1、Designation: D 4963 04Standard Test Method forIgnition Loss of Glass Strands and Fabrics1This standard is issued under the fixed designation D 4963; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe
2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers primarily the determination ofignition loss of glass textiles. This method applies to glass fiberstrands, twisted o
3、r untwisted, coated or uncoated; and fabrics,woven, nonwoven, knitted, coated, and uncoated, and choppedstrand. This procedure may be applied to other glass textileswhere the amount of organic content obtained by ignition lossis required.NOTE 1This test method may be used with other glass fiber clas
4、sifi-cations, such as C or D, but a different ignition temperature and exposuretime may be required. In these cases the manufacturer should be consultedfor the appropriate ignition conditions.1.2 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The v
5、alues stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in nonconformancewith the standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with
6、 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 123 Terminology Relating to TextilesD 578 Specification for Glass
7、Fiber StrandsD 7018 Terminology Relating to Glass Fiber and Its Prod-ucts3. Terminology3.1 DefinitionsFor all terminology related to Subcommit-tee D13.18 on Glass Fibers, see Terminology D 7018.3.2 For definitions of other textile terms used in this testmethod, refer to Terminology D 123. For inform
8、ation on thedesignation of construction of glass strands, refer to Specifi-cation D 578.4. Summary of Test Method4.1 The organic content on glass textiles is determined byweighing the specimen before and after ignition. The amountof ignition loss on a sample is reported as a percentage of themass be
9、fore ignition.5. Significance and Use5.1 This test method is considered satisfactory for accep-tance testing of commercial shipments because current esti-mates of between-laboratory precision are acceptable.5.1.1 In cases of a dispute arising from differences inreported test results when using this
10、test method for acceptancetesting of commercial shipments, the purchaser and the sup-plier should conduct comparative tests to determine if there isa statistical bias between their laboratories. Competent statis-tical assistance is recommended for the investigation of bias.As a minimum, the two part
11、ies should take a group of testspecimens which are as homogeneous as possible and whichare from a lot of material of the type in question. The testspecimens should then be randomly assigned in equal numbersto each laboratory for testing. The average results from the twolaboratories should be compare
12、d using Students t-test forunpaired data and an acceptable probability level chosen by thetwo parties before the testing begins. If a bias is found, eitherits cause must be found and corrected or the purchaser and thesupplier must agree to interpret future test results in the view ofthe known bias.5
13、.2 Glass textiles are provided with various sizings orcoatings. These provide a protection for the individual fibers,yarns, or fabric that may compose the glass textile as well ascompatibility with further finishing requirements. The amountof sizing or coating on glass textiles as determined by this
14、procedure is used for process control.6. Apparatus and Materials6.1 ReelA hand- or motor-driven reel having at least a1-m (1-yd) perimeter. The reel shall be fitted with a traversingmechanism that will avoid bunching the successive wraps, and1This test method is under the jurisdiction of ASTM Commit
15、tee D13 on Textilesand is the direct responsibility of Subcommittee D13.18 on Glass Fiber and ItsProducts.Current edition approved Dec. 1, 2004. Published January 2005. Originallyapproved in 1989. Last previous edition approved in 1999 as D 4963 99.2For referenced ASTM standards, visit the ASTM webs
16、ite, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Stat
17、es.with an indicator of the length wound. A warning bell that willring at a specified length is recommended. It is advisable thatone arm will be collapsible to allow for easy removal of skeins.6.2 Muffle Furnace, capable of maintaining 625 6 25C(1157 6 45F).6.3 Air Circulating Drying Oven, capable o
18、f maintaining atemperature of 105 6 2C (220 6 4F).6.4 Thermometer, or thermcouple, for muffle furnace ca-pable of registering 625C with 25C maximum increments(1157F with 45F maximum increments).6.5 Analytical Balance, 200-g capacity, readable to 0.001 g.6.6 Weighing Containers.36.7 Hood, suitable fo
19、r removing combustion products.6.8 Desiccator, of sufficient size to hold the weighingcontainers and an efficient desiccant.6.9 Tongs, long handle, heat-resistant.6.10 Gloves, heat-resistant.7. Safety Hazards7.1 PrecautionsAvoid contact with the hot muffle fur-nace. Use tongs to remove samples. Pres
20、cribed safety glovesshould be worn when performing high-temperature (over 45Cor 100F) testing. Place hazard warning safety signs in aconspicuous place. The muffle furnace must be located under ahood suitable for removing combustion products.8. Sampling and Number of Specimens8.1 Lot SizeA lot is def
21、ined as a single shipment of asingle type of glass textile. A lot may constitute all or part of asingle customer order.8.2 Lot SampleAs a lot sample for acceptance testing,take the number of sampling units of glass textiles directed inan applicable material specification or other agreement be-tween
22、the purchaser and the supplier.8.3 Laboratory SampleConsider strand packages or fabricrolls or chopped strand quantities of at least 50 g to be alaboratory sample unless otherwise agreed upon between thepurchaser and the supplier.8.4 Test SpecimensAs test specimens for acceptance test-ing, proceed a
23、s follows:8.4.1 For strands, take two lengths of strand, each weighingat least 1 g from each package in the laboratory sample.8.4.2 For fabrics, cut two test specimens at least 103 cm2(16 in.2) from the laboratory sample in such a way that nospecimen is closer than one tenth the width of the swatch
24、fromthe selvage with no two specimens cut perpendicular to thewarp containing the same set of warp ends or if cut parallel tothe filling, containing the same set of filling picks, and thespecimens from different swatches are each taken from adifferent part of the width of the swatches, with no speci
25、menbeing taken within1m(1yd)ofthevery outside of the roll.8.4.3 For bulk glass textiles, such as chopped strand, taketwo quantities randomly as test specimens, each weighing atleast 6 g from each laboratory sampling unit.9. Procedure9.1 Precondition each test specimen by drying for1hat1056 2C (220 6
26、 4F), unless otherwise specified. Remove thetest specimens from the drying oven and cool in the desiccatorfor a minimum of 10 min in the standard atmosphere for testingglass textiles.NOTE 2Conditioning is often omitted in current lab practices, butmust be used to resolve finish level conflicts betwe
27、en purchaser andsupplier.9.2 Precondition the weighing containers by placing theempty containers in the muffle furnace at 625 6 25C (1157 645F). After 30 min, remove and cool in the standard atmo-sphere for testing glass textiles for 30 min.9.3 Weigh the empty container to the nearest 0.001 g.Record
28、 this as the tare mass, T.9.4 Identify each container with respect to each test speci-men.NOTE 3When it is known that no ash residue separates from thespecimen during the weighing and igniting process, the specimen isallowed to be weighed separately without the container. When this occurs,T equals z
29、ero.9.5 Place the test specimen in the container and weigh to thenearest 0.001 g. Record this as the initial mass, A.9.6 With the test specimen in the container, place in themuffle furnace. Ignite at 625 6 25C (1157 6 45F) for at least30 min.NOTE 4For fabrics with less than 3 % loss on ignition, som
30、emanufacturers have found that ignition time of 10 min is sufficient. In caseof dispute, the conditions in 9.6 shall be used.9.7 Remove the container with specimen residue from themuffle furnace and cool in the desiccator for at least 30 min inthe standard atmosphere for testing glass textiles.9.8 R
31、emove each container and test specimen separatelyfrom the desiccator, and immediately weigh to the nearest0.001 g. Record this as the ignited mass, B.10. Calculation10.1 Calculate the ignition loss of the glass textile in percentto three significant digits for each specimen using Eq 1:10.2 Calculate
32、 the average ignition loss for each samplingunit and for the lot as directed in an applicable materialspecification or contract order.Ignition loss, % 5 100 3 A 2 B!/A 2 T! (1)where:A = initial mass of container and specimen before ignition,g,B = mass of container and glass residue after ignition, g
33、,andT = mass of container (Note 3).11. Report11.1 Report that the specimens were tested for ignition lossas directed in Test Method D 4963. Include the productdescription.11.2 Report, for each laboratory sampling unit of glasstextile, the average ignition loss.3Porcelain Crucible, Coors No. E-7, or
34、other containers or holders, suitable forexposure to 625 6 25C (1157 6 45F), have been found satisfactory for thispurpose.D496304211.3 Report, for the lot average, the average ignition loss forall laboratory sampling units that were tested.12. Precision and Bias12.1 SummaryIn 95 out of 100 cases whe
35、n comparingtwo averages of two determinations each, the differencesshould not exceed the following amounts when all of thedeterminations are taken by the same well trained operatorusing the same piece of test equipment and specimens ran-domly drawn from the same sample of material but tested atdiffe
36、rent times.Class 1 vinyl-coated glass yarn0.8 % of the averageClass 2 vinyl-coated glass yarn1.5 % of the averageLarger differences are likely to occur under all other condi-tions. This test method has no bias since the true value ofignition loss can only be defined in a specific test method.Paragra
37、phs 12.2-12.4 explain the basis for this summary andfor evaluations made under other conditions.12.1.1 The values in Table 1 are shown in percent of theaverage. It is expected that the values will also apply to otherforms of glass textiles.12.2 Interlaboratory Test Data4An interlaboratory testwas ru
38、n in 1986 in which randomly drawn specimens of aClass 1 vinyl-coated glass yarn and a Class 2 vinyl-coated glassyarn were tested in each of four laboratories. Each laboratoryused two operators, each of whom tested two specimens ofeach material at different times. The components of varianceexpressed
39、as coefficients of variation are listed in Table 1.NOTE 5The square roots of the components of variance are beingreported to express the variability as percent ignition loss rather than as thesquare of that unit of measure.12.3 PrecisionFor the components of variance reported inTable 1, two averages
40、 of observed values should be consideredsignificantly different at the 95 % probability level if thedifference equals or exceeds the critical differences listed inTable 2.NOTE 6Since the interlaboratory test included only four laboratories,estimates of between-laboratory precision should be used wit
41、h specialcaution.NOTE 7The tabulated values of the critical differences should beconsidered to be a general statement particularly with respect to between-laboratory precision. Before a meaningful statement can be made aboutany two specific laboratories, the amount of statistical bias if any, betwee
42、nthem must be established, with each comparison based on recent dataobtained on specimens taken from a lot of material of the type beingevaluated and nearly homogeneous as possible and then randomlyassigned in equal numbers to the two laboratories.12.4 BiasThe procedure in this test method has no bi
43、asbecause the value of ignition loss can be defined only in termsof a test method.13. Keywords13.1 glass fabrics; glass textiles; glass yarns; ignition loss4ASTM Research Report No. D-13-1078. A copy is available from ASTMHeadquarters.TABLE 1 Coefficients of Variation, Vinyl-Coated Glass Yarns,Perce
44、nt of AverageMaterialSingle-OperatorComponentWithin-LaboratoryComponentBetween-LaboratoryComponentClass 1Single-Material 0.41 0.91 0.00Multi-Material 0.41 0.91 0.99Class 2Single-Material 0.77 0.00 0.85Multi-Material 1.23 0.00 0.85TABLE 2 Critical Differences for the Conditions Noted, Vinyl-Coated Gl
45、ass Yarns, 95 % Probability Level, Percent of AverageNumber ofObservations inEach AverageSingle-OperatorPrecisionWithin-LaboratoryPrecisionBetween-LaboratoryPrecisionClass 1Single-Material Comparison1 1.1 2.8 2.82 0.8 2.6 2.65 0.5 2.6 2.610 0.4 2.5 2.5Class 1Multi-Material Comparisons1 1.1 2.8 3.92
46、0.8 2.6 3.85 0.5 2.6 3.810 0.4 2.5 3.7Class 2Single-Material Comparisons1 2.1 2.1 3.22 1.5 1.5 2.85 1.0 1.0 2.510 0.7 0.7 2.5Class 2Multi-Material Comparisons1 2.5 2.5 3.42 2.0 2.0 3.15 1.6 1.6 2.910 1.4 1.4 2.8D4963043ASTM International takes no position respecting the validity of any patent rights
47、 asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any ti
48、me by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will
49、receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone)
