Section 04 - ConstructionVolume 04.01, January 2005Cement; Lime; Gypsum

C0005-03 Specification for Quicklime for Structural PurposesC0011-05 Terminology Relating to Gypsum and Related Building Materials and SystemsC0022_C0022M-00 Specification for GypsumC0025-99 Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated LimeC0028_C0028M-00E01 Specification for Gypsum PlastersC0035-01 Specification for Inorganic Aggregates for Use in Gypsum PlasterC0036_C0036M Specification for Gypsum WallboardC0037_C0037M Specification for Gypsum LathC0050-00 Practice for Sampling, Sample Preparation, Packaging, and Marking of Lime and Limestone ProductsC0051-05 Terminology Relating to Lime and Limestone (as used by the Industry)C0059_C0059M-00 Specification for Gypsum Casting Plaster and Gypsum Molding PlasterC0061_C0061M-00 Specification for Gypsum Keene's CementC0079_C0079M Specification for Gypsum Sheathing BoardC0091-03A Specification for Masonry CementC0109_C0109M-02 Test Method for Compressive Strength of Hydraulic Cement Mortars (Using 2-in. or [50-mm] Cube Specimens)C0110-05 Test Methods for Physical Testing of Quicklime, Hydrated Lime, and LimestoneC0114-05 Test Methods for Chemical Analysis of Hydraulic CementC0115-96AR03 Test Method for Fineness of Portland Cement by the TurbidimeterC0141-97 Specification for Hydraulic Hydrated Lime for Structural PurposesC0150-04AE01 Specification for Portland CementC0151-00 Test Method for Autoclave Expansion of Portland CementC0183-02 Practice for Sampling and the Amount of Testing of Hydraulic CementC0184 Test Method for Fineness of Hydraulic Cement by the 150-|gmm (No. 100) and 75-|gmm (No. 200) SievesC0185-02 Test Method for Air Content of Hydraulic Cement MortarC0186-98 Test Method for Heat of Hydration of Hydraulic CementC0187-04 Test Method for Normal Consistency of Hydraulic CementC0188-95R03 Test Method for Density of Hydraulic CementC0191-04B Test Methods for Time of Setting of Hydraulic Cement by Vicat NeedleC0204-00 Test Method for Fineness of Hydraulic Cement by Air-Permeability ApparatusC0206-03 Specification for Finishing Hydrated LimeC0207-05 Specification for Hydrated Lime for Masonry PurposesC0219-03 Terminology Relating to Hydraulic CementC0226-02 Specification for Air-Entraining Additions for Use in the Manufacture of Air-Entraining Hydraulic CementC0230_C0230M-03 Specification for Flow Table for Use in Tests of Hydraulic CementC0265-03A Test Method for Water-Extractable Sulfate in Hydrated Hydraulic Cement MortarC0266-04 Test Method for Time of Setting of Hydraulic-Cement Paste by Gillmore NeedlesC0305-99E01 Practice for Mechanical Mixing of Hydraulic Cement Pastes and Mortars of Plastic ConsistencyC0317_C0317M-00R05 Specification for Gypsum ConcreteC0318_C0318M-00R05 Specification for Gypsum FormboardC0348-02 Test Method for Flexural Strength of Hydraulic-Cement MortarsC0349-02 Test Method for Compressive Strength of Hydraulic-Cement Mortars (Using Portions of Prisms Broken in Flexure)C0359-04 Test Method for Early Stiffening of Hydraulic Cement (Mortar Method)C0400-98 Test Methods for Quicklime and Hydrated Lime for Neutralization of Waste AcidC0430-96R03 Test Method for Fineness of Hydraulic Cement by the 45-|gmm (No. 325) SieveC0442_C0442M Specification for Gypsum Backing Board, Gypsum Coreboard, and Gypsum Shaftliner BoardC0451-05 Test Method for Early Stiffening of Hydraulic Cement (Paste Method)C0452-02 Test Method for Potential Expansion of Portland-Cement Mortars Exposed to SulfateC0465-99 Specification for Processing Additions for Use in the Manufacture of Hydraulic CementsC0471M-01 Test Methods for Chemical Analysis of Gypsum and Gypsum Products \[Metric\]C0472-99R04 Test Methods for Physical Testing of Gypsum, Gypsum Plasters and Gypsum ConcreteC0473-03 Test Methods for Physical Testing of Gypsum Panel ProductsC0474-05 Test Methods for Joint Treatment Materials for Gypsum Board ConstructionC0475_C0475M-02 Specification for Joint Compound and Joint Tape for Finishing Gypsum BoardC0490-04 Practice for Use of Apparatus for the Determination of Length Change of Hardened Cement Paste, Mortar, and ConcreteC0511-05 Specification for Mixing Rooms, Moist Cabinets, Moist Rooms, and Water Storage Tanks Used in the Testing of Hydraulic Cements and ConcretesC0514-04 Specification for Nails for the Application of Gypsum BoardC0563-04 Test Method for Optimum SO in Hydraulic Cement Using 24-h Compressive StrengthC0587-04 Specification for Gypsum Veneer PlasterC0588_C0588M-03E01 Specification for Gypsum Base for Veneer PlastersC0593-95R00 Specification for Fly Ash and Other Pozzolans for Use With LimeC0595-03 Specification for Blended Hydraulic CementsC0596-01 Test Method for Drying Shrinkage of Mortar Containing Hydraulic CementC0602-95AR01 Specification for Agricultural Liming MaterialsC0630_C0630M Specification for Water-Resistant Gypsum Backing BoardC0631-95AR04 Specification for Bonding Compounds for Interior Gypsum PlasteringC0645-04A Specification for Nonstructural Steel Framing MembersC0688-00 Specification for Functional Additions for Use in Hydraulic CementsC0706-02 Specification for Limestone for Animal Feed UseC0737-02 Specification for Limestone for Dusting of Coal MinesC0754-04 Specification for Installation of Steel Framing Members to Receive Screw-Attached Gypsum Panel ProductsC0778-02 Specification for Standard SandC0786-96R03 Test Method for Fineness of Hydraulic Cement and Raw Materials by the 300-|gmm (No. 50), 150-|gmm (No. 100), and 75-|gmm (No. 200) Sieves by Wet MethodsC0806-04 Test Method for Restrained Expansion of Expansive Cement MortarC0807-05 Test Method for Time of Setting of Hydraulic Cement Mortar by Modified Vicat NeedleC0821-78R00 Specification for Lime for Use with PozzolansC0840-04A Specification for Application and Finishing of Gypsum BoardC0841-03 Specification for Installation of Interior Lathing and FurringC0842-05 Specification for Application of Interior Gypsum PlasterC0843-99E01 Specification for Application of Gypsum Veneer PlasterC0844-04 Specification for Application of Gypsum Base to Receive Gypsum Veneer PlasterC0845-04 Specification for Expansive Hydraulic CementC0847-04 Specification for Metal LathC0897-00 Specification for Aggregate for Job-Mixed Portland Cement-Based PlastersC0911-05 Specification for Quicklime, Hydrated Lime, and Limestone for Chemical and Industrial UsesC0917-05 Test Method for Evaluation of Cement Strength Uniformity From a Single SourceC0926-98A Specification for Application of Portland Cement-Based PlasterC0931_C0931M Specification for Exterior Gypsum Soffit BoardC0932-05 Specification for Surface-Applied Bonding Compounds for Exterior PlasteringC0933-04 Specification for Welded Wire LathC0954-04 Specification for Steel Drill Screws for the Application of Gypsum Panel Products or Metal Plaster Bases to Steel Studs from 0.033 in. (0.84 mm) to 0.112 in. (2.84 mm) in ThicknessC0955-03 Specification for Load-Bearing (Transverse and Axial) Steel Studs, Runners (Tracks), and Bracing or Bridging for Screw Application of Gypsum Panel Products and Metal Plaster BasesC0956-04 Specification for Installation of Cast-In-Place Reinforced Gypsum ConcreteC0960_C0960M Specification for Predecorated Gypsum BoardC0977-03 Specification for Quicklime and Hydrated Lime for Soil StabilizationC1002-04 Specification for Steel Self-Piercing Tapping Screws for the Application of Gypsum Panel Products or Metal Plaster Bases to Wood Studs or Steel StudsC1005-00 Specification for Reference Masses and Devices for Determining Mass and Volume for Use in the Physical Testing of Hydraulic CementsC1007-04 Specification for Installation of Load Bearing (Transverse and Axial) Steel Studs and Related AccessoriesC1012-04 Test Method for Length Change of Hydraulic-Cement Mortars Exposed to a Sulfate SolutionC1032-04 Specification for Woven Wire Plaster BaseC1038-04 Test Method for Expansion of Hydraulic Cement Mortar Bars Stored in WaterC1047-05 Specification for Accessories for Gypsum Wallboard and Gypsum Veneer BaseC1063-03 Specification for Installation of Lathing and Furring to Receive Interior and Exterior Portland Cement-Based PlasterC1097-95R01 Specification for Hydrated Lime for Use in Asphaltic-Concrete MixturesC1157-03 Performance Specification for Hydraulic CementC1164-92R03 Practice for Evaluation of Limestone or Lime Uniformity From a Single SourceC1177_C1177M-04E01 Specification for Glass Mat Gypsum Substrate for Use as SheathingC1178_C1178M-04E01 Specification for Glass Mat Water-Resistant Gypsum Backing PanelC1222-03 Practice for Evaluation of Laboratories Testing Hydraulic CementC1264-05 Specification for Sampling, Inspection, Rejection, Certification, Packaging, Marking, Shipping, Handling, and Storage of Gypsum Panel ProductsC1271-99 Test Method for X-ray Spectrometric Analysis of Lime and LimestoneC1278_C1278M-03E01 Specification for Fiber-Reinforced Gypsum PanelC1280-04 Specification for Application of Gypsum SheathingC1301-95R01 Test Method for Major and Trace Elements in Limestone and Lime by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP) and Atomic Absorption (AA)C1318-95R01 Test Method for Determination of Total Neutralizing Capability and Dissolved Calcium and Magnesium Oxide in Lime for Flue Gas Desulfurization (FGD)C1328-03A Specification for Plastic (Stucco) CementC1329-04 Specification for Mortar CementC1355_C1355M-96R01 Specification for Glass Fiber Reinforced Gypsum CompositesC1356-96R01 Test Method for Quantitative Determination of Phases in Portland Cement Clinker by Microscopical Point-Count ProcedureC1365-98R04 Test Method for Determination of Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction AnalysisC1381-97R02E01 Specification for Molded Glass Fiber Reinforced Gypsum PartsC1395_C1395M Specification for Gypsum Ceiling Board

C1396_C1396M-04 Specification for Gypsum BoardC1397-04 Practice for Application of Class PB Exterior Insulation and Finish SystemsC1437-01 Test Method for Flow of Hydraulic Cement MortarC1467_C1467M-00 Specification for Installation of Molded Glass Fiber Reinforced Gypsum PartsC1489-01 Specification for Lime Putty for Structural PurposesC1506-03 Test Method for Water Retention of Hydraulic Cement-Based Mortars and PlastersC1513-04 Specification for Steel Tapping Screws for Cold-Formed Steel Framing ConnectionsC1516-02 Practice for Application of Direct-Applied Exterior Finish SystemsC1529-02A Specification for Quicklime, Hydrated Lime, and Limestone for Environmental UsesC1535-04 Practice for Application of Exterior Insulation and Finish Systems Class PIC1546-02 Guide for Installation of Gypsum Products in Concealed Radiant Ceiling Heating SystemsC1565-04 Test Method for Determination of Pack-Set Index of Portland CementC1597M-04 Specification for Gypsum Wallboard (Hard Metric Sizes)D6249-98R04 Guide for Alkaline Stabilization of Wastewater Treatment Plant Residuals

Designation: C 5 03

Standard Specification forQuicklime for Structural Purposes1

This standard is issued under the fixed designation C 5; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) 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 This specification covers all classes of quicklime such as

crushed lime, granular lime, ground lime, lump lime, pebblelime, and pulverized lime, used for structural purposes.

2. Referenced Documents2.1 ASTM Standards:C 25 Test Methods for Chemical Analysis of Limestone,

Quicklime, and Hydrated Lime2C 50 Practice for Sampling, Inspection, Packing, and Mark-

ing of Lime and Limestone Products2C 51 Terminology Relating to Lime and Limestone (As

Used by the Industry)2C 110 Test Methods for Physical Testing of Quicklime,

Hydrated Lime, and Limestone2C 1489 Specification of Lime Putty for Structural Purposes2E 11 Specification for Wire-Cloth Sieves for Testing Pur-

poses3

3. Terminology3.1 DefinitionsUnless otherwise specified, for definitions

of terms used in this standard, refer to Terminology C 51.

4. Chemical Composition4.1 The quicklime shall conform to the following require-

ments as to chemical composition, calculated on a nonvolatilebasis:

Calcium Lime Magnesium Lime

Calcium oxide, min, % 75Magnesium oxide, min, % 20Calcium and magnesium oxide,

min, %95 95

Silica, alumina, and oxide of iron,max, %

5 5

Carbon dioxide, max, %:If sample is taken at place of

manufacture3 3

If sample is taken at any otherplace

10 10

5. Residue5.1 The quicklime shall contain no more than 15 weight %

of residue.

6. General Requirements6.1 Quicklime shall be slaked and aged in accordance with

the printed directions of the manufacturer. The resulting limeputty shall be stored until cool.

6.2 Lime putty prepared in accordance with AppendixX1.4.2 must conform to the requirements of SpecificationC 1489.

7. Sampling, Inspection, etc.7.1 The sampling, inspection, rejection, retesting, packag-

ing, and marking shall be conducted in accordance withMethods C 50.

8. Test Methods8.1 Conformance to chemical requirements shall be deter-

mined in accordance with Test Methods C 25.8.2 Conformance to plasticity and residue requirements

shall be determined in accordance with Test Methods C 110.

9. Keywords9.1 building (structural); calcium oxide; dolomitic lime;

high calcium lime; lime putty; magnesium oxide; plasticity;quicklime; residue; slaking

1 This specification is under the jurisdiction of ASTM Committee C07 on Limeand is the direct responsibility of Subcommittee C07.02 on Structural Lime.

Current edition approved May 10, 2003. Published July 2003. Originallyapproved in 1913. Last previous edition approved in 1997 as C 5 79 (1997).

2 Annual Book of ASTM Standards, Vol 04.01.3 Annual Book of ASTM Standards, Vol 14.02.

1

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

APPENDIX

(Nonmandatory Information)

X1. SLAKING AND PREPARATION OF LIME PUTTY

X1.1 IntroductionX1.1.1 Quicklime can never be used as such for structural

purposes; it must always be slaked first. Since the method ofslaking is an important factor in determining the quality of thefinished product, the following directions for the preparation oflime putty are given, not as a part of the specification, but asinformation for the further protection of the purchaser.

X1.1.2 Different kinds of lime vary considerably in the wayin which they behave with water. A little supervision over theoperation of slaking will amply pay for itself by ensuring theproduction of the greatest possible quantity and the bestpossible quality of putty. To find out how to slake a new lot oflime, it is safest to try a little of it and see how it works. Sincedifferent lots of the same brand of lime vary somewhat, andsince the weather conditions at the time have a decidedinfluence, it is wise to try a sample from each lot used, whetherfamiliar with the brand or not.

X1.2 Classification of LimesX1.2.1 In a bucket, put two or three lumps of lime about the

size of ones fist, or, in the case of granular lime, an equivalentamount. Add sufficient water to just barely cover the lime, andnote how long it takes for slaking to begin. Slaking has begunwhen pieces split off from the lumps or when the lumpscrumble. Water of the same temperature should be used for testand field practice.

X1.2.2 If slaking begins in less than 5 min, the lime is quickslaking; from 5 to 30 min, medium slaking; over 30 min, slowslaking.

X1.3 Directions for SlakingX1.3.1 Slake quicklime in accordance with the printed

directions of the manufacturer. When such directions are notprovided, proceed as follows:

X1.3.2 For quick-slaking lime, always add the lime to thewater, not the water to the lime. Have sufficient water at first tocover all the lime completely. Have a plentiful supply of water

available for immediate usea hose throwing a good stream,if possible. Watch the lime constantly. At the slightest appear-ance of escaping steam, hoe thoroughly and quickly, and addenough water to stop the steaming. Do not be afraid of usingtoo much water with this kind of lime.

X1.3.3 For mediumslaking lime, add the water to the lime.Add enough water so that the lime is about half submerged.Hoe occasionally if steam starts to escape. Add a little waternow and then if necessary to prevent the putty from becomingdry and crumbly. Be careful not to add any more water thanrequired, and not too much at a time.

X1.3.4 For slowslaking lime, add enough water to the limeto moisten it thoroughly. Let it stand until the reaction hasstarted. Cautiously add more water, a little at a time, takingcare that the mass is not cooled by the fresh water. Do not hoeuntil the slaking is practically complete. If the weather is verycold, it is preferable to use hot water, but if this is not available,the mortar box may be covered in some way to retain the heat.

X1.4 Preparation of Putty for UseX1.4.1 After slaking, prepare putty for use as follows:X1.4.2 White CoatAfter slaking and aging finishing

quicklime in accordance with the printed directions of themanufacturer, store the putty until cool. If no printed directionsare provided by the manufacturer, prepare the putty for use asfollows: After the action has ceased, run off the putty througha No. 10 (2.00-mm) sieve conforming to Specification E 11,and store for a minimum of 2 weeks.

X1.4.3 Base CoatsAfter the action has ceased, run off theputty through a No. 8 (2.36-mm) sieve conforming to Speci-fication E 11. Add sand up to equal parts by weight, all of thehair or other fibers required, and store for a minimum of 2weeks.

X1.4.4 Masons MortarAfter the action has ceased, addpart or all of the sand required, and store for a minimum of 24h.

ASTM International takes no position respecting the validity of any patent rights 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 time 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 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), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website(www.astm.org).

C 5 03

2

Designation: C 11 03d

Standard Terminology Relating toGypsum and Related Building Materials and Systems1

This standard is issued under the fixed designation C 11; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope1.1 This standard covers terminology relating to gypsum

and related building materials and systems. The terms aregenerically defined. More specific and expanded definitionsmay appear in appropriate standards.

2. Referenced Documents2.1 ASTM Standards: 2C 22/C 22M Standard Specification for GypsumC 28/C 28M Specification for Gypsum PlastersC 35 Specification for Inorganic Aggregates for Use in

Gypsum PlasterC 36/C M Specification for Gypsum WallboardC 37 Specification for Gypsum LathC 52 Specification for Gypsum Partition Tile or Block3C 59/C 59M Specification for Gypsum Casting and Mold-

ing PlasterC 61/C 61M Specification for Gypsum Keenes CementC 79/C 79M Specification for Treated Core and Nontreated

Core Gypsum Sheathing BoardC 317/C 317M Specification for Gypsum ConcreteC 318/C 318M Specification for Gypsum FormboardC 472 Test Methods for Physical Testing of Gypsum, Gyp-

sum Plasters and Gypsum ConcreteC 473 Test Methods for Physical Testing of Gypsum Panel

ProductsC 475/C 475M Specification for Joint Compound and Joint

Tape for Finishing Gypsum BoardC 557 Specification for Adhesives for Fastening Gypsum

Wallboard to Wood FramingC 587 Specification for Gypsum Veneer PlasterC 588/C 588M Specification for Gypsum Base for Veneer

Plasters

E 84 Test Method for Surface Burning Characteristics ofBuilding Materials

E 96 Test Methods for Water Vapor Transmission of Mate-rials

E 119 Test Methods for Fire Tests of Building Constructionand Materials

E 337 Test Method for Measuring Humidity With a Psy-chrometer (The Measurement of Wet- and Dry-Bulb Tem-peratures)

3. Terminologyaccelerator, na material that reduces setting time.accessories, nproducts fabricated for the purpose of forming

corners, edges, control joints, or decorative effects.adhesive, na substance capable of holding materials together

by surface attachment.admixture, na material other than water, aggregates, hy-

draulic cementitious material, and fiber reinforcement that isused as an ingredient to modify properties and is added to thebatch before or during its mixture.

aggregate, nan inert granular material which may be addedto gypsum plasters. (C 35)

all purpose compound, na compound formulated andmanufactured to serve as a taping or finishing compound, orboth.

anhydrite, nthe mineral consisting primarily of anhydrouscalcium sulfate, CaSO4.

arris (of an arch), nthe outside corner or angle formed bythe meeting of a wall surface with the curved surface of anarch (see Fig. 1).

basecoat, nthe first layer or layers of plaster applied overlath or other substrate.

DISCUSSIONThe first application is normally called a scratch coatand the second application is referred to as a brown coat.

bedding coat, nthat coat of plaster to receive aggregate orother decorative material of any size, impinged or embeddedinto its surface, before it sets.

bond plaster, na calcined gypsum plaster specially formu-lated for application over rough monolithic concrete as abonding coat for a subsequent gypsum plaster layer.

(C 28/C 28M)

1 This terminology is under the jurisdiction of ASTM Committee C11 onGypsum and Related Building Materials and Systems and is the direct responsibilityof Subcommittee C11.91 on Terminology and Editorial.

Current edition approved Oct. 1, 2003. Published November 2003. Originallyapproved in 1916. Last previous edition approved in 2003 as C 11 03c.

2 For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at service@astm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.

3 Withdrawn.

1

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

bridging, nin framing, sections of wood or metal piecesused between framing members to stiffen, give lateralsupport, and minimize rotation.

brown coat, nthe second layer in three-coat plaster applica-tion.

building construction joint, na designed division of abuilding that allows movement of all component parts of thebuilding, in any plane, which may be caused by thermal,seismic, wind loading, or any other force. The constructionof the separation is accomplished by one of the followingmethods: (1) manufactured devices suitable for this applica-tion, or (2) by field fabrication of suitable materials.

calcined gypsum, na dry powder; primarily calcium sulfatehemihydrate, resulting from calcination of gypsum; cemen-titious base for production of most gypsum plasters: alsocalled plaster of paris, sometimes called stucco.

calcium sulfate, nthe chemical compound CaSO4.cementitious material, na material that, when mixed with

water, with or without aggregate, provides the plasticity andthe cohesive and adhesive properties necessary for place-ment, and the formation of a rigid mass.

coat, na layer of plaster applied in a single operation.combined water, nthe water chemically held, as water of

crystallization, by the calcium sulfate dihydrate or hemihy-drate crystal.

compressive strength, nthe maximum load sustained by astandard specimen of a material when subjected to a crush-ing force.

consistency, na property of a material determined by thecomplete flow force relation. (C 557)

consistency (normal), nthe number of millilitres of waterper 100 g of gypsum plaster or gypsum concrete required toproduce a mortar or a slurry of specified fluidity. (C 472)

control (expansion-contraction) joint, na designed separa-tion in the system materials that allows for movement causedby expansion or contraction of the system. The constructionof the separation is accomplished by one of the followingmethods: (1) manufactured devices suitable for this applica-tion, or (2) by field fabrication of suitable materials.

core (of gypsum board), nthe hardened material filling thespace between the face and back papers consisting substan-tially of rehydrated gypsum with additives.

cored tile or block, nsee gypsum tile or block. (C 52)

cornerbead, nan accessory for outside corners.corner reinforcement, exterior, na preformed section of

wire or expanded sheet steel, for the reinforcement ofexterior stucco external corners (arrises).

cure (portland cement plaster or stucco), v(1) to provideconditions conducive to the hydration process of portlandcement plaster or stucco, or (2) to maintain proper tempera-ture and a sufficient quantity of water within the plaster toensure cement hydration.

density, nthe weight per unit volume of a material.(C 472)

edge (of gypsum board), nthe paper-bound edge as manu-factured.

edge trim, nan accessory to cover exposed ends or edges ofgypsum board.

embedding compoundsee taping compound.end (of gypsum board), nthe end perpendicular to the

paper-bound edge. The gypsum core is always exposed.expansion joint, nsee control (expansion-contraction)

joint.face, nthe surface designed to be left exposed to view or to

receive decoration or additional finishes.featured edge, nan edge configuration of the paper bound

edge of gypsum board that provides special design orperformance.

fineness modulus, nan empirical factor obtained by addingtotal percentages of a sample of aggregate retained on eachof a specified series of sieves and dividing by 100. The sievesizes used are: No. 100 (150 m), No. 50 (300 m), No. 30(600 m), No. 16 (1.18 mm), No. 8 (2.36 mm), No. 4 (4.75mm), 38 in. (9.5 mm), 34 in. (19.0 mm), 112 in. (38.1 mm)and larger, increasing in the ratio of 2 to 1.

finish coat, nthe final layer of plaster applied over a basecoator other substrate.

finishing compound, n(sometimes called topping com-pound) a compound specifically formulated and manufac-tured for use over taping or all purpose compounds toprovide a smooth and level surface for the application ofdecoration.

fire-resistance classification, na standard rating of fire-resistance and protective characteristics of a building con-struction or assembly. (E 119)

flame spread classification, na standard rating of relativesurface burning characteristics of a building material ascompared to a standard material. (E 84)

flexural strength, nthe maximum load sustained by astandard specimen of a sheet material when subjected to abending force.

floating, vthe act of spreading, compacting, or consolidatingto achieve a specified uniform appearance.

framing member, nstud, plate, track, joist, furring, andother support to which a gypsum panel product, or metalplaster base is attached.

free water, nall water contained by gypsum board or plasterin excess of that chemically held as water of crystallization.

gauging plaster, na calcined gypsum plaster designed to bemixed with lime putty. (C 28/C 28M)

FIG. 1 Arris (of an Arch)

C 11 03d

2

grout, ngypsum or portland cement plaster used to fillcrevices or to fill hollow metal frames.

gypsum, nthe mineral consisting primarily of fully hydratedcalcium sulfate, CaSO42H2O or calcium sulfate dihydrate.

(C 22/C 22M)gypsum backing board, na 14 in. to 58 in. gypsum board for

use as a backing for gypsum wallboard, acoustical tile, orother dry cladding.water resistant gypsum backing boarda gypsum boarddesigned for use on walls primarily as a base for theapplication of ceramic, or plastic tile.

gypsum base for veneer plasters, na gypsum board used asthe base for application of a gypsum veneer plaster.

(C 588/C 588M)gypsum board, nthe generic name for a family of sheet

products consisting of a noncombustible core primarily ofgypsum with paper surfacing.

gypsum concrete, na calcined gypsum mixed with woodchips or aggregate, or both. (C 317/C 317M)

gypsum core board, na 34 in. (19.0 mm) to 1 in. (25.4 mm)gypsum board consisting of a single board or factorylaminated multiple boards, used as a gypsum stud or core insemisolid or solid gypsum board partitions.

gypsum formboard, na gypsum panel product used as thepermanent form for poured gypsum roof decks. (C 318/

C 318M)gypsum lath, na gypsum board used as the base for

application of gypsum plaster. (C 37)perforated gypsum latha gypsum lath having perforationsto provide mechanical keying of the basecoat plaster.foil-backed gypsum laththe same as plain gypsum lathexcept that in addition, the back surface shall be coveredwith a continuous sheet of pure bright finished aluminumfoil.type X latha gypsum lath specially manufactured toprovide specific fire-resistant characteristics.

gypsum molding plaster, na calcined gypsum plaster usedprimarily for plaster casts or molds, sometimes used as agauging plaster. (C 59/C 59M, C 28/C 28M)

gypsum neat plaster, na calcined gypsum mixed at the millwith ingredients to control working quality and setting time.

(C 28/C 28M)DISCUSSIONNeat plaster is either fibered or unfibered. The addition

of aggregate is required on the job.gypsum panel products, nthe general name for a family of

sheet products consisting essentially of gypsum.gypsum plaster, nthe generic name for a family of pow-

dered cementitious products consisting primarily of calcinedgypsum with additives to modify physical characteristics,and having the ability, when mixed with water, to produce aplastic mortar or slurry which can be formed to the desiredshape by various methods and will subsequently set to ahard, rigid mass. (C 28/C 28M)

gypsum sheathing, na gypsum board used as a backing forexterior surface materials, manufactured with water-repellant paper and may be manufactured with a water-

resistant core. (C 79/C 79M)gypsum tile or block, na cast gypsum building unit.

(C 52)gypsum wallboard, na gypsum board used primarily as an

interior surfacing for building structures. (C 36/C 36M)foil-backed gypsum wallboarda gypsum wallboard withthe back surface covered with a continuous sheet of purebright finished aluminum foil. (C 36/C 36M)type X gypsum wallboarda gypsum wallboard speciallymanufactured to provide specific fire-resistant characteristics

(C 36/C 36M).gypsum wood-fibered plaster, na calcined gypsum plaster

containing shredded or ground wood fiber added duringmanufacture.

hemihydrate, nthe dry powder, calcium sulfate hemihy-drate, resulting from calcination of CaSO42H2O, calciumsulfate dihydrate. See calcined gypsum.

joining, nthe juncture of two separate plaster applications ofthe same coat, usually within a single surface plane.

joint compound, na compound used for taping or finishinggypsum board, or both.

joint tape, na type of paper, metal, fabric, glass mesh, orother material, commonly used with a cementitious com-pound, to reinforce the joints between adjacent gypsumboards. (C 475/C 475M)

Keenes cement, nan anhydrous gypsum plaster character-ized by a low mixing water requirement and special settingproperties, primarily used with lime to produce hard, densefinish coats. (C 61/C 61M)

key, nthe grip or mechanical bond of one coat of plaster toanother coat, or to a substrate.

DISCUSSIONIt may be accomplished physically by the penetration ofwet mortar or crystals into paper fibers, perforations, scoring irregu-larities, or by the embedment of the lath.

lathsee gypsum lath.load-bearing partition, na partition designed to support a

portion of the building structure.machine direction, nthe direction parallel to the paper-

bound edge of the gypsum board.masonry cement, na hydraulic cement for use in mortars for

masonry construction, containing one or more of the follow-ing materials: portland cement, portland blast furnace slagcement, portland-pozzolan cement, natural cement, slagcement, or hydraulic lime; and in addition usually containingone or more materials such as hydrated lime, limestone,chalk, calcareous shell, talc, slag, or clay as prepared for thispurpose.

mechanical bonds, nthe attachment created when plasterpenetrates, into or through, the substrate, or envelops irregu-larities in the surface of the substrate.

mill-mixed plaster (ready-mixed plaster), nmaterial for-mulated and dry-blended by the manufacturer, requiring onlythe addition of and mixing with water.

mortar, na mixture of gypsum plaster with aggregate orhydrate lime, or both, and water to produce a trowelablefluidity.

C 11 03d

3

neat gypsum plastersee gypsum neat plaster.perm, na unit of measurement of water vapor permeance; a

metric perm, or 1 g/24 hm2mm Hg. U.S. unit, 1 grain/hft2in. Hg. (E 96)

permeability, nthe property of a porous material that per-mits a fluid (or gas) to pass through it; in construction,commonly refers to water vapor permeability of a sheetmaterial or assembly and is defined as water vapor per-meance per unit thickness. Metric unit of measurement,metric perms per centimetre of thickness. See water vaportransmission, perm, permeance. (E 96)

permeance (water vapor), nthe ratio of the rate of watervapor transmission (WVT) through a material or assemblybetween its two parallel surfaces to the vapor pressuredifferential between the surfaces. Metric unit of measure-ment is the metric perm, 1 g/24 hm2mm Hg; U.S. unit, 1grain/hft2in. Hg. See water vapor transmission, perme-ability, perm. (E 96)

plastersee gypsum plaster, gypsum neat plaster.plaster bond, nthe adhesion between plaster coats or be-

tween plaster and substrate.plastic cement, na hydraulic cement to which one or more

plasticizing agents (but not more than 12 % by volume) havebeen added during intergrinding or blending to increase theworkability and molding qualities of the resultant cementpaste, mortar, or plaster.

plasticity, nthe property of freshly mixed cement paste,mortar, or plaster which determines its workability andmolding qualities.

portland cement, na hydraulic cement produced by pulver-izing clinker consisting essentially of hydraulic calciumsilicates, and usually containing one or more forms ofcalcium sulfate as an interground addition.

portland cement plaster, na plaster mix in which portlandcement or combinations of portland and masonry cements orportland cement and lime are the principal cementitiousmaterials mixed with aggregate.

purity, nthe percentage of CaSO412 H2O in the calcinedgypsum portion of a gypsum plaster or gypsum concrete, asdefined by Specification C 28/C 28M, for Gypsum Plasters.The percentage of CaSO42H2O in the gypsum or thegypsum portion of fully hydrated, dry, set gypsum plaster.

(C 472, C 28/C 28M)ready-mixed plaster, na calcined gypsum plaster with

aggregate added during manufacture. (C 28/C 28M)recessed edge, nsee tapered edgerelative humidity, nthe ratio of actual water vapor pressure

to the saturation water vapor pressure at the same tempera-ture, expressed as a percentage. (E 337)

retarder, na material that extends setting time.round edge, na rounded, paper-bound edge formation on

gypsum board, commonly used for gypsum lath. (C 37,C 473)

saddle-tie, for furring, na single or double strand of wireused to attach furring members to framing members of wallor ceiling assemblies. See Fig. 2.

saddle-tie, for furring, vto attach furring members to fram-ing members of wall or ceiling assemblies using a single ordouble strand of wire. See Fig. 2.

saddle-tie, for wire hangers, vto attach wire hangers to mainrunners. See Fig. 3.

scratch coat, nthe first layer of plaster applied over lath orother substrate.

set, nthe chemical and physical change in plaster as it goesfrom a plastic, workable state to a rigid state. See settingtime. (C 472)

FIG. 2 Saddle-Tie

FIG. 3 Saddle-Tie

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setting time, nthe elapsed time required for a gypsumplaster to attain a specified hardness and strength aftermixing with water. (C 472)

smooth-trowel finish, na uniform finish free of grainy orcoarse areas, trowel marks, or other avoidable imperfections.

stucco, na portland cement-aggregate plaster mix designedfor use on exterior surfaces. See portland cement plaster.

synthetic gypsum, na chemical product, consisting prima-rily of calcium sulfate dihydrate (CaSO42H2O) resultingprimarily from an industrial process.

tapered edge, nan edge formation of gypsum board whichprovides a shallow depression at the paper-bound edge toreceive joint reinforcement. Also known as a recessed edge.

(C 473, C 36/C 36M)taping compound, n(sometimes called embedding com-

pound) a compound specifically formulated and manufac-tured for use in embedding of joint reinforcing tape atgypsum board joints.

temper, vto mix or restore to a workable consistency.texture finish, nany applied decorative finish other than

smooth.three-coat work, nplaster applied in three successive coats

with time between coats for setting or drying, or both.topping compoundsee finishing compound.veneer plaster, na calcined gypsum plaster formulated to be

applied in thin coats. (C 587)wallboardsee gypsum wallboard. (C 36/C 36M)water absorption, nthe amount of water absorbed by a

material under specified test conditions commonly expressedas weight percent of the test specimen.

water-repellent paper, ngypsum board paper surfacingwhich has been formulated or treated to resist water pen-etration.

water-resistant core, na gypsum board specially formulatedto resist water penetration.

water vapor transmission (WVT), nthe rate of water vaporflow, under steady specified conditions, through a unit areaof a material, between its two parallel surfaces and normal tothe surfaces. Metric unit of measurement is 1 g/24 hm2. Seepermeability,permeance, perm. (E 96)

wood-fibered plaster, na calcined gypsum plaster contain-ing shredded or ground wood fiber added during manufac-ture. (C 28/C 28M)

This standard is subject to revision at any time 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 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), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website(www.astm.org).

C 11 03d

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Designation: C 22/C 22M 00

Standard Specification forGypsum1

This standard is issued under the fixed designation C 22/C 22M; the number immediately following the designation indicates the yearof original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope *1.1 This specification covers gypsum, calcium sulfate com-

bined with two molecules of water in crystalline form andhaving the approximate chemical formula CaSO42H2O.

1.2 The values stated in either inch-pound units or SI(metric) are to be regarded separately as the standard. Withinthe text, the SI units are shown in brackets. The values statedin each system shall be used independently of the other. Valuesfrom the two systems shall not be combined.

2. Referenced Documents2.1 ASTM Standards:C 11 Terminology Relating to Gypsum and Related Build-

ing Materials and Systems2C 471 Test Methods for Chemical Analysis of Gypsum and

Gypsum Products2C 472 Test Methods for Physical Testing of Gypsum, Gyp-

sum Plasters and Gypsum Concrete2

3. Terminology3.1 DefinitionsDefinitions shall be in accordance with

Terminology C 11.

4. Chemical Composition4.1 Gypsum shall contain not less than 70.0 weight percent

CaSO42H2O.4.2 The chemical composition, within the limits prescribed

by 4.1, shall be specified in the purchase order or contract.

5. Physical Properties5.1 SizeIf necessary, gypsum shall be crushed or ground,

or both, to the size specified in the purchase order.

6. Sampling6.1 BulkWhen gypsum is shipped in bulk, samples of

approximately 5 lb (2 kg) each shall be taken at regularintervals during the complete loading or unloading of thecarrier, in such a way as to accumulate not less than 200 lb (90kg) of material and to represent correctly the percentages of

both the coarse particles and the fines in the shipment. Thismaterial shall be broken to pass a 1-in. (25.0-mm) sieve,thoroughly mixed, and reduced by quartering to provide notless than a 1-lb (0.5-kg) sample for the laboratory.

6.2 PackagesWhen gypsum is shipped in packages, notless than 1 % of the packages shall be sampled. Samples shallbe taken from both the surface and the center of the packages.These samples shall then be broken, mixed, and quartered inaccordance with 6.1.

6.3 Laboratory SamplesEach laboratory sample shall beplaced immediately in an airtight container and shipped to thelaboratory for testing.

7. Test Methods7.1 The chemical composition of gypsum shall be deter-

mined in accordance with Test Methods C 471.7.2 The physical properties of gypsum shall be determined

in accordance with Test Methods C 472.

8. Inspection8.1 Inspection of the gypsum shall be agreed upon between

the purchaser and the supplier as part of the purchase agree-ment.

9. Rejection9.1 Rejection of gypsum that fails to conform to the

requirements of this specification shall be reported to theproducer or supplier promptly and in writing. The notice ofrejection shall contain a statement documenting how thegypsum has failed to conform to the requirements of thisspecification.

10. Certification10.1 When specified in the purchase agreement, a manufac-

turers or suppliers report shall be furnished at the time ofshipment certifying that the product is in compliance with thisspecification.

11. Packaging and Package Marking11.1 Gypsum shall be shipped either in packages or in bulk.11.2 When shipped in packages for resale, the following

information (Note) shall be legibly marked on each package oron a tag of suitable size attached thereto:

11.2.1 Name of manufacturer,11.2.2 Description of material, and

1 This specification is under the jurisdiction of ASTM Committee C11 onGypsum and Related Building Materials and Systems and is the direct responsibilityof Subcommittee C11.01 on Specifications and Test Methods for Gypsum Products.

Current edition approved May 10, 2000. Published July 2000. Originallypublished as C 22 19.Last previous edition C 22 96{1.

2 Annual Book of ASTM Standards, Vol 04.01.

1

*A Summary of Changes section appears at the end of this standard.Copyright ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

11.2.3 Net or gross weights, or both, of the package.11.3 When shipped in bulk, a card containing the required

information in accordance with 11.2 shall be conspicuouslyplaced in the carrier.

NOTE 1State law may require additional information.

12. Keywords12.1 calcium sulfate; gypsum

SUMMARY OF CHANGES

This section identifies the location of changes to this specification that have been incorporated since the lastissue. Committee C-11 has identified those changes that affect the technical interpretation or use of thespecification.

(1) Section 9.1 was revised.

The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connectionwith any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any suchpatent rights, and the risk of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time 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 Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make yourviews known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM, 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 above address or at610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website (www.astm.org).

C 22/C 22M

2

Designation: C 25 99

Standard Test Methods forChemical Analysis of Limestone, Quicklime, and HydratedLime1

This standard is issued under the fixed designation C 25; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) 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 chemical analysis of

high-calcium and dolomitic limestone, quicklime, and hy-drated lime. These test methods are classified as either standard(preferred) or alternative (optional).

1.2 The standard test methods are those that employ classi-cal gravimetric or volumetric analytical procedures and aretypically those required for referee analyses where chemicalspecification requirements are an essential part of contractualagreement between buyer and seller.

1.3 Alternative or optional test methods are provided forthose who wish to use procedures shorter or more convenientthan the standard methods for the routine determinations ofcertain constituents. Optional test methods may sometimes bepreferred to the standard test methods, but frequently the use ofmodern and expensive instrumentation is indicated which maynot be accessible to everyone. Therefore, the use of these testmethods must be left to the discretion of each laboratory.

1.4 The analytical procedures appear in the following order:Section

Aluminum Oxide 15Available Lime Index 28Calcium and Magnesium Oxide:

Alternative EDTA Titration Method 31Calcium Carbonate Equivalent 33Calcium Oxide:

Gravimetric Method 16Volumetric Method 17

Carbon Dioxide by Standard Method 22Combined Oxides of Iron and Aluminum 12Ferrous Iron Appendix X5Free Calcium Oxide Appendix X6Free Moisture in Hydrated Lime 21Free Moisture in Limestone 20Free Silica 29Insoluble Matter Including Silicon Dioxide:

Standard Method 8Optional Perchloric Acid Method 9

Insoluble Matter Other Than Silicon Diox-ide

11

Loss on Ignition 19Magnesium Oxide 18Manganese:

Bismuthate Method Appendix X4Periodate (Photometric) Method 27

pH Determination of Alkaline Earth Solu-tions

34

Phosphorus:Titrimetric Method Appendix X3Molybdovanadate Method 26

Silicon Dioxide 10Strontium Oxide Appendix X2Sulfur Trioxide 23Total Carbon:

Direct Combustion-Thermal Conductiv-ity Cell Method

32

Total Carbon and Sulfur:Combustion/Infrared Detection Method 35

Total Iron:Standard Method, Potassium Dichro-

mate Titration13

Potassium Permanganate TitrationMethod

Appendix X1

Ortho-Phenanthroline, PhotometricMethod

14

Total Sulfur:Sodium Carbonate Fusion 24Combustion-Iodate Titration Method 25Unhydrated Oxides 30

1.5 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. For specificprecautionary statements, see Note 11, Note 13, Note 27, Note51, Note X2.1, and Note X5.1.

2. Referenced Documents2.1 ASTM Standards:C 50 Practice for Sampling, Inspection, Packing, and Mark-

ing of Lime and Limestone Products2C 51 Terminology Relating to Lime and Limestone (as

Used by the Industry)2C 911 Specification for Quicklime, Hydrated Lime, and

Limestone for Chemical Uses2D 1193 Specification for Reagent Water3E 29 Practice for Using Significant Digits in Test Data to

Determine Conformance with Specifications4

1 These test methods are under the jurisdiction of ASTM Committee C-7 on Limeand are the direct responsibility of Subcommittee C07.05 on Chemical Tests.

Current edition approved Aug. 10, 1999. Published September 1999. Originallypublished as C 2519T. Last previous edition C 2598.

2 Annual Book of ASTM Standards, Vol 04.01.3 Annual Book of ASTM Standards, Vol 11.01.4 Annual Book of ASTM Standards, Vol 14.02.

1

Copyright ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

E 50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of Metals5

E 70 Test Method for pH of Aqueous Solutions with theGlass Electrode6

E 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals6

E 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis7

E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method4

E 832 Specification for Laboratory Filter Papers4

3. Terminology3.1 DefinitionsUnless otherwise specified, for definitions

of terms used in these test methods refer to Terminology C 51.

4. Significance and Use4.1 These test methods provide accurate and reliable ana-

lytical procedures to determine the chemical constituents oflimestone, quicklime, and hydrated lime (Note 1). The percent-ages of specific constituents which determine a materialsquality or fitness for use are of significance depending upon thepurpose or end use of the material. Results obtained may beused in relation to specification requirements.

4.2 Because quicklime and hydrated lime quickly absorbwater and carbon dioxide from the air, precision and bias areextremely dependent upon precautions taken during samplepreparation and analysis to minimize excessive exposure toambient conditions.

NOTE 1These test methods can be applied to other calcareousmaterials if provisions are made to compensate for known interferences.

5. General Apparatus and Materials and Reagents5.1 General Apparatus and Materials:5.1.1 BalanceThe balance shall be of an analytical type

with a capacity not to exceed 200 g. It may be of conventionaldesign or it may be a constant-load, direct-reading type. It shallbe capable of reproducing weighings within 0.0002 g with anaccuracy of 60.0002 g. Rapid weighing devices that may beprovided such as a chain, damper, or heavy riders shall notincrease the basic inaccuracy by more than 0.0001 g at anyreading and with any load within the rated capacity of thebalance.

5.1.2 WeightsWeights used for analysis shall conform toClass S-1 requirements of the National Institute of Standardsand Technology as described in NIST Circular 547.8 They shallbe checked at least once a year or when questioned, andadjusted to within allowable tolerances for Class S-1 weights.All new sets of weights purchased shall have the weights of 1g and larger made of stainless steel or other corrosion-resistantalloy not requiring protective coating and shall meet thedensity requirements for Class S.

5.1.3 Glassware and Laboratory ContainersStandardvolumetric flasks, burets, pipets, dispensers, etc., shall becarefully selected precision grade or better and shall becalibrated, if necessary, to meet the requirements of eachoperation. Standard-type interchangeable ground glass or TFE-fluorocarbon joints are recommended for all volumetric glass-ware. Polyethylene containers are recommended for all aque-ous solutions of alkalies and for standard solutions where thepresence of dissolved silica or alkali from the glass would beobjectionable.

5.1.4 DesiccatorsDesiccators shall be provided with agood desiccant such as anhydrous magnesium perchlorate,activated alumina, sulfuric acid, or phosphoric anhydride.Anhydrous calcium sulfate may also be used provided it hasbeen treated with a color-changing indicator to show when thedesiccant has lost its effectiveness. Calcium chloride and silicagel are not satisfactory desiccants for this type of analysis.

5.1.5 Filter PaperFilter paper shall conform to the re-quirements of Specification E 832, Type II (quantitative). ClassE shall be used for coarse and gelatinous precipitates. Whenmedium-textured paper is required, Class F filter paper shall beused. When a retentive paper is needed, Class G shall be used.

Recommendations:Class

Filter Pore Size(microns)

Filter Speed

E 20 to 25 fast speedF 8 medium speedG 2.5 slow speed

5.1.6 CruciblesPlatinum crucibles and tight fitting lidsshould preferably be made of pure unalloyed platinum and beof 25 to 35-mL capacity. Where alloyed platinum is used forgreater stiffness or to obviate sticking of fused material tocrucible or lid, the alloyed platinum should not decrease inweight by more than 0.2 mg when heated at 1200C for 1 h.

5.1.7 Muffle FurnaceThe electric muffle furnace shouldbe capable of continuous operation up to 1000C and becapable of intermittent operation at higher temperatures ifrequired. It should have an indicating pyrometer accurate to625C.

5.2 Reagents:5.2.1 Purity of ReagentsReagent grade chemicals shall be

used in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society9where such specifications are available. Other grades may beused provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination. In addition to this, it is desirablein many cases for the analyst to ensure the accuracy of hisresults by running blanks or checking against a comparablesample of known composition.

5.2.2 Purity of WaterUnless otherwise indicated, refer-ences to water are understood to mean distilled water or otherwater of equivalent purity. Water conforming to Specification

5 Annual Book of ASTM Standards, Vol 03.05.6 Discontinued 1997; see 1997 Annual Book of ASTM Standards, Vol 03.05.7 Annual Book of ASTM Standards, Vol 15.05.8 Available from National Institute of Standards and Technology, Gaithersburg,

MD 20899.

9 Reagent 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., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,MD.

C 25

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D 1193 meets these requirements.5.2.3 Concentration of Reagents:5.2.3.1 Concentrated Acids and Ammonium Hydroxide

When acids and ammonium hydroxide are specified by nameor chemical formula only, it shall be understood that concen-trated reagents approximating the following specific gravitiesor concentrations are intended:

Acetic acid (HC2H3O2) 99.5 %Hydrochloric acid (HCl) sp gr 1.19Hydrofluoric acid (HF) 48 %Nitric acid (HNO3) sp gr 1.42Perchloric acid (HClO4) 70 %Phosphoric acid (H3PO4) 85 %Sulfuric acid (H2SO4) sp gr 1.84Ammonium hydroxide (NH4OH) sp gr 0.90

5.2.3.2 Dilute ReagentsThe concentration of dilute acidsand NH4OH except when standardized, are specified as a ratiostating the number of measured volumes of the concentratedreagent to be diluted with a given number of measured volumesof water. In conformance with international practice, new andrevised methods will use the plus designation instead of theratio (:) symbol as the specified designation of dilution; forexample, H2SO4 (5 + 95) means 5 volumes of concentratedH2SO4(sp gr 1.84) diluted with 95 volumes of water.

5.2.3.3 Standard SolutionsConcentrations of standard so-lutions shall be expressed as normalities (N) or as equivalentsin grams per millilitre of the component to be determined, forexample: 0.1 N K2Cr2O7 solution (1 mL 5 0.004 g Fe2O3).The average of at least three determinations shall be used forall standardizations. The standardization used to determine thestrength of the standard solutions is described in the text undereach of the appropriate procedures.

6. General Procedures6.1 SamplingSamples of lime and limestone for chemical

analysis shall be taken and prepared in accordance with therequirements of Methods C 50 applicable to the material to betested.

6.2 Tared or Weighed CruciblesThe tare weight of cru-cibles shall be determined by preheating the empty crucible toconstant weight at the same temperature and under the sameconditions as shall be used for the final ignition of a residue andcooling in a desiccator for the same period of time used for thecrucible containing the residue.

6.3 Constancy of Weight of Ignited ResidueTo definitelyestablish the constancy of weight of the ignited residue, theresidue and container shall be ignited at the specified tempera-ture and time, cooled to room temperature in a desiccator, andweighed. The residue and container shall then be reheated forat least 30 min at the same temperature, cooled in a desiccatorfor the same period of time, and reweighed. Additional ignitionperiods may be required until two consecutive weights do notdiffer by more than 0.2 mg, at which time it shall be consideredthat constant weight has been attained. For ignition loss, eachreheating period shall be 5 min.

6.4 Calculation:6.4.1 The calculations included in the individual procedures

sometimes assume that the exact weight specified has beenused. Accurately weighed samples which are approximatelybut not exactly equal to the weight specified may be used

provided appropriate corrections are made in the calculation.Unless otherwise stated, weights of all samples and residuesshould be recorded to the nearest 0.0001 g.

6.4.2 In all mathematical operations on a set of observedvalues, the equivalent of two more places of figures than in thesingle observed values shall be retained. For example, ifobserved values are read or determined to the nearest 0.1 mg,carry numbers to the nearest 0.001 mg in calculation.

6.5 Rounding FiguresRounding figures to the nearestsignificant place required in the report should be done after thecalculations are completed, in order to keep the final resultsfree from calculation errors. The rounding procedure shouldfollow the principle outlined in Practice E 29.

7. Performance Requirements for Test Methods7.1 Referee AnalysesThe reference test methods that ap-

pear in Sections 8 through 32, or any other test methodsqualified in accordance with 7.3, are required for refereeanalysis in those cases where conformance to the requirementsof a chemical specification are questioned. In these cases alimestone, quicklime, or hydrated lime shall not be rejected forfailure to conform to chemical requirements unless all samplepreparation and analysis of any one constituent is made entirelyby reference test methods prescribed in the appropriate sectionsof this test method or by other qualified test methods. Excep-tion can be made when specific test methods are prescribed inthe standard specification for the limestone, quicklime, orhydrated lime in question. The test methods actually used forthe analysis shall be designated.

7.1.1 When there is a question regarding acceptance, refereeanalyses shall be made in duplicate. If the two results do notagree within the permissible variation given in Table 1, thedetermination including sample preparation shall be repeatedin duplicate until the results agree within the permissiblevariation. When the results agree within the permissiblevariation, their average shall be accepted as the correct value.For the purpose of comparing results, the percentages shall becalculated to one more significant figure than reported as

TABLE 1 Maximum Permissible Variations in ResultsA

(Column 1)Constituent

(Column 2)Maximum DifferenceBetween Duplicates

(Column 3)Maximum Difference of

the Average of Duplicatesfrom SRM Certificate

ValuesB

Al as Al2O3 0.20 60.30Ca as CaO 0.20 60.30Mg as MgO 0.20 60.30C (lime and hydrated lime) 0.20 60.30C (limestone) 0.60 60.60Fe as Fe2O3 0.10 60.15Si as SiO2 0.15 60.30Mn 0.05 60.10P 0.02 60.05Sr as SrO 0.05 CS 0.03 60.05

A For demonstrating the performance of rapid test methods the SRM closest inoverall composition to the limestone shall be used (Table 2). In the case ofquicklime or hydrated lime, the SRM closest in overall composition, after heatingat 1000C for 1 h, to the product composition shall be used, except for C and Sdeterminations (Note 3).

B Interelement corrections may be used for any standardization providedimproved accuracy can be demonstrated.

C No SRM currently available.

C 25

3

indicated in the test methods. When a blank determination isspecified, one shall be made with each individual analysis orwith each group of two or more samples analyzed on the sameday for a given constituent.

7.1.2 Test results from Referee methods intended for use asa basis for product acceptance or rejection, or for manufactur-ers certification, can be used only after demonstration ofprecise and accurate analyses by meeting the requirements of7.1.3, or except when demonstrated under 7.3.2.1. Such dem-onstrations may be made concurrently with analysis of thelimestone, quicklime, or hydrated lime product being tested.The demonstration is required only for those constituents beingused as a basis for acceptance, rejection, or certification of alimestone, quicklime, or hydrated lime, but may be made forany constituent of limestone, quicklime, or hydrated limeproduct for which a standard exists. Such demonstrations mustbe made annually.

7.1.3 Demonstrations shall be made by analysis of eachconstituent of concern in a SRM limestone, quicklime, orhydrated lime (Notes 2 and 3). Duplicate samples shall be runon different days. The same test methods to be used for analysisof the limestone, quicklime, or hydrated lime being tested shallbe used for analysis of the SRM. If the duplicate results do notagree within the permissible variation given in Table 1, thedeterminations shall be repeated, following identification andcorrection of problems or errors, until a set of duplicate resultsdo agree within the permissible variation.

NOTE 2The term SRM refers to approved Standard Reference Mate-rials listed in Table 2.

NOTE 3There are no SRMs that are quicklime or hydrated lime assupplied. When analyzing a quicklime or hydrated lime the SRM incarbonate form needs to be converted to closely resemble the matrix of theproduct being tested. To accomplish this conversion, heat the chosen SRMfor 1 h at 1000C, immediately prior to analysis and protect it fromhydration or carbonation with sealed containers and desiccation duringcooling. Carbon and sulfur may be driven off during heating, rendering theconverted SRM unsuitable as a standard for carbon and sulfur determi-nations. For carbon and sulfur determinations use the appropriate SRM inits normal matrix.

7.1.4 The average of the results of acceptable duplicate

determinations for each constituent may differ from the SRMcertificate value by no more than the value shown in Column3 of Table 1. When no SRM certificate value is given, agenerally accepted accuracy standard for that constituent hasnot been identified. In such cases, only the differences betweenduplicate values as specified in 7.1.3 shall apply and notifica-tion of this exception shall be reported.

7.1.5 In questions concerning the acceptance or rejection ofa limestone, quicklime, or hydrated lime product, upon requestdata shall be made available to all parties involved demonstrat-ing that precise and accurate results were obtained with SRMsamples by the same analyst making the acceptance determi-nation.

7.2 Optional AnalysesThe alternative test methods, asopposed to reference methods, provide procedures that are, insome cases, shorter or more convenient to use for routinedetermination of some constituents (Note 4). In some instanceslonger, more complex procedures have been retained as alter-native test methods to permit comparison of results by differentprocedures or for use when unusual materials are beingexamined, or when unusual preparation for analysis is required.Results from alternative test methods may be used as a basisfor acceptance or rejection.

NOTE 4It is not intended that the use of reference test methods beconfined to referee analysis. A reference test method may be used inpreference to an alternative test method when so desired. A reference testmethod must be used where an alternative test method is not provided.

7.2.1 Duplicate analyses and blank determinations are leftto the discretion of the analyst when using the alternative testmethods. The final results should include the number ofdeterminations performed and whether or not they werecorrected for blank values.

7.3 Performance Requirements for Alternative Test Meth-ods:

7.3.1 Definition and ScopeWhen analytical data obtainedin accordance with this section is required, any test methodmay be used that meets the requirements of 7.3.2. A testmethod is considered to consist of the specific procedures,reagents, supplies, equipment, instrument, etc. selected and

TABLE 2 Approved SRM List

(SRM)Al as %Al2O3

Ca as %CaO

Mg as %MgO

Fe as %Fe2O3

Si as %SiO2 % Mn % P

Sr as %SrO % S

Ti as %TiO2

K as %K2O

Na as%

Na2O % L.O.I.ECRM-752-1A 0.12 55.4 0.15 0.045 0.70 0.008 NCB 0.019 0.007 0.009 0.02 NC 43.4IPT 35 0.24 53.8 0.70 0.14 1.98 0.009 0.003 0.04 NC 0.013 0.10 0.004 43.0IPT 44 0.33 50.5 2.93 0.30 2.69 0.012 0.006 0.04 NC 0.019 0.12 0.002 42.9IRSID DO 1-1C 0.55 52.69 0.60 1.04 1.99 0.022 0.022 NC 0.040 0.030 NC NC NCNIST 1C 1.30 50.3 0.42 0.55 6.84 0.019 0.017 0.030 NC 0.07 0.28 0.020 39.9NIST 88B 0.34 29.95 21.0 0.277 1.13 0.012 0.002 0.0076 NC (0.016)D 0.103 0.029 (46.98)BCS 368 0.17 30.8 20.9 0.23 0.92 0.05 NC 0.0089 NC

used in a consistent manner by a specific laboratory.7.3.1.1 If more than one instrument is used for the same

analysis, use of each instrument shall constitute a separate testmethod and each must be qualified separately.

7.3.2 Qualification of a Test MethodPrior to use each testmethod (see 7.3.1) must be qualified for each material that willbe tested. Qualification data or, if applicable, requalificationdata shall be made available.

7.3.2.1 Using the test method chosen, make single determi-nations for each constituent under consideration on the SRMwhich in overall composition most closely resembles thelimestone, quicklime, or hydrated lime to be tested (Note 2).Complete two rounds of tests on nonconsecutive days repeat-ing all steps of sample preparations. Calculate the differencesbetween values and the averages of values from the two roundsof tests. Blank determinations are not required, if it has beendetermined that blank values do not affect the validity of thedata. Blank or interference-corrected data must be so desig-nated.

7.3.2.2 The differences between duplicates obtained for anysingle constituent shall not exceed the limits shown in Column2 of Table 1.

7.3.2.3 For each constituent the average of the duplicatesobtained shall be compared to the SRM Certificate value andshall not differ from the certified value by more than the valuein Column 3 of Table 1. The qualification testing shall beconducted with newly prepared specimens.

7.3.2.4 The standardization, if applicable, used for qualifi-cation and analysis of each constituent shall be determined byvalid curve-fitting procedures (Note 5). Restandardization shallbe performed as frequently as required to ensure that theaccuracy and precision in Table 1 are maintained.

NOTE 5An actual drawing of a curve is not required, if such a curveis not needed for the method in use. A point-to-point, saw-tooth curve thatis artificially made to fit a set of data points does not constitute a validcurve-fitting procedure.

7.3.3 Partial ResultsTest methods that provide acceptableresults for some constituents, but not for others, may be usedonly for those components for which acceptable results areobtained.

7.3.4 Report of ResultsChemical analyses obtained byqualified alternative test methods shall be indicated as havingbeen obtained by alternative methods and the type of testmethod used shall be designated.

7.3.5 Rejection of MaterialSee 7.1 and 7.2.7.3.6 Requalification of a Test Method:7.3.6.1 Requalification of a test method, as defined in 7.3.2,

shall be required annually.7.3.6.2 Requalification also shall be required upon receipt of

substantial evidence that the test method may not be providingdata in accordance with Table 1. Such requalification may belimited to those constituents indicated to be in error and shallbe carried out prior to further use of the method for analysis ofthose constituents.

7.3.6.3 Substantial evidence that a test method may not beproviding data in accordance with Table 1 shall be consideredto have been received when a laboratory is informed thatanalysis of the same material by Reference Test Methods run in

accordance with 7.1.1, a certified value of an approved SRM,or an accepted value of a known secondary standard differsfrom the value obtained by the test method in question by morethan twice the value of Column 2 of Table 1 for one or moreconstituents. When indirect test methods are involved, as whena value is obtained by difference, corrections shall be made forminor constituents in order to put the analyses on a comparablebasis prior to determining the differences (Note 6). For anyconstituents affected, a test method also shall be requalifiedafter any substantial repair or replacement of one or morecritical components of an instrument essential to the testmethod.

NOTE 6Instrumental analyses can usually detect only the elementsought. Therefore, to avoid controversy, the actual procedure used for theelemental analysis should be noted when differences with referenceprocedures exist. For example, Combined Oxides of Iron and Aluminumby Wet Test should be compared to the sum of Fe2O3 and Al2O3 obtainedinstrumentally.

7.3.6.4 If an instrument or piece of equipment is replacedeven by one of identical make and model, or is significantlymodified, a previously qualified test method using such new ormodified instrument or equipment shall be considered a newmethod and must be qualified in accordance with 7.3.2.

7.4 Precision and BiasDifferent analytical test methodsare subject to individual limits of precision and bias. It is theresponsibility of the user to demonstrate that the test methodsused at least meet the requirements shown in Table 1.

8. Insoluble Matter Including Silicon Dioxide (StandardMethod)

8.1 ScopeThis test method is based on a double evapora-tion to dryness of the hydrochloric acid solution of thelimestone or lime sample to convert silicon dioxide (SiO2) tothe insoluble form. The acid-insoluble residue of a typicallimestone consists of free silica and a mixture of minerals suchas clay, mica, feldspar, tourmaline, barytes, garnet, zircon,rutile, etc.

8.2 Summary of Test MethodAfter dissolution in hydro-chloric acid, the silica is dehydrated by a double evaporation todryness. After each dehydration, the dry salts are redissolvedwith dilute hydrochloric acid, the solution is filtered, and thesiliceous residue and other insoluble matter separated. The twopapers containing the residues are combined, ignited, andweighed.

8.3 Procedure:8.3.1 Weigh 0.5 g of quicklime or hydrated lime, or 1.0 g of

limestone ground to pass a No. 50 (250-m) sieve (Note 7). Ifthe sample is a limestone or hydrated lime, ignite in a coveredplatinum crucible in an electric muffle (Note 8) at 950C for 15min or longer to effect complete decomposition. Transfer to anevaporating dish, preferably of platinum (Note 9), containingabout 10 mL of water, mix to a thin slurry, add 5 to 10 mL ofHCl, and digest with the aid of gentle heat and agitation untilsolution is complete (Note 10).

NOTE 7Due to the rapidity with which quicklime and hydrated limeabsorb water and carbon dioxide from the air, samples must be protectedin tightly stoppered containers at all times. Samples for analysis are to beweighed quickly and the sample container re-stoppered immediately afterthe sample has been removed.

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NOTE 8Ignition of the sample in an electric muffle is far superior toflame ignition. However, if an electric muffle is not available, flameignition and the blast lamp may be used.

NOTE 9If a platinum dish is not available, porcelain may be used. Aglass container positively must not be used.

NOTE 10Alternatively, the loss on ignition (LOI) can be determinedfirst, using 0.5 g of sample. The insoluble matter including silicon dioxidecan then be assayed using the ignited product that remains in the LOIcrucible.

8.3.2 Evaporate the solution to dryness on a steam bath.When dry or nearly so, cover the dish and place it in an air bathor drying oven or on a metal triangle resting on a hot plate.Heat for 1 h at 100C, remove the dish from the heat, and allowthe dish and contents to cool slightly.

8.3.3 Drench the cooled mass with 20 mL (1 + 1) HCl andplace on the water bath for 10 min. Filter the mixturecontaining the insoluble residue through a retentive filter ofsuitable size. Wash filter thoroughly with warm, diluted(5 + 95) HCl and then twice with hot water. Reserve the paperand residue.

8.3.4 Evaporate the filtrate to dryness, dehydrate and extractthe residue with HCl as before, but this time heat the acidifiedsolution for 1 to 2 min. Filter through a second and smallerpiece of retentive filter paper and wash as before. Retain thefiltrate for iron, aluminum, calcium, and magnesium determi-nations; combine the two wet papers containing the separatedresidues and transfer to a weighed platinum crucible.

8.3.5 Char carefully without allowing the paper to inflame,and then ignite at 1000C for 30 min in an electric mufflefurnace (Note 8). Cool in a desiccator and weigh. The increasein weight represents the insoluble matter including SiO2.

8.4 CalculationCalculate the percentage of insoluble mat-ter including silicon dioxide to the nearest 0.01 % as follows:

Insoluble matter including SiO25~A/B!3100 (1)

where:A 5 mass of ignited residue, g, andB 5 original mass of sample, g.

8.5 Precision and BiasThis test method was originallyapproved for publication before the inclusion of precision andbias statements within standards was mandated. The user iscautioned to verify by the use of reference materials, ifavailable, that the precision and bias of this test method areadequate for the contemplated use.

9. Insoluble Matter Including Silicon Dioxide (OptionalPerchloric Acid Method)

9.1 ScopeIn this test method the insoluble matter includ-ing silicon dioxide is determined gravimetrically as in thestandard method except that perchloric acid is used to dehy-drate the silica. The procedure is more rapid than in thestandard method because only a single dehydration is neces-sary. Fuming perchloric acid is a very powerful dehydratingagent, and silicic acid can usually be completely converted tothe insoluble silicon dioxide in less than 20 min. This testmethod has been determined by other agencies such as theAssociation of Official Agricultural Chemists (AOAC) to becomparable to the standard hydrochloric acid method.

9.2 Summary of Test MethodThe sample is decomposedwithout prior ignition by a mixture of nitric (HNO3) and

perchloric (HClO4) acids and evaporated to fumes of HClO4.The fuming perchloric acid is refluxed at this temperature fora short period of time to completely dehydrate the silica. Theresidue of silica and insoluble matter is filtered and washed freeof acids and salts. The filter paper containing the residue isburned off, the resultant ash is ignited at high temperature untilthe ash is white, and then is weighed.

9.3 Procedure:NOTE 11Precaution: Perchloric acid (HClO4) is an extremely reac-

tive liquid. When using HClO4, there are precautions to be followedwhich, if unheeded, may lead to serious explosions. Contact of the hotconcentrated acid with organic matter must be absolutely avoided. Anyorganic matter in the sample must first be destroyed by the addition ofnitric acid (HNO3) to the sample prior to fuming with HClO4. Allevaporations involving HClO4 must be done in a well-ventilated hoodmade of nonporous and inorganic material, preferably Type 316L stainlesssteel. Facilities should be provided for washdown procedures that shouldbe performed regularly and thoroughly. These precautions on perchloricacid use are fully discussed in Practices E 50.

9.3.1 Weigh 0.5 g of quicklime or hydrated lime, or 1 g oflimestone ground to pass a No. 50 (250-m) sieve. Transfer thesample to a 250-mL beaker, wet carefully with a few millilitresof water, and dissolve cautiously with 10 mL of concentratednitric acid. Add 20 mL of perchloric acid and boil until densewhite fumes appear. If the solution darkens at this point, addseveral millilitres of HNO3 until the solution clears. Heat againto fumes.

9.3.2 With the beaker covered, boil gently for 15 min tocompletely dehydrate the silica. Never allow contents tobecome solid or go to dryness, otherwise the separation ofsilica will be incomplete. If this happens, add more HClO4 andrepeat the dehydration.

9.3.3 Cool, add 50 mL of water, heat to boiling, and filterimmediately using medium textured paper. Wash paper andresidue thoroughly (at least 15 times) with hot water. Test withpH paper until washings are free of acid (Note 12). Reserve thefiltrate for iron, aluminum, calcium, and magnesium determi-nations.

NOTE 12The filter paper and silica residue must be washed free ofperchlorate salts to prevent small explosions from occurring in thecrucible when the filter paper is charred and ignited.

9.3.4 Place the filter paper and contents in a weighedplatinum or porcelain crucible and heat gently with a low flameuntil paper chars without inflaming, or alternatively char in anelectric muffle at 300 to 400C. Slowly raise the temperatureuntil the carbon has been burned and the ash is white. Finally,ignite at 1000C for 30 min. Cool in a desiccator and weigh asinsoluble matter including SiO2.

9.4 CalculationCalculate the percentage of insoluble mat-ter including silicon dioxide to the nearest 0.01 % as follows:

Insoluble matter including SiO2, %5~A/B!3100 (2)

where:A 5 mass of ignited residue, g, andB 5 original mass of sample, g.

9.5 Precision and Bias:9.5.1 Four laboratories cooperated in testing on four lime-

stone samples and three laboratories cooperated in testing onan additional eight limestone samples thereby obtaining the

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precision data summarized in Table 3.9.5.2 The user is cautioned to verify by the use of reference

materials, if available, that the bias of this test method isadequate for the contemplated use.

10. Silicon Dioxide10.1 ScopeFor control purposes or routine determina-

tions, a separate analysis of SiO2 may not be necessary.However, for certain applications in process industries, theamount of silica derived from the lime or limestone could beimportant. To satisfy situations such as this, silicon dioxidemay be determined by volatilizing the SiO2 from the insolubleresidue with hydrofluoric acid and the percent SiO2 determinedby the difference in mass obtained.

10.2 Procedure:10.2.1 To the ignited residue in the platinum crucible (8.3.5

or 9.3.4), add 5 mL of water, 5 mL of hydrofluoric acid (HF),and 1 or 2 drops of H2SO4.

NOTE 13Precaution: All acids should be handled with care, but extraprecaution is required with hydrofluoric acid. This is a very dangerousacid, harmful to eyes and skin; rubber gloves and goggles should be wornwhen using this acid. It does its work silently and leaves a festering sorethat is slow to heal. Any acid that touches the skin should be immediatelywashed off with copious quantities of water. A physician should benotified immediately if any acid is sprayed into the eyes or if prolongedcontact with the skin occurs.

10.2.2 Evaporate to dryness on a hot plate and heat in anelectric muffle at 1000C (Note 8) for 2 or 3 min. Cool in adesiccator and weigh. The difference between this mass and themass of insoluble matter including silicon dioxide is the massof SiO2.

10.3 CalculationCalculate the percent of silicon dioxideto the nearest 0.01 % as follows:

SiO2, % 5 ~@A2B!/C#3100 (3)

where:A 5 mass of ignited residue, g (insoluble matter including

SiO2),B 5 mass of ignited residue less SiO2, g, andC 5 original mass of sample, g.

10.4 Precision and Bias:10.4.1 Three laboratories cooperated in testing on four

limestone samples and two laboratories cooperated in testing

on an additional eight limestone samples thereby obtaining theprecision data summarized in Table 3.

10.4.2 The user is cautioned to verify by the use of referencematerials, if available, that the bias of this test method isadequate for the contemplated use.

11. Insoluble Matter11.1 ScopeThe difference between the mass of insoluble

matter (including silicon dioxide) and silicon dioxide repre-sents the mass of insoluble matter other than silicon dioxide.The insoluble matter contains the remnants of any clay,siliceous minerals, or other refractory material present inlimestone. The elemental components are mainly iron andaluminum which should be removed and added to the mainfiltrate from the SiO2 separation. If the insoluble matterincluding silica is reported as such and no hydrofluoric acidtreatment is indicated, then there is no need to make a recoveryof the metals and the insoluble residue may be discarded.

11.2 ProcedureThe insoluble matter left in the crucibleafter the silica is volatilized with HF may be dissolved byfusing the residue with 2 to 3 g of sodium carbonate (Na2CO3)(Note 14). Cool the melt and dissolve it in diluted HCl. Add thesolution to the filtrate from the dehydration and separation ofinsoluble matter including silicon dioxide (8.3.4 or 9.3.3).

NOTE 14Fusion with pyrosulfate is to be avoided because this willintroduce undesirable sulfates into the solution.

11.3 An alternative fusion can also be made using eitherlithium metaborate or lithium tetraborate as opposed to usingsodium carbonate.

11.4 CalculationCalculate the percentage of insolublematter other than silicon dioxide to the nearest 0.01 % asfollows:

Insoluble matter other than SiO2, %5A2B (4)

where:A 5 insoluble matter including SiO2, %, andB 5 SiO2, %.

11.5 Precision and Bias:11.5.1 Three laboratories cooperated in testing on four

limestone samples and two laboratories cooperated in testingon an additional eight limestone samples thereby obtaining theprecision data summarized in Table 3.

TABLE 3 Precision Summary of Classical Test Methods

Section Test MethodAverage,A% Found

Range,A %Found

Repeatability(R1, E 173)

Reproducibility(R2, E 173)

8 Insol + SiO2 . . . . . . . . . . . .(Standard)

9 Insol + SiO2 1.405 0.096.40 0.184 0.351(Optional)

10 SiO2 1.177 0.035.36 0.128 0.14611 Insoluble Matter 0.242 0.020.93 0.169 0.20412 Combined Oxides 0.459 0.221.21 0.181 0.28213 Fe2O3 0.180 0.050.36 0.064 0.18315 Al2O3 0.268 0.100.88 0.165 0.22316 CaO (Gravimetric) 54.46 53.455.1 0.558 1.02017 CaO (Volumetric) 30.57 30.430.7 0.371 1.13217 CaO (Volumetric) 53.82 49.655.3 0.187 0.29818 MgO (Gravimetric) 0.817 0.192.28 0.158 0.21018 MgO (Gravimetric) 21.34 21.121.5 0.652 1.71619 Loss on Ignition 43.73 43.643.9 0.158 0.463

A Average and range of the limestones tested.

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11.5.2 The user is cautioned to verify by the use of referencematerials, if available, that the bias of this test method isadequate for the contemplated use.

12. Combined Oxides (Iron, Aluminum, Phosphorus,Titanium, Manganese)

12.1 ScopeThe combined oxides describe a group ofmetals that form precipitates with ammonium hydroxide whichmay then be ignited to their respective oxides. Historically, ithas been the practice to report the combined oxides present inlimestone samples as a group because it was not always easy ordesirable to determine each metal oxide separately. The groupof metal oxides consists primarily of the oxides of iron andaluminum, with minor amounts of titanium dioxide (TiO2),phosphorus pentoxide (P2O5), and manganese oxide (Mn3O4)also present. Where separate determinations are preferred, thecombined oxides are usually weighed first, iron oxide is thenassayed separately, and aluminum oxide is finally determinedby calculating the difference between the percent combinedoxides and the percent Fe2O3. The other metal oxides aregenerally assumed to be present in trace amounts and are oftendisregarded. When necessary, these metals may be analyzedseparately and appropriate corrections made in the Al2O3analysis.

12.2 Summary of Test MethodIn this test method, alumi-num, iron, titanium, and phosphorus are precipitated from thefiltrate after SiO2 removal, by means of ammonium hydroxide.With care, little if any manganese will be precipitated. Theprecipitate is ignited and weighed as the combined metaloxides.

12.3 Special Solution:12.3.1 Methyl Red Solution (0.2 %)Dissolve 2 g of me-

thyl red indicator