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Comparison of conventional rheology and FT rheology analysis for commercial toothpaste formulations
Seher Ozkan, William E. Prosise, Fu Chen, and Germain Puccetti Ashland Specialty Ingredients, Corporate Research Center, Bridgewater, NJ
INTRODUCTION
Materials
CONCLUSIONS
RESULTS
Materials: In this study, full and 1:1, 2:1 and 9:1 dilutions of ten commercial toothpaste formulations were characterized :
Results show that, multivariate Principle Component Analysis with covariance matrix on the rheological parameters of different toothpaste formulations, is an effective method to map out the relationships between the formulations as well as between the parameters. Interestingly, the formulations that are mapped out as similar on PCA graph have similarities in their LAOS “fingerprints” as well. Future work will investigate the links between the FT rheology (LAOS) parameters with conventional parameters and their correlation with sensorial attributes.
The utilization of Fourier Transform (FT) Rheology with Large Amplitude Oscillatory Flow data (LAOS) for determining the relationship between sensorial perception and rheological parameters is a fairly new method in the Personal Care industry, specifically within Oral Care. Lissajous curves of LAOS data provide a very effective visual aid to differentiate formulations via “fingerprinting” them, but there is insufficient data to interpret these material “fingerprints” in the context of consumer perception
Methods Dynamic oscillatory flow, steady torsional flow, continuous shear rate ramp, and compression / extension tests without suppressing wall slip were conducted. Diluted formulations were centrifuged and the supernatant fluid’s static surface tension values were measured. Extensional viscosity indices were also characterized by a microcapillary rheometer. All samples were tested with the LAOS method without suppressing wall slip and FT analysis was applied to calculate material parameters besides their “fingerprints”. All results were correlated using principle component analysis (PCA).
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.s Cohesive work
Compressive work
Variable Unit Notes
Variable
name on
graphCohesive work N.s Full formulation CHW
Compressive work N.s Full formulation CMW
Static surface tension (2:1) mN/m 2:1 diluted ST
Shear viscosity at 1s-1 (1:1) Pa.s 1:1 diluted SV111
Shear viscosity at 100s-1 (1:1) Pa.s 1:1 diluted SV10011
Shear viscosity at 1000s-1 (1:1) Pa.s 1:1 diluted SV100011
Shear viscosity at 1s-1 (2:1) Pa.s 2:1 diluted SV121
Shear viscosity at 100s-1 (2:1) Pa.s 2:1 diluted SV10021
Shear viscosity at 1000s-1 (2:1) Pa.s 2:1 diluted SV100021
Strain sweep, tand at 0.1% strain tand Full formulation SStand01
Strain sweep, complex viscosity at 0.1% strain Pa.s Full formulation SSCV01
Strain sweep, tand at 100% strain tand Full formulation SStand100
Strain sweep, complex viscosity at 100% strain Pa.s Full formulation SSCV100
Strain Sweep Max. Elastic stress (G'xstrain) Pa.s Full formulation MES
Frequency sweep, tand at w=1rad/s tand Full formulation FStand1
Frequency sweep, complex viscosity at w=1rad/s Pa.s Full formulation FSCV1
Frequency sweep, tand at w=100rad/s tand Full formulation FStand100
Frequency sweep, complex viscosity at w=100rad/s Pa.s Full formulation FSCV100
Frequency sweep, tand at w=1rad/s tand 1:1 diluted FStand1dil1
Frequency sweep, complex viscosity at w=1rad/s Pa.s 1:1 diluted FSCV1dil1
Frequency sweep, tand at w=100rad/s tand 1:1 diluted FStand100dil1
Frequency sweep, complex viscosity at w=100rad/s Pa.s 1:1 diluted FSCV100dil1
PowerLaw consistency index m, Full before shear PLm
PowerLaw index n Full before shear PLn
HB Yield Stress T0, Pa Full after shear HBT0
HB consistency index m, Full after shear HBm
HB Power law index n Full after shear HBn
2nd Harmonic I Full formulation, 100% strain 2ndH
3rd Harmonic I Full formulation, 100% strain 3rdH
5th Harmonic I Full formulation, 100% strain 5thHLarge strain modulus Pa Full Formulation 100% strain GL100Minimum strain modulus Pa Full Formulation 100% strain GM100Large strain rate viscosity Pa.s Full Formulation 100% strain VL100Minimum strain rate viscosity Pa.s Full Formulation 100% strain VM100Q-value Full Formulation 100% strain Q100Stiffening ratio Full Formulation 100% strain S100Thickening ratio Full Formulation 100% strain T 100Chebishev e3 intensity Full Formulation 100% strain e3100Chebishev v3 intensity Full Formulation 100% strain v3100Large strain modulus Pa Full Formulation 400% strain GL400Minimum strain modulus Pa Full Formulation 400% strain GM400Large strain rate viscosity Pa.s Full Formulation 400% strain VL400Minimum strain rate viscosity Pa.s Full Formulation 400% strain VM400Q-value Full Formulation 400% strain Q400Stiffening ratio Full Formulation 400% strain S400Thickening ratio Full Formulation 400% strain T 100Chebishev e3 intensity Full Formulation 400% strain e3400Chebishev v3 intensity Full Formulation 400% strain v3400
Large strain modulus Pa 1to1 diluted 400% strain DilGL400
Minimum strain modulus Pa 1to1 diluted 400% strain DilGM400
Large strain rate viscosity Pa.s 1to1 diluted 400% strain DilVL400
Minimum strain rate viscosity Pa.s 1to1 diluted 400% strain DilVM400
Q-value 1to1 diluted 400% strain DilQ400
Stiffening ratio 1to1 diluted 400% strain DilS400
Thickening ratio 1to1 diluted 400% strain DilT 100
Chebishev e3 intensity 1to1 diluted 400% strain Dile3400
Chebishev v3 intensity 1to1 diluted 400% strain Dilv3400
Normalized extensional viscosity index 2:1 diluted 5000s-1 shear rate ExtV
RESULTS
0 500
-200
0
200-0.5 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
-0.5
0.0
0.5
Colgate Total Advanced
Crest Pro-Health
Colgate 2in1
Colgate Optic White
Crest 3D White
Arm&Hammer Advanced White
LG Bamboo Salt
Cnice
Lion Zack
Prin
cip
al C
om
po
ne
nt
2
Principal Component 1
0 500
-200
0
200-0.5 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
-0.5
0.0
0.5
CHW
CMW
STSV111SV10011SStand01SStand100
SSCV100
MES
FStand1FStand100
FSCV100
PLmPLn
HBT0
HBm
HBn
GL100
GM100
VL100
VM100
Q100S100T 100e3100v3100
GL400
GM400 VL400
VM400
Q400S400T 400e3400v3400DilGL400DilGM400DilVL400DilVM400DilQ400DilS400DilT 100Dile3400Dilv3400ExtV
Colgate Total Advanced
Crest Pro-Health
Colgate 2in1
Colgate Optic White
Crest 3D White
Arm&Hammer Advanced White
LG Bamboo Salt
Cnice
Lion Zack
Prin
cip
al C
om
po
ne
nt
2
Principal Component 1
-130 -125 -120 -115
-12.5
-10.0
-7.5-0.50
-0.035
-0.030
-0.025
CHW
CMW
ST
SV111
SV10011SStand01SStand100
SSCV100
MES
FStand1FStand100
FSCV100
PLm
PLn
HBT0
HBm
HBn
GL100
GM100
VL100
VM100
Q100
S100
T 100
e3100
v3100
GL400
GM400
VL400
VM400
Q400
S400
T 400
e3400
v3400
DilGL400DilGM400
DilVL400DilVM400
DilQ400DilS400
DilT 100
Dile3400
Dilv3400
ExtV
Colgate Total Advanced
Crest Pro-Health
Colgate 2in1
Colgate Optic White
Crest 3D White
Arm&Hammer Advanced White
LG Bamboo Salt
Cnice
Lion Zack
Prin
cip
al C
om
po
ne
nt
2
Principal Component 1
-124 -123 -122 -121
-11.6
-11.4
-11.2
-11.0
-10.8
-10.6
-10.4-0.49
-0.0365
-0.0360
-0.0355
-0.0350
-0.0345
-0.0340
-0.0335
-0.0330
CHW
CMW
ST
SV111
SV10011 SStand01
SStand100
SSCV100
MES
FStand1
FStand100
FSCV100
PLm
PLn
HBT0
HBm
HBn
GL100
GM100
VL100
VM100
Q100
S100
T 100
e3100
v3100
GL400
GM400
VL400
VM400
Q400
S400
T 400
e3400
v3400
DilGL400
DilGM400
DilVL400
DilVM400
DilQ400
DilS400
DilT 100
Dile3400
Dilv3400
ExtV
Colgate Total Advanced
Crest Pro-Health
Colgate 2in1
Colgate Optic White
Crest 3D White
Arm&Hammer Advanced White
LG Bamboo Salt
Cnice
Lion Zack
Prin
cip
al C
om
po
ne
nt
2
Principal Component 1
-124 -123 -122
-11.4
-11.2
-11.0
-10.8-0.494 -0.493 -0.492 -0.491 -0.490 -0.489 -0.488 -0.487
-0.0360
-0.0355
-0.0350
-0.0345
CHW
CMW
ST
SV111
SV10011
SStand01
SStand100
SSCV100
MES
FStand1
FStand100
FSCV100
PLm
PLn
HBT0
HBm
HBn
GL100
GM100
VL100
VM100
Q100
S100
T 100
e3100
v3100
GL400
GM400
VL400
VM400
Q400
S400
T 400
e3400
v3400
DilGL400
DilGM400
DilVL400
DilVM400
DilQ400
DilS400
DilT 100
Dile3400
Dilv3400
ExtV
Colgate Total Advanced
Crest Pro-Health
Colgate 2in1
Colgate Optic White
Crest 3D White
Arm&Hammer Advanced White
LG Bamboo Salt
Cnice
Lion Zack
Prin
cip
al C
om
po
ne
nt
2
Principal Component 1
