Accepted Manuscript

Agglomeration during spray drying: Physical and rehydration properties of whole milk/
sugar mixture powders

S. Chever, S. Méjean, A. Dolivet, F. Mei, C.M. Den Boer, G. Le Barzic, R. Jeantet, P.

Schuck

PII: S0023-6438(17)30307-9
DOI: 10.1016/j.lwt.2017.05.002
Reference: YFSTL 6218

To appear in: LWT - Food Science and Technology

Received Date: 29 October 2016

Revised Date: 2 May 2017
Accepted Date: 3 May 2017

Please cite this article as: Chever, S., Méjean, S., Dolivet, A., Mei, F., Den Boer, C.M., Le Barzic,
G., Jeantet, R., Schuck, P., Agglomeration during spray drying: Physical and rehydration properties
of whole milk/sugar mixture powders, LWT - Food Science and Technology (2017), doi: 10.1016/
j.lwt.2017.05.002.

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 ACCEPTED MANUSCRIPT
1 Agglomeration during spray drying: physical and rehydration properties of whole milk/sugar mixture

2 powders

3 S. Chevera, S. Méjeana,b, A. Doliveta, F. Meic, C.M. Den Boerd, G. Le Barzicd, R. Jeanteta and P.

4 Schucka,*

a
5 STLO, UMR1253, INRA, Agrocampus Ouest, 35000 Rennes, France

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b
6 BIONOV, 85 rue de Saint Brieuc, 35042 Rennes, France

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c
7 Mondelez International, 200 Deforest Avenue, East Hanover, New Jersey 07936, United States of

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8 America

d
9 Mondelez UK R&D Ltd, Banbury, Oxon, OX16 2QU, United Kingdom

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*Corresponding author. Address: INRA UMR 1253, 35000 Rennes, France. Fax: +33 (0)2 23 48 53
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11 50.
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12 E-mail address: pierre.schuck@inra.fr

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Abstract
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14

15 In general, milk powders are submitted to agglomeration in order to enhance their rehydration
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16 properties. This study evaluated the impact of six different methods of agglomeration of the same

17 sweet whole milk powder on the physical and rehydration properties of the final product: non-
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18 agglomerated powder (control); agglomerated powder with fines returned to the top of the dryer,
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19 above the internal fluid bed (IFB) or above the cone; and agglomerated powder with fines returned

20 above the IFB with a nozzle that injects steam or sprays water in the middle of the IFB, respectively.

21 As expected, the biochemistry results showed no difference since the same concentrate was used in the

22 whole set of experiments. The physical properties led to higher bulk densities, tapped densities and

23 interstitial air for the control, and higher occluded air and particle size for agglomerated powders,

24 regardless of the agglomeration process. All of these physical properties influenced the

25 rehydratability. In fact, the wetting time and the dispersibility of sweet whole milk powder were
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26 significantly improved by the agglomeration method, with the return of fines and steam injection in

27 the IFB. An experimental design of the agglomeration process was devised for this agglomeration

28 approach.

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30 Keywords: Rehydratability, Dairy powder, Granulation, Fine recirculation

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31

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32 1. Introduction

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33 The rehydratability of a powder in water is an essential property of food powders for the consumer

34 (King, 1966). Three main stages are usually distinguished in the rehydration process: wetting,

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35 dispersion and solubilization (Freudig, Hogekamp, & Schubert, 1999; Písecký, 1997). These stages are
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36 characterized by three indices: the wettability index (WI), the dispersibility index (DI) and the

37 solubility index (SI), respectively. The WI measures the ability of the powder to adsorb water on its
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38 surface, to be wetted, and to penetrate the free surface of still water (Sharma, Jana, & Chavan, 2012).

39 The DI represents the ability of a powder to separate into individual particles when dispersed in water
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40 with gentle mixing (Sharma, Jana, & Chavan, 2012), and the SI provides an overall measurement of
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41 the ability of a powder to dissolve in water (Schuck et al., 2012). In order to realistically consider the

42 rehydratability of a powder, Schuck, Dolivet, & Jeantet (2012) proposed considering the ‘instant’
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43 criterion (IC), which applies to powders that are wettable (WI < 20 s), dispersible (DI > 95%) and

44 soluble (SI > 99%) at the same time.

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45 Rehydratability depends on the composition and structure of a powder, especially the affinity

46 between its components and water (Dupas-Langlet, Benali, Pezron, Saleh, & Metlas-Komunjer, 2012;

47 Crowley, Kelly, Schuck, Jeantet, & O’Mahony, 2016) and the accessibility of the water to its

48 components, and on the rehydration conditions (Jeantet, Schuck, Six, Andre, & Delaplace, 2010).

49 Whole milk powder cannot be wetted within a reasonable time (Kim, Chen, & Pearce, 2002) and the

50 dispersibility is not satisfactory compared to skim milk powder (Vignolles et al., 2009; Tamime, 2009)

51 due to the hydrophobic nature of the surface of the particle incorporating free fat (Petit et al., 2017).

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52 To improve these rehydration properties, manufacturers are required to add natural surfactants such as

53 oil lecithin or a hygroscopic ingredient such as an amorphous carbohydrate.

54 Apart from this approach based on modifying the composition, powder agglomeration is

55 recognized to be one way to control and improve certain properties of a disperse system, especially

56 with regard to rehydratability (Buffo, Probst, Zehentbauer, Luo, & Reineccius, 2002; Gaiani, Banon,

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57 Scher, Schuck, & Hardy, 2005). Indeed, agglomeration is known to have an impact on certain physical

58 properties of powders such as density, granulometry, stickiness and cakiness, as well as on instant

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59 properties. The latter are mainly determined by the agglomeration process and then by the

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60 time/temperature to which the product is subjected in the system, including the processing steps prior

61 to spray drying. The agglomeration mechanism consists of joining fines or small primary particles in

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62 order to form larger particles. Different agglomeration techniques, either in the dry or the wet state, are
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63 currently proposed, but the wet granulation process in a fluid bed is by far the most commonly used in

64 the food industry (Gaiani, Schuck, Scher, Hardy, Desobry, & Banon, 2007; Turchiuli, Barkouti,
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65 Dumoulin, & Carcel, 2011; Turchiuli, Smail, & Dumoulin, 2012; Cuq, Mandato, Jeantet, Saleh, &

66 Ruiz, 2013).
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67 The aim of this study was to determine the impact of six configurations of a semi-industrial drying
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68 pilot on the physical and rehydration properties of a given dairy formulation consisting of a sweet

69 whole milk powder whose biochemical composition was kept constant. The efficacy of five different
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70 agglomeration processes was compared to a control non-agglomeration process.

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71
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72 2. Material and methods

73 2.1. Preparation of the concentrate

74 Concentrates with 40 g.100 g-1 total solids (TS) were recombined at Bionov (Rennes, France) from

75 a non-agglomerated medium-heat Whole Milk Powder (WMP, Lactalis Ingredients, Bourgbarré,

76 France) and a mix of carbohydrates composed of sucrose (Begin-say, Tereos, Lille, France) and

77 lactose (Lactalis Ingredients, Bourgbarré, France) at a 40/60 g/g sucrose/lactose ratio. The final target

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78 of the carbohydrate content was 55 g/100 g TS. The carbohydrate solution was dissolved at 70 °C to

79 obtain a carbohydrate in amorphous form, and the temperature was then decreased to 51 °C before

80 incorporation in the whole milk solution. The temperature of the final concentrate before drying was

81 maintained at 51 ± 2 °C.

82 The TS in the concentrates were checked by calculation of the weight loss after drying 5 g of the

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83 concentrate mixed with sand in an oven at 105 °C for 7 h.

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84 The fat globule size distribution was measured in the concentrate by Static Laser Light Scattering

85 (SLS) using the Mastersizer 2000 device (Malvern Instruments, Orsay, France) with 1 mL of

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86 ethylenediaminetetraacetic acid (EDTA, 35 mM, pH 7.0), which is a chelating agent of calcium ions

87 used to dissociate casein micelles. Measurements were performed in duplicate at room temperature to

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88 reach obscuration of between 4 and 12% with the water circulating in the sampling unit at a stirring
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89 speed of 1500 rpm, using refractive indices of water and milk fat of 1.33 and 1.458, respectively. The

90 results (fat globule size distribution) were based on volume and expressed as sphere-equivalent
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91 diameters. The diameter D[4.3], i.e., the mean volume diameter, was calculated.
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92
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93 2.2. Spray drying

94 Spray drying of the concentrates were performed at Bionov in a 3-stage pilot plant spray dryer
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95 (GEA, Niro Atomizer, Saint Quentin en Yvelines, France) (Fig. 1). Six trials were performed,

96 corresponding to six different spray-drying configurations (Fig. 2): (i) non-agglomerated powder (NA
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97 - control); (ii) agglomerated powder with fines returned to the top of the dryer (AT) (Fig. 3); (iii)
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98 agglomerated powder with fines returned above the internal fluid bed (IFB) (AIFB); (iv) agglomerated

99 powder with fines returned above the cone, without IFB (AC); (v) agglomerated powder with returned

100 fines and steam injection in the middle of the IFB at 8 kg/h maximum as the fluidized powder layer

101 rose in order to boost agglomeration (outlet steam temperature = 99 °C) (AS); and (vi) agglomerated

102 powder with returned fines and spraying of water (water temperature: 20 °C) in the middle of the IFB

103 at 6 kg/h as the fluidized powder layer rose in order to boost agglomeration (AW). All agglomerated

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104 powders were obtained by reintroduction of the fine particles from the cyclones. A 2-mm diameter

105 sieve was previously installed to collect powders.

106 Each spray-drying parameter for each trial was maintained at the same confidence interval, i.e., as

107 close as possible to a mean constant value, regardless of the spray-drying configuration being tested.

108 The atomizer was equipped with a 72/21 pressure nozzle throughout the trial (Spraying System Emani,

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109 Nantes, France). The flow rate of the concentrate was 101 ± 2 L/h, the inlet air temperature was set at

110 208 ± 7 °C, and the outlet air temperature at 90 ± 2 °C (Table 1). The air temperature of the first and

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111 second section of the external fluid bed was at 50 ± 2 °C and 22 ± 2 °C, respectively. All inlet airs

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112 were monitored and adjusted by a dehumidifier (Munters, Sollentuna, Sweden) to obtain an absolute

113 humidity close to 1 g water per kg of dry air. The duration of each trial was at least 1 h to obtain stable

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114 spray-drying parameters. The air velocity in Table 1 was measured before the heat exchanger on a
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115 straight pipe by using a pitot tube (Kimo, Rennes, France).

116
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117 2.3. Biochemical analysis

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118 A range of biochemical analyses was performed on the resulting powders, including protein,
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119 carbohydrate, ash and total fat content, to validate the identical biochemistry of the powders and

120 moisture and free fat content, which can have an impact on the rehydration properties. All these
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121 analyses were performed according to the protocols described in Schuck, Dolivet, & Jeantet (2012).

122 Each powder was analyzed in duplicate.

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123
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124 2.3.1. Protein content

125 The nitrogen content (TN) and non-protein nitrogen (NPN) of the powders were determined

126 by the Kjeldahl method according to the IDF Standards (2001a,b), respectively. The protein content

127 was calculated according to TN-NPN.

128

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129 2.3.2. Ash content

130 Ash content was measured after incineration at 550 °C for 5 h. Each powder was analyzed

131 twice, according to the protocols described in Schuck, Dolivet, & Jeantet (2012)

132

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133 2.3.3. Total fat content

134 The total fat was measured by Gerber’s acid-butyrometric method after dissolution of proteins

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135 by the addition of sulfuric acid and of amyl alcohol to facilitate the separation of milk fat by

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136 centrifugation. Each powder was analyzed twice.

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138 2.3.4. Sugar content

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139 The carbohydrate content was calculated according to the following formula:
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140 Carbohydrate content = 100 - (humidity + protein content + ash content + total fat content) (1)

141
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142 2.3.5. Free fat content

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143 The amount of free fat was evaluated by solvent extraction. Two extractions were performed
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144 by stirring a mixture of 10 ± 0.05 g powder with 50 mL petroleum ether and filtration on a 110-mm

145 diameter filter paper (Whatman paper, n° 40, Cat n°1440 125, Whatman International Ltd Maidstone,
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146 England). The solvent was evaporated at 55 °C under vacuum with a rotary evaporator (Heidolph,
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147 Serlabo Technologies, Entraigues sur la Sorgue, France) and then kept in an oven at 105 °C overnight.

148 The free fat content was determined by weight after evaporation of the solvent. Each powder was

149 analyzed twice.

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151 2.4. Physical analysis

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152 Various physical analyses were performed on the resulting powders: water activity (aw),

153 density, particle size and friability. These physical properties can differ according to the agglomeration

154 method implemented and can have an impact on the rehydration properties. All these determinations

155 were performed according to the protocols described in Schuck, Dolivet, & Jeantet (2012). Each

156 powder was analyzed in duplicate.

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157

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158 2.4.1. Humidity or moisture content

159 The moisture content of the powder was calculated by weight loss after drying 2 g of the

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160 powder mixed with sand in an oven at 105 °C for 7 h. Each powder was analyzed twice.

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161
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162 2.4.2. Water activity (aw)

163 The aw was measured in a water activity meter (aw-meter; Novasina RTD 200/0 and RTD 33,
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164 Lachen, Switzerland). Each powder was analyzed three times.

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165
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166 2.4.3. Bulk and tapped density and air content

Bulk density (ρB) (kg m-3) was obtained by weighing a cylinder, and tapped density (ρT) (kg.m-
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167
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168 ) by tapping the cylinder used for measuring bulk density 180 times. The difference between bulk and
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169 tapped density provides the interstitial air (IA) according to the following equation:
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170 = − × 100000 (2)

171 where ρT is the tapped density (kg m-3) and ρB the bulk density (kg m-3).

172 Occluded air (OA) (cm3.100 g-1) is the difference between the tapped density (ρT) and the true

173 density measured using a gas pycnometer with both helium and nitrogen on an ATC pycnometer

174 (Thermo Fisher Scientific, Courtaboeuf, France). It takes account of the air included in the powder

175 particle. OA was calculated as follows:

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176 = − × 100000 (3)

177 where ρT is the tapped density (kg m-3) and ρTR the true density (kg.m-3). The total air content (kg.m-3)

178 is the sum of IA and OA.

179

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180 2.4.4. Particle size and friability

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181 Particle size distributions and friability were measured by SLS using a Malvern Mastersizer

182 2000 device. The powder was placed on the optical bench and illuminated by laser light. The

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183 compressed air pressure was fixed at 50 kPa or 400 kPa for friability for particle size analysis and the

184 vibration at 30%. Each powder was analyzed twice. The results (particle size distribution) are based on

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185 volume and expressed as sphere-equivalent diameters. The diameter D[4.3], i.e., the mean volume
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186 diameter, was calculated. Different diameters were also calculated: i.e., D[0.1], D[0.5] and D[0.9],

187 which means that 10, 50 and 90% of the sample were below this diameter, respectively. Using these
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188 diameters, the dispersion of the sample or the span (s) can be determined as follows:
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[ [ . [ .
189 = × 100 (4)
[ .
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190 The compressed air pressure was fixed at 4 bars for the friability analysis and the vibration at

191 30%. The friability (F) can be deduced from the result obtained by laser particle size analysis. F (%) is
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192 equal to:

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[ . [ . !
193 = × 100 (5)
[ .
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194

195 2.5. Rehydration analysis

196 Each powder was analyzed in quadruplicate.

197 The wettability index (WI) was determined by adding 13 g of powder to 100 g of water at 40 °C

198 without stirring. The wettability index is the time (s) required for a powder to become completely wet.

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199 For wettability > 120 s, the results should be considered as purely informative (Schuck, Dolivet, &

200 Jeantet, 2012).

201 The dispersibility index (DI) was determined by adding 13 g of powder to 100 g of water at 40

202 °C with stirring with a spatula for 15 s. The dispersibility index is the amount of dry matter dispersed

203 in water, expressed as a percentage (w/w), which can pass through a 200-µm sieve.

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204 Solubility (SI) was determined by adding 13 g of powder to 100 g of water at 40 °C and

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205 mixing in a blender for 90 s after adding two droplets of defoaming agent (octan-1-ol). SI is the

206 percentage (v/v) of soluble particles (or supernatant).

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207 In order to consider the rehydratability of the powder at an overall level, the ‘instant’ criterion

208 (IC), which applies to powders that are wettable (WI < 20 s), dispersible (DI > 95%) and soluble (SI >

209
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99%) at the same time was considered for each powder produced, as proposed by Schuck, Dolivet, &
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210 Jeantet (2012).
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211

212 2.6. Statistical analysis

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213 Principal Component Analysis (PCA) was carried out with R software (R Development Core

214 Team) to summarize the main information from the collected data. The first two principal components
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215 (PC) were used to show the correlations between variables and the main differences between products.

216 The experimental set was projected onto the map determined by PC1 and PC2 with samples. A map
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217 was also defined by the first and the third principal component of the PCA . One-way analysis of
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218 variance, followed by Tukey’s HSD test, were used on each variable to determine whether there were

219 any statistical differences between any pairs of products at a 95% confidence level (test conducted

220 with JMP software).

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222 3. Results and Discussion

223 3.1. Concentrate

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224 As explained above, the dry matter of the concentrate was good at 40.00 ± 0.01 g/100 g . The

225 D[4.3] of the fat droplet size in the presence of EDTA was 0.76 ± 0.01 µm. The correlation between

226 the free fat content and greater fat droplet diameters has already been established: to achieve low free

227 fat content in powders, the fat droplet size in the concentrate has to be less than 1 µm before spray

228 drying (Vignolles et al., 2009).

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229

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230 3.2. Biochemical composition of powders

231 The average biochemical composition of all the powders was 17.5 ± 3.0 g/100 g DM, 56.5 ± 0.5

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232 g/100 g DM, 4.6 ± 0.1 g/100 g DM and 18.6 ± 0.1 g/100 g DM for protein content, carbohydrate

233 content, ash content and total fat content, respectively. The results show that the biochemical

234
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composition (protein, ash, fat and carbohydrate content) was the same for all powders. Since each of
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235 the powders showed the predictable composition, it confirmed that the dilution and recombining step

236 had been correctly validated. Moreover, the differences in powder properties were assumed to
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237 originate from the process and, in particular, from the agglomeration method implemented.
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238 The free fat, hydrophobic component present at the surface of the powder particles can have a
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239 negative impact on rehydration properties, on flowability and on oxidation during storage. Statistical

240 analysis showed significant differences between the free fat content of powders, with a lower free fat
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241 content for AT (Table 2). However, free fat content varied only from 1.5 ± 0.0 to 3.3 ± 0.2 g/100 g fat

242 . These values were low considering that the free fat content of standard spray-dried whole milk
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243 powders is around 2 g/100 g fat (Písecký, 1990). It can thus be concluded that these differences in free
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244 fat content were not great enough to affect rehydration properties.

245

246 3.3. Physical properties of powders

247 The humidity (Table 3) was in the range of 1.3 to 2.9 g/100 g, which is common for milk

248 powders (Schuck, Dolivet, & Jeantet, 2012). Powder humidity may be affected by the biochemical

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249 composition, the outlet temperature and the drying time. Písecký (1997) showed that the moisture

250 content decreased when the outlet air temperature increased, and even a small variation in the outlet

251 temperature (e.g., a 1 °C increase) can have substantial consequences on the humidity of the powder (a

252 0.2 g/100 g decrease) (Písecký, 1997; Schuck, Dolivet, & Jeantet, 2012). In this study, the outlet

253 temperature (Table 1) and biochemical composition (Table 2) were the same, and it could be

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254 considered that differences in humidity were the consequences of residence time in the dryer. In fact,

255 the longer the powder residence time is, the lower the humidity will be (Das & Langrish, 2012). The

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256 residence time of the product was affected by the dryer configuration, with a shorter residence time

257 when fines were returned to the top of the dryer because of better agglomeration (Jeantet, Ducept,

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258 Dolivet, Méjean, & Schuck, 2008).

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259 aw is one of the most important factors that significantly influence the shelf-life of milk
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260 powder (Roos, 2002). Efstathiou, Feuardent, Méjean, & Schuck (2002) showed that, in general,

261 product preservation is optimal when aw is 0.2 at 25 °C. The aw of powders is correlated with moisture
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262 content: the higher the humidity value is, the higher the aw value will be (Schuck, Dolivet, Méjean, &

263 Jeantet, 2008). aw in this study ranged from 0.103 to 0.173, i.e., ≤ 0.2. This aw range corresponds to a
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264 strongly bound monolayer of water, which is fairly difficult to eliminate (Brunauer, Emmett, & Teller,
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265 1938).

266 Particle size is an important physical property of powder, which can be linked to its
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267 appearance, reconstitution and flow characteristics. Significant differences (P ≤ 0.1) were obtained for

268 D[4.3] diameter with the different configurations (Table 3). D[4.3] values were the highest with
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269 agglomeration by a nozzle in the IFB, which spayed steam (AS: D[4.3] = 308 ± 1 µm), and the lowest
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270 without agglomeration (NA: D[4.3] = 54 ± 0 µm). Between these extreme values, powders were

271 ranked by descending order, i.e., AW, AT, AIFB and AC (D[4.3] = 287 ± 1, 255 ± 9, 140 ± 10 and

272 133 ± 2 µm, respectively). All agglomerated powders presented higher mean particle sizes compared

273 to the non-agglomerated control powder. Indeed, the aim of powder agglomeration is to join fine

274 particles to make larger particles. The largest particle size was obtained with agglomeration in the IFB

275 with the injection of steam or water spraying. Agglomeration was favored in this case, as in the wet

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276 granulation process (Banjac., Stamenić, Lečić, & Stakić, 2009). Compared with the approaches that

277 return the fines above the IFB, recirculation of fines to the top of the dryer increased agglomeration

278 efficacy: a cloud of fine particles clustered around the nozzle and stuck together with sprayed droplets

279 of the concentrate before final drying (Jeantet, Ducept, Dolivet, Méjean, & Schuck, 2008).

280 Agglomeration above the IFB provided smaller particle size since agglomeration was even more

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281 limited with IFB recirculation, in which case the fine particles were mixed with almost dried particles

282 (Jeantet, Ducept, Dolivet, Méjean, & Schuck, 2008).

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283 Principal component analysis (PCA) was carried out to obtain an overall representation of the

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284 experimental dataset (Fig. 4a). The results are represented by a map defined by the first and the second

285 principal components (PC1 and PC2) of the PCA, which explained 81% of the overall inertia of the

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286 data, and the projection of the individual sets on this map. The biochemistry results are not represented
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287 on this map because of the lack of difference between powders. aw and powder humidity are not

288 included since they depend on the outlet temperature rather than on the agglomeration approach.
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289 Particle size, i.e., D[4,3], was better represented on the PC1 and PC3 maps (Fig. 4a, not shown), and

290 was highly correlated with wettability and dispersibility. This confirms that rehydration properties are
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291 improved with higher D[4.3]. Very dispersible powders were agglomerated and DI increased with
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292 particle size to an optimum of approximately 150 to 200 µm (Schuchmann, Hogekamp, & Schubert,

293 1993; Sharma, Jana, & Chavan, 2012), whereas the D[4,3] value of NA was 54.4 ± 0.0 µm and the
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294 D[4,3] for agglomerated powders ranged from 133 ± 2 to 308 ± 0 µm, closer to this optimum range.

295
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296 The span (uniformity index) also showed differences between configurations (Table 3). The

297 agglomeration of powders at the top of the dryer or above the IFB (without a nozzle) resulted in

298 powders with spans of 1.3 and 1.4, respectively, corresponding to very uniform particle size. One aim

299 of agglomeration is in fact to achieve uniform particle size (Greensmith, 1998). Without

300 agglomeration, particle size was not as uniform. For agglomeration above the IFB with injection of

301 steam or water spraying, it was very difficult to control the particle size, and a class of particles as

302 large as 1000 µm was observed for powders AS and AW (Fig. 5). Lastly, all the powders could be

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303 considered to be friable according to their friability values, ranging from 30 to 41.2% (Table 3)

304 (Schuck, Dolivet, & Jeantet, 2012).

305 Tapped densities and, to a lesser extent, bulk densities were higher for NA than for

306 agglomerated powders, in agreement with the literature (Banjac., Stamenić, Lečić, & Stakić, 2009;

307 Sharma, Jana, & Chavan, 2012).The density of a non-agglomerated powder is generally higher than

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308 that of the corresponding agglomerated powder because of the formation of a porous structure during

309 the agglomeration process, which involves occluded air or a vacuole (Barkouti, Turchiuli, Carcel, &

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310 Dumoulin, 2013). The OA for agglomerated powders was at least twice that of NA (from 123 to 135

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311 cm3/100 g of powder compared to 61 cm3/100 g of powder) (Table 3). The IA was greater for the non-

312 agglomerated powder NA. IA content decreased due to agglomeration, whereas OA content increased,

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313 resulting in a higher total air content in all of the agglomerated powders (AT to AW, between 186 to
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314 228 cm3/100 g) compared to the non-agglomerated powder NA (168 cm3/100 g). This can be

315 explained by the part of the IA that would be trapped by the particle during agglomeration, thus
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316 leading to an increase in the OA content and the total air content.

317
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318 3.4. Rehydration properties

319 Dispersibility and wettability were well represented on the PC1 (Fig. 4a). Solubility was not
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320 included in the PCA because of the lack of variation between the powders. Greater dispersibility

321 corresponded to positive scores on the PC1, in contrast to better wettability, diametrically represented
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322 by negative scores. Wettability and dispersibility appeared to be negatively correlated. On the other
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323 hand, dispersibility was significantly positively correlated with partial or total occluded air (p = 0.023)

324 and negatively correlated with tapped density (p = 0.017). Indeed, dispersible powders are obtained by

325 production of agglomerated powders that contain a large quantity of occluded air and that can rapidly

326 fill with water on contact (Písecký, 1997). Moreover, bulk and tapped density are also influenced by

327 agglomeration: in general, the larger the particle size is, the lower the density will be (Börjesson,

328 Innings, Trägårdh, Bergenståhl, & Paulsson, 2014). Tapped density and occluded air were also

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329 significantly correlated (p = 0.002). Occluded air is in fact a key factor for density control: as occluded

330 air increases, particle volume increases and, thus, particle density decreases.

331 All the agglomerated powders produced in this study were considered to be wettable since

332 their WI was lower than 120 s (Haugaard Sorensen, Ktag, Pisecky, & Westergaard, 1978). In contrast,

333 the non-agglomerated NA powder was not wettable (Table 4). The presence of large agglomerated

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334 particles (Table 3 and Fig. 4) promoted wetting. In fact, the larger the diameter is, the lower the

335 particle surface-to-volume ratio is and the easier the wetting step will be. Several authors have

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336 reported that particle sizes greater than 200 µm provided better wettability (Szulc and Lenart, 2012;

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337 Písecký, 1997). In agreement with this, the best wettability was obtained for AS and AW, the powders

338 with the largest particles, and the worst wettability for ACNA powder with the smallest particles.

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339 These results are confirmed by negative correlation between particle size distribution and wettability
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340 time with an R2 close to 0.85. The agglomeration approach that returns the fines to the top of the

341 drying chamber seemed to enhance wettability more effectively than the agglomeration approach
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342 above the IFB.

343 Similarly, since their DI was over 95%, all agglomerated powders were dispersible (Haugaard
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344 Sorensen, Ktag, Pisecky, & Westergaard, 1978), regardless of the technological approach, whereas the
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345 non-agglomerated NA powders were not dispersible. However, and using this index, AW did not show

346 the best behavior. Rapid dispersion required particle sizes in the range of 150 to 200 µm, but
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347 dispersibility was probably increased even more because a hygroscopic agent (carbohydrates) had

348 been added.

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349 Milk powders are considered soluble if the SI is more than 99% (Haugaard Sorensen, Ktag,

350 Pisecky, & Westergaard, 1978). Thus, all powders considered in this study were soluble. Their

351 insoluble particles probably originated from the raw WMP material used, which presented an initial

352 0.4% content of insoluble particles. It can thus be concluded that there was no effect of the

353 agglomeration approach on the solubility of these powders.

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354 In view of the simultaneous WI of less than 20 s, a DI of more than 99% and an SI of more

355 than 99%, our results showed overall that AS was an instant powder (Schuck, Dolivet, & Jeantet,

356 2012). In general, this study emphasized the fact that agglomeration enhanced rehydration properties,

357 in agreement with previous results (Buffo, Probst, Zehentbauer, Luo, & Reineccius, 2012).

358

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359 Regarding the influence of agglomeration methods on rehydration properties, the experimental

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360 set of individual powders was projected onto the map determined by PC1 and PC2 (Fig. 4b). This map

361 made it possible to define just three groups: non-agglomerated powder (NA), powders agglomerated at

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362 the top of the dryer and above the IFB (ATAT, AIFB and AC), and agglomerated powders above the

363 IFB with steam injection or water spraying in the IFB (AS and AW). Better wettability and

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364 dispersibility were found for samples on the right of this map, i.e., AS and AW. In contrast, NA, i.e.,
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365 the non-agglomerated powder, had the poorest rehydration properties. The rehydration behaviors of

366 ATAT, AIFB and AC were intermediate, with medium DI and low WI.
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367 Since AS had the best rehydration properties among the different powders considered in this
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368 study, it was concluded that the best agglomeration approach to enhance rehydration properties was
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369 the one with fine recirculation and steam injection. In this configuration, droplets were formed by

370 steam condensation in the IFB on the cold particle surface of primary or agglomerated particles. Steam
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371 injection thus increased both the water content and the temperature T of the powder. Since increasing

372 the water content leads to a decrease in the glass transition temperature Tg of the powder, the injection
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373 of steam in the IFB resulted in an increase in the (T-Tg) difference, which is suitable for the
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374 agglomeration process (Roos, 1997). The resulting liquid layer on the surface of the particles may

375 dissolve the hydrophilic substances in the particle core to constitute a sticky surface (Roos, 1997).

376 Agglomerates were formed by collision of sticky particles joined by viscous liquid bridges, which

377 were further solidified by the drying process (Schuchmann, Hogekamp, & Schubert, 1993).

378

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379 Thus, wet agglomeration seems to be a better approach to obtaining instant powders than dry

380 agglomeration, in agreement with previous studies (Barkouti, Turchiuli, Carcel, & Dumoulin, 2013;

381 Schuchmann, Hogekamp, & Schubert, 1993; Turchiuli, Barkouti, Dumoulin, & Carcel, 2011).

382 However, in contrast to the latter, wet agglomeration was directly conducted in our study in the drying

383 chamber, and not post-drying using other granulation equipment.

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384

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385 5. Conclusion

386 This study showed that different dryer configurations may have an impact on the physical

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387 properties of powders, influencing rehydration properties. In general, powder agglomeration enhanced

388 rehydration properties. For instance, the best technological approach from a rehydratability point of

389
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view appeared to be a combination of the reintroduction of fine particles with simultaneous steam
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390 injection in the internal fluid bed, but this approach is highly dependent on the specific drying tower

391 considered and the drying conditions applied in the tower. Further work on this new agglomeration
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392 configuration will focus on optimizing the steam or water flow rate in relation to the mass of powder
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393 being used in order to more effectively control particle size.

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394

395 References
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396 Banjac, M., Stamenić, M., Lečić, M., Stakić, M. (2009). Size distribution of agglomerates of milk
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397 powder in wet granulation process in a vibro-fluidized bed. Brazillian Journal of Chemical
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398 Engineering, 26, 515–525.

399 Barkouti, A., Turchiuli, C., Carcel, J.A., Dumoulin, E. (2013). Milk powder agglomerate growth and

400 properties in fluidized bed agglomeration. Dairy Sciences and Technology, 93, 523–535.

401 Börjesson, E., Innings, F., Trägårdh, C., Bergenståhl, B., Paulsson, M., 2014. Evaluation of particle

402 measures relevant for powder bed porosity - A study of spray dried dairy powders. Powder

403 Technology, 253, 453–463.

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404 Brunauer, S., Emmett, P.H., Teller, E. (1938). Adsorption of Gases in Multimolecular Layers. Journal

405 of the American Chemical Society, 60, 309–319.

406 Buffo, R.A., Probst, K., Zehentbauer, G., Luo, Z., Reineccius, G.A. (2002). Effects of agglomeration

407 on the properties of spray-dried encapsulated flavours. Flavour and Fragrance Journal, 17, 292–

408 299.

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409 Crowley S.V., Kelly A.L., Schuck P., Jeantet R. & O’Mahony J.A. (2016). Rehydration and solubility

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410 characteristics of high-protein dairy powders. In P.L.H. McSweeney & J.A. O’Mahony (Eds.),

411 Advanced Dairy Chemistry-1B Proteins: Applied Aspects, (pp.99-131). Springer Publishers, New

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412 York.

413 Cuq, B., Mandato, S., Jeantet, R., Saleh, K., Ruiz, T. (2013). Food powder agglomeration. In:

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Bhandari, B., Bansal, N., Zhang, M., Schuck, P. (Eds.), Handbook of Food Powders (pp.200-
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415 229).Cambridge: Woodhead Publishing Series in Food Science, Technology and Nutrition.
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416 Das, D., Langrish, T.A.G. (2012). Combined Crystallization and Drying in a Pilot-Scale Spray Dryer.

417 Drying Technology, 30, 998-1007.

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418 Dupas-Langlet, M., Benali, M., Pezron, I., Saleh, K., Metlas-Komunjer L. (2012). Deliquescence
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419 lowering in mixtures of NaCl and sucrose powders elucidated by modeling the water activity of

420 corresponding solutions. Journal of Food Engineering, 115, 391-397.

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421 Efstathiou, T., Feuardent, C., Méjean, S., Schuck, P. (2002). The use of carbonyl analysis to follow the
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422 main reactions involved in the process of deterioration of deshydrated dairy products: predeiction
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423 of most favorable degree of dehydration. Le Lait 82, 423-439.

424 Freudig, B., Hogekamp, S., Schubert, H. (1999). Dispersion of powders in liquids in a stirred vessel.

425 Chemical Engineering Processing, 38,525-532.

426 Gaiani C., Banon S., Scher J., Schuck P. Hardy J. (2005). Use of a turbidity sensor to characterize

427 micellar casein powder rehydration: influence of some technological effects. Journal of Dairy

428 Science, 88, 2700-2706.

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429 Gaiani C., Schuck P., Scher J., Hardy J., Desobry S., Banon S. (2007). Dairy powder rehydration:

430 Influence of protein state, incorporation mode, and agglomeration. Journal of Dairy Science, 90,

431 570-581.Greensmith, M. (1998). Practical Dehydration. (2nd ed). Cambridge: Woodhead

432 Publishing, 274p.

433 Haugaard Sorensen, I., Ktag, J., Pisecky, J., Westergaard, V. (1978). Méthodes d’analyses des

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434 produits laitiers déshydratés. Niro Atomizer, Copenhague, Danemark.

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435 IDF, 2001a. International standard 20-1: Milk - Determination of nitrogen-content - Part1: Kjeldahl

436 method.

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437 IDF, 2001b. International standard 20-4: Milk - Determination of nitrogen-content - Part 4:

438 Determination of non-protein-nitrogen content.

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439 Jeantet, R., Ducept, F., Dolivet, A., Méjean, S., Schuck, P. (2008). Residence time distribution: a tool

440 to improve spray-drying control. Dairy Science and Technology, 88, 31-43.
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441 Jeantet, R., Schuck, P., Six, T., Andre, C., Delaplace, G. (2010). The influence of stirring speed,

442 temperature and solid concentration on the rehydration time of micellar casein powder. Dairy
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443 Science and Technology, 90, 225-236.

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444 Kim, E.H.-J., Chen, X.D., Pearce, D. (2002). Surface characterization of four industrial spray-dried
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445 dairy powders in relation to chemical composition, structure and wetting property. Colloids and

446 Surfaces B: Biointerfaces, 26, 197–212.

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447 King, N. (1966). Dispersibility and reconstitutability of dried milk. Dairy Science Abstracts, 28, 105–
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448 118.

449 Petit, J., Michaux, F., Jacquot, C., Chavez Montes, E., Dupas, J., Girard, V., Gianfrancesco, A., Scher,

450 J. & Gaiani, C. (2017). Storage-induced caking of cocoa powder. Journal of Food Engineering,

451 199, 42-53.

452 Písecký, J. (1990). 20 years of instant whole milk powder. Scandinavian Dairy Information. 2, 1–5.

453 Písecký, J. (1997). Handbook of Milk Powder Manufacture. Copenhagen: Niro A/S. ,.
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454 Roos, Y. H. (1997). Water in milk products. In P.F. Fox (Ed), Advanced dairy chemistry (pAIFB03-

455 346). London: Chapman et Hall

456 Roos, Y.H. (2002). Importance of glass transition and water activity to spray drying and stability of

457 dairy powders. Le Lait, 82, 475–484.

458 Schuchmann, H., Hogekamp, S., Schubert, H. (1993). Jet agglomeration processes for instant food.

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459 Food Science and Technology, 4, 179–183.

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460 Schuck, P., Dolivet, A., Jeantet, R. (2012). Analytical Methods for Food and Dairy Powders. (First ed)

461 Chichester:John Willey & Sons, Ltd, 228p.

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462 Schuck, P., Dolivet, A., Méjean, S., Jeantet, R. (2008). Relative humidity of outlet air: the key

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463 parameter to optimize moisture content and water activity of dairy powders. Dairy Science and
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464 Technology, 88, 45–52.

465 Sharma, A., Jana, A.H., Chavan, R.S. (2012). Functionality of Milk Powders and Milk-Based Powders
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466 for End Use Applications - A Review. Comprehensive Reviews in Food Science and Food Safety,

467 11, 518–528.

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468 Szulc, K., Lenart A. (2012). Water vapour adsorption properties of agglomerated baby food

469 powders. Journal of Food Engineering, 109, 135-141

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470 Tamime, A.Y. (2009). Dairy Powders and Concentrated Products. (First ed) Chichester:John Willey

471 & Sons, Ltd,.380p.

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472 Turchiuli, C., Barkouti, A., Dumoulin, E., Carcel, J.A. (2011). Skim milk agglomerates growth furing
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473 fluidized bed wet agglomeration and drying. Eur. Dry. Conf.

474 Turchiuli, C., Smail, R., Dumoulin, E. (2012). Fluidized bed agglomeration of skim milk powder:

475 analysis of sampling for the follow-up of agglomerate growth. Powder Technology, 238, 161–168.

476 Vignolles M.L., Lopez C., Madec M.N., Ehrhardt J.J., Méjean S., Schuck P, Jeantet R. (2009). Fat

477 properties during homogenization, spray-drying and storage affect the physical properties of dairy

478 powders. Journal of Dairy Science, 92, 58–70.

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479

480

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Table 1. Spray-drying parameters for the six powders.

Unit NA AT AIFB AC AS AW

Feed Flow rate L/h 100 102 101 104 100 100

Inlet air °C 206 206 197 208 215 215

IFB air °C 55 55 55 55 70 70
Temperature

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IFB plate °C 53 63 57 - 76 73

IFB powder °C 58 68 63 - 78 75

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Outlet air °C 93 89 88 92 89 90

IFB air m/s 11 10 11 12 12 15

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velocity
Air

Major air m/s 15 15 15 16 14 14

NB: “-“ is indicated when there is no value.

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Legend: IFB: Integrated Fluid Bed; NA = Non-Agglomerated powder; AT = Agglomerated powder at
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the Top of the dryer; AIFB = Agglomerated powder above the Internal Fluid Bed; AC =
Agglomerated powder above the Cone, without integrated fluid bed; AS = Agglomerated powder
above the integrated fluid bed with a nozzle in the middle of the integrated fluid bed that sprayed
Steam in the fluidized powder layer; AW = Agglomerated powder above the integrated fluid bed with
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a nozzle in the middle of the integrated fluid bed that sprayed Water in the fluidized powder layer.
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Table 2. Free fat content expressed per g for 100 g of fat. Samples with the same letter (a,b,c) in a

group of the same composition were not statistically different (P < 0.05) (n=2).

Sample Unit NA AT AIFB AC AS AW

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Total free
g/100 g fat 2.4 ± 0.5b 1.5 ± 0.0c 2.8 ± 0.1a,b 2.8 ± 0.0a,b 3.3 ± 0.2a 2.9 ± 0.1a,b
fat

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Legend : NA = Non-Agglomerated powder; AT = Agglomerated powder at the Top of the dryer;
AIFB = Agglomerated powder above the Internal Fluid Bed; AC = Agglomerated powder above the
Cone, without integrated fluid bed; AS = Agglomerated powder above the integrated fluid bed with a

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nozzle in the middle of the integrated fluid bed that sprayed Steam in the fluidized powder layer; AW
= Agglomerated powder above the integrated fluid bed with a nozzle in the middle of the integrated
fluid bed that sprayed Water in the fluidized powder layer.

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Table 3. Properties of powders: moisture content, water activity (aw), density and particle size. Samples with the same letter (a,b,c) in a group of the same

Sample Unit NA AT AIFB AC AS AW

Moisture % 2.5 ± 0.0 2.9 ± 0.0 1.5 ±0.0 1.5 ± 0.0 2.0 ± 0.1 1.3 ± 0.0

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aw - 0.14 ± 0.00 0.17 ± 0.01 0.11 ± 0.01 0.12 ± 0.00 0.11 ± 0.00 0.10 ± 0.02

kg/m3

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Bulk density 407 ± 4 370 ± 2 332 ± 3 330 ± 2 339 ± 3 373 ± 2

Tapped density kg/m3 720 ± 2 500 ± 4 495 ± 1 484 ± 3 454 ± 1 494 ± 2

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Partial true density kg/m3 1288 ± 2 1294 ± 1 1259 ± 3 1273 ± 2 1177 ± 5 1214 ± 3

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Total true density kg/m3 1309 ± 1 1319 ± 2 1291 ± 4 1302 ± 2 1244 ± 3 1269 ± 4

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Interstitial air cm3/100 g 107 ± 3 70 ± 1 99 ± 2 96 ± 1 75 ± 2 66 ± 1

cm3/100 g

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Occluded air 61 ± 1 123 ± 3 123 ± 0 128 ± 2 135 ± 0 120 ± 1

Total air cm3/100 g 168 ± 4 193 ± 4 222 ± 2 224 ± 3 210 ± 2 186 ± 2

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D [4,3] µm 54 ± 0a 255 ± 9b 133 ± 2c 140 ± 10c 308 ± 0d 287 ± 10e

Span - 2.0 ± 0.0b

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1.3 ± 0.0c 1.4 ± 0.0c 1.4 ± 0.0c 3.3 ± 0.1a 2.0 ± 0.0b
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Friability % 30 ± 0 30 ± 2 38 ± 1 41 ± 4 38 ± 2 35 ± 1

composition are not statistically different (P < 0.05) (n=2).

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Legend: NA = Non-Agglomerated powder; AT = Agglomerated powder at the Top of the dryer; AIFB = Agglomerated powder above the Internal Fluid Bed;
AC = Agglomerated powder above the Cone, without integrated fluid bed; AS = Agglomerated powder above the integrated fluid bed with a nozzle in the
middle of the integrated fluid bed that sprayed Steam in the fluidized powder layer; AW = Agglomerated powder above the integrated fluid bed with a nozzle
in the middle of the integrated fluid bed that sprayed Water in the fluidized powder layer.
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Table 4: Rehydration ability of powders: wettability, dispersibility and solubility. Samples with the

same letter (a,b,c) in a group of the analysis were not statistically different (P < 0.05) (n=4).

Sample Unit NA AT AIFB AC AS AW

Wettability

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s > 120 ± 1e 47 ± 2b 66 ± 2c 112 ± 1d 16 ± 1a 14 ± 1a
index
Dispersibility
% 62.0 ± 0.1a 99.7 ± 0.1c 97.8 ± 3.4b,c 94.9 ± 0.2b 99.7 ± 2.2c 97.5 ± 0.3b,c

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index
Solubility
% 99.6 ± 0.0a 99.6 ± 0.0 a 99.6 ± 0.0 a 99.6 ± 0.0 a 99.6 ± 0.0 a 99.6 ± 0.0 a

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index
Legend: NA = Non-Agglomerated powder; AT = Agglomerated powder at the Top of the dryer; AIFB
= Agglomerated powder above the Internal Fluid Bed; AC = Agglomerated powder above the Cone,

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without integrated fluid bed; AS = Agglomerated powder above the integrated fluid bed with a nozzle
in the middle of the integrated fluid bed that sprayed Steam in the fluidized powder layer; AW =
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Agglomerated powder above the integrated fluid bed with a nozzle in the middle of the integrated fluid
bed that sprayed Water in the fluidized powder layer.
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2.00 m
0.37 m

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0.25 m

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1.50 m Area of each section:

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: 3.18 m2
: 9.42 m2

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: 8.83 m2
: 0.52 m2
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Total area: 21.95 m2
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2.12 m
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0.33 m
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0.50 m
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Fig.1. Dimensions of the spray dryer (not to scale).

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Fig. 2. Simplified diagram explaining the different approaches to agglomeration (NA = Non-
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Agglomerated powder; AT = Agglomerated powder at the Top of the dryer; AIFB = Agglomerated

powder above the Internal Fluid Bed; AC = Agglomerated powder above the Cone, without integrated
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fluid bed; AS = Agglomerated powder above the integrated fluid bed with a nozzle in the middle of
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the integrated fluid bed that sprayed Steam in the fluidized powder layer; AW = Agglomerated

powder above the integrated fluid bed with a nozzle in the middle of the integrated fluid bed that

sprayed Water in the fluidized powder layer).

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Fig. 3. Diagram showing the recirculation of fine particles on the spray nozzle.

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1.0

Total true
density Partial true density Total air

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0.5
Wettability Partial occluded air Dispersibility

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Interstitial air
Total occluded air
Dim 2 (22.31%)

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0.0

d(4.3)

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Tapped
density Free fat
-0.5
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Bulk
density Span
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-1.0
D

-1.0 -0.5 0.0 0.5 1.0

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Dim 1 (59.06%)
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Fig. 4a. Map defined by the first two principal components of the principal component analysis

(PCA), which was carried out to obtain an overall representation of the experimental dataset.
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Legend: IFB: Integrated Fluid Bed; NA = Non-Agglomerated powder; AT = Agglomerated powder at

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the Top of the dryer; AIFB = Agglomerated powder above the Internal Fluid Bed; AC =
Agglomerated powder above the Cone, without integrated fluid bed; AS = Agglomerated powder
above the integrated fluid bed with a nozzle in the middle of the integrated fluid bed that sprayed
Steam in the fluidized powder layer; AW = Agglomerated powder above the integrated fluid bed with
a nozzle in the middle of the integrated fluid bed that sprayed Water in the fluidized powder layer.
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2
AIFB
AT
Dim 2 (22.31%)

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0

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-1

AW
-2 NA AS

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-6 -4 -2 0 2 4
Dim 1 (59.06%)

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Fig. 4b. Projection of the experimental set on the map defined by the first two principal components of
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the principal component analysis (PCA). Sample classification was obtained by hierarchical cluster

analysis
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Legend: IFB: Integrated Fluid Bed; NA = Non-Agglomerated powder; AT = Agglomerated powder at

the Top of the dryer; AIFB = Agglomerated powder above the Internal Fluid Bed; AC =
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Agglomerated powder above the Cone, without integrated fluid bed; AS = Agglomerated powder
above the integrated fluid bed with a nozzle in the middle of the integrated fluid bed that sprayed
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Steam in the fluidized powder layer; AW = Agglomerated powder above the integrated fluid bed with
a nozzle in the middle of the integrated fluid bed that sprayed Water in the fluidized powder layer.
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10

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Volume (%)

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4

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2

0
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1 10 Size (µm) 100 1000
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NA AT AIFB AC AS AW

Fig. 5. Particle size distribution of powders resulting from different agglomeration approaches.
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Legend : NA = Non-Agglomerated powder; AT = Agglomerated powder at the Top of the dryer;

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AIFB = Agglomerated powder above the Internal Fluid Bed; AC = Agglomerated powder above the
Cone, without integrated fluid bed; AS = Agglomerated powder above the integrated fluid bed with a
nozzle in the middle of the integrated fluid bed that sprayed Steam in the fluidized powder layer; AW
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= Agglomerated powder above the integrated fluid bed with a nozzle in the middle of the integrated
fluid bed that sprayed Water in the fluidized powder layer.
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1 Figure captions

3 Figure 1

4 Dimensions of the spray dryer (not to scale)

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5

6 Figure 2

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7 Simplified diagram explaining the different approaches to agglomeration (NA = Non-Agglomerated

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8 powder; AT = Agglomerated powder at the Top of the dryer; AIFB = Agglomerated powder above

9 the Internal Fluid Bed; AC = Agglomerated powder above the Cone, without integrated fluid bed; AS

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10 = Agglomerated powder above the integrated fluid bed with a nozzle in the middle of the integrated
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11 fluid bed that sprayed Steam in the fluidized powder layer; AW = Agglomerated powder above the

12 integrated fluid bed with a nozzle in the middle of the integrated fluid bed that sprayed Water in the
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13 fluidized powder layer).

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14
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15 Figure 3

16 Diagram showing the recirculation of fine particles on the spray nozzle.

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17
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18 Figure 4
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19 (a): Map defined by the first two principal components of the principal component analysis (PCA),

20 which was carried out to obtain an overall representation of the experimental dataset.

21 (b): Projection of the experimental set on the map defined by the first two principal components of

22 the principal component analysis (PCA). Sample classification was obtained by hierarchical

23 cluster analysis.

24

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25 Figure 5

26 Particle size distribution of powders resulting from different agglomeration approaches.

27

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Highlights

• Various agglomeration steps to rehydrate sweet milk powders were studied.

• The rehydration properties depended on the configuration of the dryer.

• The optimal scheme consisted of steam injection in the internal fluidized bed.

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Gail WAGMAN
French-English Translator and Interpreter
13 rue du Terrail
30610 SAUVE
France
Tel.: 04 66 77 55 00
Email: gail.wagman@wanadoo.fr

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CERTIFICATE OF PROOFREADING

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This is to certify that I, the undersigned, Gail WAGMAN, a native English speaker and
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professional translator and interpreter, have read and corrected the following paper,

“Agglomeration during spray drying: physical and rehydration properties of whole milk/sugar
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mixture powders”, written by S. Chever, S. Méjean, A. Dolivet, F. Mei, C.M. Den Boer, G. Le

Barzic, R. Jeantet and P. Schuck, and that it has met with my entire satisfaction.
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Gail Wagman
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Sauve, May 2, 2017

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