In
this work, the in-tip thermal infrared enthalpimetry (in-tip
TIE) method is proposed for fast enthalpimetric analysis. In this
method, the reactions inside the tips of a multichannel pipette were
combined with temperature monitoring by an infrared camera. The filter
paper was used inside the tips to retain reagents as solutions (wetted
paper mode) or as solids (dried paper mode) to perform neutralization,
redox, or precipitation reactions. The dried reagents inside the tips
were obtained by oven drying a solution retained in the filter paper.
The determination of the total acidity of the vinegar, ascorbic acid
in vitamin C tablets, and chloride in soy sauces and saline inhalation
solutions was performed as examples of the application of the proposed
method. The agreement with reference methods ranged from 98 to 107%.
The use of reagents dried inside the tip was feasible, leading to
a simple aspiration of sample solution within the 12 tips of the pipette
to perform a rapid analysis (1 min). Therefore, up to 720 measurements
in 1 h were feasible for in-tip TIE over up to 12 measurements for
the reference methods. Moreover, miniaturization reduced reagent consumption
and residue generation. For example, for in-tip TIE, only 3.6 mL of
residues was generated (n = 12) over 60–240
mL in reference methods (n = 3). Contrarily to other
TIE methods, no microplates or stirring was required, opening possibilities
for field analysis since the multichannel pipette and the infrared
camera are both operated with batteries.
The determination of eugenol in clove essential oil was performed using a smartphone-operated device, which was used for image capture and processing. The colorimetric reaction with the Folin-Ciocalteu reagent was used, and the lighting conditions were evaluated to capture images directly in 2 mL disposable vessels. The free application PhotoMetrix UVC was used for partial least squares regression calibration with suitable values (R² greater than 0.99). The accuracy of the proposed method was compared with traditional methods, such as gas chromatography (GC) and spectrophotometry, and it can be observed that there were no significant differences (Student’s t-test (P > 0.05), with agreements from 97% to 101%. The smartphone method allowed the evaluation of several samples in a few minutes, with simple analysis steps and easy interpretation of the results. The miniaturized scale allowed the use of small amounts of reagents with minimal waste generation. Therefore, the proposed method can be easily operated in the field and allows the evaluation of the quality of clove essential oil in places of restricted access without the need for a laboratory structure and specialized analysts.
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