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DETERMINATION OF TOTAL FATTY MATTER

1. AIM
To outline the procedure for the Determination of Total Fatty Matter (and resin)
acids, and any unsaponifiable matter present in soap sample.
1. PERSONNEL INVOLVED
The QA Laboratory Analyst, QA Laboratory Assistants,
2. EQUIPMENTS AND GLASSWARES NEEDED
Retort tands, !onical Flas"s (#$% ml), eparatin& Funnels (#$%ml), 'ea"ers
(#$%ml, $%ml), Measurin& !ylinders ((%%ml, $%ml),
3. REAGENTS NEEDED.
i. Diethyl )ther*
ii. Tetrao+osulphate (,-) Acid (M !oncentration.
iii. .otassium /ydro+ide (01/)* appro+ %.$M.
i2. Methyl 1ran&e -ndicator* %.%34 in A5ueous olution
2. .henolphthalein -ndicator (.%4 in 6eutral )thanol.

PROCEDURE
(. 7ei&h accurately and as 5uic"ly as possible, $& (7() of sample into a #$%ml
conical flas". Dissol2e the soap in (%%ml of hot 8ater.
#. Add # drops of a5ueous methyl oran&e indicator.
9. Drop 8ise add (M Tetrao+osulphate (2i) Acid until acidic. Add $ml e+cess acid.
3. Thorou&hly mi+ the contents of the conical flas". -nsert a small funnel into the
nec" and heat (to a temperature not e+ceedin& :%
o
!) until the fatty acid
separates as a clear layer .Allo8 to cool to room temperature.
$. Transfer 5ualitati2ely into a separatin& funnel, 8ashin& 8ith fresh portions of
Diethyl ether.
:. )+tract the fatty matter 8ith $%ml diethyl ether. Dra8 off the a5ueous layer into
another separatin& funnel and 8ash $ times 8ith 9%ml portions of diethyl ether,
addin& the ether 8ashin&s to the ori&inal ether solution.
;. 7ash the combined ether e+tracts 8ith (%ml portions of distilled 8ater until the
8ash 8ater is neutral to methyl oran&e. A2oid loss of fatty matter as an
emulsion.
<. Mi+ the 8ater portion used for 8ashin& and sha"e 8ith #%ml ether. Add the
ether to the fatty acid=ether solution.
>. Run the ether solution into a tarred bea"er and rinse the separatin& funnel 8ith
portions of neutral ethanol up to a total of $%ml.
(%. )2aporate the fatty acid=ether solution until only residual 5uantities of ether are
discernible. Dry the fatty acids to constant 8ei&ht in an o2en at (%%? (%$
%
!
((. Allo8 to cool and 8ei&h the residue of fatty and rosin acids (7#)
The total fatty matter is calculated thus,
4Total Fatty Matter @ 7# + (%%
7(


FOR % ANHYDROUS SOAP
(#. Ta"e up the residue in (%%ml of 8arm neutral >$4 ethanol
(9. Titrate a&ainst %.$M 01/ usin& phenolphthalein as indicator.
4 Anhydrous soap @ AW 2 B ( V + M + 0.0381 ) + 100C
W1
Acid number (i.e. m& of 01/ re5uired to neutraliDe (& acid)
@ V + M + 56.1
W2

7here, ,@ E ml of standard al"ali
M@ Molarity of standard al"ali.
NOTE
This method is not applicable to samples containin& lar&e amount s of
soluble silicates or finely di2ided matter insoluble in 8ater, and soap products
containin& synthetic deter&ents


DETERMINATION OF % MOISTURE CONTENT
1. AIM
To outline the procedure for the Determination of The percenta&e (4) Moisture
!ontent present a in soap sample, usin& the moisture analyDer.
2. PERSONNEL INVOLVED
The QA Laboratory Analyst, QA Laboratory Assistants,
3. EQUIPMENTS NEEDED
Moisture AnalyDer, Mortar and .estle.
!. REFERENCE
i. 1. Moisture AnalyDer.
5. PRINCIPLE
Moisture content of a ubstance is the amount of 8ater present in the
ubstance. This is based on the difference in 8ei&ht before and after dryin& the
sample. -t can be calculated thus, usin& the relation belo8*
4Moisture content @ 7 F D + (%%
7
7 @ 7et sample mass.
D@ Dried sample mass.
!. PROCEDURE
a Ta"e a considerable amount of the soap sample.
b. !rush (%& of the sample to uniform po8der usin& the mortar and pestle.
c. 8itch on the moisture analyDer,
d. 1pen the heater co2er.
e. Gsin& the le2el indicator and 8ei&hin& mode on the Moisture AnalyDer,
f. Measure $& of the po8dered sample into the sample pan.
&. Gse a spatula to spread the sample as e2enly as possible.
h. !lose the heater co2er.
i. .ress the TART button.
H. Allo8 the Moisture AnalyDer to run until the buDDer beeps.
". Read and record the result.
DETERMINATION OF FREE CAUSTIC AL"ALI
1. AIM
To outline the procedure for the Determination of Free caustic al"ali in soap
products=amples.
2. PERSONNEL INVOLVED
The QA Laboratory Analyst, QA Laboratory Assistants,
3. EQUIPMENTS AND GLASSWARES NEEDED
!onical Flas"s (#$% ml), 'urettes, 'ea"ers (#$%ml), Measurin& !ylinders ((%%ml),
7ater bath.
!. REAGENTS NEEDED
i. >$42=2 6eutral )thanol* Freshly distilled )thanol, at >$4 and neutral to
phenolphthalein.
ii. %.$48=2 )thanolic solution of .henolphthalein
iii. (%4 'arium !hloride
-2. %.(M /ydrochloric Acid.

5. PROCEDURE
i. 7ei&h accurately and as 5uic"ly as possible, (%& (7) of sample into a #$%ml
conical flas".
ii. Dissol2e the sample in (%%ml of >$42=2 )thanol containin& %.$ml of %.$48=2
)thanolic solution of phenolphthalein.
iii. Add $ml of (%4 'arium chloride solution pre2iously heated and neutraliDed.
i2. Mi+ thorou&hly and titrate 8ith %.(M /ydrochloric acid at ;%o!, until pin"
colour disappears.
Then,
48=8 Free !austic Al"ali @ Titre I %.9(
7ei&ht of sample

CHLORIDE TEST.
Reagents
1. Silver Nitrate (AgNO3) solution.0.1N accurately standardised against reagent
grade sodium chloride which has dried at 105oc.
2. 2SO! solution 0.1N.
3. "otassium chromate indicator solution# dissolve 5g o$ %2&rO! in distil water and
add AgNO3 solution until a slight orange#red 'reci'itate is $ormed. (ilter and
dilute to 100ml with distilled water.
!. "henol'hthalein indicator solution 1) in *5) alcohol.
5. +agnesium nitrate solution 20) in distilled water. Solution must ,e neutral and
chloride $ree.
-. &alcium car,onate .reagent grade.

"rocedure/
1. 0eigh accurately 5g o$ the sam'le into 500ml ,ea%er and add 300ml o$ chloride
$ree distilled water. 1oil to e$$ect the solution.
2. Add a,out 25ml o$ 20) solution o$ +g (NO3).$ilter with sintered glass aided with
vacuum 'um'2 then wash thoroughly with chloride#$ree distilled water to remove
all chloride.
3. &ool to room tem'erature (20#25) o
c
. 3$ the solution is al%aline2 add a little
'henol'hthalein and the 0.1N 2SO! until 4ust colourless2 avoiding an e5cess o$
more than one dro' o$ acid. Add 1ml o$ %2&rO! indicator $or every 100ml solution
and titrate with .01n AgNO3 to the $irst 'ermanent reddish tinge.
!. "re'are a ,lan% in a 500ml ,ea%er containing the same volume o$ distilled water
+g (NO3) solution and indicator. Add su$$icient &a&O3 to the ,lan% to ma%e the
tur,idity e6uivalent to that o$ the sam'le when ,oth are swirled.
5. 7sing the ,lan% $or com'arison2 continue the titration o$ the sam'le until a $aint
,ut distinct colour change occur. At the end 'oint2 the colour o$ the sam'le
solution should not ,e dar%2 ,ut 4ust distinctly di$$erent $rom that o$ the ,lan%.
-. Add su$$icient .01 AgNO3 to the ,lan% so that the colour o$ the ,lan% and the
sam'le match.
&alculation/
&hloride as Na&l2 ) 8 (S#1) 5 N 5 5.95.
0t o$ sam'le used.
&hloride as :&l2 ) 8 (S#1) 5 N 5 ;.!-.
0t o$ sam'le used.
Where:
S8titre value o$ the sam'le
18titre value o$ the ,lan%. N8 normality o$ AgNO3.
Note
&aution/ :2&rO! is carcinogenic and should not ,e ingested or inhaled.
D)T)RM-6AT-16 1F )T/A61L -61LG'L).
0eigh 5.0g o$ soa' sam'le and dissolve in 90 ml hot alcohol and 20ml o$ distilled water.
eat to dissolve and 6uantitatively trans$er the solution into an already dried and weighed
$ilter 'a'er.
<ry the residue in the oven at 105oc $or one hour.
&ool in the desiccator and weigh to a constant weight (.0001g)
) alcohol insolu,le 8 w 5 100
0
w 8 weight o$ residue.
08 wt o$ sam'le ta%en.
D)T)RM-6AT-16 1F 7AT)R -61LG'L).
0eigh 5.0g o$ soa' sam'le and dissolve in 100 ml o$ water. eat to dissolve and
6uantitatively trans$er the solution into an already dried and weighed $ilter 'a'er.
<ry the residue in the oven at 105oc $or one hour.
&ool in the desiccator and weigh to a constant weight (.0001g)
) alcohol insolu,le 8 w 5 100
0
w 8 weight o$ residue.
08 wt o$ sam'le ta%en.
D)T)RM-6AT-16 1F G6A.16-F-)D MATT)R.
0eigh 5.0g o$ soa' sam'le and dissolve in 100 ml o$ 0.1+ ethanolic 'otassium
hydro5ide.
=rans$er in to a se'arating $unnel adda,out50ml o$ 'etroleum s'irit and 50ml o$ water.
7se 3 dro's o$ 'henol'hthalein where necessary and sha%e 'ro'erly. >5tract in to a
weighed ,ea%er and heat to eva'orate the s'irit. <ry in an oven and allow to cool.
&alculate the ) unsa'oni$ied matter as/
0t o$ ,ea%er and oil .wt o$ em'ty ,ea%er 5 100
0t o$ sam'le.
DETERMINATION OF TOTAL FATTY MATTER
1. AIM
To outline the procedure for the Determination of Total Fatty Matter (and resin)
acids, and any unsaponifiable matter present in soap sample.
5. PERSONNEL INVOLVED
The QA Laboratory Analyst, QA Laboratory Assistants,
6. EQUIPMENTS AND GLASSWARES NEEDED
Retort tands, !onical Flas"s (#$% ml), eparatin& Funnels (#$%ml), 'ea"ers
(#$%ml, $%ml), Measurin& !ylinders ((%%ml, $%ml),
#. REAGENTS NEEDED.
2i. Diethyl )ther*
vii. Tetrao+osulphate (,-) Acid (M !oncentration.
2iii. .otassium /ydro+ide (01/)* appro+ %.$M.
i+. Methyl 1ran&e -ndicator* %.%34 in A5ueous olution
+. .henolphthalein -ndicator (.%4 in 6eutral )thanol.

PROCEDURE
(3. 7ei&h accurately and as 5uic"ly as possible, $& (7() of sample into a #$%ml
conical flas". Dissol2e the soap in (%%ml of hot 8ater.
($. Add # drops of a5ueous methyl oran&e indicator.
(:. Drop 8ise add (M Tetrao+osulphate (2i) Acid until acidic. Add $ml e+cess acid.
(;. Thorou&hly mi+ the contents of the conical flas". -nsert a small funnel into the
nec" and heat (to a temperature not e+ceedin& :%
o
!) until the fatty acid
separates as a clear layer .Allo8 to cool to room temperature.
(<. Transfer 5ualitati2ely into a separatin& funnel, 8ashin& 8ith fresh portions of
Diethyl ether.
(>. )+tract the fatty matter 8ith $%ml diethyl ether. Dra8 off the a5ueous layer into
another separatin& funnel and 8ash $ times 8ith 9%ml portions of diethyl ether,
addin& the ether 8ashin&s to the ori&inal ether solution.
#%. 7ash the combined ether e+tracts 8ith (%ml portions of distilled 8ater until the
8ash 8ater is neutral to methyl oran&e. A2oid loss of fatty matter as an
emulsion.
#(. Mi+ the 8ater portion used for 8ashin& and sha"e 8ith #%ml ether. Add the
ether to the fatty acid=ether solution.
##. Run the ether solution into a tarred bea"er and rinse the separatin& funnel 8ith
portions of neutral ethanol up to a total of $%ml.
#9. )2aporate the fatty acid=ether solution until only residual 5uantities of ether are
discernible. Dry the fatty acids to constant 8ei&ht in an o2en at (%%? (%$
%
!
#3. Allo8 to cool and 8ei&h the residue of fatty and rosin acids (7#)
The total fatty matter is calculated thus,
4Total Fatty Matter @ 7# + (%%
7(

DETERMINATION OF TOTAL FREE AL"ALI
1. AIM
To outline the procedure for the Determination of Total Free Al"ali in soap
sample.
2. PERSONNEL INVOLVE
The QA Laboratory Analyst, QA Laboratory Assistants.
3. EQUIPMENTS AND GLASSWARES NEEDED
Retort stand, pipette, burette, !onical Flas"s (#$% ml), 'ea"ers (#$%ml, $%ml),
Measurin& !ylinders ((%%ml, $%ml),
!. REAGENTS NEEDED.
-. >$4 )thanol.
--. Tetrao+osulphate (,-) Acid %.$ M !oncentrations.
---. .henolphthalein -ndicator %.$4 in 6eutral )thanol.
5. PROCEDURE
-. 'oil (%%ml of >$4 2=2 ethanol on under reflu+ for (%minutes.
--. Add %.$4 )thanolic solution of phenolphthalein and allo8 to cool to ;%
1
c, then
neutralised 8ith %.(M )thanolic potassium hydro+ide solution
---. Add (%& of the soap sample and dissol2e it as 5uic"ly as possible by heatin&.
-,. Add 9ml of %.$M sulphuric acid and boil in 8ater bath for at least (%mins to
neutralise the solution to colourless.
,. -f the solution appears pin" after boilin& add a further 5uantity of %.$M sulphuric
acid.
,-. Titrate the colourless solution 8ith (M odium /ydro+ide solution until the pin"
colour appears.
4 8=8 Total free al"ali (calculated as 6a#1)
@ (' F A) I 9.(
7
7hereJ A@ ml of (M odium hydro+ide solution re5uired.
' @ ml of %.$M ulphuric acid solution added.

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