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Assessment of quality assurance Measures
Abstract:
Assessment of quality assurance measures in species analysis in the course of monitoring campaigns.
Validation of a procedure for determination of tin organic compounds in sediments and biological samples.

TetraOZV

TriOZV

DiOZV, MonoOZV
initial product anti fouling colors
 - biocide
agriculture
 - fungicide
 - acaricide
wooden shield
desinfection
textiles
PVC
 - heat stabilizer
 - light stabilizer
homogeneous catalysts
 - silicones, urethanes
esterfications
precurser
 - SnO2 on glas
anti worm agent for poultry
textiles
Pathes of tin species in the environment:
Quality assuring measures
  • · regular participation in intercomparisons and EU certifications
  • · measurement of control samples
  • · measurement of reference material
  • · keeping of control sheets for blind value and mean value, recovery control
      sheets, range control sheets
  • · The reconstruction of processes is assured by extensive documentation of
      quality
  • · regular control of measuring equipment
  • · description of our quality management system in a quality management
      manual
  • · regular execution of audits and reviews
  • · regular training of our staff
  • · GALAB is member of numerous commissions of standardization (DIN, VDI)
Toxicity of tributyl tin


Toxicities - quality target - standard datat
TBT Water
ng Sn/l
Sediment
µg Sn/kg
Fish
µg Sn/kg
toxicity 1
(oysters)
1
(dogwhelks)
 
quality targets 1
(IKSE)
25
(ARGE)
<1
(draft)
standard values none 250
(dredged material)
35
(ADI values)
Validation of the NaBEt4 method
  • development of the NaBEt4 method
  • application on actual matrices
  • determination of performance characteristics
  • screening with certified refernce material
  • verification by participating in intercomparisons

Sodiumtetraethylborate method


In an intercomparison which was carried out in 1998 by the BCR for charaterizing the refernce material CRM 646 the following performance characteristics were determined:

Compound MPhT DPhT TPhT
number of all laboratories (L) 8 10 10
number of all pieces of test data (N) 40 50 48
proportion of outliers (NAP) /% 25 20 27
total mean value (Xm) / µg/kg 68.6 36.4 29.2
between lab standard deviation (SR) /µg/kg 15.6 8.01 9.55
between lab variation coefficient (VR) / % 22.7 22.0 32.7
repeatability standard deviation (SI) / µg/kg 8.47 5.28 4.15
repeatability variation coefficient (VI) / % 12.3 14.5 14.2


Compound TBT DBT MBT
number of all laboratories (L) 17 16 13
number of all pieces of test data (N) 85 80 65
proportion of outliers (NAP) /% 17 19 23
total mean value (Xm) / µg/kg 476 771 606.6
between lab standard deviation (SR) /µg/kg 74.89 114.6 141.6
between lab variation coefficient (VR) / % 15.7 14.9 23.3
repeatability standard deviation (SI) / µg/kg 39.75 58.64 45.8
repeatability variation coefficient (VI) / % 8.35 7.61 7.55


GC-AAS chromatogram: spiked sediment sample (500 ng Sn/g) reconditioning with the soduimtetraethylborate method

  1 trimethyltin(IV)
  2 dimethyltin(IV)
  3 monomethyltinn(IV)
  4 inorg. tin
  5 monobutyltin(IV)
  6 tetrapropyltin
  7 dibutyltin(IV)
  8 tributyltin(IV)
  9 monooktyltin(IV)
 10 tetrabutyltin
 11 diphenyltin(IV)
 12 dioktyltin(IV)
 13 triphenyltin(IV)

Routine AQA:
  • · determination of requirements
    •    · arrangement with the customer
    •    · standard values, quality targets
  • · set-up of a control sheet system
    •    · matrix
    •    · parameter
  • · intercomparisons

Summary:
  • · high expenditure for quality assuring measures (> 50%)
  • · control sheet system:
       high repeatability
       low uncertainty of measurement
  • intercomparisons:
       refernce labority for the determination of tinorganic compounds

Bioakkumulation of butyltin species in fish


Influence on the bioakkumulation of tin species
  • partitioning equilibrium
    • · water / suspended matters / sediment / biological samples
  • · complexing behaviour
    •    · organic carbon
    •    · humic substances
    •    · biofilms
    •    · mineral components
  • · phys./chem. dimensions
    •    · solubility
    •    · octanol/water coefficient

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