ASTM C400-1998(2013) Standard Test Methods for Quicklime and Hydrated Lime for Neutralization of Waste Acid《中和废酸用生石灰和熟石灰的标准试验方法》.pdf

1、Designation: C400 98 (Reapproved 2013)Standard Test Methods forQuicklime and Hydrated Lime for Neutralization of WasteAcid1This standard is issued under the fixed designation C400; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th

2、e year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the testing of quicklime andhydrated lime for use in the treatment of waste acid sol

3、utionsand includes the characterization of the liming material and ofthe acid waste.NOTE 1When agreed upon by the manufacturer and the purchaser,this method may be used directly to evaluate the lime requirement for aplant waste acid and in the preparation of the lime slurry; the pH, the time,tempera

4、ture, and other conditions of treatment may be adjusted toconform to plant practice. Otherwise the test shall be performed asdescribed in this method.NOTE 2Under some conditions of test the lime requirement may varysubstantially from that indicated by ultimate chemical analysis or by theuse of a det

5、ermination of available alkalinity by titration to a stoichio-metric end point.1.2 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 appro-priate safety and health practices and dete

6、rmine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C50 Practice for Sampling, Sample Preparation, Packaging,and Marking of Lime and Limestone ProductsE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Terminology3.1 Definitio

7、ns:3.1.1 neutralization coeffcientthe number of parts of limerequired to neutralize one million parts by weight of sulfuricacid solution (1.5 %) to a pH of 4.4 in 30 min (see Note 1).3.1.2 pHa measure of the hydrogen ion concentration of asample and representing the logarithm of the reciprocal (nega

8、-tive logarithm) of the activity of hydrogen ions, calculated asfollows:pH 5 log1H!152logH1!where:H+= activity of hydrogen ions.4. Significance and Use4.1 Since all limes and waste acid solutions are different,this test method evaluates the relative quantity of a given limeneeded for the neutralizat

9、ion of a specific quantity of acid.4.2 Liming materials have a specific basicity factor ormeasure of alkalinity which can be used for comparing theirrelative neutralizing power. It avoids dependence on chemicalanalysis and is determined as grams of calcium oxide equiva-lents per kilogram of liming m

10、aterial.4.3 Likewise, specific waste acids have an acid value thatcan be expressed as grams of hydrochloric acid equivalent perlitre of acid waste. This value is related on a stoichiometricbasis to lime neutralization requirements of a liquid acid waste.5. Apparatus5.1 pH Measuring Apparatus, confor

11、ming to the require-ments of Section 5, Apparatus, and Section 6, Reagents andMaterials, of Test Method E70. A time-pH recording device orattachment is desirable but not required.5.2 Analytical Balance, capable of reproducing resultswithin 0.005 g.5.3 Stirrer, motorized, capable of rotating at speed

12、s from120 to 600 r/min.5.4 Miscellaneous EquipmentChemically resistantglassware,3metal stands for support of the equipment, etc.6. Purity of Reagents6.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shall1These test methods are under

13、the jurisdiction of ASTM Committee C07 onLime and are the direct responsibility of Subcommittee C07.05 on Chemical Tests.Current edition approved July 1, 2013. Published August 2013. Originallyapproved in 1957. Last previous edition approved in 2006 as C400 98 (2006).DOI: 10.1520/C0400-98R13.2For re

14、ferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Borosilicate glass has been found satisfactory for this purpose.Cop

15、yright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1conform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.4Other grades may be used, pro-vided it is firs

16、t ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Unless otherwise indicated, references to water shall beunderstood to mean distilled water.7. Test Method Afor Determining Lime Requirement forthe neutralization of a

17、 standard sulfuric acid or waste acidsolution within a time limit of thirty minutes.7.1 Reagents:7.1.1 Sulfuric Acid, Standard Solution (1.5 6 0.05 %)Thoroughly mix 15.8 g of concentrated sulfuric acid (95 %H2SO4) with water, dilute to 1 L, analyze to within 0.005 %H2SO4, and store in a suitable sto

18、ppered bottle.7.2 Preparation of Sample:7.2.1 Take samples of quicklime and hydrated lime inaccordance with Methods C50.7.2.2 QuicklimeWeigh a sample of quicklime (2.50 60.01 g) ground to pass a No. 50 mesh sieve. Add to a 500-mLtall-form beaker containing 50 mL of boiling water andcontinue to boil

19、for 2 min. Remove from hot plate and continuestirring with a magnetic stirrer until the slurry reaches roomtemperature (at least 10 min).7.2.3 Hydrated LimeMix a sample of hydrated lime (2.506 0.01 g) with 50 mL of water in a 500-mL tall-form beakerfor at least 10 min.7.3 Procedure:7.3.1 Place the p

20、H electrodes within the beaker about12 in.(13 mm) above the surface of the lime slurry sample. Set themotor stirrer to the highest speed at which splattering orimmersion of the electrodes does not occur. Measure 250 g ofH2SO4(1.5 6 0.05 %) into a separate 500-mLbeaker.Add thisacid to the sample in a

21、 single motion and record the pH as afunction of time for a period of 30 min (see Note 1).7.3.2 Test a second slurry sample using more or less than250gofH2SO4(1.5 6 0.05 %), as indicated by the pH valueobserved after 30 min reaction in the first test. Repeat theprocedure at least four times or until

22、 sufficient data areavailable to give a family of curves that indicate pH at 30 minas a function of grams of lime per 1000 g of H2SO4(1.5 %),with particular emphasis in the region of pH equals 4.4.7.4 Results:7.4.1 Neutralization Rate Curves:7.4.1.1 Plot pH versus time in minutes for each of thelime

23、-acid ratios used in the initial series of tests. This family ofcurves serves as the basis for calculation of the lime require-ments.7.4.2 Lime Requirement Curve:7.4.2.1 Plot the pH in 30 min, as determined from theneutralization rate curves described in Section 10, againstgrams of lime used per 100

24、0 g of H2SO4(1.5 %).7.4.3 Neutralization Coeffcient:7.4.3.1 Interpolate the quantity of lime required to achieve apH of 4.4 in 30 min from the lime requirement curve (Section11), correct for the actual acid concentration, and calculate asparts of lime required per million parts of H2SO4(1.5 %) asfol

25、lows:N 5 1.5/Z! 3X 31000where:N = neutralization coefficient (see 3.1.1),X = grams of lime per 1000 g of H2SO4(1.5 %), andZ = concentration of the H2SO4to the nearest 0.005 %, asdetermined by analysis.7.5 Precision and Bias:7.5.1 The precision and bias of this test method has not beendetermined at t

26、his time. Replicate samples are recommended.8. Test Method BFor Determining Acid Value-BasicityFactor Relationship8.1 Procedure:8.1.1 Basicity FactorWeigh 2.804 g 6 1 mg of the samplethat has been prepared to pass a No. 100 (150-m) sieve andtransfer to a 500-mL Erlenmeyer flask containing approxi-ma

27、tely 20 mL of cold water. (For quicklime samples, heat toboiling to ensure complete slaking). Add from a buret 100 mLof 1.0 N hydrochloric acid and stopper with a two-hole rubberstopper (Note 3). The quantity of acid may be increased ordecreased depending on the equivalent strength of the materialbe

28、ing tested. Place the flask on a hot plate and boil for 15 min.(Glass beads may be added to prevent bumping.) Remove theflask from the hot plate and cool in water. Add several drops ofphenolphthalein indicator solution and titrate the excess acidwith 0.5 N sodium hydroxide solution. Calculate the ba

29、sicityfactor as follows:Basicity factor 5 V1N12 V2N2!/W# 30.02804where:V1= HCl (mL) required for titration of the sample,N1= normality of HCl,V2= NaOH solution (mL) required for titration of the excessacid,N2= normality of NaOH solution, andW = sample (g).NOTE 3A water-cooled condenser with a tapere

30、d, ground-glass jointand a magnetic stir plate may be used during the boiling step.8.1.2 Acid ValuePipet 10 mLof the sample of acidic wasteinto a 250-mL Erlenmeyer flask. This quantity may be in-creased or decreased depending on the strength of the acidicwaste. Add an excess of 25 to 30 mL of 0.5 N

31、sodiumhydroxide solution and boil for 3 min. Filter through a smallBchner funnel with the aid of vacuum. Wash the residue onthe funnel with water. Add several drops of phenolphthaleinindicator solution to the filtrate and titrate the excess sodium4“Reagent Chemicals, American Chemical Society Specif

32、ications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D. Van Nostrand Co., Inc., New York, NY, and the “United StatesPharmacopeia.”C400 98 (2013)2hydroxide with 1.0

33、N hydrochloric acid solution. Calculate acidvalue as follows:Acid value 5 V1N12 V2N2!/V# 30.03646where:V1= NaOH solution (mL) required for titration of thesample,N1= normality of NaOH solution,V2= HCl (mL) required for titration of the excess NaOHsolution,N2= normality of HCl, andV = sample (mL).8.1

34、.3 Relationship of Acid Value to Basicity FactorCalculate the acid value-basicity factor relationship as follows:Acid valueBasicity factor30.76915 lime or limestone productkg! per litre of Acidic Waste.NOTE 4When agreed upon between the manufacturer and thepurchaser, Test Method A may also be used.8

35、.2 Precision and Bias:8.2.1 The precision and bias of this test method has not beendetermined at this time. Replicate samples are recommended.9. Keywords9.1 acid value; alkalinity; basicity; lime requirement; limingmaterial; neutralization; neutralization coefficient; pH; wasteacidASTM International

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39、t 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).C400 98 (2013)3