定义Definition
重量分析法是把被测组分以沉淀、气化或电解等方式从试样中分离出来,转化为一定组成的称量形式,通过称量其质量来计算被测组分含量的经典定量分析方法。它准确度很高(相对误差可达 0.1%–0.2%),不需要标准物质校准。
Gravimetric analysis separates the analyte from a sample by precipitation, volatilisation or electrolysis, converts it to a weighing form of definite composition and calculates its amount from the mass. A classical quantitative method, it is very accurate (relative errors of 0.1–0.2%) and needs no calibration standard.
原理与步骤Principle and steps
沉淀重量法最常用:试样溶解 → 加沉淀剂生成沉淀形式 → 陈化 → 过滤、洗涤 → 烘干或灼烧成称量形式 → 称量至恒重 → 计算。例如测硫酸根:加 BaCl₂ 生成 BaSO₄ 沉淀,灼烧后称量;测铁:沉淀为 Fe(OH)₃,灼烧为 Fe₂O₃ 称量。含量 w = m(称量形式) × F / m(试样),F 为换算因数。理想沉淀要求溶解度小、纯度高、易过滤,称量形式组成固定、稳定、摩尔质量大。
Precipitation gravimetry is most common: dissolve the sample → add precipitant to form the precipitate → digest → filter and wash → dry or ignite to the weighing form → weigh to constant mass → calculate. Sulfate, for example, is precipitated as BaSO₄ with BaCl₂ and ignited; iron is precipitated as Fe(OH)₃ and ignited to Fe₂O₃. Content w = m(weighing form) × F / m(sample), with F the gravimetric factor. A good precipitate is insoluble, pure and easy to filter, and the weighing form has fixed composition, stability and a large molar mass.
历史History
重量分析是最古老的定量分析方法之一。18 世纪布莱克、拉瓦锡用精确称量研究化学反应,建立了质量守恒定律。19 世纪贝采利乌斯用重量法精确测定了数十种元素的原子量。1914 年理查兹因精确测定原子量获诺贝尔化学奖,他的工作大量采用重量分析。
Gravimetry is among the oldest quantitative methods. In the eighteenth century Black and Lavoisier studied reactions by accurate weighing and established conservation of mass. In the nineteenth century Berzelius determined the atomic weights of dozens of elements gravimetrically, and Theodore Richards, who received the 1914 Nobel Prize in Chemistry for precise atomic weights, relied heavily on gravimetric analysis.
其他形式与现状Other forms and status
气化法测定水分、结晶水和灰分(如干燥失重);电解重量法在电极上析出金属称量(如铜的测定);热重分析是现代仪器化的重量法。重量法操作繁琐耗时,已在多数场合被仪器分析取代,但仍是校准其他方法的基准方法。
Volatilisation methods determine moisture, water of crystallisation and ash (as loss on drying); electrogravimetry weighs metal deposited on an electrode, as for copper; and thermogravimetric analysis is gravimetry instrumentalised. Gravimetry is slow and laborious and has largely given way to instrumental methods, but it remains a reference method for calibrating others.
反应Reactions
热的稀盐酸溶液中慢慢加入 BaCl₂,陈化后过滤。
Add BaCl₂ slowly to a hot dilute HCl solution, digest and filter.
丁二酮肟重量法测镍
Dimethylglyoxime gravimetry for nickel
年表Timeline
- 1774
拉瓦锡用称量研究燃烧
Lavoisier studies combustion by weighing
- 1818
贝采利乌斯发表原子量表
Berzelius publishes a table of atomic weights
- 1914
理查兹获诺贝尔化学奖
Richards receives the Nobel Prize in Chemistry
相关公式Formulas
例题Worked example
由 Fe₂O₃ 求 Fe₃O₄:F = 2M(Fe₃O₄)/(3M(Fe₂O₃)) = 2×231.5/(3×159.7) = 0.9666。
Fe₃O₄ from Fe₂O₃: F = 0.9666.