Innovation, Pharma-4-0 24 April 2025

Raw material analysis: identification (RMID), verification and classification

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Raw material analysis with Visum Palm GxP™

Raw material analysis identification (RMID) is a critical process in the pharmaceutical industry because it ensures the identity and quality of all materials and substances to be used in the production process. A practical and efficient way to be able to analyse and confirm the identity of all substances is by using a Visum Palm GxP™ portable NIR analyzer, being able to perform the analysis directly in the warehouse and obtain results in less than 3 seconds, thus avoiding laboratory overload and reducing cycle times.

No single technology provides a universal solution for the manufacturer’s entire list of materials.

While NIR is particularly effective for identifying primarily organic compounds, it can also be applied to certain inorganics under specific conditions, such as when they are hygroscopic, associated with water molecules (hydrates), or dissolved in an aqueous solution.

On the other hand, Raman spectroscopy has notable limitations with:

  • Organic compounds that exhibit fluorescence (such as dyes and certain APIs).
  • Substances with inherently weak Raman signals.
  • Pure ionic inorganic compounds, such as NaCl, KCl, and HCl.
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handheld nir visum palm analyzing pharmaceutical raw material

Why Visum Palm GxP™ in raw material analysis?

  • It is a self-contained analyser and does not need to be connected or linked to any external device (smartphone, tablet or PC).
  • It has double-functionality as a hand-held and benchtop device.
  • It is useful for identification and also for quantitative methods.
  • The sample measurement area is 10 mm and the illumination area is 50 mm. This allows to acquire more chemical information and to mitigate heterogeneities.
  • It has a spectral resolution of 5 nm and 256 pixels, providing the highest spectral resolution across the entire range of portable analysers.

Figure 1: Benchtop mode with Visum Palm GxP™, allows the attachment of sample holders for powders, solids and liquids. 

CFR and GMP full compliance: 

  • Defined user roles for Analyst, Supervisor, and User Manager, with unlimited users.
  • Password expiration settings configurable according to security policies.
  • Audit Trail records stored in an encrypted binary file, along with a Results Audit Trail.
  • Two-level electronic signature system (Analyst and Supervisor).
  • Date and time settings aligned with CFR requirements.
  • Secure system backup and restoration processes.
  • IQ & OQ protocols in compliance with USP <1119>, PE 2.2.40, GMP, and GAMP 5 standards.

Analysis Modes with Visum Palm GxP™

The Visum Palm GxP™ analyzer enables fast identification or verification of various solid, granulated, powdered, or liquid compounds in just seconds. It works by comparing the acquired spectrum with the reference spectrum of substances stored in its library. This comparison is based on a mathematical similarity index (HQI), which translates spectral differences into a numerical value.

As a result, the analyzer provides the most similar class or substance (see Figure 3), followed by a ranked list of other possible matches, ordered from highest to lowest similarity.

Unlike raw material analysis identification, which is agnostic to the material, the verification mode (see Figure 4) allows the analyst to select a specific substance from the library to confirm its identity. The result is presented as PASS or FAIL. In the case of FAIL, the system also suggests the most similar substance identified during the analysis.

Main screens Visum Palm™

  Figure 2: Main Menu    Figure 3: Identification analysis    Figure 4: Verification analysis, PASS and FAIL with confirmation of correct substance.

Classification analysis - Raw material analysis

In contrast to the above, raw material analysis classification (Figure 5) is a function that allows to properly distinguish (classify) very subtle spectral differences such as particle size or concentration of a particular analyte, even if it is the same API or excipient. It is a very useful function to identify anomalies in the raw material or to perform a confirmation of the identification analysis in problematic or doubtful cases. 

In all of the above cases, in addition to the result, the spectrum of the analysed substance is obtained for each measurement (Figure 6).

raw material analysis

Figure 5: Raw material analysis classification        Figure 6: Spectrum of each measurement

Develop your bespoke libraries with Visum Master™ software - Raw material analysis

Figure 7: Visum Master™ – Main Menu        Figure 8: Visum Master™ – Develop from scratch a library or method for raw material analysis

Figure 9: Insert spectra and the reference to create the model.

The Visum Palm GxP™ is the only NIR analyzer on the market that allows end users to easily and automatically develop their own libraries for identification, classification, or even quantitative testing methodsall without requiring complex software or advanced knowledge of chemometrics.

Users simply need to import the training sample spectra and their reference values (quantitative or qualitative, as provided by the official method) into the built-in Model Builder. The software will then automatically generate the library or method, along with a technical report that includes details on the model’s construction and key performance metrics.

This report follows the criteria and recommendations outlined in ICH Q2(R2) “Validation of Analytical Procedures – Scientific Guideline”, making it suitable for internal and external validation, and helpful for identifying potential improvements or updates.

By IRIS Technology Solutions
Industry-4-0, Innovation 22 April 2025

IRIS Technology: Leading the Way in Material Detection with Hyperspectral Imaging for RECLAIM project

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IRIS Technology: Leading the Way in Material Detection with Hyperspectral Imaging

IRIS Technology Solutions, a pioneer in photonics and artificial intelligence, is playing a key role in the European RECLAIM project as leader of Work Package 3 (WP3). The company is spearheading the development of an advanced material classification system prototype based on optical and spectroscopic techniques, with the aim of revolutionizing how waste materials are identified and categorized for recycling purposes.

Cutting-Edge Detection Using Hyperspectral Imaging

At the heart of IRIS’s contribution is a prototype system built around hyperspectral imaging (HSI). This technology captures detailed spectral data for each pixel in an image, producing a three-dimensional dataset—two spatial dimensions plus a spectral dimension. Each pixel carries a unique spectral signature that reflects the chemical composition of the material it represents.

To harness this powerful technology for waste classification, IRIS has designed and assembled a linear HSI system that has been posteriorly integrated in the portable robotic Material Recovery Facilities (prMRF) developed under the RECLAIM project allowing real-time monitoring and analysis of waste materials as they move along the belt of the pilot plant. 

To ensure the maximization and quality of the spectral features of the analyzed material, various optical configurations were tested to identify the best setup for reliable spectra acquisition and consequent classification.

Advanced AI Algorithms

To interpret the massive amount of spectral data generated by the HSI system, IRIS has developed AI algorithms that analyze the chemical characteristics of materials. These models have been developed both by data collected at IRIS facilities and by real waste spectral data, to access the most representative data and ensure effective material prediction.  The development process involved creating AI models that combined the spectral and spatial information provided by the HSI system to obtain trustworthy classification outputs. To support the classification AI models development, various data treatments and advanced AI algorithms have been tested and evaluated. IRIS has tested multiple system configurations, adjusting key variables such as camera frame rates, conveyor speeds, and the distance between the camera and the conveyor, to optimize detection performance under different operational scenarios.

A Breakthrough in Material Classification

One of the most significant achievements so far is the creation of an extensive classification model that goes beyond traditional broad categories. The model distinguishes between multiple waste types with high accuracy, identifying the following classes:

  • METAL
  • PAPER
  • PET (Polyethylene Terephthalate)
  • PE (Polyethylene with concrete differentiation between the High and Low Density)
  • PP (Polypropylene)
  • PS (Polystyrene)

This is a major milestone in plastic waste sorting, marking the first time that such detailed sub-classification of plastic polymers has been integrated into an operational industrial spectroscopic sorting system. By enabling the separation of similar-looking but chemically distinct plastics, this advancement significantly improves the quality and value of recycled materials.

By IRIS Technology Solutions
Innovation 4 December 2024

Real-time monitoring of free lacticide during the production of PLA (polylactic acid)

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Monitoring of free lacticide levels during PLA (polylactic acid) production in real-time.

Reactive extrusion - REX

Reactive extrusion (REX) is a method of chemically modifying polymers during the extrusion process to improve their properties. Combining reaction and extrusion means taking advantage of the synergistic effects of shear forces and temperature to complete the reaction in less time, while the product is obtained directly in its final form.

One of the advantages of reactive extrusion is that the reactions are carried out without solvents or with a minimal amount compared to traditional batch polymerization processes. The result is a considerable reduction in costs and emissions, which makes the process more sustainable.

However, since each reactive extrusion process involves several characteristics, such as extruder geometry, screw speed, temperature profile, as well as the ratio and feed rate of the reactive species, which, in turn, are closely related to the throughput and residence time, the process is particularly complex and usually cannot be adequately modelled in terms of simple recipes or simple manufacturing rules.

Polylactic acid (PLA)

ATOM

PLA structural unit

Polylactic acid is a monomer used for the synthesis of PLA and is a bioplastic, i.e. bio-based and biodegradable, obtained from the anaerobic fermentation of renewable food sources and has numerous applications in the compostable packaging industry, its use as a filament in 3D printing and in the medical or surgical industry. It is also a rigid thermoplastic that can be semi-crystalline or fully amorphous, depending on the purity of the stereoisomer.

Visum NIR In-Line Probe™ as a control tool to monitor PLA synthesis by reactive extrusion

The use of analytical tools based on NIR spectroscopy provides a source of real-time information about what happens inside the reactive extruder during the L-lactide Ring Opening Polymerisation (ROP) process.

In this case, the most important source of information is the amount of L-lactide that has not reacted or polymerised during the process. Both the purity and the yield in terms of molecular weights as well as the mechanical and thermal properties of the product are highly dependent on the efficiency of the process.

Visum NIR In-LIne Probe™ monitoring of free lacticide

Visum NIR In-Line Probe™ monitoring PLA synthesis in ROP process

The process analyser Visum NIR In-Line Probe™  -designed, manufactured and marketed by IRIS Technology Solutions, S.L.- (Spain) has been successfully used to monitor the polycondensation reaction of lactic acid that normally takes place at temperatures above 180 °C. 

Unlike its sibling Visum NIR In-Line™ analyser, the Probe version has been specifically designed to work in even more aggressive environments using transmittance, reflectance or transflectance optical probes depending on the characteristics of the matrix to be monitored and the particular process conditions such as temperature, viscosity, pressure and explosion risk.

To monitor the reaction, a reflectance probe was used, attached to a reactor port suitably machined for this purpose.

As can be seen below, the predicted lactide concentration values have an RMSEP of 1.6% w/w when compared to the reference laboratory analysis, which is a more than acceptable uncertainty because  the typical amount of lactide remaining is between 5 and 10%. The alternative, off-line analysis by chromatography (HPLC) could involve a waiting time of about 1 day, which is not suitable for any efficient process control task. 

The ultimate goal is to optimise the residence time in the reactor: the shorter the better, as long as the concentration of remaining lactide (which has not polymerised) is kept low enough to guarantee the quality and purity of the final product. Incorrect extrusion settings result in loss of time, energy and raw materials, as the process is not reversible.

FREE_LACTICIDE_GRAPHIC

Machine learning predictive model metrics and regression lines. Grey dots represent modelling (“training”) spectra, while red dots represent validation spectra, which have not been included in the training set. Ordinates: Predicted L-lactide concentrations. Abscissae: Reference L-lactide concentrations provided by the traditional (HPLC) method.

In relation to the machine learning model, using the Model Builder of the proprietary Visum Master™ software, a non-expert user can easily create tailor-made calibrations as long as some reference spectra and the respective analyte concentrations are available. Since the Model Builder works according to AI heuristics, the best combination of mathematical pre-treatments and machine learning algorithms is found automatically without any input from the user. This means that the user could extend the applicability of the online analyser to a wider range of future applications beyond the specific case of PLA manufacturing.

In summary, since the Visum NIR In-Line Probe™ analyzer can acquire and mathematically process a representative spectrum in a fraction of a second, the entire reactive extrusion process can be automatically inspected in terms of the remaining amount of L-lactide so that the user can make real-time decisions on the updated optimal parameters.

By IRIS Technology Solutions

Innovation in industrial process control thanks to the Visum Raman In-Line™ Raman process analyzer

Raman technology has revolutionised the way industrial sectors conduct chemical analysis, enabling precise, real-time measurements without direct contact with the material. At IRIS Technology Solutions, we are proud to introduce the Visum Raman In-Line™, a robust, high-performance Raman process analyzer designed to meet the demands of modern industry and facilitate industrial process control in critical applications.

What is Raman spectroscopy?

Raman spectroscopy is an analytical technique based on the interaction of laser light with the molecules of a sample. When the laser strikes the sample, part of the light is scattered at frequencies different from that of the original laser. These frequency differences, known as Raman shifts, are unique characteristics of each molecule, allowing precise identification and quantification of compounds.

Applications of Raman technology in industry

Raman technology is widely used in sectors such as pharmaceuticals, chemicals, biotechnology, and food and beverage, where precise, real-time monitoring of various parameters is essential for optimising processes, reducing times, and standardising quality. Raman technology enables:

  • Real-time monitoring of chemical reactions.
  • Optimisation of mixing and dissolution processes.
  • Quality control of products without the need for direct contact.
  • Non-invasive analysis of the chemical composition of different matrices or products.

Raman Process Analyzer: Visum Raman In-Line™

Raman Process Analyzer Visum Raman In-Line™: Innovation and precision for in-line analysis

The Visum Raman In-Line™ analyzer from IRIS Technology Solutions stands out as a cutting-edge analytical tool specifically designed to monitor industrial processes in real time. Here are some key features of this equipment:

  • High stability laser: Equipped with a 785 nm laser, which reduces the risk of fluorescence and ensures precise measurements in various matrices, whether solid, liquid, or semi-solid.
  • High power and speed: Features a Class 4 laser with 500 mW output, allowing for better signal acquisition at different stages of the process, regardless of matrix absorption, and enabling clearer, more accurate, and faster data collection.
  • Reduced warm-up time: Unlike most industrial process Raman analyzers, the laser light source has a warm-up time of only 5 minutes.
  • In-Line integration: The compact and durable design of the Raman process analyzer Visum Raman In-Line™, with a measurement module and a safety and monitoring module, allows for direct integration into production lines using an immersion probe. Consult our team of experts for the full range of possibilities.
  • High-resolution sensors: Uses advanced sensors that provide high spectral resolution data (11 cm⁻¹) over the 150 – 3,000 cm⁻¹ range, enabling precise identification and quantification of components even at concentrations as low as 0.01 w/w.
  • Automated modelling: Our Visum Master™ software is unique in its ability to generate predictive models automatically and without expert knowledge, using a Model Builder. It also includes a version specifically for GMP, meeting all requirements of the pharmaceutical industry.
  • Full connectivity: The Visum Raman In-Line™ can communicate with PLCs or information systems on the line using protocols such as OPC, Ethernet, Modbus, Profinet, and many more. Your data, wherever and however you need it.
  • Versatility: Although exclusively designed for quantitative analysis in production lines, it can be mounted on a wheeled rack for use across different processes or in at-line applications. It includes a sampling module to analyse solids, liquids, or semi-solids in Falcon-type vials, with all necessary protections for safe and agile operation outside the line.

Why choose the Raman Process Analyzer Visum Raman In-Line™?

At IRIS Technology Solutions, we understand that precision and reliability are essential to the success of industrial processes. The Visum Raman In-Line™ raman process analyzer has been developed to the highest quality standards and is supported by our team of experts, who provide guidance and support to ensure successful implementation in any production environment.

Interested in learning more? Contact us to discover how the Visum Raman In-Line™ can enhance the efficiency and precision of your production processes.

By IRIS Technology Solutions
Innovation 9 October 2024

NIRS analysis of Brix degrees in whole apples in real time

NIRS analysis of Brix degrees
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Analysis of Brix degrees

The agri-food industry has advanced significantly in recent years through the implementation of technologies to improve quality control and the efficiency of production processes. One of the most relevant technologies in this regard is Near-Infrared Spectroscopy (NIRS). This technology has shown great potential for the non-destructive and rapid analysis of agricultural products, such as apples, allowing the measurement of a wide range of quality parameters. This paper aims to present a detailed analysis of the application of NIRS technology in the continuous analysis of whole Golden Delicious apples with a special focus on analysis of brix degrees, which is the main parameter for controlling the ripening of the fruit, as well as for its preservation and commercialization.

Traditional analysis of brix degrees in apples

The traditional method of analysis of Brix degrees of apples used in the industry is refractometry. Although it is a simple and fairly inexpensive method, it is destructive, off-line, based on random and slow sampling, making it impossible to analyse large volumes of production.

Advantages of NIRS technology

  • Non-destructive: Unlike traditional methods, NIRS does not require the destruction of the sample, allowing the fruit to be analysed in its entirety and keeping it suitable for marketing.
  • Fast: Analysis is immediate, with response times in milliseconds.
  • Multiparametric: A single NIRS analysis can provide information on several quality parameters simultaneously.
  • Reduced wastage: By identifying poor quality fruit immediately, they can be diverted before they continue in the packing process, reducing wasted resources.
  • Storage optimisation: NIRS technology can identify which fruits have the greatest storage potential, helping companies to better manage their inventories.

Brix analysis of apples with NIR spectroscopy

The following NIRS model for analysis of brix degrees was performed with 40 samples and references of the Golden Delicious apple variety. The spectra and references were obtained from 4 different points (replicates) of each apple from the calibration set with the Visum NIR In-Line™ process analyser. Finally, a digital refractometer was used to obtain the set of reference values.

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Figure 1: Brix degrees – Key Figures of Merit Visum NIR In-Line™ process analyser

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Figure 2: Samples used during model training (grey) and automatically split internal validation samples (blue).                 Figure 3: Risk of overfitting for the brix model for Golden Delicious apples.

Conclusions: NIRS analysis of Brix degrees

For the sample range of the calibration set (11.1 – 15.8 brix), an RMSEP (Root Mean Square Error of Prediction) of ±0.3 and a correlation coefficient (R2) of 0.93 were obtained with respect to the results obtained using the reference method. The Model Builder Visum Master™ software also automatically runs a spectral quality routine to eliminate spectral outliers , i.e. data that are identified outside the model field during the training phase and finally a permutation test to determine the risk of overfitting, which can be understood as the probability that the calibration performed does not respond adequately to future samples (not used during calibration). For this model the risk of overfitting was only 0.0015, demonstrating the usefulness and accuracy of the Visum NIR In-Line™ process analyser for continuous analysis on apple sorting lines.

By IRIS Technology Solutions
Innovation 7 October 2024

Water Activity Analysis in animal feed with Visum Palm™ portable NIR

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Water Activity Analysis in animal feed with Visum Palm™ portable NIR

The water content in animal feed is a critical factor in feed quality and safety. Water is not only essential for the biological functions of animals, but also plays a crucial role in feed stability during storage, preservation, microbial activity, and food safety. Moisture, or more specifically water activity (Aw), directly influences the stability of the product and the likelihood of reactions affecting its quality.

In this paper we present the analysis of water content in animal feed by real-time infrared spectroscopy with the Visum Palm™ handheld analyser property of IRIS Technology Solutions SL.

Analyse de l'activité de l'eau

Water Activity Analysis in animal feed

Water activity (Aw) is a more accurate measure than moisture content for predicting microbiological stability and feed shelf life. Water activity is defined as the ratio of the vapour pressure of water in the feed to the vapour pressure of pure water at the same temperature. It is expressed on a scale from 0 to 1, where 1 indicates the presence of pure water. 

In animal feeds, the typical Aw value is typically in the range of 0.2 to 0.7 for dry products, which allows for greater stability during storage. When the water activity is higher than 0.7, the growth of microorganisms such as moulds and pathogenic bacteria is facilitated.

Thus, keeping water activity below 0.70 is crucial to prevent microbial growth and ensure feed safety.

Water Activity Analysis in animal feed with Visum Palm™ Análisis de Actividad de Agua

Left: Resultant regression curve for Aw – calibration samples (grey) and validation samples (blue)        Right: Fisher-Pitman permutation test to determine the risk of overfitting the Aw model.

Traditional Analysis Method

The most common traditional method in the industry for measuring the water content in animal feed is oven drying. This procedure involves the following steps:

  • Feed sample: A specified amount of sample is extracted and weighed.
  • Drying: The sample is placed in an oven at a constant temperature (usually between 105°C and 110°C) for a certain period of time (usually between 2 and 4 hours).
  • Calculation of water content: At the end of drying, the sample is reweighed and the weight loss is calculated as the amount of water evaporated.

This method is widely used due to its accuracy and simplicity, although it is time-consuming, labour-intensive in terms of sampling.

Determination of water activity with NIRS in seconds

For the development of the predictive model for water activity determination, we worked closely with a Mexican pet food manufacturer. A total of 345 calibration samples in the 0.1 – 1 % Aw range were used, of which 20% were automatically separated by the Model Builder Visum Master™ software for internal validation of the NIRS method.

As the processing of the data (spectra and laboratory references) is fully automated, the software itself executes and applies the most convenient processing routine and parameterisations according to the input data. At the end, it automatically applies a permutation test to check that the resulting model is useful for analysing future samples and that it is not the product of overfitting, which is also known as overfitting risk, an indicator of confidence in the analytical method.

As a result, the model developed to predict water activity in animal feed yielded a correlation coefficient (R²) of 0.96 and an RMSEP (root mean squared error of prediction) of ± 0.04. This validates the use of the Visum Palm™ portable NIR analyser as a real-time (< 3 seconds) method to determine water activity in feed and animal feed as a much more efficient alternative to the traditional method.

Importance of Water Content Analysis for Food Safety

Controlling water content and water activity in animal feed is essential for food safety for several reasons:

  • Prevention of microbial growth: Microorganisms need free water to grow and reproduce. If moisture content and Aw are too high, this facilitates the growth of pathogens such as Salmonella, E. coli and moulds, which can cause disease in both animals and humans, as they are linked to the food chain.
  • Product preservation: A feed with controlled water activity has a longer shelf life. Microbial growth and chemical reactions that cause nutrient deterioration are minimised when Aw is in optimal ranges.
  • Toxin control: Poor management of water content can allow the appearance of fungal toxins, such as aflatoxins, which can be highly hazardous to animals and thus to the human food chain.
  • Maintenance of nutritional quality: An adequate moisture level ensures that the nutrients present in the feed remain stable. Fat oxidation and vitamin degradation are accelerated in high moisture conditions, which reduces the nutritional quality of the feed.
  • Costs and efficiency: Controlled water content reduces economic losses, as the feed will have better stability during transport and storage, reducing the risk of losses due to contamination or spoilage.

Conclusions of analysis of water activity in animal feed

Visum Palm™ handheld or laboratory analyser

 

 

Controlling water content and water activity in animal feed is vital not only to maintain the nutritional quality of the feed, but also to ensure food safety and prevent risks associated with microbial growth and contamination. 

Traditional methods of analysis such as oven drying provide essential tools to keep these factors under control but are resource and time intensive compared to water activity analysis using NIRS infrared spectroscopy.

The portable Visum Palm™ analyser is capable of predicting Aw in feed samples in less than 3 seconds with an accuracy of ± 0.04, contributing to proper management of water activity during the production process, which is key to ensuring feed quality, animal health and sustainability of food production. As a handheld or benchtop (laboratory) multiparametric analyser, it can be used simultaneously to determine moisture, fat and fibre content, to mention the most important parameters in the production of pet food, thus constituting a fundamental tool for efficient analytical and product controls, even for agri-food raw materials.

By IRIS Technology Solutions

Real-time cooking degree monitoring of gummies with Visum Raman In-Line™

Jelly sweets, also called jelly candies, jelly beans, jelly fruit candies or gummies, are a broad category of chewy jelly-based candies that have been popular around the world for more than a century and more recently also include vitamins in their recipes for the production of healthy candies.

Depending on the recipe, gummies are made from starch, pectin, gelatin, glucose syrup, sugar, water, sodium citrate, fruit and plant extracts, flavourings, colourings and other additives, all of these ingredients are mixed together and various characteristics are controlled to obtain the best taste and texture. In order to meet these requirements, a critical factor during the production of gummy dough is the degree of starch gelatinisation and therefore a critical factor is to analyse the residual starch after the cooking process.

Level of starch cooking: the gelatinisation process

To achieve the gelatinisation of the gummy mass, starch is often used, of which potato and corn starch are the most popular and are available in a width range of modifications.

Gelatinisation, or ‘cooking’, is the process by which the starch granules are subjected to the action of water and temperature, which breaks the hydrogen bonds and dissolves the granules into the candy mass. After being subjected to a subsequent depositing and drying process, the final texture and consistency of the gummy is obtained.

In the confectionery industry, gelatinisation usually takes place in continuous cooking systems

Traditional analysis

At present, there is no inline method to monitor the degree of cooking continuously during production. Although there are several methods to determine the degree of cooking, they are all based on taking samples and analysing them off-line. This technique is labor intensive and requires qualified personnel, in addition to the difficulty it poses to make decisions and be able to correct process parameters in real time and thus avoid soft gummies, with an incorrect texture or subsequent problems in the demoulding process.

One of the methods used to control the end point of the cooking process is carried out in the laboratory using the technique of counting starch granules with a polarised light microscope.

This technique consists of the visual counting of starch particles and, depending on the quantity of particles present in the sample, the analyst can determine whether the cooking has been satisfactory or whether it is necessary to modify process parameters (temperature) or extend the cooking time. If the number of starch granules in the sample is less than or equal to 10, the degree of cooking is considered to be adequate, whereas if the number is higher, the degree of cooking is considered to be insufficient.

 

Starch granules under the polarised light microscope with the area marked in red for counting.

Real-time cooking degree monitoring of gummies

A partnership for the future of the industry

IRIS Technology Solutions SL, a leading Spanish manufacturer of spectroscopy-based solutions for the control and monitoring of industrial processes, in collaboration with the Dutch manufacturer Tanis Confectionery B.V., a worldwide manufacturer of machinery for the production of gummies, have teamed up to develop a real-time method for monitoring the starch gelatinisation and thus offer an alternative, value-added solution to the entire industry. 

Within this framework of collaboration, tests have been carried out for months in the facilities of the Tanis Innovation Center (The Netherlands) using the Visum Raman In-Line™ analyser property of IRIS Technology Solutions SL

Raman spectroscopy is an analytical technique used to observe vibrational, rotational and other low-frequency modes in a system. It relies on the inelastic scattering of monochromatic light, a laser, to provide detailed information on molecular vibrations and chemical composition. Unlike NIR spectroscopy, it is particularly suitable for monitoring aqueous matrices or for determining the concentration of an analyte dissolved in water.

 

This technology is a non-invasive analytical technique that analyses in real time the product flow, in this case the gummy dough, by inserting a food grade immersion probe, capable of providing real time results of what is happening in the process with the appropriate calibration

raman in-line RAMAN_INLINE_TEST

Developing a real-time analytical method

During the test phase, different recipes based on potato starch, corn starch and with a combination of gelatin with starch were manufactured and monitored and cooked at different temperatures to obtain different degrees of starch gelatinisation during the cooking process in order to develop the cooking level prediction algorithm (adequately cooked / undercooked).

While the Visum Raman In-Line™ analyser was acquiring spectra throughout the cooking process of the different batches or recipes, samples were extracted and analysed by the reference method of visual counting using polarised light microscopy.

For the monitoring of the continuous process, the model was developed to determine two final classifications, “Adequately cooked” (≤10 starch granules) and “Undercooked” (>10 starch granules). The result obtained is the outcome of 3 consecutive analyses to confirm the degree of gelatinisation and to avoid any misclassification.

 

Left: comparison of the average pre-processed Raman spectrum of the different recipes used. Right: classification results of the model for five of the recipes. The points above the red dotted line correspond to measurements classified as adequately cooked.

Real-time cooking degree monitoring of gummies Real-time cooking degree monitoring of gummies

Conclusions

From the tests carried out, it could be concluded that the same predictive model can be used to make cooking level predictions for both corn and potato starch-based recipes.

For all batches made from both potato and corn starch the Visum Raman In-Line™ correctly classified their cooking level.

Next to the developed models it is possible to create unique models for unique candy recipes and ingredients with this inline method.

For the recipes with gelatin or modified starch that were analysed, more significant spectral differences were observed, so specific classificatory predictive models were performed for these formulations with similar validation results. 

It is therefore possible to successfully predict the cooking level of both corn and potato starch-based jelly bean dough as well as different modified gelatines with the real-time raman process analyser, a truly more efficient alternative to the traditional and current method of analysis.

Key features of the Visum Raman In-Line™ Process Analyser

  • Sensor ready for use after switch-on (no warm-up required).
  • Analyser designed to operate in industrial environments.
  • Computer and embedded operating system.
  • 785 nm laser excitation source.
  • Internal cooling system stable at -40°C.
  • IP 65-68.
  • Connection to the process via a food grade immersion probe.
  • Compatible with different communication drivers with PLC or SCADA of the plant.
  • It can be easily integrated in any position of the pipe.
  • Low-maintenance device.
  • With the Visum Master™ SMART version software, the user has an AI-supported Model Builder for developing, adjusting or updating predictive models for different recipes or formulations.

 

 

raman analyzer RENDER

Visum Raman In-Line™ process analyser

By IRIS Technology Solutions
Industry-4-0, Innovation 25 January 2024

Plastic identification, verification and classification using Visum Palm™

identificación, verificación y clasificación
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Plastic identification, verification and classification using Visum Palm™

In this article we will address the problem of classification and plastic identification using the Visum Palm™ handheld NIR analyser as an agile, real-time and non-destructive technique useful in different processes, whether in the recycling of post-industrial plastic, in the analysis and classification of post-consumer plastic, in the identification of polymeric raw materials for their industrialisation, or even in areas of research and development of new plastic.

In all these cases, near infrared spectroscopy is presented as a valuable tool used for the characterisation of plastic compared to traditional methods of analysis.

Identification and sorting is important in plastic recycling and in manufacturing when using recycled plastic, as in both cases it must be ensured that the plastic materials are as pure and clean as possible because low levels of impurities can significantly affect the quality and performance of a recycled batch.

Although there are several portable NIR analyzers on the market, it is important to consider the spectral range that the equipment works with, the size of the measurement area (spectrum acquisition) and the spectral resolution (the quality of the spectrum obtained). The new Visum Palm™ analyser has a measuring area of 10 mm diameter, operates in the spectral range 900-1700 nm with a resolution of only 3 nm (↓ nm = ↑ spectral resolution). It is a self-contained device with an embedded computer and touchscreen and therefore does not need to be connected to a computer or smartphone to work with it.

The new Visum Palm™, which includes a polymers library, allows readings and determinations to be made at the line without the need for sample preparation in less than 3 seconds. It is also possible to use it as a laboratory device as it has a support base that allows the attachment of different sample holders for the analysis of pellets, flakes or plastic up to 2 mm.

The factory library included in the analyser has the following classes: PMMA, PE, PC, PETG, EVA, PVC, PET, PU, PS, ABS, PA, PP, VIN, PLA, PBT, PMP, POMC, PPS, PVA, PPSU, EMA, PHBV, PAEK, PBAT, PBS, TPES, TPS, MABS, HIPS, MBS, SBC, PCL, PEEK, PHB, SAN, PI, PB.

Extend and develop your own library with Visum Master™

Visum Master™ is a computer software that allows the end user to create, extend and strengthen their own identification, classification and quantification methods or libraries without the need for a specialist or technical knowledge of spectroscopy, making the analyser a truly open system to meet present and future analysis needs (new polymer classes, new suppliers, etc.).

As shown below, it is possible to incorporate spectra of new samples within an existing class or to incorporate new classes and thus keep the library as robust and up-to-date as possible in order to be able to classify or identify plastic.

plastics

Plastic identification

It is a working method that allows the plastic identification analysed within the library available in the analyser. The result obtained, as can be seen below, is the type of polymer with the highest similarity and the following (from highest to lowest similarity).

Image 1: Visum Palm™ screen performing plastic identification

Plastic identification screen visum palm polymers identification

Polymer Verification

As with plastic identification, it is based on a mathematical procedure of similarity but it allows choosing a type of material to be analysed within the identification library to confirm its identity. The result of the verification analysis is PASS / FAIL. In case of a negative result (FAIL), it provides the class corresponding to the type of plastic analysed. Both cases are shown below.

polymers_identification

Plastic classification

In contrast to plastic identification analysis, classification uses machine learning algorithms to accurately analyse and classify samples that are spectrally very similar to each other, where a double check is necessary to determine the polymer class (PET/PETG, for example). Through the Visum Master™ software, the user can create his own classification libraries for the most problematic cases.

As a result of the analysis, the user obtains the corresponding class.

In conclusion, NIR spectroscopy is a very valuable and effective tool for plastic identification or classification and, although not covered in this article, it is also useful for manufacturers of plastic and new formulations to quantify blends. The open nature of the analyser through the Visum Master™ software makes the Visum Palm™ analyser an open, self-contained system that can continuously introduce new samples, spectra and generate different libraries without the need for a specialist.

By IRIS Technology Solutions
Industry-4-0, Innovation 10 October 2023

IRIS Technology Solutions at Alimentaria FoodTech 2023

FoodTech trade show
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IRIS Technology Solutions at Alimentaria FoodTech 2023

At the end of September, IRIS Technology Solutions presented at Alimentaria FoodTech trade show 2023 Barcelona the various real-time quality and process control solutions for the industry that the Catalan company manufactures and markets under the Visum® brand.

Alimentaria-FoodTech is the machinery, technology and ingredients show that integrates the food processing and preservation value chain. It is a transversal fair that serves the food and beverage production industry from raw materials to commercial distribution.

Visum® Solutions

Visum® solutions optimize and digitize quality control on different production lines. They operate on the basis of NIR, Raman, Hyperspectral and Machine Vision spectroscopy, providing real-time information for decision making and rectification of production processes. In addition, trade show participants were able to see first-hand the new Visum Palm™ handheld NIR analyser.

The new Visum Palm™ analyzer has an innovative and ergonomic design, as well as the possibility to perform analysis at any time and place without the need to connect it to any external electronic device. This is possible because it incorporates an embedded touch screen and computer, which allow all the routine functionalities of the device.

In addition, it has the Visum Master™, this software, unlike the most common modeling and calibration software on the market, with which the user has to have certain technical knowledge about chemometrics or entrust such a task to a third party.

It allows to perform calibrations in an automated and agile way only by incorporating spectra and references (quantitative or qualitative), in addition to other functionalities.

Shealthy Project

shealthy

IRIS Technology Solutions has also presented at FoodTech the European SHEALTHY project, which seeks to evaluate and develop an optimal combination of non-thermal sanitization, preservation and stabilization methods to improve safety (inactivation of pathogens and spoilage microorganisms) while preserving nutritional quality (up to 30%) and extending shelf life (up to 50%) of F&V products. By combining and modulating non-thermal technologies with minimal processing operations, SHEALTHY’s approach will finally be able to meet today’s growing consumer demand for healthy food.

By IRIS Technology Solutions
Ai, Digitalization, Industry-4-0, Innovation, Pharma-4-0 5 September 2023

New Visum Palm™ AI-assisted handheld NIR analyser

handheld nir analyser
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New Visum Palm™ AI-assisted handheld NIR analyser

IRIS Technology Solutions introduces the latest version of its Visum Palm™ portable NIR analyser to complement its Visum® range of real-time process analysers for industry.

The new Visum Palm™ is a fully portable NIR spectrophotometer that allows real-time analysis of different substances, products or mixtures, without the need for traditional laboratory and sampling techniques, allowing industry to obtain results on the spot to make decisions or correct production process parameters.

The new generation Visum Palm™ brings with it an innovative design and a radical change in the way users experience NIR technology, now assisted by AI with the Visum Master™ software, so that each manufacturer can automatically create their own predictive models or calibrations according to their control and analysis needs.

 

Design, autonomy and robustness

The Visum Palm™ handheld nir analyser offers an innovative and ergonomic design, as well as the possibility to perform analysis at any time and place without having to connect it to any external electronic device. This is possible because it incorporates an embedded touch screen and computer, which enable all the routine functionalities of the device.

The Visum Palm™ operates in the 900 to 1700 nm range, as this is the band that best combines availability of chemical information with price and technological maturity. It operates mainly in diffuse reflectance mode, for which it has specially designed and patented optics to extract as much information as possible from the sample. Specifically, it has a large illumination area (50 mm diameter) and a collection area of 10 mm. These features differentiate it from similar analysers in terms of its suitability for analysing heterogeneous samples, which is most often the case in real working conditions. In cases where heterogeneity is more evident, the device is configurable to calculate and report the average of a given number of repetitions.

The Visum Palm™ handheld NIR analyser is IP65 compliant, making it resistant to dust, moisture and water. It is also rugged enough to be carried and tested almost anywhere indoors or outdoors and even comes with a stand for desktop or tabletop use.

 

A new AI-assisted user experience

Unlike most common modelling and calibration software on the market, which requires the user to have some technical knowledge of chemometrics or entrust the task to a third party, Visum Master™ PC-based software makes NIR technology even more accessible by automating pre-processing, multivariate analysis algorithm selection and validation. This allows any user to generate models by simply inputting spectra and references (quantitative or qualitative) for routine real-time analysis to replace traditional analysis.

handheld nir analyser

The new software also allows to extend and edit pre-existing models, synchronise with the portable analyser to import spectra, export models, download measurement results, automatically generate analytical method validation reports and audit reports for GMP environments, and to check the metrological performance of the device in a guided manner when needed.

 

For industry and GMP environments

While NIR technology has a myriad of applications in numerous industries such as plastics, food, chemical, agribusiness, wood, biofuels, to mention the most relevant but not the only ones; it is for the pharmaceutical industry and GMP environments where the new Visum Palm™ device introduces significant novelties at the level of usability and functionality. It is 21 CFR Part 11 compliant, allowing the generation and display of an automatic Audit Trail report, the record of all device activity, where comments and observations can be incorporated. It also allows the user to automatically generate the analytical method validations developed and perform metrological checks of the device when required and download the results at a later date.

“NIR technology today must be easy to use and understand, and at the same time it must give the user the freedom and autonomy to exploit it to the full and facilitate their day-to-day work. Technology must be an enabler. We will continue to take further steps in terms of automation and new functionalities because we are convinced that this is the right way forward and what the industry and the people in it need”, says Oonagh Mc Nerney, Director of IRIS Technology Solutions, S.L.

 

The new Visum Palm™ handheld NIR analyser is now available here, where you can also find technical information about the device, videos and contact IRIS Technology Solutions, S.L. for a demonstration or specific enquiry.

 

By IRIS Technology Solutions