{"id":3899,"date":"2025-09-04T10:56:14","date_gmt":"2025-09-04T02:56:14","guid":{"rendered":"https:\/\/www.pgeneral.com\/?p=3899"},"modified":"2025-09-04T10:56:14","modified_gmt":"2025-09-04T02:56:14","slug":"determination-of-lead-in-olive-oil-graphite-furnace-atomic-absorption-spectrometry","status":"publish","type":"post","link":"https:\/\/www.pgeneral.com\/tr\/basvuru\/determination-of-lead-in-olive-oil-graphite-furnace-atomic-absorption-spectrometry\/","title":{"rendered":"Zeytinya\u011f\u0131ndaki Kur\u015fun Belirlenmesi (Grafit F\u0131r\u0131n\u0131 Atom Emme Spektrometrisi)"},"content":{"rendered":"

1. Y\u00f6ntem Genel Bak\u0131\u015f<\/h2>\n
\u00d6rnek mikrodalga ile sindirildikten sonra, atomik emim spektrofotometrinin grafit f\u0131r\u0131n\u0131na enjekte edilir. Elektrotermal atomizasyondan sonra \u00f6rnek 283,3 nm'de rezonans hatt\u0131n\u0131 emir. Belirli bir konsantrasyon aral\u0131\u011f\u0131nda, emici de\u011fer kur\u015fun i\u00e7eri\u011fine orant\u0131l\u0131d\u0131r ve miqdarl\u0131k standart bir seriyle kar\u015f\u0131la\u015ft\u0131r\u0131larak ger\u00e7ekle\u015ftirilir.<\/div>\n
\n

2. Aletler ve Reagentler<\/h2>\n

2.1 Aletler ve Ekipmanlar<\/h3>\n

2.1.1 Test Aletleri<\/h4>\n
\n
\n\n\n\n\n\n\n\n
Seri numaras\u0131.<\/th>\n\u0130sim<\/th>\nMiktar<\/th>\nTeknik Gereksinimler<\/th>\nAksesuarlar<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nGrafit F\u0131r\u0131n Atom Emme Spektrofotometri<\/td>\n1 set<\/td>\n–<\/td>\nKur\u015fun Bo\u015f Katod Lambas\u0131<\/td>\n<\/tr>\n
2<\/td>\nArgon Gaz\u0131<\/td>\n1 silindir<\/td>\nSafl\u0131k \u2265% 99,99<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nSirk\u00fclasyon So\u011futma Su Sistemi<\/td>\n1 set<\/td>\n–<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.1.2 \u00d6rnek \u00d6n Tedavi Ekipmanlar\u0131<\/h4>\n
\n
\n\n\n\n\n\n\n\n\n\n\n
Seri numaras\u0131.<\/th>\n\u0130sim<\/th>\nMiktar<\/th>\nTeknik Gereksinimler<\/th>\nAksesuarlar<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nMikrodalga Sindirim Sistemi<\/td>\n1 set<\/td>\nPlatin direnci ve k\u0131z\u0131l\u00f6tesi s\u0131cakl\u0131k \u00f6l\u00e7\u00fcm\u00fc ile donat\u0131lm\u0131\u015ft\u0131r; bas\u0131n\u00e7 \u00f6l\u00e7\u00fcm do\u011frulu\u011fu: \u00b1 0.1 \u2103<\/td>\n–<\/td>\n<\/tr>\n
2<\/td>\nS\u0131cakl\u0131k Kontrollu S\u0131cak Plaka<\/td>\n1 set<\/td>\n–<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nElektronik Denge<\/td>\n1 set<\/td>\nHassasiyet: 0.1 mg<\/td>\n–<\/td>\n<\/tr>\n
4<\/td>\nUltrasaf Su Sistemi<\/td>\n1 set<\/td>\n–<\/td>\n–<\/td>\n<\/tr>\n
5<\/td>\nhacimli \u015fi\u015fe<\/td>\nBirka\u00e7<\/td>\nHacim: 100 ml<\/td>\n–<\/td>\n<\/tr>\n
6<\/td>\nTest T\u00fcp\u00fc<\/td>\nBirka\u00e7<\/td>\nHacim: 10 ml<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.2 Reagentler<\/h3>\n

2.2.1 Ham Reagentler<\/h4>\n
\n
\n\n\n\n\n\n\n\n\n
Seri numaras\u0131.<\/th>\n\u0130sim<\/th>\nTeknik Gereksinimler<\/th>\nNotlar<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nDiammoniyum Hidrojen Fosfat<\/td>\nAnalitik Reagent (AR)<\/td>\n–<\/td>\n<\/tr>\n
2<\/td>\nHidroklorik Asit<\/td>\nGarantili Reagent (GR)<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nNitrik Asit<\/td>\nMOS S\u0131n\u0131f\u0131<\/td>\n–<\/td>\n<\/tr>\n
4<\/td>\nPaladyum Nitrat<\/td>\nAnalitik Reagent (AR)<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.2 Haz\u0131rlanan Reagentler<\/h4>\n
\n
\n\n\n\n\n\n\n\n
Seri numaras\u0131.<\/th>\n\u0130sim<\/th>\nHaz\u0131rlama Y\u00f6ntemi<\/th>\nNotlar<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nNitrik Asit \u00c7\u00f6z\u00fcm\u00fc (1 99)<\/td>\n10 mL nitrik asit \u00f6l\u00e7\u00fcn, yava\u015f yava\u015f 990 mL suya ekleyin ve iyi kar\u0131\u015ft\u0131r\u0131n.<\/td>\n–<\/td>\n<\/tr>\n
2<\/td>\nNitrik Asit \u00c7\u00f6z\u00fcm\u00fc (5 95)<\/td>\n5 mL nitrik asit \u00f6l\u00e7\u00fcn, yava\u015f yava\u015f 95 mL suya ekleyin ve iyi kar\u0131\u015ft\u0131r\u0131n.<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nDiammoniyum Hidrojen Fosfat-Paladiyum Nitrat \u00c7\u00f6z\u00fcm\u00fc<\/td>\n0,02 g paladyum nitrat a\u011f\u0131rl\u0131k, az miktarda nitrik asit \u00e7\u00f6z\u00fcm\u00fc ile \u00e7\u00f6z\u00fcn (19), sonra 2 g amonyum dihidrojen fosfat ekleyin. \u00c7\u00f6z\u00fcnd\u00fckten sonra, nitrik asit \u00e7\u00f6z\u00fcm\u00fc ile 100 mL'ye seyreltin (5 95) ve iyi kar\u0131\u015ft\u0131r\u0131n.<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.3 Referans Standartlar\u0131<\/h3>\n

2.3.1 Stok \u00c7\u00f6z\u00fcm\u00fc<\/h4>\n
\n
\n\n\n\n\n\n
Seri numaras\u0131.<\/th>\n- Hay\u0131r. - Hay\u0131r.<\/th>\n\u0130sim<\/th>\nTeknik Gereksinimler<\/th>\nNotlar<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nGBW 08619'\u0131<\/td>\nKur\u015fun Tek Elemanl\u0131 Standart \u00c7\u00f6z\u00fcm<\/td>\nKonsantrasyon: 1000 \u03bcg \/ mL<\/td>\nUlusal Metroloji Enstit\u00fcs\u00fc, \u00c7in<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

3. Operasyon Prosed\u00fcr\u00fc<\/h2>\n

3.1 \u00d6rnek Haz\u0131rlama<\/h3>\n

3.1.1 Test \u00c7\u00f6z\u00fcm\u00fcn\u00fcn Haz\u0131rlanmas\u0131<\/h4>\n
Kat\u0131 \u00f6rne\u011fin 0,2 g'ini (hassasiyeti 0,001 g'e kadar) mikrodalga sindirim kap\u0131na do\u011fru bir \u015fekilde a\u011f\u0131rlay\u0131n, 5 mL nitrik asit ekleyin ve \u00f6rne\u011fi mikrodalga sindirim sisteminin \u00e7al\u0131\u015fma prosed\u00fcrlerine g\u00f6re sindirin. So\u011futuktan sonra sindirim kap\u0131s\u0131n\u0131 \u00e7\u0131kar\u0131n ve asiti 140 \u2103 ~ 160 \u2103 s\u0131cak bir plakada buharla\u015ft\u0131r\u0131n hacim yakla\u015f\u0131k 1 mL'ye d\u00fc\u015fene kadar. Sindirim kap\u0131s\u0131 so\u011fulduktan sonra, sindirilmi\u015f \u00e7\u00f6z\u00fcm\u00fc 25 mL hacimli bir kolba deiyonla\u015ft\u0131r\u0131lm\u0131\u015f su ile aktar\u0131n. Sindirim damar\u0131n\u0131 k\u00fc\u00e7\u00fck miktarda su ile 2 ~ 3 kez y\u0131kay\u0131n, y\u0131kama \u00e7\u00f6z\u00fcmlerini hacimli kolba birle\u015ftirin ve i\u015faretlenmi\u015f hacime su ile seyredin. Daha sonraki kullan\u0131m i\u00e7in iyi kar\u0131\u015ft\u0131r\u0131n; Bu \u00f6rnek test \u00e7\u00f6z\u00fcm\u00fcd\u00fcr. Ayn\u0131 anda bir reaktif bo\u015f testi haz\u0131rlay\u0131n.<\/div>\n


<\/p>\n

Mikrodalga Is\u0131tma Program\u0131<\/strong><\/div>\n


<\/p>\n

\n
\n\n\n\n\n\n\n\n\n\n
Ad\u0131m<\/th>\nS\u0131cakl\u0131k \/ \u2103<\/th>\nTutma S\u00fcresi \/ dakika<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\n100<\/td>\n3<\/td>\n<\/tr>\n
2<\/td>\n120<\/td>\n3<\/td>\n<\/tr>\n
3<\/td>\n140<\/td>\n3<\/td>\n<\/tr>\n
4<\/td>\n160<\/td>\n3<\/td>\n<\/tr>\n
5<\/td>\n180<\/td>\n30<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

3.1.2 Standart \u00c7\u00f6z\u00fcmlerin Haz\u0131rlanmas\u0131<\/h4>\n
    \n
  1. \n
    Kur\u015fun Standart Ara \u00c7\u00f6z\u00fcm\u00fcn\u00fcn Haz\u0131rlanmas\u0131: Kur\u015fun standart \u00e7\u00f6z\u00fcm\u00fc (1,0 \u03bcg\/mL) i\u00e7in, 0,1 mL kur\u015fun standart stok \u00e7\u00f6z\u00fcm\u00fcn\u00fc (1000 \u03bcg\/mL) 100 mL hacimli bir kolba do\u011fru bir \u015fekilde pipet edin, (1 99) nitrik asit \u00e7\u00f6z\u00fcm\u00fc ile i\u015faretlenmi\u015f hacime seyreltin ve iyi sallay\u0131n.<\/div>\n<\/li>\n
  2. \n
    Kur\u015fun Standart Serisinin Haz\u0131rlanmas\u0131: Kur\u015fun standart \u00e7\u00f6z\u00fcm\u00fcn\u00fcn (1,0 \u03bcg\/mL) 0,0, 0,1, 0,2, 0,3 ve 0,4 mL'sini s\u0131ras\u0131yla ayr\u0131 10 mL hacimli \u015fi\u015felere do\u011fru bir \u015fekilde pipetleyin. 0,0, 10,0, 20,0, 30,0 ve 40,0 ng\/mL konsantrasyonlar\u0131nda kur\u015fun standart serisi \u00e7\u00f6z\u00fcmleri elde etmek i\u00e7in (99) nitrik asit \u00e7\u00f6z\u00fcm\u00fc ile i\u015faretlenmi\u015f hacime seyreltin.<\/div>\n<\/li>\n<\/ol>\n

    3.2 \u00d6rnek Testi<\/h3>\n
      \n
    1. Test Ko\u015fullar\u0131 Grafit f\u0131r\u0131n atomik emim spektrofotometri i\u00e7in referans test ko\u015fullar\u0131: | Parametre | \u00d6zellikler (Kur\u015fun) | | — | — Dalga Boyu (nm) | 283.3 | | Spektral Bant Geni\u015fli\u011fi (nm) | 0.4 | | Element Lamba Ak\u0131m\u0131 (mA) | 2 | | Arka Plan\u0131 D\u00fczeltme Y\u00f6ntemi | Deuterium Lamba |<\/li>\n<\/ol>\n


      <\/p>\n

      Grafit F\u0131r\u0131n Is\u0131tma Program\u0131<\/strong><\/div>\n


      <\/p>\n

      \n
      \n\n\n\n\n\n\n\n\n
      Ad\u0131m<\/th>\nProsed\u00fcr<\/th>\nS\u0131cakl\u0131k (\u2103)<\/th>\nIs\u0131tma S\u00fcresi (s)<\/th>\nTutma S\u00fcresi (s)<\/th>\n<\/tr>\n<\/thead>\n
      1<\/td>\nKurutma<\/td>\n120<\/td>\n10<\/td>\n10<\/td>\n<\/tr>\n
      2<\/td>\nAshing'in<\/td>\n650<\/td>\n10<\/td>\n15<\/td>\n<\/tr>\n
      3<\/td>\nAtomizasyon<\/td>\n1900<\/td>\n0<\/td>\n2<\/td>\n<\/tr>\n
      4<\/td>\nTemizlik<\/td>\n2000<\/td>\n1<\/td>\n2<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n


      <\/p>\n

        \n
      1. \u00d6rnek Testi K\u00fctle konsantrasyonunun y\u00fckselen s\u0131ras\u0131nda, 10 \u03bcL kur\u015fun standart serisi \u00e7\u00f6z\u00fcm\u00fcn\u00fc ve 5 \u03bcL diyamonyum hidrojen fosfat-paladyum nitrat \u00e7\u00f6z\u00fcm\u00fcn\u00fc ayn\u0131 anda grafit f\u0131r\u0131n\u0131na enjekte edin. Atomizasyondan sonra, emici de\u011ferleri \u00f6l\u00e7\u00fcn. Absisa olarak k\u00fctle konsantrasyonu ve ordinat olarak emici de\u011feri olan standart bir e\u011fri \u00e7izin. Verileri okuyun, \u00f6rnek a\u011f\u0131rl\u0131\u011f\u0131n\u0131 girin ve sonu\u00e7lar\u0131 kontrol edin ve kaydedin.<\/li>\n<\/ol>\n

        3.3 Sonu\u00e7 Hesaplamas\u0131<\/h3>\n
        Numunedeki kur\u015fun i\u00e7eri\u011fi a\u015fa\u011f\u0131daki form\u00fcl\u00fc kullanarak hesaplan\u0131r:<\/div>\n<\/div>\n
        \"\"<\/div>\n

        <\/p>\n
        Nerede:<\/div>\n
          \n
        • X<\/span>\u00a0= Numunedeki kur\u015fun i\u00e7eri\u011fi, birim: kilogram ba\u015f\u0131na miligram (mg\/kg);<\/li>\n
        • C1'nin<\/span>\u00a0= \u00d6rnek test \u00e7\u00f6z\u00fcm\u00fcnde kur\u015fun k\u00fctle konsantrasyonu, birim: mililitre ba\u015f\u0131na nanogram (ng\/mL);<\/li>\n
        • C2'nin<\/span>= Bo\u015f \u00e7\u00f6z\u00fcmdeki kur\u015fun k\u00fctle konsantrasyonu, birim: mililitre ba\u015f\u0131na nanogram (ng \/ mL);<\/li>\n
        • V'nin<\/span>\u00a0= Sabit hacmdan sonra \u00f6rne\u011fin hacmi, birim: mililitre (mL);<\/li>\n
        • M<\/span>\u00a0= \u00d6rne\u011fin k\u00fctlesi, birim: gram (g);<\/li>\n
        • 1000 = D\u00f6n\u00fc\u015f\u00fcm fakt\u00f6r\u00fc.<\/li>\n<\/ul>\n<\/div>\n