1352
6, 1973)
FEEDS
Hoist Filtration Apparatus for Van Soest Detergent Fiber Analyses
DAVID 0. HOLST
Experiment Station Chemical Laboratories, Agriculture
Columbia, Mo. 65201
New filtration e q u i p m e n t was developed t o
i m p r o v e t h e a c i d - d e t e r g e n t m e t h o d of fiber
fractionation. This apparatus incorporates a
v a c u u m m a n i f o l d w i t h a n a i r m e t e r i n g device
t h a t provides t h e o p e r a t o r very p r e c i s e c o n t r o l
over t h e p a r t i a l v a c u u m , p e r m i t t i n g a very
g r a d u a l c h a n g e i n v a c u u m level as n e e d e d for
p r o p e r f i l t r a t i o n . T h e p a r t i a l p r e s s u r e is p r o -
vided by a w a t e r a s p i r a t o r . A h o t w a t e r j a c k e t
p e r m i t s a c o n t i n u o u s flow of h o t w a t e r a r o u n d
t h e s a m p l e d u r i n g t h e filtering process t o
k e e p t h e s a m p l e h o t . T h i s s p e e d s filtering o n
p r a c t i c a l l y all s a m p l e s a n d is e s s e n t i a l for reli-
able results on samples high in carbohydrates
a n d s a l t s . As a r e s u l t of t h i s n e w filtration
e q u i p m e n t we d o n o t n e e d a s b e s t o s for a filter
a i d . T h i s e l i m i n a t e s t h e n e e d for d u p l i c a t e
a c i d - d e t e r g e n t fiber a n a l y s e s w h e n u s i n g 7 2 %
H2SO4 for t h e cellulose a n d l i g n i n d e t e r m i n a -
t i o n s . Six i n d e p e n d e n t a n a l y s e s w e r e p e r -
f o r m e d o n e a c h of 9 s a m p l e s (3 feces, 3 o r t s ,
a n d 3 feeds) for t h e d e t e r m i n a t i o n of a c i d -
d e t e r g e n t fiber a n d i t s c o n s t i t u e n t s . T h e aver-
a g e m a x i m u m differences for t h e s e a n a l y s e s
i n d i c a t e t h a t t h i s filtration a p p a r a t u s a n d t h e
m e t h o d are reproducible and have reduced t h e
filtration t i m e f r o m several h o u r s , o n s o m e
s a m p l e s , t o 15 m i n .
T h i s work was u n d e r t a k e n to develop an a p p a -
r a t u s for the new detergent system of fiber
fractionation (1) reported b y Goering a n d Van
Soest. T h e reagents, procedures, and processing
times as prescribed in Agricultural Handbook No.
879, " F o r a g e Fiber Analysis" (1), were used with
no a t t e m p t at modification. However, we found
t h a t t h e filtration a p p a r a t u s as described in t h e
above publication was inadequate in 2 specific
areas: (a) T h e r e was no way to provide a definite
or specific a m o u n t of v a c u u m on the sample, or
no way to v a r y it uniformly as the need arose.
(6) N o provisions were m a d e to keep t h e sample
h o t during the filtering process. Our modified fil-
t r a t i o n a p p a r a t u s is described below:
Received November 15, 1972.
JOURNAL OF THE AOAC (Vol. 56, N o .
Building, University of Missouri,
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Filtration Method
Apparatus {Patent Pending) (Fig. 1)
(a) Vacuum manifold.—Acts mainly as reservoir
to cushion any sudden change in pressure and per-
mits uniform or gradual buildup of vacuum. Each
filtering unit has separate manifold with aspirator to
provide vacuum.
(b) Stopcock.—120°, to shut off vacuum to sample,
for washing, while retaining vacuum in manifold.
(c) Stopcock with metering device.—To bleed air
into vacuum manifold to control amount of vacuum.
(d) Receptacle.—To receive filter crucible. This
contains cone-shaped hard rubber gasket to provide
vacuum seal with crucible.
(e) Vacuum gauge.—To indicate vacuum on each
filtering crucible.
(f) Hot water jacket.
(g) Stopcock in hot water line.—These last 2 items
permit continuous flow of hot water around filter
crucible to keep sample hot during filtration.
Analytical System
Third filter unit has two 3-way stopcocks installed
in waste line so vacuum can be routed through filter-
ing Erlenmeyer flask, making it possible to save fil-
trate for further analysis (Fig. 2). This figure shows
how new Hoist filter apparatus is accommodated in
equipment used for processing crude fiber. A bank of
6 reflux units sits on either side of hot water tank
(Item 2). Supply of distilled water is held in the
reservoir (Item 5) and flows by gravity through coil
of copper tubing in hot water tank and then through
rubber tubing (Items 3 and 4). Item 4 leads to stop-
cock (Item 7, Fig. 1) on filter apparatus while Item 3
is approximately 10' long and is used to wash sam-
ples from reflux beakers into filter crucibles. Item 6
shows filter crucible in place, and how hot water is
flowed around crucible while filtering. (This appara-
tus is available from Analytical Biochemistry Lab-
oratories, Box 1097, Columbia, Mo. 65201.)
Procedure
Procedures as outlined by Goering and Van Soest
(1) were followed with the exception of filtering pro-
cess and placing of samples on reflux apparatus.
Place samples on reflux apparatus at 5 min intervals
as this is speed at which they can subsequently be
filtered with 3 filter units in filter apparatus.
HOLST: FILTRATION APPARATUS FOR ACID-DETERGENT ANALYSES
FIG. 1—Hoist filtration apparatus.
Place crucible in receptacle, flow hot water around
and into crucible to warm it, and set vacuum so indi-
cator needle on pressure gauge is just lifted from peg
(0-1" Hg).
Remove reflux beaker with sample from hot plate
(do not swirl sample) and add hot water inside cruci-
ble again just before pouring sample. Pour sample
very gently into filtering crucible so most of liquid is
decanted before solid enters crucible. Wash sample
from beaker with minimum of hot distilled water.
Continue to flow hot water around crucible until
filtering process is completed.
Observe rate of flow of filtrate through system; if
it slows or stops, gradually increase vacuum until
flow resumes. It is very important to maintain flow
of filtrate through fritted glass because, if flow of hot
filtrate stops, fritted glass cools, and then salts and
starches precipitate and gel, clogging fritted glass.
Shut off vacuum (for washing sample) by 1 of 3
methods: Use stopcock (Item 2, Fig. 1) to shut off
vacuum and still maintain same level of vacuum in
manifold; use metering device (Item 3, Fig. 1) to
lower vacuum in entire system; and, if pressure is
<4" Hg, lift crucible from receptacle for washing.
However, using metering device is recommended as
this will always start vacuum at 0 after each washing.
Vacuum is provided for filtering unit by water
aspirator with water valve wide open so vacuum can
be increased to 30" Hg, if needed, just by turning
metering device.
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Discussion
Our modified apparatus can be used for any
filtering operation. We have used it in the Experi-
ment Station Chemical Laboratories for filtering
difficult crude fiber samples and in the sulfur
analysis procedure. It has also been useful for
backwashing (2) the Van Soest filter crucibles.
This is accomplished by inverting the crucible on
the rubber gasket and flowing water through it
under vacuum. This technique is used on hard-
to-clean crucibles.
Another significant application of the Hoist fil-
tration apparatus was found in the 72% H2SO4
method for lignin determination (1, 3-5). With
this filtration apparatus, the use of asbestos as a
filtering aid is eliminated, saving considerable
time and manipulation in the acid lignin analysis.
The deletion of asbestos as a filter aid resulted
in the following H2SO4 method for acid-detergent
fiber, cellulose, lignin, residual ash, silica, and
cutin determination:
Analyze for acid-detergent fiber (ADF) in
normal way as prescribed (1), using the new
filtration apparatus, and determine ADF content.
Treat fiber residue with 72% H 2 S0 4 for 3 hr.
Some H2SO4 will filter through fritted glass, so
add more as needed. After 3 hr, filter excess acid
1354
FIG. 2—Hoist filtration apparatus with reflux units and hot water supply.
and wash 5 times with hot distilled water to re-
move acid. Dry overnight in 100°C oven. Remove
from oven, place in desiccator to cool, and weigh.
Difference of this weight and final weight from
ADF analysis (1) is calculated as per cent cellu-
lose.
Ash residue overnight at 500°C, remove from
furnace, desiccate until cool, and weigh. Differ-
ence of this weight and cellulose weight is calcu-
lated as per cent lignin. Difference between empty
dried crucible weight and ashed weight is calcu-
lated as per cent residual ash.
Treat residual ash with 4-5 ml 48% HBr for
1.5 hr; add more acid if red color appears. Wash
out excess HBr twice with acetone, filtering ace-
tone after each washing. Ash overnight at 500°C,
remove from furnace, desiccate to cool, and
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weigh. Difference between this weight and empty
dried crucible weight is calculated as per cent
silica.
Our modifications are sufficient for the deter-
mination of ADF, cellulose, lignin, residual ash,
and silica in most of the common forages which
normally are low in cutin. However, with feed
grains or rations that contain seed hulls high in
cutin, the ashing to determine lignin will be mis-
leading as the cutin fraction will ash and erro-
neously be reported as lignin. With samples
known to contain seed hulls, the cutin fraction
can be determined as follows: Instead of ashing
to determine lignin, use the potassium perman-
ganate method as reported by Van Soest et al.
(1, 2) to determine per cent lignin. The loss in
weight on ignition is calculated as per cent cutin.
HOLST: FILTRATION APPARATUS FOR ACID-DETERGENT ANALYSES 1355

Calculate per cent residual ash as above and Table 1. C o m p a r i s o n of m o d i f i e d H2SO4 m e t h o d "
with KM11O4 m e t h o d 6
determine silica as above.
Table 1 shows the greater precision obtained Cellu-
lose, Lignin,
with the Missouri Station H2SO4 method over Sample Method av. %c Range av. %c Range
the KMnC>4 method for determining cellulose and
Feces KMn04 25.85 0.84 11.20 0.88
lignin in acid-detergent fiber.
H2S04 25.10 0.01 11.54 0.12
With the Van Soest detergent fiber technique,
Feces KMn04 27.13 0.70 10.23 1.28
the analysis of 12 samples per day was considered H2SO4 26.94 0.14 10.12 0.21

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satisfactory, writh some samples requiring several Feces 26.96 0.89 10.06 0.81
KMn04
hours to filter. With the Hoist filtration apparatus H2SO4 27.58 0.42 10.30 0.00
even the most difficult samples can be filtered in Orts KMn04 29.88 0.73 6.55 0.44
less than 15 min and it is possible to analyze 60 H2SO4 31.26 0.30 4.98 0.23

or more samples per day. In the Van Soest meth- Orts KMn04 28.16 1.09 6.70 1.88
od, crude fiber filters were used with no way to H2SO4 29.66 0.44 5.61 0.14

control the vacuum. With this new filtration Orts KMn04 29.82 1.92 10.62 1.49
H2SO4 30.94 0.79 9.66 0.27
apparatus the vacuum can be controlled with the
Feed KMn04 27.03 0.32 6.74 1.06
air bleed-in valve (Fig. 1, Item 3). In the Van 28.04 0.26 5.37 0.04
H2SO4
Soest method, the vacuum leads directly from the Feed KMn04 23.62 0.05 5.68 0.65
aspirator to the filter crucible, while in this new H2SO4 24.88 0.52 4.94 0.05
equipment the vacuum manifold (Fig. 1, Item 1) Feed KMn04 22.94 1.29 5.52 0.89
prevents any sudden change in water pressure H2SO4 24.42 0.49 4.32 0.01
which would adversely affect the filtering sample. Std dev. KMn04 0.77 0.92
The bleed-in valve bleeds air into the manifold so H2SO4 0.33 0.11
that any change in vacuum level has to take place 0
M i s s o u r i S t a t i o n H2SO4 m e t h o d d e s c r i b e d i n t h i s
in the manifold before the filtering sample is paper.
6
affected. This permits a very gradual change in c
K M n 0 4 m e t h o d , r e f . 1.
A v e r a g e s c o n s i s t of 2 i n d e p e n d e n t a n a l y s e s o n
vacuum level on the sample. different days.
With the Van Soest method, no provisions were
made to keep samples warm during filtration. The data presented here and the routine service
This is very important because samples high in work performed in the Missouri Experiment Sta-
carbohydrates would form a starchy gel and sam- tion Chemical Laboratories show that the Hoist
ples high in salts would precipitate upon cooling filtration apparatus is fully capable of filtering
during the filtering process. Both of these condi- feeds and feces for the determination of Van Soest
tions would result in clogged fritted glass, pre- fiber, cellulose, and lignin with a high degree of
venting or impeding the filtering process, and precision. We have no other method of detergent
giving erroneously high fiber results. This diffi- fiber analysis for a comparative study but the
culty was overcome by the use of the hot water researchers for whom our service work has been
jacket (Fig. 1, Item 6). performed are highly pleased with the results
With the former method, it was very difficult obtained.
to obtain duplicate analyses that agreed because
of the filtering problems. Table 2 shows the preci- Acknowledgments
sion possible with the Hoist apparatus, with the The author is extremely grateful to C. W.
original analysis and the duplicate analyses by Gehrke and W. H. Pfander for their evaluation
different operators. Table 3 shows comparative of the significance of this work and suggestions in
results for samples submitted by Van Soest. the preparation of the manuscript. Robbie Wren,
It is very important to start the filtration Glassblowing Service, University of Missouri,
process at a very low vacuum and increase it as Columbia, is also to be commended and thanked
needed to maintain a continuous flow of filtrate for his work in the construction of the model
through the fritted glass. apparatus.

Contribution from the Missouri Agricultural Experiment This paper was presented at the 86th Annual Meeting of the
Station, Journal Series No. 6792. Approved by the Director. AOAC, Oct. 9-12, 1972, at Washington, D.C.
1356 JOURNAL OP THE AOAC (Vol. 56, N o . 6, 1973)

T a b l e 2. Precision of a c i d - d e t e r g e n t f i b e r ( A D F ) and n e u t r a l - d e t e r g e n t f i b e r ( N D F ) a n a l y s e s
with Hoist a p p a r a t u s

NDF + residual ash ADF + I gnin (H2S04) ADF+silica

Lig- Sili-
Wt, NDF, Ash, Wt, ADF, nin, Wt, ADF, ca,
Sample g % % Sample g % % Sample g % %
Feces 1A° 0.5000 58.2 2.7 Feces 6A 1.0000 45.0 10.1 Feces 11A 1.0000 44.4 7.1
IB6 0.5000 58.1 2.9 6B 1.0000 44.6 9.7 11B 1.0000 44.3 6.9

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Feces 2A 0.5000 65.9 1.7 Feces 7A 1.0000 44.0 11.7 Feces 12A 1.0000 44.5 5.9
2B 0.5000 65.3 2.0 7B 1.0000 44.0 11.5 12B 1.0000 44.4 5.8

Orts 3A 0.5000 70.3 1.7 Orts 8A 1.0000 33.8 4.8 Feces 13A 1.0000 44.0 4.9
3B 0.5000 69.0 1.8 8B 1.0000 33.7 5.2 13B 1.0000 44.1 5.2

Feed 4A 0.5000 52.7 1.4 Orts 9A 1.0000 53.3 12.4 Orts 14A 1.0000 39.5 1.9
4B 0.5000 52.5 1.5 9B 1.0000 53.4 12.3 14 B 1.0000 39.4 1.7
Feed 5A 0.6226 0.0 0.0 Feed 10A 1.0000 32.3 4.7 Feed 15A 1.0000 33.9 3.2
5B 3.0172 0.4 0.1 10 B 1.0000 33.0 4.9 15B 1.0000 33.6 3.0

a
A l l A s a m p l e s w e r e a n a l y z e d by t h e a u t h o r a n d w e r e t h e o r i g i n a l a n a l y s e s of a l a r g e g r o u p of s a m p l e s s u b m i t t e d
to t h e Station Laboratory.
b
A l l B s a m p l e s w e r e a n a l y z e d by S t u d e n t A s s i s t a n t V. W o l f a p p r o x i m a t e l y 10 d a y s l a t e r as n o r m a l p r o c e d u r e f o r
r e - a n a l y z i n g 10% of s a m p l e s t o c h e c k o r i g i n a l a n a l y s e s .

T a b l e 3. C o m p a r a t i v e results for a c i d - d e t e r g e n t fiber ( A D F ) and n e u t r a l - d e t e r g e n t fiber ( N D F )

of s a m p l e s s u b m i t t e d by V a n Soest, Cornell University 1 1

ADF Lignin (KM n 0 4 ) NDF

6 c
Sample Hoist Va n Soest Hoist Va n S o e s t Hoist Ve n S o e s t

Alfalfa 35.9 36.2 12.2 12.2 49.6 48.3

Orchard grass 40.0 40.2 — — 67.5 66.7
Wheat straw 56.6 56.1 — — 81.1 78.8
Timothy 46.2 47.6 10.3 11.5 76.8 75.2
Barley straw 56.7 54.6 11.6 11.3 85.7 81.1
Soybean oil m e a l 6.6 6.1 1.8 1.8 7.6 6.6

0
T h i s w a s n o t r u n as a c o l l a b o r a t i v e s t u d y a s we h a d v e r y l i t t l e i n f o r m a t i o n as t o h o w V a n Soest s a m p l e s w e r e
h a n d l e d in h i s l a b o r a t o r y .
6
S a m p l e s f i l t e r e d w i t h t h e new filter a p p a r a t u s .
c
A n a l y s i s s u b m i t t e d by V a n S o e s t .

REFERENCES (3) Van Soest, P. J., & Wine, R. H. (1967) Determi-

(1) Goering, H. K., & Van Soest, P. J. (1970) Forage
Fiber Analysis, Agricultural Handbook 379, U.S.
Department of Agriculture, Washington, D.C.
(2) Van Soest, P. J., & Wine, R. H. (1966) Use of
Detergents in Analysis of Fiberous Feeds IV, Ani-
mal Husbandry Research Division, U.S. Depart-
ment of Agriculture, Beltsville, Md.
nation of Lignin and Cellulose in Acid-Detergent
Fiber with Permanganate, Animal Husbandry
Research Division, U.S. Department of Agrieul-
ture, Beltsville, Md.
(4) Crampton, E. W., & Maynard, L. A. (1938) J.
Nutr. 15, 383-395
(5) Van Soest, P. J. (1973) J AOAC 56, 781-784