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Food and Nutrition Board Committee on Food Chemicals Codex Institute of Medicine Food and Nutrition Board Committee on Food Chemicals Codex Revised Monograph - Carbon Dioxide Please send comments to the Committee on Food Chemicals Codex, National Academy of Sciences, FO 3042, 2101 Constitution Avenue, N.W., Washington, DC 20418 or email them to [email protected]. All comments must be received by December 15, 1996, for consideration for the First Supplement. ______________________________________________________________________________ July 9, 1996 Carbon Dioxide CO2 Formula wt 44.01 INS: 290 CAS: [124-38-9] DESCRIPTION A colorless, odorless gas, 1 L of which weighs about 1.98 g at 0° and a pressure of 760 mm of mercury. Under a pressure of about 59 atmospheres it may be condensed to a liquid, a portion of which forms a white solid ("dry ice") upon rapid vaporization. Solid Carbon Dioxide evaporates without melting upon exposure to air. One volume of the gas dissolves in about 1 volume of water, forming a solution that is acid to litmus. Functional Use in Foods Propellant and aerating agent; direct-contact freezing agent. REQUIREMENTS Identification A. Pass 100 ± 5 mL, released from the vapor phase of the contents of the container, through a carbon dioxide detector tube (see Detector Tubes under Solutions and Indicators) at the rate specified for the tube: The indicator change extends throughout the entire indicating range of the tube. B. The gas, when passed through barium hydroxide TS, forms a precipitate that dissolves with effervescence in acetic acid. Assay Not less than 99.5% of CO2, by volume. Carbonyl Sulfide Not more than 0.5 ppm, by volume. Hydrogen Sulfide Not more than 0.5 ppm, by volume. Nitric Oxide (NO) and Nitrogen Dioxide (NO2) Not more than 2.5 5 ppm each total, by volume. Nonvolatile Hydrocarbons Not more than 10 mg/kg. Sulfur Dioxide Not more than 5 ppm, by volume. Volatile Hydrocarbons (as methane) Not more than 0.005%, by volume. Water Passes test. TESTS Note: The following TESTS are designed to reflect the quality of Carbon Dioxide in both its vapor and liquid phases, which are present in previously unopened cylinders. Reduce the container pressure by means of a regulator. 1 Withdraw the specimens for the TESTS with the least possible release of Carbon Dioxide consistent with proper purging of the sampling apparatus. Measure the gases with a gas volume meter downstream from the detector tubes to minimize contamination of or changes to the specimens. Perform TESTS in the sequence in which they are listed. The various detector tubes called for in the respective TESTS are listed under Detector Tubes in Solutions and Indicators. Assay (Note: Sampling for this Assay may be done from the vapor phase for convenience, but this results in more residual volume. If the specification of 0.5 mL is exceeded from the vapor phase, a liquid specimen may be taken.) Assemble a 100-mL gas buret provided with a leveling bulb and a two-way stopcock to a gas absorption pipet of suitable capacity by connecting the pipet to one of the buret outlets. Fill the buret with slightly acidified water (turned pink with methyl orange), and fill the pipet with potassium hydroxide solution (1 in 2). By manipulating the leveling bulb and leveling water, draw the potassium hydroxide solution to fill the pipet and capillary connection up to the stopcock, and then fill the buret with the leveling water, and draw it through the other stopcock opening in such a manner that all gas bubbles are eliminated from the system. Draw into the buret 100.0 mL of specimen taken from the liquid phase as directed below in the test for Nitric Oxide and Nitrogen Dioxide. By raising the leveling bottle, force the measured specimen into the pipet. The absorption may be facilitated by rocking the pipet or by flowing the specimen between pipet and buret. Draw any residual gas into the buret, and measure its volume: Not more than 0.5 mL of gas remains. Carbonyl Sulfide Standard Preparation Flush a 500-mL glass septum-equipped sampling bulb with helium, and inject into the bulb a 0.25-mL sample of pure carbonyl sulfide. Allow the bulb to stand for 15 min to permit the gases to mix, and then inject 0.50 mL of the mixture into a second 500-mL sampling bulb, also flushed with helium, and allow this tube to stand for 15 min to permit the gases to mix. This mixture is a nominal 0.5 ppm v/v standard. Determine the exact concentration from the exact volumes of the gas-sampling bulbs. To determine these volumes, weigh the empty tubes, fill them with water, and reweigh. From the weight of the water, and its temperature, calculate the volumes of the tubes. Chromatographic System The gas chromatograph is equipped with a Sievers 350 (or equivalent)1 Chemiluminescence Detector (SCD) and a Supelco (or equivalent) 30-m ´ 0.53-mm id, 5-mm DB-5 capillary column. The carrier gas is helium set at a head-pressure of 5 psig. The split/splitless injection port is set at 100°, and the split ratio is set at 1:1. The column temperature is set at 30°. The retention time for carbonyl sulfide is approximately 3 min. The SCD is operated with 190 mL/min of hydrogen and 396 mL/min of air. The gas flows and probe position of the SCD are optimized for maximum sensitivity. Procedure Inject, in triplicate, 5.00 mL of the Standard Preparation into the gas chromatograph, record the chromatograms, and average the peak area responses. The relative standard deviation does not exceed 5.0%. Similarly, inject, in triplicate, 5.00 mL of the sample, average the peak area responses, and calculate the ppm v/v in the sample by the formula ppm = S(AU/AS), in which S is the calculated ppm of carbonyl sulfide in the Standard Preparation (approximately 0.5 ppm), AU is the average of the sample peak area responses, and AS is the average area of the Standard Preparation area responses. Hydrogen Sulfide Pass 10,050 ± 50 mL, released from the vapor phase, through a hydrogen sulfide detector tube at the rate specified for the tube: The indicator change corresponds to not more than 5 ppm, which is not more than 0.5 ppm, for the volume of carbon dioxide specified in this test. 1Any sulfur-selective detector may be used; e.g., electrolytic conductivity, flame photometric, or sulfur chemiluminescence. The detector must be capable of detecting less than 0.1 ppm v/v of carbonyl sulfide with a signal-to-noise ratio of 10:1. 2 Nitric Oxide (NO) and Nitrogen Dioxide (NO2) Position the sample container so that when its valve is opened, the liquid phase can be sampled (generally this requires that the cylinder be inverted). Attach a section of tubing long enough to act as a vaporizer for the small quantity of liquid to be sampled. Connect one end of a nitric oxide– nitrogen dioxide detector tube to the tubing and the other end to a gas flow meter. Pass 500 mL of the liquid sample through the tube at a suitable rate. No frost should reach the tube inlet from the expanding sample. The indicator change corresponds to not more than 2.5 5 ppm. Repeat the test, using another identical detector tube but taking the sample from the gaseous phase. The indicator change from this second test corresponds to not more than 2.5 ppm. Nonvolatile Hydrocarbons Pass a sample of liquid Carbon Dioxide from a storage container or sample cylinder through a commercial carbon dioxide snow horn directly into an open, clean container. Collect the resulting Carbon Dioxide snow in this container. Weigh 500 g of this sample into a clean beaker. Allow the Carbon Dioxide solid to sublime completely, with a watch-glass placed over the beaker to prevent ambient contamination. Wash the beaker with a residue-free solvent, and transfer the solvent from the beaker to a clean, tared watch-glass or petri dish with two additional rinses of the beaker with the solvent. Allow the solvent to evaporate, using heating to 104°, until the watch-glass or petri dish is at a constant weight. Determine the weight of the residue by difference. The weight of the residue does not exceed 5 mg (10 mg/kg). Sulfur Dioxide Pass 1050 ± 50 mL, taken from the liquid phase as described in the test for Nitric Oxide and Nitrogen Dioxide, through a sulfur dioxide detector tube at the rate specified for the tube: The indicator change corresponds to not more than 5 ppm. Volatile Hydrocarbons Standard Preparation Flush a 500-mL glass septum-equipped sampling bulb with helium, and inject into the bulb a 5.00-mL sample of methane. Allow the bulb to stand for 15 min to permit the gases to mix, and then inject 2.50 mL of the mixture into a second 500-mL sampling bulb, also flushed with helium, and allow this tube to stand for 15 min to permit the gases to mix. This mixture is a nominal 50 ppm v/v standard. Determine the exact concentration from the exact volumes of the gas-sampling bulbs. To determine these volumes, weigh the empty tubes, fill them with water, and reweigh. From the weight of the water and its temperature, calculate the volumes of the tubes. Chromatographic System The gas chromatograph is equipped with a flame ionization detector and a 1.8-m ´ 3-mm od metal column packed with 80- to 100-mesh Hayesep Q (or equivalent). The carrier gas is helium at a flow rate of 30 mL/min.
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