qu 3,6%.
Ch
6. Phng php th
6.1 tinh khit
Bari
Magnesi v cc mui
kim
Ha tan 500 mg mu th vo hn hp gm 30 ml nc ct
v 10 ml dung dch acid hydrocloric long (TS) v un si
trong 1 pht. Thm nhanh 40 ml dung dch acid oxalic
(TS), khuy mnh. Thm 2 git dung dch methyl (TS),
sau trung ha dung dch bng dung dch amoniac (TS)
n khi calci kt ta hon ton. un nng hn hp trn b
cch thy trong 1 gi, ngui, pha long n 100 ml
bng nc ct, trn u v lc. Ly 50 ml dch lc trong,
thm t t 0,5 ml acid sulfuric c v cho hn hp bay hi
n kh v nung n khi lng khng i trong chn nung
platin ( cn b).
Cht khng tan trong acid Ti 5 g mu, trn vi 100 ml nc ct v thm tng git
acid hydrocloric n va ho tan. un si hn hp,
ngui v thm acid hydrocloric (nu cn) to mi
trng acid, lc qua mt chn lc cn b, ra cn bng
nc ct n khi ht clorid. Sy 105 oC trong 1 gi,
ngui v cn.
6.2 nh lng
Nung 1 g mu th nhit ~800 oC n khi lng
khng i. Cn chnh xc lng cn v ha tan trong 20
ml dung dch acid hydrocloric long (TS). ngui dung
dch, pha long vi nc ct n 500 ml v trn u. Ht
ly 50 ml dung dch ny vo bnh nn c dung tch thch
hp v thm 50 ml nc ct, 15 ml dung dch natri
hydroxyd (TS), 40 mg hn hp ch th murexid v 3 ml
dung dch xanh lc naphtol (TS). Chun vi dung dch
dinatri ethylendiamintetraacetat 0,05M n khi dung dch c
mu xanh da tri m.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05M
tng ng vi 2,804 mg CaO.
Ph lc 29
YU CU K THUT V PHNG PHP TH
I VI NATRI NHM PHOSPHAT - ACID
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Cng thc ha hc
Na3Al2H15(PO4)8
NaAl3H14(PO4)8.4H2O
Na3Al2H15(PO4)8 : 897,82
NaAl3H14(PO4)8.4H2O : 949,88
3. Cm quan
Bt mu trng, khng mi
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Phosphat
Nhm
Florid
Arsen
Ch
5.3. Hm lng
6. Phng php th
6.1. nh lng
Ph lc 30
YU CU K THUT V PHNG PHP TH
I VI NATRI NHM PHOSPHAT KIM
1. Tn khc, ch s
2. nh ngha
3. Cm quan
Bt mu trng, khng mi
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Natri
Phosphat
Nhm
Florid
Arsen
Ch
6. Phng php th
6.1. nh lng
Ph lc 31
YU CU K THUT V PHNG PHP TH
I VI GLUCONO delta-LACTON
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
90-80-2
C6H10O6
Cng thc cu to
CH2OH
H
H
OH
OH
OH
178,14
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Phn ng mu
Gluconat
Tro sulfat
Cc hp cht kh
Ch
6. Phng php th
6.1. tinh khit
Cc hp cht kh
6.2. nh lng
Ph lc 32
YU CU K THUT V PHNG PHP TH I VI ACID ACETIC BNG
1. Tn khc, ch s
INS 260
ADI khng gii hn i vi acid acetic v mui kali v natri
ca acid acetic
2. nh ngha
Tn ha hc
M s C.A.S.
64-19-7
Cng thc ha hc
C2H4O2
Cng thc cu to
H3C
OH
O
60,05
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Acid
Acetat
Cn khng bay hi
Cc cht d b xy ho
Ch
6.2. nh lng
Ph lc 33
YU CU K THUT V PHNG PHP TH I VI ACID ADIPIC
1. Tn khc, ch s
INS 355
ADI = 0 - 5 mg/kg th trng
2. nh ngha
Tn ha hc
M s C.A.S.
124-04-9
C6H10O4
Cng thc cu to
O
HO
OH
O
146,14
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
151,5oC - 154oC.
Tro sulfat
Ch
6. Phng php th
6.1 tinh khit
Tro sulfat
6.2. nh lng
Cn 3 g (chnh xc n mg) mu th, cho vo bnh nn
250 ml, thm 50 ml methanol v ha tan bng cch un
nng nh trong b cch thy, ngui v thm dung dch
phenolphtalein (TS) v chun vi natri hydroxyd 1N.
Tin hnh lm mu trng song song v hiu chnh kt qu
chun nu cn.
Mi ml dung dch natri hydroxyd 1N tng ng vi 73,07
mg C6H10O4.
Ph lc 34
YU CU K THUT V PHNG PHP TH
I VI MONOCALCI ortho-PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Calci
Phosphat
o
Gim khi lng khi nung Dng khan: gia 14,0 v 15,5% (800 C trong 3 pht).
Florid
Arsen
Ch
5.3. Hm lng Ca
6. Phng php th
6.1 tinh khit
Ch
6.2. nh lng