5.17
يعتمد قياس الجاذبية للترسيب على تحويل المادة الحليلة إلى راسب قليل الذوبان، والذي يتم فصله عن طريق الترشيح ووزنه. يجب أن يكون الراسب المثالي نقيًا، وغ…
في قياس الجاذبية لهطول الأمطار ، يتفاعل التحليل مع مرسب لينتج راسب معزول ووزن.
يجب أن يكون الراسب منخفض الذوبان ، ودرجة نقاء عالية ، وتكوين معروف ، ويمكن فصله بسهولة عن خليط التفاعل.
على سبيل المثال ، في تقدير النيكل ، يكون المرسب هو ثنائي ميثيل جليوكسيم إيثانولي ، والذي ينتج رواسب حمراء من النيكل مكرر (ثنائي ميثيل جليوكسيميت).
يتم التلاعب بدرجة الحموضة في التفاعل لضمان هطول الأمطار الكامل.
بعد ذلك ، يتم هضم الراسب لزيادة حجم الجسيمات ، متبوعا بالترشيح باستخدام قمع ترشيح موزون مسبقا.
يغسل هذا الراسب بالماء البارد ، ويجفف في الفرن ، ويترك ليبرد في المجفف.
بعد ذلك ، يتم الحصول على كتلة الراسب ، وبعد ذلك يتم تطبيق العلاقات المتكافئة لحساب محتوى النيكل.
View the full transcript and gain access to JoVE Core videos
Q1: What are the key requirements for an ideal precipitate in gravimetric analysis?
An ideal precipitate must be pure, insoluble, and of known composition to ensure accurate results. It should be easily separable from the reaction mixture and have low solubility to prevent loss during filtration and washing. These properties enable reliable mass determination and stoichiometric calculations for quantifying the analyte.
Q2: How does digestion improve the quality of a precipitate in gravimetry?
Digestion involves heating the precipitate over a hot water bath for several hours, allowing impurities occluded during initial formation to dissolve and the precipitate to slowly reform. This process removes contaminants and increases particle size, resulting in a purer, more easily filterable precipitate that yields more accurate mass measurements.
Q3: Why is pH control important during precipitation gravimetry?
Manipulating reaction pH ensures complete precipitation of the analyte from solution, preventing loss of target material. In nickel gravimetry, dilute ammonia is added dropwise until precipitation occurs, with slight excess ensuring all nickel ions convert to the red nickel bis(dimethylglyoximate) precipitate needed for accurate quantification.
Q4: What is the role of washing and drying in the gravimetric procedure?
After filtration, the precipitate is washed with cold water to remove soluble impurities and residual reagents. Drying in an oven removes moisture, and cooling in a desiccator prevents reabsorption of atmospheric water. These steps ensure that the final mass reflects only the pure, dry precipitate for accurate analyte calculation.
Q5: How is the analyte concentration determined from the precipitate mass?
After obtaining the dried precipitate mass, stoichiometric mole relationships are applied to calculate the original analyte content. In nickel gravimetry, the mass of nickel dimethylglyoximate is converted to moles, then to moles of nickel using the known 1:1 stoichiometry, allowing calculation of nickel concentration in the original sample.
Q6: Why is ethanolic dimethylglyoxime used as the precipitant for nickel determination?
Ethanolic dimethylglyoxime selectively reacts with nickel ions to form a red precipitate of nickel bis(dimethylglyoximate) that is sparingly soluble and easily filtered. This organic precipitating agent produces a pure, stable product of known composition, making it ideal for accurate gravimetric analysis of nickel in samples.
Q7: What is the purpose of cooling the precipitate in a desiccator before weighing?
Cooling in a desiccator prevents the dried precipitate from reabsorbing moisture from the air, which would artificially increase its mass and introduce error into calculations. The desiccator maintains a dry environment, ensuring the measured mass accurately represents only the pure, anhydrous precipitate needed for reliable analyte quantification.