Standard Practice for Determination of Adsorptive Capacity of Activated Carbon by a Micro-Isotherm Technique for Adsorbates at ppb Concentrations

SIGNIFICANCE AND USE
5.1 This practice allows the adsorption capacity at equilibrium of an activated carbon for adsorbable constituents present in water to be determined. The Freundlich K and 1/n constants that can be calculated based upon information collected using this practice can be used to estimate carbon loading capacities and usages rates for the constituent present in a water stream at other concentrations.
SCOPE
1.1 This practice covers the assessment of activated carbon for the removal of low concentrations of adsorbable constituents from water and wastewater using the bottle point isotherm technique. It can be used to characterize the adsorptive properties of virgin and reactivated activated carbons.  
1.2 This practice can be used in systems with constituent concentrations in the low milligrams per litre or micrograms per litre concentration ranges.  
1.3 This practice can be used to determine the adsorptive capacity of and Freundlich constants for volatile organic compounds provided the handling procedures described in this practice are followed carefully.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The following safety caveat applies to the procedure section of this practice: 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.

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28-Feb-2017
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ASTM D5919-96(2017) - Standard Practice for Determination of Adsorptive Capacity of Activated Carbon by a Micro-Isotherm Technique for Adsorbates at ppb Concentrations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5919 − 96 (Reapproved 2017)
Standard Practice for
Determination of Adsorptive Capacity of Activated Carbon
by a Micro-Isotherm Technique for Adsorbates at ppb
Concentrations
This standard is issued under the fixed designation D5919; 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.
1. Scope 3. Terminology
1.1 This practice covers the assessment of activated carbon 3.1 Definitions:
for the removal of low concentrations of adsorbable constitu- 3.1.1 Fordefinitionsoftermsusedinthispracticerelatingto
entsfromwaterandwastewaterusingthebottlepointisotherm activated carbon, refer to Terminology D2652.
technique. It can be used to characterize the adsorptive 3.1.2 Fordefinitionsoftermsusedinthispracticerelatingto
properties of virgin and reactivated activated carbons. water, refer to Terminology D1129.
1.2 This practice can be used in systems with constituent
4. Summary of Practice
concentrations in the low milligrams per litre or micrograms
4.1 This practice consists of the determination of the ad-
per litre concentration ranges.
sorptive capacity of activated carbon for adsorbable constitu-
1.3 This practice can be used to determine the adsorptive
ents by contacting the aqueous solution contained in an
capacity of and Freundlich constants for volatile organic
essentially zero headspace container with activated carbon,
compounds provided the handling procedures described in this
determining the amount of the constituents removed, and
practice are followed carefully.
calculating the adsorptive capacity and the Freundlich
1.4 The values stated in SI units are to be regarded as
constants, K and 1/n, from a Freundlich isotherm plot.
standard. No other units of measurement are included in this
4.1.1 The weights of activated carbon used in this practice
standard.
may have to be adjusted to achieve reasonable levels of
removal of the constituent. The best data is obtained when
1.5 The following safety caveat applies to the procedure
section of this practice: This standard does not purport to carbondosagesareselectedthatresultinnomorethan90%or
address all of the safety concerns, if any, associated with its nolessthan10%oftheadsorbableconstituentsbeingremoved
use. It is the responsibility of the user of this standard to from the water by the carbon.
establish appropriate safety and health practices and deter- 4.1.2 If carbon dosages used are less than 1 mg, larger
mine the applicability of regulatory limitations prior to use. volumes of the aqueous solution may be used, such as
1000mL.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
D1129Terminology Relating to Water
5.1 This practice allows the adsorption capacity at equilib-
D1193Specification for Reagent Water
riumofanactivatedcarbonforadsorbableconstituentspresent
D2652Terminology Relating to Activated Carbon
in water to be determined.The Freundlich K and 1/n constants
D2867Test Methods for Moisture in Activated Carbon
that can be calculated based upon information collected using
D3370Practices for Sampling Water from Closed Conduits
this practice can be used to estimate carbon loading capacities
andusagesratesfortheconstituentpresentinawaterstreamat
other concentrations.
This practice is under the jurisdiction of ASTM Committee D28 on Activated
Carbon and is the direct responsibility of Subcommittee D28.02 on Liquid Phase
6. Interferences
Evaluation.
Current edition approved March 1, 2017. Published March 2017. Originally
6.1 The water shall not contain any nondissolved compo-
approved in 1996. Last previous edition approved in 2011 as D5919–96 (2011).
nents.
DOI: 10.1520/D5919-96R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.2 The presence of naturally occurring organic compounds
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
such as humic acids in the water being studied may signifi-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. cantly affect the ability of the carbon to adsorb the constituent
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5919 − 96 (2017)
of interest. Results obtained when using water other than 10. Preparation of the Activated Carbon
reagent grade water may be unique for the particular water
10.1 This practice requires the use of well washed activated
used and it may not be possible to apply these results to other
carbon that has been reduced in particle size so that 90% or
water systems.
greater passes through a U.S. No. 325-mesh (45-µm) sieve by
6.3 The adsorption isotherm data collected using this prac- wet screening or equivalent.
tice can be affected by the ionic strength, pH and temperature
10.2 Approximately 25 g of the powdered activated carbon
of the water, and the presence and growth of microorganisms.
sample is placed into each of four clean 250-mL bottles. The
remainder of the bottle is filled with reagent grade water.
7. Apparatus
10.3 The bottle is tightly capped and inverted three to five
7.1 Equilibrator(orotherrotatingmixingdevice),arotating
times to mix the contents.
device operating at 25 rpm which can rotate the isotherm
10.4 Thebottlesarethencentrifugedat2000rpmfor15min
bottles end-over-end, ensuring good dispersion of the pow-
to settle the activated carbon. The supernate is poured off and
dered activated carbon in the water being treated.
the procedure is repeated until the supernatant is clear.Allow-
7.2 Grinding Mill,capableofgrindingmaterialsothat90%
ing the mixture to sit for a period of time to allow the carbon
passes through a U.S. No. 325-mesh (45-µm) sieve.
to settle prior to decanting is also acceptable.
7.3 Isotherm Bottles, narrow neck amber bottles with poly-
10.5 The wet carbon is next dried in an oven at 110°C to a
tetrafluoroethylene (PTFE)-coated septum sealed caps of 250-,
constant weight and placed in a desiccator to cool.
500-, and 1000-mL capacity suitable for use in a centrifuge
10.6 As an alternate technique to drying the carbon sample,
operating at 2000 rpm.
carbon may be placed in a soxhlet extraction device and
7.4 Solution Delivery Tank, a 10-L, 316 stainless steel
extractedforaperiodofupto1weekwithreagentgrade(Type
container equipped with a PTFE-coated floating lid and a 316
II) water.
stainless ball valve to control flow during bottle filling.
10.7 The dry activated carbon is transferred to clean 1-L
7.5 Analytical Balance, capable of weighing to the nearest
brown borosilicate bottles with PTFE liners in the caps and
0.1 mg.
stored in an inert atmosphere such as nitrogen for future use.
7.6 Oven, forced-air circulation, capable of temperature
11. Activated Carbon Sample Weighing Procedure
regulation up to 250°C.
11.1 This procedure allows the carbon to be handled at
7.7 Centrifuge, capable of handling isotherm bottles up to
ambient conditions by calculating a correction for water
1L in size at 2000 rpm.
adsorbed from the air.
7.8 Magnetic Stirring Bars and Stirrers.
11.2 The powdered activated carbon sample is allowed to
come to equilibrium in a desiccator containing a saturated salt
8. Reagents
solution that will produce a relative humidity comparable to
ambient laboratory conditions. During the 24-h conditioning
8.1 Reagent Water,inaccordancewithSpecificationD1193,
period, care shall be taken not to expose the carbon to organic
Type II.
vapors.
8.2 Methanol, high purity HPLC grade.
11.3 The moisture picked up by the conditioned activated
8.3 Potassium Monobasic Phosphate (KHPO4), 1 M solu-
carbon is determined by weighing approximately 500 mg into
tion.
a tared (constant weight) bottle, drying for2hat110°C,
cooling in a desiccator, and re-weighing to determine weight
8.4 Sodium Hydroxide (NaOH), 1 M solution.
change(refertoTestMethodsD2867forstandardprocedures).
The ratio of change in weight between the activated carbon at
9. Cleaning Procedures
equilibrium with air and after drying is calculated and used as
9.1 This practice is capable of generating activated carbon
a correction factor for the weighed carbon dosages.
adsorptioncapacitydataonaqueoussolutionscontainingppbw
11.4 The carbon dosages are weighed by first taking a
(µg/L) levels of adsorbable constituents. It is therefore very
weighing boat, adding the desired mass of equilibrated acti-
important that all equipment and glassware that come in
vated carbon, and re-weighing the boat after transferring the
contact with the activated carbon or the water being treated be
carbon to the bottle. The carbon dosage is the difference
cleaned thoroughly to remove trace organic compounds.
between the carbon plus the boat weight and the final boat
9.2 All equipment and glassware should first be rigorously
weight.The weighed activated carbon dosage is then corrected
cleanedusingproceduresrecommendedbytheEPAforpriority
for ambient conditions and the actual dried carbon dosage
pollutantanalysis,hotwateranddetergentwash,reagentgrade
recorded.
water, and solvent (high purity methanol) rinse followed by a
bake-out.
12. Alternative Procedure for Addition of Known
Quantities of Activated Carbon to Isotherm Bottles
9.3 The glassware is baked out in an oven at 250°C for a
minimum of one hour. All PTFE and stainless steel apparatus 12.1 This alternate procedure makes use of a clean, dry
are dried at 110°C for one hour. activated carbon sample prepared according to procedures
D5919 − 96 (2017)
described in Section 10. Desired concentrations of carbon are phosphate buffer will change the ionic strength of the solution
added to each isotherm bottle volumetrically using a carbon and may promote biological activity. Other buffer relations
slurry of known concentration. may be used provided that they do not interfere with the
adsorption process.
12.2 Theconcentrationsoftheslurriesarechosensothat5-,
10-, and 20-mL volumes of each slurry would contai
...


This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5919 − 96 (Reapproved 2011) D5919 − 96 (Reapproved 2017)
Standard Practice for
Determination of Adsorptive Capacity of Activated Carbon
by a Micro-Isotherm Technique for Adsorbates at ppb
Concentrations
This standard is issued under the fixed designation D5919; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice covers the assessment of activated carbon for the removal of low concentrations of adsorbable constituents
from water and wastewater using the bottle point isotherm technique. It can be used to characterize the adsorptive properties of
virgin and reactivated activated carbons.
1.2 This practice can be used in systems with constituent concentrations in the low milligrams per litre or micrograms per litre
concentration ranges.
1.3 This practice can be used to determine the adsorptive capacity of and Freundlich constants for volatile organic compounds
provided the handling procedures described in this practice are followed carefully.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 The following safety caveat applies to the procedure section of this practice: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.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Closed Conduits
D2652 Terminology Relating to Activated Carbon
D2867 Test Methods for Moisture in Activated Carbon
D3370 Practices for Sampling Water from Closed Conduits
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this practice relating to activated carbon, refer to Terminology D2652.
3.1.2 For definitions of terms used in this practice relating to water, refer to Terminology D1129.
4. Summary of Practice
4.1 This practice consists of the determination of the adsorptive capacity of activated carbon for adsorbable constituents by
contacting the aqueous solution contained in an essentially zero head space headspace container with activated carbon, determining
the amount of the constituents removed, and calculating the adsorptive capacity and the Freundlich constants, K and 1/n, from a
Freundlich isotherm plot.
4.1.1 The weights of activated carbon used in this practice may have to be adjusted to achieve reasonable levels of removal of
the constituent. The best data is obtained when carbon dosages are selected that result in no more than 90 % or no less than 10 %
of the adsorbable constituents being removed from the water by the carbon.
This practice is under the jurisdiction of ASTM Committee D28 on Activated Carbon and is the direct responsibility of Subcommittee D28.02 on Liquid Phase Evaluation.
Current edition approved March 1, 2011March 1, 2017. Published May 2011March 2017. Originally approved in 1996. Last previous edition approved in 20062011 as
D5919 – 96 (2006).(2011). DOI: 10.1520/D5919-96R11.10.1520/D5919-96R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5919 − 96 (2017)
4.1.2 If carbon dosages used are less than 1 mg, larger volumes of the aqueous solution may be used, such as 1000 mL.
1000 mL.
5. Significance and Use
5.1 This practice allows the adsorption capacity at equilibrium of an activated carbon for adsorbable constituents present in
water to be determined. The Freundlich K and 1/n constants that can be calculated based upon information collected using this
practice can be used to estimate carbon loading capacities and usages rates for the constituent present in a water stream at other
concentrations.
6. Interferences
6.1 The water shall not contain any nondissolved components.
6.2 The presence of naturally occurring organic compounds such as humic acids in the water being studied may significantly
affect the ability of the carbon to adsorb the constituent of interest. Results obtained when using water other than reagent grade
water may be unique for the particular water used and it may not be possible to apply these results to other water systems.
6.3 The adsorption isotherm data collected using this practice can be affected by the ionic strength, pH and temperature of the
water, and the presence and growth of microorganisms.
7. Apparatus
7.1 Equilibrator (or other rotating mixing device), a rotating device operating at 25 rpm which can rotate the isotherm bottles
end over end end-over-end, ensuring good dispersion of the powdered activated carbon in the water being treated.
7.2 Grinding Mill, capable of grinding material so that 90 % passes through a U.S. No. 325-mesh (45 μm) (45-μm) sieve.
7.3 Isotherm Bottles, narrow neck amber bottles with polytetrafluoroethylene (PTFE) coated (PTFE)-coated septum sealed caps
of 250, 500, and 1000 mL 250-, 500-, and 1000-mL capacity suitable for use in a centrifuge operating at 2000 rpm.
7.4 Solution Delivery Tank, a 10-L, 316 stainless steel container equipped with a PTFE coated PTFE-coated floating lid and a
316 stainless ball valve to control flow during bottle filling.
7.5 Analytical Balance, capable of weighing to the nearest 0.1 mg.
7.6 Oven, forced-air circulation, capable of temperature regulation up to 250°C.250 °C.
7.7 Centrifuge, capable of handling isotherm bottles up to 1 L 1 L in size at 2000 rpm.
7.8 Magnetic Stirring Bars and Stirrers.
8. Reagents
8.1 Reagent Water, in accordance with Specification D1193, Type II.
8.2 Methanol, high purity HPLC grade.
8.3 Potassium Monobasic Phosphate (KHPO4), 1 M solution.
8.4 Sodium Hydroxide (NaOH), 1 M solution.
9. Cleaning Procedures
9.1 This practice is capable of generating activated carbon adsorption capacity data on aqueous solutions containing ppbw
(μg/L) levels of adsorbable constituents. It is therefore very important that all equipment and glassware that come in contact with
the activated carbon or the water being treated be cleaned thoroughly to remove trace organic compounds.
9.2 All equipment and glassware should first be rigorously cleaned using procedures recommended by the EPA for priority
pollutant analysis, hot water and detergent wash, reagent grade water, and solvent (high purity methanol) rinse followed by a
bake-out.
9.3 The glassware is baked out in an oven at 250°C250 °C for a minimum of one hour. All PTFE and stainless steel apparatus
are dried at 110°C110 °C for one hour.
10. Preparation of the Activated Carbon
10.1 This practice requires the use of well washed activated carbon that has been reduced in particle size so that 90 % or greater
passes through a U.S. No. 325-mesh (45 μm) (45-μm) sieve by wet screening or equivalent.
10.2 Approximately 25 g of the powdered activated carbon sample is placed into each of four clean 250-mL bottles. The
remainder of the bottle is filled with reagent grade water.
10.3 The bottle is tightly capped and inverted three to five times to mix the contents.
D5919 − 96 (2017)
10.4 The bottles are then centrifuged at 2000 rpm for 15 min to settle the activated carbon. The supernate is poured off and the
procedure is repeated until the supernatant is clear. Allowing the mixture to sit for a period of time to allow the carbon to settle
prior to decanting is also acceptable.
10.5 The wet carbon is next dried in an oven at 110°C110 °C to a constant weight and placed in a desiccator to cool.
10.6 As an alternate technique to drying the carbon sample, carbon may be placed in a soxhlet extraction device and extracted
for a period of up to 1 week with reagent grade (Type II) water.
10.7 The dry activated carbon is transferred to clean 1-L brown borosilicate bottles with PTFE liners in the caps and stored in
an inert atmosphere such as nitrogen for future use.
11. Activated Carbon Sample Weighing Procedure
11.1 This procedure allows the carbon to be handled at ambient conditions by calculating a correction for water adsorbed from
the air.
11.2 The powdered activated carbon sample is allowed to come to equilibrium in a desiccator containing a saturated salt solution
that will produce a relative humidity comparable to ambient laboratory conditions. During the 24 h 24-h conditioning period, care
shall be taken not to expose the carbon to organic vapors.
11.3 The moisture picked up by the conditioned activated carbon is determined by weighing approximately 500 mg into a tared
(constant weight) bottle, drying for 2 h at 110°C,110 °C, cooling in a desiccator, and re-weighing to determine weight change (refer
to Test MethodMethods D2867 for standard procedures). The ratio of change in weight between the activated carbon at equilibrium
with air and after drying is calculated and used as a correction factor for the weighed carbon dosages.
11.4 The carbon dosages are weighed by first taking a weighing boat, adding the desired mass of equilibrated activated carbon,
and re-weighing the boat after transferring the carbon to the bottle. The carbon dosage is the difference between the carbon plus
the boat weight and the final boat weight. The weighed activated carbon dosage is then corrected for ambient conditions and the
actual dried carbon dosage recorded.
12. Alternative Procedure for Addition of Known Quantities of Activated Carbon to Isotherm Bottles
12.1 This alternate procedure makes use of a clean, dry activated carbon sample prepared according to procedures described
in Section 10. Desired concentrations of carbon are added to each isotherm bottle volumetrically using a carbon slurry of known
concentration.
12.2 The concentrations of the slurries are chosen so that 5, 10, and 20 mL 5-, 10-, and 20-mL volumes of each slurry would
contain appropriate amounts of carbo
...

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