TI U CHUN VIT NAM TCVN 6971-2001

NC TNG HP DNG CHO NH BP

Synthetic detergent for kitchen

1 Phm vi p dng
Tiu chun ny p dng cho nc ra tng hp dng ra rau, qu v dng cho n
ung trong nh bp, s dng cht hot ng b mt d b phn hu sinh hc v mt s
ph gia khc ang c b Y T cho php s dng trong thc phm.
2 Tiu chun trch dn
TCVN 1056 - 86 Thuc th. Phng php chun b cc thuc th dung dch v hn hp
ph dng trong phn tch trc quang v phn tch c khuych tn.
TCVN 3778 - 82 Thuc th. Phng php xc nh asen.
TCVN 4851 - 89 ( ISO 3696 - 1987) Nc dng phn tch trong phng th nghim.
Yu cu k thut v phng php th.
TCVN 5454 - 1999 (ISO 607 - 1980) Cht hot ng b mt v cht ty ra - Phng
php phn chia mu.
TCVN 5456 - 91 Cht ty ra tng hp. Phng php xc nh ch s nng ion hidro
( pH). TCVN 5491 - 91 (ISO 8212 - 1986) Cht hot ng b mt v cht ty ra.
Ly mu trong sn xut.
TCVN 6969 : 2001 Phng php th phn hu sinh hc ca cht ty ra tng hp.
3 Yu cu k thut
3.1 Nc ra dng cho nh bp phi ph hp vi cc quy nh trong bng 1 v bng 2.

Bng 1 - Cc ch tiu ngoi quan
Tn ch tiu Yu cu
1.Trng thi


2. Mu
3. Mi
Lng snh, ng nht, khng phn lp v kt ta nhit
nh hn 20
0
C
ng nht v theo mu ng k
Khng mi hoc c mi d chu

Bng 2 - Cc ch cht lng
Tn ch tiu Mc cht lng
1.Hm lng cht hot ng b mt , tnh bng phn
trm i khi lng, khng nh hn
2. pH ca dung dch sn phm
3. Hm lng metanol, tnh bng mg/kg khng ln hn
10

6 - 8
1000
4. Hm lng asen, tnh bng mg/kg, khng ln hn
5. Hm lng kim loi nng, tnh theo ch, tnh bng
mg/kg, khng ln hn
6. Cht lm sng hunh quang
7. phn hu sinh hc, tnh bng phn trm khi
lng, khng nh hn
1
2

khng c php
90
4 Phng php th
4.1 Quy nh chung
Ho cht dng phn tch l loi TKPT hoc TKHH
Nc ct s dng theo TCVN 4851 - 89 (ISO 3696 - 1987).
Cn phn tch c chnh xc ti thiu 0,001 g .
4.2 Ly mu v chun b mu
Ly mu v chun b mu theo TCVN 5454 - 1999 v TCVN 5491 - 1991 vi lng mu
trung bnh ti thiu l 1000 g.
Mu th nghim c cho vo bnh sch, kh, c nt kn, ngoi bnh c ghi nhn:
tn cht ty ra;
tn ni sn xut;
ngy sn xut ;
ngy v ni ly mu;
k hiu tiu chun.
4.3 nh gi ngoi quan sn phm
Ly khong 200 ml mu vo cc thu tinh dung tich 500 ml. Dng mt quan st mu,
cn tin hnh ni c nh sng, trnh nh sng trc tip , khng c mu sc khc
gn v khng c mi l. Quan st cc c tnh sau:
trng thi: m t trng thi quan st c, c bit lu v tnh ng nht ca sn
phm;
mu sc: m t mu sc quan st c;
mi: m t mi cm nhn c.
Th mu nhit nh hn 20
0
C : Ly khong 200 g mu vo cc thu tinh dung tch
250 ml v t trong bnh n nhit nhit 20
0
C. Sau 10 pht mu t nhit ny,
ly ra quan st.
nh gi mu th theo cc yu cu qui nh iu 3.1 bng 1.
4.4 Xc nh hm lng cht hot ng b mt
4.4.1 Nguyn tc
Cc cht hot ng b mt c tch khi nc ra dng cho nh bp bng etanol v
c tnh sau khi tr i nhng thnh phn khc cng tan trong etanol nh clorua,
glyxerin.
Chun mui clorua (quy ra NaCl) bng bc nitrat vi ch th mu kali cromat.
Da vo phn ng oxy ho kh ca glyxerin vi kali periodat trong mi trng axit,
lng periodat d tc dng vi kali iodua gii phng iot. nh lng iot mi sinh bng
natri thiosunfat v tnh ra hm lng glyxerin.
4.4.2 Ho cht v thuc th
etanol 99%;
bc nitrat, dung dch 0,1N;
kali cromat, dung dch 10 %;
axit nitric, dung dch 1 : 4;
methyl , dung dch 0,1% pha trong etanol;
axit clohidric, d =1,19 v dung dch 1 + 1;
natri thiosunfat, dung dch 0,1 N;
kali periodat, dung dch 0,1 N;
kali iodua, dung dch 10 %;
h tinh bt, dung dch 1 %.
4.4.3 Thit b v dng c
t sy duy tr nhit 105
0
C;
bp cch thu;
bnh tam gic, dung tch 100 ml;
bnh tam gic c nt nhm, dung tch 250 ml;
cc thu tinh, dung tch 250 ml;
buret 25 ml.
4.4.4 Cch tin hnh
4.4.4.1 Xc nh tng hm lng cht tan trong etanol
Cn khong 5 g mu (chnh xc n 0,001 g) vo cc thu tinh dung tch 250 ml, thm
vo 40 ml etanol. y cc bng mt knh ng h, un nng trn bp cch thu v
khuy cho mu phn tn hon ton. Lc mu qua giy lc vo bnh tam gic dung tch
100 ml c sy kh v cn trc n khi lng khng i m
0
(chnh xc n 0,001
g).
Tip tc qu trnh ho tan trn hai ln na, mi ln vi 20 ml etanol. Thu gp tt c dung
dch lc vo bnh tam gic trn, v c nh bnh ny trn bp cch thu cho n khi ch
cn li cn. Sy bnh tam gic ny nhit 105
0
C trong mt gi. ngui bnh trong
bnh ht m, sau 30 pht em cn l gi tr m
1
(chnh xc n 0,001 g).
Lp li gi tr sy ny n khi chnh lch gia hai ln cn lin tip khng ln 0,001 g.
4.4.4.2 Xc nh hm lng mui clorua tan trong etanol
Ho tan phn cn sau khi xc nh cht tan trong etanol (4.4.4.1) trong 20 ml nc ct
v thm hai git methyl . Nu dung dch c mu vng th trung ho bng axit nitric 1 +
4 n mu hng. Thm 2,5 ml dung dch kali cromat 10 %. Chun bng dung dch bc
nitrat 0,1 N n khi xut hin mu gch, th tch chun l V
1
. ng thi tin hnh
th nghim mu trng vi y cc thuc th nhng khng c mu, th tch chun l
V
2
.
4.4.4.3 Xc nh hm lng glyxerin tan trong etanol
Ho tan phn cn cht tan trong etanol (4.4.4.1) trong khong 25 ml nc v 5 ml dung
dch HCl (1 +1), chuyn dung dch vo bnh tam gic c nt nhm dung tch 250 ml,
thm chnh xc 25 ml dung dch kali periodat,y nt, lc u mu, yn 15 pht. Ly
mu ra, cho thm 20 ml dung dch axit clohidric (1 + 1) v 20 ml dung dch kali iodua.
y nt, lc trn, yn trong bng ti
5 pht. Sau chun dung dch bng natri thiosunfat n mu vng nht, thm vo
1 ml dung dch h tinh bt v tip tc chun n khi mt mu xanh ca dung dch, th
tch chun ny l V
4
. ng thi tin hnh th nghim mu trng, th tch chun l
V
3
.
4.4.5 Tnh kt qu
4.4.5.1 Tng hm lng cht tan trong etanol
Tng hm lng cht tan trong etanol (X
1
), tnh bng phn trm khi lng, theo cng
thc sau:

28,84 x ( V
1
V
0
) x C
O

X
1
=
m
trong
m
0
- khi lng bnh, tnh bng gam;
m
1
- khi lng ca cn v bnh, tnh bng gam;
m - khi lng mu th, tnh bng gam.
4.4.5.2 Hm lng mui clorua tan trong etanol
Hm lng mui clorua tan trong etanol (X
2
), quy ra NaCl, tnh bng phn trm khi
lng, theo cng thc sau:
(V
1
- V
2
) x 0,0058 x 100
X
2
=
m
trong
V
1
- th tch bc nitrat 0,1 N dng chun mu th, tnh bng mililt;
V
2
- th tch bc nitrat 0,1 N dng chun mu trng, tnh bng mililt;
m - khi lng mu th, tnh bng gam;
0,0058 - lng gam natri clorua tng ng vi 1 ml bc nitrat 0,1 N.
4.4.5.3 Hm lng glyxerin tan trong etanol
Hm lng glyxerin tan trong etanol X
3
, tnh bng phn trm khi lng (%), theo cng
thc sau:

(V
3
- V
4
) x 0,0023 x 100
X
3
=
m
trong
V
4
-

th tch natri thiosunfat 0,1 N dng chun mu th, tnh bng mililt;
V
3
- th tch natri thiosunfat 0,1 N dng chun mu trng, tnh bng mililt;
m - khi lng mu th, tnh bng gam;
0,0023 - lng gam glyxerin tng ng 1 ml natri thiosunfat 0,1 N.
4.4.5.4 Tng hm lng cht hot ng b mt tan trong etanol (X), tnh bng phn trm
khi lng, theo cng thc sau:
X =X
1
- (X
2
+X
3
)
trong
X
1
-

tng hm lng cht tan trong etanol, tnh bng %;
X
2
- hm lng mui natri clorua tan trong etanol, tnh bng %;
X
3
- hm lng glyxerin tan trong etanol, tnh bng %.
4.4.6 chnh xc ca phng php
4.4.6.1 lp li
Chnh lch tuyt i gia hai kt qu xc nh song song tin hnh trn cng mt mu
th hoc c thc hin lin tip, do cng mt ngi phn tch, s dng cng loi thit
b khng c vt qu 0,3 % cht hot ng b mt.
4.4.6.2 ti lp
Chnh lch tuyt i gia hai kt qu thu c trn cng mt mu th hai phng th
nghim khng c vt qu 0,5 % cht hot ng b mt .
4.5 Xc nh hm lng asen v kim loi nng
4.5.1 Chun b dung dch th
Cn khong 10 g mu (chnh xc n 0,01 g) vo bnh tam gic chu nhit dung tch 250
ml. Thm 10 ml axit sunfuric c v un nh trn bp in, sau tng dn nhit
mu chy thnh dung dch snh mu nu en. ngui dung dch v thm dn tng git
khong 5 ml axit nitric c v tip tc un si nh n khi dung dch tr thnh trong sut.
ngui dung dch v trng thnh bnh bng khong 20 ml nc ct, thm 5 ml dung
dch axit axetic, un si li dung dch mt ln na. Dung dch trong bnh trong sut,
khng mu l t. ngui chuyn dung dch vo bnh nh mc dung tch 100 ml, thm
nc n vch mc v lc k. Dung dch ny dng xc nh asen v kim loi nng.
4.5.2 Xc nh hm lng kim loi nng, tnh theo ch
4.5.2.1 Nguyn tc
Cc ion kim loi nng to vi dung dch natri sunfua kt ta mu en hay nu trong mi
trng axit axetic pH = 3,5 - 4. So snh mu ca dung dch mu vi mu ca dung dch
tiu chun ch.
4.5.2.2 Ho cht v thuc th
axit sunfuric, d =1,84;
axit nitric, d =14,3
axit axetic, dung dch 30 % v (1 + 15);
natri sunfua, dung dch 2 %;
amoniac, dung dch 25 % v (1 +2);
dung dch ch tiu chun A, 1 mg/ml, chun b theo TCVN1056-86;
dung dch ch tiu chun B, 0,010 mg/ml, ly 10 ml dung dch A cho vo bnh nh
mc
1000 ml, nh mc ti vch bng nc v lc k;
dung dch ch tiu chun C, 0,0001 mg/ml, ly 10 ml dung dch B cho vo bnh nh
mc 1000 ml, nh mc ti vch bng nc v lc k.
Dung dch B v C ch pha trc khi dng.
4.5.2.3 Dng c
ng so mu Nessler 50 ml;
bnh nh mc dung tch 100 ml, 1000 ml.
4.5.2.4 Cch tin hnh
Ht 10 ml mu iu 4.5.1 vo ng so mu Nessler. ng thi ly 20 ml dung dch ch
tiu chun C vo ng so mu khc. Trung ho dung dch mu v dung dch tiu chun
bng dung dch amoniac (1 + 2) theo ch th phenolphtalein n pht hng. Thm vo
mi ng th 1 ml axit axetic v 0,5 ml dung dch natri sunfua. y nt v lc u. Sau 1
pht so snh mu ca ng dung dch th khng c m mu hn dung dch ca ng so
snh. Khi so snh mu phi nhn t trn xung di, trn nn trng.

4.5.3 Xc nh hm lng asen
Ly 10 ml dung dch iu 4.5.1 v xc nh asen theo TCVN 3778 - 82.
So snh mu giy ca mu vi mu giy ca dung dch tiu chun c 0,001 mg As.
4.6 Xc nh hm lng metanol
4.6.1 Nguyn tc
Metanol trong mu c ho tan trong dung dch nn 2-propanol v c xc nh bng
phng php sc k kh, s dng ct nhi l cht cao phn t v detector ion ho ngn
la (FID).
4.6.2 Ho cht v thuc th
2-propanol 99 %, hm lng metanol nh hn 0,005 %;
metanol 99 %.
4.6.3 Thit b v dng c
4.6.3.1 My sc k kh bao gm:
bung bm mu, gi nhit cao hn bung ct 50
0
C, ct c ng knh 3 - 4 mm,
di 2 - 3 m, lm bng thu tinh Bo;
- detector FID;
my ghi: chiu cao th 2 mV l cc i, rng ca giy ghi ti thiu l 150 mm , tc
bt cho ton chiu cao l 3 giy, tc giy ghi ti thiu 10 mm/pht v c kh nng
iu chnh ln hn;
thit b iu chnh nhy;
bnh kh: nit hay heli;
bm mu: micro xylanh, dung tch 10 ml, phn chia vch t 0,1 - 1ml;
bnh nh mc, dung tch 100 ml v 1000 ml;
cc dung tch 250 ml;
ct nhi, cht c nhi l cc ht cao phn t c l v kch thc ht 170 - 300 mm
nh Porapak-Q.
4.6.4 Chun b mu th v dung dch tiu chun
Dung dch mu th: Cn 10 g mu lng ( chnh xc n 0,1 g) v 10,0 g 2-propanol
vo bnh nh mc dung tch 100 ml. Thm nc ti vch v lc k.
Dung dch tiu chun: Cn 10 g metanol (chnh xc n 0,01 g) vo bnh nh mc
dung tch 1000 ml. Thm nc ti vch bng v lc k. Ht 10 ml dung dch ny vo
bnh nh mc dung tch 100 ml cn trc 10,0 g 2-propanol. Thm nc n vch v
lc k.
Dung dch nn 2-propanol: Cn 10,0 g 2-propanol vo bnh nh mc dung tch 100
ml. Thmnc ti vch v lc k.
4.6.5 Cch tin hnh
4.6.5.1 Tun th theo qui trnh ca my sc k kh:
Ni kh vo my sc k kh, iu chnh van p xut 300 - 500 kPa, ri iu chnh dn
kh vo khong 100 kPa.
Ni my sc k kh vi my ghi, t bung ct ch 130 - 150
0
C, t nhit
bung bm mu v detector cao hn bung ct 50
0
C.
iu chnh nhy cc i, bt u ghi v khng nh ng nn thng c nh (nu
ct mi nhi th phi tng nhit bung ct ln 10 - 20
0
C.
Bm nhanh 1 ml dung dch 2-propanol vo bung bm mu, t bt vo im xut
pht trn trc thi gian ca giy ghi. iu chnh tc kh mang v nhit bung ct
sao cho pic
2-propanol xut hin vo khong sau 8 - 10 pht, iu chnh nhy ca my v tc
giy sao cho chiu cao ca pic 2-propanol khng thp hn 50 % v khng cao hn 90 %
rng giy ghi.
4.6.5.2 o mu

Bm nhanh 1 ml dung dch tiu chun vo bung bm mu v thc hin tip tng t
nh phn 4.6.5.1. Ghi sc k , pic metanol xut hin sau khong 2 - 2,5 pht v pic 2-
propanol sau khong 8 - 10 pht. T s din tch ca hai pic metanol v 2-propanol ca
dung dch tiu chun l A
tc.

Bm nhanh 1 ml dung dch mu th vo bung bm mu v thc hin tip nh dung
dch tiu chun, trong iu kin hon ton ging nhau. Ghi sc k .T s din tch ca
hai pic metanol v 2-propanol mu th l A
m
.
4.6.6 Tnh kt qu
So snh hai t s A
m
< =A
tc.

4.6.7 Ghi ch: Pic etanol khng gy nh hng n kt qu.
4.7 Cht lm sng hunh quang
4.7.1 Nguyn tc
Chiu n cc tm vo giy lc c nhng vo dung dch mu th v xc nh s c
mt ca cht lm sng quang hc trong mu.
4.7.2 Dng c
n chiu tia cc tm, s dng bc sng khong 360 nm;
giy lc nh tnh (giy lc thng), kch thc l 20 - 25 mm, kch thc giy 25 mm x
50 mm;
cc thu tinh, dung tch 250 ml;
4.7.3 Cch tin hnh
Ho tan 2,0 gam mu vo 100 ml nc nng 40
0
C. Nhng giy lc vo dung dch
trong khong 30 pht. Sau nhng di giy lc ny vo 100 ml nc nng 40
0
C
trong 5 pht, lp li qu trnh ny mt ln na. ng thi lm giy mu trng so snh,
giy ny ch nhng trong nc. kh giy v dng n tia cc tm chiu giy trong
bung ti, t giy cch n 20 - 30 cm.
4.7.4 Tnh kt qu
So snh giy c nhng vo mu v giy nhng vo mu trng.
4.8 Xc nh pH
Thc hin theo TCVN 5456-91 Cht ty ra tng hp. Phng php xc nh ch s nng
ion hidro ( pH).
4.9 Xc nh phn hu sinh hc
Xc nh theo TCVN 6969 : 2001 Phng php th phn hu sinh hc ca cht ty
ra tng hp.
5 Bo co kt qu
Bo co kt qu xc nh gm nhng mc sau y:
tt c cc thng tin cn thit nhn bit y d v mu th;
cc phng php s dng (theo tiu chun ny);
cc kt qu thu c v cch biu th cc kt qu;
cc chi tit ca mi thao tc khng qui nh trong tiu chun ny hoc cc tiu chun
khc, hoc bt k thao tc tu no cng nh cc s c xy ra nh hng n kt qu.
6 Bao gi, ghi nhn, vn chuyn v bo qun sn phm
6.1 Bao gi
Nc ra dng cho nh bp c ng trong cc chai bng nha.
Cc chai nc ra dng trong nh bp c xp trong cc thng bng cc tng. m bo
chc chn v an ton trong qu trnh vn chuyn v bo qun. S lng ng gi theo
tho thun gia hai bn sn xut v tiu th.
6.2 Ghi nhn
Trn mi chai nc ra dng cho nh bp u c nhn ghi:
tn hng ho;
tn v a ch c s sn xut;
thnh phn nguyn liu chnh;
Ch tiu cht lng chnh;
hng dn s dng;
ngy sn xut;
hn s dng;
Trn mi thng cc tng c nhn ghi:
tn hng ho;
tn v a ch c s sn xut;
s lng chai;
hng dn bo qun (k hiu che ma, nng);
ngy sn xut.
6.3 Vn chuyn
Vn chuyn bng phng tin thng dng. Trong qu trnh vn chuyn khng c
chng, xp qu cao trnh gy v, bp bao b sn phm v phi c che ma nng.
6.4 Bo qun
Bo qun nc ra dng cho nh bp trong kho kh mt, trnh ni c hi.

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