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Measuring Reactive Silica in Water

Published in Water Quality Analysis 4 mins read

Certainly! Measuring reactive silica in water is crucial for various applications, particularly in industries like power generation, semiconductor manufacturing, and environmental monitoring. Reactive silica primarily refers to dissolved silica species, mainly silicic acid [Si(OH)₄], which readily reacts with molybdate reagents under acidic conditions.

The amount of reactive silica in water, alongside unreactive silica (colloidal or particulate forms), can be determined using various analytical techniques. The choice of method often depends on the required sensitivity, the matrix of the water sample, and the form of silica being targeted.

Based on the provided reference, the amount of reactive and unreactive silica in ultrapure (UP) water can be determined by various analytical methods. These methods include:

Analytical Methods for Silica Measurement

Here are some common methods used to measure silica, as mentioned in the reference, and how they relate to reactive silica:

  • Colorimetry: This is one of the most common and widely used methods for measuring reactive silica. It typically involves the molybdate method, where silicic acid reacts with ammonium molybdate under acidic conditions to form a yellow silicomolybdic acid complex. This complex can then be reduced to form a blue complex for increased sensitivity. The intensity of the color is proportional to the concentration of reactive silica and is measured using a spectrophotometer. This method is specifically designed to measure dissolved, reactive silica.
  • Inductively Coupled Plasma-Mass Spectrometry (ICP-MS): ICP-MS is a highly sensitive technique capable of measuring trace levels of many elements, including silicon. It can be used to measure total silicon (and thus total silica) after appropriate sample preparation, which might include digestion to convert unreactive forms into reactive forms. With careful sample handling that avoids digestion, ICP-MS can also be used to measure dissolved reactive silica.
  • Graphite Furnace Atomic Absorption Spectroscopy (GFAAS): Like ICP-MS, GFAAS is a sensitive atomic spectroscopy technique. It measures the absorption of light by free silicon atoms generated in a graphite furnace. GFAAS can measure total silica after digestion or potentially reactive silica depending on the sample introduction and furnace program.
  • Ion Chromatography (IC): IC is primarily used for separating and detecting ions. Silica exists in water as silicic acid, which is uncharged at neutral pH but can deprotonate to form silicate anions at higher pH. IC can be used to measure silicate anions, which represent reactive silica species, especially in alkaline samples or after converting silicic acid to its anionic form.
  • Gravimetry: This method involves precipitating silica, usually as silicates or silicic acid, and then weighing the precipitate after ignition to silicon dioxide (SiO₂). This method is generally less sensitive than spectroscopic methods and is typically used for measuring higher concentrations of total silica (both reactive and unreactive forms converted to SiO₂).
  • Scanning Electron Microscopy (SEM): While mentioned in the reference alongside other analytical methods, SEM is primarily a surface imaging technique that uses a beam of electrons to create an image of a sample's surface. SEM is typically used to analyze the morphology and composition of solid silica particles (unreactive silica or precipitates) rather than dissolved reactive silica in the water itself. Energy-dispersive X-ray spectroscopy (EDX or EDS) is often coupled with SEM to determine the elemental composition of solid samples, including silicon in particulate form.

In summary, while methods like GFAAS, ICP-MS, IC, and gravimetry can be used to measure silica in various forms (total or reactive depending on sample preparation), colorimetry (the molybdate method) is the most direct and commonly used method specifically for measuring reactive silica in water due to its chemical selectivity for silicic acid. SEM is primarily used for analyzing solid silica particles.

Understanding the concentration of reactive silica is important as it can impact process efficiency in industries, contribute to scaling, or affect aquatic life.

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