1、Designation: E1584 11E1584 17Standard Test Method forAssay of Nitric Acid1This standard is issued under the fixed designation E1584; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses
2、 indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers determination of the assay of nitric acid by total acidity. This test method is suitable forconcentrations between approximat
3、ely 50 and 70 %, calculated as nitric acid.1.2 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 Material Safety Data Sheets (MSDS)(SDS) for detailed information concerning toxicity, first aidprocedures, a
4、nd safety precautions.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to
5、 use. Specific precautionary statements are given in Section 8.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations
6、 issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE180 Practice for Determi
7、ning the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical AnalysisE300 Practice for Sampling Industrial Chemicals3. Summary of Test Metho
8、d3.1 A weighed sample of acid is diluted in water and titrated with 1.0 N sodium hydroxide solution, using phenolphthalein asthe end-point indicator.4. Significance and Use4.1 This test method provides a means for assaying nitric acid, based on total acidity. The concentration of nitric acid isimpor
9、tant in many of the uses of nitric acid, including specification compliance and manufacturing control.5. Interferences5.1 Acids other than nitric, and compounds that consume sodium hydroxide, will yield erroneously high results.6. Apparatus6.1 Erlenmeyer Flask, 250 mL, glass stoppered.6.2 Buret, 50
10、mL, Class A.1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of Subcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved Aug. 1, 2011June
11、 1, 2017. Published September 2011July 2017. Originally approved in 1993. Last previous edition approved in 20052011 asE1584 00 (2005)E1584 11.1. DOI: 10.1520/E1584-11.10.1520/E1584-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm
12、.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM
13、standard an indication of what changes have been made to the previous version. Becauseit 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 versionof the standard as published by
14、 ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1NOTE 1A digital buret or automated titrator capable of measuring volumes
15、to the nearest 0.01 mL may be used in place of a conventional buret.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American C
16、hemical Society where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, references to water
17、shall be understood to mean reagent water as defined byType II or Type III of Specification D1193.7.3 Phenolphthalein Indicator Solution (10 g/L)Dissolve 1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol, orisopropanol.54 Reagent Chemicals, American Chemical Society Specifications, Americ
18、an Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USP
19、C), Rockville, MD.5 This reagent is also described in Practice E200.E1584 1727.4 Sodium Hydroxide, Standard Solution (1.0N)Prepare and standardize in accordance with Practice E200, remembering torecord the temperature of the NaOH solution during the standardization to the nearest C.NOTE 2Because of
20、atmospheric CO2 absorption by NaOH, 1.0 N NaOH solutions will need frequent standardization.8. Safety Precautions8.1 Nitric acid is dangerous if handled improperly. It is a strong corrosive acid and a strong oxidizer. Contact with other materialmay cause fire. Avoid inhalation of fumes or mist and a
21、ny contact with skin or eyes.8.2 Clean up all spills immediately by covering the spill with vermiculite or some other inert absorbent material and sweepingit into a pan. Dispose of the vermiculite by flooding with water and discarding in a suitable container. Flush the area with water.9. Sampling9.1
22、 Sampling of nitric acid is not within the scope of this test method. General guidelines for sampling may be found in PracticeE300.9.2 The sample to be analyzed shall be considered to be that sample in a single bottle submitted to the analytical laboratory.10. Procedure10.1 Tare to the nearest 0.1 m
23、g a glass stoppered 250-mL Erlenmeyer flask containing approximately 15 mL of water.10.2 Remove the stopper. Using a suitable pipet, quickly add an appropriate volume of sample (depending on the acid strengthas given in Table 1), while keeping the tip of the pipet just above the surface of the liqui
24、d. Immediately replace the stopper, andreweigh the flask to the nearest 0.1 mg to obtain the weight of the sample.NOTE 3A disposable dropping pipet is convenient for the sample transfer.10.3 Remove the stopper, add 50 mL of water and 4 drops of phenolphthalein indicator solution to the flask, and sw
25、irl to mixthe contents. Record the temperature of the 1.0 N NaOH solution, and then titrate the sample to a pale pink end point. Record thevolume of the titrant to the nearest 0.01 mL.11. Calculation11.1 If necessary, correct the buret reading for calibration errors, and record the volume of the tit
26、rant as V and its temperatureduring the titration as t.11.2 Correct the normality of the sodium hydroxide standard solution for any difference in temperature between time ofstandardization and time of use in accordance with the following equation:N 5Ns10.00035 s 2t! (1)where:N = normality of NaOH so
27、lution at time of titration,Ns = normality of NaOH solution at time of standardization,s = temperature of NaOH during standardization, C, andt = temperature of NaOH during titration C.11.3 Calculate the assay as percent nitric acid as follows:nitric acid,%by weight5VN36.301W (2)where:V = corrected N
28、aOH solution required for titration of the sample, mL,N = normality of the NaOH solution corrected for temperature at time of titration, andW = sample used, g.TABLE 1 Sample Size for Assay of Nitric AcidAHNO3, % Sample Size, mL Nominal Weight, g70 2.5 0.2 3.665 2.8 0.2 3.960 3.1 0.2 4.355 3.4 0.2 4.
29、650 3.8 0.2 5.0A In some cases, where the concentration range of the sample is unknown, apreliminary test may be required to determine the proper size test sample to use.E1584 17312. Report12.1 Report the percent of nitric acid to the nearest 0.01 %.13. Precision and Bias13.1 PrecisionThe following
30、criteria should be used for judging the acceptability of results (Note 4):13.1.1 Repeatability (Single Analyst)The standard deviation for a single determination has been estimated to be 0.0914 %absolute at 54 df. The 95 % limit for the difference between two such runs is 0.26 % absolute.13.1.2 Labor
31、atory Precision (Within-Laboratory, Between-Days Variability), Formerly Called Repeatability)The standarddeviation of results (each the average of duplicates), obtained by the same analyst on different days, has been estimated to be0.0892 % absolute at 27 df. The 95 % limit for the difference betwee
32、n two such averages is 0.25 % absolute.13.1.3 Reproducibility (Multilaboratory)The standard deviation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be 0.1720 % absolute at 8 df. The 95 % limit for the difference betweentwo such aver
33、ages is 0.48 % absolute.NOTE 4The preceding precision estimates are based on an interlaboratory study of analyses performed in 1993 to 1994 on three samples of nitricacid with average assays of 56.49 %, 65.54 %, and 69.65 %. One analyst in each of nine laboratories performed duplicate determinations
34、 and repeatedone day later, for a total of 108 determinations.6 Practice E180 was used in developing these precision estimates.13.2 BiasThe bias of this test method cannot be determined unless a suitable reference material becomes available.14. Quality Guidelines14.1 Laboratories shall have a qualit
35、y control system in place.14.1.1 Confirm the performance of the test instrument or test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.14.1.2 Aquality control sample is a stable material isolated from the production process and
36、representative of the sample beinganalyzed.14.1.3 When QA/QC protocols are already established in the testing facility, these protocols are acceptable when they confirmthe validity of test results.14.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines descri
37、bed in Guide D6809 orsimilar quality control practices.15. Keywords15.1 assay; nitric acid; titrimetric methodSUMMARY OF CHANGESSubcommittee D16.16 has identified the location of selected changes to this standard since the last issue(E1584-11) that may impact the use of this standard. (Approved June
38、 1, 2017.)(1) Added Quality Guidelines as Section 14.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent ri
39、ghts, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for
40、 revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing
41、 you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may
42、 be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E15-1041. Contact ASTM CustomerService at serviceastm.org.E1584 174
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