1、Designation: D 7262 07Standard Test Method forEstimating the Permanganate Natural Oxidant Demand ofSoil and Aquifer Solids1This standard is issued under the fixed designation D 7262; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses 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 covers the estimation of the perman-ganate natural oxidant demand (PNOD) through the det
3、ermi-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 oxidizable inorganic
4、ions, 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 demand (PNOD) of 60
5、 gKMnO4 per 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 D 6026.1.4 UnitsThe values stated in SI units are to be regardedas stand
6、ard. 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 use.1.6 This stan
7、dard 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 Documents2.1 A
8、STM Standards:2D 1193 Specification for Reagent WaterD 3740 Practice for Minimum Requirements for AgenciesEngaged in the Testing and/or Inspection of Soil and Rockas Used in Engineering Design and ConstructionD 4753 Guide for Evaluating, Selecting, and SpecifyingBalances and Standard Masses for Use
9、in Soil, Rock, andConstruction Materials TestingD 6026 Practice for Using Significant Digits in Geotechni-cal DataD 6051 Guide for Composite Sampling and Field Subsam-pling for Environmental Waste Management ActivitiesD 6169 Guide for Selection of Soil and Rock SamplingDevices Used With Drill Rigs f
10、or Environmental Investi-gationsD 6282 Guide for Direct Push Soil Sampling for Environ-mental Site CharacterizationsD 6286 Guide for Selection of Drilling Methods for Envi-ronmental Site Characterization2.2 Other Standards:3Method 4500KMnO4Standard Methods for the Exami-nation of Water and Wastewate
11、r, 20th Ed. 1998ANSI/AWWA B603-03. Standard for Permanganates3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 permanganate natural oxidant demand (PNODt)themass of potassium permanganate consumed per mass of soil oraquifer solids as a function of time.3.1.2 maximum permanganate
12、 natural oxidant demand(PNODmax)the maximum mass of potassium permanganateconsumed per mass of soil or aquifer solids over time.3.1.3 permanganate natural oxidant demand kineticstherate at which potassium permanganate is consumed by soil oraquifer solids.1This test method is under the jurisdiction o
13、fASTM Committee D18 on Soil andRock and is the direct responsibility of Subcommittee D18.21 on Ground Water andVadose Zone Investigations.Current edition approved June 15, 2007. Published August 2007.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
14、e at serviceastm.org. For 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.1Copyright ASTM International, 100 Barr Harbor
15、Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 amount of soil or aquifer
16、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 inorganic substances pre
17、sentin 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 permanganatenatural oxid
18、ant 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) with permanganate(Test M
19、ethod 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 PNODmax.5.3 Due to m
20、ass 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 personnel performing it, an
21、d thesuitability of the equipment and facilities used. Agencies that meet thecriteria of Practice D 3740 are generally considered capable of competentand objective testing/sampling/inspection/and so forth.6. Interferences6.1 Manganese oxides produced as a result of permanganatereduction may interfer
22、e with the analysis of permanganate(Method 4500-KMnO4).7. Apparatus7.1 Reactor ApparatusA 250 mL glass vial (Pyrex orequivalent) with an oxidant resistant screw cap is recom-mended. Zero headspace is not required.7.2 Apparatus for Drying SamplesA laboratory ovencapable of delivering sufficient contr
23、olled heat to maintain atemperature of 105C.7.3 Balance ScalesA balance having a minimum capacityof 100g and meeting the requirements of Guide D 4753,readable (with no estimation) to 0.1 % of the test mass orbetter.8. Hazards8.1 When performing laboratory analysis and handlingchemicals, safety is a
24、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, refer to the specificMSDS for a proper clea
25、n-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 disposed of in an approvedmanner. Paper or clot
26、h 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 agent. Excess heat can be generated and ther
27、eis a potential for an unwanted reaction.49. Sampling9.1 Collect the sample(s) in accordance with PracticesD 6051, D 6169, D 6282,orD 6286.Aminimum of 600 gramsof soil or aquifer solids is required from each samplinglocation.9.2 Samples can be preserved at 4C for up to 28 days.However, it is the res
28、ponsibility of the users of the test methodto ensure the maximum holding time for their samples.4Additional 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/pr
29、og_chemlabsafety.asp.D7262072TEST METHOD A48-HOUR PERMANGANATE NATURAL OXIDANT DEMAND10. Scope10.1 The test method is appropriate for the determination ofthe 48-hour permanganate natural oxidant demand of soil andaquifer solids. The test is designed to be used for site screeningpurposes only. Resear
30、ch 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 mass of oxidantrequired for the treatment of hazardous waste sites beingconsidered for ISCO with perman
31、ganate.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 to water shall be under-stood to mean reagent g
32、rade water that meets the purityspecifications of Type I or Type II water according to Specifi-cation D 1193.12.3 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 solution for a minimumof 2 hours to make cert
33、ain the KMnO4crystals have com-pletely dissolved.NOTE 2In place of potassium permanganate, sodium permanganatecan be used. However, since the concentration of a commercially availableNaMnO4 solution may vary, standardization is required. This may beaccomplished using ANSI/AWWA B603-03.13. Procedure1
34、3.1 Dry each sample in the laboratory oven at 105C for aperiod of 24 hours.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 (2.00 mm).13.3 Place 100 ml of 20 000 mg/l KMnO4sto
35、ck solution ina 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 KMnO4 stock solution ineach of the three 250 ml glass vials containing the driedsample. Seal each o
36、f the vials and invert once to mix thereagents. Store vials at room temperature (2022C).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 sampleprior to analysis using Method 4500KMnO4.14
37、. Calculations14.1 PNODtvalues are expressed in units of mass ofpotassium permanganate per mass of dry aquifer solids usingthe following equation:PNODt5VKMnO4#0KMnO4#t!msoil(1)where:PNODt= permanganate natural oxidant demand at time= t (g KMnO4/kg soil or aquifer solids),V = volume of the aqueous ph
38、ase (l),KMnO40= initial potassium permanganate concentration(g/l),KMnO41= potassium permanganate concentration (g/l)at time = t, andmsoil= mass of dry soil or aquifer solids (kg).15. Precision and Bias15.1 PrecisionTest data on precision is not presented dueto the nature of the soil and aquifer soli
39、ds 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 physical properties. Anyvariation observed in the
40、 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 BiasThere is no accepted reference value for this
41、testmethod, therefore, bias cannot be determined.D7262073TEST 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. A curve fitting software package can be
42、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. Summary of Test Method17.1 The sample and perm
43、anganate 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 required.18.2 Apparatus for Drying Sampl
44、eA laboratory ovencapable of delivering sufficient controlled heat to maintain atemperature of 105C.18.3 Balances/ScalesAbalance having a minimum capac-ity of 100g and meeting the requirements of Guide D 4573,readable (with no estimation) to 0.1% of the test mass or better.19. Reagents and Materials
45、19.1 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-cation D 1193.19.3 Potassium Permanganate Stock Solution (30 000 mg/
46、L)Dissolve 30.0 g of potassium permanganate (KMnO4)inwater and dilute to 1 L. Mix the stock solution for a minimumof 2 hours to make certain the KMnO4crystals have com-pletely dissolved.19.4 Potassium Permanganate Stock Solution (20 000 mg/L)Dilute 333.3 ml of 30 000 mg/L potassium permanganatestock
47、 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 for aperiod of 24 hours.20.2 Homogenize the dried sample by gently mixing byh
48、and. 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 solution ina 250 ml glass vial for the blank determination.20.4 Place 50 g of dried sample in each of three 250 mlglass vials
49、 (each experiment is run in triplicate).20.5 Place 100 ml of 30 000 mg/l KMnO4 stock solution ineach of the three 250 ml glass vials containing the driedsample. Seal each of the vials and invert once to mix thereagents. Store vials at room temperature (20 - 22C).20.6 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 sampleprior to analysis using Method 4500KMnO4.20.7 Repeat 20.3 through 20.6 using the 20 000 and 10 000mg/l KMnO
