XAM-1  Combined sampling and nir measurement device

XAM-1, a collaboration with Carl Zeiss MicroImaging GmbH and Hellma GmbH, introduces a new generation of valves combining on-line measurement
of residual solvents with solid product sampling.

Main Functions

Solids Sampling
Starting from the rest position, the plug
valve moves into the drying chamber
and collects the sample.
Then, it pulls back to the discharge position, deposits the sample into a removable container, and finally returns to the rest position.

In-line NIR spectroscopy of residual solvent
The plug has an internal cavity that houses a diffused-reflection probe, with a sapphire window on the end.
The probe is connected to a NIR spectrometer via a fiber optic cable.
This system generates real-time, quantitative analytical data corresponding to the residual solvent amount that remains in the solid, which can be used for automatic control of the drying process.
The measurements are automatic, and can be made at set intervals or continuously.

Washing
An actuated ball valve, with a pass-through hole, is positioned between the sampling valve and the drying chamber.
In the sample discharge position, the ball valve can be closed to wash the product contact surface area, preventing contamination between subsequent samples and guaranteeing the elimination of eventual crusts on the sapphire window.

Calibration
The functional integration of the solids sampling and the NIR spectroscopy measurement in the same unit allows
for a quick chemometric model on
which to base the quantitative analysis.

Features

"Intrusive" plug-type sampling valve

• Perfectly flush mounted to the internal wall of the vessel

• Linear pneumatical actuator with three positions

• The end of the plug is provided with a pocket in which solids sample is collected

• Gas purge connection helps the discharge of the solids sample into a container, attached below the discharge position

• Sampling without breaking vacuum or venting the pressure inside the vessel 

• Contact parts : AISI 316 L, HC 22 and many others 

• Gaskets: PTFE, FEP, EPDM 

• Diffused reflection NIR probe (Hellma), separated from the process by a sapphire window, internal structure made up of illuminating optical fibers (halogen light source integrated into the NIR spectrometer) and receiving optical fibers. 

• Optical fibers have an adequate length to bridge the distance between probe and NIR spectrometer. 

• NIR diode array spectrometer (Zeiss), to be placed in a safe area 

• Light source: Halogen Lamp

• Lamp drift correction:Internal reference over a second, Measuring channel

• Multiplexer:
 Shutter control, 2 channels

• Optical Sensor:
 Monolithic with a diode array technique

• Wavelength range: 960nm - 1690nm or 1350nm - 2000nm

• Number of pixel: 256

• Wavelength accuracy:
 +- 1nm

• Photometric accuracy: +- 1% reflection

• Software:
ProcessXplorer

• Main software features: Trend monitoring, integration of PLS-models (Grams® and/or Unscambler®), CFR 21 Compliance

• System Characteristics 

• Applications: Determination of residual humidity/solvent at set intervals or continuously)

• Range: 0 - 20% (humidity/residual solvent)

• Accuracy: < 0,5% (in the range from 0 - 5 %)

Advantages

• Representative sample of the solids in the vessel

• Reduction in the number of samples taken 

• Reduction in the dead time during 
the drying phase


• Technical implementation of the PAT 
(Process Analytical Technology) control for 
the optimization of the drying process 

• Reduction in operator exposure and in 
product contamination 

• Pilot trials to test the suitability 
of the applications