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Commission Regulation (EC) No 2870/2000Show full title

Commission Regulation (EC) No 2870/2000 of 19 December 2000 laying down Community reference methods for the analysis of spirits drinks

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  1. Introductory TextNext Match

  2. Article 1.The Community reference methods for the analysis of spirits drinks...Previous MatchNext Match

  3. Article 2.Notwithstanding the first indent of Article 1, other analytical methods...Previous MatchNext Match

  4. Article 3.(1.) Where ... analytical reference methods are not laid down...Previous MatchNext Match

  5. Article 4.For the purposes of this Regulation: ‘repeatability limit’: shall be...Previous MatchNext Match

  6. Article 5.This Regulation shall enter into force on the seventh day...Previous MatchNext Match

  7. SignaturePrevious MatchNext Match

    1. ANNEXPrevious MatchNext Match

      1. I. DETERMINATION OF ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS Previous MatchNext Match

        1. Introduction Previous MatchNext Match

          1. 1. Scope Previous MatchNext Match

          2. 2. Normative References Previous MatchNext Match

          3. 3. Terms and Definitions Previous MatchNext Match

            1. 3.1. Reference temperature: Previous MatchNext Match

              1. Note 1: Previous MatchNext Match

                1. Previous MatchNext Match

            2. 3.2. Density: Previous MatchNext Match

            3. 3.3. Specific gravity: Previous MatchNext Match

              1. Note 2: Previous MatchNext Match

                1. Previous MatchNext Match

            4. 3.4. Real alcoholic strength by volume: Previous MatchNext Match

              1. Note 3: Previous MatchNext Match

                1. Previous MatchNext Match

          4. 4. Principle Previous MatchNext Match

        2. APPENDIX I: PREPARATION OF DISTILLATE Previous MatchNext Match

          1. 1. Scope Previous MatchNext Match

          2. 2. Principle Previous MatchNext Match

          3. 3. Reagents and Materials Previous MatchNext Match

            1. 3.1. Anti-bumping granules. Previous MatchNext Match

            2. 3.2. Concentrated antifoam emulsion (for crème liqueurs). Previous MatchNext Match

          4. 4. Apparatus and equipment Previous MatchNext Match

            1. Note: Previous MatchNext Match

              1. Previous MatchNext Match

          5. 5. Storage of test samples Previous MatchNext Match

          6. 6. Procedure Previous MatchNext Match

            1. 6.1. Distillation apparatus verification. Previous MatchNext Match

            2. 6.2. Spirit drinks with alcoholic strength below 50 % vol. Previous MatchNext Match

              1. Note: Previous MatchNext Match

                1. Previous MatchNext Match

            3. 6.3. Spirit drinks with alcoholic strength above 50 % vol. Previous MatchNext Match

              1. Note: Previous MatchNext Match

                1. Previous MatchNext Match

        3. APPENDIX II: MEASUREMENT OF DENSITY OF DISTILLATE Previous MatchNext Match

          1. METHOD A: DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS...Previous MatchNext Match

            1. A.1. Principle Previous MatchNext Match

            2. A.2. Reagents and materials Previous MatchNext Match

              1. A.2.1. Sodium chloride solution (2 % w/v) Previous MatchNext Match

            3. A.3. Apparatus and Equipment Previous MatchNext Match

              1. Note 1: Previous MatchNext Match

                1. Previous MatchNext Match

            4. A.4. Procedure Previous MatchNext Match

              1. A.4.1. Calibration of pycnometer Previous MatchNext Match

                1. A.4.1.1. Calibration using a single-pan balance: Previous MatchNext Match

                  1. A.4.1.1.1. Weigh the clean, dry pycnometer (P). Previous MatchNext Match

                  2. A.4.1.1.2. Fill the pycnometer carefully with distilled water at ambient temperature...Previous MatchNext Match

                  3. A.4.1.1.3. Weigh the tare bottle (T0). Previous MatchNext Match

                  4. A.4.1.1.4. Calculation Previous MatchNext Match

                2. A.4.1.2. Calibration method using a twin-pan balance: Previous MatchNext Match

              2. A.4.2. Determination of alcoholic strength of test sample Previous MatchNext Match

            5. A.5. Method performance characteristics (precision) Previous MatchNext Match

              1. A.5.1. Statistical results of the interlaboratory test Previous MatchNext Match

          2. METHOD B: DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS...Previous MatchNext Match

            1. B.1. Principle Previous MatchNext Match

            2. B.2. Reagents and materials Previous MatchNext Match

            3. B.3. Apparatus and equipment Previous MatchNext Match

            4. B.4. Procedure Previous MatchNext Match

            5. B.5. Method performance characteristics (precision) Previous MatchNext Match

              1. B.5.1. Statistical results of the interlaboratory test Previous MatchNext Match

          3. METHOD C: DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS...Previous MatchNext Match

            1. C.1. Principle Previous MatchNext Match

            2. C.2. Reagents and materials Previous MatchNext Match

              1. C.2.1. Float cleaning solution (sodium hydroxide, 30 % w/v) Previous MatchNext Match

            3. C.3. Apparatus and Equipment Previous MatchNext Match

              1. Note 1: Previous MatchNext Match

                1. Previous MatchNext Match

            4. C.4. Procedure Previous MatchNext Match

            5. C.5. Method performance characteristics (precision) Previous MatchNext Match

              1. C.5.1. Statistical results of the interlaboratory test Previous MatchNext Match

      2. II. DETERMINATION OF TOTAL DRY EXTRACT OF SPIRIT DRINKS BY GRAVIMETRY...Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative References Previous MatchNext Match

        3. 3. Definition Previous MatchNext Match

        4. 4. Principle Previous MatchNext Match

        5. 5. Apparatus and Equipment Previous MatchNext Match

        6. 6. Sampling and samples Previous MatchNext Match

        7. 7. Procedure Previous MatchNext Match

          1. 7.1. Pipette 25 ml of the spirit containing less than 15...Previous MatchNext Match

          2. 7.2. Complete the drying by placing the evaporating dish in a...Previous MatchNext Match

        8. 8. Calculation Previous MatchNext Match

        9. 9. Method performance characteristics (precision) Previous MatchNext Match

          1. 9.1. Statistical results of the interlaboratory test Previous MatchNext Match

      3. III. DETERMINATION OF VOLATILE SUBSTANCES AND METHANOL OF SPIRIT DRINKS Previous MatchNext Match

        1. III.1. GENERAL REMARKS Previous MatchNext Match

          1. 1. Definitions Previous MatchNext Match

          2. 2. Gas chromatographic analysis of volatile compounds Previous MatchNext Match

        2. III.2. GAS CHROMATOGRAPHIC DETERMINATION OF VOLATILE CONGENERS: ALDEHYDES, HIGHER ALCOHOLS, ETHYL...Previous MatchNext Match

          1. 1. Scope Previous MatchNext Match

          2. 2. Normative References Previous MatchNext Match

          3. 3. Definition Previous MatchNext Match

          4. 4. Principle Previous MatchNext Match

          5. 5. Reagents and materials Previous MatchNext Match

          6. 6. Apparatus and equipment Previous MatchNext Match

          7. 7. Sampling and samples. Previous MatchNext Match

          8. 8. Procedure (used for the validated method) Previous MatchNext Match

          9. 9. Calculation Previous MatchNext Match

          10. 10. Quality assurance and control (used for the validated method) Previous MatchNext Match

          11. 11. Method performance characteristics (precision) Previous MatchNext Match

        3. III.3. DETERMINATION OF VOLATILE ACIDITY OF SPIRIT DRINKS Previous MatchNext Match

          1. 1. Scope Previous MatchNext Match

          2. 2. Normative references Previous MatchNext Match

          3. 3. Definitions Previous MatchNext Match

            1. 3.1. Volatile acidity is calculated by deducting the fixed acidity from...Previous MatchNext Match

            2. 3.2. Total acidity is the sum of titratable acidities. Previous MatchNext Match

            3. 3.3. Fixed acidity is the acidity of the residue left after...Previous MatchNext Match

          4. 4. Principle Previous MatchNext Match

          5. 5. Reagents and materials Previous MatchNext Match

            1. 5.1. 0,01 M sodium hydroxide solution (NaOH) Previous MatchNext Match

            2. 5.2. Mixed indicator solution: Previous MatchNext Match

          6. 6. Apparatus and equipment Previous MatchNext Match

          7. 7. Sampling and samples Previous MatchNext Match

          8. 8. Procedure Previous MatchNext Match

            1. 8.1. Total acidity Previous MatchNext Match

              1. 8.1.1. Preparation of sample Previous MatchNext Match

              2. 8.1.2. Titration Previous MatchNext Match

              3. 8.1.3. Calculation Previous MatchNext Match

            2. 8.2. Fixed acidity Previous MatchNext Match

              1. 8.2.1. Preparation of sample Previous MatchNext Match

              2. 8.2.2. Titration Previous MatchNext Match

              3. 8.2.3. Calculation Previous MatchNext Match

          9. 9. Calculation of volatile acidity Previous MatchNext Match

            1. 9.1. Expression in milliequivalents per l: Previous MatchNext Match

            2. 9.2. Expression in mg of acetic acid per l: Previous MatchNext Match

            3. 9.3. Expression in g of acetic acid per hl of pure...Previous MatchNext Match

          10. 10. Method performance characteristics (Precision) Previous MatchNext Match

            1. 10.1. Statistical results of the interlaboratory test Previous MatchNext Match

              1. (1) ‘Protocol for the design, conduct and interpretation of method-performance studies’,...Previous MatchNext Match

              2. (2) Horwitz, W. (1982) Analytical Chemistry , 54, 67A-76A. Previous MatchNext Match

      4. V. ANETHOLE. GAS CHROMATOGRAPHIC DETERMINATION OF TRANS-ANETHOLE IN SPIRIT DRINKS Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative references Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents and materials Previous MatchNext Match

          1. 4.1. Ethanol 96 % vol. (CAS 64-17-5) Previous MatchNext Match

          2. 4.2. 1-methoxy-4-(1-propenyl) benzene; (trans-anethole) (CAS 4180-23-8) Previous MatchNext Match

          3. 4.3. 4-allylanisole, (estragole) (CAS 140-67-0), suggested internal standard (IS) Previous MatchNext Match

          4. 4.4. Ethanol 45 % vol. Previous MatchNext Match

          5. 4.5. Preparation of standard solutions Previous MatchNext Match

            1. 4.5.1. Standard solution A Previous MatchNext Match

            2. 4.5.2. Internal standard solution B Previous MatchNext Match

            3. 4.5.3. Solutions used to check the linearity response of the flame...Previous MatchNext Match

            4. 4.5.4. Standard solution C Previous MatchNext Match

        5. 5. Apparatus and equipment Previous MatchNext Match

          1. 5.1. A capillary gas chromatograph fitted with a flame ionisation detector...Previous MatchNext Match

          2. 5.2. Split/splitless injector Previous MatchNext Match

          3. 5.3. Capillary column, for example: Previous MatchNext Match

          4. 5.4. Common laboratory equipment: A grade volumetric glassware, analytical balance (precision:...Previous MatchNext Match

        6. 6. Chromatography conditions Previous MatchNext Match

        7. 7. Samples Previous MatchNext Match

        8. 8. Procedure Previous MatchNext Match

          1. 8.1. Sample screening for estragole Previous MatchNext Match

          2. 8.2. Preparation of unknown samples Previous MatchNext Match

          3. 8.3. Blank Previous MatchNext Match

          4. 8.4. Linearity test Previous MatchNext Match

          5. 8.5. Determination Previous MatchNext Match

        9. 9. Calculation of response factor Previous MatchNext Match

          1. 9.1. Response factor (RF i ) calculation Previous MatchNext Match

          2. 9.2. Analysis of the linearity response test solutions Previous MatchNext Match

          3. 9.3. Analysis of the sample Previous MatchNext Match

        10. 10. Calculation of results Previous MatchNext Match

        11. 11. Quality assurance and control Previous MatchNext Match

        12. 12. Treatment of spirits sample containing large amount of sugar and...Previous MatchNext Match

          1. 12.1. Principle Previous MatchNext Match

          2. 12.2. Reagents and materials Previous MatchNext Match

            1. 12.2.1. Ammonium sulphate, anhydrous, (CAS 7783-20-2). Previous MatchNext Match

            2. 12.2.2. Sodium phosphate, dibasic, dodecahydrate, (CAS 10039-32-4). Previous MatchNext Match

          3. 12.3. Apparatus and equipment Previous MatchNext Match

          4. 12.4. Procedure Previous MatchNext Match

            1. 12.4.1. Sample screening for estragole Previous MatchNext Match

            2. 12.4.2. Extraction Previous MatchNext Match

            3. 12.4.3. Preparation of the extracted sample to be analysed Previous MatchNext Match

          5. 12.5. Determination Previous MatchNext Match

          6. 12.6. Calculation of results Previous MatchNext Match

          7. 12.7. Quality control and assurance Previous MatchNext Match

        13. 13. Method performance characteristics (precision) Previous MatchNext Match

      5. VI. GLYCYRRHIZIC ACID. DETERMINATION OF GLYCYRRHIZIC ACID USING HIGH PERFORMANCE LIQUID...Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative references Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents and materials Previous MatchNext Match

          1. 4.1. Ethanol 96 % vol. (CAS 64-17-5). Previous MatchNext Match

          2. 4.2. Ammonium glycyrrhizinate, C 42 H 62 O 16 .NH 3...Previous MatchNext Match

          3. 4.3. Glacial acetic acid, CH 3 COOH, (CAS 64-19-7). Previous MatchNext Match

          4. 4.4. Methanol, CH 3 OH (CAS 67-56-1). Previous MatchNext Match

          5. 4.5. Ethanol 50 % vol. Previous MatchNext Match

          6. 4.6. Preparation of the HPLC elution solutions Previous MatchNext Match

            1. 4.6.1. Elution solvent A (example) Previous MatchNext Match

              1. Note: Previous MatchNext Match

                1. Previous MatchNext Match

            2. 4.6.2. Elution solvent B Previous MatchNext Match

          7. 4.7. Preparation of standard solutions Previous MatchNext Match

            1. 4.7.1. Reference solution C Previous MatchNext Match

            2. 4.7.2. Standard solutions used to check the linearity of the response...Previous MatchNext Match

        5. 5. Apparatus and equipment Previous MatchNext Match

          1. 5.1. Separation system Previous MatchNext Match

            1. 5.1.1. High-performance liquid chromatograph. Previous MatchNext Match

            2. 5.1.2. Pumping system enabling one to achieve and maintain a constant...Previous MatchNext Match

            3. 5.1.3. UV spectrophotometric detection system: to be set at 254 nm....Previous MatchNext Match

            4. 5.1.4. Solvent degassing system. Previous MatchNext Match

          2. 5.2. Computational integrator or recorder, the performance of which is compatible...Previous MatchNext Match

          3. 5.3. Column (example): Previous MatchNext Match

          4. 5.4. Laboratory equipment Previous MatchNext Match

            1. 5.4.1. Analytical balance with a precision of 0,1 mg Previous MatchNext Match

            2. 5.4.2. A-grade volumetric glassware Previous MatchNext Match

            3. 5.4.3. Micromembrane filtration arrangement for small volumes. Previous MatchNext Match

        6. 6. Chromatography conditions Previous MatchNext Match

          1. 6.1. Elution characteristics: (example) Previous MatchNext Match

          2. 6.2. Detection: Previous MatchNext Match

        7. 7. Procedure Previous MatchNext Match

          1. 7.1. Preparation of the spirit sample Previous MatchNext Match

          2. 7.2. Determination Previous MatchNext Match

        8. 8. Method performance characteristics (precision) Previous MatchNext Match

      6. VII. CHALCONES. HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR VERIFYING THE PRESENCE OF...Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative references Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents and materials Previous MatchNext Match

          1. 4.1. Ethanol 96 % vol. (CAS 64-17-5) Previous MatchNext Match

          2. 4.2. Acetonitrile, CH 3 CN, (CAS 75-05-8) Previous MatchNext Match

          3. 4.3. Reference substance: Glycyrrhiza glabra : liquorice, ‘sweet root’ Previous MatchNext Match

          4. 4.4. Sodium acetate, CH 3 COONa, (CAS 127-09-3) Previous MatchNext Match

          5. 4.5. Glacial acetic acid, CH 3 COOH, (CAS 64-19-7) Previous MatchNext Match

          6. 4.6. Preparation of solutions Previous MatchNext Match

            1. 4.6.1. Ethanol 50 % volume Previous MatchNext Match

            2. 4.6.2. Solvent A: acetonitrile Previous MatchNext Match

            3. 4.6.3. Solvent B: 0,1 M sodium acetate buffer solution, pH 4,66....Previous MatchNext Match

        5. 5. Preparation of the reference extract from Glycyrrhiza glabra (4.3) Previous MatchNext Match

          1. 5.1. Weigh 10 g of ground liquorice root ( Glycyrrhiza glabra...Previous MatchNext Match

          2. 5.2. Recover the liquorice extract from the filter Previous MatchNext Match

          3. 5.3. The liquorice root extraction must be performed three times in...Previous MatchNext Match

          4. 5.4. Combine the three filtrates. Previous MatchNext Match

          5. 5.5. Evaporate the solvent phase (of 5.4) on a rotary evaporator....Previous MatchNext Match

          6. 5.6. Take up the residual extract (of 5.5) with 100 ml...Previous MatchNext Match

        6. 6. Apparatus and equipment Previous MatchNext Match

          1. 6.1. Separation system. Previous MatchNext Match

            1. 6.1.1. High-performance liquid chromatograph. Previous MatchNext Match

            2. 6.1.2. Pumping system capable of achieving and maintaining a constant or...Previous MatchNext Match

            3. 6.1.3. UV/visible spectrophotometric detection system that can be set at 254...Previous MatchNext Match

            4. 6.1.4. Solvent degassing system: Previous MatchNext Match

            5. 6.1.5. Column oven that can be set at a temperature of...Previous MatchNext Match

          2. 6.2. Computational integrator or recorder, the performance of which is compatible...Previous MatchNext Match

          3. 6.3. Column Previous MatchNext Match

          4. 6.4. Common laboratory equipment, including: Previous MatchNext Match

          5. 6.5. Chromatography conditions (example). Previous MatchNext Match

            1. 6.5.1. Elution characteristics of solvents A (4.6.2) and B (4.6.3): Previous MatchNext Match

            2. 6.5.2. Flow rate: 1 ml/minute. Previous MatchNext Match

            3. 6.5.3. UV detector settings: Previous MatchNext Match

        7. 7. Procedure Previous MatchNext Match

          1. 7.1. Preparation of the spirit sample Previous MatchNext Match

          2. 7.2. Preparation of the residual liquorice extract (5.6) Previous MatchNext Match

          3. 7.3. Determination Previous MatchNext Match

            1. 7.3.1. Inject 20 μl of the prepared liquorice extract (7.2). Perform...Previous MatchNext Match

            2. 7.3.2. Inject 20 μl of the sample (7.1) (aniseed-flavoured spirit sample)....Previous MatchNext Match

            3. 7.3.3. Compare the two chromatograms. There must be a great similarity...Previous MatchNext Match

        8. 8. Characteristic chromatogram for a pastis Previous MatchNext Match

        9. 9. Method performance characteristics (precision) Previous MatchNext Match

      7. VIII. TOTAL SUGARS Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative references Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents and materials Previous MatchNext Match

          1. 4.1. Glucose (CAS 50-99-7), at least 99 % pure. Previous MatchNext Match

          2. 4.2. Fructose (CAS 57-48-7), at least 99 % pure. Previous MatchNext Match

          3. 4.3. Sucrose (CAS 57-50-1), at least 99 % pure. Previous MatchNext Match

          4. 4.4. Lactose (CAS 5965-66-2), at least 99 % pure. Previous MatchNext Match

          5. 4.5. Maltose monohydrate (CAS 6363-53-7), at least 99 % pure. Previous MatchNext Match

          6. 4.6. Pure acetonitrile (CAS 75-05-8) for HPLC analysis. Previous MatchNext Match

          7. 4.7. Distilled or demineralised water, preferably microfiltered. Previous MatchNext Match

          8. 4.8. Solvents (example) Previous MatchNext Match

          9. 4.9. Ethanol absolute (CAS 64-17-5). Previous MatchNext Match

          10. 4.10. Ethanol solution (5 %, v/v). Previous MatchNext Match

          11. 4.11. Preparation of stock standard solution (20 g/l) Previous MatchNext Match

          12. 4.12. Preparation of working standard solutions (2,5, 5,0, 7,5, 10,0 and...Previous MatchNext Match

        5. 5. Apparatus and Equipment Previous MatchNext Match

          1. 5.1. HPLC system capable of achieving baseline resolution of all of...Previous MatchNext Match

            1. 5.1.1. High-performance liquid chromatograph with a six-way injection valve fitted with...Previous MatchNext Match

            2. 5.1.2. Pumping system enabling one to achieve and maintain a constant...Previous MatchNext Match

            3. 5.1.3. Differential refractometer. Previous MatchNext Match

            4. 5.1.4. Computational integrator or recorder, the performance of which is compatible...Previous MatchNext Match

            5. 5.1.5. Pre-column: Previous MatchNext Match

            6. 5.1.6. Column (example): Previous MatchNext Match

            7. 5.1.7. Chromatography conditions (example): Previous MatchNext Match

          2. 5.2. Analytical balance accurate to 0,1 mg. Previous MatchNext Match

          3. 5.3. Filtration set-up for small volumes using a 0,45 μm micromembrane....Previous MatchNext Match

        6. 6. Sample storage Previous MatchNext Match

        7. 7. Procedure Previous MatchNext Match

          1. 7.1. PART A: Sample preparation Previous MatchNext Match

            1. 7.1.1. Shake the sample. Previous MatchNext Match

            2. 7.1.2. Filter the sample through a filter with a pore size...Previous MatchNext Match

          2. 7.2. PART B: HPLC Previous MatchNext Match

            1. 7.2.1. Determination Previous MatchNext Match

            2. 7.2.2. Should any peak of a sample have a greater area...Previous MatchNext Match

        8. 8. Calculation Previous MatchNext Match

        9. 9. Method performance characteristics (precision) Previous MatchNext Match

          1. 9.1. Statistical results of the interlaboratory test Previous MatchNext Match

            1. (1) ‘ Protocol for the design, conduct and interpretation of method-performance...Previous MatchNext Match

            2. (2) Horwitz, W. (1982) Analytical Chemistry , 54, 67A-76A. Previous MatchNext Match

      8. IX. EGG YOLK. DETERMINATION OF EGG YOLK CONCENTRATION IN SPIRIT DRINKS...Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative references Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents and materials Previous MatchNext Match

          1. 4.1. Double-distilled water Previous MatchNext Match

          2. 4.2. Diatomaceous earth Previous MatchNext Match

          3. 4.3. Ethanol 96 % vol. (CAS 64-17-5) Previous MatchNext Match

          4. 4.4. 15 % magnesium acetate (CAS 16674-78-5) solution Previous MatchNext Match

          5. 4.5. 10 % sulphuric acid (CAS 7664-93-9) Previous MatchNext Match

          6. 4.6. 1 N sulphuric acid. Previous MatchNext Match

          7. 4.7. 0,16 g/l potassium dihydrogen phosphate (CAS 778-77-0), KH 2 PO...Previous MatchNext Match

          8. 4.8. Reagent for phosphate determination: Previous MatchNext Match

        5. 5. Apparatus and equipment Previous MatchNext Match

          1. 5.1. 100 ml conical flask Previous MatchNext Match

          2. 5.2. Ultrasonic bath (or magnetic stirrer) Previous MatchNext Match

          3. 5.3. 100 ml volumetric flask Previous MatchNext Match

          4. 5.4. 20 o C water bath Previous MatchNext Match

          5. 5.5. Filter (Whatman No 4 or equivalent) Previous MatchNext Match

          6. 5.6. Porcelain (or platinum) crucible Previous MatchNext Match

          7. 5.7. Boiling water bath Previous MatchNext Match

          8. 5.8. Hot plate Previous MatchNext Match

          9. 5.9. Muffle furnace Previous MatchNext Match

          10. 5.10. 50 ml volumetric flask Previous MatchNext Match

          11. 5.11. 20 ml volumetric flask Previous MatchNext Match

          12. 5.12. Spectrophotometer set at 420 nm Previous MatchNext Match

          13. 5.13. 1 cm cuvette. Previous MatchNext Match

        6. 6. Samples Previous MatchNext Match

        7. 7. Procedure Previous MatchNext Match

          1. 7.1. Sample preparation Previous MatchNext Match

            1. 7.1.1. Weigh 10 g of the sample into a 100 ml...Previous MatchNext Match

            2. 7.1.2. Add gradually 70 ml of ethanol (4.3) in small portions,...Previous MatchNext Match

            3. 7.1.3. Transfer the contents of the flask to a 100 ml...Previous MatchNext Match

            4. 7.1.4. Add a small amount of diatomaceous earth (4.2) and filter...Previous MatchNext Match

            5. 7.1.5. Transfer 25 ml of the filtrate to a porcelain (or...Previous MatchNext Match

            6. 7.1.6. Place the crucibles on a hot plate (5.8) and heat...Previous MatchNext Match

            7. 7.1.7. Ash the residue by heating to incandescence at 600 o...Previous MatchNext Match

            8. 7.1.8. Take up the ash with 10 ml of 10 %...Previous MatchNext Match

          2. 7.2. Photometric phosphate assay Previous MatchNext Match

            1. 7.2.1. Comparative solution Previous MatchNext Match

              1. 7.2.1.1. Place 10 ml of 10 % sulphuric acid (4.5) in...Previous MatchNext Match

              2. 7.2.1.2. Add to a 5 ml aliquot of this solution (7.2.1.1),...Previous MatchNext Match

              3. 7.2.1.3. Stopper with a loosely inserted stopper, shake, and heat in...Previous MatchNext Match

              4. 7.2.1.4. Fill a 1 cm cuvette (5.13) with this comparative solution....Previous MatchNext Match

            2. 7.2.2. Sample solution Previous MatchNext Match

              1. 7.2.2.1. Add to a 5 ml aliquot of the ash solution...Previous MatchNext Match

              2. 7.2.2.2. Stopper with a loosely inserted stopper, shake, and heat in...Previous MatchNext Match

              3. 7.2.2.3. The yellow solution that develops is immediately analysed spectrophotometrically (5.12)...Previous MatchNext Match

            3. 7.2.3. Calibration curve Previous MatchNext Match

              1. 7.2.3.1. To construct the calibration curve, add 2 ml aliquots of...Previous MatchNext Match

              2. 7.2.3.2. Stopper with a loosely inserted stopper, shake, and heat in...Previous MatchNext Match

              3. 7.2.3.3. Construction of the calibration curve: Previous MatchNext Match

        8. 8. Expression of results Previous MatchNext Match

        9. 9. Method performance characteristics (precision) Previous MatchNext Match

      9. X. DETERMINATION OF THE FOLLOWING WOOD COMPOUNDS IN SPIRIT DRINKS BY...Previous MatchNext Match

        1. 1. Scope Previous MatchNext Match

        2. 2. Normative reference Previous MatchNext Match

        3. 3. Principle Previous MatchNext Match

        4. 4. Reagents Previous MatchNext Match

          1. 4.1. 96 % vol. alcohol. Previous MatchNext Match

          2. 4.2. HPLC-quality methanol (Solvent B). Previous MatchNext Match

          3. 4.3. Acetic acid diluted to 0,5 % vol. (Solvent A). Previous MatchNext Match

          4. 4.4. Mobile phases: (given as an example only). Previous MatchNext Match

          5. 4.5. Reference standards of 99 % minimum purity: furfural, 5-hydroxymethyl furfural,...Previous MatchNext Match

          6. 4.6. Reference solution: the standard substances are dissolved in a 50...Previous MatchNext Match

        5. 5. Apparatus Previous MatchNext Match

          1. 5.1. A high-performance liquid chromatograph capable of functioning in binary gradient...Previous MatchNext Match

          2. 5.2. Syringes for HPLC. Previous MatchNext Match

          3. 5.3. Device for membrane-filtration of small volumes. Previous MatchNext Match

          4. 5.4. Integrator-computer or recorder with performance compatible with the entire apparatus,...Previous MatchNext Match

        6. 6. Procedure Previous MatchNext Match

          1. 6.1. Preparation of the solution to be injected Previous MatchNext Match

          2. 6.2. Chromatographic operating conditions: carry out the analysis at ambient temperature...Previous MatchNext Match

          3. 6.3. Determination Previous MatchNext Match

            1. 6.3.1. Inject the reference standards separately, then mixed. Previous MatchNext Match

            2. 6.3.2. Inject the sample as prepared in 6.1. Previous MatchNext Match

            3. 6.3.3. Measure the area of the peaks in the reference solution...Previous MatchNext Match

        7. 7. Expression of results Previous MatchNext Match

        8. 8. Performance characteristics of the method (precision) Previous MatchNext Match

          1. 8.1. Furfural Previous MatchNext Match

          2. 8.2. 5-Hydroxymethylfurfural Previous MatchNext Match

          3. 8.3. 5-Methylfurfural Previous MatchNext Match

          4. 8.4. Vanillin Previous MatchNext Match

          5. 8.5. Syringaldehyde Previous MatchNext Match

          6. 8.6. Coniferaldehyde Previous MatchNext Match

          7. 8.7. Sinapaldehyde Previous MatchNext Match

          8. 8.8. Gallic acid Previous MatchNext Match

          9. 8.9. Ellagic acid Previous MatchNext Match

          10. 8.10. Vanillic acid Previous MatchNext Match

          11. 8.11. Syringic acid Previous MatchNext Match

          12. 8.12. Scopoletin Previous MatchNext Match

            1. (1) ‘Protocol for the design, conduct and interpretation of method-performance studies’,...Previous MatchNext Match

            2. (2) Horwitz, W. (1982) Analytical Chemistry , 54, 67A-76A. Previous MatchNext Match

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