32a
500 D 01/2012
4.1 Crack Set
Method:
Dissolution and decomplexation of heavy metals with
sulfuric acid and potassium peroxodisulfate
NANOCOLOR
®
reagent set:
Crack set (REF 918 08)
Requisite
accessories:
NANOCOLOR
®
heating block, decomposition apparatus (REF 916 29), piston
pipette with tips
Precautions:
Beware of samples containing high concentrations of cyanides – poisonous
vapours will develop!
Procedure:
Switch on heating block, set to 100 °C and 1 h 00 min.
Fill decomposition tube with
10 mL homogenized sample, add
1 mL R1 and
1 level measuring spoon R2, shake slightly, attach absorption tube and place
decomposition tube into the heating block, press START key.
After 1 h remove decomposition tube from heating block, cool, add
1 mL R3 and mix.
The pH value should be between a pH of 2 and 5,
otherwise add more or less R3.
A. Tube tests
The decomposed solution can be used directly for the test. Insert test tube and
select method number according to the following table:
Method
Lead 5
test 0-09
0.10–5.00 mg/L Pb
0093
Cadmium 2
test 0-14
0.10–2.00 mg/L Cd
0143
Iron 3*
test 0-37
0.10–3.00 mg/L Fe
0373
Copper 7
test 0-54
0.10–7.00 mg/L Cu
0543
Nickel 7
test 0-61
0.10–7.00 mg/L Ni
0613
Zinc 4
test 0-96
0.10–4.00 mg/L Zn
0963
B. Standard tests
Pour decomposed solution into a volumetric flask 25 mL, rinse decomposition
tube with some distilled water and fill flask to about 20 mL with distilled water
(corresponds to the 20 mL sample volume mentioned in the test procedures).
Measure according to original procedures. Multiply results by 2!
Suited for: Iron* test 1-36, Cobalt test 1-51, Copper test 1-53, Nickel test 1-62,
Zinc test 1-95.
* An exact determination of iron requires a reagent blank value, because even analytical grade chemicals
may contain traces of Fe.
C. Extraction methods
Pour decomposed solution into a separation funnel 100 mL and rinse decompo-
sition tube with about 40 mL distilled water (corresponds to the 50 mL sample so-
lution mentioned in the procedures). Measure according to original procedures.
Multiply results by 5!
Suited for: Lead test 1-10, Cadmium test 1-13.