1、Designation: D7262 10 (Reapproved 2016)1Standard Test Method forEstimating the Permanganate Natural Oxidant Demand ofSoil and Aquifer Solids1This standard is issued under the fixed designation D7262; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase of revision, the 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. Scope*1.1 This test method covers the estimation of the perman-ganate natural oxidant demand (PNOD
3、) through the determi-nation of the quantity of potassium permanganate (KMnO4)that organic matter and other naturally occurring oxidizablespecies present in soil or aquifer solids will consume underspecified conditions as a function of time. Oxidizable speciesmay include organic constituents and oxi
4、dizable inorganicions, such as ferrous iron and sulfides. The following testmethods are included:Test Method A48-hour Permanganate Natural OxidantDemandTest Method BPermanganate Natural Oxidant DemandKinetics1.2 This test method is limited by the reagents employed toa permanganate natural oxidant de
5、mand (PNOD) of 60 gKMnO4per kg soil or aquifer solids after a period of 48 hours(Method A) or two weeks (Method B).1.3 All observed and calculated values shall conform to theguidelines for significant digits and rounding established inPractice D6026.1.4 UnitsThe values stated in SI units are to be r
6、egardedas standard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to interpret the results ofthe data. It is the responsibility of the user of this standard tointerpret the results obtained and to determine the applicabilityof these results prior to us
7、e.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 determine the applica-bility of regulatory limitations prior to use.2. Referenced
8、 Documents2.1 ASTM Standards:2D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1193 Specification for Reagent WaterD3740 Practice for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionD4753 Guide for Evalua
9、ting, Selecting, and Specifying Bal-ances and Standard Masses for Use in Soil, Rock, andConstruction Materials TestingD6026 Practice for Using Significant Digits in GeotechnicalDataD6051 Guide for Composite Sampling and Field Subsam-pling for Environmental Waste Management ActivitiesD6169 Guide for
10、Selection of Soil and Rock SamplingDevices Used With Drill Rigs for Environmental Investi-gationsD6282 Guide for Direct Push Soil Sampling for Environ-mental Site CharacterizationsD6286 Guide for Selection of Drilling Methods for Environ-mental Site Characterization2.2 Other Standards:3Method 4500KM
11、nO4Standard Methods for the Examina-tion of Water and Wastewater, 20th Ed. 1998ANSI/AWWA B603-03 Standard for Permanganates3. Terminology3.1 For common definitions of technical terms in thisstandard, refer to Terminology D653.3.2 Definitions of Terms Specific to This Standard:3.2.1 permanganate natu
12、ral oxidant demand (PNODt)themass of potassium permanganate consumed per mass of soil oraquifer solids as a function of time.1This test method is under the jurisdiction ofASTM Committee D18 on Soil andRock and is the direct responsibility of Subcommittee D18.21 on Groundwater andVadose Zone Investig
13、ations.Current edition approved July 15, 2016. Published August 2016. Originallyapproved in 2007. Last previous edition approved in 2010 as D726210. DOI:10.1520/D7262-10R16E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. Fo
14、r Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American Water Works Association (AWWA), 6666 W. QuincyAve., Denver, CO 80235, http:/www.awwa.org.*A Summary of Changes section appears at the end of this standardCopyri
15、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.2 maximum permanganate natural oxidant demand(PNODmax)the maximum mass of potassium permanganateconsumed per mass of soil or aquifer solids over time.3.2.3 permanganate natural oxidant dem
16、and kineticstherate at which potassium permanganate is consumed by soil oraquifer solids.4. Summary of Test Method4.1 Many organic and reduced inorganic substances presentin soil and aquifer solids can be oxidized by permanganate. Astandard potassium permanganate solution is added to aspecific amoun
17、t of soil or aquifer solids and allowed to reactfor a period of 48 hours (Method A) or two weeks (Method B).The residual permanganate concentration is measured at pre-scribed sampling times and the difference in concentration isused to calculate the PNODtat that time.4.2 Many organic and reduced ino
18、rganic substances presentin soil and aquifer solids can be oxidized by permanganate.However, some organic compounds react slowly and may notbe completely oxidized within the test period while others mayresist oxidation altogether.5. Significance and Use5.1 The test method is used to estimate the per
19、manganatenatural oxidant demand exerted by the soil or aquifer solids bydetermining the quantity of potassium permanganate that isconsumed by naturally occurring species as a function of time.Typically the measurement of PNOD is used to screen potentialsites for in situ chemical oxidation (ISCO) wit
20、h permanganate(Test Method A) and provide information to aid in the designof remediation systems (Test Method B).5.2 While some oxidizable species react relatively quickly(that is, days to weeks), others react more slower (weeks tomonths). Consequently, the PNODtis expected to be somefraction of the
21、 PNODmax.5.3 Due to mass transport related issues at the field-scale itis reasonable to assume that the PNODtmeasured using the testmethod may overestimate the demand exerted during ISCOapplications.NOTE 1The quality of the result produced by this standard isdependent on the competence of the person
22、nel performing it, and thesuitability of the equipment and facilities used. Agencies that meet thecriteria of Practice D3740 are generally considered capable of competentand objective testing/sampling/inspection/and so forth.6. Interferences6.1 Manganese oxides produced as a result of permanganatere
23、duction may interfere with the analysis of permanganate(Method 4500-KMnO4).7. Apparatus7.1 Reactor ApparatusA 250-mL glass vial (borosilicateglass or equivalent) with an oxidant resistant screw cap isrecommended. Zero headspace is not required.7.2 Apparatus for Drying SamplesA laboratory oven ca-pab
24、le of delivering sufficient controlled heat to maintain atemperature of 105C (610C).7.3 Balance ScalesA balance having a minimum capacityof 100 g and meeting the requirements of Guide D4753,readable (with no estimation) to 0.1 % of the test mass orbetter.8. Hazards8.1 When performing laboratory anal
25、ysis and handlingchemicals, safety is a critical component. For this procedure,contact lenses may not be worn. Recommended personalprotective equipment (PPE) for this procedure includes rubbergloves, safety glasses or goggles and a lab coat or rubber apron.8.2 In the event of any chemical spill, ref
26、er to the specificMSDS for a proper clean-up procedure. In the case of solidpotassium permanganate, sweep the solid into a clean containerand dispose according to state and local regulations. A potas-sium permanganate spill should be diluted with water to lessthan 4 % strength, collected and dispose
27、d of in an approvedmanner. Paper or cloth towels should not be used to clean anypermanganate spill.8.3 Excess permanganate solutions can also be neutralizedby sodium thiosulfate, citric acid, or other reducing agents.Solution concentrations must be less than 4 % prior to additionof any reducing agen
28、t. Excess heat can be generated and thereis a potential for an unwanted reaction.49. Sampling9.1 Collect the sample(s) in accordance with PracticesD6051, D6169, D6282,orD6286.Aminimum of 600 grams ofsoil or aquifer solids is required from each sampling location.9.2 Samples can be preserved at 4C for
29、 up to 28 days.However, it is the responsibility of the users of the test methodto ensure the maximum holding time for their samples.TEST METHOD A48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND10. Scope10.1 The test method is appropriate for the determination ofthe 48-hour permanganate natural oxidant d
30、emand of soil andaquifer solids. The test is designed to be used for site screeningpurposes only. Research has shown that a large percentage ofthe total permanganate natural oxidant demand can be ex-pressed after a period of 48 hours. Consequently, this testmethod should not be used to determine the
31、 mass of oxidant4Additional references on general laboratory safety and procedures can be foundat: http:/www.ceet.niu.edu/labs/safety.html, http:/keats.admin.virginia.edu/lsm/home.html, and http:/www.ehs.iupui.edu/ehs/prog_chemlabsafety.asp.D7262 10 (2016)12required for the treatment of hazardous wa
32、ste sites beingconsidered for ISCO with permanganate.11. Summary of Test Method11.1 The sample and permanganate solutions are analyzedfor permanganate after a 48-hour reaction period.12. Reagents and Materials12.1 Purity of ReagentsReagent grade chemicals shall beused.12.2 Purity of WaterReference t
33、o water shall be under-stood to mean reagent grade water that meets the purityspecifications of Type I or Type II water according to Specifi-cation D1193.12.3 Potassium Permanganate Stock Solution (20 000 mg/L)Dissolve 20.0 g of potassium permanganate (KMnO4)inwater and dilute to 1 L. Mix the stock
34、solution for a minimumof two hours to make certain the KMnO4crystals havecompletely dissolved.NOTE 2In place of potassium permanganate, sodium permanganatecan be used. However, since the concentration of a commercially availableNaMnO4solution may vary, standardization is required. This may beaccompl
35、ished using ANSI/AWWA B603-03.13. Procedure13.1 Dry each sample in the laboratory oven at 105C(610C) for a period of 24 h.13.2 Homogenize the dried sample by gently mixing byhand. If large stones or rocks are present they should beremoved prior to analysis using a No. 10 U.S. standard meshsieve (2.0
36、0 mm).13.3 Place 100 mL of 20 000 mg/L KMnO4stock solutionin a 250 mL glass vial for the blank determination.13.4 Place 50 g of dried sample in each of three 250 mLglass vials (each experiment is run in triplicate).13.5 Place 100 mL of 20 000 mg/L KMnO4stock solutionin each of the three 250 mL glass
37、 vials containing the driedsample. Seal each of the vials and invert once to mix thereagents. Store vials at room temperature (20-22C).13.6 Sample each vial at 48 hours by removinga1mLsample aliquot. A centrifuge or oxidant resistant filter (20 m)should be used to remove manganese oxides from the sa
38、mpleprior to analysis using Method 4500KMnO4.14. Calculations14.1 PNODtvalues are expressed in units of mass ofpotassium permanganate per mass of dry aquifer solids usingthe following equation:PNODt5VKMnO4#02 KMnO4#t!msoil(1)where:PNODt= permanganate natural oxidant demand at time= t (g KMnO4/kg soi
39、l or aquifer solids),V = volume of the aqueous phase (L),KMnO40= initial potassium permanganate concentration(g/L),KMnO41= potassium permanganate concentration (g/L) attime = t, andmsoil= mass of dry soil or aquifer solids (kg).15. Precision and Bias15.1 PrecisionTest data on precision is not presen
40、ted dueto the nature of the soil and aquifer solids used by this testmethod. It is either not feasible or too costly at this time to haveten or more laboratories participate in a round-robin testingprogram. Also, it is either not feasible or too costly to producemultiple specimens that have uniform
41、physical properties. Anyvariation observed in the data is just as likely to be due tospecimen variation as to operator or laboratory testing varia-tion.15.2 The Subcommittee D18.21 is seeking any data fromthe users of this test method that might be used to make alimited statement on precision.15.3 B
42、iasThere is no accepted reference value for this testmethod, therefore, bias cannot be determined.TEST METHOD BPERMANGANATE NATURAL OXIDANT DEMAND KINETICS16. Scope16.1 The test method is appropriate for the determination ofthe permanganate natural oxidant demand kinetics for soil andaquifer solids.
43、 A curve fitting software package can be used todetermine best-fit curves and kinetic parameters for each dataset using the independent first-order model described below.The curve fitting software can also be used to predict thePNODmaxof the soil or aquifer solids based on the kinetic data.17. Summa
44、ry of Test Method17.1 The sample and permanganate solutions are analyzedfor permanganate after reaction periods of 1, 3, 7, 24, 48, 168,and 336 hours.18. Apparatus18.1 Reactor ApparatusA 250-mL glass vial (Pyrex orequivalent) with an oxidant resistant screw cap is recom-mended. Zero headspace is not
45、 required.18.2 Apparatus for Drying SampleA laboratory ovencapable of delivering sufficient controlled heat to maintain atemperature of 105C (610C).18.3 Balances/ScalesAbalance having a minimum capac-ity of 100g and meeting the requirements of Guide D4753,readable (with no estimation) to 0.1 % of th
46、e test mass orbetter.D7262 10 (2016)1319. Reagents and Materials19.1 Purity of ReagentsReagent grade chemicals shall beused.19.2 Purity of WaterReference to water shall be under-stood to mean reagent grade water that meets the purityspecifications of Type I or Type II water according to Specifi-cati
47、on D1193.19.3 Potassium Permanganate Stock Solution (30 000 mg/L)Dissolve 30.0 g of potassium permanganate (KMnO4)inwater and dilute to 1 L. Mix the stock solution for a minimumof two hours to make certain the KMnO4crystals havecompletely dissolved.19.4 Potassium Permanganate Stock Solution (20 000
48、mg/L)Dilute 333.3 mL of 30 000 mg/L potassium permanganatestock solution to 500 mL.19.5 Potassium Permanganate Stock Solution (10 000 mg/L)P Dilute 166.7 mL of 30 000 mg/L potassium perman-ganate stock solution to 500 mL.20. Procedure20.1 Dry each sample in the laboratory oven at 105C(610C) for a pe
49、riod of 24 h.20.2 Homogenize the dried sample by gently mixing byhand. If large stones or rocks are present they should beremoved prior to analysis using a No. 10 U.S. standard meshsieve (2.00 mm).20.3 Place 100 mL of 30 000 mg/L KMnO4stock solutionin a 250 mL glass vial for the blank determination.20.4 Place 50 g of dried sample in each of three 250 mLglass vials (each experiment is run in triplicate).20.5 Place 100 mL of 30 000 mg/L KMnO4stock solutionin each of the three 250 mL glass vials containing the driedsample. Seal ea
