28.02.2013 Views

Handbook of Size Exclusion Chromatography and Related ...

Handbook of Size Exclusion Chromatography and Related ...

Handbook of Size Exclusion Chromatography and Related ...

SHOW MORE
SHOW LESS

Create successful ePaper yourself

Turn your PDF publications into a flip-book with our unique Google optimized e-Paper software.

Table 10 Refractive Index Increment (dn/dc) <strong>of</strong> Cellulose Used for the Evaluation <strong>of</strong><br />

SEC by On-Line Laser Light-Scattering Detectors a<br />

Sample Solvent<br />

The accuracy <strong>of</strong> the obtained M w value presupposes that the dn/dc has been<br />

properly determined under the conditions used for the SEC. Sample solutions<br />

should preferably be dialyzed against pure solvent prior to determination, but this<br />

is not possible for LiCl/DMAc solutions because the solvent will swell or dissolve<br />

the dialysis membranes. It is important to prepare the solvent in a reproducible way<br />

because an increase in the concentration <strong>of</strong> LiCl decreases the dn/dc value (222).<br />

In Table 10, reported dn/dc values <strong>of</strong> some types <strong>of</strong> celluloses used for evaluation<br />

<strong>of</strong> chromatograms by on-line light-scattering detectors are shown.<br />

7 CONCLUSIONS<br />

dn/dc<br />

(mL/g)<br />

Wavelength<br />

(nm)<br />

Temperature<br />

(8C) References<br />

CTC THF 0.163 632.8 — 231<br />

CTC THF 0.155 633 25 121<br />

CTC THF 0.163 690 Ambient 117<br />

TMSC THF 0.059 646 25 101<br />

CMC 0.02 M or<br />

0.1 M<br />

0.163 633 25 156<br />

NaNO3<br />

Cellulose ethers b<br />

0.01 M NaCl 0.128–0.132 632.8 30 224<br />

Cellulose ethers b<br />

Phosphate buffer<br />

I ¼ 0.1, pH 6.5<br />

0.15 632.18 — 165<br />

Cellulose 0.5% LiCl/<br />

DMAc<br />

0.163 690 — 194<br />

Cellulose 0.5% LiCl/<br />

DMAc<br />

0.104 633 40 198<br />

Cellulose 0.5% LiCl/<br />

DMAc<br />

0.108 488 Ambient 225<br />

a The literature reference contains dn/dc values <strong>of</strong> different types <strong>of</strong> carbanilates.<br />

b Nonionic.<br />

The great number <strong>of</strong> applications shows that SEC is the preferred technique to gain<br />

information about cellulose <strong>and</strong> its derivatives. During the past decade, SEC <strong>of</strong><br />

cellulose has been focused on carbanilated cellulose samples or direct dissolution<br />

<strong>of</strong> cellulose samples in lithium chloride/N,N-dimethylacetamide (LiCl/DMAc).<br />

For derivatives, the trend is to perform derivatization <strong>of</strong> cellulose in homogeneous<br />

phase using LiCl/DMAc. Qualified evaluation <strong>of</strong> SEC results has<br />

become possible by using dual detection including differential viscometry (DV)/<br />

© 2004 by Marcel Dekker, Inc.

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!