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Testing of cotton for Fineness and Maturity – Instruments and Precautions

N.Balasubramanian

Retired Jt. Director (BTRA) and Consultant1


Different methods of testing cotton for fineness and maturity are reviewed and the
precautions to be taken to get accurate results are discussed. Merits and limitations of the
methods are indicated. Relationship between the values from different methods are
discussed.

Fibre fineness and Maturity are important quality parameters of cotton. Fineness
determines strength, evenness, spinning value of cotton. Maturity determines
processing performance and yarn and fabric appearance. Immature fibres lead to
sticking tendency, roller lapping, fibre breakages and nep generation. Dye uptake
is poor and uneven. In this article an attempt is made to critically review various
test methods for determine fineness and maturity, their relative merits and
precautions to get accurate results.

Fibre fineness
1. Geometric Fineness
Cross section
Fibre cross section is prepared and viewed under microscope. Image is projected
on a monitor and pen is used to trace the boundary. Initially polar perimeter is
used to measure cross sectional area and curvimeter was used to determine
perimeter`1. Hebert2 et al use a graphic digitizer to trace the outline of cross
sections viewed under microscope. The data processed by a computer program is
used to calculate cross sectional area, perimeter and major minor axes of
equivalent ellipse. Merit - provides estimate of variability in cross sectional area,
perimeter and circularity. Limitation – It is time consuming and laborious.
Measurement of area and perimeter were later automated by the use of
computer.
Image analysis system
Cross sectional measurements
Xu3 et al developed a method for fully automated measurement of cross sectional
shape by image processing technique. Area, roundness, ellipticity and cumulative
angular function of cross sectional boundary are measured. Xu and Huang have 4
developed special algorithms for cross sectional images which improve
automation and accuracy of separating fibres contacting each other. Using a
special software program with a macro, cross sectional area, perimeter, wall
thickness area, lumen area and circularity have been measured. Another macro is
used to get maturity parameters from this. Two softwares viz; FIAS and CSIRO are
available to determine maturity and fineness from image analysis. Hequet 5 et al
has developed a set of reference cottons with preset maturity and fineness by
using FIAS. However FIAS introduced immature fibre bias and tended to

1
Tel No 9869716298, ba1ja2@yahoo.co.uk
2

overestimate maturity by8- 9 % . FIAS was upgraded by Xu and Guv 6 to overcome


this problem. Higgerson7 et al found good agreement in the perimeter values by
the two methods. But cell wall area and consequently maturity and fineness are
5 % lower with CSIRO software. FIAS software miscalculates lumen area in some
cases.

Longitudinal Measurement
Image analysis for longitudinal views under microscope is also used to determine
fineness and maturity. An adaptive threshold method helps to reduce errors from
unfocussed fibres8. Look up table and double scanning algorithm improve
efficiency of tracing and accuracy. Longitudinal data show a good correlation with
fineness measurements by traditional methods. Boylston compared maturity
measurement by longitudinal and cross section method. Maximum projection
along the length of the fibre agree with cross sectional measurement while
minimum projections do not. Cross sectional area provides true measure of
maturity9.
Maturity
Circularity
Circularity θ, is given by the ratio of fibre wall thickness (shown as shaded area in
Fig 1 ) by the area of the circle of same perimeter10.

Fig 1 :Circularity

4π A
θ=
P2
Where
A = cross sectional area of wall thickness
P = Perimeter
Θ = 0.577 when maturity factor is unity. Empirical relation between % mature
and dead fibres and Θ is
Θ = .00309(N-D) + 0.403
A value of N-D = 60 is taken as standard, Θs, standard circularity is given by
Θs = 0.59
Maturity ratio can be estimated by the following equation
Θ N −D
Maturity Ratio = Θ s = 200 + 0.7
Where N = % of fibres with Θ > .5 and
D = % of fibres with Θ < .25
3

Degree of thickening

Fig 2 : Degree of thickening


2π T
Degree of thickening is given by P (Fig 2)
Where T= wall thickness and
P = Perimeter
Xu4 et al found good correlation between degree of thickness and circularity
which represent independent measures of maturity. Matic-Leigh and Cauthen
found a curvilinear relationship between the two as shown in Fig 3
.
1

0.9

0.8
C
i 0.7
r
0.6
c
u
0.5
l
a 0.4
r
i 0.3
t
y 0.2

0.1

0
0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1

Degree of Thickening

Fig 3 : Relation between circularity and Degree of Thickening

Fineness (H)
Fineness expressed as weight per unit length (H) is related to area of
wall thickness (A) by
H=ρA
Where
4

ρ is density of cellulose in wall, which is 1.52 gms/cm 3

Specific surface area (S)


HS which is standard hair weight per cm is given by H/M
Specific surface area per gm S = P/H = 3.8 √HS /H = 3.8/√MH
as Perimeter P = 3.8√HS
Maturity Factor
Matic-Leigh and Cauthen11 define maturity factor by (Fig 4)

Fig 4 : Maturity Factor


2t
Maturity Factor, Mf=100 ×( D )

Where D = Effective circular diameter obtained by dividing perimeter P by π ,


t = Wall thickness of cross sectional area,
L = Lumen diameter
100× 2× π × t
Mf = P
( D−L )
Wall thickness is given by
2

Wall thickness area is obtained by subtracting lumen area from cross sectional
area11. Ratio of maximum to minimum fibre width along longitudinal direction
is correlated with maturity12. Xu and Huang4 contend that from maximum,
minimum, mean and Standard deviation of widths of each fibre maturity can
be obtained by the equation
Wsd
M=
Wmean
Where Wmean = Mean width of fibre
Wsd = SD of width
13
Barker has developed a method for determining circularity of fibre cross section
from longitudinal measurement.
Fullness
Fullness, which is considered a better estimate of maturity14, is given by

A− Al
P2¿ A max
4 π ( A− Al)
= P2
5

Where A = Overall area of cross section,


Al = Area of lumen cross section
Amax = Area of the circle with same perimeter P

Gravimetric method 
Fibres are counted either as whole fibres or after being cut to a finite length
(about 1.5 cm) under a microscope and weighed in a sensitive balance. About 500
to 1000 fibres have to be weighed to get accurate results Time consuming

Maturity

Caustic soda method (ASTM D1442- 06)

Fibres irrigated in 18% caustic soda are examined under microscope. Mature
fibres swell and assume a round cross section and immature fibres take a ribbon
like shape. Based on the ratio of lumen width to wall thickness upon viewing
under microscope of 400X magnification, fibres are classified as Mature, Half
Mature and Immature based on the following criteria
Mature (M) –(L/W < 1)
Half Mature (HM) – ( 1 < L/W < 2)
Immature (I) –( L/W > 2) where,

W = wall thickness and L = Lumen width

If M, IM and I are expressed as % then

Matrurity ratio Mr according to Shirley Institute is

Mr = (M-I)/200 +0.7

Iyengar and Ahmad15 of C TRL uses a term Matrurity coefficient Mc to define


maturity. This is given by
Mc = (M + .6*H + .4 * I)

This method has the merit that it takes into account half mature fibres.
American Method
Mature (N) – L/W < 2
Immature (D) – L/W => 2

This has the merit that it reduces subjectivity and is faster

According to Raes and Verchrabge16 microscopic measurements on swollen fibres


do not give a correct measure of biological maturity. Measurements made on
unswollen fibres give the correct measure and should be used to calibrate
instruments for measuring maturity like Arealometer and Shirley FMIT.

Polarised Microscope Method (ASTM D1442- 06)


6

Maturity is determined by interference colour of fibres under polarized


microscope of 100 X with first order retardation plate.
Immature – Blue, Purple
Half mature - Green – Yellow with blue parts, Green, Blue
Mature - Orange or Yellow, Green
Schwarz and Hotte17 have given a detailed account of how the test should be done
and the precautions to be taken.
Merits – Less subjective than caustic soda method as there is less confusion
between mature and immature fibres
Limitation – Measurement is likely to be influenced by total wall area. Lower
maturity is obtained with cottons with lower maturity.

Differential Dyeing
Fibres dyed in boiling dye bath containing .036g Diphenyl Fast Red 5 BL and .084g
Chloarantine Fast green BLL in 120g of water. Red dye has specific affinity for thick
walled mature fibres and green dye has affinity for thin walled immature fibres.
As a result
Mature fibre is dyed to red
Immature fibre is dyed to Green 

By visual comparison of the dyed samples against standards, maturity of the


sample is estimated. Rebenfeld and Wu18 present a method for quantitative
estimation of maturity to minimize subjective errors. Dyes from differentially dyed
sample are extracted and analysed under spectrophotometer to determine
Green/Red uptake. Green/Red uptake shows a highly significant correlation with
maturity. Estimation of maturity by differential technique is based on the fact
that immature fibres being less crystalline absorb more dye19.

Merits – Quick method, useful for mill application

Limitation – Not very accurate

Air Flow Methods

Airflow methods are based on resistance to flow of through a plug of fibres. The
rate of airflow is proportional to the reciprocal of square of specific surface area
of fibre. If M is maturity ratio, H is fibre weight per unit length then specific
surface area S is given by

1
S = 3.8 ×
√M H
o Micronaire ASTM D1448-11)

Determines rate of flow of air through a known mass of fibres (3.24 grams )
packed in a cylinder of known dimensions under constant pressure. This is
expressed in mirograms/inch. Micronaire value is dependent upon not only liner
density but also on maturity of fibres. Micronaire, Mc which indicates rate of
14.4
airflow is therefore proportional to MH as shown earlier. Based on a study of 100
cottons Lord20 found the following relation between Micronaire and Fineness and
maturity of cotton.
7

MH = 3.86 (Mc)2 + 18.16 Mc +13

H in turn is equal to M ×HS where HS is intrinsic fineness or fibre weight. HS


depends upon the perimeter of fibre crosssection.

Precaution :The cotton should be opened into a fluffy mass before being packed
into the sample older. Trash and foreign matter should be removed by cleaning.
Tests should be carried out in a laboratory where humidity and temperature are
maintained at standard level. Calibration should be done with International
cotton calibration standards with a low Micronaire and high Micronaire cotton.

Micronaire is calibrated on the basis of testing of American upland cottons in


terms of microgms/inch and therefore a correction may be needed while testing
India and Egyptian cottons.

Maturity by variable volume

The volume of the sample holder is increased by .3927 cu in by use of an 0.5 inch
spacer. Difference in Micronaire readings with and without spacer shows a
significant correlation with fibre maturity. This is offered as rapid method of
measuring maturity. Chapman and Staten21 found a correlation of .9 between
maturity from Micronaire by spacer and causticaire. Sundaram and Iyengar22 who
3
used a 8 inch spacer in place of 0.5 inch spacer, found a correlation of 0.8
between maturity by spacer and maturity by caustic soda swelling method.
Seshan23 et al varied the porosity of plug by varying the weight of the sample
instead of spacer. Difference in Micronaire value with 50 gr ad 40 gr sample
showed a correlation of 0.86 with maturity coeffiecient by caustic soda method
and the correlation is nearly same as spacer method. Balasubramanian24 showed
that the difference in Micronaire value at 2 porosity levels (by spacer or varying
the mass) is related to MH in the same way as Micronaire in the standard test.
Correlation between Micronaire difference and maturity arises mainly because of
this. Therefore, not much additional information about maturity than that
provided by Micronaire at standard test, is obtained by tests at 2 porosity levels.
Chapman’s work25 confirmed these findings. Correlation between micronaire and
causticaire maturity is same or slightly better than that between difference in
Micronaire with and without spacer and causticaire maturity.Chapman further
found that the curvilinear correlation between Micronaire and causticaire
maturity and fineness is slightly but consistently better than linear correlation.

Causticaire

After usual Micronaire test, sample is treated with 18 – 20 % caustic soda, with
1
1 2 , % wetting agent, by volume. Caustic soda is removed by thorough washing
and sample is dried to low moisture content and conditioned. Micronaire test is
again carried out on fluffed sample using causticaire scale. Maturity index and
fineness are calculated using a formula26. The following formula gives relation
between causticaire fineness and maturity index.

C =1.185+0.00075 T 2-0.020 MI,


8

Where C = Causticare fineness and MI = Maturity index.

The following formula gives relation between Causticaire Fineness and Micronaire
value.

C = 2.20 M - 4.34

Where C= Causticaire fineness and M= Micronaire. Du Bois and Van De Riet 27


found that all cottons with MI <76 lie on the left side of the line given by the
above formula and all cottons with MI>76 lie on the right side of the line. The
formula therefore needs correction. Further they found that comber waste has a
lower maturity than comber sliver as determined by causticaire. This is because
comber removes immature cluster of fibres. Instrument for automatic treatment
of caustic soda, washing and drying is also available which reduces the time for
testing28. A batch of samples of around 60 can be treated in about 50 min. A
dryer has to be used to dry and recondition the samples which may take 1.5 hrs.

Lord29 found results from causticaire are slightly biased depending upon
coarseness of fibre and has developed a correction to remove bias. Airflow
through mercerized cotton depends primarily on H√M .Calibration of instrument
on the basis of MH for unmercerised cotton and H√M for mercerised cotton
enables separate estimation of M, H and Hs

Micromat Fineness and Maturity Tester by SDL

The instrument provides independent estimates of fineness and maturity of


cotton from measurements of pressure drop through a plug of cotton at 2 levels
of compression.

Arealometer

The instrument determines specific surface area, fineness and maturity of fibres.
Resistance to air flow through a plug of fibres is measured at two pressure levels.
The increase in resistance to air flow at low porosity (high compression) over that
at high porosity is correlated to immaturity of cotton. It is proposed that immature
fibres get flattened at high compression and therefore offer higher resistance to
air flow30. While the instrument is useful for measuring of fineness and maturity
on raw cotton, it does not give accurate results on mechanically processed
material31. On the other hand, Balasubramanian32 et al found that Micronaire
value by both conventional and HVI testing do not show any significant change
from raw cotton to Lap, card sliver, comber sliver and finisher drawing sliver.
Worley33 et al found the following relationship between Micronaire (Mic) and
Arealometer (Ar)

Mic = 17.146 -0.044268 Ar + 0.000032 Ar 2

The instrument is not widely used like Micronaire.

Speedar

Speedar34 is a high speed airflow instrument to measure specific surface area.


Instrument is much faster as there is no need to weigh the specimen. Using
9

specimen between 5 to 10 gm, equipment automatically adjusts itself to weight of


specimen. Merits – Much faster, not widely used.

Port Air

Port air is a portable instrument which uses 8 gm sample. It gives Micronaire


value and Equivalent thickness (FT). Its main merit is that it can be used in the
field.

FT = 2000/A

Where A = specific surface area

HVI (ASTM D5867-05)

HVI incorporates Micronaire or Micromat as one of the modules for determining


fibre fineness. Testing procedure is same as in standard Micronaire except that
that the sample need not be weighed to the exact level. Microcomputers are
incorporated to test the specimen for a range of weights. For estimating maturity,
Shirley HMT instrument or near infrared spectroscopy is used.

Advanced Fibre Information System (AFIS)

AFIS employs scattered infra red light from a single fibre to determine fineness
and maturity. An aeromechanical separator separates the fibres to individual level
Shape of the fibre is viewed by sensor optically to determine fineness. Each fibre
is viewed at different angles to determine the shape. Maturity ratio of fibre is
given by the ratio of high degree (θ ≥ 0.5) and low degree (θ ≤ 0.25) wall
thickening of fibres . Instrument also gives fibre fineness fraction which is % of
fibres with fibre cross sectional area by number, less than 60µm2.

Merits – Rapid, requires small sample about 500mg, no subjective errors,

Limitation – requires calibration, costly

Near Infrared spectroscopy (NRI)

Maturity is determined by distinctly different absorbance spectra. It has 3


components viz; spectrophotometer, sample presentation system and
chemometric software. Photons in the light that strike the fibre are scattered
away from detector and do not fall on detector. Specific surface area of the fibre
determines the intensity of light falling on the detector. NRI uses this principle for
determining fineness and maturity of fibre35. A minimum of 5 gm of cotton fibre
10

compressed in a cell is placed in quartz bottom cell and NRI spectrophotometer


placed in it scans the sample. Software determines Miconaire, maturity ratio and
fineness from the spectral analysis. As NRI is a secondary measurement, it should
be calibrated with HVI or other classical instruments. Maturity and Fineness by
bench type and portable NRI systems show good agreement but the former is
more accurate. NRI measurements show good agreement with FMT in regard to
maturity, fineness and Micronaire36. Optimum instrumental conditions for NRI is
with the use of a glass-covered sampling port and increased instrumental gain,
with high R 2 values, low residuals, and with < or = 12% outliers37.

Ramsey38 used NRI instrument with wavelengths 1.53, 1.97 and 2.32µm to
determine fineness properties. High correlation (.89 and above) was found with
Micronaire and Arealometer in regard to Micronaire value, causticaire maturity
index, specific surface area and cross sectional area. Technical and instrumental
time are less with NRI compared to other instruments except for Micronaire.

Merits

Test is very rapid compared to FMT, Arealometer and Micronaire. It is easy to use,
more accurate and non destructive.

Limitation

Equipment is costly and requires to be calibrated with calibration cottons

Fourier transform infrared spectroscopy39 can also be used to determine


Micronaire and specific surface area of cotton with good accuracy. But it cannot
be used for accurate measurement of maturity.

Thermogravimetric (TGA)

Weight loss in Thermogravimetric (TGA) analysis in the region 225 to 425 0C is


significantly related to maturity of cotton. Weight loss shows a significant
negative correlation with HVI Micronaire, and maturity ratio by AFIS. This method
can also used to determine maturity and Micronaire40.
Cottonscan

Cottonscan is an instrument by CSIRO for determining fibre fineness. Fineness is


estimated from total length and weight of fibres cut to short lengths or snippets.
Pre weighed fibre snippets are suspended in an aqueous medium and image
analysis is used to measure total length.

Cottonscope

Cottonscope is an automated instrument for measuring fineness and maturity of


cotton employing birefringence property of the fibre. The equipment is based on
image analysis and polarized microscopy on small cut fibres (snippets) suspended
in water medium. Mature fibres appear with a red hue and immature fibres
appear translucent. From the total length and weight of snippets fineness is
estimated. Standard test involves measurement on 2000 snippets in 25 - 35 sec.
11

Merits – Rapid, accurate, requires small sample about 50 mg, free from subjective
errors

Limitation – Needs calibration, Costly, Maintenance of temperature and humidity


at the level used in calibration is important to get accurate results of fineness.

Siromat

Siromat is an automated polarized microscope for measuring maturity. Use of


digital colour cameras, Image analysis and powerful computer enables accurate
measurement of interference colours transmitted by fibre, from which fibre
maturity is estimated. The instrument is calibrated in terms of maturity ratio.

Meits – Rapid

Limitation – Not accurate, shows poor correlation with manual results.

UAK-1+ by ITRU

The tester uses image analysis of longitudinal images of single fibres to determine
fibre fineness and maturity through sophisticated algorithms. Other parameters
displayed are circularity coefficient., fibre perimeter,area of wall, standard fibre
fineness, causticare maturity %, degree of fibre flatness and micronaire value.
Time taken for test is 20 – 40 sec.
Merits – Rapid
Limitation – Expensive, accuracy not well established

Comparison of results from different instruments

Nair42 et al found close agreement in fineness values by HVI and gravimetric


method. This is surprising as HVI fineness is influenced both by gravimetric
fineness and maturity. AFIS and gravimetric fineness are close to each other in the
medium range (150 – 160 mtex). AFIS gives higher linear density in finer cottons
and lower linear density in coarser cottons. Agreement between maturity by AFIS
and caustic soda swelling method is found to be poor. On the contrary, Xu4 et al
found good correlation between Fineness by AFIS and perimeter by Image
analysis as also between maturity by AFIS and circularity by image analysis. Kim43
et al concluded that AFIS does not give accurate measurement of maturity on
developing immature fibres during growth. HVI, Cottonscope and Image analysis
results correlate well for developing fibres. But for fully developed fibres,
maturity by AFIS agrees with that of Image analysis, Maturity ratio by AFIS is
greater than that from Cottonscope. Further, Cottonscope is more sensitive to
maturity than AFIS. Fineness from Cottonscope is 20 % higher than AFIS.
Rodgers44et al found Cottonscope to be more responsive to maturity of
developing fibres during growth and is a useful aid in breeding program. Rodgers 45
et al also found good correlation between measurements of fineness and
maturity by Cottonscope and standard image analysis. Frydrych 46 et al found
good correlation between Cottonscan and AFIS but AFIS values are lower than
that of Cottonscan. Siromat results show poor correlation with other methods of
measuring maturity. Micronaire by UAK - 1 shows good correlation with digital
microscope estimates. Micronaire by airflow methods have a lower correlation
12

with digital microscope estimates46. Abidi and Hequet47 found good correlation
between FTIR measurements and HVI Micronaire and specific surface area by
AFIS.
Long48 et al report that polarised light technique underestimates maturity with
cottons having lower perimeter whereas crosssection method overestimates
maturity for such cottons. However, Schwarz and Hotte35 have shown that wall
thickness of mature low perimeter cotton is higher than that of immature and half
mature high perimeter (coarse) cottons. So the criticism that polarised light
technique cannot distinguish between mature low perimeter and immature large
perimeter fibre is not justified. D. P. Thibodeaux and K. Rajasekaran49 conclude
that image analysis method can be used as a reference technique for measuring
maturity of cotton and for calibration of instruments just like ITMF robin test
cottons. Image analysis can be used to predict Micronaire value. Hussain 50 et al
found that for a given variety of Indian cotton perimeter is nearly constant
irrespective of maturity. So Micronaire value gives a good indication of maturity
for a given variety. Webb and Burley26 found a better correlation between
causticaire maturity and nep generation in processing, yarn appearance and
strength than caustic soda maturity and Arealometer. Montalavo51 found that
Micronaire is more sensitive to wall thickness than perimeter. This is because
Micronaire varies as square of maturity and linearly with perimeter. However for
high Micronaire cottons influence of perimeter is higher. Goynes52 found that
differences in maturity of cotton grown at different locations is not shown by
Image analysis and AFIS pro though all other methods show the difference clearly.
When samples are hand combed to remove clumps of fibres a greater amount of
fibre gets removed from immature sample than from mature sample. So sample
preparation and the extent of combing to remove clumps of fibres affect maturity
measurement.

References
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Associated Cross-Sectional Features: TheirComparison by Means of
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28. https://archive.org/stream/apparatusforcaus32gaus#page/n1/mode/2up
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14

31. W.E. Morton and S. Radhakrishnan, The Performance of the Arealometer


in the Measurement of Fineness and Maturity of Raw Cotton, J Textile
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32. N.Balasubramanian , A. Basu and Ay.Ravindranathan, Fibre properties by
HVI and conventional testing at different stages of spinning, I Journal of
Fibre & Textile Research 1995 June p 63
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Micronaire Reading to Arealometer Specific-Surface-Area Values in Cotton,
Textile Research J, 1975, 45, p 326
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