toothpasterheology_sor_ozkan etal 2014v1

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