Scribd
Upload
26 views91 pages

Analytical Test Methods

Uploaded by

ALLAWADI ADJI
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF or read online on Scribd
26 views91 pages

Analytical Test Methods

Uploaded by

ALLAWADI ADJI
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF or read online on Scribd
Agro Tech Foods Limited COMPENDIUM OF ANALYTICAL TEST METHODS Date of Release : 20" March 2005 Superceding : None Reason for release : First release Prepared By Reviewed By , Approved eo Nowy V. Supkarao S. Manish Singh Navneet Mehta Mai jahgal Manager - R&D Head Of QA and R&D X > ee Agro Tech Foods Limited Compendium of Analytical Test Methods Released: 20March/05 | Superceding : None QA and R&D -CHO | Poqe 2 of 7h INDEX 28/10/04 10/03/02 Per oxide Value 10/03/02 Fat Content 28/10/04 ‘Salt Content 28/10/04 Todine Value 10/03/02 Moisture and Volatile Matter 10/03/02 Colour Of Git 10/03/02 ‘Cloud Point 10/03/02 Refractive indax 10/03/02 ‘Saponification Value 40/03/02 Melting Point 10/03/02 ‘Unsaponifiable Matter o/03/02 Particle Size Determination 28/70/04 ‘Oxygen Content Analysis 28/10/04 Com Pop Volume 28/10/04. Total Ash Content 28/10/04 ‘Acid insoluble Ash Content 26/10/04 [’p- Anisidine Vaiue (09/02/05. TBHQ Determination - Refined Oils Lime Powder Analysis |'Mono Sodium Glutamate Purity Flash Point ['Coid Acetone Insalubles 10/03/02 ‘Bleachability [Wax Content 10/03/02, 1 Wesson Loss. Specific Gravity Halphen Test Baudouin Test Holde’s Test Castor oil Bolliar-Turbidity Temperature Test Hexabromide Test ‘Argemone Oil Test Kusum Oil Test ja Oil Test [Cold Test 40/03/02 Insoluble impuri 0/03/02 FM F0103 | Oil content in Spent Earth 10/03/02 Test for Phosphoric Acid 10/03/02 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, ‘Secunderabad. 500003 Controlled Document DO NOT PHOTOCOPY CONTROLLED coPY u Compendium of Analytical Test Methods Agro Tech Foods Limited a Supercesng have [Grattan 59 ‘AOCS Bieachabilty Test ____AM046" 10/0302 ‘Acetone Insolubles ‘AMO49 10/03/02 ‘Phosphorus Content ‘AMO50- 10/0302 i 2 ‘Soap PPM in Oil ‘AMO51 yo/o3/02 i GLC Analysis AMO52, (05/02/05 > “Test for Bleaching Earth ‘AMO53 (05/02/05 “Test for Oryzanol in Rice Bran Oi ‘AMO54 (05/02/05 a 3 ) > i ) 0 ited, 31, Sarojini Devi Marg, Controlled Document ; Seeundorabad,cooons 7 Swehnt Dee Mer Bonior pHoTocory L CONTROLLED copy Compendium of Analytical Test Method: Kgro Tech Foods Limited oe cat Released : 20/March/i05 QA and RAD -CHO | Page d of 75 ‘Superceding : AM 001 : Bulk Density Measurement —_—— q a Ly & es s vd COUw ds Cuvd vwuoueut ae a G a a ‘Object To determine the bulk density of material Principle: ‘Aknown volume of the sample is taken and then its weight is measured. Scope: ‘This method is applicable for checking the Bulk Density of Un-Fri corn / popped com / wheat / etc. and Fried polato popz pellets / raw Equipment : 1. Welghing Batance - 2 Kg capacity 2. Cylindrical vessel of 2 litre brim capacity. Procedure: Fill the given sample in the cylindrical vessel upto the brim. Even out the surface by a scale. Pour out the sample ina 1 litre beaker of known weight. Determine the weight of the sample. Calculation: Bulk Density (gr Lir)= Weight ofthe sample Volume ofthe sample {Agro Tech Foods Limited, 31, Sarolini Devi Marg, Contrattad Document Secunderabad, 500003 DO NOT PHOTOCOPY . CONTROLLED copy w Owree 4 PLE Compendium of Analytical Test Method: Agro Tech Foods Limited aaa Released : 20/Maichi05 --! Superceding : None QA and R&D ~CHO | Page Saf 73 ‘AM 002 : Free Fatty Acid (FFA) Content ‘The number of miligrams of Potassium Hydroxide required for neutralizing the Free Fally Acid present in ‘one gram of the oll or fat under the prescribed conditions. The aciity of the ol or fat indicated by iis acid value is frequently expressed as Free Fatty Acids present in the sample, The acid value is determined by directly trating the material in an alcoholic medium with aqueous sodium or potassium hydroxide solulon, Free Fatty Acid is celculated as oleic, laut, iinoeio or palmitic acids, Scop Applicable to all vegetable oils. Reagents: ‘Standard aqueous NaOH / KOH of 0.05 normality ‘Apparatus Required : 1. Volumetric flask titre 2. Burette ‘Standard 0.05N NaOH | KOH : Weigh accurately 2 gms of NaOH or 2.80 gms of KOH crystals and dissolva in a 1 Ilr volumotric flask with distilled water and standardize with Potasslum Hydragan Phihalate. Neutral Ethy! Alcohol: Neutralize the alcohol by titrating with NaOH by adding phenolphthalein indicator til light pink colour ‘appears. Phenolphthalein indicator Solution: Dissolve 1 gm of phenolphthalein in 100 ml of Ethyl alcohol. Procedure: Weigh § ~ 10 gms of the oil in case of crude oil and 18-20 gms in case of refined ol! add 50 mi of neutral ‘ethyl alcohol. Warm the sample on a hot plate until boiling. Then add 2 ~ 3 drops of indicator and titrate against NaOH tl the light pink colour appears. The pink colour should persists for 30 seconds. Calculation In terms of Oleic Acid 282xVxN/W Lauric Acid 20xVxNIW Ricinoleic 298xVxN/W Patmitic = 26xVxNIW \V = Volume in mi of std of NaOH solution used \W-= Weight in grams of the material taken for the test. Reference: BIS ————1Is 548 ( part 4 )- 1964 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 DO NOT PHOTOCOPY CONTROLLED COPY O-O4CED & Agro Tech Foods Limited Released : 20/March/05 AM 003 : Peroxide Value ‘Superceding : None Definition: TITS \which oxidize potassium iodide under the conditions of tho test. The substances are generally assumed io be peroxides or other simniar products of fat oxidation. Scope: Applicable to all normal ols & fats, Including margarine, This method is highly empirical and any vaviation in the test procedure may result in variation of results Apparatus: 1 Pipettes 25 mi and 0.5 mi 2 Burette 50 mi 3 IV flask 250 mi Reagents: 1. ‘Acetic acid and chloroform solution 3.2 VV 2. KI solution saturated 3 ‘Sodium thiosulphate solution 0.1N/0.01N Standardization: Dissolve 24.9 gms of hypo in distilled water and dilute to 1 ltr will give 0.1 hypo solution. Weigh 0.16 to 0.22 grams of potassium dichromate in to @ 500 mi flask or bottle. Dissolve in 25 mi of distilled water, add 5 ml of concentrated HC! and add 20 mi of KI solution ( saturated) swirl the flask and see that thoroughly ‘mix, Allow to stand for § minutes then add 100 mi of distilled water. Titrate with hypo solution, ‘Shake continuously unt! yellow colour has almost disappeared. Add 1 to 2 mlof starch indicator and Continue the titration adding the hypo solution, slowly until the blue colour just disappears. The strength of hypo solution is expressed in terms of its normality, ° Normality of Hypo = —=—=—20.384 X Weight of Potassium Dichromate Volume of Hypo rundown Hypo 0.01 N: Accurately standardized. The solution prepared by accurately pipetting 1 mi of 0.1 sodium thiosulphate in to @ 100 mi volumetric flask and accurately diluted to volume with recently boiled disilled water, a Starch Indicator: Triturate 5 gms of starch and 0.01 gms of mercuric iodide with 30 mi of cold water and slowly pour it with stiring in to one ltr of boiling water. Boil for 3 minutes allow to cool and decant off the supernatant clear liquh Procedur Weigh 5 +/- 0.05 gms of sample into a 250 ml Erlenmeyer ftask with stopper. Add 30 mi of the 3:2 glacial acetic acid and chloroform solution, Swi it to dissolve the sample. Add 0.5 mi of saturated potassium lodide solution prepared freshly by using a suitable volumetric pipette. Allow the solution to stand with ‘occasional shaking for exactly one minute then immediately add 30 mi of distilled water titrate with 0.01 N hypo solution with constant agitation continue the titration until the yellow colour almost disappears. Then ‘add 0.5 mi of starch indicator solution continue the titration with constant agitation especially near the end Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003, DO NOT PHOTOCOPY CONTROLLED copy Compendium of Analytical Test Methods None QA and R&D - CHO. point to liberate all af the lodine from the solvent layor. Add the hypo solution drop wise until the blue Colour just disappears. Conduct a blank determination of tho reagents daily. Tho blank titration volume should not exceed 0.1 ml of hypo solution, Agro Tech Foods Limited 20MMarchvOs Superceding Page 7 of 73 Calculation: Peroxide value ($B) XNX 1000 aa Weight of the sample Hypo rundown in blank Hypo rundown in sample = Normality of Hypo zoo Safety: , 1. Chioroform is known carcinogen. Ils toxle by inhalation and anesthetic properties, Avoid contac with skin ‘ 2. Acetic acid in the pure state is moderately toxic an > Re fence: Aocs————______-cp asa Biss: 548 (part 1 )- 1964 Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 DO NoT PHOTOCOPY CONTROLLED COPY ‘Compendium of Analytical Test Methods Agro Tech Foods Limit e cat Te * Roloased : 20/MarchioS | Superceding : None [oA and Rao cHo Pago of 73 >) ‘AM 004 : Fat Content Determination Objective: $F dolermine-oL/at-content-in the. given product ‘Scope: ‘This method is applicable for determining the Fat content in Fried Potato popz/ Corn Chips / Atta / Popcom / Raw Com / Wheat Prinelpto: - Ethor soluble material In a food is extracted from an oven-driod sample using a Soxhlet extraction ‘apparatus. The ether is evaporated and the residue woighed. ‘The ether extract or crude fal of a food represents, besides the true fat other materials such a5 phospholipids, sterols, essential oils fat ~ soluble pigments, etc. Extractable with ether. Reagents and Apparatus: 4. Weighing Scale 2. Soxhlet Apparatus 3. Water Bath 4. Oven 6. Petroleum Ether (40-60 C Bolling Point) Procedure: ‘Take 10 g of sample to a thimble and plug the top of the thimble with a wad of fat-ree cotton, Drop the thimble into the fat extraction tube of a Soxhlet apparatus. Attach the botiom of the extraction tube to a ‘Soxhlet flask. Pour approximately 75mi-100mi of anhydrous ether through the sample in the tube into the flask. Attach the top of fat extraction tube fo the condensor. Extract the sample for 4 hours on a water bath: ‘The water bath should be regulated so that the ether which volailizes condenses and drops Continuously upon the samplo without any appreciable loss. ‘Al the end of the extraction period, remove the thimble from the apparatus and distil off most of the ether by allowing Ilo collect in the Soxhiet tube. Pour off the ether when the tube is nearly ful. When the ether has reached a small volume, pour it into a small, dry, (previously weighed )beaker through a small funnel conlaining a plug of cotton .. Rinse the flask and filer thoroughly, using several small portions of ether - Evaporate the ethor on a steam bath at ow heal, preferably under a current of ar. Dry at 100 deg C for 1 hr, cool and walgh. The difference in the weights gives the ether-soluble material present in tho sample. Calculation : % Crude fat = Wt of ether soluble material_x_100 ‘WL. of sample taken for extraction ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlied Document Secunderabad. 500003 00 NOT PHOTOCOPY CONTROLLED COPY (ote Anca Compendium of Analytical Test Methods Tech Foods Limited ed : 20/March/0S | Superceding : None AM 005 : Salt Content Determination 3 Determination of Salt Content in the given sample. es ‘Scope ‘This method is applicable for determining Total Salt content as Sodium Chloride percentage in the given ‘sample of seasoning powders / Com Chips / Potato popz and Commercial salt powder. Equipment: 1. Weighing scale 2, 250 ml volumetric flask 3. 1miBuretto aww Reagents: 4.0.1 NNaOH 2. Phenolphthalein 3. 0.4 Neilver nitrate 4. 5% solution of potassium chromate Procedure: Weigh 259 of sari with cistlled water, a tind it (in case of Com chips and Potato Popz) without any losses and dilute id neutralize with 0.1 N NaOH using phenolphthalein as indicator. Transfer to a 250 ‘mi volumetric flask, make up fo volume with distilled water with shaking, and fiter. Titrate an aliquot with O-1 N silver nitrate using about 1 ml of 5% solution of Potassium chromate in water as indicator. Nole the volume of silver nitrate solution required to produce the red-brown end point colour. Carry out @ blank titration using 100 ml of distiled water and 1.0 mi of the indicator. wo ° Calculation: } ‘Sodium Chloride %= {Samole tire ~ Blank thre} x Normality of AgNO; x Volume made up x 58.45 x 100 ‘mi of sample taken x Wtof sample x 1000 ? Note: I the end point is not clear, overcome the masking by fairly heavy dilution of the fitrate before ) titrating. 5 2 Referencs Handbook of Analysis and Quality Control for Fruit and Vegetable products 2” edition by [Link]. > Tata McGraw Hill Publishing Company Limited, ) ) 3 3 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document 7 ‘Secunderabad. 500003 Do Nor PHOTOCOPY ie CONTROLLED COPY MGIC DOLE u 2 Compendium of Analytical Test Methods Agro Tech Foods Limited Releasod : 20/March/05 upercacig None [Ama “GH | pun 1 0179 AM 006: lodine Value Definition: solution. The lodine value of the oll or ‘constituent fatty glycerides. ives an indication of the degree of unsaturation of the Principl The material Is treated, in carbon tetra chloride medium, with a known excess of iodine mono chloride solution in glacial acetic acid (Wi's solution). The excess of iodine mono chloride is treated with Potassium iodide and the liberated iodine estimated by titration with sodium thiosulphate solution. ‘Scope: Applicable to all normal vegelable fats & olls which do nol contain conjugated double bonds, Apparatus: 4. Glass stoppered iodine flask 500 mt 2 Pipette 25 mi 3. Volumetric flasks 500, 1000 mi 1, Glacial acetic acid unaffected by chromic avid 2. Potassium iodide reagent grade 3. Soluble starch 4. Potassium dichromate reagent grade 5. Sodium thiosulphate 8. Carbon tetra chloride or chloroform 7. 8 Hydrochloric acid lodine mono chloride Solutions: 1 Potassium lodide solution: Prepare by dissolving 10 gms of potassium iodide in 100 mi distilod water. 2 Soluble starch: Triturate 5 gms of starch and 0.01 gms of mercuric Iodide with 30 mi of cold water ‘and slowly pour it with string in to one itr of bolling water. Boil for 3 minutes allow to cool and decant off the supematant clear liquid. 3. Potassium Dichromate: Welgh accurately about 5 gms of finely ground potassium dichromate which has been previously dried in to @ constant weight at 105 C ¥/- 2C in to a clean 1 ltr volumetric flask. Dissolve in water, make up to the mark, shake thoroughly and keep the solution In a cool dark place. For standardization of sodium sulphate, pipette 25 ml of this solution in to a ‘clean glass stoppered 250 mi conical flask, add 5 mi of concentrated hydrochioric acid and 15 mi Cf 10% potassium jodide solution., Allow to stand in the dark for 5 minutes and titrate the mixture with the solution of sodium thiosulphate, using starch solution as an internal indicator towards the ‘end, The end point is taken when the biue colour changes to green. Calculate the normality (N ) Of the sodium thiosulphate solution as follows 25xW N= 49.03 xV Where W = weight in grams of the potassium dichromate & V = volume in ml of sodium thiosulphate solution required for the titration Agro Tech Foods Limited, 31, Sarojini Devi Marg, Contrellad Document Secunderabad. 500003 Do Nor PHOTOCOPY CONTROLLED COPY 2 5 3 2 wy OVUTO ws 2 5 3 > 2 SC yee Y Un ” ee Compendium of Analytical Test Methods Agro Tech Foods Limited i of 73 Folens 70NooW05 _[Supereding ‘ow [OAsnda0-chO [+ 4. Standard sodium thiosulphate solution: ( Approximately 0.1 N ) Dissolve approximately 24.8 gms of sodium thiosulphate crystals in water which has been well boiled to free it from carbon dioxide and make up to 1000 mi. Store the solution in a cool place in 5. Wis Solution Stock solution: Add an ample of 60 mi iodine monochloride to 250 ml volumetric flask and. makeup with glacial acetic acid. Working Solution: Draw accurately 42 mi [Link] solution in to 600 ml volumetric flask and make vp with glacial acetic acid, Procedure Malt the sample If itis not already liquld and fier through filter paper to remove any solid impurities and last traces of moisture, Welgh the sample accurately into a 600m flask to which has been added 26 mi of ‘carbon tetra chloride or chloroform, Burette the 25 mi of Wis solution into flask containing the sample, ‘stopper the flask and swirl to ensure an Intimate mixture. Add a litle of KI solution in the iodine flask stopper cover. Store the flask in dark for 30 minutes at room temperature . Remove the tlask from storage ‘and add 15 mi of potassium iodide solution, followed by 100 mi of starch indicator solution and continue the titration untl the blue colour has just disappearod. Prepare and conduct a blank detarminaticn in all respect to the sample. Calculation: The lodine Value = (B-S)xNx 12.69 Weight of the sample Volume of thiosuiphate rundown in bank Volume of thiosulphate rundown in sample Normally of thiosulphate solution ‘Agro. Tech Foods Limited, 31, Sarojini Devi Marg, Cantrolled Document Secunderabad. 500003, BO NOT PHOTOCOPY CONTROLLED COPY Compendium of Analytical Test Methods ay hah 5 Ohana OH0 [Pope 12047 ) Sizo of tho samplo Wl gms of samplo Woighing 2 To woigh lodi Min. Wt Max WL Accuracy <3 110.0000 10.0000 9 3 8.4613 10.5760 5 5.070 6.3460 » 10 3.1730 . 20 1.5865 40 0.7935 i 60 0.5288 4 80 0.3173 a 400 0.2538 7 420 0.2115 440 0.1813 160 0.1587 180 0.1410 > 200 0.1269 > Note: . 2 41. AllWijs solutions are sensitive to temperature, moisture and light. Store in a cool and dark place and 7 never allow to come to a temperature above 30 C. ) 2. Store samples with an IV > 150 per one hour. 9 Roferanc AQCS———————Cd 125 , BIS. 18548( part-1) 1964 » ¥ 7 ¥ 9 , 5 : ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document > ‘Secunderabad. 500003 Do NOT PHOTOCOPY CONTROLLED copy utd G ws age & oA Compendium of Analytical Agro Tech Foods Limited 'pendium of Analytical Test Methods Released : 20/March/05...| Superceding : None QA and R&D -CHO | Pago 13 of 73 AM 007 : Moisture and Volatile Matter Definition : ‘Apparatus: 4. Alroven maintained at 105°C + 2° C / 190°C + 2°C 2. Porcelain or glass moisture dishes 60 - 80 mm dia and 20 - 40 mm depth 3. __Desiccator, desiccant: Anhydrous calcium sulphate. 4, Balance 200 gms pracision 0.0001 gms. Method I: Applicable to all edible oils / fats Procedu ‘Weigh exactly 10 gms of sample in to a tarred moisture dish which has been dried for 1 hour at 105 + 2° C and cool to room temperature in a desiccators. Dry the sample fo constant weight in an air oven at 105 +/ =2.C for 1 hour and cool to room temperature and weigh. Constant weight is attained when successive ‘one hour heating period show a loss or gain of not more than 0.1%. ‘Method Il: Applicable to finished food products (com chips and potato popz) Procedure: ‘Weigh exactly 10 gms of sample in to a tarred moisture dish which has been dried for 6 hours at 105 + 2° and coo! to room temperature in a desiccators, Dry the sample to constant weight in an air oven at 105 +12. for 1 hour and cool to room temperature and weigh. Constant weight is attained when successive ‘one hour heating period show a loss or gain of not more than 0.1%. Method It! : Applicable to food stuffs (com grains, salt, dried green peas) Procedure: Welgh exactly 10 gms of sample in to a tarred moisture dish which has been dried for 1 hour at 130 + 2° C and coo! to room temperature in a desiccators. Dry the sample to constant weight in an air oven at 105 + 2°C for 1 hour and cool to room temperature and weigh. Constant weight is attained when successive ‘one hour heating period show a loss or gain of not more than 0.1%. Calculation (applicable to Method 1/11 //1V) : Moisture & Volatile Matter % © = Loss in weight X 100, Weight of the sample Method IV : Determination Of Moisture Content By The Entrainment Toluene Distillation Technique (Dean & Stark Method) Principle : ‘The amount of water is determined by first distiling the material with an organic liquid not miscible with ‘water, and then collecting the distillate in a graduated tube. Agro Tech Foods Limited, 31, Sarojinl Devi Marg, Cont olled Document Secunderabad. 500003 DO NOT PHOTOCOPY CONTROLLED COPY 2 o a oO Compendium of Analytical Test Methods Agro Tech Foods Limited fasted 20Morcw08 _| Supereeding Nove Gh enanad 6H ‘Scope: This method is applicable for determination of moisture to all all spices by co-distillation with toluene, with the exception of capsloums , rod peppers, paprika, chilies, saffron, dehydrated garlic. onion, and Equipments: |. 500 mil or 1000 mi round-bottom, short neck flask with a T.S 24/40 joint ‘West condenser with dip tip, 400 mm in length with a T.S.24/40 joint. Bidwell ~ Sterling trap, T.S.24/40 joint. 5 mi capacity graduated with 0.1 ml intervals . Heating mantle capabie of refluxing toluene. ‘Nylon bristle burette brush % inch in diameter or a wire loop. It should be long enough to extend through the condenser { about 450 mm), The diameter ofthe spiral should be such that iis snugly ‘wthin the graduated portion of the Eniralnment Distllaton Apparatus which comprises a glass Task heated by sullable. means end provided with a reflux condenser discharging into a trap and ‘connected to the flask. The connections between this trap and the condenser and the flask should be interchangeable ground-glass joints. The trap serves to colect and measure the condensed water, and to retum the solvent to the flask. 6. Water cooled , glass reflux condenser, having a jacket approximately 400mm long and an inner tube Of 8.5 to 12.5 mm outside dlameter. “The tip of the condenser to be inserted inthe trap, may bo ground at an angle of 30 degree from the vertical axis of the condenser .. When inserted into the ffap, the tip of the condenser should be 6 107 mm above the surface of the liquid In the trap after distilling conditions have been established. 7. Receiver ( also called as trap ) Is a receiver of 5 mi capacity made of high resistance glass, well ‘annealed and as free as possible from striations and defects, provided with ground glass joints, onelating essential of the upper chember , together wilh tha tube and ground joint leading to the flask, and the graduated tube. The graduated portion has a capacity of 5 mi when filled to the highest graduation mark. The scale covers the range of 0 to 5 mi and is graduated at intervals of ‘0.1 mi. The graduation marks corresponds to each millilter and are numbered and carried ‘completely round the tube. The graduation marks midway between the numbered marks are Carried % way and the remaining marks are carried halfway around the tube . The error at any indicated capacity should not exceed 0.05 mn. Procedure : Place 409 of the spice ( or enough to yield 2-5 mi H20 ) in distlation flask. Add enough solvent to cover sample completely ( never less than 75 mi). Fill the rocelving tube with solvent, pouring through top of ‘condenser. Insert loose cotton plug in top of condenser to prevent condensation of atmospheric moisture in tube . Bring to boil and distil slowly @ about 2 drops /sec , until most of H2O distills over, then increase tale of disilation to about @ 4 drops /. sec . Continue distiling until 2 consecutive reading 15 min apart ‘show no change. Dislodge any H20 held up in condenser with brush of wiro loop. Rinse condonsor ‘carefully wilh about 5 mi toluene. Continue distillation for 3 to 5 minutes, cool receiver to room temp about 25 deg C allowing itt stand in air or immersing it in H2O . Solvent and H20 layers should now be clear, if rot let it stand tll clearing occurs, Read volume , of H20 , estimating to nearest 0,01 ml and caleulate to percent, Calculation + Vol. Of water (mi) Percentage moisture = ~~ ‘Wtol sample ( 9) x 100 Precautions : 1. The apparatus , including the condenser , should be cleaned with potassium dichromate-sulfuric acid cleaning solution, rinse with water, followed by a rinse with 0.05N potassium hydroxide inse with alcohol and drain for 10 min, The apparatus must be dried properly . This solution. Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 BO NOT PHOTOCOPY CONTROLLED COPY 2 kad A uw G&G wut © we ‘eee 6 6 UL o Compendium of Analytical Test Methods SAI RED-EWO [i (Sv procedure will minimize the adherence of water droplets to the surface of the conduiser and BidwellSterling trap. 2, Acomection blank for toluene must be conducted periodically by adding 100 mi of distilled water lo stilation flask and run the method as described under procedure, This this test Use ‘of toluene for substances such as red pepper an Genydraled vegetables which contain large amounis of sugars and other materials which ray acompose at 100 deg C to form water. Vacuum oven method is the preferred method for these products. 4, The remnants of the sample material should not be used for other tests. # TRS (Ett materials being hygroscopic should be transferred immediately ater opening the pack and Weighing the required quaniily and instantaneously covering it with toluene to ward off moisture Vaporizalion of hygroscopic absorption of moisture. Reference AOCS. ca 2-38 ‘Agro Tech Foods Limited, 31, Sarojinl Devi Marg. Controlled Document Secunderabad. 500003 Do NoT PHOTOCOPY CONTROLLED COPY c woe gow “UO 6 OOP & © YU a re ou oad ou ‘ Agro Tech Foods Limited AM 008 : Color Of Olt initio Compendium of Analytical Test Methods Released: 20/Marciv05__ | Superceding : None QAand RD-CHO [Page oof 73 | nes characteristics, The colour Is expressed as the sum of yellow and red slides used to match the colour of the given oll in a cell of the specified size in lovibond tintometer, ‘Scope ‘Applicable to all types of raw, in process and finished oils of Sunflower, Groundnut, Soya and Palmolein. Apparatus: 4. Lovibond Tintometer 2. Required size of Cells 5 1/4", 1°, 1/2", 1/4" 3. Whatman Filter Paper No 1 4, Tissue Paper Procedure: Filler the sample through Whatman Filer Paper to remove any impurities and last traces of moisture. Make sure that the sample is absolutely clear and free from turbidity. Clean the glass calls of desired size ‘with carbon tetrachloride and dry. Fill it with oll and put in the Tintometer. Adj red and yellow slides to match the colour shade of the oll by observing the colour of the oil and the combination of the glass slides through the eyepiece. Calculation: ‘The colour ofthe oil in terms of lovibond units is as follows. Colour AY + 58R Where, 1e sum of yellow slides used rhe sum of various red slides used Note: 1, For Raw Expelled Sunflower Oil 2. For Raw Solvent Sunfiower Oil 3. For Raw Expeller Ground Nut Oil 4, For Raw Solvent GN Oil 5. For Solvont Soya Oi 6. For Raw Solvent Cotton Seed Ot 7. For Refined oils = Ref: 1S 548 - Part! ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, ‘Secunderabad. 500003 Y+5R in 1° Cell YeSRin 1/4" Ye5R in 1/2" Y+5R in 112° YetOR in 14" YeSR in 1/4" YeSR ind 1/4" Controlled Document Do Not PHOTOCOPY CONTROLLED cOPY Compendium of Analytical Test Methods Agro Tech Foods Limited Released: 20Marclv05 | Superceding None | and R8D-cHO aa Tease 170i ‘AM 009 : Cloud Point Of Oil i z patatio ee a The cloud point is thal temperature al which, under the conditions of this Test, @ cloud Is induced In the ‘sample caused by the first stage of crystallization, Apparatus: 4. Oil sample bottle 116 mi 3 2, Thermometer range ~2 deg. C to 68 deg. C 3. Water bath made up of water, chipped ice and water; or chipped ice, salt and water, depencing upon the temperature required. The temperature of the cloud point bath shall nol be less than 2 deg. C nor more than § deg. C below the cloud point. Eilher a beaker or insulaled container is convenient for the test 5 Procedure: 1. ‘The sample must be completely dry before making the test. If the sample contains traces of moisture, it should be fitered through suitable filter paper. Heat 60 ~ 75 grams of sample to 130 C just before making the test. Pour 45 mi, of the heatad fat in o the oil sample bottle. } 2. Begin to cool the bottle and contents in the water bath, stiring enough to keep the temperature uniform. When tha sample has reached a temperature about 10C above the cloud point begin stiring steadily and rapidly In a circular motion so as to prevent super ’ cooling and solidification of fat crystals on the sides or bottom ofthe bottle. 3. From this point onwards do not remove the thermometer from the sample, since to do so may Introduce air bubbles which will interfere with the test. The test bottle is maintained in such a position that the upper level of the sample in the bottle Is level with the water in the bath. 4. Remove the bottle from the bath and inspect regularly. The cloud pont is tho temperature at ‘which the portion of the thermometer immersed In the oll Is no longer visible when viewed horizontally through the bottle and sample. Notes ‘ tis essential that the sample be heated to 130" to destroy any crystal nucle. ’ Reference: 5 AOCS. CC 6-25 ‘ Agro Tech Foods Limited, 31, Sarojinl Devi Marg, Controlled Document J ‘Secunderabad. 500003 D0 NOT PHOTOCOPY CONTROLLED COPY 3 3 a Om > PN Compendium of Analytical Test Methods Agro Tech Foods ited Ralated;20MorcvO5 | Supereeding ono [Amd RAD-CHO [Pape Iho 7 ‘AM 010 : Refractive Index Of Oil ices with respect to air rather than vacuum The index or retraction of olis is characteristic within certain limits for ‘each kind of ol. It is related to the degree of saturation but itis affected by the other factors such as free fatty acid content, oxidation and heat treatment. Scope: ‘Applicable to all normal oils and liquid fats, Apparatus: 4. Thermostaticaly controled water bath 2. Abbey's Retractometor 3. Toluene 4 ‘Thermometer 0-110 deg. C with graduation 1 deg. C wmple if it is not already liquid. Filter through filter paper to remove last traces of moisture and Adjust the temperature of the sample to 40 deg. C then place few drops of the sample on the lower prism. Close the prism tighten firmly withthe screw head and allow to stand for one or two minutes. ‘Adjust the Instrument and light to obtain the most distinct reading possible fo determine refractive index. Take atleast three readings and calculate the average of all readings Note: Approximate temperature corractions may be made bythe folowing calculations RI+K(T1-T) Where R ‘The reading reduced to the specified temperature RI ‘The reading at T1 C T ‘Tho standard temperature ( 40 deg. C ) uw ‘The temperature which the reading R is made K (0.000365 for fats and 0.000385 for oils Precautions: 4. Ensure that the prism is clean and dry 2. The instrument should be standardized with a liquid of known refractive index ( distiled water R1 = 1,333 at 20C) 3. Clean the prism with toluene Safety: ‘Toluene is Nammable and fire risk a fume hood should be used at all the times when using toluene. Reference: AQCS———CC 7-25 Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 DO NoT PHOTOCOPY CONTROLLED COPY UA Compendium of Analytical Test Methods ——_C_ Agro Tech Foods Limited Rates 2060s [supereding: Nowe [Nana waO-ovO [gh Nar ‘AM 011 : Saponification Value Of Oil the amount of alkali required to saponily a definite qui ly of the sample, Scope: Applicable to all normal fats and oils Apparatus: 4. Erlenmeyer flask 250 mi of 300 mi with 24/40 ground glass joint. 2. Ar condensers, minimum 65 om long with T 24/40 ground glass Joint to fit Erlenmeyer ask 3. Distilaion ask 2 I for refluxing éthy alcohol with joints fitted with water cooled condenser. Reagents: 1,” Hydrochloric acid 0.6N accurately standardize 2. Alcoholic KOH prepared by placing 5 to 10 gms of reagent grade KOH pellets in a 2 Itr flask and adding 1 ltr to 1.5 Irs of 95% ethy! alcohol and boil on a water bath under reflux for 30 to 60 ‘minutes. Distill and collect the alcohol in a clean glass stoppered receiver. Dissolve 40 grams of KOH in 1 tr of the distilled alcohol with cooling to keep the temperature at or below 15°C, The solution should remain clear 3. Phenolphthalein indicator solution: 1% in 95% ethyl alcoho! ready liquid and fitter through a filter paper to remove any impuritios and ‘moisture, The sample must be completely dry. Mix the sample thoroughly and weigh accurately by difference 1.5 to'2 grams of the sample in @ conical flask. Add 25 mi of alcoholic potassium hydroxide solution and connect the reflux air condenser to the flask. Heat the flask on water bath or electric hot plate for not more than an hour. Boil gently but steadily until the sample Is completely saponified as indicated by absence of any oily matter and appearance of clear solution. Afler the flask and condenser have ‘cooled somewhat, wash down the inside of the condenser with about 10 mi of hot elhy! alcohol neutral to Phenolphthalein. Add about 1 ml of phenolphthalein indicator solution, and titrate with standard hydrochloric acid while hot. Prepare and conduct a blank determination at the same time, Calculation: Saponification value = 56.1(B-S)N w Volume in ml of standard HCI required for the blank Volume in mi of standard HCI required for the sample Normality of the standard HCI = Weight in gms of the material taken for the test Safety: ‘When working with extremely with caustic material ike KOH always add pellets to water nol viso versa References: AOCS———__cd 3.25 BiS——————1S 548( part 1) - 1964 . Agro Tech Foods Limited, 31, Sarojin! Devi Marg, Controlled Document ‘Secunderabad. 500003 DO NOT PHOTOCOPY CONTROLLED COPY Bp) ww 2) wy AM 012 : Melting Point Of Ol! General: point. Therefore, the term ‘melting point’ does not imply the same characteristics thal it does with pure crystalline substances. Fats pass through a stage of gradual soflening before they become completely ligula. The melting point, therefore, defined by the specie condions of the method by which tis jetermined. ‘The melting point Is determined by taking the solid fat inside a small capillary tube and two mathads are prescribed for the purpose. Both of these are applicable to all types of normal animal and vegetable fals ‘and the method used shall be specified while stating the results. ‘Open-Tubs Capillary-Slip Method: Apparatus: Melting point tubes ~ thin walled, uniformly bored capillary glass tubes open at both ends and with the following dimensions. a) Length, 50 to 60 mm; b) Inside diameter 0.8 to 1.1 mm; and c) Outside diameter, 1.2 10 1.5 mm. ‘Thermometer — with 0.2 deg. Subdivisions and a suitable range. The thermometer should be checked against a standard thermometer which has been calibrated and certed by the National Physical Laboratory, New Delhi, or any other laboratory recognized for such work. Beaker ~ with a side-tube heating arrangement, Thicle melting point tube may be used. Heal source - gas bumer or a spirit lamp. Procedur 1.” Melt the sample and filter it through a filter paper o remove any impurities and the last traces of ‘moisture. Make sure that the sample is absolutely dry. Mix the sample thoroughly. 2. _ Insert a clean melting point tube into the molten sample product so that a column of the material, ‘about 10 mm long, is forced into the tube. 3. Chill the sample in the tube at once by placing the end of the tube containing the sample against a piece of the ice until the fat has solidified. 4, Place the melting point tube in a test-tube and hold it for one hour either in a refrigerator or in water maintained at 4 to 10 deg. C. 5, Remove the melting point tube and attach with a rubber band or any other suitable means to the thermometer so that the lower end of the melting point tube is even with the bottam of the bulb of the thermometer. 6. Pour water at about 10 deg. C into the beaker of the Thicle tube, and suspend the thermometer in the center of the apparatus, s0 that the lower end of the sample column is about 30 mm below the ‘surface of water. 7. Heat the side tube of the apparatus gently, so that the temperature of the water rises slowly at the rate of 2 deg. C per minute til the temperature reaches 25 deg. C, and thereafter at the rate of 0.5, deg. C per minute. 8. _Nole the temperature of the water when the sample column commences to rise in the melting point tube. 9. Report the average of two such separate determinations as the melting point, provided that the readings do not differ by more than 0.5 deg. C. Ref: 1s 548—Part! Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 DO NOT PHOTOCOPY CONTROLLED copy UUs WU & 3 be saponified by the usual caustic treatment but, which are solubl UBL se uw ‘Compendium of Analytical Test Methods Agro Tech Foods Limited FuleosedZoNorciOs | Supwending Nave [OAwdRGD-GHO [Page 21 of 78 ‘AM 013 : Unsaponifiable Matter Definition: ‘group Includes compounds of higher aliphatic alcohols, sterols, pigments and hydrocarbons. Principle: ial Is completely saponified with alcoholic potassium hydroxide solution and extracted with er. The petroleum ether extract is washed with aqueous alcohol and then again with water. tether extract is evaporated and the rasidun weighed. Unsaponifiable matter is this residue minus the fatty acid present in it, which is determined by titration with sodium hydroxide solution in alcoholic medium. Scop: Applicable to all oils and fats Apparatus 1, Flat bottom flask 250 mi 2. Separating funnels 600 mi capacity 3, Weighing balance 4, Alrcondenser Reagents: 1. Alcoholic KOH Solution: Dissolve 70 ~ 80 gms of KOH in an equal quantity of distilled water, and ‘add sufficient aldehyde free methy! alcohol (95% by volume) or aldehyde-free rectified spirit to make up to 1000 ml, Allow to stand overnight decant the clear liquid and keep in a amber coloured bottle close tightly with a cork or stopper. 2. Ethyl alcohol 95%. 3. Phenolphthalein indicator: Dissolve 1 gm of phenolphthalein in 100 mi of ethyl alcohol. 4. Petroleum ether 5. Aqueous alcohol: Containing 10% of ethyl alcoho! 6. Standard NaOH Solution: 0.02 N 7. Acetone Procedur ‘Weigh accurately 5 grams of the well mixed sample in to the flask add 50 ml of alcoholic KOH solution. Boll gently but steadily under a reflux condenser for 1 hour until the saponification is complete. Wash the condenser with about 10 ml of ethyl alcohol. Cool the mixture and transfer it into @ separating funnel. Complete the transfer by washing the flakes with some ethyl alcohol and then with cold water. Altogether ‘add 50 mi of water to the separating funnel followed by an addition of 50 ml of petroleum ether. Insert the stopper and shake vigorously for al least one minute and allow to settle uni both the layers are clear, Transfer the lower layer containing the soap solution to another separating funnel, and repeat the ether extraction at least six times more using 50 m! of petroleum ether for each extraction, if any emulsion is, formed add 2 small qty of ethyl alcohol or alcoholic KOH solution collect all the ether extracis in a separaling funnel. Wash the combined extracts in the funnel three times with 25 mi portions of aqueous alcohol shaking vigorously and drawing off the alcohol water layer after each washing. Again wash the ether layer successively with 20 mi portions of water until the wash water no longer tums pink on addition of a few ‘drops of phenolphthalein indicator. Do not remove any of the ether layer. Transfer the ether layer in a tarred flask containing a few pieces of pumice stone, and evaporate to dryness by connecting in to the Agro Tech Foods Limited, 31, Sarojin! Devi Marg, Controlled Document ‘Secunderabad. 500003, DO NOT PHOTOCOPY CONTROLLED COPY Compendium of Analytical Test Methods [ew eea me6 eno | png 2017 ‘soxhlot condenser, and heat on mantel, Collect the other to ramove last traces of ether, place the flask in 5 i ‘Again keep in the oven and dry for further 15 minutes, then coo! it in the desiccator, then weigh it Continue the procedure til you will gat constant weight. After weighing, take up the residue in 50 mi of ‘warm neutral ethyl alcohol, containing a few drops of phenolphthalein indicator and tiate with standard NaOH solution, Calculation: Weight in gms of fatty acids in the extract at olele acid = B 8 0.282 XVXN Where v Volume in ml of NaOH rundown N Normality of standard NaOH Unsaponiffable matter, percent by weight = 100(A~B) w Where A Weight in grams of the residue ” B Weight in grams ofthe fatty acids in the extract w Weight in gms of the material taken for the test 8 - Notes: 4, Ethyl alcohol is fammable ° 2, Petroleum ether is flammable 3. KOHisa strong alkall > > Reference: BIS————Is: 548 ( part 4 )- 1964 2 > > > > > > a 5 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document : ‘Secunderabad. 500003, DO NoT PHOTOCOPY CONTROLLED tad COPY YC PBMEM PSE YP GG BEOY G Lohlg YW MEU Sew » ) y Compendium of Analytical Test Methods Agro Tech Foods Limited Roleasod : 20/Marchi0S | Superceding : None [anansRao-cHo [Page 22 oF 78 [Relensod: 20/MarchiOS_| Superceding :N | i : soxhlet condenser, and heat on mantel. Collect the ether to remove last traces of ether, place the flask in ‘oven at 80 - 90 C for about an hour. Remove Irom the oven and cool in a desiccator. Then weight ‘Again keep in the oven and dry for further 15 minutes, then cool tin the desiccator, then weigh it Continue the procedure tl you will get constant weight. After weighing, take up the residue in 50 mi of warm neutral ethyl alcohol, containing @ few drops of phenoiphthalein indicator and lirate with standard NaOH solution. Calculation: ‘Weight in gms of fatty acids in the extract at oleic acid = B 8 0.282 XV XN Where v Volume in mi of NaOH rundown N = Normality of standard NaOH Unsaponifiable matter, percent by weight = 100(A-B) w Where A Weight in grams of the residue 8 Weight in grams of the fatty acids in the extract w ‘Weight in gms of the material taken forthe test Notes: 1, Ethyl alcohol is flammable 2, Petroleum ether is flammable 3. KOHisa strong alkali Reference: BiIS—————Is: 548 ( part 1 )- 1964 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad, 500003 DO NOT PHOTOCOPY CONTROLLED copy Compendium of Analytical 1 st Methods, Agro Tech Foods Limited aa aio as Released : 20/Marctvos | Superceding : Nono QA and RAD -CHIO | npn bat 14 AM 014 : Particle Size Distribution Objective: To determi VouwuUL 5 Principle: : felalnanee ees afte, determination of partite size distibuton of @ given sample. Percentage O Felalnance of the partcies on the siave is calculated in this process, J Equipments: 2 1 2. Sieves of required microns a 3, Blectronic balance Procedure: d The required series of sieves is placed in sscending order. 100 gm of sample is dispensed ) 1 ipesigve and sieved for § minutes, The machine is then slopped and the sample adhering to tno a Sides of the sieve is brushed off individually into the sieves and sieved again for 3 munuies a The material from individual sieves Is collected and weighed in an electronic balance, The retainance on i each sieve is recorded individually and expressed as percontage. D dD Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controtied Document ‘Secunderabad, 500003 Do NOT PHOTOCOPY CONTROLLED COPY ‘AM 015 : Oxygen Content Analysis Ue Lee Objectiv 5 Principle 5 ‘The instrument probe measures the oxygen content in the pouch environment. Equipment Oxygen Analyzer (Make-PBI-OANENSOR A/S DENMARK) PROCEDURE: ‘Switch on Instrument Calibrate the instrument by pressing both the buttons at a ime, for fraction of second and allow it for y u vy Results: Displayed valued alter analysis is the % Oxygen Content in the pouch, wow Precautions: Instrument is very sophisticated, so handle very carefully whi ‘septum as it may give erroneous results, sing it. Don't use instrument without Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document Secunderabad, 500003 DO NOT PHOTOCOPY CONTROLLED copy Compendium of Analytical Tost Methods Agro Tech Foods Limited | Paar 26 0 73 ‘AM 016 : Corn Pop-Volume Measurement Objective Principle: Best and time tested method of evaluation of any food finally percolates to actually making the product ‘and testing the same using a hard bottom pressure cooker and actually cooking the product and allowing the com to pop to its maximum volume. Oulline of the process is mentioned as below: Equipments: 1. Measuring Cylinder-2 L 2. Cooker 3, Stove with gas cylinder Procedure: 4. Take 50 g of the pop com 2, Add 2.8 gm common salt earmarked as per the specification 3, Add 18.0 ml of the Oil earmarked for the product 4, Empty each of these ingredients into any small cup, blend the three 5. Empty the blended contents into a thick bottom pressure cooker 6. Heat to medium flame withthe lid inverted on the pressure cooker 7. Mix the material intermittently unt the first pop sound is heard 8. Close the lid partially, allowing the steam to escape out while the popping continues until rapidly, slows down further and stops after @ while, Shake the cooker intermittently during the popping process 9. Examine the pop volume by pouring the corn into a standard vessel / casserole. 40, Undertake a tasting session and focus into product attributes like 41) Appearance - Volume, expansion of the corn (floweriness) etc 2) Crunchiness 3) Texture 44) Dispersion of salt 5) Overall likeabilty of the product ‘A similar test can also be done with the flavoured varieties where flavour dosage details are given in the following section, This is # sure, time-tested, easy and the best method to confirm the suitability of the flavours for use in product. Controlled Document DO NOT PHOTOCOPY CONTROLLED copy ‘Agro Tech Foods Limited, 31, Sarojint Devi Marg, ‘Secunderabad. 500003 ——— Kgro Tech Foods timited | Superceding : None Rand HAY -CHO | Page 20 of 15 | Compendium of Analytical Test Methods Released : 20/MarchiU AM 017 : Total Ash Content Objective: To determine ash content in the food sample. Principk ‘Ash content is a measure of minerals present inthe food sample, Ash in any food is the inorganic residue remaining ater the organic matter has been bum. The sample is ashed to get id of the organic mater. Equipment: 1. Mufle Fumace 2. Electronic Balance 3. Dessicator 4. Silica Crucible Weigh 5 gm of sample in a weighed silica crucible. The sample is ignited on flame until the fame ceases. Ashing is carried out in a muffle furnace at 600 degree Centigrade unt) the ash is white in colour. After ashing, the crucible Is removed, cooled in a dessicator and weighed. Calculation: (WLof crucible + ash) ~ (Wt of empty crucible) Ash = x 100 {as is basis) Weight of the sample (WLof crucible + ash) - (Wt of empty crucible) Ash = ——— X10 (dry basis) ‘Weight of the sample ~ {(Wt of sample x Moisture%)/100} Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document Secunderabad. 500003 (00 NOT PHOTOCOPY CONTROLLED COPY Compendium of Analytical Test Methods Agro Tech Foods Limited ‘Superceding : None [on and Rao -cH0 [Pn 27 of Th ‘AM 018 : Acid Insoluble Ash Content Principle: Acid Insoluble Ash is an ing JT Sane cataract a ia proper quality/cleaning of wheat duo to stone particles ontering the atta during grinding process. The sample is fist usw to remove organic matter, vuYyUY D ‘washed in dilute aci, filered through ashiess fter paper and re-shed to estimate the acid insoluble ash, 3 Equipments: D 1. Muffle Fumace 2. Electronic Balance 3 3. Dessicator 4. Silica Crucible ey 5. Conical Flask 6. Funnel 3 7. .Phpaper ) 8. “Whatman fter paper No, 42 (Ashiess) > Reagents: ) OS NHCI 2 Procedure: > Weigh 5 om of sample in a weighed silica crucible. The sample is ignited on flame unt the flame cease: Ashing is carried out in & muffle furace at 600 degree Centigrade unill the ash is white in colour. After > ashing, the crucibe is removed, caoled in # dessicator and weighed. 25 mi of 0.5 N HCI is added to the ash, The solution is fitered using Whatman fiter paper No 42 (Ashless). The crucible and fter paper is ) washed with distiled water until the acid is removed completely. Ph paper is used to check if the filter paper Is free from acid, ‘Tho acid free fiter paper is ignited on a flame ceases. Ashing of the filer paper was carried out in a muffle furnace at 600 deg C unt the ash is white in colour. Ash is removed from the furnace, cooled in a ) dessicator and weighed. Calculation: (of crucible + acid insoluble ash) ~ (Wt of empty crucible) > %Ash = tne — X 100 5 (ass basis) Weight ofthe sample > (Wt of crucible + acid insoluble ash ~ (Wt of empty crucible) % Ash = x 100 (dry basis) Weight ofthe sample — (Wt of sarnpe x Meisture%4y'100) > ; Agro Tech Foods Limited, 31, Sarojinl Devi Marg, Controlled Document Secunderabad, 500003 DONOT PHOTOCOPY CONTROLLED COPY Compendium of Analytical Test Methous Agro Tech Foods Limited Released : 20/March/05 uprcedng: Nove [OAenaRa-cH0 | Fuge aiTS AM 019 : p-Anisidine Value Determination Definition: of the oil in 100 ML of a mixture uf solvent solution containing 1 reagent according to the method described. Scop This standard describes a method for the determination of the amount of aldehydes (principally 2- alkenals) inthe oils and fats of vegetable and animal Principle: Reaction in an acetic solution of the aldehyde compounds in an oll and P-Anisidine and then determination of absorbency at 350 NM. Apparatus: |. 10 ML minimum test tubes, with ground glass stoppers 25 ML graduated flasks ‘Automatic pipette or automatic burette Spectrophotometer suitable for observation at 350Nm 41.00 (+/-0.01) CM glass cells, the two cells of each pair must be identical Volumetric flask SOML 1 2 3 4 5. 6 agents: Isooctane (2, 2, 4-trimethy! pentane), optically clear Glacial acetic acid, analytical quality alytical reagent quality 2. 5 g/l solution in glacial acetic acid to be perfectly clear and dry. Weigh 0. 5 - 4 grams of the sample, to the nearest 0.0001 gm into a volumetric flask. Dissolve and dilute with Isooctane . Measure the absorbency( Ab) of the solution at 360 NM in a cell with the Spectrophotometer, using reference cell filed with blank. Pipelte exactly SML of {he fat solution into one test tube and exactly SMI of the solvent inio a second test tube by means of aulomalic pipette. Add exactly 1 ML of the P-ansidine reagont to each tube and shake woll, Afler exactly 10 minutes measure the Absorbance (As) of the solution in the fist test tube in a coll at 350 NM, using the solution from the second test tube as a blank in the reference cel Calculation: PAV = 25 X(1.2As-Ab) M Where, ‘As = Absorbeney of the fat solution after reaction with P-ansidine ssorbency if the solution of the fat M.'s the mass in grams of the test portion Note: 1. In the presence of acetic acid, P-ansidine reacts with aldehyde compounds in oils or fats. The intensity of colour of the yellowish reaction products formed depends not only on the mount of ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document Secunderabad. 500003 DO NOT PHOTOCOPY CONTROLLED COPY ) aw Yau 5 Compendium of Analytical Test Methods Agro Tech Foods Limited Faleaned2aMrev0s [Supereding:None [Oana RAD-CHO [Pogo of aldehydle compounds present but also on their structure. It has been found that a double bond in the carbon chain conjugated with the carbonyl double bond increases the molar absorbency four or five times. This means that 2-alkenals, especially, will contribute substantially to the value found amounts of oxidised fatty acid will not dissolve completely in N-hexane. For such ols isooctane ‘should be used as the solvent. the absorbency of the solvent used (\sooctane or N-hexane) ‘measure in a 1.00 cm cell between 300 and 380 NM, must be nil or nearly nil. The commercial product can be freed from absorptive material by percolating i through a glass column (2-5 cm intemal diameter, and [Link] long) filed with sila gel 3, The reaction between P-ansidine and aldehydes involves the formation of water. Hence, the presence of moisture in any of the reagents or in the sample leads to incomplete reaction and, consequently low values. Since glacial acetic acid is highly hygroscope, itis essential to check its ‘moisture content by a Kart Fisher determination. If the content exceeds 0.1% the acetic acid must be discarded. 4. In storage, P-ansidine tands to darken as a result of oxidation. A discoloured reagent can be reducad and discoloured as follows dissolve 40 grams of P-ansidine in 1 lie of water at 75 c add 2 ‘grams of sodium sulphite and 20 gr. of active carbon and stir for § minutes. Then fier through a double filer paper. If carbon passes through, repeat filtration. Cool the filtered solution to about 0 deg. C. Allow to stand af this temperature for at least 4 hours, or preferably overnight. Filter off the crystallized P-ansidine and wash with a small amount of water at a temperature of about 0 deg.C. After drying In a vacuum desiccator, transfer the crystals into a brown glass botlle. I stored in dark and at low temperature, the crystals obtained should not darken appreciably during tyear. '5, Reagent solutions having an absorbency greater than 0. 2, when measured in a 1 cm cell at 350 'NM against Isooctane or N-hexane as a blank should be discarded. Reference: Standard Methods For The Analysis Of Oils, Fats And Derivatives : Page No 211 ‘Author : Hautfenne, University Catholic De Louvain Agro Tech Foods Limited, 31, Sarojin! Devi Marg, Controlled Document Secunderabad. 500003 D0 NoT PHOTOCOPY CONTROLLED COPY 71BHA Content Determine eh eee A TBHS ppm Rapin dt dA by Spectra photornttore melisd eae Aa Whim att Gaonets having [ov Colo [Sem jroctaated — Aopponel Teboe 1D Howl Div Speeborit © 0 qubew le Dimetty] Aono Cama), remand, Kett, N- Butend oon [apne ped Temnt eeetlans ) ° Spjecchwt ? Go determine hs preesee take ot andadd Sm! 4 Dianella arin » glen bebe Flaw add Jol checholse ct emists' be + eeu © : Fame Sot pyar Shy 4 (gant WR Anck Shee Iran Clown Caw the top lage Of I tobe Uz Kagel to Chawel Pe bch ae ead a g THe Allow ee te ee Pramtfor tte Sup ernoet leap dots Tee 1" gparty cots Tham Prmrmedatty — pode te uy. abtovbtues inte yee Clots al- Goo men WIR per blak boraie ve of pagan And Crrelee Rrra — Cal rretren geek te he Tate gpm lence joke Mh we he ms tons ree the Heme g Seton” Chau nt be mnere Mon 1S mm aa the c : pant Letes (oration ett” by nalt S de> docetspd — Cobore 2 Supe : vere Compendium of Analytical Test Methods Agro Tech Foods Limited sara auntcnas —[Supaceding nino [@dandRa-chO | ago 173 AM 021 : Lime Powder Analysis Objective > Totoletmine ine avaliable lime {as CaO) by loging meted, Scope: ‘This method is applicable for determining the available lime in the given sample. Applicability : ‘Applicable for routine analysis { This is a prescribed BIS method 1514:1990) Apparatus : 4. 250 ml Stoppered Conical flask 2. 100 mL Beaker 3, 600 mL Volumetric ask. 4. 25 mL Pipette 5. 80 mL Buretio. Reagents: 0.1 N Standard Sodium Thiosulphate solution recently standardized 0.4 N Standard lodine Solution recently standardized against standard sodium thiosulphate solution Starch Indicator Solution: Triturate 5g starch and 0.01 9 of Mercuric lodide with 30 ml. of cold water and slowly pour it, with stirring, into 4 litre of boiting water. Boil for three minutes. Allow the solution to cool and: ‘decant off the supematant clear liquid, Procedure ‘Take 1 g of material, accurately weighed , in a glass sloppered conical flask and add about 30 mL. of bling water. Shake for 5 to 10 minutes. Coal the solution and add an amount of lodine solution sufficient to provide an excess of about 5 mL and slir occasionally until the lime has gone In solution, any insoluble silica present is easily distinguished from the milky appearing lime. When the solution of lime is complete ( about 10 minutes are required) , dilute the solution in a volumetric flask to 500 ml. Pipette out 25 ml of the solution and titrate the excess Iodine with standard sodium thiosulphate solution, adding starch indicator towards the end ofthe titration, Carry out a blank determination using the same amount of iodine solution as with the sample . Calculations: Available Lime ( as CaO) % = $6.08 ( V1-V2) N M Where : V1 = volume in ml of standard sodium thiosulphate solution used in the blank] V2 = volume in mi of standard sodium thiosulphate solution used with the material. N= normality of the standard sodium thiosulphate solution and M= mass in g, of the material taken for the test. Precautions : Use Pipette Bulb while pipetting out the solution. ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controlled Document ‘Secunderabad. 500003 00 NOT PHOTOCOPY CONTROLLED COPY ‘Compendium of Analytical Test Methods Agro Tech Foods Limited ‘Superceding : None ‘QA and R&D - CHO. ‘AM 022: Monosodlum Glutamate Purity Analysis, aye 320073 ‘To determine the purity of Monosodium Glutamate. Scope: ‘This method is applicable for Monosodium L. Glutamate salt (reference: BIS 9505-1980) Apparatus : 4, 250 ml Conical flask 2. Measuring cylinder — 100 mL. 3. Burette ~ 50 mL. Reagents: Glacial Acetic Acid Perchloric Acid ~ 0.1 N Procedure : Dissolve 250 mg of sample accurately weighed in 100 mi of glacial acetic acid. A few drops of water may ‘be added prior to the addition of acelic acid to effect faster dissolution of the sample. Titrate with 0.1N Perchloric acid in glacial acetic, determining the end point potentiometrically . Each mi of 0.1 mi of Perchloric acid is equivalent to 9.36 mg of Monosodium L glutamate ( CsHs0,NNa.H,0). Reference: BIS 9505-1980 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controtiedt Document Secunderabad. 500003, 00 NOT PHOTOCOPY CONTROLLED COPY Se Compendium of Analytical Test Methods Agro Tech Foods Limited a ti waa 610 [Pa tT AM 023 : Flash Point Definition: Scope Applicable to Sunflower/GroundnulSoya Solvent oils. Apparatus 1. Pensky Martin closed cup flash test, ASTM designation 0 93 ~ 80 ( AOCS ) either hand or motor stiring is allowable, but the latter is preferred. ‘The specified low ranga Pensky Martins centigrade and Fahrenheit Thermometers are replaced by a single centigrade or Fahrenheit Thormomeler as described below, 2. Thermometers 0-360 deg. C. closed cup flash point Thermometers. 3. Match box. Procedure: F'll the cup with the oll sample so that the top of the meniscus Is exactly atthe filing line, placa the lid on the cup and properly engage the locating devices. Insert the thermometer and suspend so thatthe bottom of the bulb Is exactly 1 % inches below the lave ofthe rim of the cup, which corresponds to the lovel of tha lower surface of the portion of the lid inside the cim_ ena Light the test flame and adjust so that itis the size of a bead approximately 5/32 inch in diameter. Al every 5 C rise in temperature, discontinue siting and apply the test flame by operating the device which controls the shutter and lowers the test flame in 0.5 second and leave in a lowered position for 1 Heat the sample so that the temperature increases not loss than § C not more than 6 C per minute, During the heating adjust the stiring device at one to two revolutions per second. Al every 5 C rise in temperature, discontinue stiring and apply the test flame by operating the device which controls the shutter and lowers the test flame in 0.5 second and leave in a lowered position for 1 Second, then quickly retum to raised or high position. As soon as the test flame has been relumed to the high position, resume stirring, The flash point is the temperature indicated on the thermometer. At the time of the flame application that Causes a distinct flash in the interior of the cup. The true flash must not be confused with the bivish halo that sometimes surrounds the test flame. Reference AOCS———---______cc 98-55 ‘Agro Tech Foods Limited, 31, Sarojini Devi Marg, Controtled Document Secunderabad. 500003 00 NoT PHOTOCOPY CONTROLLED copy

You might also like