Tiêu chuẩn iso tr 18196 2016

5.2.2 Nano-o ject parameter Conc ntration, siz , an siz dis ribution.. 5.3.2 Nano-o ject parameter Siz dis ribution.. 5.6.2 Nano-o ject parameter Conc ntration e ondary ele tron ima ing

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Nanotechnolog ies — Measurement

Na ote h olo ie s — Matrice de méth de s de me sur p ur le s n n

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written permis ion Permis ion c n be req esed from either ISO at the ad r es below or ISO’s member bod y in the c u try of

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F reword vii

Introduction ix

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms an definitions 1

3.1 General te ms 1

3.2 Nano-o je t p ramete s 2

4 Parameter s included in the matr ix 3

5 Me surement techniques included in the matr ix 5

5.1 General 5

5.2 A cous ic spe tr osco y 5

5.2.1 Desc iption 5

5.2.2 Nano-o je t paramete s 6

5.2.3 A d vantag es 6

5.2.4 Limitations 6

5.2.5 Measur an 6

5.2.6 Relev nt s andar ds .6

5.3 A nalytical c ntrifugation (AC) 6

5.3.1 Desc iption 6

5.3.4 Limitations 7

5.3.5 Measur an 7

5.4 Ele tr oacoustic spe tr osco y 7

5.4.1 Desc iption

7 5.4.2 Nano-o je t paramete s 7

5.4.4 Limitations 8

5.4.5 Measur an 8

5.5 A er osol p rticle mas analyse (A MS) 8

5.5.1 Desc iption 8

5.5.4 Limitations 9

5.5.5 Measur an 9

5.6 Aug er ele tr on spe tr osco y (A ES) 9

5.6.1 Desc iption 9

5.6.4 Limitations 1

5.6.5 Measur an 1

5.7 Bru aue -Emmett-Tele (BET) method for physical adsorption — Surfac ar ea dete mination 1

5.7.1 Desc iption 1

5.7.4 Limitations 1

5.7.5 Measur an 1

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5.7.6 Relev nt standar ds .1

5.8 Condensation p rticle cou te (CPC) 1

5.8.1 Descr iption 1

5.8.2 Nano-o je t par amete s 1

5.8.3 Adv ntag es 1

5.8.4 Limitations 1

5.8.5 Measuran 1

5.9 Diferential mo i ty analysis sys em (DMAS) 1

5.9.3 Adv ntag es 1

5.9.4 Limitations 1

5.9.5 Measuran 1

5.1 Diferential scan ing calorimetry (DSC) 1

5.1 1 Descr iption 1

5.1 2 Nano-o je t par amete s 1

5.1 3 Adv ntag es 1

5.1 4 Limitations 14

5.1 5 Measuran 14

5.1 6 Relev nt standar ds .14

5.1 Dynamic lght scate ing (DLS) 14

5.1 3 Adv ntag es 1

5.1 4 Limitations 1

5.1 5 Measuran 1

5.1 Ele tr on ener g y los spe tr osco y ( ransmis ion E LS) 1

5.1 3 Adv ntag es 1

5.1 4 Limitations 1

5.1 5 Measuran 1

5.1 Ele tr ophor esis/ca i ary ele tr ophor esis 1

5.1 3 Adv ntag es 1

5.1 4 Limitations 1

5.1 5 Measuran s 1

5.14 Ener g y dispe sive X-ra y spe tr ometry (EDS/EDX an WDS) 1

5.14.3 Adv ntag es 1

5.14.4 Limitations 1

5.14.5 Measuran 1

5.1 Field flow fractionation (F F) 1

5.1 3 Adv ntag es 2

5.1 4 Limitations 2

5.1 5 Measuran 2

5.1 Fluor esc nc spe tr osco y 2

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5.1 1 Desc iption 2

5.1 2 Nano-o je t paramete s 2

5.1 3 A d vantag es 2

5.1 4 Limitations 2

5.1 5 Measur an 2

5.1 6 Relev nt s andar ds .2

5.1 Fourie trans orm infrared (FT-IR ) spe tr osco y an FT-IR imag ing 2

5.1 1 Desc iption 2

5.1 4 Limitations 2

5.1 5 Measur an 2

5.1 6 Relev nt s andar ds for FT-IR 2

5.1 In uc d g rating method (IG) 2

5.1 1 Desc iption 2

5.1 4 Limitations 2

5.1 5 Measur an 2

5.1 In uctively coupled plasma mas spe tr ometry (ICP-MS) an single p rticle in uctively coupled plasma mas spe tr ometry (SP-ICP-MS) 2

5.1 1 Desc iption 2

5.1 4 Limitations 2

5.1 5 Measur an 24

5.1 7 Nano-hyphenated ICP/MS te h iq es 24

5.2 L se difraction 2

5.2 1 Desc iption 2

5.2 4 Limitations 2

5.2 5 Measur an 2

5.2 Liq id chromatog r aphy mas spe trometry (L -MS) 2

5.2 1 Desc iption 2

5.2 4 Limitations 2

5.2 5 Measur an 2

5.2 Particle tracking analysis (P A ) 2

5.2 1 Desc iption 2

5.2 4 Limitations 2

5.2 5 Measur an 2

5.2 Optical a sorption spe tr osco y (UV/Vis/NIR ) 2

5.2 1 Desc iption 2

5.2 4 Limitations 2

5.2 5 Measur an 2

5.2 6 Relev nt s andar ds for 2

5.24 Q uartz c ys al micr ob lanc (Q CM) .2

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5.24.3 Adv ntag es 2

5.24.5 Measuran 2

5.2 Raman spe tr osco y/Raman imag ing 3

5.2 3 Adv ntag es 3

5.2 4 Limitations 3

5.2 5 Measuran 3

5.2 6 Relev nt standar ds for Raman 3

5.2 Resonant mas measur ement R MM) 3

5.2 3 Adv ntag es 3

5.2 4 Limitations 3

5.2 5 Measuran 3

5.2 S an ing ele tr on micr osco y (SEM) 3

5.2 3 Adv ntag es 3

5.2 4 Limitations 3

5.2 5 Measuran 3

5.2 S an ing pr obe microsco y (SPM) .3

5.2 3 Adv ntag es 34

5.2 5 Measuran ( ) 3

5.2 S con ary ion mas spe trometry (SIMS) an Time of Flg ht SIMS (TOF -SIMS) 3

5.2 3 Adv ntag es 3

5.2 4 Limitations 3

5.2 5 Measuran 3

5.3 Smal ang le X-r a y scate ing (SA XS) 3

5.3 3 Adv ntag es 3

5.3 4 Limitations 3

5.3 5 Measuran 3

5.3 Static lght scatte ing (SLS) an static multiple lg ht cate ing (SMLS) 3

5.3 3 Adv ntag es 3

5.3 4 Limitations 3

5.3 5 Measuran s (SLS) 3

5.3 6 Measuran s (SMLS) 3

5.3 Single p rticle lg ht interaction methods 3

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5.3 2 Nano-o je t p ramete s 40

5.3 5 Measur an 40

5.3 The mog ra vimetric analysis (T A ) 40

5.3 1 Desc iption 40

5.3 5 Measur an 41

5.3 7 Hyphenated TGA te h iq es 41

5.34 Transmis ion ele tr on micr osco y (TEM) 41

5.34.1 Desc iption 41

5.34.5 Measur an 42

5.3 X-r a y difraction (X R D) 43

5.3 1 Desc iption 43

5.3 5 Measur an 43

5.3 X-r a y photoele tron spe tr osco y (X PS) 4

5.3 1 Desc iption 4

5.3 4 Limitations 4

5.3 5 Measur an 4

A nne x A (informative)S mple separatio /pr eparatio 46

Biblog raphy 49

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ISO (he Int ernational Org nization for Stan ardization) is a worldwidefede ation of national s an ards

b dies (ISO membe b dies) The work of pr p ring Int ernational Stan ards is normaly car ied out

through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical

committ ee has be n es a lshed has the right t o be r pr sent ed on that committ ee Int ernational

org nizations, g ove nmental an non-g ove nmental, in laison with ISO, also take part in the work

ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of

ele trot ech ical s an ardization

The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar

desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the

dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the

edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www.iso.org dir ctives)

A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of

p t ent right ISO shal not be held r sponsible for identifying any or al such p t ent right Detais of

any p t ent right identified d ring the develo ment of the document wi be in the Introd ction an / r

on the ISO ls of p t ent de larations r c ived ( e www.iso.org p t ent )

Any trade name used in this document is information given for the convenienc of use s an does not

cons itut e an en orsement

For an ex lanation on the meaning of ISO spe ific t erms an ex r s ions r lated to conformity as es ment,

as wel as information a out ISO’s adhe enc to the Wor ld Trade Org nization (WTO) principles in the

Te h ical Bar ie s to Trade (TBT) se the folowing URL: www.iso.org/ iso/for word.html

The committ ee r sp nsible for thisdocument is ISO/TC2 9, Na otechn lo ies

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This document con e t the nano-o je t paramet ers that mos commonly ne d t o be measur d with

cor esp n ing measur ment t ech iq es This document wi l be a useful t ool for nanot echnolo y

int er st ed p rties t o ra idly identify r lev nt information for measuring nano-o je t The common

nano-o je t p ramet ers ar lst ed along the t op row of the Q uick-Use-Matrix ( e Ta le 1) If a

measur ment t ech iq e lst ed in the f irs column of the matrix is a pl ca le, the b x in the matrix wi l

be marked Onc a measur ment t ech iq e of int er s is identif ied, it is r commen ed that the r ade

then ent er this document’s b dy of t ext ( e Clause 5), w he e you wi l f in an alpha etical l s ing of

the measur ment t ech iq es and desc iptions of the adv ntag es, l mitations, r lev nt s an ards,

measurand(), an a plca le nano-o je t p ramet ers of each t ech iq e

As scientific adv nc s ar made an ad itional comme cial measur ment t ech iq es be ome a ai a le,

this document wi l be pe iodical y r viewed an updat ed t o maintain it r lev nc

Many of the t ech iq es l st ed in this document ha e not be n v ldat ed through rou d-ro in t es ing or

any othe means for the measur ment of nano-o je t This document is int en ed as a s arting p int an

r sour e t o help identify p t entialy useful an r lev nt t echniq es; it is not an exhaus ive or primary

sour e It is r commen ed that onc a t ech iq e has be n identif ied, the r ade r fe s t o r lev nt

int ernational s an ards an con uct a lt eratur sear h for simi ar or comp ra le a plcations Othe

sour es of information inclu e ins rument man factur r’ s a plcations not es an t echnical lt eratur

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Nanotechnolog ies — Measurement technique matrix for

This document pro ides a matrix that guides use s t o comme cial y a ai a le t ech iq es r lev nt t o

the measur ment of common phy siochemical p ramet ers for nano-o je t Some t ech iq es ar also

a plca le t o nanos ructur d mat erials

NOTE Guidance on sample separation an preparation is given in An e A

2 Normati ve r eferences

The e ar no normative r fe enc s in this document

3 Terms and definitions

F or the purposes of this document, the t erms an definitions given in ISO/TS80 04-1, ISO/TS 8 0 4-6

an the folowing a ply

ISO an IEC maintain t erminolo ical data ases for use in s an ardization at the folowing ad r s es:

— IECEle tro edia: a aia le at ht p:/ www.ele tro edia.org

— ISO Onlne brow sing plat orm:a ai a le at ht p:/ www.iso.org o p

disc et e pie e of mat erial with one, two or thr e ext ernal dimensions in the nanoscale

Not e 1 t o entry: T e secon an third e t ernal dimensions are orthog onal t o the f ir t dimension an t o e ch other

[ SOURCE:ISO/TS8 0 4- 2:2 1 , 2.2]

3.1.4

nanostructured material

mat erial ha ing int ernal or surfac s ructur in the nanoscale

Note 1t o entry: If e t ernal dimensions are in the nanos ale, the term n n -o je t (3.1.3)is recommen ed

[ SOURCE:ISO/TS8 0 4-4:2 1 , 2.1 ]

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3.2 Nano-object parameter

cont ent of nano-o je t in a sample, q antif ied as n mbe , ar a, v lume or mas cont ent

Not e 1 to entry: Transformation calculation from one ty e of q antity to another (e.g n mb r t o volume)

req ires the k owledg of the complet e particle size distribution an the as umption of a size-n epen ent

shape, porosity or density

[6]

3.2.3

c y stal pro erty

efe t d e t o the pr senc of thr e-dimensional orde at he level of mole ular dimensions

Not e 1t o entry: S e R eference [1]

3.2.4

electrokinetic potential

dife enc in ele tric p t ential betwe n that at the slp ing plane an that of the bulk lq id

Not e 2t o entry: Electrokinetic potential is e pres ed in volts

Not e 3t o entry: Of en cal ed “ zeta pot ential”

3.2.5

shape

ext ernal g eometric form of a p rticle

Not e 2 t o entry: For q antitative des ription by mac oshape, mesoshape or mic oshape des ript or , se

R eference [9]

3.2.6

size

l near dimensions of a p rticle det ermined b a spe if ied measur ment method an un e spe if ied

measur ment con itions

Not e 1t o entry: S e R eference [1 ]

Not e 2 to entry: Diferent methods of analysis are b sed on the me surement of diferent p y sical properties

In epen ent of the particle property actualy me sured, the particle size is reported as a line r dimension, e.g as

the eq ivalent sp erical diameter

Not e 3 t o entry: Ex mples of size des riptor are those b sed at the opening of a sieve or a statistical diameter,

e.g the F eret diameter, me sured by ima e analysis

Not e 4 to entry: In ISO 9 7 6-1, the symb l x is used t o denote the particle size However, it is reco nized that he

symb l d is also widely used to designate these values T erefore, the symb l x can b replaced by d

3.2.7

particle size distrib tio

cumulative dis ribution of p rticle conc ntration as a function of p rticle siz

[ SOURCE:ISO 14644-1:2 1 , 3.2.4 ]

Not e 1 to entry: Particle size distribution is of statistical nature so it can b e pres ed as a fu ction of particle

[1 ]

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Note 2 t o entry: T e ty e of q antity (n mb r, are , volume or mass) as wel as the me suran , the me sured

eq ivalent sp ericaldiamet er,shal b in icat ed

Note 3 t o entry: Particle size distribution can b e pres ed as cumulative distribution or a distribution density

(distribution of the fraction of material in a size clas , divided by the width of that class)

3.2.8

surface are

ext ent of a ai a le surfac ar a as det ermined b given method un e s at ed con itions

Note 1t o entry: S e R eference [1 ]

Note 2 to entry: Surface are is the q antity of ac es ible surface of a sample when e posed to either g se us or

liq id adsorb te p ase Surface are is conventional y e pres ed as a mas -specif ic surface are or as

volume-specif ic surface are where the t otal q antity of are has b en normalized either t o the sample’ s mas or

volume

[1 ]

4 P arameters included in the matrix

S ve al compr hensive lt eratur sear hes, input from ISO/TC 2 9 ex e t , an a r view of cur ent ISO

work ha e identif ied fr q ently sought nano-o je t paramet ers that ar lst ed ac os the t op of the

Quick-Use-Matrix ( e Ta le 1) The paramet ers lst ed from lef t o right ar in alpha etical orde A

single t echniq e alone oft en cannot pro ide sufficient information a out al p ramet ers of int er s for a

p rticular nano-o je t u de s u y, nor isone t ech iq e lkely t o ful y ca tur r lev nt information for

a single paramet er The efor , w hen a aia le, it is r commen ed that mor than one t ech iq e should

be used for any p ramet er inves ig tion

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Single particle light

int eraction methods

X-ray p oto lectron

In the folowing subcla uses, measur ment t echniq es ar l st ed in alpha etical orde (with some

ex ceptions w he e simi ar t echniq es ar grouped t og ethe ) Inclu ed u de each t ech iq e ar

the nano-o je t p ramet ers that can be measur d b the t echniq e an a l s ing of the t ech iq e’ s

adv ntag es, l mitations, measuran s, an r lev nt s an ards Gene aly, a single t echniq e can ot

pro ide charact erization of al nano-o je t p ramet ers of int er s Also, a t echniq e ma be useful

t o det ermine othe p ramet ers not lst ed F or compr hensive analy sis of a single p ramet er, use of

multiple t ech iq es, w he e a plca le, is highly r commen ed

In some cases, the e ar multiple t echniq es that shar a simiar un e lying theory of o e ation or

phy sical phenomenon, but w hich ha e dife enc s that make them u iq ely a plca le t o dife ent

ty es of mat erials an measur ment con itions F or ex mple, dife ent ele troma netic scatt ering

t ech iq es ar bett er suit ed for the analysis of dife ent mat erials (e.g metals, p lyme s or r fract ories)

or mat erials in dife ent s at es (e.g suspen ed in a lq id or incorp rat ed int o a sol d matrix)

5.2 Ac oustic spectr osc opy

5.2.1 Des ription

The b sic conc pt is t o measur the fr q ency-depen ent att en ation or velocity of ultrasoun as it

pro a at es through a het erog eneous sample, e.g coloids, dispe sions an emulsions The e ar two

main ty es of vibrations: fr ean for ed Fr e vibrations ar the natural or normal modesof vibration

for a subs anc F or ed vibrations ar caused b some sort of ex citation t o make the analyt e r sonat e

bey n it normal modes

Both acous ic an ele tro cous ic spe trosco ies ( e 5.4) ar l n ed t o a sou d pro a ation through

a het erog eneous sy st em such as a suspension or an emulsion An acous ic spe tromet er measur s

only the chang es in the pro e ties of the soun wa e, w he eas an ele tro cous ic spe tromet er deals

with conne tion betwe n ele trodynamic phenomena an the sou d wa e pr s ur field A cous ic

an ele tro cous ic spe trosco ies ar indepen ent methods be ause the att en ation has l t le efe t

Table 1 (c ontin ed)

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on the ele tro cous ic spe tra an conve sely, ele trokinetic phenomena ha e neglgible efe t on the

att en ation spe tra

5.2.2 Nano-o ject parameter

Conc ntration, siz , an siz dis ribution

5.2.3 Advantag es

5.2.3.1 Does not req ire sample diution;a plca le for conc ntr ated samples

5.2.3.2 Method is suita le for char acte izing ag g r egated an s ructur ed sys ems

5.2.3.3 Measur ement isnot afe ted b s ir ing an / r pumping of the sample

5.2.3.4 Absolute method;does not r eq ir e siz calbration

5.2.3.5 Instrument ve ification can be cond cted b measur ement of wate with k own acous ic

pr ope ties

5.2.3.6 Solvent-b sed samples (non-aq eous) can be analysed

5.2.4 Limitatio s

5.2.4.1 A pplca le only to lq id-b rne p rticles

5.2.4.2 L we siz lmit ≈10 nm;uppe siz lmit ≈3 mm

5.2.4.3 L we v lume fraction lmit is ≈0,1 %;uppe v lume fraction lmit is ≈5 %

5.2.5 Me surand

Eq iv lent sphe ical p rticle siz dis ribution on a volume b sis calculat ed from the ultrasou d

att en ation fr q ency spe trum

5.2.6 Relevant standar ds

— ISO 2 9 8-1, Meas ur ment a d charac teri zatio o p rticles b ac ous tic meth ds — Part 1: Co c epts

a d proc edur s in ultrasonic at en atio s pec trosc op

— ISO 2 99 - 2, Meas ur ment a d ch rac te i zatio o p rticles b ac ous tic meth ds — Part 2 : Guidelnes

fr lnear theory

5.3 A nal ytical c entrifugation (AC)

5.3.1 Des r iption

Analytical c ntrifug tion (AC) is chosen he e as the g ene ic t erm for a n mbe of c ntrifug l

sedimentation t echniq es, ( ome of w hich ar ) also k own as c ntrifug l lq id sedimentation (C S),

analytical ultrac ntrifug tion (AUC) or dife ential c ntrifug l sedimentation (DCS) Tog ethe , this is

a ve sati e famiy of methods with bro d diamet er rang e (1 nm t o 5 00 nm) an high r solution The

nano articles ar for ed t o mo e through a pr dominantly aq eous medium inside an AC measuring c l

un e a c ntrifug l for e of 5 0 t o 5 0 0 0 × g (rot or spe d 1 0 r/min t o 6 0 0 r/ min) S dimentation

causes fractionation t o take plac , be ause the larg er p rticles mo e fast er The sedimentation

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velocities ofthe dife ent fractions ar measur d with r fractive in ex, ultra iolet (UV) a sorption or

l ght catt ering turbidity det ect ors The diamet ers of the dife ent fractions can be calculat ed from the

dife enc in sedimentation velocity, i.e the complet e p rticle siz dis ribution, ac ording t o St okes’

law The r solution of the AC method is so high be ause, ac ording t o St okes, velocity is pro ortional t o

the sq ar of p rticle diamet er

Siz dis ribution

5.3.3 Advantag es

5.3.3.1 High diamete r esolution

5.3.3.2 Br oad diamete rang e (1 nm to 5 0 0 nm)

5.3.4 Limitatio s

The AUC p rticle siz dis ribution method can give spurious r sult if p rticle siz is t oo high, i.e if the

p rticles form a sediment t oo q ickly or if they displa a bro d chemical het erog eneity ( i.e no uniform

p rticle density)

5.3.5 Me surand

5.3.5.1 S ttlng velocity in c ntrifugal field

5.3.5.2 Refractive in ex, ultra violet (UV)-a sorption or lg ht scate ing /tur bidity

5.3.6 Relevant standards

— ISO 1 3 8-1, Dete min tio o p rticle s i ze di s trib tio b c entrif g l lq id s edimentatio meth ds —

Part 1: G ene al princ iples a d g idelnes

— ISO 1 3 8- 2, Dete min tio o p rticle s i ze di s trib tio b c entrif g l lq id sedimentatio meth ds —

Part 2 : Ph toc entrif ge meth d

— ISO 1 3 8-3, Dete min tio o p rticle s i ze di s trib tio b c entrif g l lq id sedimentatio meth ds —

Part 3: Centrif g l X-ra meth d

5.4 Electroac oustic spectrosc opy

5.4.1 Des ription

Ele tro cous ic phenomena arise from the coupl ng between the ultrasou d f ield an ele tric f ield in

a lq id that contains ions Eithe of these f ields can be a primary driving for e The lq id might be

a simple Newt onian lq id or a complex het erog eneous dispe sion, emulsion or even a p rous body

The e ar seve al dife ent ele tro cous ic efe t , depending on the natur of the lq id an the ty e of

driving for e Ele tro cous ic ins rument ar buit as a pro e, w hich inclu es element for g ene ating

(measuring) ultrasoun field an element for g ene ating (measuring) ele tric f ield (cur ent)

Ele trokinetic p t ential

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5.4.3 Advantag es

5.4.3.1 Does not req ire sample diution;a plca le for conc ntr ated samples

5.4.3.2 Method is suita le for char acte izing ag g r egated an s ructur ed sys ems

5.4.3.3 Mix ing an pumping of the sample ar e alowed

5.4.3.4 S nsor desig n is a pr obe that can be inser ted into the s atic or into the mixed or pumped sample

5.4.3.5 Measur ement time is u de 1 min

5.4.3.6 Sample v lume can beas lttle as0,1 ml

5.4.3.7 A pplca le for high ionic streng th up to several mole pe ltr e

5.4.3.8 Solvent-b sed samples (non-aq eous) ar e alowed

5.4.3.9 Wel suited for pHand surfactant titr ations of the intact conc ntrated samples

5.4.4 Limitatio s

5.4.4.1 A pplca le only to lq id-b rne nano articles

5.4.4.2 There is no r es riction on the lowe siz lmit; up e siz lmit ≈0,1 mm

5.4.4.3 L we v lume fraction lmit is ≈1 %; up e v lume fraction lmit is ≈5 %

5.4.5 Me surand

— ISO 1 0 9-1, Coloidal sys tems — Meth ds fr zeta p tential dete min tio — Part 1: Elec tro c ous tic

a d elec trokinetic p en men

— ISO 1 0 9-3, Coloidal sys tems — Meth ds fr zeta p tential dete min tio — Part 3 : Ac ous tic meth ds

5.5 Aerosol particle mas anal yser (A MS)

5.5.1 Des r iption

This t ech iq e clas ifies ae osol particles int o fractions b sed on the mas -t o-charg e ratio The b sic

conc pt is t o flow ae osol with a Boltzmann charg e dis ribution through an an ulus in a cy lin rical

c ntrifug e with a DC v ltag e a pled It is the principle of the for e eq ation w he e the c ntrifug l

ac ele ation of the particles iscount erb lanc d b the ele tros atic for e on a particle

The ae osol shal f irs p s through a neutralzing se tion A t the outlet of the devic , an ae osol

det ection sy st em is r q ir d t o det ermine the p rticle n mbe siz dis ribution The a pled voltag e

an rotational velocity can be v ried t o o tain siz fractions sele t ed b p rticlemas

Trang 19

Conc ntration an siz

NOTE Size is calculat ed from particle mas

5.5.3 Advantag es

5.5.3.1 High mas r esolution

5.5.3.2 No mas dis ribution as umptions r eq ir ed

5.5.3.3 Near r eal-time measur ement

5.5.3.4 Efe tive density information when coupled to difer ential mo i ty analysis ( e 5.9)

5.5.3.5 Direct measur ement of p rticle mas

5.5.3.6 Dete mination of n mbe conc ntration b mas b sis

5.5.4 Limitatio s

5.5.4.1 A pplca le only to air borne nano articles ( uspensions or p wde s are r eq ir ed to be

aerosolz d)

5.5.4.2 L we mas lmit a out 0,01 fg ; up e lmit a out 1 0 fg (rom a out 3 nm to 5 0 nm in siz

as uming that the sha e of p rticles is sphe ical with density of 1 g /cm

A ug er ele tron spe trosco y (AES) is an ele tron beam t ech iq e that is commonly used t o det ermine

the chemical comp sition of surfac s Ex citation of the sample with an ene g etic ele tron beam r sult

in the g ene ation of a cor hole R ela ation from thisex cit ed s at e oc urs w hen this cor hole isfil ed b

an ele tron from a highe ene g s at e with the simultaneous emis ion of eithe an X-ra phot on or an

A ug er ele tron Due t o the r latively low ene gies (< ke V)of the emitt ed A ug er ele trons, it mean fr e

p th within thesample is lmit ed t o les than 1 nm, making AESin e ently surfac sensitive

Conc ntration ( e ondary ele tron ima ing or elemental ma ping), siz ( e ondary ele tron ima ing or

elemental ma ping), chemical comp sition an sha e

Trang 20

5.6.3 Advantag es

5.6.3.1 High spatial (< μm) an surfac (≈0,1 nm) r esolution [sp tial in this contex t r efe s to

horizontal plane of analysis (x-y dir ection) an surfac r efe s to depth]

5.6.3.2 Elemental ma ping p s ible when employing a scan ing ele tr on beam

5.6.3.3 Depth pr ofi ng ca a i ity when combined with ion spute ing

5.5.3.4 High dete tion sensitivity;ca a le of analysing a fr action of a surfac monola ye

5.6.4 Limitatio s

5.6.4.1 A nalysis of non-con ucting samples can be pr oblematic d e to surfac char g ing efe t

5.6.4.2 Surfac contamination can complcate data analysis

5.6.5 Me surand

5.6.5.1 Ele tr on ener g ies (eV) an sig nal intensity (counts)

5.6.5.2 Leng th an w idth (A or nm)measur ed fr om se on ary ele tr on imag e or elemental ma ping

5.6.5.3 Depth (A or nm)using ion spute ing an measured agains a s andar d of k own thick es

— ISO 1 5 1, S rfc e chemic al a alys i s — Depth profi n — Meth ds fr io beam alg ment a d the

as soc iated meas ur ment o c urrent or c ur ent dens it y fr depth profi n in AES a d XPS

— ISO 2 90 , S r fac c hemi cal a al y sis — Au e electro spe t rosco y a d X-ra p otoelectro

spe tros co y — Meth d s us ed to deter mine peak intensi ti es a d i nfr mati on r q ired when

r p r ting r sult s

— ISO/TR 141 7, S rfc e chemic al a alys i s — Ch rac te i zatio o n n s truc tur d materials

— ASTM E8 7-08, Sta dard prac tic e fr identify in elements b the peak s in Au e Elec tro S ec tros c op

— ASTM E9 4-1 , Sta dard g ide fr identify in chemic al efec ts a d matri x efec ts in Au e Elec tro

S ec trosc op

— ASTM E9 6-1 Sta dard prac tic e fr r p rtin data in Au e Elec tro S ec tros c op a d X-ra

Ph toelec tro S ec tros c op

— ASTM E12 7-1 , Sta dard prac tic e fr dete min tio o the s pec imen ar a c ontrib tin to the detec ted

s ig al in Au e Elec tro S ec tromete s a d s ome X-Ra Ph toelec tro S ec tromete s

5.7 Br unauer -Emmet -Tel er (BET) method for physical adsorption — Surface ar ea

determination

5.7.1 Des r iption

A t echniq e for the det ermination of the t otal spe if ic surfac ar a of f inely divided an p rous solds

b measuring the amount of phy sicaly adsorbed g suti izing the model develo ed b Bru a ue , Emmet

an Tele for int erpr ting g s adsorption isothe ms

[17]

Trang 21

BET is a plca le only t o adsorption isothe ms of ty e I (nonp rous or mac o orous solds) an ty e

IV (meso orous solds) ac ording t o the IUPAC clas ification of adsorption isothe ms F or these cases,

the BET ar a can be r g rded as the “ pro e ac es ible ar a ” ( i.e the efe tive ar a a ai a le for the

adsorption of the chosen adsorptive)

5.7.4.1 Generaly restricted to dry p wde s an p r oussolds

5.7.4.2 Prior to analysis, the sample is usualy outgas ed (ag g r egation might oc ur) at elev ted

temper atur es

5.7.4.3 The BE method can ot r ela ly bea pled to solds which a sor b the measuring gas

— ISO 9 7 , Dete min tio o the s pec ific s urfc e ar a o s olds b g s ads orptio — BET meth d

— ISO 1 9 1- 2, Por s i ze di s trib tio a d p ros it y o sold mate ials b me c ur y p ros imetry a d g s

adsorptio — Part 2 : An lys i s o mes op r s a d mac ro or s b g s adsorptio

— ISO 1 7 7, Fine c eramic s (adv nc ed c eramic s, adva c ed te h ic al c eramic s) — Dete min tio o

s pec ific s urf c e ar a o c eramic p wde s b g s ads orptio us in the BETmeth d

— ASTM C 2 4-1 , Sta dard tes t meth d fr adva c ed c eramic s pec ific s urfc e ar a b p ys ic al adsorptio

— ASTM D 1 9 -0 , Sta dard tes t meth d fr pr c ipitated s ilc a — S rf c e ar a b multip int BET

nitro en adsorptio

— ASTM B9 2-1 , Sta dard tes t meth d fr metal p wde s pec ific s urf c e ar a b p ys ic al ads orptio

— ASTM C1 6 -0 , Sta dard tes t meth d fr s pec ific s urfc e ar a o alumin or q artz b nitro en

adsorptio

5.8 Condensation particle c ounter (CPC)

5.8.1 Des ription

The common principle of al dife ent CPC ty esis that con ensation of supe saturat ed v p ursis used

t o grow ultra-f ine an nano articles t o dro let of siz sthat can be det ect ed o ticaly

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Conc ntration

5.8.3 Advantag es

5.8.3.1 Real-time measur ement

5.8.3.2 Ca a le of time-depen ent measurement

5.8.3.3 Wel-es a lshed q alty as uranc pr oc d res

5.8.3.4 Measur ement isg eneraly indepen ent of p rticle pr ope ties o e a wide siz rang e

5.8.4 Limitatio s

5.8.4.1 A pplca le only to air borne nano articles

5.8.4.2 L we siz lmit ≈1nm;up e siz lmit ≈5 μm

5.8.4.3 Up e n mbe conc ntration lmit subje t o the onset of coincidenc

5.8.4.4 L we siz lmit is depen ent on particle comp sition

5.8.5 Me surand

Particle n mbe conc ntration

— ISO 2 89 , Ae os ol p rticle n mbe c onc entratio — Calbratio o c ondens atio p rticle c ou te s

5.9 Diferential mobi ity anal ysis system (DMAS)

5.9.1 Des r iption

A t ech iq e t o measur the siz dis ribution of submic ometr ae osols

[18]

The dife ential mo i ty analy sis syst em (DMAS) consis s of charg e neutral zation, dife ential

ele trical mo i ty clas if ie (DEMC), p rticle det ect or, plumbing, pump an ele tronics The DEMC

consis s of chan el with an o ening in the wal at a downs r am location pe pen icular t o the flow

An ae osol with a Boltzman charg e dis ribution flow s down the channel with a DC v ltag e a pled

t o the wal s of the chan el The a pled voltag e gradient wi l cause the charg ed p rticles t o drif with

a migration velocity ac ording t o the mo i ty of the p rticle t o the wal with the o ening The siz of

the p rticles clas if ied b p s ing through the side wal o ening depen s on the p rticle siz , p rticle

charg e, voltag e gradient, width of the channel, length along the chan el t o the o ening and flow

velocity

[1 ][2 ]

Thisis a f irs principles measur ment

A con ensation particle cou t er (CPC) is one p s ible det ect or suita le for use with a dife ential

mo i ity analy sis sy st em ( e 5.8) The common principle of CPCins rument ty es is that con ensation

of supe saturat ed v pour is used t o grow ultra-f ine an nano articles t o dro let of siz s that can be

det ect ed o ticaly

NOTE A C C do s not dis riminat e by size; it is a detect or that provides a cou t of particles within the

operational size rang over a period of time If cou led with a size clas if ier, then the combination tech iq e can

Trang 23

Conc ntration, siz an siz dis ribution

NOTE T e size is an electrical mo ility sp erical eq ivalent size

5.9.3 Advantag es

5.9.3.1 High siz resolution (< % u c rtainty at 2,5nm for commer cial ins rument )

5.9.3.2 No siz distribution as umptions r eq ir ed

5.9.3.3 Near r eal-time measur ement

5.9.3.4 Ca a le of time-depen ent measur ement

5.9.3.5 Wel-establshed q alty as uranc pr oc d r es

5.9.4 Limitatio s

5.9.4.1 A pplca le only to air borne nano articles ( uspensions or p wde s are r eq ir ed to be

aerosolz d)

NOTE An electrospray device is commonly used in conju ction with a DMAS to g nerate predominantly

singly-charg d a rosolized mat erial from a particle suspension

5.9.4.2 L we siz lmit ≈2nm;up e siz lmit ≈1 00 nm (up e siz lmit is ≈5 μm w ith CPC)

5.9.4.3 L we numbe conc ntration lmit ≈1

A t ech iq e in w hich the dife enc in the ene g input int o a subs anc an a r fe enc mat erial is

measur d as a function of t empe atur w hie the subs anc an r fe enc mat erial ar subje t ed t o a

controled t empe atur pro ram

Chemical comp sition

5.10.3 Advantag es

5.10.3.1 Minimal sample pr ep ration r eq ir ed

Trang 24

5.10.3.2 Fas scan ing alows sup r es ion of mate ial de omp sition at highe temperatur es ( can at

40 °C/min an fas e )

5.10.3.3 Wide temperatur e rang es

5.10.3.4 Measur ement can be con ucted in difer ent atmospher es

5.10.3.5 Can characte iz q altative b nd s r eng th betwe n nano-fi e an ep x y in nanocomposites

( trong or weak) an examines rig id amorphousfraction (R A F) of nanocomp site sys em

[2 ][2 ]

5.10.4 Limitatio s

Many DSCins rument cannot scan at 40 °C min or cole t data at those spe ds

5.10.5 Me surand

5.10.5.1 J/g : E er g y input pe mas in en othe mic or ex the mic r eactions

5.10.5.2 J/(g K ): heat ca acity, spe ific hea

— ISO 1 3 7-1, Plas tic s — Dife ential sc an in c alorimetr y (DSC) — Part 1: G ene al princ iples

— ISO 1 3 7- 2, Plas tic s — Dife ential s c an in c alorimetry (DSC) — Part 2 : Dete min tio o glas s

tra s itio tempe atur a d glas s tra s itio s tep heig t

— ISO 1 3 7-3, Plas tic s — Dife ential sc an in c alorimetr y (DSC) — Part 3 : Dete min tio o tempe atur

a d enth lp o meltin a d c r ys tali zatio

— ISO 1 3 7-4, Plas tic s — Dife ential s c an in c alorimetr y (DSC) — Part 4 : Determin tio o s pec ific

heat c ap c it y

— ISO 1 3 7-5, Plas tic s — Dife ential sc an in c alorimetry (DSC) — Part 5: Dete min tion o

charac te i s tic r ac tion-c urve tempe atur s a d times , enth lp o r ac tio a d degr e o c on e s ion

— ISO 1 3 7-6, Plas tic s — Dife ential s c an in c alorimetr y (DSC) — Part 6 : Dete min tio o ox idatio

induc tio time (i sothe mal O IT) a d ox idation induc tion tempe atur (dynamic O IT)

— ISO 1 3 7-7, Plas tic s — Dife ential s c an in c alorimetry (DSC) — Part 7: Determin tio o

c rys tali zatio kinetic s

5.11 Dynamic l ght s at er ing (DLS)

5.11.1 Des r iption

DLS, also r fe r d t o as q asi-elas ic lght scatt ering (QELS), is an ensemble t ech iq e for measuring

the siz of particles un e g oing Brownian motion in lq id suspension DLS inclu es phot on cor elation

spe trosco y (PCS), phot on c os -cor elation spe trosco y (PC S) an fr q ency analysis, although

PCS is b far the mos common sub-t ech iq e The ran om motion of the p rticles r sult in a

fluctuating phot on count rat e measur d o e ve y smal inc ement of time (orde of mic ose on s)

an a smal shif in the fr q ency of l ght The rat e of fluctuation or the ma nitu e of the fr q ency

shif is r lat ed t o the spe d of particle motion, w hich is r lat ed t o their hydrodynamic siz

NOTE Cor elation analysis of the time-depen ent intensity of the s at ered light, or analysis of the freq ency

shif of the s at ered light in freq ency domain, can yield the translational dif usion co ff icient an hence the

eq ivalent sp ericalhydrod namic diamet er via the Stokes-Einstein relationship

Trang 25

Siz an siz dis ribution (polydispe sity)

5.11.3 Advantag es

5.11.3.1 Ra id measur ement se onds to min tes)

5.11.3.2 Pr ovides robus mean siz for p rticles in diute dispe sion if p lydispe sity is low

5.11.3.3 Can pr ovide r epr od cible results in ag r eement w ith othe methods for sphe ical p rticles with

a narr ow siz dis ribution

5.11.3.4 Some o tical setups alow measur ement of conc ntrated samples, wher e multiple scatte ing

would othe wise inte fere with analysis

5.11.3.5 Statis icaly sou d; measur es sig nals fr om mi ions of p rticles

5.11.3.6 Firs principles; no calbr ation r eq ir ed; trac a i ty to the SI u it , the metr e, is p s ible

through k owledg e of the incident lase wa veleng th

5.11.3.7 Non-destructive an non-inv sive

5.11.4 Limitatio s

5.11.4.1 Br oad dis ributions cannot be dete mined ac urately be ause scate ing eficiency incr eases

str ongly with p rticle siz

5.11.4.2 L we lmit ≈1 nm; up e lmit is a few micr ometr es depen ing on dete tion scheme (1 nm to

6 0 0nm) The up e lmit is usualy lmited b pr ecipitation an particle n mbe fluctuations sensitive

to lar g e p rticles (In the < 0 nm rang e, scate ing is pr oportional to r adius raised to the 6th p we of

the diamete )

5.11.4.3 Siz dis ributions ar e sensitive to data q alty an the deg ree of p lydispe sity, an r eq ir e use

of non-s an ar diz d inve sion alg orithms with use adjus a le paramete s that impact the r esolution

and noise a p r ent in the r esulting dis ribution

5.11.4.4 Deviations from sphe icity an high conc ntr ations of the dispe sed p rticles negatively afe t

the measur ement ac uracy

5.11.5 Me surand

Eq iv lent sphe ical hydrodynamic diamet er

NOTE C mulants analysis of autocor elation fu ction deliver a ro ust avera e — the harmonic me n of

intensity weighed size distribution fu ction, i.e the z-avera e diameter (ZD)

— ISO 1 3 1, Particle s i ze a alys i s — Ph to c or elatio s pec trosc op

— ISO 2 41 , Particle s i ze a alys i s — Dynamic lg t s c at e in (DL )

— ASTM E2490, Sta dard g ide fr meas ur ment o p rticle s i ze di s trib tio o n n mate ial s in

s us pens io b Ph to Cor elatio S ec trosc op (PCS)

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5.12 Electron ener g y los spectrosc opy ( ransmis ion EELS)

5.12.1 Des r iption

A t ech iq e in w hich an ele tron spe tromet er measur s the ene g spe trum of ele trons (from a

nominal y monoene g etic sour e) w hie they u de g o inelas ic int eractions with the sample, oft en

exhibiting featur s d et o spe ific inelas ic los proc s es Transmis ion EELS is pe formed with a TEM

ins rument ( e 5.34)

[2 ]

NOTE 1 T e spectrum o tained using an incident-electron b am of a out he same energy as an aug r electron

spectros op (AES) or X-ray p oto lectron spectros op (X S) pe k ap ro imat es to the energy los spectrum

as ociat ed with that pe k

NOTE 2 T e electron energy los spectrum, me sured with an incident-electron b am, is a fu ction of the

b am energy, the angle of incidence of the b am, the angle of emis ion an the electronic properties of the sample

5.12.3 Advantag es

5.12.3.1 Spatial r esolution of the or de of the ele tr on beam siz

5.12.3.2 A ny sold can be analysed

5.12.3.3 Quantitative analysis is p s ible

5.12.3.4 Sig nal inclu es chemical information

5.12.3.5 Dir ect information can be o tained on the structur e of solds an ox idative state of the element

5.12.4 Limitatio s

5.12.4.1 Ne d ve y thin spe imens, < 0 nm

5.12.4.2 Intensity weak for ener g y los es > 0 eV

5.12.4.3 Can only bedone using transmis ion ele tr on micr osco y (TEM) ( e 5.34)

5.12.5 Me surand

The chang es in the ene g dis ribution of an ele tron beam transmitt ed through a thin spe imen (e V)

Stan ard being draft ed in ISO/TC 2 2

5.13 Electrophoresis/capi lary electrophoresis

5.13.1 Des r iption

Ele tro hor sis isa sep ration t ech iq e b sed on the dife ential transp rtation velocities of charg ed

spe ies in an ele tric f ield through a con uctive medium The ele trokinetic separation methods ar

pe formed in sub-mi imetr ca i laries and in mic o- and nanofluidic chan els Ele tro hor sis is

Trang 27

sometimes used with phase analy sis lght scatt ering or cor elation spe trosco y for det ermining the

ele trokinetic p t ential

Trang 28

5.13.3 Advantag es

5.13.3.1 Many types of ele tr ophor esis ex is (afinity, ca i ary, g el, etc.) which can be used to taior to

the sep ration of analytes

5.13.3.2 Some ele tr ophor esis te h iq es can be coupled to othe te h iq es

5.13.3.3 Quantitative analysis can be done if calbration s an ar ds ar e a vaia le

5.13.3.4 Do ple an phase analysis o tical-b sed te hniq es for dete mination of ele tr ophor etic

mo i ty ar e firs principle an do not r eq ir e calbration; howeve , z ta p tential calculation is model

depen ent

5.13.4 Limitatio s

5.13.4.1 Liq ids/dispe sions only No sold or gas analysis

5.13.4.2 Req ires o timization for bes sep r ation

5.13.4.3 Might req ire la el ng of analyte for dete tion

5.13.5 Me surands

Ele tro hor tic velocity pe ele tric field s r ngth (ele tro hor tic mo i ty)

— ISO 1 0 9-1, Coloidal sys tems — Meth ds fr zeta-p tential dete min tion — Part 1: Elec tro c ous tic

a d elec trokinetic p en men

— ISO 1 0 9- 2, Coloidal sys tems — Meth ds fr zeta-p tential dete min tion — Part 2 : Optic al meth ds

— ASTM E2 6 -1 , Sta dard Guide fr Meas ur ment o Elec tro h r tic Mo i t y a d Zeta Potential o

Na os i zed B iolo ic al Material s

5.14 Ener g y disper i ve X-ray spectr ometr y (EDS EDX and WDS)

5.14.1 Des r iption

X-ra spe trometry is a t echniq e that uses an ele tron beam an the surfac of the sample t o prod c

in ivid al phot ons that ar measur d b a p ralel det ect or One ele tron is r mo ed t o c eat e a

v cancy int o w hich anothe can “ al” from an out er orbit The X-ray s r sult from transitions between

in e orbitals, w hich ar normaly ful This is then used t o buid up a hist ogram r pr senting the

dis ribution of X-ra emis ion ene gies

WDS (wa elength-dispe sive X-ra spe trosco y)and EDS /EDX (ene g -dispe sive X-ra spe trosco y)

sy st ems ar commonly used with scan ing or transmis ion ele tron mic osco es

[24]

Trang 29

5.14.3 Advantag es

5.14.3.1 EDS is ca a le of semiq antitative or with the a pr opriate contr ols an sample pr ep ration

q antitative analysis

5.14.3.2 EDS can be used to g enerate complex multi-dimensional elemental comp sition ma s

5.14.3.3 WDS is mor e sensitive to low atomic n mbe element than EDS an has the ca acity for

q antitative analysis

5.14.4 Limitatio s

5.14.4.1 Samples should be wel-p lshed an r epr esentative of the bulk mate ial It ma y be ne es ary

to co t non-con uctive samples with a thin la ye of car bon, g old, or platin m

5.14.4.2 Stan ar ds might be r eq ir ed for high-ac uracy q antification

5.14.5 Me surand

Elemental comp sition of a spe if ic p int or ar a or volume, inclu ing the ty e, dis ribution an r lative

q antity of element

— ISO 1 6 2, Mic ro eam a alys i s — Selec ted ins trumental pe frma c e p ramete s fr the s pec ific atio

a d checkin o ene g -di s pe s i ve X-ra s pec tromete s fr us e in elec tro pro e mic ro n lys i s

— ISO 2 3 9, Mic ro eam a alys i s — Qu ntitati ve a alys i s us in ene g -di s pe s i ve s pec trometry (E S)

fr elements w ith a atomic n mbe o 1 (Na) or a o e

5.15 Field flow fractionation (FFF)

5.15.1 Des ription

A separation t ech iq e w he e a field is a pled t o a lq id suspension ty icaly pas ed along a thin

an flat chan el in orde t o cause separation of the particles pr sent in the lq id, depen ent on

their dife ent int eractions with the a pled f ield Holow f ibr sep rations ar also comme cialy

a ai a le

[2 ]

NOTE 1 T e f ield can b , for e ample, gravitational, centrifug l, flow, electrical or ma netic; flow F F is the

most widely used an commer ialized F F sub-tech iq e Flow F F separates ac ording to hydrod namic size

NOTE 2 Using a suita le detector aft er or d ring separation alows det ermination of the size, size distribution

an concentration of nano-o jects

NOTE 3 S paration by F F can b sensitive to size, length, an shape of the analyte

NOTE 4 C an el flow is para olic u der operational con itions, with particles moving at diferent rates

depen ing on the location within the para olic flow prof ile

Siz , siz dis ribution, conc ntration (with an ad itional det ect or), chemical comp sition (with an

ad itional det ect or)

Trang 30

5.15.3 Advantag es

5.15.3.1 Can fractionate highly p lydispe se samples into in ivid al p pulations

5.15.3.2 Can emplo a v riety of dete tors, e.g difer ential r efractomete , UV/Vis a sor banc ,

fluor esc nc , dynamic lg ht scate ing , multi-angle s atic lg ht scate ing , or an in uctively coupled

plasma mas spe tr omete

5.15.4 Limitatio s

5.15.4.1 L we siz lmit depen s on p rticle density an the F F method used but is typicaly 2 nm to

5 nm Siz can only be dete mined ac urately b calbr ation, retention time, or b se on ary dete tion

5.15.4.2 Dis ributions that rang e fr om the nm scale to g r eate than 1 μ m w il not be proper ly sep rated,

as the elution or de inve t a o e roughly 1μm

5.15.4.3 Sample r eq ir ed to be dispe sed in lq id

5.15.5 Me surand

5.1 5.1 Depen ent on dete tor s used: v lume, intensity or mas weighted siz or siz dis r ibution (nm)

5.15.5.2 Conc ntration via UV/Vis a sor banc or fluoresc nc intensity

4.14.5.3 Hydr od ynamic diamete b sed on r etention time; g r eate ac uracy is o tained if calbrated

with p rticles of know n siz u de identical elution con itions

A ty e of ele troma netic spe trosco y w hich analy ses fluor sc nc from a sample It inv lves

i luminating the sample, ty ical y with ultra iolet or visible l ght, t o g ene at e an ele tronical y ex cit ed

s at e w hich then emit l ght ( fluor sc nc ) of long er wa elength

Conc ntration

5.16.3 Advantag es

5.16.3.1 S nsitive te h iq e, down to single fluor ophore level

5.16.3.2 Ra id te h iq e for q altative measur ements

5.16.3.3 Comp tible w ith v rious sample formats

5.16.3.4 S nsitive to chang es in nano-o je t iz an sha e

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5.16.4 Limitatio s

5.16.4.1 Inte fer enc fr om backg rou d fluor esc nc for some samples

5.16.4.2 Q uantitative measur ements ar e time-consuming and r eq ir e calbr ation s andar ds

5.16.4.3 Corrections for scate ing ar e fr eq en y r eq ir ed for q antitative measurement for

nano-o je t

5.16.5 Me surand

5.16.5.1 Fluor esc nc spe trum, intensity vs wa veleng th (nm)

5.16.5.2 Q uantum yield/eficiency

— ASTM E5 8-0 , Sta dard Tes t Meth d fr Linearit y o Flu r sc enc e Meas urin Sys tems

— ASTM E5 9-04, Sta dard Tes t Meth d fr Limit o Detec tio o Flu r sc enc e o Quinine S lf te in

S lutio

— ASTM E3 8-04, Sta dard Tes t Meth d fr Wa elen th Ac c uracy a d S ec tral B andw idth o Flu r s c ence

S ec tromete s

— Res h-Geng r U DeRose P C Clas if ication, t erminolo y, an r commen ations on their sele tion,

use, and prod ction (IUPACTe hnical R ep rt) Pur Ap l Chem 2 1 , 82 p 2 1 – 23 5

5.17 F urier transform infrared (FT- R) spectrosc opy and FT- R imag ing

5.17.1 Des ription

A t ech iq e in w hich a sample is subje t ed t o ex citation of mole ular b n s b bro d-b n infra-r d

radiation, an the F ourie trans orm mathematical t echniq e is used t o o tain an a sorption spe trum

Spe tra can be o tained asa function of p sition x an y within a sample an is caled FT-IR ima ing

5.17.3 Advantag es

5.17.3.1 Can dete mine chemical s ructure an comp sitional analysis of chemical mix tur es in sold or

gas phase

5.17.3.2 High thr oughput ,high sig nal-to-noise ratio an hig h wa veleng th ac ur acy

5.17.3.3 Samples can be ru u de eithe ambient emperatur e (in pur g ed air) or ex tr eme envir onmental

con itions such as ultr a-high v cu m, c y -temperatur e, high pr es ure, high temper atur e

5.17.3.4 T ypicaly non-destructive an r eq ir es lttle sample pr ep ration

5.17.3.5 Insensitive to s r a y lght

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5.17.3.6 L r g e penetration depth;can acq ir e spe tra thr oug h low b n gap semicond ctors.

5.17.4.3 Spe tral complexity req ir es ex pe ienc d use s or ac es to spe tr al lbr ary for pr ope b n

as ig nment

5.17.5 Me surand

5.17.5.1 Chang es in dipole moment of the excited vibr ational modes (complementary te h iq e to

Raman spe tr osco y)

5.17.5.2 Chemical vibrations ar e measured in wa ve n mbe (cm

−

)

5.17.5.3 Coupled with IR-micr osco eor scan ing tip, it mig ht be ca a le of siz dete mination

5.17.5.4 Coupled w ith atten ated total refle tion (ATR) c ys als, it can dete t ultra-thin (monola ye

thick es ) fim or mole ular spe ies in aq eous phase ( pe ial setup ne ded)

5.17.6 Relevant standar ds for FT- R

— ISO/TS 141 1, S rfc e charac te i zatio o g ld n n p rticles fr n n mate ial s pec ific tox ic it y

sc re nin : FT-IR meth d

5.18 Induc ed g rating method (IG)

5.18.1 Des r iption

A t ech iq e b sed on a principle for measuring the siz of nano articles using the phenomenon of

diele tro hor sis an difract ed lght

Siz , siz dis ribution

5.18.3 Advantag es

5.18.3.1 Simple, rapid measur ement

5.18.3.2 Smal dis urb nc from lar g er p rticles

5.18.3.3 S nsitive to siz measur ements u de 1 nm

5.18.4 Limitatio s

5.18.4.1 L we lmit 0,5 nm to 1 nm; up e lmit 20 nm to 5 0 nm

5.18.4.2 Sample r eq ir ed to be dispe sed in lq id

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5.18.4.3 Dispe sion lq id req ired to be diele tric an not con uctive.

5.18.5 Me surand

Hydrodynamic eq iv lent diamet er

No s an ards we e identified

5.19 Inducti vel y c oupled plasma–mas spectrometr y (ICP-MS) and single par ticle

inducti vel y c oupled plasma–mas spectr ometry (SP-ICP-MS)

5.19.1 Des ription

An analytical t echniq e used for elemental det erminations, in w hich ions ar g ene at ed in a high

t empe atur , atmosphe ic pr s ur , arg on plasma an det ect ed using a mas spe tromet er

ICP-MS sy st ems can be ru in single p rticle mode ( SP-ICP-MS) w hen analy sing nano-o je t These

p rticles pr sent in an aq eous solution ar introd c d t o the arg on plasma As the dro let ar

desolv t ed in the plasma, the r sulting p rticles ar ioniz d, prod cing a burs of ions (one ion clou

pe p rticle) The ions then p s int o the q adrup le for analy sis The p rticles ar cou t ed using fas

data acq isition spe ds of up t o 1 0 00 pt /s (data p int o se ved b the det ect or) an using ve y

short dwel times

[26]

Conc ntration (p rticle n mbe an ionic), siz , siz dis ribution, chemical comp sition

5.19.3 Advantag es

5.19.3.1 High sensiti vity analysis — dete tion lmit of mos element ar e on the or de of ng /l (ng /kg )

or lowe

5.19.3.2 Multi-element analysis p s ible

5.19.3.3 Can dete mine element identity an q antity, typicaly in les than one min te

5.19.3.4 Wide lnear dynamic rang e w ith eight or de s ofmag nitude (in conventional mode)

5.19.3.5 Isoto ic information p s ible

5.19.3.6 Isoto e diution calbr ation pos ible

5.19.3.7 Can difer entiate betwe n dis olved an p rticulate analytes

5.19.4 Limitatio s

5.19.4.1 Spe tral inte fer enc oc urs when the instrument cannot dis ing uish the spe trum of an analyte

ion fr om the spe trum of a concomitant ha ving the same nominal mas -to-char g e ratio Mole ular ion

inte fer enc scan ofen be mitigated using col sion/r eaction c ls; elemental iso ars should be a voided

5.19.4.2 Contamination in blan s (acids, wate , etc.) can sometimeslmit dete tion an q antification

Tiêu đề	Nanotechnologies — Measurement Technique Matrix For The Characterization Of Nano-Objects
Trường học	ISO
Chuyên ngành	Nanotechnologies
Thể loại	Technical report
Năm xuất bản	2016
Thành phố	Geneva

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Số trang	66
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