Christophe Bressot
email: christophe.bressot@ineris.fr

Neeraj Shandilya
email: neeraj.shandilya@utc.fr

Thangavelu Jayabalan
email: thangavelu.jayabalan@ineris.fr

Guillaume Fayet
email: guillaume.fayet@ineris.fr

Matthias Voetz
email: matthias.voetz@bayer.com

Laurent Meunier
email: laurent.meunier@ineris.fr

Olivier Le Bihan
email: olivier.le-bihan@ineris.fr

Olivier Aguerre-Chariol
email: olivier.aguerre-chariol@ineris.fr

Martin Morgeneyer
email: martin.morgeneyer@utc.fr

Authors Bressot

Thangavalu Jayabalan

Le Bihan

Laurent Laurent

Exposure assessment of Nanomaterials at production sites by a Short Time Sampling (STS) approach : Strategy and first results of measurement campaigns

Keywords: Nanoparticle, NOAA, Exposure, Measurement campaign, Short Time Sampling, Nanosafety, risk assessment and management

des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.

Introduction

The current work on assessing the hazards of engineered nanomaterials (ENMs) solely based on laboratory tests is time-consuming (Christophe Bressot, 2017;Shandilya et al., 2015), resource intensive (Bressot et al., 2016), and in the case of toxicological studies lengthy (Privalova et al., 2014) and constrained by ethical considerations (Chen et al., 2017). For this, various secondary studies are carried out, focusing on aspects such as cellular uptake of particles (Phuc and Taniguchi, 2017) or environmental release (Plazas-Tuttle et al., 2015;Salehi et al., 2017).

In the framework of industrial workplaces, the operations dealing with the processing of the nanomaterials, nanoparticles (NPs) or Nano Objects, Agglomerates and Aggregates (NOAA) can lead to potential exposures unless proper safety measures are taken (ISO, 2012;Pavlovska et al., 2016). Prior exposure studies have been performed in the real workplaces dealing with the production and handling of nanomaterials (Bello et al., 2008;Bello et al., 2009;Brouwer et al., 2009;Demou et al., 2008;Demou et al., 2009;Fujitani et al., 2008;Johnson et al., 2010;Kuhlbusch and Fissan, 2006;Lee et al., 2011;Pavlovska et al., 2016). These works have led to general recommendations for exposure measurement assessments (Consent Report, 2011;INERIS -CEA -INRS et al., 2012.;nanoGEM;Ramachandran et al., 2011). Moreover, recent reviews highlight the need for an extensive description of workplaces to facilitate the comprehension of the mechanisms involved in particle release (Ding et al., 2016), (Privalova et al., 2014). The practical consequences in an aerosol characterization have been the use Mixed Cellulose Ester (MCE) filter (Methner et al., 2010) and performing intensive campaign with SMPS or FMPS, respectively (Kaminski et al., 2015;Kuhlbusch et al., 2011).

In order to make these studies successful, whilst considering various background aerosols originating from the general work environment or the process itself, , the measurement campaigns are intensive and time consuming (Kuhlbusch et al., 2011). For such campaigns, the size and time-resolved instruments like APS, SMPS etc. are an obvious choice in which the aerosol particle detection Moreover various studies were had difficulties to distinguish process generated NPs or NOAA from ambient particles (Bekker et al., 2015;Brouwer et al., 2014b). In addition, many nanomaterial emissions occur for a very brief period (i.e. for a second or fraction of a second) and are observed as number concentration peaks (Pietroiusti and Magrini, 2014). In this case, the use of samplers, By the developed technique, 9 out of 37 of the studied steps By the developed technique, 9 out of 37 of the studied steps For nanosafety measures, For nanosafety measures, the the of the nanomaterials of the nanomaterials in ampaign, Short Time Sampling, ampaign, Short Time Sampling,

The current work on assessing the hazards of engineered nanomaterials (ENMs) solely based on The current work on assessing the hazards of engineered nanomaterials (ENMs) solely based on 2017; Shandilya et al., 2015 Shandilya et al., 2015 toxicological toxicological studies lengthy studies lengthy Chen et al., 2017Chen et al., 2017). For this, various secondary . For this, various secondary such as cellular uptake of such as cellular uptake of particles particles Tuttle et al., 2015;Salehi et al., 2017Salehi et al., 2017 In the framework of industrial workplaces, the In the framework of industrial workplaces, the operat operation ions de s de or Nano Objects, Agglomerates or Nano Objects, Agglomerates proper safety measures proper safety measures performed performed in the real workplaces dealing with the production and in the real workplaces dealing with the production and Bello Bello et al., 2008et al., 2008Fujitani et al., 2008Fujitani et al., 2008Pavlovska et al., 2016Pavlovska et al., 2016) ). Th . Th measurement assessment measurement assessments ( (Consent Report, 2011Consent Report, 2011Ramachandran et al., 2011Ramachandran et al., 2011) ). . Moreover Moreover places to facilitate the comprehension of to facilitate the comprehension of , ( (Privalova et al., 2014 Privalova et al., In order to make these studies successful, whilst c In order to make these studies successful, whilst c from the general work environment or the process itself, , the measurement campaigns from the general work environment or the process itself, , the measurement campaigns and and time consuming time consuming requiring long sampling durations, becomes obsolete. Considering these critical points while carrying out the measurement campaigns, the Short Time Sampling (STS) approach presented in the present article may lead to a global improvement in NP exposure assessment at workplaces. Alternative samplers have been previously used but required a long-term exposure (Hedmer et al., 2014;Methner et al., 2012) or sample preparations (Asbach et al., 2014;Gorner et al., 2010;Hedmer et al., 2014;Koponen et al., 2015;Methner et al., 2012). The Micro Inertial Impactor (MINI) is an interesting short-term sampler used at workplace exposure assessments but the D50 cut-off at 0.05 and 0.9 µm aerodynamic diameter prevents a comprehensive inhalable study (Kandler et al., 2011;Kling et al., 2016).

The STS approach is illustrated in Figure 1. The first step is basic information gathering about the process and materials which may come from different sources (literature, Material Safety data Sheet, companies, etc). Although the presented method does not directly involve toxicological considerations, the knowledg evaluation of the analytical detection limits and/or background noise level are appropriate for the substance under consideration. For this, any related available toxicological data is also documented in the proposed procedure and compared to these limits. In the case of unavailable data, detection limits are furthermore documented allowing for rapidly reevaluating the exposure levels once such toxicological data becomes available. This is then followed by a semi-quantitative exposure measurement campaign through visual observations, inventory of process and operations. If a step is potentially emissive, a sampling within or near the breathing zone of the worker is carried out systematically using Mini Particle Sampler, MPS (Bressot et al., 2015;R'mili et al., 2013). A short sampling duration is possible because of the high collection efficiency. The efficiency is minimum at 30 nm i.e. 15-18 % and maximum at 5 nm i.e. 70 % (R'mili et al., 2013).The subsequent offline microscopic characterization of the TEM grid can differentiate between the ambient particles and NP or NOAA. This methodology decision criterion is the key factor of the campaign strategy. The existing tiered approach requires a stable background counting for a threshold limit between emission and background counting. By contrast, the present approach only necessitates a simple comparison between the background and process generated NP which is done by an offline emission checking using MPS. If an average of one nanoparticle or NOAA is collected per TEM grid square (41µm x 41 µm) and the same holds true for a minimum of 10 squares on the grid, then we consider it in the present approach to be an effective exposure. That value approximately corresponds to a spherical nanoparticle concentration between 200 to 500 cm -3 for a 5 minute sampling duration.

A particle counter was also used in conjunction for a quantitative measurement. Considering the mobility and dominance of submicronic sized particle in the ambience of the workplaces, the exposure analysis was consequently performed using a Condensation Particle Counter (CPC 3007, TSI Inc.) which has a relevant accuracy in the frame of handheld CPC (Asbach et al., 2012).

basic information gathering about the basic information gathering about the Material Safety data Sheet Material Safety data Sheet, and/or background noise level are appropriate for the and/or background noise level are appropriate for the substance under consideration. For this, any related available toxicological data is substance under consideration. For this, any related available toxicological data is also also documented in documented in In the case of unavailable data, detection limits In the case of unavailable data, detection limits are furthermore documented allowing for rapidly reevaluating the exposure levels once such are furthermore documented allowing for rapidly reevaluating the exposure levels once such This is then followed by a semi This is then followed by a semi--quantitative exposure quantitative exposure visual observations, inventory of process and operations. If a visual observations, inventory of process and operations. If a or near the breathing zone or near the breathing zone of the worker is carried out of the worker is carried out Bressot et al., 2015Bressot et al., 2015;R'mili et al., 2013 sampling duration is possible because of the high collection efficiency. The efficiency is minimum at sampling duration is possible because of the high collection efficiency. The efficiency is minimum at (R'mili et al., 2013 R'mili et al., 2013 can differentiate between the ambient particles and differentiate between the ambient particles and This methodology decision criterion is the key factor of the c This methodology decision criterion is the key factor of the c a stable background counting a stable background counting By contrast, By contrast, t the present approach only necessitates he present approach only necessitates between the background and process generated between the background and process generated NP nano nanoparticle particle or NOAA is collected per TEM grid square (41µm x 41 µm) and the same holds true for a minimum of µm) and the same holds true for a minimum of to be an effective exposure. to be an effective exposure. nanoparticle concentration between nanoparticle concentration between A particle counter wa A particle counter was also used in conjunction for a quantitative measurement.

s also used in conjunction for a quantitative measurement. dominance of submicronic sized particle in t dominance of submicronic sized particle in t analysis was analysis was consequently performed consequently performed which has a relevant accuracy in the frame of handheld CPC which has a relevant accuracy in the frame of handheld CPC A systematic STS measurement campaign was carried out on six different process lines PL dealing with the production and manipulation of NMs to test the STS approach.

Materials and Methods

Instruments

A portable Condensation Particle Counter (CPC Model 3007; TSI Inc.) was used to carry out the measurement campaign. Its measurable particle size range is distributed from 10 nm to approximately 1 µm. A Mini Particle Sampler (MPS; Ecomesure Inc.) was used for the offline microscopic analysis of the sampled aerosol particles. It collects the particle on a porous copper mesh grid (Model S143-3; Quantifoil Micro Tools GmbH Germany) using a filtration technique. A Scanning Mobility Particle Yes sizer (SMPS Model 3936; including a CPC Model 3010; TSI Inc.) classifies the aerosol particles according to their electrical mobility diameter. The SMPS operates in the size range of 5 to 350 nm with a resolution of up to 64 channels per decade. With a sampling time or time resolution of 5 min 25 s, the air flow rate was kept at 0.3 l/min. A Fast Mobility Particle Sizer (FMPS Model 3091; TSI Inc.) measures aerosol particles in the size range of 6 to 523 nm with a resolution of 16 channels per decade. With a time resolution of 1 s, the FMPS is faster than SMPS. Both SMPS and FMPS were used to compare the observations obtained using CPC and MPS. The measurement ability of all these three instruments i.e. SMPS, FMPS and CPC are provided in the literature (Asbach et al., 2012;Kaminski et al., 2013). Due to a comparatively lower time resolution of FMPS, a discrepancy of size distribution between FMPS and SMPS is generally observed and is attributed to the manner of handling with particle size and morphology. The inaccuracy of the FMPS when measuring NOAA seems to be a known difficulty (Kaminski et al., 2013). To facilitate comparison, SMPS data are also favored in this paper.

Nanomaterials and their Process Lines

For this study, six pilot scale nanomaterial PLs concern the production and manipulation of seven nanomaterials: (a) ZrO2 NPs, (b) Polyamide nanofibers, (c) TiO2 nanofibers, (d) TiO2 & Ag nanosols and (e) MWCNT, were selected. Table 1 summarizes the overall data of the production lines dealing with the production, using nanomaterials and comparison between short time sampling and, on PL1, three tiered approaches.

Results

Process Line 1

The PL1 is devoted to ZrO2 NPs production from sol gel dispersion by drying in an oven. Before starting the PL1 operation, the ambient aerosol particles were examined to study the background noise (BG). Some particles were sampled at the fume hood containing the sol-gel reactor for their microscopic analysis.

The handling of the suspension involved steps 1 and 2 (see Table 1). The results obtained during these two steps are mentioned in the Table 1. The number concentration of the ambient aerosol particles during the step 1 did not seem to be significantly influenced by these steps. No ZrO2 particles, but soot, oil droplet and debris of building materials were detected.

The impact of opening the oven and transport (step 5) was studied. Both times a significant impact on the number concentration of the ambient aerosol particles was observed: a sudden increase to 200,000 cm -3 . It is important to note that the step 5 concerns only one product that has reached a solid state, but is not yet totally dry. The sampled particles with the size larger than 1 µm had two different compositions-metallic particles, and zirconium particles, constituting the majority (see Figure 3 a). Only one type of the particles dominated the size range of 0.1 to 1 µm-the ones that tended to degrade or "melt" under the microscope beam, and consisted of sodium, silicon and sulphur. Elements like calcium, carbon and silicon were present in the majority of the particles having size less than 100 nm. size size NOAA NOAA comparison, SMPS data comparison, SMPS data are are also also the production and manipulation of the production and manipulation of 2 nanofibers nanofibers, (d) TiO (d) TiO Table 1 summarizes the overall data of the production lines dealing Table 1 summarizes the overall data of the production lines dealing nanomaterials and comparison between short time sampling and, on PL1, nanomaterials and comparison between short time sampling and, on PL1, NPs production from sol gel dispersion by drying in NPs production from sol gel dispersion by drying in starting the PL1 operation, t starting the PL1 operation, the ambie he ambient aerosol particles w nt aerosol particles w . Some particles were sampled at the fume hood containing the sol . Some particles were sampled at the fume hood containing the sol microscopic analysis. microscopic analysis.

The handling of the suspension involved

The handling of the suspension involved two steps are mentioned in the two steps are mentioned in the during the step 1 did not seem to be during the step 1 did not seem to be soot, oil droplet and soot, oil droplet and The impact of opening the oven and transport ( The impact of opening the oven and transport ( the number concentration of the ambient aerosol particles the number concentration of the ambient aerosol particles cm cm --3 3 . . I

The opening of the oven and the transport of the product (step 5) clearly led to a very significant increase in the number concentration of the ambient aerosol particles, going beyond the limit of the CPC display (200,000 cm -3 ). This is a critical step clearly giving rise to the ZrO2 NPs exposure in the laboratory workplace.

Process Line 1: STS-three tiered approach comparison

In order to verify the applicability of the STS approach vis-à-vis the three-tiered approach, CPC and MPS sampling results were compared with an intensive campaign carried out using SMPS and FMPS on PL1. The results are shown in Table 1. As per the three-tiered approach, an exposure is detected when the net number concentration of the aerosol particles (obtained after deducting the BG from the instantaneous particles number concentration) surpasses the two times of its standard deviation of BG. Using this criterion, all the steps involved in PL1 were found to be potentially emissive. However, considering the ubiquitous nature of the NPs, the sole use of reading instruments in this approach does not provide information on certain specificities such as morphology or composition. By contrast, the STS approach, which is capable of determining their morphology or composition, plays a complimentary role in this aspect. On the basis of the microscopic observations, it successfully refines the step 5 as potentially emissive as it is the only task where ZrO2 NPs and sub-micron particles emission were detected. The particle size distributions (or size resolution) measured using SMPS and FMPS are shown in Figure 2 (a). The two instruments detect an almost unimodal size distribution of the emitted aerosol particles (initial aberrations for smaller sizes neglected) with the same size mode at 81 nm. The time resolution or the sampling time kept for SMPS was 5 min 25 s whereas for FMPS, it was 1 s. the step 5 as potentially emissive as it is the only task where ZrO the step 5 as potentially emissive as it is the only task where ZrO tiered approach, CPC and tiered approach, CPC and compared with an intensive campaign carried out using SMPS and FMPS compared with an intensive campaign carried out using SMPS and FMPS detected detected e BG from the e BG from the of its standard deviation of BG. of its standard deviation of BG. Using this criterion, all the steps involved in PL1 were found to be potentially emissive. However, Using this criterion, all the steps involved in PL1 were found to be potentially emissive. However, e NPs, the sole use of reading instruments in this approach does e NPs, the sole use of reading instruments in this approach does morphology or composition. By contrast, the morphology or composition. By contrast, the which is capable of determining their morphology or composition which is capable of determining their morphology or composition, plays a plays a role in this aspect. On the basis of the microscopic observations, it successfully refines role in this aspect. On the basis of the microscopic observations, it successfully refines 2 2 NPs and sub NPs and sub (or size resolution) (or size resolution) measured using SMPS and measured using SMPS and . The two instruments detect an almost unimodal size distribution of . The two instruments detect an almost unimodal size distribution of the emitted aerosol particles (initial aberrations for smaller sizes neglected) with the same size mode at the emitted aerosol particles (initial aberrations for smaller sizes neglected) with the same size mode at ime resolution or the sampling time kept for SMPS was 5 min 25 s whereas for FMPS, it ime resolution or the sampling time kept for SMPS was 5 min 25 s whereas for FMPS, it Step no.

Step Bold: suspected source There is a higher particle size measurement range in the case of FMPS which allows detection of more particles than SMPS but here the difference is low because the aerosol size is mainly nanometric. Time resolved distributions of the emitted aerosol particles which were measured by the two sizers i.e. SMPS and FMPS and one counter i.e. CPC are shown in Figure 2 (b). The aim of this comparison is to validate the number concentrations obtained using CPC which are already shown in the Table 1. All the changes observed in the number concentration measured by CPC are also present in the cases of FMPS and SMPS, e.g. the increase in the number concentration as soon as the oven starts warming up and maximum concentrations when the oven attains the temperature set-point. The number concentration measured by FMPS illustrates short-term peaks whereas SMPS counting corresponds to an approximate average of these peaks (see Figure 2 (b)). However, there are differences in their measured values. These differences can be due to two facts: (i) the difference in the measurable size ranges of the three instruments; (ii) different conditions in the workplace during which these measurements were taken. Process Line 2

PL2 uses a confined spray drying chamber to generate aggregated or agglomerated powders of ZrO2 NPs. The operation to test the BG was carried out in the solution preparation room before starting the spray drying process of the ZrO2 NPs (see Table 1). The number concentration of the BG particles in the room was about 4,000 cm -3 . The fluctuations observed, once the process started, are provided in the Table 1. Apart from a single micronic NOAA of ZrO2 (during step 7), no significant emission was detected. Since no particle containing Zr was found over other ten grid squares, this emission can be neglected.

Process Line 3 The operation to test the spray drying spray drying the room was the room was the the Table 1 Table 1 term peaks whereas SMPS counting corresponds to term peaks whereas SMPS counting corresponds to However, there are differences in their However, there are differences in their difference in the measurable size difference in the measurable size during which these during which these PL3 produces polyamide nanofibers using an electrospinning process. While doing the BG characterization for the PL3, the absence of a chemical element that can act as a polyamide nanofiber tracer (a reference to identify the presence of polyamide nanofibers) for its detection complicated the task. Indeed, carbon and oxygen, which are main constituents of polyamide nanofibers, were commonly detected in the particles present in the ambient air. Nitrogen was the only element present in the nanomaterial that was less commonly detected in the ambient air particulates collected on the TEM grids. The task therefore got oriented towards the search of fibers in the ambient air samples that contained nitrogen. As detailed in the Table 1, no exposures were detected obtained during the entire PL.

Process Line 4

PL4 uses an electrospinning process to generate TiO2 nanofibers. Five minutes prior to turning on the oven, the background particles analysis was carried out. The results, provided in the Table 1, account from the point when the electrospinned fibers calcination starts, i.e. when the fibers were placed in an oven at 240°C for a few minutes and were then collected, ground and weighed. The number concentration variation with time, during these steps, is summarized in Table 1.

The TEM images of the aerosol particles, which were sampled during the manipulation processes are shown in Figure 3 (a) and (b). Out of the twenty TEM grid squares analyzed, all contained at least two fibers with a maximum of 14 fibers and an average of nearly 8 fibers per quadrant. As a result, the cleaning step of the PL4 led to an exposure of submicronic fibers (see Table 1).

Process Line 5

The dispersion spraying on tiles is a common process to modify their surface properties. PL5 aims to produce such modified tiles by using pulverized dispersions of TiO2 and Ag NPs respectively. Prior to the PL operation, no Ti or Ag objects were detected in collected samples during BG sampling (see Table 1).

The spraying step was performed in two stages. The first stage consists of spraying a dispersion containing 1 wt% of TiO2 NPs onto a first batch of tiles. Twenty minutes later, the operator sprays a similar dispersion of Ag NPs on another batch of tiles of the same type. The Table 1 shows the results. Throughout the entire period, a slow increase in the count was observed, followed by a sharp increase in the particle concentration a few minutes after the silver-based aqueous dispersion was sprayed. The microscopic images of the particles sampled during cleaning, filling and spraying steps are shown in Figure 3 (e) (g). Five out of six steps of PL5 were found to be prone to an exposure (see also Table 1).

minutes prior to turning on the minutes prior to turning on the provided in provided in the the Table 1 Table 1 i.e. when the fibers i.e. when the fibers were placed in an were placed in an collected, ground and weighed. The collected, ground and weighed. The number number is summarized in is summarized in Table 1 Table 1. . which were sampled during t which were sampled during the manipulation processes are he manipulation processes are (b). Out of the twenty TEM grid squares analyzed, all contained at least two (b). Out of the twenty TEM grid squares analyzed, all contained at least two fibers with a maximum of 14 fibers and an average of nearly 8 fibers per quadrant. fibers with a maximum of 14 fibers and an average of nearly 8 fibers per quadrant.

exposure of submicronic fiber exposure of submicronic fibers s (see (see ispersion spraying on tiles is a common process to modify ispersion spraying on tiles is a common process to modify by using by using pulverized pulverized o Ti or Ag objects o Ti or Ag objects were were was performed in two stages. The first stage consists of spraying a dispersion was performed in two stages. The first stage consists of spraying a dispersion % of TiO % of TiO2 NPs NPs dispersion of Ag dispersion of Ag NPs NPs Throughout the entire period, a slow increase in the count was observed, followed by a sharp increase Throughout the entire period, a slow increase in the count was observed, followed by a sharp increase in the particle concentration a few minutes after the silver in the particle concentration a few minutes after the silver microscopic images of the particles sampled during microscopic images of the particles sampled during Figure Figure 3 3 ( (e e) ) 1). ).

Process Line 6

PL6 is based on extrusion of a MWCNT reinforced polymer matrix. No NOAA of CNT were identified during BG sampling (see Table 1). The extrusion produced a slow increase in the number concentration with short peaks particularly in the cleaning step (see Table 1). CNT objects collected during extrusion (Figure 4 (a-e) and cleaning (Figure 4 (f)) highlight these two steps as emissive one. Two steps out of seven, i.e. the extrusion and the cleaning, were identified as emissive. Both free CNT as well as inhalable NOAA (bundles or submicronic objects), made of CNT and polymeric matrix, were detected in this emission.

Process Lines Ranking

Based on the results in Table 1 and the microscopic observations, the six PLs are ranked in Table 2. An exposure is declared in case of NP or NOAA on the sample obtained in the PL. The emission levels ratio is then estimated using a ratio between the emissive step counting and the BG counting. Based on the results in Table 1 and the microscopic observations, t Based on the results in Table 1 and the microscopic observations, t exposure is declared in case of NP or NOAA on the sample exposure is declared in case of NP or NOAA on the sample levels ratio is then estimated using a ratio between the emissive step counting and the BG counting. levels ratio is then estimated using a ratio between the emissive step counting and the BG counting. No emission of ZrO2 particles (except one NOAA of ZrO2 during powder retrieval and transport which is considered to be negligible as per the STS approach criterion) 4000 --

3

No exposure detected

No emission of the polyamide nanofibers 3200 --

Discussion

The present article deals with the results of a semi-quantitative exposure assessment campaign which was carried out at six different PL concerned with the production and manipulation of nanomaterials. Apart from ZrO2 nanoparticles, the types of the nanomaterials chosen for the present study belong to the pool of the most widely-used nanomaterials in Europe and the world (Piccinno et al., 2012). The typical workplaces involved with the nanomaterials production and their manipulation i.e. R&D laboratories and commercial manufacturing sites with varying surface sizes (from 20 to 300 m 2 ) are also considered in this study. Some of these workplaces had natural ventilation systems. We were also able to track and characterize NP or NOAA emission in workplaces having diverse characteristics like co-activities (e.g. welding) different air flow patterns, or dimension variability.

Data gathering

Before starting the semi-quantification of the aerosol particles, a step-wise information gathering about the processes, materials and workplaces is required and done through preliminary visits. Once all the information is gathered and analyzed, the exposure assessment campaign is then carried out. Such a campaign provides a visual perception of the workplaces (process and work practices). At the same time, the information collected during this visit could provide useful inputs like exposure scenarios, process information, details regarding ventilation and the need of the personal protection equipment to carry out the risk assessment studies.

Approach comparison in PL1

The number concentration results obtained by the CPC, SMPS and FMPS on the PL1 were validated by showing a good agreement between the three. The PL1 was chosen for the comparison purpose because the conditions like forced ventilation in the absence of a co-activity and small size of the production facility were ideal to do so A prior increase in the number concentration (during steps 1 to 4), attributed to the incidental emission of particles during production process, was observed. This can be proved by noting the corresponding value of Cnet-BG equal to 6288 cm -3 , in the Table 1 during the exposure assessment campaign which exposure assessment campaign which was carried out at six different PL concerned with the production and manipulation of nanomaterials. was carried out at six different PL concerned with the production and manipulation of nanomaterials.

f the nanomaterials chosen for the present study f the nanomaterials chosen for the present study used nanomaterials in Europe and the world used nanomaterials in Europe and the world ( (Piccinno et al., 2012 Piccinno et al., 2012 typical workplaces involved with the nanomaterials production and their manipulation i.e. R&D typical workplaces involved with the nanomaterials production and their manipulation i.e. R&D laboratories and commercial manufacturing sites with varying surface sizes (from 20 to 300 m laboratories and commercial manufacturing sites with varying surface sizes (from 20 to 300 m e of these workplaces had natural ventilation systems. e of these workplaces had natural ventilation systems. NP or NOAA emission in workplaces having diverse characteristics like NP or NOAA emission in workplaces having diverse characteristics like . welding) different air flow patterns, or dimension variability. . welding) different air flow patterns, or dimension variability. quantification of the aerosol particles, quantification of the aerosol particles, materials and workplaces materials and workplaces all the information is gathered and analyzed, the exposure assessment campaign is then carried out. all the information is gathered and analyzed, the exposure assessment campaign is then carried out. Such a campaign provides a visual perception of the workplaces (process and work practices). At the Such a campaign provides a visual perception of the workplaces (process and work practices). At the same time, the information collected during this v same time, the information collected during this v scenarios, process information, details regarding ventilation and the need of the personal protection scenarios, process information, details regarding ventilation and the need of the personal protection equipment to carry out the risk assessment studies. equipment to carry out the risk assessment studies.

Approach comparison in PL1 Approach comparison in PL1

opening of an empty warm oven door. This value of Cnet-BG can be explained on the basis of (i) an ambient air agitation due to the warming up of the oven, and (ii) drying of the material with the contained residual moisture in the oven by the evaporation of residual moisture which in turn produces water droplets counted as particles by FMPS, SMPS or CPC. Nevertheless, the detected particles on the TEM grid are solely solid objects. These two facts can also explain the high particle number concentrations during steps 3 and 4 but with a total absence of ZrO2 particles in the sample particles population. The specific cases of incidental emissions due to oven warming-up or water droplets generation are regularly observed at workplaces and perturb a precise assessment (Dolez and Debia, 2015). The STS and three-tiered approaches are in accordance with each other, thus confirming the exposure in the PL1. But the results included in the Table 1 illustrate that the STS approach can specifically detect a NP emission by identifying a huge number of ZrO2 particles (confirmed by EDS analyses), during a unique step i.e. step 5 of oven opening in the PL1 in the middle of incidental emissions.

Hence, while employing the three-tiered approach on PL1, we identified the inherent complimentary nature of the STS approach to the three-tiered. The three-tiered approach is an important tool to identify and evaluate the potential exposure sources. However, the STS approach gives the opportunity to refine these potential sources because of short-term exposure distinctions. This is of utmost importance to the Small or Medium Enterprise (SME) which represented 75 % of the EU companies dealing directly with nanotechnology and manufactured nanomaterials in 2012 (EU OSHA, 2012). Identifications of exposure sources becomes also easier for them and can lead to the opportunity to modify the certain identified steps rather than the entire PL.

STS Approach Advantages

Thanks to the MPS-TEM couple, the major advantage of the STS approach is the opportunity to distinguish easily NP or NOAA from BG. The emission determination is hugely facilitated (as shown in Table 1). In this case, even the emissions with very short durations are observable and can be characterized, as done, for instance, in the step 7 (cleaning) of the PL4, all spraying related steps of the PL5 and steps 6 and 7 (extrusion and cleaning) of the PL6. The cleaning steps are crucial to the exposure assessment (Ham et al., 2012;Kaminski et al., 2015;Zimmermann et al., 2012). Similarly, the spraying step is known as one of the highest emission sources (Bekker et al., 2015;Wake et al., 2002). Regarding the extrusion process, previous studies highlight the difficulties to assess an emission (Brouwer et al., 2014a;Dahm et al., 2013).

The STS approach offers an opportunity to characterize an emission of the nanomaterials or inhalable objects with any size or shape. Their emissions may even occur without any increase in the aerosol particles number concentration. The exposure in the case of PL4 number 7 illustrates such condition. The sampled TiO2 fibers were of submicron length with diameters varying from 150 to 500 nm. Despite these dimensions, an exposure has been clearly detected while the corresponding number concentration level was close to the BG number concentration (5000 cm -3 , R=1.1; see Table 1).

The STS approach has led to characterize free CNTs as well as different inhalable NOAA like CNT bundles or CNT composites, nano-Ag and nano-TiO2. Moreover, the relative magnitude of such an reathing zone of workers can also be easily determined using the STS approach. es (confirmed by EDS es (confirmed by EDS step 5 of oven opening in the PL1 in the middle of incidental step 5 of oven opening in the PL1 in the middle of incidental inherent complimentary inherent complimentary tiered approach is an important tool to tiered approach is an important tool to he STS approach he STS approach gives the gives the term exposure distinctions term exposure distinctions which represent which represented ed 75 % of the EU dealing directly with nanotechnology and manufactured nanomaterials dealing directly with nanotechnology and manufactured nanomaterials easier for them easier for them and can lead to the and can lead to the modify the certain identified steps rather than the entire PL. modify the certain identified steps rather than the entire PL. he major advantage of the STS approach is the opportunity to he major advantage of the STS approach is the opportunity to distinguish easily NP or NOAA from distinguish easily NP or NOAA from BG BG. The e

The emission determination is hugely facilitated In this case, even the emissions with very short durations are observable and can be In this case, even the emissions with very short durations are observable and can be for instance, for instance, in the in the step 7 (cleaning) step 7 (cleaning) 7 (extrusion and cleaning) 7 (extrusion and cleaning) Ham et al., 2012Ham et al., 2012 is known as one of the highest emission source is known as one of the highest emission source Regarding Regarding the the extrusion process extrusion process Brouwer et al., 2014aBrouwer et al., 2014a The STS approach offers an opportunity to characterize an emission of the nanomaterials or inhalable The STS approach offers an opportunity to characterize an emission of the nanomaterials or inhalable objects with any size or shape. objects with any size or shape. particles number concentration. particles number concentration. condition condition. The sampled TiO . The sampled TiO nm. Despite these dimensions, an nm. Despite these dimensions, an concentration level was concentration level was

The easy NOAA distinction from the stray particles is another potential advantage of the STS approach as confirmed by the results obtained in the cases of PL5 and PL6 (see Table 1).

In this context, some previous studies describe NOAA characterization at workplaces (Bekker et al., 2015;Brouwer et al., 2014b;Brouwer et al., 2013). The more recent paper uses nickel coated polycarbonate filters in the IOM sampler followed by SEM characterization in the absence of step-bystep information (Bekker et al., 2015).

Emissions from the PL

The ranking proposed in Table 2 shows that the PL1 (oven opening in particular) renders highest emission followed by the PL6 (extrusion and cleaning) and then the PL5 (spraying and curing). Regarding the PL4, the unique emission is a cleaning step. The spray drying process (i.e. PL2) and the production of polyamide nanofibers (i.e. PL3) are considered as non-emissive because of the absence of NP / NOAA or nanofiber upon sampling. In our study, 8 out of 37 steps were found to be prone to a NP or NOAA exposure. Only one of the 37 steps highlights solely NP exposure (i.e. oven opening of PL1). This observation confirms the important part of NOAA exposure at workplace instead of NP one in accordance with recent literature (Bekker et al., 2015;Brouwer et al., 2014a;Brouwer et al., 2014b;Brouwer et al., 2013). In addition, one step leads to an exposure of submicronic fiber (cleaning, step 7 of PL4). In other words, 24 % (9 out 37) of the steps highlight exposures whatever the emitted materials i.e. submicronic fiber, NOAA or NP but two thirds of the PLs are implicated in almost one exposure step. Some of these nine steps giving rise to an exposure (e.g. cleaning step of the PL4) were not accompanied with a significant number concentration increase. The interest of our STS approach is thus confirmed by the possibility to distinguish an exposure in such conditions.

A complementary approach yet to be improved

Apart from these added values, the STS approach does suffer from some limitations. The first worthy of mention is the absence of the information on size resolved number concentration.

Sizing (using three-tiered approach) has been performed on the PL1 but limited to the comparison purpose. The use of counters in this approach allows the integration of the exposure, reducing measures quickly and cheaply into any production or manipulation step.

Quantitative sizing measurement could improve emissions data to provide a more precise assessment of NP fraction of the aerosol. Another limitation noted during the exposure evaluations involved the upper dynamic measurement range of the CPC which is equal to 10 5 cm -3 . Therefore, all data exceeding this value (as shown in figure 2 (b) and Table 1) should be interpreted with caution because an underestimation of the true particle number concentration will result (Asbach et al., 2012). Another drawback of this approach shows is the absence of long-term exposure assessment. As a result, the data presented here cannot be used for a thorough toxicological assessment or control banding.

Conclusions s highest s highest and curing). curing).

The spray drying process ( The spray drying process (i.e. i.e. PL2) and the PL2) and the because of because of the the absence steps were found to be prone to a steps were found to be prone to a solely NP exposure solely NP exposure ( (i.e. oven opening of oven opening of xposure at workplace instead of NP xposure at workplace instead of NP Brouwer et al., 2014aBrouwer et al., 2014a exposure of submicronic fiber exposure of submicronic fiber of the steps highlight exposures of the steps highlight exposures the emitted materials i.e. submicronic fiber, NOAA or NP but two thirds of the PL but two thirds of the PL steps giving rise to an exposure ( steps giving rise to an exposure ( t number concentration increase t number concentration increase to distinguish an exposure in such conditions to distinguish an exposure in such conditions to to be be improve improve Apart from these added values, the STS approach does suffer from some limitations. The first worthy Apart from these added values, the STS approach does suffer from some limitations. The first worthy is the absence of the information on of the information on tiered approach) has been performed on the PL1 but tiered approach) has been performed on the PL1 but se of se of counters counters in this approach quickly quickly and cheaply and cheaply ative sizing measurement could imp ative sizing measurement could imp of NP fraction of the aerosol. of NP fraction of the aerosol. upper dynamic measurement range of the CPC which is equal upper dynamic measurement range of the CPC which is equal exceeding this value (as shown in exceeding this value (as shown in an underestimation of the true particle number concentration an underestimation of the true particle number concentration drawback of drawback of

The study presented here aims at verifying the applicability of the STS approach in a representative set of European SME dealing with nanomaterials, which is today needed in industry (De Rademaeker et al., 2014) on the basis of interdisciplinary approaches (Gehin et al., 2016). A comparison has been performed with the three-tiered approach. The results confirm exposures at some workplaces. The STS approach identified eight steps prone to short-term exposures of nanoparticles or NOAA out of total 37 steps distributed in six process lines (PL). Another additional exposure of submicronic fibers of TiO2 has been characterized thanks to TEM sampling and despite a low counting increase. During the entire study, the leading potential exposure sources were found to be the steps like manipulation (e.g. PL1, 4, 5 and 6), spraying (e.g. PL5) and cleaning (e.g. PL4 and 6). In addition, high emissions observed in the handling steps are consistent with the large amounts of nanoparticles reported in the basic information gathering of the PL1, 4, 5 and 6.

The process like spray drying (i.e. PL2) or electrospinning (i.e. PL3) are generally performed in a complete confinement and therefore exhibited no detectable emissions. The low intrinsic emissivity of the nanofibers or the containment of the machines producing the nanofibers effectively prevented their emission in the workplace. As a result, the handling of ZrO2 NP (i.e. PL1) was observed to impart maximum potential exposure and minimum for the polyamide nanofiber production (i.e. PL3). In most cases where the exposure was detected, it was seen that no free primary particles but only NOAA (both > and < 100 nm) got emitted (e.g. PL5). In the case of fibrous materials, like fibers of TiO2 (i.e. PL4) and MWCNT (i.e. PL6), their emission was found to be intermittent. The presence of their free strands as well as their bundles was detected in the ambience. As long as the nanomaterials existed in the form of suspension (e.g. PL2 and 3), no exposure was detected. The use of an oven (as in the cases of PL1 and 5) was also found to be critical in the terms of exposure.

Figure 1 :

 1 Figure 1: Schematic representation of the global approach for Exposure Assessment at work places through STS methodology integrating data gathering and measurement campaigns at workplaces. The near filed zone corresponds to vicinity of the worker.

  production/handling/manipulation of the nanomaterials (NM) and comparison between dealing with the production/handling/manipulation of the nanomaterials (NM) and comparison between : Ventilation; : Ventilation; N/F N/F: Natural or Forced; : Natural or Forced; : Standard deviation; : Standard deviation; Background Background particles (obtained using TEM of the sampled aerosol particles) present in the particles (obtained using TEM of the sampled aerosol particles) present in the BG BG before starting the production or manipulation of the nanomaterials; ion obtained by subtracting the mean particle number concentration of ion obtained by subtracting the mean particle number concentration of Exposure limit set to 1 particle per grid square on ten grid squares; Exposure limit set to 1 particle per grid square on ten grid squares; § § § § : Indicative value, beyond the meas : Indicative value, beyond the meas) is given because the ) is given because the BG BG is evaluated for each step is evaluated for each step

Figure 2 :

 2 Figure 2: Comparison between (a) averaged particle size distributions of the emitted aerosol particles measured by SMPS and FMPS during the entire operation of PL1 (std. dev. for SMPS: 4 to 2094 cm -3 and for FMPS: 0.4 to 3615 cm -3 ); (b) total number concentrations measured by SMPS and FMPS with the number concentration measured by CPC during the entire operation of PL1

:

  Comparison between (a) averaged particle size distributions of the emitted aerosol : Comparison between (a) averaged particle size distributions of the emitted aerosol by SMPS and FMPS during the entire operation of PL1 (std. dev. for SMPS: 4 to 2094 cm by SMPS and FMPS during the entire operation of PL1 (std. dev. for SMPS: 4 to 2094 cm ); (b) total number concentrations measured by SMPS and FMPS with the number concentration ); (b) total number concentrations measured by SMPS and FMPS with the number concentration measured by CPC during the e measured by CPC during the entire operation of PL1

Figure 3 :

 3 Figure 3: (a) TEM image of a particle containing Zr observed during opening of the oven and transport of the dried powder. (b) & (c) TEM image of the sampled aerosol particles during PL4 operation. (d) & (e) TEM images of the particles sampled during cleaning and filling steps; TiO2 content: 1-2%; (f) Examples of NOAA of Ag and their clusters sampled during Ag based dispersion spray

  of the oven and transport of the observed during opening of the oven and transport of the ) TEM image of the sampled aerosol particles during PL4 operation. ( ) TEM image of the sampled aerosol particles during PL4 operation. ( TEM images of the particles sampled during cleaning and filling steps; TiO TEM images of the particles sampled during cleaning and filling steps; TiO Ag and their clusters sampled during Ag based dispersion spray Ag and their clusters sampled during Ag based dispersion spray extrusion of extrusion of a MWCNT reinforced MWCNT reinforced during BG sampling during BG sampling (see (see concentration with short peaks particularly in the cleaning step (see concentration with short peaks particularly in the cleaning step (see extrusion ( extrusion (Figure Figure 4 4 Two steps out of seven Two steps out of seven as well as inhalable NOAA as well as inhalable NOAA were detected in this emission. were detected in this emission.

Figure 4 :

 4 Figure 4: (a) -(d) Different forms of the sampled CNTs during extrusion process; (e) submicronic NOAA made of CNT and polymeric matrix (f) CNT bundle sampled during cleaning step of the PL6

  Different forms of the sampled CNTs during extrusion process Different forms of the sampled CNTs during extrusion process; ; (e) submicronic NOAA made CNT bundle sampled during cleaning CNT bundle sampled during cleaning

  step 5; no emissive step in PL2 and 3; emissive step in PL4: step 7; emissive steps in PL5: steps in PL1: step 5; no emissive step in PL2 and 3; emissive step in PL4: step 7; emissive steps in PL5: steps 1, 2, 4, 5 and 6; emissive steps in PL6: steps 6 and 7) 1, 2, 4, 5 and 6; emissive steps in PL6: steps 6 and 7) particles present in the background before starting the production or manipulation of the nanomaterials;

Table 1 :

 1 Summary of the production lines (PL) dealing with the production/handling/manipulation of the nanomaterials (NM) and comparison between short time sampling

	); § § § : Exposure limit set to 3xSD
	cm -3
	e. 10 5

(STS) and three tiered approaches on PL1. NPs: Nanoparticles; Vent: Ventilation; N/F: Natural or Forced; CA: Co-activity; Y/N: Yes/No; WS: Workspace; S: Small (< 40m ); M ); B: Big (> 100 m ); SD: Standard deviation; Background (BG): Average number concentration (obtained using CPC) and type of the particles (obtained using TEM of the sampled aerosol particles) present in the BG before starting the production or manipulation of the nanomaterials; Cnet: Net particle number concentration obtained by subtracting the mean particle number concentration of BG from the mean of instantaneous number concentration; N/A: Not available; § : Exposure limit set to 1 particle per grid square on ten grid squares; § § : Indicative value, beyond the measuring limit of the CPC (i.> Cnet; *: A range of BG values (Cnet or SD) is given because the BG is evaluated for each step; MWCNT: Multiwalled Carbon Nanotubes PL/NM Facility type

Table 2 ratio ; :

 2; Mean of individual CPCmean of the emissive steps in a PL from Table 1 (emissive step

	in PL1: step 5; no emissive step in PL2 and 3; emissive step in PL4: step 7; emissive steps in PL5: steps
	1, 2, 4, 5 and 6; emissive steps in PL6: steps 6 and 7); BG: Average number concentration of the
	particles present in the background before starting the production or manipulation of the nanomaterials;
	R =	/BG;
	PLs Exposure level	Remarks on exposure from sampling analysis	BG (cm -3 )	(cm -3 )	(#)

Author contribution

Bressot, Christophe directed, prepared and performed the experiments with the assistance of Shandilya, Neeraj, who also edited parts of the manuscript. Jayabalan, Thangavelu, Le Bihan, Olivier, Voetz, Matthias and Meunier, Laurent contributed to the measurement campaings. Fayet, Guillaume provided input to the assessment method. Morgeneyer, Martin and Aguerre-Chariol, Olivier contributed to the scientific analysis of the measurement data and to the conceptual implementation of the method.

Acknowledgment

The research leading to these results is part of SANOWORK project which has received funding from the European Union Seventh Framework Programme (FP7) under grant agreement no. 280716. Note: amounts of nanoparticles reported in the amounts of nanoparticles reported in the performed performed in a in a he low intrinsic emissivity of he low intrinsic emissivity of producing the nanofibers effectively prevent producing the nanofibers effectively prevented ed was observed to impart was observed to impart polyamide nanofiber production (i.e. polyamide nanofiber production (i.e. primary particles but only NOAA primary particles but only NOAA In the case of fibrous materials, like fibers of TiO In the case of fibrous materials, like fibers of TiO ermittent. The presence of their free ermittent. The presence of their free strands as well as their bundles was detected in the ambience. As long as the nanomaterials existed in strands as well as their bundles was detected in the ambience. As long as the nanomaterials existed in detected detected. . The use of an oven The use of an oven was also found to be critical in the terms of exposure. was also found to be critical in the terms of exposure.

prepared and performed the experiments with the assistance of prepared and performed the experiments with the assistance of ya, Neeraj, who also edited ya, Neeraj, who also edited parts of the manuscript. Jayabalan, Thangavelu, parts of the manuscript. Jayabalan, Thangavelu, Meunier, Laurent contribute Meunier, Laurent contribute Fayet, Guillaume provided input to the assessment method. Morgeneyer, Martin and Aguerre Fayet, Guillaume provided input to the assessment method. Morgeneyer, Martin and Aguerre Chariol, Olivier contributed to the scientific analysis of the measur Chariol, Olivier contributed to the scientific analysis of the measur conceptual implementation of the method. conceptual implementation of the method.

Acknowledgment Acknowledgment

The research leading to these results The research leading to these results the European Union Seventh Framework Programme (FP7) under grant agreement n the European Union Seventh Framework Programme (FP7) under grant agreement n


Valérie-Inés De

La Ville
email: delaville@iae.univ-poitiers.fr

Benjamin Dreveton
email: bdreveton@iae.univ-poitiers.fr

The ongoing monitoring of societal responsibility in management research activities: A secondary analysis and a heuristic instrumentation

Keywords:

The ongoing monitoring of societal responsibility in management research activities A secondary analysis and a heuristic instrumentation

Benjamin Dreveton, Valérie-Inès de La Ville

Introduction

In a praxeological sense 1 management sciences contribute to making the managerial practices they analyze more efficient, effective and insightful. The activity of the researcher in management sciences is far too often portrayed as a solitary activity [START_REF] Avenier | Élaborer des savoirs actionnables et les communiquer à des managers[END_REF], despite the fact that more and more management research is carried out within a contractual framework, whether that be as a research-intervention within a particular organization or a response to a call for projects by the National Research Agency through which government bodies proactively prioritise the research topics. Thus, in a context where research projects do not emerge purely from a strict scientific rationale specific to the discipline, but meet at the juncture of political and social issues, the question of societal responsibility within management research activity is an important issue, not only from the public policy standpoint, but also in terms of the scientific discipline itself [START_REF] Royer | La responsabilité sociale des chercheurs en gestion[END_REF]. In fact, although many researchers in management sciences describe, analyze and demonstrate the importance for companies to implement « responsible » practices, few question the need to implement these same principles within their own professional activity... This paper proposes an initial exploration of the following question: How can we characterise the societal responsibility of researchers in management sciences? If each research project is specific (according to its epistemological, methodological and theoretical affiliation), work carried out in management sciences cannot avoid the responsibility for the changes that their models and experiments bring about, not only within companies and organizations, but also beyond the company boundaries [START_REF] Delacour | Toutes les recherches doivent-elles être menées ? Performativité, surpâturage et responsabilité du chercheur en finance[END_REF]. Therefore, the researcher must be aware of the consequences that his work is likely to have for the company.

Our argument is structured in three parts. The first returns to the idea of responsibility in order to specify its characteristics, particularly when described as « societal ». The second part presents a secondary analysis of a research process with the aim of exploring the consequences a researcher's work has for a company. Finally, the last part defines the concept of social responsibility for a researcher in management sciences by identifying two types of responsibility: professional and institutional.

I.

The responsibility of the researcher in management sciences: a multi-faceted responsibility

This first section proposes a definition of the researcher's responsibility applied specifically to the activity of the researcher in management sciences. This transition enables us to highlight two levels of responsibility for the researcher in management: the first refers to his scientific responsibility, the second stresses the societal responsibility of his activity.

1.1

What should be the definition of a researcher's responsibility?

According to the dictionary (Robert 1964), a researcher's responsibility is seen to be « the moral and intellectual obligation or necessity [he has] to carry out his work in full awareness that the way in which he works -both theoretically and practicallywill carry consequences, and in accepting being named as the author, the willful cause of these consequences » (quote by Schlemmer 1998, p. 229). This definition applies to the activities of management researchers who study organizations and their managerial practices. In fact, rather than denying that which justifies its value, management research activity in a praxeological sense should at the very least take a share of the responsibility for the procedures observed within organizations since the research results contribute directly to transforming the company, its projects, its innovation processes, its control procedures, its tools, etc.

The responsibility of the researcher in management therefore is in full play at the very heart of the two aspects that characterize his research work: both in the choices he makes to advance his project of knowledge and in the manner in which he communicates the contribution provided by his work to members of the company being studied, and to the scientific community to which he belongs. The responsibility of the researcher in management must therefore be analyzed on two levels: individual and collective.

Scientific responsibility

Individual responsibility has been addressed extensively through the concept of reflexivity. Indeed, the value of reflexivity within research activities has been emphasized repeatedly [START_REF] Schön | The Reflective Practitioner[END_REF][START_REF] Schön | Educating the Reflective Practitioner[END_REF][START_REF] Alvesson | Reflexive methodology -New vistas for Qualitative Research[END_REF][START_REF] Yanow | What Is Reflection-in-Action? A Phenomenological Account[END_REF] because, just like the practitioner, the researcher must be capable of analyzing the impact of his own activity on the organization he is observing. Reflexivity is an essential dynamic in mastering the progress of a research activity and has three dimensions (de La [START_REF] Ville | Rendre compte de la singularité : quels enjeux pour la recherche en management stratégique ?[END_REF]:

Operational reflexivity: this reflexivity refers to the way in which the researcher uses his skills (apparent and inherent) to do his job as a researcher. These skills are too often disregarded in research reports and yet they have a decisive influence on the quality of the exchanges established with the different actors in the organization. If [START_REF] Schön | The Reflective Practitioner[END_REF] defines reflexivity as a reflection of the actions already accomplished by the manager or researcher, [START_REF] Yanow | What Is Reflection-in-Action? A Phenomenological Account[END_REF] emphasize the importance of developing a phenomenological approach to reflexivity that can incorporate the prior activity as well as guiding the ongoing activity of the researchers. Indeed, some unusual situations have called upon the improvisational skills of the researcher where the implementation reveals the ethical choices that the latter made « in vivo » in order to advance his work.

Conceptual reflexivity: the researcher's work should not be limited to promoting a set of management practices developed by an organization in a given context. In order to surpass situated events, the management researcher, during his activity, must structure and organize his analytical work according to the themes under discussion within his affiliated discipline. Thus, for example, the selection of significant elements, the definition of categories for analysis, the choice of an architecture in which to develop a piece of work all emphasise the need for the researcher to make a certain number of controlled moves. By allowing the creation of categories, concepts and classifications, these moves lead to an enrichment of knowledge by reorganizing the experiences of the players in the field and result in a new command of the real situation, as much for the researcher as for the actors in the organization [START_REF] Goody | La raison graphique -La domestication de la pensée sauvage[END_REF].

Scriptural reflexivity: through his commitment to the writing process, the researcher no longer merely describes the organization: he contributes directly to its evolution. As Morin recalls: « Responsibility begins with the decision to be an author in what we describe as our world » (quote by Besnier 2008, p.161). Management research activity then can be analyzed as a scriptural game: « The scriptural game, the production of a system, opportunity realm for formalisation, means returning to the reality from which it was differenciated in order to change it » (Certeau (de) 1990, p. 200). This level of reflexivity assumes the researcher can clarify the assumptions on which his writing project is based and which progressively crystallize as the interpretation progresses. Thus, the real scope of the modeling can be assessed when the researcher masters the underpinnings of the transformative perspective it opens in order to change the organization.

These three dimensions of reflexivity emerge during the course of the researcher's everyday activities and indicate the need for him to investigate many diverse ethical issues. This reflexivity is « disciplining » 2 by nature: the researcher has to record the results of his work within the context of current debates within the scientific community to which he belongs. Indeed, if reflexivity claims to create « actionable knowledge » [START_REF] Argyris | A life full of learning[END_REF], which is teachable and useable in practice by managers (Le Moigne 1995), researchers in management sciences cannot avoid the question of their commitment, which goes beyond their own scientific community, to open up to society in its widest sense.

Societal responsibility

Considering the societal responsibility of the researcher enables us to record and describe the relationships that exist between the management researcher's activity and the different components of the company. We associate the term « societal » to that of social in its broadest sense 3 , as Capron and Quairel suggest « common usage tends more and more to include the term social (in the context of CSR) in its original meaning derived from the Anglo-American which encompasses societal aspects ». (2010, p. 27). The researcher's responsibility widens beyond the scientific sphere and its nature changes: it becomes « social » insofar as the researcher has not only to incorporate the social expectations at the heart of his everyday activities but also be able to identify the societal consequences of his activity.

In fact, management researchers are asked increasingly to disseminate knowledge to an everwider audience: research participants, the academic community, the media, NGOs, policy makers and society at large [START_REF] Royer | La responsabilité sociale des chercheurs en gestion[END_REF]. This is why taking into consideration the societal responsibility of research activity should lead to developing the means for a dialogue with the various interested parties of the management researcher's work: « more should be done to educate scientists in dialogue with the public and the media. This activity should be incorporated into careers, and here we have a long way to go » (Alix 2009, p.48).

This type of question has already been widely discussed by the sociology of sciences that critically analyzes the relationships that exist between science, citizenship and public policy (Weber 1959 4 , Latour 1989 and 2001). The difficulties encountered by researchers in establishing a dialogue with non-specialist stakeholders, that is those outside of their affiliated discipline, have been highlighted in numerous studies (Crettaz von Rotten and Moeschlmer 2008). Researchers in social sciences are expected to respond to requests for public involvement to help identify the conditions for applying certain scientific discoveries that present potential risks (Irwin 1995). Thus, if they are absolutely necessary to guarantee a transparent scientific debate, the scrupulous implementation of codes of conduct and ethics or the re-editing operations concerning third parties, are only a first step in the consideration of research issues for the company.

The issue of a researcher's social responsibility should require him to question his ability to adopt innovative behaviour that aims to place the company at the centre of his activity. The researcher should be open to dialogue with stakeholders as, in order to be able to argue and claim how useful he is to the company, his own scientific project will inevitably be confronted by numerous projects, scales of value and ideologies [START_REF] Le Menestrel | Ethics in Operations Research and Management Sciences: A never ending effort to combine rigor and passion[END_REF]. New debates about the links between researchers and companies crystallize around issues of communication, participatory government and citizen involvement, in order to control the irreversibility established by the socio-technical developments produced through research (Irwin 2010).

As the societal responsibility of a researcher gradually builds through interaction with the institutional context and the various research partners (Béji-Bécheur et al., 2011), it seemed important to identify which management tool might help the management researcher to monitor such issues ... For, as Hatchuel reminds us: « defining a responsibility without providing the cognitive instruments that allow us to build and appreciate it, means taking away any possibility for it to exist ... » (2012, p. 169). In fact, as Pesqueux (2011) noted, social responsibility gives rise to a double movement: the consideration of stakeholders and the integration of this concept at the very heart of management practices. The instrumentation proposal outlined in the following section attempts to take up this double challenge.

II. Ideas for a heuristic instrumentation for monitoring the social responsibility issues of research in management sciences

To progress with this question we will first use a secondary analysis and then a research intervention. Our secondary analysis 5 seeks to reinterpret the difficulties related to conducting research and is based on the model « research design and methodological advancement » highlighted by Corti (2007, p. 42-45). The choice to revisit a research intervention relates to the very characteristics of that methodology that makes the researcher confront directly the different stakeholders of the company: partner organizations, stakeholders, customers, NGOs, political institutions, etc. (Pichault et al. 2009). The purpose of the secondary analysis is to examine the conditions that facilitate the establishment of a systematic dialogue with the various interested parties of the research so as to enable an ongoing co-monitoring of the different dimensions of societal responsibility likely to emerge during the course of the research.

Presentation of the principle characteristics of the research

This research was carried out with the Environment and Energy Management Agency (ADEME). The objective was to produce for local authorities a costing device to manage the financial excesses of the public waste disposal service. To create this instrumentation, the Agency decided to involve all the actors interested in this issue and invited local authorities to become actively involved in the project, as well as associations, regional councils, a business federation and researchers (see Diagram n° 1).

Diagram n°1 -The actors in the project

This research study [START_REF] Jönsson | There and back again. Doing interventionist research in management accounting[END_REF]Lukka 2007, David 2002) began with an audit of six local authorities in order to understand the specifics of the management of this public service, and also the needs of officials with regard to instrumenting its management. The process of constructing the device to measure the cost of waste took two years in close interaction with five communities. During this period, the researcher actively participated in the device's creation: the administration of a questionnaire (233 questionnaires sent to local authorities that managed a public waste disposal service), conducting semi-directive interviews (30 hours of interviews), the formalization of various processes (such as that of waste disposal), participation in working-group meetings (once a month during the creation process) and steering committee meetings (every two months).

This research intervention did not run smoothly with misunderstandings between the various parties involved in the development and diffusion of the device. Our secondary analysis enables us to illustrate this point. For example, debates developed regarding:

The role of the researcher: Members of the ADEME progressively insisted that the researcher should increasingly deal with the technical aspects relating to the creation of the device, which directly called into question his role in the project because when the contract was signed, it was clearly stated that the research should focus on the mechanisms to enable the community to appropriate the device. This unethical deflection slowed the progress of the work because the researcher had once again to explain and even negotiate his role so as not to move away from the initial requirement expressed in the contract.

The involvement of the local authorities: Another difficulty arose when the authorities involved in the implementation of the device blocked the project driven by the ADEME. The authorities wishing to develop a device to control their activity did not understand the benefits of the monitoring device being created by and for the Agency.

It was only after several months that the members of the ADEME understood the significance of this blockage which nearly sabotaged the whole project...

The agreements necessary for the operation of the device:

When the choice of device was finally agreed upon by the members of the Agency and the authorities, difficulties emerged regarding the social and technical agreements required to allocate the costs. For example, how to define the waste collection activity? How to formalise the process of waste disposal? Or, from a more technical point of view, the issue of qualifying the costs generated crucial questions: were they direct or indirect? How could they be allocated to the activities? ... Though this list is by no means exhaustive, the review of these various difficulties, led us to question afterwards how one could establish a meaningful dialogue in order to monitor the issues of societal responsibility of research. What tool could enable us to foresee certain problems and help to promote discussion between the stakeholders involved in the research project? We believe that the joint development of a Balanced Scorecard (BSC) could potentially be a way of initiating this dialogue with the various stakeholders in research.

Conceiving a management tool to help clarify a researcher's social responsibility

The Balanced Scorecard (Kaplan and Norton 1996[START_REF] Latour | L'Espoir de Pandore. Pour une version réaliste de l'activité scientifique[END_REF][START_REF] Pesqueux | Un modèle culturaliste de la RSE ?[END_REF][START_REF] Corti | Re-using archive qualitative data -Where, how, why ?[END_REF]), a scoring system regularly used to carry out strategic monitoring of an organisation's activities, would appear to be a particularly appropriate tool to address the concept of a researcher's responsibility with regard to company stakeholders. Indeed, using this tool, many researchers have demonstrated its usefulness in exploring and mastering the issues related to corporate societal responsibility (Johnson 1998[START_REF] Bieker | Toward a Substainability Balanced Scorecard[END_REF][START_REF] Figge | The Sustainability Balanced Scorecard -Linking Sustainability Management to Business Strategy[END_REF][START_REF] Zingales | Balanced Scorecard and Sustainability: examples from literature and practice[END_REF]. However, the benefit of adapting this system for research activity is not in measuring and monitoring a researcher's performance, but rather in gaining a more comprehensive appreciation of the complex functions that can be assigned to a research activity. Therefore, rather than simply implementing the tool its use should be « deviated »: with this modification the Balanced Scorecard becomes a « mediating artifact », a medium for initiating discussion on the social issues of research activity. From this observation, score indicators may be defined using the four axes of the BSC:

-Client satisfaction axis: This axis allows us to understand the medium and long-term consequences of the project for its principal stakeholders. This measure refers to how useful the device is for communities: the societal responsibility of the actors in the project here consists of constructing a device that is accepted and actually used by the members of the communities (Number of local communities using the device). It also helps to expand the evaluation of the impact of research activity on society (Number of organizations, institutions, associations participating in the steering committee).

-Shareholder satisfaction axis: As the research is funded entirely by two organizations (the University and the ADEME), the researcher should be able to explain the costs incurred in relation to the objectives that were assigned to him (Use of financial resources provided by the ADEME and the University). However, this justification should not lead the researcher to take into account only the needs of his financial backers and avoid questioning how the practices of different stakeholders might be affected by their participation in the research process (Research results presented in the documents of partner organizations). This axis also includes communication about the project made within the scientific and professional communities (Number of scientific and professional publications).

-Internal procedures axis: This axis describes the main features of the research that are generating the production of valid scientific knowledge (Number of steering committee meetings per quarter). However, the researcher must also be sure to include all of the stakeholders in the monitoring methods of the research (Number of new institutions involved in the project). In order to debate the conditions for appropriation of the research results, members of the Agency, local authorities, associations and researchers could discuss the research results (interim study reports, model proposals).

-Organizational training axis: This axis highlights the researcher's ability to adapt and react to his research topic. Within the project, this ability could be measured by the number of communities who join the project during the construction process of the device (Number of communities participating in the process), by the degree of involvement of each of the communities in the project (Number of communities having recently implemented the device) or even by the number of transformations made to the device (Number of changes observed in the device).

If this deviated use of the BSC might be likely to contribute to the emergence and ongoing monitoring of certain societal responsibility issues of management science research activity, it constitutes only a first and very imperfect step forward. For this deviation cannot escape the traditional criticisms of the BSC: the difficulty in selecting score indicators (which would not be objective nor free of the power struggles in the dialogue between stakeholders), the effective impossibility of putting into operation some of the score indicators, or even the subtle combination of certain indicators (an association that could ultimately promote research with conflicting objectives). Nevertheless, reconsidering the difficulties that may be encountered during a research intervention allows us to suggest that the construction of a BSC could help to avoid some of the misunderstandings, prevarications, surreptitious dilutions or conflicts that may arise during the course of the research.

Diagram n° 2 -Proposal for a BSC formulation

In summary, diagram n° 2 takes up the four axes of the scoring system in order to propose a model for a BSC adapted to the research project developed with the ADEME. The deviation from the Kaplan and Norton model can be used to address very effectively certain aspects of the responsibility of research activity vis-à-vis company stakeholders. This tool could also support a thorough and systematic dialogue with stakeholders in order to involve them in a co-monitoring of the societal responsibility issues of the research project, which cannot be unilaterally defined by only the researcher but which are always the result of a situated and provisional compromise... intended in practice to move the research project forward.

III. Discussion -Besides its instrumentation, the societal responsibility of research poses two new questions…

This attempt at an « instrumentation » enables us to characterise the concept of a researcher's societal responsibility as a combination of two dimensions: a professional and an institutional responsibility (see Table n° 1). Thus, besides a proposal to instrument the ongoing monitoring of the societal responsibility of the research, this third section provides a more general view of these two dimensions of responsibility for researchers in management sciences.

Client satisfaction axis

The degree of involvement of organisations, institutions or associations participating in the steering committee of the research.

The diversity of the organisations, institutions or associations participating in the steering committee. The number of local communities using the device.

Shareholder satisfaction axis

Results of the research present in the procedures of the partner organisations. Number of communication about the results of the research in academic and professional seminars.

Use of the financial resources provided by the ADEME and the University. Number of publications of the research results in academic and professional journals.

Internal procedures axis

Diversity of the topics covered each quarter by the steering committees. Diversity of the people involved in the steering committees.

Number of new institutions involved in the project

Organisational training axis

Diversity of the local authorities participating in the implantation of the device. Statistical measures of the objective of progress associated with the implementation of the device.

Number of communities having recently installed the device. Number of changes made to the device.

Professional responsibility

At the heart of his work, the researcher in management sciences is obliged to clarify his role in controlling his social experiments and the conditions for reproducing his scientific progress to produce actionable knowledge of the subject being researched. According to Bernard Schlemmer, « It is remarkable to note that the issue of a researcher's obligations is so rarely put forward for group discussion; everything takes place as if the issue did not exist or was seen strictly as an individual choice, as if the given response did not have any effect on our actual professional approach » (1998, p. 242). In fact, the researcher does not work in a social vacuum: he builds on work already recognised, through cooperation networks and through his declared affiliation to a school of thought and participates in power games between institutions that fund and justify research work. No research can claim to be responsible if it does not enforce the recommendations made by the supervisory bodies on which it depends: for example, the protocols to be applied in animal experimentation or in the use of personal data collected during research work. The researcher must therefore be aware of whether his work is in accordance with his respective scientific community and how his results might transform the methods of governing research and also transform the knowledge of citizens in everyday life. However, beyond these aspects relating to his practice, the very fact that he is a member of a profession whose independence is guaranteed by the French constitution, the researcher is morally bound to report on his research activities to the State, his employer, and also to the whole of society. The rules laid down by the professional community to which he is affiliated, allow the researcher to achieve a detached but cooperative relationship with political spheres, whether they be private or public. Edgar Morin reminds us that the scientific experience has always had an ambivalent relationship with technology and also with the political sphere, and rues the fact that: « Only a minority of scientists have perceived this link, in particular those who have grouped themselves under the Universal Movement for Scientific Responsibility (MURS) 6 (...) » (2004, p. 75). Thus, we are joined in a so-called « European » perspective in an attempt to incorporate societal responsibility within the principles that guide the activity of researchers [START_REF] Pesqueux | Un modèle culturaliste de la RSE ?[END_REF].

Institutional responsibility

Can the management researcher ignore the fact that business practices in general outpace the rules of law, which today enables certain transnational corporations to act with impunity in the absence of an international criminal law that remains to be devised and implemented? [START_REF] Bourdon | Face aux crimes du marché, quelles armes juridiques pour le citoyen ?[END_REF]. The Grenelle Environment Forum, the Bioethics Committees, the debates organized by the OECD and the commissions set up by the European Union to organize the public debate on controversial scientific advances, are many examples where the societal responsibility of research activity is in play. Through the new knowledge that it brings, the societal responsibility of research activity is likely to lead to changes in the fundamental concepts of law and policy that aim to control certain societal risks. Thus, laws, regulations, benchmarks can be imposed on organizations as a result of research that is keen to participate in democratic debate and demonstrate its usefulness to society. For example, [START_REF] Delacour | Toutes les recherches doivent-elles être menées ? Performativité, surpâturage et responsabilité du chercheur en finance[END_REF] point out how the institutional environment of researchers in finance influences the orientation of their work and favours a situation of saturation. Research advances challenge the fundamental schools of thought and systems of values on which the organization of society is based at a given time. External aspects induced by entrepreneurial activity and the actual market function (CO2 emissions and pollution, depletion of natural resources, changes in dietary habits contributing to an obesity pandemic, nanotechnology, etc.) lead to a review of the concept of wealth created by business and challenge the maximization of value created for shareholders at the expense of other stakeholders, such as government, public health insurance or pension contributions systems, etc. Edgar Morin stresses that « in these conditions it is clear that the time when value judgments do not interfere with scientific activity is over » (Morin 2004, p. 75). Management researchers are morally bound to take part in the inter-institutional adjustments between scientific, legal and political bodies that guide the purpose and the activity of business in contemporary society. Research activity can therefore explicitly claim a progressive and committed dimension, being fully aware that exploring facts from an innovative angle, its results will be likely to challenge certain conceptual boundaries, transform certain inter-institutional power struggles, and lead to the establishment of new regulatory frameworks...

Conclusion

If the activity of research in management sciences claims any social usefulness, it is that it professes to transform business practices to make them more lucid, more effective and more efficient, that is to say, sustainable and socially responsible. Re-examining a research project from this particular perspective enabled us to propose a possible instrumentationfrom a virtualisation approach 7likely to enable all the stakeholders in research to participate in the development of indicators that contribute to the clarification of a sufficiently shared axiology to guide the advancement of the knowledge project. Nevertheless, we wish to emphasize that the value of this formulation attempt is not to propose universal measure indicators but to focus more on the work they generate: the possibility of inviting -and initiating -a renewal of research practices by integrating quite explicitly the societal responsibility issues at the very heart of research activity. In addition, the indicators selected in the context of the dialogue with stakeholders for the joint development of a BSC constitute a tool that enables us to cope with the surprises that inevitably arise during the course of a research project. Indeed, as each research project is unique because of the configuration of the partners involved, the monitoring assumes creatively imagining and implementing the indicators of social responsibility issues that characterize and justify it. The fact remains that the relevance of the approach we have outlined can only be verified in practice by testing the effect of developing a BSC on the quality of the dialogue with stakeholders during the set up and progress of a new research project.



  Number of local communities using the device  Degree of involvement of organisations, institutions or associations participating in the steering committee of the research  Diversity of the organisations, institutions, associations participating in the steering committee  Internal procedures axis  Diversity of the people involved in the steering committee  Diversity of the topics dealt with during steering committee meetings per quarter  Number of new institutions progressively involved in the project Organisational training axis  Diversity of the communities participating in the implementation stage of the device  Quantified indicators for the progress expected after implementation of the device  Number of modifications made to the device Shareholder satisfaction axis  Research results present in the procedures of partner organisations  Number of scientific and professional communications / publications  Use of the financial resources provided by the ADEME and the University

Table n°1 -

 n°1 The double dimension of societal responsibility

	Professional responsibility	Institutional responsibility