ASTM E449-08(2013)
(Test Method)Standard Test Methods for Analysis of Calcium Chloride
Standard Test Methods for Analysis of Calcium Chloride
SIGNIFICANCE AND USE
3.1 Calcium chloride is available in various forms and purities. A major use is the de-icing and dust control of roads. It is also used in the coal industry for dustproofing and freezeproofing, in foods, in electrolytic cells, and in refrigeration brines. The test methods listed in 1.2 provide procedures for analyzing calcium chloride to determine if it is suitable for its intended use.
SCOPE
1.1 These test methods cover the analysis of calcium chloride and solutions.
1.2 Procedures are given for the determination of calcium chloride, magnesium chloride, potassium chloride, sodium chloride, and calcium hydroxide. The test methods appear in the following order:
Sections
Calcium Chloride
8 to 16
Magnesium Chloride, Potassium Chloride,
and Sodium Chloride
17 to 26
Calcium Hydroxide
27 to 33
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
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 hazard statements are given in Section 5.
1.5 Review the current Material Safety Data Sheet (MSDS) for detailed information concerning toxicity, first aid procedures, handling, and safety precautions.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: E449 − 08 (Reapproved 2013)
Standard Test Methods for
Analysis of Calcium Chloride
This standard is issued under the fixed designation E449; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope cialty Chemicals (Withdrawn 2009)
E200Practice for Preparation, Standardization, and Storage
1.1 These test methods cover the analysis of calcium chlo-
of Standard and Reagent Solutions for ChemicalAnalysis
ride and solutions.
E663PracticeforFlameAtomicAbsorptionAnalysis(With-
1.2 Procedures are given for the determination of calcium 3
drawn 1997)
chloride, magnesium chloride, potassium chloride, sodium
chloride, and calcium hydroxide. The test methods appear in
3. Significance and Use
the following order:
3.1 Calcium chloride is available in various forms and
Sections
purities.Amajor use is the de-icing and dust control of roads.
Calcium Chloride 8 to 16
It is also used in the coal industry for dustproofing and
Magnesium Chloride, Potassium Chloride, 17 to 26
and Sodium Chloride
freezeproofing, in foods, in electrolytic cells, and in refrigera-
Calcium Hydroxide 27 to 33
tion brines. The test methods listed in 1.2 provide procedures
1.3 The values stated in SI units are to be regarded as
for analyzing calcium chloride to determine if it is suitable for
standard. The values given in parentheses are for information
its intended use.
only.
4. Reagents
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 Purity of Reagents—Reagent grade chemicals shall be
responsibility of the user of this standard to establish appro- used in all tests. Unless otherwise indicated, these shall
priate safety and health practices and determine the applica- conform to the specifications of the Committee on Analytical
bility of regulatory limitations prior to use. Specific hazard Reagents of the American Chemical Society, where such
statements are given in Section 5. specifications are available. Other grades may be used, pro-
1.5 Review the current Material Safety Data Sheet (MSDS)
vided it is first ascertained that the reagent is of sufficiently
for detailed information concerning toxicity, first aid high purity to permit its use without lessening the accuracy of
procedures, handling, and safety precautions.
the determination.
4.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents
to water shall be understood to mean Type II or Type III
2.1 ASTM Standards: reagent water conforming to Specification D1193.
D345Test Method for Sampling and Testing Calcium Chlo-
5. Hazards
ride for Roads and Structural Applications
D1193Specification for Reagent Water
5.1 Whilecalciumchlorideisarelativelyharmlessmaterial,
E180Practice for Determining the Precision of ASTM
some of the reagents used in these methods present possible
Methods for Analysis and Testing of Industrial and Spe-
safety hazards. Potassium cyanide is extremely hazardous and
must be handled with great care. In addition to being
poisonous,solutionscontainingcyanideshouldneverbemixed
These test methods are under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of
Subcommittee D16.16 on Industrial and Specialty Product Standards. The last approved version of this historical standard is referenced on
Current edition approved June 1, 2013. Published June 2013. Originally www.astm.org.
approved in 1972. Last previous edition approved in 2008 as E449–08. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/E0449-08R13. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary,U.S.PharmaceuticalConvention,Inc.(USPC),Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E449 − 08 (2013)
with acids to preclude the release of poisonous hydrogen Erlenmeyer flask and dilute to 200 mL with water. Proceed as
cyanide gas. Concentrated hydrochloric acid and sodium hy- directed in 13.2. Calculate the CaCl equivalent of the EDTA
droxide also are hazardous chemicals which may produce solution as follows:
serious burns on contact.
Calciumchlorideequivalent, g/mL 50.416/A (1)
6. Atomic Absorption Spectrophotometers where:
A = millilitres of EDTAsolution required for the titration of
6.1 Photometers and photometric practice used in these
the CaCl solution.
methods shall conform to Practice E663.
12.3 Hydrochloric Acid(1+3)—Mix 1 volume of concen-
7. Sampling
trated hydrochloric acid (HCl, sp gr 1.19) and 3 volumes of
7.1 Sampling of calcium chloride is not within the scope of
water.
thesetestmethods.SeetheappropriatesectionsofTestMethod
12.4 Hydroxylamine Hydrochloride Solution—(10 %)—
D345.
Dissolve 10 g of hydroxylamine hydrochloride (NH OH·HCl)
7.2 Thesampletobeanalyzedshallbeconsideredtobethat
in 90 mL of water.
sample in a single bottle submitted to the analytical laboratory.
12.5 α-Hydroxynaphthol Blue.
7.3 The size of the sample shall be sufficient to perform all
12.6 Modified Calcein Indicator.
analyses without the reuse of any portion of the sample.
12.7 Potassium Cyanide (KCN).
CALCIUM CHLORIDE
12.8 Sodium Hydroxide Solution(80g/L)—Addslowly80g
of sodium hydroxide (NaOH) in 300 mL of water stirring
8. Scope
constantly. Cool, transfer to a 1-L volumetric flask, dilute to
8.1 This test method covers the determination of calcium
volume with water, and mix.
chloride in the range from 0 to 100%.
12.9 Sugar, granulated.
9. Summary of Test Method
13. Procedure
9.1 Calcium in an alkaline solution is titrated with standard
13.1 Solid Samples—Weigh 100.0 g of sample and wash
ethylenediaminetetraacetate solution, using modified calcein II
intoa1000-mLvolumetricflaskwithwater.Add10mLofHCl
as an indicator. The color change is from green to purple. α
(1+3) and swirl to dissolve the sample. Cool to room
-hydroxynaphtholblueisalsosuitableasanindicator,inwhich
temperature, make to volume with water, and mix. Pipet a
case the color change is from red to blue.
20-mL aliquot into a 500-mL volumetric flask, dilute to
10. Interferences
volume, and mix. Proceed as in 13.3.
10.1 Strontium and other cations not complexed with cya-
13.2 Liquid Samples—Weigh 100.0 g of sample and wash
nide at pH of at least 10 will consume ethylenediaminetetraac- intoa1000-mLvolumetricflaskwithwater.Add10mLofHCl
etate solution and will affect the accuracy of this test method.
(1+3)andmix.Cooltoroomtemperature,makeuptovolume
with water, and mix. Pipet an aliquot containing about2gof
11. Apparatus
CaCl into a 500-mL volumetric flask, dilute to volume, and
mix. Appropriate aliquot volumes are indicated in the table
11.1 Buret, 50-mL, Class A.
below. Interpolate if necessary.
11.2 Weighing Bottle, glass-stoppered, 100-mL.
Expected CaCl Aliquot
Concentration, % Size, mL
12. Reagents
10 200
20 100
12.1 Calcium Chloride, Standard Solution (1 mL=0.00832
30 75
gCaCl )—Weigh7.500gofprimarystandardcalciumcarbon-
40 50
ate (CaCO ). Transfer to a 600-mLbeaker and add 300 mLof
3 50 40
water. Cover with a watch glass and slowly add to the beaker,
13.3 Pipeta100-mLaliquotofthesolutionpreparedin13.1
while stirring, 15 mL of concentrated hydrochloric acid (HCl)
or13.2intoa500-mLErlenmeyerflaskanddilutetoabout200
delivered from a pipet inserted between the lip of the beaker
mL with water. Add in order 10 mL of hydroxylamine
and the edge of the watch glass. When dissolution of the
hydrochloridesolutionand3gofsugar.Swirltodissolve.Add
CaCO is complete, boil gently to expel CO . Cool, and
3 2
40 mLof NaOH solution (12.8) and swirl to mix.Add 0.1 g of
transfer to a 1-Lvolumetric flask. Dilute to volume with water
KCN, and swirl to dissolve and mix. Add about 0.2 g of
and mix.
calcium indicator.
12.2 Ethylenediaminetetraacetate, Standard Solution (0.1
13.4 Titrate with 0.1 M EDTA solution until the indicator
mol/L (M))—Dissolve 37.22 g of disodium dihydrogen ethyl-
changes from green to purple.
enediaminetetraacetate dihydrate (EDTA) in water. Transfer to
a 1-L volumetric flask, dilute to volume with water, and mix.
Standardize as follows: Transfer a 50-mL aliquot of CaCl
2 Available from Mallinckrodt Inc., Paris, KY.
standard solution (1 mL=0.00832 g CaCl ) to a 500-mL Available from the G. Frederick Smith Co., Columbus, OH.
E449 − 08 (2013)
NOTE 1—If α-hydroxynaphthol blue indicator is used, 0.4 g should be
is measured and compared with the response of the instrument
added and the solution titrated to a blue end point.
to calibration solutions of the same elements. Recommended
lines are: magnesium (2852 Å), potassium (7664 Å), and
14. Calculation
sodium (5889 Å).
14.1 Calculate the calcium chloride concentration as fol-
lows:
19. Concentration Range
Calciumchloride,% 5 @~A 3 B!/C'# 3100 2 D (2)
19.1 The concentration range for each cation must be
selected to correspond with the optimum range of the instru-
where:
ment employed. Higher or lower concentration ranges may be
A = millilitres of EDTAsolution required for titration of the
required for different instruments or different source lamps.
sample,
B = calcium chloride equivalent of the EDTA solution,
20. Interferences
g/mL,
20.1 Elements normally present in calcium chloride do not
C' = mass of sample in the aliquot used, and
D = percent calcium hydroxide expressed as calcium chlo-
interfere with these determinations.
ride (see 31.1.1).
21. Apparatus
15. Report
21.1 Atomic Absorption Spectrophotometer, capable of iso-
15.1 Report the percentage of CaCl to the nearest 0.1%.
2 lating the resonance line chosen for each cation sufficiently to
Duplicate determinations that agree within 0.3% absolute are
avoid interference from other elements in the samples being
acceptable for averaging (95% confidence level).
analyzed.
16. Precision and
...
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