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31973L0082

Council Directive 73/82/EEC of 26 March 1973 on the implementation of Article 18 of the Directive of 4 March 1969 on the harmonization of provisions laid down by law, regulation or administrative action in respect of inward processing

Official Journal L 106 , 20/04/1973 P. 0007 - 0008 Greek special edition: Chapter 02 Volume 1 P. 0200

++++COUNCIL DIRECTIVE  OF 26 MARCH 1973  ON THE IMPLEMENTATION OF ARTICLE 18 OF THE DIRECTIVE OF 4 MARCH 1969 ON THE HARMONIZATION OF PROVISIONS LAID DOWN BY LAW , REGULATION OR ADMINISTRATIVE ACTION IN RESPECT OF INWARD PROCESSING   ( 73/82/EEC )  THE COUNCIL OF THE EUROPEAN COMMUNITIES ,  HAVING REGARD TO THE TREATY ESTABLISHING THE EUROPEAN ECONOMIC COMMUNITY .  HAVING REGARD TO THE COUNCIL DIRECTIVE OF 4 MARCH 1969 ( 1 ) ON THE HARMONIZATION OF PROVISIONS LAID DOWN BY LAW , REGULATION OR ADMINISTRATIVE ACTION IN RESPECT OF INWARD PROCESSING , AND IN PARTICULAR ARTICLE 18 THEREOF ;  HAVING REGARD TO THE PROPOSAL FROM THE COMMISSION ;  WHEREAS OPERATIONS CARRIED OUT UNDER THE INWARD PROCESSING ARRANGEMENTS MAY GIVE RISE TO THE MARKETING OF MANUFACTURING SCRAP AND WASTE IN THE CUSTOMS TERRITORY OF THE COMMUNITY IF THE CONDITIONS FOR THEIR MARKETING LAID DOWN BY ARTICLES 14 AND 15 OF THE SAID DIRECTIVE ARE FULFILLED ;  WHEREAS IN THE EVENT OF SUCH MARKETING OF SCRAP AND WASTE IN THESE CONDITIONS , THE IMPLEMENTATION OF ARTICLES 16 AND 17 OF THE SAID DIRECTIVE MAY BE OF SUCH A KIND AS TO ENDANGER THE ECONOMIC INTEREST OF THE OPERATIONS WHICH GAVE RISE TO THE GRANTING OF THE INWARD PROCESSING ARRANGEMENTS AND THUS PREVENT THE PURPOSE OF THE ARRANGEMENTS FROM BEING ACHIEVED , NAMELY TO CREATE THE MOST FAVOURABLE CONDITIONS FOR THE EXPORT OF COMPENSATING PRODUCTS ;  WHEREAS AT PRESENT CERTAIN MEMBER STATES LEVY TAXES ON SCRAP AND WASTE BY APPLYING , IN ACCORDANCE WITH ARTICLE 35 OF THE SAID DIRECTIVE , CUSTOMS DUTIES , CHARGES HAVING EQUIVALENT EFFECT AND AGRICULTURAL LEVIES PERTAINING THERETO , WHILE OTHER MEMBER STATES MUST APPLY THE TAXATION RULES LAID DOWN IN ARTICLES 16 AND 17 OF THE SAID DIRECTIVE ;  WHEREAS IT IS THEREFORE APPROPRIATE TO LAY DOWN STANDARD TAXATION LAWS AT COMMUNITY LEVEL FOR THE MARKETING OF MANUFACTURING SCRAP AND WASTE ;  WHEREAS TAXATION ACCORDING TO THE SPECIAL CONDITIONS OF ARTICLE 18 OF THE SAID DIRECTIVE ALSO MAKES IT POSSIBLE TO SIMPLIFY THE ADMINISTRATIVE PROCEDURES FOR DETERMINING AND CALCULATING THE AMOUNT OF CUSTOMS DUTIES , CHARGES HAVING EQUIVALENT EFFECT AND AGRICULTURAL LEVIES RELATING TO SUCH SCRAP AND WASTE ;  WHEREAS IT IS THEREFORE APPROPRIATE TO SETTLE THIS PROBLEM IMMEDIATELY WITHOUT THE PROPOSED SOLUTION HAVING ANY DETRIMENTAL EFFECT FOR THE TIME BEING ON THE IMPLEMENTATION OF OTHER PROVISIONS EXISTING AT NATIONAL LEVEL , WHICH MAY , AS LAID DOWN IN ARTICLE 35 OF THE SAID DIRECTIVE , REMAIN APPLICABLE ,  HAS ADOPTED THIS DIRECTIVE :  ARTICLE 1  1 . WHERE SCRAP AND WASTE FROM PROCESSING CARRIED OUT UNDER THE INWARD PROCESSING ARRANGEMENTS ARE MARKETED IN ACCORDANCE WITH THE CONDITIONS SET OUT IN ARTICLES 14 ( 1 ) AND 15 OF THE COUNCIL DIRECTIVE OF 4 MARCH 1969 ON THE HARMONIZATION OF PROVISIONS LAID DOWN BY LAW , REGULATION OR ADMINISTRATIVE ACTION IN RESPECT OF INWARD PROCESSING , THEY SHALL BE TAXED SUBJECT TO THE APPLICATION OF THE CUSTOMS DUTIES , CHARGES HAVING EQUIVALENT EFFECT AND AGRICULTURAL LEVIES PERTAINING TO THEM AT THE TIME WHEN THEY ARE PUT ON THE MARKET .  2 . WITH REGARD TO TAXATION LAID DOWN IN ( 1 ) ABOVE , MAXIMUM TAXES SHALL BE LEVIED ON THAT QUANTITY OF SCRAP AND WASTE WHICH CORRESPONDS PROPORTIONALLY TO THE QUANTITY OF OTHER COMPENSATING PRODUCTS EXPORTED . HOWEVER , PERSONS AUTHORIZED TO CARRY OUT INWARD PROCESSING MAY REQUEST THAT THESE SCRAP AND WASTE BE TAXED ACCORDING TO THE CONDITIONS OF ARTICLES 16 AND 17 OF THE DIRECTIVE REFERED TO IN ( 1 ) .  ARTICLE 2  THE MEMBER STATES SHALL INTRODUCE THE MEASURES NECESSARY SO AS TO COMPLY WITH THIS DIRECTIVE NOT LATER THAN 1 JULY 1973 .  ARTICLE 3  THIS DIRECTIVE IS ADDRESSED TO THE MEMBER STATES .  DONE AT BRUSSELS , 26 MARCH 1973 .  BY THE COUNCIL  THE PRESIDENT  A . LAVENS


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31993L0117

Twelfth Commission Directive 93/117/EC of 17 December 1993 establishing Community analysis methods for official control of feedingstuffs

Official Journal L 329 , 30/12/1993 P. 0054 - 0062 Finnish special edition: Chapter 3 Volume 54 P. 0186  Swedish special edition: Chapter 3 Volume 54 P. 0186

TWELFTH COMMISSION DIRECTIVE 93/117/EC of 17 December 1993 establishing Community analysis methods for official control of feedingstuffsTHE COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Community,  Having regard to Council Directive 70/373/EEC of 20 July 1970 on the introduction of Community methods of sampling and analysis for the official control of feedingstuffs (1), as last amended by Regulation (EEC) No 3768/85 (2), and in particular Article  2 thereof,  Whereas Directive 70/373/EEC requires that official controls on feedingstuffs for the purpose of checking compliance with requirements arising under quality and composition provisions laid down by law, regulation or administrative action shall be  carried out using Community sampling and analysis methods;  Whereas Community analysis methods for the additives robenidine and methyl benzoquate should be established for use in checking compliance with the conditions for its use in animal feedingstuffs;  Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Feedingstuffs,  HAS ADOPTED THIS DIRECTIVE:   Article 1  Member States shall require that analyses conducted in the course of official checks on feedingstuffs to identify their robenidine and methyl benzoquate content be made using the methods described in the Annex hereto.   Article 2  Member States shall bring into force the laws, regulations and administrative provisions required for compliance with this Directive by 30 November 1994 at the latest and shall forthwith inform the Commission thereof.  When Member States adopt these provisions, these shall contain a reference to this Directive or shall be accompanied by such reference at the time of their official publication. The procedure for such reference shall be adopted by Member States.   Article 3  This Directive shall enter into force on the third day following that of its publication in the Official Journal of the European Communities.  Done at Brussels, 17 December 1993.  For the Commission René STEICHEN Member of the Commission  (1) OJ No L 170, 3. 8. 1970, p. 2.  (2) OJ No L 362, 31. 12. 1985, p. 8.     ANNEX   1. DETERMINATON OF ROBENIDINE  1,3-bis[(4-chlorobenzylidene)amino] guanidine-hydrochloride 1. Purpose and scope  This method is for the determination of robenidine in feedingstuffs. the lower limit of determination is 5 mg/kg.  2. Principle  The sample is extracted with acidified methanol. The extract is dried and an aliquot portion subjected to a clean-up on an aluminium oxide column. Robenidine is eluted from the column with methanol, concentrated, and made up to a suitable volume with  mobile phase. The content of robenidine is determined by reversed-phase high-performance liquid chromatography (HPLC) using an UV detector.  3. Reagents 3.1. Methanol 3.2. Acidified methanol  Transfer 4,0 ml hydrochloric acid (P20c., 1,18 g/ml) into a 500 ml graduated flask, make up to the mark with methanol (3.1) and mix. This solution should be freshly prepared before use.  3.3. Acetonitrile, HPLC grade 3.4. Molecular sieve  Type 3A, 8 to 12 mesh beads (1,6-2,5 mm beads, crystalline alumino-silicate, diameter of pores 0,3 mm) 3.5. Aluminium oxide: acidic activity grade I for column chromatography  Transfer 100 g aluminium oxide into a suitable container and add 2,0 ml of water. Stopper and shake for approximately 20 minutes. Store in a well stoppered container.  3.6. Potassium dihydrogen phosphate solution, c = 0,025 mol/l  Dissolve 3,40 g of potassium dihydrogen phosphate in water (HPLC grade) in a 1000 ml graduated flask, make up to the mark and mix.  3.7. Di-sodium hydrogen phosphate solution, c = 0,025 mol/l  Dissolve 3,55 g of anhydrous (or 4,45 g of dihydrate or 8,95 g of dodecahydrate) di-sodium hydrogen phosphate in water (HPLC grade) in a 1,000 ml graduated flask, make up to the mark and mix.  3.8. HPLC mobile phase  Mix together the following reagents:   650 ml acetonitrile (3.3),   250 ml water (HPLC-grade),   50 ml potassium di-hydrogen phosphate solution (3.6),   50 ml di-sodium hydrogen phosphate solution (3.7).   Filter through a 0,22 mm filter (4.6) and degas the solution, (e.g. by ultrasonification for 10 minutes).  3.9. Standard substance  Pure robenidine: 1.3-bis[4-chlorobenzylidene)amino] guanidine hydrochloride, E 750.  3.9.1. Robenidine stock standard solution: 300 mg/ml:   Weigh to the nearest 0,1 mg, 30 mg of robenidine standard substance (3.9). Dissolve in acidified methanol (3.2) in a 100 ml graduated flask, make up to the mark with the same solvent and mix. Wrap the flask with aluminium foil and store in a dark  place.  3.9.2. Robenidine intermediate standard solution: 12 mg/ml  Transfer 10,0 ml of the stock standard solution (3.9.1) into a 250 ml graduated flask, make up to the mark with the mobile phase (3.8) and mix. Wrap the flask with aluminium foil and store in a dark place.  3.9.3. Calibration solutions  Into a series of 50 ml calibrated flasks, transfer 5,0, 10,0, 15,0, 20,0 and 25,0 ml of the intermediate standard solution (3.9.2). Make up to the mark with mobile phase (3.8) and mix. These solutions correspond to 1,2, 2,4, 3,6, 4,8 and 6,0 mg/ml of  robenidine respectively. These solutions must be freshly prepared before use.  4. Apparatus 4.1. Glass column  Constructed of amber glass fitted with a stopcock and a reservoir of approximately 150 ml capacity, internal diameter 10 to 15 mm, length 250 mm.  4.2. Laboratory wrist-action shaker 4.3. Rotary film evaporator 4.4. HPLC equipment with variable wavelength ultraviolet detector or diode array detector operating in the range of 250 to 400 mm 4.4.1. Liquid chromatographic column: 300 mm × 4 mm, C18, 10 mm packing or equivalent 4.5. Glass fibre filter paper (Whatman GF/A or equivalent) 4.6. Membrane filters, 0,22 mm 4.7. Membrane filters, 0,45 mm 5. Procedure  Note: Robenidine is light-sensitive. Amber glassware should be used in all operations.  5.1. General 5.1.1. A blank feed should be analysed to check that neither robenidine nor interfering substances are present.  5.1.2. A recovery test should be carried out by analysing the blank feed (5.1.1) which has been fortified by addition of a quantity of robenidine, similar to that present in the sample. To fortify at a level of 60 mg/kg, transfer 3,0 ml of the stock  standard solution (3.9.1) to a 250 ml conical flask. Evaporate the solution to c. 0,5 ml in a stream of nitrogen. Add 15 g of the blank feed, mix and wait for 10 minutes before proceeding with the extraction step (5.2).   Note: for the purpose of this method, the blank feed should be similar in type to that of the sample and on analysis robenidine should not be detected.  5.2. Extraction  Weigh to the nearest 0,01 g, approximately 15 g of the prepared sample. Transfer to a 250 ml conical flask and add 100,0 ml of acidified methanol (3.2), stopper and shake for one hour on the shaker (4.2). Filter the solution through a glass fibre  filter paper (4.5) and collect the whole filtrate in a 150 ml conical flask. Add 7,5 g molecular sieve (3.4), stopper and shake for five minutes. Filter immediately through a glass-fibre filter paper. Retain this solution for the purification step  (5.3).  5.3. Purification 5.3.1. Preparation of the aluminium-oxide column  Insert a small glass-wool plug into the lower end of a glass column (4.1) and tamp it down using a glass rod. Weigh out 11,0 g of the prepared aluminium oxide (3.5) and transfer to the column. Care should be taken to minimize the exposure to the  atmosphere during this stage. Gently tap the loaded column at its lower end to settle the aluminium oxide.  5.3.2. Sample purification  Transfer onto the column by pipette 5,0 ml of the sample extract prepared in (5.2). Rest the pipette tip close to the column wall and allow the solution to be absorbed onto the aluminium oxide. Elute the robenidine from the column using 100 ml methanol  (3.1), at a flow rate of 2 to 3 ml/minute and collect the eluate in a 250 ml round bottomed flask. Evaporate the methanol solution to dryness under reduced pressure at 40 C by means of a rotary film evaporator (4.3). Re-dissolve the residue in 3 to 4 ml  of mobile phase (3.8) and transfer quantitatively to a 10 ml graduated flask. Rinse the flask with several 1 to 2 ml portions of mobile phase and transfer these rinsings to the graduated flask. Make up to the mark with the same solvent and mix. An  aliquot is filtered through a 0,45 mm (4.7). Reserve this solution for HPLC determination (5.4).  5.4. HPLC determination 5.4.1. Parameters  The following conditions are offered for guidance, other conditions may be used provided they yield equivalent results:   Liquid chromatographic column (4.4.1),   HPLC mobile phase (3.8),   Flow rate: 1,5 to 2 ml/minute,   Detector wavelength: 317 nm,   Injection volume: 20 to 50 ml.   Check the stability of the chromatographic system, injecting the calibration solution (3.9.3) containing 3,6 mg/ml several times, until constant peak heights and retention times are achieved.  5.4.2. Calibration graph  Inject each calibration solution (3.9.3) several times and measure the peak heights (areas) for each concentration. Plot a calibration curve using the mean peak heights or areas of the calibration solutions as the ordinates and corresponding  concentrations in mg per ml as abscissae.  5.4.3. Sample solution  Inject the sample extract (5.3.2) several times, using the same volume as taken for the calibration solutions and determine the mean peak height (area) of the robenidine peaks.  6. Calculation of results  From the mean height (area) of the robenidine peaks of the sample solution determine the concentration of the sample solution in mg/ml by reference to the calibration graph (5.4.2).   The content of robenidine w (mg/kg) in the sample is given by the following formula:    in which:   c = robenidine concentration of the sample solution in mg/ml,   m = mass of the test position in grams.  7. Validation of the results 7.1. Identity  The identity of the analyte can be confirmed by co-chromatography, or by using a diode-array detector by which the spectra of the sample extract and the calibration solution (3.9.3) containing 6 mg/ml are compared.  7.1.1. Co-chromatography  A sample extract is fortified by addition of an appropriate amount of calibration solution (3.9.3). The amount of added robenidine should be similar to the estimated amount of robenidine found in the sample extract.   Only the height of the robenidine peak should be enhanced after taking into account both the amount added and the dilution of the extract. The peak width, at half of its maximum height, must be within approximately 10 % of the original width.  7.1.2. Diode-array detection  The results are evaluated according to the following criteria:   (a) the wavelength of maximum absorption of the sample and of the standard spectra, recorded at the peak apex on the chromatogram, must be the same within a margin determined by the resolving power of the detection system. For diode-array detection,  this is typically within approximately 2 nm;   (b) between 250 and 400 nm, the sample and standard spectra recorded at the peak apex on the chromatogram, must not be different for those parts of the spectrum within the range 10 to 100 % of relative absorbance. This criterion is met when the same  maxima are present and at no observed point the deviation between the two spectra exceeds 15 % of the absorbance of the standard analyte;   (c) between 250 and 400 nm, the spectra of the upslope, apex and downslope of the peak produced by the sample extract must not be different from each other for those parts of the spectrum within the range 10 to 100 % of relative absorbance. This  criterion is met when the same maxima are present and when at all observed points the deviation between the spectra does not exceed 15 % of the absorbance of the spectrum of the apex.   If one of these criteria is not met the presence of the analyte has not been confirmed.  7.2. Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed 10 % of the higher result for robenidine content higher than 15 mg/kg.  7.3. Recovery  For a fortified blank sample the recovery should be at least 85 %.  8. Results of a collaborative study  A collaborative study was arranged by the Community in which four samples of poultry and rabbit feed, in meal or pelleted form were analysed by 12 laboratories. Duplicate analyses were performed on each sample. The results are given in the table below:    "" ID="1">Mean mg/kg> ID="2">27,00> ID="3">27,99> ID="4">43,6 > ID="5">40,1 "> ID="1">Sr (mg/kg)> ID="2">1,46> ID="3">1,26> ID="4">1,44> ID="5">1,66"> ID="1">CVr (%)> ID="2">5,4> ID="3">4,5> ID="4">3,3> ID="5">4,1"> ID="1">Sr (mg/kg)>  ID="2">4,36> ID="3">3,36> ID="4">4,61> ID="5">3,91"> ID="1">CVR (%)> ID="2">16,1 > ID="3">12,0 > ID="4">10,6 > ID="5">9,7"> ID="1">Recovery (%)> ID="2">90,0 > ID="3">93,3 > ID="4">87,2 > ID="5">80,2 ""   Sr = standard deviation of repeatability.  CVr = coefficient of variation of repeatability SR = standard deviation of reproducibility CVR = coefficient of variation of reproducibility.  > 2. DETERMINATION OF METHYL BENZOQUATE 7-benzyloxy-6-butyl-3-methoxycarbonyl-4-quinolone 1. Purpose and scope  This method is for the determination of methyl benzoquate in feedingstuffs. The lower limit of determination is 1 mg/kg.  2. Principle  Methyl benzoquate is extracted from the sample with methanolic methanesulfonic acid solution. The extract is purified with dichloromethane, by ion-exchange chromatography and then again with dichloromethane. The methyl benzoquate content is determined  by reversed-phase high-performance liquid chromatography (HPLC) with an UV detector.  3. Reagents 3.1. Dichloromethane 3.2. Methanol, HPLC grade 3.3. HPLC mobile phase:   mixture of methanol (3.2) and water (HPLC grade) 75 + 25 (v + v).   Filter through a 0,22 mm filter (4.5) and degas the solution (e.g. by ultrasonification for 10 minutes).  3.4. Methanesulfonic acid solution, s = 2 %  Dilute 20,0 ml methanesulfonic acid to 1000 ml with methanol (3.2).  3.5. Hydrochloric acid solution, s = 10 %  Dilute 100 ml hydrochloric acid (P20 c. 1,18 g/ml) to 1000 ml with water.  3.6. Cation-exchange resin Amberlite CG-120 (Na), 100 to 200 mesh  The resin is pretreated before use: slurry 100 g resin with 500 ml hydrochloric acid solution (3.5) and heat on a hot plate to boiling, stirring continuously. Allow to cool and decant off the acid. Filter through a filter paper under vacuum. Wash the  resin twice with 500 ml portions of water and then with 250 ml of methanol (3.2). Rinse the resin with a further 250 ml portion of methanol and dry by passing air through the filter cake. Store the dried resin in a stoppered bottle.  3.7. Standard substance: pure methyl benzoquate (7-benzyloxy-6-butyl-3-methoxycarbonyl-4-quinolone) 3.7.1. Methyl benzoquate stock standard solution, 500 mg/ml  Weigh to the nearest 0,1 mg, 50 mg of standard substance (3.7), dissolve in methanesulfonic acid solution (3.4) in a 100 ml graduated flask, make up to the mark and mix.  3.7.2. Methyl benzoquate intermediate standard solution, 50 mg/ml  Transfer 5,0 ml of methyl benzoquate stock standard solution (3.7.1) into a 50 ml graduated flask, make up to the mark with methanol (3.2) and mix.  3.7.3. Calibration solutions  Transfer 1,0, 2,0, 3,0, 4,0 and 5,0 ml of methyl benzoquate intermediate standard solution (3.7.2) into a series of 25 ml graduated flasks. Make up to the mark with the mobile phase (3.3) and mix. These solutions have concentrations of 2,0, 4,0, 6,0,  8,0 and 10,0 mg/ml methyl benzoquate respectively. These solutions must be freshly prepared before use.  4. Apparatus 4.1. Laboratory shaker 4.2. Rotary film evaporator 4.3. Glass column (250 mm × 15 mm) fitted with a stopcock and reservoir of approximately 200 ml capacity 4.4. HPLC equipment with variable wavelength ultraviolet detector or diode-array detector 4.4.1. Liquid chromatographic column: 300 mm × 4 mm, C-18, 10 mm packing or equivalent 4.5. Membrane filters, 0,22 mm 4.5. Membrane filters, 0,45 mm 5. Procedure 5.1. General 5.1.1. A blank feed should be analysed to check that neither methyl benzoquate nor interfering substances are present.  5.1.2. A recovery test should be carried out by analysing the blank feed which has been fortified by addition of a quantity of methyl benzoquate, similar to that present in the sample. To fortify at a level of 15 mg/kg, add 600 ml of the stock standard  solution (3.7.1) to 20 g of the blank feed, mix and wait for 10 minutes before proceeding with the extraction step (5.2).   Note: for the purpose of this method, the blank feed should be similar in type to that of the sample and on analysis methyl benzoquate should not be detected.  5.2. Extraction  Weigh to the nearest 0,01 g, approximately 20 g of the prepared sample and transfer to a 250 ml conical flask. Add 100,0 ml of methanesulfonic acid solution (3.4) and shake mechanically (4.1) for 30 minutes. Filter the solution through a filter paper  and retain the filtrate for the liquid-liquid partition step (5.3).  5.3. Liquid-liquid partition  Transfer into a 500 ml separating funnel containing 100 ml of hydrochloric acid solution (3.5), 25,0 ml of the filtrate obtained in (5.2). Add 100 ml dichloromethane (3.1) to the funnel and shake for one minute. Allow the layers to separate and run off  the lower (dichloromethane) layer into a 500 ml round-bottomed flask. Repeat the extraction of the aqueous phase with two further 40-ml portions of dichloromethane and combine these with the first extract in the round-bottomed flask. Evaporate the  dichloromethane extract down to dryness on the rotary evaporator (4.2) operating under reduced pressure at 40° C. Dissolve the residue in 20 to 25 ml methanol (3.2), stopper the flask and retain the whole of the extract for ion-exchange chromatography  (5.4).  5.4. Ion-exchange chromatography 5.4.1. Preparation of the cation-exchange column  Insert a plug of glass wool into the lower end of a glass column (4.3). Prepare a slurry of 5,0 g of the treated cation-exchange resin (3.6) with 50 ml of hydrochloric acid (3.5), pour into the glass column and allow to settle. Run out the excess acid  to just above the resin surface and wash the column with water until the effluent is neutral to litmus. Transfer 50 ml methanol (3.2) onto the column and allow to drain down to the resin surface.  5.4.2. Column chromatography  By means of a pipette, carefully transfer the extract obtained in (5.3) onto the column. Rinse the round-bottomed flask with two portions of 5 to 10 ml methanol (3.2) and transfer these washings to the column. Run the extract down to the resin surface  and wash the column with 50 ml methanol, ensuring that the flow rate does not exceed 5 ml per minute. Discard the effluent. Elute the methyl benzoquate from the column using 150 ml of methanesulfonic acid solution (3,4) and collect the column eluate in  a 250 ml conical flask.  5.5. Liquid-liquid partition  Transfer the eluate obtained in (5.4.2) into a 1 litre separating funnel. Rinse the conical flask with 5 to 10 ml methanol (3.2) and combine the washings with the contents of the separating funnel. Add 300 ml of hydrochloric acid solution (3.5) and 130  ml of dichloromethane (3.1). Shake for 1 minute and allow the phases to separate. Run off the lower (dichloromethane) layer into a 500 ml round-bottomed flask. Repeat the extraction of the aqueous phase with two further 70 ml portions of dichloromethane  and combine these extracts with the first in the round-bottomed flask.   Evaporate the dichloromethane extract down to dyrness on the rotary evaporator (4.2) operating under reduced pressure at 40° C. Dissolve the residue in the flask with approximately 5 ml of methanol (3.2) and transfer this solution quantitatively to a  10 ml graduated flask. Rinse the round-bottomed flask with a further two portions of 1 to 2 ml of methanol and transfer these to the graduated flask. Make up to the mark with methanol and mix. An aliquot portion is filtered through a membrane filter  (4.6). Reserve this solution for HPLC-determination (5.6).  5.6. HPLC determination 5.6.1. Parameters  The following conditions are offered for guidance, other conditions may be used provided that they give equivalent results:   - liquid chromatograhic column (4.4.1),   - HPLC mobile phase: methanol-water mixture (3.3),   - flow rate: 1 to 1,5 ml/minute,   - detection wavelength: 265 nm,   - Injection volume: 20 to 50 ml.   Check the stability of the chromatographic system, injecting the calibration solution (3.7.3) containing 4 mg/ml several times, until contant peak heights or areas and retention times are achieved.  5.6.2. Calibration graph  Inject each calibration solution (3.7.3) several times and measure the peak heights (areas) for each concentration. Plot a calibration graph using the mean peak heights or areas of the calibration solutions as the ordinates and the corresponding  concentrations in mg/ml as the abscissae.  5.6.3. Sample solution  Inject the sample extract (5.5) several times, using the same volume as taken for the calibration solutions and determine the mean peak height (area) of the methyl benzoquate peaks.  6. Calculation of results  Determine the concentration of the sample solution in mg/ml from the mean height (area) of the methyl benzoquate peaks of the sample solution by reference to the calibration graph (5.6.2).   The content of methyl benzoquate w (mg/kg) of the sample is given by the following formula:    in which:   c = methyl benzoquate concentration of the sample solution in mg/ml,   m = mass of the test portion in grams.  7. Validation of the results 7.1. Identity  The identity of the analyte can be confirmed by co-chromatography, or by using a diode-array detector by which the spectra of the sample extract and the calibration solution (3.7.3) containing 10 mg/ml are compared.  7.1.1. Co-chromatography  A sample extract is fortified by addition of an appropriate amount of the intermediate standard solution (3.7.2). The amount of added methyl benzoquate should be similar to the estimated amount of methyl benzoquate in the sample extract. Only the  height of the methyl-benzoquate peak should be enhanced after taking into account both the amount added and the dilution of the extract. The peak width, at half of its maximum height, must be within approximately 10 % of the original width,  7.1.2. Diode-array detection  The results are evaluated according to the following criteria:   (a) the wavelength of maximum absorption of the sample and of the standard spectra recorded at the peak apex on the chromatogram must be the same within a margin determined by the resolving power of the detection system. For diode-array detection, this  is typically within approximately 2 nm;   (b) between 220 and 350 nm, the sample and standard spectra recorded at the peak apex on the chromatogram must not be different for those parts of the spectrum within the range 10 to 100 % of relative absorbance. This criterion is met when the same  maxima are present and at no observed point the deviation between the two spectra exceeds 15 % of the absorbance of the standard analyte;   (c) between 220 and 350 nm, the spectra of the upslope, apex and downslope of the peak produced by the sample extract must not be different from each other for those parts of the spectrum within the range 10 to 100 % of relative absorbance. This  criterion is met when the same maxima are present and when at all observed points the deviation between the spectra does not exceed 15 % of the absorbance of the spectrum of the apex.   If one of these criteria is not met the presence of the analyte has not been confirmed.  7.2. Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed: 10 % relative to the higher result for methyl benzoquate contents between 4 and 20 mg/kg.  7.3. Recovery  For a fortified blank sample the recovery should be at least 90 %.  8. Results of a collaborative study  Five samples were analysed by 10 laboratories. Duplicate analyses were performed on each sample.  Results "" ID="1">Mean (mg/kg)> ID="2">n.d.> ID="3">4,50> ID="4">4,50> ID="5">8,90> ID="6">8,70"> ID="1">Sr (mg/kg)> ID="2">-> ID="3">0,30> ID="4">0,20> ID="5">0,60> ID="6">0,50"> ID="1">CVr (%)> ID="2">-> ID="3">6,70> ID="4">4,40> ID="5">6,70>  ID="6">5,70"> ID="1">Sr (mg/kg)> ID="2">-> ID="3">0,40> ID="4">0,50> ID="5">0,90> ID="6">1,00"> ID="1">CVR (%)> ID="2">-> ID="3">8,90> ID="4">11,10> ID="5">10,10> ID="6">11,50"> ID="1">Recovery (%)> ID="2">-> ID="3">92,00> ID="4">93,00> ID="5">92,00>  ID="6">89,00""    n.d. = not detected.  Sr = standard deviation of repeatability.  CVr = coefficient of variation of repeatability.  SR = standard deviation of reproducibility.  CVR = coefficient of variation of reproducibility.  >


title: Commission Directive 2005/12/EC of 18 February 2005 amending Annexes I and II to Directive 2003/25/EC of the European Parliament and of the Council on specific stability requirements for ro-ro passenger shipsText with EEA relevance

text:
               19.2.2005

               EN

               Official Journal of the European Union

               L 48/19

      COMMISSION DIRECTIVE 2005/12/EC
   of 18 February 2005
   amending Annexes I and II to Directive 2003/25/EC of the European Parliament and of the Council on specific stability requirements for ro-ro passenger ships
   (Text with EEA relevance)
   THE COMMISSION OF THE EUROPEAN COMMUNITIES,
   Having regard to the Treaty establishing the European Community,
   Having regard to Directive 2003/25/EC of the European Parliament and of the Council of 14 April 2003 on specific stability requirements for ro-ro passenger ships (1), and in particular Article 10 thereof,
   Whereas:

               (1)

               Directive 2003/25/EC applies to all ro-ro passenger ships operating to or from a port of a Member State on a regular service, regardless of their flag, when engaged on international voyages.

               (2)

               Article 6 of Directive 2003/25/EC provides that ro-ro passenger ships shall comply with specific stability requirements which are set out in detail in Annex I to that Directive and that Member States shall use in the application of these requirements the guidelines set out in Annex II thereto.

               (3)

               Article 10 of Directive 2003/25/EC provides that the Annexes to the Directive may be amended in accordance with the procedure referred to in Article 11(2), in order to take account of developments at international level and particularly at the International Maritime Organisation (IMO).

               (4)

               IMO Resolution MSC 141(76) of 5 December 2002 introduced a revised model test method and associated guidance notes under Resolution 14 of the 1995 SOLAS (Safety of Life at Sea) Conference. Resolution 14 concerns regional agreements on specific stability requirements for ro-ro passenger ships.

               (5)

               The revised model test method should supersede the previously applied model test method provided for in Directive 2003/25/EC. Any ship having passed the test according to the previously applied model test method need not to do the test again.

               (6)

               Directive 2003/25/EC should therefore be amended accordingly.

               (7)

               The measures provided for in this Directive are in accordance with the opinion of the Committee on Safe Seas and the Prevention of Pollution from Ships, set up by Regulation (EC) No 2099/2002 of the European Parliament and of the Council (2),

         HAS ADOPTED THIS DIRECTIVE:
   Article 1
   Directive 2003/25/EC is amended as follows:

               1.

               Annex I is amended as follows:

                           (a)

                           paragraph 2.3 is replaced by the following:

                                       ‘2.3.

                                       the tightness of transverse or longitudinal bulkheads which are taken into account as effective to confine the assumed accumulated sea water in the compartment concerned in the damaged ro-ro deck shall be commensurate with the drainage system, and shall withstand hydrostatic pressure in accordance with the results of the damage calculation. Such bulkheads shall be at least 4 m in height unless the height of water is less than 0,5 m. In such cases the height of the bulkhead may be calculated in accordance with the following:

                                                   Bh = 8hw
                                                   where:

                                                               Bh is the bulkhead height;

                                                               and hw is the height of water.

                                             In any event, the minimum height of the bulkhead should be not less than 2,2 m. However, in case of a ship with hanging car decks, the minimum height of the bulkhead shall be not less than the height to the underside of the hanging deck when in its lowered position;’

                           (b)

                           the Appendix entitled ‘Model test method’, is replaced by the text shown in Annex I to this Directive;

               2.

               in Annex II, Part II, entitled ‘Model testing’, is replaced by the text shown in Annex II to this Directive.

         Article 2
   1.   Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive within 12 months after its date of entry into force at the latest. They shall forthwith communicate to the Commission the text of those provisions and a correlation table between those provisions and this Directive.
   When Member States adopt those provisions, they shall contain a reference to this Directive or be accompanied by such a reference on the occasion of their official publication. Member States shall determine how such reference is to be made.
   2.   Member States shall communicate to the Commission the text of the main provisions of national law which they adopt in the field covered by this Directive.
   Article 3
   This Directive shall enter into force on the twentieth day of its publication in the Official Journal of the European Union.
   Article 4
   This Directive is addressed to the Member States.

      Done at Brussels, 18 February 2005.

            For the Commission

         Jacques BARROT

            Vice-President

      (1)  OJ L 123, 17.5.2003, p. 22.

      (2)  OJ L 324, 29.11.2002, p. 1. Regulation as amended by Regulation (EC) No 415/2004 (OJ L 68, 6.3.2004, p. 10).

      ANNEX I

            ‘Appendix
            Model test method
            1.   Objectives
            This revised model test method is a revision of the method contained in the Appendix to the Annex to resolution 14 of the 1995 SOLAS Conference. Since the entry into force of the Stockholm Agreement a number of model tests has been carried out in accordance with the test method previously in force. During these tests a number of refinements in the procedures have been identified. This new model test method aims to include these refinements and, together with the appended Guidance Notes, provide a more robust procedure for the assessment of survivability of a damaged ro-ro passenger ship in a seaway. In the tests provided for in paragraph 1.4 of the stability requirements included in Annex I, the ship should be capable of withstanding a seaway as defined in paragraph 4 hereunder in the worst-damage-case scenario.
            2.   Definitions

                        LBP

                        is the length between perpendiculars

                        HS

                        is the significant wave height

                        B

                        is the moulded breadth of the ship

                        TP

                        is the peak period

                        TZ

                        is the zero crossing period

                  3.   Ship model
            3.1.   The model should copy the actual ship for both outer configuration and internal arrangement, in particular all damaged spaces having an effect on the process of flooding and shipping of water. Intact draught, trim, heel and limiting operational KG corresponding to the worst damage case should be used. Furthermore, the test case(s) to be considered should represent the worst damage case(s) defined in accordance with SOLAS regulation II-1/8.2.3.2 (SOLAS 90) with regard to the total area under the positive GZ curve and the centreline of the damage opening should be located within the following range:
            3.1.1.   ± 35 % LBP from midship;
            3.1.2.   an additional test will be required for the worst damage within ± 10 % LBP from midship if the damage case referred to in .1 is outside of ± 10 % LBP from midship.
            3.2.   The model should comply with the following:
            3.2.1.   length between perpendiculars (LBP) is to be at least 3 m or a length corresponding to a model scale of 1:40, whichever is greater, and the vertical extent up to at least three superstructure standard heights above the bulkhead (freeboard) deck;
            3.2.2.   hull thickness of flooded spaces should not exceed 4 mm;
            3.2.3.   in both intact and damaged conditions, the model should satisfy the correct displacement and draught marks (TA, TM, TF, port and starboard) with a maximum tolerance in any one draught mark of + 2 mm. Draught marks forward and aft should be located as near FP and AP as practicable;
            3.2.4.   all damaged compartments and ro-ro spaces should be modelled with the correct surface and volume permeabilities (actual values and distributions) ensuring that floodwater mass and mass distribution are correctly represented;
            3.2.5.   the characteristics of motion of the actual ship should be modelled properly, paying particular attention to the intact GM tolerance and radii of gyration in roll and pitch motion. Both radii should be measured in air and be in the range of 0,35B to 0,4B for roll motion, and 0,2LOA to 0,25LOA for pitch motion;
            3.2.6.   main design features such as watertight bulkheads, air escapes, etc., above and below the bulkhead deck that can result in asymmetric flooding should be modelled properly as far as practicable to represent the real situation; Ventilating and cross-flooding arrangements should be constructed to a minimum cross section of 500 mm2;
            3.2.7.   the shape of the damage opening should be as follows:

                        1.

                        trapezoidal profile with side at 15° slope to the vertical and the width at the design waterline defined according to SOLAS regulation II-1/8.4.1;

                        2.

                        isosceles triangular profile in the horizontal plane with the height equal to B/5 according to SOLAS regulation II-1/8.4.2. If side casings are fitted within B/5, the damaged length in way of the side casings should not be less than 25 mm;

                        3.

                        notwithstanding the provisions of subparagraphs 3.2.7.1 and 3.2.7.2 above, all compartments taken as damaged in calculating the worst damage case(s) referred to in paragraph 3.1 should be flooded in the model tests;

                  3.3.   The model in the flooded equilibrium condition should be heeled by an additional angle corresponding to that induced by the heeling moment Mh = max (Mpass; Mlaunch)-Mwind, but in no case should the final heel be less than 1° towards damage. Mpass, Mlaunch and Mwind are as specified in SOLAS regulation II-1/8.2.3.4. For existing ships this angle may be taken as 1°.
            4.   Procedure for experiments
            4.1.   The model should be tested in a long-crested irregular seaway defined by the JONSWAP spectrum with significant wave height HS, a peak enhancement factor γ = 3,3 and a peak period . HS is the significant wave height for the area of operation, which is not exceeded by a probability of more than 10 % on a yearly basis, but limited to a maximum of 4 m.
            Furthermore,
            4.1.1.   the basin width should be sufficient to avoid contact or other interaction with the sides of the basin and is recommended not to be less than LBP + 2 m;
            4.1.2.   the basin depth should be sufficient for proper wave modelling but should not be less than 1 m;
            4.1.3.   for a representative wave realisation to be used, measurements should be performed prior to the test at three different locations within the drift range;
            4.1.4.   the wave probe closer to the wave maker should be located at the position where the model is placed when the test starts;
            4.1.5.   variation in HS and TP should be within ± 5 % for the three locations; and
            4.1.6.   during the tests, for approval purposes, a tolerance of + 2,5 % in HS, ± 2,5 % in TP and ± 5 % in TZ should be allowed with reference to the probe closer to the wave maker.
            4.2.   The model should be free to drift and placed in beam seas (90° heading) with the damage hole facing the oncoming waves, with no mooring system permanently attached to the model used. To maintain a beam sea heading of approximately 90° during the model test the following requirements should be satisfied:
            4.2.1.   heading control lines, intended for minor adjustment, should be located at the centre line of the stem and stern, in a symmetrical fashion and at a level between the position of KG and the damaged waterline; and
            4.2.2.   the carriage speed should be equal to the actual drift speed of the model with speed adjustment made when necessary.
            4.3.   At least 10 experiments should be carried out. The test period for each experiment should be of a duration such that a stationary state is reached, but not less than 30 min in full-scale. A different wave realisation train should be used for each experiment.
            5.   Survival criteria
            The model should be considered as surviving if a stationary state is reached for the successive test runs as required in paragraph 4.3. The model should be considered as capsized if angles of roll of more than 30° to the vertical axis or steady (average) heel greater than 20° for a period longer than three minutes full-scale occur, even if a stationary state is reached.
            6.   Test documentation
            6.1.   The model test programme should be approved by the Administration in advance.
            6.2.   Tests should be documented by means of a report and a video or other visual records containing all relevant information on the model and the test results, which are to be approved by the Administration. These should include, as a minimum, the theoretical and measured wave spectra and statistics (HS, TP, TZ) of the wave elevation at the three different locations in the basin for a representative realisation, and for the tests with the model, the time series of main statistics of the measured wave elevation close to the wave maker and records of model roll, heave and pitch motions, and of the drift speed.’

      ANNEX II

         ‘PART II
         MODEL TESTING
         The purpose of these guidelines is to ensure uniformity in the methods employed in the construction and verification of the model as well as in the undertaking and analyses of the model tests.
         The contents of paragraphs 1 and 2 of the Appendix to Annex I are considered self-explanatory.
         Paragraph 3 — Ship model
         3.1.   The material of which the model is made is not important in itself, provided that the model both in the intact and damaged condition is sufficiently rigid to ensure that its hydrostatic properties are the same as those of the actual ship and also that the flexural response of the hull in waves is negligible.
         It is also important to ensure that the damaged compartments are modelled as accurately as practicably possible to ensure that the correct volume of flood water is represented.
         Since ingress of water (even small amounts) into the intact parts of the model will affect its behaviour, measures must be taken to ensure that this ingress does not occur.
         In model tests involving worst SOLAS damages near the ship ends, it has been observed that progressive flooding was not possible because of the tendency of the water on deck to accumulate near the damage opening and hence flow out. As such models were able to survive very high sea states, while they capsized in lesser sea states with less onerous SOLAS damages, away from the ends, the limit ± 35 % was introduced to prevent this.
         Extensive research carried out for the purpose of developing appropriate criteria for new vessels has clearly shown that in addition to the GM and freeboard being important parameters in the survivability of passenger ships, the area under the residual stability curve is also another major factor. Consequently in choosing the worst SOLAS damage for compliance with the requirement of paragraph 3.1 the worst damage is to be taken as that which gives the least area under the residual stability curve.
         3.2.   Model particulars
         3.2.1.   In recognising that scale effects play an important role in the behaviour of the model during tests, it is important to ensure that these effects are minimised as much as practically possible. The model should be as large as possible since details of damaged compartments are easier constructed in larger models and the scale effects are reduced. It is therefore required that the model length is not less than that corresponding to 1:40 scale or 3 m, whichever is greater.
         It has been found during tests that the vertical extent of the model can affect the results when tested dynamically. It is therefore required that the ship is modelled to at least three super structure standard heights above the bulkhead (freeboard) deck so that the large waves of the wave train do not break over the model.
         3.2.2.   The model in way of the assumed damages must be as thin as practically possible to ensure that the amount of flood water and its centre of gravity is adequately represented. The hull thickness should not exceed 4 mm. It is recognised that it may not be possible for the model hull and the elements of primary and secondary subdivision in way of the damage to be constructed with sufficient detail and due to these constructional limitations it may not be possible to calculate accurately the assumed permeability of the space.
         3.2.3.   It is important that not only the draughts in the intact condition are verified, but also that the draughts of the damaged model are accurately measured for correlation with those derived from the damaged stability calculation. For practical reasons a tolerance of + 2 mm in any draught is accepted.
         3.2.4.   After measuring the damaged draughts it may be found necessary to make adjustments to the permeability of the damaged compartment by either introducing intact volumes or by adding weights. However it is also important to ensure that the centre of gravity of the flood water is accurately represented. In this case any adjustments made must err on the side of safety.
         If the model is required to be fitted with barriers on deck and the barriers are less than the bulkhead height indicated below, the model is to be fitted with CCTV so that any “splashing over” and any accumulation of water on the undamaged area of the deck can be monitored. In this case a video recording of the event is to form part of the test records.
         The height of transverse or longitudinal bulkheads which are taken into account as effective to confine the assumed accumulated sea water in the compartment concerned in the damaged ro-ro deck should be at least 4 m in height unless the height of water is less than 0,5 m. In such cases the height of the bulkhead may be calculated in accordance with the following:

                     Bh = 8hw

                     where Bh is the bulkhead height; and

                     hw is the height of water.

               In any event, the minimum height of the bulkhead should be not less than 2,2 m. However, in the case of a ship with hanging car decks, the minimum height of the bulkhead should be not less than the height to the underside of the hanging car deck when in its lowered position.
         3.2.5.   In order to ensure that the model motion characteristics represent those of the actual ship it is important that the model is both inclined and rolled in the intact condition so that the intact GM and the mass distribution are verified. The mass distribution should be measured in air. The transverse radius of gyration of the actual ship should be in the range 0,35B to 0,4B and the longitudinal radius of gyration should be in the range 0,2L to 0,25L.

            Note: While inclining and rolling the model in the damaged condition may be accepted as a check for the purpose of verifying the residual stability curve, such tests should not be accepted in lieu of the intact tests.
         3.2.6.   It is assumed that the ventilators of the damage compartment of the actual ship are adequate for unhindered flooding and movement of the flood water. However in trying to scale down the ventilating arrangements of the actual ship undesirable scale effects may be introduced in the model. In order to ensure that no such effects occur it is recommended to construct the ventilating arrangements to a larger scale than that of the model, ensuring that this does not affect the flow of water on the car deck.
         3.2.7.   It is deemed appropriate to consider a damage shape representative of a cross section of the striking ship in the bow region. The 15° angle is based on a study of the cross section at a distance of B/5 from the bow for a representative selection of vessels of different types and sizes.
         The isosceles triangular profile of the prismatic damage shape is that corresponding to the load waterline.
         Additionally in cases where side casings of width less than B/5 are fitted and in order to avoid any possible scale effects, the damage length in way of the side casings must not be less than 25 mm.
         3.3.   In the original model test method of resolution 14 of the 1995 SOLAS Conference the effect of heeling induced by the maximum moment deriving from any of passenger crowding, launching of survival craft, wind and turning was not considered even though this effect was part of SOLAS. Results from an investigation have shown, however, that it would be prudent to take these effects into account and to retain the minimum of 1° heel towards the damage for practical purposes. It is to be noted that heeling due to turning was considered not to be relevant.
         3.4.   In cases where there is a margin in GM in the actual loading conditions compared to the GM limiting curve (derived from SOLAS 90), the Administration may accept that this margin is taken advantage of in the model test. In such cases the GM limiting curve should be adjusted. This adjustment can be done as follows:

         d = dS-0,6 (dS-dLS)
         where: dS is the subdivision draught; and dLS is the lightship draught.
         The adjusted curve is a straight line between the GM used in the model test at the subdivision draught and the intersection of the original SOLAS 90 curve and draught d.
         Paragraph 4 — Procedure for experiments
         4.1.   Wave spectra
         The JONSWAP spectrum should be used as this describes fetch- and duration- limited seas which correspond to the majority of conditions world wide. In this respect it is important that not only the peak period of the wave train is verified but also that the zero crossing period is correct.
         It is required that for every test run the wave spectrum is recorded and documented. Measurements for this recording should be taken at the probe closest to the wave making machine.
         It is also required that the model is instrumented so that its motions (roll, heave and pitch) as well as its attitude (heel, sinkage and trim) are monitored and recorded through-out the test.
         It has been found that it is not practical to set absolute limits for significant wave heights, peak periods and zero crossing periods of the model wave spectra. An acceptable margin has therefore been introduced.
         4.2.   To avoid interference of the mooring system with the ship dynamics, the towing carriage (to which the mooring system is attached) should follow the model at its actual drifting speed. In a sea state with irregular waves the drift speed will not be constant; a constant carriage speed would result in low frequency, large amplitude drift oscillations, which may affect the model behaviour.
         4.3.   A sufficient number of tests in different wave trains is necessary to ensure statistical reliability, i.e. the objective is to determine with a high degree of confidence that an unsafe ship will capsize in the selected conditions. A minimum number of 10 runs is considered to provide a reasonable level of reliability.
         Paragraph 5 — Survival criteria
         The contents of this paragraph are considered self-explanatory.
         Paragraph 6 — Test approval
         The following documents are to be part of the report to the administration:

                     (a)

                     damage stability calculations for worst SOLAS and mid-ship damage (if different);

                     (b)

                     general arrangement drawing of the model together with details of construction and instrumentation;

                     (c)

                     inclining experiment and measurements of radii of gyration;

                     (d)

                     nominal and measured wave spectra (at the three different locations for a representative realisation and for the tests with the model from the probe closest to the wave maker);

                     (e)

                     representative record of model motions, attitude and drift;

                     (f)

                     relevant video recordings.

               Note:
         All tests must be witnessed by the administration.’