Análises de Leite - Funke-Dr.N.Gerber Labortechnik GmbH / Milch

CATÁLOGO DE LABORATÓRIO para Análises de Leite 8VgVhHZc]dgVh!8VgdhHZc]dgZh! DcdbZ;jc`Z"<ZgWZggZegZhZciVVc{a^hZYZaZîZ^cdkVYdgV!a^\VYV|fjVa^YVYZ! 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Uma contribuição do Eng.º K. Schäfer. *. 9[djh_\k]WZehWckbj_\kdY_edWbIkf[hLWh_e#D +( 8Wdêi#cWh_W +) +, 7Y[iih_eifWhWY[djh_\k]WZehWi :[j[hc_dWeZ[d_jhe]d_ei[]kdZecjeZeZ[A`[bZW^b Uma contribuição da Eng.a Anna Politis ;gk_fWc[djei[kj[dib_eifWhWZ[j[hc_dWeZ[fhej[dWii[]kdZeA`[bZW^b ,' C[Z_eZef>"ef[hWe[cWdkj[deZ[c[Z_Zeh[if> ,) 7fWh[bêi[WY[iih_eifWhWWZ[j[hc_dWeZelWbehf> ,+ 7fWh[bêiZ[j_jkbWe%Z[j[hc_dWeZWWY_Z[p ,. 7dWb_iWZehZ[i[Z_c[djei Papéis de filtro, Sedilab, Aspilac, etc -& ;ij_cWj_lWZ[YedjW][cZ[][hc[i -' FheZkjei][hW_iZ[bWXehWjh_e -( Copo para derreter manteiga, colher de teste, espátula, película de alumínio, areia de cristal de quartzo, bico de Bunsen, funil de decantação, cromatografia de camada fina, etc. H[\hWYjc[jhe -+ C[Z_eZ[^kc_ZWZ[ -, 8WbWdWiZ[bWXehWjh_e -/ ;ijk\Wi"_dYkXWZehWi"_dYkXWZehWiW\h_e"\ehdebWXehWjeh_Wb .& C[Z_eZWl_iYei_ZWZ["f[igk_iWZ[_d_X_Zeh[i .' C[Z_eZWZ[di_ZWZ[%Wh[c[jhei .( ., C[Z_eZefedjeZ[Yed][bWe Um tema fulcral da Funke - Dr. N. Gerber Labortechnik GmbH Eng.º K. Schäfer, físico W. Spindler /& 9hoeIjWh?"9hoeIjWhWkjecWj_Y[WY[iih_ei /, J[hcc[jhei"WfWh[bêiZ[c[Z_eZ[^kc_ZWZ[ ) 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ C_ijkhWZehZ[dZ_Y[Z[iebkX_b_ZWZ["lebc[jheZ[YWbYWc[dje '&& 9ecfhelWeZ[Wgk[Y_c[dje[Z[cWij_j[ '&' Kj[dib_eiZ[bWXehWjh_e '&( 7fWh[bêibWXehWjeh_W_i Aparelho de contagem de germes ColonyStar, autoclaves, incubadoras, misturadores magnéticos, fotómetros, microscópios, aparelhos de destilação de água, banhos-maria '&, 7Wfb_YWeZ[cWj[h_W_iZ[h[\[hdY_W[cbWXehWjh_e Uma contribuição do Dr. Ulrich Leist, DRRR GmbH ''( L_ZhebWXehWjeh_Wb '(& CWj[h_W_iZ[bWXehWjh_e '(, ßdZ_Y[h[c_ii_leWb\WXj_Ye ')( 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ * TRADIÇÃO PROGRESSO CONTINUIDADE ;jc`Z"9g#C#<ZgWZgAVWdgiZX]c^`<bW= Parceiro da indústria de lacticínios desde 1904 9ZhYZ&.%)!V;jc`Z"<ZgWZgjbeVgXZ^gd^bedgiVciZ YV^cYhig^VYZaVXi^Xc^dhiVcidcV6aZbVc]VXdbd cdZhigVc\Z^gd#:cigZVhVXi^k^YVYZhfjZhZYZhiVXVb ^cXaj^"hZd[VWg^XdYZVeVgZa]dhaVWdgVidg^V^heVgVV Vc{a^hZYZaZîZZYZegdYjidhVa^bZciVgZh# IVaXdbdVXdciZX^VcdeVhhVYd!d[VWg^XdYZXZcig^[j" \VYdgVhZWji^gbZigdh!WZbXdbdYZdjigdhZfjêV" bZcidheVgVVYZiZgb^cVdYdiZdgWji^gdhdhZ\jcYd d9g#C#<ZgWZgXdci^cjVVhZgdeâVg[jaXgVaYVZbegZ" hV#EVgVVabYZhiV{gZVXa{hh^XV!VZbegZhVYZhZc" kdakZZ[VWg^XVVeVgZa]dhZaZXigc^XdhbdYZgcdheVgV VVc{a^hZYZaZîZ# DhVeVgZa]dheVgVVYZiZgb^cVdYdedcidYZXdc" \ZaVdYVa^c]VÇ9hoeIjWhÈhdVegZX^VYdheZaVhjV ZaZkVYVegZX^hdYZbZY^dZXdcÒVWâ^YVYZ!ZhiVcYd ^chiVaVYdhZbbjîVhaZîVg^VhZ^chiîjidhYZhYZ]{ k{g^dhVcdh# 8dbdhcdkdhVeVgZa]dhÇBWYjeIjWhÈZÇBWYje<bWi^È ^c^X^dj"hZjbVcdkVZgVcVVc{a^hZYZgdi^cV# DÆ@cdl=dlÇdWi^YdVdadc\dYdhVcdhZdXdcicjd VeZg[Z^dVbZcid[VoZbYV;jc`Z"<ZgWZgjbeVgXZ^gd ^bedgiVciZcV^cYhig^VYZaVXi^Xc^dh# :bXdc_jcidXdbbjîdheVgXZ^gdhXdbZgX^V^h!fjZ gZegZhZciVbV;jc`Z"<ZgWZgcdhhZjhgZheZXi^kdh eVhZh!bVgXVYVedgjbVXddeZgVdYZXdcÒVcVfjZ eZgYjgV]{YXVYVh!V;jc`Z"<ZgWZgY^heZYVegZ" hZcV\adWVacZXZhh{g^VeVgV\VgVci^gdViZcY^bZcid YVhcZXZhh^YVYZhYdhXa^ZciZhXdbdhZfjêVbZcidh YZaVWdgVig^dcZXZhh{g^dh# 9ZhYZ&.%)!dcdbZ;jc`Z"<ZgWZggZegZhZciVfjVa^" YVYZ!XdcÒVWâ^YVYZZXdci^cj^YVYZ# + 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ PRODUCTOS: 7[cfh[iWZ[i[dlebl["\WXh_YW[Yec[hY_Wb_pWckdZ_Wbc[dj[ei i[]k_dj[iWfWh[bêiZ[bWXehWjh_e[WY[iih_ei0 IdYdhdhVeVgZa]dhZVXZhhg^dheVgVVÆYZiZgb^cVd<ZgWZgYdiZdgWji^gdhdÇ/ Y[djh_\k]WZehWi"XWdêi#cWh_W"b~cfWZWZ[YedikbjW"Xkj_hc[jhei 6eVgZa]dheVgVYZiZgb^cVdYdedcidYZXdc\ZaVdØ9hoeIjWhÇ 6eVgZa]dhYZVc{a^hZYdaZîZØBWYjeIjWhÇZØBWYje<bWi^Ç C[Z_Zeh[if> EgdYjXidh\ZgV^hYZaVWdgVig^d ACTIVIDADES: ?dijWbWeÇY^Wl[dWceÈekfhe`[YjeZ[bWXehWjh_eiYecfb[jei fWhWWii[]k_dj[i|h[WiZ[[if[Y_Wb_pWe >cYhig^VYZaVXi^Xc^dh AZîVg^Vh!XZcigdhYZgZXda]VYZaZîZ FjZ^_Vg^Vh!jc^YVYZhegdYjidgVhYZbVciZ^\V![{Wg^XVhYZ\ZaVYdh! 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V \dgYjgV a^WZgiV" YVhZeVgVYVVigVkhYVXZcig^[j\Vd!ZbfjZVVY^dYZ {aXddaVba^Xd[VXâîVVhZeVgVdYVh[VhZhZeZgbîZdWiZg jbVa^c]VYZhZeVgVdci^YVZcigZ\dgYjgVZhdajd{X^YV# CV ZhXVaV Yd Wji^gbZigd edhhkZa aZg d iZdg Wji^gdhd cd aZîZXdbdiZdgYZbVhhVhdWV[dgbVYZeZgXZciV\Zb# ÂMBITO DE APLICAÇÃO D egdXZhhd edYZ"hZ Vea^XVg eVgV aZîZ ejgd Z aZîZ YZ Xdchjbd Xdb iZdg Wji^gdhd YZ % V &+ ! eVgV aZîZ fjZ iZc]V h^Yd b^hijgVYdXdbjbV\ZciZXdchZgkVciZVYZfjVYd!WZbXdbdaZîZ]dbd\ZcZôVYd# 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ &( PRODUTOS QUÍMICOS NECESSÁRIOS &# ÜY_Zeikb\h_Ye">(IE* GZfj^hîdh/ 9Zch^YVYZV'%8 &!-&-¥%!%%(\ba Ä& HbWdadYZeZg^\d/ 8aVhh^[^XVdYZeZg^\dh/ 8'G(* H'"'+"(% • incolor ou apenas ligeiramente tingido e isento de componentes que influenciem o resultado CdiVh/ 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. '# ÜbYeebWcb_Ye eVgVVYZiZgb^cVdYdiZdgWji^gdhdhZ\jcYd<ZgWZg Mistura de isómeros 2-metilbutan-1-ol e 3-metilbutan-1-ol GZfj^hîdh/ 9Zch^YVYZV'%8 %!-&&¥%!%%(\ba Ä& • 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. HbWdadYZeZg^\d/ 8aVhh^[^XVdYZeZg^\dh/ McG&%"'% H')$'* KW;6>> CdiVh/ • 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. &) 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ EQUIPAMENTOS NECESSÁRIOS &#8kj_hc[jheYWb_XhWZeXdbgda]VVYZfjVYV 9>C&'-(+"6)!9>C&'-(+"6+!9>C&'-(+"6-!9>C"&'-(+"6* '#F_f[jW9>C&%'-("efWhWb[_j[djf_f[jW9>C&'-(,"6fWhWb[_j[ (#F_f[jW9>C&'-(,"7djjehd[_hWZ[c[Z_e'&cbfWhW|Y_Zeikb\h_Ye )#F_f[jW9>C&'-(,"8&baV[Zg^YVeVgV{aXddaVba^Xd *#9[djh_\k]WZehWfWhWZ[j[hc_dWeZej[ehXkj_heiedeb[_j[XdbXdciVYdgYZgdiVZh! VfjZXkZa# 6 XZcig^[j\VYdgV iZg{ YZ XdchZ\j^g dWiZg! hdW XVg\V b{m^bV Z d bV^h iVgYVg Veh'b^cjidh!jbVVXZaZgVdYZXZcig^[j\VdYZ(*%¥*%\cVeVgiZ^c[Zg^dgYVgda]V YdWji^gbZigd#8dbjbgV^dYZgdiVdYZe#Zm#'+¥%!*XbViVdaVYd^ciZg^dgYVgda]V YdWji^gbZigd!dfjZXdggZhedcYZ|Y^hi}cX^VZcigZdedcidYZgdiVdZVgda]VYdWji^g" bZigd!ZhiVVXZaZgVdVaXVcVYVXdbjbVgdiVdYZ&&%%¥-%b^cÄ&# +# :_ifei_j_le Z[ h[]kbWe ZW j[cf[hWjkhW fWhW Xkj_hc[jhei e#Zm# WVc]d"bVg^V +*¥'8#:bXdbW^cVdXdbjbVXZcig^[j\VYdgVVfjZX^YV!iVbWbedYZg{hZg jhVYVjbVbVc\VYVXZcig^[j\VYdgVeVgVVgZXda]VYdWji^gbZigdZbWVc]d"bVg^V# 9jgVciZVaZîjgV!ViZbeZgVijgVYZkZg{hZgYZ+*¥'8# PREPARAÇÃ O DA AMOSTRA DaZîZYZkZhZgVfjZX^Ydcd[gVhXdYZVbdhigVViVdh'%8Zb^hijgVYdXj^YVYdhV ZZmVjhi^kVbZciZVigVkhYZk^gV\Zch#6hh^b!YZkZg"hZdWiZgjbVY^hig^Wj^d]dbd" \cZVYV\dgYjgV!ZkîVcYd"hZ!XdcijYd!V[dgbVdYZZhejbVZbVc^[ZhiVZhYZ [dgbVdYZbVciZ^\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. HZVXVbVYVYZcViVhcdejYZghZgY^hig^WjYVYZ[dgbV]dbd\cZVYZhiV[dgbV! d aZîZYZkZhZgVfjZX^YdV (*Vi )%8V\îVcYdXj^YVYdhVbZciZ!VihZgdWi^YVV Y^hig^Wj^d]dbd\cZVYV\dgYjgV#:bhZ\j^YVZVciZhYVeêZiV\Zb!daZîZYZkZ hZgVggZ[ZX^YdeVgV'%8# 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. 6eh V gZ\jaVd YV iZbeZgVijgV! d aZîZ YZ^mVYd V gZedjhVg ( V ) b^cjidh eVgV Za^b^cVgdVgXdci^Yd# 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. 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ &* EXECUÇÃO DA ANÁLISE = PRESCRIÇÃO DE TRABALHO 9ZkZhZg[ZîVjbVYZiZgb^cVdYjeaVYZjbVbZhbVVbdhigVYZaZîZ &# 9ZkZb hZg XdadXVYdh ' Wji^gbZigdh cjb hjedgiZ hjedgiZ YZ Wji^gbZigd# &% ba YZ {X^Yd hja[g^Xd hd ^cigdYjo^Ydh cd Wji^gbZigd Xdb V idgcZ^gV YZ bZY^d! hZb fjZ d eZhXdd YdWji^gbZigdÒfjZbda]VYd#Ò\#& '# D [gVhXd YZ VbdhigV YZkZ hZg V\îVYd Xj^YVYdhVbZciZ igh V fjVigdkZoZh#>bZY^ViVbZciZYZed^h!YZkZbhZgeêZiVYdh&%!,* baYZaZîZeVgVdWji^gbZigd!YZbdYdfjZdeZhXddYdWji^g" bZigdcdÒfjZbda]VYdZcd]V_Vb^hijgVYdaZîZXdbd{X^Yd hja[g^Xd#EVgViVa!VedciVYVeêZiVYZaZîZZcXdhiVYVdbV^h egd[jcYVbZciZedhhkZacVWdgYVYdWji^gbZigdZdaZîZXdad" XVYdZbXVbVYVhdWgZd{X^Ydhja[g^Xd#Ò\#' 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. (# wVea^XVYd&baYZ{aXddaVba^XdhdWgZdaZîZVigVkhYVidgcZ^gV YZbZY^ddjeêZiV# ;^\#& 9jgVciZV^cigdYjdYd{X^Ydhja[g^XdYZkZbhZg jhVYdhXjadhYZegdiZXdZajkVhYZWdggVX]V Devido à baixa densidade do álcool amílico não haverá mistura dos líquidos. )# HZbb^hijgVgdhafj^Ydh!dWji^gbZigd[ZX]VYdXdbVgda]V# Por regra, a parte inferior da rolha mergulha no líquido. *# D Wji^gbZigd XdadXVYd cjbV bVc\V YZ Wji^gbZigd Xdb d WdaWd kdaiVYd eVgV WV^md# :b hZ\j^YV! d Wji^gbZigd V\îVYd k^\dgdhVbZciZ Vi fjZ d afj^Yd ZhiZ_V XdbeaZiVbZciZ b^hij" gVYd# 9jgVciZ ZhiZ egdXZhhd! d edaZ\Vg Xdbeg^bZ Xdb ÒgbZoV V gda]V Yd Wji^gbZigd# 6 k^gV\Zb gZeZi^YV Yd Wji^gbZigd YZhi^cV"hZ|Y^hig^Wj^dYd{X^Ydhja[g^XdfjZeZgbVcZXZjcd WdaWd#Ò\#( 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. ;^\#' &%!,*baYZaZîZhdeêZiVYdheVgVYZcigdYd Wji^gbZigd &+ 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ ;^\#( DWji^gbZigdZm^hiZciZcV bVc\VV\îVYdjhVgXjadhYZ egdiZXdZajkVhYZWdggVX]V Uma agitação demasiado suave ou uma inclinação desnecessária impede a rápida mistura e, assim, o rápido efeito de oxidação em todo o líquido e destrói o efeito da formação cuidadosa das diversas camadas. ;^\#) :cX]^bZcidYVXZcig^[j\VYdgV ;^\#* :bWVc]d"bVg^V!dhWji^gbZigdhhdXdadXVYdheVgV ViZbeZgVijgVYZXdchjaiVZmVXiV +# >bZY^ViVbZciZ Veh V V\îVd Z k^gV\Zb! dh Wji^gbZigdh V^cYV fjZciZhhd^chZg^YdhXdbVgda]VeVgVWV^mdcjbVea^fjZYZbVc\V YVXZcig^[j\VYdgVVfjZX^YVÒ\#)!cdfjVadhWji^gbZigdhibYZ ZhiVgY^hedhidhZmVXiVbZciZZbdedh^djbeVgVddjigd# 6ciZh! V XdajcV YZ \dgYjgV YZkZ! VigVkh YV gdiVd YV gda]V! hZg gZ\jaVYVeVgVVVaijgVYdiZdgWji^gdhdZheZgVYd# 6eh V gZ\jaVd Yd iZbed YZ XZcig^[j\Vd cV XZcig^[j\VYdgV! VXZcig^[j\VYdgVa^\VYV#FjVcYdi^kZgh^YdVaXVcVYVVkZadX^YVYZ YZ XZcig^[j\Vd YZ (*% ¥ *% \! Zb \ZgVa! Veh & b^cjid! V gZh" eZXi^kVgdiVdYZ&&%%¥*%edgb^cjidYZkZhZgbVci^YVYjgVciZ )b^cjidh# 6 XZcig^[j\VYdgV YZkZ ZhiVg ZfjêVYV Xdb jb [ZX]d YZ iVbeV# FjVcYdiZgb^cVgdiZbedYZXZcig^[j\Vd!dgdidgigVkVYdVjid" bVi^XVbZciZ# ,# :bhZ\j^YV!dhWji^gbZigdhhdgZi^gVYdhYVXZcig^[j\VYdgVhZb ^cXa^c{"adhZXdadXVYdh!XdbVgda]VeVgVWV^md!YjgVciZ*b^cjidh ZbWVc]d"bVg^VVfjZX^YdV+*8#Ò\#* 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. ;^\#+ 8dbdVjma^dYVa}beVYVYZXdchjaiVYZhZ\jgVcV! dhkVadgZhYZbZY^dedYZbhZgXdchjaiVYdhXdb hZ\jgVcVZegZX^hd 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ &, RESULTADO DE MEDIÇÃO E PRECISÃO -# 6eh V gZbdd Yd WVc]d"bVg^V! d Wji^gbZigd YZkZ hZg bVci^Yd ZaZkVYd Zb edh^dkZgi^XVa!YZbdYdfjZdbZc^hXdYVXdajcVYZ\dgYjgVhZZcXdcigZVd ckZaYdhda]dh#8dbdVjma^dYVgda]V!Va^c]VYZhZeVgVdYdafj^YdYZhdaj" WâôVd$\dgYjgVYZkZhZgV_jhiVYVeVgVjbVbVgXVYZ\gVYjVdYVZhXVaVYd Wji^gbZigdZVVaijgVYVXdajcVYZ\dgYjgVYZkZhZgXdchjaiVYVcdedcidbV^h WV^mdYdbZc^hXd#HZVaZîjgVYZbdgVgbjîd!dWji^gbZigdiZbYZhZgXdadXVYd cdkVbZciZZbWVc]d"bVg^V#Ò\#+!Ò\#, HZdda]dZdbZc^hXdYVXdajcVYZ\dgYjgVcdhZZcXdcigVgZb|bZhbVVaijgV! dXdggZdZggdYZeVgVaVmZ# BZc^hXd Da]d ;^\#, )!%" )!%" (!." (!." (!-" (!-" ;^\#,V/>cY^XVd)!%" ;^\#,W/>cY^XVd(!.*" D gZhjaiVYd edYZ hZg a^Yd Zb bZ^dh kVadgZh YZ ZhXVaV! ^hid ! Zb %!%* # JbgZhjaiVYdbV^hZmVXidcdedYZhZgdWi^YdcdhWji^gbZigdhYZaZîZ^ciZ\gVa#HZ dbZc^hXdidXVgcVbVgXVYZ\gVYjVd!Zcidk{a^YddgZhjaiVYda^YdÒ\jgV,V# HZdbZc^hXdXdgiVgVbVgXVYZ\gVYjVd!ZcidhZg{^cY^XVYddkVadgbV^hWV^md Ò\jgV,W# 6hYZiZgb^cVZhYjeaVhcdYZkZbY^kZg\^gbV^hYdfjZ%!&%!^hid!VXVeVX^" YVYZYZgZeZi^dYZ%!&%# 6^cY^XVdYdgZhjaiVYdYZkZXdciZgVVY^dÆIZdgWji^gdhdhZ\jcYd<ZgWZgÇ#HZV VbdhigVYjeaVY^kZg\^gZb%!&!^cY^XVYddkVadgbY^dYVYZiZgb^cVdYjeaV# 6bdhigV&/)!'%q6bdhigV'/)!(%qGZhjaiVYd/)!'*<dgYjgV HZ! cd ZciVcid! cV VbdhigV YjeaV [dgZb a^Ydh )!'% Z )!'* YZ \dgYjgV! Zcid hZ Vea^XV! hZ\jcYd d Æeg^cXe^d YV egZXVjdÇ! d kVadg bV^h WV^md YZ )!'% Xdbd gZhjaiVYdYVVc{a^hZ# &- 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ :[j[hc_dWeZej[ehXkj_heieZ[b[_j[êce][d[_pWZei[]kdZe=[hX[h EVgV^beZY^gV[dgbVdYZcViV!daZîZYZXdchjbd]dbd\ZcZôVYd#9jgVciZZhiZ egdXZhhd!VhZh[ZgVhYZ\dgYjgVYZY^[ZgZciZhiVbVc]dhhdgZYjo^YVheVgVjbY^}" bZigd egVi^XVbZciZ ^\jVa YZ & Vi ' b^XgbZigdh# D Z[Zîd YZ hZeVgVd YjgVciZ V XZcig^[j\Vd ÒXV WVhiVciZ gZYjo^Yd YZk^Yd V ^hhd# EVgV hZeVgVg XdbeaZiVbZciZ V \dgYjgVa^WZgiVYV!hdcZXZhh{g^dheZgdYdhYZXZcig^[j\VdbV^hadc\dh# Hd gZVaôVYVh Vh [VhZh YZ egdXZhhVbZcid & Vi- iVa Xdbd cV Vc{a^hZ YZ aZîZ cd ]dbd\ZcZôVYdZdgZhjaiVYdVedciVYd# 9Zed^h!dWji^gbZigdVfjZX^YdcdkVbZciZ!cdbc^bd!*b^cjidhZbWVc]d"bVg^V V+*8Z!ZbhZ\j^YV!cdkVbZciZXZcig^[j\VYdYjgVciZ*b^cjidhZdgZhjaiVYdXdc" hjaiVYdXdbdVciZg^dgbZciZ# HZdkVadgdWi^YdVehVhZ\jcYVXZcig^[j\VdhZhîjVgbV^hYdfjZ%!%*VX^bVYd kVadgYVeg^bZ^gVXZcig^[j\Vd!ZciddgZVfjZX^bZcidZVXZcig^[j\VdYZkZbhZg gZeZi^Ydh!cdb{m^bd!bV^hYjVhkZoZh# 8dcijYd!hZdkVadgi^kZgVjbZciVYdVeZcVh%!%*djbZcdhZbgZaVdVdeg^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\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ &. 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^cVdYdiZdgWji^gdhdcdaZîZZY^kZghdhegdYjidha{XiZdh# 2.0 VOLUMES HZcd]djkZgcVYVYZhXgîdZbXdcig{g^d!hdhZbegZk{a^YVhVhhZ\j^ciZh fjVci^YVYZheVgVdhegdYjidhfjb^XdhZVbdhigVhYZVc{a^hZjiâôVYVh/ ÛX^Ydhja[g^Xd/ &%!%ba'%8 '8 ÛaXddaVba^Xd/ &!%ba'%8 '8 AZîZdjegdYjida{XiZd/ &%!,*ba'%8 '8 3.0 BREVES DESCRIÇÕES DA DETERMINAÇÃO DO TEOR BUTIROSO 3.1 ... NO LEITE (SEGUNDO GERBER): Wji^gbZigdh YZ aZîZ ^beZXVkZabZciZ a^bedh! ZheZX^VabZciZ hZb gZhYjdh YZ \dg" YjgV!hdZcX]^YdhcVhZ\j^ciZdgYZb/&%baYZ{X^Ydhja[g^XdYZch^YVYZ/&!-&- $" %!%%(\$ba!&%!,*baYZaZîZZ&baYZ{aXddaVba^Xd#DaZîZZd{aXddaVba^XdYZkZb hZg^cigdYjo^Ydh[dgbVcYdXVbVYVhY^[ZgZciZh!YZbdYdfjZcddXdggVjbVb^hijgV VciZh YV V\îVd# 6eh d [ZX]d! d iZdg Yd Wji^gbZigd WZb b^hijgVYd VigVkh YV V\îVdZY^kZghVhk^gV\Zch#6igVkhYZjbVgZ\jaVdXj^YVYdhVYVgda]V!diZdgYd Wji^gbZigdgZ\jaVYdYZbdYdfjZVZhXVaVÒfjZX]Z^V!bVhcd]V_Vafj^YdcdWda" Wd#8Zcig^[j\VgdWji^gbZigdcVXZcig^[j\VYdgVVfjZX^YV!YZ^mVgVfjZXZg*b^cjidhV +* 8 Zb WVc]d"bVg^V! V_jhiVg V a^c]V YZ hZeVgVd YV b^hijgV YZ {X^Yd hja[g^Xd$ XdajcVYZ\dgYjgVeVgVjbVbVgXVYZ\gVYjVdXdbeaZiV!XdchjaiVgVZmigZb^YVYZ hjeZg^dgYVXdajcVYZ\dgYjgVcdbZc^hXd^c[Zg^dg# 3.2 ... EM LEITE HOMOGENEIZADO Xdbd YZhXgîd VX^bV! bVh XZcig^[j\Vg igh kZoZh! * b^cjidh YZ XVYV kZo# :cigZ Vh XZcig^[j\VZh! dh Wji^gbZigdh 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\Vd YjeaV Xdb XdadXVd ^ciZgbîZciZ Ydh Wji^gbZigdh * b^cjidh Zb WVc]d"bVg^VV+*8# 3.4 ... EM LEITE CONDENSADO (NÃO AÇUCARADO) DaZîZXdcYZchVYdVfjZX^YdegZk^VbZciZV*%8Z!YZed^h!cdkVbZciZVggZ[ZX^Ydb^hijgVYd Xdb {\jV cjbV gZaVd YZ &/&# :hiV Yâj^d VcVa^hVYV Xdbd aZîZ hZ\jcYd <ZgWZg# IZdg Wji^gdhd2kVadga^Ydm'# '% 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ 3.5 ... EM SORO DE MANTEIGA (MODIFICAÇÃO SEGUNDO MOHR E BAUR) DWji^gbZigdX]Z^dXdb&%baYZ{X^Ydhja[g^XdYZch^YVYZ&!-(% $"%!%%(\$ba#:b kZoYZ&%!,*ba!hdeêZiVYdh&%baYZhdgdYZbVciZ^\VZ'!%baYZ{aXddaVba^Xd#6eh d[ZX]dYdhWji^gbZigdh!V\î{"adhZXZcig^[j\Vg^bZY^ViVbZciZedg&%b^c#9ZhiZbdYd ZkîVYVVeZgijgWVYdgV[dgbVdYZgda]V#6aZîjgVdXdggZVeZcVhVeh*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^gbZigd X]Z^d Xdb &% ba YZ {X^Yd hja[g^Xd YZch^YVYZ/ &!-&- $" %!%%( \$ba# HdWgZZhiZhhdXdadXVYdhZbXVbVYV,!*baYZ{\jVZ&baYZ{aXddaVba^Xd#CjbV aVcVYZ^gVYZeZhV\ZbhdeZhVYdh'!*\YZaZîZZbeZ^cigdYjo^YdhVigVkhYZjb [jcâjhVcYdjbe^cXZaÒcdeVgVYZcigdYdWji^gbZigd#DWji^gbZigdV\îVYdZmVjhi^" kVbZciZVehZhiVg[ZX]VYdZXdadXVYd^ciZgbîZciZbZciZY^kZghVhkZoZhZbWVc]d"bV" g^VV+*8!XZcig^[j\Vg'm*b^c#cVXZcig^[j\VYdgVVfjZX^YVZegdXZYZg|aZîjgVVehV XdadXVdZbWVc]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#6igVkhYVVWZgijgVhjeZg^dgYdWji^gbZigd^cigdYjo^Yd{X^Ydhja[g^XdYZc" h^YVYZ/&!*'' $"%!%%*\$baVigVkhYVWdgYVhjeZg^dgYdXdedYZk^Ygd#6ehd[ZX]d! dWji^gbZigdXdadXVYdZbWVc]d"bVg^VV,%8YjgVciZjbVV\îVdgZeZi^YVVi| Y^hhdajdXdbeaZiVYVhegdiZcVh#6i|VaijgVYd^cX^dYVZhXVaVVY^X^dcVYd{X^Yd hja[g^XdZ!YZed^h!&baYZ{aXddaVba^Xd!dWji^gbZigd[ZX]VYd!V\îVYdZYjgVciZbV^h *b^cjidhXdadXVYdZbWVc]d"bVg^VV,%8#:bhZ\j^YV/XZcig^[j\Vg*b^c#Z!YZed^h! VfjZXZgV+*8ZbWVc]d"bVg^V#6XdchjaiV[ZîVV+*8!V_jhiZYdiZdgWji^gdhdeVgV dedcidoZgd!aZîjgVcdbZc^hXd^c[Zg^dg# 3.8 ... EM NATA SEGUNDO SCHULZ-KLEY (MÉTODO DE PESAGEM) Utilização de butirómetro de nata segundo Schulz. CdWji^gbZigdhd^cigdYjo^YdhhjXZhh^kVbZciZ/&%baYZ{X^Ydhja[g^XdYZch^YV" YZ/&!-&- $"%!%%(\$ba!*baYZ{\jV!Vegdm#*\YZcViVeZhVYdhVigVkhYZeZhV" \ZbY^[ZgZcX^VaXdbjbVhZg^c\VZbWVaVcVdjeêZiVYZeZhV\Zb!&baYZ{aXdda Vba^Xd#6eh[ZX]VYddWji^gbZigd!dXdciZYdb^hijgVYdedgV\îVdZk^gV\Zch! ZdWji^gbZigdXZcig^[j\VYdZbXZcig^[j\VYdgVVfjZX^YVYjgVciZ*b^cjidh#6aZ^" ijgVgZVaôVYVVeh*b^cjidhYZVfjZX^bZcidZbWVc]d"bVg^VV+*8#6iZcd/ YZk^Yd|edhh^Wâ^YVYZYZgZYjdYdXVadgYZgZVXdVigVkhYVVY^dYZ{\jV!cd YZkZbhZgYZXdgg^YdhbV^hYZ&*b^cjidhZcigZdZcX]^bZcidXdb{\jVZVV\îVd! degdXZY^bZcidYZY^hhdajdYZkZhZgXdcXajYdZbcdb{m^bd+%hZ\# IZdgWji^gdhd2kVadga^Ydm*$bVhhVYZcViV# 3.9 ... EM NATA SEGUNDO KÖHLER (MÉTODO DE MEDIÇÃO) Utilização de butirómetro de nata segundo Köhler. Cd Wji^gbZigd YZ cViVh hd ^cigdYjo^Ydh hjXZhh^kVbZciZ/ &% ba YZ {X^Yd hja[g^Xd YZch^YVYZ/&!-&- $"%!%%(\$ba!*!%*baYZcViV!*baYZ{\jV!&baYZ{aXddaVba^Xd# 6igVkhYVjiâôVdYZjbVhZg^c\VYZcViVh!YZkZ"hZ!VciZhYVVY^dYdh*baYZ {\jV!aVkVgVhZg^c\VeZadZcX]^bZcidgZeZi^YdXdb{\jV#DWji^gbZigd[ZX]VYd! V\îVYd!XZcig^[j\VYdedg*b^cjidh!Za^YdVeh*b^cjidhYZVfjZX^bZcidZbWVc]d" bVg^VV+*8#6aZîjgV[ZîVVeVgi^gYdedcidoZgd# 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ '& 3.10 ... EM QUEIJO SEGUNDO VAN GULIK (MÉTODO DE PESAGEM) (consultar ISO 3433) Utilização de butirómetro de queijo segundo van Gulik. CdWji^gbZigdkVc<ja^`[ZX]VYdcdaVYdYdÒbYVZhXVaV!VehV^cigdYjdYZ Vegdm^bVYVbZciZ &* ba YZ {X^Yd hja[g^Xd YZch^YVYZ/ &!*'' $" %!%%* \$ba! ( \ $"%!'\YZfjZ^_dVigVkhYZaVcVYZ^gVYZeZhV\ZbZe^cXZaÒcd!hZcYd!YZed^h! [ZX]VYdddg^[X^dYZ^cigdYjd#6hVbdhigVhYZfjZ^_deVhidhVhibYZhZgeZhV" YVhcdXdedYZk^YgdeZg[jgVYdeZgiZcXZciZVdWji^gbZigdYZkVc<ja^`Z^cigdYj" o^YVhcdWji^gbZigd#DWji^gbZigd[ZX]VYdXdadXVYd!XdbVZhXVaVeVgVX^bV! ZbWVc]d"bVg^VV,%8"-%8ZV\îVYdY^kZghVhkZoZhVi|XdbeaZiVY^hhdajd YdfjZ^_d#:bhZ\j^YV!VigVkhYVVWZgijgVYVZhXVaVVY^X^dcVYd&baYZ{aXdda Vba^XdZ!YZed^h!{X^Ydhja[g^XdVegdm^bVYVbZciZVi|bVgXVYdh&*YVZhXVaV# :bhZ\j^YV[ZX]VYd!b^hijgVYd!VfjZX^YdYjgVciZX^cXdb^cjidhZbWVc]d"bVg^V V+*8ZXZcig^[j\VdYjgVciZ*b^cjidh0cdkVXdadXVdZbWVc]d"bVg^VV+8! V_jhiZYVXdajcVYZ\dgYjgVeVgVVbVgXVoZgdZaZîjgVYdiZdgWji^gdhdVWhdajid# 6aZîjgV[ZîVcVZmigZb^YVYZ^c[Zg^dgYdbZc^hXd#IZdgWji^gdhd2kVadga^Ydm($ bVhhVYZfjZ^_d# 3.11 ... EM GELADO SEGUNDO KÖHLER (MÉTODO DE MEDIÇÃO) Utilização de butirómetro de gelado segundo Köhler. :kZcijV^h XdWZgijgVh dj eVgiXjaVh 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!VigVkhYZVea^XVd YZk{Xjd#CdWji^gbZigdYZ\ZaVYdhhd^cigdYjo^YdhhjXZhh^kVbZciZ/&%baYZ {X^Ydhja[g^XdYZch^YVYZ/&!-&- $"%!%%(\$ba!*baYZ\ZaVYd!*baYZ{\jV!& baYZ{aXddaYZVba^Xd#CVjiâôVdYZjbVhZg^c\V!YZkZ"hZ!VciZhYVVY^dYdh *baYZ{\jV!aVkVgVhZg^c\VeZadZcX]^bZcidgZeZi^YdXdb{\jV#HZdWji^gbZigd cdZhi^kZgXdbeaZiVbZciZX]Z^d!edYZ"hZVY^X^dcVgVi'baYZ{\jV#DWji^gbZ" igd[ZX]VYd!V\îVYd!XZcig^[j\VYdYjgVciZ*b^cjidhZa^Yd!Veh*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^gbZigd#6igVkhYVVWZgijgVhjeZg^dgYdWji^gbZigd^cigdYjo^Yd{X^Yd hja[g^XdYZch^YVYZ/&!*'' $"%!%%*\$baVigVkhYVWdgYVhjeZg^dgYdXdedYZk^Ygd# 6ehd[ZX]d!dWji^gbZigdXdadXVYdZbWVc]d"bVg^VV,%8YjgVciZjbVV\îVdgZ" eZi^YVVi|Y^hhdajdXdbeaZiVYVhegdiZcVh#wVY^X^dcVYd&baYZ{aXddaVba^XdZ!Vi |bVgXVYdh&%cVZhXVaV!{X^Ydhja[g^Xd!dWji^gbZigd[ZX]VYd!V\îVYdZYjgVciZ bV^h&%b^cjidhXdadXVYdZbWVc]d"bVg^VV,%8#9jgVciZZhiZiZbed!dhXdbedcZciZh hdV\îVYdhZb^ciZgkVadhgZ\jaVgZh#:bhZ\j^YV/XZcig^[j\Vg,b^c#Z!YZed^h!VfjZXZg V+*8ZbWVc]d"bVg^V#6aZîjgV[ZîVV+*8!V_jhiZYdiZdgWji^gdhdeVgVdedcidoZgd! aZîjgVcdbZc^hXd^c[Zg^dg# 3.13 ... EM MANTEIGA SEGUNDO ROEDER (MÉTODO DE PESAGEM) Utilização de butirómetro de manteiga segundo Roeder. 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EêZiV/Vegdeg^VYVeVgVdYZheZ_dYZ&baYZhdajdYZhja[VidYZXdWgZ'#'# (#&% 7VadYZ:gaZcbZnZg!kdajbZcdb^cVa*%%ba *$Fh[fWhWe 6VbdhigVYZaZîZVfjZX^YVZbjbWVc]d"bVg^VV(-¥&8!aZkZbZciZb^hijgVYV!cdkVbZciZgZh[g^VYVViZbeZgVijgV VbW^ZciZ!Z*¥%!&\hdeZhVYdhcdWVadYZhdajWâôVdXdbegZX^hdYZ%!&b\# +$FheY[Z_c[dje 1 IebkX_b_pWe IZbedidiVaYZhdajWâôVd/&!,*Ä'!*]#7j[de0fheY[Z[hWf[dWiieXYWf[bW EgdiZcVh ='HD) @'HD) 8jHD)¬C=)'HD) Cd WVad YZ hdajWâôVd hd VY^X^dcVYdh &' \ YZ hja[Vid YZ edi{hh^d! & ba YZ hdajd YZ hja[Vid YZ XdWgZ '#'! * ¥ %!& \ YZ VbdhigV YZ aZîZ VfjZX^YV Z b^hijgVYV Z '% ba YZ {X^Yd hja[g^Xd# V fjVci^YVYZ ZmViV YZ aZîZ YZkZ hZg YZiZgb^cVYV Xdb egZX^hd YZ ¥%!&b\ZVcdiVYV!ed^hhZgk^g{XdbWVhZeVgVdX{aXjad Ydcîgd\c^d#KZgÆ8{aXjadÇ#DWVadYZhdajWâôVd b^hijgVYdXj^YVYdhVbZciZ#CdVeVgVidYZhdajWâôVd ZhXda]^Yd jb egd\gVbV YZ iZbeZgVijgV VYZfjVYd Z ZbhZ\j^YVdWVadYZhdajWâôVdedhidhdWgZdWadXd YZVfjZX^bZcid#6XVYVWVadYZhdajWâôVdÒmVYd Xj^YVYdhVbZciZ jb XdaZXidg YZ \VhZh YZ ZhXVeZ Zb k^Ygd#DVeVgVid^ciZ^gda^\VYdVigVkhYZjbVbVc\jZ^gV V jb hZ\jcYd VeVgVid 7Z]gdhd\ (! Vgi# c#d/ )'%(! XVeVoYZcZjigVaôVgkVedgZheZg^\dhdh#GZXdbZcYV"hZ hZaZXX^dcVgdhZ\j^ciZegd\gVbVYZiZbeZgVijgV/ &Eg"VfjZXZgdWadXdYZVfjZX^bZcid edg&%b^cV'%%8 '6fjZXZgVVbdhigVVegdm#(%b^c#V'%%8# (EgdXZYZgedgVegdm#.%b^c#V)'%8eVgV hdajWâôVdVjbiVmVYZ&%8$b^c# DiZbedYZhdajWâôVdYZkZhZgV_jhiVYdYZ[dgbViVa fjZ fjVci^YVYZh b{m^bVh YZ cîgd\c^d hZ_Vb dWi^YVh# IZbedh YZ hdajWâôVd bjîd Xjgidh dj bjîd adc\dh edYZb aZkVg V kVadgZh ZcXdcigVYdh bV^h WV^mdh# 6eh V hdajWâôVd!VhVbdhigVhhdgZi^gVYVhYdWadXdYZVfjZ" X^bZcidZgZh[g^VYVhedg'*b^cViZbeZgVijgVVbW^ZciZ# :bhZ\j^YV!ZaVhhdigVo^YVhVdVeVgVidYZYZhiâVd# 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. 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ *, DETERMINAÇÃO DE NITROGÉNIO SEGUNDO KJELDAHL 2 :[ij_bWe IZbedidiVaYZYZhiâVd/*",b^c A^WZgVdYZVbdcVXd 6WhdgdYZVbdcVXd C=)'HD) 'CVD=¤CV'HD) 'C=)D= C=)D= =(7D(¤='D C=)='7D( CdVeVgVidYZYZhiâVdhdegd\gVb{kZ^hVhfjVci^YVYZhYZ{\jVZhdYV X{jhi^XV! iZbed YZ gZVXd! iZbed YZ YZhiâVd! XVeVX^YVYZ YZ VfjZX^" bZcidYd\ZgVYdgYZkVedgZdiZbedYZhjXdeVgVdgZhYjdYZVbdhigV YZhiâVYd#6igVkhYZ\^gdYdWdidZcXdcigV"hZdbZcjYZhZ_VYdZegZhh^d" cVcYd"hZ!ZhiZZhXda]^Yd#Jbcdkd\^gdbjYVdkVadgZdegZhh^dcVbZcid XdchZXji^kddhVakV# DVeVgVidYZYZhiâVdYZkZhZgejg\VYdYZVg!XVhdcdiZc]Vh^YdjhVYd edgbjîdiZbed!djXVhdhZ_VVeg^bZ^gVjiâôVd#EVgV^hhd!hZaZXX^dcV"hZ dbZcjeg^cXêVaDeZhZZcid:cigVYVY^gZiV#Eg^bZ^gdYZkZ"hZhZaZXX^d" cVgÆ='DcVVbdhigVÇZbVciZgdWdidegZhh^dcVYdVifjZ{\jVhZ_VkZgi^YV cdZfjêVbZcidYZhdajWâôVd#:cidhZaZXX^dcV"hZÆCVD=ÇZegZhh^dcV"hZ VifjZhdYVX{jhi^XVhZ_VkZgi^YVcdgZXê^ZciZYZhdajWâôVd#;^cVabZciZ hZaZXX^dcV"hZVigVkhYZÆ6Y^VciZÇdbZcjÆHjXdÇZegZhh^dcV"hZdWdid YZXdbVcYdVifjZdhegdYjXidhfjb^XdhhZ_VbhjXX^dcVYdhYdgZXê^ZciZ YZhdajWâôVd#8db^hhdiZgb^cVdegdXZY^bZcidYZejg\VYZVg# 9^Vg^VbZciZ! VciZh Yd ^cX^d YV YZhiâVd! YZkZ"hZ iVbWb gZVaôVg jbV Xdgg^YVYZiZhiZhZbVbdhigV#EVgV^hhdVXdeaV"hZVbVc\jZ^gVYZ^cigdYj" dcdgZXê^ZciZYZhdajWâôVd!hZaZXX^dcV"hZdbZcjeg^cXêVaÆDeZhÇ ZZcidÆ:cigVYVY^gZiVÇ#Eg^bZ^gdYZkZ"hZhZaZXX^dcVgÆKVedgÇ#6igVkhYZ cdkdegZhh^dcVbZcidXjgidYdWdidYZXdbVcYd!VZcigVYVYZkVedg^c^" X^VYV#CdkdegZhh^dcVbZcidYdWdidiZgb^cVdegdXZhhd#9ZkZ"hZiZgb^" cVgdegdXZhhdhdbZciZVeh]VkZg&XbYZYZhiâVYdcdWVad:gaZcbZnZg# ;^cVabZciZhZaZXX^dcV"hZÆHjXdÇZegZhh^dcV"hZdWdidYZXdbVcYdVi fjZV{\jVhZ_VhjXX^dcVYVYdgZXê^ZciZYZhdajWâôVd# 6ehVejg\VYZVgZYVXdgg^YVYZiZhiZ!egdXZYZ"hZXdbVYZhiâVdYV VbdhigV#6WV^mdYdYgZcdYdVeVgVidYZYZhiâVdXdadXV"hZjbWVadYZ :gaZcbZnZgYZ*%%baeVgVVhdajdYZ{X^YdWg^Xd#8dbdbZcjÆHiVgiÇ! ^c^X^V"hZdegd\gVbVYZYZhiâVd#GZXdbZcYV"hZZmZXjiVgdhZ\j^ciZegd" \gVbVYZYZhiâVd/ Û\jVW^YZhi/ ,%ba*hZ\# CVD=/ ,%baYZhdajd(%,hZ\# IZbedYZYZhiâVd/ *b^c 8VeVX^YVYZYZkVedg/ .% HjXdYVVbdhigV/ (%hZ\# 6Y^dYZ{X^YdWg^Xd/*%ba)hZ\# 6 YZhiâVd YZ kVedg YZ {\jV ^c^X^VYV Z d VbdcVXd a^WZgVYd YZk^Yd | VY^d YZ hdYV X{jhi^XV hdWgZYZhiâVYd Xdb kVedg# D YZhiâVYd VWhdgk^Yd cV hdajd YZ {X^Yd Wg^Xd# 9Zed^h YZ YZXdgg^Yd d egd\gVbV YZ YZhiâVd! d gZXê^ZciZ YZ hdajWâôVd gZbdk^Yd! V bVc\jZ^gV YZ hVYVYZYZhiâVYdaVkVYVXdb{\jVYZhiâVYVZdWVad:gaZcbZnZgXdb VVbdhigVgZbdk^YdYdVeVgVid# *- 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ CdidfjZZbcZc]jbVeVgiZYdVeVgVid YZYZhiâVdYjgVciZVYZhiâVd!cZb edgjb^ciZgkVadYZiZbedVehVbZhbV# 6heVgiZhedYZbZhiVgfjZciZh# 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. 3 J_jkbWe'c_d C=)='7D( =8a¤C=)8a =(7D( 6 hdajd YZ VWhdgd YZ {X^Yd Wg^Xd XdciZcYd d ^cY^" XVYdg iîjaVYV Xdb hdajd eVYgd YZ {X^Yd XadgYg^Xd %!& B# D {X^Yd XadgYg^Xd VY^X^dcVYd Vi fjZ d eg^bZ^gd igVdYZXdadgVdgdhVVeVgZV#DkdajbZYZ{X^YdXadg" Yg^XdjhVYda^YdcVWjgZiVXdbegZX^hdYZ%!%*ba#JbV eaVXVâjb^cVYVedYZhZgk^gXdbd[jcYdcZjigdZedhh^Wâ^" iVVdjhj{g^dVYZiZgb^cVdZmViVYVbjYVcVYZXdgcd ÒcVaYZiîjaVd# 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. J[ij[Y[]e DiZhiZXZ\dZmZXjiVYdXdbdbZhbdegdXZY^bZcid YZhXgîd VX^bV# 6 VbdhigV hjWhiîjYV edg * ba YZ{\jVZ%!-*\YZhVXVgdhZ#6cdiV"hZdkdajbZ YZ{X^YdXadgYg^XdjhVYdcViîjaVd# O teste cego é importante para o cálculo do teor de nitrogénio. 9|bYkbe[WlWb_We DiZdgYZcîgd\c^d!ZheZX^ÒXVYdZb\YZcîgd\c^d edg&%%\YZegdYjXid!XVaXjaVYdhZ\jcYdVhZ\j^ciZ [gbjaV/ Md0iZdgYZcîgd\c^dYVVbdhigV L0 kdajbZYZhdajdYZ{X^YdXadgYg^XdjhVYdcV iîjaVdYVVbdhigV Le0kdajbZYZhdajdYZ{X^YdXadgYg^XdjhVYdcV iîjaVdYVVbdhigVXZ\VkZgIZhiZXZ\d 9i0XdcXZcigVdbdaVgZmViVYd{X^YdXadgYg^Xd! ZheZX^ÒXVYdVifjVigdXVhVhYZX^bV^h Mj0bVhhVYVVbdhigVZb\gVbVhZheZX^ÒXVYVXdb egZX^hdVi%!&b\# EVgVXVaXjaVgdiZdgYZegdiZcVhYVVbdhigV!YZkZ"hZ bjaiêa^XVgdkVadgLceZad[VXidg+!(-# ;n[cfbeZ[Y|bYkbe HZVYZiZgb^cVdYZ@_ZaYV]agZhjaidjZbjbiZdgYZ cîgd\c^dYZ**!ZciddiZdgZbegdiZcVhYZ(!*/ %!**m+!(- 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). 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ *. DETERMINAÇÃO DE NITROGÉNIO SEGUNDO KJELDAHL CjeZeWbj[hdWj_le"h|f_Ze :m^hiZjbegdXZY^bZcidYZZmZXjdbV^hg{e^YV!cVYZiZgb^cVd YZ @_ZaYV]a! fjZ d egdXZhhd eVYgd# 9Z VXdgYd Xdb V cdgbV >HD-.+-"(!hdjhVYVhfjVci^YVYZhbZcdgZhYZVbdhigVYZaZîZ '\eZhVYVhXdbegZX^hdYZ&b\#:bjbWVadYZhdajWâôVd YZ '*% ba hd ^cigdYjo^Ydh dh ' \ YZ VbdhigV! jb iVWaZiZ YZXViVa^hVYdgXdbedhidYZ*\@'HD)!%!&%*\8jHD)*='DZ%!&%* \I^D'!&%baYZ{X^Ydhja[g^Xd.-!Va\jbVh\diVhYZV\ZciZ Vci^ZhejbVciZ (% YZ egZeVgVYd YZ hâ^XdcZ# B^hijgV"hZ Xj^YVYdhVbZciZ!ZheZgV"hZ*b^cZYZed^hhZYZ^mVZhXdggZgYZ [dgbVWVhiVciZXj^YVYdhVZaZciV*baYZeZgm^YdYZ]^Ygd\c^d (%eZaVheVgZYZhYdgZXê^ZciZ#6ciZhYVhdajWâôVd!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^YVVVbdhigVgZh[g^VYVViZbeZgVijgV VbW^ZciZZYâjYVXdb*%baYZ{\jV#CVYZhiâVdhdjhVYdh **baYZCVD=(%Z*%baYZ{X^YdWg^Xd)eVgVVWhdgd Yd YZhiâVYd# IîjaV"hZ Xdb =8a %!%* B# 8dbd ^cY^XVYdg jhV"hZ %!' ba YZ jbV b^hijgV YZ kZgbZa]d YZ bZiâV %!%( Z kZgYZ WgdbdXgZhda%!&,ZbZiVcda.*# 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. Ced_jehWeZefheY[iie 6VhhZgi^k^YVYZYdegdXZhhdYZkZhZggZ\jaVgbZciZXdbegdkVYV# 9ZkZ"hZ iZhiVg hZ ]{ jbV eZgYV YZ cîgd\c^d# 8dbd VbdhigV jhV"hZ eVgV ^hhd %!&' \ YZ hja[Vid YZ Vbc^d PC=)'HD)R _jcid Xdb%!-*\YZhVXVgdhZ#6YZiZgb^cVdYZ@_ZaYV]aZmZXjiVYV hdW Vh bZhbVh XdcY^Zh fjZ eVgV VbdhigVh cdgbV^h Z d iZdg eZgXZcijVaZbcîgd\c^dYZkZZcXdcigVg"hZZcigZ..!%Z&%%#6 YZiZgb^cVdXdbhja[VidYZVbc^dhZgkZeVgVYZhXdWg^geZgYVh YZcîgd\c^dYjgVciZVhdajWâôVddjYZhiâVdZY^[ZgZcVh YZXdcXZcigVdYdV\ZciZYZiîjaVd# 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. :[j[hc_dWeZej[ehZ[d_jhe]d_eZ[fheZkYjeiZ[b[_j[ DegdXZY^bZcideVYgdYZgZ[ZgcX^ViVbWbedYZhZgVYVeiVYdeVgVdjigdhegdYjXidhYZaZîZ DbidYdkVg^VVeZcVhcVfjVci^YVYZYZVbdhigV#6VbdhigVYZkZXdciZgjbVfjVci^YVYZYZegdiZcVhZcigZ%!&*Z%!(%\# Edg^hhd!gZXdbZcYV"hZjiâôVgVhhZ\j^ciZhfjVci^YVYZhYZVbdhigV# AZîZXdcYZchVYd/ (\ AZîZZbebV\gd/ &\ HdgdYZaZîZ/ &%\ FjZ^_d[gZhXd/ (\ DbidYdZmZXjiVYdXdbdcdegdXZY^bZcideVYgd# +% 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ 7fWhWjeZ[iebkX_b_pWeZ[A`[bZW^bA. 7adXdYZVfjZX^bZcidZh^hiZbVYZhjXdZbk^Ygd eVgV-VbdhigVheVgVXdcZmd|ZhiVdYZhjXd 7Z]gdhd\#8dbeVikZaXdbWVadYZhdajWâôVd YZ'*%ba#DaVYd[gdciVaYdhjedgiZYZVbdhigVh XdWZgid#8dchigjdZhi{kZaZgdWjhiV#IVcidV VgbVdYdWadXdXdbdiVbWbdhjedgiZeVgVdh gZXê^ZciZhYZhdajWâôVdZVXVeZaVYZhjXdhd YZVd^cdm^Y{kZa!gZh^hiZciZV{X^Ydh# Egd\gVb{kZaVi&%YZ\gVjh YZiZbeZgVijgVY^[ZgZciZh# IZbeZgVijgVb{m^bV)*%8! 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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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EgZX^hd¥%!(8 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ SENSOR DE PERFURAÇÃO / IMERSÃO I[diehZ[fh[Y_iegdWjhid 7122 £)bb!Xdbeg^bZcid&&%bb I[diehZ[Wb_c[djei ZbVd^cdm^Y{kZa! 7123 £)bb!Xdbeg^bZcid&'*bb I[diehZ[W]kb^W eVgVbZY^Zhg{e^YVh hZb[jgdk^hkZa! 7124 £&!)bb!Xdbeg^bZcid&*%bb I[diehZ[Yed][bWZeh[i 7125 ojb:^chX]gVjWZcd]cZKdgWd]gZc! £-bb!Xdbeg^bZcid&&%bb JefIW\[ 7127 8VeVYZegdiZXdXdcigVhj_^YVYZ! {\jVZ^beVXidh 8Vi{ad\dYZaVWdgVig^deVgVVc{a^hZhYZaZîZ -. DETERMINAÇÃO DO PONTO DE CONGELAÇÃO 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. 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Análises de Leite - Funke-Dr.N.Gerber Labortechnik GmbH / Milch

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