ASTM C471M-01(2012)
(Test Method)Standard Test Methods for Chemical Analysis of Gypsum and Gypsum Products (Metric)
Standard Test Methods for Chemical Analysis of Gypsum and Gypsum Products (Metric)
SIGNIFICANCE AND USE
This test method covers the determination of calcium sulfate in gypsum and gypsum products by extraction with ammonium acetate solution.
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:
Sections Alternative Procedure for Analysis for Calcium Sulfate by Ammonium Acetate Method
17-22 Alternative Procedure for Analysis for Sodium Chloride by the Coulometric Method
23-29 Complete Procedure 5-16 Determination of Sand in Set Plaster30-36 Optional Procedure for Analysis for Sodium by Flame Photometry47-54 Optional Procedure for Analysis for Sodium by the Atomic Absorption Method
40-46 Preparation of Sample4 Wood-Fiber Content in Wood-Fiber Gypsum Plaster37-39
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.
1.5 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.
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Designation: C471M − 01(Reapproved 2012)
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.
1. Scope C22/C22M Specification for Gypsum
C28/C28M Specification for Gypsum Plasters
1.1 These test methods cover the chemical analysis of
C59 Specification for Gypsum Casting Plaster and Gypsum
gypsum and gypsum products, including gypsum ready-mixed
Molding Plaster
plaster, gypsum wood-fibered plaster and gypsum concrete.
C61 Specification for Gypsum Keene’s Cement
1.2 The test methods appear in the following order:
C317/C317M Specification for Gypsum Concrete
Sections
C842 Specification forApplication of Interior Gypsum Plas-
Alternative Procedure for Analysis for Calcium Sulfate by Ammonium Acetate
ter
Method 17-22
D1193 Specification for Reagent Water
Alternative Procedure for Analysis for Sodium Chloride by the Coulometric
Method 23-29
D1428 Test Method for Test for Sodium and Potassium In
Complete Procedure 5-16
Water and Water-Formed Deposits by Flame Photometry
Determination of Sand in Set Plaster 30-36
(Withdrawn 1989)
Optional Procedure for Analysis for Sodium by Flame Photometry 47-54
Optional Procedure for Analysis for Sodium by the Atomic Absorption Method
D2013 Practice for Preparing Coal Samples for Analysis
40-46
E11 Specification for Woven Wire Test Sieve Cloth and Test
Preparation of Sample 4
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.
3.2 Definitions of Terms Specific to This Standard:
1.4 The values stated in SI units are to be regarded as the
3.2.1 sample as received, n—a representative portion of raw
standard.
gypsum or gypsum product in the state received by the testing
1.5 This standard does not purport to address all of the
laboratory, including aggregates, impurities and water content.
safety concerns, if any, associated with its use. It is the
3.2.2 dried sample, n—a sample devoid of free water.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.2.3 riffle, n—a hand feed sample divider device that
divides the sample into parts of approximately the same
bility of regulatory limitations prior to use.
weight. (D2013)
2. Referenced Documents
2 4. Preparation of Sample
2.1 ASTM Standards:
4.1 General Procedures—Details of sample preparation will
C11 Terminology Relating to Gypsum and Related Building
Materials and Systems vary according to the type of material being tested.
4.1.1 Sample As Received—Use a sufficient amount of
sample such that, after sieving, not less than 50 g of sample
These test methods are under the jurisdiction of ASTM Committee C11 on will remain for testing. Weigh the entire sample immediately
Gypsum and Related Building Materials and Systems and are the direct responsi-
after opening the container in which the material was received.
bility of Subcommittee C11.01 on Specifications and Test Methods for Gypsum
This will become the weight of the sample as received.
Products.
4.1.2 Drying—DrythesampleinaccordancewithSection7.
CurrenteditionapprovedJune1,2012.PublishedJuly2012.Originallyapproved
´1
in 1961. Last previous edition approved in 2006 as C471 – 01 (2006) . DOI:
This will be the weight of the dried sample.
10.1520/C0471M-01R12.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*A Summary of Changes section appears at the end of this standard
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C471M − 01 (2012)
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.
equipment thoroughly between samples. Thoroughly remix the
5.2 Balance—Capable of weighing not less than 100 g at a
ground sample and store it in an airtight container to avoid
precision of 0.001 g.
contamination.
5.3 Drying Oven—A mechanical convection oven set at 45
4.1.4 Rehydrating—Thoroughly blend and rehydrate
6 3 °C.
samples which contain calcium sulfate in forms other than
CaSO ·2H O and natural anhydrite. Place the sample in
5.4 Desiccator—Capable of being tightly sealed and con-
4 2
distilled water and keep it wet for not less than 48 h. Dry the
taining calcium chloride or equivalent desiccant.
hydrated sample in an oven at 45 6 3 °C to constant weight
5.5 Calcining Oven or Furnace—Capable of achieving and
and recrush or grind it in accordance with 4.1.3.
maintaining temperatures to not less than 1000 °C.
4.1.5 Sample Reduction—Thoroughly mix and reduce large
5.6 Weighing Bottles—Borosilicate glass or ceramic con-
samples as required by quartering or by the use of a riffle to
tainers with tightly sealable lids.
obtain a specimen of approximately 50 g.
5.7 Hot Plate—A controllable hot plate capable of heating
4.2 Gypsum (C22/C22M)—Gypsum samples will be re-
casseroles to approximately 120 °C.
ceived in the form of rocks, powder or both. If necessary crush
andreducetheentiredriedsampleinaccordancewith4.1.3and 5.8 Porcelain Casseroles—Withacapacityof50to100mL.
4.1.5.
5.9 Filtering Funnels.
4.3 Gypsum Plaster, (C28/C28M).
5.10 Filter Paper.
4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFi-
5.11 Porcelain Crucibles.
bered Plaster—Screen the dried sample through a 150-µm (No.
100) sieve and discard the residue retained on the sieve. 5.12 Mortar and Pestle.
Reweigh the remaining sample and calculate the percentage of
5.13 Mechanical Jaw Crusher—Capable of crushing gyp-
the dried sample. Reduce the sample in accordance with 4.1.5.
sum rocks up to 50 mm diameter.
Thoroughly blend and rehydrate the specimen in accordance
5.14 Mechanical Grinder—Burr mill or equivalent capable
with 4.1.4.
of grinding the granular output of the jaw crusher specified in
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster—
5.13.
Reduce the dried sample in accordance with 4.1.5. Thoroughly
blend and rehydrate the specimen in accordance with 4.1.4.
6. Reagents
4.4 Gypsum Casting and Molding Plaster,(C59)—Reduce
6.1 Purity of Reagents—Use reagent grade chemicals in all
the dried sample in accordance with 4.1.5. Thoroughly blend
tests. Unless otherwise indicated, use reagents that conform to
and rehydrate the specimen in accordance with 4.1.4.
the specifications of the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are
4.5 Gypsum Keene’s Cement,(C61)—Reduce the dried
available. If it is necessary to use other grades first ascertain
sample in accordance with 4.1.5. Blend in no more than 1 %
that the reagent is of sufficiently high purity so that its use will
molding plaster or K SO and rehydrate the specimen in
2 4
not lessen the accuracy of the determination.
accordance with 4.1.4.
6.1.1 Ammonium Chloride (NH Cl).
4.6 Gypsum Concrete,(C317/C317M)—Screen the dried
6.1.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated
sample through a 150-µm (No. 100) sieve and discard the
ammonium hydroxide (NH OH).
residue retained on the sieve. Reweigh the remaining sample
6.1.3 Ammonium Nitrate (25 g/L)—Dissolve 25 g of ammo-
and calculate the percentage of the dried sample. Reduce the
nium nitrate (NH NO ) in water and dilute to 1 L.
4 3
sample in accordance with 4.1.5. Thoroughly blend and rehy-
6.1.4 Ammonium Oxalate ((NH ) C O ).
4 2 2 4
drate the specimen in accordance with 4.1.4.
6.1.5 BariumChloride(100g/L)—Dissolve100gofbarium
4.7 Gypsum Board—Cut or break the dried sample into
chloride (BaCl ·2H O) in water and dilute to 1 L.
2 2
small pieces. Using a mortar and pestle, strike the pieces of the
6.1.6 Calcium Chloride (CaCl )—Anhydrous Calcium
sampletoloosenthepaperface.Removethepiecesofpaperby
Chloride with a combined water of not more than 5 %.
hand as they are separated from the core of the gypsum board.
6.1.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
Carefully scrape any remaining powder from the paper. When
chloric acid (HCl).
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.
C471M − 01 (2012)
6.1.8 Hydrochloric Acid(1+4) —Mix 1 volume of HCl (sp used to calculate the purity of gypsum or the amount of
gr 1.19) with 4 volumes of water. gypsum or gypsum plaster in gypsum products.
6.1.9 Hydrochloric Acid(1+5) —Mix 1 volume of HCl (sp
8.2 Interferences—Some materials, such as organic and
gr 1.19) with 5 volumes of water.
hydrated compounds that decompose within the same tempera-
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.
g of potassium chromate (K CrO ) in 50 mLof water, mix, add
2 4
8.3 Procedure:
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 ).
4 4
to a precision of 0.0001 g in the previously tared weighing
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric
bottles and record the total weight with lids.
acid (H SO ).
2 4
8.3.3 Place the specimens in the calcining oven with the lids
6.1.16 Sulfuric Acid (1+6) —Carefully mix 1 volume of
H SO (sp gr 1.84) with 6 volumes of water. placed loosely on each bottle or crucible for2hor until
2 4
constant weight has been obtained.
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO (sp gr
1.42) with 200 mL of water. 8.3.4 Place the lids tightly on the weighing bottles, remove
6.1.18 Phenolphthalein Indicator Solution— Dissolve 0.25 from the oven, and place in the desiccator to cool to room
g of phenolphthalein in 30 mLof methanol and dilute to 50 mL temperature.
with water. 8.3.5 Weigh each specimen to a precision of 0.0001 g and
6.1.19 Sodium Hydroxide Solution (0.1 N)—Dissolve1gof
record the weights.
sodium hydroxide (NaOH) in 250 mL of water.
8.3.6 Retain the residues for carbon dioxide analysis.
6.1.20 Water—Reagent water shall be in accordance with
8.4 Calculation and Report—Calculate and report the aver-
Specification D1193, type II. Specification D1193 gives the
age loss in weight of the three specimens as a percentage of the
following values for type II grade water.
sample as received or of the dried sample, as required, to the
Electrical conductivity, max, µS/cm at 298 K (25-C) 1.0
nearest 0.001 g and record the tare weights.
Electrical resistivity, min, MΩ·cm at 298 K (25-C) 1.0
Total organic carbon (TOC), max, µg/L 50.0
8.5 Precision and Bias—Neither the precision nor the bias
Sodium, max, µg/L 5.0
for the combined water analysis has been determined.
Chlorides max, µg/L 5.0
Total silica, max, µg/L 5.0
9. Carbon Dioxide
7. Free Water
9.1 Summary of Test Method—The sample is decomposed
7.1 Significance and Use—The free water analysis deter-
with HCl and the liberated CO is passed through a series of
mines the amount of free water contained in the sample as
scrubbers to remove water and sulfides. The CO is absorbed
opposed to chemically combined water, and prepares the
with Ascarite, a special sodium hydroxide absorbent, and the
sample for further analysis.
gain in weight of the absorption tube is determined and
7.2 Procedure:
calculated as percent CO .
7.2.1 Weigh a sample of the material as received of not less
9.2 Significance and Use—The carbon dioxide analysis is
than 50 g to a precision of 0.001 g and spread it out in a thin
useful in estimating carbonates and organic carbon for chemi-
layer in a suitable vessel. Place in an oven and dry at 45 6 3
cal balance.
°C for 2 h, then cool in a desiccator and weigh again. The loss
of weight corresponds to the free water. 9.3 Special Reagents:
7.2.2 Retain the sample in a sealed container or in the
9.3.1 Magnesium Perchlorate Desiccant—for drying.
desiccator for further analysis.
9.3.2 Sodium Hydroxide Absorbent—a coarse sodium hy-
droxide coated silica.
7.3 Calculation and Report—Calculate and report loss in
weight as a percentage of the sample as received or of the dried
9.4 Special Apparatus—The apparatus illustrated in Fig. 1
sample as required.
consists of the following:
9.4.1 Purifying Jar A, Fleming, containing sulfuric acid.
7.4 Precision and Bias—Neither the precision nor the bias
9.4.2 Drying Tube B, U-shaped with side arms and glass-
for the free water analysis has been determined.
stoppers. Side arms are shaped to
...
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