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Application hints 

Instruction Manual, Feb-17 

18

 

6.4

 

System leaks 

Telltale signs of system leaks 

Before you even see your first drip from a fitting, your system can tell you that the 
problem exists. The most common signs of system leaks are as follows: 
1. 

No flow or pressure 

2. 

Pump pressures up, but no flow 

3. 

Noisy baseline 

4. 

Baseline drift 

While all of these symptoms could also indicate problems completely unrelated to leaking 
fittings, it is always easiest to start there. Not only are fitting leaks usually easy to repair, 
they are also the least expensive part of the system that can cause problems. 

Check to make sure your tubing is seated properly 

When using finger tight fittings, the tubing must bottom out in the receiving port before 
the nut and ferrule are tightened. If a gentle tug disengages your tubing after the fittings 
have been tightened, loosen the fitting, push the tubing to the bottom of the receiving 
port, and re-tighten the fitting. 

The fitting may not be tightened enough 

Stainless steel nuts and ferrules require a wrench to tighten them, even after repeated 
use. Finger tight fittings also require a good turn; however, don’t use a wrench unless 
instructed to do so, or you may damage the fitting. 
Notice: Over tightening can cause leakage too! 

You may be using incompatible fittings 

Make sure you are using a nut and ferrule that are compatible with each other and with 
the components of your system 

Check the condition of the nut and ferrule 

After repeated use, nuts (and especially ferrules) will gradually become de-formed to the 
point of being incapable of creating the seal they were de-signed to make. Always keep 
an extra supply of all the nuts and ferrules you are using so that you can replace them 
quickly and avoid unnecessary down time. 

Check the receiving port for damage 

Sometimes a leaking connection has nothing at all to do with the nut and ferrule, but 
with the receiving port. Ports that have had stainless steel fittings swaged into them are 
especially susceptible to damage. Check the receiving port for visible burrs or scratches 
and replace if necessary. 

Evaluate chemical compatibility 

Using fittings made of material that is incompatible with your mobile phase is a sure way 
of creating leaks. 

Summary of Contents for TLC-MS INTERFACE 2

Page 1: ...INSTRUCTION MANUAL TLC MS INTERFACE 2...

Page 2: ...Maintenance and Service 10 4 1 Cleaning 10 4 2 Decontamination 10 4 3 User maintenance 11 4 4 Maintenance Data Sheet 11 4 5 Replacing of elution head 12 5 Technical data 12 6 Application hints 13 6 1...

Page 3: ...ive detergents Only authorized personnel may open the instrument Service and repair is only to be performed by trained specialists Use spare parts and consumables supplied by CAMAG only The warranty i...

Page 4: ...are kept in the equipment for a long time electrolyte leakage may occur and cause damage to the instrument Laser class 1 inside Do not look directly into the laser beam 1 2 Parts supplied Part no Desc...

Page 5: ...from HPLC pump to TLC MS interface 2 and from there to the MS Bench space Width 27 5 cm Depth 45 cm Height 30 cm Operating temperature The temperature should be within a range of 15 to 35 degrees cent...

Page 6: ...tion Manual Feb 17 5 2 4 Connection of the valve Bypass position Elution position 1 2 3 4 5 6 From LC pump Compressed air at cleaning To inline filter and LCMS Color sleeve Elution head Internal filte...

Page 7: ...this manual 3 2 Instrument Fig 2 Control elements 1 Laser cross hair on off 2 Piston up down 3 Cleaning on off 4 Screw for fixing the security cover 5 Piston with elution head 6 Positioning table 7 Le...

Page 8: ...ght of about the thickness of the plate layer When the elution head is pressed onto a foil or glass plate the cutting edge seal cuts into the adsorption layer and creates a leak free seal In bypass po...

Page 9: ...he cleaning button at least 3 times for 3 seconds The capillary from the plate to the valve and internal frit are cleaned with the help of compressed air At the same time the cleaning sledge moves und...

Page 10: ...r and ruler on the instrument table accordingly Toggle the Piston up down switch to lower the elution head onto the plate foil Switching the valve to front Elution position will start the elution An e...

Page 11: ...on a regular basis in an appropriate way assures problem free functionality over a long period A good way to perform a cleaning would be to follow the decontamination instruction outlined below 4 2 De...

Page 12: ...trument as well as the proposal for IQ OQ interval if applicable In addition it identifies parts subject to wear with the respective replacement cycle and CAMAG order number Maintenance interval Maint...

Page 13: ...blue top cover Mount the security cover Make an fake extraction to check if the elution head is properly positioned and no leaks are visible 5 Technical data General data Plate types TLC HPTLC glass...

Page 14: ...alve and port 1 directly to the MS it is recommended to bypass the UV detector cell because it is sensitive to back pressure from the TLC MS Interface 2 It is highly recommended to use an inlet filter...

Page 15: ...et a clean mass spectrum Fig 6 Flow injection analysis FIA of 1 L of 0 113 mg mL diclofenac in methanol upper curve total ion current TIC lower curve single ion monitoring SIM of the masses 296 00 297...

Page 16: ...different samples on the same plate a short band of 4 mm may be adequate For fewer samples which are to be analyzed more than once a band length of 10 to 20 mm is preferred Alternatively samples can...

Page 17: ...the smaller tubing in receiving ports normally designed for the larger 1 16 OD tubing Generally the high pressure receiving ports in most of the equipment on the market have an internal geometry supp...

Page 18: ...ry tubing into a receiving port is the method of preference unless the receiving port is specifically designed for use with the size of tubing you are using 6 3 Dead volumes One of the concerns you wi...

Page 19: ...d ferrules require a wrench to tighten them even after repeated use Finger tight fittings also require a good turn however don t use a wrench unless instructed to do so or you may damage the fitting N...

Page 20: ...54nm mark zones with a soft pencil Fig 11 Different volumes of 0 113 mg mL diclofenac in methanol 8 mm bands MS measurement Start the HPLC pump The eluent used in the presented example was 95 methanol...

Page 21: ...the process This procedure allows you to register a series of samples into one MS file Fig 12 Elution of three consecutive sample zones of diclofenac 2 4 and 10 L per 8 mm band Upper curve TIC lower...

Page 22: ...e 60 mm drying time 5 minutes Documentation CAMAG Visualizer or DigiStore 2 Documentation System at 254nm Fig 14 Separation of Paracetamol Caffeine Acetylsalicylic Acid mixture from left to right 25 g...

Page 23: ...ted manually CAMAG TLC MS Interface 2 The selected sample zone is positioned below the elution head either by means of the laser crosshairs or by means of the x y scale The elution head is lowered ont...

Page 24: ...the TIC total ion current is registered Known substances can be measured with a much higher sensitivity if only the ion of interest e g the ion with a m z of 195 1 Da in the case of caffeine In this...

Page 25: ...tion of the TIC total ion cur rent baseline shows relative high noise Lower part MS of caffeine with APCI ionization M H ion 195 1 Da is still clearly visible background noise from the plate reaches a...

Page 26: ...7 34 34 Fax 41 61 461 07 02 E Mail info camag com CAMAG Germany Bismarckstra e 27 29 D 12169 Berlin Telephone 49 30 516 55 50 Fax 49 30 795 70 73 E Mail infoberlin camag com CAMAG Scientific Inc USA 5...

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