Particle size distributions by laser diffraction: sensitivity of granular matter strength to analytical operating procedures

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1 Soli Erth, 1, 5 8, 1 Author(s) 1. This work is istriut unr th Crtiv Commons Attriution 3. Lins. Soli Erth Prtil siz istriutions y lsr iffrtion: snsitivity of grnulr mttr strngth to nlytil oprting prours F. Storti n F. Blsmo Diprtimnto i Sinz Gologih, Univrsità Rom Tr, Lrgo S. L. Murilo 1, 1 Rom, Itly Riv: Novmr 9 Pulish in Soli Erth Disuss.: 1 Dmr 9 Rvis: Mrh 1 Apt: April 1 Pulish: 19 April 1 Astrt. W tst lsr iffrtion prtil siz nlysis in poorly ohrnt ront pltform tlsti ris n unfult qurtz-rih olin sns, rprsnting lown high-strngth grnulr mtrils, rsptivly. W us two iffrnt instrumnts with iffrnt smpl isprsion n pumping systms n svrl wt nlytil prours tht inlu iffrnt pump sps, msurmnt prision tsts with n without smpl ultrsonition, n iffrnt isprsnt liquis. Rsults of our work init tht high strngth mtril is not strongly fft y nlytil oprting prours, whrs low strngth mtrils r vry snsitiv to th pump sp, ultrsonition intnsity, n msurmnt run tim. To ru suh t vriility, w propos workflow of nlytil tsts prliminry to th st up of th most pproprit SOP. 1 Introution Prtil siz istriutions provi funmntl informtion for rok hrtriztion n gologil pross sription in rth sins, inluing simntology, strtigrphy, struturl gology, pology, n volnology (.g. Krumin, 191; Irni n Cllis, 193; Englr, 197; Frimn, 1979; Shrin t l., 1987; Riu n Sposito, 1991). In th lst thr s, lsr iffrtion prtil siz nlysrs hv prov to n fftiv tool for proviing prtil siz istriutions of poorly ohrnt roks n soils (Wiss n Frok, 197; MCv t l., 198; Bor t l., 1987; Wnogho t l., 1987; Agrwl t l., 1991; Loizu t l., 199; Py n Blott, ; Blott n Py, ). This is us thy rquir littl tim for nlysis, ovr wi siz rng, n rquir smll siz smpls (.g. Buslink t l., Corrsponn to: F. Storti ([email protected]) 1998), thus filitting vry til stuis of prtil siz istriutions in gologil struturs. Lsr iffrtion prtil siz nlysrs provi inirt siz msurmnts of sphrilly quivlnt prtils, s on th prinipl tht prtils of givn siz iffrt light through givn ngl tht inrss logrithmilly with rsing siz (.g. Buslink t l., 1998). In wt prours, fw grms of mtril r isprs into liqui tht irults ross qurtz msurmnt ll illumint y lsr m (Fig. 1). Diffrnt instrumnts hv iffrntly sign systms for stirring th isprsnt liqui into th tnk n nsuring its irultion through th msurmnt ll y mhnil pumping. A wi vrity of stnr oprting prours (SOP) n st up in lsr iffrtion prtil siz nlysrs. Thy inlu th pump sp, th numr of msurmnt runs, th lngth of th msurmnt tim, n th us of isprsing gnts n/or ultrsonition to i smpl isggrgtion n isprsion (.g. Blott t l., ; Sprzz t l., ). It follows tht msurmnt rsults, prtiulrly whn ling with tsts prou y iffrnt oprtors n/or iffrnt instrumnts, n influn y th opt SOP. Smpl ultrsonition, for xmpl, n i prtil isggrgtion y ollision or, in som ss, prtil gglomrtion (.g. Mson t l., 3; Blott t l., ). In this stuy w nlys prtil siz istriutions of unfult qurtz-rih (83% qurtz, 9% plgiols, n 8% flspr) olin sns from th Privrno qurry, on th Tyrrhnin si of th Cntrl Apnnins (.g. Anglui n Plmrini, 191), n ront tlsti ris from th tiv Assrgi xtnsionl fult systm, whih ouns to th south th Grn Ssso Mssif in th Cntrl Apnnins, Itly (.g. D Agostino t l., 1998). Our rsults init tht prtil siz t msurmnt y lsr iffrtion grnulomtry is not strightforwr in frgil grnulr mtrils. W provi n nlytil workflow for prliminry tsting, whih is proputi to finl SOP trmintion Pulish y Coprnius Pulitions on hlf of th Europn Gosins Union.

2 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Stirring n ultrsonition Tnk Lsr Pump Projtion lns Lsr m Fourir lns Wtr-prtil suspnsion Computr Msur ll Dttor Fig. 1. Shmti rtoon showing th min omponnts of lsr iffrtion prtil siz nlysr. S txt for tils. in grnulr roks. Th propos tsting prour n rsult pproprit for wi vrity of rok typs, inluing tlsti roks in fult zons n lsti simnts tht unrwnt uril-rlt grin mirofrturing. Instrumnts ovrviw Most grnulomtri nlyss wr prform with Mstrsizr lsr iffrtion grnulomtr n ssoit isprsion units mnuftur y Mlvrn Instrumnts Lt. This lsr iffrtion prtil siz nlysr is sign for msuring prtil sizs in th. to µm rng y using lu (88. µm wvlngth LED) n r (33.8 µm wvlngth H-N lsr) light ul-wvlngth, singl-lns ttion systm. Th light nrgy iffrt y th ilut suspnsion irulting through th ll is msur y 5 snsors. Th light intnsity sor y th mtril is msur s osurtion n inits th mount of smpl to th isprsnt liqui. Light sttring t r umult in 1 siz frtions ins, whih r nlys t 1 rings pr son, n ompil with Mlvrn s Mstrsizr softwr y using ithr full Mi or Frunhofr iffrtion thoris ( Bor t l., 1987). Light sttring t quir y th Mstrsizr grnulomtr wr ll mthmtilly invrt using th Mi thory, whih utilizs th rfrtiv inx (RI) n sorption (ABS) of th isprs grnulr mtril, n RI of th isprsnt liqui. This thory is s on th ssumption tht: (1) prtils r minrlogilly homognous; () prtils r sphril; (3) th optil proprtis of prtil n isprsion mium r known; () suspnsion ilution gurnts tht light sttr y on prtils is msur for ing-r-sttr y othr prtils. Prtil siz istriutions wr msur from wt isprsions using oth smll (Mlvrn Hyro S) n lrg (Mlvrn Hyro MU) volum smpl isprsion units vill for th Mstrsizr grnulomtr. Th Hyro S unit hs pity of 5 to ml n is quipp with ontinuously vril singl shft ntrifugl pump n stirrr (up to 35 rvolutions pr minut; in th following rpm), n y ontinuously vril ultrsoni pro. Th Hyro MU unit hs isprsion mhnism onsisting of smpl rirultion h immrg into stnr lortory kr (pity of to 1 ml), whih ontins uilt-in stirrr n smpl rirultion ntrifugl pump (from to rpm), n ontinuously vril ultrsoni pro (mximum powr is µm of tip isplmnt). A omprtiv wt nlysis ws prform y Cils 93 lsr iffrtion grnulomtr mnuftur y Cils, whih msurs prtil siz istriutions in th. to 5 µm siz rng of wt isprsions y iffrtion of lsr light of 83 nm wvlngth, s ithr on th Frunhofr or Mi iffrtion thoris. Smpl rirultion is hiv y two pristlti pumps. Th nlys ront fult ri smpl, nm CABRE3, ws ollt in th sm sit of smpl CABRE1 sri in Storti n Blsmo (1), n ws siv t 5 µm to ount for th nlytil siz rng of th Cils 93 lsr iffrtion prtil siz nlysr. Rprouil su-smpling up to out g wight of th totl smpl mount ws hiv y using Qunthrom Siving Rifflr-Rotry Smpl Splittr. Su-smpl liquots nssry to prou lsr osurtion vlus twn 1% n 15% wr rnomly slt from su-smpls (from.5 g to fw grms) n into th liqui-fill kr for nlysis. 3 Ftors influning t quisition n prossing from ilut suspnsions: tsting strtgy Both hmil n mhnil ftors n influn light sttring t otin from ilut suspnsions (.g. Sprzz t l., ). Chmil intrtions n in ft our twn isprsion mium, th nlys mtril n, possily, isprsing gnt. Mhnil smpl ltrtion n prou y two mjor ftors: (i) ultrsonition uring smpl rirultion n (ii) ntrifugl pump n stirrr sp. Morovr, th onvrsion of light sttring t into prtil siz istriutions pns on th optil proprtis of oth nlys mtril n isprsnt liqui. Th high vriility of th optil proprtis of roks n simnts ommonly rquirs itrtiv t rprossing unlss ssntilly monominrli mtrils r nlys (.g. Sprzz t l., ). To invstigt on th influn of prmtrs list ov, w st up th following tsts on monominrli mtrils lik olin qurtz sn (susmpl liquots SAND1x) n ront tlsti ri Soli Erth, 1, 5 8, 1

3 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 7 (su-smpl liquots CABRE3x): pump sp tst, msurmnt prision tst (instrumnt prision tst of Blott t l., ), ultrsonition tst, hmil tst, n rprossing tst. Th pump sp tst is lll P t -tst, whr t is th msurmnt run tim (i.. th numr of rings tht r vrg in singl msurmnt), n onsists of msurmnt runs prform on givn su-smpl liquot, t iffrnt stirrr n pump sp (in th following simply rfrr to s pump sp) for givn t. Th tst strts with th st up of lsr osurtion vlus twn 1% n 15% t hlf of th mximum pump sp. Th pump sp is thn lowr to th minimum vlu n fw (typilly 1) msurmnt runs r prform for inrsing th pump sp (typilly y 1 rpm). Progrssiv msurmnt stps r rri out up to th mximum pump sp. Rsults r plott in mn imtr vrsus pump sp grph to slt th most pproprit rpm vlu for furthr nlyss. Th msurmnt prision tst is lll MPt S, whr S is th pump sp, n onsists of msurmnt runs quir t givn pump sp n msurmnt run tim uring su-smpl rirultion through th msurmnt ll. Our MPt S nlyss typilly onsist of 1 msurmnt runs, whih mns som hunr thousns of instrumnt rings. Anlysis of t trns is inlu in th msurmnt prision tst to hlp slting th most pproprit numr of msurmnt runs n to prvnt signifint mhnil is. Aition of su-smpl ultrsonition to th msurmnt prision tst prous th ultrsonition tst US, whih is lll s US S, whr is th pro tip isplmnt in th Hyro MU isprsion unit. Chmil ffts wr invstigt y rpting th ov mntion smpl tsts using iffrnt isprsion liquis. Th suffix l is to th pproprit tst llling in orr to init th isprsion liqui us, whih n solution with isprsing gnt. W i not us spifi llling for lifi tp wtr y oupl mgnti n hmil ommril vis, whih ws us in most of our nlyss. Th rprossing tst onsists of hnging th optil proprtis of oth grnulr mtril n isprsnt liqui uring light sttring t prossing of givn nlysis y th Mi thory through th Mstrsizr softwr. Our prfrr workflow (Fig. ) strts with pump sp tst to provi initions on th pump sp rng for furthr tsting. Short msurmnt run tims (typilly 5 s s strting vlu) r us in pump sp nlyss, in orr to minimis su-smpl mhnil ltrtion without ompromising th sttistil roustnss of th t. Rsults from th P-tst provi onstrints for MP n US tst pirs prform t th sm pump sp vlus. Mor thn on tst pir n prform to invstigt unrtintis ssoit with th pump tst. Cross hking of rsults from th MP n US tsts is ommonly hiv y ompring th hviour of mn imtrs, of th orrsponing lsr osurtion vlus, n of othr sttistil prmtrs inluing 1 n pump sp rng MPt S1 + US S1 P tst t MPt Sn + US Sn st smpl rirultion n msur run tim prmtrs Chmil tst st isprsnt liqui Rprossing tst Finl SOP SP tst P = pump sp tst MP = msurmnt prision tst US = Ultrsonition tst t = msurmnt run tim s = pump sp = pro tip isplmnt Fig.. Flow hrt illustrting th min stps tht onstitut th propos workflow to slt th most pproprit oprting prour for nlyzing grnulr mtrils. S txt for tils. th mo n prntils, mong whih D 1, D 5, n D 9 r th most ommon ons. On th most pproprit prmtrs in trms of st smpl rirultion, msurmnt run tim, n msurmnt run numr r slt, ll informtion for fining th most pproprit SOP is vill for givn isprsion liqui. Th nxt stp is to hk th fftivnss of th slt isprsion mium y running th sm tst with iffrnt isprsion liquis. Comprison of ll rsults ls to th sltion of th finl SOP, whih n rpt for svrl su-smpls to prform smpling prision tst (Blott t l., ) tht llows vluting msurmnt rprouiility (Fig. ). Th squntil logi of ths tsts implis tht rsults from on tst r thn us to proprly st up th following ons. Consquntly, t intrprttion is irtly provi in sustions ssoit with th orrsponing tst sriptions. In most tsts, for omprtiv purposs w quir 1 Soli Erth, 1, 5 8, 1

4 8 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Pump sp (rvolutions pr minut) Osurtion (%) 1 3 Pump sp (rvolutions pr minut) Dimtr (mm) 1 3 Pump sp (rvolutions pr minut) D 9 D 5 D rpm rpm 15 ly siz 1 rpm 5 rpm 11 rpm 3 rpm 8 silt siz sn siz rpm 35 rpm 13 rpm rpm 1 rpm 15 rpm Pump sp (rpm) Fig. 3. Rsults of th pump sp tst P 5 prform on su-smpl liquot SAND1 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th pump sp from up to rpm. () Lsr osurtion vlu progrssion uring th sm tst. () Progrssion of D 1, D 5, n D 9 uring th sm tst. () Grnulomtri urvs otin y vrging t from th orrsponing 1 msurmnt runs uring rprsnttiv pump sp stps. () Distriution of ly, silt, n sn siz frtions uring th tst. Not tht th sn frtion quikly rhs 1% of th smpl mtril. S txt for tils. msurmnt runs rgrlss of initions from prvious tsts. This us of th short tim rquir y lsr iffrtion prtil siz nlysrs to quir light sttring t, thus nourging th olltion of lrg tsts from whih su-sts n thn sily xtrt. Pump sp tst Rsults of th P 5 -tst of su-smpl liquot SAND1 (i.. 5 rings of th sttr light nrgy istriution for h msurmnt run) r illustrt in Fig. 3. Mn imtrs show n symmtri ll-shp trn hrtriz y vry low vlus t n 7 rpm, mximum t 1 to rpm, n n lmost flt nvlop of mn imtr vlus t pump sp highr thn rpm (Fig. 3). Th orrsponing lsr osurtion vlus show muh highr vriility, with pk t 9 rpm n minimum t 13 rpm, follow y nr onstnt inrs t highr pump sp vlus (Fig. 3). Th trn of D 1, D 5, n D 9 prntil t points strongly rsmls th istriution of th mn imtrs (Fig. 3). Grnulomtri urvs vrg ovr 1 msurmnt runs init strongly unimol prtil siz istriution with som vriility of oth volum prntg n mol pk siz twn 9 n 15 rpm. Convrsly, lmost ovrlpping urvs support strongly onsistnt rsults t pump sp vlus grtr thn rpm (Fig. 3). Th wll sort prtil siz istriution of th smpl is illustrt y th pttrn of ly, silt, n sn siz frtions: strting from 7 rpm, th lttr inlus 1% of th nlys mtril (Fig. 3). Th P 5 -tst of su-smpl liquot CABRE3 shows n symmtri ll-shp trn hrtriz y vry low vlus of mn imtrs t to 8 rpm, follow y n rupt inrs up to 11 rpm (Fig. ). With inrsing th pump sp, mn imtr vlus rpily rs up to 15 rpm n thn ontinu to ovrlly rs quit slowly Soli Erth, 1, 5 8, 1

5 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Pump sp (rvolutions pr minut) Osurtion (%) 1 3 Pump sp (rvolutions pr minut) Dimtr (mm) D 1 D Pump sp (rvolutions pr minut) D rpm 1 rpm 11 rpm rpm 13 rpm 1 rpm 15 rpm rpm 5 rpm 3 rpm 35 rpm rpm 8 ly siz silt siz sn siz Pump sp (rpm) Fig.. Rsults of th pump sp tst P 5 prform on su-smpl liquot CABRE3 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th pump sp from up to rpm. () Lsr osurtion vlu progrssion uring th sm tst. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Grnulomtri urvs otin y vrging t from th orrsponing 1 msurmnt runs uring rprsnttiv pump sp stps. () Distriution of ly, silt, n sn siz frtions uring th tst. up to th mximum pump sp. Th orrsponing lsr osurtion vlus show rpi initil inrs up to out % t 1 rpm, follow y rpi rs towrs th initil rfrn vlu (twn 1.8% n 15.%). A short-liv pltu ours up to rpm n thn osurtion onstntly inrss with inrsing th pump sp (Fig. ). Th D 1, D 5, n D 9 prntils show ll-shp nvlops, qulittivly similr to tht of th mn imtr (Fig. ). From to rpm, th D 9 t point nvlop shows onstnt n signifint rs, whil D 5 is hrtriz y highr sttring n only slightly rsing trn. D 1 vlus rs s wll n t rpm rh lmost hlf of th vlu t rpm. Grnulomtri urvs vrg ovr 1 msurmnt runs, r hrtris y strongly symmtri shp tht inlus mjor pk in th orsr frtions n suorr long til in th finr ons (Fig. ). With inrsing th pump sp, th hight of th mjor pk rss n shifts towrs finr mol vlus, n th volum prntg of finr prtils (quivlnt imtr smllr thn out 1 µm) orrsponingly inrss. Th pttrn of ly, silt, n sn siz frtion urvs inits n initil ominn of silt sizs, follow y thir rupt rs n orrsponing inrs of sn siz frtions t pump sp vlus orrsponing to th mximum mn imtr (Fig. ). At pump sp vlus highr thn 15 rpm, th sn siz frtion slightly vris out pltu vlu, th silt siz frtion slightly rss, n th ly siz frtion slightly inrss. Rsults of th P 1 -tst of su-smpl liquot CABRE3 r illustrt in Fig. 5. Th ovrll hviour of this tst is similr to th prvious on, with slightly highr sttring of mn imtr n prntil vlus. Grnulomtri urvs o not show th lmost onstnt shp volution tht hrtriss thos quir t 5 s of msurmnt run tim, spit th ovrll trn is omprl with th lttr. Soli Erth, 1, 5 8, 1

6 3 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Osurtion (%) 8 Dimtr (mm) D Pump sp (rvolutions pr minut) Pump sp (rvolutions pr minut) Pump sp (rvolutions pr minut) D rpm 1 rpm 11 rpm rpm 13 rpm 1 rpm 15 rpm rpm 5 rpm 3 rpm 35 rpm rpm ly siz silt siz sn siz 1 3 Pump sp (rpm) Fig. 5. Rsults of th pump sp tst P 1 prform on su-smpl liquot CABRE3 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th pump sp from up to rpm. () Lsr osurtion vlu progrssion uring th sm tst. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Grnulomtri urvs otin y vrging t from th orrsponing 1 msurmnt runs uring rprsnttiv pump sp stps. () Distriution of ly, silt, n sn siz frtions uring th tst. A omprtiv P 5 -tst of su-smpl liquot CABRE3 ws prform with th Hyro S isprsion unit. Th ovrll hviour is quit similr to th prvious tst, with vry low mn imtr vlus t 5 rpm, mximum t rpm, n rs up to rpm. Th lst stps, with pump sp inrmnts of 5 rpm, show quit smll vritions (Fig. ). A P 5 -tst y th Hyro S isprsion unit of su-smpl liquot SAND1, from 5 to 5 rpm, shows ll-shp istriution of mn imtr vlus similr to tht prou y using th Hyro MU isprsion unit (Fig. ). Comprison of pump sp tst rsults from smpl CABRE, quir t 5 s of msurmnt run tim y th Hyro MU n S isprsion units, shows tht th formr systmtilly provis highr mn imtr vlus t low pump sp rngs up to 11 rpm, inluing th highst on (Fig. ). In th to 1 rpm rng, highr mn imtr vlus r provi y th Hyro S unit. At highr pump sp, vlus provi y th two isprsion units r similr. Intrprttion of th pump sp tst rsults Th mning of th ll-shp urv provi y pump sp tsts is not strightforwr. Low vloity stirring n pumping fvour simnttion of orsr prtils t th ottom of th kr n/or slow motion in th rirultion unit n msurmnt ll, thus prouing initil siz istriutions is towrs th finr prtils. Th rpi inrs of mn imtr vlus rivs from th improv rirultion of progrssivly orsr prtils with inrsing th pump n stirrr sp. Th highst mn imtr vlus n ithr rlt to th tul prtil siz istriution, or to n rtft us y stgntion/slow motion of orsr mtril in th msurmnt ll. In th first s, th susqunt rs of mn imtr vlus shoul init ongoing prtil siz rution, ompni y signifint inrs of lsr osurtion t vlus highr thn th initil rfrn intrvl. For su-smpl liquot CABRE3, suh n inrs ours t pump sp vlus highr thn Soli Erth, 1, 5 8, 1

7 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 31 5 ront ri II Pump sp (rvolutions pr minut) Hyro MU Hyro S olin sn Pump sp (rvolutions pr minut) 8 1 Pump sp (rvolutions pr minut) Fig.. () Pump sp tst P 5 prform on su-smpl liquot CABRE3 y th Hyro S isprsion unit; mn imtr vlu volution with inrsing th pump sp from 5 up to 35 rpm. () Pump sp tst P 5 prform on su-smpl liquot SAND1 y th Hyro S isprsion unit; mn imtr vlu volution with inrsing th pump sp from 5 up to 5 rpm. () Comprison, in th rng 5 rpm, of th trns of mn imtr vlus otin from pump sp tsts on smpl CABRE. Th soli lin rfrs to t in Fig. 3; th rokn lin rfrs to t in Fig.. I finwr is orswr is III ngligil siz rution IV signifint siz rution Pump sp (rvolutions pr minut) Fig. 7. Conptul skth showing th four min stgs hrtrising th typil symmtri ll shp urv rsulting from th progrssion of mn imtr vlus uring pump sp tsts of grnulr mtrils. S txt for tils. 1 rpm, whrs osurtion rmins lmost onstnt n within th initil rfrn intrvl from 15 to rpm (Fig. ). This vin suggsts tht highst mn imtr vlus r orswr is through inffiint smpl rirultion, n tht vlus in th pltu hrtrizing oth mn imtr n lsr osurtion vlus, orrspon to th most likly msurmnt runs. In CABRE3 th osurtion t point pltu jnt to th mximum vlu is not wll vlop n, onvrsly, it sms to init slight inrs of finr mtril uring msurmnt. Howvr, nlysis of th D 1, D 5, n D 9 prntils os not init signifint prtil siz rution spit signifint sttring. Th hviour of osurtion vlus ssoit with susmpl liquot SAND1 is iffrnt n this n rlt to th iffrnt rok typ n siz. Initil vlus vry los to zro n xplin y th vry goo sorting of th smpl, lmost totlly onsisting of sn-siz prtils tht, t vry low pump sp, r lmost ntirly posit t th ottom of th kr. Th onstnt inrs of lsr osurtion vlus t pump sp highr thn 13 rpm inits n inrs of th mtril mount in th isprsion unit. Prntils, howvr, woul support muh smllr siz vritions (Fig. 3). This pprntly ontrsting vin n ronil y mitting n inrs of vry fin prtils n ngligil ovrll prtil siz rution. Th sour of suh xtrmly fin grin mtril is likly ollision-inu surf polishing of qurtz grins, whih r originlly ot y iron hyroxi thin films imprting thm slightly orng olour. Th sm olour hrtriz wtr in th kr t th n of th nlyss. Soli Erth, 1, 5 8, 1

8 3 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 5 Osurtion (%) 1 Dimtr (mm) urv 1 1 urv 1 urv 1 urv 3 urv urv 5 1 urv urv 7 8 urv 8 urv 9 urv 1 Linr Fit: Y = * X Avrg Y = Rsiul sum of squrs = 8.71 Rgrssion sum of squrs =.13 R-squr = msurmnt run numr msurmnt run numr Msurmnt run numr L inr fit: Y = * X Avrg Y =.7 Rsiul sum of squrs =.535 Rgrssion sum of squrs =.378 R-squr = D 9 D msurmnt run numr sn siz D msur run numr Fig. 8. Rsults of th msurmnt prision tst MP5 5 prform on su-smpl liquot SAND1 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Grnulomtri urvs rprsnttiv of th prtil siz volution. Not thir virtully prft ovrlp. Th orrsponing mol vlus (sm olour o) r illustrt in th inst grph, whos sttistis r lso provi. Not how vrg mol n mn vlus r vry similr. () Distriution of th sn siz frtions uring th tst. It rprsnts 1% of th smpl, without ny signifint mount of ly n silt. Rsults from th pump sp tsts illustrt ov n shmtilly xplin y omposit trn of mn vlus s funtion of pump sp vlus, whr four mjor stgs n intifi (Fig. 7): (1) n initil sgmnt hrtriz y vry low mn imtr vlus, whih is intrprt to init finwr is y infftiv mtril rirultion into th isprsion unit n msurmnt ll; () th jnt, ll-shp sgmnt ontining th mximum mn imtr vlus, whih is intrprt to init orswr is y infftiv mtril rirultion; (3) th thir, flt-lying or slowly ipping sgmnt, whih is intrprt to init fftiv mtril rirultion without signifint mhnil ltrtion, thus proviing th most fftiv pump sp siz rng for furthr nlyss; () th fourth sgmnt, hrtris y progrssivly rsing mn imtr vlus initing th ourrn of signifint mhnil ltrtion n onsqunt finwr ising of th smpl mtril t. Th gomtry of this lst sgmnt might lso influn y iffrntil vloity twn ors n fin prtils: ing th rirultion of th lttr fstr, this might rt th illusion of highr ontnt of fins. 5 Msurmnt prision tst Rsults from th pump sp tst on th SAND1 smpl init ngligil influn of this prmtr for vlus highr thn rpm. W prform MP5 5 tst (i.. 5 rpm of pump sp n 5 s of msurmnt run tim) on susmpl liquot SAND1 (Fig. 8). Mn imtr vlus isply only slight vrition twn th 1 runs, s o th D 1, D 5, n D 9 prntils, whil osurtion vlus r sttr n progrssivly inrs. Grnulomtri urvs slt to monitor th volution of th tst show virtully intil shps, s support y th vry low vritions of Soli Erth, 1, 5 8, 1

9 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 33 Osurtion (%) 5 Linr Fit: Y = * X Avrg Y =. 15 Rsiul sum of squrs = 59.7 Rgrssion sum of squrs = 8.8 R-squr = msurmnt run numr urv 1 urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv Linr Fit: Y =.7755 * X Rsiul sum of squrs =.138 Rgrssion sum of squrs =.98 R-squr = msurmnt run numr Msurmnt run numr Dimtr (mm) D 1 D 5 D msurmnt run numr ly siz silt siz sn siz 8 1 msurmnt run numr Fig. 9. Rsults of th msurmnt prision tst MP 5 prform on su-smpl liquot CABRE3 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Grnulomtri urvs rprsnttiv of th prtil siz volution. Th orrsponing mol vlus (sm olour o) r illustrt in th inst grph. () Distriution of th ly, silt n sn siz frtions uring th tst. th orrsponing mo vlus (Fig. 8). This inits tht no mtril finr thn sn ws prou uring msurmnt runs (Fig. 8). Th pump sp tst for smpl CABRE3 inits tht rpm is th most suitl pump sp vlu to nsur fftiv mtril rirultion without vry invsiv mhnil ltrtion. Morovr, 5 s of msurmnt run tim r xpt to provi mor sttistilly roust rsults thn 1 s. Aoringly, w initilly prform MP 5, tst on susmpl liquot CABRE3 (Fig. 9). Mn imtr vlus show signifint sttring n slightly rsing trn with tim, whil lsr osurtion progrssivly inrs. Th vlu of D 5, n D 9 prntils show pttrn similr to th mn imtr, ing th sttring of th formr prtiulrly highr. On th othr hn, D 1 prntil vlus r xtrmly smll. Slt grnulomtri urvs r quit similr prt from th first run (Fig. 9). Th orrsponing mol vlus show muh highr mo for th first run, follow y rop of out 1 µm in th son on. Slightly highr vlus hrtriz runs 3 to 5, n thn vry similr vlus prtin to th following runs (out 35 µm) with th xption of th lst on, whih hs highr mo, slightly highr thn µm. Th istriution of sn, silt n ly siz frtions shows sttr pttrn out slightly rsing trn for th sn siz, lss sttring out slightly inrsing trn for th silt siz, n ngligil sttring with nr onstnt vlus for th ly siz frtion (Fig. 9). Dt from MP tsts t rpm n rpm pump sp, rsptivly, prform for omprtiv purposs on th influn of pump sp, r illustrt in Fig. 1. Th first tst is hrtris y xtrmly high t sttring, whrs in th son s sttring is quit smll, vrg imtr vlus r lowr, n lsr osurtion vlus inrs t highr rt thn th orrsponing ons quir t rpm. Comprtiv msurmnt prision Soli Erth, 1, 5 8, 1

10 3 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Linr Fit: Y =.13 * X Avrg Y = 31.5 Rsiul sum of squrs = Rgrssion sum of squrs = 15.3 R-squr = msur run numr rpm Linr Fit: Y = * X Avrg Y =.587 Rsiul sum of squrs = Rgrssion sum of squrs = 9. R-squr =.395 rpm Osurtion (%) 8 1 msur run numr Osurtion (%) Linr Fit Y = * X Rsiul sum of squrs = Rgrssion sum of squrs = R-squr = msur run numr 8 1 msur run numr Linr Fit: Y = * X Rsiul sum of squrs =.833 Rgrssion sum of squrs = R-squr =.957 Dimtr (mm) Dimtr (mm) 8 D 1 D msur run numr f D 9 D 5 D 9 D msur run numr Fig. 1. Comprison twn msurmnt prision tst rsults prform on smpl CABRE3 t th pump sp vloity orrsponing to th mn imtr pk vlu of th pump sp tst (Fig. 3), n t th mximum pump sp, rsptivly. () Tst MP 5 prform on su-smpl liquot CABRE3 y th Hyro MU isprsion unit; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Tst MP 5 prform on su-smpl liquot CABRE3f y th Hyro MU isprsion unit; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. (f) Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. Not th vry lrg iffrn twn th vrg mn imtr otin from th first (31.5 µm) n th son tst (.587 µm), rsptivly. Both thm r fft y strong rirultion-rlt mhnil is. i tsts sign to invstigt th influn of msurmnt run tim wr prform t rpm pump sp n 1 s, 1 s, s, n s of msurmnt run tim, rsptivly. Th MP 1, tst on su-smpl liquot CABRE3g (Fig. 11) is hrtris y intns sttring of mn imtr vlus tht show n inrsing trn with inrsing th run numr (i.. tim). Intns sttring lso ours in D 5, n D 9 prntils n in th sn, silt n ly siz frtion t. Th slt grnulomtri urvs show highr vriility n non systmti trn, ompr to th orrsponing ons quir t 5 s of msurmnt run tim, s lso init y th orrsponing mol vlus (Fig. 11). For onstnt totl urtion of th msurmnt prision tst, inrsing th msurmnt run tim uss rs of mn imtr t sttring n mor linrly inrsing trns of lsr osurtion vlus (Fig. ). W lso rn MP 5 tst on su-smpl liquot CABRE3k y using th Cils 93 lsr iffrtion prtil siz nlysr. Rsults provi signifintly smllr mn imtr vlus with rspt to thos provi y th Mstrsizr, n ths vlus systmtilly rs through tim, s init y th vry goo linr st fit (Fig. 13). Plotting mn imtrs of tst MP 5 vrg vry fiv msurmnt runs, inits progrssiv rs of vlus with tim. In prtiulr, suh rs n fftivly fitt y n xponntil urv, n th highst vrition ours twn th first two points (Fig. 1). A similr trn hrtriss th orrsponing mol vlus, spit highr sttring (Fig. 1). A til of lsr osurtion t for th first tn runs shows vry slight, lmost linr inrs, whih rhs out 1% t th n of th tst (Fig. 1). Th orrsponing grnulomtri urvs init tht only th first n thir runs provi orsr istriutions, with mol pk of out 51 µm, whil th rmining ight ons Soli Erth, 1, 5 8, 1

11 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 35 5 L inr fit: Y = * X Avrg Y = 9.7 Rsiul sum of squrs = 9 Osurtion (%) 11 Dimtr (mm) 8 D Rgrssion sum of squrs = R-squr =.59 8 msur run numr urv 1 urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv L inr fit: Y =.8997 * X Rsiul sum of squrs =.5579 Rgrssion sum of squrs =.17 R-squr = msur run numr msur run numr Msurmnt run numr 1 8 ly siz silt siz sn siz D 5 D msur run numr Fig. 11. Rsults of th msurmnt prision tst MP 1 prform on su-smpl liquot CABRE3g y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. () Progrssion of D 1, D 5, n D 9 prntils uring th sm tst. () Grnulomtri urvs rprsnttiv of th prtil siz volution. Th orrsponing mol vlus (sm olour o) r illustrt in th inst grph. () Distriution of th ly, silt n sn siz frtions uring th tst. r quit similr n hv mol pk of out µm tht rmins unhng lso ftr 5 n 1 runs (Fig. 1). In prtiulr, th thir run urv provis th orsst istriution, n th orrsponing D 1, D 5, n D 9 prntils n mol vlu r outlirs with rspt to th ovrll trn of th othr t (Fig. 1 g). This vin qustions th vliity of th thir run t. Intrprttion of th msurmnt prision tst rsults Th msurmnt prision tst provi ontrsting rsults pning on th rok typ. Cront tlsti ris r snsitiv to th mtril rirultion tim (i.. th numr of msurmnt runs n/or th msurmnt run tim), whrs olin sn t rmins lmost unltr through tim. In prtiulr, in ront tlsti ris signifint iffrn ours twn th first run n th following ons, suggsting tht only short rirultion tims nsur smll mhnil is to prtil siz t from wt suspnsion nlyss. Ultrsonition tst An ultrsonition tst on olin sn ws prform on susmpl liquot SAND1, using th mximum ultrsonition pro tip isplmnt ( µm), 5 rpm of pump sp, n 5 s of msurmnt run tim (US 5 ). Mn imtrs rmin lmost onstnt in th first runs, with n vrg vlu of 7.8 µm, n thn sunly stps own to n vrg vlu of.3 µm in th rmining 73 runs of th tst. Th vrg vlu ovr 1 runs is.5 µm (Fig. 15). Lsr osurtion vlus inrs of out.5% uring th tst (Fig. 15). Whn only th first 1 grnulomtri urvs r ompr, thy show virtully onstnt mol pk t Soli Erth, 1, 5 8, 1

12 3 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 5 Linr Fit: Y = * X Avrg Y = Rsiul sum of squrs = Rgrssion sum of squrs = 53. R-squr = Linr Fit: Y = * X Avrg Y = 17. Rsiul sum of squrs = 13. Rgrssion sum of squrs = R-squr = Linr Fit: Y = * X Avrg Y = 7.3 Rsiul sum of squrs = 9.3 Rgrssion sum of squrs = 3.78 R-squr = msurmnt run tim = 1s 15 msurmnt run tim = s 1 msurmnt run tim = s Osurtion (%) msur run numr msur run numr msur run numr Fig.. Rsults of msurmnt prision tsts prform t iffrnt run tims on smpl CABRE3 y th Hyro MU isprsion unit. () Tst MP 1 on su-smpl liquot CABRE3h; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. () Tst MP on su-smpl liquot CABRE3i; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. () Tst MP on su-smpl liquot CABRE3j; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. (f) Lsr osurtion vlu progrssion uring th sm tst. 11 f out 59 µm. Th orrsponing volum prntg rops of out 1.75% from urv 7 onwr (Fig. 15). Mol vlus rmin lmost onstnt for th ntir tst, out n vrg vlu of 58.5 µm (Fig. 15). Contrsting ths 1 urvs from th ultrsonition tst, ginst th first on from th msurmnt prision tst on su-smpl liquot SAND1 inits ngligil iffrns (Fig. 15). Ultrsonition intnsitis of.5 µm, 5 µm, 1 µm, n µm of tip isplmnt wr ppli to th ront tlsti ri, using pump sp of rpm n 5 s of msurmnt run tim. Rsults init tht inrsing th ultrsoun nrgy uss (i) fstr rs of mn imtr vlus, whih psss from linr to powr lw st fit urvs, (ii) highr inrss of lsr osurtion, n (iii) rs of vrg mol vlus up to 1 µm, whih rmin lmost onstnt whn th mximum pro tip isplmnt is us (Fig. 1). Anlysis of grnulomtri urvs prtining to th first 1 runs n to runs 5 n 1 in h tst shows progrssivly inrsing iffrn twn first run urvs n th rmining ons with inrsing th ultrsonition pro tip isplmnt (Fig. 17). Morovr, shp iffrns mong urvs inrs, prtiulrly twn tst US.5 5 n th rmining ons, n th mol pk volum prntg of th ulk of th urvs in h tst rss with inrsing ultrsonition intnsity. Comprison of th first run urvs from tsts with n without ultrsonition shows tht th lttr provi signifintly orsr prtil siz istriution in th mol pk (Fig. 17). Th influn of ultrsonition is lso illustrt y th iffrn twn first-run mol vlus n thos vrg ovr th first 1 runs of th orrsponing tsts. Th grtr iffrn ours whn no ultrsonition ws us. Th smllr iffrn ours t th minimum ultrsonition intnsity n thn it inrss up to th US1 5 tst. Intrprttion of th ultrsonition tst rsults Rsults from ultrsonition tsts init ngligil ffts on olin sn, prtiulrly whn only th first 1 to runs r onsir, oring to th msurmnt prision Soli Erth, 1, 5 8, 1

13 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion Linr Fit: Y = * X Avrg Y = 1.1 Rsiul sum of squrs = Rgrssion sum of squrs = 88. R-squr = mm mm 13. mm 13.9 mm 1 3 msur numr Fig. 13. Rsults of msurmnt prision tsts prform on susmpl liquot CABRE3k y th Cils 93 lsr iffrtion prtil siz nlysr; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. tst vin. On th othr hn, in th ront tlsti ri su-smpl liquots, ultrsonition hs muh grtr influn using signifint prtil siz rutions ftr fw msurmnt runs, s init y th onomitnt rution of mn imtr n mo vlus, y th inrs of lsr osurtion, n y th inrs of volum prntgs in th.5 µm to 1 µm sgmnts of grnulomtri urvs. Evn ftr singl msurmnt run, ultrsonition is l to shift finwr th mol pk vlu of prtil siz istriutions y to 8 µm. 7 Chmil tst In wt nlyss, liqui isprsnts n wt mirofrturs n hlp ohsion loss, thus fvouring isintgrtion of mirofrtur prtils. Frtur prtur thrshols for pillrity prmility pn on th surf tnsion of th isprsnt liqui. Aoringly, isprsnt liquis with low surf tnsions r xpt to nhn prtil isintgrtion in tlsti mtrils, whrs this fft shoul ngligil for intt prtils. To tst this hypothsis, nturt thyl lohol ws us s isprsnt liqui for t quisition from olin sn y prforming MP5 5l, tst on su-smpl liquot SAND1. Rsults r vry onsistnt, s illustrt y th lmost onstnt mn imtr vlus, y th flt lying st fit lin of mo vlus, n y th vry similr grnulomtri urvs in th first 1 runs, whih provi n xtrmly goo ovrlp with th first urv from th sm tst using lifi tp wtr s isprsnt liqui (Fig. ). Th orrsponing mol vlus show n initil rs of lss thn 5 µm, rhing pltu vlu ftr runs. Two msurmnt prision tst wr prform on CABRE3p n CABRE3q su-smpl liquots, using nturt thyl lohol n minrlis wtr, rsptivly (Fig. 19). Th first tst provi quit sttr mn imtr n mo vlus, oth hrtriz y flt-lying st fit lins, whih r smllr thn th orrsponing ons otin from minrlis wtr of out 7 µm n 53 µm, rsptivly. Th inrs of lsr osurtion vlus is grtr for th isprsion in nturt thyl lohol. Anlysis of grnulomtri urvs prtining to th first 1 runs inits highr vriility for msurmnts quir in nturt thyl lohol, of oth urv shp n mol pk lvtion (Fig. 19g, h). Suh highr vriility is onfirm y th nlysis of th orrsponing mol vlus. Finlly, omprison with th first run urv from th sm tst using lifi tp wtr s isprsnt liqui, inits tht grnulomtri urvs otin from th nturt thyl lohol suspnsion hv muh grtr iffrns with rspt to th orrsponing ons quir using minrlis wtr s isprsnt liqui. Intrprttion of th hmil tst rsults Tst rsults init tht th us of nturt thyl lohol hs ngligil influn on t quisition in qurtz olin sn. Vritions of mn imtr n mo vlus r lss thn 5 µm, whih fll insi th vriility ssoit with su-smpling, vn in wll sort simnts lik un sns. On th othr hn, th sm isprsnt liqui uss rs of out 75 µm of mn imtr vlus whn ront tlsti ri is nlys. Th vin tht, whn minrlis wtr is us, rsults r vry similr to thos from th orrsponing tst in lifi tp wtr ruls out ny signifint is prou y su-smpling n supports prtil frgmnttion uring suspnsion rirultion. This is wll illustrt y th systmti rs of mol pk volums n siz, n y th orrsponing inrs of volum prntg vlus in th.5 µm to 11 µm sgmnts of grnulomtri urvs in Fig. 19g. Highr vritions ours ftr only two runs. It is worth noting tht mny othr isprsnts oul us, s wll s vrious prtrtmnts. Howvr, prforming til invstigtions on this is out of our purposs in this ppr. 8 Rprossing tst Th first run of th MP5 5 tst ws slt for t rprossing following fvourl hviour in prvious tsts. Chnging RI vlus from 1. to 1.8 uss ngligil ffts in olin qurtz sn (su-smpl liquot SAND1), s illustrt in Fig.. Th orrsponing grnulomtri urvs lmost prftly ovrlp n prntils n mol Soli Erth, 1, 5 8, 1

14 38 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion nlysis tim (s) Osurtion (%) 1 Msur n Dimtr (mm) 8 D 9 D nlysis tim (s) Dimtr (mm) Msurmnt numr 3.5 D 1 3 f urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 urv 5 urv Msurmnt numr 5 8 g Msurmnt run numr Fig. 1. Anlysis of t from th tst MP 5 on -smpl liquot CABRE3 (Fig. 9). () Mn imtr vlus vrg vry fiv msurmnt runs. () Avrg mol vlus orrsponing to t in (). In oth ss, th st fits init n xponntil y. () Lsr osurtion vlus ror uring th first 1 runs (lk ots), ompr with th vlus ftr 5 (r ot) n 1 (lu ot) msurmnt runs. () Grnulomtri urvs omput for th first 1 runs, ompr with th ons from th 5th n 1th run. () Progrssion of D 5 n D 9 prntils uring th first 1 msurmnt runs. Dt ftr 5 (r ot) n 1 (lu ot) runs r provi for omprison. (f) Progrssion of D 1 prntils uring th first 1 msurmnt runs. Dt ftr 5 (r ot) n 1 (lu ot) runs r provi for omprison. (g) Progrssion of mol vlus uring th first 1 msurmnt runs (olour o s in ()). Dt ftr 5 (gry ot) n 1 (lk ot) runs r provi for omprison. vlus show vry smll vriility. Th sm rsult ws otin whn vrying ABS vlus from 1. to.1 (Fig. 1). Chnging RI in ront tlsti ri (first run of tst MP 5 on su-smpl liquot CABRE3) uss som vriility in th orrsponing grin siz istriutions, prtiulrly from RI = 1. to RI = 1. (Fig. ). Anlysis of rsiuls ssoit with st fit urvs inits tht th most pproprit RI vlu is 1.. Highr vlus, howvr, o not signifintly influn th omput prtil siz istriutions, s lowr vlus o prtiulrly for th volum prntg of sizs lowr thn out µm (Fig. ). Th mjor fft of hnging ABS vlus from 1. to.1 on CABRE mtril is to progrssivly shortn th til of grnulomtri urvs, from out.5 µm (ABS = 1..5) to. µm whn ABS =.1 (Fig. 3). For ABS lowr thn 1., rsing prtil sorption uss n inrs of prntil Soli Erth, 1, 5 8, 1

15 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion L inr fit on th first runs Y =.8179 * X Avrg Y = R-squr =.8513 Linr fit on th rmining 73 t Y = * X Avrg Y =. R-squr = Linr fit: Y = * X Avrg Y =.9 Rsiul sum of squrs = Rgrssion sum of squrs = 113. R-squr = msur numr urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 urv 1 no US Osurtion (%) msur numr 8 7 L inr fit: Y = * X Avrg Y = Rsiul sum of squrs = 1.93 Rgrssion sum of squrs = R-squr = msur numr Fig. 15. Rsults of th ultrsonition tst US 5 prform on su-smpl liquot SAND1 y th Hyro MU isprsion unit. () Mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi for th umultiv tst, for th first runs, n for th rmining 73 runs, rsptivly. () Lsr osurtion vlu progrssion uring th sm tst. () Grnulomtri urvs omput for th first 1 runs, ompr with th first urv from th tst MP5 5 on su-smpl liquot SAND1 (Fig. 8). Progrssion of mol vlus with inrsing th numr of msurmnt runs. Dt sttistis r provi. vlus n rs of mol vlus. Anlysis of rsiuls ssoit with st fit urvs inits tht th most pproprit ABS vlu is.1. Finlly, hnging th RI vlus of th isprsnt liqui hs ngligil ffts on olin qurtz sn, n n influn on CABRE mtril tht is omprl to wht is prou y hnging RI of ront prtils (Fig. ). Intrprttion of rprossing tst rsults Rsults of ths tsts init tht in th s of th nlyz mtrils, th snsitivity of light sttring t rprossing y th Mi thory is minly govrn y th prtil siz rng, rthr thn y thir optil proprtis. In ft, th vry goo sorting of smpl SAND1 rsults in virtully insnsitiv hviour to rprossing, whil th lrg spnning of sizs in CABRE3 nhns th snsitivity of prtils finr tht out µm. 9 Disussion Rsults illustrt ov init tht prtils with iffrnt strngth rspon in vry iffrnt wy to th sm tsting strtgy uring prtil siz trmintion y lsr iffrtion. Qurtz olin sn provi virtully intil prtil siz istriutions rgrlss of th opt oprting prour. On th othr hn, ront tlsti ri is vry snsitiv to oprting prours. Suh ontrst inits tht th vriility ssoit with th smpl CABRE3 os not pn on instrumntl is, ut inst it rlts to th pulir fri of tlsti roks riv from mssiv protoliths lik pltform ronts. Soli Erth, 1, 5 8, 1

16 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 5 3 Linr Fit: Y = * X Avrg Y = Rsiul sum of squrs = 3919 Rgrssion sum of squrs = 37. R-squr = Osurtion (%) Powr Lw Fit: Y = pow(x,.378) * Rsiul sum of squrs =.7981 Rgrssion sum of squrs = R-squr = Sigm-ht-sq' =.9395E- 1 5 L inr fit: Y = * X Avrg Y = 3.8 Rsiul sum of squrs = 333. Rgrssion sum of squrs = 115. R-squr = US =.5 mm 8 msur numr msur numr msur numr Powr Lw Fit Y = pow(x, ) *.3531 Rsiul sum of squrs = Rgrssion sum of squrs = R-squr =.5 US = 5. mm 8 1 msur numr US = 1. mm 8 1 msur numr Powr Lw Fit: Y = pow(x, ) * Rsiul sum of squrs = 1.9 Rgrssion sum of squrs = 1.95 R-squr = Powr Lw Fit: Y = pow(x, ) * Rsiul sum of squrs =.859 Rgrssion sum of squrs =.7871 R-squr =.5571 US =. mm 8 1 msur numr g l Osurtion (%) Osurtion (%) Osurtion (%) Powr Lw Fit: Y = pow(x, ) * Rsiul sum of squrs = Rgrssion sum of squrs =.113 R-squr = msur numr msur numr 1 1 Powr Lw Fit: Y = pow(x, ) * Rsiul sum of squrs = Rgrssion sum of squrs = R-squr =.995 Powr Lw Fit Y = pow(x, ) * Rsiul sum of squrs =.17 Rgrssion sum of squrs =.8 R-squr = m msur numr h L inr fit: Y = * X Avrg Y = Rsiul sum of squrs = Rgrssion sum of squrs = R-squr = msur numr L inr fit: Y = * X Avrg Y = 31.7 Rsiul sum of squrs = Rgrssion sum of squrs = 3.9 R-squr = msur numr L inr fit: Y = * X Avrg Y = Rsiul sum of squrs = 1979 Rgrssion sum of squrs = R-squr = n 8 1 msur numr Fig. 1. Ultrsonition tsts on smpl CABRE3 y th Hyro MU isprsion unit. () Ultrsonition tst US.5 5 prform on su-smpl liquot CABRE3l; mn imtr vlu volution with inrsing th numr of msurmnt runs. () Lsr osurtion vlu progrssion uring th sm tst. () Mo vlu progrssion uring th sm tst. () Ultrsonition tst US5 5 prform on su-smpl liquot CABRE3m; mn imtr vlu volution with inrsing th numr of msurmnt runs. () Lsr osurtion vlu progrssion uring th sm tst. (f) Mo vlu progrssion uring th sm tst. (g) Ultrsonition tst US1 5 prform on su-smpl liquot CABRE3n; mn imtr vlu volution with inrsing th numr of msurmnt runs. (h) Lsr osurtion vlu progrssion uring th sm tst. (i) Mo vlu progrssion uring th sm tst. (l) Ultrsonition tst US 5 prform on su-smpl liquot CABRE3o; mn imtr vlu volution with inrsing th numr of msurmnt runs. (m) Lsr osurtion vlu progrssion uring th sm tst. (n) Mo vlu progrssion uring th sm tst. Dt sttistis r provi for ll plots. f i Soli Erth, 1, 5 8, 1

17 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 1 urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 urv 5 urv 1 US =.5 mm urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 US = 5 mm urv 5 urv urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 US = 1 mm urv 5 urv 1 urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 US = mm urv 5 urv no US US US.5 5 US 1 US US =.5 mm US = 5 mm US = 1 mm US = mm no US Fig. 17. () Grnulomtri urvs omput for th first 1 runs of tst US.5 5 prform on su-smpl liquot CABRE3l, ompr with th ons from th 5th n 1th run. () Grnulomtri urvs omput for th first 1 runs of tst US5 5 prform on su-smpl liquot CABRE3m, ompr with th ons from th 5th n 1th run. () Grnulomtri urvs omput for th first 1 runs of tst US1 5 prform on su-smpl liquot CABRE3n, ompr with th ons from th 5th n 1th run. () Grnulomtri urvs omput for th first 1 runs of tst US 5 prform on su-smpl liquot CABRE3o, ompr with th ons from th 5th n 1th run. () First run grnulomtri urvs from th four tsts list ov, ompr with th first run urv from tst MP 5 on su-smpl liquot CABRE3 (Fig. 9). Th inst grph shows th mol vlus of th sm first run uvs (fill ots, sm olour o) ompr with mol vlus vrg ovr th first 1 runs of th orrsponing tsts (mpty ots, sm olour o). Soli Erth, 1, 5 8, 1

18 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 5 3 Linr Fit: Y = * X Avrg Y = 8.39 Rsiul sum of squrs = Rgrssion sum of squrs =.851 R-squr = Sigm-ht-sq' = msurmnt run numr Osurtion (%) msurmnt run numr L inr fit: Y =.555 * X Avrg Y = 57.8 Rsiul sum of squrs = Rgrssion sum of squrs =.5397 R-squr = msurmnt run numr urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 urv 1 tp wtr 7 Avrg Y = Msurmnt run numr Fig.. Rsults of th hmil tst MP5 5l prform on su-smpl liquot SAND1 y th Hyro MU isprsion unit, using nturt thyl lohol s isprsnt liqui. () Mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis is provi. () Lsr osurtion vlu progrssion uring th sm tst. () Progrssion of mol vlus with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Grnulomtri urvs omput for th first 1 runs, ompr with th first urv from th tst MP5 5 on su-smpl liquot SAND1 (Fig. 8). () Mol vlus orrsponing to th urvs in (). In ft, in this s prtils r prou y multipl frturing, rolling n grining of mtril within fult zons (.g. Borg t l., 19; Storti t l., 3; Smmis n Bn Zion, 8). Prtil siz pns on th rltiv strngth istriution long lvg n mirofrtur sts s funtion of th ppli strss (.g. Smmis t l., 1987). Aoringly, th mhnil hviour of ths ront tlsti prtils n ompr to tht of simntry prtils m of ohsiv ggrgt grins. Convrsly, multipl ollisions of qurtz prtils uring olin trnsport long ostl uns nsurs fftiv xploiting of prxisting flws. Th rsulting roun prtils r strong nough for ing not signifintly influn y mhnil soliittions in lsr iffrtion prtil siz nlysrs. It follows tht trmining th pproprit oprting prour rs funmntl importn for hvily mirofrtur mtrils, whil it hs sonry fft whn high strngth prtils r nlys. In th lttr s, only pump sp n influn th finl rsults y not nsuring fftiv prtil rirultion in th isprsion unit. Howvr, givn th high strngth of this mtril, pump sp vlus los or highr thn hlf of mximum sp (.g. 3 rpm) n us without xpting ny signifint mhnil is. On th othr hn, oprting prours s lss invsiv s possil r rquir whn nlysing frgil grnulr mtrils. In this s, fining th propr nlytil workflow nfits of som gnrl guilins for ro smpl tgoris, follow y furthr spifi rfinmnts. Morovr, slting n fftiv instrumnttion plys funmntl rol to trmin prtil siz istriutions of frgil mtrils. Aoring to our tsts, pristlti pumping uring smpl rirultion introus systmti is to th finl rsults n, onsquntly, lsr iffrtion nlysrs opting this thnil solution r inpproprit. On th othr hn, ntrifugl pumping provis muh mor flxil n fftiv solution for nlysing frgil mtrils. Btwn th two Mlvrn isprsion units w us, th lrg volum Hyro MU nsur fftiv smpl rirultion t lowr pump sp vlus ompr to th Hyro S. Soli Erth, 1, 5 8, 1

19 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion 3 Osurtion (%) 5 17 Linr Fit: Y = * X +.53 Avrg Y = 9. Rsiul sum of squrs = Rgrssion sum of squrs = 5.8 R-squr = msurmnt run numr 15 Powr Lw Fit: Y = pow(x,.1793) * Rsiul sum of squrs =.31 Rgrssion sum of squrs =.53 R-squr =.95 L inr fit: Eqution Y = * X Avrg Y = Rsiul sum of squrs = Rgrssion sum of squrs = 33. nturt thyli R-squr =.1953 lohol msurmnt run numr msurmnt run numr msurmnt run numr Osurtion (%) 5 Linr Fit: 1 5 Y =.7538 * X Powr Lw Fit: Avrg Y =.8 Y = pow(x, ) * Rsiul sum of squrs = 377. Rsiul sum of squrs =.7 Rgrssion sum of squrs = Rgrssion sum of squrs =.359 R-squr =.1991 R-squr = Linr fit: Eqution Y = * X Avrg Y = Rsiul sum of squrs = Rgrssion sum of squrs = R-squr =. 1 minrlis wtr 8 1 msurmnt run numr msurmnt run numr f urv 1 urv urv 3 urv urv 5 urv urv 7 urv 8 urv 9 urv 1 urv 1 tp wtr Msurmnt run numr g h Fig. 19. Rsults of hmil tsts prform on smpl CABRE3 y th Hyro MU isprsion unit. () Tst MP 5l prform on su-smpl liquot CABRE3p using nturt thyl lohol s isprsnt liqui; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. () Progrssion of mol vlus with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Tst MP 5w prform on su-smpl liquot CABRE3q using minrlis wtr s isprsnt liqui; mn imtr vlu volution with inrsing th numr of msurmnt runs. Dt sttistis r provi. () Lsr osurtion vlu progrssion uring th sm tst. Dt sttistis r provi. (f) Progrssion of mol vlus with inrsing th numr of msurmnt runs. Dt sttistis r provi. (g) Grnulomtri urvs omput for th first 1 runs in (), ompr with th first urv from th tst MP 5 on su-smpl liquot CABRE3 (Fig. 9). (h) Grnulomtri urvs omput for th first 1 runs in (), ompr with th first urv from th tst MP 5 on su-smpl liquot CABRE3 (Fig. 9). Th inst grph show th omprison twn mol vlus orrsponing to th urvs in (g) (fill ots) n in (h) (mpty ots). Soli Erth, 1, 5 8, 1

20 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion D 9 (mm) RI = 1. RI = 1.5 RI = 1. RI = 1.7 RI = Rfrtiv inx Rfrtiv inx Rfrtiv inx Rfrtiv inx Fig.. Rprossing of th first run t from tst MP5 5 on su-smpl liquot SAND1 (Fig. 8). () Light sttring t (lk urv) n orrsponing st fits for vril RI vlus of qurtz from 1. to 1.8 (olour o in ()), onstnt ABS vlus of qurtz =.1, n onstnt RI vlus of lifi tp wtr = () Grnulomtri urvs omput from rpross t in (). () D 1 prntils for t in th 5 urvs illustrt in (). () D 5 prntils for t in th 5 urvs illustrt in (). () D 9 prntils for t in th 5 urvs illustrt in (). (f) Mol vlus for t in th 5 urvs illustrt in (). It is worth noting tht hnging RI of qurtz prous ngligil hngs in th rpross t. D 1 (mm) D 5 (mm) f Finlly, it is worth noting tht, spit th fftivnss of sttistil prmtrs lik mn imtr, prntils, n othrs, thy nnot rpl th us of grnulomtri urvs for ompring rsults from iffrnt tsts. This us vry similr vrg vlus n rlt to vry iffrnt grnulomtri urvs (.g. Slly, ). 1 Conlusions Prtil siz istriutions signifintly ontriut to th sription of mny gologil prosss inluing simnttion, rok frgmnttion n soil formtion. Morn lsr iffrtion prtil siz nlysrs nsur fst t quisition ovr wi siz rng, oupl with th pproprit flxiility for nlysing vry iffrnt grnulr mtrils. This flxiility, howvr, n prou svrly is rsults whn inpproprit nlytil oprting prours r us, prtiulrly on frgil mtrils. W nlys oth high strngth (olin qurtz sn) n low strngth (ront tlsti ri) ssntilly monominrli mtrils to tst th impt of iffrnt nlytil oprting prours involving prtil isprsion into liqui, on th otin prtil siz istriutions. Our rsults n summris y th following points: 1. ntrifugl pumping th prtil-liqui ilut isprsion t th most pproprit pump sp is ruil in wt nlyss of grnulr mtril to prvnt (i) rmti unrstimting orsr prtils whn Soli Erth, 1, 5 8, 1

21 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion D 1 (mm) D 9 (mm) ABI = 1. ABI =.5 ABI =.1 ABI =.5 ABI = Prtil sorption Prtil sorption D 5 (mm) Prtil sorption Prtil sorption Fig. 1. Rprossing of th first run t from tst MP5 5 on su-smpl liquot SAND1 (Fig. 8). () Light sttring t (lk urv) n orrsponing st fits for onstnt RI vlus of qurtz = 1.5, vril ABS vlus of qurtz from.1 to 1. (olour o in ()), n onstnt RI vlus of lifi tp wtr = () Grnulomtri urvs omput from rpross t in (). () D 1 prntils for t in th 5 urvs illustrt in (). () D 5 prntils for t in th 5 urvs illustrt in (). () D 9 prntils for t in th 5 urvs illustrt in (). (f) Mol vlus for t in th 5 urvs illustrt in (). It is worth noting tht hnging lso ABS of qurtz prous ngligil hngs in th rpross t. f infftiv pumping n stirring llow prtil simnttion; (ii) ovrstimting orsr prtils whn infftiv pumping n stirring llow trnsint prtil stgntion within th msurmnt ll; (iii) unrstimting orsr prtils whn fst pumping n stirring prou signifint prtil siz rution in low strngth mtril uring msurmnt running;. high strngth mtril is not signifintly influn y th opt instrumnttion n stnr oprting prour, provi tht fftiv smpl rirultion is otin in th isprsion unit; 3. ing ultrsonition in wt nlyss of low strngth mtril systmtilly uss mhnil prtil siz rution uring msurmnt tht, howvr, is lss fftiv thn tht us y fst pumping n stirring uring smpl rirultion n minly prous vry fin prtils y polishing of th lrgr ons;. in low strngth mtril, th numr of vrg msurmnt runs hs to rfully trmin y sttistil t nlysis of lrg tsts in orr to nsur roust outputs n minimiz mhnil ising of prtil siz uring rirultion in th isprsion unit; 5. Slting pproprit optil proprtis for th nlys smpl mtril n isprsnt liqui, rsptivly, is prtiulrly importnt for fin n vry fin prtils, s orsr prtils r lss fft y this prmtr. Soli Erth, 1, 5 8, 1

22 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion D 9 (mm) D 1 (mm) RI = 1. RI = 1.5 RI = 1. RI = 1.7 RI = Rfrtiv inx Rfrtiv inx D 5 (mm) Rfrtiv inx Rfrtiv inx Fig.. Rprossing of th first run t from tst MP 5 on su-smpl liquot CABRE3 (Fig. 9). () Light sttring t (lk urv) n orrsponing st fits for vril RI vlus of lium ront from 1. to 1.8 (olour o in ()), onstnt ABS vlus of lium ront =.1, n onstnt RI vlus of lifi tp wtr = () Grnulomtri urvs omput from rpross t in (). () D 1 prntils for t in th 5 urvs illustrt in (). () D 5 prntils for t in th 5 urvs illustrt in (). () D 9 prntils for t in th 5 urvs illustrt in (). (f) Mol vlus for t in th 5 urvs illustrt in (). f W propos workflow s guilin for rssing prtil siz trmintions y lsr iffrtion grnulomtry. Applition of this prour is typilly flxil u to th grt vriility of nlys mtrils n th ommon n of svrl itrtions for rhing th most sttistilly roust rsults. Systmti support of lsr iffrtion grnulomtri t y prliminry tst rsults prform to slt th opt oprting prour is nssry. Th lk of informtion on this n ontriut to misling t intrprttion n t omprison. Aknowlgmnts. W r grtful to R. M. Jokl, J. Mson, n A. Young for thir hlpful rviws of th sumitt mnusript. Construtiv ritiism n vi from T. Blnkinsop n S. Blott on n rly vrsion of th mnusript wr vry usful for signifintly improving it. Funing for this work ws provi y th Rom Tr Univrsity Lortory Upgr Progrmm, grnts to F. Storti, n y th Itlin MIUR (Ministro ll Istruzion, ll Univrsità ll Rir). L. Alg, C. Gimpolo n S. Lo Mstro kinly provi th omposition of th Privrno sn y X-ry iffrtion. W r grtful to Mlvrn Instrumnts Lt. (prtiulrly to B. Flour, P. Kippx n A. Virn) n to Alftst s.r.l. (prtiulrly to M. Congi n V. Polhi) for thir thnil support n vi. Eit y: R. M. Jokl Soli Erth, 1, 5 8, 1

23 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion D 9 (mm) D 1 (mm) ABI = 1. ABI =.5 ABI =.1 ABI =.5 ABI =.1 7 Prtil sorption Prtil sorption Prtil sorption Prtil sorption Fig. 3. Rprossing of th first run t from tst MP 5 on su-smpl liquot CABRE3 (Fig. 9). () Light sttring t (lk urv) n orrsponing st fits for onstnt RI vlus of lium ront = 1., vril ABS vlus of lium ront from.1 to 1. (olour o in ()), n onstnt RI vlus of lifi tp wtr = () Grnulomtri urvs omput from rpross t in (). () D 1 prntils for t in th 5 urvs illustrt in (). () D 5 prntils for t in th 5 urvs illustrt in (). () D 9 prntils for t in th 5 urvs illustrt in (). (f) Mol vlus for t in th 5 urvs illustrt in () D 5 (mm) f Rfrns Agrwl, Y. C., MCv, I. N., n Rily, J. B.: Lsr iffrtion siz nlysis, in: Prinipls, Mthos n Applition of Prtil Siz Anlysis, it y: Syvitski, J. P. M., Cmrig Univrsity Prss, Cmrig, 119 8, Anglui, A. n Plmrini, V.: Stuio simntologio ll si ross i Privrno (Lzio su-ointl), Gologi Romn, 3, 3 5, 191. Buslink, L., Govrs, G., Posn, J., Dgrr, G., n Froyn, L.: Grin-siz nlysis y lsr iffrtomtry: omprison with th siv-piptt mtho, Ctn, 3, 193 8, Blott, S. J., Croft, D. J., Py, K., Sy, S. E., n Wilson, H. E.: Prtil siz nlysis y lsr iffrtion, in: Fornsi Gosin: Prinipls, Thniqus n Applitions, it y: Py, K. n Croft, D. J., Gologil Soity, Lonon, Spil Pulition, 3, 3 73,. Blott, S. J. n Py, K.: Prtil siz istriution nlysis of snsiz prtils y lsr iffrtion: n xprimntl invstigtion of instrumnt snsitivity n th ffts of prtil shp, Simntology, 53, 71 85,. Borg, I., Frimn, M., Hnin, J., n Higgs, D. V.: Exprimntl formtion of S. Ptr sn: stuy of tlsti flow, Gol. So. Am. Mm., 79, , 19. D Agostino, N., Chmot-Rook, N., Funiillo, R., Jolivt, L., n Sprnz, F.: Th rol of pr-xisting thrust fults n topogrphy on th styls of xtnsion in th Grn Ssso rng (ntrl Itly), Ttonophysis, 9, 9 5, Bor, G. B. J., Wr, C., Thons, D., n Goossns, H. W. J.: Lsr iffrtion sptromtry: Frunhofr iffrtion vrsus Mi sttring, Prtil Chrtriztion,, 138 1, Englr, J. T.: Ctlsis n th gnrtion of fult goug, Gol. So. Am. Bull. 85, , Soli Erth, 1, 5 8, 1

24 8 F. Storti n F. Blsmo: Prtil siz istriutions y lsr iffrtion isprsnt RI = 1.33 isprsnt RI = 1.3 isprsnt RI = 1.39 isprsnt RI = 1. isprsnt RI = 1.5 isprsnt RI = 1.33 isprsnt RI = 1.3 isprsnt RI = 1.39 isprsnt RI = 1. isprsnt RI = Fig.. () Grnulomtri urvs otin y rprossing th first run t from tst MP5 5 on su-smpl liquot SAND1 (Fig. 8) using qurtz RI = 1.5, qurtz ABS =.1, n vril RI vlus of lifi tp wtr from 1.33 to 1.5. () Grnulomtri urvs otin y rprossing th first run t from tst MP 5 on su-smpl liquot CABRE3 (Fig. 9) using lium ront RI = 1., qurtz ABS =.1, n vril RI vlus of lifi tp wtr from 1.33 to 1.5. Frimn, G. M.: Diffrns in siz istriutions of popultions of prtils mong sns of vrious origins, Simntology,, 3 3, Irni, R. R. n Cllis, C. F.: Prtil siz: msurmnts, intrprttion, n pplition, John Wily n Sons, Nw York, 193. Krumin, W. C.: Msurmnt n gologi signifin of shp n rounnss of simntry prtils, J. S. Ptr., 11, 7, 191. Loizu, J. L., Arouill, D., Sntigo, S., n Vrnt, J. P.: Evlution of wi rng lsr iffrtion grin siz nlyzr for us with simnts, Simntology, 1, , 199. Mson, J. A., Jos, P. M., Grn, R. S. B. n Nttlton, W. D.: Simntry ggrgts in th Pori Loss of Nrsk, USA, Ctn, 53, , 3. MCv, I. N., Brynt, R. J., Cook, H. F., n Coughnowr, C. A.: Evlution of lsr-iffrtion-siz nlyzr for us with nturl simnts, J. S. Ptr., 5, 51 5, 198. Py, K. n Blott, S. J.: Prtil siz nlysis of simnts, soils n rlt prtiult mtrils for fornsi purposs using lsr grnulomtry, Fornsi Sin Int., 1, 19 7,. Riu, M. n Sposito, G.: Frtl frgmnttion, soil porosity n soil wtr proprtis: I. Thory, Soil Si. So. Am. J., 55, 31 38, Smmis, C. G. n Bn Zion, Y.: Mhnis of grin-siz rution in fult zons, J. Gophys. Rs., 113, B3, oi:1.9/jb89, 8. Smmis, C. G., King, G., n Bigl, R.: Th kinmtis of goug formtion, Pur Appl. Gophys., 5, 777 8, Slly, R. C.: Appli Simntology, son ition, Ami Prss, Sn Digo,. Shrin, M. F., Wohltz, K. H., n Dhn, J.: Disrimintion of grin-siz su-popultions in pyrolsti posits, Gology, 15, 37 37, Sprzz, M., Moor, J. N., n Hnrix, M. S.: High-rsolution prtil siz nlysis of nturlly ourring vry fin-grin simnt through lsr iffrtomtry, J. Sim. Rs., 7, 73 73,. Storti, F. n Blsmo, F.: Impt of phmrl tlsti fris on lsr iffrtion prtil siz istriution nlysis in loos ront fult ri, J. Strut. Gol., in prss, 1. Storti, F., Billi, A., n Slvini, F.: Prtil siz istriutions in nturl ront fult roks: insights for non-slf-similr tlsis, Erth Plnt. Si. Ltt.,, 173, 3. Wnogho, S., Gttiny, G., n Cy, B.: Prtil siz istriution nlysis of soils using lsr iffrtion, Fornsi Si. Int., 33, 117 8, Wiss, E. L. n Frok, H. N.: Rpi nlysis of prtil-siz istriutions y lsr light sttring, Powr Thnol., 1, 87 93, 197. Soli Erth, 1, 5 8, 1