1、Designation: C 1580 09Standard 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 () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 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 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 theresponsibility of the user of this standard to establish appro-priate safety and hea
5、lth practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C114 Test Methods for Chemical Analysis of HydraulicCementD 1193 Specification for Reagent WaterE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecul
6、ar Absorption SpectrometryE 275 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 adverse reaction with hydraulic cement concrete.4. Apparatus4.1 PhotometerOne of th
7、e 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 and photometric practices
8、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 Balance, shall be capable of rep
9、roducing 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 as a chain, damped motion,
10、 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 propeller.5. Reagents and Mat
11、erials5.1 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 Specification D 1193, Type I. O
12、ther 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 responsibility of Subcommitteeon C09.69 Miscellaneous Tests.Current edition approved April
13、 1, 2009. Published May 2009. Originallyapproved in 2005. Last previous edition approved in 2005 as C 1580 05.2For 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 st
14、andards 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 Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Pool
15、e, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
16、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 testingof this test method.5.3 Barium ChlorideCrystals of barium chloride(BaCl22H2O) screened to 850
17、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 Conditioning ReagentPlace 30 mL of concentratedhydrochloric acid (HCl, sp gr 1.19), 300 mL reagent water, 100m
18、L 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 (Na2SO4)inwater, and dilute with water to 1 L in a volumetric flask.5.6 pH paper, readable to at l
19、east 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 gr 1.19) to 1L with water6. Permissible Variations6.1 Both the referee method and qualified method
20、s asdescribed in Test Methods C114are 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, and 40.0 mL of standard sulfate solution with waterto 100-mL volumes in volumetric flasks. These s
21、olutions 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 sulfatesolution prepared in accordance with 5.5 and prepare acalibration curve showing sulfate ion conte
22、nt 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 cell, lamp, or filter, or if any other alterations ofinstrument or reagents are made. Check the curve
23、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 this method.8. Procedure8.1 Collect at least 100 g of representative soil for analysis.Dry the samp
24、le 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 approximately 3 g. Recordthe mass of each sample to the nearest 0.001 g. Add 250 mL ofdeionized wate
25、r 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. Repeat the filtration if solution is notclear. Check the pH of the filtrate using pH paper and, ifneeded
26、, 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 10 mL for specimen A1, 20 mL forspecimenA2, 10 mL for specimen B1, and 20 mL for specimenB2. Dilute t
27、o 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 and magnetic stirrer.Add 0.3 g of the prepared BaCl2crystals using a measuringspoon and start the tim
28、er.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 theturbidity at 4.0 min after pouring the solution into the cell.8.6 Determine the mg of SO4from the calibrat
29、ion 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 calibration curveW = mass of soil placed into 400 mL beaker, in gA = volume of aliquot specimen, in mL
30、9.2 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 limits2. Discard those that do not3. Average all results that complyNOTE 3These values were derived from
31、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, see the Annex.10. Report10.1 Report the average obtained as % sulfate by mass ofsample. If milligr
32、ams 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 Bias11.1 PrecisionThe standard deviation was found to varywith concentration, so therefore, a coefficient of variation wasused for the precision s
33、tatement. The single operator coefficientof variation was found 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 foundC1580092to be 21.2 %. T
34、herefore, results of two different laboratories onidentical samples 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; soi
35、l; Sulfate; turbidimeterANNEX(Mandatory Information)A1. REDUCING THE 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/ord
36、ilutions 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 the mg SO4from the turbidimeter readingshall be maintained within 5 to 40 mg/L. If another procedureis used, then validation shall be provide
37、d showing that theresults are within the linear range of the calibration.SUMMARY OF CHANGESCommittee C09 has identified the location of selected changes to this test method since the last issue,C 1580 05, that may impact the use of this test method. (Approved April 1, 2009)(1) Revised 8.1.ASTM Inter
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41、dards, 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).C1580093
