{"id":3999,"date":"2025-10-10T16:58:32","date_gmt":"2025-10-10T08:58:32","guid":{"rendered":"https:\/\/www.pgeneral.com\/?p=3999"},"modified":"2025-10-10T16:58:32","modified_gmt":"2025-10-10T08:58:32","slug":"determination-of-potassium-oxide-in-alumina-powder-flame-atomic-absorption-spectrometry","status":"publish","type":"post","link":"https:\/\/www.pgeneral.com\/de\/applications\/determination-of-potassium-oxide-in-alumina-powder-flame-atomic-absorption-spectrometry\/","title":{"rendered":"Bestimmung von Kaliumoxid in Aluminiumpulver (Flammenabsorptionsspektrometrie)"},"content":{"rendered":"

1. Method Overview<\/h2>\n
The sample is dissolved by heating in a quartz beaker with a sulfuric acid-phosphoric acid mixed acid. After dilution with water, an air-acetylene flame is used to measure the absorbance of potassium at a wavelength of 766.5 nm using an atomic absorption spectrometer. Within a certain concentration range, the absorbance of potassium is proportional to its content, and quantitative determination is performed by comparison with a standard series.<\/div>\n
\n

2. Instruments and Reagents<\/h2>\n

2.1 Instruments and Equipment<\/h3>\n

2.1.1 Testing Instruments<\/h4>\n
\n
\n\n\n\n\n\n\n\n
Serial No.<\/th>\nName<\/th>\nQuantity<\/th>\nTechnical Requirements<\/th>\nAccessories<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nAtomic Absorption Spectrophotometer (Model: TAS-990)<\/td>\n1 set<\/td>\n–<\/td>\nPotassium Hollow Cathode Lamp<\/td>\n<\/tr>\n
2<\/td>\nAir Compressor<\/td>\n1 set<\/td>\nRated discharge pressure: 0.3 MPa<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nAcetylene Gas<\/td>\n1 cylinder<\/td>\nPurity \u2265 99.99%<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.1.2 Sample Pretreatment Equipment<\/h4>\n
\n
\n\n\n\n\n\n\n\n\n\n\n\n\n\n
Serial No.<\/th>\nName<\/th>\nQuantity<\/th>\nTechnical Requirements<\/th>\nAccessories<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nQuartz Beaker<\/td>\n6 pieces<\/td>\nVolume: 50 mL<\/td>\n6 watch glasses<\/td>\n<\/tr>\n
2<\/td>\nGlass Stirring Rod<\/td>\n1 piece<\/td>\nLength: 20 cm<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nElectric Furnace<\/td>\n1 set<\/td>\nTemperature-adjustable<\/td>\n–<\/td>\n<\/tr>\n
4<\/td>\nStandard Sieve<\/td>\n1 piece<\/td>\nMesh size: 0.125 mm<\/td>\n–<\/td>\n<\/tr>\n
5<\/td>\nAdjustable Hot Plate<\/td>\n1 set<\/td>\nRated temperature range: Room temperature ~ 300 \u2103<\/td>\n–<\/td>\n<\/tr>\n
6<\/td>\nOven<\/td>\n1 set<\/td>\nRated temperature range: Room temperature ~ 200 \u2103<\/td>\n–<\/td>\n<\/tr>\n
7<\/td>\nMicropipette<\/td>\n1 each<\/td>\nRanges: 100 \u03bcL ~ 1000 \u03bcL, 1000 \u03bcL ~ 5000 \u03bcL<\/td>\n–<\/td>\n<\/tr>\n
8<\/td>\nVolumetric Flask<\/td>\nSeveral<\/td>\nVolume: 100 mL<\/td>\n–<\/td>\n<\/tr>\n
9<\/td>\nVolumetric Flask<\/td>\n1 piece<\/td>\nVolume: 500 mL<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.2 Reagents<\/h3>\n

2.2.1 Raw Reagents<\/h4>\n
\n
\n\n\n\n\n\n\n\n\n
Serial No.<\/th>\nName<\/th>\nTechnical Requirements<\/th>\nRemarks<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nSulfuric Acid<\/td>\nGuaranteed Reagent (GR)<\/td>\n–<\/td>\n<\/tr>\n
2<\/td>\nPhosphoric Acid<\/td>\nGuaranteed Reagent (GR)<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nAluminum Powder<\/td>\nGuaranteed Reagent (GR)<\/td>\n–<\/td>\n<\/tr>\n
4<\/td>\nCesium Chloride<\/td>\nGuaranteed Reagent (GR)<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.2.2 Prepared Reagents<\/h4>\n
\n
\n\n\n\n\n\n\n\n
Serial No.<\/th>\nName<\/th>\nPreparation Method<\/th>\nRemarks<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nCesium Chloride Solution (1000 \u03bcg\/mL)<\/td>\nAccurately weigh 0.1 g of cesium chloride into a 100 mL volumetric flask, dilute to the marked volume with deionized water, and mix well.<\/td>\n–<\/td>\n<\/tr>\n
2<\/td>\nAluminum Matrix Solution<\/td>\nCover with a watch glass, place on an electric furnace, and heat while shaking to dissolve the sample. After complete dissolution, immediately remove and cool to 40 \u2103 ~ 70 \u2103. Rinse the watch glass with hot water at 50 \u2103, and transfer the washing solution into the original beaker. Rinse the solution into a 500 mL volumetric flask with hot water at 50 \u2103, dilute to approximately 400 mL with pure water, shake evenly, cool to room temperature, then dilute to the marked volume with pure water and mix well. Store in a polyethylene bottle. This solution contains 12.5 mg of alumina per 1 mL.<\/td>\n–<\/td>\n<\/tr>\n
3<\/td>\nNitric Acid Solution (1+99)<\/td>\nMeasure 10 mL of nitric acid, pour it into 990 mL of pure water, and mix well.<\/td>\n–<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

2.3 Reference Standards<\/h3>\n

2.3.1 Stock Solution<\/h4>\n
\n
\n\n\n\n\n\n
Serial No.<\/th>\nNo.<\/th>\nName<\/th>\nTechnical Requirements<\/th>\nRemarks<\/th>\n<\/tr>\n<\/thead>\n
1<\/td>\nGSB G 62011-90-(1901)<\/td>\nNational Potassium Standard Solution<\/td>\nConcentration: 1000 \u03bcg\/mL<\/td>\nCentral Iron and Steel Research Institute<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

3. Operational Procedures<\/h2>\n

3.1 Sample Preparation<\/h3>\n

3.1.1 Preparation of Test Solution<\/h4>\n
    \n
  1. \n
    Sample Pretreatment<\/p>\n
    <\/div>\n

    Pass the sample through a 0.125 mm standard sieve, dry it in an oven at 300 \u2103 \u00b1 10 \u2103 for 2 hours, and cool to room temperature.<\/p><\/div>\n<\/li>\n

  2. \n
    Sample Digestion<\/p>\n
    <\/div>\n

    Weigh 0.25 g of the sample (accurate to 0.0001 g) into a 50 mL quartz beaker. Add 25 mL of phosphoric acid and 5 mL of sulfuric acid, cover with a watch glass, place on an electric furnace, and heat while shaking to dissolve the sample. After complete dissolution, immediately remove and cool to 40 \u2103 ~ 70 \u2103. Rinse the watch glass with hot water at 50 \u2103, and transfer the washing solution into the original beaker. Rinse the sample solution into a 100 mL volumetric flask with hot water at 50 \u2103, dilute to approximately 80 mL with pure water, shake evenly, cool to room temperature, then dilute to the marked volume with pure water and mix well for testing. Weigh 0.1323 g of aluminum powder and perform a blank test following the same procedure as the sample.<\/p><\/div>\n<\/li>\n<\/ol>\n

    3.1.2 Preparation of Standard Solutions<\/h4>\n
      \n
    1. \n
      Preparation of Potassium Standard Intermediate Solution (100 \u03bcg\/mL)<\/p>\n
      <\/div>\n

      Accurately pipette 5 mL of the potassium standard solution (1000 \u03bcg\/mL) into a 50 mL volumetric flask, dilute to the marked volume with (1+99) nitric acid solution, and mix well.<\/p><\/div>\n<\/li>\n

    2. \n
      Preparation of Potassium Standard Series<\/p>\n
      <\/div>\n

      Pipette 0.0 mL, 0.4 mL, 0.8 mL, and 1.2 mL of the potassium standard intermediate solution (100 \u03bcg\/mL) into a set of 100 mL volumetric flasks that have been pre-added with 4 mL of aluminum matrix solution respectively. Dilute to the marked volume with pure water, mix well, and store in polyethylene bottles. The concentrations of this potassium standard series are 0.0 \u03bcg\/mL, 0.4 \u03bcg\/mL, 0.8 \u03bcg\/mL, and 1.2 \u03bcg\/mL.<\/p><\/div>\n<\/li>\n<\/ol>\n

      3.2 Sample Testing<\/h3>\n

      1) Testing Conditions<\/h4>\n
      Reference Conditions for Flame Atomic Absorption Spectrophotometer<\/strong><\/div>\n
      <\/div>\n
      \n
      \n\n\n\n\n\n\n\n\n\n
      Parameter<\/th>\nSpecification<\/th>\n<\/tr>\n<\/thead>\n
      Wavelength (nm)<\/td>\n766.5<\/td>\n<\/tr>\n
      Spectral Bandwidth (nm)<\/td>\n0.4<\/td>\n<\/tr>\n
      Element Lamp Current (mA)<\/td>\n2.0<\/td>\n<\/tr>\n
      Burner Height (mm)<\/td>\n5.0<\/td>\n<\/tr>\n
      Air Compressor Pressure<\/td>\n0.22 MPa<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/div>\n<\/div>\n

      2) Sample Testing<\/h4>\n
      Use an air-acetylene flame. On the atomic absorption spectrometer, set the wavelength to 766.5 nm, zero the instrument with water, and measure the absorbance. Subtract the absorbance of the “zero-concentration” solution in the standard series, then plot a working curve.<\/div>\n<\/div>\n