Chemical Analysis of Soda-Lime and Borosilicate Glass: Standard Test Methods For

 

 

Designation: C169 − 92 (Reapproved 2011)

Standard Test Methods for

Chemical Analysis of Soda-Lime and Borosilicate Glass 1 This standard is issued under the fixed designation C169; the number immediately following the designation indicates the year of  original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript 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. Sco Scope pe

1.1 These These tes testt met method hodss cov cover er the qua quanti ntitat tative ive che chemic mical al analysis of soda-lime and borosilicate glass compositions for both referee and routine analysis. This would be for the usual consti con stitue tuents nts pre presen sentt in gla glasse ssess of the fol follow lowing ing typ types: es: (1) soda-lime silicate glass, (2) soda-lime fluoride opal glass, and (3) boros borosilic ilicate ate glass glass.. The foll followin owing g common oxides, oxides, when present in concentrations greater than indicated, are known to interfere with some of the determinations in this method: 2 % barium bar ium oxi oxide de (Ba (BaO), O), 0.2 % pho phosph sphoro orous us pen pentox toxide ide (P2O5), 0.05 0.0 5 % zin zincc oxi oxide de (Zn (ZnO), O), 0.0 0.05 5 % ant antimo imony ny oxi oxide de (Sb2O3), 0.05 % lead oxide (PbO). 1.2 The ana analyt lytica icall pro proced cedure ures, s, div divide ided d into into two genera generall grou gr oups ps,, th thos osee fo forr re refe fere reee an anal alys ysis is,, an and d th thos osee fo forr ro rout utin inee analysis, appear in the following order: Sections Procedures for Referee Analysis: Silica   BaO, R2O2  (Al 2O3 + P2O5), CaO, and MgO   Fe2O3, TiO2, ZrO2  by Photometry and Al2O3   by Complexiometric Titration Cr2O3   by Volumetric and Photometric Methods   MnO by the Periodate Oxidation Method   Na2O by the Zinc Uranyl Acetate Method and K 2O by the Tetraphenylborate Method SO3  (Total Sulfur)   As2O3  by Volumetric Method   Procedures for Routine Analysis: Silica by the Single Dehydration Method   Al2O3, CaO, and MgO by Complexiometric Titration, and BaO, Na2O, and K2O by Gravimetric Method BaO, Al2O3, CaO, and MgO by Atomic Absorption; and Na 2O and K2O by Flame Emissi Emission on Spectroscopy Spectroscopy SO3  (Total Sulfur)   B2O3   Fluorine Fluori ne by Pyrohy Pyrohydrolys drolysis is Separa Separation tion and Specifi Specific c Ion Electrode Measurement P2O5   by the Molybdo-Vanadate Method   Colorimetric Colori metric Determination Determination of Ferrou Ferrous s Iron Using 1,10 Phen Ph enan an thro th roli line ne

10 11-15 16-22 23-25 26-29 30-33 34  to  35 34 to 36-40 42-44 45-51 52-59 60 61 to 61  to  62 63-66 67-70 71-76

1.3   This standar standard d doe doess not purport purport to addre address ss all of the safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciate ted d wit with h its use. use. It is the the 1

responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use.

2. Referenc Referenced ed Documents

2.1   ASTM Standards:2 C146 Test C146  Test Methods for Chemical Analysis of Glass Sand C225   Test Metho C225 Methods ds for Resis Resistance tance of Glass Containers Containers to Chemical Attack  D1193 Specification D1193  Specification for Reagent Water E50 Practices E50  Practices for Apparatus, Reagents, and Safety Consideration erat ionss for Che Chemic mical al Ana Analys lysis is of Met Metals als,, Ore Ores, s, and Related Materials E60   Pra E60 Practi ctice ce for Analysis Analysis of Met Metals als,, Ore Ores, s, and Rel Relate ated d Materials by Spectrophotometry 3. Signi Significanc ficancee and Use

3.1 Th 3.1 Thes esee te test st me meth thod odss ca can n be us used ed to en ensu sure re th that at th thee chemical chemi cal compo compositio sition n of the glass meets the compo compositi sitional onal specification required for the finished glass product. 3.2 The These se tes testt met method hodss do not pre preclu clude de the use of other methods that yield results within permissible variations. In any case, the analy analyst st shou should ld verif verify y the procedure and techn technique ique employed by means of a National Institute of Standards and Technology (NIST) standard reference material having a componentt comparable ponen comparable with that of the material material under test. A list of  sta standa ndard rd ref refere erence nce materi mat erials als is giv given en in the NIS NIST T   Special Publication 260 ,3 current edition. 3.3 Ty Typical pical examples of products manufactured manufactured using sodalime silicate glass are containers, tableware, and flat glass. 3.4 Ty Typical pical examples of products manufactured manufactured using borosilicate glass are bakeware, labware, and fiberglass. 3.5 Typica ypicall examp examples les of produ products cts manufactured manufactured using fluoridee opa rid opall gla glass ss are con contai tainer ners, s, tab tablew leware are,, and dec decora orativ tivee glassware. 2

These test methods are under the jurisdiction of ASTM Committee   C14   on Glass and Glass Products and are the direct responsibility of Subcommittee  C14.02 on Chemical Properties and Analysis. Current Curre nt editio edition n approv approved ed Oct. 1, 2011 2011.. Publis Published hed October 201 2011. 1. Origin Originally ally approved in 1941. Last previous edition approved in 2005 as C169 – 92(2005). DOI:

For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For  Annual Book of ASTM  Standards volume information, refer to the standard’s Document Summary page on the ASTM website. 3 Available from National Institute of Standards and Technology, Gaithersburg,

10.1520/C0169-92R11.

MD 20899.

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C169 − 92 (2011)

4. Puri Purity ty of Reagents Reagents

4.1 Reagen Reagentt gra grade de che chemic micals als sha shall ll be use used d thr throug oughou hout. t. Unless otherwise indicated, it is intended that reagents shall conform to the specifications of the Committee on Analytical Reagen Rea gents ts of the American American Che Chemic mical al Soc Societ iety y, whe where re suc such h 4 specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of  the determination. 4.2  Purity of Water— Unless Unless otherwise indicated, reference to water shall be understood to mean reagent water as defined by Type I, II, or III of Specification  D1193  D1193.. 5. Conc Concentr entratio ation n of Acids and Ammo Ammonium nium Hydroxide Hydroxide

5.1 When acids and ammonium ammonium hydroxide hydroxide are speci specified fied by name or chemical formula only, concentrated reagents of the following percent concentrations are intended: Hydrochloric acid (HCl) Hydrofluoric acid (HF) Nitric acid (HNO3) Perchloric acid (HClO4) Sulfuric acid (H2SO4) Ammonium hydroxide (NH4OH)

36 48 69 70 95 28

% to to to to to to

38 51 71 72 98 30

5.2 Concen Concentra tratio tions ns of dil dilute uted d aci acids ds and NH4OH exc except ept when standardized are specified as a ratio, stating the number of volumes of the concentrated reagent to be added to a given numberr of volumes of water, numbe water, as follows: follows: HCl HCl (1 + 99) means 1 volume of concentrated HCl (approximately 37 %) added to 99 volumes of water. 5.3 The hyg hygros roscop copic ic nat nature ure of the ign ignite ited d pre precip cipita itates tes of  silica sil ica,, alu alumin minum um oxi oxide, de, and cal calciu cium m oxi oxide de obt obtain ained ed in the methods to be described, requires the use of fresh and highly activee desicc activ desiccants. ants. For this purpose, magnes magnesium ium perch perchlorat loratee (Mg(ClO4)2) and barium oxide (BaO) are recommended. 6. Filt Filter er Papers Papers

6.1 Througho Throughout ut the these se tes testt met method hods, s, filt filter er pap papers ers wil willl be designated as “coarse,” “medium,” or “fine,” without naming brands manufacturers. All filter of the doub double le acid washedor ashless type. “Coarse” filterpapers paperare refers to the porosity common com monly ly use used d for the filt filtrat ration ion of alu alumin minum um hyd hydrox roxide ide.. “Med “M ediu ium” m” fil filte terr pa pape perr re refe fers rs to th that at us used ed fo forr fil filtr trat atio ion n of  calcium calciu m oxalate, and “fine” filter paper to that used for bariu barium m sulfate. 7. Photometer Photometerss and Photometric Practice Practice

7.1 Photome Photometer terss and pho photom tometr etric ic pra practi ctice ce pre prescr scribe ibed d in these methods shall conform to Practice   E60 E60..

4  Reagent Chemicals, American Chemical Society Specifications, Americ American an Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American American Chemic Chemical al Societ Society, y, see  Analar Standa Standards rds for Labor Laboratory atory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the   United States Pharmacopeia

and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.

7.2 The con consid sidera eratio tions ns of ins instru trumen mentat tation ion giv given en in Test Methods C146 Methods  C146 are  are equally applicable to these test methods. 8. Pre Prepara paration tion of Sample

8.1 Glass crushed crushed in a ste steel el mor mortar tar as des descri cribed bed in Test Methods C225 Methods  C225,,  and sieved through a 150-µm (No. 100) mesh sieve, is generally suitable for analysis, except for the determination of iron oxide (Fe2O3). After crushing and sieving, place the powder on a sheet of paper and pass a small magnet through it to remove adventitious iron. Then store in a tightly closed container and keep in a desiccator. 8.2 A sa 8.2 samp mple le pr prep epar ared ed in an ir iron on mo mort rtar ar is no nott re reco commmended for the determination of Fe2O3. Instead, glass should be ground in an agate mortar after ascertaining it is free of  contamination. 8.3 A samp sample le pre prepar pared ed for the det determ ermina inatio tion n of fluo fluorin rinee should be sieved through a 75-µm (No. 200) mesh sieve rather than a 150-µm (No. 100) sieve. 8.4 The practice practice of drying samples samples in a drying oven at 105 to 11 110°C 0°C aft after er pre prepar parati ation on is not reco recomme mmende nded. d. Pow Powder dered ed glass can fix CO2  and water as readily at this temperature as at room temperature. A freshly prepared sample, if exposed but a short time to the atmosphere, will not have acquired an ignition loss of much analytical significance. If ignition loss is determined, use the following temperature schedules: Soda-lime glass, 800°C for 1 h Fluorine opal glass, 500 to 550°C for 1 h Borosilicate glass, 800°C for 1 h

Determ Dete rmin inee th thee ig igni niti tion on lo loss ss on a 1 to 33-g g sa samp mple le in a platinum crucible. 9. Pre Precisi cision on and Bias

9.1 The probable probable precision of results results that can be expected by the use of the procedures described in these test methods is show sh own n in th thee fo foll llow owin ing g ta tabu bula lati tion on.. Pr Prec ecis isio ion n is gi give ven n as absolute error, and is dependent on the quantity of constituent present as well as the procedure used. Probable Probab le Precision Precision of Result Results, s, weight % Cons Co nsti titu tuen entt Refe Re fere ree e An Anal alys ysis is Rout Ro utin ine e An Anal alys ysis is Silica ±0.1 ±0.25 BaO ±0.02 ±0.05 Al2O3 + P2O5   ±0.05 ±0.10 (−P2O5) CaO ±0.05 ±0.15 MgO ±0.05 ±0.02 to 0.10 Fe2O3   ±0.003 ... TiO2   ±0.005 ... ZrO2   ±0.001 to 0.005 ... Cr2O3   (volumetric) ±0.005 ... Cr2O3   (photometric) ±0.0001 to 0.001 ... MnO ±0.001 to 0.005 ... Na2O ±0.05 ±0.25 (flame emission) K2O ±0.02 to 0.05 ±0.02 to 0.10 (flame emission) SO3   ±0.02 ±0.05 As2O3   ±0.005 ... P2O5   ... ±0.005 to 0.02 B2O3   ... ±0.05 to 0.15 Fluorine ... ±0.01 to 0.20 (0.1 to 6.0 %)

9.2 It is recommended recommended that  reported  results be rounded as follows:

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C169 − 92 (2011) Percent

 

1 to 100 0.1 to 0.99 0.01 to 0.09