LimsPulse
TROUBLESHOOTING FINDER

Something wrong with an instrument?

Describe the symptom and see the likely causes and what to do — 358 problems across 72 instruments.

358 of 358 problems

  • HPLCHigh back-pressure
    Likely causes
    • • Blocked column frit or guard column
    • • Precipitated buffer in tubing
    • • Blocked in-line filter
    What to do
    • • Replace the guard column or in-line filter
    • • Back-flush the column if the supplier allows
    • • Flush the system with warm water to dissolve buffer salts
  • HPLCPressure fluctuating
    Likely causes
    • • Air bubble in the pump head
    • • Faulty or dirty check valve
    • • Leaking pump seal
    What to do
    • • Degas mobile phase and purge the pump
    • • Sonicate or replace check valves
    • • Replace pump seals
  • HPLCRetention time shifting
    Likely causes
    • • Change in mobile-phase composition or pH
    • • Column temperature not controlled
    • • Flow rate error or leak
    • • Column not equilibrated
    What to do
    • • Prepare fresh mobile phase exactly as per the method
    • • Use the column oven
    • • Check for leaks and verify flow rate
    • • Equilibrate for longer
  • HPLCBaseline drift or noise
    Likely causes
    • • Contaminated mobile phase
    • • Lamp near end of life
    • • Air in the detector cell
    • • Room temperature changes
    What to do
    • • Use fresh HPLC-grade solvents
    • • Check lamp energy and replace if low
    • • Flush the flow cell
    • • Keep the instrument away from draughts and direct sunlight
  • HPLCPeak tailing
    Likely causes
    • • Column degradation or void
    • • Secondary interactions with silanol groups
    • • Mobile-phase pH close to analyte pKa
    What to do
    • • Replace the column
    • • Use an end-capped column or adjust buffer
    • • Adjust pH as permitted by the method
  • HPLCGhost / extra peaks
    Likely causes
    • • Carry-over from a previous injection
    • • Contaminated diluent or vials
    • • Late-eluting peaks from an earlier run
    What to do
    • • Increase needle wash; run blanks
    • • Use fresh diluent and clean vials
    • • Extend run time or add a wash step
  • HPLCNo peaks
    Likely causes
    • • Lamp off or failed
    • • Injection did not happen (empty vial, needle blocked)
    • • Wrong wavelength
    What to do
    • • Check lamp status
    • • Check vial volume and needle
    • • Verify method settings
  • Analytical balanceReading drifts continuously
    Likely causes
    • • Draught or open door
    • • Sample warmer or colder than the room
    • • Static charge on the container or sample
    • • Sample is absorbing moisture or evaporating
    What to do
    • • Close all doors and remove draught sources
    • • Let the sample reach room temperature
    • • Use an anti-static gun or ionising bar, or a metal container
    • • Weigh quickly in a closed weighing bottle
  • Analytical balanceReading does not return to zero
    Likely causes
    • • Material left on the pan
    • • Pan touching the draught shield
    • • Temperature change since the last zero
    What to do
    • • Clean the pan and press zero again
    • • Re-seat the pan correctly
    • • Allow the balance to stabilise and re-zero
  • Analytical balanceUnstable reading, stability indicator never appears
    Likely causes
    • • Vibration from nearby equipment or traffic
    • • Balance not level
    • • Air conditioning blowing on the balance
    What to do
    • • Move the balance to an anti-vibration table away from pumps and centrifuges
    • • Level the balance
    • • Redirect the air flow or fit a cover
  • Analytical balanceDaily check fails
    Likely causes
    • • Balance not adjusted after a temperature change
    • • Dirty or damaged check weight
    • • Weight handled with bare fingers
    What to do
    • • Run the internal adjustment and repeat
    • • Clean the weight with a lint-free cloth; use another calibrated weight
    • • Always handle weights with forceps or gloves
  • Analytical balanceDifferent readings at different pan positions
    Likely causes
    • • Eccentricity error in the weighing cell
    • • Pan bent or not seated
    What to do
    • • Always place samples in the centre
    • • Re-seat the pan; call service if the eccentricity test fails
  • Analytical balanceError message or 'overload'
    Likely causes
    • • Load above capacity
    • • Pan missing or blocked
    • • Internal fault
    What to do
    • • Remove the load and check capacity
    • • Fit the pan correctly
    • • Restart the balance; call service if it continues
  • pH meterSlow or drifting reading
    Likely causes
    • • Blocked or dirty junction
    • • Low ionic strength sample (e.g. purified water)
    • • Old electrode
    • • Refill hole closed
    What to do
    • • Clean the junction; soak in warm KCl
    • • Use a low-ionic-strength electrode or add KCl as the method allows
    • • Replace the electrode
    • • Open the refill hole during measurement
  • pH meterSlope below 95%
    Likely causes
    • • Aged or dehydrated glass membrane
    • • Contaminated or expired buffers
    • • Deposits on the bulb
    What to do
    • • Rehydrate in storage solution for some hours
    • • Use fresh buffers from a new bottle
    • • Clean the electrode; replace it if the slope stays low
  • pH meterOffset outside ±30 mV
    Likely causes
    • • Contaminated reference electrolyte
    • • Poisoned reference (e.g. sulfide, proteins)
    • • Wrong buffer used for the first point
    What to do
    • • Replace the reference electrolyte
    • • Clean or replace the electrode
    • • Check buffer identity and value
  • pH meterUnstable, jumping reading
    Likely causes
    • • Air bubble in the bulb
    • • Electrolyte level too low
    • • Damaged cable or connector
    • • Static or earth loop with the stirrer
    What to do
    • • Shake the electrode downwards like a thermometer
    • • Top up electrolyte
    • • Check or replace the cable
    • • Stop the stirrer briefly or earth the set-up
  • pH meterCheck buffer reads outside limit after a passing calibration
    Likely causes
    • • Check buffer contaminated or at a different temperature
    • • Electrode response not linear across the range
    What to do
    • • Use fresh check buffer at the same temperature
    • • Recalibrate with buffers closer to the sample pH; replace the electrode if it persists
  • pH meterReading changes with stirring speed
    Likely causes
    • • Junction potential problem
    • • Low ionic strength sample
    What to do
    • • Clean the junction
    • • Use a constant stirring rate for buffers and samples, or read without stirring as the method states
  • Conductivity meterReading higher than expected in purified water
    Likely causes
    • • Carbon dioxide absorbed from air
    • • Contaminated sampling container
    • • Cell not rinsed
    • • Real water system problem
    What to do
    • • Measure immediately, minimise air contact; continue to Stage 2/3 if needed
    • • Use a clean, dedicated container
    • • Rinse the cell repeatedly with sample
    • • Check the water system and online trend
  • Conductivity meterUnstable or noisy reading
    Likely causes
    • • Air bubbles on the electrodes
    • • Cell not fully immersed
    • • Electrical interference from a stirrer or pump
    What to do
    • • Tap the cell to dislodge bubbles
    • • Increase immersion depth
    • • Move away from interference or earth the set-up
  • Conductivity meterCell constant drifts from its nominal value
    Likely causes
    • • Coating or deposits on the electrodes
    • • Damaged electrode surface
    • • Old or contaminated standard
    What to do
    • • Clean the cell as recommended
    • • Replace the cell if damaged
    • • Use a fresh standard in date
  • Conductivity meterStandard check fails
    Likely causes
    • • Wrong cell constant entered in the meter
    • • Temperature compensation set incorrectly for the standard
    • • Standard contaminated by air or by a dirty cell
    What to do
    • • Re-enter or re-determine the cell constant
    • • Use the certificate value at the measured temperature, or the correct compensation
    • • Pour a fresh portion of standard; rinse cell with standard first
  • Conductivity meterTemperature reading wrong
    Likely causes
    • • Faulty temperature sensor
    • • Cell not fully immersed so sensor is in air
    What to do
    • • Check against a reference thermometer and replace if needed
    • • Immerse the cell fully
  • UV-VisNoisy or drifting baseline
    Likely causes
    • • Lamps not fully warmed up
    • • Deuterium lamp near end of life
    • • Dirty optics or cuvette windows
    • • Temperature changes in the room
    What to do
    • • Allow a longer warm-up
    • • Check lamp energy and replace the lamp if low
    • • Clean the cuvettes; get optics cleaned by service
    • • Keep the instrument away from draughts and direct sunlight
  • UV-VisNegative absorbance readings
    Likely causes
    • • Blank absorbs more than the sample
    • • Baseline taken with a dirty or different cuvette
    • • Cuvettes not matched
    What to do
    • • Prepare the blank from the same solvent lot
    • • Repeat the baseline with clean cuvettes
    • • Use a matched pair or always use the same cell
  • UV-VisResults not reproducible
    Likely causes
    • • Cuvette placed in different orientations
    • • Air bubbles or particles in the solution
    • • Fingerprints on the optical faces
    What to do
    • • Mark the cuvette and always insert it the same way
    • • Tap out bubbles; filter or centrifuge turbid solutions
    • • Wipe the cuvette with lint-free tissue
  • UV-VisAbsorbance lower than expected at high concentration
    Likely causes
    • • Stray light at high absorbance
    • • Solution outside the linear range
    • • Chemical effects such as association at high concentration
    What to do
    • • Dilute so the reading falls in the linear range
    • • Check stray-light performance
    • • Use the dilution specified in the method
  • UV-Visλmax shifted from the expected value
    Likely causes
    • • Wavelength calibration error
    • • Wrong solvent or pH (many drugs shift with pH)
    • • Contaminated sample
    What to do
    • • Run a wavelength accuracy check (holmium oxide or deuterium lines)
    • • Check the solvent and pH specified in the monograph
    • • Prepare a fresh solution
  • UV-VisVery high or 'over-range' absorbance in the low UV
    Likely causes
    • • Solvent cut-off (solvent absorbs strongly)
    • • Glass or plastic cuvette used in the UV
    • • Lamp failure
    What to do
    • • Use a solvent with a suitable UV cut-off
    • • Use quartz cuvettes below about 320 nm
    • • Check lamp status and energy
  • FTIRLarge water vapour or CO₂ bands
    Likely causes
    • • Old background spectrum
    • • Exhausted desiccant or no purge
    • • Sample compartment left open
    What to do
    • • Collect a new background just before the sample
    • • Replace the desiccant or restore purge
    • • Keep the compartment closed and allow it to settle
  • FTIRWeak spectrum, low band intensities (ATR)
    Likely causes
    • • Poor contact between sample and crystal
    • • Too little sample
    • • Hard crystalline sample
    What to do
    • • Increase clamp pressure to the set position
    • • Cover the whole crystal area
    • • Grind the sample finely before measuring
  • FTIRCloudy KBr disc or sloping baseline
    Likely causes
    • • Wet KBr
    • • Sample not ground finely enough (scattering)
    • • Too much sample
    What to do
    • • Dry the KBr and work quickly in low humidity
    • • Grind sample and KBr together thoroughly
    • • Reduce the amount of sample
  • FTIRBroad band near 3400 cm⁻¹ and band near 1640 cm⁻¹ in a KBr spectrum
    Likely causes
    • • Moisture absorbed by KBr
    What to do
    • • Dry the KBr, store it in a desiccator and prepare discs quickly
    • • Compare against a blank KBr disc
  • FTIRFlat-topped (saturated) bands
    Likely causes
    • • Disc too concentrated or too thick
    What to do
    • • Reduce the amount of sample in the disc or use ATR
  • FTIRLow energy or no interferogram
    Likely causes
    • • Source failure
    • • Misalignment
    • • Laser fault
    • • Fogged KBr optics from humidity
    What to do
    • • Check the diagnostic page
    • • Run the auto-alignment if available
    • • Call service for source, laser or optics replacement
  • FTIRSample and reference spectra differ but the material is expected to be correct
    Likely causes
    • • Different polymorph or hydrate
    • • Different measurement technique (ATR vs KBr)
    • • Contamination on the crystal
    What to do
    • • Follow the monograph's instructions to recrystallise or dissolve and evaporate both sample and reference, then repeat
    • • Use the same technique for both
    • • Clean the crystal and re-measure
  • KF titrator (volumetric)High or unstable drift
    Likely causes
    • • Leaking septum or ground-glass joint
    • • Exhausted molecular sieve
    • • Exhausted solvent
    • • Side reaction with the sample
    What to do
    • • Replace the septum and check all joints
    • • Replace or regenerate the molecular sieve
    • • Exchange the solvent
    • • Use a reagent or solvent suitable for the sample, or a KF oven
  • KF titrator (volumetric)Endpoint never reached (titration runs on)
    Likely causes
    • • Side reaction consuming iodine, for example with ketones or aldehydes
    • • Very large water content
    • • Contaminated or wet solvent
    What to do
    • • Use ketone-compatible reagents for such samples
    • • Reduce the sample mass
    • • Replace the solvent
  • KF titrator (volumetric)Results too high
    Likely causes
    • • Moisture picked up during weighing or transfer
    • • Wrong titre (too old, or determined incorrectly)
    • • Drift not corrected
    What to do
    • • Weigh quickly and add the sample promptly
    • • Redetermine the titre
    • • Check drift correction is enabled
  • KF titrator (volumetric)Results too low or poor repeatability
    Likely causes
    • • Sample not fully dissolved, so water is not released
    • • Endpoint criteria too loose (stop too early)
    • • Sample mass too small
    What to do
    • • Use a co-solvent (for example formamide), longer extraction or a KF oven
    • • Review endpoint and stop-drift settings
    • • Increase sample mass so more reagent is consumed
  • Likely causes
    • • Exhausted solvent
    • • Dirty platinum electrode
    • • pH outside the optimum range
    What to do
    • • Exchange the solvent
    • • Clean the electrode
    • • Buffer the solvent for acidic or basic samples
  • KF titrator (volumetric)Air bubbles in the burette
    Likely causes
    • • Loose tubing connection
    • • Reagent outgassing
    • • Empty reagent bottle
    What to do
    • • Tighten connections
    • • Run several prepare / rinse cycles to expel bubbles
    • • Refill the reagent bottle
  • Potentiometric titratorNo clear equivalence point
    Likely causes
    • • Wrong electrode for the titration type
    • • Very weak acid or base in the chosen solvent
    • • Sample mass too small
    What to do
    • • Use the electrode the method specifies
    • • Use a non-aqueous solvent system if the method allows
    • • Increase sample mass to consume more titrant
  • Potentiometric titratorNoisy or drifting potential
    Likely causes
    • • Blocked or dirty diaphragm
    • • Low reference electrolyte
    • • Static or poor earthing in non-aqueous solvents
    • • Air bubble under the glass membrane
    What to do
    • • Clean the diaphragm or replace the electrode
    • • Refill electrolyte and open the refill port during titration
    • • Use an electrode suited to non-aqueous media
    • • Shake the electrode to remove the bubble
  • Potentiometric titratorResults high or low compared with expected
    Likely causes
    • • Old or wrong titre of the titrant
    • • Air bubbles in the burette
    • • Blank not subtracted
    • • Wrong sample mass entry
    What to do
    • • Restandardise the titrant
    • • Flush the burette
    • • Run and apply the blank
    • • Check the mass transfer from the balance
  • Potentiometric titratorSlow electrode response
    Likely causes
    • • Ageing glass membrane
    • • Protein or fat film on the membrane
    • • Electrode stored dry
    What to do
    • • Clean or recondition the membrane as per supplier
    • • Replace the electrode if slope and response remain poor
  • Potentiometric titratorTwo or more equivalence points detected
    Likely causes
    • • Polyprotic analyte or impurity
    • • Equivalence point recognition set too sensitive
    What to do
    • • Confirm which point the method uses
    • • Adjust the recognition threshold or window within the validated range
  • Potentiometric titratorLeaking burette tip or dripping
    Likely causes
    • • Worn piston seal or valve
    • • Loose tubing connection
    What to do
    • • Tighten fittings
    • • Replace the seal or service the burette unit
  • Hot air ovenOven does not reach set temperature
    Likely causes
    • • Failed heating element
    • • Door seal damaged or door left open
    • • Controller fault
    What to do
    • • Have the element checked and replaced
    • • Replace the gasket and close the door properly
    • • Service the controller
  • Hot air ovenTemperature overshoots or cycles widely
    Likely causes
    • • Poorly tuned controller
    • • Sensor displaced or faulty
    What to do
    • • Retune the PID controller
    • • Reposition or replace the sensor and recalibrate
  • Hot air ovenDisplay reading differs from reference thermometer
    Likely causes
    • • Sensor drift
    • • Controller offset not adjusted
    What to do
    • • Recalibrate and apply the offset as per SOP
    • • Replace the sensor if drift is large
  • Hot air ovenPoor uniformity (hot or cold spots)
    Likely causes
    • • Fan not working
    • • Overloaded shelves
    • • Blocked vents
    What to do
    • • Repair the fan
    • • Reduce load and space containers
    • • Clear the vents and repeat mapping
  • Hot air ovenLOD results variable between analysts
    Likely causes
    • • Different shelf positions
    • • Samples weighed while warm
    • • Inconsistent cooling time in the desiccator
    What to do
    • • Use only mapped positions
    • • Cool to room temperature before weighing
    • • Fix the cooling time in the method
  • Hot air ovenOver-temperature alarm or cut-out trips
    Likely causes
    • • Controller failure
    • • Cut-out set too close to the working temperature
    What to do
    • • Stop use and have the controller checked
    • • Set the cut-out as per manufacturer guidance
  • Dissolution testerResults lower than expected or highly variable
    Likely causes
    • • Dissolved air forming bubbles on the unit or basket
    • • Coning of powder under the paddle
    • • Vessel not centred or shaft wobbling
    • • Incorrect paddle or basket height
    What to do
    • • Deaerate the medium as per the method
    • • Confirm coning is real and discuss with method owners (the method, not the analyst, decides on changes)
    • • Recheck centring, wobble and height
    • • Repeat the mechanical calibration
  • Dissolution testerOne vessel always gives different results
    Likely causes
    • • Scratched or deformed vessel
    • • Damaged paddle or bent shaft at that position
    • • Vessel not seated in its centring ring
    • • Local temperature difference
    What to do
    • • Swap the vessel and paddle to another position to find the cause
    • • Replace the damaged part
    • • Check temperature in that vessel with a calibrated probe
  • Dissolution testerResults higher than expected
    Likely causes
    • • Vibration from nearby equipment or a worn drive
    • • Sampling too close to the paddle
    • • Rotation speed too high
    • • Evaporation of medium without covers
    What to do
    • • Isolate the bench from vibration sources
    • • Use the correct sampling position
    • • Verify speed with a tachometer
    • • Use vessel covers
  • Dissolution testerTemperature out of range
    Likely causes
    • • Low bath water level
    • • Heater or circulator fault
    • • Medium added cold
    • • Faulty temperature sensor
    What to do
    • • Top up the bath
    • • Service the heater or pump
    • • Pre-warm the medium
    • • Check the sensor against a calibrated thermometer
  • Dissolution testerUnits floating
    Likely causes
    • • Capsule shells trapping air
    • • Low-density formulation
    What to do
    • • Use the sinker type specified or permitted by the method
    • • Use the basket apparatus only if the method allows it
  • Dissolution testerFilter blocked or slow sampling
    Likely causes
    • • High excipient load
    • • Unsuitable filter pore size or material
    What to do
    • • Use the validated filter and pre-filter if the method allows
    • • Check filter compatibility and adsorption during validation
  • Dissolution testerFailed performance verification test
    Likely causes
    • • Mechanical parameters at the edge of tolerance
    • • Poor deaeration
    • • Vibration
    • • Analyst technique (timing, sampling, filtration)
    What to do
    • • Repeat the mechanical checks
    • • Review deaeration and sampling
    • • Investigate as per your SOP before repeating; do not just retest until it passes
  • Disintegration testerDisintegration time longer than usual
    Likely causes
    • • Fluid temperature low
    • • Stroke rate slow
    • • Product hardness higher than usual (compression force)
    • • Wrong or old immersion fluid
    What to do
    • • Check temperature and stroke rate
    • • Review in-process hardness data
    • • Prepare fresh fluid
  • Disintegration testerFragments pass through too quickly (false pass)
    Likely causes
    • • Torn or enlarged mesh
    • • Wrong mesh fitted
    What to do
    • • Replace the mesh with one of the correct aperture and check it against the drawing
  • Disintegration testerUnits float or stick to the mesh
    Likely causes
    • • Air trapped in capsules
    • • Sticky coating or soft gelatin
    What to do
    • • Use discs only if the monograph allows
    • • Record the observation and follow the monograph instructions for that dosage form
  • Disintegration testerRack movement uneven or noisy
    Likely causes
    • • Worn drive or loose arm
    • • Rack not hung correctly
    What to do
    • • Re-seat the rack
    • • Service the drive and recalibrate the stroke
  • Disintegration testerTemperature not stable
    Likely causes
    • • Low bath level
    • • Heater or sensor fault
    What to do
    • • Top up the bath
    • • Check against a calibrated thermometer and service the heater
  • Hardness testerReadings drift or do not return to zero
    Likely causes
    • • Load cell fault
    • • Debris on the jaw
    • • Temperature change
    What to do
    • • Clean the jaws and re-zero
    • • Recalibrate; service the load cell if it still drifts
  • Hardness testerHigh variability between tablets
    Likely causes
    • • Inconsistent orientation
    • • Variable compression on the press
    • • Laminated or capped tablets
    What to do
    • • Standardise orientation
    • • Check press settings and weight variation
    • • Inspect tablets for capping
  • Hardness testerResults differ between two testers
    Likely causes
    • • Different loading rates
    • • Calibration difference
    • • Different jaw geometry
    What to do
    • • Compare settings
    • • Check both calibrations
    • • Use the same tester for trend data
  • Hardness testerTablet slips or rotates in the jaws
    Likely causes
    • • Curved or irregular shape
    • • Wrong orientation fixture
    What to do
    • • Use the specified fixture or orientation and document it in the procedure
  • Friability testerWeight gain after the test
    Likely causes
    • • Tablets absorbed moisture
    • • Uneven dedusting
    What to do
    • • Test in controlled humidity and weigh promptly
    • • Dedust consistently
  • Friability testerTablets do not tumble (slide or jam)
    Likely causes
    • • Large or unusual tablet shape
    • • Damaged drum projection
    What to do
    • • Use the tilted-drum set-up permitted by the chapter
    • • Replace the drum
  • Friability testerRevolution count or time wrong
    Likely causes
    • • Motor speed drift
    • • Counter fault
    What to do
    • • Verify speed with a stopwatch or tachometer and service the drive
  • Friability testerHigh friability on a batch that is usually fine
    Likely causes
    • • Low hardness from the press
    • • Capping or lamination
    What to do
    • • Check in-process hardness and press settings
    • • Inform production and investigate
  • GCNo peaks
    Likely causes
    • • FID flame not lit or blown out
    • • Syringe blocked or empty vial
    • • Column broken or not connected
    • • Carrier gas cylinder empty
    What to do
    • • Check hydrogen and air flows and re-ignite
    • • Replace the syringe and check vial volume
    • • Inspect the column and its connections
    • • Replace the cylinder and purge the lines
  • GCGhost peaks or rising baseline
    Likely causes
    • • Septum bleed (siloxane peaks)
    • • Carry-over from a previous injection
    • • Contaminated carrier gas or saturated traps
    • • Column bleed at high temperature
    What to do
    • • Use a low-bleed septum and replace it
    • • Increase syringe washes and run blanks
    • • Replace gas traps or cylinder
    • • Condition the column; stay below its temperature limit
  • GCPeak tailing
    Likely causes
    • • Active sites in a dirty liner or column inlet
    • • Poorly cut column end or wrong insertion depth
    • • Column contamination
    What to do
    • • Replace the liner (deactivated)
    • • Recut the column squarely and reinstall at the correct depth
    • • Trim the front of the column
  • GCRetention time shifting
    Likely causes
    • • Leak at the inlet or septum
    • • Changed column length after trimming
    • • Wrong carrier gas pressure or flow
    • • Oven temperature not reproducible
    What to do
    • • Leak-check and replace the septum
    • • Update column dimensions in the method and adjust flow
    • • Verify flow with a calibrated flow meter
    • • Check oven calibration
  • GCPoor area precision
    Likely causes
    • • Septum leak or cored septum
    • • Syringe plunger sticking or air bubbles
    • • Liner packed with septum fragments
    • • Split ratio drifting
    What to do
    • • Replace the septum
    • • Replace or clean the syringe; adjust draw speed
    • • Replace the liner
    • • Check split vent flow and trap
  • GCSplit or broad peaks
    Likely causes
    • • Solvent and stationary phase poorly matched in splitless mode
    • • Initial oven temperature too high for solvent focusing
    • • Column installed too high in the inlet
    What to do
    • • Use a solvent compatible with the phase or a retention gap
    • • Start the oven 10–20 °C below the solvent boiling point
    • • Reinstall at the correct insertion depth
  • GCFID noise or spikes
    Likely causes
    • • Dirty jet or collector
    • • Incorrect hydrogen/air ratio
    • • Particles from a broken column or septum
    What to do
    • • Clean or replace the jet
    • • Reset gas flows to the manufacturer's values
    • • Clean the detector and replace the septum
  • HeadspaceLow or variable peak areas
    Likely causes
    • • Vial not sealed properly or septum punctured
    • • Equilibration time too short
    • • Inconsistent fill volume or sample weight
    What to do
    • • Recrimp with a new cap and check the crimper setting
    • • Extend equilibration time to the plateau
    • • Use calibrated pipettes and weigh accurately
  • HeadspaceCarry-over in blank
    Likely causes
    • • Loop or transfer line too cold so analytes condense
    • • Contaminated needle
    • • High-concentration sample run just before
    What to do
    • • Keep loop and line hotter than the vial oven
    • • Purge or clean the needle
    • • Add blank vials after high samples
  • HeadspaceSolvent peaks in blank
    Likely causes
    • • Contaminated vials, septa or diluent
    • • Laboratory air contaminated with solvent
    What to do
    • • Use fresh headspace-grade diluent and baked vials
    • • Prepare vials away from solvent-handling areas
  • HeadspacePressure or leak error
    Likely causes
    • • Worn needle seal
    • • Loose transfer-line fitting
    • • Bent needle
    What to do
    • • Replace the seal
    • • Tighten the fitting and leak-check
    • • Replace the needle
  • HeadspaceBroad early peaks
    Likely causes
    • • Split ratio too low for 1 mL gas injection
    • • Transfer line dead volume
    • • Inlet liner unsuitable
    What to do
    • • Increase split ratio within method allowance
    • • Check connections and use a narrow-bore liner
    • • Use the liner type the method specifies
  • HeadspaceResponse falls over the sequence
    Likely causes
    • • Vials waiting too long in a heated oven
    • • Gas supply pressure dropping
    What to do
    • • Use timed overlap so each vial gets the same heating time
    • • Check the cylinder and regulator
  • TLCStreaking or tailing spots
    Likely causes
    • • Sample overloaded
    • • Sample too polar or ionised
    • • Spot not dried before development
    What to do
    • • Apply less sample or dilute it
    • • Add a little acid or base (e.g. acetic acid or ammonia) to the mobile phase if the method allows
    • • Dry spots fully before developing
  • TLCUneven or curved solvent front
    Likely causes
    • • Chamber not saturated
    • • Plate touching the filter paper or wall
    • • Uneven layer or damaged plate edge
    What to do
    • • Saturate for longer with a paper lining
    • • Position the plate carefully
    • • Use a new plate
  • TLCAll spots near the origin
    Likely causes
    • • Mobile phase not polar enough
    • • Wrong plate type
    What to do
    • • Check mobile-phase composition against the method
    • • Confirm plate type and activation
  • TLCAll spots near the solvent front
    Likely causes
    • • Mobile phase too polar
    • • Plate deactivated by humidity
    What to do
    • • Check mobile-phase composition
    • • Activate plates and store them dry
  • TLCRf values differ from expected
    Likely causes
    • • Temperature or humidity differences
    • • Different plate batch
    • • Old or evaporated mobile phase
    What to do
    • • Always compare with a reference on the same plate
    • • Use fresh mobile phase each time
    • • Control saturation time
  • TLCSpots not visible
    Likely causes
    • • Compound does not absorb at 254 nm
    • • Too little sample applied
    • • Wrong visualisation reagent
    What to do
    • • Use a suitable chemical reagent or iodine
    • • Increase application volume within the method
    • • Check the reagent preparation and heating step
  • AutoclaveBowie-Dick test sheet shows a pale or uneven centre
    Likely causes
    • • Air leak into the chamber
    • • Inadequate vacuum pulses
    • • Non-condensable gases in the steam supply
    What to do
    • • Run a vacuum leak test and replace the door gasket or leaking valves
    • • Have the vacuum pump and air removal stage serviced
    • • Check steam quality and the feed water
    • • Do not use the autoclave for porous loads until the test passes
  • AutoclaveCycle does not reach set temperature or heat-up is very slow
    Likely causes
    • • Low steam supply or generator water level
    • • Blocked drain or steam trap
    • • Overloaded chamber
    • • Faulty heating element
    What to do
    • • Check water and steam supply
    • • Clean the drain strainer and trap
    • • Reduce the load to the validated pattern
    • • Call service for the heater or generator
  • AutoclaveBiological indicator shows growth
    Likely causes
    • • Cold spot in the load not reaching temperature
    • • Air trapped in the load
    • • Indicator placed in a non-validated position or mishandled
    • • Cycle time too short for the load
    What to do
    • • Treat the load as not sterile and quarantine it
    • • Investigate the cycle record and load configuration
    • • Check positive and negative controls of the indicator
    • • Repeat mapping and BI challenge after correction
  • AutoclaveMedia boil over or bottles lose volume
    Likely causes
    • • Containers overfilled
    • • Pressure released too quickly at the end of the cycle
    • • Wrong cycle selected (porous instead of liquid cycle)
    What to do
    • • Fill containers to no more than two-thirds
    • • Use the liquid cycle with slow exhaust
    • • Check the cycle programme settings
  • AutoclaveWet load at the end of a porous cycle
    Likely causes
    • • Wet steam or a blocked steam trap
    • • Load packed too densely or wrapped in non-breathable material
    • • Drying vacuum too short
    What to do
    • • Check steam quality and the trap
    • • Repack the load as per the validated pattern
    • • Review the drying phase settings
  • AutoclavePressure and temperature do not agree with the steam table
    Likely causes
    • • Air in the chamber
    • • Faulty temperature probe or pressure transducer
    • • Superheated steam
    What to do
    • • Repeat air removal and run a Bowie-Dick test
    • • Check the instruments against a calibrated reference
    • • Investigate the steam supply
  • AutoclaveDoor will not open after the cycle
    Likely causes
    • • Chamber still under pressure or above the safe temperature
    • • Vacuum remaining in the chamber
    • • Faulty door switch or seal
    What to do
    • • Wait for the cycle to finish and the chamber to vent
    • • Do not force the door; call maintenance if it remains locked
  • LAFLow air velocity
    Likely causes
    • • Blocked or loaded pre-filter or HEPA filter
    • • Fan speed set too low or motor fault
    • • Obstruction in front of the filter face
    What to do
    • • Replace the pre-filter and check differential pressure
    • • Adjust fan speed and re-measure
    • • Replace the HEPA filter if loaded, then re-qualify
  • LAFHigh particle counts in the work zone
    Likely causes
    • • HEPA filter leak or damaged seal
    • • Turbulence from room air or operator movement
    • • Unit switched on too recently
    • • Dirty work surface
    What to do
    • • Run a HEPA integrity (aerosol) test and repair or replace the filter
    • • Check room airflow, close doors and reposition the unit
    • • Allow the full stabilisation time
    • • Clean the unit and repeat the count
  • LAFMicrobial growth on Grade A settle or contact plates
    Likely causes
    • • Poor aseptic technique
    • • Inadequate cleaning or disinfectant contact time
    • • Airflow disturbed or filter leak
    • • Contaminated plates or materials
    What to do
    • • Raise a deviation and investigate as per the EM procedure
    • • Identify the organism to find the likely source
    • • Check air velocity and filter integrity
    • • Review cleaning and operator training
  • LAFDifferential pressure gauge reading rising
    Likely causes
    • • HEPA or pre-filter loading with dust
    What to do
    • • Replace the pre-filter first
    • • If the reading stays high and velocity drops, plan HEPA replacement
  • LAFDifferential pressure suddenly drops
    Likely causes
    • • Filter seal failure or torn filter
    • • Fan failure or belt slip
    What to do
    • • Stop using the unit
    • • Inspect the filter and fan; call service; re-qualify after repair
  • LAFAlarm or unusual noise from the blower
    Likely causes
    • • Worn motor bearing
    • • Loose panel or fan imbalance
    What to do
    • • Switch off and call maintenance
    • • Do not use until the fault is fixed and velocity is re-checked
  • IncubatorTemperature above set point
    Likely causes
    • • Faulty sensor or controller
    • • Room too hot for a heating-only unit
    • • Refrigeration failure (BOD)
    • • Heater relay stuck on
    What to do
    • • Check the reading with a calibrated thermometer
    • • Move the unit or use a BOD incubator
    • • Call service for the compressor or relay
    • • Assess plates incubated during the excursion
  • IncubatorTemperature below set point
    Likely causes
    • • Door left open or poor gasket seal
    • • Heater failure
    • • Ice build-up on the evaporator (BOD)
    What to do
    • • Close the door and replace a damaged gasket
    • • Call service for the heater
    • • Defrost and check the defrost cycle
  • IncubatorPoor uniformity between shelves
    Likely causes
    • • Overloading or blocked air paths
    • • Fan failure
    • • Plates against the walls or fan
    What to do
    • • Reduce load and leave space between stacks
    • • Check fan operation
    • • Use only mapped positions
  • IncubatorDisplay differs from reference thermometer
    Likely causes
    • • Sensor drift
    • • Wrong calibration offset
    What to do
    • • Recalibrate and apply the correct offset
    • • Replace the sensor if drift continues
  • IncubatorCondensation inside plates or chamber
    Likely causes
    • • Plates not inverted
    • • Large temperature difference between media and chamber
    • • Water spills or humid samples
    What to do
    • • Incubate plates inverted
    • • Pre-warm or dry plates before use
    • • Clean and dry the chamber
  • IncubatorFrequent alarms
    Likely causes
    • • Alarm limits set too tight
    • • Frequent door opening
    • • Monitoring probe in an unrepresentative position
    What to do
    • • Review alarm limits against the requirement
    • • Plan access to reduce door openings
    • • Relocate the probe to a mapped representative position
  • UHPLCPressure rising steadily over a sequence
    Likely causes
    • • Particles from samples collecting on the column inlet frit
    • • Blocked in-line filter
    • • Buffer precipitating in high organic
    What to do
    • • Replace the in-line filter
    • • Filter or centrifuge samples more thoroughly
    • • Check buffer solubility at the highest organic content in the gradient
  • UHPLCBroad or split peaks on a new column
    Likely causes
    • • Fitting not fully seated (dead volume)
    • • Sample solvent much stronger than the starting mobile phase
    • • Injection volume too large for the column
    What to do
    • • Remake the connection with the correct fitting
    • • Dissolve the sample in a solvent close to the starting mobile phase
    • • Reduce the injection volume
  • UHPLCPeaks look flat-topped or jagged
    Likely causes
    • • Data rate too low
    • • Detector time constant too long
    What to do
    • • Increase the sampling rate so there are at least 15–20 points per peak
    • • Use a shorter filter time constant
  • UHPLCRetention times differ from the HPLC method after transfer
    Likely causes
    • • Different dwell volume
    • • Gradient not scaled to the new column
    • • Frictional heating in the column
    What to do
    • • Add an isocratic hold or adjust the gradient start to compensate for dwell volume
    • • Re-scale gradient time and flow to the new column dimensions
    • • Use a narrower column or control temperature
  • UHPLCCarry-over in blanks
    Likely causes
    • • Weak needle wash
    • • Sample adsorbed on the needle seat or rotor seal
    What to do
    • • Use a stronger or two-solvent needle wash
    • • Replace the needle seat or rotor seal
  • HPTLCRf values differ from the reference
    Likely causes
    • • Chamber not saturated
    • • Humidity or temperature different
    • • Mobile phase prepared wrongly or reused
    What to do
    • • Saturate for the specified time
    • • Condition the plate to controlled humidity
    • • Prepare fresh mobile phase each time
  • HPTLCSmile or curved solvent front
    Likely causes
    • • Uneven saturation
    • • Plate not vertical
    • • Edge effects
    What to do
    • • Use a twin-trough chamber with filter paper
    • • Check the plate sits level
    • • Keep tracks away from the plate edges
  • HPTLCDiffuse or tailing zones
    Likely causes
    • • Sample applied in too strong a solvent or too large a volume
    • • Overloaded track
    • • Plate too active or contaminated
    What to do
    • • Use spray-on band application and a weaker solvent
    • • Reduce the amount applied
    • • Pre-wash and activate plates
  • HPTLCUneven colour after derivatisation
    Likely causes
    • • Hand spraying
    • • Uneven heating
    What to do
    • • Use a dipping or automatic spraying device
    • • Use a calibrated plate heater
  • ICHigh background conductivity
    Likely causes
    • • Suppressor exhausted or failing
    • • Contaminated eluent or water
    • • Eluent too concentrated
    What to do
    • • Regenerate or replace the suppressor
    • • Prepare fresh eluent with ultrapure water
    • • Check eluent concentration and generator settings
  • ICRetention times getting shorter
    Likely causes
    • • Column capacity lost through contamination
    • • Eluent concentration too high
    • • Temperature change
    What to do
    • • Clean the column as per the supplier's guide or replace it
    • • Re-prepare eluent
    • • Use the column oven
  • ICGhost peaks of chloride or sulfate in blanks
    Likely causes
    • • Contaminated water, vials or filters
    • • Contaminated eluent reservoir
    What to do
    • • Use fresh ultrapure water and IC-grade vials
    • • Rinse filters and vials before use
    • • Clean the reservoir
  • ICNoisy or drifting baseline
    Likely causes
    • • Air bubble in the conductivity cell
    • • Unstable cell temperature
    • • Pump pulsation
    What to do
    • • Purge the cell
    • • Check the cell and column temperature control
    • • Service check valves
  • ICPoor peak shape for early ions
    Likely causes
    • • Sample matrix too concentrated
    • • Carbonate interference
    • • Overloaded column
    What to do
    • • Dilute the sample
    • • Use eluent generation with a carbonate trap
    • • Reduce injection volume
  • GPC / SECMolecular weights drifting between runs
    Likely causes
    • • Flow rate variation
    • • Temperature change
    • • Column ageing
    What to do
    • • Verify flow and use a flow marker correction
    • • Control column and detector temperature
    • • Re-run calibration standards; replace the column if needed
  • GPC / SECLate-eluting tail or peaks after total permeation
    Likely causes
    • • Adsorption of sample to the packing
    • • Wrong salt concentration or pH
    What to do
    • • Increase ionic strength or adjust pH as the method allows
    • • Use a column with a more inert surface
  • GPC / SECUnstable RI baseline
    Likely causes
    • • Reference cell not purged
    • • Temperature fluctuation
    • • Mobile phase not degassed or changing
    What to do
    • • Purge the reference cell with fresh mobile phase
    • • Stabilise room and detector temperature
    • • Degas and use a single mobile-phase batch
  • GPC / SECIncreasing back-pressure
    Likely causes
    • • Undissolved sample or gel particles
    • • Microbial growth in aqueous systems
    What to do
    • • Filter samples; dissolve more completely
    • • Use fresh buffer with an antimicrobial agent for storage
  • GPC / SECUnexpected aggregate peak in protein samples
    Likely causes
    • • Sample handling (shaking, freeze–thaw)
    • • Carry-over from a previous sample
    What to do
    • • Handle samples gently and as per stability data
    • • Run blanks and clean the injector
  • LC-MSLoss of sensitivity
    Likely causes
    • • Dirty ion source or cone
    • • Ion suppression from matrix
    • • Detector ageing
    • • Wrong tune or mass calibration
    What to do
    • • Clean the source
    • • Improve sample clean-up or chromatographic separation
    • • Increase detector voltage within limits or replace the detector
    • • Re-tune and recalibrate
  • LC-MSUnstable spray or noisy signal
    Likely causes
    • • Partly blocked ESI needle or capillary
    • • Air in the LC flow
    • • Gas supply problems
    What to do
    • • Clean or replace the needle
    • • Degas solvents and purge the LC
    • • Check nitrogen pressure and purity
  • LC-MSMass shift / wrong m/z
    Likely causes
    • • Calibration out of date
    • • Room temperature change affecting the analyser
    What to do
    • • Recalibrate with the reference solution
    • • Stabilise room temperature; use a lock mass on HRMS
  • LC-MSHigh background ions
    Likely causes
    • • Contaminated solvents or additives
    • • Plasticisers from tubing or containers
    • • Column bleed
    What to do
    • • Use fresh LC-MS grade solvents
    • • Use MS-compatible tubing and glass containers
    • • Condition or replace the column
  • LC-MSVacuum fault
    Likely causes
    • • Leak at a seal
    • • Rough pump failing
    • • Turbo pump fault
    What to do
    • • Stop work and contact service
    • • Check pump oil and running noise
    • • Do not run samples until vacuum is restored
  • GC-MSHigh air / water in tune (m/z 18, 28, 32)
    Likely causes
    • • Leak at the column nut or transfer line
    • • Recently vented system not fully pumped down
    • • Leaking vent valve or seal
    What to do
    • • Check and tighten fittings; use a leak-check gas
    • • Allow longer pump-down
    • • Replace the faulty seal
  • GC-MSTune fails / electron multiplier voltage high
    Likely causes
    • • Dirty ion source
    • • Ageing detector
    • • Low calibrant level
    What to do
    • • Clean the source
    • • Replace the electron multiplier if voltage is near its maximum
    • • Refill or check the PFTBA vial
  • GC-MSPeak tailing of active compounds
    Likely causes
    • • Dirty or active inlet liner
    • • Column contamination at the inlet end
    What to do
    • • Replace the liner with a deactivated one
    • • Trim 10–50 cm from the column inlet
  • GC-MSRising baseline with siloxane ions (m/z 207, 281)
    Likely causes
    • • Column bleed at high temperature
    • • Septum bleed
    What to do
    • • Use a low-bleed MS column and stay within its temperature limit
    • • Use low-bleed septa and replace them regularly
  • GC-MSPoor library match
    Likely causes
    • • Co-eluting peaks
    • • Background not subtracted
    • • Spectral skew from scanning a fast peak
    What to do
    • • Improve separation
    • • Subtract background near the peak
    • • Increase scan speed or use more points across the peak
  • AASLow absorbance (poor sensitivity)
    Likely causes
    • • Nebuliser partly blocked
    • • Burner not aligned or wrong height
    • • Lamp weak or wrong current
    • • Wrong fuel/oxidant ratio
    What to do
    • • Clean or replace the nebuliser
    • • Re-optimise burner position with a standard
    • • Check lamp energy and replace if needed
    • • Re-optimise gas flows
  • AASNoisy or drifting signal
    Likely causes
    • • Lamp not warmed up
    • • Salt build-up on burner slot
    • • Unstable aspiration rate
    What to do
    • • Allow full lamp warm-up
    • • Clean the burner head
    • • Check capillary tubing and nebuliser
  • AASResults biased high in a heavy matrix
    Likely causes
    • • Background absorption not corrected
    • • Spectral overlap
    What to do
    • • Switch on deuterium or Zeeman correction
    • • Use an alternative line or matrix-matched standards
  • AASResults biased low for Ca or Mg
    Likely causes
    • • Chemical interference from phosphate or silicate
    What to do
    • • Add a lanthanum or strontium releasing agent
    • • Use a nitrous oxide–acetylene flame
  • AASFlame will not ignite
    Likely causes
    • • Low gas pressure
    • • Burner head not seated
    • • Drain trap interlock open
    • • Exhaust interlock
    What to do
    • • Check cylinder and regulator
    • • Re-seat burner head
    • • Fill the drain trap
    • • Confirm exhaust is on
  • ICP-OESPlasma will not ignite or goes out
    Likely causes
    • • Air leak in torch or connections
    • • Low argon pressure
    • • Wet or contaminated torch
    • • Sample too high in solids or organics
    What to do
    • • Check torch fitting and O-rings
    • • Check argon supply
    • • Dry and clean the torch
    • • Dilute the sample; use organic-solvent settings if needed
  • ICP-OESPoor precision (high %RSD)
    Likely causes
    • • Worn pump tubing
    • • Partly blocked nebuliser
    • • Air bubbles in sample line
    What to do
    • • Replace pump tubing
    • • Clean nebuliser by back-flushing (never with a wire)
    • • Check uptake tube and connections
  • ICP-OESSignal drift during the run
    Likely causes
    • • Salt deposits on injector
    • • Temperature changes
    • • Plasma not stable
    What to do
    • • Use internal standard correction
    • • Clean the torch injector
    • • Allow longer warm-up
  • ICP-OESUnexpected high result for one element
    Likely causes
    • • Spectral interference from a matrix element
    • • Contamination or carry-over
    What to do
    • • Check a second line for the same element
    • • Run blanks; extend rinse time
  • ICP-OESWavelength calibration fails
    Likely causes
    • • Spectrometer temperature not stable
    • • Wrong or old calibration solution
    What to do
    • • Allow the optics to reach temperature
    • • Prepare fresh calibration solution and repeat
  • ICP-MSLow sensitivity in tune
    Likely causes
    • • Dirty or worn cones
    • • Partly blocked nebuliser
    • • Worn pump tubing
    • • Dirty ion lenses
    What to do
    • • Clean or replace cones
    • • Clean the nebuliser
    • • Replace pump tubing
    • • Clean lenses as per manual
  • ICP-MSHigh oxide (CeO⁺/Ce⁺) ratio
    Likely causes
    • • Nebuliser gas flow too high
    • • Spray chamber temperature too high
    • • Torch position not optimised
    What to do
    • • Re-tune nebuliser gas flow
    • • Check spray chamber cooling
    • • Re-optimise torch alignment
  • ICP-MSHigh arsenic or selenium in blanks
    Likely causes
    • • Polyatomic interference (ArCl⁺, ArAr⁺)
    • • Contaminated reagents
    What to do
    • • Use helium collision or reaction mode
    • • Use high-purity acids and fresh blank
  • ICP-MSMercury carry-over
    Likely causes
    • • Hg adsorbing to tubing and spray chamber
    What to do
    • • Add HCl or gold to rinse and solutions
    • • Lengthen rinse time
  • ICP-MSInternal standard recovery falling during run
    Likely causes
    • • Matrix deposits on cones
    • • High dissolved solids
    • • Drift
    What to do
    • • Dilute samples further
    • • Clean cones
    • • Re-calibrate and repeat affected samples
  • ICP-MSVacuum fault
    Likely causes
    • • Interface or cone O-ring leak
    • • Rotary pump oil low or degraded
    What to do
    • • Check cone seating and O-rings
    • • Service the rotary pump
  • FluorimeterWeak or no signal
    Likely causes
    • • Lamp failed or near end of life
    • • Wrong wavelengths or slits
    • • Shutter closed
    • • PMT voltage too low
    What to do
    • • Check lamp and replace
    • • Check method settings
    • • Check shutter status
    • • Increase PMT voltage within the linear range
  • FluorimeterSignal saturating
    Likely causes
    • • Concentration too high
    • • PMT voltage too high
    • • Slits too wide
    What to do
    • • Dilute the sample
    • • Lower PMT voltage
    • • Narrow the slits
  • FluorimeterCalibration curve bends at high concentration
    Likely causes
    • • Inner-filter effect
    • • Self-quenching
    What to do
    • • Work at lower concentrations
    • • Keep absorbance at λex low
  • FluorimeterUnexpected peak in blank
    Likely causes
    • • Solvent Raman band
    • • Fluorescent impurity in solvent or cuvette
    • • Second-order scatter
    What to do
    • • Change λex to move the Raman band
    • • Use fluorescence-grade solvent and clean cuvettes
    • • Use an emission cut-off filter
  • FluorimeterReadings drift
    Likely causes
    • • Lamp not warmed up
    • • Sample temperature changing
    • • Photobleaching
    What to do
    • • Allow full warm-up
    • • Use a thermostatted holder
    • • Reduce slit width or exposure time
  • NIRKnown good material fails library identity
    Likely causes
    • • New supplier, grade or particle size not represented in the library
    • • Different packaging film or measurement through a fold
    • • Moisture uptake by the material
    • • Instrument drift since the library was built
    What to do
    • • Re-measure on a clean, flat part of the bag or in a vial
    • • Check the performance test and calibration
    • • Investigate and, if justified, add new representative lots to the library under change control
  • NIRTwo different materials both pass as each other
    Likely causes
    • • Library uses a simple correlation that cannot separate similar materials
    • • Threshold set too wide
    What to do
    • • Use a more selective algorithm (e.g. PCA/Mahalanobis or SIMCA) for that pair
    • • Re-validate specificity with challenge samples
  • NIRNoisy spectrum
    Likely causes
    • • Lamp near end of life
    • • Dirty window or probe
    • • Too few scans or poor contact with the sample
    What to do
    • • Check energy and replace the lamp
    • • Clean the window
    • • Increase scans and press the probe firmly
  • NIRPerformance test fails wavelength check
    Likely causes
    • • Internal standard contaminated or damaged
    • • Laser or interferometer fault (FT-NIR)
    • • Temperature change
    What to do
    • • Clean or replace the standard
    • • Call service
    • • Let the instrument stabilise and repeat
  • NIRQuantitative predictions biased
    Likely causes
    • • Model built on a different instrument or old lamp
    • • Samples outside the calibration range
    • • Changed sample presentation
    What to do
    • • Check outlier statistics; do not report outliers
    • • Transfer or update the model
    • • Standardise the presentation method
  • RamanLarge sloping background, no clear bands
    Likely causes
    • • Fluorescence from the sample, impurities or the packaging
    • • Coloured sample
    What to do
    • • Increase integration time or use fluorescence-reduction settings if validated
    • • Measure in a glass vial instead of the bag
    • • Use a 1064 nm instrument or another identity test
  • RamanAuthentic material fails
    Likely causes
    • • Different polymorph, hydrate or grade from the library material
    • • Measurement through a fold, label or tinted bag
    • • Probe not in contact or misaligned
    What to do
    • • Re-measure on a clear, flat area
    • • Check the library contains this grade or form
    • • Investigate before adding material to the library
  • RamanWeak signal
    Likely causes
    • • Laser power low
    • • Dirty window
    • • Sample out of focus
    What to do
    • • Check laser power
    • • Clean optics
    • • Use the correct nose cone or vial position
  • RamanSample discoloured or burnt
    Likely causes
    • • Laser power too high for a dark or absorbing sample
    What to do
    • • Reduce power, defocus or use a rotating stage
    • • Use another identity method
  • RamanWavenumber check fails
    Likely causes
    • • Temperature drift
    • • Contaminated reference standard
    • • Spectrograph misalignment or laser wavelength change
    What to do
    • • Let the instrument stabilise and repeat
    • • Use a fresh standard
    • • Call service and recalibrate
  • NMRCannot lock
    Likely causes
    • • Wrong solvent selected
    • • Too little deuterated solvent
    • • Sample not at the correct depth
    What to do
    • • Select the correct solvent
    • • Make the sample to the correct volume
    • • Reset the depth with the gauge
  • NMRBroad or distorted lines
    Likely causes
    • • Poor shimming
    • • Solid particles or paramagnetic impurities in the sample
    • • Low-quality or scratched tube
    What to do
    • • Re-shim or load a good shim file
    • • Filter the sample
    • • Use a good-quality tube
  • NMRPoor signal-to-noise
    Likely causes
    • • Too little sample
    • • Probe not tuned
    • • Too few scans
    What to do
    • • Use more sample or a smaller-volume tube
    • • Tune and match
    • • Increase the number of scans
  • NMRqNMR purity too low or variable
    Likely causes
    • • Relaxation delay too short
    • • Weighing error with small masses
    • • Overlapping signals
    • • Poor baseline or phasing
    What to do
    • • Measure T1 and set delay ≥ 5 × T1
    • • Use a microbalance and larger masses
    • • Choose non-overlapping signals or another internal standard
    • • Correct the phase and baseline carefully
  • NMRLarge water signal
    Likely causes
    • • Wet solvent or hygroscopic sample
    What to do
    • • Use fresh, dry solvent ampoules
    • • Use solvent suppression if validated
  • XRPDAll peaks shifted by the same amount
    Likely causes
    • • Sample surface above or below the reference plane (displacement)
    • • Goniometer zero error
    What to do
    • • Re-prepare the sample level with the holder rim
    • • Run the silicon standard; realign if it fails
  • XRPDRelative intensities differ from the reference
    Likely causes
    • • Preferred orientation
    • • Large crystallites (grainy pattern)
    • • Different sample thickness
    What to do
    • • Use back-loading or side-loading and spin the sample
    • • Gently reduce particle size
    • • Use the same holder and preparation as the reference
  • XRPDUnexpected extra peaks
    Likely causes
    • • Another polymorph or hydrate present
    • • Contamination
    • • Peaks from the holder or Kβ radiation
    What to do
    • • Compare with known forms and investigate
    • • Run a blank holder
    • • Check the filter or monochromator
  • XRPDBroad hump, few sharp peaks
    Likely causes
    • • Amorphous or poorly crystalline material
    • • Very small crystallite size
    What to do
    • • Confirm with DSC or other techniques
    • • Investigate the process step that caused amorphisation
  • XRPDLow intensity overall
    Likely causes
    • • Ageing X-ray tube
    • • Wrong slits or generator settings
    • • Too little sample
    What to do
    • • Check tube hours and intensity trend
    • • Load the correct method
    • • Fill the holder properly
  • MicrobalanceReading drifts up or down by many micrograms
    Likely causes
    • • Static charge on the container or sample
    • • Sample or container not at room temperature
    • • Draught from air-conditioning or an open door
    What to do
    • • Use the ioniser and anti-static containers
    • • Allow more time to equilibrate; handle with forceps
    • • Close doors, redirect air flow, use a smaller draught shield
  • MicrobalanceStability symbol never appears
    Likely causes
    • • Vibration from nearby equipment or people walking
    • • Balance not level
    • • Weighing table touching the bench or wall
    What to do
    • • Move vibrating equipment away; weigh at quieter times
    • • Level the balance
    • • Make sure the stone table stands free
  • MicrobalanceZero is not stable after removing the sample
    Likely causes
    • • Material left on the pan
    • • Temperature changed since the last tare
    • • Pan touching the draught shield
    What to do
    • • Clean the pan and re-zero
    • • Wait for stabilisation, then re-zero
    • • Re-seat the pan correctly
  • MicrobalanceRepeatability or minimum weight check fails
    Likely causes
    • • Poor environment at the place of use
    • • Weight handled with fingers
    • • Worn or dirty weighing cell parts
    What to do
    • • Improve the environment and repeat
    • • Use forceps and a clean, calibrated weight
    • • Call service; raise the working minimum weight until fixed
  • MicrobalanceReading slowly increases for a hygroscopic sample
    Likely causes
    • • Sample absorbs moisture from the air
    What to do
    • • Weigh quickly in a closed container
    • • Weigh by difference
    • • Control the room humidity
  • PolarimeterUnstable or noisy reading
    Likely causes
    • • Air bubble in the light path
    • • Turbid sample
    • • Temperature not yet stable
    What to do
    • • Refill the tube and move bubbles into the bubble trap
    • • Filter the solution
    • • Wait until the cell temperature is stable
  • PolarimeterBlank does not read zero
    Likely causes
    • • Dirty or strained windows
    • • Tube placed in a different orientation
    • • Contaminated solvent
    What to do
    • • Clean or replace the windows
    • • Always insert the tube the same way
    • • Use fresh solvent
  • PolarimeterLow light / 'low transmission' error
    Likely causes
    • • Strongly coloured or concentrated sample
    • • Lamp ageing
    • • Dirty optics
    What to do
    • • Use a shorter tube or dilute as the monograph allows
    • • Replace the lamp
    • • Clean the windows and compartment
  • PolarimeterQuartz plate check out of limit
    Likely causes
    • • Plate dirty or at the wrong temperature
    • • Instrument scale drift
    • • Wrong wavelength selected
    What to do
    • • Clean the plate and let it equilibrate
    • • Repeat; if it still fails, call service
    • • Check the wavelength setting
  • PolarimeterResults drift during a series
    Likely causes
    • • Mutarotation of the sample
    • • Room or cell temperature changing
    • • Evaporation of a volatile solvent
    What to do
    • • Measure at the time the monograph states
    • • Check temperature control
    • • Cap the tube and measure quickly
  • RefractometerBlurred or no light–dark boundary
    Likely causes
    • • Too little sample
    • • Bubbles or particles on the prism
    • • Sample too dark or opaque
    What to do
    • • Cover the prism fully
    • • Clean and reload without bubbles
    • • Use reflected light mode or another method if the sample is opaque
  • RefractometerWater check reads wrong
    Likely causes
    • • Prism not at 20 °C
    • • Residue on the prism
    • • Water not fresh or not pure
    What to do
    • • Wait for temperature stability
    • • Clean the prism thoroughly
    • • Use fresh purified water
  • RefractometerReadings drift with time
    Likely causes
    • • Evaporation of a volatile sample
    • • Temperature not stable
    What to do
    • • Close the cover and read quickly
    • • Allow more time for equilibration
  • RefractometerColour fringes on the boundary (Abbe)
    Likely causes
    • • Compensator not adjusted with white light
    What to do
    • • Turn the compensator knob until the boundary is sharp and colourless
  • RefractometerResults differ between two instruments
    Likely causes
    • • Different temperatures
    • • One instrument out of calibration
    What to do
    • • Measure both at the same temperature
    • • Check both with the reference liquid
  • ViscometerReading keeps falling with time
    Likely causes
    • • Shear-thinning or thixotropic sample
    • • Sample warming from friction or room
    What to do
    • • Read at a fixed time as the STP states
    • • Check bath temperature and container immersion
  • ViscometerError or 'EEEE' / reading above 100% torque
    Likely causes
    • • Sample too thick for spindle/speed combination
    What to do
    • • Use a smaller spindle or lower speed as the STP permits
  • ViscometerVery low % torque, poor repeatability
    Likely causes
    • • Sample too thin for the spindle/speed
    • • Instrument not zeroed
    What to do
    • • Use a larger spindle or higher speed
    • • Auto-zero with no spindle attached
  • ViscometerViscosity standard reads out of tolerance
    Likely causes
    • • Wrong temperature
    • • Bent spindle
    • • Wrong container size or guard leg missing
    • • Instrument not level
    What to do
    • • Check temperature with a calibrated probe
    • • Replace the spindle
    • • Use the container and guard leg the calibration requires
    • • Level the instrument
  • ViscometerResults differ between analysts
    Likely causes
    • • Different immersion depth or air bubbles
    • • Different sample mixing or reading time
    What to do
    • • Immerse to the mark at an angle
    • • Write exact mixing and reading time into the STP
  • Density meterWater check reads high
    Likely causes
    • • Residue or deposit in the tube
    • • Bubble in the tube
    • • Water not pure or not degassed
    What to do
    • • Clean the tube thoroughly and dry
    • • Refill slowly; check the camera
    • • Use fresh, freshly boiled and cooled purified water
  • Density meterAir reading does not match
    Likely causes
    • • Tube not dry
    • • Solvent vapour still in the tube
    What to do
    • • Dry longer with the air pump
    • • Rinse with a volatile solvent, then dry
  • Density meterUnstable readings
    Likely causes
    • • Bubbles forming as the sample warms
    • • Temperature not stable
    • • Vibration from nearby equipment
    What to do
    • • Degas the sample
    • • Wait for temperature stability
    • • Move the instrument away from vibration sources
  • Density meterResults higher than expected for a thick syrup
    Likely causes
    • • Viscosity effect not corrected
    What to do
    • • Turn on viscosity correction or use a method designed for viscous samples
  • Density meterDuplicates disagree
    Likely causes
    • • Sample not mixed
    • • Particles settling in the tube
    What to do
    • • Mix before filling
    • • Filter if the method allows, or use another technique
  • OsmometerSample freezes too early (pre-freeze)
    Likely causes
    • • Dirty probe or tube
    • • Particles or ice crystals in the sample
    • • Cooling bath too cold
    What to do
    • • Clean the probe and use a new tube
    • • Filter or centrifuge the sample if the method allows
    • • Check the cooling system
  • OsmometerSample does not freeze
    Likely causes
    • • Freeze-induction wire not working
    • • Sample volume wrong
    What to do
    • • Check and adjust the wire
    • • Pipette the correct volume
  • OsmometerReference solution reads out of limit
    Likely causes
    • • Standard contaminated or evaporated
    • • Probe dirty
    • • Calibration drift
    What to do
    • • Use a fresh ampoule of standard
    • • Clean the probe
    • • Recalibrate with certified standards
  • OsmometerPoor repeatability
    Likely causes
    • • Inconsistent sample volume
    • • Bubbles in the sample
    • • Carry-over between samples
    What to do
    • • Check the pipette
    • • Pipette slowly to avoid bubbles
    • • Clean and dry the probe between samples
  • OsmometerResults drift upwards when sample tubes stand open
    Likely causes
    • • Evaporation of water from the sample
    What to do
    • • Measure immediately after pipetting; keep tubes covered
  • Turbidity meterReading high and unstable
    Likely causes
    • • Air bubbles in the sample
    • • Particles settling or rising
    What to do
    • • Let the sample stand, invert gently or degas
    • • Read promptly after gentle mixing
  • Turbidity meterBlank (low-turbidity water) reads too high
    Likely causes
    • • Scratched or dirty cuvette
    • • Fingerprints or condensation
    • • Contaminated water
    What to do
    • • Clean or replace the cuvette
    • • Wipe and handle only by the top
    • • Use freshly filtered water
  • Turbidity meterResults differ when the cuvette is turned
    Likely causes
    • • Cuvette not uniform or scratched
    • • Orientation mark not aligned
    What to do
    • • Index the cuvette (find the lowest reading position) and always use that position
    • • Replace the cuvette
  • Turbidity meterVerification standard out of limit
    Likely causes
    • • Standard expired or contaminated
    • • Lamp ageing
    • • Calibration drift
    What to do
    • • Use a new standard
    • • Replace the lamp
    • • Recalibrate with formazin
  • Turbidity meterColoured sample reads lower than expected
    Likely causes
    • • Colour absorbs the scattered light
    What to do
    • • Use ratio mode if available, or follow the monograph's visual method
  • Melting point apparatusMelting points consistently too high
    Likely causes
    • • Heating rate too fast
    • • Capillary too thick-walled or too wide
    • • Sensor out of calibration
    What to do
    • • Use the specified ramp rate
    • • Use pharmacopoeial capillaries
    • • Calibrate with reference standards
  • Melting point apparatusWide melting range
    Likely causes
    • • Sample impure or not dried
    • • Powder too coarse or loosely packed
    • • Column too tall
    What to do
    • • Dry the sample as per the monograph
    • • Grind finely and pack well
    • • Fill to about 3 mm only
  • Melting point apparatusDuplicates disagree
    Likely causes
    • • Different packing in each capillary
    • • Capillaries inserted at different start temperatures
    What to do
    • • Pack each capillary the same way
    • • Insert all capillaries at the same stabilised start temperature
  • Melting point apparatusSample darkens or bubbles before melting
    Likely causes
    • • Melting with decomposition
    • • Residual solvent or moisture
    What to do
    • • Follow the monograph instructions for decomposing substances
    • • Dry the sample properly
  • Melting point apparatusAutomatic detection gives a wrong point
    Likely causes
    • • Dirty window or poor lighting
    • • Sample shrinks or sublimes before melting
    What to do
    • • Clean the optics
    • • Review the video and confirm visually; set the evaluation threshold as validated
  • DSCNoisy or drifting baseline
    Likely causes
    • • Contaminated sensor
    • • Unstable purge gas flow
    • • Pan not sitting flat
    What to do
    • • Clean the cell by bake-out
    • • Check gas regulator and flow
    • • Use flat, undamaged pans
  • DSCIndium onset out of limits
    Likely causes
    • • Calibration out of date
    • • Wrong heating rate or pan type compared with the calibration
    • • Contaminated indium
    What to do
    • • Recalibrate
    • • Calibrate under the same conditions as the method
    • • Use fresh indium
  • DSCUnexpected sharp exotherm
    Likely causes
    • • Decomposition
    • • Pan burst or lid moved
    What to do
    • • Check the sample by TGA
    • • Use vented pans and lower end temperature
  • DSCBroad, unclear melting peak
    Likely causes
    • • Large or uneven sample
    • • Heating rate too high
    • • Impure or mixed polymorphic sample
    What to do
    • • Use a smaller, flatter sample
    • • Reduce the heating rate
    • • Confirm with XRPD or microscopy
  • DSCSmall endotherm near 100 °C
    Likely causes
    • • Water in the sample or condensation in the cell
    What to do
    • • Use a pierced lid or dry the sample
    • • Check the purge gas is dry
  • TGANoisy mass signal
    Likely causes
    • • Vibration or draughts
    • • Gas flow too high or unstable
    • • Pan touching the furnace
    What to do
    • • Move the instrument to a stable bench
    • • Reduce and stabilise gas flow
    • • Re-centre the pan
  • TGAApparent mass gain at start
    Likely causes
    • • Buoyancy effect
    • • Oxidation in air
    What to do
    • • Subtract a blank curve
    • • Use nitrogen if oxidation is not wanted
  • TGAStep temperatures shifted
    Likely causes
    • • Temperature calibration out of date
    • • Different heating rate or sample mass from the method
    What to do
    • • Recalibrate with Curie point standards
    • • Use the method conditions
  • TGAMass loss does not match theory for a hydrate
    Likely causes
    • • Sample partly dehydrated or extra surface water
    • • Weighing error at the start
    What to do
    • • Check storage and sample handling
    • • Let the starting mass stabilise; check mass calibration
  • TGAResidue sticks in pan
    Likely causes
    • • Sample melted and charred
    • • Wrong pan material
    What to do
    • • Clean by heating in air
    • • Use a platinum or alumina pan as appropriate
  • Muffle furnaceSlow to reach set point
    Likely causes
    • • Ageing heating element
    • • Door seal damaged
    • • Supply voltage low
    What to do
    • • Have elements checked and replaced
    • • Replace the seal
    • • Check the electrical supply
  • Muffle furnaceTemperature overshoots
    Likely causes
    • • Controller tuning poor
    • • Thermocouple loose or moved
    What to do
    • • Re-tune the PID controller
    • • Refit the thermocouple
  • Muffle furnaceDisplay differs from reference thermocouple
    Likely causes
    • • Controller thermocouple drifted
    • • Probe placed in a cooler zone
    What to do
    • • Calibrate or replace the thermocouple
    • • Measure in the working zone
  • Muffle furnaceSulphated ash results variable
    Likely causes
    • • Crucibles placed near the door
    • • Cooling time not controlled
    • • Incomplete charring
    What to do
    • • Use the central working zone
    • • Use a fixed desiccator cooling time
    • • Char completely before ignition
  • Vacuum ovenVacuum not reached
    Likely causes
    • • Leaking door gasket
    • • Vent valve open
    • • Pump oil contaminated
    What to do
    • • Clean or replace the gasket
    • • Close the vent valve
    • • Change the pump oil
  • Vacuum ovenPressure rises when the valve is closed
    Likely causes
    • • Leak in fittings or door
    • • Sample still releasing vapour
    What to do
    • • Leak-test fittings
    • • Allow longer drying
  • Vacuum ovenResults higher than expected
    Likely causes
    • • Powder lost when vacuum applied or released
    • • Temperature too high
    What to do
    • • Apply and release vacuum slowly
    • • Check temperature accuracy
  • Vacuum ovenSlow drying
    Likely causes
    • • Poor shelf contact
    • • Overloaded chamber
    What to do
    • • Use flat-bottomed containers on the shelf
    • • Dry fewer samples at a time
  • Moisture analyserResults lower than oven LOD
    Likely causes
    • • Temperature too low
    • • Switch-off criterion too loose
    • • Sample too thick
    What to do
    • • Re-validate method settings
    • • Tighten the criterion
    • • Use a thinner, even layer
  • Moisture analyserSample burns or turns brown
    Likely causes
    • • Temperature too high
    • • Sample sensitive to heat
    What to do
    • • Lower the temperature and lengthen the time
    • • Use a glass fibre filter over the sample
  • Moisture analyserUnstable reading
    Likely causes
    • • Draughts or vibration
    • • Instrument not level
    What to do
    • • Move to a stable location
    • • Level the instrument
  • Moisture analyserPoor repeatability
    Likely causes
    • • Variable sample mass or spreading
    • • Non-uniform sample
    What to do
    • • Use the same mass and spreading each time
    • • Mix the sample before sampling
  • Laser diffraction PSAHigh or noisy background
    Likely causes
    • • Dirty or scratched cell windows
    • • Air bubbles in the wet unit
    • • Contaminated dispersant
    What to do
    • • Clean or replace windows
    • • Degas the dispersant and lower the stirrer speed
    • • Use fresh, filtered dispersant
  • Laser diffraction PSAResults keep getting smaller across replicates
    Likely causes
    • • Agglomerates still breaking up
    • • Sample dissolving in the dispersant
    • • Sonication too strong, breaking primary particles
    What to do
    • • Extend the pre-measurement dispersion time
    • • Use a saturated or different dispersant
    • • Review sonication settings during method development
  • Laser diffraction PSAUnexpected coarse peak
    Likely causes
    • • Agglomerates not dispersed
    • • Air bubbles seen as large particles
    • • Dust in the cell
    What to do
    • • Increase dispersion energy within the validated range
    • • Remove bubbles; avoid vigorous stirring
    • • Clean the cell and re-run background
  • Laser diffraction PSAHigh fit residual
    Likely causes
    • • Wrong refractive index
    • • Obscuration outside range
    • • Non-spherical particles
    What to do
    • • Confirm optical properties in the method
    • • Adjust sample amount
    • • Check shape by microscopy and document it
  • Laser diffraction PSACannot reach obscuration
    Likely causes
    • • Blocked feeder (dry)
    • • Sample sticking to tray
    • • Too little sample
    What to do
    • • Clean the feeder and venturi
    • • Adjust feed rate or vibration
    • • Add more sample
  • Laser diffraction PSACRM check fails
    Likely causes
    • • Misalignment
    • • Dirty optics
    • • Poor CRM dispersion or handling
    What to do
    • • Run alignment and clean optics
    • • Repeat with fresh CRM using the certificate conditions
    • • Call service if it fails again
  • Tap density testerPoor repeatability between duplicates
    Likely causes
    • • Different filling technique
    • • Sample not sieved or not representative
    • • Uneven powder surface
    What to do
    • • Standardise pouring; train analysts
    • • Sieve and mix before sampling
    • • Read at the mean level of the surface
  • Tap density testerVolume keeps decreasing after many taps
    Likely causes
    • • Very cohesive or fragile powder
    • • Particles breaking under tapping
    What to do
    • • Continue tapping in increments as the method allows
    • • Report the number of taps used
  • Tap density testerTap count wrong
    Likely causes
    • • Faulty counter or sensor
    • • Belt slipping
    What to do
    • • Verify by manual count; service the counter
    • • Replace the belt
  • Tap density testerDrop height out of tolerance
    Likely causes
    • • Worn cam or anvil
    • • Loose holder
    What to do
    • • Replace worn parts and recalibrate
    • • Tighten fixings
  • Sieve shakerMass balance poor (loss above limit)
    Likely causes
    • • Dust escaping
    • • Material stuck in sieves
    • • Weighing errors
    What to do
    • • Fit the lid and seals properly
    • • Brush out sieves and re-weigh
    • • Check balance and tare values
  • Sieve shakerResults coarser than expected
    Likely causes
    • • Sieve blinding
    • • Sieving time too short
    • • Agglomerated or electrostatically charged powder
    What to do
    • • Clean sieves; use sieving aids if validated
    • • Confirm the end-point
    • • Condition the sample or use air-jet sieving
  • Sieve shakerResults finer than expected
    Likely causes
    • • Torn or stretched mesh
    • • Granule attrition during shaking
    What to do
    • • Inspect and replace damaged sieves
    • • Reduce amplitude or time within validated limits
  • Sieve shakerShaker noisy or stack moving
    Likely causes
    • • Loose clamp
    • • Worn rubber mounts
    What to do
    • • Tighten the clamp
    • • Replace mounts
  • Optical microscopeImage blurred
    Likely causes
    • • Dirty lens or slide
    • • Wrong cover slip thickness
    • • Oil on a dry objective
    What to do
    • • Clean optics
    • • Use the correct cover slip
    • • Clean the objective with lens tissue
  • Optical microscopeUneven illumination
    Likely causes
    • • Condenser not centred
    • • Lamp misaligned
    What to do
    • • Set Köhler illumination
    • • Re-align the lamp
  • Optical microscopeParticles all clumped
    Likely causes
    • • Poor dispersion
    • • Wrong mounting fluid
    What to do
    • • Disperse more gently and use less sample
    • • Choose a fluid with suitable wetting
  • Optical microscopeSize results differ between analysts
    Likely causes
    • • Different particle selection
    • • Graticule not calibrated
    What to do
    • • Use a defined field-scanning pattern
    • • Calibrate and document for each objective
  • Leak testerCannot reach set vacuum
    Likely causes
    • • Worn lid gasket
    • • Pump oil low or contaminated
    • • Leaking tubing
    What to do
    • • Replace the gasket; grease if allowed
    • • Change pump oil
    • • Replace tubing
  • Leak testerAll packs fail (vacuum decay)
    Likely causes
    • • Chamber or seal leak
    • • Wet or dirty containers
    • • Wrong recipe
    What to do
    • • Run an empty-chamber test
    • • Clean and dry samples
    • • Load the validated recipe
  • Leak testerPositive control passes
    Likely causes
    • • Blocked defect in the control
    • • Test time too short
    • • Transducer drift
    What to do
    • • Use a new, certified positive control
    • • Check the recipe
    • • Recalibrate transducers
  • Leak testerFaint dye in pockets
    Likely causes
    • • Inadequate rinse
    • • Borderline leak
    What to do
    • • Rinse properly and re-inspect
    • • Treat as a fail and investigate the sealing process
  • Franz cellLow, variable release in some cells
    Likely causes
    • • Air bubble under the membrane
    • • Uneven dosing
    • • Membrane wrinkled
    What to do
    • • Remove bubbles before dosing
    • • Weigh the dose and spread evenly
    • • Mount membrane flat
  • Franz cellReceptor medium leaking
    Likely causes
    • • Clamp loose
    • • Chipped joint
    What to do
    • • Tighten clamp
    • • Replace damaged cell
  • Franz cellRelease levels off early
    Likely causes
    • • Loss of sink conditions
    • • Product drying out
    What to do
    • • Use a larger receptor volume or add solubiliser
    • • Occlude the donor chamber
  • Franz cellTemperature out of range
    Likely causes
    • • Water bath set wrongly
    • • Poor circulation
    What to do
    • • Adjust bath to give 32 °C at the membrane
    • • Check circulation tubing
  • Liquid particle counterHigh blank counts
    Likely causes
    • • Dirty glassware or water
    • • Contaminated sensor
    • • Poor environment
    What to do
    • • Re-clean glassware; use freshly filtered water
    • • Flush the sensor with detergent then water
    • • Work in LAF and wear gloves
  • Liquid particle counterCounts falling between portions
    Likely causes
    • • Bubbles settling or dissolving
    • • Particles settling
    What to do
    • • Degas properly before running
    • • Stir gently during measurement
  • Liquid particle counterVery high counts at small sizes
    Likely causes
    • • Air bubbles
    • • Product precipitating
    What to do
    • • Degas and re-run
    • • Check product compatibility; consider the microscopic method
  • Liquid particle counterCount accuracy check fails
    Likely causes
    • • Coincidence errors
    • • Wrong volume
    • • Sensor drift
    What to do
    • • Check dilution
    • • Verify syringe volume
    • • Recalibrate the sensor
  • BSCAirflow alarm sounds during work
    Likely causes
    • • Sash raised above the working height
    • • Front grille blocked by arms or items
    • • HEPA filters loaded with dust
    • • Exhaust duct fan failure (ducted cabinets)
    What to do
    • • Return the sash to the marked height
    • • Clear the grille
    • • Stop work, close cultures and call service if the alarm stays on
    • • Check the building exhaust system
  • BSCLow inflow velocity at certification
    Likely causes
    • • Exhaust filter loading
    • • Fan speed set too low
    • • Exhaust damper or duct partly closed
    What to do
    • • Adjust the fan speed and re-balance by a certified engineer
    • • Replace the exhaust filter if adjustment is not enough
    • • Check the duct and damper settings
  • BSCSmoke escapes from the front opening during the smoke test
    Likely causes
    • • Inflow too low or downflow too high
    • • Air currents in the room from doors, vents or traffic
    What to do
    • • Re-balance the cabinet
    • • Relocate the cabinet away from doors and supply vents
    • • Repeat the smoke and velocity tests
  • BSCLeak found in HEPA filter scan
    Likely causes
    • • Damaged filter media
    • • Gasket or seal leak
    • • Filter not seated correctly
    What to do
    • • Repair within the allowed area or replace the filter
    • • Reseat the filter or replace the gasket
    • • Repeat the integrity test
  • BSCContamination on negative controls handled in the cabinet
    Likely causes
    • • Poor disinfection
    • • Cluttered work area disturbing airflow
    • • Filter leak
    • • Poor aseptic technique
    What to do
    • • Review the cleaning record and disinfectant
    • • Reduce items in the cabinet
    • • Check filter integrity
    • • Retrain the analyst
  • Colony counterAutomated count much higher than manual count
    Likely causes
    • • Debris, bubbles or precipitate counted as colonies
    • • Detection threshold too low
    What to do
    • • Review the image and edit marks
    • • Re-set the detection parameters within the validated range
    • • Filter or dilute samples that leave particles
  • Colony counterAutomated count lower than manual count
    Likely causes
    • • Small or pale colonies missed
    • • Merged colonies counted as one
    • • Poor lighting
    What to do
    • • Adjust lighting and threshold within the validated settings
    • • Use the separation tool or count manually
  • Colony counterPen does not register counts
    Likely causes
    • • Pen tip worn or cable loose
    • • Battery low
    What to do
    • • Replace the pen tip or battery
    • • Check the connection
  • Colony counterDifferent analysts get different counts
    Likely causes
    • • Unclear rules for spreading or merged colonies
    • • Training gaps
    What to do
    • • Define counting rules in the SOP
    • • Run periodic analyst comparison counts
  • Air samplerFlow error alarm during sampling
    Likely causes
    • • Blocked head holes
    • • Fan or sensor fault
    • • Low battery
    What to do
    • • Clean the head and check holes
    • • Charge or replace the battery
    • • Send for service and recalibration
  • Air samplerUnexpected growth on Grade A air samples
    Likely causes
    • • Contaminated head or poor plate handling
    • • Real excursion in the area
    • • Sampler placed in turbulent air
    What to do
    • • Review handling and head sanitisation
    • • Start an investigation with particle data and other EM results
    • • Identify the isolate and check placement
  • Air samplerAgar surface dried or cracked after sampling
    Likely causes
    • • Large sample volume in one plate
    • • Low agar fill volume
    What to do
    • • Split the volume across plates or use thicker plates
    • • Validate the maximum volume per plate
  • Air samplerCalibration shows flow outside tolerance
    Likely causes
    • • Sensor drift
    • • Worn fan or leaking seal
    What to do
    • • Adjust and recalibrate
    • • Assess impact on results since the last passing calibration
  • Particle counterCounts with the purge filter fitted
    Likely causes
    • • Contaminated sensor or inlet
    • • Leak at the filter connection
    • • Electronic noise or laser fault
    What to do
    • • Purge for longer and re-check
    • • Refit the filter
    • • Send for cleaning and service
  • Likely causes
    • • Blocked inlet or kinked tubing
    • • Pump wear
    What to do
    • • Clear the inlet and straighten tubing
    • • Service and recalibrate the pump
  • Particle counterSudden high counts in Grade A
    Likely causes
    • • Real excursion: intervention, HEPA leak or HVAC failure
    • • Probe disturbed or touched
    What to do
    • • Follow the excursion SOP and assess the impact on product
    • • Check the HVAC and filter status
    • • Review video and operator activity
  • Particle counterVery low ≥5.0 µm counts compared with history
    Likely causes
    • • Long tubing or bends losing large particles
    • • Sensor degraded
    What to do
    • • Shorten tubing
    • • Check calibration and counting efficiency
  • Endotoxin readerStandard curve |r| below 0.980
    Likely causes
    • • Poor CSE dilution or vortexing
    • • Pipetting errors
    • • Temperature not uniform
    What to do
    • • Prepare fresh standards with full vortexing
    • • Check pipette calibration and technique
    • • Check reader temperature calibration
  • Endotoxin readerNegative control shows endotoxin
    Likely causes
    • • Contaminated LRW, tips or tubes
    • • Environmental contamination during set-up
    What to do
    • • Use a new lot of LRW and consumables
    • • Clean the work area and repeat
  • Endotoxin readerPPC recovery below 50%
    Likely causes
    • • Product inhibition (pH, chelators, protein binding)
    • • Spike added incorrectly
    What to do
    • • Dilute further (not beyond the MVD)
    • • Adjust pH or use a dispersing buffer
    • • Repeat with correct spiking
  • Endotoxin readerPPC recovery above 200%
    Likely causes
    • • Product enhancement
    • • Glucan interference
    • • Endotoxin contamination of the spiked sample
    What to do
    • • Dilute further
    • • Use a glucan-blocking buffer or glucan-insensitive reagent
    • • Repeat with fresh consumables
  • Endotoxin readerVery short onset in all wells
    Likely causes
    • • Contaminated LAL reagent
    • • Reader temperature too high
    What to do
    • • Use a new reagent vial
    • • Check temperature
  • Filtration unitFiltration very slow or stops
    Likely causes
    • • Sample with particles or high viscosity
    • • Weak vacuum or leak
    What to do
    • • Pre-dilute or use several membranes
    • • Check seals and pump
  • Filtration unitGrowth on negative controls
    Likely causes
    • • Non-sterile funnels or rinse fluid
    • • Poor aseptic technique
    • • Contaminated environment
    What to do
    • • Check sterilisation records
    • • Retrain analyst and review EM data
    • • Repeat with fresh materials
  • Filtration unitLow recovery in method suitability
    Likely causes
    • • Residual antimicrobial on the membrane
    • • Wrong membrane type
    What to do
    • • Increase rinse volume or add neutraliser
    • • Try another membrane material
  • Filtration unitLiquid in vacuum line
    Likely causes
    • • Trap full
    • • Hydrophobic filter missing or wet
    What to do
    • • Empty trap and replace filter
    • • Service the pump
  • KF titrator (coulometric)High or unstable drift
    Likely causes
    • • Worn septum or leaking joint
    • • Exhausted molecular sieve
    • • Wet glassware or electrodes after cleaning
    • • Exhausted or contaminated anolyte
    What to do
    • • Replace the septum and grease or tighten joints
    • • Replace the molecular sieve
    • • Dry the glassware before filling
    • • Replace the reagent
  • KF titrator (coulometric)Low recovery of the water standard
    Likely causes
    • • Error in syringe weighing
    • • Standard opened too long or past expiry
    • • Reagent near the end of its capacity
    • • Endpoint settings too loose
    What to do
    • • Weigh by difference on a calibrated balance
    • • Use a fresh ampoule of standard
    • • Replace the reagent
    • • Review the endpoint and stop-drift settings
  • KF titrator (coulometric)High recovery or results that keep increasing
    Likely causes
    • • Moisture picked up by the syringe or needle
    • • Side reaction with the sample
    • • Drift not correctly subtracted
    What to do
    • • Dry syringes and needles; rinse with sample
    • • Use a KF oven or suitable reagent
    • • Check drift correction
  • KF titrator (coulometric)Error message about generator electrode
    Likely causes
    • • Catholyte exhausted or contaminated
    • • Deposits on the diaphragm or electrode
    • • Cable or connector fault
    What to do
    • • Replace the catholyte
    • • Clean the generator electrode as advised by the supplier
    • • Check connections; call service if the fault remains
  • KF titrator (coulometric)Very long determination times
    Likely causes
    • • Sample contains too much water
    • • Sample dissolves slowly
    • • Reagent nearly exhausted
    What to do
    • • Reduce sample size or use volumetric KF
    • • Use a co-solvent or a KF oven
    • • Replace the reagent
  • TOC analyserHigh blank values
    Likely causes
    • • Contaminated reagent water
    • • Dirty vials or caps
    • • Contaminated reagent
    • • Carry-over from a high sample
    What to do
    • • Use fresh TOC-free reagent water
    • • Use certified low-TOC vials
    • • Replace reagents
    • • Run extra rinses or blanks after high samples
  • TOC analyserResponse efficiency outside 85–115%
    Likely causes
    • • UV lamp or catalyst losing performance
    • • Wrong standard concentration
    • • Oxidiser exhausted
    What to do
    • • Replace the lamp or catalyst
    • • Prepare fresh standards and check calculations
    • • Replace the oxidiser reagent
  • TOC analyserPoor repeatability
    Likely causes
    • • Air bubbles in the sample line
    • • Contamination during sampling
    • • Detector or membrane problem
    What to do
    • • Purge lines and check fittings
    • • Review sampling technique and gloves
    • • Inspect and replace the membrane or call service
  • TOC analyserSudden rise in online TOC
    Likely causes
    • • Real contamination of the water system
    • • Sanitisation residues
    • • Sensor fault
    What to do
    • • Take a grab sample and test offline
    • • Check recent maintenance or sanitisation activities
    • • Verify the sensor with a standard
  • TOC analyserResults higher than expected after calibration
    Likely causes
    • • Calibration standards prepared in water with high TOC
    • • Blank not subtracted correctly
    What to do
    • • Prepare standards in fresh reagent water and repeat
    • • Review the blank correction settings
  • DO meterReadings drift continuously
    Likely causes
    • • Probe not fully polarised
    • • Temperature not stable
    • • Membrane damaged or fouled
    What to do
    • • Allow the full polarisation time
    • • Let the probe reach the sample temperature
    • • Replace the membrane or sensor cap
  • DO meterCalibration fails (slope out of range)
    Likely causes
    • • Wrong pressure or salinity setting
    • • Dry membrane or wrinkled membrane
    • • Exhausted electrolyte or old sensor cap
    What to do
    • • Correct the settings
    • • Refit the membrane
    • • Replace electrolyte or sensor cap
  • DO meterReadings too low in a flowing sample
    Likely causes
    • • Insufficient flow or stirring (electrochemical sensor)
    • • Air bubble on the membrane
    What to do
    • • Increase stirring or flow
    • • Remove bubbles by tapping the probe gently
  • DO meterZero reading too high
    Likely causes
    • • Zero solution old or exposed to air
    • • Slow sensor response
    What to do
    • • Use freshly prepared zero solution
    • • Wait longer or service the sensor
  • Lab water systemResistivity below specification
    Likely causes
    • • Exhausted ion-exchange cartridge
    • • Poor feed water quality
    • • Faulty or dirty resistivity cell
    What to do
    • • Replace the polishing cartridge
    • • Check pretreatment and RO performance
    • • Verify the sensor and clean or replace it
  • Likely causes
    • • UV lamp at end of life
    • • New cartridge not rinsed
    • • Contaminated reservoir
    What to do
    • • Replace the UV lamp
    • • Rinse new cartridges as instructed
    • • Sanitise the reservoir
  • Lab water systemLow flow at dispenser
    Likely causes
    • • Blocked point-of-use filter
    • • Low reservoir level
    • • Pump fault
    What to do
    • • Replace the final filter
    • • Check RO production
    • • Call service
  • Lab water systemMicrobial counts out of limit
    Likely causes
    • • Infrequent sanitisation
    • • Contaminated outlet or filter
    • • Water standing in lines
    What to do
    • • Sanitise the system
    • • Replace the final filter and clean the outlet
    • • Increase recirculation or use frequency
  • MicropipetteDrop forms at the tip or volume falls
    Likely causes
    • • Tip not fitted tightly
    • • Worn seal or O-ring
    • • Damaged tip cone
    What to do
    • • Use the correct tip and fit it firmly
    • • Replace the seal
    • • Replace the tip cone
  • MicropipetteDelivered volume consistently low
    Likely causes
    • • No pre-wetting
    • • Tip immersed too deep or aspiration too fast
    • • Pipette warmer than liquid
    What to do
    • • Pre-wet tips
    • • Improve technique
    • • Equilibrate pipette and liquid
  • MicropipettePoor precision
    Likely causes
    • • Inconsistent plunger speed
    • • Holding the pipette at an angle
    • • Hand warming the pipette
    What to do
    • • Train for a steady rhythm
    • • Aspirate vertically
    • • Do not hold the pipette for long periods; rest it on the stand
  • MicropipettePlunger stiff or jerky
    Likely causes
    • • Dried liquid in the shaft
    • • Damaged piston
    What to do
    • • Clean and grease as instructed
    • • Send for service
  • Burette & glasswareDrops cling to the inside wall
    Likely causes
    • • Grease or dirt on the glass
    What to do
    • • Clean with laboratory detergent or a suitable cleaning solution and rinse well
  • Burette & glasswareBurette reading drifts with stopcock closed
    Likely causes
    • • Leaking stopcock
    What to do
    • • Tighten or replace the stopcock
  • Burette & glasswareAir bubble in the tip changes during titration
    Likely causes
    • • Tip not cleared before setting zero
    What to do
    • • Run titrant through the tip before setting zero
  • Burette & glasswareGravimetric check fails
    Likely causes
    • • Chipped tip
    • • Wrong delivery or waiting time
    • • Temperature not recorded or wrong Z factor
    What to do
    • • Withdraw chipped glassware
    • • Follow the delivery time marked
    • • Measure water temperature and use the correct Z factor
  • Thermometer / loggerReading differs from reference by more than the limit
    Likely causes
    • • Sensor drift
    • • Poor thermal contact or immersion
    • • Not stabilised
    What to do
    • • Recalibrate or replace the sensor
    • • Improve immersion and stirring
    • • Wait longer before reading
  • Thermometer / loggerGaps in logged data
    Likely causes
    • • Battery failure
    • • Memory full
    • • Logger not started correctly
    What to do
    • • Replace the battery
    • • Download and clear memory as per procedure
    • • Check start settings
  • Thermometer / loggerErratic or jumping readings
    Likely causes
    • • Damaged cable or connector
    • • Electrical interference
    What to do
    • • Replace the probe or cable
    • • Move away from sources of interference
  • Stability chamberRH below set point
    Likely causes
    • • Humidifier water supply empty
    • • Scaled or failed humidifier element
    • • Door gasket leaking
    What to do
    • • Refill with purified water and check the supply line
    • • Descale or replace the humidifier element
    • • Replace the door gasket
  • Stability chamberRH above set point
    Likely causes
    • • Dehumidifying coil iced or not cooling
    • • Wet samples or open water container inside
    • • Blocked condensate drain
    What to do
    • • Defrost and check the refrigeration system
    • • Remove the source of moisture
    • • Clear the drain
  • Stability chamberTemperature slowly drifting high
    Likely causes
    • • Dirty condenser coil
    • • Low refrigerant
    • • Room too warm around the chamber
    What to do
    • • Clean the condenser
    • • Call service to check refrigerant
    • • Improve room ventilation or air conditioning
  • Stability chamberDisplay and monitoring system disagree
    Likely causes
    • • Sensor drift
    • • Probes in different positions
    • • Monitoring probe out of calibration
    What to do
    • • Calibrate both sensors against a reference
    • • Check probe locations against the mapping report
    • • Recalibrate or replace the drifting probe
  • Stability chamberFrequent short alarms
    Likely causes
    • • Frequent or long door openings
    • • Alarm delay set too short
    • • Controller tuning poor
    What to do
    • • Plan sample pulls together
    • • Set a justified alarm delay in the SOP
    • • Ask service to re-tune the controller
  • Stability chamberUneven conditions between shelves
    Likely causes
    • • Overloading or blocked air paths
    • • Fan fault
    What to do
    • • Reduce load and keep space around packs
    • • Check and repair fans; re-map if needed
  • Fridge / freezerTemperature too high
    Likely causes
    • • Door left open or not sealing
    • • Dirty condenser
    • • Overloading blocking airflow
    • • Compressor fault
    What to do
    • • Close the door and replace a worn gasket
    • • Clean the condenser
    • • Reduce the load
    • • Call service
  • Fridge / freezerTemperature below 2 °C in a refrigerator (risk of freezing)
    Likely causes
    • • Controller set point drifted
    • • Items touching the cold evaporator plate
    • • Room very cold
    What to do
    • • Recalibrate or reset the controller
    • • Move items away from the cold plate
    • • Relocate the unit
  • Fridge / freezerHeavy ice build-up in freezer
    Likely causes
    • • Frequent door opening
    • • Door seal leaking
    • • Defrost failure
    What to do
    • • Reduce door openings
    • • Replace the seal
    • • Defrost and service the unit
  • Fridge / freezerLogger and display disagree
    Likely causes
    • • Probes in different positions
    • • Air probe versus buffered probe
    • • Calibration drift
    What to do
    • • Compare positions with the mapping report
    • • Remember buffered probes respond more slowly
    • • Calibrate both against a reference
  • Fridge / freezerFrequent alarms
    Likely causes
    • • Alarm limits too tight or no delay
    • • Defrost cycle
    • • Unit near a heat source
    What to do
    • • Set justified alarm limits and delay
    • • Check defrost schedule
    • • Relocate the unit
  • SonicatorWeak or no cavitation
    Likely causes
    • • Water level too low or too high
    • • Fresh water not degassed
    • • Transducer or generator failure
    What to do
    • • Fill to the marked line
    • • Run in degas mode before use
    • • Have the unit serviced
  • SonicatorLow or variable assay recovery
    Likely causes
    • • Sonication time too short
    • • Flask in a dead spot
    • • Sample overheated and degraded
    What to do
    • • Follow the method time exactly
    • • Use the same rack positions; use sweep mode
    • • Control bath temperature, add ice if needed
  • SonicatorBath gets very hot
    Likely causes
    • • Long continuous runs
    • • Heater left on
    What to do
    • • Change or cool the water between runs
    • • Switch off the heater when not required
  • SonicatorTank floor pitted or leaking
    Likely causes
    • • Abrasive material on the floor
    • • Long-term cavitation erosion
    What to do
    • • Always use a basket or rack
    • • Replace the tank or unit
  • CentrifugeImbalance alarm or vibration
    Likely causes
    • • Unequal tube masses
    • • Tubes not placed opposite each other
    • • Missing bucket
    What to do
    • • Re-balance tubes by mass
    • • Load symmetrically
    • • Fit all buckets, even if empty
  • CentrifugeSupernatant still cloudy
    Likely causes
    • • RCF too low
    • • Time too short
    • • Fine colloidal particles
    What to do
    • • Check the method RCF and radius
    • • Increase time within method limits
    • • Use a higher-speed rotor or filtration as allowed
  • CentrifugeLid will not open
    Likely causes
    • • Rotor still turning
    • • Power failure
    What to do
    • • Wait for the rotor to stop
    • • Use the manual emergency release only after confirming the rotor has stopped
  • CentrifugeDoes not reach set speed
    Likely causes
    • • Worn motor brushes or drive fault
    • • Rotor not recognised
    What to do
    • • Call service
    • • Check rotor seating and identification
  • CentrifugeTubes cracked
    Likely causes
    • • Tube RCF rating exceeded
    • • Old or solvent-damaged tubes
    What to do
    • • Use tubes rated for the RCF
    • • Use solvent-compatible tubes and replace old stock
  • Water bathTemperature below set point
    Likely causes
    • • Lid left off
    • • Water level low
    • • Heater or controller fault
    What to do
    • • Close the lid
    • • Top up the water
    • • Have the unit serviced
  • Water bathDifferent temperatures at different positions
    Likely causes
    • • No circulation
    • • Overloaded tank
    What to do
    • • Use a circulating model or stir
    • • Reduce load and leave gaps
  • Water bathGreen or cloudy water
    Likely causes
    • • Algae and bacterial growth
    What to do
    • • Drain, disinfect and refill; add an approved antimicrobial additive; change water weekly
  • Water bathHeater cuts out
    Likely causes
    • • Low-level or over-temperature protection tripped
    What to do
    • • Top up and reset; call service if it repeats
  • Fume hoodLow-flow alarm
    Likely causes
    • • Sash raised too high
    • • Fan or belt fault
    • • Damper closed
    What to do
    • • Lower the sash
    • • Report to engineering for fan repair
    • • Check and open the damper
  • Fume hoodOdours escaping into the lab
    Likely causes
    • • Working too close to the opening
    • • Clutter blocking baffles
    • • Cross-draughts from doors or air vents
    What to do
    • • Work 15 cm inside the hood
    • • Clear the hood
    • • Redirect air vents or relocate activities
  • Fume hoodFace velocity uneven across the opening
    Likely causes
    • • Blocked baffle slots
    • • Large equipment inside
    What to do
    • • Clear the slots
    • • Raise or move equipment
  • Fume hoodSash will not stay in place
    Likely causes
    • • Broken counterweight cable
    What to do
    • • Stop using the hood and arrange repair