ASTM C471M-14
(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
17.1 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 panel products, including gypsum ready-mixed plaster, gypsum wood-fibered plaster, and gypsum concrete.
1.2 The test methods appear in the following order:
Sections
Preparation of Sample
4
Complete Procedure
5 – 16
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
Determination of Sand in Set Plaster
30 – 36
Wood-Fiber Content in Wood-Fiber Gypsum Plaster
37 – 39
Optional Procedure for Analysis for Sodium by the Atomic Absorption Method
40 – 46
Optional Procedure for Analysis for Sodium by Flame Photometry
47 – 54
Determination of Orthorhombic Cyclooctasulfur (S8) in Ggypsum Panel Products—General Provisions
55
Determination of Orthorhombic Cyclooctasulfur (S8) in Gypsum Panel Products by Gas Chromatograph Equipped with a Mass Spectrometer (GS/MS)
56
Determination of Orthorhombic Cyclooctasulfur (S8) in Gypsum Panel Products by Gas Chromatograph Equipped with an Electron Capture Detector (GC/ECD)
57
Determination of Orthorhombic Cyclooctasulfur (S8) in Gypsum Panel Products by High-performance Liquid Chromatograph Equipped with and Ultraviolet Detector (HPLC/UV)
58
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.
General Information
Relations
Buy Standard
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: C471M − 14
StandardTest 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* 1.4 The values stated in SI units are to be regarded as the
standard.
1.1 These test methods cover the chemical analysis of
1.5 This standard does not purport to address all of the
gypsum and gypsum panel products, including gypsum ready-
safety concerns, if any, associated with its use. It is the
mixed plaster, gypsum wood-fibered plaster, and gypsum
responsibility of the user of this standard to establish appro-
concrete.
priate safety and health practices and determine the applica-
1.2 The test methods appear in the following order:
bility of regulatory limitations prior to use.
Sections
Preparation of Sample 4
2. Referenced Documents
Complete Procedure 5–16
Alternative Procedure for Analysis for
2.1 ASTM Standards:
Calcium Sulfate by Ammonium Acetate 17–22
C11 Terminology Relating to Gypsum and Related Building
Method
Alternative Procedure for Analysis for Materials and Systems
Sodium Chloride by the Coulometric 23–29
C22/C22M Specification for Gypsum
Method
C28/C28M Specification for Gypsum Plasters
Determination of Sand in Set Plaster 30–36
Wood-Fiber Content in Wood-Fiber Gyp- 37–39
C59 Specification for Gypsum Casting Plaster and Gypsum
sum Plaster
Molding Plaster
Optional Procedure for Analysis for So-
C61 Specification for Gypsum Keene’s Cement
dium by the Atomic Absorption Method 40–46
Optional Procedure for Analysis for So- 47–54
C317/C317M Specification for Gypsum Concrete
dium by Flame Photometry
C778 Specification for Standard Sand
Determination of Orthorhombic Cyclooc- 55
C842 Specification forApplication of Interior Gypsum Plas-
tasulfur (S ) in Ggypsum Panel
Products—General Provisions
ter
Determination of Orthorhombic Cyclooc- 56
D1193 Specification for Reagent Water
tasulfur (S ) in Gypsum Panel Prod-
D1428 Test Method for Test for Sodium and Potassium In
ucts by Gas Chromatograph Equipped
with a Mass Spectrometer (GS/MS)
Water and Water-Formed Deposits by Flame Photometry
Determination of Orthorhombic Cyclooc- 57 3
(Withdrawn 1989)
tasulfur (S ) in Gypsum Panel Prod-
D2013 Practice for Preparing Coal Samples for Analysis
ucts by Gas Chromatograph Equipped
with an Electron Capture Detector
E11 Specification for Woven Wire Test Sieve Cloth and Test
(GC/ECD)
Sieves
Determination of Orthorhombic Cyclooc- 58
tasulfur (S ) in Gypsum Panel Prod-
ucts by High-performance Liquid Chro- 3. Terminology
matograph Equipped with and
3.1 Definitions—Definitions shall be in accordance with
Ultraviolet Detector (HPLC/UV)
Terminology C11.
1.3 The text of this standard references notes and footnotes
3.2 Definitions of Terms Specific to This Standard:
that provide explanatory material. These notes and footnotes
3.2.1 calibration standard, n—a chemical mixture contain-
(excluding those in tables and figures) shall not be considered
ing a known quantity of the analyte used to relate the measured
as requirements of the standard.
analytical signal to the concentration of the analyte.
These test methods are under the jurisdiction of ASTM Committee C11 on
Gypsum and Related Building Materials and Systems and are the direct responsi- For referenced ASTM standards, visit the ASTM website, www.astm.org, or
bility of Subcommittee C11.01 on Specifications and Test Methods for Gypsum contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2014. Published November 2014. Originally the ASTM website.
approved in 1961. Last previous edition approved in 2013 as C471 – 13. DOI: The last approved version of this historical standard is referenced on
10.1520/C0471M-14. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C471M − 14
3.2.2 dried sample, n—a sample devoid of free water. 4.4 Gypsum Casting and Molding Plaster,(C59)—Reduce
the dried sample in accordance with 4.1.5. Thoroughly blend
3.2.3 internal standard, n—a chemical used in the quantifi-
and rehydrate the specimen in accordance with 4.1.4.
cationofS bymonitoringandadjustingforminorvariancesin
instrument performance.
4.5 Gypsum Keene’s Cement,(C61)—Reduce the dried
sample in accordance with 4.1.5. Blend in no more than 1 %
3.2.4 riffle, n—a hand feed sample divider device that
molding plaster or K SO and rehydrate the specimen in
divides the sample into parts of approximately the same 2 4
accordance with 4.1.4.
weight. (D2013)
4.6 Gypsum Concrete,(C317/C317M)—Screen the dried
3.2.5 sample as received, n—a representative portion of raw
sample through a 150-µm (No. 100) sieve and discard the
gypsum or gypsum product in the state received by the testing
residue retained on the sieve. Reweigh the remaining sample
laboratory, including aggregates, impurities and water content.
and calculate the percentage of the dried sample. Reduce the
3.2.6 surrogate standard, n—a chemical used to account for
sample in accordance with 4.1.5. Thoroughly blend and rehy-
extraction efficiency of S .
drate the specimen in accordance with 4.1.4.
4. Preparation of Sample
4.7 Gypsum Panel Products—Cut or break the dried sample
4.1 General Procedures—Details of sample preparation will
into small pieces. Using a mortar and pestle, strike the pieces
vary according to the type of material being tested. of the sample to loosen the paper face. Remove the pieces of
4.1.1 Sample As Received—Use a sufficient amount of
paper by hand as they are separated from the core of the
sample such that, after sieving, not less than 50 g of sample gypsum board. Carefully scrape any remaining powder from
will remain for testing. Weigh the entire sample immediately
the paper. When all the paper has been removed from the
after opening the container in which the material was received. pieces of the sample, reduce the sample in accordance with
This will become the weight of the sample as received.
4.1.5.
4.1.2 Drying—DrythesampleinaccordancewithSection7.
COMPLETE PROCEDURE
This will be the weight of the dried sample.
4.1.3 Crushing and Grinding—Crush and grind the sample
5. Apparatus
by hand with a mortar and pestle or by mechanical crushing
and grinding equipment to pass a 250-µm (No. 60) sieve. Take 5.1 Analytical Balance—Capable of weighing the weighing
care,particularlywithmechanicalequipment,nottoexposethe bottles, lids and samples.
sample to temperatures of more than 52°C. Clean the equip-
5.2 Balance—Capable of weighing not less than 100 g at a
ment thoroughly between samples. Thoroughly remix the
precision of 0.001 g.
ground sample and store it in an airtight container to avoid
5.3 Drying Oven—A mechanical convection oven set at 45
contamination.
6 3°C.
4.1.4 Rehydrating—Thoroughly blend and rehydrate
samples which contain calcium sulfate in forms other than
5.4 Desiccator—Capable of being tightly sealed and con-
CaSO ·2H O and natural anhydrite. Place the sample in
taining calcium chloride or equivalent desiccant.
4 2
distilled water and keep it wet for not less than 48 h. Dry the
5.5 Calcining Oven or Furnace—Capable of achieving and
hydratedsampleinanovenat45 63°Ctoconstantweightand
maintaining temperatures to not less than 1000°C.
recrush or grind it in accordance with 4.1.3.
5.6 Weighing Bottles—Borosilicate glass or ceramic con-
4.1.5 Sample Reduction—Thoroughly mix and reduce large
tainers with tightly sealable lids.
samples as required by quartering or by the use of a riffle to
obtain a specimen of approximately 50 g.
5.7 Hot Plate—A controllable hot plate capable of heating
casseroles to approximately 120°C.
4.2 Gypsum (C22/C22M)—Gypsum samples will be re-
ceived in the form of rocks or powder, or both. If necessary
5.8 Porcelain Casseroles—Withacapacityof50to100mL.
crush and reduce the entire dried sample in accordance with
5.9 Filtering Funnels.
4.1.3 and 4.1.5.
5.10 Filter Paper.
4.3 Gypsum Plaster, (C28/C28M).
5.11 Porcelain Crucibles.
4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFi-
bered Plaster—Screen the dried sample through a 150-µm
5.12 Mortar and Pestle.
(No. 100) sieve and discard the residue retained on the sieve.
5.13 Mechanical Jaw Crusher—Capable of crushing gyp-
Reweigh the remaining sample and calculate the percentage of
sum rocks up to 50 mm diameter.
the dried sample. Reduce the sample in accordance with 4.1.5.
5.14 Mechanical Grinder—Burr mill or equivalent capable
Thoroughly blend and rehydrate the specimen in accordance
of grinding the granular output of the jaw crusher specified in
with 4.1.4.
5.13.
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster—
Reduce the dried sample in accordance with 4.1.5. Thoroughly
6. Reagents
blend and rehydrate the specimen in accordance with 4.1.4.
6.1 Purity of Reagents—Use reagent grade chemicals in all
Detailed requirements for this sieve are given in Specification E11. tests. Unless otherwise indicated, use reagents that conform to
C471M − 14
the specifications of the Committee on Analytical Reagents of 7. Free Water
the American Chemical Society, where such specifications are
7.1 Significance and Use—The free water analysis deter-
available. If it is necessary to use other grades, first ascertain
mines the amount of free water contained in the sample as
that the reagent is of sufficiently high purity so that its use will
opposed to chemically combined water, and prepares the
not lessen the accuracy of the determination.
sample for further analysis.
6.1.1 Ammonium Chloride (NH Cl).
7.2 Procedure:
6.1.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated
7.2.1 Weigh a sample of the material as received of not less
ammonium hydroxide (NH OH).
6.1.3 Ammonium Nitrate (25 g/L)—Dissolve 25 g of ammo- than 50 g to a precision of 0.001 g and spread it out in a thin
layer in a suitable vessel. Place in an oven and dry at 45 6 3°C
nium nitrate (NH NO ) in water and dilute to 1 L.
4 3
6.1.4 Ammonium Oxalate ((NH ) C O ). for 2 h, then cool in a desiccator and weigh again. The loss of
4 2 2 4
weight corresponds to the free water.
6.1.5 BariumChloride(100g/L)—Dissolve100gofbarium
chloride (BaCl ·2H O) in water and dilute to 1 L.
7.2.2 Retain the sample in a sealed container or in the
2 2
6.1.6 Calcium Chloride (CaCl )—Anhydrous Calcium desiccator for further analysis.
Chloride with a combined water of not more than 5 %.
7.3 Calculation and Report—Calculate and report loss in
6.1.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
weightasapercentageofthesampleasreceivedorofthedried
chloric acid (HCl).
sample as required.
6.1.8 Hydrochloric Acid(1+4)—Mix 1 volume of HCl (sp
7.4 Precision and Bias—Neither the precision nor the bias
gr 1.19) with 4 volumes of water.
6.1.9 Hydrochloric Acid(1+5)—Mix 1 volume of HCl (sp for the free water analysis has been determined.
gr 1.19) with 5 volumes of water.
6.1.10 Nitric Acid (sp gr 1.42)—Concentrated nitric acid 8. Combined Water
(HNO ).
8.1 Significance and Use—The combined water analysis
6.1.11 Potassium Chromate Solution (100 g/L)—Dissolve
determines the percent of chemically combined water and is
5 g of potassium chromate (K CrO ) in 50 mL of water, mix,
2 4
used to calculate the purity of gypsum or the amount of
add 10 drops of 0.05 N silver nitrate (AgNO ) solution, allow
gypsum or gypsum plaster in gypsum products.
to stand for 5 min, and filter.
8.2 Interferences—Some materials, such as organic and
6.1.12 Potassium Permanganate (5.6339 g/L)—Dissolve
hydrated compounds that decompose within the same tempera-
5.6339 g of potassium permanganate (KMnO ) in water and
ture range as gypsum, will cause high results. When the
dilute to 1 L.
maximum temperature is exceeded, some carbonates undergo
6.1.13 Silver Nitrate, Standard Solution (0.05 N)—Prepare
decomposition, which will result in high results.
and standardize a 0.05 N silver nitrate (AgNO ) solution.
6.1.14 Sodium Ammonium Phosphate—(NaNH HPO ).
4 4
8.3 Procedure:
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric
8.3.1 For each sample, place three weighing bottles with
acid (H SO ).
2 4
lids in the preheated calcining oven or furnace and heat for 2 h
6.1.16 Sulfuric Acid (1+6)—Carefully mix 1 volume of
at 215 to 230°C. Place in the desiccator and allow to cool to
H SO (sp gr 1.84) with 6 volumes of water.
2 4
room temperature. Weigh the bottles and lids to the nearest
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO (sp gr
0.0001 g and record the tare weights.
1.42) with 200 mL of water.
8.3.2 Weigh out three specimens of approximately 1 g each
6.1.18 Phenolphthalein Indicator Solution—Dissolve0.25 g
of the sample as prepared in Section 4 and dried in Section 7
of phenolphthalein in 30 mL of methanol and dilute to 50 mL
to a precision of 0.0001 g in the previously tared weighing
with water.
bottles and record the total weight with lids.
6.1.19 Sodium Hydroxide Solution (0.1 N)—Dissolve1gof
8.3.3 Place the specimens in the calcining oven with the lids
sodium hydroxide (NaOH) in 250 mL of water.
placed loosely on each bottle or crucible for2hor until
6.1.20 Water—Reagent water shall be in accordance with
constant weight has been obtained.
Specification D1193, type II. Specification D1193 gives the
8.3.4 Place the lids tightly on the weighing bottles, remove
following values for type II grade water.
from the oven, and place in the desiccator to cool to room
Electrical conductivity, max, µS/cm at 298 K (25-C) 1.0
temperature.
Electrical resistivity, min, MΩ·cm at 298 K (25-C) 1.0
Total organic carbon (TOC), max, µg/L 50.0
8.3.5 Weigh each specimen to a precision of 0.0001 g and
Sodium, max, µg/L 5.0
record the weights.
Chlorides max, µg/L 5.0
Total silica, max, µg/L 5.0
8.3.6 Retain the residues for carbon dioxide analysis.
8.4 Calculation and Report—Calculate and report the aver-
age loss in weight of the three specimens as a percentage of the
Reagent Chemicals, American Chemical Society Specifications , American
sample as received or of the dried sample, as required, to the
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
nearest 0.001 g and record the tare weights.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and t
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C471M − 13 C471M − 14
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 Scope*
1.1 These test methods cover the chemical analysis of gypsum and gypsum panel products, including gypsum ready-mixed
plaster, gypsum wood-fibered plaster, and gypsum concrete.
1.2 The test methods appear in the following order:
Sections
Preparation of Sample 4
Complete Procedure 5 – 16
Alternative Procedure for Analysis for
Calcium Sulfate by Ammonium Acetate 17 – 22
Method
Alternative Procedure for Analysis for
Sodium Chloride by the Coulometric 23 – 29
Method
Determination of Sand in Set Plaster 30 – 36
Wood-Fiber Content in Wood-Fiber Gyp- 37 – 39
sum Plaster
Optional Procedure for Analysis for So-
dium by the Atomic Absorption Method 40 – 46
Optional Procedure for Analysis for So- 47 – 54
dium by Flame Photometry
Determination of Sulfur (S ) in Gypsum 55–65
Panel Products by Liquid Extraction for
Analysis by Liquid or Gas Chromatog-
raphy
Determination of Orthorhombic Cyclooc- 55
tasulfur (S ) in Ggypsum Panel
Products—General Provisions
Determination of Orthorhombic Cyclooc- 56
tasulfur (S ) in Gypsum Panel Prod-
ucts by Gas Chromatograph Equipped
with a Mass Spectrometer (GS/MS)
Determination of Orthorhombic Cyclooc- 57
tasulfur (S ) in Gypsum Panel Prod-
ucts by Gas Chromatograph Equipped
with an Electron Capture Detector
(GC/ECD)
Determination of Orthorhombic Cyclooc- 58
tasulfur (S ) in Gypsum Panel Prod-
ucts by High-performance Liquid Chro-
matograph Equipped with and
Ultraviolet Detector (HPLC/UV)
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.
These test methods are under the jurisdiction of ASTM Committee C11 on Gypsum and Related Building Materials and Systems and are the direct responsibility of
Subcommittee C11.01 on Specifications and Test Methods for Gypsum Products.
Current edition approved Dec. 1, 2013Nov. 1, 2014. Published January 2014November 2014. Originally approved in 1961. Last previous edition approved in 20122013
as C471C471 – 13. – 01 (Reapproved 2012). DOI: 10.1520/C0471M-13.DOI: 10.1520/C0471M-14.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C471M − 14
2. Referenced Documents
2.1 ASTM Standards:
C11 Terminology Relating to Gypsum and Related Building Materials and Systems
C22/C22M Specification for Gypsum
C28/C28M Specification for Gypsum Plasters
C59 Specification for Gypsum Casting Plaster and Gypsum Molding Plaster
C61 Specification for Gypsum Keene’s Cement
C317/C317M Specification for Gypsum Concrete
C778 Specification for Sand
C842 Specification for Application of Interior Gypsum Plaster
D1193 Specification for Reagent Water
D1428 Test Method for Test for Sodium and Potassium In Water and Water-Formed Deposits by Flame Photometry (Withdrawn
1989)
D2013 Practice for Preparing Coal Samples for Analysis
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 Definitions—Definitions shall be in accordance with Terminology C11.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 calibration standard, n—a chemical mixture containing a known quantity of the analyte used to relate the measured
analytical signal to the concentration of the analyte.
3.2.2 dried sample, n—a sample devoid of free water.
3.2.3 internal standard, n—a chemical used in the quantification of S by monitoring and adjusting for minor variances in
instrument performance.
3.2.4 riffle, n—a hand feed sample divider device that divides the sample into parts of approximately the same weight. (D2013)
3.2.5 sample as received, n—a representative portion of raw gypsum or gypsum product in the state received by the testing
laboratory, including aggregates, impurities and water content.
3.2.6 surrogate standard,,standard, n—a chemical used to account for extraction efficiency of S .
4. Preparation of Sample
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 sample such that, after sieving, not less than 50 g of sample will remain
for testing. Weigh the entire sample immediately after opening the container in which the material was received. This will become
the weight of the sample as received.
4.1.2 Drying—Dry the sample in accordance with Section 7. This will be the weight of the dried sample.
4.1.3 Crushing and Grinding—Crush and grind the sample by hand with a mortar and pestle or by mechanical crushing and
grinding equipment to pass a 250-μm (No. 60) sieve. Take care, particularly with mechanical equipment, not to expose the sample
to temperatures of more than 52 °C. 52°C. Clean the equipment thoroughly between samples. Thoroughly remix the ground sample
and store it in an airtight container to avoid contamination.
4.1.4 Rehydrating—Thoroughly blend and rehydrate samples which contain calcium sulfate in forms other than CaSO ·2H O
4 2
and natural anhydrite. Place the sample in distilled water and keep it wet for not less than 48 h. Dry the hydrated sample in an
oven at 45 6 3 °C 3°C to constant weight and recrush or grind it in accordance with 4.1.3.
4.1.5 Sample Reduction—Thoroughly mix and reduce large samples as required by quartering or by the use of a riffle to obtain
a specimen of approximately 50 g.
4.2 Gypsum (C22/C22M)—Gypsum samples will be received in the form of rocks, powder or rocks or powder, or both. If
necessary crush and reduce the entire dried sample in accordance with 4.1.3 and 4.1.5.
4.3 Gypsum Plaster, (C28/C28M).
4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFibered Plaster—Screen the dried sample through a 150-μm (No. 100)
(No. 100) sieve and discard the residue retained on the sieve. Reweigh the remaining sample and calculate the percentage of the
dried sample. Reduce the sample in accordance with 4.1.5. Thoroughly blend and rehydrate the specimen in accordance with 4.1.4.
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 ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Detailed requirements for this sieve are given in Specification E11.
C471M − 14
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster—Reduce the dried sample in accordance with 4.1.5. Thoroughly blend
and rehydrate the specimen in accordance with 4.1.4.
4.4 Gypsum Casting and Molding Plaster, (C59)—Reduce the dried sample in accordance with 4.1.5. Thoroughly blend and
rehydrate the specimen in accordance with 4.1.4.
4.5 Gypsum Keene’s Cement, (C61)—Reduce the dried sample in accordance with 4.1.5. Blend in no more than 1 % molding
plaster or K SO and rehydrate the specimen in accordance with 4.1.4.
2 4
4.6 Gypsum Concrete, (C317/C317M)—Screen the dried sample through a 150-μm (No. 100) sieve and discard the residue
retained on the sieve. Reweigh the remaining sample and calculate the percentage of the dried sample. Reduce the sample in
accordance with 4.1.5. Thoroughly blend and rehydrate the specimen in accordance with 4.1.4.
4.7 Gypsum Panel Products—Cut or break the dried sample into small pieces. Using a mortar and pestle, strike the pieces of
the sample to loosen the paper face. Remove the pieces of paper by hand as they are separated from the core of the gypsum board.
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.
COMPLETE PROCEDURE
5. Apparatus
5.1 Analytical Balance—Capable of weighing the weighing bottles, lids and samples.
5.2 Balance—Capable of weighing not less than 100 g at a precision of 0.001 g.
5.3 Drying Oven—A mechanical convection oven set at 45 6 3 °C.3°C.
5.4 Desiccator—Capable of being tightly sealed and containing calcium chloride or equivalent desiccant.
5.5 Calcining Oven or Furnace—Capable of achieving and maintaining temperatures to not less than 1000 °C.1000°C.
5.6 Weighing Bottles—Borosilicate glass or ceramic containers with tightly sealable lids.
5.7 Hot Plate—A controllable hot plate capable of heating casseroles to approximately 120 °C.120°C.
5.8 Porcelain Casseroles—With a capacity of 50 to 100 mL.
5.9 Filtering Funnels.
5.10 Filter Paper.
5.11 Porcelain Crucibles.
5.12 Mortar and Pestle.
5.13 Mechanical Jaw Crusher—Capable of crushing gypsum rocks up to 50 mm diameter.
5.14 Mechanical Grinder—Burr mill or equivalent capable of grinding the granular output of the jaw crusher specified in 5.13.
6. Reagents
6.1 Purity of Reagents—Use reagent grade chemicals in all tests. Unless otherwise indicated, use reagents that conform to the
specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
available. If it is necessary to use other grades, first ascertain that the reagent is of sufficiently high purity so that its use will not
lessen the accuracy of the determination.
6.1.1 Ammonium Chloride (NH Cl).
6.1.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated ammonium hydroxide (NH OH).
6.1.3 Ammonium Nitrate (25 g/L)—Dissolve 25 g of ammonium nitrate (NH NO ) in water and dilute to 1 L.
4 3
6.1.4 Ammonium Oxalate ((NH ) C O ).
4 2 2 4
6.1.5 Barium Chloride (100 g/L)—Dissolve 100 g of barium chloride (BaCl ·2H O) in water and dilute to 1 L.
2 2
6.1.6 Calcium Chloride (CaCl )—Anhydrous Calcium Chloride with a combined water of not more than 5 %.
6.1.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
6.1.8 Hydrochloric Acid (1 + 4)—Mix 1 volume of HCl (sp gr 1.19) with 4 volumes of water.
6.1.9 Hydrochloric Acid (1 + 5)—Mix 1 volume of HCl (sp gr 1.19) with 5 volumes of water.
6.1.10 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
6.1.11 Potassium Chromate Solution (100 g/L)—Dissolve 5 g 5 g of potassium chromate (K CrO ) in 50 mL of water, mix, add
2 4
10 drops of 0.05 N silver nitrate (AgNO ) solution, allow to stand for 5 min, and filter.
Reagent Chemicals, American Chemical Society Specifications , American 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, MD.
C471M − 14
6.1.12 Potassium Permanganate (5.6339 g/L)—Dissolve 5.6339 g of potassium permanganate (KMnO ) in water and dilute to
1 L.
6.1.13 Silver Nitrate, Standard Solution (0.05 N)—Prepare and standardize a 0.05 N silver nitrate (AgNO ) solution.
6.1.14 Sodium Ammonium Phosphate—(NaNH HPO ).
4 4
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid (H SO ).
2 4
6.1.16 Sulfuric Acid (1 + 6)—Carefully mix 1 volume of H SO (sp gr 1.84) with 6 volumes of water.
2 4
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO (sp gr 1.42) with 200 mL of water.
6.1.18 Phenolphthalein Indicator Solution—Dissolve 0.25 g 0.25 g of phenolphthalein in 30 mL of methanol and dilute to 50
mL 50 mL with water.
6.1.19 Sodium Hydroxide Solution (0.1 N)—Dissolve 1 g of sodium hydroxide (NaOH) in 250 mL of water.
6.1.20 Water—Reagent water shall be in accordance with Specification D1193, type II. Specification D1193 gives the following
values for type II grade water.
Electrical conductivity, max, μS/cm at 298 K (25-C) 1.0
Electrical resistivity, min, MΩ·cm at 298 K (25-C) 1.0
Total organic carbon (TOC), max, μg/L 50.0
Sodium, max, μg/L 5.0
Chlorides max, μg/L 5.0
Total silica, max, μg/L 5.0
7. Free Water
7.1 Significance and Use—The free water analysis determines the amount of free water contained in the sample as opposed to
chemically combined water, and prepares the sample for further analysis.
7.2 Procedure:
7.2.1 Weigh a sample of the material as received of not less than 50 g to a precision of 0.001 g and spread it out in a thin layer
in a suitable vessel. Place in an oven and dry at 45 6 3 °C 3°C for 2 h, then cool in a desiccator and weigh again. The loss of
weight corresponds to the free water.
7.2.2 Retain the sample in a sealed container or in the desiccator for further analysis.
7.3 Calculation and Report—Calculate and report loss in weight as a percentage of the sample as received or of the dried sample
as required.
7.4 Precision and Bias—Neither the precision nor the bias for the free water analysis has been determined.
8. Combined Water
8.1 Significance and Use—The combined water analysis determines the percent of chemically combined water and is used to
calculate the purity of gypsum or the amount of gypsum or gypsum plaster in gypsum products.
8.2 Interferences—Some materials, such as organic and hydrated compounds that decompose within the same temperature range
as gypsum, will cause high results. When the maximum temperature is exceeded, some carbonates undergo decomposition, which
will result in high results.
8.3 Procedure:
8.3.1 For each sample, place three weighing bottles with lids in the preheated calcining oven or furnace and heat for 2 h 2 h
at 215 to 230 °C. 230°C. Place in the desiccator and allow to cool to room temperature. Weigh the bottles and lids to the nearest
0.0001 g and record the tare weights.
8.3.2 Weigh out three specimens of ap
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.