1、Designation: F 1115 95 (Reapproved 2001)Standard Test Method forDetermining the Carbon Dioxide Loss of BeverageContainers1This standard is issued under the fixed designation F 1115; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 The objective of this test method is to determine thecarbon dioxide (CO2) loss from plastic beverage conta
3、inersafter a specified period of storage time.1.2 Factors contributing to this pressure loss are volumeexpansion and the gas transport characteristics of the packageincluding permeation and leakage.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its u
4、se. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specification for Reagent Water
5、E 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 380 Practice for the Use of International System of Units(SI) (the Modernized Metric System)3E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Units, symbols,
6、and abbreviations used in this testmethod are those recommended by Practice E 380.3.2 Definitions of Terms Specific to This Standard:3.2.1 carbonation volumethe volume of CO2(at 0C, 1atm pressure) that is dissolved in the carbonated water, dividedby the volume of the liquid (based on water volume at
7、 3.98Cequals 1.000 g/cm3). The conversion of pressure to carbonationvolumes should be made using a carbonation volumes table. Atable for carbonated water would not necessarily apply toliquids containing additional substances, such as carbonatedbeverages containing sugar.3.2.2 initial pressurethe equ
8、ilibrium pressure in the testbottles as measured at 24 h after filling with carbonated water.(The filled bottles are allowed to stand for 24 h to obtaintemperature equilibrium with the test environment and to allowtime for pressure adjustment and equilibration of the CO2inthe headspace and liquid.)3
9、.2.3 samplea set of bottles produced on the same equip-ment in a single run and using the same material and processconditions. Bottles should represent normal thickness distribu-tion.3.2.4 shelf lifethe number of weeks a sample set of bottlesretain a specified carbonation level, or a percent of the
10、initiallevel.3.2.5 pressure monitoring devicea pressure gage or trans-ducer assembly with support electronics for indicating internalpressure level of the bottle. This device is used with brassclosure fitting-equipped bottles.3.2.5.1 temperature monitoring devicea thermocouplewith support electronic
11、s (same equipment as described in7.2.2). A precision glass thermometer may be used provided abottle filled with noncarbonated water is used as a control ineach sample set (Procedure A).3.2.6 Terriss CO2Analyzeran electronic unit that willpierce the roll-on closure and automatically read pressure,tem
12、perature, and volume of gas (Procedure B).3.2.7 Zahm-Nagle Pressure Testera unit that manuallypierces the closure and measures container pressure; an at-tached thermometer is then used to measure temperature(Procedure B).1This test method is under the jurisdiction of ASTM Committee F2 on FlexibleBar
13、rier Materials and is the direct responsibility of Subcommittee F02.10 onPermeation.Current edition approved Sept. 10, 1995. Published March 1996. Originallypublished as F 1115 87. Last previous edition F 1115 87.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cu
14、stomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.8 support ringa pr
15、otrusion below the bottle finishwhich is used to support or stabilize the bottle during fillingand capping.3.2.9 finishthe threaded part of the bottle which receivesthe cap.3.3 For other terms used in this test method, refer toTerminology D 1129.4. Summary of Test Method4.1 Test bottles are filled w
16、ith carbonated water or beverageand, after closure application, are exposed to test environmentsfor specified time periods. By periodically measuring the initialand final carbonation levels in the container, the loss and ratecan be calculated.5. Significance and Use5.1 Two procedures, A and B, are o
17、utlined in this testmethod. Procedure A is used most often for development ofvarious beverage container designs to determine the functionalcharacteristics of the package in regard to shelf life. ProcedureB is recommended for use in beverage filling operations as aquality control tool in maintaining
18、the desired CO2fill pres-sure. A loss of CO2will affect product taste.5.1.1 Procedure A involves the use of sensitive pressure andtemperature monitoring equipment where a high degree ofaccuracy is essential, for example, a micro-pressure transducerand thermocouple for measuring pressure and temperat
19、ure ofthe package in a closed system. Alternatively, this proceduremay also use bottles closed with roll-on aluminum capscontaining rubber septums. The septum is pierced with ahypodermic needle attached to a pressure transducer to obtainpressure readings. This procedure should be confined tolaborato
20、ries that are practiced in this type of analytical testing.5.1.2 Procedure B is more widely used when measuring thecarbonation level of the package due to the simplicity of thetechnique. A simple Zahm-Nagle pressure assembly or TerrisCO2Analyzer is utilized.6. Interferences6.1 The following conditio
21、ns can interfere with the testresults:6.1.1 CO2leakage at closure due to defective bottle finish orimproper sealing of closure apparatus,6.1.2 CO2leakage due to improper equipment set-up,6.1.3 Change in ambient temperature, upsetting the equilib-rium of the headspace and dissolved CO2gas,6.1.4 Measu
22、rement of pressure before the bottle and liquidhave reached ambient temperature,6.1.5 Inaccurate thermocouple device used for measuringthe liquid temperature,6.1.6 Excessive air in the bottle headspace or dissolved inthe liquid,6.1.7 Inaccurate or erratic pressure monitoring device,6.1.8 Ambient hum
23、idity in the test area,6.1.9 Age of bottles, and6.1.10 Excessive bottle-to-bottle variation in the materialdistribution, which may result in a wide variation from bottle tobottle within the sample population.7. Apparatus7.1 Procedures A and B:7.1.1 Bottle Stand, optional.7.1.2 Height Measuring Devic
24、e, capable of measuring towithin 0.001 in. (optional).7.1.3 Top Loading Balance, capable of weighing to 2500 gwith an accuracy of 60.01 g (optional).7.1.4 Outside Diameter Measuring Device, p tape or similardevice (optional).47.1.5 Carbonated Water or Beverage Dispensing Equip-ment.7.1.6 Micrometer
25、or Ultrasonic Thickness Gage, capable ofmeasuring to within 0.001 in. or less (optional).7.2 Procedure A:7.2.1 Machined Metal Cap (see Fig. 1).7.2.2 Temperature-Measuring Device, capable of accuratelymeasuring temperature in increments of 0.1C or less in arange from 18 to 32C (65 to 100F).54Tape 573
26、99, available from PI Company, Box 397, Lemon Grove, CA 92045,has been found satisfactory for this purpose.5Doric Trendicator 410 with copper constantan thermocouple, available fromDoric Scientific Div., Emerson Electric Co., 3883 Ruffin Rd., San Diego, CA 92123,has been found satisfactory for this
27、purpose.NOTE 1Break sharp edges. All dimensions are inches unless other-wise stated. If conversion of dimension is desired, use standard equiva-lence table.Material: Brass.FIG. 1 Machined Metal Cap for PET Beverage Bottle TestingF 1115 95 (2001)27.2.3 Pressure-Monitoring Device6. 7.2.4 Fillpoint-Lev
28、el Syringe Assembly (see Fig. 2).7.3 Procedure B:6APressure Transducer ModelAB 0 to 100 psi, available from Data Instruments,Inc., 6 Hartwell Pl., Lexington, MA 02173, with support electronics consisting of avoltmeter calibrated for pressure measurement to within 0.1 psi, has been foundsatisfactory
29、for this purpose. A calibrated pressure gage has also been found to besatisfactory, for example, an Ashcraft Model 25-1009A02L.NOTE 1Dimensions are in inches and millimetres. Other styles of suction bulbs may be used, including an in-line bulb for use with flexible tubingattached to the gage. The as
30、sembly must be adjusted for the specified fill point (from the top down) for the specific bottle size and style being evaluated.The gage may be adjusted using a preset syringe adjusting device or other measuring devices such as the vertical height gage (see 7.1.2). The gage shouldbe set 0.050 in. (1
31、.27 mm) less than the specified value to compensate for the extra liquid withdrawn due to the effect of surface tension.FIG. 2 Fillpoint Level Adjustment SyringeF 1115 95 (2001)37.3.1 Pressure- and Temperature-Measuring Device7.8. Reagents and Materials8.1 Water carbonated to a level sufficient to e
32、nsure aminimum carbonation level of 4.5 volumes in the filled bottles.Reagent water conforming to Type IV of Specifications D 1193or better shall be used.8.2 Carbon Dioxide, compressed (CO2).8.3 Leak-Detecting Solution.89. Conditioning9.1 Test bottles must be conditioned for at least 72 h andtested
33、at 23C (73.4F) 6 2C, and 50 6 5 % relativehumidity, unless other conditions are agreed upon by theparties involved.9.2 Bottles may be tested with or without base cup attached.10. Procedure A10.1 Apparatus Preparation:10.1.1 Assemble and calibrate pressure- and temperature-monitoring equipment.10.1.2
34、 Pressure test assembly at 60 psi using leak detectingsolution.10.1.3 Check calibration of monitoring equipment.10.2 Record weight and dimensions of empty and filledbottles (optional).10.2.1 Weigh each empty bottle to at least 0.01 g.10.2.2 Measure the outside diameter of each empty bottleusing a p
35、tape. Measure at the center of the label panel, or otherpreviously agreed upon location(s).10.2.3 Measure the height of each empty bottle to thebottom of the support ring using a vertical height gage orsimilar equipment.10.3 Filling Bottles:10.3.1 Using a carbonating unit or similar equipment, fillc
36、ontainers to the nominal fill level with carbonated watercooled to 5C (41F) or below, preferably 1C (34F). Samplesmust be carbonated to no less than 4.5 volumes CO2. UseTables X1.1-X1.4 or another table agreed upon by the partiesinvolved to determine CO2content by measuring pressure andtemperature w
37、ith the equipment described in Section 7.10.3.2 Using a fillpoint-level syringe, draw liquid leveldown to the specified fillpoint.10.3.3 Immediately after the fillpoint-level adjustment, ap-ply the pressure monitoring apparatus tightly to the bottle. DONOT AGITATE THE BOTTLE. A brass closure fitted
38、with amicropressure transducer or pressure gage (see Fig. 3) and athermocouple capable of reading within increments of 0.1Cand 1.0 psi, respectively, or a roll-on aluminum closure fittedwith a rubber septum have been found satisfactory for thispurpose.10.3.4 Fill a minimum set of five bottles for ea
39、ch sample.10.3.5 If the testing device used does not have a temperaturesensing probe inside the bottle, fill another bottle with coldnoncarbonated water to use as a temperature control for this setof bottles. This bottle should be kept with this set duringstorage, agitation, and testing. Its tempera
40、ture shall be used forthe temperature of each bottle in the set when determiningcarbonation level.10.4 Pressure Adjustment and Equilibration of FilledBottles:10.4.1 Allow filled bottles to come to ambient storagetemperature, and let stand for 24 h in the test environment.10.4.2 After bottles have eq
41、uilibrated for 22 h at ambienttemperature, agitate the bottles for at least one min using handshaking or mechanical agitation to ensure proper equilibrationof headspace and dissolved CO2. Snift pressure or add CO2gasas required to adjust the carbonation level to 4.0 volumes 60.05 volumes according t
42、o a carbonation volumes table. Thestarting CO2level is critical.10.4.3 After a total of 24-h equilibration, again agitate thetest bottles and determine their carbonation level. If any bottlehas a carbonation level of 3.95 volumes or less, discontinuetesting of that bottle.10.5 Measurements:10.5.1 Be
43、fore filling bottles for the carbonation level test,measure wall thickness profile using suitable equipment todetermine the quality of the material distribution (optional).10.5.2 Twenty-four hours after filling, agitate each testbottle to equilibrium pressure for at least 1 min to obtain theinitial
44、values as outlined below:10.5.2.1 Equilibrium pressure of each bottle,10.5.2.2 Temperature of each bottle or the control bottles,10.5.2.3 Carbonation level (from a carbonation volumestable),10.5.2.4 Bottle height to the bottom of the support ring(optional),10.5.2.5 Bottle outside diameter (optional)
45、.10.5.3 Repeat measurements, and agitate bottle for at least 1min prior to measuring pressure and temperature at 3 days, 1week, 3 weeks, 6 weeks, 8 weeks, 12 weeks, and 16 weeks. Ifattached pressure transducers or gages are used, pressure andtemperature may be measured more frequently (for example,w
46、eekly) either to allow early prediction of shelf life or to obtaina more precise measure of the end point.10.5.4 If the attached septum method is used, a set of sixglass control bottles of the same capacity must be tested alongwith the plastic bottles. Average loss of these bottles must besubtracted
47、 from the loss of the plastic bottles to compensate forCO2lost from the septum.11. Procedure B11.1 Apparatus Preparation:11.1.1 Ensure proper calibration of the Terris Unit orZahm-Nagle Apparatus using appropriate manufacturersguidelines.11.1.2 Pressure test assembly to ensure no pressure leakagewil
48、l occur.11.2 Test Initiation:7A Terriss Unit, available from Terriss-Consolidated Industries, Box 110B,Asbury Park, NJ 07712, and a Zahm-Nagel apparatus, available from Zahm andNagel Co., Inc., 74 Hewett Ave., Buffalo, NY 14214, have been found satisfactoryfor this purpose.8Snoop Leak Detector, avai
49、lable from Nupro Company, 15635 Saramac Rd.,Cleveland, OH 44110, has been found satisfactory for this purpose.F 1115 95 (2001)411.2.1 This test method usually involves filled productcontainers selected from a commercial beverage location.Select a random sample of at least 50 bottles.11.2.2 If commercially filled and capped bottles are notavailable, fill the bottles with either carbonated water orproduct and apply aluminum roll-on closures using a capper.11.2.3 Using the Terris Unit, Zahm-Nagle Apparatus, orsimilar device, pierce the closure and measure
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