Journal Pre-proof

Effect of coffee cherry maturity on the performance of the drying process of the bean:
Sorption isotherms and dielectric spectroscopy

Sebastián Velásquez, Arlet P. Franco, Nestor Peña, Juan Carlos Bohórquez, Nelson
Gutierrez

PII: S0956-7135(20)30608-3
DOI: https://doi.org/10.1016/j.foodcont.2020.107692
Reference: JFCO 107692

To appear in: Food Control

Received Date: 9 July 2020

Revised Date: 1 October 2020
Accepted Date: 10 October 2020

Please cite this article as: Velásquez Sebastiá., Franco A.P., Peña N., Bohórquez J.C. & Gutierrez N.,
Effect of coffee cherry maturity on the performance of the drying process of the bean: Sorption isotherms
and dielectric spectroscopy, Food Control (2020), doi: https://doi.org/10.1016/j.foodcont.2020.107692.

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 AUTHORSHIP STATEMENT
Manuscript title: Effect of coffee cherry maturity on the performance of the drying process of the
bean: sorption isotherms and dielectric spectroscopy

All persons who meet authorship criteria are listed as authors, and all authors certify that they have
participated sufficiently in the work to take public responsibility for the content, including participation in
the concept, design, analysis, writing, or revision of the manuscript.

Authorship contributions
Each of the authors has contributed in the following tasks:

Sebastian Velasquez: Methodology, Software, Formal Analysis, Investigation, Writing – Original Draft

Arlet Franco: Methodology, Validation, Visualization, Writing - Review & Editing

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Juan Carlos Bohorquez: Conceptualization, Project administration, Funding acquisition

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Nestor Peña: Conceptualization, Data Curation, Supervision
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Nelson Gutierrez: Conceptualization, Methodology, Investigation, Resources
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Acknowledgements
All persons who have made substantial contributions to the work reported in the manuscript (e.g., technical
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help, writing and editing assistance, general support), but who do not meet the criteria for authorship, are
named in the Acknowledgements and have given us their written permission to be named. If we have not
included an Acknowledgements, then that indicates that we have not received substantial contributions
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from non-authors.
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This statement is signed by all the authors:

Author name Signature Date
Jo

Sebastián Velásquez 07-10-2020

Arlet P. Franco 07-10-2020

Juan C. Bohórquez 07-10-2020

Néstor Peña 07-10-2020

Nelson Gutierrez 07-10-2020

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re
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na
ur
Jo
 Dear A Achuthan,

You are right on the affiliations. I rectify the information below:

(a) Author (s): Sebastian Velasquez / Affiliation: Research & Development department, Industria

Colombiana de Café, Medellín, Antioquia, Colombia

(b) Author(s): Arlet P. Franco / Affiliation: DANM/ Desarrollo y Aplicación de Nuevos Materiales,

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School of Engineering and Architecture, Universidad Pontificia Bolivariana, Montería, Colombia

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(c) Author(s): Juan Carlos Bohorquez, Nestor Peña / Affiliation: Department of Electrical and
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Electronics Engineering, Universidad de los Andes, Bogotá
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(d) Author(s): Nelson Gutierrez / Affiliation: Department of Agriculture Engineering, Universidad

Surcolombiana, Neiva Huila, Colombia

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na

Best regards,
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Jo
 1

1 Effect of coffee cherry maturity on the performance of the drying process of the bean:
2 sorption isotherms and dielectric spectroscopy
3
4 Sebastián Velásquez a*, Arlet P. Francob , Nestor Peña c, Juan Carlos Bohórquez c, Nelson
5 Gutierrezd
6
a
7 Research & Development department, Industria Colombiana de Café, Medellín, Antioquia,
8 Colombia; b DANM/ Desarrollo y Aplicación de Nuevos Materiales, School of Engineering and
9 Architecture, Universidad Pontificia Bolivariana, Montería, Colombia; aDepartment of Electrical
10 and Electronics Engineering, Universidad de los Andes, Bogota

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d
11 Colombia; Department of Agriculture Engineering, Universidad Surcolombiana, Neiva Huila,

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12 Colombia
13
14
Abstract -p
The study of the dynamic sorption isotherms of parchment coffee revealed that the maturity stage has an
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15 effect on the water availability of the bean, and that such dependence might affect the bean drying. The
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16 cultivar had an impact on the dispersion at high water activity values (aw > 0.8); hence, depicting dissimilar
17 conditions before the drying is actually performed. The Guggenheim-Anderson-de Boer (GAB) sorption
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18 model revealed that stages 2, 3 and 7 present higher monolayer moisture content (Xm), K values close to one
19 for all stages indicated a multilayer behaviour close to free water mobility and low C values for stages 2 and
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20 7 represented a stronger water binding to the monolayer for these stages. Under static conditions and the
21 drying conditions defined according to the moisture content of the beans, the unripe stages depicted an
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22 accelerated water activity decay that might promote stalling after roasting due to low values of the attribute
23 (aw < 0.4). In a second phase of the study, the dielectric spectroscopy technique was used to evaluate the
24 effect of the maturity and the drying category, and the response depended on the drying category rather than
25 on the maturity stage except for the drying category with the higher moisture content range. The dielectric
26 constant was utilized to predict both the moisture content and the water activity of the beans. The kernel-
27 based ridge method with radial basis function for the moisture content and sigmoid function for the water
28 activity model had good performance (R2: 0.82 – 0.88). A feature selection model based on a pipelined
29 framework to include the whole spectra selected the 0.3 GHz to 0.9 GHz range as the optimal estimator,
30 which was consistent with the performance of the single frequency models at 0.3 GHz. Although the errors
31 were lower for the feature selection model, the single frequency is preferable as it has minimal complexity.
32 As a non-linear dependence was evidenced, the machine learning strategies were necessary to respond to this

*Corresponding author.
Email addresses: svelasquez@colcafe.com.co - Phone: +573508844100 - Address: Calle 8 sur # 50-67 – Medellín –
Colombia (Sebastián Velásquez), arletfranco@gmail.com (Arlet P. Franco), jubohorq@uniandes.edu.co (Juan
Carlos Bohórquez), npena@uniandes.edu.co (Néstor Peña), ngutierrezg@usco.edu.co (Nelson Gutiérrez)
33 condition. Consequently, the technology could be considered for the assessment of the water features of the
34 bean during coffee drying or the storage of green coffee.

35 Keywords: Coffee drying • Complex permittivity • Machine learning • Coffee postharvest • Coffee

36 quality

37 1 Introduction
38 As one of the most consumed products, coffee goes through an extensive post-harvest

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39 process to produce beans adequate for the brewing of the worldwide consumed beverage. A critical

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40 step before roasting is the drying process, which must be performed to obtain parchment coffee

41 -p
with a moisture content of 12%. In the case of natural coffees, the cherries go straight to the drying
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42 stage and hulled to remove the peel after reaching the desired moisture content (Arcila et al., 2007).
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43 Despite of the process, the drying is delicate as the hygroscopic nature of coffee and could impact

44 both the aroma and flavour, as it has a crucial role on how the Maillard and Strecker reactions occur
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45 inside the bean during the roasting process (Corrêa et al., 2010).
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46 The behaviour of the moisture content of coffee can be described in two phases: the wet (30
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47 – 60% w.b.) and the hygroscopic phases (11 – 30% w.b.). As the dehydration of the bean is a

48 vapour/liquid diffusion process, heat and mass transfer phenomena occur as the bean losses water

49 (Singh & Heldman, 2007). In the wet phase, the moisture content decreases at a constant drying

50 rate. Contrarily, the hygroscopic phase follows a falling drying rate. Hence, inadequate handling

51 during the falling drying rate phase might promote spoilage of the beans. There are four conditions

52 that must be checked during the drying process (Tavares-de-Andrade & Borém, 2019; Wintgens,

53 2014): the bean temperature should not exceed 40 °C, the coffee mass should be homogeneous by

54 stirring the mass and having beans of similar characteristics. Additionally, the temperature, air flow

55 and relative humidity conditions should be controlled, while drying rates should not be altered to

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56 avoid unstable water mobility outside the bean. Often, bean spoilage occurs due to uncontrolled

57 bean temperature or steep temperature gradients that lead to over-drying of the mass (Isquierdo et

58 al., 2013; Tavares-de-Andrade & Borém, 2019), and failure of the pericarp and endosperm (Borém

59 et al., 2008). This spoilage also impacts the beverage (Clarke & Macrae, 1987), as roasting of

60 cracked beans is related to the presence stale notes in the cup (Hameed et al., 2018). As coffee is

61 not immediately roasted, safe storage must be also guaranteed. The moisture content is often used to

62 indicate the drying rate, whereas the water activity is the physical parameter that should be assessed

63 for storage and shelf life evaluations (Singh & Heldman, 2007). Although a water activity value

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64 below 0.4 guarantees food safety, Maillard reactions perform best at water activity values close to

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65 0.65 (Mathlouthi, 2001).

66
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Measuring the moisture content and the water activity, especially at the crop is not always
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67 an easy task (Caporaso et al., 2018). Although technology for both is widely available (Bogart,
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68 2014), not all are compatible with the crop and farm. As the drying process is often performed close
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69 to the crop, a good understanding of the thermodynamics involved in the process serves as a quality

70 assessment alternative (Escribano et al., 2017; Goneli et al., 2013).

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71 Considering the potential and versatility of the technology, microwave-based applications

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72 are an attractive alternative. The technology has served as backbone for moisture content sensors

73 (Bogart, 2014), and extended to operate as drying technology as well (Muñoz-neira et al., 2020;

74 Wintgens, 2014). These applications suggest that the technology evidently responds to the water

75 availability of the matrix. The complex permittivity of the samples, if considered in the microwave

76 range, is indicative of the molecular composition and is represented by a complex number (Eq. (1))

77 that depends on both the frequency and the temperature (Franco et al., 2015).

̂= − (1)

78 The real part of ̂ is the relative electrical permittivity or dielectric constant ( ), and the

79 imaginary part of ̂ is the dielectric loss factor ( ) with = √−1 . The electrical permittivity

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 80 represents the ability of the material to polarize and to store electric energy in response to an

81 applied electric field, and the loss factor is associated with the dissipation of energy as heat (Sosa-

82 Morales et al., 2017).

83 The technique has been successfully used in similar food matrices to characterize the

84 moisture content and water activity (Trabelsi et al., 2019), and allowed for the study of the moisture

85 content and water features in parchment, green and roasted coffee (Berbert et al., 2008; Iaccheri et

86 al., 2015, 2019). These applications often assume linear dependences, but if this is not the case, the

87 application of the technology is restricted.

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88 Machine learning techniques allow the implementation of multivariate non-linear models.

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89 The combination of feature selection strategies (Li et al., 2018), meta-parameter optimization (Fashi

90
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et al., 2019; Yang et al., 2019) and pipelined frameworks for module integration result in versatile
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91 and accurate models (Piedad et al., 2018) that are compatible with post-harvest processes
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92 (Rungpichayapichet et al., 2016).

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93 This paper presents the dynamic sorption isotherms by the DDI method to evaluate the

94 effect of the maturity stage on the dynamics related to the drying process. The dielectric
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95 spectroscopy technique was used to obtain the permittivity of the beans according to the maturity
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96 stage and specific drying moments. After evaluating the effect of the described factors on the

97 dielectric features of the beans, the potential of the technique to predict both the moisture content

98 and water activity was considered by implementing machine learning based regression models. The

99 accuracy of the models was finally evaluated and discussed.

100 2 MATERIAL AND METHODS

101 2.1 Coffee samples

102 Coffee cherries at 7 maturity stages were harvested, with 3 biological replicates for each of

103 the maturity-cultivar combinations. Maturity stage 1 represents green unripe cherries, which occur

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104 196 days after flowering (DAF) (Marín et al., 2004). Stage 2 corresponds to green-yellow cherries

105 (i.e., 203 days), and stages 3 and 4 to almost ripe or "pintón" cherries (i.e., 208-215 days). The

106 separation between these stages was performed according to variations of the redness and firmness

107 of the fruit. Stages 5 and 6 represent ripe cherries (i.e., 217-224 days) while stage 7 (i.e., after 224

108 days) represents overripe fruits. Only red varietals were considered for this study. The origins of the

109 coffee cultivars were two farms from northern Huila and one from southern Huila. Once collected,

110 the cherries were stored at 8 °C and processed within a maximum timeframe of 6 – 8 h at the South

111 Colombian Coffee Research Centre – CESURCAFE pilot plant (Neiva, Colombia).

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112 2.2 Coffee processing
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Once the samples were received at the plant, the cherries were pulped in a Gaviota 300 thresher
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114 (Bogotá, Colombia) and dry fermented during 18 h in plastic containers without cover. Then, the
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115 samples were thoroughly washed to remove any mucilage residues. The drying of the seeds was

116 performed in a parabolic sun dryer with African beds, at an average temperature of 42 °C on the
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117 beds and a relative moisture of 65%, according to the measurements of data-loggers that were
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118 installed in the dryer and the beds. The seeds were stirred every 5 h to avoid over-drying or
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119 breakage of the beans. After stirring, a portion of the samples was carried back to the laboratory for

120 moisture content and water activity measurements. The drying progress was discriminated in

121 categories from A to E according to the moisture content: beans with moisture content superior or

122 equivalent to 40% (A), between 40 and 30 (B), between 30 and 20 (C), between 20 and 12 (D) and

123 values below 12% (E). Categories A and B correspond to the wet phase, and the remaining to the

124 hygroscopic phase.

125 2.3 Moisture content and water activity

126 The moisture content of high moisture samples (i.e., stages A to D) was measured by the wet

127 basis gravimetrical method according to ISO 6673 standard (Adnan et al., 2017). The sample

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128 containers were aluminium tins that were previously weighed (i.e., WT). Then, a 5 g of coffee

129 sample was deposited into the tin and weighed again (i.e., WW+WT) and dried at 105 °C for 24 h

130 in a Memmert 55 oven (Schwabach, Germany). After removing the samples from the oven, the

131 weight of the tins was measured again (i.e., DW+WT). The moisture content of each sample was

132 calculated according to Equation (2) (Adnan et al., 2017).

( + )−( + ) (2)
% = ⋅ 100
100 ( + )−

133 For low moisture content samples (i.e., E), the measurements were carried out with a

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134 Gehaka Agri Moisture Tester G600 (Sao Paulo, Brazil) and a moisture sensor (Kett PM−450,

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135 Science of Sensing, Japan) for validation.

136
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For the water activity measurements, the dynamic dew point method (DDI) was employed
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137 (Gentil et al., 2019; Iaccheri et al., 2015) and utilized in dynamic mode for isotherm generation and
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138 in static mode for water activity characterization of the drying categories in a vapour sorption
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139 analyser (VSA Aqualab Decagon Device, Inc. Pullman, WA, USA). For dynamic isotherm analysis,

140 a sample (2 to 3 g) of whole parchment coffee beans classified according to the maturity stage and
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141 cultivar was inserted into the receptacle after being washed according to section 2.2. By applying
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142 desiccated dry air to the sample, the desorption curves were obtained. Once the equilibrium weight

143 was reached at a specific water activity value, the moisture content was calculated according to the

144 formerly presented procedure. The isotherms were characterized between 0.1 and 0.9 for every

145 maturity - variety combination at 25 °C. The flow rate was set to 100 ml ⋅ min$% , with water

146 activity steps of 0.05. The second set of tests were performed on static mode, once the samples were

147 classified according to the drying category. A portion of 2 to 3 g from the batch separated for

148 dielectric analysis was inserted into the receptacle and the water activity recorded once equilibrium

149 was reached. These measurements were also performed at 25 °C. These water activity values were

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150 analysed in triplicate. Finally, samples were chilled at 4 °C under vacuum conditions until dielectric

151 analysis.

152 2.4 Dielectric spectroscopy characterization

153 The dielectric spectroscopy characterization was performed on a planar dielectric platform

154 (Velasquez et al., 2018) and a Rohde & Schwarz ZVB20 4-port network analyser (Munich,

155 Germany). The device was calibrated with the thru-open-short-line (TOSL) method from 0.3 to 10

156 GHz, with 801 frequency points and an intermediate frequency filter configuration of 10 kHz. Prior

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157 to analysis, the vector network analyser was warmed up for at least 90 min. After calibration, the

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158 cables were fixed to avoid any interference. A LabView (National Instruments, Austin, United

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States) API was developed to retrieve the S parameter matrix, and it automatically computed the
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160 dielectric permittivity and the loss factor from the acquired matrix. The platform accuracy was first
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161 validated with distilled water, ethanol, and methanol samples at 20 °C. This validation was

162 performed for every sample measurement and updated the correction parameters loaded in the API.
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163 A batch of 40 g of parchment coffee stored at 4 °C under vacuum conditions for no longer than
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164 1-2 weeks after drying was used for testing. Thermal stabilization was allowed for 90 min, in a
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165 room with controlled temperature (20 °C) and relative moisture (65%) conditions. After this period,

166 the temperature of the batch was validated and the measurement started once the temperature of the

167 sample was 20±0.5 °C.

168 Previous studies report the effect of the bulk density on the dielectric properties of grains

169 (Trabelsi et al., 2019). Consequently, to preserve the bulk density constant for every replicate, the

170 sample was poured into a bottom-closed funnel, located above the sensing zone of the device. After

171 depositing the sample inside the funnel, the sample was allowed to freely flow into the sensing zone

172 of the platform until it overflowed out of the container. The excess beans were removed with a

173 standard.

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174 After each measurement, the sensing zone of the platform was cleaned with distilled water and

175 dried with soft paper. All the dielectric properties measurements were performed in independent

176 triplicates.

177 2.5 Data analysis

178 The modified Guggenheim-Anderson-de Boer (GAB) equation was used to model the isotherms

179 (Goneli et al., 2013), as presented in Equation (3) (Singh & Heldman, 2007)

&( )*+, (3)

&' =
(1 − *+, ) ⋅ (1 − *+, + )*+, )

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180 Where &' represents the equilibrium moisture content (%, wet basis), +, represents the water

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181 activity, &( represents the monolayer moisture content, and C and K are constants related to the

182
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monolayer and multilayer properties. Non-linear least squares method was used to fit the models.
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183 The estimated fit was analysed to evaluate the effect of maturity. The GAB model was obtained
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184 for each maturity-cultivar isotherm. An analysis of variance (ANOVA) test was computed for each
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185 fitted parameter with maturity as the fixed factor and the cultivar as the blocking effect. After

186 computing the least squares mean, Tukey pairwise comparisons were computed to validate the
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187 effect of the maturity of cherries on the model parameters. For the dielectric results, the same
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188 procedure was employed to evidence the effect of the maturity and drying stage at each frequency.

189 This procedure was performed for the dielectric constant, the loss factor and the loss tangent.

190 As the dielectric behaviour was considered the input for moisture content and water activity

191 values as drying advanced, two types of models were used: feature selection (Yang et al., 2019) to

192 consider the whole spectra, and single frequency as an univariate model. For the feature selection

193 approach, extremely randomized trees methodology was considered with recursive variable

194 elimination to select the most relevant features. The root mean squared error (RMSE) was

195 considered as the cross-validation criteria.

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196 The selected features were then mean-centered and scaled. This new matrix was analysed by

197 principal component analysis (PCA) (Costa et al., 2012) by SVD decomposition. Subsequently, the

198 PCA components were used as the input of the regression model which were fed to a pipelined

199 framework: component selection, hyper-parameter calculation, and model fitting.

200 Three regression techniques were considered (Yang et al., 2019): random forests, support vector

201 machine (SVM) and k nearest neighbours (k-NN). The data was partitioned into two sets: a segment

202 for training and the remaining for validation, stratifying the observations by the drying categories.

203 This partition was randomly performed 100 times as a quasi-bootstrapping approach.

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204 For the single frequency models, kernel based ridge regression was considered. The dielectric

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205 constant at 300 MHz, 6 GHz and 10 GHz were selected as the exogenous parameter. According to

206
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the response seen for the dielectric constant, the moisture content was modelled with a radial basis
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207 function and the water activity with a sigmoid function. Hyper-parameter selection and dataset
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208 partitioning was identical to the feature selection strategy.

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209 Linear mixed effect models were computed with the lmer and lsmeans R packages version 3.3.6

210 and machine learning models were implemented with the scikit-learn package in Anaconda with
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211 Python 3.7.

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212 3 RESULTS AND DISCUSSION

213 3.1 Sorption isotherms and maturity

214 Figure 1 presents the sorption isotherms for each maturity stage. The response obtained agreed

215 with previous results reported for green coffee in the literature, especially the monolayer moisture

216 content (Goneli et al., 2013; Iaccheri et al., 2015).

217
218 The curve form agrees with Type III isotherms that are representative of crystalline structures

219 (Corrêa et al., 2010; Iaccheri et al., 2019). Possible differences might be related to the presence of

220 the hull in parchment coffee.

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221 The isotherms depict a higher dispersion at water activity values above 0.8, which suggests that

222 the cultivar has an effect on the initial moisture content after fermentation and washing. This effect

223 is more important at low maturity stages (1 and 2), and reduces as the cherry develops. The crossing

224 of the curves might also suggest that the thermodynamics of drying might be affected by the

225 maturity stage. In a physical sense, the dependence of the bulk density on the bean development

226 (Marín et al., 2004) and the response of the isotherms behaviour suggest that drying might be non-

227 uniform if the mass maturity is not homogeneous (Tavares-de-Andrade & Borém, 2019). The mean

228 values for each stage and the statistical significance of the GAB model parameters are presented in

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229 Table 1.

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230 C and K values indicate that the monolayer and the multilayer are different, and that the

231
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multilayer behaves similar to the bulk liquid (Quirijns et al., 2005). K presented a high value for
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232 stage 1, decreased for stage 2 and the it slowly increased towards stage 6, with a considerable
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233 reduction for stage 7. If the structure of the bean is considered (De Castro & Marraccini, 2006), in
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234 stage 1 the endosperm reaches its maximum fresh weight and the pericarp is not fully developed.

235 Hence, as most of the weight of the endosperm comes from the water content, the multilayer depicts
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236 liquid mobility and rapidly decays towards stage 2 as the moisture content of the endosperm is
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237 considerably reduced during the following development days. In stage 7, the pericarp has its

238 maximum weight and the endosperm weight is reduced. Consequently, water availability decays

239 and again the multilayer depicts a different behaviour as the major weight gain is associated to the

240 perisperm. Consequently, the multilayer is specifically defined for stages 2 and 7, while mobility in

241 the remaining stages is associated to the liquid phase. Parameter C, which is mainly related to the

242 enthalpy, is maximum for stage 1 and decreases towards stage 3. It has values close to 15 for stages

243 4, 5, and 6 and has a minimum for stage 7. Consequently, water is highly bounded to the monolayer

244 for stage 1 and weakly bounded for stage 7. This might be also related to the process of weight

245 gaining for unripe stages and the weight gain of the perisperm and weight loss of the endosperm for

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246 overripe beans. The monolayer moisture content depicted values close to 5.5 for stages 1, 4, 5 and 6

247 while it depicted elevated values for stages 2 and 3, with a maximum for stage 7. As this parameter

248 represents the active sites for water sorption, higher Xm might result in hazardous conditions for the

249 product as water adsorption is promoted. Hence, respiration and protection against fungal

250 development might be more critical at overripe stages and during the posterior development of the

251 bean (stages 2 and 3).

252 From the drying side, the coffee cherries considered for this study presented a full elongation of

253 the endosperm and where in the pericarp maturation phase (De Castro & Marraccini, 2006).

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254 Consequently, the major changes occurring inside the cherry were the development of the exocarp,

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255 mesocarp and endocarp. As the exocarp and mesocarp are fully removed during wet processing, the

256
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permeability and development of the endocarp (parchment) and the endosperm define the water
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257 availability and mobility during the drying process. Values close to 1 for K suggest that a more
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258 accelerated decay of the moisture content after aw - 0.7 for ripe stages is possible, which might have
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259 an impact on the falling drying rate regime and inadequate water removal if not well handled

260 (Wintgens, 2014).

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261 The desorption isotherms were considered as an exploratory tool to identify possible differences
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262 on the water availability in parchment coffee during the bean drying. However, the phenomena

263 occurring at the cellular level and other features related to the thermodynamics of drying need to be

264 further study. The study of the glass transition temperature provides information on the stability of

265 the process and solid-liquid transitions (Iaccheri et al., 2019), which can be extracted from dynamic

266 scanning calorimetry. The analysis of the inflection points of the dynamic sorption isotherms at

267 different temperatures are also indicative of this parameter (Carter & Schmidt, 2012).

268 3.2 Moisture content and water activity: maturity and drying
269 Figure 3 presents the bar plot for the moisture content of the parchment coffee samples as a

270 function of drying and maturity.

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271 Figure 2 depicts the classification consistency according to the moisture content. The highest

272 moisture contents were evidenced for unripe beans. The moisture content for stage A ranged

273 between 52 and 61% and presented significant differences across the maturity stage. This result

274 supports the dispersion seen around aw – 0.9 of the isotherms. Furthermore, as the moisture content

275 is reduced, the differences are also dissipated. Higher stability was achieved once the falling rate

276 phase was reached (stages C, D and E). Figure 3 presents the water activity values for the same

277 analysis.

278 Drying categories A, B and C (i.e., moisture contents between 20 and 60%) are in the free-

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279 solvent water region. For these categories, maintaining the bean mass temperature is not critical as

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280 water availability restricts steep temperature rates (Wintgens, 2014). Nevertheless, categories D and

281
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E depict an accelerated decay when compared to the aforementioned stages. This behaviour is more
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282 evident for unripe beans, which reach values below 0.5 once the final moisture content was reached.
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283 Therefore, flavour stalling might occur due to the oxidation and loss of certain flavour precursors
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284 that occur at this water activity values (Mathlouthi, 2001). Figure 3 confirms that although all

285 samples started at the free-solvent water phase with similar water activity values, the impact of
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286 maturity is more critical for the falling drying rate regime. Consequently, the water activity
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287 exhibited that immature beans might promote defect generation during the falling drying rate phase

288 due to fast variations with marginal moisture content reduction.

289 3.3 Dielectric spectroscopy response

290 Figure 4 presents the dielectric permittivity of the samples as a function of frequency. The

291 dielectric permittivity of parchment coffee depicted higher values for green unripe (stage 1)

292 samples, which agrees with the elevated moisture content seen for this stage in drying categories A

293 and B. For drying, the higher dielectric permittivity was seen for category B and gradually reduced

294 for the following categories. Figure 5 presents the response of the loss factor.

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295 The highest losses were obtained for green unripe beans, with the maximum losses reached at 10

296 GHz. An effect on the transition from the ionic conduction to the dipolar rotation region were

297 perceived when maturity was considered. Drying category B depicted the highest losses and the

298 parameter reduced as the moisture content of the bean decreased. A slight increase of the transition

299 frequency was evidenced for category E. These findings result useful when considering the design

300 of microwave-based technologies for parchment coffee moisture removal (Muñoz-neira et al.,

301 2020). Figure 6 presents the response for the loss tangent.

302 This feature presented the lowest dispersion of the three. The region between 1.5 and 3 GHz

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303 shows no intersections of the curves; hence, it could be used for classification of the drying phase.

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304 The dielectric permittivity at 300 MHz is presented in Figure 7.

305
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The behaviour seen for the dielectric permittivity resembles the results for the moisture content.
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306 Consequently, the dielectric constant is responding to the moisture content reduction , except for
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307 category B in which the maturity is a significant factor (Berbert et al., 2008; Iaccheri et al., 2015).
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308 The presented values for the dielectric constant are lower than those reported for other grains (S.

309 Trabelsi & S. O. Nelson, 2012), but the losses are higher. These results are in agreement with
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310 previous studies of parchment coffee (Berbert et al., 2001). The comparison between specifics of
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311 the coffee matrix, the temperature and the bulk density should be further considered to extend the

312 application of these findings.

313 3.4 Modelling of the moisture content and water activity

314 The dataset employed for modelling is presented in Figure 8, with the clustering for each of the

315 drying categories according to the covariance. This information was considered as the input of the

316 dielectric spectroscopy-based models.

317 With this dataset, that clearly reflects the response seen for the isotherms and the dispersion

318 associated to the maturity at high water activity values, the dielectric permittivity at 300 MHz was

319 plotted versus the moisture content and the water activity to evaluate their correlation (Figure 9).

13
320 The fitted non-linear regression of the kernel-based ridge regression is included as a dashed line in

321 the plot.

322 The correlation between the two variables can be addressed in two sections: stages D and E that

323 depict an exponential increase, and a logarithmic trend for stages B and C. Consequently, this

324 performance motivated the selection of the radial basis function for prediction. A higher dispersion

325 was obtained for categories B and C, as expected. Therefore, the radial basis function at this

326 frequency represents a stable response for the moisture content. Figure 10 presents the correlation

327 with the water activity.

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328 The category clustering was more disperse for all categories when compared to the moisture

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329 content. The form of the response suggested a sigmoid behaviour, which again depicted a coherent

330
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fit with the data. Previous studies reported a quadratic dependence of the water activity on the
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331 dielectric properties, when a density-independent dielectric function was used (Trabelsi et al.,
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332 2019). However, saturation after aw-0.8 could not be properly modelled with a quadratic function.
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333 To account for the information contained in all frequencies, the bi-plot from the principal

334 component analysis is displayed in Figure 11.

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335 Stages B and C depict more disperse clustering; hence, higher dispersion for these categories is
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336 seen as presented in previous results. The first component, which represents more than 99% of the

337 variability, is segregating across sorption behaviour: free water and constant rate phase in the

338 positive side, and linear or monolayer regime in the negative side. The second component is more

339 related to maturity, although not forcefully.

340 The feature selection model selected the 0.3 - 0.9 GHz frequency range as the best predictor for

341 both the moisture content and water activity. Table 2 presents the RMSE and determination

342 coefficients for the single frequency and feature selection models for the moisture content

343

14
344 The information on the meta parameters for each technique is presented in Table S1 in the

345 supplementary material. Table S2 and S3 present the results for the remaining attributes: the loss

346 factor and the loss tangent for the feature selection models. The supplementary data file also counts

347 with averaged predicted vs. real and residuals plots for the feature selection models. The single

348 frequency models performed best for the dielectric constant also. The determination coefficient for

349 the averaged test sets fluctuated between 0.86 and 0.88 for both approaches. The errors varied

350 between 11.6 and 14.9, which is important for categories D and E but might be appealing for the

351 remaining as technology to measure the feature on site is scarce. The statistics were slightly better

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352 for the feature selection model; nevertheless, required of a more complicated model. The radial

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353 basis function seems adequate for moisture content modelling. The frequency with the best

354
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performance was 300 MHz, oppositely to other models that use frequencies close to 6 GHz or those
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355 close to the dipolar relaxation of water (Trabelsi, 2019). However, the results clearly suggest that
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356 non-linear and machine learning techniques are more adequate for this specific application that has
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357 a wide dynamic range (10 – 60%). Table 3 displays the fit statistics for the water activity models.

358 With similar results, the determination coefficient for the water activity model fluctuated
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359 between 0.82 and 0.88. The errors varied between 3.0·10-3 and 4.5·10-3. Considering that the
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360 resolution for the dynamic sorption isotherms was 0.05 and that this allowed the identification of

361 basic phenomena related to water availability, the dielectric constant has remarkable performance

362 for water activity prediction. As with the moisture content model, the feature selection model

363 depicts a slight improvement when compared to the single frequency model but at the cost of higher

364 complexity. The frequency with the best performance was 300 MHz as with the moisture content.

365 The sigmoid assumption for the kernel selection was also adequate. The kernel-based strategies

366 used in this work allowed for good prediction models despite of not compensating for temperature

367 and bulk density effects. Further studies on the influence of these parameters could serve for model

368 improvement.

15
369 4 CONCLUSION

370 The dynamic sorption isotherms by the DDI method depicted that the drying behaviour

371 might depend on the maturity of the beans, especially for the constant drying rate regime. The

372 impact of the varietals was more evident at water activity values above 0.9. As the bulk density and

373 water availability depend on the maturity, having beans at different development phases might

374 result in non-uniform drying of the mass and therefore deterioration of the product due to

375 inadequate drying. The statistical comparison of the averaged GAB parameters supported this

376 conclusion. Most of the behaviour associated to the bean development is related to the weight

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377 reduction of the endosperm and weight gaining of the perisperm. Considering temperature related

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378 phenomena and the cellular structure of the beans could provide more information on the

379 thermodynamics and possibilities for coffee drying.

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380 The dielectric spectroscopy analysis depicted that all features (dielectric constant, loss factor
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381 and loss tangent) responded to the effect of drying, while only responded to the maturity stage for
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382 category B. Nevertheless, the dielectric constant is varying accordingly for the two drying regimes:
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383 constant and falling drying rate. The effects of the drying temperature and bulk density of the beans

384 should be also considered to deepen the findings of this work.

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385 The use of machine learning strategies was pertinent as non-linear behaviour was identified

386 for both the moisture content and the water activity when correlated to the dielectric constant. The

387 single frequency models are a better alternative, as they are simpler and resulted in similar results

388 than those found for the feature selection models. The improvement of the latter might be related to

389 the augmentation of the predictor matrix rank. The results of this study contribute to the

390 understanding of the effects of maturity on the drying of parchment coffee, while revealing that the

391 dielectric spectroscopy technique is an appealing alternative to study water availability features for

392 coffee processing.

16
393 5 ACKNOWLEDGMENTS
394 Physicochemical analyses of coffee and sample collection were performed by members of

395 the Cesurcafé research centre at Universidad Surcolombiana. Dielectric spectroscopy measurements

396 were performed by William Romero at Universidad de los Andes, Bogota, Colombia.

397 6 FUNDING
398 This project was funded by the Colombian Science Council - Colciencias (The science,

399 technology, and development management department). Specifically, by grant “Proyecto CAFES”,

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400 number 120471551893.

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515 classification of apricots (Prunus armeniaca L.) based on shape features. Scientia
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516 Horticulturae, 256(May), 108524. https://doi.org/10.1016/j.scienta.2019.05.051

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517
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518

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519 Tables & Figures

520 Table 1. Average K, C and Xm parameters of the GAB model according to the maturity stage.
521 Group discrimination by significance is presented in the superscript.
522 Table 2. Root mean squared error (RMSE) and determination coefficient (R2) for the single
523 frequency and feature selection models for moisture content prediction. The training and test
524 information for both are reported. Frequencies for single frequency and technique for feature
525 selection are reported in the columns.
526 Table 3. Root mean squared error (RMSE) and determination coefficient (R2) for the single
527 frequency and feature selection models for water activity prediction. The training and test
528 information for both are reported. Frequencies for single frequency and technique for feature
529 selection are reported in the columns.
530 Figure 1. Dynamic sorption isotherms for each maturity stage - desorption.

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531 Figure 2. Moisture content of parchment coffee – effect of maturity (categories in X axis) and

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532 drying (coded in bar colour)
533 Figure 3. Water activity of parchment coffee – effect of maturity (categories in X axis) and drying
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534 (coded in bar colour)
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535 Figure 4. Dielectric constant of parchment coffee – effect of maturity (left plot) and drying stage
536 (right plot) – frequency in GHz is represented in a log-axis
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537 Figure 5. Dielectric loss factor of parchment coffee – effect of maturity (left plot) and drying stage
538 (right plot) – frequency in GHz is represented in a log-axis
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539 Figure 6. Dielectric loss tangent of parchment coffee – effect of maturity (left plot) and drying
540 stage (right plot) – frequency in GHz is represented in a log-axis
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541 Figure 7. Dielectric constant of parchment coffee at 300 MHz – effect of maturity (categories in X
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542 axis) and drying (coded in bar colour)

543 Figure 8. Moisture content and water activity: DDI method in static mode. Colour of the markers
544 represents the drying category and the marker shape represents the maturity stage.
545 Figure 9. Moisture content and the dielectric constant at 300 MHz. Colour of the markers
546 represents the drying category and the marker shape represents the maturity stage. Shaded regions
547 represents covariance ellipse for clustering. Dashed line represents fitted model with kernel-based
548 ridge regression with a radial basis function.
549 Figure 10. Water activity and the dielectric constant at 300 MHz. Colour of the markers represents
550 the drying category and the marker shape represents the maturity stage. Shaded regions represents
551 covariance ellipse for clustering. Dashed line represents fitted model with kernel-based ridge
552 regression with a sigmoid function.
553 Figure 11. PCA bi-plot - Left plot represents the scores. Marker colour represents the drying
554 category while the marker shape represents the maturity stage. Shaded regions represent the
555 covariance ellipse. The plot to the right represents the loadings, with the identification of three
556 critical frequencies: 300 MHz, 6 GHz and 10 GHz.

23
Table 1. Coefficient determination for the sorption isotherms for each maturity stage – GAB model

Stage K C Xm R2 RMSE
1 0.94±0.02cd 22.27±3.95c 5.74±0.64ab 0.99 0.73
2 0.84±0.24a 15.64±7.61b 6.67±3.84b 0.98 1.87
3 0.90±0.04bc 8.59±6.94a 6.52±1.34ab 0.98 1.59
4 0.92±0.06cd 15.63±7.62b 5.70±0.32ab 0.99 1.16
5 0.93±0.04bcd 13.94±7.05b 5.55±0.80ab 0.99 0.51
6 0.98±0.03d 15.48±7.89b 5.35±0.65a 0.99 0.51
7 0.88±0.05b 6.35±7.95a 7.23±1.79c 0.97 2.09

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Table 2. Determination coefficient and RMSE for moisture content models

Single frequency Feature selection

0.3GHz 6GHz 10GHz RF SVM k-NN
R2 – Tr. (%) 0.89 0.88 0.86 0.98 0.89 0.91
R2 – T. (%) 0.88 0.87 0.86 0.87 0.88 0.88
RMSE – Tr. 11.3 12.5 14.5 1.8 11.3 9.33
RMSE – T. 12.1 13.6 14.9 12.7 11.7 11.6

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Table 3. Determination coefficient and RMSE for water activity models

Single frequency Feature selection

0.3GHz 6GHz 10GHz RF SVM k-NN
R2 - Train 0.88 0.86 0.83 0.98 0.90 0.90
R2 - Test 0.86 0.84 0.82 0.86 0.87 0.88
RMSE – Tr.
Tr. 3.2x10-3 3.8x10-3 4.4x10-3 4.5x10-4 2.7x10-3 2.6x10-3
RMSE – T. 3.7x10-3 4.0x10-3 4.5x10-3 3.6x10-3 3.3x10-3 3.0x10-3

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 1 2 3 4 5 6 7

45
Water content (gH2O/100g of solids)[%]

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35

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15

10

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
aw
 1 22 33 44 5 6 7 Drying category: B C D E
1.0

0.9

f
0.8

oor
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0.7

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aw

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0.6

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0.5
Kernel based
ridge regression
0.4
1.2 1.4 1.6 1.8 2.0 2.2 2.4
ε’r @ 300MHz
 1 22 33 44 5 6 7 Drying category: B C D E
Scores plot Loadings plot
0.06
8
300 MHz
0.04
6
PC2:0.5% explained variance

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-0.04
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-40 -20 0 20 40 60 80 100 0.03 0.04 0.05 0.06

PC1: 99.51% explained variance
 Drying category: A B C D E
60
Water content (gH2O/100g of solids)[%]

50

40

f
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1 2 3 4 5 6 7
Maturity stage
 Drying category: A B C D E
1.0

0.9

0.8

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0.7

pr-
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P re
0.6

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0.4

0.3
1 2 3 4 5 6 7
Maturity stage
 1 2 3 4 5 6 7 Drying category: B C D E
Factor: Maturity 2.2 Factor: Drying
1.8
Relative dielectric permittivity – ε’

2.0
1.7

f
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1.8

pr
1.6

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1.6

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1.5

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1.4 1.4

1.3
1.2

0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0 0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0
Frequency [GHz] Frequency [GHz]
 1 2 3 4 5 6 7 Drying category: B C D E
0.35 Factor: Maturity 0.5
Factor: Drying

0.30
0.4
Relative dielectric loss – ε’’

0.25

f
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0.1
0.05

0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0 0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0
Frequency [GHz] Frequency [GHz]
 1 2 3 4 5 6 7 Drying category: B C D E
Factor: Maturity Factor: Drying
0.16 0.16

0.14 0.14
Loss tangent – tan δ

0.12 0.12

f
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0.10 0.10

e-
Pr
0.08 0.08

al
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0.06 0.06

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0.04 0.04

0.02 0.02

0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0 0.3 0.5 1.0 2.0 3.0 5.0 7.5 10.0
Frequency [GHz] Frequency [GHz]
 Drying category: B C D E
2.2

2.0

1.8

f
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pr
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Maturity stage
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5
0.4 0.5 0.6 0.7 0.8 0.9 1.0
aw
 1 22 33 44 5 6 7 Drying category: B C D E

40
Water content (gH2O/100g of solids)[%]

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Kernel based
ridge regression
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1.2 1.4 1.6 1.8 2.0 2.2 2.4
ε’r @ 300MHz
Highlights
• The dynamic sorption isotherms revealed that maturity might have an effect on coffee
drying
• Stalling and bean spoilage for unripe stages is possible due to accelerated water activity
decay
• Maturity affects the dielectric response of parchment coffee at high water activity values
• Radial basis and sigmoid functions were employed to model the water features of
parchment coffee
• Single frequency models are preferred over feature selection due to similar accuracy and
reduced complexity

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 DECLARATION OF INTEREST

We wish to confirm that there are no known conflicts of interest associated with this
publication and there has been no significant financial support for this work that could have
influenced its outcome, or personal relationships that could have appeared to influence the
work reported in this paper.

We confirm that the manuscript has been read and approved by all named authors and that
there are no other persons who satisfied the criteria for authorship but are not listed. We
further confirm that the order of authors listed in the manuscript has been approved by all of
us.

We confirm that we have given due consideration to the protection of intellectual property
associated with this work and that there are no impediments to publication, including the

of
timing of publication, with respect to intellectual property. In so doing we confirm that we
have followed the regulations of our institutions concerning intellectual property.

ro
We understand that the Corresponding Author is the sole contact for the Editorial process
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(including Editorial Manager and direct communications with the office). He is responsible
for communicating with the other authors about progress, submissions of revisions and final
re
approval of proofs. We confirm that we have provided a current, correct email address which
is accessible by the Corresponding Author and which has been configured to accept email
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lP

Signed by all authors as follows:

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Author name Signature Date

Sebastián Velásquez 07-10-2020
ur
Jo

Arlet P. Franco 07-10-2020

Juan C. Bohórquez 07-10-2020

Néstor Peña 07-10-2020

Nelson Gutierrez 07-10-2020