1、Designation: C1580 091C1580 15Standard 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 p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEAdded research report information to Section 11 editorially in September 2010.1. Scope*1.1 This test method is for the determination of water-soluble su
3、lfate in soils.1.2 This test method was developed for concentrations of water-soluble sulfate in soils between 0.02 and 3.33 % sulfate bymass.1.3 This test method does not determine sulfur in any form except as sulfate.1.4 Some governing bodies regulate the movement of soils from one area to another
4、. It is up to the sampler and laboratory tocomply with all regulations.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its u
5、se. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C125 Terminology Relating to Concrete and Concrete AggregatesC114 Test Met
6、hods for Chemical Analysis of Hydraulic CementD1193 Specification for Reagent WaterE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers3. Terminology3.1 For definition
7、s of terms used in this test method, refer to Terminology C125.4. Significance and Use4.1 This test method can be used to determine if soils could have an adverse reaction with hydraulic cement concrete.5. Apparatus5.1 PhotometerOne of the following, given in order of preference:5.1.1 Nephelometer o
8、r turbidimeter,5.1.2 Spectrophotometer for use at 420 nm with light path of 4 to 5 cm, and5.1.3 Filter photometer with a violet filter having a maximum near 420 nm and a light path of 4 to 5 cm. Filter photometersand photometric practices prescribed in this test method shall conform to Practice E60;
9、 spectrophotometer practices shall conformto Practice E275.5.2 Stopwatch, readable to 0.1 minutes.1 This test method is under the jurisdiction of ASTM Committee C09 on Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee C09.69 onMiscellaneous Tests.Current edition appro
10、ved April 1, 2009Oct. 1, 2015. Published May 2009December 2015. Originally approved in 2005. Last previous edition approved in 20052010 asC1580 05.C1580 091. DOI: 10.1520/C1580-09E01.10.1520/C1580-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service
11、 at serviceastm.org. ForAnnual Book ofASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous ver
12、sion. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes sec
13、tion appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Measuring Spoon, capacity 0.2 to 0.3 mL.5.4 Drying oven, capable of continuously heating at 110 6 5 C.5.5 Balance, shall be capable of reprodu
14、cing results within 0.0002 g with an accuracy of 60.0002 g. Direct-reading balancesshall have a sensitivity not exceeding 0.0001 g. Conventional two-pan balances shall have a maximum sensibility reciprocal of0.0003 g. Any rapid weighing device that may be provided, such as a chain, damped motion, or
15、 heavy riders, shall not increasethe basic inaccuracy by more than 0.0001 g at any reading and with any load within the rated capacity of the balance.5.6 Stirrer, magnetic variable speed, with a TFE-fluorocarbon coated magnetic stirring rod or an overhead stirrer with apropeller.6. Reagents and Mate
16、rials6.1 Purity of ReagentsAll reagents shall conform to the specifications of the Committee on Analytical Reagents of theAmerican Chemical Society.36.2 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water conforming toSpecification D1193, Type I. O
17、ther reagent water types (See Note 1) may be used, provided it is first ascertained that the wateris of sufficiently high purity to permit its use without adversely affecting the precision and bias of the test method.NOTE 1Type II water was specified at the time of round robin testing of this test m
18、ethod.6.3 Barium ChlorideCrystals of barium chloride (BaCl22H2O) screened to 850 to 600 m. To prepare in the laboratory,spread crystals over a large watch glass, desiccate for 24 h, screen to remove any crystals that are not 850 to 600 m, and storein a clean, dry jar.6.4 Conditioning ReagentPlace 30
19、 mL of concentrated hydrochloric acid (HCl, sp gr 1.19), 300 mL reagent water, 100 mL95 % ethanol or isopropanol and 75 g sodium chloride (NaCl) in a container. Add 50 mL glycerol and mix.6.5 Sulfate Solution, Standard (1 mL = 0.100 mg SO4)Dissolve 0.1479 g of anhydrous sodium sulfate (Na2SO4) in wa
20、ter, anddilute with water to 1 L in a volumetric flask.6.6 pH paper, readable to at least 0.5 pH units.6.7 Sodium Hydroxide, (0.1N)Dissolve 4 g of sodium hydroxide (NaOH) in water and dilute with water to 1L6.8 Hydrochloric Acid (0.1N)Dilute 8.6 mL of concentrated hydrochloric acid (HCl sp gr 1.19)
21、to 1L with water7. Permissible Variations7.1 Both the referee method and qualified methods as described in Test Methods C114 are permissible as alternatives to theturbidimetric procedure.8. Calibration and Standardization8.1 Prepare standards by diluting 0.0, 2.0, 5.0, 10.0, 15.0, 20.0, 30.0, and 40
22、.0 mL of standard sulfate solution with water to100-mL volumes in volumetric flasks. These solutions will have 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 given in Section 89 using appropriate amounts of the standard sulfate s
23、olutionprepared in accordance with 5.56.5 and prepare a calibration curve showing sulfate ion content in mg/L plotted against thecorresponding photometer readings.8.2 A separate calibration curve must be prepared for each photometer and a new curve must be prepared if it is necessary tochange the ce
24、ll, lamp, or filter, or if any other alterations of instrument or reagents are made. Check the curve with each series oftests by running two or more solutions of known sulfate 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 40 mg SO4/L
25、for this method.9. Procedure9.1 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 600 msieve. In a 400 mL beaker labeled Sample A, put a sample consisting of approximately 30 g. In a second 400 mL beaker labeledSample B, place a sampl
26、e of approximately 3 g. Record the mass of each sample to the nearest 0.001 g. Add 250 mL of deionizedwater to each beaker, and stir on a magnetic stirrer for at least 1.0 h but no more than 1.2 h. Filter the extraction through two drymedium texture filter papers under suction. Do not wash the resid
27、ue. Repeat the filtration if solution is not clear. Check the pHof the filtrate using pH paper and, if needed, neutralize each filtrate to pH of 7 6 1 using either 0.1N HCl or 0.1N NaOH.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For sugg
28、estions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.C1580 1529.2 Adjust the te
29、mperature of the solution in the volumetric flasks to between 20 and 25 C 68 to 77 F.9.3 Use an aliquot of 10 mL for specimen A1, 20 mL for specimen A2, 10 mL for specimen B1, and 20 mL for specimen B2.Dilute to a volume of 100 mL in a volumetric flask and follow the procedure below or Test Methods
30、C114. Pour the 100 mL intoa 250 mLbeaker.Add 5.0 mLof conditioning reagent. Mix by stirring with a stir bar and magnetic stirrer.Add 0.3 g of the preparedBaCl2 crystals using a measuring spoon and start the timer.9.4 Stir exactly 1.0 min, at the same constant speed for all determinations.9.5 Remove
31、the beaker from the stirrer, pour solution into the cell, and put the cell into the photometer. Record the turbidityat 4.0 min after pouring the solution into the cell.9.6 Determine the mg of SO4 from the calibration curve.10. Calculation or Interpretation of Results10.1 Calculate the sulfate conten
32、t (% by mass) for each specimen as follows:P 52.5*MA*W (1)where:P = % SO4 in dried soilM = mg/L of SO4 calculated from calibration curveW = mass of soil placed into 400 mL beaker, in gA = volume of aliquot specimen, in mL10.2 Limits of values for results to be valid. (See Note 3)Specimen Lower Limit
33、 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 the limits on the sulfate test of 5 to 40 mg/L, and a solubility of sulfate of
34、 1.6 g/L at pH 7 when calciumsulfate is present. The method is not applicable for soils outside this range. For those samples, see the Annex.11. Report11.1 Report the average obtained as % sulfate by mass of sample. If milligrams sulfate in kilograms of soil (mg SO4/kg soil)is desired, multiply % su
35、lfate by 10 000. Report results to nearest 0.01 % or 100 mg/kg.12. Precision and Bias412.1 PrecisionThe standard deviation was found to vary with concentration, so therefore, a coefficient of variation was usedfor the precision statement. The single operator coefficient of variation was found to be
36、4.4 %. Therefore, results of two properlyconducted tests by the same operator on the same material should not differ by more than 12.4 % of their average. Themultilaboratory coefficient of variation was found to be 21.2 %. Therefore, results of two different laboratories on identical samplesof a mat
37、erial should not differ from each other by more than 60 % of their average.12.2 BiasSince there is no accepted reference material suitable for determining bias, bias can not be determined.13. Keywords13.1 hydraulic cement; soil; Sulfate; turbidimeter4 Supporting data have been filed at ASTM Internat
38、ional Headquarters and may be obtained by requesting Research Report RR:C09-1029. Contact ASTM CustomerService at serviceastm.org.C1580 153ANNEX(Mandatory Information)A1. REDUCING THE NUMBER OF SUB-SAMPLES AND SAMPLES OUT OF COMPLIANCEA1.1 This procedure was written to accommodate laboratories that
39、are not familiar with the soil under test. If prior knowledge isavailable, a lesser number of sub-samples, and/or dilutions may be used.A1.2 If a sample falls above 3.33 % sulfate, then different sample masses and/or dilutions can be used. If this procedure isfollowed, then the mg SO4 from the turbi
40、dimeter reading shall be maintained within 5 to 40 mg/L. If another procedure is used,then validation shall be provided showing that the results are within the linear range of the calibration.SUMMARY OF CHANGESCommittee C09 has identified the location of selected changes to this test method since th
41、e last issue,C1580 05C1580 091, that may impact the use of this test method. (Approved Oct. 1, 2015April 1, 2009.).)(1) Revised Added Section 8.13.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users o
42、f 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 the responsible technical committee and must be reviewed every fiv
43、e 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 receive careful consideration at a meeting of theresponsible technical co
44、mmittee, 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
45、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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 154
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