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Preparation of sulfomethylated softwood kraft lignin as a dispersant for cement

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Article  in  RSC Advances · May 2015

DOI: 10.1039/C5RA04526F

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Wenming He Pedram Fatehi

Lakehead University Thunder Bay Campus Lakehead University Thunder Bay Campus
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Electronic Supplementary Material (ESI) for RSC Advances.
This journal is © The Royal Society of Chemistry 2015

Preparation of sulfomethylated softwood kraft lignin as a dispersant for cement

admixture
Wenming He and Pedram Fatehi*
Chemical Engineering Department, Lakehead University, 955 Oliver Road, Thunder Bay,
Ontario, P7B 5E1, Canada
*E-mail: pfatehi@lakeheadu.ca; Tel: 807-343-8697; Fax: 807-346-7943

Supporting information

S1-Table S1 lists the raw data for the charge density determination of OSKL, which was
produced under the conditions of 100℃, time of 1 h, and a nitric acid concentration of 20 wt.%.

Table S1. Raw data for charge density analysis of OSKL analysis
Samples PVSK Volume, mL OSKL, g Charge density,
concentration, M meq/g
OSKL 0.005 7.74 0.01 3.87

OSSKL was produced under the conditions of 100 ºC, 3 h, 1/1 HCHO to lignin and 0.5/1
Na2S2O5 to lignin molar ratios. Table S2 lists the raw data for the carboxylate and sulfonate
group analysis of OSSKL.

Table S2. Sulfonate and carboxylate group analyses via titration using DDMICI at 0.0055 M
concentration and with 0.01 g lignin (oven dried).

Samples Volume, mL Carboxylate group, Sulfonate group,

meq/g meq/g
OSKL E2: 5.52 1.69 0
OSSKL E1: 2.45 0 1.35

In Table 2S, E1 is the volume of DDMICI standard solution used for the sulfonation degree
analysis and E2 is the volume of DDMICI standard solution used for carboxylate group analysis.

Figure S1 (left) shows the titration curves of sulfonate group analysis and Figure S1 (right) shows
the titration curves of carboxylate group analysis of OSSKL, respectively. In this figure, the blue
line shows the U and red line show the ERC. U is potential of titration (mV), and ERC is
abbreviation of equivalence point recognition criterion.

1
 Figure S1. Potential and equivalence point recognition for sulfonate group (left) and carboxylate
group (right) analyses of OSSKL

S2-GPC analysis

Figure S2 shows the refractive index of GPC analysis as a function of time using viscometer and
RI detectors. In this figure, it is observable that SKL had a broad MW, due to its board retention
time in the GPC column. However, the elution time was shorter for the modified lignin samples.
The SLS and LASS had long elution times, which imply that their molecular weight distributions
were board.
Refractive index response,

350
SKL
300 OSKL
250 OSSKL
mV

SLS
200
LASS
150
100
50
0
15 16 17 18 19 20 21 22 23 24 25
Retention volume, ml

Figure S2. Chromatograms of samples of lignin

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