Standard Operating Procedure

NRCWE SOP for measurement of hydrodynamic Size-

Title Distribution and Dispersion Stability by Dynamic Light
Scattering (DLS)
Subtitle NA
NANoREG Work
WP2 Synthesis, supplying and characterization
package/task:
Keld Alstrup Jensen, (National Research Centre for the Working
Owner and co-owner(s)
Environment)
Date finalised
NANoREG D2.08 SOP 02 For measurement of hydrodynamic
Document name
Size-Distribution and Dispersion Stability by DLS
Key words:

Version Date Reason of change

This work is licensed under the Creative Commons Attribution-NonCommercial-ShareAlike 4.0

International License.
To view a copy of this license, visit http://creativecommons.org/licenses/by-nc-sa/4.0/ or send
a letter to Creative Commons, PO Box 1866, Mountain View, CA 94042, USA.

This project has received funding from the European Union

Seventh Framework Programme (FP7/2007-2013)
under grant agreement no 310584
 

NRCWE SOP for measurement of hydrodynamic Size-Distribution and Dispersion
Stability by Dynamic Light Scattering (DLS)

.H\ZRUGV'/6K\GURG\QDPLFGLDPHWHUDYHUDJH]HWDVL]H3',VL]HGLVWULEXWLRQLQWHQVLW\VWDELOLW\
Introduction
7KH SXUSRVH RI WKLV 623 6WDQGDUG 2SHUDWLRQ 3URFHGXUH LV WR JLYH D EDVLF LQWURGXFWLRQ WR G\QDPLF OLJKW
VFDWWHULQJ PHWKRG DQG WKH 1$1R5(* SURFHGXUH IRU PHDVXUHPHQW RI WKH K\GURG\QDPLF VL]HGLVWULEXWLRQV RI
VWRFNGLVSHUVLRQVDQGH[SRVXUHPHGLDDQGWKHLUVWDELOLWLHV
7KHFXUUHQW623LVEDVHGRQDSUHYLRXV623UHSRUWHGLQ1$12*(1272;-HQVHQHWDO

Basic explanation of the DLS method
'\QDPLF /LJKW 6FDWWHULQJ '/6 DOVR FDOOHG 3KRWRQ &RUUHODWLRQ 6SHFWURVFRS\ 3&6 RU 4XDVL(ODVWLF /LJKW
6FDWWHULQJ4(/6 LVDWHFKQLTXHIRUFKDUDFWHUL]DWLRQRIFROORLGDOV\VWHPVEDVHGRQWKHVFDWWHULQJRI YLVLEOH
OLJKW UHVXOWLQJ IURP WKH GLIIHUHQFH LQ UHIUDFWLYH LQGH[ EHWZHHQ WKH GLVSHUVHG FROORLGV DQG WKH GLVSHUVLRQ
PHGLXP7KHPHWKRGPD\EHDSSOLHGIRUVL]LQJSDUWLFOHVXVSHQGHGLQDOLTXLGLQWKHUDQJHIURPDERXWQP
WRDERXWPPGHSHQGLQJRQWKHLQVWUXPHQWDWLRQRSWLFDOSURSHUWLHVRIPDWHULDOPHGLXPDQGVRIWZDUH
7KHSULQFLSOHLQ'/6LVPHDVXUHPHQWRIIOXFWXDWLRQVLQODVHUOLJKWVFDWWHUHGE\YLEUDWLQJSDUWLFOHVVXVSHQGHGLQ
DOLTXLGDVIXQFWLRQRIWLPH7KHYLEUDWLRQLVGXHWR%URZQLDQPRWLRQFDXVHGE\FROOLVLRQZLWKVROYHQWPROHFXOHV
RIWKHOLTXLG7KH%URZQLDQPRWLRQYDULHVDVDIXQFWLRQRISDUWLFOHVL]HDQGFDXVHVYDULDWLRQLQWKHLQWHQVLW\RI
VFDWWHUHG OLJKW DV IXQFWLRQ RI WLPH $ FRUUHODWRU FRPSDUHV WKH VLJQDO DV IXQFWLRQ RI WLPH WL XVLQJ WKH LQLWLDO
VLJQDODWWDVUHIHUHQFH7KHUHVSRQVHLVDUHODWLYHVLJQDOFRPSDUDELOLW\ZLWKGLIIHUHQWYHU\VKRUWWLPHLQWHUYDOV
GWWKHVRFDOOHGDXWRFRUUHODWLRQ$VWKHSDUWLFOHVPRYHWKHFRUUHODWLRQEHWZHHQWDQGVXEVHTXHQWGWVLJQDOV
GHFUHDVHVZLWKWLPHIURPDSHUIHFWFRUUHODWLRQDWWWRDFRPSOHWHGHFRUUHODWLRQDWLQILQLWHWLPHRUGHURI
PLOOLVHFRQGV,QFDVHRIELJSDUWLFOHVWKHVLJQDOFKDQJHVVORZO\DQGWKHFRUUHODWLRQ SHUVLVWVIRUDORQJWLPH
ZKHUHDVVPDOOSDUWLFOHVKDYHKLJK%URZQLDQPRYHPHQWFDXVLQJUDSLGGHFRUUHODWLRQ
,Q IDFW D '/6 LQVWUXPHQW PHDVXUHV WKH YHORFLW\ RI %URZQLDQ PRWLRQ GHILQHG E\ WKH WUDQVODWLRQDO GLIIXVLRQ
FRHIILFLHQW ' RI WKH SDUWLFOHV 7KH SDUWLFOH VL]H RU PRUH SUHFLVHO\ LWV K\GURG\QDPLF GLDPHWHU G+ LV WKHQ
HVWLPDWHGXVLQJWKH6WRNHV(LQVWHLQHTXDWLRQDVVXPLQJVSKHULFDOVKDSH
N7
G+ 
SK'
N%ROW]PDQQ¶VFRQVWDQW
'WUDQVODWLRQDOGLIIXVLRQFRHIILFLHQW
7DEVROXWHWHPSHUDWXUH
ȘYLVFRVLW\

,WVKRXOGEHQRWHGWKDWHYHQLIDSDUWLFOHLVUHDOO\VSKHULFDOWKHVSKHULFDO'/6VL]HLVIXQGDPHQWDOO\GLIIHUHQW
IURPWKHSK\VLFDOVSKHULFDOVL]H7KHK\GURG\QDPLFVL]HLQFOXGHVWKHGRXEOHOD\HUZLWKKLJKO\SRODUL]HGZDWHU
PROHFXOHV DURXQG WKH SK\VLFDO SDUWLFOH :KHQ WKH SDUWLFOH PRUSKRORJ\ LV KLJKO\ QRQVSKHULFDO WKH
K\GURG\QDPLF VL]H VKRXOG EH XQGHUVWRRG DV WKH HTXLYDOHQW K\GURG\QDPLF VSKHULFDO VL]H 6LPLODU FRQFHSW LV
XVHGLQDHURG\QDPLFPHDVXUHPHQWRIDLUERUQHSDUWLFOHV(VWDEOLVKPHQWRIPHDQK\GURG\QDPLFVL]HDQGVL]H
GLVWULEXWLRQV LQWHQVLW\ QXPEHU YROXPH LV UHDFKHG E\ '76 VRIWZDUH DOJRULWKPV E\ ILWWLQJ WKH FRUUHODWLRQ
IXQFWLRQFIGDWDWUHDWPHQWVHFWLRQ
6DPSOHVIRU'/6DUHPHDVXUHGLQWUDQVSDUHQWFXYHWWHVRIJODVVRUSRO\PHU'/6PHDVXUHPHQWVUHO\RQWKH
QRQLQYDVLYH EDFNVFDWWHU 1,%6Š WHFKQRORJ\ GHYHORSHG E\ 0DOYHUQ ,QVWUXPHQWV LQ ZKLFK WKH VLJQDO LV
GHWHFWHGDWƒ)LJXUH7KHVLJQDOLVWUHDWHGE\DGLJLWDOFRUUHODWRUDQGWUDQVPLWWHGWRWKHFRPSXWHU7KH
'76 VRIWZDUH HQDEOHV ILWWLQJ RI WKH FRUUHODWLRQ GDWD HLWKHU E\ D VLQJOH H[SRQHQWLDO FDOOHG WKH FXPXODQW

Template version December 2015 Deliverable 2.8

Page 1 of 10
 

DQDO\VLVDVGHILQHGE\,623DUWWRREWDLQPHDQVL]H=DYHUDJHGLDPHWHUDQGSRO\GLVSHUVLW\LQGH[
3',RUE\DPXOWLSOHH[SRQHQWLDONQRZQDVWKH&217,1PHWKRGWRREWDLQDGLVWULEXWLRQRISDUWLFOHVL]HV

/DVHU DWWHQXDWRU

6DPSOHFHOO

&RUUHODWRU 'HWHFWRUƒ
FRPSXWHU


)LJXUH6LPSOLILHGVNHWFKRIWKHRSWLFDOFRQILJXUDWLRQIRU'/6PHDVXUHPHQWRQ=HWDVL]HU1DQR=6


Dispersions and Equipment
7KHIROORZLQJLWHPVDUHJHQHUDOO\UHTXLUHGIRUSURSHU'/6DQDO\VLV
ƒ 3HUVRQDOSURWHFWLRQHTXLSPHQWVLQFOJORYHVODEFRDWVJODVVHVDVUHTXLUHG
ƒ &OHDQZRUNHQYLURQPHQWZLWKQHJOLJLEOHGXVWDQGKLJKTXDOLW\YHQWLODWLRQV\VWHPV
ƒ 'LVSHUVLRQWREHPHDVXUHG
ƒ =HWDVL]HU1DQR=60DOYHUQ,QVWUXPHQWVPRXQWHGZLWKHJQPODVHUGLRGH
ƒ =HWDVL]HUVRIWZDUH
ƒ 9LVFRPHWHUHJ0DOYHUQ,QF699LEUR9LVFRPHWHU2SWLRQDOIRUPHDVXUHPHQWRIWUXHYLVFRVLWLHV
ƒ '/6FXYHWWHRIFOHDUGLVSRVDEOHSRO\PHUJODVVFHOOVRUIROGHGFDSLOODU\]HWDFHOOV,Q1$1R5(*ZH
UHFRPPHQGWRXVHWKHPO0DOYHUQ'/6FXYHWWH
ƒ 3LSHWWHVDQGSLSHWWHWLSV
ƒ 6\ULQJHVDQGV\ULQJHILOWHUV
ƒ &RPSXWHU


Procedure

Samples
7KH 1$1R5(* VDPSOHV DUH SURGXFHG XVLQJ WKH GLIIHUHQW GLVSHUVLRQ SURWRFROV VHOHFWHG IRU 1$1R5(* DQG
IXUWKHUVSHFLILFPHDVXUHPHQWUHTXLUHPHQWVIRUFDOLEUDWLRQSURWRFROVDQGH[SRVXUHPHGLD7DEOHVDQG
7DEOH&KDUDFWHUL]DWLRQUHTXLUHPHQWVLQWR[LFRORJLFDOWHVWVXVLQJGLVSHUVLRQV
(OHPHQWLQWKHZRUNIORZ 5HFRPPHQGDWLRQ5DQG0DQGDWRU\UHTXLUHPHQW02SWLRQDO2

%DWFKGLVSHUVLRQ 7HQUHSHDWHGPHDVXUHPHQWVRIK\GURG\QDPLFVL]H'/6DUHPDGH

ZLWKRXWSDXVHLQFRPELQDWLRQ,QYLWUR0DQGHFRWR[0

,QLWLDOH[SRVXUHPHGLXP 7HQFRQVHFXWLYHPHDVXUHPHQWVRIK\GURG\QDPLFVL]H'/6DUHPDGHLI

WHFKQLFDOO\SRVVLEOHZLWKRXWSDXVHRQWKHVDPHVDPSOH,QYLWUR0DQG
HFRWR[0

)LQDOH[SRVXUHPHGLXP 7HQFRQVHFXWLYHPHDVXUHPHQWVRIK\GURG\QDPLFVL]H'/6DUHPDGHLI

WHFKQLFDOO\SRVVLEOHZLWKRXWSDXVHRQWKHVDPHVDPSOH,QYLWUR0DQG
HFRWR[0

Template version December 2015 Deliverable 2.8

Page 2 of 10
 

6WDELOLW\RIGLVSHUVLRQGXULQJ 6HGLPHQWDWLRQUDWHVFDQEHDVVHVVHGIURPWHVWVXVLQJWKH'/6%\'/6
DVVD\ RQHPD\DQDO\]HERWKDJJORPHUDWLRQDQGVHGLPHQWDWLRQ,QYLWUR5DQG
HFRWR[5


7DEOH'LVSHUVLRQDQGSUREHVRQLFDWLRQFDOLEUDWLRQSURWRFROV

7\SHRIWHVW 3URWRFRO

&DOLEUDWLRQRIVRQLFDWRUVIRU &DORULPHWULFPHWKRGFRPELQHGZLWKDGMXVWPHQWXVLQJWKH10
LQYLWURDQG,QYLWURVWXGLHV EHQFKPDUNPDWHULDO1$12*(1272;EDWFKPHGLXP

,QYLWURVWXGLHV 1$12*(1272;

,QYLWURVWXGLHV 1$12*(1272;RU(135$

&DOLEUDWLRQRIVRQLFDWRUVIRU &DORULPHWULFPHWKRGFRPELQHGZLWKDGMXVWPHQWXVLQJWKH10
HFRWR[VWXGLHV EHQFKPDUNPDWHULDOLQZDWHU

(FRWR[LFLW\VWXGLHV (LWKHUWKH1$1R5(*ZDWHURUHQKDQFHG120 ZDWHUHFRWR[LFRORJLFDO

GLVSHUVLRQSURWRFROVIRU&17DQGK\GURSKRELF010

1DWXUDO2UJDQLF0DWWHU

0DOYHUQ DSSDUDWXV LV GHVLJQHG WR PHDVXUH VDPSOHV RYHU D ODUJH FRQFHQWUDWLRQ DQG SDUWLFOH VL]HUDQJHV
*HQHUDO VSHFLILFDWLRQV DQG OLPLWDWLRQV RI VDPSOH SURSHUWLHV FRQFHQWUDWLRQ UDQJH VL]H RI QDQRSDUWLFOHV
PHGLXPFDQEHIRXQGLQWKHGRFXPHQWDWLRQIURP0DOYHUQ,QVWUXPHQWDFFHVVLEOHRQWKHLUZHEVLWH
7KHFULWLFDOSRLQWIRUDOOPHDVXUHPHQWVLVWKDWLWLVQHFHVVDU\WKDWWKHGLVSHUVLRQLVUHDVRQDEO\VWDEOHZLWKLQWKH
WLPHIUDPHRIHDFKPHDVXUHPHQWWRREWDLQKLJKTXDOLW\GDWD
General measurement
'/6 PHDVXUHPHQWV PD\ EH SHUIRUPHG LQ GLVSRVDEOH SRO\VW\UHQH FXYHWWHV RU UHXVDEOH JODVV FXYHWWHV ,W LV
UHFRPPHQGHGWRUHSHDWWKHPHDVXUHPHQWVRQWKHVDPHVDPSOHVWLPHVWRHVWDEOLVKDYHUDJHGLDPHWHUVDQG
LQWHQVLW\VL]HGLVWULEXWLRQVZKLFKFDQEHFRQYHUWHGWRQXPEHURUYROXPHVL]HGLVWULEXWLRQ7KHKLJKQXPEHURI
UHSHDWHGDQDO\VLVDUHUHTXHVWHGWRHQDEOHEHWWHUDQDO\VLVRIVWDELOLW\RIGLVSHUVLRQDQGWKHVL]HGLVWULEXWLRQVDV
ZHOODVRPLVVLRQRIPHDVXUHPHQWVZLWKEDGFRUUHODWLRQGDWDRUDEQRUPDOVROXWLRQVWRWKHFRUUHODWLRQIXQFWLRQ
,QFRPSOH[PDWHULDOVVXFKVXGGHQ³RXWOLHUV´DUHVRPHWLPHVREVHUYHGZKLFKFDQEHGXHWRDFWXDOYDULDWLRQV
RU VXGGHQ GLVWXUEDQFHV GXH WR IOXFWXDWLRQV RU VHGLPHQWDWLRQ RI ODUJHU SDUWLFOHV 6XFK GDWD PXVW EH FDUHIXOO\
FRQVLGHUHGEHIRUHXVHDVWKH\GRQRWUHSUHVHQWWKHJHQHUDOGLVSHUVLRQ

7KLVSURFHGXUHLVWKHJHQHUDODSSURDFKIRU'/6PHDVXUHPHQWRIWKH10SUREHFDOLEUDWLRQPHGLD
EDWFKGLVSHUVLRQVDVZHOODVLQLWLDODQGILQDOH[SRVXUHPHGLD

 7XUQRQWKHFRPSXWHUDQGWKHQWKH'/6LQVWUXPHQW
 $OORZWKHLQVWUXPHQWWRZDUPXSDFFRUGLQJWRWKHPDQXIDFWRU¶VUHFRPPHQGDWLRQFDPLQXWHV
 8SORDGWKH'76VRIWZDUHDQGWKH³0HDVXUHPHQW´ZLQGRZIRUHQWHULQJPDWHULDOVSHFLILFGDWDRQ
GLVSHUVLRQPHGLXPVDQGWHVWPDWHULDOVDVZHOODVVSHFLILFDQDO\WLFDOVHWWLQJV
o 6HOHFWHQWHUWKHPHGLXPWRUHWULHYHLWVUHIUDFWLYHLQGH[5LDQGDEVRUSWLRQYDOXHV5D
GLHOHFWULFDOFRQVWDQWDQGNLQHPDWLFYLVFRVLW\ ,IDVXLWDEOHPHGLXPLVQRWHQWHUHGSOHDVH

Template version December 2015 Deliverable 2.8

Page 3 of 10
 

HQWHU\RXURZQPHGLXP,I\RXKDYHQRGDWDFKRRVHWKHGHIDXOWZDWHUDQGFRUUHFW\RXUGDWD
DIWHUZDUGVXVLQJWKH(GLWIXQFWLRQLIQHHGHG
o 6HOHFWWKHWHVWPDWHULDOWRREWDLQLWVUHIUDFWLYHLQGH[5 LDQGDEVRUSWLRQYDOXHV5D,IQRW
H[LVWLQJDQG\RXKDYHQRGDWDDGLIIHUHQWPDWHULDOPD\EHVHOHFWHG,IQHHGHG\RXUGDWDFDQ
EHFRUUHFWHGDIWHUZDUGVXVLQJWKH(GLWIXQFWLRQ 
o 6HOHFWPHDVXUHPHQWWHPSHUDWXUHq&IRUEDWFKGLVSHUVLRQV10FDOLEUDWLRQ
GLVSHUVLRQVDQGHFRWR[LFRORJLFDOWHVWPHGLDq&IRULQYLWURDQG,QYLWURH[SRVXUHPHGLD
8VHDQHTXLOLEUDWLRQWLPHRIVHFRQGV
o 6HOHFWDXWRPDWLFIRUDOOPHDVXUHPHQWFRQGLWLRQVPHDVXUHPHQWSRVLWLRQODVHUDWWHQXDWLRQ
QXPEHURIUXQVDQGVXEUXQVUHVSHFWLYHO\'R127VHOHFWH[WHQGHGPHDVXUHPHQWWLPHIRU
ODUJHSDUWLFOHV
o 6HOHFWUHSHDWHGPHDVXUHPHQWVZLWKQRWSDXVHEHWZHHQWKHPHDVXUHPHQWV
o 6HOHFWWKH³*HQHUDOSXUSRVH´PRGHOIRULQLWLDOHYDOXDWLRQRIGDWD7KLVLVWKHJHQHULFPRGHOIRU
FDOFXODWLRQRIWKHDYHUDJHVL]HDQGVL]HGLVWULEXWLRQ
 6HOHFWDP/VDPSOHFXYHWWHDQGHQVXUHWKDWLWGRHVQRWFRQWDLQGXVWQRUGHIHFWVRUVFUDWFKHVLQWKH
PHDVXUHPHQWDUHDRIWKHFXYHWWH6RPHSURGXFHUVKDYHEHHQIRXQGWRGHOLYHUFXYHWWHVZLWKVFUDWFKHV
RUIROGLQJVWUXFWXUHLQWKHPHDVXUHPHQWDUHDDWRQHVLGHRIWKHFXYHWWH'XVWPD\EHFOHDQHGRXWE\
ULQVLQJWKHFXYHWWHLQGLVSHUVLRQPHGLXP
 6DPSOHP/RIWKHGLVSHUVLRQDQGILOOLWLQWRWKHP/PHDVXUHPHQWFXYHWWHXVLQJDSLSHWWH)RUEDWFK
GLVSHUVLRQPHDVXUHPHQWVWKHP/VDPSOHLVGUDZQPLQXWHVDIWHUVRQLFDWLRQDOORZLQJWKH
GLVSHUVLRQWRVWDELOL]HDQGKDUPRQL]DWLRQRIWKHVDPSOLQJWLPH
 3ODFHWKHVDPSOHFXYHWWHLPPHGLDWHO\WKHUHDIWHULQWKH'/6VDPSOHKROGHUDQGVWDUWWKHDQDO\VLV

 ,I KLJKDFFXUDF\ VL]HGDWD DUH UHTXLUHG LW LV QHFHVVDU\ WR GHWHUPLQH WKH YLVFRVLW\ RI WKH WHVWHG GLVSHUVLRQ
7KHPHDVXUHGG\QDPLFYLVFRVLW\FDQEHGHWHUPLQHGDQGIRUGDWDFRUUHFWLRQDIWHUWKH'/6PHDVXUHPHQWKDV
EHHQ FRPSOHWHG VHH 3RLQW  DERYH VR WKHUH LV QR GHOD\ LQ WKH PHDVXUHPHQW SURFHVV 9LVFRVLW\
PHDVXUHPHQWV FDQ EH PDGH XVLQJ HJ WKH 69 9LEUR 9LVFRPHWHU )LJXUH  EHORZ JLYHV D WKHRUHWLFDO
H[DPSOHRIWKHLPSRUWDQFHRIDFRUUHFWYLVFRVLW\PHDVXUHPHQWLIH[DFWVL]HGDWDDUHUHTXLUHG


Template version December 2015 Deliverable 2.8

Page 4 of 10
 



)LJXUH7KHVHJUDSKVLOOXVWUDWHWKHLPSRUWDQFHRIYLVFRVLW\RQWKHFDOFXODWHGQXPEHUDQGYROXPH
VL]HGLVWULEXWLRQVRI10GLVSHUVHGDFFRUGLQJWRWKH1$12*(1272;GLVSHUVLRQSURWRFRO
0HDVXUHPHQWVZHUHFRQGXFWHGDWq&7KHUHGOLQHUHFRUGLVWKHUHVXOWFDOFXODWHGXVLQJWKH
VWDQGDUGYLVFRVLW\RIZDWHUF3DQGWKHJUHHQOLQHDUHWKHVDPHGDWDFDOFXODWHGXVLQJWKHW\SLFDO
F3YLVFRVLW\RIWKHGLVSHUVLRQPHGLXPDWq&7KHPD[LPXPSHDNYDOXHVRIWKHQXPEHUVL]H
GLVWULEXWLRQVDUHYROXPHDQGYROXPHQPIRUWKHZDWHUDQG%6$ZDWHU
GLVSHUVLRQYLVFRVLWLHVUHVSHFWLYHO\

7KHRSWLFDOSDUDPHWHUVRIWKHWHVWPDWHULDOGRHVQRWLQIOXHQFHRQWKHDYHUDJH]HWDVL]HVDQG3',+RZHYHU
LIGDWDDUHFRQYHUWHGWRYROXPHRUQXPEHUVL]HGLVWULEXWLRQVLWZLOOQRUPDOO\DIIHFWVKDSHDQGWKHSHDN
SRVLWLRQVRIWKHFDOFXODWHGK\GURG\QDPLFVL]HGLVWULEXWLRQV7KHHIIHFWLVSDUWLFXODUO\LPSRUWDQWLQFDOFXODWLRQV
RIYROXPHVL]HGLVWULEXWLRQV6HHH[DPSOHLQ)LJXUH

Measurement of dispersion stability
,WLVRIKLJKLQWHUHVWWRJDLQIXUWKHUXQGHUVWDQGLQJRIWKHGLVSHUVLRQEHKDYLRUGXULQJWHVWLQJ+RZHYHUWKLVLV
QRUPDOO\DYHU\GLIILFXOWWDVNWRSHUIRUPLQVLWX2QHPD\JHWLQGLUHFWLQIRUPDWLRQRQERWKVHGLPHQWDWLRQDQG
DJJORPHUDWLRQEHKDYLRUE\XVLQJWKH'/6WRPHDVXUHWKHGLVSHUVLRQEHKDYLRULQDFXYHWWHRYHUWLPH


Template version December 2015 Deliverable 2.8

Page 5 of 10
 

7KLVSURFHGXUHPD\EHDSSOLHGIRUDVVHVVPHQWRIWKHGLVSHUVLRQVWDELOLW\XVLQJD'/6FXYHWWHWR
VLPXODWHWKHGLVSHUVLRQEHKDYLRULQWKHH[SRVXUHYLDO

7KHPHDVXUHPHQWSURFHGXUHFRQVLVWVRIWZRSDUWV

3DUW&RQGXFWWKHVDPSOLQJDQGPHDVXUHPHQWDVOLVWHGDERYHXQGHUSRLQWWR

3DUW$IWHUFRPSOHWLRQRIWKHILUVWPHDVXUHPHQWVXVLQJDXWRPDWLFRSWLPL]DWLRQWKH'76VRIWZDUHLVQRZ
SURJUDPPHG WR FRQGXFW PHDVXUHPHQWV XVLQJ WKH PHDVXUHPHQW SRVLWLRQ ODVHU DWWHQXDWLRQ QXPEHU RI UXQV
DQGVXEUXQVLGHQWLILHGGXULQJWKHDXWRPDWLFRSWLPL]DWLRQ

6HWWKHQXPEHURIPHDVXUHPHQWVDQGSDXVHWRFRYHUWKHPHDVXUHPHQWSHULRGDQGWLPHUHVROXWLRQRILQWHUHVW
$SDXVHRIRUPLQXWHVEHWZHHQHDFKPHDVXUHPHQWLVXVXDOO\VXIILFLHQWWRDVVHVVWKHG\QDPLFVLQWKH
GLVSHUVLRQ

/RFNLQJWKHVHPHDVXUHPHQWSDUDPHWHUVHQDEOHVFRPSDULVRQRIIOXFWXDWLRQVLQLQWHQVLW\DQGDYHUDJH]HWDVL]H
DVGHVFULEHGLQVHFWLRQ

Evaluation of DLS size-data
&RQVXOW WKH 0DOYHUQ PDQXDO DQG KRPHSDJH IRU DGYLFH RQ GDWDLQWHUSUHWDWLRQ %HORZ D QXPEHU RI VSHFLILF
FRQVLGHUDWLRQVDUHOLVWHG
 7KHDYHUDJH]HWDVL]HPD\EHLPPHGLDWHO\DFFHSWHGLIWKH'76GHIDXOW5HVXOWTXDOLW\VD\V³*RRG´
 ,IWKHDQDO\VLVVXJJHVWVWKDWWKHVDPSOHKDVDELRUPXOWLPRGDOVL]HGLVWULEXWLRQWKHVL]HGLVWULEXWLRQ
UHVXOWPD\EHFDUHIXOO\HYDOXDWHGE\UHFDOFXODWLRQWKHGDWDXVLQJWKHKLJKUHVROXWLRQDOJRULWKPVHOHFWHG
XQGHU³'DWDSURFHVVLQJ´LQWKH³(GLWUHVXOW«´PHQX
5HPHPEHUGRQRWGHOHWHWKHRULJLQDOGDWDPHDVXUHPHQWDVWKLVGHOHWHVWKHUDZEDFNJURXQGGDWDIRU
DOOFDOFXODWLRQV


Template version December 2015 Deliverable 2.8

Page 6 of 10
 



)LJXUH7KHVHJUDSKVLOOXVWUDWHWKHLPSRUWDQFHRIWKH5HIUDFWLYH5 LDQG$EVRUSWLRQLQGLFHV5DEVRQ
WKH FDOFXODWHG QXPEHU DQG YROXPH VL]HGLVWULEXWLRQV RI 10 GLVSHUVHG DFFRUGLQJ WR WKH
1$12*(1272; GLVSHUVLRQ SURWRFRO 0HDVXUHPHQWV ZHUH FRQGXFWHG DW  q& DQG FDOFXODWHG IRU
PHGLXPYLVFRVLW\RIF35L LVIRUDQDWDVH5L LVIRUSURWHLQ5L LVIRUSRO\VW\UHQH
ODWH[DQG5L LVIRUUXWLOH7KHPD[LPXPSHDNYDOXHVLQWKHYROXPHVL]HGLVWULEXWLRQVDUH
QP IRU WKH DQDWDVH DQG UXWLOH  QP IRU WKH SRO\VW\UHQH ODWH[ DQG EHWZHHQ  DQG  IRU
SURWHLQRSWLFDOLQGLFHVUHVSHFWLYHO\

 ,I WKH GHIDXOW 5HVXOW TXDOLW\ VD\V ³5HIHU WR TXDOLW\ UHSRUW´ WKH VDPSOH VKRXOG EH IXUWKHU DQDO\]HG
&KHFNWKHVL]HGLVWULEXWLRQUHSRUWDQGWKHLQEXLOG([SHUWDGYLFHWRLQYHVWLJDWHZKHWKHUWKHUHVXOWVXIIHU
IURPKLJK SRO\GLVSHUVLW\3',GXHWRSRO\PRGDOGLVWULEXWLRQV SUHVHQFHRIGXVW FXYHWWHHUURUV ODUJH
SDUWLFOHV VHGLPHQWDWLRQ ZDOOGHSRVLWLRQ HWF 5HOLDELOLW\ LQ VL]HGLVWULEXWLRQ GDWD FDQ EH PDGH E\
FKHFNLQJ WKH ILW LQ WKH &XPXODQW DQG 'LVWULEXWLRQ ILW ZLQGRZ ,I VLJQLILFDQW GHYLDWLRQV IURP WKH ILWWLQJ
FXUYHVRFFXUWKHVL]HGLVWULEXWLRQGDWDDUHQRORQJHUUHOLDEOH
 ,IWKHVDPSOHFRQWDLQVSDUWLFOHVZLWKODUJHVSUHDGLQVL]HGLVWULEXWLRQRUWKHGDWDIDLOHGXQGHUSRLQW
RQHPD\FRQVLGHUILOWHULQJWKHVDPSOHWKURXJKGLIIHUHQWV\ULQJHILOWHUVWRLQYHVWLJDWHSUHVHQFHRIVXE
—PDQGVPDOOHUQPVL]HSDUWLFOHV'XVWKDLUDQGSDUWLFOHVDJJORPHUDWHVODUJHUWKDQWKHVL]LQJUDQJH
GLVWXUEV WKH PHDVXUHPHQWV ,Q DGGLWLRQ VPDOO QPVL]H SDUWLFOHV PD\ QRW EH IXOO\ UHVROYHG ZKHQ

FRDUVHU SDUWLFOHV DUH SUHVHQW GXH WR WKH ODUJH GURS   SHU GHFDGH LQ VFDWWHUHG OLJKW LQWHQVLW\ ZLWK
VL]H
 ,ISDUDPHWHUVVXFKDVUHIUDFWLYHLQGH[HVDEVRUSWLRQFRHIILFLHQWRUYLVFRVLW\ZHUHZURQJRUXQNQRZQDW
WKHPHDVXUHPHQWWLPHWKHFRUUHFWLRQFDQEHPDGHDIWHUZDUGVXVLQJWKHFRPPDQG(GLWULJKWFOLFNRQ
WKHPHDVXUHPHQWLQ'76VRIWZDUH

7KHRSWLFDOSDUDPHWHUVIRUPDQ\PDWHULDOVFDQEHIRXQGDWLQWHUQHWUHVRXUFHVVXFKDVKWWSZHEPLQHUDOFRP
7DEOHOLVWVVRPHH[DPSOHVRIRSWLFDOUHIUDFWLYHDQGDEVRUSWLRQLQGLFHVXVHGE\15&:(

7DEOH2SWLFDOYDOXHVXVHGDW15&:(IRUVRPHW\SLFDOQDQRPDWHULDOV
 5XWLOH $QDWDVH 6\QWKHWLF =Q2 &17
$PRUSKRXV
6LOLFD
5L       
5DEV     

Evaluation of particle behaviour in dispersions

Template version December 2015 Deliverable 2.8

Page 7 of 10
 

,IWKHSURFHGXUHLQVHFWLRQZDVIROORZHGWKHSDUWLFOHEHKDYLRULQWKHGLVSHUVLRQXQGHULQYHVWLJDWLRQPD\EH
DVVHVVHG E\ DQDO\]LQJ WKH HYROXWLRQ LQ UHODWLYH VFDWWHUHG OLJKW LQWHQVLW\ DQG DYHUDJH ]HWDVL]H  VL]H
GLVWULEXWLRQ DV IXQFWLRQ RI WLPH 7KLV VHFWLRQ GHVFULEHV WKH SURFHGXUH WR HQDEOH DQDO\VLV RI UHODWLYH LQWHQVLW\
DQGDYHUDJH]HWDVL]H=DYH
 ([SRUWWKH'/6PHDVXUHPHQWVRILQWHUHVWWRHQDEOHZRUNLQJZLWKWKHGDWDLQDVSUHDGVKHHW.H\GDWD
IRU WKH FDOFXODWLRQV DUH 'DWH DQG WLPH 'HULYHG FRXQW UDWH $YHUDJH =HWDVL]H DQG 3', $GGLWLRQDO
GDWDPD\EHXVHIXORUXVHGLQVSHFLILFDVVHVVPHQWVDQGFDQEHH[SRUWHGDVZHOO
 2SHQWKHH[SRUWHGWH[WILOHLQDVSUHDGVKHHWXVLQJHJ06([FHODQGVDYHLWLQDVXLWDEOHILOHIRUPDW
WRDYRLGORVLQJ\RXUZRUNVDYLQJWKHILOHDVW[W
 ,QVHUWDFROXPQIRUFDOFXODWLRQRIWLPHKRXUVPLQXWHVVHFRQGVDV\RXSUHIHUDVHFRQGFROXPQIRU
WKH³UHODWLYHVFDWWHUHGOLJKWLQWHQVLW\´/2*,,RDQGDWKLUGFROXPQIRUWKHUDWLREHWZHHQWKHUHODWLYH
FKDQJHLQK\GURG\QDPLF]HWDVL]H=DYH/2*==R
 &DOFXODWH WKH WLPH EHWZHHQ HDFK EHWZHHQ WL DQG WL PHDVXUHPHQW LQ WKH FROXPQ FDOOHG HJ 7LPH
>KRXUV@2QHSURFHGXUHLV
QWLWLPLQXWHVWLVHFRQGVWLVHFRQGV
 &DOFXODWHWKH³UHODWLYHVFDWWHUHGOLJKWLQWHQVLW\´LQWKH /2*,,RFROXPQXVLQJWKHGHULYHGFRXQWUDWH
GDWD6HOHFWWKHILUVWPHDVXUHPHQWDWWRRUDOWHUQDWLYHO\DQDYHUDJHRIWKHILUVWVWDEOHPHDVXUHPHQWV
WRDYH DV WKH UHIHUHQFH YDOXH IRU WKH LQWHQVLW\ IRU WKH IXOO GLVSHUVLRQ 7KH /2*,,R YDOXH LV WKHQ WKH
/2*WRWKHGHULYHGFRXQWUDWHDWWLGLYLGHGE\WKHUHIHUHQFHGHULYHGFRXQWUDWHDWWRRUWRDYH
 &DOFXODWH WKH ³UHODWLYH FKDQJH LQ K\GURG\QDPLF VL]H´ LQ WKH /2*==R FROXPQ 6HOHFW WKH ILUVW
PHDVXUHPHQW DW WR RU DOWHUQDWLYHO\ DQ DYHUDJH RI WKH ILUVW VWDEOH PHDVXUHPHQWV W RDYH DV WKH
UHIHUHQFHYDOXHIRUWKH=DYHIRUWKHIXOOGLVSHUVLRQ7KH/2*==RYDOXHLVWKHQWKH/2*WR= DYHDWWL
GLYLGHGE\WKHUHIHUHQFHYDOXH=DYHDWWRRUWRDYH
 3ORW /2*,,R DQG /2*==R RU =DYH DV IXQFWLRQ RI WLPH DQG WKH /2*==R YHUVXV /2*,,R WR
FRPSDUHWKHUHODWLYHLPSRUWDQFHRIWKHWZRSDUDPHWHUVDVQHHGHG6HHH[DPSOHLQ)LJXUHEHORZ
 (YDOXDWH WKH GDWD FRQVLGHULQJ WKDW GLIIHUHQW FKDQJHV LQ /2*,,R DQG /2*==R PD\ RFFXU
GHSHQGLQJ RQ WKH GLVSHUVLRQ EHKDYLRU VHH )LJXUH EHORZ )RU H[DPSOH ,,R PD\ LQFUHDVH GXH WR
DFFXPXODWLRQ RI SDUWLFOHV DW WKH PHDVXUHPHQW SRVLWLRQ FD  PP DERYH WKH ERWWRP RI WKH YLDO RU
JURZWK LQ SDUWLFOH VL]H GXH WR DJJORPHUDWLRQDJJUHJDWLRQ ,Q VRPH FDVH VHYHUDO SURFHVVHV DUH
LPSRUWDQWDWWKHVDPHWLPH
 ,IGDWDDOORZVHVWDEOLVKDUHJUHVVLRQFXUYHIRU7LPHYHUVXV/2*,,RWRFDOFXODWHWKHDSSDUHQW
/2*,,R    /2*,,R   DQG  /2*,,R   VHGLPHQWDWLRQ WLPHV VHH
)LJXUH

Comments on the use of DLS data
'/6LVYHU\VXLWDEOHIRUVL]HDQGVWDELOLW\DQDO\VLVRISDUWLFOHVLQOLTXLGGLVSHUVLRQV+RZHYHUJUHDWFDUHVKRXOG
EHWDNHQLQLQWHUSUHWDWLRQRIGDWDHVSHFLDOO\ZKHQWKH VDPSOHFRQWDLQVERWKPPDQGVPDOOQPVL]HSDUWLFOHV
DQGSDUWLFOHVZLWKQRQVSKHULFDOPRUSKRORJLHVVXFKDVGLVSHUVHGILEHUV
)RU EHWWHU DFFXUDF\ LQ GHWHUPLQDWLRQV RI VL]HGLVWULEXWLRQV LW LV LPSRUWDQW WR REWDLQ WUXH YDOXHV RI WKH RSWLFDO
SURSHUWLHVDQGYLVFRVLW\RIWKHGLVSHUVLRQOLTXLG

References
-HQVHQ.$&ODXVHQ3$%LUNHGDO5.HPERXFKH<&KULVWLDQVHQ(-DFREVHQ15/HYLQ0.RSRQHQ,DQG
:DOOLQ+'H7HPPHUPDQ3-0DVW-*XLRW&6SDOOD20RW]NXV&6KLYDFKHY%5RXVVHW'%DX6DQG
:LWVFKJHU 2  'HOLYHUDEOH  6WDQGDUG RSHUDWLQJ SURFHGXUHV IRU FKDUDFWHULVDWLRQ RI WKH VHOHFWHG 010

Template version December 2015 Deliverable 2.8

Page 8 of 10
 

W\SHV(GLWHGE\.$-HQVHQDQG17KLHUHW'HOLYHUDEOHRIWKH1$12*(1272;3URMHFW)UHQFK$JHQF\IRU
)RRG(QYLURQPHQWDODQG2FFXSDWLRQDO+HDOWK 6DIHW\$16(60DLVRQV$OIRUW&HGH[)UDQFHSS

2 Sedimentation with accumulation
Sedimentation and agglomeration
of suspended particles and agglomeration of suspended
particles
LOG(Z/Zo)

0
NM-101
NM-110
NM-400

Sedimentation and fining of Sedimentation with accumulation

suspended particles and fining of suspended particles
-2
-2 0 2
LOG(I/Io)
D 

1.0 1.0
LOG(I/Io) NM-101
0.8 LOG(I/Io) NM-110 0.8
LOG(I/Io) NM-400
0.6 LOG(Z/Zo) NM-400 0.6
LOG(Z/Zo) NM-101
0.4 LOG(Z/Zo) NM-110 0.4

0.2 0.2
LOG(Z/Zo)
LOG/I/Io)

0.0 0.0

-0.2 -0.2

-0.4 -0.4

-0.6 -0.6

-0.8 -0.8

-1.0 -1.0
0 500 1000 1500
E Time (min) 
)LJXUH  $ 3ORW RI /2* ==R YHUVXV /2* ,,R WHPSRUDO YDULDWLRQV IRU WKUHH GLIIHUHQW 010
GLVSHUVLRQV LQ D FHOO PHGLXP 7KH GLVSHUVLRQV VKRZ GLIIHUHQW EHKDYLRXU % 3ORW RI WKH WHPSRUDO
HYROXWLRQ LQ /2* ,,R IRU WKH WKUHH GLVSHUVLRQV LQ )LJXUH $ 7KH SORWV VKRZ YHU\ IDVW VHGLPHQWDWLRQ
DQGGHSRVLWLRQRI10DQGVORZHUVHGLPHQWDWLRQRI106ORWWRPRGHUDWHGHSRVLWLRQRFFXUVLQ
WKHPHGLXPZLWK10HQGLQJZLWKDFFXPXODWLRQRI10FORVHWRWKHERWWRPDWFDKRXUV


Template version December 2015 Deliverable 2.8

Page 9 of 10
 

600

500

y = -1928.2x + 20.159
400
R² = 0.9064
Time (min)

300 y = -417.94x - 44.224

R² = 0.9363

y = 3.2901e-4.343x
200
R² = 0.9578

100

0
-1 -0.75 -0.5 -0.25 0 0.25 0.5 0.75 1
LOG(I/Io)

)LJXUH  $ 3ORW RI 7LPH YHUVXV /2* ==R IRU GDWD DVVHVVPHQW WR HVWDEOLVK UHJUHVVLRQ FXUYHV IRU
FDOFXODWLRQ RI GLVSHUVHG 010 VHGLPHQWDWLRQ WLPHV 'DWD DUH RQO\ SORWWHG LQ WKH WLPHIUDPH GXULQJ
ZKLFKWKHUHLVDV\VWHPDWLFGHFUHDVHLQ/2*,,RDQGVHGLPHQWDWLRQLVSUHGRPLQDQW


Template version December 2015 Deliverable 2.8

Page 10 of 10