1、Designation: F 1115 95 (Reapproved 2008)e1Standard 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,
2、 the 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.e1NOTEEditorial corrections were made throughout in March 2008.1. Scope1.1 The objective of this test method is to d
3、etermine thecarbon dioxide (CO2) loss from plastic beverage containersafter 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
4、 address all of thesafety concerns, if any, associated with its use. 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 Te
5、rminology Relating to WaterD 1193 Specification for Reagent WaterE 380 Practice for the Use of International System of Units(SI) (the Modernized Metric System)33. Terminology3.1 Units, symbols, and abbreviations used in this testmethod are those recommended by Practice E 380.3.2 Definitions of Terms
6、 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 3.98Cequals 1.000 g/cm3). The conversion of pressure to carbonationvolumes should be made using a carbona
7、tion volumes table. Atable for carbonated water would not necessarily apply toliquids containing additional substances, such as carbonatedbeverages containing sugar.3.2.2 initial pressurethe equilibrium pressure in the testbottles as measured at 24 h after filling with carbonated water.(The filled b
8、ottles 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.)3.2.3 samplea set of bottles produced on the same equip-ment in a single run and using the same material an
9、d 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 initiallevel.3.2.5 pressure monitoring devicea pressure gage or trans-ducer assembly with support electron
10、ics 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 electronics (same equipment as described in7.2.2). A precision glass thermometer may be used provided abottle filled
11、 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 andtemperature and calculate volume of gas (Procedure B).3.2.7 Zahm-Nagle Pressure Testera unit that manually
12、pierces the closure and measures container pressure; an at-tached thermometer is then used to measure temperature(Procedure B).3.2.8 support ringa protrusion below the bottle finishwhich is used to support or stabilize the bottle during fillingand capping.3.2.9 finishthe threaded part of the bottle
13、which receivesthe cap.3.3 For other terms used in this test method, refer toTerminology D 1129.1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02.10 onPermeation.Current edition approved Feb. 1, 2008. Pu
14、blished March 2008. Originallyapproved in 1987. Last previous edition approved in 2001 as F 1115 95 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the stand
15、ards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Test Method4.1 Test bottles are filled with carbonated water or beverageand, after closure application, are expose
16、d to test environmentsfor specified time periods. By periodically measuring the initialand final carbonation levels in the container, the carbonationloss and carbonation transfer rate can be calculated.5. Significance and Use5.1 Two procedures, A and B, are outlined in this testmethod. Procedure A i
17、s 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 the desired CO2fill pres-sure. A loss of
18、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 temperature ofthe package in a closed system. Alt
19、ernatively, 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 tolaboratories that are practiced in this type of a
20、nalytical 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 conditions can interfere with the testresults:6.1
21、.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 Measurement of pressure before the bottle and
22、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 humidity in the test area,6.1.9 Age of bottl
23、es, 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 Device, capable of measuring towithin 0.001 in
24、. (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).7.1.5 Carbonated Water or Beverage Dispensing Equip-ment.7.1.6 Micrometer or Ultrasonic Thickness Gage, capable ofme
25、asuring 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).7.2.3 Pressure-Monitoring Device.7.2.4 Fillpoint-Lev
26、el Syringe Assembly (see Fig. 2).7.3 Procedure B:7.3.1 Pressure- and Temperature-Measuring Device.48. Reagents and Materials8.1 Water carbonated to a level sufficient to ensure aminimum carbonation level of 4.5 volumes in the filled bottles.Reagent water conforming to Type IV of Specification D 1193
27、or better shall be used.4The sole sources of supply of the apparatus (Terriss Unit or Zahm-Nagelapparatus) known to the committee at this time is Terriss-Consolidated Industries,Box 110B, Asbury Park, NJ 07712, and Zahm and Nagel Co., Inc., 74 Hewett Ave.,Buffalo, NY 14214. If you are aware of alter
28、native suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.NOTE 1Break sharp edges. All dimensions are inches unless other-wise stated. If conversion of
29、dimension is desired, use standard equiva-lence table.Material: Brass.FIG. 1 Machined Metal Cap for PET Beverage Bottle TestingF 1115 95 (2008)e128.2 Carbon Dioxide, compressed (CO2).8.3 Leak-Detecting Solution.9. Conditioning9.1 Test bottles must be conditioned at 23C (73.4F) 6 2Cand 50 6 5 % relat
30、ive humidity for at least 72 h and tested atthe same conditions unless other conditions are agreed upon bythe parties 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 equi
31、pment.10.1.2 Pressure test assembly at 60 psi using leak detectingsolution.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 assembly must be adjusted for the specified fill point
32、 (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. (1.27 mm) less than the specified value to compensate
33、for the extra liquid withdrawn due to the effect of surface tension.FIG. 2 Fillpoint Level Adjustment SyringeF 1115 95 (2008)e1310.1.3 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.1
34、0.2.2 Measure the outside diameter of each empty bottleusing a p 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 Bo
35、ttles:10.3.1 Using a carbonating unit or similar equipment, fillcontainers 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. Use TableX1.1 or another table agreed upon by the parties involved to
36、determine CO2content by measuring pressure and temperaturewith 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 th
37、e bottle. DONOT AGITATE THE BOTTLE. A brass closure fitted 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 t
38、hispurpose.10.3.4 Fill a minimum set of five bottles for each 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
39、this set duringstorage, agitation, and testing. Its temperature 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 fo
40、r 24 h in the test environment.10.4.2 After bottles have equilibrated 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. Shift pressure or add CO2gasas required to adjust the
41、 carbonation level to 4.0 volumes60.05 volumes according to 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, dis
42、continuetesting of that bottle.10.5 Measurements:10.5.1 Before 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 equ
43、ilibrium pressure for at least 1 min to obtain theinitial 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
44、ring(optional), and10.5.2.5 Bottle outside diameter (optional).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
45、 andtemperature may be measured more frequently (for example,weekly) 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 pl
46、astic bottles. Average loss of these bottles must besubtracted 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 Terriss Unit orZahm-Nagle Apparatus using appropriate manufacturersguidelines
47、.11.1.2 Pressure test assembly to ensure no pressure leakagewill occur.11.2 Test Initiation:11.2.1 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 ar
48、e notavailable, fill the bottles with either carbonated water orproduct and apply aluminum roll-on closures using a capper.11.2.3 Using the Terriss Unit, Zahm-Nagle Apparatus, orsimilar device, pierce the closure and measure the pressure andtemperature of at least six bottles.11.2.4 Agitate each bot
49、tle for at least 1 min until theequilibrated pressure and temperature is achieved. This isindicated when the maximum pressure is reached.11.3 Measurements:11.3.1 Follow the procedure given in 10.5.2 and 10.5.3.11.3.2 A sample size of at least 50 bottles is needed for along-term test. Since each bottle is destroyed at each testinterval, a minimum of five bottles are needed at each intervaloutlined in 10.5.3.12. Calculation12.1 Calculate the percent of CO2retention for each bottleafter each measurement (based on an initial carbonation levelof 100 %). Calcul
