Food Analysis Practical

Food Analysis and Quality Control
A Practical Manual

VedpalYadav,LecturerinFoodTechnology,GovernmentPolytechnic,MandiAdampur,Hisar,
Haryana,India125052.

emailvedpalp@yahoo.com
Cell +919416589819

6.2FOODANALYSISANDQUALITYCONTROL
LISTOFPRACTICALS
1. Proximateanalysisofmarketedfoodproducts
1.1. Moisture
1.2. Ash
1.3. CrudeFat
1.4. CrudeProtein
1.5. CrudeFibre
1.6. Carbohydrates
2. Detectionofadulterationinfoodproductsviz.
2.1. milk,
2.2. ghee,
2.3. honey,
2.4. spices,
2.5. pulses,
2.6. oils,
2.7. sweetsetc.
3. Detectionofnonpermittedfoodadditivesinmarketfoodsamples,
3.1. sweetsand
3.2. savoryproducts
4. Cutoutanalysisofcannedfood
5. Testofsensoryevaluation
1.1. Hedonicscale
1.2. Duotriotest
1.3. Rankingdifference
1.4. Triangletest
6. Detectionofbasictastesandtheirthresholdvalues
7. Consumeracceptabilitytrial
8. Statisticalanalysisofsensorydata
9. Laboratorypreparationoffoodproductsandtheirsensoryanalysis
10. Determinationofinsecticidesresidueingivenfoodsample
11. Visits to the quality control laboratories of the food industry, educational institutions and testing
centres
Table of Contents
Experiment1MoistureContentLabOvenMethod.....................................................................................4
Experiment2MoistureContentUsingMoistureMeter...............................................................................7
Experiment3AshTotal..............................................................................................................................10
Experiment4AshAcidInsoluble................................................................................................................14
Experiment5CrudeProteinKjeldahlMethod............................................................................................17
Experiment6CrudeFatSoxhletApparatusMethod..................................................................................28
Experiment7TotalCarbohydrates..............................................................................................................32
Experiment8CrudeFiber............................................................................................................................34
Experiment9CutouttestforCannedFisheryProducts..............................................................................39
Experiment10Detectionofadulterantsindifferentfoodproducts...........................................................43
Experiment11OrganochlorinePesticidesinWaterbyGasChromatgraphic(GC)Method.......................57
Experiment12NMethylcarbamoyloximesandNMethylcarbamatesinFinishedDrinkingWaterbyHigh
PerformanceLiquidChromatography(HPLC)................................................................................................62
Experiment13AcesulfameKDetectionandDeterminationinSweets.......................................................66
Experiment14SensoryEvaluationGeneralConcepts................................................................................71
Experiment14SensoryEvaluationTasteIdentificationTest.....................................................................80
Experiment15SensoryEvaluationTasteIntensityTests...........................................................................83
Experiment16SensoryEvaluationPreferenceTestPairedPreferenceTest............................................87
Experiment17SensoryEvaluationPreferenceTestHedonicRatingScale...............................................92
Experiment18SensoryEvaluationPreferenceTestFoodAction/AttitudeRatingTest..........................98
Experiment19SensoryEvaluationPreferenceTestPreferenceRankingTest.......................................103
Experiment20SensoryEvaluationDifferenceTestPairedComparisonTest.........................................109
Experiment21SensoryEvaluationDifferenceTestTriangleTest...........................................................120
Experiment22SensoryEvaluationDifferenceTestDuoTrioTest..........................................................126
Experiment23SensoryEvaluationDescriptiveTestDescriptiveRankingTest.......................................132
Experiment24SensoryEvaluationDescriptiveTestDescriptiveRatingTestsLineScales....................137
Experiment25SensoryEvaluationDescriptiveTestDescriptiveRatingTestStarDiagrams.................145
Appendix1SummaryofSensoryAnalysisTestsSuitablefortheClassroom..............................................155
Appendix2Scales........................................................................................................................................156
Appendix3PresentationofResults............................................................................................................162
Appendix4GlossaryofTermsUsedinSensoryAnalysis............................................................................165
Bibliography..................................................................................................................................................166
Index.............................................................................................................................................................167

VedpalYadav,LecturerinFoodTechnology,GovernmentPolytechnic,MandiAdampur,Hisar,Haryana,India125052.
emailvedpalp@yahoo.com +919416589819 Page4of168
Experiment1MoistureContentLabOvenMethod
Objective:
Tofindoutthemoisturecontentfromagivenfoodsamplebylabovenmethod.
Theory:
Uponheatingwaterevaporatesandlossofweightisequaltothemoisturecontentofmaterial.
Materials:
1. Enoughfoodsampletosupplythree20gramsamples.
2. Oven (almost any oven will do, provided the temperature can be set reliably at 130C for an
extendedperiodoftime).
3. AnalyticalBalance.
4. Tray(toplacethepaddygrainsamplesonbeforedryingintheoven).
5. Simpleplasticcontainersorsmallpaperbagstoholdgrain.
6. Pen/pencil, paper and calculator to compute the average of three samples and record the
moisturecontent.
Procedure:
1. Settheoventemperatureto130C.
2. Fromyourpaddygrainsupply,useyourscaletomeasurethree20grampaddygrainsamples.
3. Placethethreesamplesinsidetheovenandleavefor1624hours.
4. Measurethefinalweightofeachsampleafterthe16to24hours.
5. Computethemoisturecontentforeachsampleusingtheequation.
6. Younowhavethreeseparatemoisturecontentresults.Computetheaverageoftheseresultsby
addingthemtogetheranddividingby3.
Calculation:
MoistureContent(%) = {(W2W1)/(W1W)}x100
Where,
W = Weightofemptymoisturedish
W1 = Weightofemptymoisturedish+Sample
W2 = Weightofemptymoisturedish+DriedSample
Observations:
Sample
WheatFlour
Name
Weightof
WeightofEmpty WeightofMoisture
Sample Moisture
MoistureDish(W) Dish+DriedSample
Number Dish+Sample(W1)
(ingms.) (W2)(ingms.)
(ingms.)


Weightof
Weightof
Sample %
Moisture(W2W1) Moisture% AverageMoisture%
(W1W) RSD
(ingms.)
(ingms.)
Conclusions:
1. Dideachofyoursamplescontainapproximatelythesameamountofmoisturecontent?
2. Whatwastheaveragemoistureofallthreesamples?
3. Basedonwhatyouknowaboutcorrectmoisturecontentformilling(14%),isthepaddyriceyou
sampledreadyformilling?Whyorwhynot?
Sample
WheatFlour
Name
Weightof
WeightofEmpty WeightofMoisture
Sample Moisture
MoistureDish(W) Dish+DriedSample
Number Dish+Sample(W1)
(ingms.) (W2)(ingms.)
(ingms.)
A 34.5679 39.6384 39.5173
B 34.3369 39.7865 39.6652
C 34.1256 39.5596 39.4396
Weightof
Weightof
Sample %
Moisture(W2W1) Moisture% AverageMoisture%
(W1W) RSD
(ingms.)
(ingms.)
5.0705 0.1211 2.39
5.4496 0.1213 2.23 2.28 4.327
5.4340 0.1200 2.21

SpaceforObservationsandCalculations

Experiment2MoistureContentUsingMoistureMeter
Objective:
Tofindoutthemoisturecontentfromagivensamplebyusingmoisturemeter.
Materials:
1. Moisturemeterandinstructionsforuse
2. Paddyriceenoughtoprovidethreesamplesforthemoisturemeter(approximatelyonehandful)
3. Simpleplasticcontainersorsmallpaperbagstoholdgrain
4. Pen/pencil, paper and calculator to compute the average of three samples and record the
moisturecontent
Procedure:
1. Readtheoperatorsinstructions.
2. Turnthemoisturemeteron.
3. Ensurethemachineissetforpaddyrice.
4. Fillthetrayorbowlofthemoisturetesterwithasampleofthepaddyricetobetested
5. Turnorpresstheknobuntilthemoisturereadingisdisplayed.
6. Testatleastthreesamplesandcalculatetheaverageofthethreereadings.
Observations&Calculations:
Sample

Volume

Thickness

SampleNo. Moisture%
AverageMoistureContent

%RSD

Conclusions:
1. Dideachofyoursamplescontainapproximatelythesameamountofmoisturecontent?
2. Whatwastheaveragemoisturecontentofallthreesamples?
3. Isthepaddyriceyousampledreadyformilling?Whyorwhynot?


Sample Paddy
Volume C
Thickness 3.25
SampleNo. Moisture%
1 10.30
2 10.40
3 10.80
AverageMoistureContent 10.50
%RSD 2.52


Experiment3AshTotal
Objective:
Tofindouttheashinthegivenfoodsample.
Theory:
Organicmatterisburntoffataslowtemperatureaspossible.Heatingisdoneinstages,firsttocharthe
productthoroughlyandfinallytoashat550Cinamufflefurnace.Theinorganicmatterleftafterburning
organicmatteriscooledandweighed.
Apparatus:
1. Crucible
2. HeatingPlate
3. MuffleFurnace
4. Dessicator
5. AnalyticalBalance
Procedure:
1. Placethecruciblesinmufflefurnacetoheatat550Cfor15minutes.
2. Removethecrucibles,coolinadessicatorforonehourandweighthecrucible(W).
3. Weigh2gofsampleinthecrucible(W1).
4. Keep the sample on a hot plate till smoking ceases and sample become thoroughly
charred.
5. Placethecruciblesinsidethemufflefurnaceandheatto550Cfor5to6hours.
6. Let the furnace cool and take out crucibles containing ash, clean and white in
appearance.
7. Iftracesofcarbonarestillevident,coolthecrucible,add 1 2 mlofwaterandstir
withaglassrodtobreakuptheash.Dryonsteambathandplaceinmufflefurnace
andagainheatat550C.
8. Coolthecrucibleinadessicatorandreweigh(W2)thecruciblecontainingash.
Calculation:
Ash% = {(W2W)/(W1W)}x100
Where,
W = Weightofemptycrucible
W1 = Weightofemptycrucible+Sample
W2 = Weightofemptycrucible+AshedSample
Observations:

SampleName ___________________________

WeightofEmpty WeightofSilica WeightofSilica
Sample
SilicaCrucible(W) Crucible+Sample Crucible+AshedSample
Number
(ingms.) (W1)(ingms.) (W2)(ingms.)
A

C

Weightof
WeightofAsh(W2 %
Sample(W1 Ash% AverageAsh%
W)(ingms.) RSD
W)(ingms.)
SampleName WheatFlour
WeightofEmpty WeightofSilica WeightofSilica
Sample
SilicaCrucible(W) Crucible+Sample Crucible+AshedSample
Number
(ingms.) (W1)(ingms.) (W2)(ingms.)
A 10.2569 12.2698 10.2762
B 10.2444 12.3009 10.2642
C 10.3597 12.4001 10.3801
Weightof
WeightofAsh(W2 %
Sample(W1 Ash% AverageAsh%
W)(ingms.) RSD
W)(ingms.)
2.0129 0.0193 0.96
2.0565 0.0198 0.96 0.97 2.381
2.0404 0.0204 1.00


Experiment4AshAcidInsoluble
Objective:
Tofindouttheacidinsolubleashfromagivenfoodsample.
Reagents:
DilHCLapproximately0.5Npreparedfromconc.HCl
Procedure:
Totheashcontainedinadish,add25mlofdil,HCl.Coverwithawatchglassandheatonawaterbathfor
10minutes.AllowtocoolandfitterthecontentsofthedishthroughaWatmanfilterpaperNo.42orits
equivalent.Washthefilterpaperwithwateruntilthewashingarefreefromtheacidandreturnittothe
dish.Keepitinanelectricovenmaintainedat13520Cforabout3hrs.Igniteinamufflefurnaceat550
6000Cfor1hr.
Cool the dish in a dessicator and weigh. Repeat the process of igniting in muffle furnace, cooling and
weighingathalfhoursintervaluntilthedifferenceinmassbetween2successiveweighingsislessthan1
mg.Note:thelowestmass.
Calculation
%AshInsolubleash(ondrybasis)
100( W2 W)
( W1 W)
%bymass=
Where
W2 Massingofdish+acidinsoluble
W Massingofemptydish
W1 Massingofdishwiththedriedmaterial
ObservationandResult
Acidinsolubleash%ofagivensample
100(37.7816 37.7786)
( 45.7786 37.7786)

100 0.0030
0.037 %
= 8
Where
W2 = 37.7816g
W1 = 45.7786g
W = 37.7786g

Sample
WheatFlour
Name
WeightofSilica WeightofSilicaCrucible+Acid
Sample WeightofEmptySilica
Crucible+Sample InsolubleAshedSample(W2)
Number Crucible(W)(ingms.)
(W1)(ingms.) (ingms.)
A 10.2569 12.2698 10.2641
B 10.2444 12.3009 10.2521
C 10.3597 12.4001 10.3671
Weightof WeightofAcid
AcidInsoluble
Sample(W1 InsolubleAsh(W2W) AverageAcidInsolubleAsh% %RSD
Ash%
W)(ingms.) (ingms.)
2.0129 0.0072 0.36
2.0565 0.0077 0.37 0.36 1.604
2.0404 0.0074 0.36


Experiment5CrudeProteinKjeldahlMethod
Objective:
Tofindouttheamountofcrudeproteininagivenfoodsample.
Introduction
The protein content of foods can be determined by numerous methods. The Kjeldahl, nitrogen
combustion (Dumas) and infrared spectroscopy methods for protein analysis are based on nitrogen
determination.ThemethodsarefromtheOfficialMethodsofAnalysisofAOACInternational(1),andare
usedcommonlyinresearchlaboratoriesworkingonproteins.
Theory
Nitrogen is one of the five major elements found in organic materials such as protein. This fact was
recognizedbyaDanishchemist,JohanKjeldahl,whouseditasamethodofdeterminingtheamountof
protein in samples taken from a wide variety of organisms. In 1883 Kjeldahl presented to the Danish
Chemical Society a method (much revised since his day) for determining the amount of nitrogen in
mixturesofsubstancescontainingammoniumsalts,nitrate,ororganicnitrogencompounds.
The central basis used in this procedure is the oxidation of the organic compound using strong sulfuric
acid. As the organic material is oxidized the carbon it contains is converted to carbon dioxide and the
hydrogenisconvertedintowater.
Thenitrogen,fromtheaminegroupsfoundinthepeptidebondsofthepolypeptidechains,isconverted
toammoniumion,whichdissolvesintheoxidizingsolution,andcanlaterbeconvertedtoammoniagas.
TheKjeldahlmethodofnitrogenanalysisistheworldwidestandardforcalculatingtheproteincontentina
widevarietyofmaterialsrangingfromhumanandanimalfood,fertilizer,wastewaterandfossilfules.
Principle
TheKjeldahlprocedurecanbebasicallydividedintothreeparts:(1)digestion,(2)distillation,(3)titration.
In the digestion step, organic nitrogen is converted to an ammonium in the presence of a catalyst at
approximately 370C. In this experiment, the sample is digested in H2SO4, using Copperbased catalyst,

convertingNtoNH3whichisdistilledandtitrated.
Sulfuricacid

Protein (NH4)2SO4
Heat,catalyst
InthedistillationstepthedigestedsampleismadealkalinewithNaOHandthenitrogenisdistilledoffas
NH3.ThisNH3istrappedinaboricacidsolution.
(NH4)2SO4+2NaOH2NH3+Na2SO4+2H2O

NH3+H3BO3(boricacid) NH4+H2BO3
(borateion)
TheamountofammonianitrogeninthissolutionisquantifiedbytitrationwithastandardHClsolution.A
reagent blank is carried through the analysis and the volume of HCl titrant required for this blank is
subtractedfromeachdetermination.

H BO +H+ H3BO3
2 3
Thisanalysisdeterminestotalnitrogenandnotusablenitrogenandthisisthereasonitiscalledacrude
proteinanalysis.
Athreestepprocedure
TheKjeldahlmethodconsistsofthreesteps,whichhavetobecarefullycarriedoutinsequence:
1. thesampleisfirstdigestedinstrongsulfuricacidinthepresenceofacatalyst,whichhelpsinthe
conversionoftheaminenitrogentoammoniumions,
2. theammoniumionsarethenconvertedintoammoniagas,heatedanddistilled.Theammoniagas
isledintoatrappingsolutionwhereitdissolvesandbecomesanammoniumiononceagain,
3. finally the amount of the ammonia that has been trapped is determined by titration with a
standardsolution,andacalculationmade.
StepOne:DigestionoftheSample
Thisisthemosttimeconsumingstepintheanalysis.Thepurposeofthisstepistobreakdownthebonds
thatholdthepolypeptidestogether,andconvertthemtosimplerchemicalssuchaswater,carbondioxide
and,ofcourse,ammonia.
Suchreactionscanbeconsiderablyspeededupbythepresenceofacatalystandbyaneutralsubstance,
such as potassium sulfate (K2SO4), which raises the boiling point of the digesting acid and thus the
temperatureofthereaction.
Catalysts are also used to help in the digestion process; many different one have been tried including
selenium,mercury,copper,orionsofmercuryorcopper.


Digestionisaccomplishedby:
1. Weighingoutapproximately1gmofthesamplecontainingprotein,makinganoteoftheweight,
and placing the sample into a digestion flask, along with 1215 ml of concentrated sulfuric acid
(H2SO4).
2. Addingsevengramsofpotassiumsulfateandacatalyst,usuallycopper.
3. Bringing the digestion tube/flask and mixture to a "rolling boil" (about 370oC to 400oC) using a
heatingablock.
4. Heating the mixture in the tube/flask until white fumes can be seen, and then continuing the
heatingforabout6090mins.
5. Coolingthetube/flaskandcautiouslyadding250mlsofwater.
StepTwo:Distillation
The purpose of the next step, distillation, is to separate the ammonia (that is, the nitrogen) from the
digestionmixture.Thisisdoneby,
1. raisingthepHofthemixtureusingsodiumhydroxide(45%NaOHsolution).Thishastheeffectof
changingtheammonium(NH4+)ions(whicharedissolvedintheliquid)toammonia(NH3),whichis
agas.
2. separatingthenitrogenawayfromthedigestionmixturebydistillingtheammonia(convertingit
toavolatilegas,byraisingthetemperaturetoboilingpoint)andthentrappingthedistilledvapors
inaspecialtrappingsolutionofabout15mlHCl(hydrochloricacid)in70mlofwater.
3. removingthetrappingflaskandrinsingthecondenserwithwatersoastomakesurethatallthe
ammoniahasbeendissolved.

StepThree:Titration
Astheammoniadissolvesintheacidtrappingsolution,itneutralizessomeoftheHClitfindsthere.What
acid is left can then be "back titrated", that is titrated with a standard, known solution of base (usually
NaOH).Inthiswaytheamountofammoniadistilledofffromthedigestivesolutioncanbecalculated,and
hencetheamountofnitrogenintheproteindetermined.

Thequantitiesofacid,andhenceammoniaaredeterminedby,
1. adding an indicator dye to the acid/ammonia trapping solution. This dye should turn a strong
color,indicatingthatasignificantamountoftheoriginaltrappingacidisstillpresent.
2. puttingastandardsolutionofNaOH(sodiumhydroxide)intotheburet(alongtubewithatapat
the end),andslowly, slowly addingsmall amountsofthesodiumhydroxidesolutiontotheacid
solutionwiththedye.
3. watching for the point at which the dye turns orange, indicating that the "endpoint" has been
reachedandthatnowalltheacidhasbeenneutralizedbythebase.
4. recordingthevolumeoftheneutralizingbase(sodiumhydroxidesolution)thatwasnecessaryto
reachtheendoint.
5. performingacalculationtofindtheamountofammonia,andthusnitrogen,thatcamefromthe
originalsample.
Calculations

Onemoleofammoniacomingfromthedigestionmixture(andhencefromtheoriginalprotein)will
neutralizeexactlyonemoleoftheacidinthetrappingflask.
Thefirstcalculation,therefore,istofindthenumberofmolesofammoniathathavebeenproducedand
thentrappedfromyoursample(s).
Thisisdoneby,
calculatingthenumberofmolesofacidinthetrappingflaskoriginally(beforeanyammoniawas
trapped)bymultiplyingthemolarityoftheacidsolutionbythevolumeofthetrappingsolution
molesofacid=molarityofacidxvolumeusedinflask
(molesA=MxV)
calculatingthenumberofmolesofbase(NaOH)thatwereaddedfromtheburettoneutralizethe
remainingacid(thatNOTneutralizedbytheammonia).
molesofbase=molarityofbasexvolumeaddedfromburet
(molesB=MxV)
subtractingthe"molesofbase"addedfromthe"molesofacid"presentatthebeginning,toget,
thenumberof"molesofammonia"comingfromtheprotein,
thenumberof"molesofammonia"isthesameasthe"molesofnitrogen",
so...tocalculatethenumberofgramsofnitrogenintheoriginalsampleofprotein,multiplythe
"molesofnitrogen"bytheatomicmassofnitrogen(massofatomsofnitrogen),
gmsnitrogen=molesnitrogenxatomicmass
(gN=molesNx14.0067)
percentNitrogen
Thepercentageofnitrogenfoundintheorginalsamplecannowbecalculatedby:
%nitrogen=(gmsnitrogen/gmssample)x100
%N=(gN/gS)x100
Itisalsopossibletocalculatetheamountofcrudeproteininthesample.Althoughtherearedifferences
betweendifferentsamples,theamountof"crudeprotein"(CP)canbefoundbymultiplingthepercent
Nitrogenbyafactor(usually6.25).
CP=%Nx6.25
Apparatus/Instrument/Chemicals/Samples
Sulfuricacid98%min.
Catalysttabletstobeused:KjeltabsCX
Causticsoda32%
Boricacidsolution2%

IndicatorSolutionM5(Merck)orsimilar
Standardacid0.1Norc=0.1mol/,alternativelysulfuricacid0.1Norc=0.05mol/l
Mechanicalcomminutinginstrument
Analyticalbalance(0.001g)
KjeldahldigestionblockKjeldatherm,Turbotherm,flaskheaterforKjeldahlflaskwithwideneck
opening
VapodestdistillationSystem
Burette,50mlnominalcapacity,withascaleon0.05mlortitrationsystem(notwiththeVap50)
orpHmeterwithcombinedelectrode
Procedure
1. SamplePreparation
1. Weighaccurately2.00gcomminutedsampleasastartonapieceofafilterpaper.
2. Storethesampleairtightsothatanychangesordecayofthecompositionisavoided.Priortothe
analysisthesampleshouldbeatroomtemperature.Theexaminationofthethuspreparedsample
hastobedonewithinthefollowing24h.
2. Digestionchemicals
1. The chemicals are added. Sulfuric acid is used to wash down any sample residue, which might
remainattheglasswalls.
Chemicals
Sulfuricacid 20ml
Kjeltabs 2
Indicatorsolution
M5
Standardacid0.1Norc=0.1mol/L;
alternativelysulfuricacid0.1Nor
c=0.05mol/L
3. DigestionwithKjeldatherm
WhenworkingwithaKjeldathermSystemwith250mlKjeldathermdigestiontubes,thefollowing
digestionparametersarerecommended:
Timeinmin TemperatureinC Comments

40 400 Digestiontubesareputintothepreheatedblockand
timeittakesforthesampletobecometranslucent
30 400 Dehydratethesample
Foamingduringthedigestionhastobeexpected,however,thefoamingshouldnotgohigherthen
2/3oftheglass.
Ifexcessivereactionsshouldoccur,takeouttheinsertrack.
Duringthedigestionblackparticlesremainingattheglasswallarewashedbackwithcondensing
sulfuricacid.
Thesampleglasshastobetranslucentafterthedigestioninordertoobtaingoodresults.
4. DigestionwithTurbotherm
WhenworkingwithaTurbothermSystemwith250mlKjeldathermdigestiontubes,thefollowing
programparameterarerecommended:
Timein Powerin% Comment

min
10to15 100 Heatingupofthesystemtobringdigestionsolutionto
boiling
60 70to80 Digestionsolutionisturningtranslucentafterca20to30
min
5. DigestionwithFlaskheater
ForSerialFlaskHeaterwith500or750mlKjeldahlflaskwithwideneckopeningthefollowing
procedureisrecommended:
Timein Power Comments

min
20 3 Heatinguptillthedigestionsolutionisboiling
50 1,5 After 2030 min. the sample should turn translucent.
Wash down remaining sample particles with
condensingsulfuricacidintotheflask.
6. Suction
Duringtheentiredigestionperiodthescrubbershouldbeon.About1200mlofa15%causticsoda
isrecommendedforthewashingbottle;thisamountissufficienttoneutralizedigestiongasesof
about60digestions.
Thecoolingoffperiodaftertheliftingoftheinsertrackorthecoolingoffperiodafterturningoff
theheatingisabout30minutes;duringthistimethescrubbershouldbeworkingaswell.
7. Distillation
After the digested sample has cooled off the water steam distillation is done according to the
followingprogram:
Programparameter Vap50
Wateradditionins 9
NaOHadditionins 8
Reactiontimeins 0
Distillationtimeins 240
Steamoutputin% 100
Suctionsampleins 25
Boricacidadditionins 6s
Suctionreceiverins 25
Titration Auto
Calculation Auto
8. Titration(isdoneautomaticallywhenusingtheVap50)
34dropsofanindicatormixtureM5areaddedtothereceivingsolutionanditisthentitrated
with0.1Ntitrationacidtillthecolorchangesfromgreentogrey/violet.
If the determination of the endpoint is done with a pHmeter or a titrator, the addition of the
indicatormixtureisobsolete.
9. BlankValue
Forthedeterminationoftheblankvaluetheanalysis(digestionanddistillation)isrunjustusing
thegivenchemicals.
The consumption of those chemicals has then to be taken into account when the calculation is
done.

10. Calculation
%N=1.4007*c*(VVb)
Sampleweight(g)
c:Concentrationofthestandardacidsolution:Hydrochloricacid0.1Norc=0.1mol/l
Alternative:sulfuricacid0.1Norc=0.05mol/l
V:Consumptionofthestandardacidinml(Sample)
Vb:Consumptionofthestandardacidinml(BlankSample)

%rawprotein=%N*6.25
NitrogentoProteinConversionFactorsforVariousFoods
Product Factor
Eggormeat 6.25
Dairyproducts 6.38
Wheat 5.70
Othercerealgrainsoroilseeds 6.25
Almonds 5.18
PeanutandBrazilnuts 5.46
Othertreenutsandcoconut 5.30
Soybeanproducts 6.08
ProteinbyKjeltec
Principle
All nitrogen in the sample is converted to NH4+ by digestion with concentrated H2SO4 and H2O2 using
inorganicsaltcatalystsatahightemperature.Thesolutionisthenmadealkaline(withNaOH)andsteamis
passedthroughandtheammoniaisdistilledintoasolutionofboricacidthatcontainsanindicator(methyl
orange).Finallythedistilledammonia,nowdissolvedintheboricacid,istitratedagainst0.1MHCl.
The Kjeldahl method described above is the standard method for determining protein content. The
Kjeltecisasemiautomatedversionofthismethod.
1Digestion
WearGlovesandSafetyGlassesthroughoutthisProcedure
1. Collect two Kjeldahl digestion tubes and label them with a permanent marker close to the top.
Alwayscarrytheminatuberack(sharewithyourcolleagues).
2. Accuratelyweighout(tonearestmg)induplicateapproximately0.1gofdrysampleontoafilter
paper(W1).
3. If using a wet sample, pipette about 1 g (to nearest mg) directly into the bottom of a labelled
digestiontube.
4. Foldupthepapercontainingthedrysampleandcarefullytransferthewholeparceltoalabelled
digestiontube.
5. Placeafilterpaperinafurtherdigestiontubetoactasablank.
6. Add 2 catalyst tablets (copper sulphate + potassium sulphate) to each tube. Then add 10 cm3
concentratedH2SO4andmixbygentleswirling.Takecare.Seethedemonstratorbeforemaking
theseadditions.
7. Now add 10 cm3 H2O2 in a fume cupboard and beware of frothing. Add the peroxide slowly at
first.
8. Placethe tubes inthe digestion block and digestuntilclear(30minutes to 2 hours).Checkthat
therearenoblackcarbonparticlesvisible.

9. Allowthetubestocooluntilbarelywarmbutstillliquid.Thenaddapproximately70cm3 distilled
water.
CAREaddthewaterslowlyintheearlystages andbewareof spitting.Ifnecessarythedigestiontubes

maybeleftatthisstagebycoveringthetopofthetubeswithParafilm.
2 DistillationandTitration
a) Inturnplacethetubesintothedistillationunitandtwisttoseal.Ifthisisnotdoneproperlythetube
contentsmayleakoutandtheresultsbeuseless.
b) Closethedoorontheapparatusandstartthecycle.
c) Theexactsequencewilldependonwhichinstrumentyouareusing.
d) The apparatus will automatically add alkali to the tube and then bubble steam to distil off the
ammonia.Thisiscollectedinboricacid.TheFossKjeltecmachineusedboriccontainingindicatorbut
theBuchimachinemeasurepH.Thetitrationisautomatic.Thevolumeofacidusedisdisplayedonthe
front of the apparatus. With both instruments the results are saved and can be accessed later if
necessary.
e) When the titration is finished the tubes will be emptied automatically. Record the volume of acid
used.
f) Insertthenexttubeandcontinue.
Weightoffoodsample =W1
Volumeofacidinsampletitration=V1
Volumeofacidinblanktitration=BL
Concentrationofacid,M=0.1M
Seebelowforcalculationoftotalandpercentagevalues
TotalNitrogenandProteininthefood,measuredindrysample:
TotalNitrogen=(V1BL)x0.1x0.0014xTotalDryMatterofFood
W1
where0.1ismolarconcentrationoftheHCland0.0014isfactorforequivalenceofHCltoNH3
Toconverttoproteinmultiplybytheappropriatefactor:
x6.25formeatandgeneralprotein
x6.38formilkprotein
x5.70forcerealprotein.
NBThesearenotperfectandyoumustchooseaccordingtothemajortypeoffoodinthesample.In
mostcasesthiswillbethefirstone.
PercentageNitrogenandProtein
Inoriginal,wetsample:
Nitrogen,%=(V1BL)x0.1x0.0014x100x%DryMatter
W1100
Toconverttoproteinmultiplybytheappropriatefactor:

x6.25formeatandgeneralprotein
x6.38formilkprotein
x5.70forcerealprotein.
NBThesearenotperfectandyoumustchooseaccordingtothemajortypeoffoodinthesample.In
mostcasesthiswillbethefirstone.

Experiment6CrudeFatSoxhletApparatusMethod
Objective:
Tofindouttheamountofcrudefatinagivenfoodsample.
Principle:
A Soxhlet extractor is a piece of laboratory apparatus invented in 1879 by Franz von Soxhlet. It is a
proceduretoremovelipids(fats)fromfood.Asolventisusedtowashthesolidusingarefluxapparatus.
The sample is dried and ground and placed in a tube above the extraction solvent. When heated, the
solventevaporatesintoagas,thencoolsintoaliquidinacondenser.Itthenleaksintothesampletube.
Thiscontinuesseveralhoursuntilthelipidisremovedfromthesample.Thesolventisevaporatedoff,and
theamountoflipidisdetermined.
Apparatus
Soxhlet extraction apparatus A glass Soxhlet extraction apparatus of suitable size (100 mL) for
containing the sample and a 250 mL collection flask is required for the conventional Soxhlet
procedure. An automated extraction apparatus (Brinkmann Buchi B810 or equivalent) with
circulatingoilbathandassociatedglasswareisrequiredfortheautomatedSoxhletprocedure.
Alundum extraction thimbles Medium porosity (10 15 mm pore), sized to fit the Soxhlet
extractor.
AnalyticalbalanceSensitiveto0.1mg.
RotaryevaporatorwithvacuumandwaterbathRotaryevaporatorequippedwitha"bump"trap,
condenser,receivingvessel,andvacuumsourcesufficienttopullavacuumoflessthan150torr.
VacuumovenordryingovenVacuumovenshouldbecontrollabletoatemperatureof401C
andvacuum ofbetween 75to100torr.Ifdryingovenisusedinplaceofthevacuumoven,the
dryingovenmustbeabletomaintain452C
ReagentsandMaterials
Ethylalcohol,95%inwater(190proof),USPgrade.
Boilingchips.
Glasswool.
Buchnerfunnel.
Desiccator.
Procedure
1. DrytheSoxhletextractionthimbleat105Ctoconstantweight.Remove,cooltoroomtemperaturein
adesiccator,andweightothenearest0.1mg.
2. Carefullyaddthesampletotheextractionthimble.Donotoverfillthethimble,leaveatleasta1cm
gapbetweenthesampleandthetopofthethimble.Weighthefilledthimbletothenearest0.1mg.
Placeaplugofglasswoolontopofthesampletopreventsamplelossduringtheextraction.
Note: Samples for total solids determination (following Laboratory Analytical Procedure #001,
DeterminationofTotalSolidsandMoistureinBiomass)mustbeweighedoutatthesametimeas
the samples for the extractives determination. If this determination is done at a later time, an
errorinthecalculationoftheamountofextractiveswillbeintroduced,sincethemoisturecontent
ofabiomasssamplecanchangerapidlywhenexposedtoair.
3. Placeseveralboilingchipsintoaclean,dryreceivingflaskorbeaker.Weighthecontainer,withchips,
tothenearest0.1mgandrecordasthetareweightofthecontainer.
4. ForaconventionalSoxhletextraction(thisprocedurewasreproducedfromtheChemicalTechnologies
ResearchBranchProcedure#001c,DeterminationofExtractivesContent):
4.1. AssembletheSoxhletapparatususingatleast160mLof95%ethanol.Insertthethimbleandheat
atrefluxfor24hours.Periodicallychecktherefluxrateandadjusttheheatingratetogivefourto
fivesolventexchangesperhourintheSoxhletthimble.Approximately100120solventexchanges
arerequiredduringthe24hourperiod.

4.2. Whentheextractiontimeiscomplete,removethethimbleandcarefullytransferthesampletoa
Buchner funnel. Remove any residual solvent by vacuum filtration and wash the sample
thoroughly with 95% ethanol, collecting all of the filtrate. Allow the biomass to air dry in the
Buchnerfunnelwhileitisstillattachedtothevacuumsystem.
4.3. CombinethefiltratefromthepreviousstepandanysolventfromtheuppersectionoftheSoxhlet
apparatus with the solvent in the 250 mL flask. Place the flask on the rotary evaporator and
removethesolventundervacuum.Useawaterbathtemperatureof455Ctoheattheflask
duringevaporation.
4.4. After all of the visible solvent is removed by the rotary evaporator, place the flask in a vacuum
oven(75100torr)at401Cfor241hour.Removetheflaskatthistimeandallowtocoolto
roomtemperatureinadesiccator.Weightheflaskandrecordthistotalweighttothenearest0.1
mg.

AschematicrepresentationofaSoxhletextractor
1:Stirrerbar2:Stillpot(thestillpotshouldnotbeoverfilledandthevolumeofsolventinthestillpot
shouldbe3to4timesthevolumeofthesoxhletchamber)3:Distillationpath4:Thimble5:Solid6:Siphon
top7:Siphonexit8:Expansionadapter9:Condensor10:Coolingwaterin11:Coolingwaterout

MechanismofSoxhletextractor
Calculations
1. Calculatetheovendryweightofthesample,usingtheaveragetotalsolidscontent.

2. Calculatetheamountofextractivesinthesample,onapercentdryweightbasis.

Experiment7TotalCarbohydrates
Objective
Tofindouttheamountoftotalcarbohydratesinagivenfoodsample.
Theory
Carbohydratesaretheimportantcomponentsofstorageandstructuralmaterialsintheplants.Theyexist
as free sugars and polysaccharides. The basic units of carbohydrates are the monosaccharides which
cannot be split by hydrolysis into more simpler sugars. The carbohydrate content can be measured by
hydrolyzing the polysaccharides into simples sugars by acid hydrolysis and estimating the resultant
monosaccharides.
Principle
Carbohydratesarefirsthydrolysedintosimplesugarsusingdilutehydrochloricacid.Inhotacidicmedium
glucose is dehydrated to hydroxymethyl furfural. This compound forms with anthrone a gree colored
productwithanabsorptionmaximumat630nm.
Materials
2.5NHCl
AnthroneReagent:Dissolve200mganthronein100mLoficecold95%H2SO4.Preparefreshbefore
use.
Standard Glucose: Stock Dissolve 100mg in 100mL water. Working standard 10mL of stock
dilutedto100mLwithdistilledwater.Storerefrigeratedafteraddingafewdropsoftoluene.
Procedure
1. Weigh100mgofthesampleintoaboilingtube.
2. Hydrolyse by keeping it in boiling water bath for 3 hours with 5mL of 2.5 NHCl and cool to room
temperature.
3. Neutraliseitwithsolidsodiumcarbonateuntiltheeffervescenceceases.
4. Makeupthevolumeto100mLandcentrifuge.
5. Collectthesupernatantandtake0.5and1mLaliquotsforanalysis.
6. Prepare the standards by taking 0, 0.2, 0.4, 0.6, 0.8 and 1mL of the working standard. 0 serves as
blank.
7. Makeupthevolumeto1mLinallthetubesincludingthesampletubesbyaddingdistilledwater.
8. Thenadd4mLofanthronereagent.
9. Heatforeightminutesinaboilingwaterbath.
10. Coolrapidlyandreadthegreentodarkgreencolorat630nm.
11. DrawastandardgraphbyplottingconcentrationofthestandardontheXaxisversusabsorbanceon
theYaxis.
12. Fromthegraphcalculatetheamountofcarbohydratepresentinthesampletube.
Calculation
mgofglucose
Amountofcarbohydratepresentin100mgofthesample= Volume of test X100
sample

Note
Coolthecontentsofallthetubesonicebeforeaddingicecoldanthronereagent.


Experiment8CrudeFiber
Objective
Tofindouttheamountofcrudefiberinagivenfoodsample.
Theory
Crudefiberconsistslargelyofcelluloseandlignin(97%)plussomemineralmatter.Itrepresentsonly60%
to80%ofthecelluloseand4%to6%ofthelignin.Thecrudefibercontentiscommonlyusedasameasure
of the nutritive value of poultry and livestock feeds and also in the analysis of various foods and food
productstodetectadulteration,qualityandquantity.
Principle
Duringtheacidandsubsequentalkalitreatment,oxidativehydrolyticdegradationofthenativecellulose
and considerable degradation of lignin occur. The residue obtained after final filteration is weighed,
incinerated,cooledandweighedagain.Thelossinweightgivesthecrudefibercontent.
Materials
1. Sulphuric acid solution (0.255 0.005N) : 1.25g concentrated sulphuric acid diluted to 100mL
(concentrationmustbecheckedbytitration)
2. Sodium hydroxide solution (0.313 0.005N) : 1.25g sodium hydroxide in 100mL distilled water
(concentrationmustbechecedbytitrationwithstandardacid)
Procedure
1. Extract2gofgroundmaterialwithetherorpetroleumethertoremovefat(Initialboilingtemperature
3538Candfinaltemperature52C).iffatcontentisbelow1%,extractionmaybeomitted.
2. After extraction with ether boil 2g of dried material with 200mL of sulphuric acid for 30min with
bumpingchips.
3. Filterthroughmuslinandwashwithboilingwateruntilwashingarenolongeracidic.
4. Boilwith200mLofsodiumhydroxidesolutionfor30min.
5. Filterthroughmuslinclothagainandwashwith25mLofboiling1.25%H2SO4,three50mLportionsof
waterand25mLalcohol.
6. Removetheresidueandtransfertoashingdish(preweigheddishW1).
7. Drytheresiduefor2hat1302C.Coolthedishinadesiccatorandweigh(W2).
8. Ignitefor30minat60015C.
9. Coolinadesiccatorandreweigh(W3).
Calculation
Lossinweightonignition(W2W1)(W3W1)
%crudefiberingroundsample= x100
Weightofthesample
DeterminationofCrudeFibreUsingFibrebag(GerhardtMethod)
Objective
Todeterminefibrecontentinwholebranbreadandspinach.
Apparatus/Instrument/Chemicals/Samples
Hotplate
1LBeakerglasswithoutspoutandglasscondenserwithriffle
FibreBagCarouselfor6FibreBagswithbayonetcoupling
Bagwith100FibreBags
Glassspacer
Accessory:crucibleforincineration
DryingChamber,Temp.105C
Mufflefurnace,Temp.600C
Waterheater
Desiccator
Timeroralarmclock
Analyticalbalance
Fumecabinet
Sulfuricacidc(H2SO4)=0.13mol/l
Potassiumhydroxidesolutionc(KOH)=0.23mol/l
Petroleumether,boilingrange40to60
Waterdistilledordemineralized
SodiumHydroxidec(NaOH)=0.313mol/l
Hydrochlorideacidc(HCl)=0.1mol/l
SystemDescription:
1. Preparation
a. FibreBagisdriedat1051Cfor1hinthedryingchamber.TheweightoftheFibreBagisthevalue
Aforthebalanceprotocol.WhenstoringtheFibreBagsinadesiccatortheyonlyhavetobedried
onceandthen,canbeweighteddirectly.
b. Put 1g sample into the FibreBag and weight with 1 mg preciseness; this gives value B for the
weighing protocol. A determination of the blank value should be done parallel to the regular
analysis. The value should be 1 mg/FibreBag. The dry matter of the sample should be
determinedseparatelyandisimportantforthecalculationofthecontent(resultrelatedtothedry
matter).
c. PuttheglassspacerintotheFibreBagandinsertthebagincarousel.
d. Defattingofthesample,especiallyimportantforsampleswithafatcontentof5%:Immerse
the carousel three times in a row into 100ml 40/60 petroleum ether. By turning it as well as
moving it up and down the sample is defatted. This facilitates the washing and filtration, which
will follow. Furthermore, no crude fibre content is lost. Throw away the first petroleum ether
fractionbutthefollowingcanbereused.Afterashortdryingprocessinthefumecupboard(about
2minutes),immersethecarouselinthefirstwashingsolution.
2. WashingPhaseI(Instrumentmethod)
a. Measure360mlH2SO4=0.13mol/lintothefirstbeaker.
b. Attachhandlingtooltothecarouselandloweritgentlyintothebeaker.
c. Mixit by rotating the carousel for about 1 minute sothat the sample is entirely soaked
andmakesurethattheFibreBagisfilledwithwashingsolution.
d. Placethebeakeronthehotplate,whichhasbeenpreheatedforabout5minutes.
e. Bring ittoaboil by setting itfull (takes about35minutes); reduce thehotplatesetting
whenitstartstoboil(atabout90C).
f. Adjustthehotplatesettingtoobtainaverygentlesimmeringforabout30minutes.During
thisboilingstagethesampleshouldfloatfreelyintheFibreBag.

g. This can be helped by gently rotating the carousel with the handling tool or by softly
swirlingthebeaker.
h. After exactly 30 minutes from the boiling point remove the beaker from the hotplate.
Also, take the carousel out of the beaker using the handling tool thus draining the acid
fromtheFibreBag.
i. Washingoutoftheacid:
1. Discardtheacidandsolubleswithinthebeaker.
2. Rinsethecarouselseveraltimeswithhotwater.
3. WashingPhaseII(InstrumentMethod)
a. Measure360mlpotassiumhydroxidesolutionc(KOH)=0.23mol/lintothebeaker.
b. Attach handling tool to the carousel and lower it gently into the beaker of solution. Mix it by
rotatingthecarouselforabout1minutesothattheFibreBagisfilledcompletelywiththesolution.
c. Placeagaintheextractionbeakeronapreheatedhotplate.
d. Again, bring it to a boil by setting it full (takes about 35 minutes); reduce the hotplate setting
whenitstartstoboil.
e. Adjustthehotplatesettingtoobtainaverygentlesimmeringforabout30minutes.
f. During this boiling stage the sample should float freely in the FibreBag. This can be helped by
gentlyrotatingthecarouselwiththehandlingtoolorbysoftlyswirlingthebeaker.
g. Afterexactly30minutesfromtheboilingpointremovethebeakerfromthehotplate.
h. Also,takeoutthecarouselfromthebeakerusingthehandlingtoolthusdrainingthesolutionfrom
theFibreBags.
i. Washingoutthealkalis:
Discardthealkaliandsolublewithinthebeaker.
Rinsethecarouselseveraltimeswithhotwater.(CheckbyusingpHindicatorpaper)
Dry the FibreBags by wiping them with a paper towel or by rotating the carousel in an
emptybeaker,
4. DryingoftheFibreBags
a. TakeoutthedrainedFibreBagsofthecarouselandputintoacrucible,whichhastobepre
ashed at 600C and weighted (value F for the balance protocol). Place it into a drying
chamberovernightat105C.FibreBagafterdigestionandcrucibleisvalueC.
5. IncinerationofSamples
a. IncineratetheFibreBagsat600Cforatleast4hoursorovernight.Theresultingvapoursarenot
hazardous!
b. Aftertheincineration,weightthecrucible,whichwasleft,tocooloffinthedesiccatorandobtain
valuefortheweighingprotocol.valueD.
6. Calculation:
Thecrudefibreisthenonsolubleswhichremainafterdigestionwithacidsandalkalisminusthecontent
ofashandiscalculatedasfollows:
%CrudeFibre = ((CA)(DE))x100
B
BlankValueE =DF
Meaning:
A=MassFibreBaging
B=MassSampleweighting(hastobeadjustedaccordingtodrycontent)
C=MassCrucibleanddriedFibreBagafterdigestioning
D=MassCrucibleandAshing
E=BlankValueoftheemptyFibreBaging
F=MassCrucibleing
Results/Weighingprotocol:BlankvalueEing:................
FibreBag Sample Crude

Aing Fing Bing Cing Ding*
Number number Fibre(%)
6
*minusblankvalueEing
Comment:Asmallbeakercanalsobeusedinsteadofacrucible.
7.Validation
ThedevelopmentoftheFibreBagsanalysishasshownthatitisofvitalimportancethatcertainparameters
have to be strictly observed. Thus, it is recommended to strictly observing the times given for cooling,
heatingandboiling.
Thisalsogoesfor:
AmountofSample
ConcentrationofAcidsandAlkalis
Timesfordryingandincinerationandtemperatures
NoothersolventsthanPetroleumether
References
1. Nielsen, S.S. 1994. Introduction to the Chemical Analysis of Foods. Boston: Jones and Bartlett
Publishers,Inc.
2. Gerhadtmanualtraining.

Experiment9CutouttestforCannedFisheryProducts
Objective
Toperformthecutouttestforthegivensampleofcannedfoodproduct.

Theory
Cutouttestisdonetoevaluatethegeneralqualityofacannedfood.Inthistest,theconditionofthefood
contents, the external and internal conditions of the Can and other characteristics of the product are
examinedbycertainorganoleptic,physicalandchemicaltests.
MaterialsandEquipments
1. Cannedfood:46nos.Cans
2. Tonetester
3. Physicalbalance
4. Vacuumgauge
5. Canopener
6. Brixrefractometer
7. Scale
8. pHpapernearneutralranges
Procedure
1. IftheCansarelabeled,notetheparticularofthelabel.
2. Recordtheembossedcodemarkonthelid.
3. Observetheexternalconditionofthecanssuchasrusting,dents,physicaldamage,seamdefects
etc.
4. Testthetoneandgetanideaaboutthefillandvacuum.
5. Determinethegrossweight.
6. Measurethevacuum.
7. Cutthelidalmostcompletely,opentheobservethefoodsurfaceandinsidethelid.Measurethe
headspace.
8. Drainthecontentsfor5min.collecttheliquidinameasuringjar.
9. Notethevolume,turbidity,colour,texture,flavouretc.Alsolookforforeignmatter.
10. ObservethebottomandinsidetheCan,lookingforsettledcurds.
11. Wash,dryandweightheemptyCan.
EvaluationSheetforCutOutTest
CanNo./Paticulars 1 2 3 4 5
Product:
Code:
Manufacturer:
Dateofproduction:
DateofTesting:
Cansize&Type:

Std.Netwt./Solidwt.:
Vacuum:
GrossWeight:
Solid+Canwt:
EmptyCanwt:
Solidwt:
Liquidwt:
Netwt:
Solidwt:
Netwt:
Packwt:
Colour:
Tecture:
Flavour:
Appearance(Style):
No.ofpieces:
Salt/Sugardegree:
Turbidity:
Acidity:
PH:
Sizeofpieces:
Brokenofflakes:
Adhesion:

Curds:
Remarks:


Experiment10Detectionofadulterantsindifferentfoodproducts
Objective
Totestdifferentgivenfoodsamplesforadulteration.
Procedure
Name of Simple Method for detection of
SlNo. Adulterant Remarks
FoodArticle CommonAdulterants
A MilkandMilkProducts
i.Thelactometerreadingshallnot
ordinarilybelessthan26.
ii.Thepresenceofwatercanbeby
Lactometerismarkedin
puttingadropofmilkonapolished
degreesrangingfrom040.
slanting surface. The drop of pure
I Milk Water The test is not valid if
milkeitherorflowslowlyleavinga
skimmed milk or other
white trail behind it, whereas milk
thickeningmaterialisadded.
adulterated water will flow
immediately without leaving a
mark
Add a few drops of tincture of
Iodine or Iodine solution.
Milk Starch
Formation of blue colour indicates
theofstarch.
The lactometer reading will go
Removal of
Milk above26whilethemilkapparently
Fat
remainsthick
Boilasmallquantityofsamplewith
some water, cool and add a few
Khoa and its
II Starch dropsofIodinesolution.Formation
products
of blue colour indicates the
presenceofstarch
Boilasmallquantityofsamplewith
some water, cool and add a few
Chhana or
III Starch dropsofIodinesolution.Formation
Paneer
of blue colour indicates the of
starch.


The test is specific for
seasame oil which is
compulsorily added to
Vanaspati and Mrgarine.
Take about one tea spoon full of Some coal tar colours also
melted sample of Ghee with equal giveapositivetest.
quantity of concentrated If the test is positive i.e. red
Hydrochloric acid in a stoppered colour develops only by
Vanaspatior
IV Ghee test tube and add to it a pinch of adding strong Hydrochloric
Margarine
sugar.Shakeforoneminuteandlet acid (without adding crystals
it for five minutes. Appearance of of sugar) then the sample is
crimson colour in lower (acid) of adulteratedwithcoaltardye.
VanaspatiorMargarine. If the crimson or red colour
develops after adding and
shaking with sugar, then
aloneVanaspatiorMargarine
ispresent
The presence of mashed potatoes
Mashed and sweet potatoes in a sample of
Potatoes, Butter can easily be detected by
Sweet addingafewdropsofIodine,which
Ghee
Potatoes is brownish in colour turns to blue
and other if mashed potatoes/sweet
starches. potatoes/other starches are
present.
The test is specific for

seasame oil which is
compulsorily added to
Vanaspati and Mrgarine.
Some coal tar colours also
Take about one teaspoon full of
giveapositivetest.
melted sample of Ghee with equal

quantity of concentrated
If the test is positive i.e. red
Hydrochloric acid in a stoppered
Vanaspatior colour develops only by
V Butter test tube and add to it a pinch of
Margarine adding strong Hydrochloric
sugar.Shakeforoneminuteandlet
acid (without adding crystals
it for five minutes. Appearance of
of sugar) then the sample is
crimson colour in lower (acid) of
adulteratedwithcoaltardye.
VanaspatiorMargarine.
If the crimson or red colour
develops after adding and
shaking with sugar, then
aloneVanaspatiorMargarine
ispresent


The presence of mashed potatoes
Mashed and sweet potatoes in a sample of
Potatoes, Butter can easily be detected by
Sweet addingafewdropsofIodine,which
Butter
Potatoes is brownish in colour turns to blue
and other if mashed potatoes/sweet
starches. potatoes/other starches are
present.
Colourless (not yellowish)
Nitric acid may be used.
Take small quantity of oil in a test
Artificialcolourifpresentwill
tube. Add equal quantity of
usually be a bright shade of
concentrated Nitric acid and shake
Argemone colour, generally redorpink.
VI OilsandFats carefully. Red to reddish brown
oil Thetestmaysometimesgive
colour in lower (Acid) layer would
misleading result. The test
indicatethepresenceofArgemone
may not respond if the
oil
Argemone oil is present in
smallquantity.
Take2mloftheoilsampleandadd
an equal quantity of N12 Alcoholic
potash. Heat in boiling water bath If mineral oil is present in
OilsandFats Mineraloil (dip in boiling water) for about 15 small quantity this test may
minutes and add 10 ml of water. notbepositive.
Any turbidity shows presence of
mineraloil.
Take about one ml of the oil, add
10mlofacedifiedpetroleumether
and mix well, Add a few drops of Ifcastoroilispresentinsmall
OilsandFats Castoroil ammonium molybdate reagent. quantity, this test may be
Immediate appearance of white positive
turbidity indicates the presence of
castoroil.
B SweeteningAgents
Dissolve10gmofsampleinaglass
Chalk
I Sugar ofwater,allowtosettle,Chalkwill
powder
settledownatthebottom.
AddfewdropsofHydrochloricacid,
Washing effervescence (give off bubbles)
II PithiSugar
Soda will indicate the presence of
washingsoda.
Dissolve10gmofsampleinaglass
Chalk
PithiSugar of water, allow to settle, chalk will
powder
settledownatthebottom.
Acottonwickdippedinpurehoney
when lighted with a match stick
burns and shows the purity of
Sugar This test is only for added
III Honey honey.Ifadulterated,thepresence
solution water.
ofwaterwillnotallowthehoneyto
burn, If it does, it will produce a
crackingsound.


Metanil Extractcolourwithlukewarmfrom
Sweetmeats, yellow (a food articles. Add few drops of
Icecream non concentrated Hydrochloric acid. If
IV
and permitted magenta red colour develops the
beverages coal tar presence of metanil yellow is
colour) indicated.
i. Taste a small quantity. Saccharin

leaves a lingering sweetness on
tongueforaconsiderabletimeand
leavesabittertasteattheend.

ii.Taketwospoonsofliquidsample
or about 5 to 10 gins of solid
Sweetmeats,
samplewithlittlequantityofwater
Icecream
Saccharin in a test tube, add few drops of SeeAppendixIl.
and
Hydrochloric acid and 10 ml of
beverages
solvent ether. Shake well. Decant
theetherlayerintoatesttubeora
beaker, evaporate the ether
spontaneously. Add one drop of
water (warm) to the residue and
taste. Sweet taste will indicate the
presenceofsaccharin
Sweetmeats, Aluminium foil is whitish grey in

Icecream Aluminium colour and is readily soluble in

and foil concentrated Hydrochloric acid
beverages whilepuresilverfoilisnot,
C FoodorainsandtheirProducts
Dust,
pebble, Damaged / discoloured
stone, grains should be as low as
straw, weed possible since they may be
Wheat, Rice, seeds, Thesemaybeexaminedvisuallyto affected by fungal toxins,
Maize,Jawar, damaged see foreign matter, damaged argemone seeds, Dhatura
I
Bajra, Ghana, grain, grains, discoloured grains, insect, seeds etc. In moderately
Barleyetc. weevilled rodentcontaminationetc. excessive amount can result
grain, in risk to health, Discard the
insects, damaged undesirable grains
rodent hair beforeuse
andexcreta.


(i)Purpleblacklongersizedgrains
in Bajra show the presence of
Ergot (a
Wheat, Rice, Ergots.
fungus
Maize,Jawar, (ii) Put some grains n a glass
containing
Bajra, Ghana, tumblercontaining20percentsalt
poisonous
Barleyetc. solution Ergot floats over the
substance)
surface while sound grains settle
down
Wheat, Rice, Dhatura seeds are flat with edges
Maize,Jawar, with blackish brown colour which
Dhatura
Bajra, Ghana, can be separated out by close
Barleyetc. examination.
Wheat, Rice,
The affected wheat kernel have a
Maize,Jawar,
KarnelBunt dull appearance, blackish in colour
Bajra, Ghana,
androttenfishsmell.
Barleyetc.
Assemblemustardseedbutshowa
protrusion on close examination.
Wheat, Rice, The surface of Argemone seed is
Maize,Jawar, Argemone grainy and rough while that of

Bajra, Ghana, seed mustard seed is smooth. When
Barleyetc. Mustard seed is pressed in side, it
is yellow whereas Argemone seed
iswhite.
Rub a few grains in the palms of
Metanil two hands. Yellow would get
yellow reduced or disappear. Add a few
Sella Rice
(a non dropsofdiluteHydrochloricacidto
II (Parboiled
permitted a few rice grains mixed with little
Rice)
coal tar water, presence of pink colour
colour) indicates presence of Metanil
yellow
Takeasmallamountofsampleina
Turmeric test tube, add some water and
Sella Rice
(colouring shake.
(Parboiled SeeAppendixI
for golden Dip Boric acid paper (filter paper
Rice)
appearance) dipped in Boric acid solution) If it
turnspinkturmericispresent
(i) Khesari dal has edged type
Dal whole appearanceshowingaslantonone
III KhesariDal
andspilt side and square in appearance in
contrasttootherdaIs.
(ii)Add50mlofdiluteHydrochloric
The test is only for Khesari
acid to the sample and keep on
dal. (Metanil yellow if
Dal whole simmering water for about 15
KhesariDal present will give a similar
andspilt minutes.Thepinkcolourdeveloped
colour immediately even
indicates the presence of Khesari
withoutsimmering).
dal.


Clay, stone,
gravels, Reject if the number of
Dal whole webs, Visual examination will detect Insectsislargeoriftheodour
andspilt insects, theseadulterants. isunpleasantandtastebitter

rodent hair orgritty
andexcreta
Metanil
Take5ginsofthesamplewith5ml.
yellow (a
of water in a test tube and add a
Dal whole non
few drops of concentrated
andspilt permitted
Hydrochloric acid. A pink colour
coaltar
showspresenceoMetanilyellow
colour)
Sand. soil,
insects,
Atta, Maida webs, These can be identified by visual
IV
Suji(Rawa) lumps. examination.
rodent hair
andexcrete
By moving a magnet through the
Atta, Maida
Ironfilings sample, iron filings can be
Suji(Rawa)
separated.
Add 50 ml of dilute Hydrochloric
The test is only for Khesari
acidto10gins.ofsampleandkeep
del (Metanil yellow, if
Kheseri on simmering water for about 15
V Besan present will give a similar
Flour minutes. The pink colour, if
colour even without
developed, indicates, the presence
simmering).
ofKhesariflour
D SpicesandCondiments
Dirt, dust,
straw,
insect,
damaged
I Wholespices Thesecanbeexaminedvisually
seeds, other
seeds,
rodent hair
andexcrete
Papayaseedscanbeseparatedout
Papaya from pepperastheyare shrunken,
(a) Blackpepper
seeds oval in shape and greenish brown
orbrownishblackincolour.
Floatthesampleofblackpepperin
alcohol (rectified spirit). The black
Light black
Blackpepper pepper berries sink while the
pepper
papaya seeds and light black
pepperfloat.
Coated with Black pepper coated with mineral
Blackpepper
mineraloil oilgivesKerosenelikesmell.


Exhausted cloves can be identified
Volatile oil
by its small size and shrunken
extracted
(b) Cloves appearance. The characteristic
(exhausted
pungent of genuine cloves is less
cloves)
pronouncedinexhaustedcloves.
Mustard seeds have a smooth
surface The argemone seed have
grainy and rough surface and are
Mustard Argemone black and hence can be separated Use magnifying glass for
(c)
seed seed out by close examination. When identification.
Mustardseedispressedinsideitis
yellow while for Argemone seed it
iswhite
Add a few drops of tincture of
Iodinetestforaddedstarchis
Powdered Added IodineorIodinesolution.Indication
II not applicable for turmeric
spices starch of blue colour shows the presence
powder.
ofstarch.
Powdered Common
Tasteforadditionofcommonsalt
spices salt
Take a tea spoon full of turmeric
powder in a test tube. Add a few
dropsofconcentratedHydrochloric
acid. Instart appearance of pink
Turmeric Coloured colourwhichdisappearsondilution This test is only for Metanil
(a)
powder sawdust with water shows the presence of yellow
turmeric If the colour persists,
metanil yellow (an artificial colour)
a now permitted coal tar colour is
present.
Take a small quantity of turmeric
powder in a test tube containing
Chalk
smallquantityofwater.Add afew
powder or
Turmeric dropsofconcentratedHydrochloric
yellow soap
powder acid, effervescence (give off
stone
bubbles) will indicate the presence
powder
of chalk or yellow soap stone
powder
Take a tea spoon full of chillies
powder in a glass of water.
Coloured water extract will show
the presence of artificial colour.
Brick Any grittiness that may be felt on
Chillies powder, salt rubbing the sediment at the This test is only for earthy
(b)
powder powder or bottom of glass confirms the material.
talc.powder presence of brick powder/sand,
soapy and smooth touch of the
white residue at the bottom
indicates the presence of soap
stone.


Water soluble artificial colour can
be detected by sprinkling a small
quantity of chilies or turmeric
Water
Chillies powder on the surface of water
soluble coal
powder contained in a glass tumbler. The
tarcolour
water soluble colour will
immediately start descending in
colourstreaks
Take 2ginsof the sample in a test
tube, add few ml of solvent ether
and shake. Decant ether layer into
Oil soluble atesttubecontaining2mlofdilute
Chillies
coal tar Hydrochloric acid (1 ml HOL plus I SeealsoAppendixI
powder
colour ml of warer). Shake it, the lower
acid layer will be coloured distinct
pink to red indicating presence of
oilsolublecolour
In compounded hing due to
Soap stone Shake little portion of the sample
presence of starch, a slight
or other with water and allow to settle.
III Hing turbid solution may be
earthy Soapstoneorotherearthymaterial
produced. However, this will
material willsettledownatthebottom.
settledownafterkeeping
Genuine saffron will not break
easilylikeartificial.Artificialsaffron
ispreparedbysoakingmaizecobin
sugarandcolouringitwithcoaltar
Dried
colour. The colour dissolves in
IV Saffron tendrils of
water if artificially coloured. A bit
maizecob
of pure saffron when allowed to
dissolved in water will continue to
give its saffron colour so long as it
lasts
E MiscellaneousFoods
Stir a spoonful of sample of salt
White inaglassofwater.Thepresence
I Commonsalt powdered ofchalkwillmakesolutionwhite
Stone and other insoluble impurities
willsettledown.


Take a filter paper and spread a
few tea leaves. Sprinkle with
water to wet the filter paper. If
coaltarcolourispresentitwould
immediately stain the filter
paper. Wash the filter paper
undertapwaterandobservethe
stainsagainstlight
Exhausted

teaorturor
Spread a little slaked lime on
II Tealeaves gram dal
whiteprocelaintileorglassplate,
husk with
sprinkle a little tea dust on the
colour
lime.Red,orangeorothershades
of colour spreading on the lime
willshowthepresenceofcoaltar
colour. In case of genuine tea,
there will be only a slight
greenish yellow colour due to
chlorophyll, which appear after
sometime.
Bymovingamagnetthroughthe
Tealeaves Ironfilings sample, iron filings can be
separated
Gently sprinkle the coffee
powdersampleonthesurfaceof
waterinaglass.Thecoffeefloats
overthewaterbutchicorybegins
III Coffee Chicory to sink down within a few
seconds. The falling chicory
powder particles leave behind
them a trail of colour, due to
largeamountofcaramel
Sprinkle the suspected coffee
Tamarind powder on white filter/blotting
seeds paper and spray I per cent
Coffee powder and sodium carbonate solution on it.
date seed Tamarind and date seed powder
powder will, if present, stain blotting
paper/filterpaperred.
Supari Pan
IV Colour Colourdissolvesinwater.
Masala
Saccharin gives excessive and
Supari Pan
Saccharin lingering sweet taste and leaves
Masala
bittertasteattheend.
Chalk gives effervescence (gives
Catachu
V Chalk off bubbles) with concentrated ThistestisonlyforChalk.
powder
Hydrochloricacid


(i). On ignition, genuine silver
leaves burn away completely,
leaving glistering white spherical
ball of the same mass whereas
aluminium leaves are reduced to
ashes of dark grey blackish
colour.
(ii),Takesilverleavesintesttube,
add diluted Hydrochloric acid.
Appearance of turbidity to white
Aluminium
VI Silverleaves precipitate indicates the
leaves
presence of silver leaves.
Aluminiumleavesdonotgiveany
turbidityorprecipitate.

(iii)Takeasmallportionofmetal
leaves and add a few drops of
concentrated Nitric acid. Silver
leaves will completely dissolve
whereas aluminium leaves will
remainundissolved.
Test with the Metanil yellow
indicator paper, in case, the
VII Vinegar Mineralacid SeeAppendixI
colour changes from yellow to
pink,mineralacidispresent
AppendixI

MethodforTest
1. TestforMetanilYellow:Takesomesampleinatesttubeandaddsomeamountofwater,shakewell.
Addfewdropsofdilutedhydrochloricacid,violetcolourinthewaterportionindicatesthepresenceof
Metanilyellow.
2. TestforStarch:Boilthesamplewithsomewaterinatesttube,coolandaddafewdropsofiodine
solution.Appearanceofbluecolourindicatesthepresenceofstarch.
3. Baudouin Test : Take about one tea spoon full of melted ghee or butter with equal quantity of
concentratedhydrochloricacidinatesttubeandaddtoitapinchofsugar.Shakewellandallowto
stand.AppearanceofcrimsonredcolourshowsthepresenceofvanaspatiorMargarine.
4. Boric Acid Test for Turmeric : Take a small amount of sample in a test tube, add some water and
shake.DipBoricacidpaper.Ifitturnspink,MetanilYellow(CoalTarDye)ispresent.Boricacidpaper,
canbepreparedbydippingastripoffilterpaperintheBoricacidsolutionprovidedinthekit.Boric
Acidsolutioncanbepreparedbydissolving5gms.ofboricacidin100mlconcentratedHydrochloric
acid.
5. MetanilYellowIndicatorPaper:Metanilyellowindicatorpapercanbepreparedbydippingastripof
filter paper in metanil yellow solution (1 gm Metanil yellow coal tar colour dissolved in 100 ml of
water).
6. Oil Soluble Coal Tar Colour : Take a small quantity of chillies powder in a beaker and add 5 ml of
rectified spirit (alcohol). Dip a small piece of white silk for two minutes. Remove the silk piece and
washwithwater,Ifthesilkclothispermanentlydyed,itindicatesthepresenceofoilsolublecoaltar
colour.

AppendixII
ListofApparatusandReagentsforDevelopingaSimpleKit
Apparatus:
1. MagnifyingGlass
2. Spatula
3. Magnet
4. Forcep
5. Lactometer
6. Beaker
7. Petridishes
8. Dropper
9. ReagentBottles
10Spiritlamp
Reagents:
1. Hydrochloricacid
2. Nitricacid
3. Petroleumether
4. Solventether
5. Rectifiedsprit
6. Iodine/Tinctureofiodine
7. PotassiumHydroxide
8. AmmoniumMolybdate
9. Boricacid
10. SodiumCarbonate
11. Metanilyellowpowder
12. Testtubeordinary
13. Testtubestoppered
14. Glassrod
15. Testtubestand
16. Smallplastictraywhite
17. Porcelaintilewhite
18. GlassCylinder
19. GlassMarkingPencil
20. FilterPaper
21. Whitesilkcloth
22. Cotton

Precautionstobetaken
Caution
1. Thetestingkitshouldbekeptbeyondthereachofthechildrenasitcontainsharmfulchemicals
2. Solventetherishighlyinflammable.Keptitawayfromfire.
3. Acids are high corrosive. In case of acid burn, wash immediately with cold water containing
sodiumbicarbonate(Meethasoda)
4. Usegloveswhileperformingthetests.


Experiment11OrganochlorinePesticidesinWaterbyGasChromatgraphic(GC)Method
Objective
Tofindouttheamountoforganochlorinepesticidesinwaterbygaschromatgraphic(GC)method
Theory
Theanalyticalmethoddescribesdeterminationofaldrin,aBHC,BHC,yBHC,dBHC,chlordane,4,4
DDD,44'DDE,4,4'DDT,dieldrin,endosulfanI,endosulfanII,endosulfansulfate,endrin,endrinaldehyde,
heptachlor,andheptochlorexpoxideinwater.
Principle
Measured volume of test portion (1L) is extracted with CH2CI2 by shaking in separatory funnel or
mechanical tumbling in bottle. CH2CI2 extract is separated, dried with anhydrous Na2SO4, solvent
exchangedwithmethyltertbutylether(MTBE),andconcentratedto5ml_.Pesiticidesareseparatedand
measuredbycapillarycolumngaschromatographywithelectroncapturedetection.
Apparatus
Separatory funnel 2000 ml_, with TFE fluorocarbon stopcock and groundglass or TFE
fluorocarbonstopper.
Tumber bottle 1.7 L, with TFEfluorocarbon lined screw cap. Cut liners to fit screw cap from
sheetsandextractovernightwithmethanebeforeuse.
KudernaDanish(KD)apparatus
o (1)Concentratortube10or25ml_,graduated(Kontes5700501025or5700502525,or
equivalent). Check calibration of concentrator tube at volumes used in method. Use
groundglassstopperstopreentevaporationofextracts
o (2) Evaporation flask 500 ml_ (Kontes 5700010500, or equivalent). Attach to
concentratortubewithsprings.
Snyder columns Threeball macro (Kontes 5030000121, or equivalent); 2ball micro (Kontes
5690010219,orequivalent).
VialsGlass,510mlcapacity,withTFEfluorocarbonlinedscrewcaps.
Separatory funnel shaker capable of holding 2 L separatory funnels and shaking them with
rockingmotiontothoroughlymixfunnelcontents(EberbachCo.,Ann.Arbor,MlUSA).
TumblerCapableofholdingandtumblingbottles,(b),endoverendat30turns/min.
BoilingstonesCarborundum,No.12granules(ThomasScientificNo.1590033),Heat30min.at
400Cbeforeuse.Coolandstoreindesiccator.
WaterbathHeated,capableofcontrol2C.Usebathinhood.
BalanceAnalytical,capableofaccuratelyweighingtonearest0.0001g.
GaschromatographyTemperatureprogrammablesystemsuitableforusewithcapillarycolumns,
including syringes, analytical columns, gases, detector, and strip chart recorder. Data system is
recommended for measuring peak areas. Primary column; 30 m x 0.25 mm id DB5 fusedsilica
capillarycolumn,0.25mfilmthickness(J&WScientific,Inc.).Conformationcolumn;30mx0.25
mmidDB1701fusedsilicacapillarycolumn,0.25mfilmthickness(J&WScientificInc.)Operating
conditions;injectionvolume2l;Hecarriergasat30cm/slinearvelocity;injector250C;detector
320C;ovenprogrammedfrom60300Cat4C/min;electroncapturedetector.
Reagents
StandardsolutionsUsestandardsoftestcompoundswithpurity>96%topreparestocksolutions
at 1 mg/mL in methyl tertbutyl ether (MTBE). Commercially prepared stock standards may be
used at any concentration if they are certified by manufacturer or independent source. Store
solutions at room temperature and protect from light. Replace stock standard solutions after 2
months,orsoonerifcomparisonwithlaboratorycontrolstandardsindicatesdegradation.

InternalstandardsolutionPreparepentachloronitrobenzene(Purity>98%)stocksolutionat0.1
mg/mLinMTBE.Add5lstocksolutionto5mltestportionextracttogivefinalinternalstandard
concentrationof0.1lpentachloronitrobenzene/mlofextract.
Surrogate solution Prepare 4,4'dichlorobiphenyl (purity >96%) stock solujtion at 0.5 mg/mL in
MTBE. Add 50 l stock solution to 1 L test sample prior to extraction to produce surrogate
concentrationof25g]4,4'dichlorobiphenyl/Lintestsampleand,assumingquantitativerecovery,
5.0g/mLinextract.
Instrument performance solution Prepare individual stock standard solutions containing
chlorothalonil, chlorpyrifos, DCPA, and d BHC at 0.10 l/mL in MTBE. For assessing instrument
performance, combine 50 l chlorothalonil stock solution, 2 l chlorpyrifos stock solution, 50 l
DCPA stock solution, and 40 l d BHC stock solutionin 100 mL volumetric flask and dilute to
volumewithMTBE.
SolventsAcetone,methylenechloride,andMTBEDistilledinglassquality,orequivalent.
PhosphatebufferpH7Mix29.6mL0.1MHCIand50mL0.1Mdipotassiumhydrogenphosphate.
SodiumsulfateGranular,anhydrous,ACSgrade.Heatinshallowtrayfor>4at450Ctoremove
interferingorganicsubstances.
SodiumchlorideCrystalsACSgrade.Heatinshallowtrayfor>24hat450Ctoremoveinterfering
organicsubstances.
ReagentwaterWaterreasonablyfreeofcontaminationthatwouldpreventdeterminationofany
analyteofinterest.
PreservativeMercuricchloridesolution.10mgHgCI(ACSgrade)/mLreagentwater
SodiumthiosulfateNa2S2O3,Granular,anhydrous,ACSgrade.
Procedure
Preparationoflaboratorysamplebottles
Add1ml_preservative,toglasslaboratorysamplebottle.Ifresidualchlorineisexpectedtobepresentin
laboratorysamples,add80mgNa2S2O3tolaboratorysamplebottlebeforecollection.
LaboratorySampleCollection
Collect 1 L grab laboratory samples in glass bottles by conventional sampling practices. Since bottles
containpreservativeandNa2S2O3,donotpreinsebottleswithlaboratorysamplebeforecollection.Add
laboratorysampletobottlecontainingpreservative,seallaboratorysamplebottle,andshakevigorously1
min. Refrigerate laboratory samples at 4C from time of collection until extracted. Protect from light.
Extractlaboratorysampleswithin7daysofsamplecollection.
LaboratorySamplePreparation
Automated extraction method Add preservative, to any laboratory samples not previously preserved.
Mark water meniscus on side of laboratory sample bottle for later determination of volume. Add 50 l
surrogatestocksolution,tolaboratorysample.Ifmechnaicalseparatoryfunelshakerisused,pourentire
laboratorysampleinto2Lseparatoryfunnel.Ifmechanicaltumblerisused,pourentirelaboratorysample
intotumblerbottle.AdjustsampletopH7byadding50ml_phosphatebuffer,C.checkpHandaddH2SO4
orNaOHifnecessary.
Add100gNaCI,seal,andshaketodissolvesalt.Add300mlCH2CI2totumblerbottleorsepaatoryfunnel,
seal,andshake30storinseinnerwalls.Transferrinsetotestportioncontainedinseparatoryfunnel or
tumbler bottle, seal, and shake 10s, venting periodically. Repeat shaking and venting until! pressure
releaseisnotobservedduringventing.Resealandplacetestportioncontainerinappropriatemechanical
mixingdevice(separatoryfunnelshakerortumbler).Shakeortumbletestportionfor1h.Afterextraction,
pour contents of tumbler bottle into 2 L separatory funnel if tumbler bottle as used. Let organic layer
separate from water phase for > 10 min. If emulsion interface between layers is more than onethird
volume of solvent layer, complete phase separation mechanically. Collect CH2CI2 extract in 500 ml_
Erlenmeyer flask contaiing ca 5 g anhydrous Na2SO4. Swirl flask to dry extract; let flask sit 15 min.
Determine original laboratory sample volume by refilling laboratory sample bottle to mark and
transferringwaterto1000ml_graduatedcylinder.Recordsamplevolumetonearest5ml.

ManualextractionmethodAddpreservativetolabroatorysamplesnotpreviouslypreserved.Markwater
meniscus on side of tumbler bottle for later determination of laboratory sample volume. Add 50 l
surrogatestocksolution,tolaboratorysample,pourentirecontentsinto2Lseparatoryfunnel.Adjustto
pH7byadding50mlphosphatebuffer.CheckpHandaddH2SO4orNaOHifnecessary.Add100gNaCIto
contents,seal,andshaketodissolvesalt.Add60mlCH2CI2totumblerbottle,sealandshakebottle30sto
rinseinnerwalls.
Transferrinsetoseparatelyfunnelandextractlaboratorysamplebyvigorouslyshakingfunnelfor2min
withperiodicventingtoreleaseexcesspressure.Letorganiclayerseparatefromwaterphasefor>10min.
Ifemulsioninterfacebetweenlayersismorethan1/3volumeofsolventlayer,completephaseseparation
mechanically.CollectCH2CI2extractin500mlErlenmeyerflaskcontainingca5ganhdyrousNa2SO4.Add
second 60 ml portion of CH2CI2 to separately funnel and repeat extraction procedure a second time,
combining extracts in Erlenmeyer flask. Perform third extraction in same manner. Swirl flask to dry
extract;letflasksitfor15min.Determineoriginallaboratorysamplevolumebyrefillinglaboratorysample
bottletomarkandtransferrngwaterto1000mlgraduatedcylinder.Recordlaboratorysamplevolumeto
nearest5ml.
Extractconcentration
Assemble KD concentrator by attaching 25 ml concentrator tube to 500 ml evaporation flask. Decant
CH2CI2 extract into concentrator. Rinse remaining Na2SO4 with two 25 ml portions of CH2CI2 and decant
rinsesintoconcentrator.
Add1or2cleanboilingstonestoevaporationflaskandattachmacroSnydercolumn.Prewetcolumnby
adding ca 1 ml CH2CI2 to top. Place KD apparatus on 6575C water bath so that concentrator tube is
partially immersed in hot water and entire lower, rounded surface of flask is bathed with hot vapour.
Adjustverticalpositionofapparatusandwatertemperatureasrequiredtocompleteconcentrationin15
20 min. At proper rate of distillation, balls of column will actively chatter, but chambers will not flood.
When apparent volume of liquid reches 2 ml remove KD apparatus and let it drain and cool > 10 min.
Remove Snyder column and rinse flask and its lower joint with 12 ml MTBE, collecting rinse in
concentratortube.Add510mlMTBEandfreshboilingstone.
AttachmicroSnydercolumntoconcentratortubeandprewetcolumnbyaddingca0.5mlMTBEtotop.
Place micro KD apparatus on water bath so that concentrator tube is partially immersed in hot water.
Adjustverticalpositionofapparatusandwatertemperatureasrequiredtocompleteconcentrationin5
10min.Whenapparentvolumeofliquidreaches2ml,removeapparatusfrombathandletitdrainand
cool.
Add510mlMTBEandboilingstoneandreconcentrateto2ml.RemovemicroKDapparatusfrombath
and let it drain and cool. Remove microSnyder column, and rinse walls of concentrator tube while
adjustingvolumeto5.0mlwithMTBE.
Add 5 l internal standard stock solution, C to laboratory sample extract, seal, and shake to distribute
internalstandard.TransferextracttoappropriatesizeTFEfluorocarbonsealed,screwcapvialandstoreat
4Cuntilanalysis.A14daymaximumextractstoragetimeisrecommended.
CaliberationofGasChromatographwithElectronCaptureDetector
Table 1 summarizes retention times and detection limits observed using this method of analysis of
chlorinatedpesticides.
Table1.Relativeretentiontimesandestimatedmethoddetectionlimitsforchlorinatedpesticides
Analyte Relativeretentiontime EstimatedMDL
Primary Confirmation
Aldrin 1.18 1.12 0.0750
aBHC 0.93 0.97 0.0200
BHC 0.98 1.187 0.0700
?BHC 1.03 1.22 0.0100
dBHC 0.99 1.04 0.0150
achlordane 1.31 1.31 0.0075
?chlordane 1.28 1.29 0.0015

4,4'ODD 1.42 1.38 0.0025

4,4'DDE 1.35 1.32 0.0100
4,4DDT 1.48 1.48 0.0600
Dieldrin 1.35 1.35 0.0200
EndosulfanI 1.30 1.28 0.0150
EndosulfanII 1.40 1.45 0.0150
Endosulfansulphate 1.47 0.0150
Heptachlor 1.11 1.04
Heptachlorexpoxide 1.24 1.24 0.0150
Calculations
Theconcentration(C)inthesamplecanbecalculatedfromthefollowingequation:
C(g/L)=(A)(V)/(Vt)(Vs)
where,
A=Amountofthematerialinjected(ng)
Vi=Volumeofextractinjected(l)
Vt=Volumeofthetotalextract(l)
Vs=Volumeofthewaterextract(ml_)
Reference
AOACOfficialmethod.17thEdition.990.06(2000).


Experiment12NMethylcarbamoyloximesandNMethylcarbamatesinFinishedDrinkingWaterby
HighPerformanceLiquidChromatography(HPLC)
Objective
To find out the Nmethylcarbamoyloximes and Nmethylcarbamates in the given samples of
finisheddrinkingwaterbyhighperformanceliquidchromatography(HPLC).
Theory
The analytical method prescribes HPLC method for determination of aldicarb, aldicarb sulfone, aldicarb
sulfoxide, baygon, carbaryl, carbofuron, 3hydroxy carbofuron, methiocarb, methomyl, and oxamyl in
drinkingwater.
Principle
WatersampleisfilteredandmeasuredvolumeisdirectlyinjectedontoreversephaseLCcolumn.Analytes
areseparatedbygradientelutionchromatography.AfterelutionfromLCcolumn,analytesarehydrolyzed
with NaOH at 95C. Methylamine formed during hydrolysis is reacted with 0phthalaldehyde and 2
mercaptoethanol to form highly fluorescent derivative, which is detected by fluorescence detector.
Estimatedmethoddetectionlimitsrangefrom0.5g/Lformethomylto4.0g/Lformethiocarb;estimated
methoddetectionlimitsfor8othercompoundsrangefrom1.0to2.0g/L.
Apparatus
a. Grab sample bottle. 60ml, borosilicate glass, screwcap vials (Pierce No. 13075 meets these
specifications)andcapswithPTFEfacedsiliconesepta(PierceNo.12722meetsthesespecifications).
Beforeuse,washvialsandseptawithsoapandwater,followedby3tapwaterrinsesand3deionized
waterrinses.
b. BalanceAnalytical,capableofaccuratelyweighingtonearest0.0001g.
c. Macrofilters.47mm0.45m,nongridded,celluloseacetatefiltersforwaterphases;47mm,0.5m
nongrided,PTFEfiltersfororganicphases.
d. Microfilters.13mmstainlesssteelfilterholderand13mmdiameter,0.2mpolysterfilters(Nuclepore
No.180406meetstheserequirements).
e. Hypodermicsyringe.lOL,glass,withLuerLoktip.
f. Syringevalve.3way.
g. Syringeneedle710cmlong,17gauge,withblunttip.
h. Microsyringes.Varioussizes.
i. Solutionstoragebottles.Amberglass,1015mLcapacitywithTFEfluorocarbonlinesscrewcap.
j. LCsystem.Capableofinjecting200400laliquotsandperformingbinarylineargradientsatconstant
flowrate.Datasystemisrecommendedformeasuringpeakareas.Primarycolumn:250mmX4.6mm
id stainless steel packed with 5 m Beckman Ultrasphere ODS. Mobile phase linear gradient from
methanolwater(15+85)tomethanolin32min at1.0mL/min. Confirmationcolumn: 250mmX 4.6
mm id stainless steel packed with 5 m supelco LC1. Mobile phase linear gradient from methanol
water(15+85)tomethanolin32minat1.0mL/min.
k. Postcolumn reactor, Reactor constructed with PTFE tubing and equipped with pumps capable of
mixing0.5ml/minOPAreactionsolution,C(i),and0.5ml/minNaOH,C(f),intomobilephase.Reactor
mustcontainmixingteesandtwo1.0mldelaycoils,onethermostatedat95C.
l. Fluorscencedetector.Capableofexcitationat230nmanddetectionofemissionenergies>418nm.
Reagents
a. Standardsolutions.Usestandardsoftestcompoundswithpurity>96%topreparestock'solutionsat
1.00g/mLinmethanol.Commerciallypreparedstockstandardsmaybeusedatanyconcentrationif
theyarecertifiedbymanufacturerorindependentsource.TransferstockstandardsolutionsintoTFE
fluorocarbonsealed screwcap vials. Store at room temperature protected from light. Replace stock
standardsolutionsafter2months,orsoonerifcomparisonwithlaboratorycontrolstandardsindicates
degradation.

b. Instrumentperformancesolution.Combine20l3hydroxycarbofuranstocksolution,(a),andl.OmL
aldicarbsulfoxidestocksolution,(a)in10mLvolumetricflaskanddilutetovolumewithmethanol.
c. Reagentwater.DistilledWaterreasonablyfreeofcontaminationthatwouldpreventdeterminationof
analytes.
d. Water.LCgrade.
e. Methanol.LCgrade.Filteranddegaswithheliumbeforeuse.
f. Sodiumhydroxide.0.05M.2.0gNaOH/l.OLreagentwaterFilter,Banddegaswithheliumbeforeuse.
g. Mercaptoethanolacetonitrile. (1+1). Mix 10.0 mL 2mercaptoethanol and 10.0 mL CH3CN. Store in
borosilicateglassvialorbottlewithPTFElinedcap.(Caution:Strongodor.Storeinhood.)
h. Sodiumborate.0.05N.19.1gNa2B4O7.10H2O/1.0LreagentwaterSodiumboratedissolvescompletely
atroomtemperatureifprepareddaybeforeuse.
i. OPA reaction solution. 100 10 mg ophthaladehyde (mp 5558)/10L CH3OH Add to 1 L 0.05M
Na2B4O7solution,(h).mix,filter,B(c),anddegaswithhelium.Add100l2mercaptoethanol,(g),and
mix.Preparesolutionfreshdaily.
j. Helium.Fordegassingsolutionsandsolvents
k. Monochloroacetic acid buffer. pH 3. mix 156 mL 2.5M monochloroacetic acid and lOOmL 2.5M
potassiumacetate.
l. Sodiumthiosulfate.Na2S2O3.granular,anhydrous.ACSgrade.
m. Bufferedreagentwater.MixlOmLmonochloroaceticacidbuffer,(k),and1Lreagentwater,(c).
n. Internal standard solution. Prepare 4bromo3.5 dimethylphenyl Nmethylcarbamate (BDMC) (Purity
98%,AldrichChemicalCo.)stocksolutionat0.1mg/mLinmethanol.
Procedure
PreparationsampleBottles
Add1.8mLmonochloroaceticacidbuffer,C(k),tosamplebottle,B(a).ifresidualchlorineisexpected,add
5mgNa2S2O3tobottlebeforesamplecollection.
Samplecollection
Collect 60mL grab samples in glass bottles by conventional sampling practices. Because bottles contain
bufferandNa2S2O3,donotprerinsewithsamplebeforecollection.Addsampletobottle,seal,andshake
vigorously 1 min. Refrigrate samples at 4 from time of collection until storage. Store at 10 until
analyzed.Analyzesampleswithin28daysofcollection.
SamplePreparation
AdjustpHofsampleorstandardtopH30.2byadding1.5mL2.5Mmonochloroaceticacidbuffer,C(k),
to50mLsample.ThisstepshouldnotbenecessaryifsamplepHwasadjustedduringsamplecollection.Fill
50mLvolumetricflasktomarkwithsample.Add5linternalstandardstocksolution,C(n),tothe50mLof
sample (final concentration 10g/L). affix 3 way valve to l0l syringe. Place clean filter in filter holder,
B(d), and affix filter holder and 710 cm syringe needle to syringe valve. Rinse needle and syringe with
reagentwater,C(C).Prewetfilterbypassing5mLreagentwaterthroughfilter.Emptysyringeandcheck
for leakes. Draw lOmL sample into syringe and expel through filter. Draw another lOmL sample into
syringe, expelthrough filter,andcollectlast 5mL for analysis. Rinse syringe with reagent water. Discard
filter.Inject400lofcollectedsampleintoLCsystemunderconditionsinB(j).
CalibrationofLCsystem
Table1presentsretentiontimesandestimatedmethoddetectionof10carbamatepesticides.
Analyte Retentiontime EDL

Aldicarb 21.4 1.6
Aldicarbsulfone 12.2 2.0
Aldicarbsulfoxide 17.5 2.0
Baygon 23.4 1.0
Carbaryl 25.4 2.0

Analyte Retentiontime EDL

Carboftiron 24.4 1.5
3hydroxycarboruron 19.0 2.0
Methiocarb 28.6 4.0
Methomyl 14.8 0.50
Oxamyl 14.6 2.0
Calculation
C(g/L)=(A)(V)/(Vt)(Vs)
where,
A=Amountofthematerialinjected(ng)
V=Volumeofextractinjected(l)
Vt=Volumeofthetotalextract(l)
Vs=Volumeofthewaterextract(ml)

Experiment13AcesulfameKDetectionandDeterminationinSweets
Objective
TofindouttheAcesulfameKinthegivensampleofsweets.
Method
QualitativeMethod(ThinlayerChromatographicdetectionofacesulfamesaccharinandcyclamate)
Apparatus:
UVlamp(360nm);
Ionexchangeresin:AmberliteLA2.
Reagents:
Polyamide
2,7dichlorofluorosein
Bromine
Formicacid
Ammonia5%
Xylol
Propanol
Methanol.
Procedure:
Extractthesweetener from acidified food productwithwaterortake acidifiedaqueous extract and
pass through the ionexchanger and wash with water. Elute the sweeteners with dilute ammonia
solution.Evaporatetheammonicalsolutionundervacuumtodrynessandtakeuptheresiduein1ml
of 50% methanol (alternatively extract these sweeteners from acidfied sample, pH 0.6, with ethyl
acetateanduseconcentratedethylacetateforTLC).
Apply210lofsamplesolutionalongwithstandardsonTLCplatescoatedwithpolyamide.Develop
theplatetoabout15cmheightwithadevelopingsolventconsistingofxylol:npropanol:formicacid
(5:5:1).Drytheplatesinacurrentofairandsprywith0.2%solutionofdichlorofluoreseinandafter
being dried, examine under UV light. To identify the spots in day light, place the plate in chamber
containingbromineandthenexposetoammoniavapour.Spotsappearonareddishbackground.
Quantitativemethod:(Analysisofacesulfamebyhighpressureliquidchromatography)

Apparatus:
Beaker,pipette,flasks,
HPLCinstrumentofanysuitablemakewithaUVdetectorat227nm,
column;LichrosorbRP18(10m).

Reagents:
(i) Mobile phase: methanol : water ( 10 : 90) : Adjust this mixture to 0.01M using
tetrabutylammoniumsulphate,
(ii) Standardsolutionofacesulfame:0.1mg/mlindistilledwater.

OperatingConditions:
(1)Pressure:160bar(2)Flowrate:40ml/hr(3)Temperature(ambient)(4)SampleVolume:1020l.

Preparationofsample:
(a)Liquidsamplessuchasjuices:filterthrough0.45mfilter(MilliporeInc.)andinject1020l.

(b) Solid samples: Stir 10 gm of sample vigorously with 100 ml distilled water for 30 minutes and
centrifuge.Passanaliquotofthissolutionthrough0.45mfilter,discardthefirstfewdropsoffiltrate
andcollectthefiltrateandchromatograph.

Procedure:
Injectstandardsolutionrangingfrom520landrecordthepeaks.Calculatethepeakareaanddraw
acalibrationgraphusinggofsubstancevspeakarea.Injectsamplessolutionrangingfrom1020l
andrecordthepeakareafor sample. Calculatetheacesulfamecontentofthesamplefromitspeak
areaandthecalibrationgraph.
Determination of Acesulphame K, Aspartame and Saccharin by High Performance Liquid

Chromatography
Principle
Extractionofsamplewithwateroreluent,ifnecessary,clarificationonsolidphaseextractioncolumn
orwithCarrezreagent,chromatographyatanHPLCreversedphasecolumnandspectrophotometrical
determinationatawavelengthof220nm.
Reagents
1. AcetonitrileforHPLC
2. MethanolforHPLC
3. Pot.dihydrogenphosphate
4. Dipotassiumhydrogenphosphate
5. Tetrabutylammoniumhydrogensulphate
6. Phosphoricacid85%(w/w)
7. Phosphoric acid 5% (w/w). Carefully pipette 6 ml of Phosphoric acid at (6) above into a 100 ml
volumetricflaskwhichalreadycontains80mlwater.Dilutetomarkwithwater.
8. Hydrochloricacid25%(w/w)
9. CarrezSolution1Dissolve15gmPotassiumhexacynoferrate(K4[Fe(CN)6]3H2O)inwaterand
diluteto100ml
10. CarrezSolution2Dissolve30gmZincSulphate(ZnSO47H2O)inwateranddiluteto100ml
11. PhosphateBuffersolutionII(KH2PO40.0125mol/litre,pH=3.5.Dissolve1.70gmpotassium
dihydrogenphosphatein800mlofwaterina1000mlbeaker.adjusttopH3.5withphosphoric
acid.Transferthesolutionstoa1000mlvol.flaskanddilutetomarkwithwater.
12. PhosphateBuffersolutionIIIpH6.5Dissolve5.46gmofpotassiumdihydrogenphosphatein500
mlwaterina1000mlbeaker.adjusttopH6.5withdrydipotassiumhydrogenphosphate.Addto
thesolution3.4gmoftetrabutylammoniumhydrogensulphateandstirtodissolve.AdjustthepH
to6.5byadditionofmoredipotassiumhydrogenphosphate.Add250mlofmethanolandadjust
thepHto4.0bydropwiseadditionofHCl(8).Transferthissolutionintoa1000volumetricflask
anddilutetothemarkwithwater.
13. MobilePhasePhosphatebufferandeitheracetnitrileormethanol.Filterthephosphatebuffer
used for the mobile phase and either acetonitrile or methanol separately through suitable
membrane filters, of pore size 0.45 m and de gas for 5 minutes in an ultrasonic bath. Add
carefullymeasuredtherequiredamountsofphosphatebufferandacetonitrileasgiveninA,5and
mix.Preparethemobilephasefreshlyonthedayofuse
14. Control solution containing acesulphame K ,Sodiumsaccharinand aspartame (andoptionally
diketopiperazine, aspartylphenyl alanine, phenylalanine,caffeine, benzoic acid, theobromine,
hydroxylmethylfurfural,andvanillin)Ina100mlvolumetricflask,weightothenearest0.1mg,30
mgofacesulphameK,20mgofsodiumsaccharin,220mgofaspartame(andoptionally60mg
caffeine,100mgbenzoicacid,100mgvanillin,10mgdiketopiperazine,10mgofphenylalanine,
10 mg of aspartylphenylalanine, 20 mg of hydroxyl methyl furfural and 70 mg of theobromine).
Dissolveanddilutetomarkwithwater.Pipette20mlofthesolutionintoa100mlvol.flaskand
dilutetomarkwithwater.

15. Stock solution Weigh to the nearst0.1 mg , 100 mg of Acesulphame K, 100 mg of sodium
saccharin and 100 mg of aspartame in the same 100 ml volumetric flask. Dissolve and dilute to
markwithwater.
16. StandardSolution1Pipette10mlofthestocksolution(15)intoa100mlvol.flaskanddiluteto
markwithwater.
17. Standardsolution2Pipette5mlofthestocksolutionintoa100mlvolflaskanddilutetomark
withwater.
18. StandardSolution3Pipette1mlofthestocksolutionintoa100mlvolflaskanddilutetomark
withwater.
Apparatus
1. AnalyticalBalance
2. Highspeedblenderorhomogenizer
3. Volumetricflasks100,250,500and1000mlcapacity.
4. Beaker1000ml
5. Pipettes1,5,10,20,25,100ml
6. Micropipette1000uL
7. Graduatedcylinder1000ml
8. Funnel
9. Flutedfilterpapers,mediumfastqualitative
10. Waterbath
11. Ultrasonicbath
12. Centrifuge
13. Degassingsystem
14. Membranefiltersporesize0.45umorsmallerwithfilterholdersandsuitablesyringe.
15. Solidphaseextractioncolumn
16. HighPerformanceLiquidChromatographequippedwithUVdetector(capableofoperatingata
wavelength of 220 nm, preferably a diode array detector) and equipped with recorder or
integratorwhichallowsmeasurementofpeakheightsandpeakareas)
17. Column,ReversephaseaRPCStationaryphaseof5um,alengthof250mm,internaldia4mm,
aguardcolumn,RPC18(optionalbutstronglyrecommendedforallsolidsamplematerials.
Performance criteria for suitable analytical columns is the baseline resolution of the respective
analyte.

Procedure

Preparationofsampletestsolution

(1) Clearliquidproducts(lemonades,cola,beverages)
Dilute 20 ml of the liquid in a 100 ml volumetric flask with water. Filter the solution through a
membranefilterofporesize0.2umbeforeinjection.

(2) Cloudyliquidsamples(juices,flavouredmilkdrimks)
Dilute20mlsamplewith50mlwaterina100mlvolumetricflask.Add2mlCarrezsolution1,mixand
2mlofCarrezsolution2,dilutetomarkwithwaterandfilterthroughaflutedfilterpaper.Passthe
filterate through a membranefilterof pore size0.45umbefore injection. To make allowancefor the
volumeofanyprecipitate,ifthefatfreeinsolublematterintheinitialsamplemassexceedsapprox3
gm,itisadvisabletocentrifugetheclarifiedsolutionfor10minutesbeforefilteringitquantitatively
intoa100mlvolumetricflask.Washthesettledmattertwicewithwaterandcentrifugeagain,collect
eachofthesupernatantinthe100mlvolflaskandthendilutethesolutiontomarkwithwater.

(3) Jams,preserves,marmaladeandrelatedproducts
Weigh to the nearest 1 mg, 20 gm of homogenized sample in a 100 ml vol. flask, add about 60 ml
waterandplacetheflaskin anultrasonicbath at40C for 20 minutes. Thetemperatureshouldnot

exceed40Csinceaspartamecangetdegraded.Cooltoroomtemp.Add2mlCarrezsolution1,mix
followedby2mlcarrezsolution2.Shakevigorouslyandallowtostandfor10minutes.Dilutetomark
with water. Filter the solution through a fluted filter paper. Pass the filterate through a membrane
filter of pore size 0.45 um before injection. To make allowance for any precipitate, if the fat free
insoluble matter in the initial mass exceeds 3 gm, it is advisable to centrifuge the clarified sample
solutionfor10minutesat1400r.p.mbeforefilteringitquantitativelyinto100mlvolflask.Washwith
waterandcentrifugeagainasincaseofcloudyliquidsamples.

(4) Semisolidandsolidproducts
Weigh1020gmofthoroughlyhomogenizedsampleina100mlvolflask.Addabout50mlwater
andplacethevolflaskinanultrasonicbathat400Cfor20minutes.Cooltoroomtemperature,add2
ml Carrez solution 1 , mix and add 2 ml of Carrez solution 2, dilute to mark with water and filter
throughaflutedfilterpaper.Incaseofverycomplexmatrices,additionalpurificationusingthesolid
phase extraction column may be necessary to protect the separating column, since colouring,
flavouringandfatcannotbeseparatedbyCarrezsolution.Inthiscaseadd2mlofclarifiedfilterateto
thecartridge,previouslyactivatedwith3mlofmethanoland20mlwaterandelutewithabout20ml
ofmobilephase.Passthefiltratethroughamembranefilterofporesize0.45umbeforeinjection.To
makeallowanceforthevolumeofanyprecipitatefollowprocedurementionedabove.

(5) CustardPowder
Weigh10gmsampleina500volumetricflask.Addabout400mlofwaterandproceedasdescribed
above.Add6mlofCarrezsolution1and2forclarification
Identification
Identify the intense sweeteners by comparing the retention times of the analyte concerned in the
sample solution with that of the standard substance or by simultaneous injection of the standard
solutionandthesamplesolution.
Determination
Integrate the peak areas or determine the peak heights and compare the results with the
corresponding values for the standard substance with the nearest peak area / height or use a
calibrationgraph.Checkthelinearityofthecalibrationgraph.
Chromatographicconditions
Typereversedphase(RP)
Stationary phase and column lengths spherical particles of 3 um, for column lengths of 100mm,
upto10umforcolumnlengthsof300mm
Internaldiameter4.0mm
Guardcolumnrecommended(optional)bondapakC18orpartisilODS3,orsuperspher60RPselect
B
Flowrate0.8ml/minto1ml/min
Injectionvolume10lupto20l
DetectionPhotometrical(UV)atawavelengthof
217nmforaspartame
227forAcesulphameK
265forsaccharin
220nmforallintensesweetenersifthedetectordoesnotallowawavelengthswitchinonerun.
MobilephaseThefollowingproportionsaresatisfactory
SolutionAphosphatebuffer=0.02mol/lpH=4.3
SolutionB=phosphatebuffer=0.0125mol/lpH=3.5
SolutionCphosphatebuffer=pH6.5
SolutionDacetonitrile
SolutionEMethanol
(a)solutionA+solutionD(90+10v/v)

(b)solutionB+solutionD(80=20v/v)
(c)solutionB+solutionD(85+15v/v)
(d)solutionB+solutionD(90+10v/v)
(e)solutionB+solutionD(95+5v/v)
(f)solutionB+solutionD(98+2v/v)
(g)solutionC+solutionE(90+10v/v)
Calculation
Calculatethemassfractionwexpressedinmg/kgormassconcentrationpinmg/litreoftheintense
sweetenerasunder
worp=(A1xV1xm1xF1x1000)/(A2xV2xm0)
WhereA1=peakareaoftheintensesweetenerconcernedobtainedwithsampletestsolution
A2=peakareaoftheintensesweetenerconcernedobtainedwiththestandardtestsolution
V1=totalvolumeofsampletestsolutioninmilliliters
V2=totalvolumeofthestandardtestsolutioninmilliliters
m1=massoftheintensesweetenerconcernedinstandardtestsolution
m0=initialsamplemassingmsormls
F1=dilutionfactorforthepurificationmethodused(e.gColumnClarification=10,Carrezclarification
=1

Experiment14SensoryEvaluationGeneralConcepts
Objective
Toexplorethegeneralconceptsofsensoryevaluationinclassactivities.
Theory
Whatissensoryevaluation?
Sensory evaluation is a scientific discipline that analyses and measures human responses to the
compositionoffoodanddrink,e.g.appearance,touch,odour,texture,temperatureandtaste.Itprovides
an ideal opportunity to analyst to evaluate and give feedback on their dishes, test products and
experimentaldesigns.
SensoryAnalysisintheFoodIndustry
Sensory analysis testing is used considerably in the food industry for product development, recipe
modificationandtheevaluationofproducts.Italsoplaysakeyroleinqualitycontrolandinthemarketing
of products. Many types of sensory analysis tests have been devised to fulfil a number of specific
objectives.Thesetestsaregroupedintothreecategories.
CategoriesofSensoryAnalysisTests
1. PreferenceTests
2. DifferenceTests
3. DescriptiveTests
Withineachcategorytherearevarioussensoryanalysisteststhatcanbecarriedout.Thetestswhichare
suitableforuseintheclassroomareincludedbelow.
1. PreferenceTests
Preferencetestssupplyinformationaboutwhetherpeoplelikeordislikeaproduct.Preferencetestsare
usedinthefoodindustrytodetermine:
ifconsumerslikeaproduct
ifoneproductispreferredoveranother
ifconsumersintendtouseaproduct.
Preferencetestsareoftenreferredtoasacceptanceorconsumertests.
PreferenceTestsSuitableforClassroomUse
PairedPreferenceTest
HedonicRatingScale
FoodActionRatingTest
PreferenceRankingTest
2. DifferenceTests
Difference tests are used to detect small differences in foods. Difference tests are used in the food
industrytoanswersomeofthefollowingquestions:
doesadifferenceexist?
wouldpeoplenoticethedifference?
howwouldyoudescribethedifference?
Differencetestsaresometimescalleddiscriminationtests.
DifferenceTestsSuitableforClassroomUse

SimpleDifferencePairedComparisonTest
DirectionalPairedComparisonTest
TriangleTest
DuoTrioTest
3. DescriptiveTests
Descriptivetestsareusedtodescribetheperceivedsensorycharacteristicsofproducts.Descriptivetests
canbeusedinthefoodindustrytoanswersomeofthefollowingquestions:
whatdoestheproducttastelike?
whatareitsperceivedsensorycharacteristics/attributes?
howdoesachangeinprocessing/packaging/storageconditionsaffectthesensoryqualityof
thisproduct?
DescriptiveTestsSuitableforClassroomUse
DescriptiveRankingTest
DescriptiveRatingTestoneproduct
DescriptiveRatingTesttwoproducts
UsesofSensoryAnalysisintheFoodIndustry
Sensoryanalysistestinghasbecomeanintegralpartofthefoodindustry.Ithasmanydifferentpurposes.
Itcanbeusedto:
evaluatearangeofexistingfoodproducts
analyseatestkitchensampleforimprovement
gaugeconsumerresponsetoaproduct
checkthatafinalproductmeetsitsoriginalspecifications
evaluatedifferencesinsimilarproducts
analysespecificattributese.g.shortnessinbiscuits.
Itisimportantthatthetestchosenshouldsuittheparticularpurpose.Veryoftenmorethanonetypeof
testwillhavetobecarriedoutonproducts.Companiesoftendevelopproductstotastelikeanother,e.g.
ownlabelfoodstotastelikethebrandleader.Ifafoodisdesignedtotastelikeanother,thenadifference
testisused.Thismaybefollowedbyapreferencetesttofindouttheacceptabilityofthenewproduct
amongconsumers.
Preferencetestscanbeusedtoresearchhowacompanysproductcomparestothatofitscompetitors.A
rankingtestmaybedoneandiftheresultsofthisarefavourabletothecompany,thismaybepresented
toretailerstopersuadethemtoallocatemoreshelfspacetothecompanysproduct.
Cost and quality are important factors in the food industry. A company may consider changing the
supplierofoneoftheingredientsinaproductforeconomicreasons.Itisimportantthatconsumersdo
notdetectthattheproducthasbeenchangedinanyway.Inthiscasethecompanymayuseapanelof
trainedtesterstocarryoutdifferenceteststodetermineifthetesterscandetectadifferencefromthe
originalproduct.
Companiesmaycontemplatechangestotheirexistingproductbasedonconsumerdemande.g.healthy
eating,byreplacingsaltwithalowsodiumalternative.Itisimportantthatfoodcompaniesareattentiveto
thedemandsoftheconsumerinordertoretaintheirmarketshare.Asaresult,sensoryanalysistestingis
ongoinginindustry.
Food companies may carry out their own sensory analysis testing or they may contract a specialist
company to do this for them. Results of sensory analysis tests are calculated either manually or by
computerprogramme.Statisticalanalysisiscarriedouttoensurereliabilityandvalidityoftheresults.

ProductDevelopmentintheFoodIndustry
Increased competition in the food industry has led to the development of new products. There is also
constantreappraisalofexistingproducts,leadingtoimprovementsine.g.flavourorpackaging.
Productdevelopmentmayinvolve:
Makingacompletelynewfoodproductdevelopingideasforanewproductbydrawingupthe
productprofilee.g.shape,size
Modifyinganexistingfoodproductmakingchangestoanoriginalrecipee.g.addingorremoving
aningredienttoimproveflavourorchangingthesizeorshapeofaproduct
Matchinganexistingfoodproductcopyingotherpopularbrandedproductsofsimilartypes.
StagesofProductDevelopment
Theprocessofproductdevelopmentinvolvesaseriesofcomplexstages,requiringthecombinedtalents
ofmanyspecialiststomakeitsuccessful.Themainstagesareoutlinedbelow.
1. Developmentofideas
Ideasaredevelopedforthenewproductandaspecificationisproduced.
2. Testingofideasonasmallscale
Ideasaretestedonasmallscale.Researchiscarriedouttoformulateanumberofrecipesandspecifythe
ingredientstobeused.Severalversionsaremade,alteringingredientsorprocesses.Inotherwordsthe
productsareprototyped,oftenbyaprofessionalcheforfoodconsultant.
3. Productmodification
Trainedtestersevaluatetheproductbeingdevelopedtoensurethatitdisplaysthedesiredcharacteristics.
Therecipemayneedtobemodifiedandfurthertestingiscarriedout.
4. Consumertesting
Theproductisthentestedtodetermineconsumeracceptability.
5. Finalproductspecification
Thefinalproductspecificationisthenagreeddetailingtheexactingredientsandmethodsofproduction.
6. Largescaleproductiontrial
Foodscientistsworktogetherinapilotplanttodeterminethebestmethodofproducinglargequantities
oftheproduct.
7. Largescaleproduction
The product is then produced on a large scale. This is done under controlled conditions to maintain
consistentproductquality.
8. Packagingandlabelling
Appropriatepackagingischosenbearinginmindshelflifeconsiderations.Labellingisdesignedtomeet
legalrequirements.
9. Productlaunch
Theproductisadvertisedandthenlaunched.
Sensoryanalysistestingiscarriedoutatmanystagesastheproductisbeingdeveloped.
SensoryAnalysisinClassRoom
Intheclass,sensoryanalysisisusedforthefollowingactivities:

evaluationofproducts/dishes
productdevelopmentandrecipemodification.
EvaluationofProducts
Whenevaluatingproductsstudentsmay:
identifyanddescribethecharacteristicsofafoode.g.flavour,appearance,shape
ratethecharacteristicsofafoode.g.colourverypaletoverydark
comparefoodse.g.intermsoftaste.
ProductDevelopmentandRecipeModification
Inproductdevelopmentandrecipemodificationstudentsmay:
drawupaproductprofilethatdescribesthedesiredcharacteristicsofafoodorproduct
designaproducte.g.arangeofbiscuitsforacakesale
modifyarecipetosuitthedesigne.g.changetheingredients,flavour,shape
compareamodifiedrecipewithanoriginalrecipe,orwithasimilarbrandedproduct
testtheendproductforacceptabilitye.g.amongtheirclassmates
assessqualityassurancee.g.shelflifeissuessuchashowtheabsorptionoffatfromafoodor
theretentionofmoisturemayaffectpackaging.
TastingandTestingintheClassroom
Beforecarryingoutsensoryanalysistestsasrequiredforanassignment,itwouldbeimportanttohavea
certainamountofpreparationdone.Thiscouldinclude:
thebasictheoryofsensoryanalysis
avocabularyofdescriptiveterms
guidelinesfortestingintheclassroom
procedurefortestsappropriatetotheassignment.

GuidelinesforTestingintheClassroom
WheretoTest
Ideally testing takes place in special testing booths. However, a quiet area of the classroom, with
adequatelightandventilation,couldbeused.Ensureadequatespacebetweentesters.
TestingSession
Itisveryimportantthatsilenceismaintainedthroughoutthesessionandthatstudentsshouldnotdiscuss
theirresults.Keepthetestingsessionshorttoavoidfatigue.
Timing
Midmorning is the best time before any aromas of cooking fill the air. If this is not possible, try and
ensurethattheroomisodourfreeandwellventilated.Testersshouldnoteatstronglyflavouredfoodin
thethirtyminutesimmediatelypriortothetest.
NumberinGroup
This will depend on the size of the class. When arranging tests in class, it is important that the people
involvedintestingthefoodsamplesshouldnotbeinvolvedinthecodingandarrangingofsamples,orin
thecollatingofresultsforthesesamples.Thisisbecausetheywillbefamiliarwiththecodedsampleson
thetraysthattheyhavesetup.
SpecialDietaryConditions
Takeintoaccountstudentswithspecialdietaryconditionse.g.acoeliacshouldnotteststarchyfoods.
Hygiene
Ensurethatthegeneralrulesofhygieneapplyforthehandlingofallfoodsamples.
Equipment
Thesizeandshapeofcontainersshouldbestandard.Polystyrenecups,paperplatesandplasticspoons
are useful equipment for testing food. These could either be disposable or a designated set of plastic
equipment.
QuantityofSample
The samples presented should be sufficient in amount. Ensure that all samples are uniform in colour,
shapeandsize.
Temperature
Itisimportantthatallsamplespresentedareatthesametemperature.
CodingofSamples
Oneofthemostimportantthingsabouttestingismakingsurethattestersareunawareoftheidentityof
products, which means that coding is necessary. This is an essential part of every test carried out.
Samples can be coded with geometric shapes e.g. triangle, square, circle. They can also be coded with
threedigitnumbers.Codesusedshouldnotinduceanybiasamongtesters.Forexampleifsamplesare
coded A and B, testers might feel that sample A is the better sample. A record should be kept of the
arrangementofsamplespresentedtoeachtester.
NumberofSamples
Inindustrylargenumbersoftestersareusedandtestsarerepeatedanumberoftimestoensurevalidity
andreliability.Thisisnotrequiredintheclassroomsituation.
SettingofTrays

Ensure that a glass of water and / or dry crackers are included on trays in order to cleanse the palate
betweenthetastingofsamples.

TastingandTestingWordBank
Appearance Flavour Smell Texture Sound

Appetising Acidic Aromatic Adhesive Bubbling
Attractive Bitter Astringent Airy Crackly
Brittle Bland Burnt Brittle Crunchy
Burnt Burnt Coffee Bubbly Grating
Cellular Buttery Fermented Chewy Fizzy
Clear Creamy Floral Coarse Percolating
Cloudy Fatty Fresh Cohesive Sizzling
Cold Herby Fruity Cold Snapping
Colourful Hot Musty Crisp
Colourless Musty Pungent Crumbly
Creamy Piquant Rancid Crunchy
Crumbly Salty Roasted Crystalline
Dark Sharp Smokey Dry
Dry Smokey Sour Effervescent
Foamy Sour Spicy Elastic
Fresh Spicy Stale Fibrous
Grained Stale Fine
Greasy Sweet Firm
Healthy Tangy Fizzy
Moist Tart Flaky
Mottled Tasty Flat
Opaque Tasteless Foamy
Pale Undercooked Grainy
Powdery Watery Greasy
Shiny Gritty
Slimy Hard
Smooth Juicy
Soggy Lumpy
Sticky Moist
Thick Mushy
Translucent Powdery
Watery Rubbery
Slimy
Smooth
Soft
Spongy
Sticky
Tender
Tough
Watery
TrainingforTastingandTestinginSensoryAnalysis
Panelsoftrainedtestersareusedinthefoodindustrytotasteandtestfoodproducts.Inordertotrain
studentsintastingandtesting,particularlyinthedescriptiveanddifferencetests,itwouldbeuseful,asis
doneinindustry,todoafewpreliminarytestswiththem.

Themostusefultestswouldbethetasteidentificationtestandtasteintensitytests.


Experiment14SensoryEvaluationTasteIdentificationTest
Aim:Toencouragestudentstodevelopanawarenessofthebasictastessweet,sour,saltandbitter.
Materialsrequiredperstudent
4cups.Codethecups1,2,3and4.
1glassofwater(torinsemouth)
Procedure
1.Preparethecupsasfollows:
Cup1 250mlwater+1teasp.sugar. Sweet
Cup2 250mlwater+teasp.salt Salt
Cup3 250mlwater+2teasp.lemonjuice... Sour
Cup4 250mlwater+100mltonicwater(decarbonated)... Bitter
2.Instructstudentstofollowinstructionsonscorecard.
Scorecard
TasteIdentificationTest

TraynumberName.

You are presented with 4 samples of solutions which represent the basic taste sensations of
sweet,sour,saltandbitter.
Startinginanyorder,chooseacup,takeasipfromit,holditinyourmouthfor10secondsand
notethetaste.
Proceedthroughtheothersamplesinasimilarmanner,rinsingyourmouthbetweeneach.
Fillinthetasteidentifiedineachcase.

Correct
Solution TasteIdentified
Incorrect

1
3.Collectscorecardsandcorrectresults.
Templates
Scorecard

TraynumberName.

notethetaste.

Correct
Incorrect

1
Scorecard

TraynumberName.

notethetaste.

Correct
Incorrect

1

Experiment15SensoryEvaluationTasteIntensityTests
Tasteintensitytestsareusedtoencouragestudentstodiscriminatebetweenconcentrationsofparticular
tastes.
TasteIntensityTest

Testersarepresentedwiththreecodedsamples
Testers must indicate the order of the samples in terms of intensity of the specified
taste
SaltIntensityTest
Aim:Todiscriminatebetweenthetasteintensityofthreesolutions.
Materialsrequiredbasedonsixtesters
6trays
6glassesofwater
18containers
6scorecards
Procedure
1.Code18containersasfollows:
6containerswithsymbol
2.Placethefollowingsolutionsintocodedcontainers:
6coded250mlwater
6coded250mlwater+teasp.salt
6coded250mlwater+1teasp.salt
Watercanbeslightlywarmtoaidthedissolvingofsalt.
3.Setuptraysnumbered16.Placeonecontainerwithsymbol,onewithsymbolandonewith
symboloneachtray.
4.Instructtesterstofollowinstructionsonscorecard.
Scorecard
SaltIntensityTest

TraynumberName.

Startinginanyorder,chooseacup,takeasipfromit,holditinyourmouthforatleast10seconds
andnotethetaste.
Pleaseindicatetheorderofthesamplesintermsoftasteintensityi.e.1fortheweakestsolution
and3forthestrongestsolution.

________________________

5.Collectandcorrectresults.

Sourandsweetintensitytestscanbecarriedoutinasimilarmanner.
Sour 250mlwater
250mlwater+1teasp.lemonjuice
250mlwater+1tablesp.lemonjuice
Sweet 250mlwater
250mlwater+1teasp.sugar
250mlwater+1tablesp.sugar
Scorecard
SourIntensityTest

TraynumberName.

andnotethetaste.

________________________

Scorecard
SweetIntensityTest

TraynumberName.

andnotethetastefromit.
Proceedthroughallthreesamplesinasimilarmanner,rinsingyourmouthoutbetweeneach.

________________________

Templates
Scorecard
SaltIntensityTest

TraynumberName...

andnotethetaste.

________________________

Scorecard
SourIntensityTest

TraynumberName.

andnotethetaste.

________________________

Scorecard
SweetIntensityTest

TraynumberName.

andnotethetastefromit.
Proceedthroughallthreesamplesinasimilarmanner,rinsingyourmouthoutbetweeneach.

________________________


Experiment16SensoryEvaluationPreferenceTestPairedPreferenceTest
Apairedpreferencetestisusedtoexpressapreferencebetweentwoproducts.

Testerispresentedwithtwocodedsamples
Testerdecideswhichonetheyprefer

ProcedureforaPairedPreferenceTest
Aim:TodeterminewhichoftwosamplesofShortbreadispreferredbytesters.
6trays
6glassesofwater
12containers
6samplesoffoodAStewartsShortbread
6samplesoffoodBGordonsShortbread
6scorecards
6recordsheets
Procedure
2.Arrangeshortbreadincontainers:
6codedStewartsShortbread
6codedGordonsShortbread
3.Setuptraysnumbered16.Placeonecontainerwithsymbolandonewithsymboloneach
tray.
Codedsamples
Tray1Scorecard

Scorecard
TraynumberName..
Infrontofyouaretwocodedsamples.Tasteeachsampleandtickthesamplethatyouprefer.
5.Collectscorecardsandtransferresultsontorecordsheet.
6.Countresults.
7.Revealcodesandpresentresults.
RecordSheet
FoodProduct Ticks TotalNumberofTicks

4
Stewarts

2
Gordons
In the above record sheet four testers ticked Stewarts Shortbread coded and two testers ticked
GordonsShortbreadcoded.ThereforethepreferredproductwasStewartsShortbread.
8.Evaluateresults.

Templates
Scorecard
TraynumberName..
Scorecard
TraynumberName..
Scorecard
TraynumberName..
Templates
RecordSheet
RecordSheet
RecordSheet
RecordSheet

Experiment17SensoryEvaluationPreferenceTestHedonicRatingScale
HedonicRatingScale
Ratingtestscanbeusedtofindouthowmuchtesterslikeordislikeaproduct.Thetermhedonicmeans
havingtodowithpleasuresoratingscalestodowithlikesordislikesarecalledhedonicratingscales.
HedonicRatingScale

Testerispresentedwithoneormorecodedsamples
Testerindicatestheirdegreeoflikingforeachproduct

ProcedureforaHedonicRatingScale
Aim:TodeterminetheextentoflikingforeachofthreebrandsofDigestiveBiscuits.
Materialsrequiredbasedonfivetesters
5trays
5glassesofwater
15containers
5samplesfoodAWhitePackDigestiveBiscuits
5samplesfoodBRedPackDigestiveBiscuits
5samplesfoodCBluePackDigestiveBiscuits
5scorecards
5recordsheets
Procedure
1.Code15foodcontainersasfollows:
2.Arrangebiscuitsincontainers:
5containerscodedWhitePackDigestiveBiscuits
5containerscodedRedPackDigestiveBiscuits
5containerscodedBluePackDigestiveBiscuits
symboloneachtray.
Codedsamples
Tray1Scorecard
Scorecard
HedonicRatingScale

TraynumberName..

Infrontofyouarethreecodedsamples.Tasteeachsampleandtickhowmuchyoulikeordislike
it.

Likealot __________________

Likealittle __________________

Neitherlikenordislike__________________

Dislikealittle __________________

Dislikealot __________________

6.Calculateresults.
Tocalculatethescoreforeachproductassigneachdescriptorascorevalue:
likealot=5 likealittle=4 neitherlikenordislike=3 dislikealittle=2 dislikealot=1.
Workouttheaveragescoreforeachproduct.
RecordSheet
HedonicRatingScale

FoodProductWhitePackDigestiveBiscuits
FoodProductRedPackDigestiveBiscuits
FoodProductBluePackDigestiveBiscuits

ScoreValueAssigned:
likealot=5likealittle=4neitherlikenordislike=3dislikealittle=2dislikealot=1

Tester AverageScore
Total
FoodProduct (total scorenumberof
1 2 3 4 5 Score
testers)
23=4.6
5pts 5pts 4pts 4pts 5pts 5points
5
18=3.6
5pts 2pts 3pts 5pts 3pts 4points
5
8=1.6
1pt 1pt 2pts 3pts 1pt 2points
5
ProductWhitePackDigestiveBiscuitswerelikedalot(5pts).
ProductRedPackDigestiveBiscuitswerelikedalittle(4pts).
ProductBluePackDigestiveBiscuitsweredislikedalittle(2pts).

ThereforeWhitePackDigestiveBiscuitswasthepreferredproduct.
8.Evaluateresults.
Templates
Scorecard
HedonicRatingScale

TraynumberName..

it.

Likealot __________________

Likealittle __________________



Dislikealot __________________

Scorecard
HedonicRatingScale

TraynumberName..

it.

Likealot __________________

Likealittle __________________



Dislikealot __________________

Templates
RecordSheet
HedonicRatingScale

FoodProduct___________________________

FoodProduct___________________________

FoodProduct___________________________

ScoreValueAssigned:

Tester AverageScore
Total
1 2 3 4 5 Score
testers)
RecordSheet
HedonicRatingScale

FoodProduct___________________________

FoodProduct___________________________

FoodProduct___________________________

ScoreValueAssigned:

Tester AverageScore
Total
1 2 3 4 5 Score
testers)

Experiment18SensoryEvaluationPreferenceTestFoodAction/AttitudeRatingTest
FoodAction/AttitudeRatingTest
In a food action rating test a scale is used to determine the attitudes of testers to a food. It is often
referredtoasaFACTScale.Thetestcanbecarriedoutononeormoresamplesoffood.
Testerispresentedwithoneormorefoodsamples
Testerindicatestheirattitudetothefoodonpreparedscales
ProcedureforaFoodActionRatingTest
Aim:TodeterminetheattitudeoftesterstoonetypeofCheddarCheese.
6trays
6glassesofwater
6containers
6samplesofCheddarCheese
6scorecards
6recordsheets
Procedure
1.Placethecheesesamplesinsixcontainers.
2.Setuptraysnumbered16.Placeonecontaineroneachtray.
Foodsample
Tray1Scorecard
Scorecard

TraynumberName.

Youarepresentedwithafoodsample.
Pleasetastethesampleandticktheboxthatbestdescribeshowyoufeelaboutit.

IwouldeatthiseveryopportunitythatIhad
Iwouldeatthisveryoften
Ilikethisandwouldeatitnowandthen
Iwouldeatthisifavailablebutwouldnotgooutofmyway
Idontlikethisbutwouldeatitonoccasion
Iwouldhardlyevereatthis
Iwouldeatthisonlyifforcedto

RecordSheet
Action TotalTicks
5.Countresults.
6.Presentresults.
Inthiscase,threetesterswouldeatthisfoodnowandthen;twowouldeatitveryoftenandone
wouldeatitifavailablebutwouldnotgooutoftheirwaytoeatit.
7.Evaluateresults.
Templates
Scorecard

TraynumberName.



Scorecard

TraynumberName.



Templates
RecordSheet
Action TotalTicks
RecordSheet
Action TotalTicks

Experiment19SensoryEvaluationPreferenceTestPreferenceRankingTest
Preferencerankingtestsareusedtorankfoodsinorderofpreference.Theyareusedwhentwoormore
samplesarebeingtested.Thenumberofsamplesusedisdependentonthetestersattentionspanand
memory.Thetesterisaskedtoassignanordertothesamplesaccordingtohis/herpreference.Ranking
testsdonotdeterminethedegreeofliking/dislikingforeachofthesamples.

Testerispresentedwithanumberofcodedsamples
Testerrankssamplesinorderofpreference

ProcedureforaPreferenceRankingTest
Aim:TodeterminewhichofthreedifferentbrandsofChocolateYoghurtispreferredbytesters.
6trays
6glassesofwater
18containers
6samplesoffoodAYellowPackChocolateYoghurt
6samplesoffoodBRedPackChocolateYoghurt
6samplesoffoodCBluePackChocolateYoghurt
6scorecards
6recordsheets
Procedure
2.Arrangeyoghurtincontainers:
6codedYellowPackChocolateYoghurt
6codedRedPackChocolateYoghurt
6codedBluePackChocolateYoghurt
symboloneachtray.
Codedsamples
Tray1Scorecard
Scorecard

TraynumberName.

Infrontofyouarethreecodedsamples.Tasteeachsample.

Pleaseindicateyourpreferencebyplacing:
1stchoicebesidethesamplethatyouprefermost
2ndchoicebesideyournextpreference
3rdchoicebesidetheoneyouleastprefer.

____________________________________________________________

6.Calculateresults.
Tocalculatetheresultsassigneachchoiceascorevalue:
1stchoicegive3points
2ndchoicegive2points
3rdchoicegive1point
Calculate the score for each product by multiplying the number of ticks in each box by the score value
assigned to that choice as in the record sheet below. The order of preference is determined from the
scorei.e.theproductwiththehighestscoreisthepreferredproduct.
RecordSheet

FoodProductYellowPackChocolateYoghurt

FoodProductRedPackChocolateYoghurt

FoodProductBluePackChocolateYoghurt

Foreachtesterplaceatickintheboxthatcorrespondstotheirchoiceforthatproduct.
ScoreValueAssigned:
3rdchoicegive1point
FoodProduct 1stchoice 2ndchoice 3rdchoice Score RankOrder


2x3=6 2x2=4 2x1=2 12points 2nd

2x3=6 3x2=6 1x1=1 13points 1st

2x3=6 1x2=2 3x1=3 11points 3rd
IntheabovecaseRedPackChocolateYoghurtwasthegrouppreference,followedbyYellowPack.Blue
PackChocolateYoghurtwastheleastpreferredofthethreesamples.
8.Evaluateresults.
Templates
Scorecard

TraynumberName.



____________________________________________________________

Scorecard

TraynumberName.



____________________________________________________________

Templates
RecordSheet

FoodProduct____________________

FoodProduct____________________

FoodProduct____________________

ScoreValueAssigned:
3rdchoicegive1point
RecordSheet

FoodProduct____________________

FoodProduct____________________

FoodProduct____________________

ScoreValueAssigned:
3rdchoicegive1point

Experiment20SensoryEvaluationDifferenceTestPairedComparisonTest
PairedComparisonTest
Thistestisusefulwhencomparingtwotypesofthesamefoode.g.bakedbeans,yoghurt,juiceetc.
Therearetwodifferenttypesofpairedcomparisontest:
Simple difference paired comparison test are the samples
different?
Directionalpairedcomparisontestwhichsampleissweeter/
saltier?

Testerisaskedifthereisadifferencebetweenthesamples

ProcedureforaSimpleDifferencePairedComparisonTest
Aim:TodetermineiftesterscandetectadifferencebetweentwosamplesofBakedBeans.
6trays
6glassesofwater
12containers
6samplesoffoodABakedBeans
6samplesoffoodBReducedSugarBakedBeans
6scorecards
6recordsheets
Procedure
2.Setuptraysnumbered16.Placeonecontainerwithsymbolandonecontainerwithsymbol
oneachtray.
Codedsamples
Tray1Scorecard
3.Arrangebeansincontainers.Itisimportanttopresentthecodedsamplesinrandomorderoneach
tray.Thesamplesonthetrayscanbethesameordifferent.Apossiblepresentationorderforsixtesters
isillustratedbelow.
PresentationOrderforSixTrays
Tray AB Tray BA Tray AB

1 2 3

Tray BA Tray AB Tray BA

4 5 6
ABakedBeans
BReducedSugarBakedBeans
Scorecard

TraynumberName.

Youarepresentedwithtwocodedsamples.Pleasetastethesamplesintheordergiven.
Canyoudetectadifferencebetweenthesamples?

Yes_______________No_______________

Note:thetasteorderisalwaysspecifiedonthescorecardforasimpledifferencepairedcomparisontest
toensurerandomtastingoffood.
5. Collectscorecardsandtransferresultsontorecordsheet.
RecordSheet

FoodProductA:BakedBeans

FoodProductB:ReducedSugarBakedBeans

When recording results, transfer responses from the scorecards by indicating whether testers
answeredYesorNo.Tickthosethatarecorrect.
Response IfCorrect
Tester1
Foodproduct A B Yes
Code
Tester2

Foodproduct B A No
Code
Tester3
Foodproduct A B Yes
Code
Tester4
Foodproduct B A Yes
Code
Tester5
Foodsample A B Yes
Code
Tester6
Foodproduct B A No
Code

Totalnumberofcorrectresponses 4

6.Countthecorrectresponses.
Asyoucansee,fourtesterscorrectlydetectedadifferencebetweenthetwosamples.
8.Evaluateresults.
Templates
Scorecard

TraynumberName.


Yes_______________No_______________

Scorecard

TraynumberName.


Yes_______________No_______________

Scorecard

TraynumberName.


Yes_______________No_______________

Templates
RecordSheet

FoodProductA:____________________

FoodProductB:____________________

When recording results, transfer responses from the scorecards by indicating whether testers
answeredYesorNo.Tickthosethatarecorrect.
Response IfCorrect
Tester1
Foodproduct A B
Code
Tester2
Foodproduct B A
Code
Tester3
Foodproduct A B
Code
Tester4
Foodproduct B A
Code
Tester5
Foodsample A B
Code
Tester6
Foodproduct B A
Code

Totalnumberofcorrectresponses

Experiment21SensoryEvaluationDifferenceTest
PairedComparisonTest
Thistestisusefulwhencomparingtwotypesofthesamefoode.g.bakedbeans,yoghurt,juiceetc.
Therearetwodifferenttypesofpairedcomparisontest:
Simple difference paired comparison test are the samples
different?
Directionalpairedcomparisontestwhichsampleissweeter/
saltier?

Testerispresentwithtwocodedsamples
Testerisaskedtodeterminewhichofthesampleshasagreaterdegreeofintensityin
termsofaparticularcharacteristic

ProcedureforaDirectionalPairedComparisonTest
Aim:TodeterminewhichoftwosamplesofOrangeJuiceissweeter.
6trays
6glassesofwater
12containers
6samplesoffoodAUnsweetenedOrangeJuice
6samplesoffoodBSweetenedOrangeJuice
6scorecards
6recordsheets
Procedure
2.Setuptraysnumbered16.Placeonecontainerwithsymbolandonewithsymbolon
eachtray.
Codedsamples
Scorecard
Tray1
3.Arrangeorangejuiceincontainers.Itisimportanttopresentthecodedsamplesinrandomorderon
eachtray.Apossiblepresentationorderforsixtestersisillustratedbelow.
Tray AB Tray BA Tray AB

1 2 3

Tray BA Tray AB Tray BA

4 5 6
AUnsweetenedOrangeJuice
BSweetenedOrangeJuice
4. Instructtesterstofollowinstructionsonscorecard.
Scorecard

TraynumberName.

Infrontofyouaretwocodedsamples.
Startingwiththesampleontheleft,tasteeachsampleandcirclethesamplethatissweeter.
Youmustmakeachoice.Youmayretasteasoftenasyouwish.

Note: the taste order is always specified on the scorecard for a directional paired comparison test to
ensure
randomtastingoffood.
RecordSheet

FoodProductA:UnsweetenedOrangeJuice

FoodProductB:SweetenedOrangeJuice

When recording results, circle the letter that corresponds with the symbol selected on the
scorecard.Tickthecorrectresponses.
IfCorrect
Tester1
Foodproduct A B
Code

Tester2
Foodproduct B A
Code
Tester3
Foodproduct A B
Code
Tester4
Foodproduct B A
Code
Tester5
Foodproduct A B
Code
Tester6
Foodproduct B A
Code
6.Countcorrectresponses.
FourpeoplecorrectlyidentifiedtheSweetenedOrangeJuiceasbeingthesweetersample.
8.Evaluateresults.

Templates
Scorecard

TraynumberName.

Startingwiththesampleontheleft,tasteeachsampleandcirclethesamplethatis_____________

Scorecard

TraynumberName.

Startingwiththesampleontheleft,tasteeachsampleandcirclethesamplethatis____________

Scorecard

TraynumberName.

Startingwiththesampleontheleft,tasteeachsampleandcirclethesamplethatis_____________

Template
RecordSheet

FoodProductA:__________________________

FoodProductB:__________________________

When recording results, circle the letter that corresponds with the symbol selected on the
scorecard.Tickthecorrectresponses.
IfCorrect
Tester1
Foodproduct A B
Code
Tester2
Foodproduct B A
Code
Tester3
Foodproduct A B
Code
Tester4
Foodproduct B A
Code
Tester5
Foodproduct A B
Code
Tester6
Foodproduct B A
Code



Experiment21SensoryEvaluationDifferenceTestTriangleTest
TriangleTest
Thetriangletestisusedtoseeifthereisadetectabledifferencebetweentwosimilarproducts.
TriangleTest

Testerispresentedwiththreecodedsamples
Twosamplesarethesame,oneisdifferent
Testerisaskedtoidentifythesamplethatisdifferent

ProcedureforaTriangleTest
Aim:TofindoutifthereisadetectabledifferencebetweentwobrandsofJaffaCakes.
6trays
6glassesofwater
18containers
9samplesoffoodAWhitePackJaffaCakes
9samplesoffoodBBluePackJaffaCakes
6scorecards
6recordsheets
Procedure
2.Setuptraysnumbered16.Placeonecontainerwithsymbol,onewithsymbolandone
withsymboloneachtray.
Codedsamples
Scorecard
Tray1
3.Arrangethefoodsamplesineachcontainer.InatriangletestBalancedPresentationOrderis
important.Thismeansthat:
(i) everypossiblecombinationofsamplesshouldbepresented

(ii) eachfoodbeingtestedisofferedanequalnumberoftimes.
In a triangle test there are six possible combinations that can be presented. The six combinations are
illustratedbelow.
BalancedPresentationOrderforSixTrays
Tray ABA Tray AAB Tray BBA

1 2 3

Tray BAB Tray ABB Tray BAA

4 5 6
AWhitePackJaffaCakes
BBluePackJaffaCakes
Ontray1:
foodcontainercontainsWhitePackJaffaCakes
foodcontainercontainsBluePackJaffaCakes
foodcontainercontainsWhitePackJaffaCakes.
Bysettingupsixtraysonecanensurethateverypossiblecombinationofsamplesisoffered.Thesamples
arealsopresentedinrandomorderandnotestergetsthesamplespresentedinthesamesequence.Each
food sample is offered an equal number of times i.e. nine times, so a balanced presentation order is
achieved. It is important to note that the codes on each tray remain the same; it is the food in the
containerthatchangeseachtime.
Scorecard
TriangleTest
TraynumberName.
Infrontofyouarethreecodedsamples,twoarethesameandoneisdifferent.
Startingfromtheleft,tastethesamplesandcircletheonethatisdifferentfromtheothertwo.
Youmayretastethesamples.Youmustmakeachoice.
Note:thetasteorderisalwaysspecifiedonthescorecardforatriangletesttoensurerandomtastingof
foods.
5.Collectscorecardsandtransferresultsontotherecordsheet.
RecordSheet
TriangleTest

FoodProductA:WhitePackJaffaCakes

FoodProductB:BluePackJaffaCakes

When recording the results circle the letter that corresponds with the symbol selected on
eachscorecard.
Ticktheappropriatecolumnifthetestercorrectlyidentifiedthesamplethatwasdifferent.
If
Tester1
Foodproduct A B A
Code
Tester2
Foodproduct A A B
Code
Tester3
Foodproduct B B A
Code
Tester4
Foodproduct B A B
Code
Tester5
Foodproduct A B B
Code
Tester6
Foodproduct B A A
Code
Inthiscasefiveoutofsixpeoplecorrectlyidentifiedthesamplethatwasdifferent.
8.Evaluateresults.
Templates
Scorecard
TriangleTest
TraynumberName.
Scorecard
TriangleTest
TraynumberName.
Scorecard
TriangleTest
TraynumberName.
Template
RecordSheet
TriangleTest

FoodProductA:__________________________

FoodProductB:__________________________

Whenrecordingtheresultscircletheletterthatcorrespondswiththesymbolselectedoneach
scorecard.
Ticktheappropriatecolumnifthetestercorrectlyidentifiedthesamplethatwasdifferent.

If
Tester1
Foodproduct A B A
Code
Tester2
Foodproduct A A B
Code
Tester3
Foodproduct B B A
Code
Tester4
Foodproduct B A B
Code
Tester5
Foodproduct A B B
Code
Tester6
Foodproduct B A A
Code



Experiment22SensoryEvaluationDifferenceTestDuoTrioTest
DuoTrioTest
Theduotriotestisanalternativetothetriangletest.Thistestisusedinthefoodindustrywhenchanges
are contemplated in a product currently available. This test is particularly useful when the product
concernedhasanintenseodourortaste.
DuoTrioTest

Testerispresentedwiththreesamples
Twosamplesarecodedandoneisidentifiedasthereference.Inindustrythereference
is
normallytheproductcurrentlybeingmanufactured
Testerisaskedtoidentifythesamplethatisdifferentfromthereference

ProcedureforaDuoTrioTest
Aim:TofindoutifthereisadetectabledifferenceintastebetweenanOriginalGarlicDiprecipeanda
ModifiedGarlicDiprecipe.
6trays
6glassesofwater
18containers
12samplesoffoodAOriginalGarlicDiprecipe
6samplesoffoodBModifiedGarlicDiprecipe
6scorecards
6recordsheets
Procedure
6containerswithsymbolR
2.Setuptraysnumbered16.PlaceonecontainerwithsymbolR,onewithsymbolandone
withsymboloneachtray.
Codedsamples
Tray1Scorecard
3.Arrangethefoodinthecontainersoneachtray.Itisimportanttopresentthefoodinarandomorder

oneachtray.Apossiblepresentationorderforsixtestersisillustratedbelow.
Tray AAB Tray ABA Tray AAB

1 R 2 R 3 R

Tray ABA Tray AAB Tray ABA

4 R 5 R 6 R
ROriginalrecipe
AOriginalrecipe
BModifiedrecipe
Thecodesoneachtrayremainthesame.Itisthefoodinthecontainerthatchangeseachtime.Thefood
placed inthecontainercodedRisalwaysthereferencefood, inthiscasetheOriginalGarlicDiprecipe.
Onlythefoodsinthecontainerscodedandchange.
Scorecard
DuoTrioTest

TraynumberName.

Youarepresentedwiththreesamples,onemarkedRandtwoothercodedsamples.
Startingfromtheleft,tastetheRsamplefollowedbythetwocodedsamplesintheordergiven.
CirclethesamplethatisdifferentfromR.Youmayretastethesamples.Youmustmakeachoice.

R


RecordSheet
DuoTrioTest
FoodProductA:OriginalGarlicDip

FoodProductB:ModifiedGarlicDip

When recording the results circle the letter that corresponds with the symbol selected on each
scorecard.
Ticktheappropriatecolumnifthetestercorrectlyidentifiedthesamplethatwasdifferentfrom
R.
IfCorrect
Tester1
Foodproduct A A B
Code R
Tester2
Foodproduct A B A
Code R
Tester3
Foodproduct A A B
Code R
Tester4
Foodproduct A B A
Code R
Tester5
Foodproduct A A B
Code R
Tester6
Foodproduct A B A
Code R
Inthiscasefourtesterscouldidentifythesamplethatwasdifferentfromthereference.
8.Evaluateresults.

Templates
Scorecard
DuoTrioTest

TraynumberName.


R

Scorecard
DuoTrioTest

TraynumberName.


R

Scorecard
DuoTrioTest

TraynumberName.


R

Template
RecordSheet
DuoTrioTest

FoodProductA:______________________

FoodProductB:______________________

When recording the results circle the letter that corresponds with the symbol selected on each
scorecard.
Ticktheappropriatecolumnifthetestercorrectlyidentifiedthesamplethatwasdifferentfrom
R.

IfCorrect
Tester1
Foodproduct A A B
Code R
Tester2
Foodproduct A B A
Code R
Tester3
Foodproduct A A B
Code R
Tester4
Foodproduct A B A
Code R
Tester5
Foodproduct A A B
Code R
Tester6
Foodproduct A B A
Code R



Experiment23SensoryEvaluationDescriptiveTestDescriptiveRankingTest
A descriptive ranking test is used to rank foods in order of intensity of a specific sensory attribute. A
sensory attribute is the term used to describe a key characteristic of a food product e.g. sweetness,
saltiness,aroma/flavour,rancidity,viscosity.

Testerispresentedwithanumberofcodedsamples
Testerrankssamplesinorderofintensityofspecifiedattribute/s

ProcedureforaDescriptiveRankingTest
Aim:ToranktheperceivedcreaminessofthreetypesofMilk.
6trays
6glassesofwater
18containers
6samplesoffoodAFullFatMilk
6samplesoffoodBLowFatMilk
6samplesoffoodCSkimmedMilk
6scorecards
6recordsheets
Procedure
2.Arrangemilkincontainers:
6codedFullFatMilk
6codedLowFatMilk
6codedSkimmedMilk
symboloneachtray.
Codedsamples
Tray1Scorecard
4.Instructthetesterstofollowinstructionsonscorecard.

Scorecard

TraynumberName.

Pleaserankthesamplesinorderofcreaminessbyplacing:
1stchoicebesidethesamplethatyouconsidertobethecreamiest
2ndchoicebesidethenextcreamiest
3rdchoicebesidetheleastcreamy.

____________________________________________________________

6.Calculateresults.
Tocalculatetheresultsassigneachchoiceascorevalue:
3rdchoicegive1point.
Calculatethescoreforeachproductbymultiplyingthenumberofticksineachboxbythevalueassigned
tothatchoiceasintherecordsheetbelow.Therankorderisdeterminedfromthescore.
RecordSheet
FoodProductFullFatMilk
FoodProductLowFatMilk
FoodProductSkimmedmilk
ScoreValueAssigned:
3rdchoicegive1point

2x3=6 3x2=6 1x1=1 13points 1st

2x3=6 2x2=4 2x1=2 12points 2nd

2x3=6 1x2=2 3x1=3 11points 3rd
Intheaboveexampletheproductcodedwasperceivedtobethecreamiestmilk.Thiswasthe
FullFatMilk.
8.Evaluateresults.

Templates
Scorecard

TraynumberName.

Pleaserankthesamplesinorderof__________________byplacing:
1stchoicebesidethesamplethatyouconsidertobethe__________________
2ndchoicebesidethenext__________________
3rdchoicebesidetheleast__________________

____________________________________________________________

Scorecard

TraynumberName.


____________________________________________________________

Scorecard

TraynumberName.


____________________________________________________________

Templates
RecordSheet
FoodProduct____________________

FoodProduct____________________

FoodProduct____________________

ScoreValueAssigned:
3rdchoicegive1point

RecordSheet
FoodProduct____________________

FoodProduct____________________

FoodProduct____________________

ScoreValueAssigned:
3rdchoicegive1point


Experiment24SensoryEvaluationDescriptiveTestDescriptiveRatingTestsLineScales
DescriptiveRatingTests
Descriptiveratingtestsareusedtoevaluateandratepreselectedsensoryattributesinafood.Asensory
attributeisthetermusedtodescribeakeycharacteristicofafoodproduct.
Theattributescanberatedonlinescalesorstardiagrams.
A sensoryprofile is a written description ofthe sensoryattributesof a food. This iscompiled from the
ratingsobtainedfortheselectedattributes.
DescriptiveRatingTestprofilingoneproductusinglinescales.
DescriptiveRatingTest

Testerispresentedwithonefoodsample
Testerisaskedtoratetheintensityofthepreselectedattributesforthesample

ProcedureforaDescriptiveRatingTest
Aim:TocompileasensoryprofileofonetypeofTomatoSoupusingfourpreselectedattributes.
6trays
6glassesofwater
6containers
6samplesofTomatoSoup
6scorecards
6recordsheets
Procedure
1. Agree four attributes to be rated. This is an important stage in the test and can be done by
brainstorming/discussionwithintheclassgroup.Eachstudentshouldhaveaclearunderstandingofthe
meaningofeachchosenattribute.
Thefourattributesagreedforthetomatosoupare:
aroma
colour(tomatocolour)
flavour(tomatoflavour)
sweetness(sweet).
2.Labelscorecardandrecordsheetwithagreedattributes.
3.Setuptraysnumbered16.Placeasampleofsouponeachtray.
Soupsample
Scorecard
Tray1
Scorecard

TraynumberName.

YouarepresentedwithasampleofTomatoSoup.
Please evaluate and rate the sample for each attribute and mark the number that best describes
yourchoiceontheaccompanyinglinescale.

1=veryweak2=weak3=neitherweaknorstrong4=strong5=verystrong

Attributes

Aroma

12345

TomatoFlavour

12345

TomatoColour

12345

Sweetness

12345

6.Calculatetheaveragescoreforeachattribute.
RecordSheet

FoodProduct:TomatoSoup

Attributes
Fillinattributesselectedforprofile
Tomato Tomato
Aroma Sweetness
Flavour Colour
Tester1
5 3 3 2
Resultsfromscorecard
Tester2
4 3 2 3
Tester3
4 5 1 3
Tester4
5 4 2 3
Tester5
3 4 2 2
Tester6
3 3 2 1
Totalscore 24 22 12 14
Averagescore
4 3.6 2 2.3
(totalscorenumberoftesters)
7.Presentresultsbyplottingtheaveragescoreforeachattributeontothelinescales.Itisacceptable
toroundoffaveragescorestothenearestwholenumber.
PresentationofResults

TraynumberName.

FoodProduct:TomatoSoup

Pleaseplottheaveragescoreforeachattributeontheaccompanyinglinescales.



Attributes

Aroma

12345

TomatoFlavour

12345

TomatoColour

12345

Sweetness

12345

8.Compileasensoryprofileofthetomatosoupbasedonthegroupresult.Foraccurateprofilingitis
importanttousetheappropriatewordsforeachnumberonthescales.
ProfileofTomatoSoup
Thissouphasastrongaromaandastrongtomatoflavour.However,ithasaweaktomatocolour
andaweaksweettaste.
9.Evaluateresults.
Template
Scorecard

TraynumberName.

Youarepresentedwithasampleof____________________

Please evaluate and rate the sample for each attribute and mark the number that best describes
yourchoiceontheaccompanyinglinescale.


Attributes

..

12345

..

12345

..

12345

..

12345

Template
RecordSheet

FoodProduct:____________________
Attributes

Tester1

Tester2

Tester3

Tester4

Tester5

Tester6

Totalscore
Averagescore

(totalscorenumberoftesters)
Template

TraynumberName.

FoodProduct:____________________

Pleaseplottheaveragescoreforeachattributeontheaccompanyinglinescales.


Attributes

..

12345

..

12345

..

12345

..

12345


Experiment25SensoryEvaluationDescriptiveTestDescriptiveRatingTestStarDiagrams
DescriptiveRatingTests
Descriptiveratingtestsareusedtoevaluateandratepreselectedsensoryattributesinafood.A
sensoryattributeisthetermusedtodescribeakeycharacteristicofafoodproduct.
Theattributescanberatedonlinescalesorstardiagrams.
A sensoryprofile is a written description ofthe sensoryattributesof a food. This iscompiled from the
ratingsobtainedfortheselectedattributes.
DescriptiveRatingTestprofilingtwoproductsusingstardiagrams.
Testerisaskedtoratetheintensityofthepreselectedattributesforeachsample
ProcedureforaDescriptiveRatingTestusingtwoproducts
Aim:TocompileasensoryprofileofeachoftwotypesofFruitSconesusingsixpreselectedattributes.
Materialsrequiredbasedonfourtesters
4trays
4glassesofwater
8containers
4samplesofFruitSconeA
4samplesofFruitSconeB
4scorecards
4recordsheets
Procedure
1.Agreesixattributes.Thisisanimportantstageinthetestandcanbedonebybrainstormingor
discussionwithintheclassgroup.Eachstudentshouldhaveaclearunderstandingofthemeaning
ofthechosenattribute.
Thesixattributesagreedforthesconesare:
colour(goldenbrown)
shape(even)
lightness(light)
sweetness(sweet)
fruitiness(fruity)
crumbliness(crumbly).
2.Labelthescorecardandrecordsheetwiththeselectedattributes.Itisimportantthatallscorecards
havetheattributeslabelledattheexactsamepointonthestardiagram.Beginlabellingbywriting
thefirstattributeatthe12oclockpositionandthenmoveclockwisearoundthestarbyinserting
theremainingattributesinsequence.

4.Arrangefoodinthecontainers:
4codedFruitSconeA
4codedFruitSconeB
5.Setuptraysnumbered14.Placeonecontainerwithsymbolandonecontainerwithsymbol
oneachtray.
Codedsamples
Scorecard
Tray1

Scorecard

TraynumberName...

You are presented with two coded samples. Beginning with sample , evaluate and rate the
attributesfrom05usingthestardiagramcoded.Beginwiththevisualattributes.Thentaste
theproduct.
Repeatthesameprocesswithsamplecoded.
Jointhedotstocompleteeachstardiagram.

Food Product _______________________ Food Product
____________________________

StardiagramcodedStardiagramcoded
Golden brown
Golden brown 5
5 4
4 3
3 Fruity Light
Fruity Light 2
2 1
1 0
0
Crumbly Sweet
Crumbly Sweet
Even shape
Even shape

0=notatall1=weak2=fairly3=moderate4=quite5=very

7.Collectscorecardsandtransfereachtestersresultontotherecordsheet.
Eachtestershouldfirstofalltransfertheirownresultsfromeachstardiagramontotheappropriate
placesontheirownrecordsheet.Theymustthentransfertheresultsofeachtesterintheirgroup
ontotherecordsheet.Averagescoresforeachattributearethencalculated.

RecordSheet

FoodProduct_________________________
Collatetheresultsfromthescorecardsinyourgroup.
Attributes

Golden Even
Light Sweet Crumbly Fruity
Brown Shape

Tester1
4 4 5 3 2 3
Resultsfromstardiagram
Tester2
3 4 5 4 2 5
Tester3
3 5 2 5 2 4
Tester4
4 5 3 5 2 5
Totalscore 14 18 15 17 8 17
Averagescore
(total score number of 3.5 4.5 3.75 4.25 2 4.25
testers)

FoodProduct_________________________
Attributes

Golden Even
Light Sweet Crumbly Fruity
Brown Shape
Tester1
4 3 5 3 3 5
Tester2
4 3 4 4 2 5
Tester3
3 3 5 3 3 4
Tester4
4 2 4 2 2 5
Totalscore 15 11 18 12 10 19
Averagescore
(total score number of 3.75 2.75 4.5 3 2.5 4.75
testers)
8.Presentresultsbyplottingtheaveragescoresfromtherecordsheetontothegroupstardiagram.
Itisacceptabletoroundoffaveragescorestothenearestwholenumber.


TraynumberName.

Foreachproductpleaseplottheaveragescoreforeachattributeonthestardiagram.
Useadifferentcolourpenforeachproduct.

GroupStarDiagram

Golden brown
5
4 3.75
3 3.5
Fruity Light
4.75
4.25 2 4.5
1 2.75
0
2.5 2
3.75
Crumbly 4.5 Sweet
3
4.25
Even shape


FoodProduct_________________________

FoodProduct_________________________

9.Compileasensoryprofileforeachproductbasedonthegroupresults.
Foraccurateprofilingitisimportanttousetheappropriatewordsforeachnumberonthestardiagram.
ProfileofFruitScone

Thisfruitsconeisquitegoldenbrown.Itisverylightandisquitesweet.Ithasquiteanevenshape,is
fairlycrumblyandquitefruity.
ProfileofFruitScone
Thisfruitsconeisalsoquitegoldenbrown.Itismoderatelylightandisverysweet.Ithasamoderately
evenshape,ismoderatelycrumblyandveryfruity.
10.Revealcodes.
11.Evaluateresults.
Template
Scorecard

TraynumberName...

You are presented with two coded samples. Beginning with sample , evaluate and rate the
attributesfrom05usingthestardiagramcoded.Beginwiththevisualattributes.Thentaste
theproduct.
Repeatthesameprocesswithsamplecoded.
Jointhedotstocompleteeachstardiagram.

Food Product _______________________ Food Product
_________________________

StardiagramcodedStardiagramcoded
5 5
4 4
3 3
2 2
1 1
0 0


Template
RecordSheet

FoodProduct_________________________
Attributes

Tester1

Tester2

Tester3

Tester4

Totalscore
Averagescore
(total score number of
testers)

FoodProduct_________________________
Attributes

Tester1

Tester2

Tester3

Tester4

Totalscore
Averagescore
(total score number of
testers)
Template
TraynumberName..
Foreachproductpleaseplottheaveragescoreforeachattributeonthestardiagram.
Useadifferentcolourpenforeachproduct.
GroupStarDiagram
FoodProduct_________________________
FoodProduct_________________________
Profile of Food Product

_________________________________________________________________________________________
_________________________________________________________________________________________
_________________________________________________________________________________________
_________________________________________________________________________________________
ProfileofFoodProduct
_________________________________________________________________________________________
_________________________________________________________________________________________
_________________________________________________________________________________________
_________________________________________________________________________________________

Appendix1SummaryofSensoryAnalysisTestsSuitablefortheClassroom
Number of
Category Tests Aim
Samples
To determine the preferred

PairedPreferenceTest 2
product.
Tofindouthowmuchaproductis
HedonicRatingScale 1ormore
liked/disliked.
Preference
Tests
Todetermineattitudebyindicating
FoodActionRatingTest 1ormore degree of liking / disliking for a
product.
To rank products in order of

PreferenceRankingTest 2ormore
preference.
SimpleDifference To determine if there is a

2
PairedComparisonTest differencebetweentwosamples.
Todeterminewhichoftwosamples
Directional Paired
2 hasagreaterdegreeofintensityin
ComparisonTest
termsofaparticularcharacteristic.
Difference
Tests
3 samples 2 are
To identify the sample that is
TriangleTest the same and 1 is
different.
different.
3 samples 2 are
To identify the sample that is
coded and 1 is
DuoTrioTest different from the control /
identified as the
reference.
control/reference.
To rank samples of a product in
DescriptiveRankingTest 2ormore order of intensity of specified
attribute/s.
To rate the intensity of pre

Descriptive DescriptiveRatingTest 1 selected attributes for a food
Tests oneproduct
sample.
To rate the intensity of pre

2 selected attributes for each food
twoproducts
sample.
Appendix2Scales
In sensory analysis many different types of scales are used. However, the choice of scale should be
consideredinlightofthetestobjective.
TargetGroups
Productdevelopmentisfrequentlyaimedatparticulartargetgroups.Simplescalesareusedtoidentify
andcollatethisinformation.
Example1Gender
Male Female
Example2AgeGroup
1525 2635 3645 4655

Example3Doyoueatyoghurt?
Yes No
Doyoueatyoghurt?

RatingScales
Manysensoryanalysistestsrequireproductstobeassessedandthenratedonsomeformofscale.The
scale chosen depends on the aim of the test and the possible outcome. It is essential to choose an
appropriate scale for the test. There are many different rating scales and some of them are
interchangeable.
The followingareexamplesofratingscaleswherethecategorieslieina specificorder.Thescalesmay

containnumbers,words,oracombinationofboth.Thelowestnumberonthescaledenotes"lessof"and
thehighestnumberdenotes"moreof.
Example1Numeric
Notsweet Extremelysweet
0 1 2 3 4 5 6 7 8 9
Example2Verbal
Not Slightly Moderately Very Extremely
sweet sweet sweet sweet sweet
Example3Hedonic

Hedonicscalesexpressdegreesoflikeordislike.Thetermhedonicmeanshavingtodowithpleasure,so
ratingscalestodowithlikesordislikesarecalledhedonicratingscales.
Threecommonlyusedhedonicscalesareincludedbelow.
(a)FacialHedonicScale
Picturesareusedtodividethescale.
(b)NumericHedonicScale
Numbersareusedtodividethescale.Thescaleisusuallyafive,sevenorninepointscalecentredona
midpoint. In other words the scale always has an uneven number of points. When using this type of
scalewithstudentsitwouldbeimportanttokeepthescaleshort.Afivepointscaleshouldbeadequate.
NumericHedonicScale

12345

DislikeLike
ExtremelyExtremely
(c)VerbalHedonicScale
Words or phrases are used to divide the scale. The words / phrases chosen are used to indicate the
degreeoflikingfortheproduct.Thescaleisusuallyafive,sevenorninepointscale.
Whendesigningverbalscalesforclassroomuseitisimportanttousewordsthatareeasilyunderstoodby
students.
FivePointVerbalHedonicScale
VerbalHedonicScale

Likeverymuch __________________

Likeslightly __________________

Neitherlikenordislike __________________

Dislikeslightly __________________


Dislikeverymuch __________________

NinePointVerbalHedonicScale
VerbalHedonicScale

Likeextremely __________________

Likeverymuch __________________

Likemoderately __________________

Likeslightly __________________

Neitherlikenordislike __________________

Dislikeslightly __________________

Dislikemoderately __________________

Dislikeverymuch __________________

Dislikeextremely __________________

Example4:LineScales
Linescalesareusuallyrepresentedasahorizontalline,withalowratingatthelefthandendoftheline
andahighratingattherighthandendoftheline.
SingleLineScales

01234

AbsentWeakModerateVeryExtreme

SeriesofLineScales


Attributes

Aroma

12345

TomatoFlavour

12345

TomatoColour

12345

Sweetness

12345

Example5StarDiagrams
Stardiagramsareusedtorateparticularattributesofafood.
Howtodrawastardiagram
(i) Draw three or four lines (depending on the number of points required), intersecting at a
centralpoint.
(ii) Labelpointsofthescale oneach line.Keepthe scaleshort.A fivepointscaleshouldbe
sufficient. For each attribute the relative intensity increases as it goes further from the
centrepoint.
(iii) Labeleachlinewiththespecificattributebeingrated.
(iv) Placeadotonthenumber,ontheappropriateline,thatbestdescribeeachattribute.
(v) Joinupthedotstomakeastarshape.
ASixPointStarDiagram
Golden brown
5
4
3
Fruity Light
2
1
0
Crumbly Sweet
Even shape
Appendix3PresentationofResults
Sensoryanalysistestresultscanbepresentedonpiecharts,barchartsandscalessuchasstardiagrams.
The method of presentation will depend on the nature of the data collected and the type of analysis
required.
PieCharts
Piechartsarebestsuitedtosimpletestswherethetesteriscarryingoutoneinstructiononlysuchas:
(i) whichproductispreferred
(ii) rankingproductsinorderofpreference.
Apiechartcanbedrawnbyhandorusingacomputerprogramme.Itisimportanttolabelthepiechart
indicating a key for each product, the percentage result for each segment and the number of testers
involvedinthetest.Anexemplarisillustratedbelow.

PieChartIndicatingPreferenceforThreeDrinks

Preference Ranking Test
Unsweetened Freshly
Orange Juice Squeezed
27% Orange Juice
40%
Concentrated
Orange Juice
33%
20 participants

Theresultsindicateaslightpreferenceforfreshlysqueezedorangejuiceanditisclearthatthe
unsweetenedorangejuiceistheleastpreferred.

BarCharts
Bar charts can be used as an alternative to pie charts to present simple information. They can also be
usedtopresentmorecomplexdata.
Abarchartcanbedrawnbyhandorusingacomputerprogramme.Bothaxesshouldbelabelled.The
number or percentage of testers should be shown clearly on the vertical axis. The products or
characteristicsofproductsbeingtestedshouldbeindicatedonthehorizontalaxis.Akeymayberequired
tohelpidentifytheproducts.Exemplarsareillustratedbelow.

Example1
ResultsofPairedPreferenceTest

Shortbread
100%
80%
Preferences
60%
40%
20%
0%
Butter Margarine

This chart illustrates a preference for shortbread made with butter as opposed to shortbread
madewithmargarine.
Example2
ResultsofDescriptiveRatingTest

Scones
5
4
3
Scores
Scone A
2 Scone B
1
0
Golden brown Even shape Sweet Light
Attributes

Thischartillustratestheratingoffourdifferentattributesoftwotypesofscones.SconeAismore
eveninshapeandlighterthansconeB.SconeBissweeterandslightlybrownerthansconeA.

StarDiagrams
While scales are generally used for rating (Appendix 2) they can also be used to present results. Star
diagramsareparticularlyuseful.
Stardiagramscanbeusedtopresentdataforoneormoreproducts.Furtherdetailsonstardiagramsare
availableonpage79.Exemplarsareillustratedbelow.
Aprofilecanbecompiledfromtheinformationpresentedonthestardiagram.

Example1StarDiagramforOneProduct
BreadRoll
Crusty
5
4 5
3
Soft Brown
2 2 5
1
0
4
Nutty 4 Doughy
3
Sweet

0=poor1=weak2=slightly3=fairly4=quite5=very
ProfileofBreadRoll
Thisbreadrollhasaverygoodbrowncolour.Itisverycrustyoutsidebutisonlyslightlysoftonthe
inside.Ithasquiteanuttyflavourandisfairlysweet,butisalsoquitedoughy.
Example2StarDiagramforTwoProducts
Golden brown
5
4 3.75
3 3.5
Fruity Light
4.25 2 4.5
4.75
1 2.75
0
2.5 2
3.75
Crumbly 4.5 Sweet
3
4.25
Even shape

Appendix4GlossaryofTermsUsedinSensoryAnalysis
Appearance Thevisibleattributesofafood.
Attribute Aperceivedsensorycharacteristicofafood.
BalancedPresentationOrder Eachfoodispresentedanequalnumberoftimesandthesamples
arepresentedinrandomorder.
ControlSample of the product being tested is chosen as a reference point against which all others are
compared.
Hedonic Relatingtolikeordislike.
HedonicScale Scalesexpressingdegreesoflikeordislike.
OrganolepticAssessment Usingthesensestoevaluatefood.
Profile Descriptionoftheperceivedsensoryattributesofafood.
RandomOrder Thepresentationorderofsamplesoneachtrayisvariedbetweentesters.
Ranking Food samples are placed in order according to preference or intensity of a specified
attribute.
Rating Foodsamplesarescoredaccordingtotheintensityofaspecifiedattribute.
RecordSheet Documentusedtocompileresultsfromasensoryanalysistest.
Reference Sampleoftheproductbeingtestedischosenasareferencepointagainstwhichallothers
arecompared.
Scorecard Sheetthattestersusetoanswerthequestion/saskedinasensoryanalysistest.
Tester Personwhoevaluatesfoodsandfillsoutascorecard.Thispersonmaybetrainedoruntrained.
Bibliography
Carpenter, R.P., Lyons, D.H. and Hasdell, T.A. (2000). Guidelines for Sensory Analysis in Food Product
DevelopmentandQualityControl(2ndedn).USA:AspenPublications.
Jellinek,B.(1985).SensoryEvaluationofFood:TheoryandPractice.England:Heywood.
Ridgwell,J.(1997).TastingandTesting.(2ndedn).London:RidgwellPress.
Stone,H.andSidel,J.L.(1993).SensoryEvaluationPractices.AcademicPress.

Index
AcesulfameKDetectionandDeterminationin Matchinganexistingfoodproduct..................73
Sweets............................................................66 MetanilYellowIndicatorPaper........................53
Appearance.......................40,44,52,53,77,167 Modifyinganexistingfoodproduct.................73
AshTotal..........................................................10 MoistureContentLabOvenMethod.................4
AshAcidInsoluble............................................14 MoistureContentUsingMoistureMeter...........7
Attribute..........................................................167 NumberinGroup..............................................75
BalancedPresentationOrder.........120,121,167 NumberofSamples...................................75,157
BarCharts........................................................164 OilSolubleCoalTarColour...............................53
BaudouinTest...................................................53 OrganolepticAssessment...............................167
BoricAcidTestforTurmeric.............................53 Packagingandlabelling....................................73
CategoriesofSensoryAnalysisTests...............71 PairedPreferenceTest.....71,87,88,89,90,157,
Caution........................................................55,63 165
CodingofSamples.............................................75 PieChart..........................................................164
Consumertesting..............................................73 PieCharts.........................................................164
Control...............................................67,167,168 Precautionstobetaken....................................55
CrudeFatSoxhletApparatusMethod..............28 PreferenceRankingTest..71,103,104,106,107,
CrudeFiber........................................................34 157
CrudeProteinKjeldahlMethod........................17 PreferenceTests................................................71
CutouttestforCannedFisheryProducts.........39 PreferenceTestsSuitableforClassroomUse..71
Descriptive.71,72,132,133,134,135,137,138, ProductDevelopmentandRecipeModification
139,141,142,143,145,147,148,150,151, .......................................................................74
153,155,157,165,166 ProductDevelopmentintheFoodIndustry.....73
DescriptiveTests.........................................71,72 Productlaunch..................................................74
DescriptiveTestsSuitableforClassroomUse..72 Productmodification........................................73
Detectionofadulterantsindifferentfood Profile..............................140,151,155,166,167
products.........................................................43 QuantityofSample...........................................75
DeterminationofCrudeFibreUsingFibrebag RandomOrder.................................................167
(GerhardtMethod).......................................35 Ranking.......71,72,103,104,106,107,132,133,
Developmentofideas.......................................73 134,135,157,167
DifferenceTests..........................................71,72 Rating......71,72,92,93,94,96,98,99,100,101,
DifferenceTestsSuitableforClassroomUse...72 137,138,139,141,142,143,145,147,148,
DirectionalPairedComparisonTest72,114,115, 150,151,153,155,157,158,165,166,167
117,118,157 DescriptiveRating........................................See
DuoTrioTest.....72,126,127,128,129,130,157 RecordSheet....88,90,93,96,99,101,104,107,
Equipment.........................................................75 110,113,115,118,122,124,128,130,133,
EvaluationofProducts......................................74 135,138,142,148,153,167
EvaluationSheetforCutOutTest....................39 Reference..................................................60,167
Finalproductspecification...............................73 SaltIntensityTest........................................83,85
FoodActionRatingTest71,98,99,100,101,157 Scorecard....80,81,83,84,85,87,88,89,92,93,
GasChromatgraphic(GC)Method....................57 94,98,99,100,103,104,106,109,110,112,
GuidelinesforTestingintheClassroom..........75 114,115,117,120,121,123,126,127,129,
Hedonic....71,92,93,94,96,157,158,159,161, 132,133,134,138,141,146,147,151,167
167 SensoryAnalysis......71,72,74,77,157,167,168
HedonicRatingScale.........71,92,93,94,96,157 SensoryAnalysisinClassRoom........................74
HedonicScale..................................159,161,167 SensoryAnalysisintheFoodIndustry.............71
HighPerformanceLiquidChromatography SensoryEvaluationGeneralConcepts..............71
HPLC...............................................................62 SettingofTrays.................................................75
Hygiene..............................................................75 SimpleDifferencePairedComparisonTest.....72,
Largescaleproduction......................................73 109,110,112,113
Largescaleproductiontrial..............................73 SourIntensityTest......................................84,85
LineScales.......................................137,161,162 SpecialDietaryConditions................................75
Makingacompletelynewfoodproduct..........73 StagesofProductDevelopment.......................73

stardiagram...145,147,148,149,150,151,153, Tester87,92,93,96,98,103,109,110,111,113,
155,162,165 114,115,116,118,120,122,124,126,128,
StarDiagram............................150,155,163,166 130,132,137,139,142,145,148,153,167
StarDiagrams..................................145,162,165 Testingofideasonasmallscale......................73
SweetIntensityTest...................................84,85 TestingSession..................................................75
TasteIdentificationTest.............................80,81 ThinlayerChromatographicdetection
TastingandTestingintheClassroom...............74 TLC.................................................................66
TastingandTestingWordBank........................77 Timing................................................................75
Temperature...................................22,57,66,75 TotalCarbohydrates..........................................32
TestforMetanilYellow.....................................53 TriangleTest......72,120,121,122,123,124,157
TestforStarch...................................................53 UsesofSensoryAnalysisintheFoodIndustry72
Whatissensoryevaluation?.............................71
WheretoTest....................................................75

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Food Analysis and Quality Control

Timeinmin TemperatureinC Comments

Timein Powerin% Comment

Timein Power Comments

CAREaddthewaterslowlyintheearlystages andbewareof spitting.Ifnecessarythedigestiontubes

FibreBag Sample Crude

Name of Simple Method for detection of

The test is specific for

Name of Simple Method for detection of

Name of Simple Method for detection of

i. Taste a small quantity. Saccharin

Sweetmeats, Aluminium foil is whitish grey in

Name of Simple Method for detection of

Name of Simple Method for detection of

andspilt insects, theseadulterants. isunpleasantandtastebitter

Name of Simple Method for detection of

Name of Simple Method for detection of

Name of Simple Method for detection of

Name of Simple Method for detection of

4,4'ODD 1.42 1.38 0.0025

Analyte Retentiontime EDL

Analyte Retentiontime EDL

Determination of Acesulphame K, Aspartame and Saccharin by High Performance Liquid

Appearance Flavour Smell Texture Sound

FoodProduct Ticks TotalNumberofTicks

FoodProduct Ticks TotalNumberofTicks

FoodProduct Ticks TotalNumberofTicks

FoodProduct Ticks TotalNumberofTicks

FoodProduct Ticks TotalNumberofTicks

Tray AB Tray BA Tray AB

Tray AB Tray BA Tray AB

Tray ABA Tray AAB Tray BBA

Tray AAB Tray ABA Tray AAB

Profile of Food Product

To determine the preferred

To rank products in order of

SimpleDifference To determine if there is a

To rate the intensity of pre

To rate the intensity of pre

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The followingareexamplesofratingscaleswherethecategorieslieina specificorder.Thescalesmay

Preference Ranking Test

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