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The Journal of The Textile
Institute
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37THE ULTRAFILTRATION OF
WOOL-SCOURING EFFLUENTS
P. E. Chisnall
a
& B. Robinson
b
a
Wool Research Organisation of New Zealand Inc. ,
Christchurch, New Zealand
b
International Wool Secretariat, Technical Centre ,
Ilkley, West Yorkshire
Published online: 01 Dec 2008.
To cite this article: P. E. Chisnall & B. Robinson (1979) 37THE ULTRAFILTRATION OF
WOOL-SCOURING EFFLUENTS, The Journal of The Textile Institute, 70:9, 397-406
To link to this article: http://dx.doi.org/10.1080/00405007908658873
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3777ie Vltrafiltration of Wool-scouring EffluentsChisnall and Robin.-ion 397
37THE ULTRAFILTRATION OF WOOL-SCOURING
EFFLUENTS
By P. E. CHISNALL and B. ROBINSON
It is shown that ultrafiliration is a feasible technique for producing an effluent completely frM
from suspended solids and wool grease together with a concentrated sludge Ironi a strong wool-
scouring liquor at a moderate cost. The process would be particularly applicable in areas where there
are stringent effluent standards.
1. INTRODUCTION
The scouring of raw wool produces a complex, highly polluting, aqueous effluent con-
taining wool grease, suint, and dirt. The removal of settlable solids, screening, centrifuging,
and recycling the clarified effluent to the scour as in the WRONZ Comprehensive Scouring
System^ result in significant economies in water, detergent, and heat-energy usage, an in-
crease in the recovery of wool grease, and a reduction in the total pollution load of the
effluent.
Although the water consumption can be reduced to 2 litre per kg of scoured wool
(excluding rinse water, which is little contaminated and can be discharged without treat-
ment), the final effluent is still highly polluting, with a chemical oxygen demand (COD) of
the order of 80 000 mg/litre. The treatment of this effluent to reduce the suspended solids
and the COD has been achieved by chemical destabilization followed by iiltration^-'*, but
this treatment has many disadvantages. It uses large amounts of expensive chemicals and
heat energy and gives variable results related to inevitable fluctuations in the feed.
The concept of using a membrane-separation process to give a physical separation of the
suspended matter (grease and dirt) regardless of liquor characteristics is very attractive in
promising a reliable performance. This relatively new filtration process depends on circu-
lating a process liquid at a high velocity past an extremely thin membrane with a pressure
differential of 200-300 kPa across it. Rapid filtration through the membrane occurs at an
almost constant rate, since there is little or no blinding of the membrane by retained solids,
as occurs in static filtration. Any build-up on the membrane surface can usually be removed
at intervals with suitable cleaning solutions. The membrane pore size is commonly 0.2-
0.4 nm, which is much smaller than the particle size, so physical plugging of the pores is
unlikely. The liquor is thus divided into an ultrafiltrate (UF), containing suint but no
suspended solids, and a stream in which the suspended solids are concentrated.
The application of ultrafiltration to wool-scouring effluents has been examined by
Pearson^, using a Dorr-Oliver 6CL pilot plant, and by Beaton^, using a larger Dorr-Oliver
IOPOR test unit. Mozes and Turpie' have also investigated the process by using a hollow-
fibre membrane configuration, while EarlyS has operated pilot plants with both hollow-fibre
and tube modules. The study reported in the present paper was undertaken to evaluate the
UF process on the final effluent from a fine-wool scour involving the use of the WRONZ
Scouring System. The process was thus tested under commercial scouring conditions, the
largest available pilot plant, with full-scale membrane cartridges, being used. Tests were
devised to establish the optimum operating parameters and the ability of the membrane
system to be operated for extended periods. ^
2. OBJECTIVES
It was desired to obtain data on the following:
(a) the rate of filtration and how this was affected by the process-liquor concentra-
tion and its velocity of flow past the membrane, the pressure differential, and the
time between cleaning cycles;
J. Text. Inst., 1979, No. 9 I
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^^^ 37The Ultrafiltration of Wool-scouring
(b) the resistance of the membrane to abrasive wear and blockage;
(c) the characteristics of the ultrafiltrate;
(cT) the effectiveness of cleaning; and
{e) the characteristics of the concentrate.
The pilot plant was operated in three modes to enable appropriate measurements and
observations to be made.
3, EQUIPMENT
The trials were carried out on a skid-mounted pilot plant supplied by Dorr-Oliver Inc.,
nme IOPOR-type FRP membrane cartridges being used. These cartridges consist of a series
of fiat membrane-coated leaves, stacked in parallel and 3.2 mm apart. The ultrafiltrate is
taken off via the porous interior of each leaf to a central header point. Each cartridge has
1.9 m2 of membrane area, and three cartridges are located inside a GRP pressure housing
to form a module. In the pilot plant, three such modules were connected in series in the
main process loop, which also contained a variable-speed recirculating pump, a shell-and-
tube heat exchanger, and a magnetic flowmeter and had suitable drain, inlet, and outlet
connexions. The unit was equipped with a pressure sensor with high- and iow-pressure cut-
outs and alarms to prevent possible membrane damage.
Tt was necessary to provide sotne ancillary components to complete a flexible, reliable
pilot plant. These included a i500-litre storage tank, a slow-speed positive-displacement
screw pump to feed and pressurize the UF loop, and a 200-litre steam-heated cleaning-
solution tank. The complete plant is illustrated diagrammatically in Fig. 1.
4. EXPERIMENTAL
4.1 Operating Modes
The three operating modes are depicted in Fig. 2.
Fig. 1
Diagram of the pilot plant: (1) scour-liquor feed; (2) storage tank
(1500 litre); (3) positive-disptacement feed pump; (4) cleaning-
solution tank (200 litre); (5) variable-speed recirculation pump;
(6) variable-speed cleaning-solution feed pump; (7) ultrafiltration
modules; (8) pressure gauge; (9) ultrafiltrate sample valves;
(10) heat exchanger; (II) temperature-control valve; (12) drain
valve; (13) pressure-relief valve; (14) steam supply; (15) concen-
trate discharge; (16) ultrafiltrate discharge; (17) flowmeter
Fig. 2
Diagram showing the three operating modes: (1) storage tank;
(2) feed pump; (3) recirculation pump; (4) memhranes; (5) heat
exchanger
J. Text. Inst,, 1979, No. 9
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EffluentsChisnall and Robinson 399
4.2 Batch-concentration Mode
After preliminary tlux determinations in which cleaning solution was used at 50"C,
206 kPa, and a velocity of 2.14 m/sec, the loop was drained and immediately refilled with
process liquor (scour effluent) by the screw feed-pump. Duritig this stage, the ultrafiltrate
ports were closed to prevent static filtration (i.e., with no liquor movement over the surface
of the membrane), and care was taken to bleed at! air from the loop while it was being filled.
The loop was then pressurized by throttling the bleed valve returning liquor to the storage
tank until the pressure was above the lower cut-out value of 175 kPa. This allowed the main
recirculation pump to be started and its speed adjusted to give the required velocity of
llow, whereupon valves could be opened to withdraw ultrafiltrate from the system.
Provided that the bleed rate from the loop to the storage tank was about ten times the
ultrafiltrate flow-rate, the contents of the loop and the storage tank were maintained at the
same (but increasing) concentration. The ultrafiltrate and the concentrate were sampled
and the ultrafiltrate flow rates measured at regular intervals of either 15 or 30 min. The
temperature was kept at 5O''C, the maximum permissible for extended operation, since
Pearson^ and Beaton* had shown that the flux increased with temperature.
i '
4.3 Total-recycle Mode
Where it was necessary to have a process liquor of constant composition in order to
test for variables such as the efiect of flow velocity over the membrane and the trans-
membrane pressure, all the ultrafiltrate was recycled to the storage tank. The loop-liquor
composition was thus held nearly constant, though some minor changes occurred because
of evaporation and splashing. The start-up procedure was identical to that described above.
A total recycle for up to 36 hr before cleaning was also used to test the decay of flux
with time because of slow fouling of the membrane.
4.4 Continuous-concentration Mode
This simulated the operation of a commercial system using a cascaded series of loops.
The pilot plant was operated as if it were one of the loops of a cascaded system, both con-
centrate and ultrafiltrate being discharged. An operating point was selected from the pre-
vious experiments, the required concentrate-discharge rate being calculated from a know-
ledge of the input membrane-retained-solids concentration (MRS), the concentrate MRS,
and the ultrafiltrate flow-rate. The plant was started up as before and the calculated con-
centrate flow for the selected operating cotiditions obtained by adjustment of the loop bleed
valve. Sampling and flow measurements of both the ultrafiltrate and the concentrate were
done at 30-min intervals.
4.5 Membrane-cleaning
A proprietary cleaning solution developed by Dorr-OHver Inc. was used for all cleaning
operations. The exact procedure was considered to be important and was as follows.
(i) All pumps were switched off, the main feed valve was closed, and the contents
of the loop were drained,
(ii) The loop was immediately refilled with a flushing solution containing 0. 1%
non-ionic detergent at 50C.
(iii) The flushing solution was circulated around the loop by the main recirculating
pump, and suflicient solution was allowed through the membranes to flush the
ultrafiltrate lines.
(iv) The unit was shut down, drained, and immediately refilled with cleaning solu-
tion at 50C.
./. Text. Inst., 1979, No. 9
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400 37Tfte Ultrafiltration of Wool-scouring
(v) The initial cleaning cycle provided for flow past the membrane surface with no
ultrafiitrate draw-off. If the initial flux was not recovered within 1.5 hr, the
ultrafiltrate valves were opened to allow cleaning solution through the mem-
branes.
This procedure was evaluated by measuring the ultrafiltrate flux at regular intervals
during the cleaning cycle. Before all scour-liquor trials, ultrafiltrate-flux determinations
were made on each membrane by using cleaning solution at 50C, a velocity of 2.14 m/sec,
and a loop pressure of 206 kPa. This allowed an evaluation of the degree of fouling occurring
during the trials and enabled the cleaning cycle necessary to restore the flux to the pre-test
conditions to be decided.
The modules were dismantled after every 50-hr operation and the membrane cartridges
examined for any signs of abrasive wear or physical blockage.
4.6 Analyses
Samples were analysed for total solids (TS), total grease, dirt, suint, and COD by
methods applicable to wool-scour liquors^-**.
4.7 Examination of the Concentrate
Destabilization of the concentrate was effected by adding concentrated sulphuric acid
to pH 2 and boiling for 30 min. The destabilized sludge was neutralized with lime and de-
watered in a Sharpies P600 horizontal decanter. A polyelectrolyte was added to the decanter
feed to improve solids capture.
Samples of the concentrate were sent to Solvent Beige for evaluating the potential for
grease recovery prior to final disposal. i
5. RESULTS AND DISCUSSION
5.1 Effect of Process Conditions
S.I.I Process-liquor Coneentration
The ultrafiltrate flux was found to be highly dependent on the concentration of the
liquor in the loop, as is typically shown in Fig. 3. Fluxes as high as 135 litre hr~^ m"- at
4.2% total solids and down to 11 litre hr-i m-^ at 26% total solids were recorded. The
results were in general agreement with those reported by Pearson^ and Beaton*".
50- .
CJtY 2.In
LOOP HIESEUat i!10 HP*
Eiiril 50'C
Fig. 3
Variation of UF flux with total solids
in the loop in batch concentration
5 10 15
Tr i TAL S O L l P S , I - .
/ . Text. Inst., 1979, No. 9
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EffluentsChisnall and Robinson 401
The flux of interest to the plant designer is the average value over the desired range of
concentrations. This can be obtained for batch operation by measuring the volume of ultra-
filtrate in a given time or by plotting the flow-rate-time curve and measuring the area under
the curve. A typical curve is shown in Fig. 4, and some fluxes derived from it are given in
Table I. Thus a fivefold concentration of the MRS {3.3 %) in this liquor gave an average UF
COM) r I mi '
vELociry 2.7 n/t
HtWI LOOP PHtSSUBt JOO eP*
Fig. 4
Variation of UF flow with time in batch concentration: L= loop total solids; U UF total solids
Table I
Average Fluxes for Varying Degrees of C<mcentration
Concentration (% w/w)
Initial
TS
5.46
5.46
5.46
5.46
MRS
3.10
3.10
3.10
3.10
Final
TS
10.82
12.78
15.58
19.65
MRS
8.02
9.76
12.32
16.13
Flux (litre hr-' m-2)
Average
50.0
45.9
42.2
39.5
Final
33.7
27.1
22.5
18.1
(lux of nearly 40 litre hr"^ m"^ Whereas it is possible to concentrate the liquor still further,
the resulting decrease in flux would generally make this impracticable. Factors to be con-
sidered in this regard would be the capital and operating costs and the ultimate disposal of
the concentrate.
5.1.2 Velocity of Liquor Flow
Dorr-Oliver have recommended the use of velocities in the range 2.5-3.0 m/sec in
3.2-mm channels to give optimum performance, with the flux, membrane wear, and energy
required for liquor circulation taken into consideration. Above this range, the increase in
the flux is outweighed by the increase in wear on the membranes and the increased cost of
pumping. The presence of abrasive particles could reduce the optimum velocity for wool-
scouring liquors, but extended periods of operation would be required to check on this
aspect. In all the trials conducted in the study reported in the present paper, the velocity
was kept below 3 m/sec to reduce the risk of damaging the membranes, and no sign of
./. Text. Inst., 1979, No. 9
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402 31The Ultrafiltration of Woohscouring
abrasive wear was found after 205 hr of operation. The long-term resistance of the mem-
branes to abrasive wear and other physical damage is, of course, critical to the viability of
the process.
The velocity ofthe liquor was found to have a large effect on the UF flux, this being
doubled by increasing the velocity from 2.15 to 2.7 m/sec. This is explained by a reduction
in the build-up of a boundary layer and the increasing rate at which the rejected matter is
carried away from the membrane surface at the higher velocity.
5.1 J Trans-membrane Pressure
Ultrafiltration theory indicates that, above about 100 kPa, the UF flux should become
independent ofthe applied pressure because of compaction ofthe boundary layer, which
would result in an increase in resistance to flow, cancelling out any gain in flux at the highei
pressure. This was found to be true at high concentrations (> 5 % TS) and at relatively low
velocities (<2. 5 m/sec). However, at lower concentrations or higher velocities, the flux
became increasingly dependent on the pressure until, with pure water, it was directly pro-
portional, since there was then no boundary layer. Thus these factors must be considered in
selecting the operating pressure for a plant, and it may be advantageous to use the maxi-
mum permissible pressure of 350 kPa. which would allow for the inevitable pressure drops
in the system and still provide an adequate pressure at the final membrane in a large unit.
I -
5.2 Membra ne-foui ing , - |
When the plant was operated under total-recycle conditions, a gradual fall in the flux
was observed with liquors of high concentration, as is shown by the lower curve of Fig. 5
for a liquor containing 12% TS. However, with more dilute liquors, an inexplicable initial
increase in flux was observed on several occasions, this being followed by the expected
decrease, as shown by the upper curve of Fig. 5. It is considered that this initial increase must
have been an artefact, probably related to some change in the physical characteristics ofthe
liquor caused by pumping, etc., since the membranes had been shown to be clean. Thus the
flux would normally be expected to fall during the first few hours of operation and then
to reach an almost steady rate with a liquor of constant composition.
I WEMTWE
XEAK LOOP f.l^-.M
VELKI tr
LOW TDTXl SOLJDS
VOW ..5.
50"C (BOTH)
(BOTH)
4 . 1 6 1 Vl/H
I RE,
Fig. 5
Variation of UF flux with time in total recycling; lower curve is that normally expected; inset upper curve
shows an unexplained initial increase in flux
5.3 Membrane-cleaning
A 2-hr cleaning cycle past the membranes was usually found to be adequate to restore
the initial flow-rate. Additional time or some cleaning through the membranes (or both)
was needed after a liquor of high concentration had been treated for a lengthy period.
J. Text. Inst., 1979, No. 9
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EffluentsChisnall and Robinson 403
Typical changes in flux during cleaning are shown in Fig. 6. The highest cleaning-solution
flux achieved was 270 litre hr-^ m"-, but it was found that the degree of cleaning did not
matter as long as the flux was increased to a level above that required in the next trial.
As a result of the trials, a daily 2-hr cleaning cycle is recommended, a Dorr-Oliver pro-
prietary cleaning solution being used at pH 10.5. (A higher pH would result in an increased
cleaning flux but could damage the membranes.) The membranes should be left to soak in
the solution when not being used.
5.4 Continuous Concentration
Operation in this mode most closely approached the commercial situation. Both ultra-
filtrate and concentrate were withdrawn from the system, which was allowed to equilibrate
before sampling commenced. Fig. 7 illustrates the results obtained. The dotted line shows a
batch-concentration curve under the same conditions, and it is significant that all but two
of the results are better than the batch-concentration curve.
(UODLTIONS:
VtLOCITY 2. 1U /
"EAN UOQP P MS SUM 206 P)1
lENPtBiTUBE M' C
COHDItlCNS!
wELDCtrv 2. as / !
nCM LQIlP PRESSURE 2*10 KpA
TEnPEmi uBi SO'C
15 5U 15 60 75 90 1D5
I I N E , "I K
Fig. 6
Cleaning-solution flux
10 12 lit 16
S OL I DS . I - V-
Fig. 7
Variation of UF flux with total solids
in loop in continuous conccn I ration; the
broken curve is for batch concentration
under the same process conditions
5.5 Characteristics of the Ultrafiltrate
The ultrafiltrate was a clear amber liquid with a strong odour of suint, free from sus-
pended matter and with a tendency to foam when shaken. I ts concentration, colour, and
COD increased with increasing concentration in the loop, as shown in Fig. 8. The total solids
content ranged from 1.55 to 2.86% and the closely related COD from 11 400 to 19 400 mg/
litre. The maximum solvent-extractable matter observed was 0.07 %., and this was considered
to be detergent rather than grease^, since the emulsified grease particles in the original
liquor were probably very much larger than the pores in the membrane.
5.6 Characteristics of the Concentrate
Concentrates with 20% total solids were produced as a matter of routine with final
UF fluxes of around 15-20 litre hr~^ m^^ and no problems were encountered in cleaning the
membranes afterwards. The highest concentration reached was 26% total solids (16.6%
wool grease, 6.7% dirt, and 2.7% suint) at a flux of 10.7 litre hr-^ m-^. This sludge was a
J. Texl. tnst., 1979, No. 9 \
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404 37The Ultrafiitration of Wool-scouring
L O O P I Q T S L S D U D S . I - / w
Fig. 8
Relation betw een U F total solids and loop total solids for three runs w ilh different liquors
thick viscous fluid above 40"C and became a greasy solid on cooling. I t may not be economic
to concentrate to this level because ofthe low flux, but this w ould depend on the subsequent
treatment ofthe sludge.
T he sludge could be destabilized by boiling w ith acid as described and dew atered in a
decanter centrifuge to give a solid sludge w ith a total solids content of 45 %.
T he sludge had a high grease content, and reports from S olvent Beige indicated thai
laboratory recoveries of 90% of the grease w ere possible from their experience w ith the
S over solvent- scouring system. T he grease could be refined and the degreased sludge dried
to a disposable pow der in a rotary- drum dryer.
6. ECO NO MI CS
T he cheapest method of effluent treatment is generally in admixture w ith domestic
w astes in a municipal treatment plant. How ever, large increases in the charges levied on
industry have recently been imposed in many ofthe w ool- processing areas, and restrictions
on the quality ofthe effluent accepted have become more severe. Both these factors favour
the use of an in- plant treatment, such as ultrafiltration. T o be economically viable, this
treatment must be cheaper than competing methods or have particular advantages, such as
the ability to achieve stringent efliuent standards relating lo suspended solids and grease.
T he cost of an ultrafiltration unit to treat the eflluent from a 2- m- w ide scouring train,
operating under the WRO NZ S couring S ystem for 5000 hours per year and handling 1000 kg
of greasy merino w ool per hour, has been estimated as about 2 p per kg of scoured w ool, as
show n by the analysis of costs given in T able I L I t should be noted that it is important in
comparing methods of treating w ool- scouring effluents to base the cost on the mass of w ool
processed, since the volume of effluent produced can vary by a factor often betw een plants.
T he costs of disposal of the ultrafiltrate and the sludge w ould be additional to this but
very variable depending on the circumstances. T hus it might be possible to lecycle part of
the ultrafiltrate to the scouring train to make savings in detergent and w ater usage at the
expense of a build- up of dissolved solids and a possibility of staining the w ool. S ince the
ultrafiltrate virtually contains only suint that is rich in potassium, it is a potential source of
potassium compounds in a fairly pure form.
T he sludge could probably be disposed of by dumping, or it may be feasible to dew ater
it, or to recover the grease from it. T he last possibility could very w ell be a viable proposition
if the concentrates from several plants could be combined for grease extraction and final
disposal at a central treatment facility.
J. Text Inst., 1979, No. 9
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EffluentsChisnall and Robinson 405
Table n
Cost of Ultrafiltration
Basis of Costing: Plant to treat effluent from scouring 1000 kg
of greasy wool per hour for 5000 hr per year. Ultrafiltration
process to separate the effluent into a grease-free and sus-
pended-solids-free ultrafiltrate and a concentrated sludge
containing 20% total solids. It is assumed that the scour
operates the WRONZ Comprehensive Scouring System and
that no other pre-treatment is required.
Capital Cost:
Installed cost of plant (100 m^)
Capital-recovery factor
Annual charge for capital
Operating Costs (annual):
Membrane replacement
Electricity
Cleaning chemicals
Labour
Maintenance
Incidentals
Total annual operating costs
Total Annual Cost
Cost per kg of greasy wool
Cost per kg of clean wool (yield 66 %)

120 000
0.25
30 000
12 000
6000
500
10 000
3 500
2 500
34 500
64 500
: 1.29 p
1.95 p
7. CONCLUSIONS
Ultrafiltration has been demonstrated to be a feasible technique for separating a strong
wool-scouring effluent into a concentrated sludge containing about 20% total solids and a
grease- and suspended-solids-free solution containing about 2-3 % total solids and with a
COD of around 15 000 mg/litre.
No problems of membrane degeneration or erosion were found to occur during the
trials, and the UF flux could be restored by suitable cleaning procedures.
The cost of the ultrafittration stage when operated on the effluent from a WRONZ
Scouring System has been estimated as about 2 p per kg of scoured wool, plus the costs of
disposal of the sludge and ultrafiltrate.
The application of ultrafiltration would appear to be only marginally economic at this
stage, but, in some areas, stringent effluent standards may favour its use as a positive method
of ensuring the complete removal of suspended solids and grease. A full-size plant has, in
fact, been operating successfully under just such circumstances for some considerable time
and has enabled a company to operate in a locality where this would not otherwise have been
possible.
ACKNOWLEDGEMENT
The authors wish to thank the management and staif of Sir James Hill & Son Ltd,
Keighley, West Yorkshire, for their co-operation in the project reported in this paper and
for making facilities available and Mr. Neil Beaton of Dorr-Oliver Ltd for supplying the
IOPOR pilot plant and for giving valuable advice on its operation.
J. Text. In-it., 1979, No. 9
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406 37The Ultrafiltration of fVool-scoitring EffluentsChisnall and Robinson
REFERENCES
' R. G. Stewart, G. V. Barker, P. E. Chisnall, and J. L. Hoare. WRONZ Report No. 25, 1974; Wool Rec.
1975, 127, Text. Mach. SuppL, 1 Feb., 8; 18 April, 13.
2 R. P. Marker. Chem. Engr, 1970, 77, Jan./Feb., CE8.
^ J. R. McCracken and M. Chaikin. Text. J. Aust., 1976, 51, No. 2. 4.
* J. R. Christoe. J. Water Polln Cont. Fed, 1977, 49, 848.
5 A. J. C. Pearson. / . Water Polln Cont. Fed., 1976, 48, 945.
'' N. C. Beaton. Text. Inst. Industr., 1975, 13, 361.
' T. E. Mo7es and D. W. F. Tiirpie. SAWTRI Technical Report No. 349, 1977.
^ D. B. Early. WRONZ Report No. 48, 1978.
' R. J. Fearn, W. H. Hetherington, S. M. Jaeckel, and C. D. Ward. J. Soc. Dyers Col., 1967, 83, 146.
(P.E.C.) Wool Research Organisation of New Zealand Inc.,
Christchurch,
New Zealand.
(B.R.) International Wool Secretariat,
Technical Centre,
Ilkley.
West Yorkshire.
Received 3\.
Accepted for publication 15.2.1979
. Text. Inst., 1979, No. 9
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