ASTM E1584-23

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: E1584 − 17 E1584 − 23
Standard Test Method for
Assay of Nitric Acid
This standard is issued under the fixed designation E1584; 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 determination of the assay of nitric acid by total acidity.
1.2 This test method covers determination of the assay of nitric acid by total acidity. This test method is suitable for concentrations
between approximately 5050 % and 70 %, calculated as nitric acid.
1.3 The following applies for the purposes of determining the conformance of the test results using this test method to applicable
specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety
precautions.
1.5 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific precautionary statements are given in For specific hazard statements, see Section 8.
1.6 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:
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
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
E300 Practice for Sampling Industrial Chemicals
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.10 on Acids.
Current edition approved June 1, 2017July 1, 2023. Published July 2017July 2023. Originally approved in 1993. Last previous edition approved in 20112017 as
E1584 – 11.E1584 – 17. DOI: 10.1520/E1584-17.10.1520/E1584-23.
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.
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
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E1584 − 23
2.2 Other Documents:
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 A weighed sample of acid is diluted in water and titrated with 1.0 N sodium hydroxide solution, using phenolphthalein as the
end-point indicator.
4. Significance and Use
4.1 This test method provides a means for assaying nitric acid, based on total acidity. The concentration of nitric acid is important
in many of the uses of nitric acid, including specification compliance and manufacturing control.
5. Interferences
5.1 Acids other than nitric, and compounds that consume sodium hydroxide, will yield erroneously high results.
6. Apparatus
6.1 Erlenmeyer Flask, 250 mL, glass stoppered.
6.2 Buret, 50 mL, Class A.
NOTE 1—A digital buret or automated titrator capable of measuring volumes to the nearest 0.01 mL may be used in place of a conventional buret.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type
III or Type IIIII of Specification D1193.
7.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve 1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol, or
isopropanol.
7.4 Sodium Hydroxide, Standard Solution (1.0N)—Prepare and standardize in accordance with Practice E200, remembering to
record the temperature of the NaOH solution during the standardization to the nearest °C.
NOTE 2—Because of atmospheric CO absorption by NaOH, 1.0 N NaOH solutions will need frequent standardization.
8. Safety Precautions Hazards
8.1 Consult current OSHA regulations, suppliers’ Safety Data Sheets, and local regulations for all materials used in this test
method.
8.2 Nitric acid is dangerous if handled improperly. It is a strong corrosive acid and a strong oxidizer. Contact with other material
may cause fire. Avoid inhalation of fumes or mist and any contact with skin or eyes. Use of safety goggles and gloves highly
recommended.
Available from Superintendent of Documents, U.S. Government Printing Office, 732 N. Capitol St. NW, Mail Stop: SDE, Washington, DC 20401.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, 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.
This reagent is also described in Practice E200.
E1584 − 23
A
TABLE 1 Sample Size for Assay of Nitric Acid
HNO , % Sample Size, mL Nominal Weight, g
70 2.5 ± 0.2 3.6
65 2.8 ± 0.2 3.9
60 3.1 ± 0.2 4.3
55 3.4 ± 0.2 4.6
50 3.8 ± 0.2 5.0
A
In some cases, where the concentration range of the sample is unknown, a
preliminary test may be required to determine the proper size test sample to use.
8.3 Clean up all spills immediately by covering the spill with vermiculite or some other inert absorbent material and sweeping it
into a pan. Dispose of the vermiculite by flooding with water and d
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