1、Designation: C1580 091Standard Test Method forWater-Soluble Sulfate in Soil1This standard is issued under the fixed designation C1580; 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 parenthes
2、es indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEAdded research report information to Section 11 editorially in September 2010.1. Scope*1.1 This test method is for the determination of water-soluble sulfate in
3、soils.1.2 This test method was developed for concentrations ofwater-soluble sulfate 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 t
4、o the sampler and laboratoryto comply with all regulations.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is there
5、sponsibility of the user of this standard to establish appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C114 Test Methods for Chemical Analysis of HydraulicCementD1193 Specification for Reagen
6、t WaterE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecular Absorption SpectrometryE275 Practice for Describing and Measuring Performanceof Ultraviolet and Visible Spectrophotometers3. Significance and Use3.1 This test method can be used to determine if soils couldhave an adv
7、erse reaction with hydraulic cement concrete.4. Apparatus4.1 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 42
8、0 nm and a light path of 4 to 5 cm. Filterphotometers and photometric practices prescribed in this testmethod shall conform to Practice E60; spectrophotometerpractices shall conform to Practice E275.4.2 Stopwatch, readable to 0.1 minutes.4.3 Measuring Spoon, capacity 0.2 to 0.3 mL.4.4 Drying oven, c
9、apable of continuously heating at 110 65 C.4.5 Balance, 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.
10、 Any rapid weighing device thatmay be provided, such 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 m
11、agnetic stirring rod or an overhead stirrerwith a propeller.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 b
12、e understood to mean reagent water conformingto Specification D1193, 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 and Concrete Aggregates and is the direct responsibili
13、ty of Subcommitteeon C09.69 Miscellaneous Tests.Current edition approved April 1, 2009. Published May 2009. Originallyapproved in 2005. Last previous edition approved in 2005 as C1580 05. DOI:10.1520/C1580-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custom
14、er Service at serviceastm.org. For 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 notli
15、sted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of this standard.C
16、opyright 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 test method.NOTE 1Type II water was specified at the time of round robin te
17、stingof 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 that are not 850 to 600m, and store in a clean, dry jar.5.4 Conditionin
18、g 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, Standard (1 mL = 0.100 mg SO4)Dissolve 0.1479 g of anhydrous sodium sulfate
19、 (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 Hydrochloric Acid (0.1N)Dilute 8.6 mL of concen-trated hydrochloric acid (HCl sp
20、 gr 1.19) to 1L with water6. Permissible Variations6.1 Both the referee method and qualified methods asdescribed in Test Methods C114 are permissible as alternativesto the turbidimetric procedure.7. Calibration and Standardization7.1 Prepare standards by diluting 0.0, 2.0, 5.0, 10.0, 15.0,20.0, 30.0
21、, 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 procedure givenin Section 8 using appropriate amounts of the standard sulf
22、atesolution 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 eachphotometer and a new curve must be prepared if it is necessaryto change the ce
23、ll, 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 2The slope of the curve may not be linear below 5 or above 40mg SO4/L for
24、 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 approximately 30 g. In a second 400 mL beakerlabeled Sample B, place a sample of
25、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 at least 1.0 h but no more than 1.2 h. Filter the extractionthrough two dry medium texture filter papers under suction. Donot wash the residue. Repe
26、at the filtration if solution is notclear. Check the pH of the filtrate using pH paper and, ifneeded, neutralize each filtrate to pH of 7 6 1 using either 0.1NHCl or 0.1N NaOH.8.2 Adjust the temperature of the solution in the volumetricflasks to between 20 and 25 C 68 to 77 F.8.3 Use an aliquot of 1
27、0 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 conditioningreagent. Mix by stirring with a stir bar a
28、nd 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 cell into the photometer. Record theturbid
29、ity 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 dried soilM = mg/L of SO4calculated from ca
30、libration 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 which results fall within the above limit
31、s2. 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 soils outside this range.For those samples
32、, 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 Bias411.1 PrecisionThe standard deviation was
33、found to varywith concentration, so therefore, a coefficient of variation wasused for the precision statement. The single operator coefficient4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:C09-1029.C1580 0912of variation was fo
34、und to be 4.4 %. Therefore, results of twoproperly conducted tests by the same operator on the samematerial 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 onidentical samples
35、of a material should not differ from eachother by more than 60 % of their average.11.2 BiasSince 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
36、 NUMBER OF SUB-SAMPLES AND SAMPLES OUT OF COMPLIANCEA1.1 This procedure was written to accommodate 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, th
37、en differentsample masses and/or dilutions can be used. If this procedureis followed, then the 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 calibra
38、tion.SUMMARY OF CHANGESCommittee C09 has identified the location of selected changes to this test method since the last issue,C1580 05, that may impact the use of this test method. (Approved April 1, 2009)(1) Revised 8.1.ASTM International takes no position respecting the validity of any patent righ
39、ts 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 rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any
40、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 revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments wil
41、l 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 you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by AST
42、M 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/).C1580 0913
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