ASTM D2187-94(2009)e1

Standard Test Methods for Physical and Chemical Properties of Particulate Ion-Exchange Resins

SIGNIFICANCE AND USE
The ionic form of an ion-exchange material affects both its equivalent mass and its equilibrium water content. These in turn influence the numerical values obtained in exchange capacity determinations, in density measurements, and in the size of the particles. To provide a uniform basis for comparison, therefore, the sample should be converted to a known ionic form before analysis. This procedure provides for the conversion of cation-exchange materials to the sodium form and anion-exchange materials to the chloride form prior to analysis. These forms are chosen since they permit samples to be weighed and dried without concern for air contamination or decomposition. If other ionic forms are used this fact should be noted in reporting the results.
SCOPE
1.1 These test methods cover the determination of the physical and chemical properties of ion-exchange resins when used for the treatment of water. They are intended for use in testing both new and used materials. The following thirteen test methods are included:
1.2 The values stated in SI units are to be regarded as the standard. The inch-pound units given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 10.8.

General Information

• Status: Historical
• Publication Date: 30-Apr-2009
• ICS: 71.100.40 - Surface active agents
• Technical Committee: D19 - Water
• Drafting Committee: D19.08 - Membranes and Ion Exchange Materials

Relations

• Replaced By: ASTM D2187-17 - Standard Test Methods and Practices for Evaluating Physical and Chemical Properties of Particulate Ion-Exchange Resins
• Effective Date: 01-Aug-2017

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: D2187 − 94 (Reapproved 2009)
Standard Test Methods for
Physical and Chemical Properties of Particulate Ion-
Exchange Resins
This standard is issued under the fixed designation D2187; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—A typo was editorially corrected in Section 47.7 in March 2010.
1. Scope priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
1.1 These test methods cover the determination of the
tionary statements are given in Section 10.8.
physical and chemical properties of ion-exchange resins when
used for the treatment of water. They are intended for use in
2. Referenced Documents
testingbothnewandusedmaterials.Thefollowingthirteentest
2.1 ASTM Standards:
methods are included:
D1129Terminology Relating to Water
Sections
D1193Specification for Reagent Water
Test MethodA—Pretreatment 6–10
D1293Test Methods for pH of Water
Test Method B—Water Retention Capacity 11–17
Test Method C—Backwashed and Settled Density 18–24
D2687PracticesforSamplingParticulateIon-ExchangeMa-
Test Method D—Particle Size Distribution 25–32
terials
Test Method E—Salt-Splitting Capacity of Cation- 33–41
D2777Practice for Determination of Precision and Bias of
Exchange Resins
Test Method F—Total Capacity of Cation-Exchange 42–50
Applicable Test Methods of Committee D19 on Water
Resins
E11Specification forWovenWireTest Sieve Cloth andTest
Test Method G—Percent Regeneration of Hydrogen- 51–58
Sieves
Form Cation-Exchange Resins
Test Method H—Total and Salt-Splitting Capacity of 59–66
3. Terminology
Anion-Exchange Resins
Test Method I—Percent Regeneration ofAnion 67–75
3.1 Definitions—For definitions of terms used in these test
Exchange Resins
Test Method J—Ionic Chloride Content ofAnion- 76–83 methods refer to Terminology D1129.
Exchange Resins
3.2 Definitions of Terms Specific to This Standard:
Test Method K—Carbonate Content ofAnion- 84–91
Exchange Resins
3.2.1 anion-exchange material—an ion-exchange material
Test Method L—Sulfate Content ofAnion Exchange 92–99
capable of the reversible exchange of negatively charged ions.
Resins
Test Method M—TotalAnion Capacity ofAnion- 100 – 108
3.2.2 cation-exchange material—an ion-exchange material
Exchange Resins
capable of the reversible exchange of positively charged ions.
1.2 The values stated in SI units are to be regarded as the
3.2.3 ion-exchange resin—a synthetic organic ion-exchange
standard. The inch-pound units given in parentheses are for
material.
information only.
3.2.4 mixed bed—a physical mixture of anion-exchange
1.3 This standard does not purport to address all of the
material and cation-exchange material.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Reagents
4.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
These test methods are under the jurisdiction of ASTM Committee D19 on
Water and are the direct responsibility of Subcommittee D19.08 on Membranes and
Ion Exchange Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2009. Published June 2009. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1963. Last previous edition approved in 2004 as D2187–94 (2004). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D2187-94R09E01. the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
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D2187 − 94 (2009)
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
4.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type IV reagent water
described in Specification D1193.
5. Sampling
5.1 Obtain a representative sample of the ion-exchange
resin in accordance with Practices D2687.
5.2 A minimum sample size of 1 L is recommended for a
complete testing program.
TEST METHOD A—PRETREATMENT
6. Scope
6.1 This test method covers the conversion of ion-exchange
resins to a known ionic form and is intended for application to
both new and used material.
7. Significance and Use
7.1 The ionic form of an ion-exchange material affects both
FIG. 1 Typical Arrangement of Apparatus for Pretreatment of Ion-
its equivalent mass and its equilibrium water content.These in
Exchange Materials
turn influence the numerical values obtained in exchange
capacity determinations, in density measurements, and in the
size of the particles. To provide a uniform basis for
comparison, therefore, the sample should be converted to a
8.1.2 Support, for the sample, so designed that the distance
known ionic form before analysis.This procedure provides for
from the sample to the column outlet is at least 50 mm.
the conversion of cation-exchange materials to the sodium
Suggested supports are corrosion-resistant screen or porous
form and anion-exchange materials to the chloride form prior
plate.
to analysis. These forms are chosen since they permit samples
to be weighed and dried without concern for air contamination
8.2 Draining Apparatus (Fig. 2):
ordecomposition.Ifotherionicformsareusedthisfactshould 8.2.1 Buchner-Type Funnel, containing a 125-mm filter
be noted in reporting the results.
paper and supported in a 1-L suction flask.
8.2.2 Open-ArmMercuryManometer,connectedbyaT-tube
8. Apparatus
to a vacuum train.
8.2.3 Gas-Humidifying Tower, of at least 500 mL capacity,
8.1 Pretreatment Apparatus (See Fig. 1):
two thirds filled with glass beads or similar material.
8.1.1 Column, transparent, vertically-supported, 25 6 2.5
8.2.4 Vacuum Pump, capable of creating a pressure differ-
mm (1.0 6 0.1 in.) inside diameter and approximately 1500
ential 40 mm Hg below atmospheric pressure.
mm(60in.)long.Thebottomofthecolumnshallbeclosedand
provided with an outlet of approximately 6-mm inside diam-
9. Reagents
eter. Connections shall be provided at top and bottom for
admissionandremovalofsolutionsasdescribedinSection10.
9.1 Hydrochloric Acid (1+9)—Carefully pour 100 mL of
Adequate means for measuring and regulating flow shall be
hydrochloric acid (HCl, sp gr 1.19) into 900 mL of water,
provided. Calibrate the column in such a manner that the
stirring constantly. Cool to 25 6 5°C.
volumereadingsrequiredbythemethodcanbemade.Makeall
9.2 Sodium Chloride Solution (100 g/L)—Dissolve 100.0 g
measurements at 25 6 5°C.
of sodium chloride (NaCl) in 800 mL of water and dilute to 1
L.
9.3 Sodium Chloride Solution (240 g/L)—Dissolve 240 g of
Reagent Chemicals, American Chemical Society Specifications, American
sodium chloride (NaCl) in 800 mL of water and dilute to 1 L.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
9.4 Sodium Hydroxide Solution (40 g/L)—Dissolve 40.0 g
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
of sodium hydroxide (NaOH) in 800 mL of water. Cool and
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. dilute to 1 L.
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D2187 − 94 (2009)
FIG. 2 Typical Arrangement of Water-Draining Apparatus
9.5 Thymol Blue Indicator Solution—Dissolve 0.1 g of the anion-exchange resin is complete, discontinue the flow of
thymol blue (thymol sulfonphthalein) in 10.75 mL of 0.02 N NaCl solution. If the separation of anion and cation-exchange
NaOH solution. Dilute to 250 mL with water. resins has not been complete and a mixed band is left in the
center, repeat the siphoning procedure to remove this band
9.6 Tropaeolin O Indicator Solution—Dissolve 0.10 g of
fromthecation-portionofthesample.Thismixedmaterialthat
tropaeolinO(p-benzene-sulfonicacid-azoresorcinol)in50mL
should not constitute more than 5% of the original sample
of water and dilute to 100 mL in a volumetric flask.
volume, is not included in subsequent tests. If more than 5%
of the sample remains unseparated, the separation should be
10. Procedure
repeated using NaCl solution (240 g/L). In either case proceed
10.1 Adjustthetemperatureofthewaterandallsolutionsto
with the separated anion and cation components as separate
be used in the procedure to 25 6 5°C and maintain this
samples as described in 10.6.
temperature throughout the test.
10.6 Allowtheresintosettleuntiltheliquidlevelis20to30
10.2 Transfer the entire sample as received to a 2-L beaker
mm above the top of the bed, and estimate its volume. Pass
using water to rinse out the container.Adjust the water level to
NaCl solution (100 g/L) downflow through the single compo-
the sample level. Let stand a minimum of 1 h. Mix thoroughly
nent sample or the separated components of the mixed bed
and transfer a representative sample to fill a 400-mL beaker.
resin at the approximate rate of 0.133 mL/min/mL of sample
10.3 Fill the pretreatment column one half full of water.
for 1 h. Discontinue the flow of NaCl solution. Backwash with
Transfer the entire contents of the 400-mL beaker to the
water for 10 min at a flow rate sufficient to maintain a 50%
column using additional water if necessary.
expansion of the bed. Discontinue the flow of water.
10.4 Backwash with water using a flow rate that will
10.7 Allow the bed to settle and then drain off the water at
maintain a 50% expansion of the bed. Adjust the backwash
a rate of approximately 100 mL/min until the water level is 20
outlet tube to a height above the bed equal to 75% of the bed
to 30 mm above the top of the bed. Estimate the volume of
height. Continue backwashing for a minimum of 10 min or
ion-exchange resin in millilitres.
until the effluent is clear. For mixed bed samples proceed in
10.8 Determine the amount of reagent and the flow rate
accordance with 10.5. For single component samples, proceed
required for the initial pretreatment from Table 1 using the
in accordance with 10.6.
10.5 If the sample is a mixed bed, displace the backwash
TABLE 1 Requirements for Initial Pretreatment
water from the bed by slowly introducing NaCl solution (100
Anion-Exchange Cation-Exchange
g/L) at the bottom of the column and allowing it to flow Resins Resins
upward through the sample. When the water has been
Reagent NaOH HCl
Concentration 40 g/L 1+9
displaced, increasetheflowrateuntiltheanion-exchangeresin
Volume required 8 sample volumes 8 sample volumes
is separated from and suspended above the cation-exchange
Contact time 1 h 1 h
resin.Lowerthebackwashoutlettubeasrequiredtosiphonoff Flow rate, mL/min-mL sample 0.133 0.133
Regeneration level:
the anion-exchange resin, collecting it in a separate pretreat-
lb/ft 20.0 21.2
ment apparatus. Exercise care to prevent the removal of
g/L 320 340
cation-exchange resin in this operation. When the transfer of
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D2187 − 94 (2009)
sample volume determined in 10.7.(Warning—Swelling of 12. Summary of Test Method
the resin in the column may occur in subsequent steps.)
12.1 This test method consists of the determination of the
10.9 Passthespecifiedvolumeofreagentthroughthebedat loss of mass on drying at 104 6 2°C.
the specified rate until only a 20 or 30 mm layer of liquid
13. Significance and Use
remainsabovethebed.Rinsethebedwithtwosamplevolumes
of water at the same rate.
13.1 The water retention capacity of an ion-exchange ma-
terial is proportional to its pore volume. For new materials of
10.10 Determine the amount of reagent and the flow rate
thesamefunctionalityandpolymertype,highervaluesindicate
required for the second pretreatment from Table 2 using the
lower effective crosslinking. Increases in water retention ca-
sample volume determined in 10.7. Note that this second
pacity of used materials as compared with the values for new
pretreatment is not used for some methods.
material serve as an indicator of polymer decrosslinking:
10.11 Pass the specified volume of reagent through a bed at
decreasesmayindicateeitherlossoffunctionalityorfoulingof
the specified rate until only a 20 to 30-mm layer of liquid
the ion-exchange material. Since the numerical value is di-
remains above the bed. Rinse the bed with one sample volume
rectly dependent on the ionic form of the material, careful
ofwateratthesamerate.Increasetherinserateto100mL/min.
preconditioning of both original and used samples to known
Rinse for 15 min. Thereafter test successive 100-mL portions
ionic forms as outlined in Section 7 is essential when such
oftheeffluentfromanion-exchangeresinsbyaddingtwodrops
comparisons are made.
of thymol blue indicator solution. Continue rinsing until a 100
mL portion of the effluent remains yellow (pH > 2.5) on the
14. Procedure
addition of the indicator. Test the effluent from the cation-
14.1 Weigh three approximately 5-g representative samples
exchange resins in the same manner with two drops of
of material pretreated in accordance with Section 10 to the
tropaeolin-O indicator solution. Continue rinsing until a
nearest 1 mg into previously tared weighing vessels.
100-mLportion of the effluent remains yellow (pH < 11.0) on
the addition of the indicator. 14.2 Dry the samples for 18 62hat104 6 2°C.
10.12 Removetheion-exchangeresinfromthepretreatment 14.3 Remove the samples from the oven. Cool 30 min in a
column, discarding any extraneous material that may have desiccator, and reweigh.
accumulated at the bottom of the bed. Transfer the resin to the
15. Calculation
Buchner funnel of the draining apparatus that has been fitted
with a medium porosity filter paper. Drain the water to the top
15.1 Calculate the water retention capacity, in percent, as
of the sample using suction if required. Cover the funnel with
follows:
a suitable vacuum-tight cover, which is fitted with an inlet for
waterretained, % 5 A 2 B /A 3100 (1)
@~ ! #
air from the water-filled humidifying tower. Apply sufficient
suction to maintain a pressure differential of 40 65mmHg where:
below atmospheric pressure. Continue passing humidified air
A = amount of wet sample used, g, and
through the sample for 10 min.
B = amount of dry sample obtained, g.
10.13 Transfertheentiredrainedsampletoac
...