1、Designation: C471M 14Standard Test Methods forChemical Analysis of Gypsum and Gypsum Products(Metric)1This standard is issued under the fixed designation C471M; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods cover the chemical analysis ofgypsum and gypsum panel products, including gypsum ready-mixed plaster, gypsum
3、 wood-fibered plaster, and gypsumconcrete.1.2 The test methods appear in the following order:SectionsPreparation of Sample 4Complete Procedure 516Alternative Procedure for Analysis forCalcium Sulfate by Ammonium AcetateMethod1722Alternative Procedure for Analysis forSodium Chloride by the Coulometri
4、cMethod2329Determination of Sand in Set Plaster 3036Wood-Fiber Content in Wood-Fiber Gyp-sum Plaster3739Optional Procedure for Analysis for So-dium by the Atomic Absorption Method 4046Optional Procedure for Analysis for So-dium by Flame Photometry4754Determination of Orthorhombic Cyclooc-tasulfur (S
5、8) in Ggypsum PanelProductsGeneral Provisions55Determination of Orthorhombic Cyclooc-tasulfur (S8) in Gypsum Panel Prod-ucts by Gas Chromatograph Equippedwith a Mass Spectrometer (GS/MS)56Determination of Orthorhombic Cyclooc-tasulfur (S8) in Gypsum Panel Prod-ucts by Gas Chromatograph Equippedwith
6、an Electron Capture Detector(GC/ECD)57Determination of Orthorhombic Cyclooc-tasulfur (S8) in Gypsum Panel Prod-ucts by High-performance Liquid Chro-matograph Equipped with andUltraviolet Detector (HPLC/UV)581.3 The text of this standard references notes and footnotesthat provide explanatory material
7、. These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
8、s 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:2C11 Terminology Relating to Gypsum and Related BuildingMaterials and SystemsC22/C2
9、2M Specification for GypsumC28/C28M Specification for Gypsum PlastersC59 Specification for Gypsum Casting Plaster and GypsumMolding PlasterC61 Specification for Gypsum Keenes CementC317/C317M Specification for Gypsum ConcreteC778 Specification for SandC842 Specification for Application of Interior G
10、ypsum Plas-terD1193 Specification for Reagent WaterD1428 Test Method for Test for Sodium and Potassium InWater and Water-Formed Deposits by Flame Photometry(Withdrawn 1989)3D2013 Practice for Preparing Coal Samples for AnalysisE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Termin
11、ology3.1 DefinitionsDefinitions shall be in accordance withTerminology C11.3.2 Definitions of Terms Specific to This Standard:3.2.1 calibration standard, na chemical mixture contain-ing a known quantity of the analyte used to relate the measuredanalytical signal to the concentration of the analyte.1
12、These test methods are under the jurisdiction of ASTM Committee C11 onGypsum and Related Building Materials and Systems and are the direct responsi-bility of Subcommittee C11.01 on Specifications and Test Methods for GypsumProducts.Current edition approved Nov. 1, 2014. Published November 2014. Orig
13、inallyapproved in 1961. Last previous edition approved in 2013 as C471 13. DOI:10.1520/C0471M-14.2For 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 standards Docum
14、ent Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13
15、.2.2 dried sample, na sample devoid of free water.3.2.3 internal standard, na chemical used in the quantifi-cation of S8by monitoring and adjusting for minor variances ininstrument performance.3.2.4 riffle, na hand feed sample divider device thatdivides the sample into parts of approximately the sam
16、eweight. (D2013)3.2.5 sample as received, na representative portion of rawgypsum or gypsum product in the state received by the testinglaboratory, including aggregates, impurities and water content.3.2.6 surrogate standard, na chemical used to account forextraction efficiency of S8.4. Preparation of
17、 Sample4.1 General ProceduresDetails of sample preparation willvary according to the type of material being tested.4.1.1 Sample As ReceivedUse a sufficient amount ofsample such that, after sieving, not less than 50 g of samplewill remain for testing. Weigh the entire sample immediatelyafter opening
18、the container in which the material was received.This will become the weight of the sample as received.4.1.2 DryingDry the sample in accordance with Section 7.This will be the weight of the dried sample.4.1.3 Crushing and GrindingCrush and grind the sampleby hand with a mortar and pestle or by mecha
19、nical crushingand grinding equipment to pass a 250-m (No. 60) sieve. Takecare, particularly with mechanical equipment, not to expose thesample to temperatures of more than 52C. Clean the equip-ment thoroughly between samples. Thoroughly remix theground sample and store it in an airtight container to
20、 avoidcontamination.4.1.4 RehydratingThoroughly blend and rehydratesamples which contain calcium sulfate in forms other thanCaSO42H2O and natural anhydrite. Place the sample indistilled water and keep it wet for not less than 48 h. Dry thehydrated sample in an oven at 45 6 3C to constant weight andr
21、ecrush or grind it in accordance with 4.1.3.4.1.5 Sample ReductionThoroughly mix and reduce largesamples as required by quartering or by the use of a riffle toobtain a specimen of approximately 50 g.4.2 Gypsum (C22/C22M)Gypsum samples will be re-ceived in the form of rocks or powder, or both. If nec
22、essarycrush and reduce the entire dried sample in accordance with4.1.3 and 4.1.5.4.3 Gypsum Plaster, (C28/C28M).4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFi-bered PlasterScreen the dried sample through a 150-m(No. 100) sieve4and discard the residue retained on the sieve.Reweigh the remaining sa
23、mple and calculate the percentage ofthe dried sample. Reduce the sample in accordance with 4.1.5.Thoroughly blend and rehydrate the specimen in accordancewith 4.1.4.4.3.2 Gypsum Neat Plaster or Gypsum Gauging PlasterReduce the dried sample in accordance with 4.1.5. Thoroughlyblend and rehydrate the
24、specimen in accordance with 4.1.4.4.4 Gypsum Casting and Molding Plaster,(C59)Reducethe dried sample in accordance with 4.1.5. Thoroughly blendand rehydrate the specimen in accordance with 4.1.4.4.5 Gypsum Keenes Cement,(C61)Reduce the driedsample in accordance with 4.1.5. Blend in no more than 1 %m
25、olding plaster or K2SO4and rehydrate the specimen inaccordance with 4.1.4.4.6 Gypsum Concrete,(C317/C317M)Screen the driedsample through a 150-m (No. 100) sieve4and discard theresidue retained on the sieve. Reweigh the remaining sampleand calculate the percentage of the dried sample. Reduce thesampl
26、e in accordance with 4.1.5. Thoroughly blend and rehy-drate the specimen in accordance with 4.1.4.4.7 Gypsum Panel ProductsCut or break the dried sampleinto small pieces. Using a mortar and pestle, strike the piecesof the sample to loosen the paper face. Remove the pieces ofpaper by hand as they are
27、 separated from the core of thegypsum board. Carefully scrape any remaining powder fromthe paper. When all the paper has been removed from thepieces of the sample, reduce the sample in accordance with4.1.5.COMPLETE PROCEDURE5. Apparatus5.1 Analytical BalanceCapable of weighing the weighingbottles, l
28、ids and samples.5.2 BalanceCapable of weighing not less than 100 g at aprecision of 0.001 g.5.3 Drying OvenA mechanical convection oven set at 456 3C.5.4 DesiccatorCapable of being tightly sealed and con-taining calcium chloride or equivalent desiccant.5.5 Calcining Oven or FurnaceCapable of achievi
29、ng andmaintaining temperatures to not less than 1000C.5.6 Weighing BottlesBorosilicate glass or ceramic con-tainers with tightly sealable lids.5.7 Hot PlateA controllable hot plate capable of heatingcasseroles to approximately 120C.5.8 Porcelain CasserolesWith a capacity of 50 to 100 mL.5.9 Filterin
30、g Funnels.5.10 Filter Paper.5.11 Porcelain Crucibles.5.12 Mortar and Pestle.5.13 Mechanical Jaw CrusherCapable of crushing gyp-sum rocks up to 50 mm diameter.5.14 Mechanical GrinderBurr mill or equivalent capableof grinding the granular output of the jaw crusher specified in5.13.6. Reagents6.1 Purit
31、y of ReagentsUse reagent grade chemicals in alltests. Unless otherwise indicated, use reagents that conform to4Detailed requirements for this sieve are given in Specification E11.C471M 142the specifications of the Committee on Analytical Reagents ofthe American Chemical Society, where such specifica
32、tions areavailable.5If it is necessary to use other grades, first ascertainthat the reagent is of sufficiently high purity so that its use willnot lessen the accuracy of the determination.6.1.1 Ammonium Chloride (NH4Cl).6.1.2 Ammonium Hydroxide (sp gr 0.90)Concentratedammonium hydroxide (NH4OH).6.1.
33、3 Ammonium Nitrate (25 g/L)Dissolve 25 g of ammo-nium nitrate (NH4NO3) in water and dilute to 1 L.6.1.4 Ammonium Oxalate (NH4)2C2O4).6.1.5 Barium Chloride (100 g/L)Dissolve 100 g of bariumchloride (BaCl22H2O) in water and dilute to 1 L.6.1.6 Calcium Chloride (CaCl2)Anhydrous CalciumChloride with a c
34、ombined water of not more than 5 %.6.1.7 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).6.1.8 Hydrochloric Acid (1+4)Mix 1 volume of HCl (spgr 1.19) with 4 volumes of water.6.1.9 Hydrochloric Acid (1+5)Mix 1 volume of HCl (spgr 1.19) with 5 volumes of water.6.1.10 Nitric Acid (s
35、p gr 1.42)Concentrated nitric acid(HNO3).6.1.11 Potassium Chromate Solution (100 g/L)Dissolve5 g of potassium chromate (K2CrO4) in 50 mL of water, mix,add 10 drops of 0.05 N silver nitrate (AgNO3) solution, allowto stand for 5 min, and filter.6.1.12 Potassium Permanganate (5.6339 g/L)Dissolve5.6339
36、g of potassium permanganate (KMnO4) in water anddilute to 1 L.6.1.13 Silver Nitrate, Standard Solution (0.05 N)Prepareand standardize a 0.05 N silver nitrate (AgNO3) solution.6.1.14 Sodium Ammonium Phosphate(NaNH4HPO4).6.1.15 Sulfuric Acid (sp gr 1.84)Concentrated sulfuricacid (H2SO4).6.1.16 Sulfuri
37、c Acid (1+6)Carefully mix 1 volume ofH2SO4(sp gr 1.84) with 6 volumes of water.6.1.17 Nitric Acid (0.1 N)Mix 1.4 mL of HNO3(sp gr1.42) with 200 mL of water.6.1.18 Phenolphthalein Indicator SolutionDissolve 0.25 gof phenolphthalein in 30 mL of methanol and dilute to 50 mLwith water.6.1.19 Sodium Hydr
38、oxide Solution (0.1 N)Dissolve1gofsodium hydroxide (NaOH) in 250 mL of water.6.1.20 WaterReagent water shall be in accordance withSpecification D1193, type II. Specification D1193 gives thefollowing values for type II grade water.Electrical conductivity, max, S/cm at 298 K (25-C) 1.0Electrical resis
39、tivity, min, Mcm at 298 K (25-C) 1.0Total organic carbon (TOC), max, g/L 50.0Sodium, max, g/L 5.0Chlorides max, g/L 5.0Total silica, max, g/L 5.07. Free Water7.1 Significance and UseThe free water analysis deter-mines the amount of free water contained in the sample asopposed to chemically combined
40、water, and prepares thesample for further analysis.7.2 Procedure:7.2.1 Weigh a sample of the material as received of not lessthan 50 g to a precision of 0.001 g and spread it out in a thinlayer in a suitable vessel. Place in an oven and dry at 45 6 3Cfor 2 h, then cool in a desiccator and weigh agai
41、n. The loss ofweight corresponds to the free water.7.2.2 Retain the sample in a sealed container or in thedesiccator for further analysis.7.3 Calculation and ReportCalculate and report loss inweight as a percentage of the sample as received or of the driedsample as required.7.4 Precision and BiasNei
42、ther the precision nor the biasfor the free water analysis has been determined.8. Combined Water8.1 Significance and UseThe combined water analysisdetermines the percent of chemically combined water and isused to calculate the purity of gypsum or the amount ofgypsum or gypsum plaster in gypsum produ
43、cts.8.2 InterferencesSome materials, such as organic andhydrated compounds that decompose within the same tempera-ture range as gypsum, will cause high results. When themaximum temperature is exceeded, some carbonates undergodecomposition, which will result in high results.8.3 Procedure:8.3.1 For ea
44、ch sample, place three weighing bottles withlids in the preheated calcining oven or furnace and heat for 2 hat 215 to 230C. Place in the desiccator and allow to cool toroom temperature. Weigh the bottles and lids to the nearest0.0001 g and record the tare weights.8.3.2 Weigh out three specimens of a
45、pproximately 1 g eachof the sample as prepared in Section 4 and dried in Section 7to a precision of 0.0001 g in the previously tared weighingbottles and record the total weight with lids.8.3.3 Place the specimens in the calcining oven with the lidsplaced loosely on each bottle or crucible for2horunt
46、ilconstant weight has been obtained.8.3.4 Place the lids tightly on the weighing bottles, removefrom the oven, and place in the desiccator to cool to roomtemperature.8.3.5 Weigh each specimen to a precision of 0.0001 g andrecord the weights.8.3.6 Retain the residues for carbon dioxide analysis.8.4 C
47、alculation and ReportCalculate and report the aver-age loss in weight of the three specimens as a percentage of thesample as received or of the dried sample, as required, to thenearest 0.001 g and record the tare weights.8.5 Precision and BiasNeither the precision nor the biasfor the combined water
48、analysis has been determined.5Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., an
49、d the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.C471M 1439. Carbon Dioxide9.1 Summary of Test MethodThe sample is decomposedwith HCl and the liberated CO2is passed through a series ofscrubbers to remove water and sulfides. The CO2is absorbedwith Ascarite, a special sodium hydroxide absorbent, and thegain in weight of the absorption tube is determined andcalculated as percent CO2.9.2 Significance and UseThe carbon dioxide analysis
