LABORATORY CATALOGUE for milk analysis - Funke

Transcription

LABORATORY CATALOGUE for milk analysis - Funke
LABORATORY
CATALOGUE
for milk analysis
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We look forward to working with you!
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CONTENTS
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A detailed description by graduate chemist Alfred Toepel
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Determination of fat content in cream, ice cream, cheese, butter, milk powder, etc.
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:[j[hc_dWj_ede\\WjYedj[djXkjohec[j[h The butyrometer – an overview of the entire product spectrum
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:[j[hc_dWj_ede\\WjYedj[djWYY[iieh_[i Implements and utensils used in the determination of fat content
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and operation of a Gerber centrifuge
K. Schaefer, graduate engineer, reports
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One of the main focuses of Funke - Dr. N. Gerber Labortechnik GmbH
K. Schaefer, graduate engineer, W. Spindler, graduate physician
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TRADITION
PROGRESS
CONTINUITY
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Partners in dairy farming since 1904
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PRODUCTS:
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j^[\ebbem_d][gk_fc[djWdZWYY[iieh_[imehbZm_Z[0
6aaZfj^ebZciVcYVXXZhhdg^Zh[dgi]Z„Gerber method of determining
fat content“/Y[djh_\k][i"mWj[hXWj^i"h[WZ_d]bWcfi"Xkjohec[j[hi
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Founded: 1904
Managing director:
Graduate engineer Konrad Schaefer
Authorised signatory:
graduate economist Georg Hoernle
Funke-Dr.N.Gerber Labortechnik GmbH
Ringstraße 42
12105 Berlin
Telephone: (+49-30) 702 006-0
Fax: (+49-30) 702 006-66
E-mail: kontakt@funke-gerber.de
Website: www.funke-gerber.de
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BUTYROMETRIC DETERMINATION
OF FAT CONTENT ACCORDING
TO GERBER’S METHOD
by graduate chemist Alfred Toepel
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YjXZYWZilZZci]Z[ViVcYi]ZVX^Yhdaji^dc#I]Z[ViXdciZci
d[i]Zb^a`XVcWZgZVYd[[VhVbVhheZgXZciXdciZcidci]Z
WjingdbZiZghXVaZ#
APPLICATION
I]^hegdXZhhXVcWZjhZY[dgjcigZViZYVcYeVhiZjg^oZYb^a`l^i]V[ViXdciZcid[%"&+[dgb^a`l]^X]XdciV^chVhj^iVWaZ
egZhZgkVi^kZVhlZaaVh[dg]dbd\Zc^oZYb^a`#
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
&(
CHEMICALS NEEDED
Ikbf^kh_YWY_Z">(IE*
GZfj^gZbZcih/
9Zch^inVi'%•8
&!-&-¥%!%%(\eZgba Ä&
=VoVgYhnbWda/
=VoVgYgVi^c\/
8'G(*
H'"'+"(%
• colourless or only slightly
discoloured and free from
any substances which might
influence the outcome
EaZVhZcdiZ/
The required density corresponds to 90 to 91 % by mass. Stronger or weaker
concentrations are to be avoided. At 65°C, more highly concentrated sulphuric acid
attacks the amyl alcohol, producing olefins through dehydration which influence the
result. Weaker concentrations reduce the oxidization effect. Destruction of the fat
globule coating is incomplete which can lead to the formation of lumps.
7cobWbYe^eb
;dgi]ZYZiZgb^cVi^dcd[[ViXdciZciVXXdgY^c\id<ZgWZgÉhbZi]dY
An isomer mixture of 2-methylbutane-1-ol and 3-methylbutance-1-ol
GZfj^gZbZcih/
9Zch^inWZ^'%•8
%!-&&¥%!%%(\ba Ä&
• Boiling boundary: 98 % (by volume)
has to distil at between 128°C and
132°C at 1 bar.
• The amyl alcohol must not contain
any substances which could
influence the result.
• A substitute for amyl alcohol can
be used provided that it will bring
about the same test results as
would be achieved with amyl
alcohol.
=VoVgYhnbWda/
=VoVgYgVi^c\/
McG&%"'%
H')$'*
KW;6>>
EaZVhZcdiZ/
• The isomers of amyl alcohol have different boiling points: 2-methylbutane-1-ol
at 128°C and 3-methylbutane-1-ol at 132°C.
• Of the 8 known isomers of amyl alcohol, only this mixture is suitable for the
Gerber method.
• Contamination with other isomers of amyl alcohol, particularly with the
tertiary amyl alcohol 2-methylbutane-2-ol, produces false results.
The obtained fat content result is too high.
&)
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
REQUIRED EQUIPMENT
&#8Va^WgViZYWjingdbZiZgl^i]hj^iVWaZhideeZg^cVXXdgYVcXZl^i]
9>C&'-(+"6)!9>C&'-(+"6+!9>C&'-(+"6-!9>C"&'-(+"6*
'#F_f[jj[9>C&%'-("e\ehc_badgf_f[jj[9>C&'-(,"6[dgb^a`
(#F_f[jj[9>C&'-(,"7dg&%bac[Wikh_d]jWf[dgikbf^kh_YWY_Z
)#F_f[jj[9>C&'-(,"8\eh'cbWcobWbYe^eb
*#9[djh_\k][\ehZ[j[hc_d_d]\WjYedj[dj_dc_ba"]ZViVWaZ!l^i]gebXdjciZg#
L]Zc jhZY jcYZg V [jaa adVY! i]^h XZcig^[j\Z bjhi WZ XVeVWaZ d[ egdYjX^c\ V
XZcig^[j\Va [dgXZ d[ (*% ¥ *% \ dc i]Z ^ch^YZ d[ i]Z WjingdbZiZg hideeZg l^i]^c
'b^cjiZhVii]Zbdhi#L^i]VgdiVi^dcgVY^jhd[Z#\#'+¥%!*Xbjeidi]Z^ch^YZd[
i]ZWjingdbZiZghideeZg!l]^X]^hi]ZY^hiVcXZWZilZZci]Zed^cid[idgfjZVcYi]Z
WjingdbZiZghideeZg!i]^hXZcig^[j\VaVXXZaZgVi^dc^hgZVX]ZYViVgdiVi^dcheZZY
d[&&%%¥-%b^cÄ&#
+#IZbeZg^c\YZk^XZh[dgWjingdbZiZgh!Z#\#V+*¥'•8lViZgWVi]
L^i]V]ZViZYXZcig^[j\Z!VXZcig^[j\ZWjh]^c\XVcWZjhZYidViiVX]i]ZWjingdbZiZg
^cidi]ZlViZgWVi]#I]ZgZVY"d[[iZbeZgVijgZbjhiWZ+*¥'•8#
PREPARATION OF THE TEST SPECIMEN
I]Zb^a`^ci]ZheZX^bZcWdiiaZ^h]ZViZYjeid'%•8VcYi]dgdj\]anb^mZYi]gdj\]
\ZciaZh]V`^c\#I]^h^hYdcZidWg^c\VWdjiVcZkZcY^hig^Wji^dcd[[ViVcYidegZkZci
[gdi]^c\VcYi]Z[dgbVi^dcd[WjiiZg#
Milk fat is lighter than water and creams if it is left standing. A fat-rich layer accumulates on the surface. Stirring and careful shaking restore the original distribution.
>[i]ZaVnZgd[XgZVbXVccdiWZZkZcanY^hig^WjiZY^ci]^hlVn!i]Zb^a`h]djaYWZhadlan
]ZViZY id (*")%•8 VcY \Zcian hl^gaZY VgdjcY jci^a V ]dbd\Zcdjh [Vi Y^hig^Wji^dc ^h
VX]^ZkZY#I]Zb^a`^hi]ZcXddaZYid'%•8WZ[dgZWZ^c\YgVlc^cidi]Ze^eZiiZ#
Foam breaks the fat globule coating. The milk may begin to turn into butter when stirred
and uniform distribution of fat is no longer possible.
The fat liquefies at 35-40° and the distribution process is speeded up.
6[iZgi]ZiZbeZgVijgZ]VhWZZchZi!i]Zb^a`XVchiVcY[dg(id)b^cjiZhidVaadlVcn
edX`Zihd[V^gidY^heZghZ#
The volumeters are calibrated at 20°C. Any variations in temperature will influence the
volume. Air pockets reduce the density and hence the mass of milk measured.
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
&*
CONDUCTING A TEST = WORK PROCEDURES
I]ZhVbZb^a`heZX^bZcbjhiWZiZhiZYil^XZ#
&# EaVXZ ' WjingdbZiZgh ^cid V XaVbe WjingdbZiZg hiVcY#
L^i]i]ZV^Yd[VbZVhjg^c\iVe!^cigdYjXZ&%bad[hjae]jg^XVX^Y
^cidi]ZWjingdbZiZgl^i]djilZii^c\i]ZcZX`d[i]ZWjingdbZiZg
hZZ;^\#&#
'# 8VgZ[jaan ijgc i]Z WdiiaZ l^i] i]Z b^a` heZX^bZc jeh^YZ Ydlc
i]gZZ dg [djg i^bZh# I]Zc ^bbZY^ViZan e^eZiiZ &%#,* ba d[ b^a`
^cid i]Z WjingdbZiZg ^c hjX] V lVn i]Vi i]Z WjingdbZiZg cZX`
YdZh cdi \Zi lZi VcY i]Z b^a` YdZh cdi b^m l^i] i]Z hjae]jg^X
VX^Y# Id Yd hd! aZVc i]Z i^e d[ i]Z e^eZiiZ aViZgVaan Vh YZZean
Vhedhh^WaZV\V^chii]ZlVaad[i]ZWjingdbZiZghdi]Vii]Zb^a`
[dgbhVaVnZgdcided[i]Zhjae]jg^XVX^YhZZ;^\#'#
When the Gerber method was first introduced, 11.0 ml of milk were used.
By reducing the quantity of milk 10.75 ml, the determined fat content more
closely matches the results of the reference method. If the butyrometer
neck is wetted with milk, residues may cling to it.
A clear dividing line between the acid and the milk, without a brownishcoloured edge, is the sign of good layering.
(# &bad[VbnaVaXd]da^he^eZiiZYdcidi]Zb^a`!dg^cigdYjXZY Wn
bZVchd[VbZVhjg^c\iVe#
;^\#& EgdiZXi^kZ\aVhhZhVcYgjWWZg\adkZhbjhiWZldgc
l]Zc]VcYa^c\hjae]jg^XVX^Y
Due to the low density of amyl alcohol, the two liquids do not mix.
)# I]Z WjingdbZiZg ^h hZVaZY l^i] V hideeZg l^i]dji b^m^c\ i]Z
a^fj^Yh#
As a rule, the lower end of the stopper comes into contact with the liquid.
*# I]ZWjingdbZiZg^heaVXZY^ci]ZWjingdbZiZgijWZl^i]i]ZWjaW
ed^ci^c\YdlclVgYh#H]V`Zi]ZWjingdbZiZgk^\dgdjhanjci^ai]Z
ilda^fj^YhVgZi]dgdj\]anb^mZY#@ZZendjgi]jbWÒgbanegZhhZY
Ydlcdci]ZWjingdbZiZghideeZgl]^aZYd^c\hd#Ijgci]ZWjin"
gdbZiZgjeVcYYdlchZkZgVai^bZh^cdgYZgidZcVWaZi]Zhjae]j"
g^XVX^YgZbV^c^c\^ci]ZWjaWidY^heZghZhZZ;^\#(#
When the liquids are mixed, a considerable amount of heat is given off. The
gas built up in this way can cause the
stopper to shoot out, or the butyrometer
to break.
The butyrometer tube is used as
a safety precaution. Instead of using a
butyrometer tube, the butyrometer can
be wrapped in a cloth.
<_]$(
'&$-+cbe\c_baWh[f_f[jj[Z_djej^[Xkjohe#
c[j[h
&+
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
;^\#(
I]ZWjingdbZiZg^hh]V`Zc^ci]Z
ijWZegdiZXi^kZ\d\\aZhVcY
gjWWZg\adkZhbjhiWZldgc
Too lax shaking of the butyrometer or
holding it unnecessarily in a slanted
position inhibits quick mixing and
therefore the rapid oxidation of the entire specimen, thus ruining the careful
work done layering the liquid.
;^\#) ;^aa^c\i]ZXZcig^[j\Z
;^\#* I]ZWjingdbZiZghVgZWgdj\]iidi]ZZmVXigZVY^c\
iZbeZgVijgZ^cVlViZgWVi]
+#>bbZY^ViZanV[iZgi]Zb^mijgZ]VhWZZch]V`ZcVcYijgcZYjeh^YZ
Ydlc V [Zl i^bZh! i]Z WjingdbZiZgh! hi^aa ]di VcY l^i] i]Z hide"
eZgh ed^ci^c\ YdlclVgYh! VgZ eaVXZY ^c WjX`Zih ^ch^YZ i]Z ]ZViZY
<ZgWZg XZcig^[j\Z hZZ ;^\# )! l]ZgZWn i]Z WjingdbZiZgh bjhi WZ
eaVXZYZmVXiandeedh^iZZVX]di]Zg#
7Z[dgZ]VcY! i]Z Xdajbc d[ [Vi h]djaY WZ hZi Vi i]Z ]Z^\]i d[ i]Z
ZmeZXiZYaZkZad[[ViXdciZciWnijgc^c\i]ZhideeZg#
6[iZg hZii^c\ i]Z i^bZ dc i]Z XZcig^[j\Z! i]Z XZcig^[j\Z ^h hiVgiZY#
6[iZggZVX]^c\VXZcig^[j\Va[dgXZd[(*%¥*%\!l]^X]^hgZVX]ZY
VhVgjaZV[iZg&b^cjiZ!i]ZXdggZhedcY^c\heZZYd[&&%%¥*%geb
h]djaYWZbV^ciV^cZY[dg)b^cjiZh#
I]ZXZcig^[j\ZbjhiWZÒiiZYl^i]Vc^ciZgadX`^c\a^Y#6[iZgi]Zi^bZ
hZi[dgi]ZXZcig^[j\Z]VhWZZcgZVX]ZY!i]ZgdidgWgV`Z^hVjidbVi^"
XVaanVeea^ZY#
,# I]Z WjingdbZiZgh VgZ cdl gZbdkZY [gdb i]Z XZcig^[j\Z! iV`^c\
XVgZcdiidi^aii]Zb!VcYVgZeaVXZYl^i]i]ZhideeZgh[VX^c\Ydlc"
lVgYh[dg*b^cjiZh^cVlViZgWVi]]ZViZYid+*•8hZZ;^\#*#
It is important to maintain an exact temperature so as to obtain accurate
results. Only a read-off at 65°C will ensure an exact result. If the
temperature is too low, the volume of the column is reduced and a fat
content reading that is too low will be indicated.
;^\#+ BZVhjgZYkVajZhXVcWZgZa^VWanVcYVXXjgViZangZVY
d[[l^i]i]ZV^Yd[VhV[ZingZVY^c\aVbe
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
&,
RESULT AND DEGREE OF ACCURACY
-# 6[iZggZbdk^c\i]ZWjingdbZiZg[gdbi]ZlViZgWVi]!^ih]djaYWZ]ZaYkZgi^XVaan
ViV]Z^\]il]ZgZi]ZbZc^hXjhd[i]ZXdajbcd[[Vi^hViZnZaZkZa#L^i]i]Z]Zae
d[i]ZhideeZg!bVg`i]ZYZbVgXVi^dca^cZWZilZZci]ZgZh^YjVab^mijgZVcY[Vi
dcVl]daZhjWY^k^h^dcd[i]ZWjingdbZiZghXVaZVcYgZVYd[[i]Z]Z^\]id[i]Z
[ViXdajbcVii]ZadlZhied^cid[i]ZbZc^hXjh#>[i]ZgZVY^c\iV`Zhiddadc\!i]Z
WjingdbZiZgbjhiWZeaVXZYWVX`^cidi]ZlViZgWVi]hZZ;^\h#+VcY,#
>[i]ZbZc^hXjhd[i]Z[ViXdajbc^hcdiViZnZaZkZa!VeVgVaaVmZggdggZhjaih#
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;^\#,
)!%"
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dWiV^cVbdgZVXXjgViZgZhjail^i]l]daZb^a`WjingdbZiZgh#>[i]ZbZc^hXjhidjX]Zh
i]Z\gVYjVi^dcbVg`!i]Zci]ZgZhjai^hidWZgZXdgYZYVhhjX];^\#,V#
>[ i]Z bZc^hXjh ^ciZghZXih i]Z \gVYjVi^dc bVg`! i]Zc i]Z adlZg kVajZ ^h iV`Zc
;^\#,W#
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i]Vc%#&%!^#Z#i]ZgZegdYjX^W^a^inVbdjcihid%#&%#
L]ZcgZXdgY^c\i]ZgZhjai!ndjbjhiVYYi]ZcdiZÆ[ViXdciZciVXXdgY^c\idi]Z<ZgWZg
bZi]dYÇ#
>[i]ZildheZX^bZchY^[[ZgWn%#&!i]ZbZVckVajZd[Wdi]gZVY^c\h^hiV`Zc#
HeZX^bZc&/)#'%qHeZX^bZc'/)#(%qGZhjai/)#'*[ViXdciZci
=dlZkZg!^[i]ZildgZVY^c\hVgZ )#'%VcY )#'* [ViXdciZci!i]ZadlZg kVajZ d[
)#'%^hgZXdgYZYÄdci]Zeg^cX^eaZi]Vi^i^hWZiiZgidZggdci]Zh^YZd[XVji^dc#
&-
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
:[j[hc_dWj_ede\j^[\WjYedj[dj_d^ece][d_p[Zc_baWYYehZ_d]je=[hX[hÊic[j^eZ
IgZViZYb^a`^h]dbd\Zc^oZYidVkd^YXgZVb^c\#I]^h^ckdakZhgZYjX^c\i]ZY^[[ZgZci"
h^oZY[Vi\adWjaZhidVcZVganZfjVaY^VbZiZgd[&id'b^XgdbZiZgh#I]^hXdch^YZgVWan
YZXgZVhZh i]Z hZeVgVi^c\ Z[[ZXi d[ i]Z XZcig^[j\^c\ egdXZhh# >c dgYZg id XdbeaZiZan
hZeVgViZd[[i]ZgZaZVhZY[Vi!i]ZheZX^bZcbjhiWZXZcig^[j\ZY[dgVadc\ZgeZg^dY
d[i^bZ#
EgdXZhhhiZeh&id-[dgi]ZiZhi^c\d[cdc"]dbd\Zc^oZYb^a`VgZXVgg^ZYdjiVcYi]Z
gZhjai^hgZXdgYZY#
I]Zc!i]ZWjingdbZiZg^hdcXZV\V^c]ZViZYid+*•8^cVlViZgWVi][dgViaZVhi*b^"
cjiZhVcYhjWhZfjZcianXZcig^[j\ZYV\V^c[dg*b^cjiZh#I]ZgZhjai^hgZVYd[[^ci]Z
hVbZlVnVhWZ[dgZ#
>[i]ZkVajZdWiV^cZYV[iZgi]ZhZXdcYXZcig^[j\^c\^hbdgZi]Vc%#%*]^\]Zgi]Vci]Z
kVajZV[iZgi]ZÒghiXZcig^[j\^c\!i]Zci]ZgZ]ZVi^c\VcYXZcig^[j\^c\^hidWZgZeZViZY
VbVm^bjbd[ildi^bZh#
=dlZkZg!^[i]^hkVajZ]Vh^cXgZVhZYWndcan%#%*dgaZhhl^i]gZheZXiidi]ZÒghi
kVajZ!i]Z]^\]ZhiiZhikVajZVeea^Zh#
:mVbeaZ/
• After the first centrifuging, the two values were read off at 3.55 % and 3.60 %.
• After the second centrifuging, the two values were 3.60 % and 3.65 %. The homogenised
milk fat content is stated to be 3.65 %.
• Should the difference still be greater than 0.05 % after the two last repetitions, i.e. after
the 3rd and 4th centrifuging, the results of this test are to be discarded.
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
&.
BUTYROMETRIC DETERMINATION OF THE
FAT CONTENT OF VARIOUS DAIRY PRODUCTS
FOREWORD:
The butyrometric determination of the fat content in milk has been and is
being replaced at a progressive rate by other routine tests (with appliances
such as LactoStar, for instance). However, milk products such as cheese,
ice cream, etc. either cannot be tested with such appliances or can only be
tested after elaborate specimen preparation. For these products, butyrometric methods are a good alternative for routine analysis.
1.0 FIELD OF APPLICATION
9ZiZgb^cVi^dcd[[ViXdciZci^cb^a`VcYkVg^djhYV^gnegdYjXih#
2.0 VOLUMES
JcaZhhhiViZYdi]Zgl^hZ!i]Z[daadl^c\fjVci^i^Zhd[X]Zb^XVahVcYiZhiheZX^bZch
VgZjhZY/
Hjae]jg^XVX^Y/ 6bnaVaXd]da/ B^a`dgYV^gnegdYjXi/
&%#%ba'%•8 '•8
&#%ba'%•8 '•8
&%#,*ba'%•8 '•8
3.0 BRIEF DESCRIPTION OF THE
BUTYROMETRIC DETERMINATION OF FAT CONTENT:
3.1 ... IN MILK (ACCORDING TO GERBER’S METHOD):
EZg[ZXian XaZVcZY b^a` WjingdbZiZgh! bdhi ^bedgiVcian [gZZ d[ [Vi gZh^YjZh! VgZ ÒaaZY
^ci]Z[daadl^c\dgYZg/&%bad[hjae]jg^XVX^YYZch^in/&#-&- $"%#%%(\$ba!&%#,*ba
d[b^a`!VcY&bad[VbnaVaXd]da#I]Zb^a`VcYVbnaVaXd]daVgZidWZÒaaZY^caVnZgh
hdi]Vii]ZnYdcdib^mWZ[dgZh]V`^c\#6[iZghZVa^c\i]ZWjingdbZiZg!i]ZXdciZcihVgZ
i]dgdj\]anb^mZYWnh]V`^c\VcYijgc^c\i]ZWjingdbZiZgjeh^YZYdlchZkZgVai^bZh#
I]gdj\]XVgZ[jaVY_jhibZcid[i]ZhZVa^c\hideeZg!i]ZXdciZcihd[i]ZWjingdbZiZgVgZ
gZ\jaViZY^chjX]VlVni]Vii]ZhXVaZ^h[jaaWjicda^fj^YZciZghi]ZWjaW#I]ZWjingd"
bZiZg^hXZcig^[j\ZY^ci]Z]ZViZYXZcig^[j\Z!VcYi]ZciZbeZgZY^cV+*•8lViZgWVi][dg
*b^cjiZh#I]ZY^k^Y^c\a^cZWZilZZci]Zhjae]jg^XVX^Yb^mijgZVcYi]Z[ViXdajbc^hhZi
ViV[jaahXVaZa^cZVcYi]ZjeeZgZcYd[i]Z[ViXdajbc^hgZVYd[[Vii]ZadlZgbZc^hXjh#
3.2 ... IN HOMOGENISED MILK
As above, except that the specimens are centrifuged three times, for 5 minutes each time.
In between centrifugings, the butyrometers are heated in a 65°C water bath for 5 minutes
(for more detail, see page 19).
3.3 ... IN SKIM MILK AND WHEY
Use of skim milk butyrometers with narrowed scales according to Sichler’s method.
7jingdbZiZghVgZXZcig^[j\ZYil^XZVcYeaVXZY^cV+*•8lViZgWVi][dg*b^cjiZh^c
WZilZZcXZcig^[j\^c\h#
3.4 ... IN CONDENSED MILK (UNSWEETENED)
I]ZXdcYZchZYb^a`^h]ZViZYid*%•8VcYVaadlZYidXddaV\V^c#I]Zc^i^hb^mZYl^i]
lViZg^cV&/&gVi^d#I]^hY^aji^dc^hi]ZciZhiZYa^`Zb^a`VXXdgY^c\id<ZgWZgÉhbZi]dY#
;ViXdciZci2gZVY"d[[kVajZm'#
'%
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
3.5 ... IN BUTTERMILK (MOHR AND BAUR’S MODIFICATION)
I]Z WjingdbZiZg ^h ÒaaZY l^i] &% ba d[ hjae]jg^X VX^Y YZch^in/ &#-(% $" %#%%( \$ba#
>chiZVYd[&%#,*ba!&%bad[WjiiZgb^a`VcY'#%bad[VbnaVaXd]daVgZe^eZiiZY^c#6[iZg
hZVa^c\! i]Z WjingdbZiZg ^h h]V`Zc VcY ^bbZY^ViZan XZcig^[j\ZY [dg &% b^cjiZh# I]^h
egZkZcihVccdn^c\WadX`V\Zh#I]ZgZVY^c\^hiV`ZcV[iZgiZbeZg^c\i]ZheZX^bZcVi+*•8
$"'•8#;ViXdciZci2gZVY"d[[kVajZm&#%,*#
3.6 ... IN POWDERED MILK ACCORDING TO TEICHERT’S METHOD
Use of powdered milk butyrometer according to Teichert’s method.
I]ZWjingdbZiZg^hÒaaZYl^i]&%bad[hjae]jg^XVX^YYZch^in/&#-&- $"%#%%(\$ba#,#*ba
d[lViZgVcY&bad[VbnaVaXd]daVgZaVnZgZYdcid^i#'#*\d[edlYZgZYb^a`VgZlZ^\]ZY^cV
lZ^\]^c\WdViVcYigVch[ZggZY^cidi]ZWjingdbZiZgi]gdj\]V[jccZa!jh^c\V]V^gWgjh]#6["
iZghZVa^c\!i]ZWjingdbZiZg^hi]dgdj\]anh]V`Zc!VcY^ciZgb^iiZcianeaVXZY^cV+*•8lViZg
WVi]hZkZgVai^bZh#>i^hXZcig^[j\ZYil^XZ!*b^cjiZhZVX]i^bZ!^ci]Z]ZViZYXZcig^[j\ZVcY
i]ZkVajZ^hgZVYd[[V[iZgi]ZWjingdbZiZg^heaVXZY^ci]ZlViZgWVi][dg*b^cjiZh#
3.7 ... IN CREAM ACC. TO ROEDER’S METH. (WEIGHING METH.)
Use of cream butyrometer according to Roeder’s method.
*\d[XgZVbVgZlZ^\]ZYdji^cidi]Z\aVhhWZV`Zgh^ijViZY^ci]ZhideeZgVcYigVch[ZggZY
^cidi]ZWjingdbZiZg#Hjae]jg^XVX^YYZch^in/&#*'' $"%#%%*\$ba^hedjgZYi]gdj\]i]Z
jeeZgdeZc^c\d[i]ZWjingdbZiZgjci^a^igZVX]Zh_jhidkZgi]ZjeeZgZY\Zd[i]Z\aVhh
WZV`Zg#6[iZghZVa^c\!i]ZWjingdbZiZg^heaVXZY^cV,%•8lViZgWVi]VcYh]V`ZcgZeZVi"
ZYanjci^ai]ZegdiZ^c^hXdbeaZiZanY^hhdakZY#Hjae]jg^XVX^Y^hedjgZY^cjci^a^igZVX]Zh
i]ZWZ\^cc^c\d[i]ZhXVaZ!&bad[VbnaVaXd]da^hVYYZYVcYi]ZWjingdbZiZg^hhZVaZY!
h]V`Zc!VcYeaVXZY^ci]Z,%•8lViZgWVi][dgVcdi]Zg*b^cjiZh#I]Zc!^i^hXZcig^[j\ZY
[dg*b^cjiZhVcYiZbeZgZY^cV+*•8lViZgWVi]#I]ZgZVY^c\^hiV`ZcVi+*•8!i]Z[Vi
XdajbcVY_jhiZYidi]ZoZgded^ci!i]ZkVajZgZVYd[[Vii]ZadlZgbZc^hXjh#
3.8 ... IN CREAM ACC. TO SCHULZ-KLEY’S METH. (WEIGHING METH.)
Use of cream butyrometer according to Schulz-Kley’s method.
&%bad[hjae]jg^XVX^YYZch^in/&#-&- $"%#%%(\$ba!*bad[lViZg!XV#*\d[XgZVb
bZVhjgZYWnY^[[ZgZci^ValZ^\]^c\jh^c\Vhng^c\ZdglZ^\]^c\e^eZiiZViiVX]ZYidi]Z
hXVaZ!VcY&bad[VbnaVaXd]daVgZhjXXZhh^kZan^cigdYjXZY^cidi]ZWjingdbZiZg#6[iZg
hZVa^c\!i]ZXdciZcihVgZb^mZYWnh]V`^c\VcYijgc^c\i]ZWjingdbZiZgjeh^YZYdlc
VcYXZcig^[j\ZY[dg*b^cjiZh^ci]Z]ZViZYXZcig^[j\Z#I]ZkVajZ^hgZVYd[[V[iZg*
b^cjiZhd[iZbeZg^c\^cV+*•8lViZgWVi]#CdiZ/YdcdiVaadlbdgZi]Vc&*b^cjiZh
ideVhhWZilZZcVYY^c\i]ZlViZgVcYh]V`^c\i]ZheZX^bZcYjZidi]Zedhh^W^a^ind[
VYZXgZVhZ^ci]Z]ZVid[gZVXi^dcVhVgZhjaid[i]ZVYY^i^dcd[lViZg#I]ZY^hhdaji^dc
egdXZhhbjhiWZXdbeaZiZYl^i]^c+%hZXdcYh#
;ViXdciZci2gZVY"d[[kVajZm*$XgZVbcZilZ^\]i#
3.9 ... IN CREAM ACC. TO KOEHLER’S METH. (MEASURING METH.)
Use of cream butyrometer according to Koehler’s method.
&%bad[hjae]jg^XVX^YYZch^in/&#-&- $"%#%%(\$ba!*#%*bad[XgZVb!*bad[lViZg!
VcY&bad[VbnaVaXd]daVgZedjgZY^cijgc^cidi]ZXgZVbWjingdbZiZg#L]Zcjh^c\V
XgZVbhng^c\Z!^ibjhiWZg^chZYhZkZgVai^bZhl^i]lViZgWZ[dgZi]Z*bad[lViZgVgZ
^cigdYjXZY#I]ZWjingdbZiZg^hhZVaZY!h]V`Zc!XZcig^[j\ZY[dg*b^cjiZh!VcYi]Zci]Z
kVajZ^hgZVYd[[V[iZgiZbeZg^c\i]ZheZX^bZc^cV+*•8lViZgWVi]#I]ZkVajZ^hgZVY
d[[[gdbi]ZoZgded^ci#
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
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3.10 ... IN CHEESE ACC. TO VAN GULIK’S METH. (WEIGHING METH.)
(see ISO 3433) Use of the cheese butyrometer according to Van Gulik’s method.
6[iZgedjg^c\&*bad[hjae]jg^XVX^YYZch^in/&#*'' $"%#%%*\$ba^cidi]ZKVc<j"
a^`WjingdbZiZg!XadhZYVii]ZhXVaZZcY!(\ $"%#'\d[X]ZZhZVgZVYYZYWnbZVch
d[VlZ^\]^c\WdViVcY]V^gWgjh]!VcYi]Zci]ZÒaaZgdeZc^c\^hhZVaZY#EVhinX]ZZhZ
hVbeaZhbjhiWZlZ^\]ZYdji^cidi]ZeZg[dgViZY\aVhhWZV`Zgl]^X]VXXdbeVc^Zh
i]Z KVc <ja^` WjingdbZiZg VcY ^cigdYjXZY ^cid i]Z WjingdbZiZg# I]Z hZVaZY Wjin"
gdbZiZg^heaVXZY^cV,%•8"-%•8lViZgWVi]l^i]i]ZhXVaZed^ci^c\jelVgYhVcY
h]V`ZcgZeZViZYanjci^ai]ZX]ZZhZ^hY^hhdakZY#6[iZglVgYh!&bad[VbnaVaXd]da^h
VYYZY![daadlZYWnhjae]jg^XVX^Yjci^a^iVeegdm^bViZangZVX]Zhi]Z&*bVg`d[
i]ZhXVaZ#I]ZcXadhZi]ZWjingdbZiZg!b^mi]ZXdciZcih!iZbeZg[dg*b^cjiZh^cV
+*•8lViZgWVi]!VY_jhii]Z[ViXdajbcidi]ZoZgded^ciVcYgZVYd[[i]ZVWhdajiZ[Vi
XdciZci#I]ZgZVY^c\^hiV`Zc[gdbi]ZadlZgZcYd[i]ZbZc^hXjh#
3.11 ... IN ICE CREAM ACC. TO KOEHLER’S METH.
(MEASURING METH.)
Use of the ice cream butyrometer according to Koehler’s method.
6cn^X^c\dggdj\]eVgi^XaZhZ#\#[gj^i!ZiX#bjhiWZgZbdkZY#I]Z^XZXgZVb^h
i]dgdj\]anb^mZYV[iZg^i]VhgZVX]ZYgddbiZbeZgVijgZ0edhh^WaZV^gedX`ZihXVc
WZVabdhiXdbeaZiZangZbdkZYWnZkVXjVi^dc#
&% b d[ hjae]jg^X VX^Y YZch^in/ #-&- $" %#%%( \$ba! * ba d[ ^XZ XgZVb! * ba d[
lViZg!VcY&bad[VbnaVaXd]daVgZ^cigdYjXZY^cijgc^cidi]Z^XZXgZVbWjingdbZiZg#
L]Zc jh^c\ V hng^c\Z! ^i bjhi WZ g^chZY hZkZgVa i^bZh l^i] lViZg WZ[dgZ i]Z * ba
d[lViZgVgZ^cigdYjXZY#H]djaYi]ZWjingdbZiZgegdkZidcdiWZhj[ÒX^Zcian[jaa!je
id ' ba d[ lViZg XVc WZ VYYZY# I]Z WjingdbZiZg ^h hZVaZY! h]V`Zc! XZcig^[j\ZY [dg
*b^cjiZh!VcY!V[iZgiZbeZg^c\^cV+*•8lViZgWVi][dg*b^cjiZh!i]ZkVajZ^hiV`Zc#
3.12 ... IN ICE CREAM ACC. TO ROEDER’S METH. (WEIGHING METH.)
Use of ice cream butyrometer according to Roeder’s method.
*\d[lZaa"b^mZY^XZXgZVbVgZlZ^\]ZYdji^cidi]Z\aVhhWZV`Zgh^ijViZY^ci]Z
hideeZg VcY igVch[ZggZY ^cid i]Z WjingdbZiZg# Hjae]jg^X VX^Y YZch^in/ &#*'' $"
%#%%*\$ba^hedjgZYi]gdj\]i]ZjeeZgdeZc^c\d[i]ZWjingdbZiZgjci^a^igZVX]Zh
_jhi dkZg i]Z jeeZg ZY\Z d[ i]Z \aVhh WZV`Zg# 6[iZg hZVa^c\! i]Z WjingdbZiZg ^h
eaVXZY^cV,%•8lViZgWVi]VcYh]V`ZcgZeZViZYanjci^ai]ZegdiZ^c^hXdbeaZiZan
Y^hhdakZY#&bad[VbnaVaXd]da^hVYYZY!VcYi]Zchjae]jg^XVX^Y^hedjgZY^cjci^a
^i gZVX]Zh i]Z &% bVg` dc i]Z hXVaZ# I]Z WjingdbZiZg ^h hZVaZY! h]V`Zc! VcY
eaVXZY^ci]Z,%•8lViZgWVi][dgVcVYY^i^dcVa&%b^cjiZh#9jg^c\i]^hi^bZ!i]Z
WjingdbZiZg^hh]V`ZcVigZ\jaVg^ciZgkVah#I]^hegdXZhh^h[daadlZYWn,b^cjiZhd[
XZcig^[j\^c\VcYiZbeZg^c\^cV+*•8lViZgWVi]#I]ZkVajZ^hiV`ZcVi+*•8!i]Z[Vi
XdajbcVY_jhiZYidi]ZoZgded^ci#I]ZkVajZ^hgZVYd[[Vii]ZadlZgbZc^hXjh#
3.13 ... IN BUTTER ACC. TO ROEDER’S METH. (WEIGHING METH.)
Use of butter butyrometer according to Roeder’s method.
*\d[WjiiZgVgZlZ^\]ZYdji^cidi]Z\aVhhWZV`Zgh^ijViZY^ci]ZhideeZgVcYigVch[ZggZY
^cidi]ZWjingdbZiZg#Hjae]jg^XVX^YYZch^in/&#*'' $"%#%%*\$ba^hedjgZYi]gdj\]i]Z
jeeZgdeZc^c\d[i]ZWjingdbZiZgjci^a^igZVX]Zh_jhidkZgi]ZjeeZgZY\Zd[i]Z\aVhh
WZV`Zg#6[iZghZVa^c\!i]ZWjingdbZiZg^heaVXZY^cV,%•8lViZgWVi]VcYh]V`ZcgZeZVi"
ZYanjci^ai]ZegdiZ^c^hXdbeaZiZanY^hhdakZY#Hjae]jg^XVX^Y^hedjgZY^cjci^a^igZVX]Zh
i]ZWZ\^cc^c\d[i]ZhXVaZ![daadlZYWn&bad[VbnaVaXd]da#I]ZWjingdbZiZg^hhZVaZY!
h]V`Zc!VcYeaVXZY^ci]Z,%•8lViZgWVi][dgVcVYY^i^dcVa&%b^cjiZh#I]^hegdXZhh^h
[daadlZYWn*b^cjiZhd[XZcig^[j\^c\VcYVeegdm^bViZan*b^cjiZhd[iZbeZg^c\^cV+*•8
lViZgWVi]#I]ZkVajZ^hgZVYd[[Vi+*•8Vii]ZadlZgbZch^Xjh#
''
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
3.14 ... IN MAYONNAISE ACC. TO ROEDER’S METH. (WEIGHING METH.)
Use of butter butyrometer according to Roeder’s method.
&\d[bVndccV^hZ^hlZ^\]ZYdji^cid\aVhhWZV`Zgh^ijViZY^ci]ZhideeZgVcYigVch"
[ZggZY ^cid i]Z WjingdbZiZg# Hjae]jg^X VX^Y YZch^in/ &#*'' $" %#%%* \$ba ^h edjgZY
i]gdj\]i]ZjeeZgdeZc^c\d[i]ZWjingdbZiZgjci^a^igZVX]Zh_jhidkZgi]ZjeeZgZY\Z
d[i]Z\aVhhWZV`Zg#6[iZghZVa^c\!i]ZWjingdbZiZg^heaVXZY^cV,%•8lViZgWVi][dg(%
b^cjiZhVcYh]V`ZcgZeZViZYanjci^ai]ZegdiZ^c^hXdbeaZiZanY^hhdakZY#Hjae]jg^XVX^Y
^hedjgZY^cjci^a^igZVX]Zhi]ZWZ\^cc^c\d[i]ZhXVaZ![daadlZYWn&bad[VbnaVaXd]da#
I]ZWjingdbZiZg^hhZVaZY!h]V`Zc!VcYeaVXZY^ci]Z,%•8lViZgWVi][dgVcVYY^i^dcVa
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bZc^hXjh#I]ZgZVY"d[[kVajZ^hbjai^ea^ZYWn*iddWiV^ci]ZXdggZXi[ViXdciZci#
3.15 BUTYROMETRIC DETERMINATION OF THE FAT CONTENT OF
MEAT AND SAUSAGE ACC. TO GERBER’S METHOD (VAN GULIK)
According to the recommended methodology of “Pohja and Associates“.
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QUIET OPERATION
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C2
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whereby:
R = effective horizontal radius in mm;
N = revolutions per minute [min-1].
SYNOPTICAL TABLE OF THE DEPENDENCE OF G-FORCE AND RPM
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**
KJELDAHL’S NITROGEN DETERMINATION METHOD
Anna Politis, graduate engineer of nutrition technology and of biotechnology, reports
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The addition of potassium sulphate serves to increase the boiling temperature of the sulphuric acid and the addition of copper sulphate serves as an
oxidation catalyst. They are also available as Kjeldahl tabs (art. no. 4230/4231).
If the process is executed with tabs, then 5± 0.1 g of milk are mixed with
20 ml of sulphuric acid and 2 Kjeldahl tabs and left to sit for 5 min. Then the
temperature program can be carried out.
During the heating of the sample, foam is not allowed to climb higher
then 4 - 5 cm below the flask opening.
The sulphuric acid is added in such a way that any copper sulphate
solution, potassium sulphate or milk which may have adhered to the flask
neck is flushed down. If the flask is sealed airtight, it can also be stored
for later digestion.
To determine the specific digestion time, it is advisable to execute
preliminary tests with samples high in protein and fat.
Substantial crystallisation is a sign of too little sulphuric acid and can
lead to low protein values. It is therefore advisable to reduce the loss of
sulphuric acid by minimising the amount sucked.
Before the hot digestion flasks can be taken from the digestion block, it
must be ensured that no condensed fluid has collected in the extraction
apparatus. If it has, the suction volume must be increased and the
condensed liquid removed.
The undiluted digestion should not be stored in the flask for a long
period of time (overnight) for any reason. There is a risk that the sample
will solidify and it is difficult to bring it into solution form again. After
the sample is cooled down and dilluted with 70 ml of water, there is no
problem to keep it overnight.
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*,
KJELDAHL’S NITROGEN DETERMINATION METHOD
2
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6cdi]Zgejh]X]Vc\Zhi]ZkVajZVcYVÒcVaejh]hVkZh^i#
I]ZY^hi^aaVi^dcVeeVgVijhbjhiWZYZ\VhhZY^[^i]VhcdiWZZcjhZY[dgVadc\
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^h]ZaYYdlcjci^alViZggjch^cidi]ZY^\Zhi^dcVeeVgVijh#CZmi!ÆCVD=Ç^h
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kZhhZa#;^cVaan!i]ZbZcjÆZmigVXi^dcEgdÇ^hhZaZXiZYWnejh]^c\ÆcZmiÇVcY
i]ZdeZgVi^c\`cdW^hejh]ZYYdlcjci^ai]ZX]Zb^XVahVgZhjX`ZY[gdb
i]ZY^\Zhi^dckZhhZa#I]ZVZgVi^dcegdXZhh^hcdlÒc^h]ZY#
6 ig^Va gjc l^i]dji V hVbeaZ bjhi WZ ZmZXjiZY YV^an WZ[dgZ WZ\^cc^c\ i]Z
Y^hi^aaVi^dcegdXZhh#IdYdi]^h!VY^hX]Vg\Z]dhZ^h^cigdYjXZY^cidVcZbein
Y^\Zhi^dckZhhZa!i]ZbV^cbZcjÆdei^dchÇVcYi]ZcÆY^gZXi^cejiÇVgZhZ"
aZXiZY#I]Zc!ÆkVedjgÇ^hX]dhZc#7nfj^X`anejh]^c\i]ZdeZgVi^c\Wjiidc
V\V^c!i]ZkVedjgY^hX]Vg\Z^hWZ\jc#GZcZlZYejh]^c\d[i]ZWjiidcZcYh
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^ci]Z:gaZcbZnZgÓVh`#;^cVaan!ÆZmigVXi^dcEgdÇ^hhZaZXiZYVcYi]ZdeZgVi"
^c\ Wjiidc ^h ejh]ZY Ydlc jci^a i]Z lViZg ^h ZmigVXiZY [gdb i]Z Y^\Zhi^dc
kZhhZa#
6[iZgYZ\Vh^c\VcYi]ZiZhigjc!i]ZY^hi^aaVi^dcd[i]ZhVbeaZ^hXVgg^ZYdji#
6*%%ba:gaZcbZnZgÓVh`[dgi]ZWdg^XVX^Yhdaji^dc^heaVXZYjcYZgi]Z
Y^hi^aaVi^dcVeeVgVijhdjiaZie^eZ#L^i]i]ZÆhiVgiÇbZcjdei^dc!i]ZY^hi^aaV"
i^dcegdXZhh^hWZ\jc#>i^hgZXdbbZcYVWaZidgjci]Z[daadl^c\Y^hi^aaVi^dc
egd\gVb/
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9^hi^aaVi^dci^bZ/*b^c
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I]Z kVedjg Y^hi^aaVi^dc ^h WZ\jc VcY i]Z Vbbdc^V! gZaZVhZY i]gdj\] i]Z
VYY^i^dc d[ hdY^jb ]nYgdm^Y! ^h Y^hi^aaZY l^i] kVedjg# I]Z Y^hi^aaViZ ^h
VWhdgWZY ^c i]Z Wdg^X VX^Y hdaji^dc '#+# 6[iZg i]Z Y^hi^aaVi^dc egd\gVb
iZgb^cViZh! i]Z Y^\Zhi^dc ÓVh` ^h gZbdkZY [gdb i]Z VeeVgVijh! i]Z
Y^hi^aaVi^dc]dhZ^hÓjh]ZYl^i]Y^hi^aaZYlViZgVcYi]Z:gaZcbZnZgÓVh`
XdciV^c^c\i]ZhVbeaZ^hVahdgZbdkZY[gdbi]ZVeeVgVijh#
*-
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9dcdiidjX]VcneVgihd[i]ZY^hi^aaVi^dc
VeeVgVijhZ^i]ZgYjg^c\VY^hi^aaVi^dcdg
[dgVl]^aZV[iZg#
I]ZnXdjaYWZ]di#
The water distiller must be set up on a stable
laboratory bench with an even, horizontal
support which is located near a cold water supply and a drain. The water pressure
must be at least 0.5 bar.
Before starting the operation, all hoses
must be connected and the coolant engaged. The storage tank must be correctly
positioned and the fluid level checked. The
water vapour discharge hose must be introduced into the digestion flask. The water
distiller is equipped with a safety gate.
During the first distillation, the water vapour comes into contact with cold pipes
and glass parts. This leads to increased
build-up of condensation which can in turn
lead to excessive sample dilution and
liquid volume in the digestion vessel.
A trial run is therefore essential. The discharge of water vapour with a temperature
of approx. 106°C creates loud noises. This
is no cause for alarm.
The distillation is conducted until a distillation volume of 150 ml is obtained.
About 2 minutes before the end of the distillation, the Erlenmeyer flask is lowered
in such a way that the end of the discharge
pipe is no longer submerged in the acid
solution. The pipe must be flushed with
water. This water is collected in the Erlenmeyer flask.
3
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XdadgVi^dcVg^hZh#I]ZkdajbZd[i]Z]nYgdX]adg^XVX^YXdc"
hjbZY^hgZVYd[[dci]ZWjgZiiZVi%#%*ba#6c^aajb^cViZY
Y^hX XVc hZgkZ Vh V cZjigVa WVX`\gdjcY VcY ZcVWaZh i]Z
jhZgidYZiZgb^cZi]ZXdadjgX]Vc\ZVXXjgViZanVii]ZZcY
d[i]Zi^igVi^dc#
The mixture of methyl red and bromcresol green (see 2.5,
2.6) serves as the indicator. The indicator is responsible for
the colour change and signals the end of the titration.
The neutral background improves the accuracy and
reproducibility of the results. This means that the titrations
are always carried out under optical conditions that are as
similar to each other as possible.
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VX^YXdchjbZYYjg^c\i^igVi^dc^hgZXdgYZY#
The blind trial is important for the calculation of the
nitrogen content of the sample.
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ZfjVi^dc/
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i^igVi^dcd[i]ZhVbeaZ
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9i0i]ZZmVXibdaVg^ind[i]Z]nYgdX]adg^XVX^Y!\^kZcid
[djgYZX^bVaeaVXZh
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%#&\gVb
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kVajZbjhiWZbjai^ea^ZYWn+#(-#
CeZ[bYWbYkbWj_ed
>[i]Z@_ZaYV]aYZiZgb^cVi^dcn^ZaYhVc^igd\ZcXdciZcid[
**!VegdiZ^cXdciZcid[(#*gZhjaih**m+#(-#
Kjeldahl’s digestion method is not specific to amino acids
and proteins and includes all organically bonded nitrogen.
Other non-protein compounds are also are digested and
collected (NPN: non-protein nitrogen). However, the proportion of these compounds is very small and is disregarded
in the calculation.
If the non-protein containing nitrogen should also be established, then method must be executed in accordance
with DIN EN ISO 8968-4. If only the protein nitrogen should
be determined, then the milk proteins must first be separated. 5±0.1 ml of milk diluted with 5±0.1 ml of water is
washed in stages with in total 60 ml of 15 % (w/v) trichloroacetic acid in accordance with DIN EN ISO 8968-5, the
proteins are precipitated and finally filtered out into a hard
paper filter. The filtrate contains the components of the
non-protein nitrogen and the filtered-out precipitate contains the protein nitrogen. The filter with the precipitate is
put into a digestion vessel and Kjeldahl’s nitrogen determination method is carried out as described above. The
protein content is calculated by multiplying by a factor of
6.38.
The value 6.38 is specific to milk and dairy products and was
established because milk proteins have a nitrogen content
of 15.65 % (100:15.65 = 6.38).
AVWdgVidgnXViVad\jZ[dgb^a`VcVanh^h
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KJELDAHL’S NITROGEN DETERMINATION METHOD
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* b^cjiZh VgZ VaadlZY id eVhh VcY i]Zc * ba d[ (% ]nYgd\Zc
eZgdm^YZVgZVYYZYVii]Zh^YZd[i]ZÓVh`#I]ZhVbeaZ^haZ[iid
h^i [dg &%"&* b^cjiZh WZ[dgZ Y^\Zhi^dc# I]Z ]ZVi^c\ WadX` ^h
egZ]ZViZY id )%%•8 [dg &% b^cjiZh VcY i]Z hVbeaZ ^h ]ZViZY Vi
)%%•8 [dg +% b^cjiZh# 6[iZglVgYh! i]Z hVbeaZ ^h XddaZY id gddb
iZbeZgVijgZVcYY^ajiZYl^i]*%bad[lViZg#**bad[(%CVD=
VcY*%bad[)Wdg^XVX^YVgZjhZYidVWhdgWi]ZY^hi^aaViZ#=8A
%#%*B^hjhZY[dgi^igVi^dc#%#'bad[Vb^mijgZd[%#%(bZi]na
gZY VcY %#&, WgdbXgZhda \gZZc ^c .* Zi]Vcda hZgkZh Vh i]Z
^cY^XVidg#
Caution! The addition of hydrogen peroxide
causes an intense reaction.
The blind trial is executed with 2 ml of water
and 0.25 g of sucrose. The effectiveness of the
decomposition is tested with 0.08 g of tryptophan
or 0.06 g of lysine hydrochloride.
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jb hjae]ViZ PC=)'HD)R VcY %#-* \ d[ hjXgdhZ VgZ jhZY ]ZgZ#
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l^i] cdgbVa hVbeaZh VcY i]Z eZgXZciV\Z d[ c^igd\Zc XdciZci
bjhiWZWZilZZc..#%VcY&%%#I]ZYZiZgb^cVi^dcl^i]Vb"
bdc^jb hjae]ViZ ^h d[ jhZ ^c YZiZXi^c\ c^igd\Zc adhhZh Yjg^c\
YZXdbedh^i^dcdgY^hi^aaVi^dcVcYY^[[ZgZcXZh^cXdcXZcigVi^dch^c
i]Zi^igVi^dcV\Zci#
In order to monitor the effectiveness of the decomposition, 0.18 g of tryptophan or 0.16 g or
lysine hydrochloride and 0.67 g of sucrose are
used. 98 % of the nitrogen content must be recovered. If that is not the case, either the decomposition temperature or time is insufficient or the
sample is charred.
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pH VALUE MEASUREMENT
Anna Politis, graduate engineer of nutrition technology and of biotechnology, reports
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To clean off fat or oil deposits, the membrane must be degreased with cotton which has
been soaked in acetone or soap solution.
If protein has settled on the diaphragm, the electrode is soaked in HCI/Pepsin solution for
approx. 1-2 hours.
In case of a silver sulphide contamination, the electrode is to be set in a thiocarbamide
solution and left to soak.
To remove inorganic films, the electrode is dipped into 0.1 M HCl or 0.1 M NaOH. With
40-50°C solutions, cleaning is more effective.
After every cleaning procedure, the electrode is to be set in a 3M KCl solution about a
quarter of an hour a new conditioning and subsequently calibrated once again.
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FREEZING POINT DETERMINATION
DcZd[i]ZbV^c[dXjhZhd[;jc`Z"9g#C#<ZgWZgAVWdgiZX]c^`<bW=
K. Schaefer, graduate engineer, W. Spindler, graduate physician report
HISTORY
The German chemist Beckmann, known for the thermometer named after him, began
using the freezing point of milk in as early as 1895 to detect if it had been adulterated
with water. The American Hortvet worked intensively with this method in 1920 and improved some of its essential features. The first thermistor cyroscopes were brought
to the market in the 1960s. However, they had to be operated entirely by hand. At the
beginning of the 1970s, the first automatic thermistor cyroscopes became available.
With this development it was possible to determine the freezing point automatically at
the push of a button.
A decisive step in the improvement of thermistor cryoscopy was displayed at the “FoodTec” tradeshow in
1984: Funke-Gerber introduced the first device with
automatic calibration. This successful and intensive
development work reached a new peak at the “FoodTec” in 1988, where Funke-Gerber presented a fully
automatic freezing point determination mechanism
with a capacity of 220 samples per hour.
With the introduction of an indirect freezing point
measurement device (e.g. LactoStar) for routine
analysis, interest was focused primarily on reference
devices which are able to determine freezing points
in accordance with the applicable standards and
regulations. These devices must satisfy the strictest
requirements with regard to measuring accuracy.
For this reason Funke-Gerber developed a programmable cryoscope with a resolution of 0.1 m °C. This
instrument has proven its accuracy and reliability in
countless laboratories all over the world. The product
range has been expanded with a multi-sample device
(CryoStarautomatic). Since January 2007, these instruments have been equipped with a graphic colour display. This makes it possible to show the entire freezing
curve, in particular the process of the plateau search,
with a patented screen presentation.
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