ASTM C471M-01(2006)e1

Standard Test Methods for Chemical Analysis of Gypsum and Gypsum Products [Metric]

SCOPE
1.1 These test methods cover the chemical analysis of gypsum and gypsum products, including gypsum ready-mixed plaster, gypsum wood-fibered plaster and gypsum concrete.
1.2 The test methods appear in the following order:
1.3 The text of this standard references notes and footnotes that provide explanatory material. These notes and footnotes (excluding those in tables and figures) shall not be considered as requirements of the standard.
1.4 The values stated in SI units are to be regarded as the standard.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Nov-2006
• ICS: 91.100.10 - Cement. Gypsum. Lime. Mortar
• Technical Committee: C11 - Gypsum and Related Building Materials and Systems
• Drafting Committee: C11.01 - Specifications and Test Methods for Gypsum Products

Relations

• Replaces: ASTM C471M-01 - Standard Test Methods for Chemical Analysis of Gypsum and Gypsum Products [Metric]
• Effective Date: 01-Dec-2006
• Replaced By: ASTM C471M-01(2012) - Standard Test Methods for Chemical Analysis of Gypsum and Gypsum Products (Metric)
• Effective Date: 01-Jun-2012
• Referred By: ASTM C563-20 - Standard Guide for Approximation of Optimum SO<inf>3</inf> in Hydraulic Cement
• Effective Date: 01-Dec-2006
• Referred By: ASTM C22/C22M-00(2021) - Standard Specification for Gypsum
• Effective Date: 01-Dec-2006
• Referred By: ASTM D34-08(2023) - Standard Guide for Chemical Analysis of White Pigments
• Effective Date: 01-Dec-2006
• Referred By: ASTM D8155-17 - Standard Practice for Shake Extraction of Solid Mining and Metallurgical Processing Waste with Water
• Effective Date: 01-Dec-2006
• Referred By: ASTM C28/C28M-10(2020) - Standard Specification for Gypsum Plasters
• Effective Date: 01-Dec-2006
• Referred By: ASTM D3987-12(2020) - Standard Practice for Shake Extraction of Solid Waste with Water
• Effective Date: 01-Dec-2006
• Referred By: ASTM E3355-23 - Standard Guide for Characterization of Coal Combustion Products (CCPs) in Storage Area(s) for Beneficial Use
• Effective Date: 01-Dec-2006
• Referred By: ASTM C59/C59M-00(2020) - Standard Specification for Gypsum Casting Plaster and Gypsum Molding Plaster
• Effective Date: 01-Dec-2006
• Referred By: ASTM C61/C61M-00(2020) - Standard Specification for Gypsum Keene's Cement
• Effective Date: 01-Dec-2006
• Referred By: ASTM C1396/C1396M-17 - Standard Specification for Gypsum Board
• Effective Date: 01-Dec-2006
• Referred By: ASTM C452-21 - Standard Test Method for Potential Expansion of Portland-Cement Mortars Exposed to Sulfate
• Effective Date: 01-Dec-2006
• Referred By: ASTM C35-01(2019) - Standard Specification for Inorganic Aggregates for Use in Gypsum Plaster
• Effective Date: 01-Dec-2006

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation:C471M–01 (Reapproved 2006)
Standard Test Methods for
Chemical Analysis of Gypsum and Gypsum Products
(Metric)
This standard is issued under the fixed designation C471M; the number immediately following the designation indicates the year of
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Note 1 and certain footnotes were removed editorially to conform to ASTM Form and Style requirements for sole
source of supply January 2007.
1. Scope Materials and Systems
C22/C22M Specification for Gypsum
1.1 These test methods cover the chemical analysis of
C28/C28M Specification for Gypsum Plasters
gypsum and gypsum products, including gypsum ready-mixed
C59 Specification for Gypsum Casting Plaster and Gypsum
plaster, gypsum wood-fibered plaster and gypsum concrete.
Molding Plaster
1.2 The test methods appear in the following order:
C61 Specification for Gypsum Keene’s Cement
Sections
C317/C317M Specification for Gypsum Concrete
Alternative Procedure for Analysis for Calcium Sulfate by Ammonium
Acetate Method 17-22
C842 Specification for Application of Interior Gypsum
Alternative Procedure for Analysis for Sodium Chloride by the Coulo-
Plaster
metric Method 23-29
D1193 Specification for Reagent Water
Complete Procedure 5-16
Determination of Sand in Set Plaster 30-36
D1428 Methods of Test for Sodium and Potassium in Water
Optional Procedure for Analysis for Sodium by Flame Photometry 47-54
and Water-Formed Deposits by Flame Photometry
Optional Procedure for Analysis for Sodium by the Atomic Absorp-
tion Method 40-46 D2013 Practice for Preparing Coal Samples for Analysis
Preparation of Sample 4
E11 SpecificationforWovenWireTestSieveClothandTest
Wood-Fiber Content in Wood-Fiber Gypsum Plaster 37-39
Sieves
1.3 The text of this standard references notes and footnotes
3. Terminology
that provide explanatory material. These notes and footnotes
(excluding those in tables and figures) shall not be considered
3.1 Definitions—Definitions shall be in accordance with
as requirements of the standard.
Terminology C11.
1.4 The values stated in SI units are to be regarded as the 3.2 Definitions of Terms Specific to This Standard:
standard.
3.2.1 sample as received, n—a representative portion of raw
1.5 This standard does not purport to address all of the gypsum or gypsum product in the state received by the testing
safety concerns, if any, associated with its use. It is the
laboratory, including aggregates, impurities and water content.
responsibility of the user of this standard to establish appro- 3.2.2 dried sample, n—a sample devoid of free water.
priate safety and health practices and determine the applica-
3.2.3 riffle, n—a hand feed sample divider device that
bility of regulatory limitations prior to use. divides the sample into parts of approximately the same
weight. (D2013)
2. Referenced Documents
4. Preparation of Sample
2.1 ASTM Standards:
C11 TerminologyRelatingtoGypsumandRelatedBuilding
4.1 General Procedures—Details of sample preparation
will vary according to the type of material being tested.
4.1.1 Sample As Received—Use a sufficient amount of
1 sample such that, after sieving, not less than 50 g of sample
These test methods are under the jurisdiction of ASTM Committee C11 on
Gypsum and Related Building Materials and Systems and are the direct responsi- will remain for testing. Weigh the entire sample immediately
bility of Subcommittee C11.01 on Specifications and Test Methods for Gypsum
after opening the container in which the material was received.
Products.
This will become the weight of the sample as received.
Current edition approved Dec. 1, 2006. Published January 2007. Originally
4.1.2 Drying—Dry the sample in accordance with Section
approved in 1961. Last previous edition approved in 2001 as C471 – 01. DOI:
10.1520/C0471M-01R06E01.
7. This will be the weight of the dried sample.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
C471M–01 (2006)
4.1.3 Crushing and Grinding—Crush and grind the sample COMPLETE PROCEDURE
by hand with a mortar and pestle or by mechanical crushing
5. Apparatus
and grinding equipment to pass a 250-µm (No. 60) sieve. Take
care,particularlywithmechanicalequipment,nottoexposethe 5.1 Analytical Balance—Capable of weighing the weighing
sample to temperatures of more than 52 °C. Clean the bottles, lids and samples.
5.2 Balance—Capable of weighing not less than 100 g at a
equipment thoroughly between samples. Thoroughly remix the
ground sample and store it in an airtight container to avoid precision of 0.001 g.
5.3 Drying Oven—A mechanical convection oven set at 45
contamination.
6 3 °C.
4.1.4 Rehydrating—Thoroughly blend and rehydrate
5.4 Desiccator—Capable of being tightly sealed and con-
samples which contain calcium sulfate in forms other than
taining calcium chloride or equivalent desiccant.
CaSO ·2H O and natural anhydrite. Place the sample in
4 2
5.5 Calcining Oven or Furnace—Capable of achieving and
distilled water and keep it wet for not less than 48 h. Dry the
maintaining temperatures to not less than 1000 °C.
hydrated sample in an oven at 45 6 3 °C to constant weight
5.6 Weighing Bottles—Borosilicate glass or ceramic con-
and recrush or grind it in accordance with 4.1.3.
tainers with tightly sealable lids.
4.1.5 Sample Reduction—Thoroughly mix and reduce large
5.7 Hot Plate—A controllable hot plate capable of heating
samples as required by quartering or by the use of a riffle to
casseroles to approximately 120 °C.
obtain a specimen of approximately 50 g.
5.8 PorcelainCasseroles—Withacapacityof50to100mL.
4.2 Gypsum (C22/C22M)—Gypsum samples will be re-
5.9 Filtering Funnels.
ceived in the form of rocks, powder or both. If necessary crush
5.10 Filter Paper.
andreducetheentiredriedsampleinaccordancewith4.1.3and
5.11 Porcelain Crucibles.
4.1.5.
5.12 Mortar and Pestle.
4.3 Gypsum Plaster,(C28/C28M). 5.13 Mechanical Jaw Crusher—Capable of crushing gyp-
sum rocks up to 50 mm diameter.
4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFi-
5.14 Mechanical Grinder—Burr mill or equivalent capable
beredPlaster—Screenthedriedsamplethrougha150-µm(No.
of grinding the granular output of the jaw crusher specified in
100) sieve and discard the residue retained on the sieve.
5.13.
Reweigh the remaining sample and calculate the percentage of
the dried sample. Reduce the sample in accordance with 4.1.5.
6. Reagents
Thoroughly blend and rehydrate the specimen in accordance
6.1 Purity of Reagents—Use reagent grade chemicals in all
with 4.1.4.
tests. Unless otherwise indicated, use reagents that conform to
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster—
the specifications of the Committee on Analytical Reagents of
Reduce the dried sample in accordance with 4.1.5. Thoroughly
the American Chemical Society, where such specifications are
blend and rehydrate the specimen in accordance with 4.1.4.
available. If it is necessary to use other grades first ascertain
4.4 Gypsum Casting and Molding Plaster , (C59)—Reduce
that the reagent is of sufficiently high purity so that its use will
the dried sample in accordance with 4.1.5. Thoroughly blend
not lessen the accuracy of the determination.
and rehydrate the specimen in accordance with 4.1.4.
6.1.1 Ammonium Chloride (NH Cl).
4.5 Gypsum Keene’s Cement, (C61)—Reduce the dried
6.1.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated
sample in accordance with 4.1.5. Blend in no more than 1 %
ammonium hydroxide (NH OH).
molding plaster or K SO and rehydrate the specimen in
2 4
6.1.3 Ammonium Nitrate (25 g/L)—Dissolve 25 g of am-
accordance with 4.1.4.
monium nitrate (NH NO ) in water and dilute to 1 L.
4 3
4.6 Gypsum Concrete, (C317/C317M)—Screen the dried
6.1.4 Ammonium Oxalate ((NH ) C O ).
4 2 2 4
sample through a 150-µm (No. 100) sieve and discard the
6.1.5 Barium Chloride (100 g/L)—Dissolve 100 g of
residue retained on the sieve. Reweigh the remaining sample
barium chloride (BaCl ·2H O) in water and dilute to 1 L.
2 2
and calculate the percentage of the dried sample. Reduce the
6.1.6 Calcium Chloride (CaCl )—Anhydrous Calcium
sample in accordance with 4.1.5. Thoroughly blend and rehy-
Chloride with a combined water of not more than 5 %.
drate the specimen in accordance with 4.1.4. 6.1.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl).
4.7 Gypsum Board—Cut or break the dried sample into
6.1.8 Hydrochloric Acid (1 + 4)—Mix 1 volume of HCl (sp
small pieces. Using a mortar and pestle, strike the pieces of the
gr 1.19) with 4 volumes of water.
sampletoloosenthepaperface.Removethepiecesofpaperby
6.1.9 Hydrochloric Acid (1 + 5)—Mix 1 volume of HCl (sp
hand as they are separated from the core of the gypsum board.
gr 1.19) with 5 volumes of water.
Carefully scrape any remaining powder from the paper. When
all the paper has been removed from the pieces of the sample,
reduce the sample in accordance with 4.1.5. Thoroughly blend
Reagent Chemicals, American Chemical Society Specifications , American
and rehydrate the specimen in accordance with 4.1.4.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Detailed requirements for this sieve are given in Specification E11. MD.
´1
C471M–01 (2006)
6.1.10 Nitric Acid (sp gr 1.42)—Concentrated nitric acid ture range as gypsum, will cause high results. When the
(HNO ). maximum temperature is exceeded, some carbonates undergo
6.1.11 Potassium Chromate Solution (100 g/L)—Dissolve 5 decomposition, which will result in high results.
gofpotassiumchromate(K CrO )in50mLofwater,mix,add 8.3 Procedure:
2 4
10 drops of 0.05 N silver nitrate (AgNO ) solution, allow to 8.3.1 For each sample, place three weighing bottles with
stand for 5 min, and filter. lids in the preheated calcining oven or furnace and heat for 2
6.1.12 Potassium Permanganate (5.6339 g/L)—Dissolve h at 215 to 230 °C. Place in the desiccator and allow to cool to
5.6339 g of potassium permanganate (KMnO ) in water and room temperature. Weigh the bottles and lids to the nearest
dilute to 1 L. 0.0001 g and record the tare weights.
6.1.13 Silver Nitrate, Standard Solution (0.05 N)—Prepare 8.3.2 Weigh out three specimens of approximately 1 g each
and standardize a 0.05 N silver nitrate (AgNO ) solution. of the sample as prepared in Section 4 and dried in Section 7
6.1.14 Sodium Ammonium Phosphate—(NaNH HPO ). to a precision of 0.0001 g in the previously tared weighing
4 4
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric bottles and record the total weight with lids.
acid (H SO ). 8.3.3 Place the specimens in the calcining oven with the lids
2 4
6.1.16 Sulfuric Acid (1 + 6)—Carefully mix 1 volume of placed loosely on each bottle or crucible for2hor until
H SO (sp gr 1.84) with 6 volumes of water. constant weight has been obtained.
2 4
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO (sp gr 8.3.4 Place the lids tightly on the weighing bottles, remove
1.42) with 200 mL of water. from the oven, and place in the desiccator to cool to room
6.1.18 Phenolphthalein Indicator Solution— Dissolve 0.25 temperature.
g of phenolphthalein in 30 mLof methanol and dilute to 50 mL 8.3.5 Weigh each specimen to a precision of 0.0001 g and
with water. record the weights.
6.1.19 Sodium Hydroxide Solution (0.1 N)—Dissolve1gof 8.3.6 Retain the residues for carbon dioxide analysis.
sodium hydroxide (NaOH) in 250 mL of water. 8.4 Calculation and Report—Calculate and report the aver-
6.1.20 Water—Reagent water shall be in accordance with age loss in weight of the three specimens as a percentage of the
Specification D1193, type II. Specification D1193 gives the sample as received or of the dried sample, as required, to the
following values for type II grade water. nearest 0.001 g and record the tare weights.
8.5 Precision and Bias—Neither the precision nor the bias
Electrical conductivity, max, µS/cm at 298 K (25-C) 1.0
Electrical resistivity, min, MV·cm at 298 K (25-C) 1.0
for the combined water analysis has been determined.
Total organic carbon (TOC), max, µg/L 50.0
Sodium, max, µg/L 5.0
9. Carbon Dioxide
Chlorides max, µg/L 5.0
Total silica, max, µg/L 5.0
9.1 Summary of Test Method—The sample is decomposed
with HCl and the liberated CO is passed through a series of
scrubbers to remove water and sulfides. The CO is absorbed
7. Free Water
with Ascarite, a special sodium hydroxide absorbent, and the
7.1 Significance and Use—The free water analysis deter-
gain in weight of the absorption tube is determined and
mines the amount of free water contained in the sample as
calculated as percent CO .
opposed to chemically combined water, and prepares the
9.2 Significance and Use—The carbon dioxide analysis is
sample for further analysis.
useful in estimating carbonates and organic carbon for chemi-
7.2 Procedure:
cal balance.
7.2.1 Weigh a sample of the material as received of not less
9.3 Special Reagents:
than 50 g to a precision of 0.001 g and spread it out in a thin
9.3.1 Magnesium Perchlorate Desiccant—for drying.
layer in a suitable vessel. Place in an oven and dry at 45 6 3
9.3.2 Sodium Hydroxide Absorbent—a coarse sodium hy-
°C for 2 h, then cool in a desiccator and weigh again. The loss
droxide coated silica.
of weight corresponds to the free water.
9.4 Special Apparatus—The apparatus illustrated in Fig. 1
7.2.2 Retain the sample in a sealed container or in the
consists of the following:
desiccator for further analysis.
9.4.1 Purifying Jar A, Fleming, containing sulfuric acid.
7.3 Calculation and Report—Calculate and report loss in
9.4.2 Drying Tube B, U-shaped with side arms and glass-
weight as a percentage of the sample as received or of the dried
stoppers. Side arms are shaped to hold rubber tubing. Contains
sample as required.
Anhydrone on left side and Ascarite on right side.
7.4 Precision and Bias—Neither the precision nor the bias
9.4.3 Erlenmeyer Flask C, 250 mL, 24/20 ground-glass
for the free water analysis has been determined.
joint.
...