ASTM D2187-94(1998)
(Test Method)Standard Test Methods for Physical and Chemical Properties of Particulate Ion-Exchange Resins
Standard Test Methods for Physical and Chemical Properties of Particulate Ion-Exchange Resins
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: Sections Test Method A--Pretreatment 6 to 10 Test Method B--Water Retention Capacity 11 to 17 Test Method C--Backwashed and Settled Density 18 to 24 Test Method D--Particle Size Distribution 25 to 32 Test Method E--Salt-Splitting Capacity of Cation- 33 to 41 Exchange Resins Test Method F--Total Capacity of Cation-Exchange 42 to 50 Resins Test Method G--Percent Regeneration of Hydrogen- 51 to 58 Form Cation-Exchange Resins Test Method H--Total and Salt-Splitting Capacity of 59 to 66 Anion-Exchange Resins Test Method I--Percent Regeneration of Anion Ex- 67 to 75 change Resins Test Method J--Ionic Chloride Content of Anion- 76 to 83 Exchange Resins Test Method K--Carbonate Content of Anion-Ex- 84 to 91 change Resins Test Method L--Sulfate Content of Anion Exchange 92 to 99 Resins Test Method M--Total Anion Capacity of Anion- 100 to 108 Exchange Resins
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 Note 1.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation: D 2187 – 94 (Reapproved 1998)
Standard Test Methods for
Physical and Chemical Properties of Particulate Ion-
Exchange Resins
This standard is issued under the fixed designation D 2187; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 These test methods cover the determination of the 2.1 ASTM Standards:
physical and chemical properties of ion-exchange resins when D 1129 Terminology Relating to Water
used for the treatment of water. They are intended for use in D 1193 Specification for Reagent Water
testing both new and used materials. The following thirteen test D 1293 Test Methods for pH of Water
methods are included: D 2687 Practices for Sampling Particulate Ion-Exchange
Materials
D 2777 Practice for Determination of Precision and Bias of
Sections
Test Method A—Pretreatment 6-10
Applicable Methods of Committee D-19 on Water
Test Method B—Water Retention Capacity 11-17
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
Test Method C—Backwashed and Settled Density 18-24
poses
Test Method D—Particle Size Distribution 25-32
Test Method E—Salt-Splitting Capacity of Cation- 33-41
Exchange Resins
3. Terminology
Test Method F—Total Capacity of Cation-Exchange 42-50
3.1 Definitions—For definitions of terms used in these test
Resins
Test Method G—Percent Regeneration of Hydrogen- 51-58
methods refer to Terminology D 1129.
Form Cation-Exchange Resins
3.2 Definitions of Terms Specific to This Standard:
Test Method H—Total and Salt-Splitting Capacity of 59-66
3.2.1 anion-exchange material—an ion-exchange material
Anion-Exchange Resins
Test Method I—Percent Regeneration of Anion 67-75
capable of the reversible exchange of negatively charged ions.
Exchange Resins
3.2.2 cation-exchange material—an ion-exchange material
Test Method J—Ionic Chloride Content of Anion- 76-83
capable of the reversible exchange of positively charged ions.
Exchange Resins
Test Method K—Carbonate Content of Anion- 84-91
3.2.3 ion-exchange resin—a synthetic organic ion-exchange
Exchange Resins
material.
Test Method L—Sulfate Content of Anion Exchange 92-99
Resins 3.2.4 mixed bed— a physical mixture of anion-exchange
Test Method M—Total Anion Capacity of Anion- 100-108
material and cation-exchange material.
Exchange Resins
4. Reagents
1.2 The values stated in SI units are to be regarded as the
standard. The inch-pound units given in parentheses are for
4.1 Purity of Reagents—Reagent grade chemicals shall be
information only.
used in all tests. Unless otherwise indicated, it is intended that
1.3 This standard does not purport to address all of the
all reagents shall conform to the specifications of the Commit-
safety concerns, if any, associated with its use. It is the
tee on Analytical Reagents of the American Chemical Society,
responsibility of the user of this standard to establish appro-
where such specifications are available. Other grades may be
priate safety and health practices and determine the applica-
used, provided it is first ascertained that the reagent is of
bility of regulatory limitations prior to use. Specific precau-
sufficiently high purity to permit its use without lessening the
tionary statements are given in Note 1.
accuracy of the determination.
These test methods are under the jurisdiction of ASTM Committee D-19 on
Water and are the direct responsibility of Subcommittee D19.08 on Membranes and
Ion Exchange Materials. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved April 15, 1994. Published June 1994. Originally Annual Book of ASTM Standards, Vol 11.02.
published as D 2187 – 63T. Last previous edition D 2187 – 93. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 2187 – 94 (1998)
4.2 Purity of Water— Unless otherwise indicated, refer-
ences to water shall be understood to mean Type IV reagent
water described in Specification D 1193.
5. Sampling
5.1 Obtain a representative sample of the ion-exchange
resin in accordance with Practices D 2687.
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
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 compari-
son, therefore, the sample should be converted to a known
ionic form before analysis. This procedure provides for the
FIG. 1 Typical Arrangement of Apparatus for Pretreatment of Ion-
conversion of cation-exchange materials to the sodium form
Exchange Materials
and anion-exchange materials to the chloride form prior to
analysis. These forms are chosen since they permit samples to
9. Reagents
be weighed and dried without concern for air contamination or
9.1 Hydrochloric Acid (1 + 9)—Carefully pour 100 mL of
decomposition. If other ionic forms are used this fact should be
hydrochloric acid (HCl, sp gr 1.19) into 900 mL of water,
noted in reporting the results.
stirring constantly. Cool to 25 6 5°C.
9.2 Sodium Chloride Solution (100 g/L)—Dissolve 100.0 g
8. Apparatus
of sodium chloride (NaCl) in 800 mL of water and dilute to 1
8.1 Pretreatment Apparatus (See Fig. 1):
L.
8.1.1 Column, transparent, vertically-supported, 25 6 2.5
9.3 Sodium Chloride Solution (240 g/L)—Dissolve 240 g of
mm (1.0 6 0.1 in.) inside diameter and approximately 1500
sodium chloride (NaCl) in 800 mL of water and dilute to 1 L.
mm (60 in.) long. The bottom of the column shall be closed and
9.4 Sodium Hydroxide Solution (40 g/L)—Dissolve 40.0 g
provided with an outlet of approximately 6-mm inside diam-
of sodium hydroxide (NaOH) in 800 mL of water. Cool and
eter. Connections shall be provided at top and bottom for
dilute to 1 L.
admission and removal of solutions as described in Section 10.
9.5 Thymol Blue Indicator Solution—Dissolve 0.1 g of
Adequate means for measuring and regulating flow shall be
thymol blue (thymol sulfonphthalein) in 10.75 mL of 0.02 N
provided. Calibrate the column in such a manner that the
NaOH solution. Dilute to 250 mL with water.
volume readings required by the method can be made. Make all
9.6 Tropaeolin O Indicator Solution—Dissolve 0.10 g of
measurements at 25 6 5°C.
tropaeolin O (p-benzene-sulfonic acid-azoresorcinol) in 50 mL
8.1.2 Support, for the sample, so designed that the distance
of water and dilute to 100 mL in a volumetric flask.
from the sample to the column outlet is at least 50 mm.
Suggested supports are corrosion-resistant screen or porous 10. Procedure
plate.
10.1 Adjust the temperature of the water and all solutions to
8.2 Draining Apparatus (Fig. 2):
be used in the procedure to 25 6 5°C and maintain this
8.2.1 Buchner-Type Funnel, containing a 125-mm filter
temperature throughout the test.
paper and supported in a 1-L suction flask.
10.2 Transfer the entire sample as received to a 2-L beaker
8.2.2 Open-Arm Mercury Manometer, connected by a
using water to rinse out the container. Adjust the water level to
T-tube to a vacuum train.
the sample level. Let stand a minimum of 1 h. Mix thoroughly
8.2.3 Gas-Humidifying Tower, of at least 500 mL capacity,
and transfer a representative sample to fill a 400-mL beaker.
two thirds filled with glass beads or similar material. 10.3 Fill the pretreatment column one half full of water.
8.2.4 Vacuum Pump, capable of creating a pressure differ- Transfer the entire contents of the 400-mL beaker to the
ential 40 mm Hg below atmospheric pressure. column using additional water if necessary.
D 2187 – 94 (1998)
FIG. 2 Typical Arrangement of Water-Draining Apparatus
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. sample volume determined in 10.7.
10.5 If the sample is a mixed bed, displace the backwash
NOTE 1—Caution: Swelling of the resin in the column may occur in
water from the bed by slowly introducing NaCl solution (100
subsequent steps.
g/L) at the bottom of the column and allowing it to flow
10.9 Pass the specified volume of reagent through the bed at
upward through the sample. When the water has been dis-
the specified rate until only a 20 or 30 mm layer of liquid
placed, increase the flow rate until the anion-exchange resin is
remains above the bed. Rinse the bed with two sample volumes
separated from and suspended above the cation-exchange
of water at the same rate.
resin. Lower the backwash outlet tube as required to siphon off
10.10 Determine the amount of reagent and the flow rate
the anion-exchange resin, collecting it in a separate pretreat-
required for the second pretreatment from Table 2 using the
ment apparatus. Exercise care to prevent the removal of
sample volume determined in 10.7. Note that this second
cation-exchange resin in this operation. When the transfer of
pretreatment is not used for some methods.
the anion-exchange resin is complete, discontinue the flow of
10.11 Pass the specified volume of reagent through a bed at
NaCl solution. If the separation of anion and cation-exchange
the specified rate until only a 20 to 30-mm layer of liquid
resins has not been complete and a mixed band is left in the
remains above the bed. Rinse the bed with one sample volume
center, repeat the siphoning procedure to remove this band
of water at the same rate. Increase the rinse rate to 100 mL/min.
from the cation-portion of the sample. This mixed material that
Rinse for 15 min. Thereafter test successive 100-mL portions
should not constitute more than 5 % of the original sample
of the effluent from anion-exchange resins by adding two drops
volume, is not included in subsequent tests. If more than 5 %
of thymol blue indicator solution. Continue rinsing until a 100
of the sample remains unseparated, the separation should be
repeated using NaCl solution (240 g/L). In either case proceed
with the separated anion and cation components as separate
TABLE 1 Requirements for Initial Pretreatment
samples as described in 10.6.
Anion-Exchange Cation-Exchange
Resins Resins
10.6 Allow the resin to settle until the liquid level is 20 to 30
mm above the top of the bed, and estimate its volume. Pass
Reagent NaOH HCl
Concentration 40 g/L 1 + 9
NaCl solution (100 g/L) downflow through the single compo-
Volume required 8 sample volumes 8 sample volumes
nent sample or the separated components of the mixed bed
Contact time 1 h 1 h
resin at the approximate rate of 0.133 mL/min/mL of sample Flow rate, mL/min-mL sample 0.133 0.133
Regeneration level:
for 1 h. Discontinue the flow of NaCl solution. Backwash with
lb/ft 20.0 21.2
water for 10 min at a flow rate sufficient to maintain a 50 %
g/L 320 340
expansion of the bed. Discontinue the flow of water.
D 2187 – 94 (1998)
TABLE 2 Requirements for Second Pretreatment
rectly dependent on the ionic form of the material, careful
Anion-Exchange Cation-Exchange preconditioning of both original and used samples to known
Resins Resins
ionic forms as outlined in Section 7 is essential when such
Reagent HCl NaOH
comparisons are made.
Concentration 1 + 9 40 g/L
Volume required 8 sample volumes 4 sample volumes
14. Procedure
Contact time 1 h 0.5 h
Flow rate, mL/min-mL sample 0.133 0.133
14.1 Weigh three approximately 5-g representative samples
Regeneration level:
of material pretreated in accordance with Section 10 to the
lb/ft 21.2 10.0
nearest 1 mg into previously tared weighing vessels.
g/L 340 160
14.2 Dry the samples for 18 6 2hat104 6 2°C.
14.3 Remove the samples from the oven. Cool 30 min in a
desiccator, and reweigh.
mL portion of the effluent remains yellow (pH > 2.5) on the
addition of the indicator. Test the effluent from the cation-
15. Calculation
exchange resins in the same manner with two drops of
15.1 Calculate the water retention capacity, in percent, as
tropaeolin-O indicator solution. Continue rinsing until a
follows:
100-mL portion of the effluent remains yellow (pH < 11.0) on
the addition of the indicator. water retained, % 5 [ A 2 B!/A] 3 100 (1)
~
10.12 Remove the ion-exchange resin from the pretreatment
where:
column, discarding any extraneous material that may have
A = amount of wet sample used, g, and
accumulated at the bottom of the bed. Transfer the resin to the
B = amount of dry sample obtained, g.
Buchner funnel of the draining apparatus that has been fitted
with a medium porosity filter paper. Drain the water to the top
16. Report
of the sample using suction if required. Cover the funnel with
16.1 Report the percent water retained as the average of the
a suitable vacuum-tight cover, which is fitted with an inlet for
three values obtained.
air from the water-filled humidifying tower. Apply sufficient
suction to maintain a pressure differential of 40 6 5mmHg
17. Precision and Bias
below atmospheric pressure. Continue passing humidified air
17.1 Precision—The precision of this test method of deter-
through the sample for 10 min.
mining water retention capacity of ion exchange resins may be
10.13 Transfer the entire drained sample to a clean, dry, 1-L
expressed as follows:
(1-qt.), wide-mouthed bottle with a screw top or other vapor-
S 5 0.017x
T
tight closure.
S 5 0.004x
o
TEST METHOD B—WATER RETENTION CAPACITY
where:
11. Scope
S = overall precision,
T
S = single-operator precision, and
o
11.1 This test method covers the determination of the
x = water retention capacity determined in percent.
amount of water retained by ion-exchange resins and is
17.1.1 Information given for the pre
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.