1、Designation: C169 92 (Reapproved 2011)Standard Test Methods forChemical Analysis of Soda-Lime and Borosilicate Glass1This standard is issued under the fixed designation C169; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、 of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods cover the quan
3、titative chemicalanalysis of soda-lime and borosilicate glass compositions forboth referee and routine analysis. This would be for the usualconstituents present in glasses of the following types: (1)soda-lime silicate glass, (2) soda-lime fluoride opal glass, and(3) borosilicate glass. The following
4、 common oxides, whenpresent in concentrations greater than indicated, are known tointerfere with some of the determinations in this method: 2 %barium oxide (BaO), 0.2 % phosphorous pentoxide (P2O5),0.05 % zinc oxide (ZnO), 0.05 % antimony oxide (Sb2O3),0.05 % lead oxide (PbO).1.2 The analytical proc
5、edures, divided into two generalgroups, those for referee analysis, and those for routineanalysis, appear in the following order:SectionsProcedures for Referee Analysis:Silica 10BaO, R2O2(Al2O3+P2O5), CaO, and MgO 11-15Fe2O3,TiO2,ZrO2by Photometry and Al2O3by Complexio-metric Titration16-22Cr2O3by V
6、olumetric and Photometric Methods 23-25MnO by the Periodate Oxidation Method 26-29Na2O by the Zinc Uranyl Acetate Method and K2ObytheTetraphenylborate Method30-33SO3(Total Sulfur) 34 to 35As2O3by Volumetric Method 36-40Procedures for Routine Analysis:Silica by the Single Dehydration Method 42-44Al2O
7、3, CaO, and MgO by Complexiometric Titration, and BaO,Na2O, and K2O by Gravimetric Method45-51BaO, Al2O3, CaO, and MgO by Atomic Absorption; and Na2Oand K2O by Flame Emission Spectroscopy52-59SO3(Total Sulfur) 60B2O361 to 62Fluorine by Pyrohydrolysis Separation and Specific Ion ElectrodeMeasurement6
8、3-66P2O5by the Molybdo-Vanadate Method 67-70Colorimetric Determination of Ferrous Iron Using 1,10Phenan throline71-761.3 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-priat
9、e safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C146 Test Methods for Chemical Analysis of Glass SandC225 Test Methods for Resistance of Glass Containers toChemical AttackD1193 Specification for Reagent
10、WaterE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Spectrophotometry3. Significance and Use3.1 These test methods can be used to ensure that thechemical c
11、omposition of the glass meets the compositionalspecification required for the finished glass product.3.2 These test methods do not preclude the use of othermethods that yield results within permissible variations. In anycase, the analyst should verify the procedure and techniqueemployed by means of
12、a National Institute of Standards andTechnology (NIST) standard reference material having a com-ponent comparable with that of the material under test.Alist ofstandard reference materials is given in the NIST SpecialPublication 260,3current edition.3.3 Typical examples of products manufactured using
13、 soda-lime silicate glass are containers, tableware, and flat glass.3.4 Typical examples of products manufactured using boro-silicate glass are bakeware, labware, and fiberglass.1These test methods are under the jurisdiction of ASTM Committee C14 onGlass and Glass Products and are the direct respons
14、ibility of Subcommittee C14.02on Chemical Properties and Analysis.Current edition approved Oct. 1, 2011. Published October 2011. Originallyapproved in 1941. Last previous edition approved in 2000 as C169 92(2005). DOI:10.1520/C0169-92R11.2For referenced ASTM standards, visit the ASTM website, www.as
15、tm.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.3Available from National Institute of Standards and Technology, Gaithersburg,MD 20899.1Copyright ASTM International, 100 Ba
16、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.5 Typical examples of products manufactured using fluo-ride opal glass are containers, tableware, and decorativeglassware.4. Purity of Reagents4.1 Reagent grade chemicals shall be used throughout.Unless otherwise indicat
17、ed, it is intended that reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.4Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit it
18、s use without lessening the accuracy ofthe determination.4.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water as definedby Type I, II, or III of Specification D1193.5. Concentration of Acids and Ammonium Hydroxide5.1 When acids and ammonium hydro
19、xide are specified byname or chemical formula only, concentrated reagents of thefollowing percent concentrations are intended:%Hydrochloric acid (HCl) 36 to 38Hydrofluoric acid (HF) 48 to 51Nitric acid (HNO3) 69to71Perchloric acid (HClO4) 70to72Sulfuric acid (H2SO4) 95to98Ammonium hydroxide (NH4OH)
20、28 to 305.2 Concentrations of diluted acids and NH4OH exceptwhen standardized are specified as a ratio, stating the numberof volumes of the concentrated reagent to be added to a givennumber of volumes of water, as follows: HCl (1 + 99) means1 volume of concentrated HCl (approximately 37 %) added to9
21、9 volumes of water.5.3 The hygroscopic nature of the ignited precipitates ofsilica, aluminum oxide, and calcium oxide obtained in themethods to be described, requires the use of fresh and highlyactive desiccants. For this purpose, magnesium perchlorate(Mg(ClO4)2) and barium oxide (BaO) are recommend
22、ed.6. Filter Papers6.1 Throughout these test methods, filter papers will bedesignated as “coarse,” “medium,” or “fine,” without namingbrands or manufacturers.All filter papers are of the double acidwashed ashless type. “Coarse” filter paper refers to the porositycommonly used for the filtration of a
23、luminum hydroxide.“Medium” filter paper refers to that used for filtration ofcalcium oxalate, and “fine” filter paper to that used for bariumsulfate.7. Photometers and Photometric Practice7.1 Photometers and photometric practice prescribed inthese methods shall conform to Practice E60.7.2 The consid
24、erations of instrumentation given in TestMethods C146 are equally applicable to these test methods.8. Preparation of Sample8.1 Glass crushed in a steel mortar as described in TestMethods C225, and sieved through a 150-m (No. 100) meshsieve, is generally suitable for analysis, except for the deter-mi
25、nation of iron oxide (Fe2O3). After crushing and sieving,place the powder on a sheet of paper and pass a small magnetthrough it to remove adventitious iron. Then store in a tightlyclosed container and keep in a desiccator.8.2 A sample prepared in an iron mortar is not recom-mended for the determinat
26、ion of Fe2O3. Instead, glass shouldbe ground in an agate mortar after ascertaining it is free ofcontamination.8.3 A sample prepared for the determination of fluorineshould be sieved through a 75-m (No. 200) mesh sieve ratherthan a 150-m (No. 100) sieve.8.4 The practice of drying samples in a drying
27、oven at 105to 110C after preparation is not recommended. Powderedglass can fix CO2and water as readily at this temperature as atroom temperature. A freshly prepared sample, if exposed but ashort time to the atmosphere, will not have acquired an ignitionloss of much analytical significance. If igniti
28、on loss is deter-mined, use the following temperature schedules:Soda-lime glass, 800C for 1 hFluorine opal glass, 500 to 550C for 1 hBorosilicate glass, 800C for 1 hDetermine the ignition loss ona1to3-gsample in aplatinum crucible.9. Precision and Bias9.1 The probable precision of results that can b
29、e expectedby the use of the procedures described in these test methods isshown in the following tabulation. Precision is given asabsolute error, and is dependent on the quantity of constituentpresent as well as the procedure used.Probable Precision of Results, weight %Constituent Referee Analysis Ro
30、utine AnalysisSilica 60.1 60.25BaO 60.02 60.05Al2O3+P2O560.05 60.10 (P2O5)CaO 60.05 60.15MgO 60.05 60.02 to 0.10Fe2O360.003 .TiO260.005 .ZrO260.001 to 0.005 .Cr2O3(volumetric) 60.005 .Cr2O3(photometric) 60.0001 to 0.001 .MnO 60.001 to 0.005 .Na2O 60.05 60.25 (flame emission)K2O 60.02 to 0.05 60.02 t
31、o 0.10(flame emission)SO360.02 60.05As2O360.005 .P2O5. 60.005 to 0.02B2O3. 60.05 to 0.15Fluorine . 60.01 to 0.20(0.1 to 6.0 %)9.2 It is recommended that reported results be rounded asfollows:4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For s
32、uggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.C169 92 (2011)2PercentNumb
33、er of Significant FiguresRetained After Rounding1to100 30.1to0.99 20.01 to 0.09 1 or 20.01 1 or 29.3 Recorded results should be carried to one more signifi-cant figure than required in 9.2.PROCEDURES FOR REFEREE ANALYSISSILICA10. Procedure10.1 Weigh 1.000 g of powdered sample and 1.5 g ofanhydrous s
34、odium carbonate (Na2CO3) for soda-lime glass, or2.0gofNa2CO3for borosilicate glass, into a clean 75-mLplatinum dish (see 10.1.1); mix well with a platinum orNichrome5wire. Tap the charge so it lies evenly in the bottomof the dish. Cover with platinum lid and heat first at a dull redheat over a clean
35、 oxidizing flame; gradually raise the tempera-ture until a clear melt is obtained. Properly carried out, little orno spattering should occur and the fusion can be performed in3 to 4 min. When melted, rotate the melt to spread it evenlyover the bottom and lower sides of the dish, graduallywithdrawing
36、 from the flame. Cover and cool to room tempera-ture. During fusion, the dish should be handled at all times withplatinum-tipped tongs and the fusion performed with a plati-num (preferably 90 % platinum and 10 % rhodium alloy) orsilica triangle.10.1.1 To obtain accurate repeat weighings, platinum wa
37、reshall be kept scrupulously clean on the outside of the vessel aswell as on the inside. It should be polished brightly with fine,round grain sand and protected from dirty surfaces. It isrecommended that porcelain plates be used for cooling fusions,and that platinum be set on paper towels or other c
38、lean materialduring filtration.10.2 Add 20 to 25 mL of HCl (1 + 1) (Note 1) under theplatinum cover and digest on a steam bath or hot plate until themelt has completely disintegrated; it is also possible to digestthe melt in the cold overnight. Police and rinse the lid with afine jet of water; rinse
39、 down the sides of the dish and evaporateto dryness on a steam bath or under an infrared lamp. Keep thedish covered with a raised cover glass during evaporation.When evaporation is complete (Note 2) (absence of HCl), cool,drench the residue with 5 mL of HCl, and then add 20 mL ofhot water. Digest fo
40、r 5 min and filter through a 9-cm mediumfilter paper. Catch the filtrate in a 250-mL platinum dish.Transfer the precipitated silica to the filter with the aid of apoliceman and a bit of paper pulp, and wash the precipitate andpaper twelve times with hot 2 % HCl. Transfer the paper andprecipitate to
41、the dish used for fusion and dehydration andreserve for subsequent ignition. Wipe the stirring rod and theperiphery of the funnel with a piece of damp filter paper andadd to the dish containing the precipitate for ignition.NOTE 1Glasses containing fluorine in small amounts (less than0.25 %) will not
42、 cause significant error. Glasses containing larger amountsof fluorine (for example, fluoride opals) are analyzed as above with thisexception: after the fusion has been made and before addition of the acid(see 10.2), add 10 mL of aluminum chloride (AlCl3) solution (10mL = 200 mg of Al) to complex fl
43、uorine. If evaporation is made on asteam bath, it is difficult to dry the residue. It is suggested that final drying,before filtration, be made in a drying oven for 30 to 45 min at 105C.Results for SiO2when analyzing fluorine opals may tend to be low by0.2 to 0.3 %. For an alternative, but more leng
44、thy procedure, consultApplied Inorganic Analysis.6NOTE 2Boron in amounts less than 5 % B2O3does not interfere.However, if boron is greater than 5 %, proceed to the point of completingthe first dehydration (see 10.2), then add 20 mL of anhydrous methanolsaturated with dry HCl (gas), and evaporate to
45、dryness on an air bath orunder an infrared lamp. Repeat once more before proceeding.10.3 Evaporate the filtrate to dryness on the steam bath orunder an infrared lamp. When dry, cool, drench with 10 mL ofHCl (1 + 1) and again evaporate just to dryness; then bake in adrying oven at 105C for 30 min. Co
46、ol, drench with 5 mL ofHCl, and add 20 mL of hot water and a small bit of filter pulp.Digest hot for 5 min and filter through a 7-cm fine paper. Policethe dish with the aid of a bit of paper pulp and wash precipitateand paper eight times with hot 2 % HCl. Transfer the paper andprecipitate to the dis
47、h containing the initial precipitation. Wipethe stirring rod and the periphery of the funnel with a piece ofdamp filter paper and add to the dish containing the precipitatefor ignition.10.4 Partially cover the dish with its platinum lid but leaveenough space so air can circulate during ignition. Pla
48、ce the dishin a cold muffle furnace and bring the temperature to 1200Cfor 30 min. Carefully and completely cover the dish beforeremoving it from the furnace and transfer to a desiccator. Coolto room temperature and weigh the covered dish (W1). Moistenthe silica with 1 to 2 mL of water and add 4 to 5
49、 mL of HF and0.5 g of oxalic acid crystals. Evaporate to dryness on a sandbath or under an infrared lamp. Carefully sublime any remain-ing oxalic acid, cover the dish with its platinum cover, heat to1000C for 2 min, cool, and weigh (W2) as before.10.5 CalculationCalculate the percent of SiO2as follows:SiO2,%5 W12 W2! 3 100 (1)BaO, R2O3(Al2O3+P2O5), CaO, AND MgO11. General Considerations11.1 The detailed analysis described below may be desirableonly infrequently. Several steps may be omitted without undueloss of accuracy, for example, the hydrogen sulfide (H2S) andth
