1、Designation: E 1584 00 (Reapproved 2005)e1Standard Test Method forAssay of Nitric Acid1This standard is issued under the fixed designation E 1584; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEThe multiplier in the numerator of Eq 2 was changed from 6301 to 6.301 editorially in April 2007.1. Scope1.1 This test method covers determination
3、of the assay ofnitric acid by total acidity. This test method is suitable forconcentrations between approximately 50 and 70 %, calculatedas nitric acid.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 Review the current M
4、aterial Safety Data Sheets (MSDS)for detailed information concerning toxicity, first aid proce-dures, and safety precautions.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish app
5、ro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE 180 Practice for Determining the Precision of AS
6、TMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysisE 300 Practice for Sampling Industrial Chemicals3. Summary of Test Method3.1 Aweighed sample of acid is diluted
7、 in water and titratedwith 1.0 N sodium hydroxide solution, using phenolphthaleinas the end-point indicator.4. Significance and Use4.1 This test method provides a means for assaying nitricacid, based on total acidity. The concentration of nitric acid isimportant in many of the uses of nitric acid, i
8、ncludingspecification compliance and manufacturing control.5. Interferences5.1 Acids other than nitric, and compounds that consumesodium hydroxide, will yield erroneously high results.6. Apparatus6.1 Erlenmeyer Flask, 250 mL, glass stoppered.6.2 Buret, 50 mL, Class A.NOTE 1A digital buret capable of
9、 measuring volumes to the nearest0.01 mL may be used in place of a conventional buret.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents o
10、f the American Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterUnless otherwise indicated, referen
11、cesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D 1193.7.3 Phenolphthalein Indicator Solution (10 g/L)Dissolve1 g of phenolphthalein in 100 mL of ethanol (95 %), methanol,or isopropanol.47.4 Sodium Hydroxide, Standard Solution (1.0 N)Prepareand
12、 standardize in accordance with Practice E 200, remember-ing to record the temperature of the NaOH solution during thestandardization to the nearest C.1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of Subcommitt
13、eeE15.02 on Product Standards.Current edition approved Oct. 1, 2005. Published November 2005. Originallyapproved in 1993. Last previous edition approved in 2000 as E 1584 00.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For
14、Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Soci
15、ety, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4This reagent is also described in Practice E 200.1Copyright ASTM International, 100 Barr Harbor Drive,
16、 PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Safety Precautions8.1 Nitric acid is dangerous if handled improperly. It is astrong corrosive acid and a strong oxidizer. Contact with othermaterial may cause fire. Avoid inhalation of fumes or mist andany contact with skin or eyes.8.2
17、 Clean up all spills immediately by covering the spillwith vermiculite or some other inert absorbent material andsweeping it into a pan. Dispose of the vermiculite by floodingwith water and discarding in a suitable container. Flush the areawith water.9. Sampling9.1 Sampling of nitric acid is not wit
18、hin the scope of thistest method. General guidelines for sampling may be found inPractice E 300.9.2 The sample to be analyzed shall be considered to be thatsample in a single bottle submitted to the analytical laboratory.10. Procedure10.1 Tare to the nearest 0.1 mg a glass stoppered 250-mLErlenmeyer
19、 flask containing approximately 15 mL of water.10.2 Remove the stopper. Using a suitable pipet, quicklyadd an appropriate volume of sample (depending on the acidstrength as given in Table 1), while keeping the tip of the pipetjust above the surface of the liquid. Immediately replace thestopper, and
20、reweigh the flask to the nearest 0.1 mg to obtainthe weight of the sample.NOTE 2A disposable dropping pipet is convenient for the sampletransfer.10.3 Remove the stopper, add 50 mL of water and 4 dropsof phenolphthalein indicator solution to the flask, and swirl tomix the contents. Record the tempera
21、ture of the 1.0 N NaOHsolution, and then titrate the sample to a pale pink end point.Record the volume of the titrant to the nearest 0.01 mL.11. Calculation11.1 If necessary, correct the buret reading for calibrationerrors, and record the volume of the titrant as V and itstemperature during the titr
22、ation as t.11.2 Correct the normality of the sodium hydroxide stan-dard solution for any difference in temperature between time ofstandardization and time of use in accordance with the follow-ing equation:N 5 Ns1 0.00035 s 2 t! (1)where:N = normality of NaOH solution at time of titration,Ns= normali
23、ty of NaOH solution at time of standardiza-tion,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 weight 5VN 3 6.301W(2)where:V = corrected NaOH solution required for titration
24、 of thesample, mL,N = normality of the NaOH solution corrected for tempera-ture at time of titration, andW = sample used, g.12. Report12.1 Report the percent of nitric acid to the nearest 0.01 %.13. Precision and Bias13.1 PrecisionThe following criteria should be used forjudging the acceptability of
25、 results (Note 3):13.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated to be0.0914 % absolute at 54 df. The 95 % limit for the differencebetween two such runs is 0.26 % absolute.13.1.2 Laboratory Precision (Within-Laboratory, Between-Days Variabi
26、lity), Formerly Called Repeatability)The stan-dard deviation of results (each the average of duplicates),obtained by the same analyst on different days, has beenestimated to be 0.0892 % absolute at 27 df. The 95 % limit forthe difference between two such averages is 0.25 % absolute.13.1.3 Reproducib
27、ility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be0.1720 % absolute at 8 df. The 95 % limit for the differencebetween two such averages is 0.48 % absolute.NOTE 3The preceding precision es
28、timates are based on an interlabo-ratory study of analyses performed in 1993 to 1994 on three samples ofnitric acid with average assays of 56.49 %, 65.54 %, and 69.65 %. Oneanalyst in each of nine laboratories performed duplicate determinationsand repeated one day later, for a total of 108 determina
29、tions.5PracticeE 180 was used in developing these precision estimates.13.2 BiasThe bias of this test method cannot be deter-mined unless a suitable reference material becomes available.14. Keywords14.1 assay; nitric acid; titrimetric method5Supporting data have been filed at ASTM International Headq
30、uarters and maybe obtained by requesting Research Report RR: E15-1041.TABLE 1 Sample Size for Assay of Nitric AcidAHNO3, % Sample Size, mL Nominal Weight, g70 2.5 6 0.2 3.665 2.8 6 0.2 3.960 3.1 6 0.2 4.355 3.4 6 0.2 4.650 3.8 6 0.2 5.0AIn some cases, where the concentration range of the sample is u
31、nknown, apreliminary test may be required to determine the proper size test sample to use.E 1584 00 (2005)e12ASTM 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
32、that determination of the validity of any such patent rights, 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 reap
33、proved or withdrawn. Your comments are invited either for 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
34、 feel that your comments have not received a fair hearing 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 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).E 1584 00 (2005)e13
