This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: C471M − 17a´1

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.

ε1 NOTE—Corrected Research Report number in December 2017.

1. Scope* 1.4 The values stated in SI units are to be regarded as the

1.1 These test methods cover the chemical analysis of standard.
gypsum and gypsum panel products, including gypsum ready- 1.5 This standard does not purport to address all of the
mixed plaster, gypsum wood-fibered plaster, and gypsum safety concerns, if any, associated with its use. It is the
concrete. responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.2 The test methods appear in the following order: mine the applicability of regulatory limitations prior to use.
Sections
Preparation of Sample 4
1.6 This international standard was developed in accor-
Complete Procedure 5 – 16 dance with internationally recognized principles on standard-
Alternative Procedure for Analysis of Free Water in 17 ization established in the Decision on Principles for the
Gypsum Using a Moisture Balance
Alternative Procedure for Analysis of Combined Water in 18
Development of International Standards, Guides and Recom-
Gypsum Using a Moisture Balance mendations issued by the World Trade Organization Technical
Alternative Procedure for Analysis for Calcium Sulfate by 19 Barriers to Trade (TBT) Committee.
Ammonium Acetate Method
Alternative Procedure for Analysis for Sodium Chloride by 20
the Coulometric Method 2. Referenced Documents
Determination of Sand in Set Plaster
Wood-Fiber Content in Wood-Fiber Gypsum Plaster
21
22
2.1 ASTM Standards:2
Optional Procedure for Analysis for Sodium by the Atomic 23 C11 Terminology Relating to Gypsum and Related Building
Absorption Method Materials and Systems
Optional Procedure for Analysis for Sodium by Flame 24
Photometry
C22/C22M Specification for Gypsum
Determination of Orthorhombic Cyclooctasulfur (S8) in 25 C28/C28M Specification for Gypsum Plasters
Ggypsum Panel Products—General Provisions C59 Specification for Gypsum Casting Plaster and Gypsum
Determination of Orthorhombic Cyclooctasulfur (S8) in 26
Gypsum Panel Products by Gas Chromatograph
Molding Plaster
Equipped with a Mass Spectrometer (GS/MS) C61 Specification for Gypsum Keene’s Cement
Determination of Orthorhombic Cyclooctasulfur (S8) in 27 C317/C317M Specification for Gypsum Concrete
Gypsum Panel Products by Gas Chromatograph
Equipped with an Electron Capture Detector (GC/ECD)
C778 Specification for Standard Sand
Determination of Orthorhombic Cyclooctasulfur (S8) in 28 C842 Specification for Application of Interior Gypsum Plas-
Gypsum Panel Products by High-performance Liquid ter
Chromatograph Equipped with and Ultraviolet Detector
(HPLC ⁄UV)
D1193 Specification for Reagent Water
D1428 Test Method for Test for Sodium and Potassium In
1.3 The text of this standard references notes and footnotes Water and Water-Formed Deposits by Flame Photometry
that provide explanatory material. These notes and footnotes (Withdrawn 1989)3
(excluding those in tables and figures) shall not be considered D2013 Practice for Preparing Coal Samples for Analysis
as requirements of the standard. E11 Specification for Woven Wire Test Sieve Cloth and Test
Sieves

1
These test methods are under the jurisdiction of ASTM Committee C11 on
2
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 [email protected]. For Annual Book of ASTM
Products. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2017. Published November 2017. Originally the ASTM website.
3
approved in 1961. Last previous edition approved in 2017 as C471M – 17. DOI: The last approved version of this historical standard is referenced on
10.1520/C0471M-17AE01. www.astm.org.

*A Summary of Changes section appears at the end of this standard

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 C471M − 17a´1
E177 Practice for Use of the Terms Precision and Bias in 4.3 Gypsum Plaster, (Specification C28/C28M).
ASTM Test Methods 4.3.1 Gypsum Ready-Mixed Plaster or Gypsum WoodFi-
E691 Practice for Conducting an Interlaboratory Study to bered Plaster—Screen the dried sample through a 150-µm
Determine the Precision of a Test Method (No. 100) sieve4 and discard the residue retained on the sieve.
Reweigh the remaining sample and calculate the percentage of
3. Terminology the dried sample. Reduce the sample in accordance with 4.1.5.
3.1 Definitions—Definitions shall be in accordance with Thoroughly blend and rehydrate the specimen in accordance
Terminology C11. with 4.1.4
4.3.2 Gypsum Neat Plaster or Gypsum Gauging Plaster—
3.2 Definitions: Reduce the dried sample in accordance with 4.1.5. Thoroughly
3.2.1 calibration standard, n—a chemical mixture contain- blend and rehydrate the specimen in accordance with 4.1.4.
ing a known quantity of the analyte used to relate the measured
analytical signal to the concentration of the analyte. 4.4 Gypsum Casting and Molding Plaster, (Specification
C59)—Reduce the dried sample in accordance with 4.1.5.
3.2.2 dried sample, n—a sample devoid of free water. Thoroughly blend and rehydrate the specimen in accordance
3.2.3 internal standard, n—a chemical used in the quantifi- with 4.1.4.
cation of S8 by monitoring and adjusting for minor variances in
4.5 Gypsum Keene’s Cement, (Specification C61)—Reduce
instrument performance.
the dried sample in accordance with 4.1.5. Blend in no more
3.2.4 riffle, n—a hand feed sample divider device that than 1 % molding plaster or K2SO4 and rehydrate the specimen
divides the sample into parts of approximately the same in accordance with 4.1.4.
weight. (D2013)
4.6 Gypsum Concrete, (Specification C317/C317M)—
3.2.5 sample as received, n—a representative portion of raw Screen the dried sample through a 150-µm (No. 100) sieve4
gypsum or gypsum product in the state received by the testing and discard the residue retained on the sieve. Reweigh the
laboratory, including aggregates, impurities and water content. remaining sample and calculate the percentage of the dried
3.2.6 surrogate standard, n—a chemical used to account for sample. Reduce the sample in accordance with 4.1.5. Thor-
extraction efficiency of S8. oughly blend and rehydrate 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—Dry the sample in accordance with Section 7.
This will be the weight of the dried sample.
COMPLETE PROCEDURE
4.1.3 Crushing and Grinding—Crush and grind the sample
by hand with a mortar and pestle or by mechanical crushing 5. Apparatus
and grinding equipment to pass a 250-µm (No. 60) sieve. Take
care, 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 equip- bottles, lids and samples.
ment thoroughly between samples. Thoroughly remix the 5.2 Balance—Capable of weighing not less than 100 g at a
ground sample and store it in an airtight container to avoid precision of 0.001 g.
contamination. 5.3 Drying Oven—A mechanical convection oven set at 45
4.1.4 Rehydrating—Thoroughly blend and rehydrate 6 3°C.
samples which contain calcium sulfate in forms other than
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 and 5.5 Calcining Oven or Furnace—Capable of achieving and
recrush or grind it in accordance with 4.1.3. maintaining temperatures to not less than 1000°C.
4.1.5 Sample Reduction—Thoroughly mix and reduce large 5.6 Weighing Bottles—Borosilicate glass or ceramic con-
samples as required by quartering or by the use of a riffle to tainers with tightly sealable lids.
obtain a specimen of approximately 50 g.
5.7 Hot Plate—A controllable hot plate capable of heating
4.2 Gypsum (Specification C22/C22M)—Gypsum samples casseroles to approximately 120°C.
will be received in the form of rocks or powder, or both. If
necessary crush and reduce the entire dried sample in accor-
dance with 4.1.3 and 4.1.5. 4
Detailed requirements for this sieve are given in Specification E11.

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 C471M − 17a´1
5.8 Porcelain Casseroles—With a capacity of 50 to 100 mL. 6.1.16 Sulfuric Acid (1 + 6)—Carefully mix one volume of
5.9 Filtering Funnels. H2SO4 (sp gr 1.84) with six volumes of water.
6.1.17 Nitric Acid (0.1 N)—Mix 1.4 mL of HNO3 (sp gr
5.10 Filter Paper. 1.42) with 200 mL of water.
5.11 Porcelain Crucibles. 6.1.18 Phenolphthalein Indicator Solution—Dissolve 0.25 g
5.12 Mortar and Pestle. of phenolphthalein in 30 mL of methanol and dilute to 50 mL
with water.
5.13 Mechanical Jaw Crusher—Capable of crushing gyp- 6.1.19 Sodium Hydroxide Solution (0.1 N)—Dissolve 1 g of
sum rocks up to 50 mm diameter. sodium hydroxide (NaOH) in 250 mL of water.
5.14 Mechanical Grinder—Burr mill or equivalent capable 6.1.20 Water—Reagent water shall be in accordance with
of grinding the granular output of the jaw crusher specified in Specification D1193, type II. Specification D1193 gives the
5.13. following values for type II grade water.
Electrical conductivity, max, µS/cm at 298 K (25-C) 1.0
6. Reagents Electrical resistivity, min, MΩ·cm at 298 K (25-C) 1.0
Total organic carbon (TOC), max, µg/L 50.0
6.1 Purity of Reagents—Use reagent grade chemicals in all Sodium, max, µg/L 5.0
Chlorides max, µg/L 5.0
tests. Unless otherwise indicated, use reagents that conform to Total silica, max, µg/L 5.0
the specifications of the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are 7. Free Water
available.5 If it is necessary to use other grades, first ascertain 7.1 Significance and Use—The free water analysis deter-
that the reagent is of sufficiently high purity so that its use will mines the amount of free water contained in the sample as
not lessen the accuracy of the determination. opposed to chemically combined water, and prepares the
6.1.1 Ammonium Chloride (NH4Cl). sample for further analysis.
6.1.2 Ammonium Hydroxide (sp gr 0.90)—Concentrated
ammonium hydroxide (NH4OH). 7.2 Procedure:
6.1.3 Ammonium Nitrate (25 g/L)—Dissolve 25 g of ammo- 7.2.1 Weigh a sample of the material as received of not less
nium nitrate (NH4NO3) in water and dilute to 1 L. than 50 g to a precision of 0.001 g and spread it out in a thin
6.1.4 Ammonium Oxalate ((NH4)2C2O4). layer in a suitable vessel. Place in an oven and dry at 45 6 3°C
6.1.5 Barium Chloride (100 g/L)—Dissolve 100 g of barium until constant mass has been obtained. The samples are to be
chloride (BaCl2·2H2O) in water and dilute to 1 L. cooled in a desiccator prior to each weighing. The loss of
6.1.6 Calcium Chloride (CaCl2)—Anhydrous Calcium weight corresponds to the free water.
Chloride with a combined water of not more than 5 %. 7.2.2 Retain the sample in a sealed container or in the
6.1.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- desiccator for further analysis.
chloric acid (HCl). 7.3 Calculation and Report—Calculate and report loss in
6.1.8 Hydrochloric Acid (1 + 4)—Mix one volume of HCl weight as a percentage of the sample as received or of the dried
(sp gr 1.19) with four volumes of water. sample as required.
6.1.9 Hydrochloric Acid (1 + 5)—Mix one volume of HCl 7.4 Precision and Bias:
(sp gr 1.19) with five volumes of water. 7.4.1 The precision of this test method is based on an
6.1.10 Nitric Acid (sp gr 1.42)—Concentrated nitric acid interlaboratory study of ASTM C471M, Standard Test Methods
(HNO3). for Chemical Analysis of Gypsum and Gypsum Products,
6.1.11 Potassium Chromate Solution (100 g/L)—Dissolve conducted in 2016. Each of 17 laboratories analyzed two
5 g of potassium chromate (K2CrO4) in 50 mL of water, mix, different gypsum sample types. Every “test result” represents
add ten drops of 0.05 N silver nitrate (AgNO3) solution, allow an individual determination, and all participants reported five
to stand for 5 min, and filter. test results per material. Practice E691 was followed for the
6.1.12 Potassium Permanganate (5.6339 g/L)—Dissolve design and analysis of the data; the details are given in ASTM
5.6339 g of potassium permanganate (KMnO4) in water and Research Report No. C11-1003.6
dilute to 1 L. 7.4.1.1 Repeatability (r)—The difference between repetitive
6.1.13 Silver Nitrate, Standard Solution (0.05 N)—Prepare results obtained by the same operator in a given laboratory
and standardize a 0.05 N silver nitrate (AgNO3) solution. applying the same test method with the same apparatus under
6.1.14 Sodium Ammonium Phosphate—(NaNH4HPO4). constant operating conditions on identical test material within
6.1.15 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric short intervals of time would in the long run, in the normal and
acid (H2SO4). correct operation of the test method, exceed the following
values only in one case in 20.
(1) Repeatability can be interpreted as maximum difference
5
Reagent Chemicals, American Chemical Society Specifications , American between two results, obtained under repeatability conditions,
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia Supporting data have been filed at ASTM International Headquarters and may
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, be obtained by requesting Research Report RR:C11-1003. Contact ASTM Customer
MD. Service at [email protected].

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 C471M − 17a´1
that is accepted as plausible due to random causes under 8.3.3 Place the specimens in the calcining oven with the lids
normal and correct operation of the test method. placed loosely on each bottle or crucible for 2 h or until
(2) Repeatability limits are listed in Table 1. constant weight has been obtained.
7.4.1.2 Reproducibility (R)—The difference between two 8.3.4 Place the lids tightly on the weighing bottles, remove
single and independent results obtained by different operators from the oven, and place in the desiccator to cool to room
applying the same test method in different laboratories using temperature.
different apparatus on identical test material would, in the long 8.3.5 Weigh each specimen to a precision of 0.0001 g and
run, in the normal and correct operation of the test method, record the weights.
exceed the following values only in one case in 20. 8.3.6 Retain the residues for carbon dioxide analysis.
(1) Reproducibility can be interpreted as maximum differ-
ence between two results, obtained under reproducibility 8.4 Calculation and Report—Calculate and report the aver-
conditions, that is accepted as plausible due to random causes age loss in weight of the three specimens as a percentage of the
under normal and correct operation of the test method. sample as received or of the dried sample, as required, to the
(2) Reproducibility limits are listed in Table 1. nearest 0.001 g and record the tare weights.
7.4.1.3 The above terms (repeatability limit and reproduc- 8.5 Precision and Bias:
ibility limit) are used as specified in Practice E177. 8.5.1 The precision of this test method is based on an
7.4.1.4 Any judgment in accordance with statements 7.4.1.1 interlaboratory study of ASTM C471M, Standard Test Methods
and 7.4.1.2 would have an approximate 95 % probability of for Chemical Analysis of Gypsum and Gypsum Products,
being correct. conducted in 2016. Each of 17 laboratories analyzed two
7.4.2 Bias—At the time of the study, there was no accepted different gypsum sample types. Every “test result” represents
reference material suitable for determining the bias for this test an individual determination, and all participants reported five
method, therefore no statement on bias is being made. test results per material. Practice E691 was followed for the
7.4.3 The precision statement was determined through sta- design and analysis of the data; the details are given in ASTM
tistical examination of 660 results, from 15 participating Research Report No. C11-1003.6
laboratories, on two types of gypsum materials.
8.5.1.1 Repeatability (r)—The difference between repetitive
7.4.4 To judge the equivalency of two test results, it is
results obtained by the same operator in a given laboratory
recommended to choose the material closest in characteristics
applying the same test method with the same apparatus under
to the test material.
constant operating conditions on identical test material within
8. Combined Water short intervals of time would in the long run, in the normal and
correct operation of the test method, exceed the following
8.1 Significance and Use—The combined water analysis
values only in one case in 20.
determines the percent of chemically combined water and is
(1) Repeatability can be interpreted as maximum difference
used to calculate the purity of gypsum or the amount of
between two results, obtained under repeatability conditions,
gypsum or gypsum plaster in gypsum products.
that is accepted as plausible due to random causes under
8.2 Interferences—Some materials, such as organic and normal and correct operation of the test method.
hydrated compounds that decompose within the same tempera- (2) Repeatability limits are listed in Table 2.
ture range as gypsum, will cause high results. When the 8.5.1.2 Reproducibility (R)—The difference between two
maximum temperature is exceeded, some carbonates undergo single and independent results obtained by different operators
decomposition, which will result in high results. applying the same test method in different laboratories using
8.3 Procedure: different apparatus on identical test material would, in the long
8.3.1 For each sample, place three weighing bottles with run, in the normal and correct operation of the test method,
lids in the preheated calcining oven or furnace and heat for 2 h exceed the following values only in one case in 20.
at 215 to 230°C. Place in the desiccator and allow to cool to (1) Reproducibility can be interpreted as maximum differ-
room temperature. Weigh the bottles and lids to the nearest ence between two results, obtained under reproducibility
0.0001 g and record the tare weights. conditions, that is accepted as plausible due to random causes
8.3.2 Weigh out three specimens of approximately 5 g each under normal and correct operation of the test method.
of the sample as prepared in Section 4 and dried in Section 7 (2) Reproducibility limits are listed in Table 2.
to a precision of 0.0001 g in the previously tared weighing 8.5.1.3 The above terms (repeatability limit and reproduc-
bottles and record the total weight with lids. ibility limit) are used as specified in Practice E177.

TABLE 1 Free Water (in Accordance with Section 7)

Repeatability Reproducibility
Repeatability Reproducibility
AverageA Standard Standard
Material Limit Limit
Deviation Deviation
x̄ Sr SR r R
natural gypsum 0.0482 0.0102 0.0217 0.0286 0.0607
flue gas desulphogypsum (FGD) 8.1699 0.7639 1.9213 2.1388 5.3797
A
The average of the laboratories’ calculated averages.

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 C471M − 17a´1
TABLE 2 Combined Water in Accordance with Section 8
Repeatability Reproducibility
Repeatability Reproducibility
AverageA Standard Standard
Material Limit Limit
Deviation Deviation
x̄ Sr SR r R
natural gypsum 18.7931 0.4718 1.4501 1.3211 4.0604
flue gas desulphogypsum (FGD) 19.3946 0.5518 1.3044 1.5449 3.6523
A
The average of the laboratories’ calculated averages.

8.5.1.4 Any judgment in accordance with statements 8.5.1.1 9.4.3 Erlenmeyer Flask C, 250 mL, 24/20 ground-glass
and 8.5.1.2 would have an approximate 95 % probability of joint.
being correct. 9.4.4 Separatory Funnel D, with ground glass stopper and
8.5.2 Bias—At the time of the study, there was no accepted interchangeable hollow ground-glass joint. A delivery tube
reference material suitable for determining the bias for this test bent at the end extends into the sample flask approximately
method, therefore no statement on bias is being made. 15 mm from the bottom and is used to introduce acid into flask.
8.5.3 The precision statement was determined through sta- 9.4.5 Condenser E.
tistical examination of 660 results, from 15 participating
9.4.6 Gas-Washing Bottle F, 250 mL, with fitted disk
laboratories, on two types of gypsum materials.
containing distilled water to retain most of the acid volatilized
8.5.4 To judge the equivalency of two test results, it is
from the alkalimeter.
recommended to choose the material closest in characteristics
to the test material. 9.4.7 U-Tube G, containing mossy zinc to remove the last
traces of HCl.
9. Carbon Dioxide 9.4.8 Gas Washing Bottle H, 250 mL, with fritted disk,
9.1 Summary of Test Method—The sample is decomposed containing concentrated H2SO4 and trap I, to remove any SO3
with HCl and the liberated CO2 is passed through a series of mist that is carried over.
scrubbers to remove water and sulfides. The CO2 is absorbed 9.4.9 Absorption Bulb J, containing Anhydrone to remove
with Ascarite, a special sodium hydroxide absorbent, and the last traces of water vapor.
gain in weight of the absorption tube is determined and 9.4.10 CO2 Absorption Bulb, containing Ascarite filled as
calculated as percent CO2. follows: On the bottom of the bulb, place a layer of glass wool
9.2 Significance and Use—The carbon dioxide analysis is extending above the bottom outlet and on top of this a layer of
useful in estimating carbonates and organic carbon for chemi- Anhydrone approximately 10 mm thick; immediately above
cal balance. this place another layer of glass wool, then add Ascarite to
almost fill the bulb. Place a top layer of Anhydrone approxi-
9.3 Special Reagents: mately 10 mm thick on top of the Ascarite and top it off with
9.3.1 Magnesium Perchlorate Desiccant—For drying. a covering of glass wool.
9.3.2 Sodium Hydroxide Absorbent—A coarse sodium hy-
9.4.11 U-Guard Tube L, filled with Anhydrone in left side
droxide coated silica.
and Ascarite in right side.
9.4 Special Apparatus—The apparatus illustrated in Fig. 1 9.4.12 Purifying Jar M, Fleming, containing H2SO4.
consists of the following:
9.4.1 Purifying Jar A, Fleming, containing sulfuric acid. 9.5 Procedure:
9.4.2 Drying Tube B, U-shaped with side arms and glass- 9.5.1 After drying as described in 8 place the residue
stoppers. Side arms are shaped to hold rubber tubing. Contains obtained in the 250 mL Erlenmeyer flask (C). Connect the flask
Anhydrone on left side and Ascarite on right side. to the apparatus as shown in Fig. 1. Purge the system free of

FIG. 1 Apparatus for Carbon Dioxide Analysis

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 C471M − 17a´1
carbon dioxide by passing a current of CO2-free air through the not less than 20 min to do the evaporation. Make a blank
apparatus for 10 to 15 min. determination with one casserole in parallel. Cool to room
9.5.2 Weigh the absorption bulb to 0.0001 g and attach it to temperature.
the train. Remove the glass stopper from the separatory funnel, 10.3.3 Add enough hydrochloric acid (sp gr 1.19) to wet the
place 50 mL of dilute HCl (1 + 1) in the separatory funnel (D), solid residue. Add 20 mL of water, boil and filter through filter
and replace the stopper with the interchangeable hollow paper. Wash the filter paper thoroughly using not less than
ground-glass joint through which passes a tube for admitting 100 mL of room temperature water to render the precipitate
purified air. Open the stopcock of the separatory funnel and chloride free. The most effective washing technique is to use
admit air through the top of the funnel to force the hydrochloric many small quantities of wash water rather than fill the funnel
acid into the Erlenmeyer flask (C). to the brim two or three times. Test the filtrate for chloride by
9.5.3 Start cold water circulating through the condenser (E) collecting a small amount and adding a few drops of 0.1
and, with CO2-free air passing at a moderate rate through the normal silver nitrate (AgNO3) solution. A white precipitate
absorption train, place a small hot plate or gas burner under the indicates more washing is needed. Discard this test solution.
sample flask and boil for approximately 2 min. Remove the hot 10.3.4 Place all the filtrate back in the same casserole.
plate and continue the flow of purified air at approximately Evaporate to dryness and heat to 120°C for 1 h and cool. To the
three bubbles per second for 10 min to sweep the apparatus free cooled casserole add enough HCl (sp gr 1.19) to wet the solid
of CO2. Close the absorption bulb, disconnect it from the train residue. Add 50 mL of water and boil.
and weigh, opening the stopper momentarily to equalize the 10.3.5 Wash the second contents of the casserole through
pressure. Use a second absorption bulb as counterpoise in all another filter paper. Thoroughly wash the residue in the filter
weighings unless a single pan balance is used. paper until chloride free as in 10.3.3. Retain the filtrate for the
iron and aluminum oxide analysis.
9.6 Calculation—Calculate the percent CO2 to the dried 10.3.6 Dry sufficient crucibles by placing in a cold muffle
sample as follows: furnace during warm up or by placing in a drying oven for 15
Percent CO2 5 ~~ A 2 B ! /C 3 100!~ 1 2 D ! (1) to 20 min, then placing in a 900°C muffle furnace. Cool
crucibles to room temperature in a desiccator.
where:
10.3.7 Transfer both filter papers to a tared crucible and char
A = mass of absorption bulb + CO2 g, slowly without flaming. Burn off all the carbon and ignite in a
B = mass of absorption bulb before the run, g, muffle furnace at 900°C for 15 min.
C = mass of specimen, g, and
10.3.8 Cool the crucibles in a desiccator and weigh to the
D = percent combined water as determined in Section 8 as
nearest 0.0001 g.
a decimal.
10.4 Calculation and Report—Calculate the average weight
Calculate the percent CO2 to the sample as received as
of the three precipitates and report as silicon dioxide (SiO2)
follows:
and other insoluble matter to the percentage of sample as
Percent CO2 5 E ~ 1 2 F ! (2) received or to the dried sample as required.
where: 10.5 Precision and Bias—Neither the precision nor the bias
E = result of Eq 1, and for the silicon dioxide and other acid insoluble matter has been
F = percent free water as determined in Section 7 as a determined.
decimal.
11. Iron and Aluminum Oxides
9.7 Precision and Bias—Neither the precision nor the bias
for the carbon dioxide analysis has been determined. 11.1 Significance and Use—The iron and aluminum oxides
(Fe2O3 + Al2O3) analysis is used to determine the quantity of
10. Silicon Dioxide and Other Acid Insoluble Matter these metal oxides in gypsum or gypsum products.

10.1 Summary of Test Method—The gypsum and other acid 11.2 Procedure—To the filtrate, obtained as described in
soluble components of the sample are dissolved in dilute Section 10, add a few drops of nitric acid (HNO3), and boil to
hydrochloric acid (HCl). The residue is weighed and calculated ensure oxidation of the iron. Add 2 g of ammonium chloride
as silicon dioxide and other acid insoluble matter. (NH4Cl) previously dissolved in water. Make alkaline with
ammonium hydroxide (NH4OH). Digest hot for a few minutes
10.2 Significance and Use—The silicon dioxide and other until the precipitate coagulates. Filter, wash, ignite the precipi-
acid insoluble matter analysis determines and is used to report tate at 1000°C for 30 min or to constant weight in a muffle
the percentage of one of the inert impurities in gypsum and furnace and weigh as Fe2O3 + Al2O3. Save the filtrate for the
gypsum products. CaO analysis.
10.3 Procedure—Perform in triplicate. NOTE 1—The addition of a pinch of ashless filter paper pulp will aid in
10.3.1 Weigh approximately 1 g of the specimen prepared in the filtration of the precipitate.
Section 4 to the nearest 0.0001 g. 11.3 Calculation—Calculate Fe2O3 + Al2O3 to the percent-
10.3.2 Place the specimen in a porcelain casserole. Add age of sample as received or the dried sample as required. This
approximately 50 mL of 1 + 5 hydrochloric acid. Evaporate precipitate may be further treated to separate the two oxides,
slowly and carefully to apparent dryness on a hot plate. Take but this is generally unnecessary.

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11.4 Precision and Bias—Neither the precision nor the bias chloride (BaCl2). The precipitate is filtered and weighed as
for the iron and aluminum oxides analysis has been deter- barium sulfate (BaSO4) and the sulfur trioxide (SO3) equiva-
mined. lent is calculated.
14.2 Significance and Use—The specification for gypsum
12. Calcium Oxide and some gypsum products specifies the amount of calcium
12.1 Significance and Use—The calcium oxide (CaO) sulfate (CaSO4) required, either in the dihydrate (CaSO4 ·
analysis is used to determine the amount of CaO and calculate 2H2O) or hemihydrate (CaSO4 · 1⁄2 H2O) form. This procedure
the amount of calcium carbonate (CaCO3) in gypsum and assumes that an insignificant amount of sulfate other than
gypsum products. calcium sulfate is present. This test method is used to deter-
12.2 Procedure: mine compliance to the gypsum and gypsum product specifi-
cations. It is also commonly used in quality control work.
12.2.1 To the filtrate obtained as described in Section 11 add
5 g of ammonium oxalate ((NH4)2C2O4) dissolved in water. 14.3 Interference—This test method has been developed for
Digest hot for 30 min, making sure that the solution is always natural gypsum and for impurities generally found associated
alkaline with NH4OH. Filter, wash, and ignite the precipitate at with natural gypsum. Synthetic gypsum will sometimes have
1000°C for 2 h to constant weight in a platinum crucible in a an additional number of interfering elements and compounds,
muffle furnace. and if so, this procedure will not give accurate results. This test
12.2.2 Alternative Method—To the filtrate obtained as de- method has a number of interferences that theoretically affect
scribed in Section 11, add 5 g of (NH4)2C2O4 dissolved in the results. Co-precipitation and occlusion are problems if the
water. Digest hot for 30 min, making sure that the solution is solution is either too acidic or too basic. Calculations using
always alkaline with NH4OH. Filter and wash, transfer the SO3 analysis are most accurate on samples that are known to be
precipitate to a beaker, and wash the filter paper with hot completely hydrated or completely dehydrated.
H2SO4 (1 + 6), catching the washing in the same beaker. Heat 14.4 Procedure:
gently to complete solution, adding more H2SO4 if necessary.
14.4.1 Having properly selected and prepared the samples
While still warm, titrate with potassium permanganate
as specified in Section 4, weigh a representative specimen of
(KMnO4) solution (5.6339 g/L) until the pink color persists.
approximately 0.5 g, to the nearest 0.0001 g.
12.3 Calculation—The number of milliliters of KMnO4 14.4.2 Place the weighed sample into a 400-mL beaker. Add
solution used gives directly the percentage of lime in the dried 50 mL of HCl (1 + 5). Boil and disperse with the flattened end
sample. Calculate the CaO to the percentage of sample as of a glass rod while stirring until the sample is completely
received or the dried sample as required. broken down. Add approximately 100 mL boiling water and
12.4 Precision and Bias—Neither the precision nor the bias continue boiling for 15 min, with this step to be extended as
for the calcium oxide analysis has been determined. required, so the combined boiling time is not less than 1 h.
14.4.3 Using filter paper, filter into a clean 600-mL flask and
13. Magnesium Oxide rinse the 400-mL beaker thoroughly with hot distilled water.
Carefully wash the sides of the 400-mL beaker while wiping
13.1 Significance and Use—The magnesium oxide (MgO) the insides with a rubber-tipped glass rod making sure all
analysis is used to determine the amount of MgO and calculate splatters and insoluble are washed into the filter paper. Dry and
the amount of magnesium carbonate MgCO3 in gypsum and burn off the filter paper leaving the residue to be dried and
gypsum products. weighed for insoluble matter, if this test method is not
13.2 Procedure—To the filtrate obtained as described in otherwise conducted.
12.2.1 or 12.2.2, add enough water to give a total volume of 14.4.4 Dilute the filtrate to 400 to 500 mL. Add one to two
approximately 600 mL. Cool, and add 10 mL of NH4OH and drops of 0.1 % methyl red indicator. Prepare a 400 to 500-mL
5 g of sodium ammonium phosphate (NaNH4HPO4) dissolved sample of 0.05 to 0.1 N HCl. Add one to two drops of 0.1 %
in water. Stir vigorously until a precipitate begins to form. Let methyl red indicator. Compare the color of this solution to the
stand overnight. Filter, using a Gooch crucible, and wash with color of the filtrate. Dilute the filtrate or add HCl (1 + 5)
NH4NO3 solution. Ignite at 1000°C for 2 h to constant weight solution as necessary to match the pH of the 0.05 to 0.1 N HCl
in a muffle furnace. solution.
13.3 Calculation—Multiply this weight by 0.36207 to find 14.4.5 Boil the filtrate solution and add 20 mL of near-
the weight of magnesium oxide (MgO). Calculate the MgO to boiling 10 % barium chloride solution, preferably with the help
the percentage of sample as received or to the dried sample as of a pipette, drop by drop while stirring. The barium chloride
required. solution should be prepared not less than one day before use.
Continue boiling the solution for 10 to 15 min and digest hot
13.4 Precision and Bias—Neither the precision nor the bias for 3 h or until the precipitate settles.
for the magnesium oxide analysis has been determined.
14.4.6 Filter and wash with approximately 125 to 150 mL of
hot water to render the precipitate chloride free. Test the filtrate
14. Sulfur Trioxide for chloride by collecting a small amount and adding a few
14.1 Summary of Test Method—In this test method, sulfate drops of 0.1 N AgNO3 solution. A white precipitate indicates
is precipitated from an acid solution of the gypsum with barium more washing is needed. Alternately, use filtering crucibles for

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 C471M − 17a´1
quick filtering if the particular crucibles to be used are tested sample to give the net titration. A 1-mL net titration is
prior to use by refiltering the filtrate from the crucibles with equivalent to 0.002923 g of sodium chloride (NaCl). Calculate
filter paper, and no more than 2 mg is collected on the filter the NaCl as a percentage of the sample as received or the dried
paper. sample as required.
14.4.7 Ignite the precipitate and paper in a tared crucible, 15.4 Precision and Bias—Neither the precision nor the bias
and slowly char the paper without inflaming. Burn off all the for the chloride analysis has been determined.
carbon and ignite in a muffle furnace at 800 to 900°C or using
bright red heat over a Bunsen burner for 15 to 20 min. Dry the 16. Report
filtering crucibles by placing in a cold muffle furnace during
16.1 Report the results obtained in the analysis as follows:
warm-up or in a drying oven prior to igniting in a muffle
furnace at 800 to 900°C for 15 to 20 min.
%
NOTE 2—Thoroughly cleans crucibles before each use and heat in a Free water ...
furnace at 800 to 900°C and cool in a desiccator before taring. Combined water ...
Carbon dioxide (CO2) ...
14.4.8 Cool all crucibles in a desiccator and weigh to the Silicon dioxide (SiO2) and insoluble matter ...
nearest 0.0001 g. Iron and aluminum oxides (Fe2O3 + Al2O3) ...
Lime (CaO) ...
14.5 Calculation—Multiply the weight of the precipitate by Magnesium oxide (MgO) ...
0.343 to determine the weight of sulfur trioxide (SO3). Calcu- Sulfur trioxide (SO3) ...
Sodium chloride (NaCl) ...
late the SO3 to the percentage of sample as received or to the Total 100.00±
dried sample as required.
14.6 Precision and Bias—Neither the precision nor the bias NOTE 3—Since it is frequently advisable to recalculate the results
for the sulfur trioxide analysis has been determined. obtained in the chemical analysis in order that they may be more
enlightening, the following is submitted for consideration:
15. Chlorides (1) Multiply the percentage of combined water by 4.778 to obtain
purity or percentage gypsum. To calculate the percentage of CaSO4 · 1⁄2
15.1 Significance and Use—Small amounts of chlorides in H2O in plasters, multiply the percentage of gypsum by 0.8430.
gypsum or gypsum products often have a detrimental effect on (2) Multiply the percentage of combined water by 2.222 to obtain the
their use. This procedure is used to measure the amount of amount of SO3 combined as gypsum.
chlorides present and report it as sodium chloride. (3) Subtract the result obtained in (2) from the total SO3 found by
analysis to obtain the excess SO3.
15.2 Procedure: (4) Multiply the excess SO3 by 1.700 to obtain the percentage
15.2.1 Weigh approximately 20.0 g of sample as prepared in anhydrite, CaSO4.
Section 4 to 0.001 g and transfer to a 400-mL beaker. Add (5) Multiply the percentage of gypsum found in (1) by 0.3257 to obtain
the percentage of CaO combined as gypsum.
150 mL of water, stir, and heat to just below the boiling point. (6) Multiply the percentage of anhydrite found in (4) by 0.4119 to
Cover with a watch glass and maintain at just below boiling obtain the percentage of CaO combined as anhydrite.
(not less than 80°C) for 1 h with occasional stirring. Filter with (7) Add (5) and (6) together. Then subtract this result from the total
suction on a Buchner funnel fitted with a medium filter paper. CaO percentage found by analysis.
Wash the residue with four 20-mL portions of hot water. (8) Multiply the excess CaO percentage by 1.785 to obtain the
percentage of calcium carbonate.
15.2.2 Add two drops of phenolphthalein indicator solution (9) Multiply the percentage of MgO by 2.091 to obtain the percentage
to the filtrate. If the filtrate fails to turn pink, add 0.1 N NaOH of magnesium carbonate.
solution dropwise with stirring until a faint pink color devel-
ops. Add 0.1 N HNO3 dropwise until the pink color just NOTE 4—Having made the calculations in Note 3, the results may be
disappears. reported as follows:
15.2.3 If the chloride content is very low, transfer the entire
%
filtrate quantitatively to a 400-mL beaker and proceed as Gypsum (CaSO4·2H2 O) ...
described in 15.2.4. If larger amounts of chloride are expected, Anhydrite (CaSO4 natural and manufactured) (Note 3) ...
transfer the filtrate quantitatively to a 250-mL volumetric flask, Silicon dioxide and insoluble (SiO2 + Ins.) ...
Iron and aluminum oxide (R2O3) ...
cool to room temperature, and dilute to 250 mL. Take a suitable Calcium carbonate (CaCO3) ...
aliquot, transfer to a 400-mL beaker, and dilute to a volume of Magnesium carbonate (MgCO3) ...
100 to 250 mL. Magnesium oxide (MgO) ...
Sulfur trioxide (SO3) ...
15.2.4 Place the beaker containing the sample on a white Sodium chloride (NaCl) ...
surface, add 0.5 mL (ten drops) of K2CrO4 solution and titrate Total 100.00±
with AgNO3 solution using a micro buret having a 10-mL
capacity and graduated in divisions of 0.02 mL. Titrate until a NOTE 5—The presence of the different forms of CaSO4 may be
faint but definite orange color is visible. determined by a microscopic examination. A paper titled “Gypsum
15.2.5 Perform a blank titration using the same volume of Analysis with the Polarizing Microscope” containing suggested methods
water as the sample volume and the same amount of K2CrO4 can be found in ASTM STP 861.7
solution. Titrate to the same color as obtained with the sample.
15.3 Calculation—Subtract the volume of AgNO3 solution 7
Green, George W., “Gypsum Analysis with the Polarizing Microscope,” The
used for the blank titration from the volume used for the Chemistry and Technology of Gypsum, ASTM STP 861, ASTM, 1984, pp. 22–47.

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 C471M − 17a´1
17. Alternative Procedure for Analysis of Free Water in applying the same test method with the same apparatus under
Gypsum Using Moisture Balance constant operating conditions on identical test material within
17.1 Significance and Use—The free water analysis deter- short intervals of time would in the long run, in the normal and
mines the amount of free water contained in the sample as correct operation of the test method, exceed the following
opposed to chemically combined water, and prepares the values only in one case in 20.
sample for further analysis. (1) Repeatability can be interpreted as maximum difference
between two results, obtained under repeatability conditions,
17.2 Equipment—A programmable moisture balance, ca- that is accepted as plausible due to random causes under
pable of temperature control of 61°C to at least 200°C. The normal and correct operation of the test method.
moisture balance must be capable of measuring a minimum of (2) Repeatability limits are listed in Table 3.
0.01 % loss in weight and be able to bring the temperature of 17.5.1.2 Reproducibility (R)—The difference between two
an empty tray from ambient conditions up to 200°C. single and independent results obtained by different operators
17.2.1 Equipment Setup—Implement a test program for applying the same test method in different laboratories using
“free water” that takes a sample of 5 to 8 g from an initial different apparatus on identical test material would, in the long
temperature to 45°C at the maximum rate of temperature rise run, in the normal and correct operation of the test method,
and holds the temperature at 45°C for up to two hours. The exceed the following values only in one case in 20.
initial temperature shall be defined as a temperature of 20 to (1) Reproducibility can be interpreted as maximum differ-
30°C. ence between two results, obtained under reproducibility
17.3 Procedure: conditions, that is accepted as plausible due to random causes
17.3.1 Prior to beginning the test, both the moisture balance under normal and correct operation of the test method.
and sample temperature must be less than 30°C. Note that (2) Reproducibility limits are listed in Table 3.
some phases of gypsum are metastable in humidity and as 17.5.1.3 The above terms (repeatability limit and reproduc-
such, samples should be stored to minimize changes due to ibility limit) are used as specified in Practice E177.
environmental conditions. 17.5.1.4 Any judgment in accordance with statements
17.3.2 Weigh and evenly distribute 5 to 8 g of a sample of 17.5.1.1 and 17.5.1.2 would have an approximate 95 % prob-
the material as received in a clean tared pan in the moisture ability of being correct.
balance. Run the described free water test program until a 17.5.2 Bias—At the time of the study, there was no accepted
constant mass is reached or two hours of time at 45°C has reference material suitable for determining the bias for this test
elapsed. Constant mass is considered reached if the percent method, therefore no statement on bias is being made.
moisture change per minute is 0.01 % or less and 45°C has 17.5.3 The precision statement was determined through
been achieved. statistical examination of 660 results, from 15 participating
17.4 Calculation and Report—Report the free water as the laboratories, on two types of gypsum materials.
percentage loss in weight at the end of the test. This can be 17.5.4 To judge the equivalency of two test results, it is
calculated by the following formula: recommended to choose the material closest in characteristics
to the test material.
% Free Water 5 mass of water evaporated⁄initial sample mass 3 100
(3) 18. Alternative Procedure for Analysis of Combined
Water in Gypsum Using Moisture Balance
17.5 Precision and Bias:
17.5.1 The precision of this test method is based on an 18.1 Significance and Use—The combined water analysis
interlaboratory study of ASTM C471M, Standard Test Methods determines the percent of chemically combined water and is
for Chemical Analysis of Gypsum and Gypsum Products, used to calculate the purity of gypsum or the amount of
conducted in 2016. Each of 17 laboratories analyzed two gypsum or gypsum plaster in gypsum products. Note that this
different gypsum sample types. Every “test result” represents test reports the combined water result on a dry basis and
an individual determination, and all participants reported five assumes that any sample measured has had any free water
test results per material. Practice E691 was followed for the removed before testing. See Section 17 for a description and
design and analysis of the data; the details are given in ASTM test for free water.
Research Report No. C11-1003.6 18.2 Interferences—Some materials, such as organic and
17.5.1.1 Repeatability (r)—The difference between repeti- hydrated compounds that decompose within the same tempera-
tive results obtained by the same operator in a given laboratory ture range as gypsum, will cause high results. When the

TABLE 3 Free Water in Gypsum in Accordance with Moisture Balance Method (%)
Repeatability Reproducibility
Repeatability Reproducibility
AverageA Standard Standard
Material Limit Limit
Deviation Deviation
x̄ Sr SR r R
natural gypsum 0.0524 0.0096 0.0361 0.0270 0.1009
flue gas desulphogypsum (FGD) 9.1226 0.2037 0.2911 0.5702 0.8151
A
The average of the laboratories’ calculated averages.

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 C471M − 17a´1
maximum temperature is exceeded, some carbonates undergo (1) Repeatability can be interpreted as maximum difference
decomposition, which will result in high results. between two results, obtained under repeatability conditions,
18.3 Equipment—A programmable moisture balance, ca- that is accepted as plausible due to random causes under
pable of temperature control of 61°C to at least 200°C. The normal and correct operation of the test method.
moisture balance must be capable of measuring a minimum of (2) Repeatability limits are listed in Table 4.
0.01% loss in weight and be able to bring the temperature of an 18.6.1.2 Reproducibility (R)—The difference between two
empty tray from ambient conditions up to 200°C. single and independent results obtained by different operators
18.3.1 Equipment Setup—Implement a test program for applying the same test method in different laboratories using
“combined water” that takes a sample of 5 to 8 g from an initial different apparatus on identical test material would, in the long
temperature to a temperature of 200°C at the maximum rate of run, in the normal and correct operation of the test method,
temperature rise and holds the temperature for up to two hours. exceed the following values only in one case in 20.
The initial temperature shall be defined as temperature of 20 to (1) Reproducibility can be interpreted as maximum differ-
45°C. ence between two results, obtained under reproducibility
conditions, that is accepted as plausible due to random causes
18.4 Procedure: under normal and correct operation of the test method.
18.4.1 Prior to beginning the test, both the moisture balance (2) Reproducibility limits are listed in Table 4.
and sample temperature must be 45°C or less. Note that some 18.6.1.3 The above terms (repeatability limit and reproduc-
phases of gypsum are metastable in humidity and as such, ibility limit) are used as specified in Practice E177.
samples should be stored to minimize changes due to environ- 18.6.1.4 Any judgment in accordance with statements
mental conditions. 18.6.1.1 and 18.6.1.2 would have an approximate 95 % prob-
18.4.2 Weigh and evenly distribute 5 to 8 g of a sample of ability of being correct.
the material as previously dried to remove free water in a clean 18.6.2 Bias—At the time of the study, there was no accepted
tared pan. Run the described combined water test program until reference material suitable for determining the bias for this test
a constant mass is reached or two hours of time at 200°C has method, therefore no statement on bias is being made.
elapsed. Constant mass is considered reached if the percent 18.6.3 The precision statement was determined through
moisture change per minute is 0.01% or less and 200°C has statistical examination of 660 results, from 15 participating
been achieved. laboratories, on two types of gypsum materials.
18.5 Calculation and Report—Report the combined water 18.6.4 To judge the equivalency of two test results, it is
as the percentage loss in weight at the end of the test. This can recommended to choose the material closest in characteristics
be calculated by the following formula: to the test material.
% Combined Water 5 mass of water evaporated⁄dry sample mass 3 100
19. Alternative Procedure for Analysis for Calcium
(4) Sulfate by Ammonium Acetate Method8
18.6 Precision and Bias: 19.1 Significance and Use—This test method covers the
18.6.1 The precision of this test method is based on an determination of calcium sulfate in gypsum and gypsum
interlaboratory study of ASTM C471M, Standard Test Methods products by extraction with ammonium acetate solution.
for Chemical Analysis of Gypsum and Gypsum Products,
conducted in 2016. Each of 17 laboratories analyzed two 19.2 Reagents and Materials:
different gypsum sample types. Every “test result” represents 19.2.1 Ammonium Acetate Solution—Dissolve 454 g of
an individual determination, and all participants reported five ammonium acetate in 2 L of water. Add sufficient NH4OH to
test results per material. Practice E691 was followed for the make the solution distinctly ammoniacal, using phenolphtha-
design and analysis of the data; the details are given in ASTM lein as the indicator.
Research Report No. C11-1003.6 19.2.2 Ammonium Hydroxide Wash Solution—Dilute
18.6.1.1 Repeatability (r)—The difference between repeti- 100 mL of concentrated ammonium hydroxide (NH4OH, sp gr
tive results obtained by the same operator in a given laboratory 0.90) to 1 L with water.
applying the same test method with the same apparatus under 19.2.3 Filter Aid—Diatomaceous silica, analytical grade.
constant operating conditions on identical test material within 19.2.4 Phenolphthalein Indicator Solutin.
short intervals of time would in the long run, in the normal and
correct operation of the test method, exceed the following 8
This procedure was developed by L. S. Wells and W. F. Clarke, National Bureau
values only in one case in 20. of Standards, and modified by B. E. Kester, United States Gypsum Co.

TABLE 4 Combined Water in Gypsum in Accordance with Moisture Balance Method (%)
Repeatability Reproducibility
Repeatability Reproducibility
AverageA Standard Standard
Material Limit Limit
Deviation Deviation
x̄ Sr SR r R
natural gypsum 19.1313 0.0229 0.0813 0.0641 0.2278
flue gas desulphogypsum (FGD) 19.3761 0.0392 0.1859 0.1098 0.5206
A
The average of the laboratories’ calculated averages.

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 C471M − 17a´1
19.3 Procedure Using Gooch Crucible: 19.5 Calculation:
19.3.1 Weigh rapidly approximately 4 g of the well-mixed 19.5.1 Calculate the percentage of loss in weight at 45°C
sample and transfer to a 600-mL beaker. Make all weighings to (free water) as follows:
0.001 g, except weigh the crucibles and their contents to Loss in weight at 45°C, % 5 @ ~ A 2 B ! /C # 3 100 (5)
0.0001 g.
19.3.2 Without delay, weigh approximately 1 g of the where:
well-mixed sample in a tared weighing bottle having a ground- A = original weight of sample and weighing bottle,
glass stopper. Dry the sample and weighing bottle to constant B = weight of sample and weighing bottle dried to constant
weight at 45°C. Stopper weighing bottles immediately upon weight at 45°C, and
removal from the oven in order to prevent absorption of C = original weight of sample.
moisture from the air upon cooling. Calculate the weight of the 4-g sample (19.3.1), corrected for
19.3.3 If the percentage by weight of combined water held loss on heating to constant weight at 45°C.
by the calcium sulfate is required, heat the sample and 19.5.2 Calculate the percentage of combined water as fol-
weighing bottle to constant weight at 220°C. lows:
19.3.4 To the contents of the 600-mL beaker (19.3.1), add
Combined water, % 5 @ ~ B 2 D ! / ~ B 2 E ! # 3 100 (6)
350 mL of the ammonium acetate solution, and stir the mixture
thoroughly to loosen all of the solid matter from the bottom of where:
the beaker. Add 0.2000 g of redried diatomaceous silica to the B = weight of sample and weighing bottle dried to constant
mixture. Heat the beaker and contents to 70°C on a steam or weight at 45°C,
hot water bath, and maintain at that temperature for 30 min, D = weight of sample and weighing bottle dried to constant
while stirring frequently. During heating, keep the solvent weight at 220°C, and
ammoniacal by additions of NH4OH and phenolphthalein, if E = weight of weighing bottle.
indicated. Meanwhile, heat a supply of the ammonium acetate
19.5.3 Calculate the percentage of CaSO4 · nH2O on the
solution to 70°C, keeping it also distinctly ammoniacal. Filter
basis of the sample dried to constant weight at 45°C as follows:
the mixture, with suction, through a tared Gooch crucible,
stirring frequently during filtration to keep the diatomaceous CaSO 4 ·nH2 O, % 5 @ F 2 ~ G 2 H ! /F # 3 100 (7)
earth suspended in the liquid. Wash the Gooch crucible where:
containing the residue with five 10-mL portions of the warm
acetate solution, draining thoroughly after each washing. Wash F = weight of sample, corrected for loss on heating to
in the same manner with eight 10-mL portions of the NH4OH constant weight at 45°C,
G = weight of dried crucible and contents (19.3.4) or weight
wash solution. Take care to wash the upper walls of the Gooch
of weighing bottle and contents (19.4.2), 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 (19.3.4), or weight of weighing bottle, diato-
crucible to cool in a desiccator before weighing.
maceous silica used as a filter aid and the weight of
NOTE 6—Avoid overheating in all oven drying of ammonium acetate filter paper (19.4.2).
residues; that is, place crucibles well away from the heating elements. This
is of particular importance for samples high in impurities, as these 19.6 Precision and Bias—Neither the precision nor the bias
impurities often have water of hydration that is lost on local overheating. for the analysis of calcium sulfate by the ammonium acetate
19.4 Procedure Using Tared Filter Papers: method has been determined.

NOTE 7—This procedure is suggested where several samples are to be 20. Alternative Procedure for Analysis for Sodium
analyzed at once. It has been found that gravity filtration on six samples
Chloride by Coulometric Method9
will proceed as rapidly as it is possible to handle the samples.
19.4.1 Dry a quarter-folded, 110-mm quantitative filter pa- 20.1 Significance and Use—This test method covers the
per overnight at 70°C in a wideform, glass-stoppered, 30 by determination of sodium chloride in gypsum and gypsum
60-mm weighing bottle. After drying, cool the weighing bottle products by the coulometric method.
and paper in a desiccator, and weigh. 20.2 Interferences—The presence of sulfide, sulfhydryl, or
19.4.2 Treat the sample exactly as described in 19.3.1, other silver reactive substances will lead to high results. Such
19.3.2, and 19.3.4 prior to the filtration. Filter the mixture by interfering substances are removed by alkaline oxidation with
gravity through a 70-mm glass funnel, stirring frequently hydrogen peroxide.
during filtration to keep the diatomaceous silica suspended in
20.3 Apparatus:
the liquid. Wash the filter paper and residue with five 10-mL
20.3.1 Chloride Meter:
portions of warm acetate solution, draining thoroughly after
each washing. Wash in the same manner with eight 10-mL 20.3.1.1 The instrument shall be equipped to measure the
portions of the NH4OH wash solution. After final draining, concentration of dissolved chloride in aqueous solutions by the
replace the paper and residue in the weighing bottle, and dry at coulometric method.
70°C to constant weight. Cool the weighing bottle, paper, and
residue in a freshly prepared desiccator before weighing; this is
essential, due to the hygroscopic character of paper. 9
This procedure was developed by Westroc Industries Limited.

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 C471M − 17a´1
20.3.1.2 The instrument shall be capable of measuring 21. Determination of Sand in Set Plaster
chloride concentrations in the range from 10 to 260 mg/L with 21.1 Summary of Test Methods—This test method for the
a repeatability of 61 mg/L. determination of the sand content of set gypsum plaster
20.4 Reagents: requires for accurate results the following determinations:
20.4.1 Acid Buffer Solution—Dissolve 100 mL of 99.5 % 21.1.1 Determination of the percentage of insoluble matter
acetic acid (HC2H3O2) and 5.5 mL of concentrated nitric acid in the sand used with the plaster,
(sp gr 1.42) in approximately 200 mL of water and dilute to 21.1.2 Determination of the percentage of insoluble matter
500 mL. in the gypsum neat plaster, and
20.4.2 Diluted Standard Solution (100 mg Cl/L)—Di- 21.1.3 Determination of the percentage of insoluble matter
lute 5.00 mL of stock standard solution to 500 mL. in the sanded calcined plaster.
20.4.3 Gelatin Solution—Add 2.5 g of gelatin and 0.5 g of
NOTE 9—If samples of the original gypsum neat plaster and the sand are
thymol blue to 250 mL of water and dissolve by stirring not available, an approximation of the insoluble matter may be obtained
continuously while bringing to a boil. With the solution just by the use of this method on plaster and sand from the same sources as
boiling, continue stirring until all the thymol blue is dissolved. those from which the plaster to be analyzed was originally prepared.
Add 0.5 g of thymol, cool, and dilute the solution to 500 mL. 21.2 Significance and Use—This test method is used for
NOTE 8—The gelatin solution holds the precipitated silver chloride determining the sand content of samples of aggregated plaster
(AgCl) in suspension and also indicates the presence of the acid buffer. taken from job sites to determine compliance with Specifica-
The solution will keep for three months at room temperature or longer if
tion C842.
refrigerated. Warm the refrigerated solution to room temperature before
use. 21.3 Reagents:
20.4.4 Stock Standard Solution (10 g Cl/L)—Dissolve 21.3.1 Ammonium Acetate (250 g/L)—Dissolve 250 g of
8.240 g of dried sodium chloride (NaCl) in water and dilute to ammonium acetate (NH4C2H3O2) in water and dilute to 1 L.
500 mL. 21.3.2 Ammonium Hydroxide (1 + 59)—Mix one volume of
20.5 Procedure: concentrated ammonium hydroxide (NH4OH) (sp gr 0.90) with
20.5.1 Weigh 20.0 g of the well-mixed sample and transfer 59 volumes of water.
to a 150-mL beaker. 21.4 Sampling—Where plaster to be tested is part of a
20.5.2 Add 50 mL of water, boil, allow the solid material to two-coat or three-coat plastering operation, take the sample for
settle, and filter off the solution. Add an additional 50 mL of analysis from that portion of the entire plaster sheet that
water to the solids, boil, and pour the contents of the beaker comprises the single coat being tested. Separate succeeding
into the filter. Wash the residue with 100 mL of hot water, coats of plaster by use of a stiff putty knife or similar
adding the washing to the filtrate. Cool and dilute with water to implement. Not less than 500 g shall be taken as a sample, the
250 mL. sample preferably being obtained from different sections of the
20.5.3 Switch on the chloride meter and allow a period of wall or ceiling under examination.
25 min before use. Set the counter to zero.
21.5 Procedure:
20.5.4 Place a magnetic stirring bar in the test beaker, add
21.5.1 In a clean porcelain mortar, grind the set plaster
10 mL of diluted standard solution, 3 mL of acid buffer
sample to the size of the largest sand particles present, or
solution, and five drops of gelatin solution. Place the test
smaller, so that approximately 100 % of the sample will pass a
beaker on the platform and lower the electrodes into the
2.36-mm (No. 8) sieve. Fine grinding makes solution of the
solution. Press the “start” button until the pilot light is
gypsum faster. Place approximately 200 g of the ground
extinguished. The counter will begin to register after a few
sample in a porcelain casserole or evaporating dish, and calcine
seconds. Do not remove the electrodes from the sample until
on a sand bath. Stir the sample continuously with a thermom-
the pilot light comes on. Read the chloride content from the
eter during the heating, and adjust the rate of heating so that 20
counter. If a reading of 100 6 1 mg Cl/L is not obtained, refer
to 30 min will be required to raise the temperature of the
to the manufacturer’s instruction manual. Reset the counter to
sample to 160 6 5°C. Cool the sample to room temperature in
zero.
a desiccator.
20.5.5 Repeat the procedure used in 20.5.4 using 10 mL of
21.5.2 After cooling, weigh accurately 20 6 0.05 g of the
the sample solution instead of the diluted standard solution.
calcined sample into a 600-mL beaker. Add 300 to 350 mL of
Read the result as milligrams of chlorine per litre. When all
NH4C2H3O2 solution. If acidic to litmus paper, add a few
tests are completed, lower the electrodes into reagent water.
millilitres of NH4OH (1 + 59) to the stock NH4C2H3O2 solu-
20.6 Calculation—Calculate the amount of NaCl as a per- tion to render it slightly alkaline prior to the addition to the test
centage of the sample as received or dried sample as follows: sample.
NaCl, % 5 0.00206 3 A (8) 21.5.3 Warm the suspension to a temperature of 70 6 5°C
and stir continuously for 20 to 30 min. Filter the warm
where:
suspension with the aid of suction through a small Büchner
A = chloride meter reading, mg Cl/L. funnel or Gooch crucible in which filter paper has previously
20.7 Precision and Bias—Neither the precision nor the bias been placed. Refilter the first 100 mL of the filtrate. Wash the
for the sodium chloride analysis by the coulometric method has sand remaining in the beaker onto the filter with an additional
been determined. 100 mL of warm ammonium acetate solution. Wash the beaker

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 C471M − 17a´1
and residue with 200 to 300 mL of water, dry the funnel and several stages of washing, stirring the charge, and quickly
sand at 100°C to constant weight. The weight of the residue is pouring upon the sieve the fiber flotations, repeating the
the weight of insoluble matter. elutriation procedure several times. Examine the fiber collected
21.5.4 Insoluble Matter in Sand—Determine the weight of on the 150-µm sieve and repeat the elutriation if necessary.
insoluble matter in sand as described in 21.5.1 – 21.5.3, except 22.2.2 Dry the sieves (or sieve) and the residue contained
that no grinding of the sample is necessary. thereon overnight in an oven maintained at a temperature of
21.5.5 Insoluble Matter in Gypsum Neat Plaster— 45°C. Carefully invert the sieves, or sieve, over a piece of
Determine the weight of insoluble matter in the gypsum neat white paper, and transfer the residual material to the paper by
plaster as described in 21.5.1 – 21.5.3, except that only a 5-g brushing the bottom of the inverted sieve. Examine the
sample is required and no grinding of the sample is necessary. transferred material visually, noting whether the separation of
21.6 Calculation: fibers from plaster has been complete. Then transfer the
21.6.1 Insoluble Matter in Plaster—Multiply by 5 the material to a weighed platinum crucible and dry to constant
weight of the insoluble matter obtained as described in 21.5.3 weight at a temperature of 45°C. If the previous visual
to obtain the percentage of insoluble matter in sanded plaster. examination of the charge on the white paper showed that the
21.6.2 Insoluble Matter in Sand—Multiply by 5 the weight fiber was practically free of particles of plaster, report as the
of the insoluble matter in sand obtained as described in 21.5.4 percentage of fiber the weight of the fiber dried at 45°C,
to obtain the percentage of insoluble matter in sand. divided by 100. If, on the other hand, the visual examination
21.6.3 Insoluble Matter in Gypsum Neat Plaster—Multiply revealed the presence of an appreciable quantity of plaster
by 20 the weight of the insoluble matter in gypsum neat plaster associated with the fiber, carefully ignite the contents of the
obtained as described in 21.5.5 to obtain the percentage of crucible to constant weight. In this case, report as the percent-
insoluble matter in gypsum neat plaster. age of fiber the loss on ignition, divided by 100.
21.6.4 Calculate the percentage of sand in the sanded plaster 22.3 Precision and Bias—Neither the precision nor the bias
as follows: for the analysis of wood-fiber content in wood-fiber gypsum
X 5 @ ~ C 2 B ! / ~ A 2 B ! # 3 100 (9) plaster has been determined.

where: 23. Optional Procedure for Analysis for Sodium by

X = % of sand in sanded plaster, Atomic Absorption Method
A = % of insoluble matter in the sand,
23.1 Significance and Use—This test method covers the
B = % of insoluble matter in the gypsum neat plaster, and
C = % of insoluble matter in the sanded plaster. determination of sodium in gypsum and gypsum products by
the atomic absorption method.
21.6.5 To express the results as a ratio of the parts of sand
per part of plaster by weight, use the following equation: 23.2 Interferences—Sodium is partially ionized in the air-
acetylene flame. The effects of ionization will be significantly
Ratio of sand to plaster 5 X/ ~ 100 2 X ! (10) overcome by the addition of 1 to 2 g/L of another alkali to
NOTE 10—The results obtained by the above procedure indicate the
blanks, standards, and samples. Alternatively, use the air-
amount of sand originally mixed with the gypsum neat plaster before it
had been gauged with water or set. hydrogen flame, as it produces less ionization and less visible
emission than the air-acetylene flame.
21.7 Precision and Bias—Neither the precision nor the bias
for the analysis of sand in set plaster has been determined. 23.3 Apparatus:
23.3.1 Atomic Absorption Spectrophotometer:
22. Wood-Fiber Content in Wood-Fiber Gypsum Plaster 23.3.1.1 The instrument shall be equipped to measure the
22.1 Significance and Use—This test method is used to concentration of dissolved sodium in aqueous solutions using
determine the weight of wood fiber in wood-fibered plaster. either the air-acetylene or air-hydrogen flame.
22.2 Procedure: 23.3.1.2 The instrument shall be capable of measuring
22.2.1 Place a 100-g sample of wood-fiber plaster, prepared sodium concentrations within the optimum analytical range of
as described in Section 4 on a 600-µm (No. 30) sieve4 nested 0.1 to 0.5 absorbance units while providing a coefficient of
over a 150-µm (No. 100) sieve.4 Wash the plaster on the variation of approximately 0.5 to 2 %.
600-µm sieve with a stream of cold water, removing the 23.4 Reagents:
600-µm sieve when the fiber on it is practically or entirely free 23.4.1 Solvent—Use deionized water to prepare all solu-
of plaster. Next, wash the material on the 150-µm sieve until tions. If an alkali is to be included for the purpose of
the bulk of the plaster has been washed through the sieve and suppressing sodium ionization, it is most convenient to add it
the residue is mainly fiber. Transfer the material retained on the to the solvent at the start. In this way a constant concentration
150-µm sieve to a 300-mL, vitreous enamel, lipped pan, adding of alkali in blank, standards, and sample solution is ensured.
the charge on the 600-µm sieve if the fiber contains any 23.4.2 Stock Standard Solution (1.000 g Na/L)—Dissolve
adhering particles of plaster. Elutriate the material in the pan 2.5418 g of dried sodium chloride (NaCl) in water and dilute to
(purify by washing and straining, effecting as clean a separa- 1 L with water.
tion of fiber from plaster as is practical), catching the elutriated 23.4.3 Dilute Standard Solutions—Prepare dilute standard
fibers on a 150-µm sieve. To avoid loss of the fine particles of solutions bracketing the absorbance range of the dilute sample
fiber, make the transfer from the pan to the 150-µm sieve by solution, using the stock standard solution. (Solutions having a

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 C471M − 17a´1
concentration less than approximately 0.500 g/L are unstable minimized by operating at the lowest practical sodium concen-
for periods of more than day.) tration range or by removal of the interfering elements. For
23.5 Procedure: example, aluminum has a depressing effect on alkali-metal
23.5.1 Take 18 g of the well-mixed sample and transfer to a emission, which is of serious consequence. Remove aluminum
150-mL beaker. from the extraction liquid prior to flame photometry if its
23.5.2 Add 50 mL of water, boil, allow the solids to settle, concentration has been found, by preliminary tests, to exceed
and decant the supernatant liquid into a filter. Add an additional that of the sodium.
50 mL of water to the solids, boil, and pour the contents of the 24.2.2 Self-absorption causes the curve of intensity versus
beaker into the filter. Wash the residue with 100 mL of hot concentration to decrease its slope at higher concentrations,
water, adding the washing to the filtrate. Cool the filtrate to tending to reduce accuracy. Bracketing the unknown by known
room temperature and dilute to 500 mL in a volumetric flask to standard solutions tends to minimize this interference.
make the stock sample solution. Take 10 mL of the solution 24.3 Apparatus and Materials:
and make up to 500 mL in a second volumetric flask, to make
24.3.1 Flame Photometer—The instrument shall consist of
the dilute sample solution.
an atomizer and burner; suitable pressure-regulating devices
23.5.3 Determine the absorbance readings on the dilute
and gauges for fuel and air or oxygen; an optical system,
standard solutions and the solvent blank at a wavelength of
consisting of suitable light-dispensing or filtering devices
589.0 to 589.6 nm, following the manufacturer’s instruction
capable of preventing excessive interference from light of
manual. Subtract the absorbance value for the blank from the
wavelengths other than that being measured; and a photosen-
absorbance values for the dilute standard solutions and prepare
sitive indicating device.
a curve relating sodium concentration in milligrams per litre to
absorbance values. 24.3.2 Supply of Fuel and Air or Oxygen—The supplies of
fuel and air or oxygen shall be maintained at pressures
NOTE 11—If the absorbance of the dilute sample solution is known to somewhat higher than the controlled operating pressure of the
lie within the linear range, that is, the sodium concentration is below instrument.
approximately 1 mg/L only one standard and the solvent blank are needed
to prepare the curve. 24.4 Reagents:
23.5.4 Determine absorbance readings on the dilute sample 24.4.1 Prepare the following stock solutions from reagents
solution using the same technique, followed with the dilute that have been dried to constant weight at 105°C. Store the
standard solutions. The concentration of sodium in the dilute stock solutions in polyethylene or equally alkali-metal-free
sample solution in milligrams per litre is then found by containers.
consulting the standard curve. 24.4.2 Sodium Chloride Solution (2.5418 g/L)—Dissolve
23.6 Calculation—Calculate the amount of NaCl as a per- 2.5418 g of sodium chloride (NaCl) in water and dilute to 1 L
centage of the sample received or the dried sample as required with water. This stock standard solution contains 1.000 g/L of
as follows: sodium ion.
Sodium calculated as % NaCl 5 A 3 6.3553/S (11) 24.4.3 Dilute Standard Solutions—Prepare dilute standard
solutions from stock standard solution, bracketing the expected
where: sodium concentration range of the diluted sample extraction
A = concentration of dilute sample solution, mg/L, and liquid. For example, if the expected range of the sample
S = weight of sample, g. extraction liquid is between 0 and 0.010 g/L, prepare eleven
23.7 Precision and Bias—Neither the precision nor the bias equally spaced standards in tenths of the maximum.
for the analysis of sodium by the atomic absorption method has 24.5 Calibration of Instrument:
been determined. 24.5.1 Select the proper photocell; the blue-sensitive pho-
totube having a range from 320 to 620 nm is required for
24. Optional Procedure for Analysis for Sodium by sodium determination. Open the slit width to approximately
Flame Photometry one fourth of the maximum opening, set the instrument to the
24.1 Significance and Use—This test method covers the maximum sensitivity range, and balance the meter to obtain
determination of sodium in gypsum and gypsum products by electrical equilibrium.
flame photometry. This test method is based on Methods 24.5.2 Feed fuel and air or oxygen to the burner and ignite
D1428. the emitted mixture. Adjust fuel and air or oxygen pressures
24.2 Interferences: and follow the procedures for warm-up time prescribed by the
24.2.1 Radiation interferences caused by elements other instrument manufacturer. Set the scale-reading dial at approxi-
than that being determined are the greatest contributor to error mately 95 % of full scale, introduce a solution containing the
in flame photometry. Some effects are positive and others maximum amount of sodium in the range to be covered, and
negative. Of the elements encountered in this analysis, the allow the emitted light to strike the photocell.
greatest effect is that of one alkali metal on another. The 24.5.3 Select the proper filter, if a filter-type instrument is
foreign-element effects cannot be entirely compensated for used. For instruments employing spectral dispersing devices,
without employing calibration standards closely duplicating turn the wavelength dial back and forth slowly and carefully in
the composition of the sample. However, the effects are the vicinity of 589 nm until the galvanometer reaches a

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 C471M − 17a´1
maximum deflection. This wavelength setting produces maxi- 24.6.6 Refer to the standard curve prepared above and read
mum sensitivity. Do not disturb the wavelength dial during the off the concentration of sodium ion in the dilute sample
test. solution in milligrams per litre.
24.5.4 Continue to atomize the maximum standard of the 24.7 Calculation—Calculate the amount of NaCl as follows:
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 Sodium, calculated as NaCl, % 5 A 3 0.04067 (12)
as to balance the galvanometer needle. where:
NOTE 12—For instruments equipped with a variable slit, carry out the A = concentration of sodium, mg/L read off the standard
procedure described above with the slit width between fully closed and curve.
one fourth open for the preliminary test. In determining the proper slit
width for optimum instrument performance, consideration must be given 24.8 Precision and Bias—Neither the precision nor bias of
to the fact that the intensity of the emission line is approximately the analysis for sodium by flame photometry has been deter-
proportional to the slit width, whereas continuous background intensity mined.
increases as the square of the slit width. A decrease in slit width results in
decreased illumination of the phototube for a given concentration and is
compensated for by increasing the gain of the instrument. The most 25. Determination of Orthorhombic Cyclooctasulfur (S8)
favorable operating conditions are obtained with the smallest slit width in Gypsum Panel Products
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 25.1 Significance and Use:
covered. When altering the slit width, determine the background by 25.1.1 This test method covers the determination of ortho-
atomizing a zero standard, and check for sensitivity setting and instrument rhombic cyclooctasulfur (S8) in the core of the gypsum panel
stability with the maximum standard in the range to be covered. Lower product.
ranges require wider slit widths. Determine and record the optimum slit
width for each range and element to be covered. Use these values in all
25.1.2 Three test methods are available: gas chromatograph
subsequent tests. equipped with a mass spectrometer (GC/MS), gas chromato-
graph equipped with an electron capture detector (GC/ECD),
24.5.5 Determine the emission intensity of all standards.
and high-performance liquid chromatograph equipped with an
24.5.6 Plot emission intensity (scale reading) versus con-
ultraviolet detector (HPLC/UV).
centration on linear graph paper. For the lower ranges, the
curve thus prepared approximates a straight line but sometimes 25.1.3 This standard does not purport to address all of the
will not intersect zero because of background intensity. At safety concerns, if any, associated with its use. It is the
higher ranges, the curves show a decrease in slope with responsibility of the user of this standard to establish appro-
increasing concentration. Record on graphs all data in regard to priate safety and health practices and to determine the appli-
slit width, fuel pressure, and air or oxygen pressure. cability of regulatory limitations prior to use.

24.6 Procedure: 25.2 Orthorhombic Cyclooctasulfur (S8) Standard for GC

24.6.1 Weigh 25 g of the well-mixed sample and transfer to and HPLC:
a 150-mL beaker. 25.2.1 Toluene, spectral quality or chromatographic grade.
24.6.2 Add 50 mL of water, boil, allow the solid material to 25.2.2 Orthorhombic Cyclooctasulfur (S8), to be used as a
settle, and decant the supernatant liquid into a filter. Add an calibration standard.
additional 50 mL of water to the solids, boil and pour the 25.2.3 OTTAWA Sand, ASTM 20-30 sand (Specification
contents of the beaker into the filter. Wash the residue with C778).
75 mL of hot water, adding the washing to the filtrate. Cool and 25.2.4 Standard Orthorhombic Cyclooctasulfur (S8) Solu-
dilute with water to 200 mL in a volumetric flask to make the tions:
stock sample solution. 25.2.4.1 Dissolve 2400 mg of S8 in 1 L of toluene.
24.6.3 Take 5 mL of the stock sample solution and make up 25.2.4.2 Prepare five calibration standards of S8 in toluene
to 100 mL in a volumetric flask to make the dilute sample at 1.0, 5.0, 25.0, 50.0, and 100.0 ppm.
solution. 25.2.4.3 To evaluate extraction efficiency, add 50 µL of each
S8 prepared standard to 1.0 g of clean OTTAWA sand, and
NOTE 13—If the concentration of sodium in the sample is found to be
greater than the maximum standard, further dilute sample solution with
follow steps for sample preparation in each method (GC or
water to bring the concentration within the range. If the concentration of HPLC).
sodium in the sample is less than one tenth of the value of the maximum
standard, prepare a new dilute sample solution from the stock sample 26. Determination of Orthorhombic Cyclooctasulfur (S8)
solution to bring the concentration within the range. in Gypsum Panel Products by Gas Chromatograph
24.6.4 Turn the instrument on and feed fuel and air or Equipped with Mass Spectrometer (GC/MS)
oxygen to the burner. Ignite the gas mixture. For instruments
26.1 Apparatus—Gas chromatograph, equipped with a mass
with an adjustment slit, set the width to the value determined as
spectrometer detector.
outlined in Note 12.
26.1.1 Software must be capable of integrating peak areas.
24.6.5 Place the scale-reading dial at maximum. Atomize
the sample and allow its emitted light to strike the photocell. 26.2 Reagents and Materials:
Set the wavelength to 589 nm as described and adjust the gain 26.2.1 Carrier Gas—Helium, chromatographic grade.
to balance the galvanometer. Determine the emission intensity 26.2.2 Internal Standard (ISTD)—4,4’-dibromobiphenyl,
of the sample. 5 µg ⁄mL in xylene.

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 C471M − 17a´1
26.2.3 Surrogate Standard—Hexabromobenzene, 26.7 Precision and Bias—An interlaboratory study of this
2.5 mg ⁄mL hexabromobenzene in xylene. test method is being conducted, and a complete precision
26.2.4 Xylene—Spectral quality or chromatographic grade. statement is expected to be available on or before 2019.
26.2.5 Decafluorotriphenylphosphine (DFTPP)—Spectral 26.8 Report—Report the quantity of orthorhombic cyclooc-
quality or chromatographic grade tasulfur (S8) calculated in 26.6, determined to the nearest
26.2.6 Specimen vials should be VOC capable. 1 mg ⁄kg.
26.3 Sample Preparation—Three specimens of the gypsum
panel product should be available for testing. Remove surfac- 27. Determination of Orthorhombic Cyclooctasulfur (S8)
ing material and crush a piece of each specimen with a mortar in Gypsum Panel Products by Gas Chromatograph
and pestle to a powder. Equipped with Electron Capture Detector (GC/ECD)
26.3.1 GC Specimen Preparation: 27.1 Apparatus—Gas chromatograph equipped with an
26.3.1.1 Collect 1.0 g of each crushed specimen and transfer electron capture detector.
to a separate, sealable 10 mL to 20 mL vial. 27.1.1 Software must be capable of integrating peak areas.
26.3.1.2 Add 50 µL of surrogate standard to each specimen 27.2 Reagents and Materials:
and mix well using a glass rod and allow sample to air dry. 27.2.1 Carrier Gas—Helium, chromatographic grade.
26.3.1.3 Add 5 mL of toluene to each vial, while rinsing 27.2.2 Internal Standard (ISTD)—4,4’-dibromobiphenyl,
particles from the glass rod. Shake vigorously or otherwise 5 µg ⁄mL in xylene.
agitate (for example, ultrasonicate) sample for a minimum of 27.2.3 Surrogate Standard—Hexabromobenzene,
2 min. Allow to settle for 5 min or filter through a fast filter 2.5 mg ⁄mL hexabromobenzene in xylene.
paper. 27.2.4 Xylene—Spectral quality or chromatographic grade.
26.3.1.4 For each specimen, transfer a clear 1.0 mL aliquot 27.2.5 Specimen Vials should be VOC capable.
of toluene solution to a GC vial. Add 20 µL of ISTD to each 27.3 Sample Preparation—Three specimens of the gypsum
vial. panel product should be available for testing. Remove surfac-
26.4 Preparation of Apparatus: ing material and crush a piece of each specimen with a mortar
and pestle to a powder.
NOTE 14—Instrument should be tuned daily using decafluorotriphenyl- 27.3.1 GC Specimen Preparation:
phosphine (DFTPP). 27.3.1.1 Collect 1.0 g of each crushed specimen and transfer
26.4.1 Column—Fused silica capillary column, 30 m by to a separate, sealable 10 mL vial.
0.32 mm; 0.5 µm film thickness; type DB-1 or DB-5, glass 27.3.1.2 Spike each specimen with 50 µL of surrogate
gooseneck inlet liner without glass wool. standard. Mix well using a glass rod and allow sample to air
26.4.2 Carrier Gas—Helium. dry.
26.4.3 Injection Port—250°C; splitless. 27.3.1.3 Add 5 mL of toluene to each vial, rinsing any
particles off of the glass rod. Shake vigorously or otherwise
26.4.4 Temperature Program—120°C for 1 min; 9°C/min to
agitate (for example, ultrasonicate) sample for a minimum of
285°C; hold for 10 min.
2 min. Allow to settle for 5 min or filter through a fast filter
26.4.5 Mass Spectrometer—Full scan (30 to 600 m/z range) paper.
in scan mode. 27.3.1.4 For each specimen, transfer a clear 1.0 mL aliquot
26.4.6 Sample Injection Amount—1.0 µL. of toluene solution to a GC vial. Add 20 µL of internal standard
26.5 Identification—S8 is identified by mass spectrum to each vial.
(64 m ⁄z will be the most abundant ion). Confirm by retention 27.4 Preparation of Apparatus:
time matching to a calibration standard. The internal standard 27.4.1 Column—Fused silica capillary column, 30 m by
will yield ions at 152 and 312 m/z. The surrogate’s most 0.32 mm; 0.5 µm film thickness; type DB-1 or DB-5, glass
abundant ions will be found at 552 m/z. gooseneck inlet liner without glass wool.
26.6 Calculation: 27.4.2 Carrier Gas—Helium
26.6.1 Integrate the S8 and ISTD areas for each calibration 27.4.3 Injection Port—250°C; splitless.
standard. Calculate the peak area ratio by dividing the S8 peak 27.4.4 Temperature Program—120°C for 1 min; 9°C/min to
area by the internal standard peak area. Build a calibration 285°; hold for 10 min.
curve based on the peak area ratios for each standard. 27.4.5 Sample Injection Amount—1.0 µL.
26.6.2 Calculate the peak area ratio for each specimen. Use 27.5 Identification—Identification can only be done by re-
the calibration curve to calculate the S8 concentration in tention time matching to a standard.
solution. 27.6 Calculation:
26.6.3 Calculate the concentration of S8 in the original 27.6.1 Integrate the S8 and internal standard peak areas for
sample in mg/kg using the sample weight, final extract volume, each calibration standard. Calculate the peak area ratio by
and concentration value obtained in 26.6.2. dividing the S8 peak area by the internal standard peak area.
26.6.4 Calculate the percent recovery of the surrogate com- Build a calibration curve based on the peak area ratios for each
pound to evaluate the extraction efficiency. standard.

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 C471M − 17a´1
27.6.2 Calculate the peak area ratio for each specimen. Use 28.3.1.3 Allow each sample to settle for 5 min and then
the calibration curve to calculate the S8 concentration in transfer each sample to a separate appropriate vial.
solution. 28.3.1.4 Centrifuge each extract for 5 min and then transfer
27.6.3 Calculate the concentration of S8 in the original the top layer of each extract to a separate HPLC crimp top vial
sample in mg/kg using the sample weight, final extract volume, for analysis.
and concentration value obtained in 27.6.2. 28.4 Preparation of HPLC/UV:
27.6.4 Calculate the percent recovery of the surrogate com- 28.4.1 Column—5 µm C18 reverse phase column (4.6 by
pound to evaluate the extraction efficiency. 250 mm).
27.7 Precision and Bias—An interlaboratory study of this 28.4.2 UV Wavelength—250 nm.
test method is being conducted, and a complete precision 28.4.3 Flow Rate—1 mL/min.
statement is expected to be available on or before 2019. 28.4.4 Eluent—95/5 methanol/water.
27.8 Report—Report the quantity of orthorhombic cyclooc- 28.4.5 Run Time—15 min.
tasulfur (S8) calculated in 27.6.3 determined to the nearest 28.5 Identification—Identification of S8 can only be done by
1 mg ⁄kg. retention time matching to a standard.
28.6 Calculation:
28. Determination of Orthorhombic Cyclooctasulfur (S8)
28.6.1 Calculate the peak area ratio for each specimen. Use
in Gypsum Panel Products by High-Performance
the calibration curve to calculate the S8 concentration in
Liquid Chromatograph Equipped with Ultraviolet
solution.
Detector (HPLC/UV)
28.6.2 Calculate the concentration of S8 in the original
28.1 Apparatus—High-performance liquid chromatograph sample in mg/kg using the sample weight, final extract volume,
(HPLC) equipped with an ultraviolet (UV) detector. and concentration value obtained in 28.6.1.
28.1.1 Software must be capable of integrating peak areas. 28.6.3 Calculate the percent recovery of the orthorhombic
28.2 Reagents and Materials: cyclooctasulfur (S8) standard matrix to evaluate the extraction
28.2.1 HPLC Methodology. efficiency for the extraction batch.
28.2.2 Tetrachloroethylene—HPLC grade. 28.7 Precision and Bias—An interlaboratory study of this
28.2.3 Methanol—HPLC grade. test method is being conducted, and a complete precision
28.2.4 Deionized water—HPLC grade. statement is expected to be available on or before 2019.
28.2.5 Specimen vials should be VOC capable.
28.8 Report—Report the quantity of orthorhombic cyclooc-
28.3 Sample Preparation—Three specimens of the gypsum tasulfur (S8) calculated in Section 28.6.3 determined to the
panel product should be available for testing. Remove surfac- nearest 1 mg/kg.
ing material and crush a piece of each specimen with a mortar
and pestle to a powder. 29. Keywords
28.3.1 HPLC Sample Preparation: 29.1 ammonium acetate method; atomic absorption; chemi-
28.3.1.1 Collect 1.0 g of each crushed specimen and transfer cal analysis; coulometric method; flame photometry; gas
to a separate, sealable 4.0 mL extraction vial. chromatography/electron capture detector; gas
28.3.1.2 Add 5 mL of tetrachloroethylene to each vial, chromatography/mass spectrometry; gypsum; gypsum con-
rinsing any particles remaining on the glass rod or in the vial. crete; gypsum board; gypsum products; high-performance
Seal and shake vigorously or otherwise agitate (for example, liquid chromatography/UV detector; plaster; sand in set plas-
ultrasonicate) the sample for a minimum of 30 min. ter; sulfur (S8); wood-fiber plaster

SUMMARY OF CHANGES

Committee C11 has identified the location of selected changes to this standard since the last issue
(C471M – 17) that may impact the use of this standard. (Approved Oct. 1, 2017.)

(1) Revised 17.4, 18.1, and 18.5. (2) Revised 7.2.1 and 8.3.2.

Committee C11 has identified the location of selected changes to this standard since the last issue
(C471M – 16a) that may impact the use of this standard. (Approved June 15, 2016.)

(1) Added 7.4 through 7.4.4 and Table 1. (3) Added 17.5 through 17.5.4 and Table 3.
(2) Added 8.5 through 8.5.4 and Table 2. (4) Added 18.6 through 18.6.4 and Table 4.

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17
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 C471M − 17a´1
Committee C11 has identified the location of selected changes to this standard since the last issue
(C471M – 16) that may impact the use of this standard. (Approved June 15, 2016.)

(1) Revised 26.3, 26.3.1.1, 27.3, 27.3.1.1, 28.3, and 28.3.1.1 to

replace “grind” or “ground” with “crush” or “crushed,” respec-
tively.

Committee C11 has identified the location of selected changes to this standard since the last issue (2014 as
C471M – 14) that may impact the use of this standard. (Approved Jan. 1, 2016.)

(1) Updated 1.2 to show new added methods. (4) Renumbered sections to improve uniformity of these Test
(2) Added Section 17 (“Alternative Procedure for Analysis of Methods.
Free Water in Gypsum Using a Moisture Balance”). (5) Revised 1.2 to show new added methods and to reflect
(3) Added Section 18 (“Alternative Procedure for Analysis of subsequent renumbering of sections.
Combined Water in Gypsum Using a Moisture Balance”).

Committee C11 has identified the location of selected changes to this standard since the last issue (2012 as
C471M – 13) that may impact the use of this standard. (Approved Nov. 1, 2014.)

(1) Replaced previous Sections 55 – 65 with new Sections 66

– 69.

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