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Received: 22 November 2020 Revised: 17 March 2021 Accepted: 6 April 2021

DOI: 10.1002/col.22671

RESEARCH ARTICLE

Assessment of the factors affecting the weathering


properties of Pigment Yellow 74 in decorative paint

Pramod Nikam | Chandrashekara R. Haramagatti | Amit Joshi

Research & Technology Centre, Asian


Paints Limited, Navi Mumbai, India
Abstract
Color or shade fading is one of the major issues observed in decorative paints.
Correspondence
Here we have carried out a systematic artificial weathering study using QUV
Chandrashekara R. Haramagatti,
Research & Technology Centre, Asian and ATLAS weathering test chambers for Pigment Yellow 74 (PY 74). Pigment
Paints Limited, Plot No. C3-B/1, TTC dispersion of PY 74 received from three different manufacturers are prepared.
MIDC, Pawane, Thane–Belapur Road,
Various factors, such as the processing parameter, for example, grinding tem-
Navi Mumbai 400703, Maharashtra, India.
Email: chandrashekara.haramagatti@ perature (with and without cooling water circulation during the processing of
asianpaints.com pigment dispersion), with respect to paints the factors such as primers and
clear base paints of different batches, and as for the ATLAS and QUV weather-
ability test concerned, test panels of different lots, and multiple QUV chambers
are evaluated. The color difference was recorded at regular time intervals for
the panels exposed to ATLAS and QUV test of 1000 hours using color spectro-
photometer. A significant color difference was recorded for the panels coated
with paints based on pigment dispersion prepared using PY 74 from different
manufacturers, and the difference in grinding temperature. These results show
the importance of process parameters such as grinding temperature on
weathering properties, and systematic testing approaches for QUV/ATLAS for
the pigments from different manufacturers.

KEYWORDS
artificial weathering, color fading, organic pigments, pigment dispersion

1 | INTRODUCTION surface preparation, wrong painting practices, and envi-


ronmental conditions.1,2 Color/shade fading is a most
Paint is used to decorate and enhance the aesthetic of the commonly observed defect in the exterior decorative
walls/house, metals, wood etc., not only that it protects paints, since the shade fading in the interior paint appears
the surface from various unfavorable elements. Therefore, over time and may not be as distinct as fading in exterior
protection of the surface from the environmental condi- paints. Variation in environmental conditions, such as
tions and increasing the life of the surface is mainly temperature, presence of salts, and moisture present in the
achieved from paints and coatings.1 However, the perfor- air makes surrounding environment more conducive and
mance of these paints and coatings under various environ- it speeds up the shade fading of exterior paints.3 Apart
mental parameters is a concern. Fading, blistering, from these factors, poor performance of paint might also
peeling, grinning, chalking, running, sagging, flaking, be due to the quality of raw material used in the paints.
blooming, wrinkling, flashing, saponification, alligatoring, The composition of paints plays a major role in withstand-
checking, cracking, pin holing, and mottling are some of ing the harsh environmental conditions. Binder and pig-
the paint defects observed due to faulty design, improper ments are the two such crucial ingredients. The main

Color Res Appl. 2021;46:1313–1320. wileyonlinelibrary.com/journal/col © 2021 Wiley Periodicals LLC. 1313
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1314 NIKAM ET AL.

function of binders is to hold the pigments, extenders etc. added and mixed at low speed of 500 rpm for
intact with the surface.4 Pigments provide color and optical 10 minutes on the dispermat. The powder ingredients
properties (opacity, reflectance) to the paint film.5 The pig- pigment, extender followed by rheology additive were
ments are also more susceptible to the heat. Exposure of the added, the mixture was mixed well for 10 minutes at
pigment to the heat results into the change in the crystal 800 rpm. Grinding was performed for 30 minutes at
structure which then leads to the fading of shade.6 Gener- 3000 rpm. The chilling (by circulation of cool water)
ally, the pigment or pigment particle surface is modified was provided during grinding stage to maintain tempera-
with functional moieties to enhance the performance prop- ture of mixer between 8 C to 25 C.
erties of the pigments.7 Inorganic pigments have low
chroma and tinting strength but they have good hiding
power, excellent lightfastness, and chemical resistance, 2.3 | QUV/ATLAS panel preparation and
whereas organic pigments have bright color, and the paint application
weather fastness is inferior compared to the inorganic
pigments.8,9 Among the various chemistries of organic The preparation of the primer for panel application
pigments, monoazo yellow pigments possess inferior started with 100 mL of water-based primer (acrylic emul-
weather fastness and chemical resistance.10,11 However, sion based, pigment volume concentration [PVC] 70%,
there were efforts to improve the storage stability, and parti- and coverage 30-33 m2/L) in a 200 mL metal container.
cle size stability of Pigment Yellow 74 (PY 74) by controlling This was diluted at 1:1 with water, and was mixed well
the crystal structure parameters.12 Besides that, the other using gyro shaker for 5 minutes.
parameters such as deviations in the quality of pigments For the prepation of the exterior paint for panel appli-
among the different manufacturers, surface preparation, cation, 100 mL of acrylic emulsion exterior paint (PVC
etc. will also lead to fading of the color. Generally artificial 40%, and coverage 16-18 m2/L) and 10 mL of pre-
weathering (UV chambers from Q-Labs [QUV], and pared PY 74 colorant were placed in a 200 mL metal con-
weather-O-meter from ATLAS) tests are performed to these tainer; then mixed well using gyro shaker for 5 minutes.
pigment dispersions to understand their performances. This paint was diluted at 1:0.4 with water and mixed well
Here in this article, pigment dispersion of monoazo for 3 minutes with a spatula.
yellow pigment (PY 74) was prepared using PY 74 from Fiber cement panels of dimension 150 mm × 75 mm
different manufacturers. The effect of various factors for QUV, and 145 mm × 65 mm for ATLAS were used in
such as temperature during dispersion process, alkalinity the study. The fiber cement panels were cleaned thor-
of the QUV and ATLAS panels, and surface preparation oughly under running tap to clean the dirt from the sur-
of QUV and ATLAS test panels on the fading of the color- face. These panels were then allowed to dry overnight at
ants is studied. room temperature. A single coat of primer was applied
by brush on these panels, and allowed to dry for 4 hours
at room temperature. This was followed by two coats
2 | EXPERIME N TAL METH OD (applied by brush) of acrylic emulsion exterior paint with
an interval of 8 hours between two coats. Then panels
2.1 | Materials were allowed to cure at room temperature for 7 days
before subjecting them to the ATLAS and QUV
The PY 74 from three different manufacturers, calcium chambers.
carbonate as extender, attapulgite as thickener,
ethoxylate of fatty oil ester, fatty acid modified emulsifier,
and soya lecithin as wetting and dispersing agents, bio- 2.4 | Characterization
cides, defoamer as additives, and DM water are used in
the study. All the raw materials are of commercial grade Infrared (IR) spectroscopy: Infrared spectra are recorded
and used as received; manufacturers details are not given using IR spectrometer from PerkinElmer. The samples
to avoid product promotion. for IR spectroscopy were prepared by grinding pigment
and KBr using mortar and pestle, and then made pellet
by using pellet die.
2.2 | Pigment dispersion Particle size: Mastersizer 2000 from Malvern instru-
ment, which operates on static light scattering principle,
Pigment dispersions were prepared in 1 L stainless steel- was used to record the particle size distribution. The sample
jacketed vessel using high speed disperser (Dispermat- was prepared by dispersing 0.5 g of pigment in 10 mL of 1%
VMA-Getzmann, Germany). Liquid ingredients were sodium lauryl sulphate solution by sonication for 1 minute.
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NIKAM ET AL. 1315

Scanning electron microscopy: Field-emission scan- scanning electron microscopy and energy dispersive X-
ning electron microscopy and energy-dispersive X-ray ray analysis. IR spectra for these three different manu-
(FESEM and EDX) analysis of the PY 74 pigment from facturers are shown in Figure 1 (IR spectra are split in
different manufacturers were carried out using Jeol to two regions for better clarity). There is no signifi-
7100F. The dispersion was prepared by sonicating the cant difference in IR spectral features except spectral
pigment in water at 33 kHz for 5 minutes using a features near 1650 cm−1 which are the characteristics
sonicator from Telsonic Ultrasonics, and then a drop of of olefinic group observed.
the dispersion was placed on double-sided tape pasted on Particle size distributions for pigments received from
stub, and was allowed to dry. Platinum sputter coating three different manufacturers are shown in Figure 2. Par-
for 30 seconds at 20 mA was given to the samples. ticle size distribution near 200 nm is quite similar among
Spectrophotometer (Gretag Macbeth Color-Eye these three pigments. However, the difference in particle
7000A and software Propallete 3.3) was used to record size distribution can be observed between 1 and 90 μm.
the color differences of the panels. QUV-accelerated The morphology and elemental analysis were per-
weathering test machine from Q-Lab USA (Operational formed for the PY74 pigments. Scanning electron micro-
conditions—Condensation at 45 C, and UV at 50 C, scopic images and EDX spectrum are shown in Figure 3.
Irradiance—0.55 watts/m2/nm, UV radiation source— SEM image of PS2 shows that, the particles are uniform
UVB 313 EL), and ATLAS chamber (operational in shape, and EDX analysis shows only carbon and oxy-
conditions—6500 W water cooled Xenon Arc burner, gen elements arising from pigment particles. Whereas
humidity of 60%-80%, black panel temperature of 63 C,
irradiance of 0.5 watts/m2/nm, 100 minutes of dry
cycle with continuous radiation followed by 15 minutes
of water spray under the continuous radiation)
were used.
The panels were taken out at regular intervals for
recording the color difference using spectrophotometer,
the water droplets on the panels were wiped out gently
using tissue paper, and the panels were allowed to cool
down to room temperature before recording the color dif-
ference. The coloristic values were recorded and stored in
the spectrophotometer.

3 | R ES U L T S A N D D I S C U S S I O N

Pigment received from three different manufacturers


(PS1, PS2, and PS3) are characterized for the func-
tional groups using infrared spectroscopy, particle size F I G U R E 2 Particle size distribution of Pigment Yellow (PY 74)
analysis by static light scattering technique, and pigment received from three different manufacturers

F I G U R E 1 Infrared spectra
of Pigment Yellow (PY 74)
pigment from three different
manufacturers PS1, PS2, and
PS3 at figure print to bending
vibrations (A), and stretching
vibrations (B)
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1316 NIKAM ET AL.

F I G U R E 3 Scanning electron microscopy and energy-dispersive X-ray (EDX) analysis of PS1, PS2, and PS3. EDX spectra are given for
2 difference spots for PS1 and PS2 to differentiate the pigment and plate-like structures. No plate-like structures found for PS2

SEM images of PS1 and PS3 shows plate-like structures oxygen arising from pigment particles, and the plate-like
in addition to regular uniform particles. EDX analysis of structures contained mostly aluminum, and silicon might
regular uniform particles are mostly of carbon and be from extender/additives. The main difference between
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NIKAM ET AL. 1317

qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
PS1 and PS3 is that, the size and abundance of plate-like
ΔE ab = ðL2 −L1Þ2 + ða2 −a1Þ2 + ðb2 −b1Þ2 ð1Þ
structures in PS3 is much higher than in PS1.
Pigments from different manufacturers PS1, PS2, and
PS3 were used to prepare pigment dispersions using the sim- where ΔE*ab is the color difference, L (Lightness), a (red-
ilar formulation. Initial colorimetric values L, a, b, and the ness/greenness), and b (yellowness/blueness) are stan-
ΔE*ab (the color difference of reference and experimental dard CIE coordinates. Throughout this article ΔE refers
QUV panels, here in this case, the initial readings of QUV to the CIELAB color difference, which is given by Equa-
panels before placing them in the ATLAS and QUV cham- tion (1).
bers are taken as the reference) of panels were recorded Experiments were conducted to rule out the variation
using spectrophotometer according to the Equation (1).13 in QUV chambers or malfunctioning and set parameters.
These initial readings are stored in the computer and used Pigment dispersion from pigment PS3 was used in the
in subsequent measurements to find the color difference of panel preparation and then the panels were exposed in
the panels exposed to QUV. The panels were prepared and four separate QUV chambers. As shown in Figure 4, no
exposed in duplicate, and the given results are the average of significant difference in ΔE was observed as a function of
two different panels with an experimental deviation <5%. exposure time of 1000 hours.
The QUV-exposed panels were taken out at the time interval The influence of primers and the base paint (clear
of 100, 250, 500, 750, 850, 1000 hours, and the coloristic of base/zero TiO2 base) of different batches on the color dif-
these panels were recorded. ference during the ATLAS and QUV exposure was stud-
ied. Primers of different batches were used while
preparing the panels keeping the pigment dispersion
from PS 3, clear base 1 the same. The influence of the
primer of different batch on the color difference even
after 1000 hours of ATLAS and QUV exposure is very
minimal as shown in Figure 5. Then the panels were pre-
pared with the paints of two different clear bases keeping
the pigment dispersion from PS 3, primer 1 same. Varia-
tion in color difference during the weatherability test for
these panels is shown in Figure 6. There is a slight differ-
ence in ΔE observed as shown in Figure 6B. However,
the difference is less than 1 unit and visually also there
was not much difference found. Since there was no sig-
nificant difference in different lots of primers and clear
bases, no change in color difference/fading was observed.
Since the panels are made up of cement reinforced
with cellulose fibers, the quality of panels may contribute
to the variation in the color difference. The panels of two
different lots were immersed overnight in DM water of
F I G U R E 4 The performance of different QUV chambers for pH 6.8. The panels were removed from the water, and
variation in color difference of pigment dispersion the pH of water was recorded. The pH of water where

FIGURE 5 Influence of primers of different batches on variation in color difference


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1318 NIKAM ET AL.

F I G U R E 6 Influence of base paint of different batches on F I G U R E 8 Variation of color difference (ΔE) of PY74 from
variation in color difference different manufacturers as a function of exposure time

The color fading in case of PS 3 is observed to be less


compared to the PS 1 and PS 2 indicating the better
weather fastness. The color difference ΔE of 5.5 to 7
was observed between PS3 and PS1/PS2 which is signifi-
cantly high, and the color difference can even be seen
visually as shown in Figure 9. Both ATLAS (Figure 9A)
and QUV (Figure 9B) exposed panels of pigment manu-
facturer 3 showed better retention of coloristics com-
pared to the other two manufacturers. The difference in
F I G U R E 7 Influence of panels of different lots on variation in ΔE observed might be due to the difference in surface
color difference treatment given to the pigments by manufacturer, or the
difference in the crystal structures obtained by different
manufacturers.14 However, the IR analysis of these three
panel of lot 1 was dipped shown pH 9.2, while panel of pigments did not show any significant difference in spec-
lot 2 showed pH 10.4 indicating the panel of lot 2 is more tral features.
alkaline than panel of lot 1. These two lot panels were Since the pigment stability depends on the processing
coated with primer 1, paint of clear base 1, and the pig- temperature, the pigment dispersion was prepared with
ment dispersion PS3. However, no significant color differ- and without providing the cooling water during the dis-
ence was observed after the ATLAS and QUV exposure persion preparation. For the dispersion prepared with
as shown in Figure 7. The panels of both the lots are cooling water circulation, the temperature during grind-
alkaline, and the pH difference between them was 1.2, ing was 8 C to 20 C. In case of the dispersions without
have not resulted in any significant difference in color cooling water circulation, the temperature during grind-
fading. ing was 48 C to 50 C. The color difference of the panels
Since there was no contribution of change in QUV prepared without cooling facility showed significantly
chambers, primers, clear base and ATLAS, and QUV greater ΔE (2.5-3) in ATLAS and QUV test at
panels on ΔE observed, the focus was given to pigment of 1000 hours of exposure compared to the panels of disper-
different manufacturers, and then the processing temper- sions prepared with cooling facility as shown in
ature of pigment dispersion. Figure 10. Color fading can also be seen visually as
The major contributor to the deviation to color differ- shown in Figure 11 for both ATLAS and QUV exposed
ence would be the pigment itself. Variation in the color panels where panels of dispersion prepared with cooling
difference of ATLAS and QUV exposed panels of differ- facility showed better color retention after 1000 h of
ent manufacturers is shown in Figure 8. Pigment from exposures. The dispersions processed at high temperature
all the three manufacturers showed quite similar ΔE (without cooling water circulation) might have lost their
value up to 150 hours of exposure. As the panels exposed stability/crystal structure and hence the inferior ATLAS
for longer duration, the color difference among PS 1 and and QUV performance. It is known that certain organic
PS 2 remains similar, whereas PS3 showed significantly pigments are sensitive to high temperature and impact
lower ΔE. The slope in increase of ΔE decreases after during grinding results in inferior color strength.15 The
500 hours of exposure for PS 3. Among the 3 manufac- trend of the data shown in Figure 10 is quite similar to
turers, PS 1 and PS 2 showed significantly greater color the trend of Figure 8 in terms of increase in difference of
difference when compared to the pigment from PS 3. ΔE as a function of ATLAS and QUV exposure time.
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NIKAM ET AL. 1319

F I G U R E 9 Images of the ATLAS and QUV panels coated with paint based on pigment dispersion prepared using three different
pigment manufacturers

F I G U R E 1 0 Effect of with cooling and without cooling water F I G U R E 1 2 Difference in color (ΔE) observed for panels of all
circulation during the grinding process on variation in color better and poor factors studied
difference at ATLAS and QUV exposures
reason for PS3 to show superior weather fastness might be
due to the presence of large and high amount of plate-like
particles contained aluminum and silicon as characterized
by SEM and EDX which are shown in Figure 3.
The above observations were tested by combining the
set of better and set of poor performance parameters
studied individually. Set of best factors includes pigment
manufacturer (PS 3), with cooling water circulation dur-
ing the pigment dispersion, along with clear base paint
(Base 1), primer 1, panel lot 1, and set of poor factors
include pigment manufacturer (PS 1), no cooling water
circulation during the pigment dispersion, along with
F I G U R E 1 1 Images of the ATLAS and QUV exposed panels of
clear base paint 1, primer 1 and panel lot 1. Though some
pigment dispersion prepared with and without cooling water
circulation
of the parameters such as clear base, primer, and
ATLAS/QUV panels did not show difference in ΔE when
studied individually, however, when combined these
The major contributors for the difference in ATLAS with pigment of different manufacturer, and the higher
and QUV performance or the color fading are found to be dispersion processing temperature resulted the difference
the quality of pigments sourced from different manufac- in the ΔE as shown in Figure 12.
turers that may arise due to difference in surface treat-
ment, crystal structures, morphology of the particles, and
the temperature during processing of the dispersion. How- 4 | CONCLUSION
ever, IR spectral features and particle size distribution data
did not show any correlation with color difference This article reveals various factors governing the color/
observed. The oil absorption (43-48 g/100 g) and bulk den- shade fading of dispersion of PY 74. The PY 74 pigment
sity (0.24-0.31 g/cm3) of PY74 from three different manu- from different manufacturers was used to prepare the dis-
facturers are not significantly different. The probable persions and the paint was subjected to ATLAS and QUV
15206378, 2021, 6, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/col.22671 by Egyptian National Sti. Network (Enstinet), Wiley Online Library on [05/02/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1320 NIKAM ET AL.

weathering test to analyze various factors on color or [12] Hoshino, R, Nagasato, S, Takayama, M, Inoue, S,
shade fading. Among the factors studied, PY 74 from pig- Matsuzaki, S, CI Pigment Yellow 74 (Insoluble Azo Pigment),
ment manufacturers 1 and 2, and/or the higher tempera- and Coloring Composition Using Same. US Patent
20140335358A1, 2014.
ture during the grinding resulted higher color difference.
[13] CIElab, Colorimetry, CIE Pub. No. 15.2 Commission Inter-
ATLAS and QUV panels applied with paint based on Pig- nationale de l'Eclairage, Austria 1986 ISBN:3-900-734-00-3
ment manufacturer 3, and/or the cooling water circulation [14] Lomax SQ. The application of x-ray powder diffraction for the
during pigment dispersion resulted better color retention analysis of synthetic organic pigments. Part 1: dry pigments.
and hence a significantly lower ΔE. There was no contri- J Coat Technol Res. 2010;7:331-346.
bution of primers, and base paint of different batches, [15] Herbst W. Dispersion of organic pigments with modern disper-
ATLAS/QUV panels of different lots, and various QUV sion equipment. Pigm Resin Technol. 1974;3:12-25.
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in identifying the effect of grinding temperature, and also
AUTHOR BIOGRAPHIES
the approaches for pigment testing for weatherability.

A C K N O WL E D G M E N T S Pramod Nikam completed an MS in analytical


The authors thank the Asian Paints Ltd. for the support chemistry in 2010 at Institute of Science, Mumbai,
to publish the research work. We also thank the modern India. For the past 11 years, he has been working at
instrumentation laboratory for analytical tests. Research & Technology Centre of Asian Paints Ltd. in
the area of quality analysis, and formulation of pig-
ORCID ment concentrates.
Chandrashekara R. Haramagatti https://orcid.org/ Chandrashekara R. Haramagatti has received an
0000-0002-1108-1606 MS in industrial chemistry from Kuvempu University,
Karnataka. India, in 2000. He did research at IISc
R EF E RE N C E S Bangalore from 2000 to 2002 before he moved to
[1] Malshe, VC, Sikchi, MA, Basics of Paint Technology, Part 1, Goettingen, Germany to work on a doctorate. In 2006
India. Mumbai, India: Basics of Paint Technology part I - V. C. received a PhD in chemistry from University of
Malshe - Google Books; 2004. Goettingen. Then moved to University of Bayreuth,
[2] Schoff CK. Surface defects: diagnosis and cure. J Coat Tech.
Germany for a postdoctoral position from 2008 to
1999;71:56-73.
2010. For the last 10 years, he has been working on
[3] Burakowski T, Wierzchon T. Surface Engineering of Metals:
Principles, Equipment, Technologies. CRC Press: USA; 1999: emulsion polymers, pigment dispersions, synthesis of
211-214. resin for paints and coatings at Research & Technol-
[4] Freitag W, Stoye D. Paints, Coatings and Solvents. 2nd ed. Ger- ogy Centre of Asian Paints Ltd.
many: Wiley-VCH verlag GmbH; 1998:1-8.
[5] Gürses A, Açıkyıldız M, Güneş K, Gürses MS. Classification of
Amit Joshi has received an MS in chemistry from
dye and pigments. MS Dyes and Pigments. Switzerland: Mumbai University in 1999 and a PhD from the Insti-
Springer; 2016:31-35. tute of Chemical Technology, Mumbai in 2005. He
[6] Berrie BH, Strumfels Y. Change is permanent; thoughts on the received a fellowship from Gretag Macbeth, United
fading of cochineal-based watercolor pigments. Heritage Sci. States for his doctoral work on coloration and color
2017;5(30):1-9. measurement of plastic and paint systems. For the
[7] Schweikart, KH, Blum, D, Grimm, FW, Schmidt, MU, Geisenberger,
past 15 years, he has been working with Asian Paints
J, Use of Pigment Composition Comprising Mixed Crystals Based on
research team mainly in the area of formulation of
CI Pigment Yellow 74. US Patent 7416596B2, 2008.
[8] Kazuyuki, H, Keisuke, I, Mineko, O, Yusuke S, Hiroko, M, pigment concentrates and color matching.
Organic and Inorganic Composite Pigments, and Paint and
Resin Composition Using the Same. European Patent
1270686A2, 2003.
[9] Baptista J. Four Steps to Effective Pigment Dispersions. New Jer- How to cite this article: Nikam P,
sey, USA: Coatings World; 2017. Haramagatti CR, Joshi A. Assessment of the factors
[10] Hays, BG, Strong Green-Shade Yellow Disazo Pigment, US
affecting the weathering properties of Pigment
Patent 5889162A, 1999
Yellow 74 in decorative paint. Color Res Appl. 2021;
[11] Benkhaya S, Rabet SM, Harfi AE. Classification, properties,
recent synthesis, and application of Azo dyes. Heliyon. 2020;6 46:1313–1320. https://doi.org/10.1002/col.22671
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