1、Designation: F1115 16Standard Test Method forDetermining the Carbon Dioxide Loss of BeverageContainers1This standard is issued under the fixed designation F1115; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 containersafter a specifie
3、d period of storage time.1.2 Factors contributing to this pressure loss are volumeexpansion and the gas transport characteristics of the package,including permeation and leakage.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandar
4、d.1.4 This standard does not purport to 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
5、 Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent Water3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 automated CO2analyzeran electronic unit that willpierce the roll-on closure and automatically read pressure andtemperature and
6、calculate volume of gas (Procedure B). Thereare multiple manufacturers of these instruments.3.1.2 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
7、 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.3.1.3 finishthe threaded part of the bottle which receivesthe cap.3.1.
8、4 initial pressurethe equilibrium 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 CO2inth
9、e headspace and liquid).3.1.5 manual pressure testera unit that manually piercesthe closure and measures container pressure; an attachedthermometer is then used to measure temperature (ProcedureB).3.1.6 pressure monitoring devicea pressure gage or trans-ducer assembly with support electronics for in
10、dicating internalpressure level of the bottle. This device is used with brassclosure fitting-equipped bottles.3.1.7 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.3.1.8
11、shelf lifethe number of weeks a sample set of bottlesretain a specified carbonation level, or a percent of the initiallevel.3.1.9 support ringa protrusion below the bottle finishwhich is used to support or stabilize the bottle during fillingand capping.3.1.10 temperature monitoring devicea thermocou
12、plewith support electronics (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 For other terms used in this test method, refer toTerminology D1129.4. Summary of Te
13、st Method4.1 Test bottles are filled with carbonated water or beverageand, after closure application, are exposed to test environments1This test method is under the jurisdiction of ASTM Committee F02 on PrimaryBarrier Packaging and is the direct responsibility of Subcommittee F02.10 onPermeation.Cur
14、rent edition approved Oct. 1, 2016. Published XXXX 2016. Originallyapproved in 1987. Last previous edition approved in 2008 as F1115 95 (2008)1.DOI: 10.1520/F1115-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1for specified time periods. By periodically measuring the initialand final carbon
16、ation 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 is used most often for development ofvarious beverage container designs to determine the functionalchara
17、cteristics 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 CO2will affect product taste.5.1.1 Procedure A involves the use of sensitive pressure andtemperature mo
18、nitoring 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. Alternatively, this proceduremay also use bottles closed with roll-on aluminum capscontaining rubber septu
19、ms. 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 analytical testing.5.1.2 Procedure B is more widely used when measuring thecarbonation level of the pack
20、age due to the simplicity of thetechnique. A simple Manual pressure assembly or an Auto-mated CO2Analyzer is utilized.6. Interferences6.1 The following conditions can interfere with the testresults:6.1.1 CO2leakage at closure due to defective bottle finish orimproper sealing of closure apparatus,6.1
21、.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 liquidhave reached ambient temperature,6.1.5 Inaccurate thermocouple device used for measuringthe l
22、iquid 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 bottles, and6.1.10 Excessive bottle-to-bottle variation in the materialdistribution, which may result in
23、 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. (optional).7.1.3 Top Loading Balance, capable of weighing to 2500 gwith an accuracy of 60.01 g (o
24、ptional).7.1.4 Outside Diameter Measuring Device, tape or similardevice (optional).7.1.5 Carbonated Water or Beverage Dispensing Equip-ment.7.1.6 Micrometer 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).
25、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-Level Syringe Assembly (see Fig. 2).7.3 Procedure B:7.3.1 Pressure- and Temperature-Measuring Device.8.
26、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 D1193or better shall be used.8.2 Carbon Dioxide, compressed (CO2).8.3 Leak-Detecting Solution.9. Conditionin
27、g9.1 Test bottles must be conditioned at 23C (73.4F) 6 2Cand 50 6 5 % relative 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.NOTE 1Break sharp edges. All dimension
28、s 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 TestingF1115 16210. Procedure A10.1 Apparatus Preparation:10.1.1 Assemble and calibrate pressure- and temperature-monitoring
29、 equipment.10.1.2 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.NOTE 1Dimensions are in inches and millimetres. O
30、ther 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 (from the top down) for the specific bottle size and style being evaluated.The gage may be adjusted using a preset syringe
31、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 for the extra liquid withdrawn due to the effect of surface tension.FIG. 2 Fillpoint Level Adjustment SyringeF1115 16310.2.2
32、 Measure the outside diameter of each empty bottleusing a 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:1
33、0.3.1 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 todetermi
34、ne 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 the bottl
35、e. 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 thispurp
36、ose.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 this se
37、t 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 for 24 h
38、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 carbon
39、ation 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, discontinu
40、etesting 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 equilibriu
41、m 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 ring(op
42、tional), 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 andtem
43、perature 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 plastic b
44、ottles. 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 automated CO2analyzer or manual apparatus using appropriate manufacturersguidelines.
45、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 are
46、 notavailable, fill the bottles with either carbonated water orproduct and apply aluminum roll-on closures using a capper.11.2.3 Using the automated CO2analyzer, manualapparatus, or similar device, pierce the closure and measure thepressure and temperature of at least six bottles.11.2.4 Agitate each
47、 bottle 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
48、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 %). Calculate the mean average of the CO2volu
49、mes todetermine the percent CO2retention of that sample.12.2 Plot this data as volumes of CO2or percent carbon-ation retention versus time from the initial reading on rectan-gular coordinate graph paper and draw a smooth curve throughthe data points.12.3 Obtain shelf-life time from the graph by noting thetime (in weeks) at which the carbonation level drops below thespecified minimum carbonation level.F1115 16412.3.1 As a guideline, tests on 2-L bottles should becontinued for at least 16 weeks; a 15 % carbonation loss can beused as a guideline to de
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