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Questa Rock Pile Stability Study SOP 33v7Page 1STANDARD OPERATING PROCEDURE NO. 33PARTICLE SIZE ANALYSIS (Including both Dry and Wet MechanicalSieving and Hydrometer Analyses)REVISION LOGRevision NumberDescriptionDate33Original SOP33.1Revisions by Dr. Catherine T. Aimone-MartinAug 19, 200433v2GMLR9-2733.3Addition of ASTM, and revisions JRM01/12/200533.4Revisions by HRS01/18/0533v4Extensive Edits & comments by LMK2/14/0533v5Revisions by RDL5/30/200633v5Minor edits LMK, sent to jack Hamilton to replace theold one on the Utah Molycorp project website7/11/0633v633v6APPENDIX FOR MECHANICAL PARTICLESIZE ANALYSES (NO. 200 SIEVE) written byKwaku Boekye, January 2007, edited by LMK andadded to original SOP 33v5 by LMK. SOP 33v6finalized by LMK and sent to Jack Hamilton to post onproject websiteLMK finalized to post on Project Website and tosend to George Robinson for lab audit, no neweditsLMK added wet sieving procedure appendix33v733v71/29/074/2/0710/26/07LMK added modification to dry sievingprocedure that increases sieve shaking time10/29/071.0 PURPOSE AND SCOPEOP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 2This Standard Operating Procedure (SOP) is based on ASTM D422-63 Standard TestMethod for Particle-Size Analysis of Soils. This SOP covers the quantitative determinationof the distribution of particle sizes in soils. The distribution of particle sizes larger than 2.0mm is determined by sieving, while the distribution of particle sizes smaller than 2.0 mm isdetermined by a sedimentation process using a hydrometer to secure the necessary data. Itprovides technical guidance and procedures to be employed for particle size analyses,including the required equipment, procedures, and personnel responsibilities.2.0 RESPONSIBILITIES AND QUALIFICATIONSThe Characterization Team Leader shall have the overall responsibility for implementingthis SOP. He/she will be responsible for assigning appropriate staff to implement thisSOP and ensuring that procedures are followed accurately.All personnel performing these procedures are required to have the appropriate health andsafety training. In addition, all personnel are required to have a complete understanding ofthe procedures described within this SOP and receive specific training regarding theseprocedures, if necessary.All staff are responsible for reporting deviations from this SOP to the CharacterizationTeam Leader.3.0 DATA QUALITY OBJECTIVESParticle size analysis is required to understand the hydrologic and structural properties of the rock pile and toestimate the soil-water characteristic curve (SWCC), which is used in modeling the seepage and stability ofthe rock piles. Accordingly, this SOP addresses objectives 2 and 8 in the data quality objectives outlined byVirginia McLemore for the "Geological and Hydrological Characterization at the Molycorp Questa Mine,Taos County, New Mexico”.4.0 RELATED STANDARD OPERATING PROCEDURESThe procedures set forth in this SOP are intended for use with the following SOPs: SOP 1SOP 2SOP 6SOP 9SOP 36SOP 54Data management (including verification and validation)Sample management (including chain of custody)Drilling, logging, and sampling of subsurface materials (solid)Test pit excavation, logging, and sampling (solid)Sample preservation, storage, and shipmentAtterberg Limits5.0 EQUIPMENT LISTThe following materials and equipment are required to perform mechanical andhydrometer grain size analyses: Sieve shakerA series of sieves, (stainless steel sieves if chemical analyses will also be required):OP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 33 inch (75 mm)2 inch (50 mm)1 ½ inch (37.5 mm)1 inch (25.0 mm)¾ inch (19.0 mm)3/8 inch (9.5 mm)No. 4 (4.75 mm)No. 6 (3.35 mm)No. 10 (2.00 mm)No. 16 (1.18 mm)No. 30 (600 μm)No. 40 (425 μm)No. 50 (300 μm)No. 70 (212 μm)No. 100 (150 μm)No. 200 (75 μm)Include a cover plate and bottom pan. The number and sizes of sieves used for testinga given soil sample will depend on the range of soil sizes in the material. Balances, sensitive to 0.01g for samples weighing less than 500g, and to 1.0g forsamples weighing over 500gContainer of known weight in which to weigh the fractionsPaintbrush or soft wire brush, for cleaning sievesSample splitter or riffleHydrometer 151H or 152H modelSedimentation cylinder with a volume of 1,000 mlThermometer with accuracy to 1 F (0.5 C)Timing device, a watch or clock with a second handBeaker with 250ml capacityContainers for drying samplesDrying ovenDispersing or antiflocuating agent, 4N of sodium hexametaphosphate (NaPO4), tradename CalgonDistilled or demineralized waterA mechanically operated stirring deviceDispersion cupWash bottlePlastic bags for different particle size fractionsWaterproof labels and indelible pensParticle size fraction forms (Appendix 1)ParafilmOP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 46.0 PROCEDURES6.1 Mechanical particle size analyses1. Fill out chain of custody forms.2. Air-dry the sample to be analyzed (if necessary). See ASTM D 421 – Dry Preparationof Soil Samples for Particle-Size Analysis and Determination of Soil Constants3. Split the sample using the sample splitter or the cone and quarter method and obtain arepresentative sample for particle size analysis. The size of the sample shall dependon the diameter of the largest particle in the sample according to the followingschedule (Department of the Army, Army Corps of Engineers, 1965):Maximum Particle Size3 inches2 inches1 inch½ inchFiner than No. 4 sieveFiner than No. 10 sieveMinimum Weight of Sample(g)60004000200010002001004. Record the total sample weight on the sample form.5. Select the top sieve as the one with openings that are slightly larger than the diameterof the largest particle in the sample. If chemical analysis of the sample is to beperformed, stainless steel sieves must be used.6. Arrange the series of sieves so that they have decreasing opening sizes from the top tothe bottom of the stack (largest openings at the top of the stack, decreasing sieveopenings through the stack, with the smallest openings at the bottom of the stack).Attach the catch pan to the bottom of the sieve stack. Place the sample in the top sieveand put the cover plate over the top of the sieve stack.7. Place the sieve stack in the shaking machine and shake it for at least 10 minutes oruntil additional shaking does not produce appreciable changes in the amounts ofmaterial on each sieve screen.8. As of August 2007, this procedure has been modified to add a wet sievingprocedure (See APPENDIX VI in this SOP for the wet sieving procedure) beforethe dry sieving and to increase the sieve shaking time for the dry sieving fromminimum 10 minutes to minimum 60 minutes. From this date on the wet sievingand the longer shaking time were used and will continue to be used for thisproject. This is because the shorter shaking time and no wet sieving did not yieldaccurate grain size distribution curves because the fines clung to the largerparticles.9. Remove the sieve stack from the mechanical shaker. Beginning with the top sieve,transfer the soil particles to a weighed container/tare (which you have already notedthe weight of or for which you have tared the balance). Carefully invert the sieve andgently brush the bottom of the sieve to remove any particles caught in the screen,catching them in the weighed container as well.OP 33v7 Particle Size Analysis4/29/2008SComment [LMK1]: Sam – pleasechange the date here so it is the actualdate you started using the longer shakingtime and the wet sieving procedure. Alsoplease review the wet sieving procedurein Appendix VI. Please make anychanges to that as well, then send thisdocument back to me for finalizing andposting.Thanks, Lynne

Questa Rock Pile Stability Study SOP 33v7Page 510. Weigh the container and sample and subtract the weight of the container from the soilmaterial retained by that sieve. Record the weight of the soil particles retained on thesieve on the data sheet.11. Save the material from each sieve in a plastic bag labeled with the sample IDinformation (See the Sieve Analysis Data Sheet in Appendix 1), the size of the sieve,and the sample weight.12. Repeat steps 7 and 8 to determine the weight of soil particles retained on each sieve,including the total amount of the material in the catch pan.13. When finished, place approximately 125g of sample passing the No. 10 sieve in aplastic bag. Mark the bag with the sample ID and the words “Hydrometer Test”.14. Thoroughly remix the portion of the sample retained by the No. 10 sieve with theportion passing the No. 10 sieve.15. Place approximately 125g of the remixed sample in a plastic bag. Mark this bag withthe sample ID and the words “Specific Gravity”.16. Using the remixed portion of the sample, obtain approximately 500g of sample passingthe No. 6 sieve. Place this material in a plastic bag marked with the sample ID and thewords “Direct Shear”.17. From the remixed portion of the sample, obtain approximately 250g of materialpassing the No. 40 sieve. Place this material in a plastic bag marked with the sampleID and the words “Atterberg Limits”.6.2 Hydrometer analyses1. Record all the identifying information for the sample on the Hydrometer AnalysisData Sheet (see Appendix 1).2. The approximate size of sample to be used for the hydrometer analysis variesaccording to the size of soil particles being tested. If the soil is predominately clay andsilt, use approximately 50g, but if the soil is mostly sand, use approximately 100g.3. Weigh out a sample of the air-dry fine fraction.4. Place the sample in a 250ml beaker and add distilled or demineralized water until thesample is submerged. Add 15ml of the dispersing agent (antiflocuant) at this time.Allow the sample to soak overnight or until all soil lumps have disintegrated.5. At the end of the soaking period, disperse the sample further by transferring thecomplete sample to the dispersion cup. Wash any residue from the beaker withdistilled or demineralized water so that all the sample is transferred.6. Add distilled water to the dispersion cup, if necessary, so the cup is more than halffull.7. Place the cup in the dispersing machine and disperse the suspension for 1 to 10minutes.8. Transfer the solution to the sedimentation cylinder and add distilled water ordemineralized water to the 1000ml mark.9. Cover the end of the cylinder with Parafilm and shake the suspension vigorously for afew seconds in order to transfer the sediment on the bottom of the cylinder into auniform suspension. Continue the agitation for the remainder of the minute by turningthe cylinder upside down and back.OP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 610. At the end of the 1-minute shaking period, set the cylinder on a stable surface, notingthe time. Slowly immerse the hydrometer into the liquid over a period of 20 to 25seconds before taking the first reading.11. Take hydrometer readings after 1 and 2 minutes have elapsed from the time thecylinder was placed on the table.12. As soon as each reading is taken, carefully remove the hydrometer from thesuspension and place it in a sedimentation cylinder full of clean water.13. Repeat steps 9 to 12 to make sure that the same readings are obtained. Many errorscan occur during the first two readings. If the same values are read for 1 minute andtwo minutes during the second hydrometer test, reshake the sample and perform asabove. Then proceed to the next steps to perform the rest of the hydrometer grain sizedistribution test.14. At the end of the second 2 minutes and after each subsequent hydrometer reading,place a thermometer in the suspension and record the temperature reading on the datasheet.15. You have already recorded the hydrometer reading at 1 minute and two minutes. Nowrecord hydrometer readings at the following time intervals: 4, 15, 30, 60 (1 hour), 120(2 hours), 240 (4 hours), 960 (16 hours) and 1440 (24 hours) minutes, removing thehydrometer from the suspension after each reading and placing it in a sedimentationcylinder of clean water.16. If the dry weight of the samples is to be obtained at the end of the test, carefully washall the suspensions into a container of known weight. Oven-dry the material, allow itto cool, weigh the sample, and record the weight on the sample form.Selected size fractions will be submitted for bulk mineral analyses (XRD) and chemicalanalyses (XRF, ICP) to assess the mineralogy of the size fractions. If chemical analysesare required, then stainless steel sieves must be used for those samples.NOTE: Wash your hands periodically. Follow normal procedures to prevent crosscontamination of grain sizes. Maintain field sample numbers throughout samplepreparation.6.3 PROCEDURAL ADDENDUMADDENDUM TO MECHANICAL PARTICLE SIZE ANALYSES (NO. 200 SIEVE PORTION OFSOP 33V5 PARTICLE SIZE ANALYSIS)1. PURPOSE AND SCOPE OF ADDENDUMThis addendum modifies part of the procedure for the mechanical dry sieving of samples and is effective asof January 22, 2007, replacing the procedure described in SOP 33vr2. RELATED STANDARD OPERATING PROCEDURESThe procedure set forth in this SOP is intended for use with the following SOPs: SOP 1 Data management (including verification and validation)SOP 2 Sample management (including chain of custody)SOP 5 Sampling outcrops, rock piles, and drill core (solid) [ Suggest deleting: method is for soilnot rock]OP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7 Page 7SOP 6 Drilling, logging, and sampling of subsurface materials (solid)SOP 9 Test pit excavation, logging, and sampling (solid)SOP 36 Samples preservation, storage, and shipmentSOP 54 Atterberg Limits3. EQUIPMENT LISTThe following materials and equipments are required to perform mechanical and hydrometer analysis: Sieve shaker A series of sieves, ( stainless steel if chemical analyses will also be required):3-in (75-mm)2-in (50-mm)11- in (37.5-mm)21-in (25.00-mm)3-in (19.00-mm)43-in (9.5-mm)8No.4 (4.75-mm)No.8 (2.36-mm)No.10 (2.00-mm)No.16 (1.18-mm)No.20 (850-µm)No.30 (600-µm)No.40 (425-µm)No.50 (300-µm)No.60 (250-µm)No.100 (150-µm)No.140 (106-µm)No.200 (75-µm)4. PROCEDURES4.1 Mechanical particle size analyses (No. 200 sieve)1.2.3.Fill out chain of custodyAir-dry the sample to be analyzed (if necessary). See ASTM D 421- Dry Preparation of the SoilSamples for Particle Analysis and Determination of Soil ConstantSplit the sample using the sample splitter and obtain a representative sample for particle sizeanalysis. The size of the sample shall depend on the diameter of the largest particle in the sampleaccording to the following schedule (Department of the Army, 1965):4.Maximum Particle Size3-in2-in1-inOP 33v7 Particle Size AnalysisMinimum Weight of Sample(g)6000400020004/29/2008S

Questa Rock Pile Stability Study SOP 33v71/2-inFiner than No.4 sieveFiner than No.10 sieve5.6.7.8.9.10.11.12.13.14.15.16.Page 81000200100Record the total sample weight on the sample form.Select the top sieve based on the weight of the sample as the one with openings that are slightlylarger than the diameter of the largest particle in the sample.Arrange the series of sieves so that they have decreasing opening size from the top to the bottom ofthe stack (largest openings at the top of the stack, decreasing sieves opening through the stack, withthe smallest openings at the bottom of the stack). Include No. 200 sieve in every stack to determinewhether to run a hydrometer test on the sample as well (Any sample that has size fractions passingthrough the no. 200 sieve will require a hydrometer test to determine the grain size distribution ofthe 75 µm fraction of the sample.). Attach the catch pan to the bottom of the sieve stack.Place the sieve stack in the shaking machine and shake it for at least 10 min or until additionalshaking does not procedure appreciable changes in the amounts of material on each sieve screen.Remove the sieve stack from the mechanical shaker. Beginning with the top sieve, transfer the soilparticles to a weighed container (which you have already noted the weight of or tared the balanceto). Carefully invert the sieve and gently brush the bottom of the sieve to remove any particlescaught in the screen, catching them in the weighed container as well.Weigh the container and sample and subtract the weight of the container from the soil materialretained by that sieve. Record the weight of the soil particles retained on the sieve on the data sheet.Save the material from each sieve in an envelope labeled with the sample ID information, the sizeof the sieve, and the sample weight. Include the same information plus the words “for hydrometertest ” on the material collected from the no. 200 sieveSave the fraction passing the No. 200 sieve in a plastic bag and label it with the sample ID and thewords “hydrometer test”. Make sure it is 125 g.If you do not have enough material for the hydrometer test, hand shake more sample through theNo. 200 sieve and add the material obtained to the material obtained from sieving to measure 125gWhen finished, place approximately 200g of sample passing the No. 6 sieve in a plastic bag. Markthe bag with the sample ID and the words “Direct Shear Test”.Place approximately 125g of the sample passing the No.4 sieve in a plastic bag. Mark this bag withthe sample ID and the words “Specific Gravity”.Place approximately 125g of the sample passing the No.40 sieve in a plastic bag. Mark this bagwith the sample ID and the words “Atterburg Limits”.7.0 DOCUMENTATIONFill out particle size analysis form (Appendix 1).Each size fraction is assigned a separate sample identification number. The first part isidentical to the field identification number (reference SOP for field identification number)and is followed by a sequential two numbers, for example SSW-HRS-001-03, shown inTable 1.Table 1. Sample identification numbering (Sample ID) as outlined in SOP 2 SampleManagement.Component 1Component 2Component 3Component 4Three letterabbreviation for theThree letter initialsof the sampleOP 33v7 Particle Size AnalysisSequential fournumber designation,Sequential twonumber designation,4/29/2008S

Questa Rock Pile Stability Study SOP 33v7mine feature, forexample SSW forSugar Shack West.collector, forexample HRS forHeather R. Shannon.Page 9for example 0001.for example 03 forsplit sample 3.In the example above, the sample ID would be SSW-HRS-0001-03.8.0 QUALITY ASSURANCE/QUALITY CONTROLNMBGMR will archive all samples for future studies. The lab manager or other supervisory personnel experienced with the test will reviewthe results, checking calculations, and check for consistency with the approved testmethodology. Depending on the DQO being satisfied, a greater frequency of tests may need to beperformed on a particular material. The reviewer needs to check that the frequency oftests is consistent with the DQO.9.0 DATA ANALYSIS AND CALCULATIONS Mechanical Analysesa) The weight percent of the material retained on the various sieves is computed asfollows:Weight percent retained air dry weight in g retained on a sieve x 100air-dry weight in g of total sampleb) Percent finer by weight is obtained by subtracting the cumulative percent retainedfrom 100%.c) Plot the relationship between sieve openings and percent finer by weight on asemi-logarithmic graph with the sieve openings as ordinates on the arithmeticalscale, and the percent finer by weight as abscissas on the logarithmic scale. Hydrometer Analysesa) Correct hydrometer reading, R, by adding the meniscus correction to the actualhydrometer reading, R’. Record the correct reading, R, on the data sheet.b) Calculate the particle diameter corresponding to a given hydrometer reading onthe basis of Stoke’s equation, using the nomograph shown in Appendix 1.c) Plot the results as the continuation of the grain-size distribution curve from thelarger size fractions of that sample on a semi-logarhithmic chartThe results of the particle size analysis are presented in the form of a grain sizedistribution curve on a semi-logarithmic chart. The curves obtained from the sieveanalysis and hydrometer tests are joined by constructing a smooth curve between them.OP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 1010. REFERENCESAimone-Martin, C. T., 2003, Soil Mechanics: Laboratory Manual, Department of Mineraland Engineering, New Mexico Institute of Mining and Technology, Socorro, NM.Liu, C. and Evett, J. B. 2003, Soil Properties: Testing, Measurements, and Evaluation, 5thedition, Upper Saddle River, NJ., pg 103 – 125.ASTM, 2001, American Society for Testing Materials. Annual Book of ASTM Standards,West Conshohocken, PA, Cited by Liu, C. and Evett, J. B., 2003.Department of the Army, 1965, Engineering Design: Laboratory Soil Testing, Department ofthe Army Headquarters, Washington, D.C., pg V1 – V28.Saskatchewan Highways and Transportation, 1993, Standard Test Procedures ManualSTP205-10: Mechanical Analysis, rts manuals/STP DOC/stp205-10.pdf (accessed06/08/2004).OP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 11APPENDIX 1FORMSOP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 12APPENDIX II, HYROMETER CALIBRATION EQUATIONS(APPLICABLE FOR THE HYDROMETERS IN THE SOIL MECHANICS LABORATORY AT NEW MEXICO TECH.)20HHydrometer -0.1917 R 18.5HEIGHT, H (cm)AB15H -0.18 R 18.01050204060CORRECTED HYDROMETER READING, RAPPENDIX III. TEMPERATURE CURRECTION FACTORS, m, FOR HYDROMETER 564.465.366.267.16868.9Correction 0.2-0.100.1OP 33v7 Particle Size Degrees Correction 1.6282929.53030.53131.53232.53333.534Degrees .5

Questa Rock Pile Stability Study SOP 33v7Page 13APPENDIX IV. Grain Size Sub FormOP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7Page 14APPENDIX V. U.S. ARMY CORPS OF ENGINEERS 1970 SIEVINGPROCEDUREOP 33v7 Particle Size Analysis4/29/2008S

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Questa Rock Pile Stability Study SOP 33v7Page 40APPENDIX VI. WET SIEVING PROCEDUREThis wet sieving procedure is used to remove the fine particles clinging to the largerpieces in the sample before dry sieving the sample to determine the grain size distribution.ADDITIONAL EQUIPMENT NEEDED BucketOP 33v7 Particle Size Analysis4/29/2008S

Questa Rock Pile Stability Study SOP 33v7 Page 41Piece of hose long enough to reach sieve area and bucket with connection to fitwater source you’re usingSet of no. 6, no. 10, and 200 sievesExtra person to helpSpatula or similar to stir fines when 200 sieve gets cloggedPROCEDURE1. Weigh container and sample in dry form first and record weights. The amount of thesample needed is determined by the largest grain size in the sample (see Table on Page4 or Page 7 in the dry sieving section of this SOP).2. After weighing, put sample in a pan, cover with tap water, and soak for at least an hour3. Stack these three sieves: No. 6, No. 10., and 200, with bucket under these three sieves4. Then pass sample thru these three sieves while running water to remove all of thefines, with one person holding the sieve set and the other directing the water from thehose and watching for overflow5. Fines may clog up the 200 sieve and cause the water to overflow, so watch the waterlevels and stop the water flow until the clog is removed6. Use a spatula or similar to stir fines clogging sieve until water can flow through itagain7. Catch the water in the bucket8. Make sure all the particles are clean (run water thru until water runs clean.9. Using the three sieves keeps the larger particles from ruining the 200 sieve.10. Then recombine the material from the No. 6, No. 10 and 200 sieves11. Air dry or oven dry the sample in a pan12. Follow the dry sieving procedure in this SOP from hereOP 33v7 Particle Size Analysis4/29/2008S

PARTICLE SIZE ANALYSIS (Including both Dry and Wet Mechanical Sieving and Hydrometer Analyses) REVISION LOG Revision Number Description Date 33 Original SOP 33.1 Revisions by Dr. Catherine T. Aimone-Martin Aug 19, 2004 33v2 GMLR 9-27 33.3 Addition of ASTM, and re