Designation: C471M − 01 (Reapproved 2012)

Standard Test Methods for

Chemical Analysis of Gypsum and Gypsum Products
(Metric)1
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

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
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 for Application of Interior Gypsum Plas-
Alternative Procedure for Analysis for Calcium Sulfate by Ammonium Acetate
Method 17-22
ter
Alternative Procedure for Analysis for Sodium Chloride by the Coulometric D1193 Specification for Reagent Water
Method 23-29 D1428 Test Method for Test for Sodium and Potassium In
Complete Procedure 5-16
Determination of Sand in Set Plaster 30-36
Water and Water-Formed Deposits by Flame Photometry
Optional Procedure for Analysis for Sodium by Flame Photometry 47-54 (Withdrawn 1989)3
Optional Procedure for Analysis for Sodium by the Atomic Absorption Method D2013 Practice for Preparing Coal Samples for Analysis
40-46
Preparation of Sample 4
E11 Specification for Woven Wire Test Sieve Cloth and Test
Wood-Fiber Content in Wood-Fiber Gypsum Plaster 37-39 Sieves
1.3 The text of this standard references notes and footnotes
that provide explanatory material. These notes and footnotes 3. Terminology
(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
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
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
2.1 ASTM Standards:2 4. Preparation of Sample
C11 Terminology Relating to Gypsum and Related Building 4.1 General Procedures—Details of sample preparation will
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
1
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
Products.
This will become the weight of the sample as received.
Current edition approved June 1, 2012. Published July 2012. Originally approved 4.1.2 Drying—Dry the sample in accordance with Section 7.
in 1961. Last previous edition approved in 2006 as C471 – 01 (2006)´1. DOI: This will be the weight of the dried sample.
10.1520/C0471M-01R12.
2
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
3
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
and grinding equipment to pass a 250-µm (No. 60) sieve. Take 5. Apparatus
care, particularly with mechanical equipment, not to expose the 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.
4.1.4 Rehydrating—Thoroughly blend and rehydrate 5.3 Drying Oven—A mechanical convection oven set at 45
samples which contain calcium sulfate in forms other than 6 3 °C.
CaSO4·2H2O and natural anhydrite. Place the sample in 5.4 Desiccator—Capable of being tightly sealed and con-
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
samples as required by quartering or by the use of a riffle to 5.6 Weighing Bottles—Borosilicate glass or ceramic con-
obtain a specimen of approximately 50 g. tainers with tightly sealable lids.
4.2 Gypsum (C22/C22M)—Gypsum samples will be re- 5.7 Hot Plate—A controllable hot plate capable of heating
ceived in the form of rocks, powder or both. If necessary crush casseroles to approximately 120 °C.
and reduce the entire dried sample in accordance with 4.1.3 and 5.8 Porcelain Casseroles—With a capacity of 50 to 100 mL.
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-
bered Plaster—Screen the dried sample through a 150-µm (No. 5.11 Porcelain Crucibles.
100) sieve4 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
with 4.1.4. 5.14 Mechanical Grinder—Burr mill or equivalent capable
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster— of grinding the granular output of the jaw crusher specified in
Reduce the dried sample in accordance with 4.1.5. Thoroughly 5.13.
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
4.5 Gypsum Keene’s Cement, (C61)—Reduce the dried the American Chemical Society, where such specifications are
sample in accordance with 4.1.5. Blend in no more than 1 % available.5 If it is necessary to use other grades first ascertain
molding plaster or K2SO4 and rehydrate the specimen in that the reagent is of sufficiently high purity so that its use will
accordance with 4.1.4. not lessen the accuracy of the determination.
6.1.1 Ammonium Chloride (NH4Cl).
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) sieve4 and discard the
ammonium hydroxide (NH4OH).
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 (NH4NO3) in water and dilute to 1 L.
sample in accordance with 4.1.5. Thoroughly blend and rehy-
6.1.4 Ammonium Oxalate ((NH4)2C2O4).
drate the specimen in accordance with 4.1.4.
6.1.5 Barium Chloride (100 g/L)—Dissolve 100 g of barium
4.7 Gypsum Board—Cut or break the dried sample into chloride (BaCl2·2H2O) in water and dilute to 1 L.
small pieces. Using a mortar and pestle, strike the pieces of the 6.1.6 Calcium Chloride (CaCl2)—Anhydrous Calcium
sample to loosen the paper face. Remove the pieces of paper by 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 5
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,
4
Detailed requirements for this sieve are given in Specification E11. MD.

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 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
(HNO3). 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 (K2CrO4) in 50 mL of water, mix, add
10 drops of 0.05 N silver nitrate (AgNO3) solution, allow to 8.3 Procedure:
stand for 5 min, and filter. 8.3.1 For each sample, place three weighing bottles with
6.1.12 Potassium Permanganate (5.6339 g/L)—Dissolve lids in the preheated calcining oven or furnace and heat for 2
5.6339 g of potassium permanganate (KMnO4) in water and h at 215 to 230 °C. Place in the desiccator and allow to cool to
dilute to 1 L. room temperature. Weigh the bottles and lids to the nearest
6.1.13 Silver Nitrate, Standard Solution (0.05 N)—Prepare 0.0001 g and record the tare weights.
and standardize a 0.05 N silver nitrate (AgNO3) solution. 8.3.2 Weigh out three specimens of approximately 1 g each
6.1.14 Sodium Ammonium Phosphate—(NaNH4HPO4). of the sample as prepared in Section 4 and dried in Section 7
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric to a precision of 0.0001 g in the previously tared weighing
acid (H2SO4). bottles and record the total weight with lids.
6.1.16 Sulfuric Acid (1 + 6) —Carefully mix 1 volume of 8.3.3 Place the specimens in the calcining oven with the lids
H2SO4 (sp gr 1.84) with 6 volumes of water. placed loosely on each bottle or crucible for 2 h or until
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO3 (sp gr constant weight has been obtained.
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 mL of 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)—Dissolve 1 g of 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
Electrical resistivity, min, MV·cm at 298 K (25-C) 1.0
nearest 0.001 g and record the tare weights.
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
Chlorides max, µg/L 5.0 for the combined water analysis has been determined.
Total silica, max, µg/L 5.0
9. Carbon Dioxide
7. Free Water
7.1 Significance and Use—The free water analysis deter- 9.1 Summary of Test Method—The sample is decomposed
mines the amount of free water contained in the sample as with HCl and the liberated CO2 is passed through a series of
opposed to chemically combined water, and prepares the scrubbers to remove water and sulfides. The CO2 is absorbed
sample for further analysis. with Ascarite, a special sodium hydroxide absorbent, and the
gain in weight of the absorption tube is determined and
7.2 Procedure: calculated as percent CO2.
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 9.2 Significance and Use—The carbon dioxide analysis is
layer in a suitable vessel. Place in an oven and dry at 45 6 3 useful in estimating carbonates and organic carbon for chemi-
°C for 2 h, then cool in a desiccator and weigh again. The loss cal balance.
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-
7.3 Calculation and Report—Calculate and report loss in droxide coated silica.
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:
7.4 Precision and Bias—Neither the precision nor the bias 9.4.1 Purifying Jar A, Fleming, containing sulfuric acid.
for the free water analysis has been determined. 9.4.2 Drying Tube B, U-shaped with side arms and glass-
stoppers. Side arms are shaped to hold rubber tubing. Contains
8. Combined Water Anhydrone on left side and Ascarite on right side.
8.1 Significance and Use—The combined water analysis 9.4.3 Erlenmeyer Flask C, 250 mL, 24/20 ground-glass
determines the percent of chemically combined water and is joint.

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FIG. 1 Apparatus for Carbon Dioxide Analysis

9.4.4 Separatory Funnel D, with ground glass stopper and sample flask and boil for approximately 2 min. Remove the hot
interchangeable hollow ground-glass joint. A delivery tube plate and continue the flow of purified air at approximately
bent at the end extends into the sample flask approximately 15 three bubbles per second for 10 min to sweep the apparatus free
mm from the bottom and is used to introduce acid into flask. of CO2. Close the absorption bulb, disconnect it from the train
9.4.5 Condenser E. and weigh, opening the stopper momentarily to equalize the
9.4.6 Gas-Washing Bottle F, 250 mL, with fitted disk pressure. Use a second absorption bulb as counterpoise in all
containing distilled water to retain most of the acid volatilized weighings unless a single pan balance is used.
from the alkalimeter. 9.6 Calculation—Calculate the percent CO2 to the dried
9.4.7 U-Tube G, containing mossy zinc to remove the last sample as follows:
traces of HCl.
9.4.8 Gas Washing Bottle H, 250 mL, with fritted disk, Percent CO2 5 ~~ A 2 B ! /C 3 100!~ 1 2 D ! (1)
containing concentrated H2SO4 and trap I, to remove any SO3 where:
mist that is carried over. A = mass of absorption bulb + CO2 g,
9.4.9 Absorption Bulb J, containing Anhydrone to remove B = mass of absorption bulb before the run, g,
last traces of water vapor. C = mass of specimen, g, and
9.4.10 CO2 Absorption Bulb, containing Ascarite filled as D = percent combined water as determined in Section 8 as
follows: On the bottom of the bulb, place a layer of glass wool a decimal.
extending above the bottom outlet and on top of this a layer of Calculate the percent CO2 to the sample as received as
Anhydrone approximately 10 mm thick; immediately above follows:
this place another layer of glass wool, then add Ascarite to
almost fill the bulb. Place a top layer of Anhydrone approxi- Percent CO2 5 E ~ 1 2 F ! (2)
mately 10 mm thick on top of the Ascarite and top it off with where:
a covering of glass wool. E = result of Eq 1, and
9.4.11 U-Guard Tube L, filled with Anhydrone in left side F = percent free water as determined in Section 7 as a
and Ascarite in right side. decimal.
9.4.12 Purifying Jar M, Fleming, containing H2SO4.
9.7 Precision and Bias—Neither the precision nor the bias
9.5 Procedure: for the carbon dioxide analysis has been determined.
9.5.1 After drying as described in Section 8 place the
residue obtained in the 250 mL Erlenmeyer flask (C). Connect 10. Silicon Dioxide and Other Acid Insoluble Matter
the flask to the apparatus as shown in Fig. 1. Purge the system 10.1 Summary of Test Method—The gypsum and other acid
free of carbon dioxide by passing a current of CO2-free air soluble components of the sample are dissolved in dilute
through the apparatus for 10 to 15 min. hydrochloric acid (HCl). The residue is weighed and calculated
9.5.2 Weigh the absorption bulb to 0.0001 g and attach it to as silicon dioxide and other acid insoluble matter.
the train. Remove the glass stopper from the separatory funnel,
place 50 mL of dilute HCl (1 + 1) in the separatory funnel (D) 10.2 Significance and Use—The silicon dioxide and other
and replace the stopper with the interchangeable hollow acid insoluble matter analysis determines and is used to report
ground-glass joint through which passes a tube for admitting the percentage of one of the inert impurities in gypsum and
purified air. Open the stopcock of the separatory funnel and gypsum products.
admit air through the top of the funnel to force the hydrochloric 10.3 Procedure—Perform in triplicate.
acid into the Erlenmeyer flask (C). 10.3.1 Weigh approximately 1 g of the specimen prepared in
9.5.3 Start cold water circulating through the condenser (E) Section 4 to the nearest 0.0001 g.
and, with CO2-free air passing at a moderate rate through the 10.3.2 Place the specimen in a porcelain casserole. Add
absorption train, place a small hot plate or gas burner under the approximately 50 mL of 1 + 5 hydrochloric acid. Evaporate

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 C471M − 01 (2012)
slowly and carefully to apparent dryness on a hot plate. Take precipitate may be further treated to separate the two oxides,
not less than 20 min to do the evaporation. Make a blank but this is generally unnecessary.
determination with one casserole in parallel. Cool to room 11.4 Precision and Bias—Neither the precision nor the bias
temperature. for the iron and aluminum oxides analysis has been deter-
10.3.3 Add enough hydrochloric acid (sp gr 1.19) to wet the mined.
solid residue. Add 20 mL of water, boil and filter through filter
paper. Wash the filter paper thoroughly using not less than 100 12. Calcium Oxide
mL of room temperature water to render the precipitate 12.1 Significance and Use—The calcium oxide (CaO)
chloride free. The most effective washing technique is to use analysis is used to determine the amount of CaO and calculate
many small quantities of wash water rather than fill the funnel the amount of calcium carbonate (CaCO3) in gypsum and
to the brim two or three times. Test the filtrate for chloride by gypsum products.
collecting a small amount and adding a few drops of 0.1
12.2 Procedure:
normal silver nitrate (AgNO3) solution. A white precipitate
12.2.1 To the filtrate obtained as described in Section 11 add
indicates more washing is needed. Discard this test solution.
5 g of ammonium oxalate ((NH4)2C2O4) dissolved in water.
10.3.4 Place all the filtrate back in the same casserole. Digest hot for 30 min, making sure that the solution is always
Evaporate to dryness and heat to 120 °C for 1 h and cool. To alkaline with NH4OH. Filter, wash, and ignite the precipitate at
the cooled casserole add enough HCl (sp gr 1.19) to wet the 1000 °C for 2 h to constant weight in a platinum crucible in a
solid residue. Add 50 mL of water and boil. muffle furnace.
10.3.5 Wash the second contents of the casserole through 12.2.2 Alternative Method—To the filtrate obtained as de-
another filter paper. Thoroughly wash the residue in the filter scribed in Section 11, add 5 g of (NH4)2C2O4 dissolved in
paper until chloride free as in 10.3.3. Retain the filtrate for the water. Digest hot for 30 min, making sure that the solution is
iron and aluminum oxide analysis. always alkaline with NH4OH. Filter and wash, transfer the
10.3.6 Dry sufficient crucibles by placing in a cold muffle precipitate to a beaker, and wash the filter paper with hot
furnace during warm up or by placing in a drying oven for 15 H2SO4 (1 + 6), catching the washing in the same beaker. Heat
to 20 min, then placing in a 900 °C muffle furnace. Cool gently to complete solution, adding more H2SO4 if necessary.
crucibles to room temperature in a desiccator. While still warm, titrate with potassium permanganate
10.3.7 Transfer both filter papers to a tared crucible and char (KMnO4) solution (5.6339 g/L) until the pink color persists.
slowly without flaming. Burn off all the carbon and ignite in a
12.3 Calculation—The number of milliliters of KMnO4
muffle furnace at 900 °C for 15 min.
solution used gives directly the percentage of lime in the dried
10.3.8 Cool the crucibles in a desiccator and weigh to the sample. Calculate the CaO to the percentage of sample as
nearest 0.0001 g. received or the dried sample as required.
10.4 Calculation and Report—Calculate the average weight 12.4 Precision and Bias—Neither the precision nor the bias
of the three precipitates and report as silicon dioxide (SiO2) for the calcium oxide analysis has been determined.
and other insoluble matter to the percentage of sample as
received or to the dried sample as required. 13. Magnesium Oxide
10.5 Precision and Bias—Neither the precision nor the bias 13.1 Significance and Use—The magnesium oxide (MgO)
for the silicon dioxide and other acid insoluble matter has been analysis is used to determine the amount of MgO and calculate
determined. the amount of magnesium carbonate MgCO3 in gypsum and
gypsum products.
11. Iron and Aluminum Oxides 13.2 Procedure—To the filtrate obtained as described in
11.1 Significance and Use—The iron and aluminum oxides 12.2.1 or 12.2.2, add enough water to give a total volume of
(Fe2O3 + Al2O3) analysis is used to determine the quantity of approximately 600 mL. Cool, and add 10 mL of NH4OH and
these metal oxides in gypsum or gypsum products. 5 g of sodium ammonium phosphate (NaNH4HPO4) dissolved
in water. Stir vigorously until a precipitate begins to form. Let
11.2 Procedure—To the filtrate, obtained as described in stand overnight. Filter, using a Gooch crucible, and wash with
Section 10, add a few drops of nitric acid (HNO3), and boil to NH4NO3 solution. Ignite at 1000°C for 2 h to constant weight
ensure oxidation of the iron. Add 2 g of ammonium chloride in a muffle furnace.
(NH4Cl) previously dissolved in water. Make alkaline with
13.3 Calculation—Multiply this weight by 0.36207 to find
ammonium hydroxide (NH4OH). Digest hot for a few minutes
the weight of magnesium oxide (MgO). Calculate the MgO to
until the precipitate coagulates. Filter, wash, ignite the precipi-
the percentage of sample as received or to the dried sample as
tate at 1000 °C for 30 min or to constant weight in a muffle
required.
furnace and weigh as Fe2O3 + Al2O3. Save the filtrate for the
CaO analysis. 13.4 Precision and Bias—Neither the precision nor the bias
for the magnesium oxide analysis has been determined.
NOTE 1—The addition of a pinch of ashless filter paper pulp will aid in
the filtration of the precipitate. 14. Sulfur Trioxide
11.3 Calculation—Calculate Fe2 O3 + Al2O3 to the percent- 14.1 Summary of Test Method—In this test method, sulfate
age of sample as received or the dried sample as required. This is precipitated from an acid solution of the gypsum with barium

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 C471M − 01 (2012)
chloride (BaCl2). The precipitate is filtered and weighed as prior to use by refiltering the filtrate from the crucibles with
barium sulfate (BaSO4) and the sulfur trioxide (SO3) equiva- filter paper, and no more than 2 mg is collected on the filter
lent is calculated. paper.
14.2 Significance and Use—The specification for gypsum 14.4.7 Ignite the precipitate and paper in a tared crucible,
and some gypsum products specifies the amount of calcium and slowly char the paper without inflaming. Burn off all the
sulfate (CaSO4) required, either in the dihydrate (CaSO4 · carbon and ignite in a muffle furnace at 800 to 900 °C or using
2H2O) or hemihydrate (CaSO4 · 1⁄2 H2O) form. This procedure bright red heat over a Bunsen burner for 15 to 20 min. Dry the
assumes that an insignificant amount of sulfate other than filtering crucibles by placing in a cold muffle furnace during
calcium sulfate is present. This test method is used to deter- warm-up or in a drying oven prior to igniting in a muffle
mine compliance to the gypsum and gypsum product specifi- furnace at 800 to 900 °C for 15 to 20 min.
cations. It is also commonly used in quality control work. NOTE 2—Thoroughly cleans crucibles before each use and heat in a
furnace at 800 to 900 °C and cool in a desiccator before taring.
14.3 Interference—This test method has been developed for
natural gypsum and for impurities generally found associated 14.4.8 Cool all crucibles in a desiccator and weigh to the
with natural gypsum. Synthetic gypsum will sometimes have nearest 0.0001 g.
an additional number of interfering elements and compounds, 14.5 Calculation—Multiply the weight of the precipitate by
and if so, this procedure will not give accurate results. This test 0.343 to determine the weight of sulfur trioxide (SO3). Calcu-
method has a number of interferences that theoretically affect late the SO3 to the percentage of sample as received or to the
the results. Co-precipitation and occlusion are problems if the dried sample as required.
solution is either too acidic or too basic. Calculations using 14.6 Precision and Bias—Neither the precision nor the bias
SO3 analysis are most accurate on samples that are known to be for the sulfur trioxide analysis has been determined.
completely hydrated or completely dehydrated.
15. Chlorides
14.4 Procedure:
14.4.1 Having properly selected and prepared the samples 15.1 Significance and Use—Small amounts of chlorides in
as specified in Section 4, weigh a representative specimen of gypsum or gypsum products often have a detrimental effect on
approximately 0.5 g, to the nearest 0.0001 g. their use. This procedure is used to measure the amount of
14.4.2 Place the weighed sample into a 400-mL beaker. Add chlorides present and report it as sodium chloride.
50 mL of HCl (1 + 5). Boil and disperse with the flattened end 15.2 Procedure:
of a glass rod while stirring until the sample is completely 15.2.1 Weigh approximately 20.0 g of sample as prepared in
broken down. Add approximately 100 mL boiling water and Section 4 to 0.001 g and transfer to a 400-mL beaker. Add 150
continue boiling for 15 min, with this step to be extended as mL of water, stir, and heat to just below the boiling point.
required, so the combined boiling time is not less than 1 h. Cover with a watch glass and maintain at just below boiling
14.4.3 Using filter paper, filter into a clean 600-mL flask and (not less than 80 °C) for 1 h with occasional stirring. Filter with
rinse the 400-mL beaker thoroughly with hot distilled water. suction on a Buchner funnel fitted with a medium filter paper.
Carefully wash the sides of the 400-mL beaker while wiping Wash the residue with four 20-mL portions of hot water.
the insides with a rubber-tipped glass rod making sure all 15.2.2 Add 2 drops of phenolphthalein indicator solution to
splatters and insoluble are washed into the filter paper. Dry and the filtrate. If the filtrate fails to turn pink, add 0.1 NNaOH
burn off the filter paper leaving the residue to be dried and solution dropwise with stirring until a faint pink color devel-
weighed for insoluble matter, if this test method is not ops. Add 0.1 NHNO3 dropwise until the pink color just
otherwise conducted. disappears.
14.4.4 Dilute the filtrate to 400 to 500 mL. Add 1 to 2 drops 15.2.3 If the chloride content is very low, transfer the entire
of 0.1 % methyl red indicator. Prepare a 400 to 500-mL sample filtrate quantitatively to a 400-mL beaker and proceed as
of 0.05 to 0.1 NHCl. Add 1 to 2 drops of 0.1 % methyl red described in 15.2.4. If larger amounts of chloride are expected,
indicator. Compare the color of this solution to the color of the transfer the filtrate quantitatively to a 250-mL volumetric flask,
filtrate. Dilute the filtrate or add HCl (1 + 5) solution as cool to room temperature, and dilute to 250 mL. Take a suitable
necessary to match the pH of the 0.05 to 0.1 NHCl solution. aliquot, transfer to a 400-mL beaker, and dilute to a volume of
14.4.5 Boil the filtrate solution and add 20 mL of near- 100 to 250 mL.
boiling 10 % barium chloride solution, preferably with the help 15.2.4 Place the beaker containing the sample on a white
of a pipette, drop by drop while stirring. The barium chloride surface, add 0.5 mL (10 drops) of K2CrO4 solution and titrate
solution should be prepared not less than one day before use. with AgNO3 solution using a micro buret having a 10-mL
Continue boiling the solution for 10 to 15 min and digest hot capacity and graduated in divisions of 0.02 mL. Titrate until a
for 3 h or until the precipitate settles. faint but definite orange color is visible.
14.4.6 Filter and wash with approximately 125 to 150 mL of 15.2.5 Perform a blank titration using the same volume of
hot water to render the precipitate chloride free. Test the filtrate water as the sample volume and the same amount of K2CrO4
for chloride by collecting a small amount and adding a few solution. Titrate to the same color as obtained with the sample.
drops of 0.1 N AgNO3 solution. A white precipitate indicates 15.3 Calculation—Subtract the volume of AgNO3 solution
more washing is needed. Alternately, use filtering crucibles for used for the blank titration from the volume used for the
quick filtering if the particular crucibles to be used are tested sample to give the net titration. A 1-mL net titration is

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 C471M − 01 (2012)
equivalent to 0.002923 g of sodium chloride (NaCl). Calculate ALTERNATIVE PROCEDURE FOR ANALYSIS FOR
the NaCl as a percentage of the sample as received or the dried CALCIUM SULFATE BY THE AMMONIUM ACETATE
sample as required. METHOD7
15.4 Precision and Bias—Neither the precision nor the bias 17. Significance and Use
for the chloride analysis has been determined.
17.1 This test method covers the determination of calcium
16. Report sulfate in gypsum and gypsum products by extraction with
16.1 Report the results obtained in the analysis as follows: ammonium acetate solution.
Percent 18. Reagents and Materials
Free water ...
Combined water ... 18.1 Ammonium Acetate Solution—Dissolve 454 g of am-
Carbon dioxide (CO2) ... monium acetate in 2 L of water. Add sufficient NH4OH to make
Silicon dioxide (SiO2) and insoluble matter ...
Iron and aluminum oxides (Fe2O3 + Al2O3) ... the solution distinctly ammoniacal, using phenolphthalein as
Lime (CaO) ... the indicator.
Magnesium oxide (MgO) ...
Sulfur trioxide (SO3) 18.2 Ammonium Hydroxide Wash Solution— Dilute 100 mL
Sodium chloride (NaCl) ... of concentrated ammonium hydroxide (NH4OH, sp gr 0.90) to
Total 100.00±
1 L with water.
NOTE 3—Since it is frequently advisable to recalculate the results
obtained in the chemical analysis in order that they may be more 18.3 Filter Aid—Diatomaceous silica, analytical grade.
enlightening, the following is submitted for consideration: 18.4 Phenolphthalein Indicator Solution.
(1) Multiply the percentage of combined water by 4.778 to obtain
purity or percentage gypsum. To calculate the percentage of 19. Procedure Using Gooch Crucible
CaSO4 · 1⁄2 H2O in plasters, multiply the percentage of gypsum by 0.8430.
(2) Multiply the percentage of combined water by 2.222 to obtain the 19.1 Weigh rapidly approximately 4 g of the well-mixed
amount of SO3 combined as gypsum. sample and transfer to a 600-mL beaker. Make all weighings to
(3) Subtract the result obtained in (2) from the total SO3 found by 0.001 g, except weigh the crucibles and their contents to
analysis to obtain the excess SO3.
(4) Multiply the excess SO3 by 1.700 to obtain the percentage
0.0001 g.
anhydrite, CaSO4. 19.2 Without delay, weigh approximately 1 g of the well-
(5) Multiply the percentage of gypsum found in (1) by 0.3257 to obtain mixed sample in a tared weighing bottle having a ground-glass
the percentage of CaO combined as gypsum.
(6) Multiply the percentage of anhydrite found in (4) by 0.4119 to stopper. Dry the sample and weighing bottle to constant weight
obtain the percentage of CaO combined as anhydrite. at 45 °C. Stopper weighing bottles immediately upon removal
(7) Add (5) and (6) together. Then subtract this result from the total from the oven in order to prevent absorption of moisture from
CaO percentage found by analysis. the air upon cooling.
(8) Multiply the excess CaO percentage by 1.785 to obtain the
percentage of calcium carbonate. 19.3 If the percentage by weight of combined water held by
(9) Multiply the percentage of MgO by 2.091 to obtain the percentage the calcium sulfate is required, heat the sample and weighing
of magnesium carbonate. bottle to constant weight at 220 °C.
NOTE 4—Having made the calculations in Note 3, the results may be
reported as follows: 19.4 To the contents of the 600-mL beaker (19.1), add 350
Percent mL of the ammonium acetate solution, and stir the mixture
Gypsum (CaSO4·2H2 O) ... thoroughly to loosen all of the solid matter from the bottom of
Anhydrite (CaSO4 natural and manufactured) (Note 3) ...
Silicon dioxide and insoluble (SiO2 + Ins.) ...
the beaker. Add 0.2000 g of redried diatomaceous silica to the
Iron and aluminum oxide (R2O3) ... mixture. Heat the beaker and contents to 70 °C on a steam or
Calcium carbonate (CaCO3) ... hot water bath, and maintain at that temperature for 30 min,
Magnesium carbonate (MgCO3) ...
Sodium chloride (NaCl) ...
while stirring frequently. During heating, keep the solvent
Total 100.00± ammoniacal by additions of NH4OH and phenolphthalein, if
indicated. Meanwhile, heat a supply of the ammonium acetate
NOTE 5—The presence of the different forms of CaSO4 may be
determined by a microscopic examination. A paper titled “Gypsum solution to 70 °C, keeping it also distinctly ammoniacal. Filter
Analysis with the Polarizing Microscope” containing suggested methods the mixture, with suction, through a tared Gooch crucible,
can be found in ASTM STP 861.6 stirring frequently during filtration to keep the diatomaceous

6 7
Green, George W., “Gypsum Analysis with the Polarizing Microscope,” The This procedure was developed by L. S. Wells and W. F. Clarke, National Bureau
Chemistry and Technology of Gypsum, ASTM STP 861, ASTM, 1984, pp. 22–47. of Standards, and modified by B. E. Kester, United States Gypsum Co.

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 C471M − 01 (2012)
earth suspended in the liquid. Wash the Gooch crucible where:
containing the residue with five 10-mL portions of the warm F = weight of sample, corrected for loss on heating to
acetate solution, draining thoroughly after each washing. Wash constant weight at 45 °C,
in the same manner with eight 10-mL portions of the NH4OH G = weight of dried crucible and contents (19.4) or weight
wash solution. Take care to wash the upper walls of the Gooch of weighing bottle and contents (20.2), and
crucible. Drain the crucible dry with suction, place in an oven H = weight of crucible plus diatomaceous silica used as
at 70 °C, and dry to constant weight (Note 6). Allow the filter aid (19.4), or weight of weighing bottle, diatoma-
crucible to cool in a desiccator before weighing. ceous silica used as a filter aid and the weight of filter
NOTE 6—Avoid overheating in all oven drying of ammonium acetate
paper (20.2).
residues; that is, place crucibles well away from the heating elements. This
is of particular importance for samples high in impurities, as these 22. Precision and Bias
impurities often have water of hydration that is lost on local overheating. 22.1 Neither the precision nor the bias for the analysis of
20. Procedure Using Tared Filter Papers calcium sulfate by the ammonium acetate method has been
NOTE 7—This procedure is suggested where several samples are to be determined.
analyzed at once. It has been found that gravity filtration on six samples
will proceed as rapidly as it is possible to handle the samples. ALTERNATIVE PROCEDURE FOR ANALYSIS FOR
SODIUM CHLORIDE BY THE COULOMETRIC
20.1 Dry a quarter-folded, 110-mm quantitative filter paper
METHOD8
overnight at 70 °C in a wideform, glass-stoppered, 30 by
60-mm weighing bottle. After drying, cool the weighing bottle 23. Significance and Use
and paper in a desiccator, and weigh.
23.1 This test method covers the determination of sodium
20.2 Treat the sample exactly as described in 19.1, 19.2, and chloride in gypsum and gypsum products by the coulometric
19.4 prior to the filtration. Filter the mixture by gravity through method.
a 70-mm glass funnel, stirring frequently during filtration to
keep the diatomaceous silica suspended in the liquid. Wash the 24. Interferences
filter paper and residue with five 10-mL portions of warm 24.1 The presence of sulfide, sulfhydryl, or other silver
acetate solution, draining thoroughly after each washing. Wash reactive substances will lead to high results. Such interfering
in the same manner with eight 10-mL portions of the NH4OH substances are removed by alkaline oxidation with hydrogen
wash solution. After final draining, replace the paper and peroxide.
residue in the weighing bottle, and dry at 70 °C to constant
weight. Cool the weighing bottle, paper, and residue in a 25. Apparatus
freshly prepared desiccator before weighing; this is essential, 25.1 Chloride Meter:
due to the hygroscopic character of paper. 25.1.1 The instrument shall be equipped to measure the
21. Calculation concentration of dissolved chloride in aqueous solutions by the
coulometric method.
21.1 Calculate the percentage of loss in weight at 45 °C 25.1.2 The instrument shall be capable of measuring chlo-
(free water) as follows: ride concentrations in the range from 10 to 260 mg/L with a
Loss in weight at 45 7C, % 5 @ ~ A 2 B ! /C # 3 100 (3) repeatability of 6 1 mg/L.
where: 26. Reagents
A = original weight of sample and weighing bottle, 26.1 Acid Buffer Solution—Dissolve 100 mL of 99.5 %
B = weight of sample and weighing bottle dried to constant
acetic acid (HC2H3O2) and 5.5 mL of concentrated nitric acid
weight at 45 °C, and
(sp gr 1.42) in approximately 200 mL of water and dilute to
C = original weight of sample.
500 mL.
Calculate the weight of the 4-g sample (19.1), corrected for
loss on heating to constant weight at 45 °C. 26.2 Diluted Standard Solution (100 mg Cl/L)—Dilute 5.00
mL of stock standard solution to 500 mL.
21.2 Calculate the percentage of combined water as follows:
26.3 Gelatin Solution—Add 2.5 g of gelatin and 0.5 g of
Combined water, % 5 @ ~ B 2 D ! / ~ B 2 E ! # 3 100 (4) thymol blue to 250 mL of water and dissolve by stirring
where: continuously while bringing to a boil. With the solution just
B = weight of sample and weighing bottle dried to constant boiling, continue stirring until all the thymol blue is dissolved.
weight at 45 °C, Add 0.5 g of thymol, cool, and dilute the solution to 500 mL.
D = weight of sample and weighing bottle dried to constant NOTE 8—The gelatin solution holds the precipitated silver chloride
weight at 220 °C, and (AgCl) in suspension and also indicates the presence of the acid buffer.
E = weight of weighing bottle. The solution will keep for 3 months at room temperature or longer if
refrigerated. Warm the refrigerated solution to room temperature before
21.3 Calculate the percentage of CaSO4 · nH2O on the basis use.
of the sample dried to constant weight at 45 °C as follows:
CaSO 4 ·nH2 O, % 5 @ F 2 ~ G 2 H ! /F # 3 100 (5) 8
This procedure was developed by Westroc Industries Limited.

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26.4 Stock Standard Solution (10 g Cl/L)—Dissolve 8.240 g by the use of this method on plaster and sand from the same sources as
of dried sodium chloride (NaCl) in water and dilute to 500 mL. those from which the plaster to be analyzed was originally prepared.

31. Significance and Use

27. Procedure
31.1 This test method is used for determining the sand
27.1 Weigh 20.0 g of the well-mixed sample and transfer to content of samples of aggregated plaster taken from job sites to
a 150-mL beaker. determine compliance with Specification C842.
27.2 Add 50 mL of water, boil, allow the solid material to
settle, and filter off the solution. Add an additional 50 mL of 32. Reagents
water to the solids, boil, and pour the contents of the beaker 32.1 Ammonium Acetate (250 g/L)—Dissolve 250 g of
into the filter. Wash the residue with 100 mL of hot water, ammonium acetate (NH4C2H3O2) in water and dilute to 1 L.
adding the washing to the filtrate. Cool and dilute with water to
32.2 Ammonium Hydroxide (1 + 59) —Mix 1 volume of
250 mL.
concentrated ammonium hydroxide (NH4OH) (sp gr 0.90) with
27.3 Switch on the chloride meter and allow a period of 25 59 volumes of water.
min before use. Set the counter to zero.
27.4 Place a magnetic stirring bar in the test beaker, add 10 33. Sampling
mL of diluted standard solution, 3 mL of acid buffer solution, 33.1 Where plaster to be tested is part of a two-coat or
and 5 drops of gelatin solution. Place the test beaker on the three-coat plastering operation, take the sample for analysis
platform and lower the electrodes into the solution. Press the from that portion of the entire plaster sheet that comprises the
“start” button until the pilot light is extinguished. The counter single coat being tested. Separate succeeding coats of plaster
will begin to register after a few seconds. Do not remove the by use of a stiff putty knife or similar implement. Not less than
electrodes from the sample until the pilot light comes on. Read 500 g shall be taken as a sample, the sample preferably being
the chloride content from the counter. If a reading of 100 6 1 obtained from different sections of the wall or ceiling under
mg Cl/L is not obtained, refer to the manufacturer’s instruction examination.
manual. Reset the counter to zero.
34. Procedure
27.5 Repeat the procedure used in 27.4, using 10 mL of the
sample solution instead of the diluted standard solution. Read 34.1 In a clean porcelain mortar, grind the set plaster sample
the result as milligrams of chlorine per litre. When all tests are to the size of the largest sand particles present, or smaller, so
completed, lower the electrodes into reagent water. that approximately 100 % of the sample will pass a 2.36-mm
(No. 8) sieve. Fine grinding makes solution of the gypsum
28. Calculation faster. Place approximately 200 g of the ground sample in a
porcelain casserole or evaporating dish, and calcine on a sand
28.1 Calculate the amount of NaCl as a percentage of the bath. Stir the sample continuously with a thermometer during
sample as received or dried sample as follows: the heating, and adjust the rate of heating so that 20 to 30 min
NaCl, % 5 0.00206 3 A (6) will be required to raise the temperature of the sample to 160
6 5 °C. Cool the sample to room temperature in a desiccator.
where:
A = chloride meter reading, mg Cl/L. 34.2 After cooling, weigh accurately 20 6 0.05 g of the
calcined sample into a 600-mL beaker. Add 300 to 350 mL of
29. Precision and Bias NH4C2H3O2 solution. If acidic to litmus paper, add a few
millilitres of NH4OH (1 + 59) to the stock NH4C2H3O2 solu-
29.1 Neither the precision nor the bias for the sodium tion to render it slightly alkaline prior to the addition to the test
chloride analysis by the coulometric method has been deter- sample.
mined.
34.3 Warm the suspension to a temperature of 70 6 5 °C
DETERMINATION OF SAND IN SET PLASTER and stir continuously for 20 to 30 min. Filter the warm
suspension with the aid of suction through a small Büchner
30. Summary of Test Method funnel or Gooch crucible in which filter paper has previously
been placed. Refilter the first 100 mL of the filtrate. Wash the
30.1 This test method for the determination of the sand
sand remaining in the beaker onto the filter with an additional
content of set gypsum plaster requires for accurate results the
100 mL of warm ammonium acetate solution. Wash the beaker
following determinations:
and residue with 200 to 300 mL of water, dry the funnel and
30.1.1 Determination of the percentage of insoluble matter
sand at 100 °C to constant weight. The weight of the residue is
in the sand used with the plaster,
the weight of insoluble matter.
30.1.2 Determination of the percentage of insoluble matter
in the gypsum neat plaster, and 34.4 Insoluble Matter in Sand—Determine the weight of
30.1.3 Determination of the percentage of insoluble matter insoluble matter in sand as described in 34.1-34.3, except that
in the sanded calcined plaster. no grinding of the sample is necessary.
NOTE 9—If samples of the original gypsum neat plaster and the sand are 34.5 Insoluble Matter in Gypsum Neat Plaster—Determine
not available, an approximation of the insoluble matter may be obtained the weight of insoluble matter in the gypsum neat plaster as

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 C471M − 01 (2012)
described in 34.1-34.3, except that only a 5-g sample is 150-µm sieve. To avoid loss of the fine particles of fiber, make
required and no grinding of the sample is necessary. the transfer from the pan to the 150-µm sieve by several stages
of washing, stirring the charge, and quickly pouring upon the
35. Calculation sieve the fiber flotations, repeating the elutriation procedure
35.1 Insoluble Matter in Plaster—Multiply by 5 the weight several times. Examine the fiber collected on the 150-µm sieve
of the insoluble matter obtained as described in 34.3 to obtain and repeat the elutriation if necessary.
the percentage of insoluble matter in sanded plaster. 38.2 Dry the sieves (or sieve) and the residue contained
35.2 Insoluble Matter in Sand—Multiply by 5 the weight of thereon overnight in an oven maintained at a temperature of 45
the insoluble matter in sand obtained as described in 34.4 to °C. Carefully invert the sieves, or sieve, over a piece of white
obtain the percentage of insoluble matter in sand. paper, and transfer the residual material to the paper by
brushing the bottom of the inverted sieve. Examine the
35.3 Insoluble Matter in Gypsum Neat Plaster—Multiply by
transferred material visually, noting whether the separation of
20 the weight of the insoluble matter in gypsum neat plaster
fibers from plaster has been complete. Then transfer the
obtained as described in 34.5 to obtain the percentage of
material to a weighed platinum crucible and dry to constant
insoluble matter in gypsum neat plaster.
weight at a temperature of 45 °C. If the previous visual
35.4 Calculate the percentage of sand in the sanded plaster examination of the charge on the white paper showed that the
as follows: fiber was practically free of particles of plaster, report as the
X 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 100 (7) percentage of fiber the weight of the fiber dried at 45 °C,
divided by 100. If, on the other hand, the visual examination
revealed the presence of an appreciable quantity of plaster
where:
associated with the fiber, carefully ignite the contents of the
X = % of sand in sanded plaster, crucible to constant weight. In this case, report as the percent-
A = % of insoluble matter in the sand, age of fiber the loss on ignition, divided by 100.
B = % of insoluble matter in the gypsum neat plaster, and
39. Precision and Bias
C = % of insoluble matter in the sanded plaster.
39.1 Neither the precision nor the bias for the analysis of
35.5 To express the results as a ratio of the parts of sand per wood-fiber content in wood-fiber gypsum plaster has been
part of plaster by weight, use the following equation: determined.
Ratio of sand to plaster 5 X/ ~ 100 2 X ! (8)
OPTIONAL PROCEDURE FOR ANALYSIS FOR
NOTE 10—The results obtained by the above procedure indicate the SODIUM BY THE ATOMIC ABSORPTION METHOD
amount of sand originally mixed with the gypsum neat plaster before it
had been gaged with water or set. 40. Significance and Use
36. Precision and Bias 40.1 This test method covers the determination of sodium in
gypsum and gypsum products by the atomic absorption
36.1 Neither the precision nor the bias for the analysis of method.
sand in set plaster has been determined.
41. Interferences
WOOD-FIBER CONTENT IN WOOD-FIBER GYPSUM
PLASTER 41.1 Sodium is partially ionized in the air-acetylene flame.
The effects of ionization will be significantly overcome by the
37. Significance and Use addition of 1 to 2 g/L of another alkali to blanks, standards, and
37.1 This test method is used to determine the weight of samples. Alternatively, use the air-hydrogen flame, as it pro-
wood fiber in wood-fibered plaster. duces less ionization and less visible emission than the
air-acetylene flame.
38. Procedure
42. Apparatus
38.1 Place a 100-g sample of wood-fiber plaster, prepared as
described in Section 4 on a 600-µm (No. 30) sieve4 nested over 42.1 Atomic Absorption Spectrophotometer:
a 150-µm (No. 100) sieve.4 Wash the plaster on the 600-µm 42.1.1 The instrument shall be equipped to measure the
sieve with a stream of cold water, removing the 600-µm sieve concentration of dissolved sodium in aqueous solutions using
when the fiber on it is practically or entirely free of plaster. either the air-acetylene or air-hydrogen flame.
Next, wash the material on the 150-µm sieve until the bulk of 42.1.2 The instrument shall be capable of measuring sodium
the plaster has been washed through the sieve and the residue concentrations within the optimum analytical range of 0.1 to
is mainly fiber. Transfer the material retained on the 150-µm 0.5 absorbance units while providing a coefficient of variation
sieve to a 300-mL, vitreous enamel, lipped pan, adding the of approximately 0.5 to 2 %.
charge on the 600-µm sieve if the fiber contains any adhering
particles of plaster. Elutriate the material in the pan (purify by 43. Reagents
washing and straining, effecting as clean a separation of fiber 43.1 Solvent—Use deionized water to prepare all solutions.
from plaster as is practical), catching the elutriated fibers on a If an alkali is to be included for the purpose of suppressing

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sodium ionization, it is most convenient to add it to the solvent OPTIONAL PROCEDURE FOR ANALYSIS FOR
at the start. In this way a constant concentration of alkali in SODIUM BY FLAME PHOTOMETRY
blank, standards, and sample solution is ensured.
47. Significance and Use
43.2 Stock Standard Solution (1.000 g Na/L)—Dissolve
2.5418 g of dried sodium chloride (NaCl) in water and dilute to 47.1 This test method covers the determination of sodium in
1 L with water. gypsum and gypsum products by flame photometry. This test
method is based on Methods D1428.
43.3 Dilute Standard Solutions—Prepare dilute standard
solutions bracketing the absorbance range of the dilute sample 48. Interferences
solution, using the stock standard solution. (Solutions having a 48.1 Radiation interferences caused by elements other than
concentration less than approximately 0.500 g/L are unstable that being determined are the greatest contributor to error in
for periods of more than one day.) flame photometry. Some effects are positive and others nega-
tive. Of the elements encountered in this analysis, the greatest
44. Procedure effect is that of one alkali metal on another. The foreign-
44.1 Take 18 g of the well-mixed sample and transfer to a element effects cannot be entirely compensated for without
150-mL beaker. employing calibration standards closely duplicating the com-
position of the sample. However, the effects are minimized by
44.2 Add 50 mL of water, boil, allow the solids to settle, and operating at the lowest practical sodium concentration range or
decant the supernatant liquid into a filter. Add an additional 50 by removal of the interfering elements. For example, aluminum
mL of water to the solids, boil, and pour the contents of the has a depressing effect on alkali-metal emission, which is of
beaker into the filter. Wash the residue with 100 mL of hot serious consequence. Remove aluminum from the extraction
water, adding the washing to the filtrate. Cool the filtrate to liquid prior to flame photometry if its concentration has been
room temperature and dilute to 500 mL in a volumetric flask to found, by preliminary tests, to exceed that of the sodium.
make the stock sample solution. Take 10 mL of the solution 48.2 Self-absorption causes the curve of intensity versus
and make up to 500 mL in a second volumetric flask, to make concentration to decrease its slope at higher concentrations,
the dilute sample solution. tending to reduce accuracy. Bracketing the unknown by known
44.3 Determine the absorbance readings on the dilute stan- standard solutions tends to minimize this interference.
dard solutions and the solvent blank at a wavelength of 589.0
49. Apparatus and Materials
to 589.6 nm, following the manufacturer’s instruction manual.
Subtract the absorbance value for the blank from the absor- 49.1 Flame Photometer—The instrument shall consist of an
bance values for the dilute standard solutions and prepare a atomizer and burner; suitable pressure-regulating devices and
curve relating sodium concentration in milligrams per litre to gages for fuel and air or oxygen; an optical system, consisting
absorbance values. of suitable light-dispensing or filtering devices capable of
preventing excessive interference from light of wavelengths
NOTE 11—If the absorbance of the dilute sample solution is known to other than that being measured; and a photosensitive indicating
lie within the linear range, that is, the sodium concentration is below device.
approximately 1 mg/L only one standard and the solvent blank are needed
to prepare the curve. 49.2 Supply of Fuel and Air or Oxygen— The supplies of
fuel and air or oxygen shall be maintained at pressures
44.4 Determine absorbance readings on the dilute sample somewhat higher than the controlled operating pressure of the
solution using the same technique, followed with the dilute instrument.
standard solutions. The concentration of sodium in the dilute
sample solution in milligrams per litre is then found by 50. Reagents
consulting the standard curve.
50.1 Prepare the following stock solutions from reagents
45. Calculation that have been dried to constant weight at 105 °C. Store the
stock solutions in polyethylene or equally alkali-metal-free
45.1 Calculate the amount of NaCl as a percentage of the containers.
sample received or the dried sample as required as follows: 50.2 Sodium Chloride Solution (2.5418 g/L)—Dissolve
Sodium calculated as % NaCl 5 A 3 6.3553/S (9) 2.5418 g of sodium chloride (NaCl) in water and dilute to 1 L
with water. This stock standard solution contains 1.000 g/L of
where:
sodium ion.
A = concentration of dilute sample solution, mg/L, and
S = weight of sample, g. 50.3 Dilute Standard Solutions—Prepare dilute standard
solutions from stock standard solution, bracketing the expected
46. Precision and Bias sodium concentration range of the diluted sample extraction
liquid. For example, if the expected range of the sample
46.1 Neither the precision nor the bias for the analysis of extraction liquid is between 0 and 0.010 g/L, prepare eleven
sodium by the atomic absorption method has been determined. equally spaced standards in tenths of the maximum.

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51. Calibration of Instrument 52. Procedure
51.1 Select the proper photocell; the blue-sensitive photo- 52.1 Weigh 25 g of the well-mixed sample and transfer to a
tube having a range from 320 to 620 nm is required for sodium 150-mL beaker.
determination. Open the slit width to approximately one fourth 52.2 Add 50 mL of water, boil, allow the solid material to
of the maximum opening, set the instrument to the maximum settle, and decant the supernatant liquid into a filter. Add an
sensitivity range, and balance the meter to obtain electrical additional 50 mL of water to the solids, boil and pour the
equilibrium. contents of the beaker into the filter. Wash the residue with 75
51.2 Feed fuel and air or oxygen to the burner and ignite the mL of hot water, adding the washing to the filtrate. Cool and
emitted mixture. Adjust fuel and air or oxygen pressures and dilute with water to 200 mL in a volumetric flask to make the
follow the procedures for warm-up time prescribed by the stock sample solution.
instrument manufacturer. Set the scale-reading dial at approxi- 52.3 Take 5 mL of the stock sample solution and make up to
mately 95 % of full scale, introduce a solution containing the 100 mL in a volumetric flask to make the dilute sample
maximum amount of sodium in the range to be covered, and solution.
allow the emitted light to strike the photocell.
NOTE 13—If the concentration of sodium in the sample is found to be
51.3 Select the proper filter, if a filter-type instrument is greater than the maximum standard, further dilute sample solution with
used. For instruments employing spectral dispersing devices, water to bring the concentration within the range. If the concentration of
turn the wavelength dial back and forth slowly and carefully in sodium in the sample is less than one tenth of the value of the maximum
the vicinity of 589 nm until the galvanometer reaches a standard, prepare a new dilute sample solution from the stock sample
solution to bring the concentration within the range.
maximum deflection. This wavelength setting produces maxi-
mum sensitivity. Do not disturb the wavelength dial during the 52.4 Turn the instrument on and feed fuel and air or oxygen
test. to the burner. Ignite the gas mixture. For instruments with an
adjustment slit, set the width to the value determined as
51.4 Continue to atomize the maximum standard of the outlined in Note 12.
range to be covered, and set the scale-reading of the dial at
exactly full scale (100 or 1000) (Note 12). Adjust the gain so 52.5 Place the scale-reading dial at maximum. Atomize the
as to balance the galvanometer needle. sample and allow its emitted light to strike the photocell. Set
the wavelength to 589 nm as described and adjust the gain to
NOTE 12—For instruments equipped with a variable slit, carry out the balance the galvanometer. Determine the emission intensity of
procedure described above with the slit width between fully closed and
one fourth open for the preliminary test. In determining the proper slit
the sample.
width for optimum instrument performance, consideration must be given 52.6 Refer to the standard curve prepared above and read off
to the fact that the intensity of the emission line is approximately the concentration of sodium ion in the dilute sample solution in
proportional to the slit width, whereas continuous background intensity
increases as the square of the slit width. A decrease in slit width results in milligrams per litre.
decreased illumination of the phototube for a given concentration and is
compensated for by increasing the gain of the instrument. The most 53. Calculation
favorable operating conditions are obtained with the smallest slit width 53.1 Calculate the amount of NaCl as follows:
that does not result in instability of the galvanometer needle when it is set
to give full-scale reading with the maximum standard in the range to be Sodium, calculated as NaCl, % 5 A 3 0.04067 (10)
covered. When altering the slit width, determine the background by
atomizing a zero standard, and check for sensitivity setting and instrument where:
stability with the maximum standard in the range to be covered. Lower A = concentration of sodium, mg/L read off the standard
ranges require wider slit widths. Determine and record the optimum slit curve.
width for each range and element to be covered. Use these values in all
subsequent tests. 54. Precision and Bias
51.5 Determine the emission intensity of all standards. 54.1 Neither the precision nor bias of the analysis for
51.6 Plot emission intensity (scale reading) versus concen- sodium by flame photometry has been determined.
tration on linear graph paper. For the lower ranges, the curve
thus prepared approximates a straight line but sometimes will 55. Keywords
not intersect zero because of background intensity. At higher 55.1 ammonium acetate method; atomic absorption; chemi-
ranges, the curves show a decrease in slope with increasing cal analysis; coulometric method; flame photometry; gypsum;
concentration. Record on graphs all data in regard to slit width, gypsum concrete; gypsum board; gypsum products; plaster;
fuel pressure, and air or oxygen pressure. sand in set plaster; wood-fiber plaster

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 C471M − 01 (2012)
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