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Understanding Hydrodynamic "J" type CCC

But first: Your safety

Scale-Up

ALL Quattro CCC™ / HPLLC™ are modular

Why utilise a Planetary Motion?

"G" Force calculation

Understanding importance of Beta Values

Value relates to things other than analysis time

Ask for predictable scale-up guarantees

Why do I not feel "G" force fluctuations?

Why does a planetary centrifuge work?

How is one phase of biphasic liquid retained?

Dr Ito, at NIH, Bethesda, USA

Is liquid - liquid chromatography radically different from solid - liquid chromatography?
AECS - QuidkPrep
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Understanding CCC/HPL-LC
Planetary Motion of Quattro "J" Type Hydrodynamic CCC / Inter-compatibility / Scale-Up

You will note that the motion in a Quattro "J" type is a PLANETARY MOTION.

That is the bobbin rotates on its own axis as it is rotating around the central axis.

The Earth does this as it rotates around the Sun.

One different CCC concept would be the Moon Motion Hydrodynamic CCC, where the bobbin will not rotate on its own axis as it rotates around the central axis. From historic literature these are usually suggested to be far inferior with respect to retaining stationary phase, or achieving resolution of certain targets, for many biphasic systems. We have ourselves compared moon to planetary designs, and confirmed the historic text results for many biphasic solvents.

Please note that there are over 60 fundamentally different CCC concepts, if you consider both Hydrodynamic CCC and the radically different concepts encompassed by the phrase, Hydrostatic CCC.

Very many design concepts are totally incompatible with alternative design concepts with respect to both their biphasic solvent choice and their resolving power.

Methodologies developed on one concept will often not transfer to a different concept.

Even within a single design concept, changing key design parameters, can for certain biphasic solvent systems, when combined with certain targets, cause methodologies to not transfer from one "J" type to another "J" type. In certain cases this occurs for one droplet CPC (Note; sun or centrifugal partition, droplet CPC, HPCPC are only one family group version of Hydrostatic CCC) to another droplet CPC design as well. This may mean that users will not achieve comparable efficiency of resolution between the different CPC designs (see literature).
COUNTER CURRENT & CENTRIFUGAL PARTITION CHROMATOGRAPHY, PLUS HPLC, IL-LC AND SFC
Together AECS-QuikPrep (UK) and Couturier (France) bring you World Leading products for
High Performance Liquid-Liquid Chromatography™ at scales from micro-gram to tonnes per annum
Let us help you to better understand operation of a "J" Type Hydrodynamic CCC, and also how Quattro HPL-LC™ compares to other CCC/CPC designs

Please watch video closely. It can be replayed by clicking on green button.

Please Note: The Quattro HPL-LC™ "Set Speed", once at dialled speed, is very constant. The judder in video is an artefact of camera and Internet technologies.
Quattro HPL-LC™ / HTPrep™ Video
(2 bobbins, 4 coils / 3 coil id’s). Door safety mechanism disabled for this demonstration video. Set spin speeds are very constant. The video judder is caused by camera/internet technology.
UNDERSTANDING HYDRODYNAMIC "J" TYPE CCC
But first: Your safety

For this demonstration we have over-ridden the door interlock safety, which would normally prevent rotation when the door is open. The door interlock not only enhances your safety, but it is a legal requirement in Europe to meet stringent EEC Safety Laws. Instruments without adequately strong door interlock or adequately safe, "Safety Cabinet Enclosures" built to contain appropriate centrifuge hazard, cannot legally be used in the EEC. It is both an offence to sell such devices, and also to use them in the EEC if now purchasing as new units. The USA has somewhat similar standards. Other Countries vary regarding legislation, but you should always consider your own safety, as not all manufacturers do.

We do, others don't.

Independent risk assessment engineers have been consulted by AECS-QuikPrep Ltd to ensure we met EEC standards for a planetary centrifuge
(much more stringent requirements than your standard bench, sun centrifuge), and they have confirmed the suitability and in fact the requirement of the equivalence of our 10 mm thick casework, massive hinges and door interlock. Other units sold in Europe have far less robust designs, and we will leave it to you to assess competitor's units' fitness for purpose. Your own safety experts should review the suitability of any unit with thin mild steel casework for a planet centrifuge, but be aware we consider them inappropriate, and unsuitable for use in Europe. Please also note our case design gives exception access to rotor chamber when the door is open, compared to other design.

The above is why ALL QUATTRO CCC™ / HPLLC™ ARE MODULAR from Mk IV onwards, and all share the same fundamental design parameters, with only coil id / chamber size normally varying between models.

Please Note; for a Quattro CCC™ / HPL-LC™ a simple generic methodology strategy is supplied, which will allow clients unfamiliar with L-LC to rapidly develop methods for their Quattro HPL-LC™ instrument.

Some competitors will not make you aware of the potential of non-transfer of methodologies between different concepts.

Certain competitors quite intentionally even try to play down the significance of this, by only showing limited ranges of target compound and solvent systems. This situation might apply to say Pharmaceutical companies utilising a very limited polarity range / backbone structure type of target, but would not be appropriate for anyone contemplating using a wide range of backbone structures or biphasic solvents.

Please be careful you are not fooled by inappropriately presented, publications or commercial marketing, as certain Research Institutes are publishing in CCC / CPC where the Institute and/or staff also have commercial interests in certain competitor's CCC / HPCCC / CPC / HPCPC designs. Possibly this has encouraged some bias in apparently academic publications? We will leave you to decide. This is often more of a problem with Industrial Scale-Up, rather than in routine laboratory situations, but may occur in all situations.
ALL QUATTRO CCC™ / HPLLC™ ARE MODULAR
We should all marvel at the thought process of Dr Ito, at NIH, Bethesda, USA who well over 30 years ago first rationalised, designed and made both design and chemistry work for so many of the modern day CCC & CPC concepts, including the "J" type.
Please click this link to read our Liquid-Liquid Chromatography / CCC / CPC Review Article

Click on either thumbnail of the Quattro CCC (above) or one of the two Partitron HPCPC brochures (below) to read full brochure content.


We stress that the complexity of interpretations of "G" Force calculations and defining the mathematics of mixing / settling cycles in a "J" Type is surprisingly still open to considerable debate.

Certain Academic Institutes and their related commercial puppet companies claim their calculations are correct as adamantly as others dispute their calculations, or they alternatively ignore each other. We will reserve judgement on this matter, but will agree that all "J" Type create a fluctuating "G" field, with the highest "G" often in the 70 to 350+ "G" range.

Videoing biphasic solvents inside "J" type planetary centrifuges have shown visibly that the fluctuation in "G" field will cause mixing and settling cycles in a "J" type CCC. These videos also show that the Beta Value (Ratio of Sun to Planet Radius) is critical.

"G" Force calculation plus full understanding of mixing / settling calculation still under debate, do not believe anyone who says otherwise.
Please remember that anything that increases your safety risk or the unit's build cost, such as increasing speed for a unit with a sun / beta value of a Quattro CCC™ / HPLLC™ above 900 rpm to achieve "240 G"; be that a Quattro HPLLC™ (High or Ultra "G" unit) or competitor's middle sized, HPCCC, has to be justifiable.

With bores of less than 1mm it is justifiable, because small bores require high "G". We agree with this requirement.

With bores of 1.6 mm or more, the timesaving of HPCCC are often very much less than portrayed by bias competitor's claims.

Please be careful to always compare same bores, when assessing flow rates. In CCC / L-LC as in HPLC, it is linear flow rate that is maintained, and this relates to bore id. We are aware competitors' comparing our 2.1mm or less than 4 mm id on our historic models to their 4 mm bore on their current models. This is totally inappropriate marketing.

The costs of necessary safety features, additional solvent costs and inconvenience of using two flows into two bobbins to match weights for 200 ml + units, to prevent out of balance, all weigh against over 900 rpm in HPCCC units with close to Quattro CCC™ / HPLLC™ sized sun / planet radii.

Please note, with competitor's mini units, with cotton reel sized sun / planet assemblies, 2000+ rpm is required to achieve same "G" as a Quattro CCC™ / HPLLC™ at ~ 900 - 1250 rpm.

A key criterion for you to consider is, does the higher speed required for "240+ G" increase cost of HPCCC for given volume? It usually does quite significantly. If so, this means that competitor's or a Quattro HPCCC requires you to purchase a smaller volume unit per equivalent price.

This can be a false economy. You may need to do four to six + separate injections on a small volume mini competitor HPCCC unit to equal the mass loading on an IntroPrep™.

The IntroPrep™ is already considerably cheaper, and has four + times the volume / mass loading. If the mini is twice as fast per cost, but has a quarter to sixth mass loading, it is very significantly inferior in mass per time usage / at given price. In fact certain smaller volume competitors units are closer to the price of the QuikPrep™, which has up to 14 times the competitors HPCCC volume.

The above is WORTH YOU THINKING ABOUT?

Quattro CCC™ / HPLLC™ offer you competitive pricing, options of PTFE or Stainless Steel etc coil material, large volume per price equivalence, custom choice of coil material / bore and number of coils, option of up to 4 different volume coils, with potentially all of different bore id. Their reliability has been proven in use around the World. They are designed for ease of use and quick maintenance. They have proven flying lead life of very many years for numerous users (excluding client induced accidental precipitation blockages). Quattro CCC™ / HPLLC™ have enhanced user safety features with standard unit, plus option of additional safety features. All mark out the Quattro CCC™ / HPLLC™ as World Leaders in CCC / HPCCC / CPC / HPCPC / HPLLC™ / HPLLE™.

Compare our prices, unit for unit, volume for volume, they are the best in the World on a price / performance / safety / convenience of use / routine maintenance criteria
ALWAYS REMEMBER THAT VALUE RELATES TO THINGS OTHER THAN ANALSIS TIME.
The Earth is a planetary system, why do I not feel these big "G" force fluctuations, as I live on a planet?

The answer relates to the Beta Value, that is the ratio of the planetary radius to the ratio of sun radius. The radius of the Earth is very, very small, compared to the distance the centre of the Earth to the centre of the Sun (that is the sun radius). As a result of the Earth's very low Beta value, the day / nighttime, that is closest Sun / furthest from Sun, are only minimally different "G" values.

The Quattro CCC™ Mk I and Mk II (all intellectual property exclusively owned by AECS-QuikPrep Ltd) of the early 1990's were the first CCC to be designed with no central sun shaft. In that way we uniquely achieved very high maximum beta values. Others use Beta Values of 0.5 or less for their minimum Beta Values. We on the majority of our designs use minimum Beta values of well over 0.6, but on some occasions our minimum Beta value is over 0.8.

Others now copy aspects of our original designs, and we have recently commissioned our legal advisors to shortly debate the legality of that with them, given their historic written legal agreements with us as. These written legal agreements were signed by both Academic Institutions and as individuals (academic staff), (now also shareholders in recently formed competitor companies)
Many novices and even some well-known users to CCC / CPC consider the science of liquid - liquid chromatography radically different chromatographically from open tubular / flash or HPLC chromatography, which is often referred to as solid - liquid chromatography.

What are AECS's views?

Dr Leslie Brown and AEC-QuikPrep Ltd believe the fundamentals of L-LC / CCC / CPC are almost exactly the same as most supposed forms of solid-liquid chromatography.

Please consider reverse phase HPLC / Flash Chromatography both of which often utilise C4 / C8 / C18 phases bonded to silica and other solid supports.

Nobody would dispute C8 is a liquid (it is after all, a major liquid constituent of petrol / gasoline).

C4 is a liquid under minimal pressure, and C18 is a wax, which liquidises easily with little heat.

Indeed the earliest texts on reverse phase HPLC referred to the science as Liquid-Liquid Chromatography (please go to the internet and search Liquid-Liquid Chromatography) and was not initially referred to as Solid-Liquid Chromatography (that misnomer has developed through muddled thinking in recent years).

Therefore any Researcher or Quality Control Chromatographer who has utilised Reverse Phase HPLC is already practising Liquid-Liquid Chromatographer.

Recently research ever more increasingly suggests that polar solvent enriched boundary layers in HPLC phase use can occur in both reverse and normal phase HPLC.

It is now being recognised that partitioning occurs between the bulk liquid and the polar solvent enriched boundary layer as a first selectivity occurrence. Only after this interaction will selectivity occur between the liquid phase immobilised on the solid surface and the target. At AECS, we are chromatographers with many decades of research experience in the design of HPLC phases (see our website www.chiral-hplc.com ). We keep aware of all advances in HPLC phase technologies as well as Liquid - Liquid Chromatography / Extraction.

If you consider aqueous reverse phase, aqueous normal phase, HILIC and even normal phase where a polar solvent constitutes part of the mobile phase, then HPLC users are themselves every day already doing High Performance Liquid-Liquid Chromatography™.

This is why we do not teach our clients the use of "suck it and see, set ratio, Witch's Brew approach" to method development such as HEWAT etc that all our competitor's teach.

We teach them chromatographic optimisation principles for their HPL-LC™.

The only difference between HPLC and HPL-LC™ is in HPLC a chemical bond is used to immobilise the liquid stationary phase, and in the Quattro HPL-LC™ a electro-mechanical instrument immobilises one phase in a biphasic mixture.

This is why we believe it is essential to teach our clients' the fundamental chromatography principles behind biphasic solvent choice and do not, as do our competitors' suggest they brew up their selection from a range of fixed solvent ratios that you chose from their pre-described list, which may or often, does not work.

We treat you as thinking researchers and chemists, not as burger bar cooks following a simple recipe.

We hope you will prefer our more scientific approach.
Please consider visiting our NEW DEMONSTRATION LABORATORY near Newquay Airport, only 1 hour flight from London Gatwick, and with good connections to many National & International Airports.

Please consider requesting Dr Leslie Brown visiting you to discuss your larger scale process needs.


If you are interested in collaborative research, please suggest a topic. We are particularly interested in high pressure SFE / SFC / SFC-MS / L-LC direct to MS applications, but have a general interest in many subjects from trace to process quantities.

During each rotation of the bobbin on its own planetary axis, in the Quattro CCC / HPLLC, a single point in the tube will twice for every revolution around the sun axis, be close to the central axis and twice close to the furthest point from the central axis.

When furthest from central axis it will experience maximum "G" Force. When closest to central axis it will experience minimum "G" Force. These "G" force differences are very considerable, and will induce alternately, near instantaneous mixing and then settling of the chosen biphasic solvent.

This would be analogous to doing not 1 to 3 separations in a standard laboratory-separating funnel, but instead using the instrument to do 100,000+ such mixing / settling cycles per hour.

This is why targets can be resolved which have very similar Partition Coefficients (K).

In a separating funnel targets with near 1 value for K would never be resolved.

In a CCC/CPC the optimum range of separation is between the K ranges of 0.5 to 2.

A Partition Coefficient of 1 should elute in 1 coil volume.

Relatively simple test tube partition/settling tests will in over 80% of cases mean K value resolution, as predicted from test tube partition/settling time tests, will be achieved with instrumentation.

Some exceptions will occur. Contact us to discuss.
Why utilise a Planetary Motion?
At low Beta values, little mixing settling occurs.

The Quattro CCC™ / HPLLC™ has depending on coil configuration chosen, the highest Beta Values ever available.

These mixing and settling cycles will happen very quickly. At 900 rpm they are occurring 1800 times per minute. Routinely for safety and to ensure long life, whilst maintaining sensible costs, most Quattro CCC™ / HPLLC™ rotate at approximately 900 rpm. But models are available with 1250 rpm or even up to 2000 rpm as customer need for their application. We have experience of 240 "G" (equivalent competitor's HPCCC, and uniquely to us 350+ "G" HPCCC).

We do not agree with statements regarding High "G" applicability as seen in published or commercial literature (Note, these are often same research group), except in certain limited biphasic solvent systems / specific target types.

Our custom Quattro High "G" units have the highest "G" values ever available in HPCCC.

Therefore from our own experience, which dates right back to our late 1990's experimentation with High "G" whilst collaborating on a BBSRC joint research programme with Brunel University (BIB) etc, we do agree with certain competitors that High "G", above 100 "G," such as 240 "G" is essential for 0.8 mm and 0.5mm bores. But we also believe for larger bores, 240 G may not even be appropriate for most laboratories, if cost/benefit criteria are examined.

Excessive component wear caused by the intrinsic out of balance forces of a "J" Type Planetary HPCCC make high volume, and therefore high spun mass bobbins of over 6 litres potentially commercially suspect for long-term, routine process usage, even at 70 to 140 "G".

For 24/7/365 process usage, a high spun bobbin mass, high volume "J" Type, HPCCC (240 G) of over 6 litres capacity is in our opinion close to commercial insanity. Certain others having seen academic prototypes operational, agree with us. We believe you would be ill advised to chose such a unit.
But if you do, please ensure your warranty with regards to scale-up success and usage reliablity is extremely effective.

We have experience of both HPCCC and HPCPC and consider it would be better for you to buy an intrinsically balanced, sun centrifuge, HPCPC for over 6 litre capacities. Ideally we would recommend a HPCPC with one or more, modular, 25 litre per rotor(s), such as the Partitron HPCPC (uniquely available with a titanium rotor).


Understanding importance of Beta Balues
Why not ask competitors to put their claims regarding predictable scale-up with their non-modular units, which have radically different, planet to sun radii, speed ranges, coil bore id etc into writing with some form of guarantee?

In the past they always refused to do this.

Also ask our competitors the time to change both sun and planetary bearings on their units? Then ask us? You might be shocked at how much quicker our maintenance procedures are, and how long certain of our competitor's repairs would take.

We do believe it is a fact that many aspects of your safety become excessively critical as speed increases above 900 rpm. To overcome these safety concerns does considerably increase cost of instrumentation for little practical gain in performance. It requires usage of procedures and additional safety features that have never been required in 20+ years for 900-rpm units.

We do believe that serious out of balance can occur when filling new biphasic solvent into a 300 to 1000+ml coils, once speeds are higher than 900rpm for unit of Quattro HPLLC™ planet and sun radii.

With competitors this forces clients to need to pump at same time into two different bobbins. So if you only wish to utilise say a 500 ml bobbin, you are with competitors High "G" units forced to fill both bobbins with stationary and mobile phase,
with resultant DOUBLING OF YOUR NEEDED SOLVENT COSTS WHEN USING COMPETITORS HPCCC as compared to a Quattro HPL-LC™!

We do believe that dogma and marketing hype, not practical science, has driven High 240 "G" research for most non-small bore applications (sub 1mm id are different)(with sub 1 mm bore unique mixing / settling / bore / wall boundary layer effects do force the requirement for higher "G").

In these small-bore circumstances we can offer the highest "G" available.

We will happily debate this in detail with you. Please contact us on
OK we see Planetary Centrifuge design creates impressive mixing and settling characteristics, but how is one phase of biphasic liquid retained, while other immiscible phase passes through, being alternately mixed and settled?

This one you can prove easily to yourself.

Your answer is based on the Archimedean Screw Principle.

If you fill a transparent tube half with water, leaving half filled with air, whilst blocking both ends. Tie a cord and now spin over your head. No matter which direction you spin, the water will go in the direction of the spin. This is defined as the
HEAD.

The less dense air will be displaced by the denser water and go in opposite direction from spin. This is defined as the
TAIL.

If you replaced the air with hexane, as hexane is less dense than water, the same would occur. In this scenario when utilising hexane or other less dense than water solvents, the water will still go to the Head, and other less dense organic solvents will go to the Tail.

But if you replaced the air with chloroform or dichloromethane or another solvent denser than water, now the denser organic solvent would go towards the Head and the Water towards the Tail.

If you combine all of the above, you will have rationalised the design of a "J" type hydrodynamic CCC.
Explain to me simply, why a planetary centrifuge works?

Let us consider an analogy. On the Planet Earth, consider two immiscible fluids AIR & WATER.

Take a relative flow of one phase compared to other. In this case the wind blowing air over the water's surface (with Quattro CCC™ the wind would be equivalent set flow of HPLC pump for mobile phase relative to stationary phase).

In your normal reality "G" stays the same and wind speed varies.

BUT CONSIDER IF WIND STAYED SAME AND "G" VARIED.

On Earth with 1 "G" a set, given wind speed creates 2-metre wave.

How big would wave be at 100 "G"? Yes you are correct if you suggested wave would be hardly noticeable?

How big would wave be at 0.01 "G"? Yes you are correct if you suggested air and water would instantly mix and both disappear off to space?

Hey you have almost re-invented a "J" type Hydrodynamic CCC
AECS & Couturier Personnel Pics
Pierre-Henri Garret, MD of Couturier
Dr Les Brown, MD of AECS-QuikPrep Ltd
Please click this link to read our article on the 25 litre, titanium sun rotor, Partitron HPCPC
Your 1st Choice for Preparative and Process Chromatography / Extraction
OUR NEWS BOX

AECS-QuikPrep Ltd has begun a three way collaboration with University of Belfast and UCL, London for EPSRC funded Grant Research into Unique Applications of IONIC LIQUID use in Quattro CCC and CPC.

Quattro HPCPC™ suitable for IONIC LIQUIDS, and LIQUID-CO2 applications such as possibly SFE, SFC, just released.


New Demonstration Only 6 litre ATEX, Partitron HPCPC™ Mk 2 available to view.

New Demonstration 4.5 litre non-ATEX, Quattro PilotPrep Mk 9 Available for demonstrations. Suitable for large scale preparations in standard laboratories.


Highly Specialist Titanium Multi-Dimensional Machining of 25 Litre Rotor which was designed by, and is machined by ourselves
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