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Ano de constituição: 1904
Gerente:
Eng.º Konrad Schäfer
Procurador:
Dipl. oec. Georg Hörnle
Funke-Dr.N.Gerber Labortechnik GmbH
Ringstraße 42
12105 Berlin
Telefone: (+49-30) 702 006-0
Fax: (+49-30) 702 006-66
E-Mail: [email protected]
Sítio: www.funke-gerber.de
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PRINCÍPIO DO MÉTODO
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ÂMBITO DE APLICAÇÃO
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PRODUTOS QUÍMICOS NECESSÁRIOS
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• incolor ou apenas
ligeiramente tingido e
isento de componentes que
influenciem o resultado
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A densidade necessária corresponde a 90 até 91 % em massa. Devem ser evitadas
concentrações mais elevadas ou reduzidas. O ácido sulfúrico mais concentrado
ataca, aos 65 °C, o álcool amílico e forma olefinas através da desidratação, o
que influencia os resultados. Concentrações mais reduzidas baixam a acção de
oxidação. A destruição do invólucro das esferas de gordura é incompleta e poderá
haver a formação de grumos.
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Mistura de isómeros 2-metilbutan-1-ol e 3-metilbutan-1-ol
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• Limites de ebulição: 98 %
(em percentagem volumétrica)
têm de sobredestilar entre 128 °C e
132 °C a 1 bar.
• O álcool amílico não pode conter
componentes que influenciem o
resultado.
• Em vez de álcool amílico poderão
ser usados materiais de
substituição, desde que levem
a resultados de teste iguais aos
do álcool amílico.
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• Os álcoois amílicos isómeros possuem pontos de ebulição diferentes,
2-metilbutan-1-ol 128 °C e 3-metilbutan-1-ol 132 °C.
• Apenas esta mistura entre os 8 álcoois amílicos isômeros conhecidos
é adequada para o método Gerber.
• As contaminações com os outros álcoois amílicos isómeros, em especial com
o álcool amílico terciário 2-metilbutan-2-ol alteram os resultados das análises.
É detectado um teor butiroso demasiado elevado.
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EQUIPAMENTOS NECESSÁRIOS
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PREPARAÇÃ O DA AMOSTRA
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[dgbVdYZbVciZ^\V#
A gordura do leite é mais leve que a água. Quando parada forma natas. À superfície
forma-se uma camada mais rica em gordura. Através da mistura e viragem cuidadosa
é possível restabelecer o antigo estado de distribuição.
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A espuma quebra o invólucro das esferas de gordura. Durante a mistura, poderão ocorrer manifestações de formação de manteiga. Assim, a gordura já não se deixa distribuir
uniformemente. A 35 até 40°C, a gordura se liquefaz. A distribuição é mais rápida.
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Os medidores de volume estão aferidos para 20°C. Os desvios na temperatura influenciam o volume. O ar contido reduz a densidade e, assim, a massa da quantidade de leite
medida.
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EXECUÇÃO DA ANÁLISE = PRESCRIÇÃO DE TRABALHO
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Durante a introdução do método de Gerber eram introduzidos 11,0 ml de leite.
Através da redução da quantidade de leite para 10,75 ml, o teor butiroso corresponde melhor aos resultados do método de referência. Em caso do pescoço do butirómetro ficar molhado com leite poderão ficar retidos resíduos.
Um sinal de uma boa formação de camada é a linha de delimitação nítida
entre ácido e leite sem margem acastanhada.
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líquidos.
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Por regra, a parte inferior da rolha mergulha no líquido.
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Durante a mistura dos líquidos é gerado muito calor. Devido à formação de
gases, a rolha poderá ser impelida a sair
ou o butirómetro quebra.
A manga do butirómetro é um dispositivo de segurança. Em vez da manga do
butirómetro, o butirómetro também
poderá ser envolvido num pano.
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Uma agitação demasiado suave ou uma
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rápida mistura e, assim, o rápido efeito
de oxidação em todo o líquido e destrói
o efeito da formação cuidadosa das
diversas camadas.
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O cumprimento da temperatura é especialmente importante para a exactidão dos resultados. Apenas a leitura a 65 °C garante um resultado exacto.
Caso a temperatura seja inferior, o volume da coluna de gordura diminui.
É apresentado um teor butiroso demasiado baixo.
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kVadgYVeg^bZ^gVXZcig^[j\Vd!ZciddgZVfjZX^bZcidZVXZcig^[j\VdYZkZbhZg
gZeZi^Ydh!cdb{m^bd!bV^hYjVhkZoZh#
8dcijYd!hZdkVadgi^kZgVjbZciVYdVeZcVh%!%*djbZcdhZbgZaVdVdeg^bZ^gd
kVadg!‚k{a^YddkVadgbV^hZaZkVYdYVVc{a^hZ#
:mZbead/
• Após a primeira centrifugação, leu-se para a amostra dupla 3,55 % e 3,60 %.
• Após a segunda centrifugação 3,60 % e 3,65 %. Como resultado do teor butiroso do leite
homogeneizado é indicado 3,65 %.
• Se, após as duas últimas repetições, isto é, após a 3ª e 4ª centrifugações ainda
continuar a haver uma diferença superior a 0,05 %, o resultado desta determinação deve
ser rejeitado.
8Vi{ad\dYZaVWdgVi‹g^deVgVVc{a^hZhYZaZ^iZ
&.
DETERMINAÇÃO DO TEOR BUTIROSO
DE DIVERSOS PRODUTOS LÁCTEOS
PREFÁCIO:
A determinação do teor butiroso no leite era e é em número cada vez mais crescente substituída por outras análises de rotina (através de aparelhos como,
p.ex. LactoStar). No entanto, com estes aparelhos os produtos lácteos como,
p.ex. queijo, gelado, etc. não podem ser medidos ou apenas o podem ser através de preparativos de amostra dispendiosos. Em produtos deste género, os
processos butirométricos continuam sendo uma boa alternativa para a análise
de rotina.
1.0 ÂMBITO DE APLICAÇÃO
9ZiZgb^cVdYdiZdgWji^gdhdcdaZ^iZZY^kZghdhegdYjidha{XiZdh#
2.0 VOLUMES
HZcd]djkZgcVYVYZhXg^idZbXdcig{g^d!hdhZbegZk{a^YVhVhhZ\j^ciZh
fjVci^YVYZheVgVdhegdYjidhfj†b^XdhZVbdhigVhYZVc{a^hZji^a^oVYVh/
ÛX^Ydhja[g^Xd/ &%!%ba'%•8 '•8
ÛaXddaVb†a^Xd/ &!%ba'%•8 '•8
AZ^iZdjegdYjida{XiZd/ &%!,*ba'%•8 '•8
3.0 BREVES DESCRIÇÕES DA
DETERMINAÇÃO DO TEOR BUTIROSO
3.1 ... NO LEITE (SEGUNDO GERBER):
Wji^g‹bZigdh YZ aZ^iZ ^beZXVkZabZciZ a^bedh! ZheZX^VabZciZ hZb gZh†Yjdh YZ \dg"
YjgV!hdZcX]^YdhcVhZ\j^ciZdgYZb/&%baYZ{X^Ydhja[g^XdYZch^YVYZ/&!-&- $"
%!%%(\$ba!&%!,*baYZaZ^iZZ&baYZ{aXddaVb†a^Xd#DaZ^iZZd{aXddaVb†a^XdYZkZb
hZg^cigdYjo^Ydh[dgbVcYdXVbVYVhY^[ZgZciZh!YZbdYdfjZcddXdggVjbVb^hijgV
VciZh YV V\^iVd# 6e‹h d [ZX]d! d iZdg Yd Wji^g‹bZigd ‚ WZb b^hijgVYd VigVk‚h YV
V\^iVdZY^kZghVhk^gV\Zch#6igVk‚hYZjbVgZ\jaVdXj^YVYdhVYVgda]V!diZdgYd
Wji^g‹bZigd‚gZ\jaVYdYZbdYdfjZVZhXVaVÒfjZX]Z^V!bVhcd]V_Va†fj^YdcdWda"
Wd#8Zcig^[j\VgdWji^g‹bZigdcVXZcig^[j\VYdgVVfjZX^YV!YZ^mVgVfjZXZg*b^cjidhV
+* •8 Zb WVc]d"bVg^V! V_jhiVg V a^c]V YZ hZeVgVd YV b^hijgV YZ {X^Yd hja[g^Xd$
XdajcVYZ\dgYjgVeVgVjbVbVgXVYZ\gVYjVdXdbeaZiV!XdchjaiVgVZmigZb^YVYZ
hjeZg^dgYVXdajcVYZ\dgYjgVcdbZc^hXd^c[Zg^dg#
3.2 ... EM LEITE HOMOGENEIZADO
Xdbd YZhXg^id VX^bV! bVh XZcig^[j\Vg ig„h kZoZh! * b^cjidh YZ XVYV kZo# :cigZ Vh
XZcig^[j\VZh! dh Wji^g‹bZigdh hd VfjZX^Ydh * b^cjidh Zb WVc]d"bVg^V V +*•8#
(mais detalhado pág. 19)
3.3 ... EM LEITE MAGRO E SORO DE LEITE
Utilização de butirómetros de leite magro com escala estreita segundo Sichler.
8Zcig^[j\Vd YjeaV Xdb XdadXVd ^ciZgb^iZciZ Ydh Wji^g‹bZigdh * b^cjidh Zb
WVc]d"bVg^VV+*•8#
3.4 ... EM LEITE CONDENSADO (NÃO AÇUCARADO)
DaZ^iZXdcYZchVYdVfjZX^YdegZk^VbZciZV*%•8Z!YZed^h!cdkVbZciZVggZ[ZX^Yd‚b^hijgVYd
Xdb {\jV cjbV gZaVd YZ &/&# :hiV Y^aj^d ‚ VcVa^hVYV Xdbd aZ^iZ hZ\jcYd <ZgWZg# IZdg
Wji^gdhd2kVadga^Ydm'#
'%
8Vi{ad\dYZaVWdgVi‹g^deVgVVc{a^hZhYZaZ^iZ
3.5 ... EM SORO DE MANTEIGA (MODIFICAÇÃO SEGUNDO MOHR E BAUR)
DWji^g‹bZigd‚X]Z^dXdb&%baYZ{X^Ydhja[g^XdYZch^YVYZ&!-(% $"%!%%(\$ba#:b
kZoYZ&%!,*ba!hde^eZiVYdh&%baYZhdgdYZbVciZ^\VZ'!%baYZ{aXddaVb†a^Xd#6e‹h
d[ZX]dYdhWji^g‹bZigdh!V\^i{"adhZXZcig^[j\Vg^bZY^ViVbZciZedg&%b^c#9ZhiZbdYd
‚Zk^iVYVVeZgijgWVYdgV[dgbVdYZgda]V#6aZ^ijgVdXdggZVeZcVhVe‹h*b^cjidhYZ
VfjZX^bZcidV+*•8 $"'•8#IZdgWji^gdhd2kVadga^Ydm&!%,*#
3.6 ... EM LEITE EM PÓ SEUNGDO TEICHERT
Utilização de butirómetros de leite em pó segundo Teichert.
D Wji^g‹bZigd ‚ X]Z^d Xdb &% ba YZ {X^Yd hja[g^Xd YZch^YVYZ/ &!-&- $" %!%%( \$ba#
HdWgZZhiZhhdXdadXVYdhZbXVbVYV,!*baYZ{\jVZ&baYZ{aXddaVb†a^Xd#CjbV
aVcVYZ^gVYZeZhV\ZbhdeZhVYdh'!*\YZaZ^iZZbe‹Z^cigdYjo^YdhVigVk‚hYZjb
[jc^ajhVcYdjbe^cXZaÒcdeVgVYZcigdYdWji^g‹bZigd#DWji^g‹bZigd‚V\^iVYdZmVjhi^"
kVbZciZVe‹hZhiVg[ZX]VYdZXdadXVYd^ciZgb^iZciZbZciZY^kZghVhkZoZhZbWVc]d"bV"
g^VV+*•8!XZcig^[j\Vg'm*b^c#cVXZcig^[j\VYdgVVfjZX^YVZegdXZYZg|aZ^ijgVVe‹hV
XdadXVdZbWVc]d"bVg^V*b^c##
3.7 ... EM NATA SEGUNDO ROEDER (MÉTODO DE PESAGEM)
Utilização de butirómetro de nata segundo Roeder.
HdeZhVYdh*\YZcViVhcdXdedYZk^YgdZm^hiZciZcVgda]VZ^cigdYjo^YdhcdWji^g‹"
bZigd#6igVk‚hYVVWZgijgVhjeZg^dgYdWji^g‹bZigd‚^cigdYjo^Yd{X^Ydhja[g^XdYZc"
h^YVYZ/&!*'' $"%!%%*\$baVigVk‚hYVWdgYVhjeZg^dgYdXdedYZk^Ygd#6e‹hd[ZX]d!
dWji^g‹bZigd‚XdadXVYdZbWVc]d"bVg^VV,%•8YjgVciZjbVV\^iVdgZeZi^YVVi‚|
Y^hhdajdXdbeaZiVYVhegdiZ†cVh#6i‚|VaijgVYd^c†X^dYVZhXVaV‚VY^X^dcVYd{X^Yd
hja[g^XdZ!YZed^h!&baYZ{aXddaVb†a^Xd!dWji^g‹bZigd[ZX]VYd!V\^iVYdZYjgVciZbV^h
*b^cjidhXdadXVYdZbWVc]d"bVg^VV,%•8#:bhZ\j^YV/XZcig^[j\Vg*b^c#Z!YZed^h!
VfjZXZgV+*•8ZbWVc]d"bVg^V#6XdchjaiV‚[Z^iVV+*•8!V_jhiZYdiZdgWji^gdhdeVgV
dedcidoZgd!aZ^ijgVcdbZc^hXd^c[Zg^dg#
3.8 ... EM NATA SEGUNDO SCHULZ-KLEY (MÉTODO DE PESAGEM)
Utilização de butirómetro de nata segundo Schulz.
CdWji^g‹bZigdhd^cigdYjo^YdhhjXZhh^kVbZciZ/&%baYZ{X^Ydhja[g^XdYZch^YV"
YZ/&!-&- $"%!%%(\$ba!*baYZ{\jV!Vegdm#*\YZcViVeZhVYdhVigVk‚hYZeZhV"
\ZbY^[ZgZcX^VaXdbjbVhZg^c\VZbWVaVcVdje^eZiVYZeZhV\Zb!&baYZ{aXdda
Vb†a^Xd#6e‹h[ZX]VYddWji^g‹bZigd!dXdciZYd‚b^hijgVYdedgV\^iVdZk^gV\Zch!
ZdWji^g‹bZigdXZcig^[j\VYdZbXZcig^[j\VYdgVVfjZX^YVYjgVciZ*b^cjidh#6aZ^"
ijgV‚gZVa^oVYVVe‹h*b^cjidhYZVfjZX^bZcidZbWVc]d"bVg^VV+*•8#6iZcd/
YZk^Yd|edhh^W^a^YVYZYZgZYjdYdXVadgYZgZVXdVigVk‚hYVVY^dYZ{\jV!cd
YZkZbhZgYZXdgg^YdhbV^hYZ&*b^cjidhZcigZdZcX]^bZcidXdb{\jVZVV\^iVd!
degdXZY^bZcidYZY^hhdajdYZkZhZgXdcXaj†YdZbcdb{m^bd+%hZ\#
IZdgWji^gdhd2kVadga^Ydm*$bVhhVYZcViV#
3.9 ... EM NATA SEGUNDO KÖHLER (MÉTODO DE MEDIÇÃO)
Utilização de butirómetro de nata segundo Köhler.
Cd Wji^g‹bZigd YZ cViVh hd ^cigdYjo^Ydh hjXZhh^kVbZciZ/ &% ba YZ {X^Yd hja[g^Xd
YZch^YVYZ/&!-&- $"%!%%(\$ba!*!%*baYZcViV!*baYZ{\jV!&baYZ{aXddaVb†a^Xd#
6igVk‚hYVji^a^oVdYZjbVhZg^c\VYZcViVh!YZkZ"hZ!VciZhYVVY^dYdh*baYZ
{\jV!aVkVgVhZg^c\VeZadZcX]^bZcidgZeZi^YdXdb{\jV#DWji^g‹bZigd‚[ZX]VYd!
V\^iVYd!XZcig^[j\VYdedg*b^cjidh!Za^YdVe‹h*b^cjidhYZVfjZX^bZcidZbWVc]d"
bVg^VV+*•8#6aZ^ijgV‚[Z^iVVeVgi^gYdedcidoZgd#
8Vi{ad\dYZaVWdgVi‹g^deVgVVc{a^hZhYZaZ^iZ
'&
3.10 ... EM QUEIJO SEGUNDO VAN GULIK (MÉTODO DE PESAGEM)
(consultar ISO 3433) Utilização de butirómetro de queijo segundo van Gulik.
CdWji^g‹bZigdkVc<ja^`[ZX]VYdcdaVYdYdÒbYVZhXVaV!Ve‹hV^cigdYjdYZ
Vegdm^bVYVbZciZ &* ba YZ {X^Yd hja[g^Xd YZch^YVYZ/ &!*'' $" %!%%* \$ba! ( \
$"%!'\YZfjZ^_dVigVk‚hYZaVcVYZ^gVYZeZhV\ZbZe^cXZaÒcd!hZcYd!YZed^h!
[ZX]VYdddg^[†X^dYZ^cigdYjd#6hVbdhigVhYZfjZ^_deVhidhVhi„bYZhZgeZhV"
YVhcdXdedYZk^YgdeZg[jgVYdeZgiZcXZciZVdWji^g‹bZigdYZkVc<ja^`Z^cigdYj"
o^YVhcdWji^g‹bZigd#DWji^g‹bZigd[ZX]VYd‚XdadXVYd!XdbVZhXVaVeVgVX^bV!
ZbWVc]d"bVg^VV,%•8"-%•8ZV\^iVYdY^kZghVhkZoZhVi‚|XdbeaZiVY^hhdajd
YdfjZ^_d#:bhZ\j^YV!VigVk‚hYVVWZgijgVYVZhXVaV‚VY^X^dcVYd&baYZ{aXdda
Vb†a^XdZ!YZed^h!{X^Ydhja[g^XdVegdm^bVYVbZciZVi‚|bVgXVYdh&*YVZhXVaV#
:bhZ\j^YV‚[ZX]VYd!b^hijgVYd!VfjZX^YdYjgVciZX^cXdb^cjidhZbWVc]d"bVg^V
V+*•8ZXZcig^[j\VdYjgVciZ*b^cjidh0cdkVXdadXVdZbWVc]d"bVg^VV+•8!
V_jhiZYVXdajcVYZ\dgYjgVeVgVVbVgXVoZgdZaZ^ijgVYdiZdgWji^gdhdVWhdajid#
6aZ^ijgV‚[Z^iVcVZmigZb^YVYZ^c[Zg^dgYdbZc^hXd#IZdgWji^gdhd2kVadga^Ydm($
bVhhVYZfjZ^_d#
3.11 ... EM GELADO SEGUNDO KÖHLER (MÉTODO DE MEDIÇÃO)
Utilização de butirómetro de gelado segundo Köhler.
:kZcijV^h XdWZgijgVh dj eVgi†XjaVh bV^dgZh e#Zm# [gjidh! ZiX# YZkZb hZg gZbd"
k^YVh# D \ZaVYd VfjZX^Yd | iZbeZgVijgV VbW^ZciZ YZkZ hZg WZb b^hijgVYd0 d Vg
ZkZcijVabZciZegZhZciZedYZhZggZbdk^Yd!cVhjVbV^dg^V!VigVk‚hYZVea^XVd
YZk{Xjd#CdWji^g‹bZigdYZ\ZaVYdhhd^cigdYjo^YdhhjXZhh^kVbZciZ/&%baYZ
{X^Ydhja[g^XdYZch^YVYZ/&!-&- $"%!%%(\$ba!*baYZ\ZaVYd!*baYZ{\jV!&
baYZ{aXddaYZVb†a^Xd#CVji^a^oVdYZjbVhZg^c\V!YZkZ"hZ!VciZhYVVY^dYdh
*baYZ{\jV!aVkVgVhZg^c\VeZadZcX]^bZcidgZeZi^YdXdb{\jV#HZdWji^g‹bZigd
cdZhi^kZgXdbeaZiVbZciZX]Z^d!edYZ"hZVY^X^dcVgVi‚'baYZ{\jV#DWji^g‹bZ"
igd‚[ZX]VYd!V\^iVYd!XZcig^[j\VYdYjgVciZ*b^cjidhZa^Yd!Ve‹h*b^cjidhYZ
VfjZX^bZcidZbWVc]d"bVg^VV+*•8#
3.12 ... EM GELADO SEGUNDO ROEDER (MÉTODO DE PESAGEM)
Utilização de butirómetro de gelado segundo Roeder.
*\YZ\ZaVYdWZbb^hijgVYdhhdeZhVYdhcdXdedYZk^YgdZm^hiZciZcVgda]VZ^cigd"
Yjo^YdhcdWji^g‹bZigd#6igVk‚hYVVWZgijgVhjeZg^dgYdWji^g‹bZigd‚^cigdYjo^Yd{X^Yd
hja[g^XdYZch^YVYZ/&!*'' $"%!%%*\$baVigVk‚hYVWdgYVhjeZg^dgYdXdedYZk^Ygd#
6e‹hd[ZX]d!dWji^g‹bZigd‚XdadXVYdZbWVc]d"bVg^VV,%•8YjgVciZjbVV\^iVdgZ"
eZi^YVVi‚|Y^hhdajdXdbeaZiVYVhegdiZ†cVh#wVY^X^dcVYd&baYZ{aXddaVb†a^XdZ!Vi‚
|bVgXVYdh&%cVZhXVaV!{X^Ydhja[g^Xd!dWji^g‹bZigd‚[ZX]VYd!V\^iVYdZYjgVciZ
bV^h&%b^cjidhXdadXVYdZbWVc]d"bVg^VV,%•8#9jgVciZZhiZiZbed!dhXdbedcZciZh
hdV\^iVYdhZb^ciZgkVadhgZ\jaVgZh#:bhZ\j^YV/XZcig^[j\Vg,b^c#Z!YZed^h!VfjZXZg
V+*•8ZbWVc]d"bVg^V#6aZ^ijgV‚[Z^iVV+*•8!V_jhiZYdiZdgWji^gdhdeVgVdedcidoZgd!
aZ^ijgVcdbZc^hXd^c[Zg^dg#
3.13 ... EM MANTEIGA SEGUNDO ROEDER (MÉTODO DE PESAGEM)
Utilização de butirómetro de manteiga segundo Roeder.
HdeZhVYdh*\YZcViVhcdXdedYZk^YgdZm^hiZciZcVgda]VZ^cigdYjo^YdhcdWji^"
g‹bZigd#6igVk‚hYVVWZgijgVhjeZg^dgYdWji^g‹bZigd‚^cigdYjo^Yd{X^Ydhja[g^Xd
YZch^YVYZ/ &!*'' $" %!%%* \$ba Vi‚ VX^bV YV WdgYV hjeZg^dg Yd Xded YZ k^Ygd#
6e‹hd[ZX]d!dWji^g‹bZigd‚XdadXVYdZbWVc]d"bVg^VV,%•8YjgVciZjbVV\^iV"
dgZeZi^YVVi‚|Y^hhdajdXdbeaZiVYVhegdiZ†cVh#6i‚VVaijgVYd^c†X^dYVZh"
XVaV‚VY^X^dcVYd{X^Ydhja[g^XdZ&baYZ{aXddaVb†a^Xd!dWji^g‹bZigd‚[ZX]VYd!
V\^iVYdZYjgVciZbV^h*b^cjidhXdadXVYdZbWVc]d"bVg^V,%•8#:bhZ\j^YV/
XZcig^[j\Vg*b^c#!VfjZXZgZbWVc]d"bVg^VV+*•8Vegdm#*b^c#9Zed^h!gZVa^oVg
VaZ^ijgVV+*•8#GZVa^oVgVaZ^ijgVcdbZc^hXd^c[Zg^dg#
''
8Vi{ad\dYZaVWdgVi‹g^deVgVVc{a^hZhYZaZ^iZ
3.14 ... EM MAIONESE SEGUNDO ROEDER (MÉTODO DE PESAGEM)
Utilização de butirómetro de manteiga segundo Roeder.
EZhV"hZ&\YZbV^dcZhZcdXdedYZk^YgdZm^hiZciZcVgda]VZ^cigdYjo"hZcdWji^"
g‹bZigd# 6igVk‚h YV VWZgijgV hjeZg^dg Yd Wji^g‹bZigd ‚ ^cigdYjo^Yd {X^Yd hja[g^Xd
YZch^YVYZ/&!*'' $"%!%%*\$baVi‚VX^bVYVWdgYVhjeZg^dgYdXdedYZk^Ygd#6e‹hd
[ZX]d!dWji^g‹bZigd‚XdadXVYdZbWVc]d"bVg^VV,%•8YjgVciZ(%b^c#XdbV\^iVd
gZeZi^YV Vi‚ | Y^hhdajd XdbeaZiV YVh egdiZ†cVh# 6i‚ V VaijgV Yd ^c†X^d YV ZhXVaV ‚
VY^X^dcVYd{X^Ydhja[g^XdZ&baYZ{aXddaVb†a^Xd!dWji^g‹bZigd‚[ZX]VYd!V\^iVYdZ
YjgVciZbV^h*b^cjidhXdadXVYdZbWVc]d"bVg^V#:bhZ\j^YV/XZcig^[j\Vg&%b^c#!
VfjZXZgZbWVc]d"bVg^VV+*•8Vegdm#*b^c##9Zed^h!gZVa^oVgVaZ^ijgVV+*•8#GZ"
Va^oVgVaZ^ijgVcdbZc^hXd^c[Zg^dg#DkVadgdWi^Yd‚bjai^ea^XVYdedg*!eVgVhZdWiZgd
iZdgWji^gdhdXdggZhedcYZciZ#
3.15 DETERMINAÇÃO DO TEOR BUTIROSO SEGUNDO GERBER
(VAN GULIK) DE CARNES E ENCHIDOS
Segundo o método recomendado por “Pohja e colaboradores”.
;gk_fWc[djei0
FheZkjeigk‡c_Yei0
'$8kj_hŒc[jhe
'$ÜY_Zeikb\‘h_Ye
7ji^g‹bZigdYZfjZ^_dhZ\jcYdÆKVc<ja^`Ç
9Zch^YVYZV'%•8&!-&- $"%!%%(\ba"&^cXdadgdj
VeZcVha^\Z^gVbZciZi^c\^YdZ^hZcidYZXdbedcZciZhfjZ
^cÓjZcX^ZbdgZhjaiVYd#
($9[djh_\k]WZehW
8Zcig^[j\VYdgVYZaZ^iZXdbjbVGO7
VXZaZgVdXZcig†[j\VgZaVi^kVYZ(*%\ $"*%\#
e#Zm#HjeZgKVg^d"CdjCdkVHV[Zin#
($ÜbYeebWc‡b_Ye
9Zch^YVYZV'%•8%!-&& $"%!%%(\ba"&
)$8Wd^e#cWh_W
7Vc]d"bVg^VXdbV\^iVdVjbViZbeZgVijgVYZ
+*•8 $"'•8#
*$FheZkjeigk‡c_Yei
+$ÜbYeebWc‡b_Ye
EVgVgZYjXdYZiVbVc]dZ]dbd\ZcZ^oVdYV
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Sendo:
R = raio horizontal efectivo em milímetros;
N = rotações por minuto [min-1].
TABELA DE REFERÊNCIA DA DEPENDÊNCIA DE VALORES G E ROTAÇÕES
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A adição de sulfato de potássio serve para aumento da temperatura de
ebulição do ácido sulfúrico e a adição de sulfato de cobre como catalisador
de oxidação. Esses productos também são adquiríveis na forma de tabletes
Kjeldahl (art. n.o: 4230/4231). Se o procedimento é realizado com tabletes,
então são misturados 5± 0,1 g do leite com 20 ml de ácido sulfúrico e
2 tabletes Kjeldahl e deixados em repouso por 5 min. Após isso pode-se
proceder com o programa de temperatura.
O ácido sulfúrico é adicionado de forma tal que resíduos de solução de sulfato
de cobre, sulfato de potássio ou leite eventualmente aderidos ao pescoço do
balão sejam arrastados para baixo. Se o balão estiver firmemente fechado,
ele pode ser guardado para uma solubilização posterior.
Durante o aquecimento da amostra forma-se espuma, a qual não pode
elevar-se mais que 4-5 cm sob a abertura do balão.
Para determinar o tempo de solubilização específico, recomenda-se
realizar testes prévios com amostras com alto teor de proteínas e ricas em
gordura.
Uma cristalização extensa é sinal de quantidade insuficiente de ácido
sulfúrico e pode levar a valores de proteínas muito baixos. Por isso é
recomendável reduzir a perda de ácido sulfúrico diminuindo-se a quantidade
de sucção.
Antes de retirar o balão de solubilização do bloco de aquecimento deve-se
assegurar que não se formou nenhum líquido de condensação no dispositivo
de sucção. Se for o caso, deve-se aumentar a capacidade de sucção e
eliminar o líquido de condensação antes da desmontagem do balão.
O producto solubilizado não diluído não pode, em nenhum caso, ser guardado
no balão por longo período (noite inteira). Existe perigo de solidificação da
amostra e é difícil trazê-la de volta a solução. Se a amostra é diluída com
70 ml de água após ser resfriada, não há problema em guardá-la por um
período longo.
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O destilador de água deve ser colocado sobre uma mesa de laboratório estável com
suporte plano e horizontal, que se encontre
próxima a uma conexão de água fria e um
sistema de drenagem. A pressão de água
deve ser de no mínimo 0,5 bar.
Antes da entrada em operação deve-se conectar todas as mangueiras e a água fria.
Os reservatórios devem ser posicionados
correctamente e o nível de enchimento
testado. A mangueira de introdução de vapor de água deve ser acoplada ao balão de
solubilização. O destilador de água é equipado com uma porta de protecção.
Na primeira destilação, o vapor de água
quente encontra tubulações e partes de
vidro ainda frias. Isso acarreta em uma
maior formação de condensado, que pode
resultar em diluição exagerada da amostra e grande volume de líquido no recipiente de solubilização. Por isso, uma corrida
de teste é necessária. A entrada de vapor
de água a uma temperatura de aprox. 106°C
causa ruídos mais ou menos intensos. Estes ruídos não representam motivo para
preocupação.
A destilação é executada até que um volume de destilado de 150 ml seja atingido.
Cerca de 2 minutos antes do final da destilação, o balão Erlenmeyer é baixado até
que o tubo de dreno não mais afunde na
solução de ácido. O tubo é lavado com um
pouco de água, e a água de lavagem recolhida no balão Erlenmeyer.
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Como indicador usa-se a mistura de vermelho de metila e
verde bromocresol (ver 2.5, 2.6). O indicador é responsável
pela mudança de cor e sinaliza o final da titulação.
O fundo neutro melhora a precisão e reprodutibilidade dos
resultados. Assim, as titulações são conduzidas sempre
sob condições ópticas iguais.
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O teste cego é importante para o cálculo do teor de
nitrogénio.
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egZX^hdVi‚%!&b\#
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A solubilização segundo Kjeldahl não é específica para aminoácidos e proteínas, e representa todo o nitrogénio ligado
a compostos orgânicos. Outros compostos não protéicos
são também solubilizados e compreendidos (NPN: nitrogénio não protéico). Porém seu conteúdo em leite e productos
do leite é reduzido e, portanto, desprezado neste cálculo.
Se o nitrogénio não protéico (NPN) também necessitar
ser determinado, então se deve proceder com o método
conforme a norma DIN EN ISO 8968-4. Se apenas o nitrogénio protéico tiver que ser obtido, então se deve primeiramente separar as proteínas do leite. 5 ± 0,1 ml de
leite diluído com 5 ± 0,1 ml de água são, segundo a norma
DIN EN ISO 8968-5, lavados gradativamente com, ao todo,
60 ml de uma solução de ácido tricloroacético 15 % (m/v),
as proteínas são precipitadas e em seguidas filtradas
através de um filtro de papel duro. O filtrado contém os
componentes de nitrogénio não protéico e o precipitado
contém o nitrogénio protéico. O filtro com o precipitado é
colocado no recipiente de solubilização e a determinação
de nitrogénio é realizada como descrito acima segundo o
método Kjeldahl. O teor em proteína é calculado por meio
da multiplicação pelo factor 6,38.
O valor 6,38 é específico para leite e productos do leite e foi
assim fixado porque as proteínas do leite têm um teor de
nitrogénio de 15,65% (100:15,65 = 6,38).
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DETERMINAÇÃO DE NITROGÉNIO SEGUNDO KJELDAHL
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\I^D'!&%baYZ{X^Ydhja[g^Xd.-!Va\jbVh\diVhYZV\ZciZ
Vci^ZhejbVciZ (% YZ egZeVgVYd YZ h^a^XdcZ# B^hijgV"hZ
Xj^YVYdhVbZciZ!ZheZgV"hZ*b^cZYZed^hhZYZ^mVZhXdggZgYZ
[dgbVWVhiVciZXj^YVYdhVZaZciV*baYZeZg‹m^YdYZ]^Ygd\‚c^d
(%eZaVheVgZYZhYdgZX^e^ZciZ#6ciZhYVhdajW^a^oVd!YZ^mV"
hZVVbdhigVYZ&%V&*b^cZbgZedjhd#DWadXdYZVfjZX^bZcid
‚ eg‚"VfjZX^Yd edg &% b^c V )%%•8! Z V VbdhigV VfjZX^YV edg
+%b^cV)%%•8#:bhZ\j^YVVVbdhigV‚gZh[g^VYVViZbeZgVijgV
VbW^ZciZZY^aj†YVXdb*%baYZ{\jV#CVYZhi^aVdhdjhVYdh
**baYZCVD=(%Z*%baYZ{X^YdW‹g^Xd)eVgVVWhdgd
Yd YZhi^aVYd# I^ijaV"hZ Xdb =8a %!%* B# 8dbd ^cY^XVYdg jhV"hZ
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Cuidado, a adição de peróxido de hidrogénio
causa uma reacção intensa.
O teste de valor cego é executado com 2 ml de
água e 0,25 g de sacarose. A efectividade de
solubilização é testada com 0,08 g de triptófano
ou 0,06 g de hidroclorito de lisina.
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hdW Vh bZhbVh XdcY^Zh fjZ eVgV VbdhigVh cdgbV^h Z d iZdg
eZgXZcijVaZbc^igd\‚c^dYZkZZcXdcigVg"hZZcigZ..!%Z&%%#6
YZiZgb^cVdXdbhja[VidYZVb‹c^dhZgkZeVgVYZhXdWg^geZgYVh
YZc^igd\‚c^dYjgVciZVhdajW^a^oVddjYZhi^aVdZY^[ZgZcVh
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Para controlar a eficiência da solubilização,
usa-se 0,18 g de triptófano ou 0,16 g de hidroclorito de lisina e 0,67 g de sacarose. 98 % do
nitrogénio devem ser reencontrados. Se não for o
caso, a temperatura de solubilização ou o tempo
é insuficiente, ou a amostra está carbonizada.
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Medição de valor pH
Enga de alimentos e biotecnologia Anna Politis
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Para depósitos de gordura ou óleo, deve-se remover a gordura da membrana com algodão
impregnado com acetona ou solução saponácea.
Se proteína houver se depositado no diafragma, o eléctrodo é imerso em uma solução de
HCl / pepsina aprox. 1 a 2 horas.
Em caso de contaminação com sulfeto de prata, o eléctrodo é posto e imerso em uma
solução de tiouréia
Para recobrimentos inorgânicos, o eléctrodo é imerso por alguns minutos em HCl 0,1 M
ou NaOH 0,1 M. Uma melhor limpeza é obtida com soluções aquecidas a 40 - 50°C.
Após cada procedimento de limpeza, deve-se colocar o eléctrodo por cerca de 15
minutos em uma solução de KCl 3M para novo condicionamento e em seguida calibra-lo
novamente.
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iZbV[jaXgVaYV;jc`Z"9g#C#<ZgWZgAVWdgiZX]c^`<bW=
Eng.º K. Schäfer, Físico W. Spindler
HISTÓRIA
Já em 1895 o químico alemão Beckmann, começou a aproveitar o “termómetro Beckmann” para comprovar a adição de água estranha através do ponto de congelação do
leite. No ano de 1920, o americano Hortvet trabalhou intensivamente com este método
e melhorou-o em alguns pontos essenciais. Os primeiros crioscópios termistores foram
introduzidos no mercado nos anos 60. Contudo, ainda tinham de ser operados de forma
totalmente manual. No início dos anos 70, encontravam-se disponíveis, pela primeira
vez, crioscópios termistores automáticos. Assim havia a possibilidade de determinar o
ponto de congelação de modo automático através do carregar de um botão.
Um passo importante para a melhoria da crioscopia
por termistor pôde ser registado na feira “FoodTec
1984”: A Funke-Gerber criou o primeiro aparelho
com aferição automática. Este trabalho de desenvolvimento intenso de sucesso encontrou outro
ponto alto na “FoodTec 1988”, em que a Funke-Gerber pôde apresentar uma unidade totalmente automática para determinação do ponto de congelação
com uma capacidade de 220 amostras/h.
Com a introdução de uma medição indirecta do ponto de congelação (p.ex. LactoStar) para análise de
rotina, o interesse voltou-se principalmente para
aparelhos de referência com a capacidade de determinar o ponto de congelação de acordo com as
normas em vigor. Estes aparelhos têm de cumprir
os mais elevados requisitos quanto à precisão de
medição, pois, assim, são aferidos os aparelhos de
rotina. Para este fim, a Funke-Gerber desenvolveu
um crioscópio de livre programação com uma resolução de 0,1 m°C. Este aparelho já foi posto à prova
em numerosos laboratórios em todo o mundo quanto à sua precisão e fiabilidade. Entretanto, a gama
de produtos foi aumentada com um aparelho de medição de múltiplas amostras (CryoStarautomatic). Desde
janeiro de 2007 esse aparelho é equipado com um
expositor gráfico colorido. Através dele é possível
mostrar toda a curva de congelação, especialmente a busca da plataforma, com uma
apresentação patenteada na tela.
.%
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PONTO DE CONGELAÇÃO:
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