Towards recycling of challenging waste fractions: Identifying flame retardants in plastics with optical spectroscopic techniques.

The use of plastics is rapidly rising around the world causing a major challenge for recycling. Lately, a lot of emphasis has been put on recycling of packaging plastics, but, in addition, there are high volume domains with low recycling rate such as automotive, building and construction, and electric and electronic equipment. Waste plastics from these domains often contain additives that restrict their recycling due to the hazardousness and challenges they bring to chemical and mechanical recycling. As such, the first step for enabling the reuse of these fractions is the identification of these additives in the waste plastics. This study compares the ability of different optical spectroscopy technologies to detect two different plastic additives, fire retardants ammonium polyphosphate and aluminium trihydrate, inside polypropylene plastic matrix. The detection techniques near-infrared (NIR), Fourier-transform infrared (FTIR) and Raman spectroscopy as well as hyperspectral imaging (HSI) in the short-wavelength infrared (SWIR) and mid-wavelength infrared (MWIR) range were evaluated. The results indicate that Raman, NIR and SWIR HSI have the potential to detect these additives inside the plastic matrix even at relatively low concentrations. As such, utilising these methods has the possibility to facilitate sorting and recycling of as of yet unused plastic waste streams, although more research is needed in applying them in actual waste sorting facilities.

Validation of a multipoint near-infrared spectroscopy method for in-line moisture content analysis during freeze-drying.

This study assessed the validity of a multipoint near-infrared (NIR) spectroscopy method for in-line moisture content analysis during a freeze-drying process. It is known that the moisture content affects the stability of a freeze-dried product and hence it is a major critical quality attribute. Therefore assessment of the validity of an analytical method for moisture content determination is vital to ensure the quality of the final product. An aqueous sucrose solution was used as the model formulation of the study. The NIR spectra were calibrated to the moisture content using partial least squares (PLS) regression with coulometric Karl Fischer (KF) titration as the reference method. Different spectral preprocessing methods were compared for the PLS models. A calibration model transfer protocol was established to enable the use of the method in the multipoint mode. The accuracy profile was used as a decision tool to determine the validity of the method. The final PLS model, in which NIR spectra were preprocessed with standard normal variate transformation (SNV), resulted in low root mean square error of prediction value of 0.04%-m/v, i.e. evidence of sufficient overall accuracy of the model. The validation results revealed that the accuracy of the model was acceptable within the moisture content range 0.16-0.70%-m/v that is specific for the latter stages of the freeze-drying process. In addition, the results demonstrated the method's reliable in-process performance and robustness. Thus, the multipoint NIR spectroscopy method was proved capable of providing in-line evaluation of moisture content and it is readily available for use in laboratory scale freeze-drying research and development.

In-line multipoint near-infrared spectroscopy for moisture content quantification during freeze-drying.

During the past decade, near-infrared (NIR) spectroscopy has been applied for in-line moisture content quantification during a freeze-drying process. However, NIR has been used as a single-vial technique and thus is not representative of the entire batch. This has been considered as one of the main barriers for NIR spectroscopy becoming widely used in process analytical technology (PAT) for freeze-drying. Clearly it would be essential to monitor samples that reliably represent the whole batch. The present study evaluated multipoint NIR spectroscopy for in-line moisture content quantification during a freeze-drying process. Aqueous sucrose solutions were used as model formulations. NIR data was calibrated to predict the moisture content using partial least-squares (PLS) regression with Karl Fischer titration being used as a reference method. PLS calibrations resulted in root-mean-square error of prediction (RMSEP) values lower than 0.13%. Three noncontact, diffuse reflectance NIR probe heads were positioned on the freeze-dryer shelf to measure the moisture content in a noninvasive manner, through the side of the glass vials. The results showed that the detection of unequal sublimation rates within a freeze-dryer shelf was possible with the multipoint NIR system in use. Furthermore, in-line moisture content quantification was reliable especially toward the end of the process. These findings indicate that the use of multipoint NIR spectroscopy can achieve representative quantification of moisture content and hence a drying end point determination to a desired residual moisture level.

Continuous direct tablet compression: effects of impeller rotation rate, total feed rate and drug content on the tablet properties and drug release.

CONTEXT: Continuous processing is becoming popular in the pharmaceutical industry for its cost and quality advantages. OBJECTIVE: This study evaluated the mechanical properties, uniformity of dosage units and drug release from the tablets prepared by continuous direct compression process. MATERIALS AND METHODS: The tablet formulations consisted of acetaminophen (3-30% (w/w)) pre-blended with 0.25% (w/w) colloidal silicon dioxide, microcrystalline cellulose (69-96% (w/w)) and magnesium stearate (1% (w/w)). The continuous tableting line consisted of three loss-in-weight feeders and a convective continuous mixer and a rotary tablet press. The process continued for 8 min and steady state was reached within 5 min. The effects of acetaminophen content, impeller rotation rate (39-254 rpm) and total feed rate (15 and 20 kg/h) on tablet properties were examined. RESULTS AND DISCUSSION: All the tablets complied with the friability requirements of European Pharmacopoeia and rapidly released acetaminophen. However, the relative standard deviation of acetaminophen content (10% (w/w)) increased with an increase in impeller rotation rate at a constant total feed rate (20 kg/h). A compression force of 12 kN tended to result in greater tablet hardness and subsequently a slower initial acetaminophen release from tablets when compared with those made with the compression force of about 8 kN. CONCLUSIONS: In conclusion, tablets could be successfully prepared by a continuous direct compression process and process conditions affected to some extent tablet properties.