Data File C:\CHEM32\ ...

G-2000\POLIETILENGLICOL-JUEVES12-SET
Sample Name: ST14BO

2013-09-12 14-32-41\001-0101.D

Data File C:\CHEM32\ ..,G-2000\POLIETILENGLICOL-JUEVES12-SET

Sample Name: ST14BO

2013-09-12 14-32-41\001-0101,D

RI01 A, Reftactive lndex Signol (PRUEBA PEG ..LlETILENGlICOLJUEVES12-SET

Acg. Operator
Acq. Instrument
Injection Date
Acq. Method
Last changed
Analysis Method
Last c-hanged

SYSTEM
HPLC 1260 RID
9/12/2013 2:33:50 PM

Seg. Line
1
Location
Vial 1
Inj
Inj Volume
Manually
C:\CHEM32\1\DATA\PRUEBA PEG-STANDARES-PEG-2000\POLIETILENGLICOL-JUEVES12SET 2013-09'-12 14-32-41\POLIETILENGLICOL.M
9/12/2013 2:32:41 PM by SYSTEM
C:\CHEM32\ 1\DATA\PRUEBP. PEG-STANDARES- PEG-2000\ POLIETILENGLICOL-JUEVES12SET 2013-09-12 14-32-41\POLIETILENGLICOL.M (Sequence Hethod)
9/12/20:3 4:14:20 PM by SYSTEM

nRIU

6000

r>

II

5000

/0 / ( (
00

.-----------------

2013-()9.12 14-32-411001-0101.0)

\\.

4000

\
\

'

\\

/
.
!
/

3000

/
/

\
\

'\

1ooo+-~~--~.-~-19

',PLC 1260 RID 9/12/2013 4:20:04 PM SYSTEM

Page

1 of 3

,
,

-- --_'.::::>-,---

2000

19.2

-r~--~~-r~--~
19.6
19.4

HPLC 1260 RIO 9/12/2013 4:20:04 PM SYSTEM

__ -'
19.8

~~--~~~-.--~~-r-.--~~
20

20.2
Page

20.4

2 of 3

mi

'R!

Se distinguen los siguientes los siguientes pesos moleculares promedio:

Peso molecular numrico medio:
Mn

= (n1M1+ n2M2+n3M3+ ... ) / (n1+ n2+n3+ ...)

Donde n1, n2, n3, etc. es el nmero de moles de las macromoleculas

de peso molecular

M1, M2, M3, etc, respectivamente.

Peso motecuter ponderal medio:

Mw = (W1M1+W2M2+W3M3+
...)
Donde W1,W2,W3,etc. son las fracciones en peso correspondientes
de peso molecular

a las macromoleculas

M1, M2, M3, etc, respectivamente.

Con el propsito de aclarar estos conceptos podemos hacer la suposicin que todas las
macromolculas

de un pollrnero

ht~otfico

constan

solo de tres pesos

moleculares

diferentes M1, M2, M3, siendo n1,n2, Y n3 el nmero de estas rnacrornoleculas de cada
peso molecular y W1,W2, W3, la fraccin en peso que cada tipo representa del peso total.
Entonces aplicando las formulas anteriores tendr-amos:

".

e 'Ro M A T o G''R

A El ~ :::b E -p E.l( M E A e IoN

EN
G'fc ==

S. E

e _

S.I..i -

GEL

ex e L US./QN

C H1.0MATOG ~ A?/4Y

CRotJ\AToGRAfIA

:be

<XCLUSION

~O~

TAMAO

LA

CROMATOG."RAf"IA.

Es.

UNA

TECNICA

l::.N <; s..oLUCIN

,

E s. F ~, e A .s

L AS

~o ~ o s, A.s:

e UL

coLUMNA.S

T ALE

LJ N

S.

Qu~

-PE~MIT(

G-~L

EN

t>:"RMEACloN

'r"oLIM!~OS

.s.<:"A~AR

MJ:/AN-r

~AeTI

::h

As.

ES

:h o L

TI 'P o

Fe RI e A oS

Efo/l.l"L~A::b.AS

N IE

CoNT.

EN

Be

?o"1.oS

G'PC.

HECHAs

soN

t. (~. c::.Hel"3.) e.s,

N ~ o

TECNICA

LA

"P A R.T "

le uLAS

saLVE. NT

I N J e o .

G- E L N o

~~

A T~ AVE~

M1i E A'Ao

'-"1

::bE

LA

CoLUMNA

-:r:qJ_(M{!.IC.A

A.

EN

MU~STRA

l7>oLI,4-1e.tt:.1c.A

uNA.

E,..,ToNCES

MISM

ee

col.UMNA.

LA

G-PC

s.oLV~NT(

FI!!Ac.c.tONAflla/ENTO

~.s()'-TA

::J::.~

ES

l'

.soLve/oN
/NyEcTAl>A
.::b~ LA

H!CHO

::::bt

~u

S oN

LA.s
o

MAc,t.o1J(jCu~S

e u I ~A.5

~E

:::t:. , F (fE/t::. -EN T f. S

.:::r::dF~1!.NT~S. TA.41A'oS

-r J e M r- o S .

Solvent reservoir

Mixing
valve

SEC columns

.
Detector

Injection port

Figure ..Schematic of a typical size-excluson chromatograph

EL

FAcc.(ONAMI~NTO

H l"b te,o :hJ N A MI

:h~

AS.

system.

MAc~aMoL(;c.u1.A.5

eo

MAS

"e u L A S.

LAs
E So S

-:p A R. T \

oL

-:;-

:bER/..bo

(M

e ~o S

e()~

ES.

I~o~

tN

~S.F"E~/CAS

E LU Y N

SoN

R(TENCJN

~-

CoNT(5N

eN

NTONCs.

~ ~ I f\1 R

L U G A f!:.

Y.sU

XCLc.;(:bOS/

Vo(..ul'i/oJ

:PE6}u~NO.

:N
SoN
LAS

'RETENJ~O.s

.N

? A~TrC OL. A.s

Los

~o1to.s

E s F~'~I C.AS

<3

L. A.

SOUC{aN

INT~!:.ST'CloS

~ E~

CJ/~

eN

~E

E NTO'NC(S

==

Small
permeating
molecules

-r--,

Large
excluded
molecule

Bulk
movement
of solvent

,
:'

Figure ._

Illustration

of the separation of polyrner rnolecules of different sizes in

size-exclusion chromatography.

VI:

+ k,J. Vi 1

Vd

Vo

VOLul4~N

MW/~O

"

Vi

L'QU/llO

"U~~A

:h~~20

EL

Vo

ui a

'RAeoN

.::h ~

EL

HAs.iA

<i}(J~

FfNAL::Jl<

Los. -:p.o~ oS .

A Ni

e ~ ue ~ E -p 1e ES t N TAl..

~E

LA

,?OL I ~ I!. 6

~L

MAT(~IA

T~AN~1-a7'1.TA~

L UM ~N

K _ e o 'N S.T

'.

~A~A

LUIACJ

CONCt:NT~ACloN

.::::bEN T

t. <3 't F u e ~ A ::z:. E too s

-.po ~o So

kJ

Vi _

~E-P~~SENTA

VO'M~N

.:bE

1:LACla'NA~A
.::bE ~

As.

e oLlJ/lAf\I

A..s.

ENTI!(E;CU~A':h6

zs e

103

r.-

rr.

G-l' C.

LA

'"PoLI

s.oN

-:PU:l:l~N

~TNCJO'f(

A LA

M ~ I!.~

=ll<:.L

FOI!CloN

ce

Hc H A~
S7At::.A(f!.

~U~

~tTA

INT(E7i?AccioN

eA

~ c:

CoL

OM N A

-=PoLI ~ s..T,,~eNo

-=r~sos

MoLc.uLA~S

/0":1.

1000

tr..--..

LOs

:bETECTO'R-E

EN

G""P'C

zs e :

SON

:::bIF~EtJC/AL~S.

Le

::l;)

1IV14( e
-:::.

o el

el

ET- cTO

ee

f:

RE F

::h E

M le I e A

'y

1"'")).1 C~

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LA

:::hL

llN
LA

(MI"b~rI

'RI

M 1::J:l <: N

S aL V

.:::2)

CoMo

UNA

G-"PC

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.s

LA

V ~s. o s:

G--=fC

:b. ~ L

:.::bt"R

el.

.s e e

::-o~MA

se-

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s. al. u. el (J N

Es.

-p~(J"po~C.IQ"".A.t....

(~C'M~~O).

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ve,c

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'PLtSTtO

(f<,I)

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sus

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Sf;X-=f'I!.ESA:D.A

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A'jU~A~j

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::b~TCTDt:!.

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re

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1t~ F~Ac<:'(oN

~d

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USA.:bs.

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eL

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EL

'RI

Cot:~-':;ACloNA~
-:poLI

CONtUNffNi

TJ?Q

CoNCNTt:.Aclo'N

~,,'~"
,

MAS

sox~~

LINEA

UNA

CALIRI!A.:bo

-:po~<VIA.ftJNit

el..

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,
MOL~CVI.A~

AL

VaLUM~N

CLcJl::bO.

( u~ VA

.::b. E

-=rLoTEo

EL

ME1JeANT

CALlghAc./aN
::]:)Ec...

Es

-r~o1Juc(l:.A

oGAt::!TMO

::bEt..

M o i: CULA I!. v 1:. .s o s

e VOt.UrfN :J::. E
-----------------,-,-~~~----~-------~---------=-.:..-

ct..UC/oN:

6(~~T~NClN)

Total exclusion

Total permeation
Selective permeation

'/-= "";.< -\- b

,--

y"'" 10 M
X=V"

f'M:::::.JS

Elution- volume

Figure. -: The general form of a calibration curve used in size-exclusinr, chromatography.

z, M - A, + VR
I~------~---------

eC.

U .
--

"]S

\f

~~s--

"\

2
2.0

2.5

3.0

':-..

\\

\\
\,l
~-b

3.5

Retention volume. mL

Fig . ';;'" Molecular weight calibration tange of polystyrene as a function of pore

size; pore size determines the MW separation scale, psm = average pore size.

~J.

107

2000000
122500
77000
2300000
1130000

10'

470000

'O

-;; 105
CII

~
..

~f~

ea
'O 104

:e

103

fl '"0.999

1~.+-~-r-.-.--r-.-.--r-.-.~r-.-.--r-+-.
~~~~~~~~~~~M~~ro~~
Retentlon

<;

volume (mL)

VR.

FIgure 1.6 Separatlon range of SEC: elution of linear polystyr!3ne standards. Circles denote
. average elotion time of trlpllcate lnJectlons of each narrow polydispersity PS standard, with error
bars substantlally smal\er than data markers and therefore not shown. Numbers next to markers
denote the peak-average molar mass, Mp, of each standard In g/mol. Solid line is a third-order
frt to the data, Wlth
0.999. Solvent, 1,2,4-trichlorobenzene
(wlth 1.5 mglmL Santonox);

,2 -

temperature, 135C; co/umns, PL~el Mlxed A;flow

wlth per:mlsslonfrom Ref. 27.)

vo co rce t

:h

rate, 0.1 mUmin;

detector,

DRI. (Reprinted

El. UC d'r{

80
70

\ W;K
....

~i\
/

60
50
h

20
10

Fig.~~

FUNCloN

::t::.

~ECol::2:.ATDI!Ic>

",--

cCJNC6NT~AC(oN

=i:::.L.

w, .

LA

IY'\

tm o.S~ J.~ v"" -- ~u~j-y __ J~ 3:oj{tM~VO

.
~
"",-CYo
40 IGoI ~ L 4.t e e, J e-t.._~ rol fr'p.~yi e . s
fI\

MM ._ w :: wi

-Mm
~..

Ni

z.

NM

Z.Wj

z Ni

- f"VM~

LA

ALTUI!A

~ E

L.A

cU~V

- e.
Mi

AL

s:

1.

G"PC
LA

MASA

VaLUI-f("N

J:

e t:e

N el o N .

Mw
'2

NM

Mw
L

c:t~.~i

i ;::

Mw -

<,

j=

h i Mi

~i
.

1= /
N

'"

:bls'PE'Rs./oN:

MW/MM

1=/

j:::. {

E"(f

1.2

c: 1.0
.S!

...

E 0.8

s:

01

0.6

:!
'E
.m
..m

0.4

0.2

::

g1mol

0.0

n4

Flgure~..o-

5 X 106
glmol

2 x 10

105
10'
MoJar masa (g1mol)

Molar mas:s av&tag:es anddtstribution

01 brominated

polystyrene.

PSBr. MMO and

molar mass avera-g:es detimnmed by SEC wIth cftfferential relractive index and sta tic multiangle
IIght-scatterlng detectlon. Soiv.ent, DMActO.5% LIC\; temperature, 3Se; flow rate, 1 mUmin;
columns, three PSS GRAUlnear 101~
cofumns and one PSS GRAL10000 10..un colurnn,
preceded by a guard column. Mn
3.26 x 105 glmol, M.,., 6.74 X 105 glmol. Mz = 1.17 X 106
g1mol:M.,.,IMn
2.07. (Adaptedtrom
Rel. 26.) I

'PROBLEMA
A size-exclusion chromatogram was obtained for a sample of poly(methyl
methacrylate) (PMMA) in tetrahydrofuran at 25C. with the data derived from
the experiment being listed below in Table 4.4. Under identical conditions. sarnpies of PS with narrow molecular weight distributions were also examined by
using SECo A linear calibration curve was produced, with M = 98000 elutinq at
a retention volume of 130 mi and M,= 1800 eluting at 165 mI. Calculate M", and
Mw for the PMMA sample.
\

Table 4.4 SEC data obtained for a sample of

poly(methyl methacrylate) in toluene (SAQ 4.6)
Retention volume (mi)

Height (cm)
1.0

130

,-...

135

12.0

140
145
150

51.4

155

51.2

160

17.8
4.4

89.0
84.0

165

Lo G-

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Certificate of Analysis
Polymer type:

Poly(2-vinylpyridine)

Part No:

PSS-pvp1k

Lot No:

pvp290113

Molar Mass Distribution

225

2.00

1.75

,.50

'25

i'
C>

.2

'.00

~
0.75

0.50

025

Molar mass [Da]

GPC/SEC - Conditions
20 JI

Sample concentration

1,00 gIl

Inject volume

Solvent

THF, N,N-Oiethylethylenediamine 0.1Vol%

Flow rate

1,00 ml/min

Precolumn [8 X 50 mm]

PSS SOV5Jm

Temperature

23e

Operator

S.Fugmann

Colurnns [analytical, each 8 X 300 mm] PSS SOV 5Jm 10e3A / 1Oe5A/1 Oe6A
Data Acquisition Software

PSSWinGPe

GPC/SEC - Results

Note:
Mw = Weight average molecular weight
Mn = Number average molecular weight
Mp = Molar mass at the peak maximum
POI = Polydispersity Index

Storage:

Store the tightly recapped polymer standard in a

dry, dark, cool area; e.g. a refrigerator (4 "C).

Explration date:

5 years after purchase date provided standard is stored as

described above.

Manufacture

Purchase date:

and control

according

Dr.

Polyrner Standard s service GmbH

In der OalheimerWiese5
Tel.: +49 (O) 6131-96239-0
Email:info@polymer.de

0-55120 Mainz
Fax:+49 (O) 6131-96239-11
www.polymer.de

(PSS'

T. Hole

produclion

(PSS'

to PSS method 01 analysis

director

Polyrner Standards service - USA Inc

160Old FarmRd, SuiteA

Phone:+1 413-835-0265
Email:pssusa@pssgpcshop.com

Amherst.MA01002
Fax:+1 413-835-0354
www.pssgpcshop.com