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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
|
| Applications of organotin compounds: |
 |
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
- 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
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| 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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 Environment |
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