Factors Affecting Moisture Analyzer Results

2022-12-13

There are many methods for moisture determination;,the coulometric Karl Fischer trace moisture analyzer is widely used for its simple operation, high accuracy and fast measurement.,However, the measurement process is affected by many factors,such as the instrument electrodes, Karl Fischer reagent, sample properties and measurement environment.,Poor consideration or selection,will make titration results inaccurate.

1. Effect of the Electrode

Karl Fischer titration judges the reaction endpoint from signals transmitted by the electrode;,therefore,,electrode sensitivity directly affects titration results. Many factors can reduce electrode sensitivity:,impurities adhering to the electrode surface,can lower electrode sensitivity,and produce falsely high results; long service,also reduces electrode sensitivity. Therefore,,inspect and maintain electrodes promptly before use.

2. Effect of the Electrolyte

In normal measurement,,each100mlbatch of electrolyte can react with no less than1 g of water. In practice,,if measurement takes too long,,atmospheric moisture affects the Karl Fischer reagent;,the stability of the mixed A/B solutions drops rapidly;,these factors reduce electrolyte sensitivity. During electrolysis, if vigorous bubbling appears in the cathode compartment or the electrolyte has been contaminated to a reddish-brown color,,endpoint time increases. Replace the electrolyte promptly when these signs appear.

3. Sampling Requirements and Sample Size

When injecting the sample into the electrolyte,,insert the needle below the liquid surface,and avoid contact with the cell wall or electrodes,to prevent sample loss. Ordinary syringe needles, being short and thick,,cannot meet these requirements. When choosing a syringe needle,,choose one with a needle length of about15 cm,,which effectively avoids the above issues. For accurate results,,sample size should match the moisture content. But if injection is slow,,the sample may evaporate or absorb atmospheric moisture,,affecting the result. To weigh and inject the sample quickly,,place a balance with a minimum division of0.01 mg next to the moisture analyzer;,after sampling, the syringe can be weighed immediately and injected,,reducing the possibility of error.

4. Effect of Side Reactions

Karl Fischer reagent solution B contains iodine,,and thiols and hydrogen sulfide consume iodine just as water does,,producing falsely high moisture results;,samples containing thiols or hydrogen sulfide,are unsuitable for Karl Fischer titration. Aldehydes and ketones are likewise unsuitable. Common Karl Fischer reagents generally use methanol as solvent;,aldehydes and ketones react with methanol to form acetals or ketals plus water,,therefore,,so choose a methanol-free reagent suitable for aldehydes and ketones.

5. Effect of Instrument Conditions

(1) Stirring speed: stirring during titration should be thorough and uniform;,adjust the stirring speed so the electrolyte mixes fully,and the stir bar does not jump,,to avoid hitting the electrode.

(2) Iodine generation rate: the iodine generation rate relates to the sample's moisture content. The lower the moisture,,the slower the iodine generation rate should be set,,ensuring the water in the sample is fully electrolyzed.

(3) Electrolysis end parameters: electrolysis is usually terminated by a set maximum time or a drift endpoint.

6. Effect of Drift Value

Many factors affect instrument drift,,mainly including: poor instrument sealing or high humidity in the measurement environment,,allowing atmospheric moisture to slowly seep into the reaction system; side reactions during measurement,such as ketalization or esterification,, all of which generate water; and using expired Karl Fischer reagent—,all of these can change the drift value. When such situations are found,,resolve them promptly,to ensure accurate and reliable measurement results.    

To ensure the accuracy of trace moisture analyzer measurements,,before measurement,,clean the electrodes and replace the electrolyte in time; during measurement,,choose a needle length ofSample injection with an approximately 15 cm syringe needle,and keep an electronic balance next to the moisture analyzer,for timely weighing; select the electrolyte according to sample properties; adjust the stirrer speed,to control the rate of iodine generation,to accurately determine the titration endpoint; gain a full understanding of factors that may cause instrument drift,and eliminate them promptly. During measurement,as long as you observe carefully,analyze thoroughly,and keep exploring,controlling and eliminating every adverse factor that affects the measurement,accurate results can be obtained.


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