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Zeta Potential Analyzer ZPA 20ZPA 20 – Zeta Potential Analyzer

The Zeta Potential Analyzer ZPA 20 uses the patented bidirectional oscillating streaming potential analysis to measure the zeta potential of fibres, powders and plate shaped solid materials. Applications that depend on the adhesion between solids, the adsorption and chemical reaction of ions/molecules, surfactants, polymers etc. can all benefit from investigating the zeta potential and its changes depending on the pH value.

Software

The ZPA 20 is controlled via the ZPASoftware. Learn more about the Software for the ZPA 20.

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                                                                                    The ZPA 20 can be used with different measuring cells for various materials. With the liquid dosing unit 
                                                                                    LDU 25 concentrations in the electrolyte can be changed automatically like e.g. the pH value. 
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The Knudsen method

The Knudsen effusion method is a dynamic gravimetric technique based on the rate of escape of vapor molecules through an orifice of known dimensions in a Knudsen cell into a vacuum at a known temperature. The rate of mass loss through the orifice is measured by the Surface Measurement Systems’ UltraBalance within the VPA system. Sample masses from 1 to 100mg can be studied typically in the temperature range from 20 to 400 °C.

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Characterization of Surface Properties of Glass Fibers by Inverse Gas Chromatography

courtesy of Surface Measurement Systems Ltd

In the present paper dispersive surface energies and specific free energies have been calculated for different modified E-glass fibre surfaces. Both different sizing and different polymer coatings have been investigated to consider changes in the surface chemistry and surface energy during different fibre treatments.

Introduction
Inverse Gas Chromatography (IGC SEA) is a wellknown technique for the characterisation of industrial and natural fibres.

A good example for the application of IGC SEA in the characterisation of natural fibres is the determination of cotton/fragrance interactions described in [ ]. The current paper is dedicated to the characterisation of industrial fibres by IGC SEA. The most common measured materials in this area are carbon and glass fibres. An extensive description of the determination of carbon fibre properties is given in [ 2].

Glass fibres are a common industrial product and used, for instance, in the production of sounda and heat-insulation materials. Another key application is a reinforcement for composites. Thus, a study of the surface chemistry of glass fibres and fibre composites holds a high level of interest.

The use of common adsorption techniques is limited for this application since glass fibres have a relatively small surface area. IGC SEA, however, provides the required sensitivity to study surface adsorption and additional physico-chemical properties.

Theory
IGC SEA pulse experiments are carried out at infinite dilution conditions. In this concentration range molecular adsorption is independent of the
surface coverage and only interactions with the highest energy sites occur. Therefore eluted peaks are symmetrical and the retention volume
can be calculated from the retention time at the peak maximum. The net retention volumes VN are computed using Equation 1.

where T is the column temperature, m the sample mass, F is the exit flow rate at 1 atm and 273.15K, tR is the retention time for the
adsorbing probe and t0 is the mobile phase holdup time (dead time). j is the James-Martin correction, which corrects the retention time for
the pressure drop in the column bed. The relation between the retention volume and free energy of sorption ΔG is given by Equation 2.

eq2

where R is the gas constant and K is a constant depending on the chosen reference state (De Boer or Kemball/Rideal) Morever ΔG is
related to the energy of adhesion WA (between probe molecule and solid) by Equation 3 (as an approximation).

eq3

where α is the cross sectional area of the adsorbate and NA the Avogadro constant. According to Fowkes [1] the dispersive
contribution of the work of adhesion WA is given by Equation 5.

eq5

with Υs D and  ΥL D as the surface tension of the adsorbent and the adsorbate respectively. Combining Equations 2, 3 and 5 leads to:

eq6

This is the most common model for the determination of the dispersive surface energy and the free energy [2].

A theoretically more rigorous approach for the determination of the free energy uses a plot of RTlnV versus the polarisation PD [3], which is
calculated according to Equation 6.

where n is the refraction index, M the molar mass and φlq the liquid density of the probe molecule.

Method
Various columns were packed with E-glass fibres provided by Johns Manville and Imperial College,London. The packing of fibres was done as
follows: a bundle of fibres, about 70 cm in length was bent in the middle. A thin metal wire was wrapped around the eye in the middle and then
pulled through a standard glass column with a 4 mm internal diameter. Both ends were cut and was bent in the middle. A thin metal wire was
wrapped around the eye in the middle and then pulled through a standard glass column with a 4mm internal diameter. Both ends were cut and
the mass of the sample could be determined by comparing the weights of the empty and filled column.

All sorption experiments were carried out on an SMS-iGC 2000. Measurements were performed with various alkanes and polar probe molecules,
all supplied by Aldrich. Prior to these measurements, the samples were pre-treated for 3 h at 373 K to remove impurities adsorbed on the surface.
For the sized fibres pre-treatment was also carried out at 313 K, 343 K and 413 K to investigate the effect of pre-treatment temperature on the results.

After the pre-treatment procedure pulse injections were performed by a 0.25 ml gas loop at 303 K.

Results
Two different sets of glass fibres were investigated. The first set represents three different E-glass fibres (Johns-Manville), one untreated and the other two sized with A1100
(silane) and A187 (silane). Surface energies and free energies have been determined. The pre-treatment temperature was also varied to study its effect on the results. This
is shown in Figure 1.

 fig1a

The graph shows that from 373 K (100 °C) onwards the change in the surface energy is relatively small. Therefore 373 K was used for all experiments as the pre-treatment temperature.
Figure 2 shows the dispersive surface energy for the first set of fibres (different sizings). The dispersive surface energy was determined by pulse injections of a row of alkanes (heptane-undecane).

fig2a

Uncoated E-glass shows the lowest surface energy (36.56 mJ/m2) while A187 (39.58 mJ/m2) and A1100 (39.39 mJ/m2) have significantly higher surface energies.
The differences between A187 and A1100 are within the experimental error margin (<3 %). 

The specific free energy of desorption was analysed using the polarisation approach [3]. As indicated in Figure 3, dichloromethane shows a similar pattern to the dispersive surface energy
whereas the other polar probes behave differently.

fig3a

Although 1-butanol, a hydrophilic acid, displays the strongest interaction with the surface it is not a very selective probe molecule in this case since its interaction doesn’t change significantly for the different samples. This indicates only a weak impact of sizing on the hydrophilic-basic sites on the surface. The interaction with DCM, however, which is hydrophobic and acidic seems to increase for both sizings. This indicates an increase in the basicity of the surface. Ethyl acetate, which is rather hydrophilic and basic and especially 1,4 dioxane (tends to be a hydrophobic and basic), show a decrease in the interaction with the surface after the sizing for the A1100 while the interaction with A187 seems to remain almost unchanged. This suggests again an increase in the basicity with sizing, especially in the case of the A1100. This agrees with the statement of Osmont and Schreiber [4] that bare E-glass fibres have a mildly acid character while sizing, especially with amino agents, makes the surface rather basic.


The second set of fibres consists of seven different E-glass fibres (Owens-Corning), one sized with A1100 and the others sized with A1100 and coated with different polymers as indicated in Table 1

 Similarly to the surface energies, the coating causes an increase in the interaction with all polar probes. The exception is again the 3265, where values are nearly unchanged compared to the uncoated E-glass. Ethanol shows even a decrease in the interaction. Apparently the polyvinyl-acetate-ethylene coating has no significant impact on the acid-base interaction. The only considerable effect is a small increase in

the hydrophobicity which explains the small raise in the toluene values and the slight decrease in the acetone and ethanol numbers.
Ethyl acetate and acetone tend to behave hydrophilic and basic while ethanol is rather hydrohilic and acidic. However, all three probe molecules can also behave amphoterically under certain circumstances, making the interpretation more difficult. Nevertheless, it can be clearly seen that 40366 shows the biggest increase in the free energies for all probe molecules. In particular, the interaction with ethanol increases significantly, indicating a rather basic surface. In fact, 40366 represents a pure PMMA coating, which is known to be Lewis-basic [4]. Sample 71446 and 71482 are blends consisting of PS and PMMA. The free energies of both samples show a significant increase with acidic and basic probe molecules.

The increase of the acidity is very interesting since PS is considered to be basic. However, it is well know that blends can show properties different to those of their individual components. This might also explain the particularly enhanced dispersive surface energies.

Conclusion
IGC SEA was shown to be a useful tool for the characterization of surface properties of different sized and different polymer coated fibres. The acid-base measurements in particular provide a unique view of changes in the surface chemistry related to the different manufacturing processes. A consideration of the surface heterogeneity, by varying the concentration of the probe molecule, could complete the obtained picture.
Acknowledgement:
SMS would like to acknowledge the contributions of Frank Thielmann, Simone Reutenauer and Asa Barbar towards this paper and Dr. Jon Bauer at Johns Manville Inc., Denver, USA for supplying the sized fibres and for his helpful suggestions.


References
[1] Fowkes, F.M., Ind. Eng. Chem. 56 (1964), 40.
[2] Dorris, G.M. and Gray, D.G., J. Coll. Interf. Sci. 77 (1980), 353.
[3] Dong, S. et al, Chromatographia 28 (1989), 469.
[4] Osmont, E. and Schreiber, H.P., in “Inverse Gas Chromatography”, Chapter 17, edited by Lloyd, D.R., Ward, T.C. and Schreiber, H.P., ACS Symposium Series 391 (1989).
[5] Dorris, G.M. and Gray, D.G., J. Coll. Interf. Sci. 77 (1980), 353.
[6] Dong, S. et al, Chromatographia 28 (1989), 469.
[7] Osmont, E. and Schreiber, H.P., in “Inverse Gas Chromatography”, Chapter 17, edited by Lloyd, D.R., Ward, T.C. and Schreiber, H.P., ACS Symposium Series 391 (1989).

Determination surface energy of Paracetamol by inverse gas chromatography (IGC-SEA)

courtesy of Surface Measurement Systems Ltd

The surface energy is a useful parameter describing the energetic properties of the surface of a solid sample. It can be determined in a fast and accurate way by IGC SEA. This paper describes the measurement of the dispersive component of the surface energy of Paracetamol.

Introduction
The surface energy is an important parameter for the characterisation of surface properties. It can provide a useful picture of the energetic situation on the surface and shows therefore a strong dependency on various macroscopic properties. For instance the dispersive component of the surface energy is a useful tool to follow changes on oxide surfaces caused by temperature treatment [1] or to highlight batch-to-batch variations in pharmaceutical production [2].
An easy way to study such effects is the use of dynamic methods. IGC SEA is a particularly suitable technique that allows a fast and accurate determination of the surface energy, either the dispersive component or the interaction with a polar probe.
In the current study N-Acetyl-p-aminophenol is used as a model substance to measure the dispersive component of the surface energy by the elution of an alkane series in the infinite dilution range.
N-Acetyl-p-aminophenol (Acetaminophen, 4-Acetamidophenol) is the active component of the well-known drug “Paracetamol” (Figure 1).

Commercially available Paracetamol contains additional ingredients supporting the tableting of the active component. Therefore tablets were also measured for comparison under the same conditions.

Theory
In an IGC SEA pulse measurement an injection of the adsorbate is made. This pulse is transported by the carrier gas, which for the SMS-iGC SEA is helium, through the GC to the column. The amount adsorbed in the column is eluted by the carrier gas.
These measurements are carried out at infinite dilution where only very few probe molecules are available for the interaction with the surface.

For this reason only the highest energy sites on the surface are covered which provides the highest sensitivity of the measured parameters.
In the infinite dilution range peaks are symmetrical (Gaussian) and the retention volume can be calculated from the retention time at the
peak maximum. The net retention volumes V0R are computed using Equation 1.

 

where T is the column temperature, m is the sample mass, F is the exit flow rate at 1 atm and 273.15K, tR is the retention time for the adsorbing
probe and t0 is the mobile phase hold-up time (dead time). j is the James-Martin correction, which corrects the retention time for the
pressure drop in the column bed. The relation between the retention volume and free energy of sorption ΔG is given by Equation 2.

eq2

where R is the gas constant and K is a constant depending on the chosen reference state (De Boer or Kemball/Rideal) [3]. Moreover
ΔG is related to the energy of adhesion WA (between probe molecule and solid) by Equation 3 (as an approximation).

eq3

where a is the cross sectional area of the adsorbate and NA the Avogadro constant. According to Fowkes [4] WA can be split into two
terms (Equation 4):

eq4

with WAD denoting the van der Waals forces and WAS the specific, mainly polar interactions. Subsequently the retention volume is a measure
for both components. However, the measurement of polar interactions will be discussed in a later application note. In the case of dispersive interactions WA is given by Equation 5.

eq5

with γsD and γLD as the surface tension of the adsorbent and the adsorbate.

Two methods are described in literature to calculate γsD which is the dispersive component of
the solid surface energy. The method of Schultz et al [3] uses a plot of ΔG versus a (γLD)1/2 for a series
of alkanes. Combining Equations 3,4 and 5 leads to:

eq6

An alternative method is based on the value of ΔG for a series of n-alkanes [5]. This leads to the expression 

eq7

where αCH2 is the surface area of a CH2 unit (6Å2) and γCH2 is its free energy (35.6 mJ/m2).

Method
Two different columns, one with a 2 mm ID and one with a 3 mm ID, were packed with N-Acetylp-aminophenol, supplied by Sigma-Aldrich (purity
99.0%). Tablets of “Paracetamol-ratiopharm” were used from Merckle, Germany, which contained 78 wt% of N-Acetyl-p-aminophenol.
The tablets were crushed and the powder was packed in a 2 mm ID column.

All the sorption experiments were carried out on an SMS-iGC 2000. Measurements of the dispersive interaction were made with 3%
undecane, decane, nonane, octane and heptane at 303 K (all solvents from Aldrich, HPLC grade). A pretreatment was made for 1 h at 303 K, 0% RH.

Results
Figure 2 shows the surface energy plot obtained from a measurement on a 3 mm column at 30°C.

graph1

The calculation of the surface energy was made according to Schultz et al [3] by the SMS-iGCanalysis software (v1.1). The obtained values for all columns are listed in Table 1.
The 3 mm column was measured twice to check the reproducibility.

Table 1. Experimental obtained dispersive surface energies.

t1

The reproducibility in the same column is excellent (only 0.5% deviation). This also suggests only a small dependence on pretreatment time as well as an exclusively reversible interaction. The difference of 1 mJ/m2 (2.5% deviation) between the values of the 2 mm column and the 3 mm column shows a very good agreement between the different column sizes and packing. The value of the 2 mm column which contained the tablet powder gave a more significant difference to the others but is still in good coincidence.
The average value of all measurements on NAcetyl-p-aminophenol is 40.13 mJ/m2 compared to 33.94 mJ/m2 in the case of the tablets.
Obviously the tableting ingredients and processing significantly lower the surface energy.

Conclusion
Surface energies may be readily studied using an IGC at infinite dilution. In the particular case of 4-Acetamidophenol the dispersive component of the surface energy was determined with a good reproducibility. Paracetamol tablets showed a smaller surface energy due to the additional tableting ingredients and processing methods.

Acknowledgement:
SMS thanks Frank Thielmann and David Butler for their contributions to the Application note.

References
[1]Papier, E. and Balard, H., Chem. Mod. Surf. 3 (1990), 15
[2] Ticehurst, M.D., Rowe, R.C. and York, P., Intern. J. Pharm.111
(1994), 241
[3]Schultz, J., Lavielle, L. and Martin, C., J. Adhesion 23 (1987), 45
[4]Fowkes, F.M., Ind. Eng. Chem. 56 (1964), 40
[5]Dorris, G.M. and Gray, D.G., J. Coll. Interf. Sci. 77 (1980), 353

Inverse Gas Chromatography-Surface Energy Analysis (iGC-SEA)

Inverse Gas Chromatography (iGC) is a gas-solid technique for characterizing surface and bulk properties of powders, particulates, fibers, films and semi solids.

A series of vapor pulses are injected through a column packed with the sample of interest. Unlike traditional analytical gas chromatography, iGC is a physical chemistry technique using vapor probes with known properties to characterize the unknown surface/ bulk properties of the solid sample.

Founding Principle of iGC-SEA

 iGC

 An experiment consists of a series of vapor pulses or frontal injections eluting through a column packed with the sample under examination. 

A pulse of constant concentration of gas is then injected down the column at a fixed carrier gas flow rate, and the time taken for the pulse or concentration front to elute down the column is measured by a detector. A series of IGC measurements with different gas phase probe molecules then allows access to a wide range of phyisco-chemical properties of the solid sample.

The injected gas molecules passing over the material adsorb on the surface with a partition coefficient KS:

Ks = Vn / Ws

Where VN is the net retention volume – the volume of carrier gas required to elute the injection through the column, and WS is the mass of the sample. VN is a measure of how strongly the probe gas interacts with the solid sample and is the fundamental data obtained from an IGC experiment; from it a wide range of surface and bulk properties can be calculated.

iGC- SEA or Inverse Gas Chromatography-Surface Energy Analyzer

It is an instrument that uses the iGC principle. The heart of its innovation is the patented injection manifold system which generates accurate solvent pulse sizes across a large concentration range, resulting in isotherms at unprecedented high and low sample surface coverages. This allows for the accurate determination of surface energy heterogeneity distributions. The fully automated iGC-SEA can be operated at different solvent vapor, flow rate, temperature, humidity and column conditions.

iGC-SEA has a unique data analysis software called Cirrus Plus, specifically designed to measure surface energy heterogeneity, isotherm properties and related physical characterization parameters. Further, bulk solid property experiments resulting from probe-bulk interaction and using solubility theory are now possible. It automatically and directly provides a wide range of surface and bulk properties of the solid samples and gives more accurate and reliable data than manual calculations. It also has a humidity control option. The impact of humidity and temperature can be determined for the physicochemical properties of solids such as moisture induced Tg, BET specific surface area, surface energy, wettability, adhesion and cohesion. Read product information or request application notes.

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Inverse Gas Chromatography-Surface Energy Analyzer (IGC-SEA)

 

      

Brochure

IGC-SEA

The Inverse Gas Chromatography-Surface Energy Analyzer or iGC-SEA continues Surface Measurement Systems’ pioneering history with inverse gas chromatography (IGC), which now spans more than fifteen years.

The iGC-SEA is a second generation Inverse Gas Chromatography instrument. It is the world’s only commercial instrument based on the IGC principle. The unique SMS injection scheme provides a wide range of injection concentrations with unrivalled accuracy and reproducibility.

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What is IGC-SEA ?
Surface energy of paracetamol
Charactersation of glass fibers 
Tg of maltose by IGC SEA
Sorbtion of microporous materials
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Lasair III                                                                 ISO 14644-1:2015 Revision Summary 

Sensitivity range: 0.3 - 25.0 µm

Sets the standard for portable aerosol particle counters and meets the requirements of ISO 14644-1:2015 and  ISO 21501-4.

The Lasair® III Aerosol Particle Counter is designed for cleanrooms with your unique needs in mind. It sets the standard for portable aerosol particle counters in highly regulated environments, so you can make sure your environment is clean.

It can be used for both remote and mobile routine cleanroom monitoring. We know the requirements and we’ve done the calculations for you; cleanroom certification results are available through a local printout, downloadable via USB in a secure format, or through the use of external software packages, such as DataAnalyst

Power is provided to the unit through the use of the on-board, hot-swappable batteries. Power can also be provided through the use of an external AC power source, which can simultaneously power the unit and charge the on-board batteries.

The Lasair III Particle Counter accepts inputs from a wide range of environmental sensors through the four built-in 4-20 mA inputs. Wireless network communications are made easy with an externally mounted wireless adapter, simplifying communications with network systems.                                                

 

 

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