1、Designation: C 1580 05Standard Test Method forWater-Soluble Sulfate in Soil1This standard is issued under the fixed designation C 1580; 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 parenthe
2、ses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is for the determination of water-soluble sulfate in soils.1.2 This test method was developed for concentrations ofwater-soluble sulfat
3、e in soils between 0.02 and 3.33 % sulfateby mass.1.3 This test method does not determine sulfur in any formexcept as sulfate.1.4 Some governing bodies regulate the movement of soilsfrom one area to another. It is up to the sampler and laboratoryto comply with all regulations.1.5 The values stated i
4、n SI units are to be regarded as thestandard.1.6 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 to determine theapplicability of regul
5、atory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C114 Test Methods for Chemical Analysis for HydraulicCementD 1193 Specification for Reagent WaterE 11 Specification for Wire and Cloth Sieves for TestingPurposesE60 Practice for Analysis of Metals, Ores, and RelatedMaterials b
6、y Molecular Absorption SpectrometryE 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near Infrared Spectrophotom-eters3. Significance and Use3.1 This test method can be used to determine if soils couldhave an adverse reaction with hydraulic cement concrete.4. Appara
7、tus4.1 PhotometerOne of the following, given in order ofpreference:4.1.1 Nephelometer or turbidimeter,4.1.2 Spectrophotometer for use at 420 nm with light path of4 to 5 cm, and4.1.3 Filter photometer with a violet filter having a maxi-mum near 420 nm and a light path of 4 to 5 cm. Filterphotometers
8、and photometric practices prescribed in this testmethod shall conform to Practice E60; spectrophotometerpractices shall conform to Practice E 275.4.2 Stopwatch, readable to 0.1 minutes.4.3 Measuring Spoon, capacity 0.2 to 0.3 mL.4.4 Drying oven, capable of continuously heating at 110 65 C.4.5 Balanc
9、e, shall be capable of reproducing results within0.0002 g with an accuracy of 60.0002 g. Direct-readingbalances shall have a sensitivity not exceeding 0.0001 g.Conventional two-pan balances shall have a maximum sensi-bility reciprocal of 0.0003 g. Any rapid weighing device thatmay be provided, such
10、as a chain, damped motion, or heavyriders, shall not increase the basic inaccuracy by more than0.0001 g at any reading and with any load within the ratedcapacity of the balance.4.6 Stirrer, magnetic variable speed, with a TFE-fluorocarbon coated magnetic stirring rod or an overhead stirrerwith a pro
11、peller.5. Reagents and Materials5.1 Purity of ReagentsAll reagents shall conform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society.35.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water conformingto Speci
12、fication D 1193, Type I. Other reagent water types (SeeNote 1) may be used, provided it is first ascertained that the1This test method is under the jurisdiction of ASTM Committee C09 onConcrete andAggregates and is the direct responsibility of Subcommittee on C09.69Miscellaneous Tests.Current editio
13、n approved March 1, 2005. Published April 2005.2For referenced 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.3Reagent Chemi
14、cals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National
15、 Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.water is of sufficiently high purity to permit its use withoutadversely affecting the precision and bias of the tes
16、t method.NOTE 1Type II water was specified at the time of round robin testingof this test method.5.3 Barium ChlorideCrystals of barium chloride(BaCl22H2O) screened to 850 to 600 m. To prepare in thelaboratory, spread crystals over a large watch glass, desiccatefor 24 h, screen to remove any crystals
17、 that are not 850 to 600m, and store in a clean, dry jar.5.4 Conditioning ReagentPlace 30 mL of concentratedhydrochloric acid (HCl, sp gr 1.19), 300 mL reagent water, 100mL 95 % ethanol or isopropanol and 75 g sodium chloride(NaCl) in a container. Add 50 mL glycerol and mix.5.5 Sulfate Solution, Sta
18、ndard (1 mL = 0.100 mg SO4)Dissolve 0.1479 g of anhydrous sodium sulfate (Na2SO4)inwater, and dilute with water to 1 L in a volumetric flask.5.6 pH paper, readable to at least 0.5 pH units.5.7 Sodium Hydroxide, (0.1N)Dissolve4gofsodiumhydroxide (NaOH) in water and dilute with water to 1L5.8 Hydrochl
19、oric Acid (0.1N)Dilute 8.6 mL of concen-trated hydrochloric acid (HCl sp gr 1.19) to 1L with water6. Permissible Variations6.1 Both the referee method and qualified methods asdescribed in Test Methods C114are permissible as alternativesto the turbidimetric procedure.7. Calibration and Standardizatio
20、n7.1 Prepare standards by diluting 0.0, 2.0, 5.0, 10.0, 15.0,20.0, 30.0, and 40.0 mL of standard sulfate solution with waterto 100-mL volumes in volumetric flasks. These solutions willhave sulfate ion concentrations of 0.0, 2.0, 5.0, 10.0, 15.0, 20.0,30.0, and 40.0 mg/L, respectively. Follow the pro
21、cedure givenin Section 8 using appropriate amounts of the standard sulfatesolution prepared in accordance with 5.5 and prepare acalibration curve showing sulfate ion content in mg/L plottedagainst the corresponding photometer readings.7.2 A separate calibration curve must be prepared for eachphotome
22、ter and a new curve must be prepared if it is necessaryto change the cell, lamp, or filter, or if any other alterations ofinstrument or reagents are made. Check the curve with eachseries of tests by running two or more solutions of knownsulfate concentrations in the range of 5 to 40 mg SO4/L.NOTE 2T
23、he slope of the curve may not be linear below 5 or above 40mg SO4/L for this method.8. Procedure8.1 Collect at least 100 g of representative soil for analysis.Dry the sample for 18 to 24 h at 110 C. Crush to pass a 600m sieve. In a 400 mL beaker labeled Sample A, put a sampleconsisting of approximat
24、ely 30 g. In a second 400 mL beakerlabeled Sample B, place a sample of approximately 3 g. Recordthe mass of each sample to the nearest 0.001 g. Add 250 mL ofdeionized water to each beaker, and stir on a magnetic stirrerfor one h. Filter the extraction through two dry medium texturefilter papers unde
25、r suction. Do not wash the residue. Repeat thefiltration if solution is not clear. Check the pH of the filtrateusing pH paper and, if needed, neutralize each filtrate to pH of7 6 1 using either 0.1N HCl or 0.1N NaOH.8.2 Adjust the temperature of the solution in the volumetricflasks to between 20 and
26、 25 C 68 to 77 F.8.3 Use an aliquot of 10 mL for specimen A1, 20 mL forspecimenA2, 10 mL for specimen B1, and 20 mL for specimenB2. Dilute to a volume of 100 mL in a volumetric flask andfollow the procedure below or Test Methods C114. Pour the100 mL into a 250 mL beaker. Add 5.0 mL of conditioningre
27、agent. Mix by stirring with a stir bar and magnetic stirrer.Add 0.3 g of the prepared BaCl2crystals using a measuringspoon and start the timer.8.4 Stir exactly 1.0 min, at the same constant speed for alldeterminations.8.5 Remove the beaker from the stirrer, pour solution intothe cell, and put the ce
28、ll into the photometer. Record theturbidity at 4.0 min after pouring the solution into the cell.8.6 Determine the mg of SO4from the calibration curve.9. Calculation or Interpretation of Results9.1 Calculate the sulfate content (% by mass) for eachspecimen as follows:P 52.5*MA*W(1)Where:P =%SO4in dri
29、ed soilM = mg/L of SO4calculated from calibration curveW = mass of soil placed into 400 mL beaker, in gA = volume of aliquot specimen, in mL9.2 Limits of values for results to be valid. (See Note 3)Specimen Lower Limit Upper LimitA1 0.04% 0.33%A2 0.02% 0.17%B1 0.41% 3.33%B2 0.21% 1.67%1. Determine w
30、hich results fall within the above limits2. Discard those that do not3. Average all results that complyNOTE 3These values were derived from the limits on the sulfate testof 5 to 40 mg/L, and a solubility of sulfate of 1.6 g/Lat pH 7 when calciumsulfate is present. The method is not applicable for so
31、ils outside this range.For those samples, see the Annex.10. Report10.1 Report the average obtained as % sulfate by mass ofsample. If milligrams sulfate in kilograms of soil (mg SO4/kgsoil) is desired, multiply % sulfate by 10 000. Report results tonearest 0.01 % or 100 mg/kg.11. Precision and Bias11
32、.1 PrecisionThe standard deviation was found to varywith concentration, so therefore, a coefficient of variation wasused for the precision statement. The single operator coefficientof variation was found to be 4.4 %. Therefore, results of twoproperly conducted tests by the same operator on the samem
33、aterial should not differ by more than 12.4 % of theiraverage. The multilaboratory coefficient of variation was foundto be 21.2 %. Therefore, results of two different laboratories onC1580052identical samples of a material should not differ from eachother by more than 60 % of their average.11.2 BiasS
34、ince there is no accepted reference materialsuitable for determining bias, bias can not be determined.12. Keywords12.1 hydraulic cement; soil; Sulfate; turbidimeterANNEX(Mandatory Information)A1. REDUCING THE NUMBER OF SUB-SAMPLES AND SAMPLES OUT OF COMPLIANCEA1.1 This procedure was written to accom
35、modate labora-tories that are not familiar with the soil under test. If priorknowledge is available, a lesser number of sub-samples, and/ordilutions may be used.A1.2 If a sample falls above 3.33 % sulfate, then differentsample masses and/or dilutions can be used. If this procedureis followed, then t
36、he mg SO4from the turbidimeter readingshall be maintained within 5 to 40 mg/L. If another procedureis used, then validation shall be provided showing that theresults are within the linear range of the calibration.ASTM International takes no position respecting the validity of any patent rights asser
37、ted in connection with any item mentionedin this standard. Users of this standard are expressly advised 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
38、the responsible technical committee and must be reviewed every five years andif not revised, either reapproved 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 receiv
39、e 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 you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM Intern
40、ational, 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).C1580053
