ASTM E410-17a

Standard Test Method for Moisture and Residue in Liquid Chlorine

SIGNIFICANCE AND USE
4.1 This test method provides for the determination of moisture and residue in liquid chlorine. The concentration levels of these impurities are important factors in many commercial uses of liquid chlorine.
SCOPE
1.1 This test method covers the determination of moisture and residue in liquid chlorine. Lower limits of detection of 10 μg/g based on a 150-mL sample are achievable.  
1.2 This test method describes operations and special apparatus for sampling liquid chlorine from cylinders. Sampling other commercial facilities such as tank cars, barges, and storage tanks require special techniques of manipulation in filling sample cylinders for testing. If conditions and facilities are favorable, the analysis apparatus may be connected directly to these larger storage and transportation units and on-the-spot tests may be completed.  
1.3 The analytical methods are empirical and are gravimetric. They are applicable to the determination of the residue and moisture content of commercial grades of liquid chlorine (condensed gaseous product).  
1.4 Residue is defined as being those substances which remain in the sample flask after sample volatilization under the conditions of the test. Moisture is defined as the volatile substances evolved during volatilization and purging of the sample-residue flask and absorbed on the desiccant contained in the absorption tubes under the conditions of the test. Some of the volatile chlorinated hydrocarbons may also be evolved from the sample residue flask during purge and absorbed, thus contributing to the apparent moisture analysis value.  
1.5 This test method may be used for determining the moisture content only of gaseous chlorine if suitable and appropriate modifications are made for sample measurement and calculation.  
1.6 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.7 The values stated in inch-pound units are to be regarded as the standard. No other units of measurement are included in this standard.  
1.8 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 hazards statements are given in Section 7.  
1.9 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.

General Information

• Status: Published
• Publication Date: 30-Jun-2017
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.13 - Chlorine

Relations

• Replaces: ASTM E410-17 - Standard Test Method for Moisture and Residue in Liquid Chlorine
• Effective Date: 01-Jul-2017
• Refers: ASTM D6809-02(2016) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Nov-2016
• Refers: ASTM D6809-02(2007) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Jun-2007
• Refers: ASTM D6809-02 - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 10-Jun-2002
• Referred By: ASTM E1547-09(2023) - Standard Terminology Relating to Industrial and Specialty Chemicals
• Effective Date: 01-Jul-2017
• Referred By: ASTM E1120-21 - Standard Specification for Liquid Chlorine
• Effective Date: 01-Jul-2017

Overview

ASTM E410-17a: Standard Test Method for Moisture and Residue in Liquid Chlorine defines a gravimetric procedure for determining the content of moisture and residue in commercial grades of liquid chlorine. Accurate measurement of these impurities is critical for industries where chlorine purity significantly impacts product performance, safety, and equipment longevity. This standard specifies techniques suitable for analyzing samples taken from cylinders and offers guidance for adapting procedures to larger storage and transport containers such as tank cars and storage tanks.

The ASTM E410-17a test method is internationally recognized and provides meaningful data to manage quality control, support regulatory compliance, and prevent chloride contamination in chemical manufacturing processes.

Key Topics

• Scope and Limitations

  • Covers determination of both moisture and residue in liquid chlorine with detection limits as low as 10 μg/g using a 150 mL sample.
  • Applicable to commercial liquid chlorine and, with modifications, gaseous chlorine.

• Definitions

  • Residue: Substances remaining after volatilization of the chlorine sample under specified test conditions.
  • Moisture: Volatile substances evolved and absorbed on a chemical desiccant during sample processing.

• Sampling Techniques

  • Describes apparatus and protocols for safe sampling from pressurized chlorine cylinders.
  • Notes special handling required for sampling from bulk containers (e.g., tank cars, barges, storage tanks).

• Analytical Method

  • Empirical, gravimetric analysis performed after careful volatilization and controlled aeration.
  • Utilizes anhydrous magnesium perchlorate to absorb moisture during volatilization and air purging steps.

• Safety and Compliance

  • Emphasizes strict adherence to safety protocols and regulatory guidelines due to chlorine’s toxic and reactive properties.
  • Users must consult current Safety Data Sheets (SDS) and comply with relevant transportation and handling regulations (e.g., CFR 49).

Applications

The ASTM E410-17a standard is valuable for any facility handling or distributing liquid chlorine, including:

• Chemical manufacturing: Ensures chlorine feedstocks meet quality standards, thus preventing costly contamination in downstream processes.
• Water treatment plants: Verifies chlorine purity to optimize disinfection and minimize corrosion or scaling in equipment.
• Chlorine producers and distributors: Offers standardized quality assurance for bulk shipments and storage.
• Industrial gas suppliers: Provides a benchmark method for internal quality control and customer specification compliance.

Routine use of this method helps identify sources of excess moisture or undesirable residues, leading to improved equipment maintenance and reduced risk of operational failures.

Related Standards

Several standards provide additional context or complementary procedures to ASTM E410-17a:

• ASTM D6809: Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials.
• ASTM E180: Withdrawn practice for determining the precision of ASTM methods for analysis and testing of industrial and specialty chemicals.
• 49 CFR 173: U.S. federal regulations covering transportation and packaging of compressed gases, including detailed requirements for chlorine cyclinders and bulk containers.

These references collectively support sound laboratory practices, regulatory compliance, and continuous improvement in quality assurance and analytical precision.

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Keywords: ASTM E410-17a, moisture in liquid chlorine, residue in chlorine, chlorine purity testing, chlorine analysis, gravimetric method, ASTM chlorine test standard, chemical analysis, quality control, commercial chlorine, industrial gas standards, chlorine sampling safety, moisture determination chlorine.

Standards Content (Sample)

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: E410 − 17a
Standard Test Method for
Moisture and Residue in Liquid Chlorine
This standard is issued under the fixed designation E410; 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* 1.8 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the determination of moisture
responsibility of the user of this standard to establish appro-
and residue in liquid chlorine. Lower limits of detection of 10
priate safety, health, and environmental practices and deter-
µg/g based on a 150-mL sample are achievable.
mine the applicability of regulatory limitations prior to use.
1.2 This test method describes operations and special appa-
Specific hazards statements are given in Section 7.
ratus for sampling liquid chlorine from cylinders. Sampling
1.9 This international standard was developed in accor-
other commercial facilities such as tank cars, barges, and
dance with internationally recognized principles on standard-
storage tanks require special techniques of manipulation in
ization established in the Decision on Principles for the
filling sample cylinders for testing. If conditions and facilities
Development of International Standards, Guides and Recom-
arefavorable,theanalysisapparatusmaybeconnecteddirectly
mendations issued by the World Trade Organization Technical
to these larger storage and transportation units and on-the-spot
Barriers to Trade (TBT) Committee.
tests may be completed.
2. Referenced Documents
1.3 The analytical methods are empirical and are gravimet-
ric.They are applicable to the determination of the residue and
2.1 ASTM Standards:
moisture content of commercial grades of liquid chlorine
D6809Guide for Quality Control and Quality Assurance
(condensed gaseous product).
Procedures for Aromatic Hydrocarbons and Related Ma-
terials
1.4 Residue is defined as being those substances which
E180Practice for Determining the Precision of ASTM
remaininthesampleflaskaftersamplevolatilizationunderthe
Methods for Analysis and Testing of Industrial and Spe-
conditions of the test. Moisture is defined as the volatile
cialty Chemicals (Withdrawn 2009)
substances evolved during volatilization and purging of the
2.2 Federal Standards:
sample-residue flask and absorbed on the desiccant contained
CFR 173 Title 49Transportation; Shippers’ General Re-
in the absorption tubes under the conditions of the test. Some
quirements for Shipments and Packagings, including Sec-
of the volatile chlorinated hydrocarbons may also be evolved
tions:
from the sample residue flask during purge and absorbed, thus
173.304Charging of Cylinders with Liquefied Compressed
contributing to the apparent moisture analysis value.
Gas
1.5 This test method may be used for determining the
173.314Requirements for Compressed Gases in Tank Cars
moisture content only of gaseous chlorine if suitable and
173.315Compressed Gases in Cargo Tanks and Portable
appropriate modifications are made for sample measurement
Tank Containers
and calculation.
3. Summary of Test Method
1.6 ReviewthecurrentSafetyDataSheet(SDS)fordetailed
informationconcerningtoxicity,firstaidprocedures,andsafety
3.1 Acommonliquidsampleofchlorineisrecommendedto
precautions.
provide the best results when determining both residue and
1.7 The values stated in inch-pound units are to be regarded moisture simultaneously.
as the standard. No other units of measurement are included in
this standard.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
This test method is under the jurisdiction of ASTM Committee D16 on the ASTM website.
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- The last approved version of this historical standard is referenced on
bility of Subcommittee D16.13 on Chlorine. www.astm.org.
CurrenteditionapprovedJuly1,2017.PublishedJuly2017.Originallyapproved Available from U.S. Government Printing Office, Superintendent of
in 1970. Last previous edition approved in 2017 as E410–17. DOI: 10.1520/ Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
E0410-17a. www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E410 − 17a
FIG. 1 Apparatus for Collection and Volatilization of Liquid Chlorine
3.2 Liquid product sample is transferred from the same 5.2 Sample-Residue Flask (H), Erlenmeyer-type, 250-mL
S
cylinder into a precalibrated, 250-mLsample-residue flask and capacity, equipped with a 35/20 J ground-ball joint. A
permitted to volatilize completely under prevailing environ- permanent calibration mark shall be inscribed on the flask at
mental conditions. The volatilized product (chlorine gas) is the 150-mL volume level for sample measurement.
S
passed through anhydrous magnesium perchlorate desiccant
5.3 Adapter (G), equipped with a 35/20 J ground-socket
for absorption of moisture. It is recommended that the exhaust
joint attached and sealed as shown in Fig. 1. In addition,
S
gas be discharged into a caustic scrubber containing an
appropriate 12/5 J joints shall be sealed to the adapter. A ball
appropriate amount of 20% caustic solution to neutralize all
joint, sealed and closed off at the end, shall be provided for
the chlorine. This reaction is exothermic and care should be
attachment to the inlet tube after collection of liquid sample in
taken to avoid excess heating by choosing a sufficiently large
the sample-residue flask.This shall be held in position with an
volume of caustic solution to serve as a heat sink.
appropriate clamp during volatilization, then removed and
replacedwithappropriateconnectionsfromthemetereddry-air
3.3 After complete volatilization of the sample from the
supply at the time of aeration and purge of the sample-residue
flask, residual chlorine and moisture are expelled from any
flask.
residue by purging with dry air through the absorption system
where moisture is recovered and determined gravimetrically.
5.4 Asecond assembly consisting of a sample-residue flask
andadaptershallbeusedtofacilitatecollectionanddisposalof
3.4 Residue remaining in the flask is determined by careful
samplepurgefromthecylindersamplelinepriortowithdrawal
analytical weighing, the weight gain calculated as residue
of the analytical sample for test.
content of the sample. Moisture is computed from the sum of
the gain in weight of the two absorption tubes containing the 5.5 Regulator—An appropriate needle valve type shall be
desiccant. Any gain in weight of the second absorber tube
attached to the cylinder outlet to control and regulate the flow
should be nominal with respect to that of the first tube in the of liquid chlorine from the sample cylinder. Connection (F)
series.
between the outlet from this valve and the adapter (G) shall be
by a short length of appropriately sized TFE-fluorocarbon
3.5 The moisture content of a chlorine gas stream is
S
tubing equipped with a 12/5 J ground-ball joint.
determined gravimetrically as above, by passing a metered
5.6 Rubber Tubing, length and size sufficient to exhaust
sample through the moisture absorption system only.
chlorine vapors to the caustic soda absorber or hood system
during sample collection and volatilization. A ground-glass
4. Significance and Use
S
12/5 J socket joint shall be fitted to one end of the rubber
4.1 This test method provides for the determination of
tubing to make appropriate connection to the adapter during
moisture and residue in liquid chlorine. The concentration
sample collection and transferred to the exhaust connection
levels of these impurities are important factors in many
from the second moisture absorption U-tube for gas discharge
commercial uses of liquid chlorine.
to disposal during volatilization of the sample.
5. Apparatus
S
The recommended sample-residue flask, equipped with a 35/20 J ground-ball
5.1 The arrangement and assembly of apparatus for collec-
S
joint and the adapter equipped with a 35/20 J ground-socket joint and associated
S
tion and measurement of the analytical sample and volatiliza-
12/5 JgroundjointsshowninFig.1,canbepurchasedfromareputableglassvendor
tion is shown in Fig. 1. or can be fabricated by a glass blower.
E410 − 17a
5.7 Watch Glass, small size, used to close the sample- 7.5 In the event chlorine is inhaled, first aid should be
residue flask during analytical weighing before and after summoned immediately and oxygen administered without
samplevolatilizationtopreventlossofresidueorabsorptionof delay.
moisture from the atmosphere.
8. Sampling Tank Cars, Barges, Large Cylinders, and
5.8 Moisture Absorption Tubes (I) (Fig. 1)—Schwartz
Storage Facilities
U-tube design, 100 mm length top of arms to center, modified
S
and equipped with ground-glass 12/5 J socket and ball joints
8.1 Sampling from tank cars, barges, storage tanks, and
sealed to the inlets and outlets. Two such absorber tubes shall
large cylinders present unique problems. Each facility,
be connected in a series arrangement.
however,mustbecapableofdeliveringliquid-sample(notgas)
for test.
5.9 Flow Meter, capable of metering air at 4.5 L/min and
equipped with appropriate ground glass connection.
8.2 Sincelocationoftheselargerfacilitiesmaynotbeatthe
immediate site of analysis, sample collection in a suitable
5.10 Caustic Scrubber, for chlorine disposal.
secondary container is recommended to facilitate its safe
6. Reagents
transport to the laboratory for tests.
6.1 Purity of Reagents—Unless otherwise indicated, it is
8.3 It is recommended that samples be collected from these
intended that all reagents should conform to the specifications
facilities in small-size sample cylinders with cylinders and
of the Committee on Analytical Reagents of the American
valves fabricated of tantalum or nickel and capable of being
Chemical Society, where such specifications are available.
negotiated in the laboratory fume hood. Technical literature
available from producers and distributors of liquid chlorine
6.2 Pulverized Dry Ice and a Small Amount of
should be consulted for instructions in filling small size
Trichloroethylene, contained in a glass crystallizing dish (190
cylinders properly from bulk storage.
by100mm),foruseincoolingthesample-residueflaskduring
sample purge, collection and measurement.
8.4 Do not allow the sample cylinder to become liquid full.
A good rule is that the weight of the chlorine in the cylinder
6.3 Granular Form of Anhydrous Magnesium Perchlorate—
should not be more that 125% of the weight of the water that
Reagent Grade.
the cylinder could contain in accordance with 49 CFR 173.
6.4 Caustic Solution—20% by mass, sodium hydroxide in
water. Dissolve 200 g of sodium hydroxide (NaOH) in water
9. Preparation of Apparatus
and dilute to 1 L. Store in a tight polyethylene container.
9.1 Thoroughly clean the absorption tubes, sample-residue
7. Hazards
flasks,andadaptersfreeofgreaseandlubricants,particularlyat
thegroundsurfacesofthejoints.Afterthoroughcleansing,dry
7.1 Chlorine is a corrosive and toxic material. A well
the apparatus thermally in an oven at 105°C. When cooled,
ventilated fume hood should be used to house the test equip-
charge the absorption tubes with desiccant.
ment when this product is analyzed in the laboratory.
9.2 Chargeeachtubewithinabout20mmofthetopineach
7.2 The analysis should be attempted only by persons who
leg with a granular form of anhydrous magnesium perchlorate,
arethoroughlyfamiliarwiththehandlingofchlorine,andeven
minimizing the use of dusty product. Place loosely packed
an experienced person should not work alone. The operator
must be provided with adequate eye protection and respirator. glass wool on the surfaces of the desiccant in both legs of the
absorber tube to avoid carry-over of chemical dust during
Splashes of liquid chlorine destroy clothing and if such
clothing is next to the skin, will produce irritations and burns. sample volatilization and air purge operations. Place the
unlubricated stoppers firmly in the ground necks of the tubes
7.3 Whensamplingandworkingwithchlorineoutofdoors,
and adjust to the “off” position preparatory to conditioning
peopledownwindfromsuchoperationshouldbewarnedofthe
with chlorine gas, air purge, and weighing.
possible release of chlorine vapors.
9.3 Connect the moisture absorption tubes in a series by
7.4 It is recommended that means should be available for
means of appropriately sized spring clamps in an upright
disposal of excess chlorine in an environmentally safe and
operatingpositionsupportedonaringstand.Attachtheground
acceptable manner. If chlorine cannot be disposed of in a
joint and rubber tubing to the outlet of the second absorber for
chlorine consuming process, a chlorine absorption system
exhausting chlorine gas to the caustic scrubber.
should be provided. When the analysis and sampling regimen
requires an initial purging of chlorine from a container, the 9.4 Attach a source of chlorine gas to the inlet of the first
purged chlorine should be similarly handled. Purging to the
absorber tube, open the ground stoppers on both tubes to
atmosphere should be avoided. permit the free flo
...

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: E410 − 17 E410 − 17a
Standard Test Method for
Moisture and Residue in Liquid Chlorine
This standard is issued under the fixed designation E410; 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 test method covers the determination of moisture and residue in liquid chlorine. Lower limits of detection of 10 μg/g
based on a 150-mL sample are achievable.
1.2 This test method describes operations and special apparatus for sampling liquid chlorine from cylinders. Sampling other
commercial facilities such as tank cars, barges, and storage tanks require special techniques of manipulation in filling sample
cylinders for testing. If conditions and facilities are favorable, the analysis apparatus may be connected directly to these larger
storage and transportation units and on-the-spot tests may be completed.
1.3 The analytical methods are empirical and are gravimetric. They are applicable to the determination of the residue and
moisture content of commercial grades of liquid chlorine (condensed gaseous product).
1.4 Residue is defined as being those substances which remain in the sample flask after sample volatilization under the
conditions of the test. Moisture is defined as the volatile substances evolved during volatilization and purging of the sample-residue
flask and absorbed on the desiccant contained in the absorption tubes under the conditions of the test. Some of the volatile
chlorinated hydrocarbons may also be evolved from the sample residue flask during purge and absorbed, thus contributing to the
apparent moisture analysis value.
1.5 This test method may be used for determining the moisture content only of gaseous chlorine if suitable and appropriate
modifications are made for sample measurement and calculation.
1.6 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first aid procedures, and safety
precautions.
1.7 The values stated in inch-pound units are to be regarded as the standard. No other units of measurement are included in this
standard.
1.8 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 hazards statements are given in Section 7.
1.9 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.
2. Referenced Documents
2.1 ASTM Standards:
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
(Withdrawn 2009)
2.2 Federal Standards:
CFR 173 Title 49 Transportation; Shippers’ General Requirements for Shipments and Packagings, including Sections:
173.304 Charging of Cylinders with Liquefied Compressed Gas
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the direct
responsibility of Subcommittee D16.16 on Industrial and Specialty Product Standards.
Current edition approved March 1, 2017July 1, 2017. Published March 2017July 2017. Originally approved in 1970. Last previous edition approved in 20082017 as
E410 – 08.E410 – 17. DOI: 10.1520/E0410-17.10.1520/E0410-17a.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available from U.S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E410 − 17a
FIG. 1 Apparatus for Collection and Volatilization of Liquid Chlorine
173.314 Requirements for Compressed Gases in Tank Cars
73.315 Compressed Gases in Cargo Tanks and Portable Tank Containers
3. Summary of Test Method
3.1 A common liquid sample of chlorine is recommended to provide the best results when determining both residue and
moisture simultaneously.
3.2 Liquid product sample is transferred from the same cylinder into a precalibrated, 250-mL sample-residue flask and permitted
to volatilize completely under prevailing environmental conditions. The volatilized product (chlorine gas) is passed through
anhydrous magnesium perchlorate desiccant for absorption of moisture. It is recommended that the exhaust gas be discharged into
a caustic scrubber containing an appropriate amount of 20 % caustic solution to neutralize all the chlorine. This reaction is
exothermic and care should be taken to avoid excess heating by choosing a sufficiently large volume of caustic solution to serve
as a heat sink.
3.3 After complete volatilization of the sample from the flask, residual chlorine and moisture are expelled from any residue by
purging with dry air through the absorption system where moisture is recovered and determined gravimetrically.
3.4 Residue remaining in the flask is determined by careful analytical weighing, the weight gain calculated as residue content
of the sample. Moisture is computed from the sum of the gain in weight of the two absorption tubes containing the desiccant. Any
gain in weight of the second absorber tube should be nominal with respect to that of the first tube in the series.
3.5 The moisture content of a chlorine gas stream is determined gravimetrically as above, by passing a metered sample through
the moisture absorption system only.
4. Significance and Use
4.1 This test method provides for the determination of moisture and residue in liquid chlorine. The concentration levels of these
impurities are important factors in many commercial uses of liquid chlorine.
5. Apparatus
5.1 The arrangement and assembly of apparatus for collection and measurement of the analytical sample and volatilization is
shown in Fig. 1.
S
5.2 Sample-Residue Flask (H), Erlenmeyer-type, 250-mL capacity, equipped with a 35/20 J ground-ball joint. A permanent
calibration mark shall be inscribed on the flask at the 150-mL volume level for sample measurement.
S
5.3 Adapter (G), equipped with a 35/20 J ground-socket joint attached and sealed as shown in Fig. 1. In addition, appropriate
S
12/5 J joints shall be sealed to the adapter. A ball joint, sealed and closed off at the end, shall be provided for attachment to the
inlet tube after collection of liquid sample in the sample-residue flask. This shall be held in position with an appropriate clamp
during volatilization, then removed and replaced with appropriate connections from the metered dry-air supply at the time of
aeration and purge of the sample-residue flask.
S S S
The recommended sample-residue flask, equipped with a 35/20 J ground-ball joint and the adapter equipped with a 35/20 J ground-socket joint and associated 12/5 J
ground joints shown in Fig. 1, can be purchased from a reputable glass vendor or can be fabricated by a glass blower.
E410 − 17a
5.4 A second assembly consisting of a sample-residue flask and adapter shall be used to facilitate collection and disposal of
sample purge from the cylinder sample line prior to withdrawal of the analytical sample for test.
5.5 Regulator—An appropriate needle valve type shall be attached to the cylinder outlet to control and regulate the flow of liquid
chlorine from the sample cylinder. Connection (F ) between the outlet from this valve and the adapter (G) shall be by a short length
S
of appropriately sized TFE-fluorocarbon tubing equipped with a 12/5 J ground-ball joint.
5.6 Rubber Tubing, length and size sufficient to exhaust chlorine vapors to the caustic soda absorber or hood system during
S
sample collection and volatilization. A ground-glass 12/5 J socket joint shall be fitted to one end of the rubber tubing to make
appropriate connection to the adapter during sample collection and transferred to the exhaust connection from the second moisture
absorption U-tube for gas discharge to disposal during volatilization of the sample.
5.7 Watch Glass, small size, used to close the sample-residue flask during analytical weighing before and after sample
volatilization to prevent loss of residue or absorption of moisture from the atmosphere.
5.8 Moisture Absorption Tubes (I) (Fig. 1)—Schwartz U-tube design, 100 mm length top of arms to center, modified and
S
equipped with ground-glass 12/5 J socket and ball joints sealed to the inlets and outlets. Two such absorber tubes shall be
connected in a series arrangement.
5.9 Flow Meter, capable of metering air at 4.5 L/min and equipped with appropriate ground glass connection.
5.10 Caustic Scrubber, for chlorine disposal.
6. Reagents
6.1 Purity of Reagents—Unless otherwise indicated, it is intended that all reagents should conform to the specifications of the
Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.
6.2 Pulverized Dry Ice and a Small Amount of Trichloroethylene, contained in a glass crystallizing dish (190 by 100 mm), for
use in cooling the sample-residue flask during sample purge, collection and measurement.
6.3 Granular Form of Anhydrous Magnesium Perchlorate—Reagent Grade.
6.4 Caustic Solution—20 % by mass, sodium hydroxide in water. Dissolve 200 g of sodium hydroxide (NaOH) in water and
dilute to 1 L. Store in a tight polyethylene container.
7. Hazards
7.1 Chlorine is a corrosive and toxic material. A well ventilated fume hood should be used to house the test equipment when
this product is analyzed in the laboratory.
7.2 The analysis should be attempted only by persons who are thoroughly familiar with the handling of chlorine, and even an
experienced person should not work alone. The operator must be provided with adequate eye protection and respirator. Splashes
of liquid chlorine destroy clothing and if such clothing is next to the skin, will produce irritations and burns.
7.3 When sampling and working with chlorine out of doors, people downwind from such operation should be warned of the
possible release of chlorine vapors.
7.4 It is recommended that means should be available for disposal of excess chlorine in an environmentally safe and acceptable
manner. If chlorine cannot be disposed of in a chlorine consuming process, a chlorine absorption system should be provided. When
the analysis and sampling regimen requires an initial purging of chlorine from a container, the purged chlorine should be similarly
handled. Purging to the atmosphere should be avoided.
7.5 In the event chlorine is inhaled, first aid should be summoned immediately and oxygen administered without delay.
8. Sampling Tank Cars, Barges, Large Cylinders, and Storage Facilities
8.1 Sampling from tank cars, barges, storage tanks, and large cylinders present unique problems. Each facility, however, must
be capable of delivering liquid-sample (not gas) for test.
8.2 Since location of these larger facilities may not be at the immediate site of analysis, sample collection in a suitable secondary
container is recommended to facilitate its safe transport to the laboratory for tests.
8.3 It is recommended that samples be collected from these facilities in small-size sample cylinders with cylinders and valves
fabricated of tantalum or nickel and capable of being negotiated in the laboratory fume hood. Technical literature available from
producers and distributors of liquid chlorine should be consulted for instructions in filling small size cylinders properly from bulk
storage.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
E410 − 17a
8.4 Do not allow the sample cylinder to become liquid full. A good rule is that the weight of the chlorine in the cylinder should
not be more that 125 % of the weight of the water that the cylinder could contain in accordance with 49 CFR 173.
9. Preparation of Apparatus
9.1 Thoroughly clean the absorption tubes, sample-residue flasks, and adapters free of grease and lubricants, particularly at the
ground surfaces of the joints. After thorough cleansing, dry the apparatus thermally in an oven at 105°C. When cooled, charge the
absorption tubes with desiccant.
9.2 Charge each tube within about 20 mm of the top in each leg with a granular form of anhydrous magnesium perchlorate,
minimizing the use of dusty product. Place loosely packed glass wool on the surfaces of the desiccant in both legs of the absorber
tube to avoid carry-over of chemical dust during sample volatilization and air purge operations. Place the unlubricated stoppers
firmly in the ground necks of the tubes and adjust to the “off” p
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