Qualitative compositions described on the labels of the capillary straighteners (A1–A4).
\\n\\n
More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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Photonics is a key enabling technology for many market segments and applications. This becomes visible by looking on current trends like [1, 2, 3]:
Augmented and virtual reality for consumer and even more relevant for industrial applications.
Assisting systems in automotive as rear/side view cameras, LED/laser lighting, lidar, night vision support, head-up displays, etc.
Industry 4.0 with connected individual productions and substitution of humans in mechanical and electric production lines by robots requires exact three-dimensional imaging, object recognition, bar code scanning, quality inspection, distance control, and absolute optical measurements.
Continuous development of displays with higher resolutions or trends like “internet of things” needs lithographic production lines with accurate positioning that relies on interferometric measurement and recording devices with precisely imaging objectives.
Enlarged usage of laser technology for cutting, engraving, or welding.
Use of cameras for security and defense applications or in drones.
Three-dimensional printing requires also three-dimensional imaging.
Due to these trends, the overall optics and photonics market will grow significantly above 600 billion USD until 2020 (see Figure 1). Taking their relevance on further products and services into account, its impact is even bigger.
\nDevelopment of the global market size of photonic products (left). The impact on the global economy is due to products and services that rely on photonic products significantly bigger as indicated by the right diagram [4].
All these photonic products have in common that they rely on optical glass. Optical glass is the raw material for the fabrication of spherical lenses, aspheres, prisms, beam splitters, optical fibers, axicons, or other optical components (see Figure 2).
\nFabricated optical components out of raw strips and blocks of optical glass (left) [5]. Profile of a digital single-lens reflex camera (Leica S) showing several components made of optical glass (right) [6].
Optical engineers use components out of various optical glasses to optimize their designs concerning resolution, aberrations, stray light, etc. Such applications take advantage of the essential combination of material features of optical glass like high light transmission, large variety but also precise light deflection (index of refraction and dispersion), high uniformity of light deflection, and sufficient environmental resistance.
\nToday, most of the optical glasses are melted in continuous tank technology. In order to melt optical glass, it is essential to keep the process parameter like composition and temperatures within tight tolerances and further control the optical features like refractive index and Abbe number in adequate loops. Right after the casting, an annealing lehr cools down the glass to avoid cracks due to mechanical stress caused by temperature gradient between inner and outer parts of the glass. This process is called coarse annealing. The composition of the glass defines the first three digits of the refractive index, but even simple optical designs require more precise refraction values. The velocity of the annealing process has an influence on the internal structure of the glass matrix and so on the optical properties. Therefore, an additional fine annealing procedure defines the final optical features. This is necessary because applications like interferometric measurements are sensitive to variations in the sixth digit of the index of refraction. While the melting of the optical glass takes in the order of magnitude of 1 day, the fine annealing procedure could take from several days (small dimensions) up to several months (large dimensions). Cold processing steps like sawing, cutting, grinding, lapping, and polishing convert the fine annealed raw glass into the required optical components to enable the optical functionalities as described above.
\nThis chapter provides a brief overview about the variety of optical glasses and their production procedure including melting, coarse, and fine annealing. Further, the author introduces the definition of the Abbe number. This value describes the dispersion and defines together with the refractive index the optical position. The Abbe diagram depicts the optical position of various optical glasses. This diagram explains the naming conventions of optical glasses. Finally, the measurement techniques in an industrial environment for the main properties of optical glasses are explained.
\nGlass has many unique properties. For each application mentioned in this book, the supplying industry breeds special glass types with adapted features to serve the requirements of their application. The most obvious feature of optical glass for a human eye is the high transparency as indicated in Figure 3. Compared to window glass, the optical path in optical glass is more than 30 times longer for achieving the same transmission, which is a huge difference.
\nComparison of the light transmission through window glass and optical glass [4].
In order to achieve such high grades of transmission, the requirements on the purity of the ingredients, the haze level, the number of bubbles, and the inclusions are significantly stronger than for window glass. Figure 4 shows the internal transmittance over the visible spectrum and the near-infrared regime.
\nSpectral development of the internal transmittance and refractive index of an optical glass (e.g., SCHOTT N-BK7®). (Data taken from [7]).
In contrast to the transmission, the optical position of an optical glass is not obvious for a human eye. Hereby, the refractive index at a specific wavelength and the Abbe number describing the dispersion define the optical position.
\nThe graphic in Figure 4 shows the decrease of the refractive index starting from the ultraviolet over the visible spectrum to the near-infrared regime. Dispersion is the name of this spectral refractive index development. The Abbe number \n
This dispersion is one of the main reasons why we need optical glasses and high sophisticated lens systems for the photonic products at all. If a single lens focuses a blue light ray (e.g., the F-line at 486.1327 nm) and a red light ray (e.g., the C-line at 656.2725 nm), both rays experience different deflections due to the varying refractive index. Therefore, the focus position of both colors differs. If an optical designer combines a flint and a crown glass lens in a proper way, the designer achieves that the focus of the blue and the red ray overlaps. This doublet is an achromatic system. Unfortunately, the focus position of other colors still varies. Therefore, a further chromatic correction and other aberrations require a complex multi-lens design as depicted in Figures 5 and 2 (right) [8]. Such lens system design relies on a broad portfolio of optical glass that spread widely in their optical position.
\nExploded view on a lens system consisting of 10 different lenses made of different optical glass types. This depicts the complexity of such setups [5].
Figure 6 shows a \n
The \n\n\nn\nd\n\n−\n\nν\nd\n\n\n diagram, also called Abbe diagram, displaying the optical position of the various glass types [11].
In earlier days, optical glass manufacturer filled pots with the ingredients of the optical glass composition, melted the raw material, reduced the bubble content by refining processes, mixed the liquid composition, casted the glass, and filled up the pot again [12]. The state-of-the-art method is to melt glass in a continuous process in a tank production. Figure 7 shows a sketch of such a tank. Compared to other glass industries mentioned in this book, the optical glass production is rather tiny. Seldom, the overall volume inside such tank exceeds more than 5 tons.
\nSketch of a melting tank for optical glasses including the spatial temperature profile. The overall time consumption from the raw material melting to the casting takes several hours (with courtesy of SCHOTT).
A glass manufacturer feeds continuously the ingredients into the melting chamber. Gas burners and electrodes heat up and finally melt the ingredients. The picture in Figure 8 shows some still solid raw material on the liquid surface in the melting chamber.
\nView inside the melting chamber with some still solid raw material on the surface of the melted material (with courtesy of SCHOTT).
The melted material contains some bubbles due to residual air inside the raw material and due to chemical reactions between the ingredients. Just driven by convection, the liquefied material flows into the neighboring refining chamber. The increased temperature in the refining chamber leads to growing gas bubbles and so to a larger buoyancy. Additionally, the higher temperature, the reduced viscosity of the melt supports this upthrust, and the gas bubbles vanish. Afterward, the melted material flows into the mixing chamber. A mechanical stirrer homogenizes the melt by rotational motion. The decreased temperature in the mixing chamber and feeder increases the viscosity of the melt in order to enable a proper hot forming during the casting. Typically, glass manufacturer produces an endless strip (width ~160 mm, height ~40 mm); sometimes the glass manufacturer uses molds to produce one block after another (length ~200 mm, width ~200 mm, height ~200 mm). Figure 9 shows the hot forming process of a strip production. The glass is not yet frozen and still glowing red due to black body radiation.
\nHot forming process to produce an endless strip of width 160 mm and height 40 mm. The still liquid glass is glowing due to the black body radiation [13].
As glass has a rather low heat conductivity (~ 1 W/(m × K)), a fast cooling process results in a high value of stress. The outer part is already frozen, but the inner part of a strip is still liquid. So, the volume change during the freezing of the inner part cannot be compensated by the already solid outer part. If this stress exceeds a certain threshold, some cracks or breakage occurs. With increasing thickness of a strip, this risk of damage rises. Therefore, a controlled cooling process is necessary for optical glass. An annealing lehr of several meter lengths after the casting minimizes the risk of damage. At the hot end of the annealing lehr has a similar temperature as the feeder and at the other end a few hundred degrees. Figure 10 shows a view through such an annealing lehr with an endless strip of optical glass inside.
\nView through an annealing lehr of roughly 12 m length that cools down the endless strip slowly to avoid stress and cracks. This procedure takes several hours (with courtesy of SCHOTT).
After the coarse annealing in the lehr, the glass manufacturer breaks or saws the glass strip into manageable length depending on the final application. Actually, the annealing rate has a significant impact on the optical position of the glass. Controlling the chemical composition tightly is mandatory to hit the target values of the refractive index and the Abbe number. The order of magnitude of the accuracy required is 10−4 to 10−6 in the refractive index depending on the application. By keeping the chemical composition constant, the glass manufacturer can control the refractive index within an accuracy of 10−3 to 10−4. The annealing velocity influences the internal glass structure and so the optical features. The fine adjustment of the refractive index takes place in the so-called fine annealing. Therefore, ovens heat up each piece of glass again. At a target temperature around the glass-type specific transformation temperature, the stress inside the glass relaxes. By cooling the glass with a constant rate, the glass manufacturer can control the refractive index with the required precision of 10−4 and 10−6. Figure 11 shows the influence of the annealing rate on the optical position. The red cross in the center of the diagram corresponds to the target value that is mentioned, e.g., in a catalog or a data sheet [5, 9]. The figure also contains the preferred tolerance steps for refractive index and Abbe number from ISO 12123 that specifies raw optical glass (bluish boxes) [14].
\nClose-up of \n\n\nν\nd\n\n\n − \n\n\nn\nd\n\n\n diagram that indicates the required precision and the impact of the annealing rate on the optical position. Data shows SCHOTT N-BK7® based on data taken from [15].
The green square depicts a piece of glass, which was annealed with a cooling rate of 0.4 K/h. Obviously, the optical position is not within the accepted maximum tolerance range (dark blue box). This piece of glass could be annealed again (reversible process) with a higher annealing rate along the annealing line inside the tolerance range [12]. So, the refractive index and Abbe number are fine-tuned by the annealing process. In this example, an annealing with 2 K/h would adapt the optical position to the target value. The printed annealing line is constant for a specific glass type but differs significantly from one glass type to another. Unfortunately, there are boundaries to the annealing rate. Below a glass-type specific annealing rate, the piece of glass tends to crystallize, which would lead to significant haze. Above a certain threshold, which depends on the glass type and the smallest dimension, stress birefringence gets significant. In general, glass is an isotropic media so there is no preferred direction inside the glass system. Nevertheless, if the glass is annealed with a high cooling rate, the inner and the outer parts of a glass blank experience a different temperature gradient (low heat conductivity ~1 W/(m × K)). This leads to mechanical stress. This mechanical stress leads to a preferred direction and so to a refractive index that depends on the polarization orientation of the transmitted light. This effect is called stress-induced birefringence or in short stress birefringence. Besides the mechanical stress, the spatially different temperature rates also influence the regional refractive index (see Figure 11). The homogeneity is the feature that summarizes the result of stress birefringence and regional refractive index variation. An interferometer measures the grade of the homogeneity. Therefore, a plane wave travels through the plane-parallel polished glass blank and overlaps afterward with an undisturbed plane wave. The space-resolved intensity distribution depicts the two-dimensional wave front distortion in false color illustration caused by the glass blank (see, e.g., Figure 12).
\nFalse color illustration of an interferometric wave front distortion of a round LF5 glass blank [16].
The maximum difference of the wave front distortion divided by the blank thickness (peak-to-valley value PV = 0.47 × 10−6) defines the homogeneity grade. The tightest homogeneity tolerance in ISO 12123 is a peak-to-valley value below 10−6, which is roughly four times smaller than the width of the green square in Figure 11. Especially for larger dimensions, this requires a very sophisticated technology of tight controlling of the chemistry and the hot forming process to avoid bubbles, inclusion, or striae. Further, experienced knowledge of the fine annealing procedure to reduce stress birefringence and regional refractive index variation to a minimum is necessary.
\nTypically, a V-block refractometer measures the optical position of the optical glass in order to monitor an accurate production [17]. Figure 13 schematically illustrates the underlying principle.
\nSketch of the principal setup of a V-block refractometer [17].
The glass manufacturer prepares out of the produced and annealed glass a cuboidal sample with dimensions of about 20 × 20 × 5 mm3. This sample fits in a V-shaped glass block with a precisely known refractive index \n
with the refractive index of the surrounding air \n
Even though the manufacture of optical glass is volume wise, the smallest production of all the productions that are mentioned in this book, it has a significant impact on almost all industries. As indicated in the introduction due to a broad variety of market trends, the worth of this key enabling product is still increasing. On the other hand, only a few companies globally still master the rather complex and highly sophisticated production of optical glass that requires a lot of knowledge and experience [20].
\nEven though optical glass is a base material with quite some history, it will remain a relevant key enabler for the entire photonic industry. As the market for photonics is globally rising over almost all market segments, also the demand for optical glass will increase. High sophisticated optical systems require a broad variety of glass types with tight tolerance of the optical position and high transmission. Such tough requirements need an elaborated melting, annealing, and measurement technology.
\nSince the late nineteenth century, optical glass manufacturer develop optical glasses. A comparison of the \n
The various new market trends and segments like augmented or virtual reality, industry 4.0, autonomous driving, robotic and display development, laser material processing, and 3D printing will evolve quickly with slightly adapted requirements. The outlook for the overall optical glass landscape is therefore that the optical glass manufacturer will marginally improve their portfolio with segment-specific variants of their current portfolio concerning optical positions, low density, high transmittance, high chemical resistance, and extreme thermal behavior.
\nThe beauty market, including toiletries, perfumes, and cosmetics, is one of the fastest growing of all market segments. According to data collected by the Brazilian Association of Personal Hygiene, Perfumes and Cosmetics Industry, Brazil is the third largest sales market with a turnover of approximately R $ 29.4 billion in 2011 and the world leader in hair straighteners and conditioners, with 37.3 and 18.8% of the market, respectively [1]. Hair is increasingly exhibited as a form of expression and affirmation of the personality, and therefore, the cosmetics market presents a range of products with the resources to treat and embellish them [2]. The progressive brush is a hair straightening procedure, introduced in the Brazilian beauty salons in recent years, which contains formaldehyde in its composition and promises a lasting smoothing, around 1–4 months, becoming a fever in beauty salons [3].
According to the National Agency of Sanitary Monitoring (ANVISA), the incorporation of formaldehyde into the hair straightener is prohibited, as it can cause serious damages to the user of the product and to the professional that applies it, such as irritation, pain, and burn in the skin, injuries in the airways, and irreversible damage to the eyes and hair [4]. Health legislation permits the use of formaldehyde in cosmetic hair products only as a preservative in a maximum concentration of 0.2% and as a nail hardener at a concentration of up to 5%, in accordance with Resolution 15 of 2013 [5].
In order to guarantee the safety and efficacy of cosmetic products, the cosmetovigilance system was created and implemented in Brazil, through Resolution RDC No. 332, dated December 1, 2005 [6]. This resolution was elaborated from the MERCOSUR resolution to the member countries to implement this system, being delegated to the competent national bodies of each associated country [7].
Cosmetovigilance has the function of monitoring the response that the product will cause in the market, analyzing the adverse events caused by cosmetics, identifying the risk involved in the use of these products, and taking pertinent behaviors according to the established cause relationship [8, 9].
Despite the risks and prohibitions, there is a variety of products sold to beauty salons that contain formaldehyde in its composition. These products are used for the hair straightening process, and there seems to be an ignorance of the legislation by hairdressers, providing the indiscriminate use of this substance for this purpose [10]. Therefore, the chapter proposes to identify and measure formaldehyde in commercial formulations of permanent hair straighteners and progressive, as well as evaluating the organoleptic and physicochemical properties and correlate results from the information provided by manufacturers on the labeling of the products, in accordance with the annexes IV and V of DRC 211/2005.
For the accomplishment of this research, the following reagents were used: formaldehyde PA 37% (Impex), 99% chromotropic acid (disodium dihydrate salt, Sigma-Aldrich), and 98% magnesium sulfate (Sigma-Aldrich), all of analytical grade. Distilled water was used for the preparation of all solutions.
Spectrum spectrophotometer SP 1102; Nova thermostatic shower, model NI 1254; pH meter Hanna, model pH 21; analog rotational viscometer MDJ-1; Centribio centrifuge, model 80-2B; and analytical balance Edutec model FA-2104 N.
For the development of the research, eight samples of permanent and progressive hair straighteners in cosmetic cream from different manufacturers were collected in salons of the municipality of Cuité, PB. The samples were named A1–A8, and their qualitative compositions are described inTables 1 and 2.
Qualitative compositions described on the labels of the capillary straighteners (A1–A4).
Qualitative compositions described on the labels of the capillary straighteners (A5–A8).
The methodology used to identify and quantify the formaldehyde content in progressive brush products was applied according to the standard method recommended by the National Institute of Occupational Safety and Health [11], followed by the modifications described by Gasparini et al. [12].
The stock solution of formaldehyde with of 1000 mg. L−1 was prepared using 2.7 ml of 37% (v/v) formaldehyde solution diluted with distilled water in a 1000 ml volumetric flask. An aqueous solution of chromotropic acid (CA) 5% (w/v) was prepared, dissolving 1.25 g of solute with distilled water in a 25 ml volumetric flask. An aqueous solution of magnesium (MgSO47.H2O) 60% (w/v) was prepared, dissolving 60 g of solute with distilled water in a volumetric flask 100 ml.
The identification of formaldehyde in the solutions was done through the reaction that occurs between the chromotropic acid and formaldehyde in the presence of magnesium after heating, thus producing a colored compound, indicating the presence of formaldehyde in a solution. For the determination of the analytical curve of formaldehyde, the following test was performed: 90, 120, 150, 180, 210, 220, and 230 μl of stock solution containing formaldehyde were transferred to test tubes. In Then, 290 μl of solution of 5% (w/v) chromotropic acid and 3.0 ml of solution of 60% (w/v) magnesium sulfate, with stirring. The tubes were heated for 60 minutes in a steam (100°C), followed by cooling to 25°C. The solutions were transferred to 25 ml flasks and the volume filled with distilled water, obtaining the concentrations of formaldehyde (ppm): 3.6, 4.8, 6.0, 7.2, 8.4, 8.8, and 9.2, respectively. The measurements of absorbance were recorded at 535 nm. All reviews were carried out in triplicate, in order to guarantee the accuracy of the results obtained.
For each commercial sample, 3.0 g was weighed and then dissolved in about 20 ml of distilled water, and the final volume was completed to 100 ml, yielding a solution with concentration (C1) of 30,000 μg ml−1. After 5.0 ml of this solution (C1) were diluted in 25 ml of distilled water (C2 = 6000 μg ml−1). Aliquots of 1.0 ml of the solutions (C2) were transferred to test tubes together with 290 μl of chromotropic acid 5% (w/v) and 3.00 ml of magnesium sulfate 60% (w/v). The tubes were heated for 60 minutes in a steam bath (100°C), followed by cooling to 25°C. The solutions were transferred to 25 ml volumetric flasks, and then the volume was filled with distilled water resulting in a concentration (C3) of 240 μg ml−1. The measurements of absorbance were performed at 535 nm.
The organoleptic and physicochemical tests were performed to assess the characteristics of the products in study. The organoleptic and physicochemical characteristics evaluated were odor, color, appearance, pH, viscosity, density, and centrifugation [13], which were correlated between samples.
For the determination of the pH, the potentiometric method was used. The samples were diluted to 10% (w/v) in distilled water, at room temperature, in triplicate [13, 14, 15].
The viscosity was measured in triplicate in an analog rotary viscometer using 40 g of sample, spindle 4 and speed of 6 rpm. Next, the rotor was inserted vertically into the sample free of blister up to the groove of the rotor rod, and the apparatus was leveled, by reading the viscosity according to the operating procedure of the device [13].
The density was determined by pycnometry. Initially the empty pycnometer (M0) was weighed, first, with distilled water (M1) and, finally, (clean and dry) with the sample (M2). The masses were noted for calculation using the following formula [13]:
where d is the sample density in g/cm3; M0 is the mass of the empty pycnometer, in grams; M1 is the mass of the pycnometer with distilled water, in grams; and M2 is the mass of the pycnometer with the sample, in grams.
From each sample, 5 g was placed in centrifugal tubes and submitted to cycles of 1000 and 2500 rpm for 15 minutes each. The homogeneity of the study formulations was evaluated by observing macroscopic separation of phases after performing the described procedure [13, 14, 16].
A qualitative analysis of the primary and secondary packaging of the tested products by a critical visual investigation was carried out, following the criteria laid down by national legislation—RDC 211/2005 which defines the labeling rules for cosmetic products [17] and RDC 332/2005 which deals with regulation and implementation of cosmetology in the cosmetic industries [6]. The analyzed items were specified according to Figure 1.
Mandatory items on labeling of capillaries straighteners according to Annexes IV and V of DRC 211/2005.
The identification of formaldehyde was evidenced by the production of a pink compound resulting from the reaction between chromotropic acid and formaldehyde in the presence of magnesium sulfate. The analytical curve data, resulting from the average of three calibration curves, were adjusted by linear regression (Figure 2), whose equation of the line is given by absorbance = 0.0922 × [formaldehyde solution, chromotropic acid, and magnesium sulfate] (ppm) − 0.0234. The correlation coefficient obtained was 0.996, a significant linear regression. Samples A1, A3, A5, and A8 developed a coloration after heating, indicating the presence of formaldehyde in these formulations, which tends to be as darker as greater the concentration of said substance. The samples A3 and A8, on the other hand, presented more intense in relation to others, which justifies a higher concentration of formaldehyde. The percentages of formaldehyde calculated by the equation from the analytical curve confirm these results and are described in Table 3.
Graphical representation of the formaldehyde analytical curve using chromotropic acid (AC) and sulfate of magnesium (MgSO4) at 535 nm where Y = 0.0922, x = 0.0234, and R = 0.996.
Absorbances, concentrations of formaldehyde in diluted samples (ppm) and percentages of formaldehyde in the formulations A1–A8.
The results obtained in organoleptic and physicochemical tests of the study samples are listed in Table 4. Regarding appearance and color, observed macroscopically, the samples presented as homogeneous creams, whether or not colored and without precipitation or exudation. The odor was checked directly through the smell, being possible to smell characteristic of formaldehyde in samples A1, A3, A5, and A8, capable of causing some mucosal irritation and burning in the eyes during observation, confirming symptoms caused by exposure to formaldehyde. The sample A5, although with a strong chocolate odor, failed to mask the presence of formaldehyde in the product. Samples A6 and A7 showed an odor of sulfur, a characteristic of thioglycolic acid. The samples A2 and A4 presented no strong or unpleasant smell, only the essence odor used in these products.
Organoleptic and physico-chemical characteristics of the formulations under study.
Samples A2 and A4 showed a pH of very acid (1.0 and 1.3, respectively), which may damage the capillary wires [18]. In the other hand, the sample A8 has a pH within the range that tends to assist in the maintenance of wires. The samples A1, A3, and A5 also have a pH slightly acidic, being able to close the capillary cuticle and help in preserving the color deposited in the hair. The samples A6 and A7 presented extremely high pH, a characteristic of products for permanent straightening.
The analyzed samples did not present significant variation in relation to the determination of the density and did not need to correct the weighing to carry out the dosing of the formaldehyde.
The formulations showed without phase separation, precipitation, formation of caking, and coalescence, except the A2 sample that presented phase separation after being subjected to the centrifugation.
The viscosity results can be in Figure 3. These results point to discrepant values between formulations, ranging from extremely low (A2) to extremely high (A6 and A7).
Average values of the viscosity (cP) of the samples A1–A8 at 25°C.
The results of the analysis of the product labels are presented in Table 5. Samples A1, A3, A5, and A8 presented formaldehyde content in the procedure spectrophotometric assay; however, only samples A1 and A8 indicated formaldehyde in their composition. Samples A3 and A5, in addition to the absence of the substance, presented other irregularities on the label, both ignoring the warning information and usage restrictions. Sample A5 does not yet have registration number granted by ANVISA, evidencing the likely clandestine origin of this product.
Analysis of the labels of the products under study according to Annexes IV and V to DRC 211/2005.
The samples A2, A4, A6, and A7, whose labels said formaldehyde-free, are not really content of the substance, being in compliance and complying with the technical requirement legislations.
According to the NIOSH 3500 [11] reference method, formaldehyde is determined by spectrophotometry through reaction with chromotropic acid in the presence of concentrated sulfuric acid, after heating, to obtain a soluble polymer violet-red that can be detected in length of wavelength of 580 nm. However, although the method is selective, not suffering interference from other aldehydes, it has some drawbacks. The main one is the use of concentrated sulfuric acid by the toxicity and corrosivity that it presents. Therefore, some authors have proposed modification methodology that could minimize these disadvantages [12, 19, 20, 21, 22, 23].
According to Toutianoush et al. [22], it is possible to dose the formaldehyde by spectrophotometry in the presence of a solution of magnesium sulfate (MgSO4∙7H2O) instead of sulfuric acid. A red/pink is produced after heating of formaldehyde with an excess of chromotropic acid in a steam bath. In the absence of magnesium sulfate, this reaction does not occur. It is likely that the oxygen atoms of the cyclotetrachromotropylene-hydroxyl are pre-arranged for complexation with magnesium. Gasparini et al. [12] used this method to dose formaldehyde disinfectants and hair care products, considering the adequate method, low operating cost, and simplicity and selectivity, meeting the requirements of green analytical chemistry.
Thus, the applicability of the proposed method to determination of formaldehyde in straightening hair products of different brands proved to be appropriate, possible to identify the presence of formaldehyde in samples A1, A3, A5, and A8 in concentrations ranging from between 1.5 and 3.83% (w/v), i.e., concentrations 7.5; 16.45; 7.9 and 19.15 times that allowed by ANVISA [5].
Some authors also dosed formaldehyde in commercial formulations of hair straighteners using methods such as HPLC, gas chromatography, and mass spectrometry, finding concentrations of 1.6–11.5%, similar results to that of this research, with concentrations above that accepted, evidencing the use of formaldehyde as a hair straightener and not just as a preservative at the maximum concentration of 0.2%, as recommended by health legislation. This shows the lack of supervision by regulatory institutions and the deep lack of knowledge or lack of concern for part of consumers and professional hairdressers in face of the risks that these products bring to health [24, 25].
In addition to the assay, it is also important to analyze the organoleptic and physicochemical characteristics of a cosmetic formulation, because usually the texture, odor, color, and appearance of the product are examined before your purchase; these being important parameters from the commercial point of view, consumers may or may not be attracted to these characteristics. The sample A5 presents a dark-brown tone and chocolate essence; these characteristics tend to seduce the consumer. The color of a product, however, has no connection with the presence or absence of formaldehyde, differently from the intense odor, which may be indicative, since even using extremely high essences fragrant, it is still possible to smell it.
The pH of the hair strands ranges from 4.5 to 5.5. Capillary formulations with extreme pH variations can damage the capillary wire, because the hair shrinks and stiffens or even dissolves completely at very high pH acid or increases porosity as the layers of cuticle dilate, resulting in a dry appearance, opaque, reaching to complete hair dissolution in strongly alkaline pH. The pH values of samples A1, A3, A5, and A8 were compatible with the hair samples, while samples A2, A4, A6, and A7 had a pH out of the tolerated range, the integrity of the capillary wire [18]. In this way, products for professional use should be used with caution and applied by trained professionals.
Viscosity is a measure of resistance of a flow system when submitted to a mechanical stress. Therefore, the higher the viscosity, the higher the resistance and the force to be applied to flow with a certain velocity [26]. In the case of the products tested, there was a considerable variation of this parameter, of samples having viscosities less than 4000 cP to samples with viscosities above of 12,000 cP, thus presenting flow profile applicability. The viscosity results can also inform the influence of the sedimentation rate of the droplets present in the cosmetic cream form, complementing the result of the centrifugation.
The centrifugation test provides quick information about phase separation, thus predicting whether the product will separate as a function of time [13], which can lead to significant differences in the content of assets. In the present study, only the A2 sample presented separation of post-centrifugation phases, which can be influenced by the low viscosity of the sample (566 ± 57.7 cP). According to Stokes’s law, the speed of sedimentation is inversely proportional to viscosity and directly proportional to the size of the droplets, the gravity, and the density difference between the dispersed medium and dispersant [27].
The evaluation of product quality parameters for progressive brush becomes essential, once beauty salons are frequently visited by sales promoters that offer products that are capable of providing a “true miracle” in straightening the hair without formaldehyde in its composition. However, they may have a high concentration, masked by an extremely fragrant and unidentified formula of its presence on the label [28], which could be proven in the present study, where 50% of the products for hair straightening analyzed were disapproved due to the presence of formaldehyde out of the concentration allowed, as well as irregularities in the labels.
The chapter is important to the cosmetovigilance system to ensure the final quality of cosmetic products, taking into safety, efficacy, and information to ANVISA, to the manufacturer, and to the consumer. In this way, this system may provide numerous benefits to the cosmetics industry as a whole. As measures, it would be important to distribute orientation books and flyers of cosmetic products since the vigilance is not only the responsibility of companies but also of the consumers and competent institutions.
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