INTRODUCTION

Dietaryfibercanbedefinedassumofpolysaccharides
and lignin that are not digested by human digestive
enzymes. The major components of dietary fiber are
cellulose, noncellulose such as hemicelluloses and
pectin,lignin,andhydrocolloids(gums,mucilages,and
algalpolysaccharides).Humanfoodstuffscontainmainly
noncellulosepolysaccharides,somecelluloseandlittle
lignin. The average proportions of noncellulose
polysaccharides. Cellulose and lignin for common
foodstuffareabout70%,20%and10%respectively.The
crude fiber method was developed in the 1850s to
estimateindigestiblecarbohydrateinanimalfeeds.Crude
fiber method is one of the gravimetric method that
measures the organic food residue remaining after
sequential digestion with 0.255N sulphuric acid and
0.313Nsodiumhydroxidesolutions,followedbyoven
dryingat104Covernightandignitioninmufflefurnace
at 600C for 3 hours. The compounds removed are
predominantlyprotein,sugar,starch,lipidsandportions
of both the structural carbohydrates and lignin. Crude
fibermethodmeasuresvariableamountsofthecellulose
andlignininthesample,buthemicelluloses,pectins,and
added gums or hydrocolloids are solubilised and
removed.Therefore,crudefibremeasurementdrastically
underestimatesdietaryfibreinfoodssinceitmeasures
onlycelluloseandlignin.Asaresult,crudefibermethod
isonlyadequatefordeterminationoffibreinanimalfeed
product, but not suitable for human food analysis as
ligninissignificanttohumanhealth
Determinationoffiber:
In the analysis of cellulosecontaining foods, the determination of crude fiber is
widelyused.Crudefiberincludestheoretically,materialsthatareindigestibleinthe
humanandanimalorganism.Itisdeterminedasmaterialinsolubleindiluteacidand
dilute alkali under specific conditions. The basic method is based on procedure
developedbyHennenberg,Stohmann,andRautenbergin1864inGermany.Inthe
determination, 2g of material are defatted with petroleum ether and boiled under
reflux for exactly 30 min with 200ml of solution containing 1.25g of sulfuric
acidper100mlofsolution.Thesolutionisfilteredthroughlinenorseverallayersof
cheeseclothonaflutedfunnelandwashedwithboilingwateruntilthewashingsare
nolongeracid.Theresidueistransferredquantitativelytoabeaker,andboiledfor30
minwith200mlofsolutioncontaining1.25gofcarbonatefreesodiumhydroxideper
100ml.Thefinalresidueisfilteredthroughathincutclosepadofwashedandignited
asbestosinaGoochcrucible,driedinanelectricoven,weighed,incinerated,cooled
andweighedagain.Thelossofweightistakenascrudefiber.Theresiduefroma
crude fiber determination contains about 97% cellulose and lignin. It does not
represent,however,allthecelluloseandligninpresentinitially.Inaddition,thecrude
fiber is a mixture of cellulosic materials and does not represent any specific
compoundorgroupofcompounds.Despiteitsnonspecificcomposition,crudefiberis
ausefulparameterinfoodandfeedanalyses.Crudefiberiscommonlyusedasan
indexofthefeedingvalueofpoulteryandstockfeeds,toevaluatetheefficiencyof
milling and separating bran from starchy endosperm and in the chemical
determinationofsucculenceoffreshvegetablesandfruits.

MaterialsandMethod
Materials
Roundbottomflask
Beaker
Refluxcondenser
Sinteredcursible(goochcrucible)
Asbestoswool
Desicator
Heatingmantle
Weighingbalance
Sulphuricaciddil
Sodiumhydroxide
LitmusPaper
Tealeaves

Determinationoffiber:

2gofteawasweighedintoa1literconicalflask.Then200mlofboilingH2SO4and
boilfor30minsoverabunenburnerwhileswirlingoccasionallytoremovesolids
fromadhereingtothesolidsfromadheringtothesidesoftheflask.Thehotsolution
was decanted through Buchner funnel fitted with whatman 52 filter paper. All
residues was transferred and rinsed with boiling water until no colour change in
litmuspaper.Thentheresiduewastransferredbyusing200ml1.25%NaOHsolution
intoa1literflaskandbroughttoboilandmaintainedagentleebullitionfor30mins
andfilteredthroughrapidhardenedfilterpaperandtransferredthefiberquantitatively
andwashedwith1%HCluntilthefiltrateisfreefromalkalifollowedbydistilled
water,15mlofalcoholand10mlofdiethylether.Thentheresiduewasquantitatively
transferredtoataredcrucibleandsiredintheovenat105OCandweighedafter
cooling.Thenthiswasincineratedat5000Candweighedaftercooling.

Calculations
MoistureContent
WeightofSample=2.0701g
WeightofSample+Crucible=15.3377g
Drysample+Crucible=15.2036g
MoistureContent=WeightLossX100
Weightofsample

=15.3377g15.2036gX100
2.0701
=6.47%
WeightofsampletakenforfiberAnalysis=2.0001g
DryweightofSample2.001gX93.53
100
=1.8707
Weightofemptycrucible=30.1927g

Crucible+filterpaper=30.8510g
Afterdryingat105oCinoven=crucible+Fiber+ash
=31.0640g(m1)
Afterincineratingat550oC=crucible+ash
=30.1965g(m2)

Fiber%=m1m2X100
Sample
=(31.0640g30.8510g)(30.1965g30.1927g)X100
1.8707g
=11.18%

Discussion
Themaximumamountofcrudefiberthatcanbepresentinteais16.5%.Theabove
valuesshowthatthisisuptostandards.Thelowlevelofcrudefibermaybedueto
the reason since this isblended tea. The rate of heating should be gently
boiled. Filtering should be done as soon as possible since latefiltration
generallyresultsinlowerresults.Toreduceevaporationlossesduringboilingthe
refluxcondenserisused. In digestion except fiber others are dissolve in
sulfuric acid and NaOH. Hemicelluloses get dissolveindilutealkaliwhile
pectinandhydrocolloidsdissolveinhotwater.Proteinisdenaturedandlostinstrong
acidtreatment.Butmineralmatterdonotgetdissolveinabovetreatments.Due to
this these remain with insoluble fiber matters. To avoid this error ash
contentisdetermined anddeductstheamountofashfromthefiber.Ateaboard
standard for crude fiber is 16.5%. The sample that tested has 11.18 %
crude fiber content.Experimentvalueislessthanthevalueofcommercialvalue.
Thereforethesampleisnotadulteratedwithothermaterials.Sinceteadoesntcontain
fat,samplewasntdefatted.Samples should be transferred quantitatively to
avoid the loss of fiber. In final filtration ash less filter paper must be
used,otherwisefibersofthefilterpapermayaddedtothefibercontent
ofthesample

INTRODU
CTION
Dietary
fibercanbe
definedas
sumof
polysacchari
desand
ligninthat
arenot
digestedby
human
digestive
enzymes.
Themajor
components
ofdietary
fiberare
cellulose,
non
cellulose
suchas
hemicellulos
esand
pectin,
lignin,and
hydrocolloid
s(gums,
mucilages,
andalgal
polysacchar
ides).
Human
foodstuffs
contain
mainlynon
cellulose
polysacchari
des,some
cellulose
andlittle
lignin.The
average
proportions
ofnon
cellulose
polysacchari
des.
Cellulose
andlignin
forcommon
foodstuff
areabout
70%,20%
and10%
respectively.
Thecrude
fiber
methodwas
developed
inthe1850s
toestimate
indigestible
carbohydrat
ein
animal
feeds.Crude
fiber
methodis
oneofthe
gravimetric
methodthat
measures
theorganic
foodresidue
remaining
after
sequential
digestion
with0.255N
sulphuric
acidand
0.313N
sodium
hydroxide
solutions,
followedby
ovendrying
at104C
overnight
andignition
inmuffle
furnace
at600Cfor
3hours.The
compounds
removedare
predominant
lyprotein,
sugar,
starch,lipids
andportions
ofboththe
structural
carbohydrat
esand
lignin.
Crudefiber
method
measures
variable
amountsof
thecellulose
andligninin
thesample,
but
hemicellulos
es,pectins,
andadded
gumsor
hydrocolloid
sare
solubilised
and
removed.
Therefore,
crudefibre
measuremen
t
drastically
underestima
tesdietary
fibrein
foodssince
itmeasures
only
cellulose
andlignin.
Asa
result,crude
fiber
methodis
only
adequatefor
determinatio
noffibrein
animalfeed
product,but
not suitable
for human
food
analysis as
lignin is
significant
to human
health
OBJECTIV
E
To
determine
thecrude
fibrecontent
infood
sample
usingacid
andalkali
digestion
method.
PROCEDU
RE
1.

1g0.001
(W)ofdried
ground
samplewas
weighed
intoa
crucible.
2.

200mL
1.25%N
H2SO4was
added.
3.

Exactly
boiledfor
30minutes.
4.

Contents
werefiltered
andwashed
theresidue
withhot
wateruntil
freefrom
acid.
5.

200mL
1.25%N
warm
NaOHwas
addedinto
thebeaker
containing
the
insoluble
materialand
boiledfor
30minutes.
6.

23dropsof
octyl
alcoholwas
addedto
prevent
foaming
during
boiling.
7.

Contents
werefiltered
andwashed
theresidue
withhot
water(four
times),then
with15
mLof1%
hydrochloric
acid(twice).
8.

Thesample
waswashed
withhot
wateragain
untilitis
neutralor
freefrom
acid.
9.

Thecrucible
was
transferred
with
insoluble
materialinto
theovenat
105

Ctoa
constant
weight.The
weightof
residueand
crucible
(W2)were
recorded.
10.

Theresidue
waschar
gentlyover
aBunsen
burneruntil
ithasceased
smoking.
11.

Theresidue
wasignited
inamuffle
furnaceat
550

Cfor3
hours.
12.

Thecrucible
wascooled
indessicator
and
weighed.
Theweight
ofashand
crucible
(W3)
were
recorded.
13.

The loss in
weight on
ignition
represents
the weight
of crude
fibre.
CALCULA
TION
gcrudefibre
per100g
sample=
(W2

W3)x100
W1
Where,
W1=weigh
ingramof
sample
taken
W2=weigh
ingramof
crucible+
dried
residue
W3=weigh
in gram of
weigh of
crucible +
ash
QUESTION
S
1.

Calculate
thevolume
of:
a.

Concentrate
dsulphuric
acid
requiredto
makeupa
litreof
1.25%MH
2
SO
4

Volume=

=13.03m

/0.01302

0.1302

ofH
2
SO
4
requiredto
makeupa
litreof
1.25%M
NaOH
b.

Weightof
NaOHused
topreparea
litreof
1.25%N
NaOH
Mole=

1.25

=

Mass

=50g
2.

Whyis
crudefibre
determinatio
nimportant
infood
analysis?
Itisusedas
anindexof
thefeeding
valueof
poultryand
stackfeeds,
seedshigh
incrude
fibrecontent
arelowin
nutritional
value.Itis
alsousedin
thechemical
determinatio
n
succulence
offresh
vegetables
andfruits.
3.

Whatarethe
factorsthat
aregreatly
affectedthe
accuracyof
crudefibre
determinatio
n?
Factorthat
aregreatly
affectedthe
accuracyof
crudefibre
determinatio
nisthe
manipulatio
n and the
procedures
of the
experiment
itself

DISCUSSI
ON
Inthis
experiment
acidand
alkali
digestion
methodis
usedto
determine
thecrude
fibre
contentin
food
sample.The
foodsample
thatweused
inthis
experiment
iscarrot.
Crudefibre
referstothe
residueofa
feedthatis
insoluble
after
successive,
boilingwith
diluteacid
and
alkali.The
alkaline
hydrolysis
will
removes
proteinand
some
carbohydrat
es.This
processalso
removes
somehemi
cellulose
andlignin.
Besides,
onlypartial
recoveryof
fibre
components
is
achieved
.
Crudefibre
isthe
portionof
thetotal
carbohydrat
eofafood
thatis
resistantto
theacid
andalkali
treatment.In
this
experiment,
wehave
usedcarrot
asasample.
Thesample
weneedto
makethis
experiment
is1g.Some
soluble
hemicellulos
esare
solubilised
intheacid
digestion
and
arealso
extensively
andvariably
solubilised
inthe
alkaline
digestion.In
addition,
this
indigestible
components
willbe
considered
aspartof
the
nitrogen
freeextract,
causinga
serious
errorinthe
calculated
nutritive
valueofthe
food.The
chemical
reagentwe
wasusedin
this
experiment
issulphuric
acid
(H2SO4)
1.25%,
sodium
hydroxide
(NaOH)
1.25%and
hydrochloric
acid(HCl)
1%.
Theresults
of
experiment
acidand
alkali
digestion
methodfor
threetrials
weretaken
and
percentage
were
calculated
byformula
given.The
mean
percentage
oftotalash
thatweget
is
91.08%