Avis juridique important

Regulation (EEC) No 1061/69 of the Commission of 6 June 1969 specifying methods of analysis for the implementation of Regulation (EEC) No 1059/69 on the trade arrangements applicable to certain goods resulting from the processing of agricultural products Official Journal L 141 , 12/06/1969 P. 0024 - 0030 Danish special edition: Series I Chapter 1969(I) P. 0244 English special edition: Series I Chapter 1969(I) P. 0260 Spanish special edition: Chapter 02 Volume 1 P. 0042 Portuguese special edition Chapter 02 Volume 1 P. 0042

++++ ( 1 ) OJ N L 14 , 21 . 1 . 1969 , P . 1 . ( 2 ) OJ N L 141 , 12 . 6 . 1969 , P . 1 . ( 3 ) OJ N 195 , 28 . 10 . 1966 , P . 3361/66 . ( 4 ) OJ N 81 , 26 . 4 . 1967 , P . 1597/67 . ( 5 ) OJ N L 311 , 28 . 12 . 1968 , P . 1 . ( 6 ) OJ N 136 , 30 . 6 . 1967 , P . 2925/67 . REGULATION ( EEC ) N 1061/69 OF THE COMMISSION OF 6 JUNE 1969 SPECIFYING METHODS OF ANALYSIS FOR THE IMPLEMENTATION OF REGULATION ( EEC ) N 1059/69 ON THE TRADE ARRANGEMENTS APPLICABLE TO CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS THE COMMISSION OF THE EUROPEAN COMMUNITIES , HAVING REGARD TO THE TREATY ESTABLISHING THE EUROPEAN ECONOMIC COMMUNITY ; HAVING REGARD TO COUNCIL REGULATION ( EEC ) N 97/69 ( 1 ) OF 16 JANUARY 1969 ON MEASURES TO BE TAKEN FOR UNIFORM APPLICATION OF THE NOMENCLATURE OF THE COMMON CUSTOMS TARIFF , AND IN PARTICULAR ARTICLE 3 THEREOF ; WHEREAS , IN ORDER TO ENSURE THAT GOODS COVERED BY COUNCIL REGULATION ( EEC ) N 1059/69 ( 2 ) OF 28 MAY 1969 LAYING DOWN THE TRADE ARRANGEMENTS APPLICABLE TO CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS ARE DEALT WITH UNIFORMLY ON IMPORT INTO THE COMMUNITY , IT IS NECESSARY TO SPECIFY METHODS OF ANALYSIS AND OTHER TECHNICAL PROVISIONS REQUIRED EITHER TO IDENTIFY CERTAIN GOODS OR TO DETERMINE THEIR COMPOSITION ; WHEREAS , IN ACCORDANCE WITH ARTICLE 4 ( 2 ) OF THAT REGULATION , SUCH METHODS OF ANALYSIS AND OTHER TECHNICAL PROVISIONS MUST BE ADOPTED IN ACCORDANCE WITH THE PROCEDURE LAID DOWN IN ARTICLE 3 ( 2 ) AND ( 3 ) OF REGULATION ( EEC ) N 97/69 ; WHEREAS REGULATION ( EEC ) N 1059/69 REPLACES COUNCIL REGULATION N 160/66/EEC ( 3 ) OF 27 OCTOBER 1966 INTRODUCING TRADE ARRANGEMENTS IN RESPECT OF CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS ; WHEREAS , FOR THE PURPOSE OF IMPLEMENTING THIS LATTER REGULATION , METHODS OF ANALYSIS WERE FIXED BY COUNCIL REGULATION N 83/67/EEC ( 4 ) OF 18 APRIL 1967 ESTABLISHING TARIFF SPECIFICATIONS RELATING TO GOODS COVERED BY COUNCIL REGULATION N 160/66/EEC AND DETERMINING THE FIXED COMPONENTS APPLICABLE TO SUCH GOODS AND THE QUANTITIES OF BASIC PRODUCTS TO BE TAKEN AS HAVING BEEN USED IN THEIR MANUFACTURE , AS LAST AMENDED BY REGULATION ( EEC ) N 2121/68 ( 5 ) ; WHEREAS , SUBJECT TO CERTAIN CHANGES WHICH HAVE PROVED NECESSARY IN PRACTICE , THOSE METHODS OF ANALYSIS SHOULD CONTINUE TO BE APPLIED ; WHEREAS , WITH REGARD TO THE DETECTION OF COMMON WHEAT FLOUR OR MEAL IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS , IT IS , HOWEVER , ADVISABLE TO ADOPT A NEW METHOD ENSURING MORE ACCURATE RESULTS ; WHEREAS THE PROVISIONS OF THIS REGULATION ARE IN ACCORDANCE WITH THE OPINION OF THE COMMITTEE ON THE COMMON CUSTOMS TARIFF NOMENCLATURE ; HAS ADOPTED THIS REGULATION : ARTICLE 1 1 . WHERE CLASSIFICATION OF GOODS REFERRED TO IN ARTICLE 1 OF REGULATION ( EEC ) N 1059/69 UNDER ONE OR OTHER OF THE SUBHEADINGS OF THE COMMON CUSTOMS TARIFF DEPENDS ON THE STARCH CONTENT BY WEIGHT , SUCH CONTENT SHALL BE DETERMINED BY REFERENCE TO THE QUANTITY OF STARCH IN THE ANHYDROUS STATE CONTAINED IN SUCH GOODS . 2 . THE STARCH CONTENT BY WEIGHT OF GOODS SHALL BE ASCERTAINED BY THE MODIFIED EWERS POLARIMETRIC METHOD AS SET OUT IN THE ANNEX TO COMMISSION REGULATION N 228/67/EEC ( 6 ) OF 28 JUNE 1967 ON THE DETERMINATION OF THE STARCH CONTENT OF COMPOUND FEEDING-STUFFS , THE STARCH AND ASH CONTENT OF BRANS AND THE DENATURING OF FLOUR OF MANIOC AND OF OTHER ROOTS . HOWEVER , WHERE THE GOODS IN QUESTION CONTAIN STARCHES OTHER THAN NATIVE BUT DO NOT ALSO CONTAIN SUCROSE OR INVERT SUGAR , THE STARCH CONTENT BY WEIGHT OF SUCH GOODS SHALL BE ASCERTAINED BY THE SACCHARIFICATION METHOD SET OUT IN ANNEX I HERETO . FOR PURPOSES OF IMPLEMENTATION OF THIS PARAGRAPH , DEXTRINS SHALL BE TREATED AS STARCHES OTHER THAN NATIVE . ARTICLE 2 FOR THE PURPOSE OF ASCERTAINING WHETHER COMMON WHEAT FLOUR OR MEAL IS PRESENT IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS FALLING WITHIN HEADING N 19.03 OF THE COMMON CUSTOMS TARIFF , THE METHOD SET OUT IN ANNEX II SHALL BE EMPLOYED . ARTICLE 3 THE MILKFAT CONTENT BY WEIGHT OF A PRODUCT SHALL BE ASCERTAINED BY THE METHOD SET OUT IN ANNEX III . ARTICLE 4 THE MANNITOL CONTENT OF PRODUCTS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED BY REFERENCE TO THE SORBITOL CONTENT , SHALL BE ASCERTAINED BY THE METHOD SET OUT IN ANNEX IV . ARTICLE 5 THIS REGULATION SHALL ENTER INTO FORCE ON 1 JULY 1969 . THIS REGULATION SHALL BE BINDING IN ITS ENTIRETY AND DIRECTLY APPLICABLE IN ALL MEMBER STATES . DONE AT BRUSSELS , 6 JUNE 1969 . FOR THE COMMISSION THE PRESIDENT JEAN REY ANNEX I DETERMINATION OF STARCH BY THE SACCHARIFICATION METHOD I . PRINCIPLE STARCH IS CONVERTED BY ACID HYDROLYSIS INTO REDUCING SUGARS WHICH ARE DETERMINED BY VOLUME USING FEHLING'S SOLUTION . II . APPARATUS AND REAGENTS 1 . 250 ML FLASK 2 . 200 ML GRADUATED FLASK 3 . 25 ML GRADUATED BURETTE 4 . HYDROCHLORIC ACID AT 1 * 19 DENSITY 5 . POTASSIUM HYDROXIDE SOLUTION 6 . DECOLOURISING CHARCOAL 7 . FEHLING'S SOLUTION 8 . METHYLENE BLUE SOLUTION ( 1 % ) III . METHOD INTO A 250 ML FLASK PLACE A SAMPLE CONTAINING ABOUT 1 G OF STARCH . ADD 100 ML OF DISTILLED WATER AND 2 ML OF HYDROCHLORIC ACID . BRING TO THE BOIL AND REFLUX FOR THREE HOURS . TRANSFER THE CONTENTS OF THE FLASK AND RINSINGS INTO A 200 ML GRADUATED FLASK . COOL AND NEARLY NEUTRALISE WITH POTASSIUM HYDROXIDE SOLUTION . ADD DISTILLED WATER TO 200 ML AND FILTER THROUGH A LITTLE DECOLOURISING CHARCOAL . THEN POUR THE SOLUTION INTO A GRADUATED BURETTE AND REDUCE 10 ML OF FEHLING'S SOLUTION BY THE FOLLOWING METHOD : INTO A FLAT-BOTTOMED FLASK OF ABOUT 250 ML POUR 10 ML OF FEHLING'S SOLUTION ( 5 ML OF SOLUTION A AND 5 ML OF SOLUTION B ) . SHAKE UNTIL CLEAR AND ADD 40 ML OF DISTILLED WATER AND A SMALL QUANTITY OF QUARTZ OR PUMICE . PLACE THE FLASK ON A SQUARE ASBESTOS PLATE WITH A ROUND HOLE OF ABOUT 6 CM DIAMETER IN THE CENTRE , THE ASBESTOS IN TURN RESTING ON A PIECE OF WIRE GAUZE . HEAT THE FLASK AT SUCH A RATE THAT THE LIQUID BEGINS BOILING AFTER ABOUT TWO MINUTES . FROM THE BURETTE , ADD TO THE BOILING LIQUID SUCCESSIVE QUANTITIES OF THE SUGAR SOLUTION UNTIL THE BLUE COLOUR OF THE FEHLING'S SOLUTION BECOMES HARDLY DISCERNIBLE ; THEN ADD 2 OR 3 DROPS OF METHYLENE BLUE SOLUTION AS INDICATOR , AND COMPLETE THE TITRATION BY ADDING FURTHER QUANTITIES OF THE SUGAR SOLUTION , DROP BY DROP , UNTIL THE BLUE COLOUR OF THE INDICATOR DISAPPEARS . FOR GREATER ACCURACY REPEAT THE TITRATION UNDER THE SAME CONDITIONS , BUT ADDING WITHOUT A BREAK ALMOST ALL THE SUGAR SOLUTION REQUIRED TO REDUCE THE FEHLING'S SOLUTION . IN THIS SECOND TITRATION , THE REDUCTION OF THE FEHLING'S SOLUTION SHOULD OCCUR WITHIN THREE MINUTES . THE PERCENTAGE BY WEIGHT OF STARCH IN THE SAMPLE IS DETERMINED BY MEANS OF THE FOLLOWING FORMULA : ( SEE O.J . ) WHERE NECESSARY , THE STARCH CONTENT SO OBTAINED IS CORRECTED BY DEDUCTING THE SUGARS PREVIOUSLY EXISTING IN THE SAMPLE CALCULATED AS STARCH . IV . PREPARATION OF FEHLING'S SOLUTIONS SOLUTION A : IN A GRADUATED FLASK DISSOLVE 69 * 278 G OF PURE CRYSTALLISED COPPER SULPHATE _ ANALYTICAL REAGENT ( CUSO4 * 5 H2O ) _ FREE FROM IRON IN DISTILLED WATER AND BRING THE VOLUME TO 1 LITRE WITH DISTILLED WATER . THE CORRECT STRENGTH OF THIS SOLUTION MUST BE VERIFIED BY A QUANTITATIVE DETERMINATION OF THE COPPER . SOLUTION B : IN A GRADUATED FLASK DISSOLVE 100 G OF SODIUM HYDROXIDE AND 346 G OF DOUBLE SODIUM POTASSIUM TARTRATE ( ROCHELLE SALT ) IN DISTILLED WATER AND BRING THE VOLUME TO 1 LITRE WITH DISTILLED WATER . THE TWO SOLUTIONS A AND B MUST BE MIXED IN EQUAL QUANTITIES IMMEDIATELY BEFORE USE . 10 ML OF FEHLING'S SOLUTION ( 5 ML OF SOLUTION A AND 5 ML OF SOLUTION B ) IS COMPLETELY REDUCED , UNDER THE CONDITIONS DESCRIBED AT III , BY 0 * 04945 G OF ANHYDROUS DEXTROSE . ANNEX II DETECTION OF COMMON WHEAT FLOUR OR MEAL IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS ( PASTA ) ( BY THE YOUNG AND GILLES METHOD , MODIFIED BY BERNAERTS AND GRUNER ) I . PRINCIPLE AN EXTRACT OF THE SAMPLE OF THE PASTA FOR ANALYSIS IS PREPARED BY USING A NON-POLAR SOLVENT . THIS EXTRACT IS CHROMATOGRAPHED ON A THIN LAYER OF SILICA GEL SO AS TO SEPARATE THE STEROLS PRESENT IN VARIOUS BAND FORM FRACTIONS . ACCORDING TO THE NUMBER OF BRIGHTLY COLOURED BANDS IT IS POSSIBLE TO DETERMINE WHETHER THE PRODUCT UNDER EXAMINATION HAS BEEN MANUFACTURED EXCLUSIVELY FROM DURUM WHEAT OR COMMON WHEAT , OR FROM A MIXTURE OF THE TWO . IT IS ALSO POSSIBLE TO DETERMINE WHETHER EGGS HAVE BEEN ADDED . II . APPARATUS AND REAGENTS 1 . HOMOGENISER OR GRINDER TO OBTAIN A GRIST THAT WILL PASS THROUGH A STANDARD SIEVE WITH A 0 * 200 MM MESH 2 . STANDARD SIEVE WITH A 0 * 200 MM MESH 3 . EVAPORATOR WITH A WATER BATH FOR EVAPORATION UNDER REDUCED PRESSURE 4 . GLASS PLATE , ALUMINIUM SHEET OR OTHER APPROPRIATE BACKING MEASURING 20 CM BY 20 CM COVERED WITH A THIN LAYER OF SILICA GEL . IF THE THIN LAYER HAS TO BE PREPARED , SILICA GEL MIXED WITH ABOUT 13 % PLASTER SHOULD BE USED , AND IT SHOULD BE APPLIED IN A 0 * 25 MM LAYER WITH SUITABLE APPARATUS IN ACCORDANCE WITH THE MANUFACTURER'S INSTRUCTIONS 5 . MICROPIPETTE FOR MEASURING 20 MICROLITRES 6 . CONTAINER WITH LID SUITABLE FOR THE DEVELOPMENT OF CHROMATOGRAMS 7 . ATOMISER 8 . PETROLEUM ETHER WITH A BOILING POINT BETWEEN 40 AND 60 C , REDISTILLED BEFORE USE 9 . ANHYDROUS ETHYL ETHER FOR ANALYSIS 10 . CARBON TETRACHLORIDE FOR CHROMATOGRAPHY , REDISTILLED BEFORE USE 11 . PHOSPHOMOLYBDIC ACID FOR ANALYSIS 12 . 94 ETHYL ALCOHOL III . METHOD GRIND ABOUT 20 G OF THE SAMPLE FOR ANALYSIS SO THAT ALL OF IT PASSES THROUGH THE SIEVE . PUT THE SAMPLE IN AN ERLENMEYER FLASK AND COVER WITH 150 ML PETROLEUM ETHER . LEAVE AT NORMAL TEMPERATURE UNTIL THE FOLLOWING DAY . SHAKE FROM TIME TO TIME . THEN FILTER ON A BUECHNER FUNNEL FITTED WITH A FILTERING AID OR ON A SINTERED FILTER . GRADUALLY TRANSFER THE CLEAR SOLUTION THUS OBTAINED INTO A 100 ML CALIBRATED FLASK . EVAPORATE THE SOLVENT UNDER REDUCED PRESSURE BY HEATING THE FLASK IN A WATER BATH AT 40 _ 50 C . WHEN THE SOLVENT HAS EVAPORATED , HEAT UNDER REDUCED PRESSURE FOR A FURTHER TEN MINUTES . WHEN THE FLASK HAS COOLED , DETERMINE THE WEIGHT OF THE EXTRACT . DILUTE THE EXTRACT IN ETHYL ETHER ON THE BASIS OF 1 ML ETHYL ETHER PER 60 MG OF EXTRACT . ACIVATE THE THIN LAYERS BY BRINGING THEM TO 130 C FOR THREE HOURS . LEAVE TO COOL IN A DESICCATOR CONTAINING SILICA GEL . PLATES WHICH ARE NOT USED IMMEDIATELY CAN BE PRESERVED IN THE SAME DESICCATOR . APPLY , DROP BY DROP , 20 MICROLITRES OF THE CLEAR SOLUTION TO FORM A BAND OF CONSTANT WIDTH AND 3 CM IN LENGTH ON A LAYER PREFERABLY NEWLY ACTIVATED . LET THE SOLVENT EVAPORATE . DEVELOP THE CHROMATOGRAM UNDER NORMAL TEMPERATURE WITH CARBON TETRACHLORIDE USING A CHROMATOGRAPHIC CONTAINER THE WALLS OF WHICH ARE COVERED WITH FILTER PAPER SOAKED IN SOLVENT . AFTER ABOUT AN HOUR THE SOLVENT WILL REACH A HEIGHT OF 18 CM . REMOVE THE PLATE AND LEAVE THE SOLVENT TO EVAPORATE IN THE OPEN . FOR BETTER SEPARATION OF THE BANDS , DEVELOP THE CHROMATOGRAM A SECOND TIME . AGAIN LET THE SOLVENT EVAPORATE IN THE OPEN . SPRAY THE THIN LAYER OF SILICA GEL WITH A SOLUTION OF 20 % PHOSPHOMOLYBDIC ACID IN ETHYL ALCOHOL . THE COLOUR OF THE LAYER MUST BE A UNIFORM YELLOW . DEVELOP THE BANDS BY HEATING THE SPRAYED PLATE AT 110 C FOR FIVE MINUTES . IV . INTERPRETATION OF THE CHROMATOGRAM IF THE CHROMATOGRAM SHOWS A SINGLE MAIN BRIGHTLY COLOURED BAND WITH AN RF OF ABOUT 0 * 4 _ 0 * 5 , THE WHEAT USED FOR THE MANUFACTURE OF THE PASTA IN QUESTION IS DURUM WHEAT . IF , ON THE OTHER HAND , TWO MAIN BANDS OF EQUAL BRIGHTNESS APPEAR , THE RAW MATERIAL USED IS COMMON WHEAT . MIXTURES OF DURUM WHEAT AND COMMON WHEAT CAN BE ASSESSED BY AN EVALUATION OF THE RELATIVE BRIGHTNESS OF THE TWO BANDS . IF THERE ARE THREE BANDS ( 2 BANDS AT THE HEIGHT WHERE THE MAIN BANDS FOR COMMON WHEAT ARE TO BE FOUND , WITH A FURTHER BAND BETWEEN THEM ) EGGS HAVE BEEN ADDED TO PASTA . IN THIS CASE , THE RAW MATERIAL USED IS DURUM WHEAT IF THE MIDDLE BAND IS BRIGHTER THAN THE UPPER BAND . ON THE OTHER HAND , IF THE UPPER BAND IS BRIGHTER THAN THE MIDDLE BAND , THE RAW MATERIAL USED IS COMMON WHEAT . ANNEX III DETERMINATION OF MILKFAT CONTENT I . PRINCIPLE AFTER DETERMINING THE PERCENTAGE BY WEIGHT OF TOTAL FAT CONTAINED IN THE SAMPLE , THE BUTYRIC INDEX OF THIS TOTAL FAT CONTENT SHOULD BE DETERMINED ; THE MILKFAT CONTENT CAN THEN BE DETERMINED BY USING 20 AS THE AVERAGE BUTYRIC INDEX OF MILKFAT . II . APPARATUS AND REAGENTS 1 . DISTILLATION APPARATUS WITH REFRIGERATED REFLUX CONDENSER 2 . BECKEL TUBES 3 . ALCOHOLIC SOLUTION OF POTASSIUM HYDROXIDE PREPARED BY MIXING 40 ML OF POTASH SOLUTION ( D = 1 * 5 ) WITH 40 ML DISTILLED WATER , AND DILUTING TO ONE LITRE WITH 95 _ 96 % ALCOHOL 4 . PURE GLYCERINE ( D = 1 * 23 ) 5 . SATURATED SOLUTION OF POTASSIUM SULPHATE 6 . SULPHURIC ACID DILUTED ( 1 VOLUME CONCENTRATED SULPHURIC ACID ( D = 1 * 84 ) AND 3 VOLUMES DISTILLED WATER ) 7 . COCONUT SOAP SOLUTION , OBTAINED AS FOLLOWS : IN A 1 LITRE FLASK , SAPONIFY 50 G OF PURE COCONUT FAT , REFINED BUT NOT HARDENED ( MELTING POINT 24 _ 26 C ) , WITH 50 G OF GLYCERINE , 15 G KOH AND 20 ML OF WATER . AFTER COOLING TO BELOW 100 C , DILUTE TO 500 ML 8 . 1 % ALCOHOLIC SOLUTION OF PHENOLPHTHALEIN 9 . AQUEOUS 0 * 01 N SOLUTION OF SODIUM HYDROXIDE III . METHOD FIRST DETERMINE THE PERCENTAGE BY WEIGHT OF THE TOTAL FAT CONTENT OF THE SAMPLE TO BE ANALYSED . THEN DETERMINE THE BUTYRIC INDEX OF THIS TOTAL FAT CONTENT BY THE GROSSFELD METHOD , AS FOLLOWS : WEIGH ACCURATELY 500 TO 550 MG OF FAT AND TRANSFER IT INTO A 50 ML FLAT-BOTTOMED FLASK WITH 5 ML OF ALCOHOLIC SOLUTION OF POTASSIUM HYDROXIDE . KEEP AT MODERATE BOIL UNDER REFLUX . WHEN THE FAT HAS BEEN COMPLETELY SAPONIFIED , REMOVE REFRIGERATED REFLUX CONDENSER , AND USING A GRADUATED PIPETTE ADD 1 ML OF GLYCERINE . CONTINUE TO HEAT UNTIL MOST OF THE ALCOHOL HAS EVAPORATED ( THIS IS INDICATED BY THE APPEARANCE OF HEAVY FROTHING ) . TO EVAPORATE THE REST OF THE ALCOHOL , PLACE THE FLASK IN AN OVEN AT 100 C FOR ONE HOUR . IMMEDIATELY AFTER REMOVAL FROM THE OVEN ADD , STIRRING WELL , 15 ML OF SATURATED SOLUTION OF POTASSIUM SULPHATE . ALLOW TO COOL TO 20 C , THEN ADD SUCCESSIVELY ( STIRRING EACH TIME ) 0 * 5 ML OF DILUTE H2SO4 , 1 ML OF THE COCONUT SOAP SOLUTION AND ABOUT 0 * 1 G OF PURIFIED KIESELGUHR . FILTER THROUGH A FLUTED FILTER 9 CM IN DIAMETER INTO THE BECKEL TUBE ( FIG . 1 ) UNTIL THE FILTRATE REACHES THE 12 * 5 ML LEVEL . IT MAY BE NECESSARY TO COMPRESS THE RESIDUE ONTO THE FILTER WITH A STIRRING ROD TO OBTAIN SUFFICIENT FILTRATE . TRANSFER THE FILTRATE INTO A 100 ML FLASK AND RINSE THE BECKEL TUBE WITH 5 ML OF WATER . POUR THE RINSINGS ALSO INTO THE BOTTLE . ADD FINE PUMICE AND DISTIL 11 ML INTO THE RECIPIENT SHOWN ( FIG . 2 ) . TRANSFER TO A BEAKER , ADD 1 TO 2 DROPS OF PHENOLPHTHALEIN SOLUTION , TITRATE WITH THE AQUEOUS SODIUM HYDROXIDE SOLUTION UNTIL A PERSISTENT RED COLOUR IS OBTAINED , RINSE THE TUBE WITH THIS NEUTRALISED SOLUTION AND REPEAT THE TITRATION UNTIL THE RED COLOUR REAPPEARS . THE BUTYRIC INDEX OF THE TOTAL FAT CONTENT IS CALCULATED BY MEANS OF THE FOLLOWING FORMULA : ( SEE O.J . ) ANNEX IV DETERMINATION OF THE MANNITOL CONTENT OF GOODS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED ON THE SORBITOL CONTENT I . PRINCIPLE GAS CHROMATOGRAPHY IS USED TO DETERMINE THE MANNITOL CONTENT OF GOODS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED ON THEIR SORBITOL CONTENT . FOR THAT PURPOSE NON-VOLATILE PRODUCTS OR THEIR ACETYLATED DERIVATIVES MUST FIRST BE PROCESSED . II . APPARATUS AND REAGENTS 1 . GAS CHROMATOGRAPH WITH FLAME-IONISATION DETECTOR 2 . COLUMN FILLED WITH " 5 % XE 60 ON AEROPAK 30 " ( GRANULATION 80 _ 100 MESH ) 3 . ANHYDROUS PYRIDINE FOR ANALYSIS 4 . ACETONE FOR ANALYSIS 5 . ACETIC ANHYDRIDE FOR ANALYSIS 6 . 25 ML CALIBRATED FLASKS III . METHOD ( A ) PREPARATION OF THE ACETYLATED DERIVATIVES 1 . SOLID PRODUCTS WEIGH ABOUT 200 MG OF THE PRODUCT . BOIL FOR ONE HOUR WITH 3 ML PYRIDINE AND 3 ML ACETIC ANHYDRIDE SO THAT THE LIQUID FLOWS BACK AFTER CONDENSATION . LEAVE TO COOL AND BRING TO 250 ML WITH ACETONE . INJECT THIS SOLUTION IN THE CHROMATOGRAPH . 2 . PRODUCTS IN AQUEOUS SOLUTION WEIGH ABOUT 3 G OF THE PRODUCT . ADD 60 ML PYRIDINE . DISTIL UNTIL THE TEMPERATURE OF THE VAPOUR REACHES 115 . THEN ADD 30 ML ACETIC ANHYDRIDE AND BOIL FOR TWO HOURS SO THAT THE LIQUID FLOWS BACK AFTER CONDENSATION . LEAVE TO COOL AND BRING TO 250 ML WITH ACETONE . INJECT THIS SOLUTION IN THE CHROMATOGRAPH . ( B ) CONDITIONS REQUIRED TO CARRY OUT CHROMATOGRAPHY INJECTION TEMPERATURE : 300 C TEMPERATURE OF THE COLUMN : 210 C FLOW OF THE CARRIER GAS STREAM ( FOR INSTANCE NITROGEN ) : 25 ML / MINUTE HYDROGEN FLOW : 25 ML / MINUTE QUANTITY INJECTED : 1 MICROLITRE THE MANNITOL PEAK APPEARS FIRST , THEN THE SORBITOL PEAK . TO DETERMINE THE MANNITOL CONTENT OF THE GOODS UNDER ANALYSIS , CALCULATED ON THEIR SORBITOL CONTENT , SIMPLY CALCULATE THE RATIO OF THE AREA OF THE TWO PEAKS .

++++

( 1 ) OJ N L 14 , 21 . 1 . 1969 , P . 1 .

( 2 ) OJ N L 141 , 12 . 6 . 1969 , P . 1 .

( 3 ) OJ N 195 , 28 . 10 . 1966 , P . 3361/66 .

( 4 ) OJ N 81 , 26 . 4 . 1967 , P . 1597/67 .

( 5 ) OJ N L 311 , 28 . 12 . 1968 , P . 1 .

( 6 ) OJ N 136 , 30 . 6 . 1967 , P . 2925/67 .

REGULATION ( EEC ) N 1061/69 OF THE COMMISSION

OF 6 JUNE 1969

SPECIFYING METHODS OF ANALYSIS FOR THE IMPLEMENTATION OF REGULATION ( EEC ) N 1059/69 ON THE TRADE ARRANGEMENTS APPLICABLE TO CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS

THE COMMISSION OF THE EUROPEAN COMMUNITIES ,

HAVING REGARD TO THE TREATY ESTABLISHING THE EUROPEAN ECONOMIC COMMUNITY ;

HAVING REGARD TO COUNCIL REGULATION ( EEC ) N 97/69 ( 1 ) OF 16 JANUARY 1969 ON MEASURES TO BE TAKEN FOR UNIFORM APPLICATION OF THE NOMENCLATURE OF THE COMMON CUSTOMS TARIFF , AND IN PARTICULAR ARTICLE 3 THEREOF ;

WHEREAS , IN ORDER TO ENSURE THAT GOODS COVERED BY COUNCIL REGULATION ( EEC ) N 1059/69 ( 2 ) OF 28 MAY 1969 LAYING DOWN THE TRADE ARRANGEMENTS APPLICABLE TO CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS ARE DEALT WITH UNIFORMLY ON IMPORT INTO THE COMMUNITY , IT IS NECESSARY TO SPECIFY METHODS OF ANALYSIS AND OTHER TECHNICAL PROVISIONS REQUIRED EITHER TO IDENTIFY CERTAIN GOODS OR TO DETERMINE THEIR COMPOSITION ; WHEREAS , IN ACCORDANCE WITH ARTICLE 4 ( 2 ) OF THAT REGULATION , SUCH METHODS OF ANALYSIS AND OTHER TECHNICAL PROVISIONS MUST BE ADOPTED IN ACCORDANCE WITH THE PROCEDURE LAID DOWN IN ARTICLE 3 ( 2 ) AND ( 3 ) OF REGULATION ( EEC ) N 97/69 ;

WHEREAS REGULATION ( EEC ) N 1059/69 REPLACES COUNCIL REGULATION N 160/66/EEC ( 3 ) OF 27 OCTOBER 1966 INTRODUCING TRADE ARRANGEMENTS IN RESPECT OF CERTAIN GOODS RESULTING FROM THE PROCESSING OF AGRICULTURAL PRODUCTS ; WHEREAS , FOR THE PURPOSE OF IMPLEMENTING THIS LATTER REGULATION , METHODS OF ANALYSIS WERE FIXED BY COUNCIL REGULATION N 83/67/EEC ( 4 ) OF 18 APRIL 1967 ESTABLISHING TARIFF SPECIFICATIONS RELATING TO GOODS COVERED BY COUNCIL REGULATION N 160/66/EEC AND DETERMINING THE FIXED COMPONENTS APPLICABLE TO SUCH GOODS AND THE QUANTITIES OF BASIC PRODUCTS TO BE TAKEN AS HAVING BEEN USED IN THEIR MANUFACTURE , AS LAST AMENDED BY REGULATION ( EEC ) N 2121/68 ( 5 ) ; WHEREAS , SUBJECT TO CERTAIN CHANGES WHICH HAVE PROVED NECESSARY IN PRACTICE , THOSE METHODS OF ANALYSIS SHOULD CONTINUE TO BE APPLIED ; WHEREAS , WITH REGARD TO THE DETECTION OF COMMON WHEAT FLOUR OR MEAL IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS , IT IS , HOWEVER , ADVISABLE TO ADOPT A NEW METHOD ENSURING MORE ACCURATE RESULTS ;

WHEREAS THE PROVISIONS OF THIS REGULATION ARE IN ACCORDANCE WITH THE OPINION OF THE COMMITTEE ON THE COMMON CUSTOMS TARIFF NOMENCLATURE ;

HAS ADOPTED THIS REGULATION :

1 . WHERE CLASSIFICATION OF GOODS REFERRED TO IN ARTICLE 1 OF REGULATION ( EEC ) N 1059/69 UNDER ONE OR OTHER OF THE SUBHEADINGS OF THE COMMON CUSTOMS TARIFF DEPENDS ON THE STARCH CONTENT BY WEIGHT , SUCH CONTENT SHALL BE DETERMINED BY REFERENCE TO THE QUANTITY OF STARCH IN THE ANHYDROUS STATE CONTAINED IN SUCH GOODS .

2 . THE STARCH CONTENT BY WEIGHT OF GOODS SHALL BE ASCERTAINED BY THE MODIFIED EWERS POLARIMETRIC METHOD AS SET OUT IN THE ANNEX TO COMMISSION REGULATION N 228/67/EEC ( 6 ) OF 28 JUNE 1967 ON THE DETERMINATION OF THE STARCH CONTENT OF COMPOUND FEEDING-STUFFS , THE STARCH AND ASH CONTENT OF BRANS AND THE DENATURING OF FLOUR OF MANIOC AND OF OTHER ROOTS .

HOWEVER , WHERE THE GOODS IN QUESTION CONTAIN STARCHES OTHER THAN NATIVE BUT DO NOT ALSO CONTAIN SUCROSE OR INVERT SUGAR , THE STARCH CONTENT BY WEIGHT OF SUCH GOODS SHALL BE ASCERTAINED BY THE SACCHARIFICATION METHOD SET OUT IN ANNEX I HERETO .

FOR PURPOSES OF IMPLEMENTATION OF THIS PARAGRAPH , DEXTRINS SHALL BE TREATED AS STARCHES OTHER THAN NATIVE .

ARTICLE 2

FOR THE PURPOSE OF ASCERTAINING WHETHER COMMON WHEAT FLOUR OR MEAL IS PRESENT IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS FALLING WITHIN HEADING N 19.03 OF THE COMMON CUSTOMS TARIFF , THE METHOD SET OUT IN ANNEX II SHALL BE EMPLOYED .

THE MILKFAT CONTENT BY WEIGHT OF A PRODUCT SHALL BE ASCERTAINED BY THE METHOD SET OUT IN ANNEX III .

THE MANNITOL CONTENT OF PRODUCTS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED BY REFERENCE TO THE SORBITOL CONTENT , SHALL BE ASCERTAINED BY THE METHOD SET OUT IN ANNEX IV .

ARTICLE 5

THIS REGULATION SHALL ENTER INTO FORCE ON 1 JULY 1969 .

THIS REGULATION SHALL BE BINDING IN ITS ENTIRETY AND DIRECTLY APPLICABLE IN ALL MEMBER STATES .

DONE AT BRUSSELS , 6 JUNE 1969 .

FOR THE COMMISSION

THE PRESIDENT

JEAN REY

ANNEX I

DETERMINATION OF STARCH BY THE SACCHARIFICATION METHOD

I . PRINCIPLE

STARCH IS CONVERTED BY ACID HYDROLYSIS INTO REDUCING SUGARS WHICH ARE DETERMINED BY VOLUME USING FEHLING'S SOLUTION .

II . APPARATUS AND REAGENTS

1 . 250 ML FLASK

2 . 200 ML GRADUATED FLASK

3 . 25 ML GRADUATED BURETTE

4 . HYDROCHLORIC ACID AT 1 * 19 DENSITY

5 . POTASSIUM HYDROXIDE SOLUTION

6 . DECOLOURISING CHARCOAL

7 . FEHLING'S SOLUTION

8 . METHYLENE BLUE SOLUTION ( 1 % )

III . METHOD

INTO A 250 ML FLASK PLACE A SAMPLE CONTAINING ABOUT 1 G OF STARCH . ADD 100 ML OF DISTILLED WATER AND 2 ML OF HYDROCHLORIC ACID . BRING TO THE BOIL AND REFLUX FOR THREE HOURS .

TRANSFER THE CONTENTS OF THE FLASK AND RINSINGS INTO A 200 ML GRADUATED FLASK . COOL AND NEARLY NEUTRALISE WITH POTASSIUM HYDROXIDE SOLUTION . ADD DISTILLED WATER TO 200 ML AND FILTER THROUGH A LITTLE DECOLOURISING CHARCOAL .

THEN POUR THE SOLUTION INTO A GRADUATED BURETTE AND REDUCE 10 ML OF FEHLING'S SOLUTION BY THE FOLLOWING METHOD :

INTO A FLAT-BOTTOMED FLASK OF ABOUT 250 ML POUR 10 ML OF FEHLING'S SOLUTION ( 5 ML OF SOLUTION A AND 5 ML OF SOLUTION B ) . SHAKE UNTIL CLEAR AND ADD 40 ML OF DISTILLED WATER AND A SMALL QUANTITY OF QUARTZ OR PUMICE .

PLACE THE FLASK ON A SQUARE ASBESTOS PLATE WITH A ROUND HOLE OF ABOUT 6 CM DIAMETER IN THE CENTRE , THE ASBESTOS IN TURN RESTING ON A PIECE OF WIRE GAUZE . HEAT THE FLASK AT SUCH A RATE THAT THE LIQUID BEGINS BOILING AFTER ABOUT TWO MINUTES .

FROM THE BURETTE , ADD TO THE BOILING LIQUID SUCCESSIVE QUANTITIES OF THE SUGAR SOLUTION UNTIL THE BLUE COLOUR OF THE FEHLING'S SOLUTION BECOMES HARDLY DISCERNIBLE ; THEN ADD 2 OR 3 DROPS OF METHYLENE BLUE SOLUTION AS INDICATOR , AND COMPLETE THE TITRATION BY ADDING FURTHER QUANTITIES OF THE SUGAR SOLUTION , DROP BY DROP , UNTIL THE BLUE COLOUR OF THE INDICATOR DISAPPEARS .

FOR GREATER ACCURACY REPEAT THE TITRATION UNDER THE SAME CONDITIONS , BUT ADDING WITHOUT A BREAK ALMOST ALL THE SUGAR SOLUTION REQUIRED TO REDUCE THE FEHLING'S SOLUTION . IN THIS SECOND TITRATION , THE REDUCTION OF THE FEHLING'S SOLUTION SHOULD OCCUR WITHIN THREE MINUTES .

THE PERCENTAGE BY WEIGHT OF STARCH IN THE SAMPLE IS DETERMINED BY MEANS OF THE FOLLOWING FORMULA : ( SEE O.J . )

WHERE NECESSARY , THE STARCH CONTENT SO OBTAINED IS CORRECTED BY DEDUCTING THE SUGARS PREVIOUSLY EXISTING IN THE SAMPLE CALCULATED AS STARCH .

IV . PREPARATION OF FEHLING'S SOLUTIONS

SOLUTION A : IN A GRADUATED FLASK DISSOLVE 69 * 278 G OF PURE CRYSTALLISED COPPER SULPHATE _ ANALYTICAL REAGENT ( CUSO4 * 5 H2O ) _ FREE FROM IRON IN DISTILLED WATER AND BRING THE VOLUME TO 1 LITRE WITH DISTILLED WATER . THE CORRECT STRENGTH OF THIS SOLUTION MUST BE VERIFIED BY A QUANTITATIVE DETERMINATION OF THE COPPER .

SOLUTION B : IN A GRADUATED FLASK DISSOLVE 100 G OF SODIUM HYDROXIDE AND 346 G OF DOUBLE SODIUM POTASSIUM TARTRATE ( ROCHELLE SALT ) IN DISTILLED WATER AND BRING THE VOLUME TO 1 LITRE WITH DISTILLED WATER .

THE TWO SOLUTIONS A AND B MUST BE MIXED IN EQUAL QUANTITIES IMMEDIATELY BEFORE USE . 10 ML OF FEHLING'S SOLUTION ( 5 ML OF SOLUTION A AND 5 ML OF SOLUTION B ) IS COMPLETELY REDUCED , UNDER THE CONDITIONS DESCRIBED AT III , BY 0 * 04945 G OF ANHYDROUS DEXTROSE .

ANNEX II

DETECTION OF COMMON WHEAT FLOUR OR MEAL IN MACARONI , SPAGHETTI AND SIMILAR PRODUCTS ( PASTA )

( BY THE YOUNG AND GILLES METHOD , MODIFIED BY BERNAERTS AND GRUNER )

I . PRINCIPLE

AN EXTRACT OF THE SAMPLE OF THE PASTA FOR ANALYSIS IS PREPARED BY USING A NON-POLAR SOLVENT .

THIS EXTRACT IS CHROMATOGRAPHED ON A THIN LAYER OF SILICA GEL SO AS TO SEPARATE THE STEROLS PRESENT IN VARIOUS BAND FORM FRACTIONS .

ACCORDING TO THE NUMBER OF BRIGHTLY COLOURED BANDS IT IS POSSIBLE TO DETERMINE WHETHER THE PRODUCT UNDER EXAMINATION HAS BEEN MANUFACTURED EXCLUSIVELY FROM DURUM WHEAT OR COMMON WHEAT , OR FROM A MIXTURE OF THE TWO . IT IS ALSO POSSIBLE TO DETERMINE WHETHER EGGS HAVE BEEN ADDED .

II . APPARATUS AND REAGENTS

1 . HOMOGENISER OR GRINDER TO OBTAIN A GRIST THAT WILL PASS THROUGH A STANDARD SIEVE WITH A 0 * 200 MM MESH

2 . STANDARD SIEVE WITH A 0 * 200 MM MESH

3 . EVAPORATOR WITH A WATER BATH FOR EVAPORATION UNDER REDUCED PRESSURE

4 . GLASS PLATE , ALUMINIUM SHEET OR OTHER APPROPRIATE BACKING MEASURING 20 CM BY 20 CM COVERED WITH A THIN LAYER OF SILICA GEL . IF THE THIN LAYER HAS TO BE PREPARED , SILICA GEL MIXED WITH ABOUT 13 % PLASTER SHOULD BE USED , AND IT SHOULD BE APPLIED IN A 0 * 25 MM LAYER WITH SUITABLE APPARATUS IN ACCORDANCE WITH THE MANUFACTURER'S INSTRUCTIONS

5 . MICROPIPETTE FOR MEASURING 20 MICROLITRES

6 . CONTAINER WITH LID SUITABLE FOR THE DEVELOPMENT OF CHROMATOGRAMS

7 . ATOMISER

8 . PETROLEUM ETHER WITH A BOILING POINT BETWEEN 40 AND 60 C , REDISTILLED BEFORE USE

9 . ANHYDROUS ETHYL ETHER FOR ANALYSIS

10 . CARBON TETRACHLORIDE FOR CHROMATOGRAPHY , REDISTILLED BEFORE USE

11 . PHOSPHOMOLYBDIC ACID FOR ANALYSIS

12 . 94 ETHYL ALCOHOL

III . METHOD

GRIND ABOUT 20 G OF THE SAMPLE FOR ANALYSIS SO THAT ALL OF IT PASSES THROUGH THE SIEVE . PUT THE SAMPLE IN AN ERLENMEYER FLASK AND COVER WITH 150 ML PETROLEUM ETHER . LEAVE AT NORMAL TEMPERATURE UNTIL THE FOLLOWING DAY . SHAKE FROM TIME TO TIME .

THEN FILTER ON A BUECHNER FUNNEL FITTED WITH A FILTERING AID OR ON A SINTERED FILTER . GRADUALLY TRANSFER THE CLEAR SOLUTION THUS OBTAINED INTO A 100 ML CALIBRATED FLASK . EVAPORATE THE SOLVENT UNDER REDUCED PRESSURE BY HEATING THE FLASK IN A WATER BATH AT 40 _ 50 C . WHEN THE SOLVENT HAS EVAPORATED , HEAT UNDER REDUCED PRESSURE FOR A FURTHER TEN MINUTES .

WHEN THE FLASK HAS COOLED , DETERMINE THE WEIGHT OF THE EXTRACT . DILUTE THE EXTRACT IN ETHYL ETHER ON THE BASIS OF 1 ML ETHYL ETHER PER 60 MG OF EXTRACT .

ACIVATE THE THIN LAYERS BY BRINGING THEM TO 130 C FOR THREE HOURS . LEAVE TO COOL IN A DESICCATOR CONTAINING SILICA GEL . PLATES WHICH ARE NOT USED IMMEDIATELY CAN BE PRESERVED IN THE SAME DESICCATOR .

APPLY , DROP BY DROP , 20 MICROLITRES OF THE CLEAR SOLUTION TO FORM A BAND OF CONSTANT WIDTH AND 3 CM IN LENGTH ON A LAYER PREFERABLY NEWLY ACTIVATED . LET THE SOLVENT EVAPORATE .

DEVELOP THE CHROMATOGRAM UNDER NORMAL TEMPERATURE WITH CARBON TETRACHLORIDE USING A CHROMATOGRAPHIC CONTAINER THE WALLS OF WHICH ARE COVERED WITH FILTER PAPER SOAKED IN SOLVENT . AFTER ABOUT AN HOUR THE SOLVENT WILL REACH A HEIGHT OF 18 CM . REMOVE THE PLATE AND LEAVE THE SOLVENT TO EVAPORATE IN THE OPEN . FOR BETTER SEPARATION OF THE BANDS , DEVELOP THE CHROMATOGRAM A SECOND TIME . AGAIN LET THE SOLVENT EVAPORATE IN THE OPEN .

SPRAY THE THIN LAYER OF SILICA GEL WITH A SOLUTION OF 20 % PHOSPHOMOLYBDIC ACID IN ETHYL ALCOHOL . THE COLOUR OF THE LAYER MUST BE A UNIFORM YELLOW . DEVELOP THE BANDS BY HEATING THE SPRAYED PLATE AT 110 C FOR FIVE MINUTES .

IV . INTERPRETATION OF THE CHROMATOGRAM

IF THE CHROMATOGRAM SHOWS A SINGLE MAIN BRIGHTLY COLOURED BAND WITH AN RF OF ABOUT 0 * 4 _ 0 * 5 , THE WHEAT USED FOR THE MANUFACTURE OF THE PASTA IN QUESTION IS DURUM WHEAT . IF , ON THE OTHER HAND , TWO MAIN BANDS OF EQUAL BRIGHTNESS APPEAR , THE RAW MATERIAL USED IS COMMON WHEAT . MIXTURES OF DURUM WHEAT AND COMMON WHEAT CAN BE ASSESSED BY AN EVALUATION OF THE RELATIVE BRIGHTNESS OF THE TWO BANDS .

IF THERE ARE THREE BANDS ( 2 BANDS AT THE HEIGHT WHERE THE MAIN BANDS FOR COMMON WHEAT ARE TO BE FOUND , WITH A FURTHER BAND BETWEEN THEM ) EGGS HAVE BEEN ADDED TO PASTA . IN THIS CASE , THE RAW MATERIAL USED IS DURUM WHEAT IF THE MIDDLE BAND IS BRIGHTER THAN THE UPPER BAND . ON THE OTHER HAND , IF THE UPPER BAND IS BRIGHTER THAN THE MIDDLE BAND , THE RAW MATERIAL USED IS COMMON WHEAT .

ANNEX III

DETERMINATION OF MILKFAT CONTENT

I . PRINCIPLE

AFTER DETERMINING THE PERCENTAGE BY WEIGHT OF TOTAL FAT CONTAINED IN THE SAMPLE , THE BUTYRIC INDEX OF THIS TOTAL FAT CONTENT SHOULD BE DETERMINED ; THE MILKFAT CONTENT CAN THEN BE DETERMINED BY USING 20 AS THE AVERAGE BUTYRIC INDEX OF MILKFAT .

II . APPARATUS AND REAGENTS

1 . DISTILLATION APPARATUS WITH REFRIGERATED REFLUX CONDENSER

2 . BECKEL TUBES

3 . ALCOHOLIC SOLUTION OF POTASSIUM HYDROXIDE PREPARED BY MIXING 40 ML OF POTASH SOLUTION ( D = 1 * 5 ) WITH 40 ML DISTILLED WATER , AND DILUTING TO ONE LITRE WITH 95 _ 96 % ALCOHOL

4 . PURE GLYCERINE ( D = 1 * 23 )

5 . SATURATED SOLUTION OF POTASSIUM SULPHATE

6 . SULPHURIC ACID DILUTED ( 1 VOLUME CONCENTRATED SULPHURIC ACID ( D = 1 * 84 ) AND 3 VOLUMES DISTILLED WATER )

7 . COCONUT SOAP SOLUTION , OBTAINED AS FOLLOWS :

IN A 1 LITRE FLASK , SAPONIFY 50 G OF PURE COCONUT FAT , REFINED BUT NOT HARDENED ( MELTING POINT 24 _ 26 C ) , WITH 50 G OF GLYCERINE , 15 G KOH AND 20 ML OF WATER . AFTER COOLING TO BELOW 100 C , DILUTE TO 500 ML

8 . 1 % ALCOHOLIC SOLUTION OF PHENOLPHTHALEIN

9 . AQUEOUS 0 * 01 N SOLUTION OF SODIUM HYDROXIDE

III . METHOD

FIRST DETERMINE THE PERCENTAGE BY WEIGHT OF THE TOTAL FAT CONTENT OF THE SAMPLE TO BE ANALYSED . THEN DETERMINE THE BUTYRIC INDEX OF THIS TOTAL FAT CONTENT BY THE GROSSFELD METHOD , AS FOLLOWS :

WEIGH ACCURATELY 500 TO 550 MG OF FAT AND TRANSFER IT INTO A 50 ML FLAT-BOTTOMED FLASK WITH 5 ML OF ALCOHOLIC SOLUTION OF POTASSIUM HYDROXIDE . KEEP AT MODERATE BOIL UNDER REFLUX . WHEN THE FAT HAS BEEN COMPLETELY SAPONIFIED , REMOVE REFRIGERATED REFLUX CONDENSER , AND USING A GRADUATED PIPETTE ADD 1 ML OF GLYCERINE . CONTINUE TO HEAT UNTIL MOST OF THE ALCOHOL HAS EVAPORATED ( THIS IS INDICATED BY THE APPEARANCE OF HEAVY FROTHING ) . TO EVAPORATE THE REST OF THE ALCOHOL , PLACE THE FLASK IN AN OVEN AT 100 C FOR ONE HOUR .

IMMEDIATELY AFTER REMOVAL FROM THE OVEN ADD , STIRRING WELL , 15 ML OF SATURATED SOLUTION OF POTASSIUM SULPHATE . ALLOW TO COOL TO 20 C , THEN ADD SUCCESSIVELY ( STIRRING EACH TIME ) 0 * 5 ML OF DILUTE H2SO4 , 1 ML OF THE COCONUT SOAP SOLUTION AND ABOUT 0 * 1 G OF PURIFIED KIESELGUHR .

FILTER THROUGH A FLUTED FILTER 9 CM IN DIAMETER INTO THE BECKEL TUBE ( FIG . 1 ) UNTIL THE FILTRATE REACHES THE 12 * 5 ML LEVEL . IT MAY BE NECESSARY TO COMPRESS THE RESIDUE ONTO THE FILTER WITH A STIRRING ROD TO OBTAIN SUFFICIENT FILTRATE . TRANSFER THE FILTRATE INTO A 100 ML FLASK AND RINSE THE BECKEL TUBE WITH 5 ML OF WATER . POUR THE RINSINGS ALSO INTO THE BOTTLE .

ADD FINE PUMICE AND DISTIL 11 ML INTO THE RECIPIENT SHOWN ( FIG . 2 ) . TRANSFER TO A BEAKER , ADD 1 TO 2 DROPS OF PHENOLPHTHALEIN SOLUTION , TITRATE WITH THE AQUEOUS SODIUM HYDROXIDE SOLUTION UNTIL A PERSISTENT RED COLOUR IS OBTAINED , RINSE THE TUBE WITH THIS NEUTRALISED SOLUTION AND REPEAT THE TITRATION UNTIL THE RED COLOUR REAPPEARS .

THE BUTYRIC INDEX OF THE TOTAL FAT CONTENT IS CALCULATED BY MEANS OF THE FOLLOWING FORMULA : ( SEE O.J . )

ANNEX IV

DETERMINATION OF THE MANNITOL CONTENT OF GOODS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED ON THE SORBITOL CONTENT

I . PRINCIPLE

GAS CHROMATOGRAPHY IS USED TO DETERMINE THE MANNITOL CONTENT OF GOODS FALLING WITHIN SUB-HEADING N 29.04 C III OF THE COMMON CUSTOMS TARIFF , CALCULATED ON THEIR SORBITOL CONTENT . FOR THAT PURPOSE NON-VOLATILE PRODUCTS OR THEIR ACETYLATED DERIVATIVES MUST FIRST BE PROCESSED .

II . APPARATUS AND REAGENTS

1 . GAS CHROMATOGRAPH WITH FLAME-IONISATION DETECTOR

2 . COLUMN FILLED WITH " 5 % XE 60 ON AEROPAK 30 " ( GRANULATION 80 _ 100 MESH )

3 . ANHYDROUS PYRIDINE FOR ANALYSIS

4 . ACETONE FOR ANALYSIS

5 . ACETIC ANHYDRIDE FOR ANALYSIS

6 . 25 ML CALIBRATED FLASKS

III . METHOD

( A ) PREPARATION OF THE ACETYLATED DERIVATIVES

1 . SOLID PRODUCTS

WEIGH ABOUT 200 MG OF THE PRODUCT . BOIL FOR ONE HOUR WITH 3 ML PYRIDINE AND 3 ML ACETIC ANHYDRIDE SO THAT THE LIQUID FLOWS BACK AFTER CONDENSATION . LEAVE TO COOL AND BRING TO 250 ML WITH ACETONE . INJECT THIS SOLUTION IN THE CHROMATOGRAPH .

2 . PRODUCTS IN AQUEOUS SOLUTION

WEIGH ABOUT 3 G OF THE PRODUCT . ADD 60 ML PYRIDINE . DISTIL UNTIL THE TEMPERATURE OF THE VAPOUR REACHES 115 . THEN ADD 30 ML ACETIC ANHYDRIDE AND BOIL FOR TWO HOURS SO THAT THE LIQUID FLOWS BACK AFTER CONDENSATION . LEAVE TO COOL AND BRING TO 250 ML WITH ACETONE . INJECT THIS SOLUTION IN THE CHROMATOGRAPH .

( B ) CONDITIONS REQUIRED TO CARRY OUT CHROMATOGRAPHY

INJECTION TEMPERATURE : 300 C

TEMPERATURE OF THE COLUMN : 210 C

FLOW OF THE CARRIER GAS STREAM ( FOR INSTANCE NITROGEN ) : 25 ML / MINUTE

HYDROGEN FLOW : 25 ML / MINUTE

QUANTITY INJECTED : 1 MICROLITRE

THE MANNITOL PEAK APPEARS FIRST , THEN THE SORBITOL PEAK .

TO DETERMINE THE MANNITOL CONTENT OF THE GOODS UNDER ANALYSIS , CALCULATED ON THEIR SORBITOL CONTENT , SIMPLY CALCULATE THE RATIO OF THE AREA OF THE TWO PEAKS .