ASTM E506-17a

Standard Test Method for Mercury in Liquid Chlorine

SIGNIFICANCE AND USE
4.1 This test method was developed primarily for the determination of traces of mercury in chlorine produced by the mercury-cell process.
SCOPE
1.1 This test method2 covers the determination of mercury in liquid chlorine with a lower limit of detection of 0.1 μg/L.  
1.2 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first-aid procedures, and safety precautions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 Sections 7, 6.3, 6.4, 6.5, and Note 2.  
1.5 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: 71.040.40 - Chemical analysis
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.13 - Chlorine

Relations

• Replaces: ASTM E506-17 - Standard Test Method for Mercury 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 D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D6809-02 - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 10-Jun-2002
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM E506-17a – Standard Test Method for Mercury in Liquid Chlorine establishes a consistent procedure for the measurement of trace amounts of mercury in liquid chlorine. Primarily intended for use with chlorine produced via the mercury-cell process, this standard is widely recognized for ensuring accurate and reliable mercury determination. With a lower detection limit of 0.1 μg/L, ASTM E506-17a provides essential guidance for operators in the chemical industry, where trace contaminants can significantly affect both product quality and regulatory compliance.

Key Topics

• Scope and Applicability

  • Covers determination of mercury in liquid chlorine with detection as low as 0.1 μg/L.
  • Values and measurements are set in SI units only.
  • Primary focus is on chlorine produced by the mercury-cell process.

• Safety and Best Practices

  • Emphasizes the need to review the current Safety Data Sheet (SDS) for toxicity and emergency procedures.
  • Includes detailed precautionary statements regarding hazardous chemicals such as sulfuric acid, nitric acid, aqua regia, and chlorine itself.
  • Advises on safe sampling and disposal methods to minimize risk to workers and the environment.
  • Recommends use of personal protective equipment (PPE), including goggles and respirators.

• Test Procedure Highlights

  • Chlorine samples are collected in chilled glass flasks and allowed to evaporate, concentrating mercury in the residue.
  • Residual mercury is dissolved in dilute nitric acid, then analyzed by atomic absorption spectrophotometry after appropriate chemical preparation.
  • Strict cleaning regimens are enforced to avoid contamination, ensuring accuracy of results.

• Precision and Quality Assurance

  • Provides guidelines for repeatability, within-laboratory precision, and reproducibility across multiple labs.
  • Recommends the inclusion of quality control samples and compliance with statistical quality control practices.

Applications

• Chlor-Alkali Plant Operations

  • Monitoring traces of mercury in chlorine before it enters industrial processes ensures product purity and supports compliance with environmental standards.
  • Critical for facilities utilizing the mercury-cell process for chlorine production, offering a robust protocol for routine mercury analysis.

• Regulatory Compliance

  • Adhering to this test method helps companies meet global regulatory requirements concerning mercury contamination.
  • Essential in industries where mercury presence is strictly regulated or where export requirements specify granular testing documentation.

• Environmental and Worker Safety

  • Ensures that mercury emissions and residues are maintained at trace levels, reducing the risk of environmental contamination and exposure to personnel.

• Quality Control in Chemical Manufacturing

  • Facilitates regular monitoring and documentation of mercury levels ensuring high-quality end products.
  • Supports internal audits and certification processes through standardized methodology.

Related Standards

• ASTM D1193 – Specification for Reagent Water: Ensures water purity used in testing.
• ASTM D6809 – Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials.
• ASTM E180 (withdrawn) – Formerly referenced for precision and bias in analytical methods.
• ASTM E200 – Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis.

Keywords

• Mercury determination
• Liquid chlorine analysis
• Mercury-cell process
• Atomic absorption spectrophotometry
• Chlorine plant quality control
• Trace mercury testing
• ASTM E506-17a compliance

---

ASTM E506-17a is an essential standard for accurate, safe, and environmentally responsible measurement of mercury in liquid chlorine, enabling manufacturers to maintain stringent control over product quality and meet industry regulations.

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: E506 − 17a
Standard Test Method for
Mercury in Liquid Chlorine
This standard is issued under the fixed designation E506; 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* D6809Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 This test method covers the determination of mercury
terials
in liquid chlorine with a lower limit of detection of 0.1 µg/L.
E180Practice for Determining the Precision of ASTM
1.2 ReviewthecurrentSafetyDataSheet(SDS)fordetailed
Methods for Analysis and Testing of Industrial and Spe-
information concerning toxicity, first-aid procedures, and
cialty Chemicals (Withdrawn 2009)
safety precautions.
E200Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for ChemicalAnalysis
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Summary of Test Method
standard.
3.1 Liquidchlorinesamplesaretakeninchilledglassflasks,
1.4 This standard does not purport to address all of the
then allowed to evaporate slowly to dryness. The mercury is
safety concerns, if any, associated with its use. It is the
left in the residue.The residue is dissolved in dilute nitric acid
responsibility of the user of this standard to establish appro-
and diluted to volume.The addition of nitric acid prevents any
priate safety, health, and environmental practices and deter-
loss of mercury from the aqueous solution on standing. For
mine the applicability of regulatory limitations prior to use.
analysis, an aliquot of the acidic aqueous solution is boiled
Specific precautionary statements are given in Sections 7, 6.3,
withexcesspermanganatetoremoveinterferingmaterials.The
6.4, 6.5, and Note 2.
mercuric ions are then reduced to metallic mercury with
1.5 This international standard was developed in accor-
stannous chloride. The solution is aerated and the mercury,
dance with internationally recognized principles on standard-
nowintheairstream,isdeterminedusinganatomicabsorption
ization established in the Decision on Principles for the
spectrophotometer.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4. Significance and Use
Barriers to Trade (TBT) Committee.
4.1 This test method was developed primarily for the
2. Referenced Documents
determinationoftracesofmercuryinchlorineproducedbythe
mercury-cell process.
2.1 ASTM Standards:
D1193Specification for Reagent Water
5. Apparatus
5.1 Atomic Absorption Spectrophotometer, equipped with
This test method is under the jurisdiction of ASTM Committee D16 on mounting to hold absorption cell and a fast response (0.5 s)
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
recorder.
bility of Subcommittee D16.13 on Chlorine.
CurrenteditionapprovedJuly1,2017.PublishedJuly2017.Originallyapproved
5.2 Mercury Hollow Cathode Lamp,primaryline253.7nm.
in 1973. Last previous edition approved in 2017 as E506–17. DOI: 10.1520/
5.3 Absorption Cell, 10-cm path length with quartz win-
E0506-17a.
Analytical Methods for Atomic Absorption Spectrophotometry, Perkin-Elmer
dows.
Ltd., September 1968.
5.4 Gas Washing Bottle, 125 mL, with extra-coarse fritted
“Determination of Mercury in Effluents and Process Streams from a Mercury-
Cell Chlorine Plant (AtomicAbsorption Flameless Method)” CAS-AM-70.13, June
bubbler. The bottle has a calibration line drawn at the 60-mL
23, 1970, Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario,
mark.
Canada.
“Determination of Mercury in Liquid Chlorine,” CSAL-M72.4, Feb. 25, 1972,
5.5 Stopcock, 3-way, with plug of TFE-fluorocarbon.
Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario, Canada.
5.6 Gas Washing Bottle, 125-mL without frit.
Chlorine Institute Reference No. MIR-104.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*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
E506 − 17a
5.7 Drying Tube. 6.7 Hydroxylamine Hydrochloride Solution (100 g/L)—See
Practice E200. This reagent is dispensed with a dropping
5.8 Flow Meter, capable of measuring and maintaining a
bottle.
flow of 42.5 L/h.
6.8 Mercury Standard Solution (50 µg Hg/mL)—As pre-
5.9 Large Dewar Flasks, two, with sufficient capacity to
pared in Practice E200.
hold a 500-mL flask and a large volume of dry ice cooling
mixture.
6.9 Mercury Standard Solution (10 µg Hg/mL)—Pipet 10
mL of the standard mercury solution containing 50 µg Hg/mL
5.10 Flexible Tygon or equivalent Connection.
into a 50-mL volumetric flask, acidify with 5 mL of 1+4
5.11 Stainless Steel Compression Nut.
H SO and dilute to volume with water. Mix well. Prepare
2 4
fresh daily.
5.12 Two-Hole Rubber Stopper.
6.10 Mercury Standard Solution (1 µg Hg/mL)—Pipet 10
5.13 Fluorocarbon Tubing.
mL of the standard mercury solution containing 10 µg Hg/mL
NOTE 1—The procedure, as described in this test method, was devel-
intoa100-mLvolumetricflask,acidifywith5mL1+4H SO
2 4
oped using a Perkin-Elmer Model 303 atomic absorption spectrophotom-
and dilute to volume with water. Mix well. Prepare fresh daily.
eter equipped with a 10-cm absorption cell. Any other equivalent atomic
absorption spectrophotometer may be used as well as one of the many
6.11 Potassium Permanganate Solution (40 g/L) (4%)—
commercial instruments specifically designed for measurement of mer-
Weigh 40 g of KMnO into a 1000-mLbeaker.Add about 800
cury by flameless atomic absorption. However, variation in instrument
mLof water and stir with a mechanical stirrer until completely
geometry,celllength,sensitivity,andmodeofresponsemeasurementmay
dissolved. Allow the solution to stand overnight and filter.
require appropriate modifications of the operating parameters.
Transfer to a 1000-mL volumetric flask, dilute to volume, and
6. Reagents store in a brown bottle.
6.1 Purity of Reagents—Unless otherwise indicated, it is 6.12 Stannous Chloride (10%)—Dissolve 20 g of stannous
intended that all reagents should conform to the specifications
chloride(SnCl ·2H O)in40mLofwarmconcentratedHCl(sp
2 2
of the Committee on Analytical Reagents of the American gr 1.19).Add 160 mL of water when all the stannous chloride
Chemical Society, where such specifications are available.
has dissolved.Allow the solution to stand overnight and filter.
Blanks should be run on all reagents to assure a negligible Mix and store in a 250-mL reagent bottle. Prepare fresh once
mercury content.
a week.Apiece of metallic tin in the bottle allows longer term
storage if the bottle is well sealed.
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type II or Type III
7. Safety Precautions
reagent water conforming to Specification D1193.
7.1 Sulfuric acid will cause severe burns if allowed to come
6.3 Aqua Regia—Carefully add 10 mL of concentrated
in contact with any part of the skin or eyes.All spillages must
HNO (sp gr 1.42) to 30 mL of concentrated HCl (sp gr 1.19)
be immediately flushed from the skin or eyes with cold water.
ina100-mLbeaker.Letthemixturestandfor5minbeforeuse.
This acid must always be added slowly to water with adequate
Thismixtureisunstableandshouldnotbestored.(Warning—
stirringsinceheatisdevelopedandspatteringoccursiftheacid
Use goggles when preparing or using this solution.)
is added too quickly.
6.4 Nitric Acid(1+9)—Pipet 25 mLof concentrated HNO
7.2 Aqua regia contains both HNO and HCl, which will
(sp gr 1.42) into a 250-mL volumetric flask containing about
cause severe burns if allowed to come in contact with any part
150 mL of water. Dilute to volume with water and mix well.
of the skin or eyes.All spillages must be immediately flushed
(Warning—Use goggles when preparing this solution.)
fromtheskinoreyeswithcoldwater.Vaporsproducedbyaqua
6.5 Sulfuric Acid(1+4)—Add slowly with stirring 200 mL
regia can cause burns if inhaled. It should be used only in a
of concentrated H SO (sp gr 1.84) to 800 mL of water.
2 4
fumehoodorwithsimilarventilation.Thissolutionisunstable
(Warning—Use goggles when preparing this solution.)
and must not be placed in a stoppered flask or bottle.
6.6 Cooling Mixture for Dewar Flasks—Fill two thirds of
7.3 Nitricacidwillcausesevereburnsifallowedtocomein
the Dewar flask with dichloromethane. Add dry ice slowly,
contact with any part of the skin or eyes.All spillages must be
allowing time for the solution to cool, until there is no
immediately flushed from the skin or eyes with cold water.
sublimation of dry ice on further addition. Replenish the dry
7.4 Chlorine is a corrosive and toxic material. A well-
ice when necessary. See the SDS sheet for dichloromethane
ventilated fume hood should be used to house all test equip-
before using this material.
ment when this product is analyzed in the laboratory.
7.5 Liquid chlorine sampling should be performed only by
those persons thoroughly familiar with the handling of this
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
material and the operation of the sampling system. Personnel
listed by the American Chemical Society, see Analar Standards for Laboratory
shouldbeequippedwithmonogoggles,gloves(ifdesired),and
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
a respirator. Sampling should be done in a well-ventilated area
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. or in a fume hood.
E506 − 17a
7.6 The analysis should be attempted only by persons who 8.5 Keeping the receiver flask in the dry ice solution, purge
arethoroughlyfamiliarwiththehandlingofchlorine,andeven thesamplingsystemallowing100to200mLofliquidchlorine
an experienced person should not work alone. The operator toflowthroughthesamplingsystemintotheflask.Thispurges
mustbeprovidedwithadequateeyeprotectionandarespirator. any residual mercury deposits from the lines and sample point.
Splashes of liquid chlorine destroy clothing and, if such
8.6 Stop the flow of liquid chlorine.
clothing is next to the skin, will produce irritations and burns.
8.7 Cap the waste liquid chlorine flask with an open,
7.7 Whensamplingandworkingwithchlorineoutofdoors,
...

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: E506 − 17 E506 − 17a
Standard Test Method for
Mercury in Liquid Chlorine
This standard is issued under the fixed designation E506; 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 mercury in liquid chlorine with a lower limit of detection of 0.1 μg/L.
1.2 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first-aid procedures, and safety
precautions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 Sections 7, 6.3, 6.4, 6.5, and Note 2.
1.4 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first-aid procedures, and safety
precautions.
1.5 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:
D1193 Specification for Reagent Water
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)
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
3. Summary of Test Method
3.1 Liquid chlorine samples are taken in chilled glass flasks, then allowed to evaporate slowly to dryness. The mercury is left
in the residue. The residue is dissolved in dilute nitric acid and diluted to volume. The addition of nitric acid prevents any loss
of mercury from the aqueous solution on standing. For analysis, an aliquot of the acidic aqueous solution is boiled with excess
permanganate to remove interfering materials. The mercuric ions are then reduced to metallic mercury with stannous chloride. The
solution is aerated and the mercury, now in the air stream, is determined using an atomic absorption spectrophotometer.
4. Significance and Use
4.1 This test method was developed primarily for the determination of traces of mercury in chlorine produced by the
mercury-cell process.
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 1973. Last previous edition approved in 20082017 as
E506 – 08.E506 – 17. DOI: 10.1520/E0506-17.10.1520/E0506-17a.
Analytical Methods for Atomic Absorption Spectrophotometry, Perkin-Elmer Ltd., September 1968.
“Determination of Mercury in Effluents and Process Streams from a Mercury-Cell Chlorine Plant (Atomic Absorption Flameless Method)” CAS-AM-70.13, June 23, 1970,
Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario, Canada.
“Determination of Mercury in Liquid Chlorine,” CSAL-M72.4, Feb. 25, 1972, Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario, Canada.
Chlorine Institute Reference No. MIR-104.
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.
*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
E506 − 17a
5. Apparatus
5.1 Atomic Absorption Spectrophotometer, equipped with mounting to hold absorption cell and a fast response (0.5 s) recorder.
5.2 Mercury Hollow Cathode Lamp, primary line 253.7 nm.
5.3 Absorption Cell, 10-cm path length with quartz windows.
5.4 Gas Washing Bottle, 125 mL, with extra-coarse fritted bubbler. The bottle has a calibration line drawn at the 60-mL mark.
5.5 Stopcock, 3-way, with plug of TFE-fluorocarbon.
5.6 Gas Washing Bottle, 125-mL without frit.
5.7 Drying Tube.
5.8 Flow Meter, capable of measuring and maintaining a flow of 42.5 L/h.
5.9 Large Dewar Flasks, two, with sufficient capacity to hold a 500-mL flask and a large volume of dry ice cooling mixture.
5.10 Flexible Tygon or equivalent Connection.
5.11 Stainless Steel Compression Nut.
5.12 Two-Hole Rubber Stopper.
5.13 Fluorocarbon Tubing.
NOTE 1—The procedure, as described in this test method, was developed using a Perkin-Elmer Model 303 atomic absorption spectrophotometer
equipped with a 10-cm absorption cell. Any other equivalent atomic absorption spectrophotometer may be used as well as one of the many commercial
instruments specifically designed for measurement of mercury by flameless atomic absorption. However, variation in instrument geometry, cell length,
sensitivity, and mode of response measurement may require appropriate modifications of the operating parameters.
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. Blanks should be
run on all reagents to assure a negligible mercury content.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean Type II or Type III reagent
water conforming to Specification D1193.
6.3 Aqua Regia—Carefully add 10 mL of concentrated HNO (sp gr 1.42) to 30 mL of concentrated HCl (sp gr 1.19) in a
100-mL beaker. Let the mixture stand for 5 min before use. This mixture is unstable and should not be stored. (Warning— Use
goggles when preparing or using this solution.)
6.4 Nitric Acid (1 + 9)—Pipet 25 mL of concentrated HNO (sp gr 1.42) into a 250-mL volumetric flask containing about 150
mL of water. Dilute to volume with water and mix well. (Warning—Use goggles when preparing this solution.)
6.5 Sulfuric Acid (1 + 4)—Add slowly with stirring 200 mL of concentrated H SO (sp gr 1.84) to 800 mL of water.
2 4
(Warning—Use goggles when preparing this solution.)
6.6 Cooling Mixture for Dewar Flasks—Fill two thirds of the Dewar flask with dichloromethane. Add dry ice slowly, allowing
time for the solution to cool, until there is no sublimation of dry ice on further addition. Replenish the dry ice when necessary.
See the SDS sheet for dichloromethane before using this material.
6.7 Hydroxylamine Hydrochloride Solution (100 g/L)—See Practice E200. This reagent is dispensed with a dropping bottle.
6.8 Mercury Standard Solution (50 μg Hg/mL)—As prepared in Practice E200.
6.9 Mercury Standard Solution (10 μg Hg/mL)—Pipet 10 mL of the standard mercury solution containing 50 μg Hg/mL into
a 50-mL volumetric flask, acidify with 5 mL of 1 + 4 H SO and dilute to volume with water. Mix well. Prepare fresh daily.
2 4
6.10 Mercury Standard Solution (1 μg Hg/mL)—Pipet 10 mL of the standard mercury solution containing 10 μg Hg/mL into
a 100-mL volumetric flask, acidify with 5 mL 1 + 4 H SO and dilute to volume with water. Mix well. Prepare fresh daily.
2 4
6.11 Potassium Permanganate Solution (40 g/L) (4 %)—Weigh 40 g of KMnO into a 1000-mL beaker. Add about 800 mL of
water and stir with a mechanical stirrer until completely dissolved. Allow the solution to stand overnight and filter. Transfer to a
1000-mL volumetric flask, dilute to volume, and store in a brown bottle.
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.
E506 − 17a
6.12 Stannous Chloride (10 %)—Dissolve 20 g of stannous chloride (SnCl ·2H O) in 40 mL of warm concentrated HCl (sp gr
2 2
1.19). Add 160 mL of water when all the stannous chloride has dissolved. Allow the solution to stand overnight and filter. Mix
and store in a 250-mL reagent bottle. Prepare fresh once a week. A piece of metallic tin in the bottle allows longer term storage
if the bottle is well sealed.
7. Safety Precautions
7.1 Sulfuric acid will cause severe burns if allowed to come in contact with any part of the skin or eyes. All spillages must be
immediately flushed from the skin or eyes with cold water. This acid must always be added slowly to water with adequate stirring
since heat is developed and spattering occurs if the acid is added too quickly.
7.2 Aqua regia contains both HNO and HCl, which will cause severe burns if allowed to come in contact with any part of the
skin or eyes. All spillages must be immediately flushed from the skin or eyes with cold water. Vapors produced by aqua regia can
cause burns if inhaled. It should be used only in a fume hood or with similar ventilation. This solution is unstable and must not
be placed in a stoppered flask or bottle.
7.3 Nitric acid will cause severe burns if allowed to come in contact with any part of the skin or eyes. All spillages must be
immediately flushed from the skin or eyes with cold water.
7.4 Chlorine is a corrosive and toxic material. A well-ventilated fume hood should be used to house all test equipment when
this product is analyzed in the laboratory.
7.5 Liquid chlorine sampling should be performed only by those persons thoroughly familiar with the handling of this material
and the operation of the sampling system. Personnel should be equipped with monogoggles, gloves (if desired), and a respirator.
Sampling should be done in a well-ventilated area or in a fume hood.
7.6 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 a respirator. Splashes
of liquid chlorine destroy clothing and, if such clothing is next to the skin, will produce irritations and burns.
7.7 When sampling and working with chlorine out of doors, people downwind from such operation should be warned of the
possible release of chlorine vapors.
7.8 It is recommended that means be available for disposal of excess chlorine in an environmentally safe
...