Sodium Chloride: Standard Specification For
Sodium Chloride: Standard Specification For
Sodium Chloride: Standard Specification For
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D632 − 12
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D632 − 12
5.1.2 Type II—The grading of Type II sodium chloride shall 9.1.1 Routine Control—Use of the “Rapid Method” in
conform to the grading requirements imposed or permitted by Annex A1 is permitted for routine control and approval.
the purchaser under conditions of the intended use. 9.1.2 Referee Testing—In case of controversy, determine the
chemical composition of the sample, using the current version
6. Permissible Variations
of Test Method E534.
6.1 In the case of sodium chloride sampled after delivery to
the purchaser, tolerances from the foregoing specified values 9.2 Grading shall be determined by Test Method C136.
shall be allowed as follows:
6.1.1 Grading—5 percentage points on the maximum value 10. Inspection
for the range for each sieve size, except the 12.5 mm (1⁄2 in.) 10.1 The purchaser or his representative shall be provided
and 9.5 mm (3⁄8 in.) for Grade 1 and 19.0 mm (3⁄4 in.) for Grade free entry and necessary facilities at the production plant or
2. storage area if he elects to sample sodium chloride at the
6.1.2 Chemical Composition—0.5 percentage point. source.
7. Condition
11. Rejection and Rehearing
7.1 The sodium chloride shall arrive at the purchaser’s
delivery point in a free-flowing and usable condition. 11.1 The sodium chloride shall be subject to rejection if it
fails to conform to any of the requirements of this specification.
8. Sampling
11.2 In the case of failure to meet the requirements on the
8.1 Not less than three sample increments shall be selected basis of an initial sample of a lot represented, two additional
at random from the lot (Note 2). Each increment shall be samples shall be taken from the lot and tested. If both
obtained by scraping aside the top layer of material to a depth additional samples meet the requirements, the lot shall be
of at least 25 mm (1 in.) and taking a 500-g (approximately accepted.
1-lb) quantity of sodium chloride to a depth of at least 150 mm
(6 in.). Sampling shall be done by means of a sampling thief or 12. Packaging and Marking
other method that will ensure a representative cross section of
the material. The sample increments shall be thoroughly mixed 12.1 The sodium chloride shall be delivered in bags or other
to constitute a composite sample representative of the lot. containers acceptable to the purchaser, or in bulk lots. The
name of the producer and the net weight shall be legibly
NOTE 2—A lot may be an amount agreed upon between purchaser and marked on each bag or container, or in the case of bulk lots, on
supplier at the time of purchase.
the shipping or delivery report.
9. Test Methods
9.1 Chemical Analysis—Test for compliance with the re- 13. Keywords
quirements for chemical composition in accordance with the 13.1 salt; snow and ice removal; sodium chloride; stabiliza-
following methods: tion; winter maintenance
ANNEX
(Mandatory Information)
A1.1. Scope A1.2.2 This rapid method of analysis does not distinguish
A1.1.1 This annex covers a rapid method for chemical between sodium chloride and other evaporite chloride com-
analysis of sodium chloride. pounds with ice-melting capabilities. Typical rock salt and
solar salt sometimes contains small amounts of CaCl2, MgCl2,
A1.1.2 This international standard was developed in accor-
and KCl, depending on the source of the material. When this
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the rapid method is used on continuing shipments from a known
Development of International Standards, Guides and Recom- source, it will provide a fast, essentially accurate determination
mendations issued by the World Trade Organization Technical of the sodium chloride content of the material furnished. Thus,
Barriers to Trade (TBT) Committee. the need for testing by the referee method, Test Method E534,
is reduced.
A1.2. Significance and Use
A1.2.1 The procedure for chemical analysis in this annex
determines the total amount of chlorides present in the sample
and expresses that value as sodium chloride.
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D632 − 12
A1.3. Apparatus where:
A1.3.1 Glassware—Standard weighing bottles, volumetric A = reagent grade NaCl used, g,
flasks (conforming to Specification E288, Class C, or better), B = 0.05 N AgNO3 solution required to titrate the reagent
and burets (conforming to Specification E287, Class B, or grade NaCl, mL,
better). C = 0.05 N AgNO3 solution required to titrate the sample
being tested, mL,
A1.3.2 Balance, having a capacity of at least 20 g, accurate D = test sampling mass, g, and
and readable to 0.01 g. P = total chlorides, expressed as sodium chloride, in the
A1.4. Reagents sample being tested, %.
A1.4.1 Nitric Acid (HNO3), dilute (HNO3:H2O, 1:4 by A1.6.1 If moisture is apparent in the sample, dry a duplicate
volume). 10-g sample of the pulverized salt at 105°C and correct the
A1.4.2 Calcium Carbonate (CaCO3)—Reagent grade-low mass of the sample accordingly.
chloride, powder.
A1.7. Precision and Bias
A1.4.3 Silver Nitrate Solution—0.05 N AgNO3.
A1.4.4 Sodium Chloride (NaCl)—Reagent grade. A1.7.1 Precision2—An interlaboratory study was conducted
and an analysis was made that included three materials ranging
A1.4.5 Potassium Chromate (K2CrO4) Solution—(50 g
from approximately 92 % to 99 % NaCl. Ten laboratories were
K2CrO4/L).
included in the study.
A1.5. Procedure
A1.7.2 Single-Operator Precision (NaCl composition
A1.5.1 Thoroughly mix the composite sample obtained 95.0 % and greater)—The single-operator standard deviation
under 8.1, and reduce by quartering or by means of a sample of a single test result for average NaCl composition 95.0 % and
splitter to approximately 500 g. Pulverize the reduced sample greater has been found to be 0.248.3 Therefore, results of two
to pass a 300-µm (No. 50) sieve. properly conducted tests by the same operator on the same
A1.5.2 Standardization—Standardize the silver nitrate material with the same equipment and under the same condi-
(AgNO3) solution daily, using 10 g of reagent grade sodium tions should not differ by more than 0.70 %.3
chloride (NaCl) following the applicable procedure in A1.5.3. A1.7.3 Multilaboratory Precision (NaCl composition
A1.5.3 From the pulverized sodium chloride, obtain a test 95.0 % and greater)—The multilaboratory standard deviation
sample with a mass of 10.00 6 0.01 g and place in a beaker of a single test result for average NaCl composition greater
with 250-mL distilled water. Add 10 mL of the diluted nitric than 95.0 % has been found to be 0.633 %.3 Therefore, results
acid solution (HNO3, 1 + 4 by volume) and stir for 20 min at of two properly conducted tests in different laboratories on the
room temperature to put the salt in solution. Transfer the same material should not differ by more than 1.79 %.3
solution, including any insoluble material, to a 2-L volumetric
flask, dilute to the mark with distilled water, and mix. With a A1.7.4 Single Operator Precision (NaCl composition less
pipet, draw off 25 mL of the solution and place in a white than 95.0 % and greater than 90.0 %)—The single-operator
porcelain casserole. Add 0.5 g of calcium carbonate (CaCO3) coefficient of variation of a single test result for average NaCl
to neutralize the excess HNO3, and adjust the pH to approxi- composition less than 95.0 % and greater than 90.0 % has been
mately 7. Add 3 mL of the potassium chromate (K2CrO4) found to be 0.427 %.3 Therefore, results of two properly
solution as an indicator and titrate dropwise with the silver conducted tests by the same operator on the same material with
nitrate (AgNO3) solution until a faint but distinct change in the same equipment and under the same conditions should not
color occurs—a persistent yellowish brown endpoint (see Note differ by more than 1.21 %.3
A1.1), comparable to standardization. Estimate the titer from A1.7.5 Multilaboratory Precision (NaCl composition less
the buret to the second decimal place. than 95.0 % and greater than 90.0 %)—The multilaboratory
NOTE A1.1—The color of the initial solution is lemon-yellow. With standard deviation of a single test result for average NaCl
addition of the calcium carbonate (CaCO3) and stirring, the initial solution composition less than 95.0 % and greater than 90.0 % has been
becomes opaque, with a creamy lemon-yellow color. Addition of the silver found to be 0.711 %.3 Therefore, results of two properly
nitrate (AgNO3) solution produces silver chloride, which begins to conducted tests in different laboratories on the same material
agglomerate as the titration progresses, and the lemon-yellow color will
begin to have whitish, opaque swirls of silver chloride. As the titration should not differ by more than 2.00 %.3
proceeds, the red color formed by addition of each drop begins to A1.7.6 Bias—No justifiable statement can be made on the
disappear more slowly. Continue the addition dropwise until a faint but
distinct change in color occurs and the yellow-brown to faint reddish- bias of this test method because the data are not available.
brown color persists. The first stable presence of red silver chromate is the
endpoint. If the endpoint is overstepped, a deep reddish-brown color
occurs
2
Supporting data have been filed at ASTM International Headquarters and may
A1.6 Calculate—Calculate the total chlorides expressed as be obtained by requesting Research Report RR:D04-1016. Contact ASTM Customer
percent NaCl as follows: Service at [email protected].
3
These numbers represent, respectively, the (1s %) and (d2s %) limits, as
P 5 @ ~ A/B ! 3 ~ C/D ! # 3 100 (A1.1) described in Practice C670.
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D632 − 12
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