(Đồ án hcmute) improving the sensory effects of hair conditioners with belsil® adm 331

MINISTRY OF EDUCATION AND TRAINING
HO CHI MINH CITY UNIVERSITY
OF TECHNOLOGY AND EDUCATION

THESE GRADUATED
ORGANIC CHEMICAL ENGINEERING

IMPROVING THE SENSORY EFFECTS OF HAIR
CONDITIONERS WITH BELSIL® ADM 331

SUPERVISOR: LE THI HONG NHAN
STUDENT: LE HOANG CONG
STUDENT ID: 15128004

SKL 0 0 5 9 9 7

HO CHI MINH CITY, AUGUST, 2019

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MINISTRY OF EDUCATION AND TRAINING
HO CHI MINH CITY UNIVERSITY
OF TECHNOLOGY AND EDUCATION
--------------------

B.Eng THESIS

IMPROVING THE SENSORY
EFFECTS OF HAIR CONDITIONERS
WITH BELSIL® ADM 331

Student: LE HOANG CONG
Student ID: 15128004
Thesis code: HC.19.01

Supervisor: Assoc. Prof. LE THI HONG NHAN

Ho Chi Minh city, August, 2019

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HO CHI MINH CITY UNIVERSITY OF TECHNOLOGY OF EDUCATION
FACULTY OF CHEMICAL AND FOOD TECHNOLOGY
DEPARTMENT OF CHEMICAL TECHNOLOGY
B.Eng. THESIS PROJECT
Full name: LE HOANG CONG

Student code: 15128004

Major: Organic Chemical Engineering
1. Name of thesis: Improving the sensory effects of hair conditioners with
Belsil® ADM 331
2. Projects:
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Choosing the target parameters from commercial hair conditioners.

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Studying effects of ingredients.

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Evaluating stability of products.

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Investigating of the market penetration of the products.

3. Started date: 16/01/2019
4. Finished date: 01/07/2019
5. Supervisor: Asscoc. Prof. Le Thi Hong Nhan
The thesis was approved by the Head of Chemical Technology Department
Ho Chi Minh city, 20th July 2019
HEAD OF Chem. Tech. DEPARTMENT

SUPERVISOR

Dr. Vo Thi Thu Nhu

Asscoc. Prof. Le Thi Hong Nhan

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ACKNOWLEDGEMENTS

First and foremost, I would like to express my profound gratitude and deep regards to
Asscoc. Prof. Le Thi Hong Nhan for her exemplary guidance, monitoring and constant
encouragement throughout the course of this thesis. I also take this opportunity to
express a deep sense of gratitude to my friends at Organic chemistry Lab for their
supports, valuable information and guidance, which helped me in completing this task
through various stages. Finally, an honorable mention goes to my family their
understandings and supports on me in completing this project. Once again, I owe my
deep gratitude to all who gave me the possibility to complete this study.

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COMMITMENT

I commit that this thesis is my own independent project. Experiment data in this
project are objective authenticity. References used in this report are clearly, fully cited.

Le Hoang Cong

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TABLE OF CONTENTS

ACKNOWLEDGEMENTS .............................................................................................i
COMMITMENT ............................................................................................................ ii
TABLE OF CONTENTS .............................................................................................. iii
LIST OF TABLES ..........................................................................................................v
LIST OF FIGURES ........................................................................................................vi
LIST OF APPENDICES ............................................................................................. viii
ABSTRACT ...................................................................................................................ix
PREAMBLE ....................................................................................................................x
CHAPTER 1: INTRODUCTION....................................................................................x
1.1. Human hair ..........................................................................................................1
1.1.1. Hair physiology ............................................................................................. 1
1.1.2. Structure of hair shaft ....................................................................................4
1.1.3. Chemical characteristics ................................................................................6
1.1.4. Physical characteristics ..................................................................................9
1.1.5. Hair classification ........................................................................................ 10
1.1.6. Healthy hair and hair damaged ....................................................................13
1.2. Hair conditioners.................................................................................................15
1.2.1. Function .......................................................................................................15
1.2.2. Types of hair conditioner.............................................................................17
1.2.3. Main ingredients .......................................................................................... 19
CHAPTER 2: EXPERIMENTAL - RESEARCH METHODOLOGIES ..................... 26

2.1. Materials and equipments. ..................................................................................26
2.2. Physicochemical properties measurement. ......................................................... 26
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2.2.1. Dryness ........................................................................................................26
2.2.2. Viscosity ......................................................................................................27
2.2.3. Color parameters ......................................................................................... 27
2.3. Sensory evaluation .............................................................................................. 27
2.3.1. Appearance ..................................................................................................28
2.3.2. Performance properties ................................................................................28
2.4. Stability evaluation ............................................................................................. 30
CHAPTER 3: RESULTS AND DISCUSSION ............................................................ 32
3.1. Cream base formula ............................................................................................ 32
3.2. Commercial product survey ................................................................................35
3.3. Studying effects of ingredients ...........................................................................41
3.3.1. Cetyl alcohol ................................................................................................ 41
3.3.2. Behentrimonium chloride and Silsoft E50 ..................................................45
3.3.3. Belsil® ADM 331 ....................................................................................... 51
3.3.4. Rheological additives ..................................................................................56
3.5. Evaluating stability of product ............................................................................67
3.5.1. Centrifugal seperation test ...........................................................................67
3.5.2. Temperature variation test ...........................................................................67
3.5.2. Cyclical temperature test .............................................................................71
3.6. Investigating the penetration of product ............................................................. 73
CONCLUSIONS ...........................................................................................................75
REFERENCES ..............................................................................................................77
APPENDICES ...............................................................................................................78

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LIST OF TABLES

Table 1. 1. Characteristics of each hair type .................................................................11
Table 1. 2. Characteristic of Assian hair (Source: Ref.[7]) ...........................................12
Table 1. 3. Common ingredient for hair conditioner .................................................... 24
Table 2. 1. Raw materials .............................................................................................. 26
Table 2. 2. Scoring system for sensory evaluation ........................................................ 27
Table 2. 3. Hair conditioners assortment protocol ........................................................ 29
Table 2. 4. The final formulation of target product ....................................................... 64
Table 3. 1. The formulation of original cream .............................................................. 34
Table 3. 2. The result of the market survey ...................................................................39
Table 3. 3. The experiment schedule of TBS and RBS series.......................................45
Table 3. 4. Content of Belsil® ADM 331 .....................................................................51
Table 3. 5. Changes in color and odor when store at 45 0C ..........................................68
Table 3. 6 Changes in color and odor when store at 15 0C ...........................................68
Table 3. 7. Changes in color and ordor during cyclical teamperature test .................... 71
Table 3. 8. The examination about ability to volume-up hair strand ............................ 74
Table 3. 9. The raw material charge for 1kg product .................................................... 75

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LIST OF FIGURES

Figure 1. 1 The anatomy of human hair (Source: Macrovector PTE Ltd) ...................... 2
Figure 1.2. Head hair growth cycle (Source: Shutterstock Ltd ) .....................................3
Figure 1.3. Schematic diagram of scalp hair (Source: Shutterstock Ltd) ........................ 4
Figure 1.4. The structure of the cuticle (Source: Ref.[5]) ...............................................6
Figure 1. 5. Chemical bonds in hair (Source: Ref.[6]) ....................................................7
Figure 1. 6. The Andre Walker hair typing system (Source: Amazon) ......................... 12
Figure 3. 1. Mixing procedure of ceam base .................................................................35
Figure 3. 2. Commercial hair conditioner as referred products.....................................37
Figure 3. 3. The general properties examination of commercial products. ...................38
Figure 3. 4. Appearance sensory evaluation of commercial products .......................... 39
Figure 3. 5. Performance sensory evaluation of commercial products ......................... 40
Figure 3. 6. Effects of cetyl alcohol on general properties ............................................43
Figure 3. 7. Effects of cetyl alcohol on appearance ...................................................... 43
Figure 3. 8. Performance sensory evaluation of CEA series .........................................44
Figure 3. 9. Effect of total conditioning agent content on general properties ...............47
Figure 3. 10. Appearance sensory evaluation of TBS series ........................................47
Figure 3. 11. Performance sensory evaluation of TBS series .......................................48
Figure 3. 12. Effects of ratio of conditioning agents on general properties ..................49
Figure 3. 13. Appearance sensory evaluation of RBS series.........................................49
Figure 3. 14. Performance sensory evaluation of RBS series .......................................50
Figure 3. 15. Effects of Belsil® ADM 311 at low content on general properties .........52
Figure 3. 16. Appearance sensory evaluation of BE#1 series .......................................52
Figure 3. 17. Performance sensory evaluation of BE#1 series ......................................53
Figure 3. 18. Effects of Belsil® ADM 311 at high content on general properties........54
Figure 3. 19. Appearance sensory evaluation of BE#2 serieres ....................................54
Figure 3. 20. Performance sensory evaluation of BE#2 series ......................................55
Figure 3. 21. Effects of hydroxylethyl cellulose on general properties ........................ 58
Figure 3. 22. Appearance sensory evaluation of HE series ...........................................58

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Figure 3. 23. Performance sensory evaluation of HE series .........................................59
Figure 3. 24. Effects of sodium chloride on general properties ....................................60
Figure 3. 25. Appearance sensory evaluation of SC series ...........................................60
Figure 3. 26. Performance sensory evaluation of SC series ..........................................61
Figure 3. 27. Effect of hybrid rhelological additives on general properties ..................62
Figure 3. 28. Appearance sensory evaluation of HS series ...........................................62
Figure 3. 29. Performance sensory evaluation of HS series ..........................................63
Figure 3. 30. Effects of scale to general properties ....................................................... 65
Figure 3. 31. Appearance sensory evaluation of samples in scale-up experiment ........65
Figure 3. 32. Performance sensory evaluation of samples in scale-up experiment ......66
Figure 3. 33. Results of centrifugal seperation test ....................................................... 67
Figure 3. 34. General properties changes when storing at 45 oC ..................................69
Figure 3. 35. Appearance changes when storing at 45 oC .............................................69
Figure 3. 36. Performance changes when storing at 45 oC............................................69
Figure 3. 37. General properties changes when storing at 15 oC ..................................70
Figure 3. 38. Appearance changes when storing at 15 oC .............................................70
Figure 3. 39. Performance changes when storing at 15 oC............................................70
Figure 3. 40. General properties changes during cyclical temperature test ..................72
Figure 3. 41. Appearance change during cyclical temperature test............................... 72
Figure 3. 42. Performance change during cyclical temperature test ............................. 72
Figure 3. 43. Testing on panels .................................................................................... 74
Figure 3. 44. Testing on volunteers ...............................................................................74
Figure 3. 45. Results of skin irritation ...........................................................................75

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LIST OF APPENDICES

Appendix 1 . The ingredients of commercial product in dosmetic market survey ....... 78
Appendix 2 . The detailed results of general properties ................................................ 80
Appendix 3 . The obtained results of sensory evaluation.............................................. 85
Appendix 4 . Customers satisfaction questionare ....................................................... 125
Appendix 5 . Results of product quality evaluation .................................................... 127

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ABSTRACT

To improve the sensory effects of hair conditioners, the original product, which was
made out of the basic ingredients and toward the smoothness line, was compared to the
commercial products for positioning the suitable segment and choosing the target
partameters. By studying effects of main ingredients (cetyl alcohol, conditioning
agents and rheological additives), the suitable content of them were determinated for
optimizing the feeling. Besides, during execution, Belsil® ADM 331 was added at
0,4% (w/w) to enhance the feel of use, especially in wet feel. The shelf-life of target
product was predicted about one year by the comom test in laboratory. After trial
period on consumers, the appearance and the feel in use of research product was
evaluate at good (4/5) grade with high accuracy level. Over 70% of volunteers (22/30)
were willing to pay from 50,000 to 70,000 VND for 1bottle / 250g. Besides, the raw

material charge for 1 kg product was only 32,000 VND. It was found that those
products came with reasonable and competitive prices. In conclusion, the research
product is available for commercial purpose.

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PREAMBLE

Hair contributes significantly to the visual image of both males and females of all
ages. Hairstyle, apparently, hides face limitations away, creates a highlight for good
looks and reveals personnel individuality. In general, traditional girl favorably chooses
classic hairstyle such as ponytail, bun, and shoulder-length. Styling hair by a pigtail or
bunches for the childlike concept. Long hair combined with a mild perm is the image
of a sweet girl. Dyeing hair is very suitable for the strong personality and short hair is
the best choice for the self-motivated.
Healthy hair is a key factor influencing the beauty of hair. It is reasonable to accept
that the weak hair isn‟t willing to build-up on hair. The non-glossy hair seems to look
like dirty and the arid hair being the same as bamboo root make a bad appearance. The
causes of hair damaged are mechanical traumas, chemical treatments, and
environmental factors. Therefore, hair care products, especially hair conditioner, are
essential demand for the fascinating hair.
I have a passion along with a curiosity in cosmetics and get a suggestion about the hair
care field by my supervisor, Assoc. Prof. Le TH Nhan. In addition, research and
development (R&D) is an aspect of my future job. For these reasons, I research on
topic "Improving the sensory effects of hair conditioners with Belsil® ADM 331" .

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CHAPTER 1: INTRODUCTION
Hair provides protective, sensory, and sexual attractiveness functions. All visible
major body surfaces are covered with some type of hair, providing endless
opportunities for cosmetic adornment. Nowadays, beautiful hair is indeed an important
part of personal beauty. In the aesthetic term, keeping hair in good conditions helps a
person feeling comfortable and confident. Changing hair into the desired color and a
fashionable style can improve attractiveness [1]. It is noticeable that, before styling,
you should pay attention to make a daily routine to take care of your hair because
healthy hair is the important factor influencing the beauty of hair. For instance, the
non-glossy hair seems to look dirty and the arid hair being the same as the bamboo
root makes a bad appearance. These are some signs of damaged hair. The causes of
hair damaged are mechanical traumas, chemical treatments, and environmental factors.
Moreover, hair is non-living material, therefore, hair care products, especially hair
conditioners, are an essential demand for fascinating hair. It is one of the key answers
for how to get healthy hair.
1.1. Human hair
1.1.1. Hair physiology
Hair is a protein filament that grows from follicles found in the dermis. Hair follicle
extends from the surface of the skin through the stratum corneum and the epidermis
into the dermis. Hair follicle is responsible for the formation and production of hair
fiber [2], in other words, impacts directly to almost the physiological of hair. All of
them are richly endowed with sensory receptors and have a highly-developed sense of
touch [3]. The difference in shape of this organ, which is specified by gene, makes the
diversity of natural hairstyle.

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Figure 1. 1 The anatomy of human hair (Source: Macrovector PTE Ltd)
The sebaceous gland located at the upper part of the follicle, being responsible for
secreting sebum, a natural hair conditioners including free fatty acid and neutral fast,
to lubricates and protects the scalp and hair [2]. Sebum is produced in increased
amounts after puberty in males and females and abundantly coats the hair shaft in
youth. With advancing age, sebum production declines in the female with a less
significant decrease in males, therefore makes some differences in hair physiology at
the elderly age between men and women.
Hair is nonliving material; however it is within a cycle of constant renewal and
shedding. Unlike other organs where limited cellular renewal can occur, hair growth
occurs at the amazing rate of 0.35mm/day [4] allowing the removal of old, damaged
hair that is readily replaced with new regrowth. Hair is the only body structure that is
completely renewable as long as the follicle remains a functioning unit. Hair growth is
in a cyclic basis with absolute accuracy periods, including three common stages below.
The growth period, known as anagen, lasts approximately 1000 days. Hair is only
produced in this stage so the duration of anagen determines the maximum length and
the thickness that the hair can be grown to. It grows more quickly in summer than in
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winter, at night than by day, and women‟s hair grows more quickly than men‟s.
Moreover, there are many factors that also influence the length of the anagen phase,
including genetics, nutrition, age and overall health [4].
The transition period, known as catagen, is the shortest period (approximately 14 days)

and it begins when the melanocytes in the hair bulb stop producing melanin. During
the catagen phase, the hair stops growing and is sheded from the blood supply. At this
stage, the hair strand attach loosely to hair follicle so can be easily shed.
The resting period, known as telogen, lasts only a few weeks. At this stage, a new hair
then begins to grow beneath the telogen follicle, pushing the old telogen fiber out. The
club hair is the final product of a hair follicle in the telogen stage, and is a dead, fully
keratinized hair [1]. When the body is subjected to extreme stress, called telogen
effluvium, as much as 70% of hair can prematurely enter the telogen phase and begin
to fall, causing a noticeable loss of hair.
Physical factors such as severe illness, surgery, weight change, pregnancy, hormonal
alterations, thyroid anomalies, dermatologic disease and emotional factors can be
affected on hair growth. However, physical alterations limited to the hair shaft like
shaving, curling, combing, dyeing is unaffected (from Ref.[2])

Figure 1.2. Head hair growth cycle (Source: Shutterstock Ltd )

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1.1.2. Structure of hair shaft
The following infomation in this section include: (i) the structure of hair shaft (from
Ref.[1] ); (ii) the hair growth cycle (from Ref.[1, 3]) and (iii) several factor influence
on hair phisiology at each stage of both males and females.
The hair shaft, which is form of keratinized cells, containing highly organized material
provide the fiber with remarkable resistannce to enviromental insults [1]. The hair
shaft is composed of three separate regions.

Figure 1.3. Schematic diagram of scalp hair (Source: Shutterstock Ltd)

The cuticle, generally contain 6–8 overlapping cell (scales), is the outermost part of
hair and takes on: (1) protecting hair strand; (2) making an important contribution to
many of the physical properties of the hair and (3) governing its specific surface
properties. This layer is the major objective of hair conditioner, deciding almost tactile
perception. In micro-dimension, it looks like the layout of the shingle on roof. It is
thought that the overlapping of cells in the vicinity of the scale edge is important in
assisting the control of water ingress and egress and hence in maintaining normal fiber
function and durability. The shape and orientation of the cuticle cells are responsible
for the differential friction effect in hair [1]. Because the cuticle layer is made up of
protein-based keratin scales, it can either rise open to receive an ingredient or close to
lock the ingredient within the hair strand by pH and temperature. When these scales
rise, chemicals and ingredients can pass through the cuticle layer to the control center
of the hair strand, the cortex. Once these changes are made to the cortex, they can‟t be
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reversed. Moreover, this state creates the roughness for hair surface and cause to the
tangle. When closed, the cuticle can prevent moisture-loss as well as act as a shield to
protect against damaging environmental forces. This makes the smooth appearance for
hair surface and this state is a part of ideal hair surface.
Discussing about cell-grade structure, each cuticle cell consists of various sub-lamellar
layers. The outer epicuticle consisting of a proteinaceous layer is covered with a thin
film of lipid (fatty acid), predominantly 18-methyleicosanoic acid (18-MEA), by
thioester linkage. This layer constitutes the outer β-layer, also called the F-layer, of the
cuticular cell membrane complex. It play an importance role in governing the surface
properties of hair, both the physical (friction) and the chemical properties (it acts like a
semi-permeable membrane) [1, 5]. The A-layer is underlying and contiguous to the
epicuticle and protecting the hair shaft from chemical, physical, and environmental

insults. A high cystine content of corresponds to rich disulfide linkage and the
presence of iso-peptide bonds result in strongly cross-links which gives this layer
considerable mechanical toughness and chemical resilience. With a dense structure, it
is predicted to high in elastic modulus. From a hair care view, an intact cuticle is
essential to the cosmetic value of the hair, and the goal of hair conditioner is to
enhance and restore order to this layer. Next two layers are less cystine than the Alayer, namely the exocuticle is around 15% and that of endocuticle is 3% [3]. The low
concentration of cystine at endocuticle causes to form a porous structure readily
accessible to water. The cell membrane complex (CMC) is intercellular matter, which
consists of the inner β-layer, the δ-layer, and the outer β-layer. The most important
layer of the CMC is called the beta-layer and it is considered to be the intercellular
cement and it is sandwiched by other layers from each cell. The CMC and the
endocuticle are very vulnerable regions to the chemical treatments. Chemical
treatments, daily mechanical impacts, enviromental factors lead to decrease in the lipid
content of the cell surface changing it from the state of hydrophobicity to a more
hydrophilic, negatively charged surface [5].

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(a) The sub-lamellar structure of the cuticle

(b) Schematic of the outer β-layer.

Figure 1.4. The structure of the cuticle (Source: Ref.[5])
The greatest mass of the hair shaft is the cortex. This layer is located between the hair
cuticle and medulla. It contain closely packed spindle-shaped cells, known as cortical
cell, which are cemented together by the intercellular binding material, known as the
cell membrane complex (CMC). The cortex is the most influence on the mechanical

properties of the hair shaft [5]. The cortical cells are quite varied in shape and size.
They are all spindle shaped, aligned along the main axis of the fibers. It is formed
mainly of macrofibrils separated by thin membranes. In addition to adhesive agent,
CMC also contains melanin pigments which determine the color of hair strand [3].
The medulla is the central of hair fiber, if present, generally makes up only a small
percentage of the mass of the whole hair so the influence on the mechanical properties
of human hair fibers of this layer are negligible [1].
1.1.3. Chemical characteristics
The following information of chemical characteristic of hair were compiled from
Ref.[6] and include: (i) the component of hair and (ii) effects of chemical bonds in hair
shaft on physical, chemical, and physicochemical properties
The major components of hair are proteins. The principal protein component of hair is
cystine-rich keratin. Keratin can be composed of about 18 types of amino acids.
Undergoing chemical treatments, these component converted to the amino acid
derivatives cause to the change in surface properties and physical characteristics.
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The chemical bonds maintain the nature and form of hair. Every cystine unit contains
two cysteine amino acids in different chains which lie near to each other and are linked
together by two sulfur atoms, forming a strong bond known as a disulfide linkage. The
difference in cystine content of various cellular structures of human hair results in a
significant effect on their physical properties. Changing hair into desired shape can
occured by redox process of disulfide bond. The next one is salt linkage formed by a
mutual electrostatic attraction between the positively charged of ammonium ion of the
lysine or arginine residues and the negatively charged of carboxylate ion of the
asparagine acid residues. This type of bonding is responsible for about 35% of the
strength of the keratin fibers and it is broke by acid or alkali solutions. It is strongest at

isoelectric point, approximately 3.7. The peptide bond formed between the -COOH of
the glutamic acid residues and the -NH2 of the lysine residues, contributing a small
influence to the physical properties. Morever, hair is also rich in CO- and NH- groups
present give rise to hydrogen bonds between groups of neighboring chain molecule.
This leads to temporary change in shape, in mechanical impacts when humidity
equibilirium has not yet occurred [6].

Figure 1. 5. Chemical bonds in hair (Source: Ref.[6])

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