Number: MS-0009526_en
Quality Management Version: 1.0
Work Instruction Page: 1 of 7
Valid as of: 2014-04-15
Determination of formaldehyde release from wood-based Created by: NMT
panels by flask method according to EN 717-3:1996
Approved by: NBHA
1. Purpose
This work instruction describes the determination of formaldehyde release from uncoated
wood-based panel sample by flask method.
2. Scope of application
TUV Rheinland Vietnam, Laboratory
3. Additional valid instructions and reference documents
This standard is one of a series which specifies methods for determining formaldehyde potential
release from wood-based panels. The other standards in this series are:
- EN 717-1: Wood-based panels – Determination of formaldehyde release –
Part 1: Formaldehyde release by the chamber method
- EN 717-2: Wood-based panels – Determination of formaldehyde release –
Part 2: Formaldehyde release by the gas analysis method
4. Definitions of terms
None
5. Duties and responsibilities
Softlines Laboratory
6. Procedure
6.1 Scope of application
For the investigation of textile-extracts according to above mentioned method within a range
of 10 – 250 mg/kg.
This work instruction only describes the colorimetric method, using a UV-Vis
spectrophotometer for detection referring to EN 717-3: 1996.
6.2 Principle
Formaldehyde release is determined by suspending test pieces of known mass over water in
a closed container, maintained at a constant temperature. Formaldehyde release from the
test pieces during a defined period of time is absorbed by the water. The formaldehyde
content of the water is determined photometrically by the acetylacetone method, and the
Number: MS-0009526_en
Quality Management Version: 1.0
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result is expressed in milligrams formaldehyde per kilogram of dry board. The quantification is
ensured by a 5 points calibration.
6.3 Inteferences
None.
6.4 Chemical
● Sulfuric acid, CH2SO4 = 1.5 mol/L
● Sodium base, CNaOH = 2 mol/L by Merck
● Sodium thiosulfate solution, CNa2S2O3 = 0.1 mol/L by Merck
● Iodine solution, CI2 = 0.05 mol/L by Merck
● Starch solution, ρ = 1 g/100 mL; dissolve starch in hot distilled water, decant turbidity, add
5 mg/L HgI2
● Acetylacetone reagent-solution, prepare always fresh; dissolve 15 g ammonium acetate
with distilled water in a 100mL volumetric flask, add 0.3 mL acetic acid anhydrous and 0.2
mL acetylacetone, then make up to the mark with distilled water.
● Dimedone solution, 5 g dimedone in 100 mL ethanol
● Formaldehyde stock solution; 2 mL formaldehyde solution (37 %) fill up to 1 L distilled
water, storage at 4-8°C up to 6 months ~ 780 mg Formaldehyde/L
● Formaldehyde standard solution; dilute stock solution 1:100 with distilled water, storage at
4-8°C up to 1 month ~ 7,8 mg Formaldehyde/L
6.5 Apparatus
6.5.1Test apparatus
● Polypropylene, or polyethylene flask-container (bottle) of 500mL volume with tightly fitting
lid of the same material
● Elastic rubber band and stainless steel hook.
6.5.2 Laboratory equipment
● Graduated cylinder 100mL
● Ground joint Erlenmeyer flask 250 mL
● Graduated flasks 25, 50, 250, 1000 mL
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● Graduated pipettes from 1 to 50 mL
● Burette 25 mL
● Shaking water bath, capable of maintaining a temperature of (40±1)˚C
● Ventilated oven (maximum volume: 60L), capable of maintaining a temperature of
(40±1)˚C at any position in the oven
● UV-VIS Spectrophotometer, capable of measuring absorbance at 412nm
● Quartz-cuvettes 1 cm
6.6 Procedure
● Duplicate sets of test pieces of 25 mm x 25 mm x board thickness shall be taken, total
mass of each set as near as possible 20 g. The individual values shall only differ from
each other by a maximum of 20% related to the higher of two single values. Otherwise a
third determination shall be carried out.
● Fix the test pieces with the rubber band as shown in the figure below. Add 50 mL of
distilled water at 20˚C to the container, attach the lid with the suspended test pieces and
close the container so that it is completely airtight. The bottom surface of the test pieces
should be approximately 40 mm above the surface of the water. A second container shall
be prepared in the same way.
● Insert the closed containers into the oven at a temperature of (40±1)˚C. This temperature
shall be maintained throughout the whole test period. The containers shall occupy less
than 10% of the whole volume of the oven. The containers shall be placed staggered and
with a distance of at least 50 mm between each other.
● After (180±1)min remove the containers from the oven and immediately take off the lids
with the test pieces attached. Transfer the solution from the containers to each of the two
250 mL flasks, close them tightly and allow the contents to cool at ambient temperature to
approximately 20˚C.
● Add 50 mL acetylacetone reagent-solution and make to the mark with distilled water, seal
flask with a ground joint glass stopper and shake well. The mixture is kept in water bath at
(40±1)°C for 15 min, then cool down to room temperature protected from light (about 30
min) and measure against blank reagent.
● Prepare one “blank reagent” (use distilled water instead of the test specimen extract and
treat in the same way as above) that has to be measured first against water. The
absorbance must not be higher than 0.025
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1) 500 mL polyethylene bottle with bottle top
2) Hook out of stainless steel
3) Elastic rubber band
4) Surface of the water
Dimensions in millimetres
Figure: Test apparatus for the flask method
6.7 Control of reagents
Reagents are tested once before first use of a new reagent lot or in case of suspicious test
results or obvious changes in the appearance of the reagents. Test results are stated in the
UV-Vis log book with shortcut of the technician and the date.
6.7.2 Absence of formaldehyde
Mix 10 mL distilled water with a) 10 mL acetylacetone reagent-solution and b) 10 mL distilled
water in a 25 mL measuring flask each. The extinction value from a) substracted by the
extinction value from b) must not be higher than 0.025.
Otherwise check chemicals for their formaldehyde content and replace them when found
positive.
6.7.2 Other compounds resulting in a staining with acetyl acetone
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Add to 10 mL sample extract 2 mL dimedone solution and keep 10 min at 40 ºC. Then add 10
mL acetylacetone reagent-solution and continue as with a regular sample. Compare to a
blank solution where the extract is replaced by 10 mL distilled water. In case the original
sample extract showed a formaldehyde content, the corrected extinction value should be
below 0.05.
7.8 Detection
Cool down the treated mixtures to room temperature for (30±5) min and measure at 412 nm
at standard settings for slit width and so forth.
For the handling of the UV-Vis Spectrophotometer, refer to the manufacturers manual.
Further details are described within the mentioned standards or within the method file.
6.9 Calibration
Prepare the standard solutions by adding the volume of standard solution as table below to
the 50 mL volumetric flask. Fill up to 50 mL by distilled water.
For each cuvette, a separate calibration is necessary.
Calibration solutions must be prepared with formaldehyde standard solution as below:
Volume of
Formaldehyde 1.59 3.18 6.35 19.1 25
standard solution in mL
Volume of
Acetylacetone 25 25 25 25 25
reagent-solution (mL)
Equal final
0.25 0.50 1.00 3.00 3.94
concentration in mg/L
The resulting amounts of the standard solution are calculated with a formaldehyde stock
concentration of 787.5 mg/L. The accurate concentration has to be determined before
according to sub item 6.10
6.10 Iodometric titration of the formaldehyde stock solution
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Before first use, each Na2S2O3-solution lot as well as each new I2 solution lot must be compared
with older lots of the same supplier or solutions of another supplier via titration. Values must be
in a range of ± 2.5 %. Otherwise replace affected solutions.
Give 25 ml stock solution in a ground joint Erlenmeyer flask; add 25 mL I2 solution and 10 mL
NaOH. Stir closed flask for 15 min. Then add 7.5 ml sulfuric acid and 1 mL aqueous starch
solution.
Use solution as titrant. The exact concentration of formaldehyde is calculated by the following
equation:
Vsample (mL): the volume of formaldehyde stock solution
(mL) : the volume of used I2 solution
(mL) : the consumption volume of Na2S2O3 solution
6.11 Calculation
The final results are given in milligrams formaldehyde per kilograms of board (mg/kg). They are
calculated according to the calibration curve A = aC + b
Where m is the mass of test pieces, in grams
Example:
6.12 Quality Control/ Uncertainty
Number: MS-0009526_en
Quality Management Version: 1.0
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Since the achieved result is varying with the test condition, the acceptable variation in this
method is 10%. The Quality Control Standard solution which is original from other brand name
was used to control the variation of the method. Once there is any point of the Control
Standard out of the acceptable variation range, the standardization procedure will be
operated. Control chart as well as analytical uncertainty method is always used for
specification any errors in time.
Process control: The internal reference material will be run after 5 batches of samples.
Further details, refer to file MS-0009403_en
Uncertainty: Refer to uncertainty folder
Note:
The calculated uncertainty relates to the photometrical determination from the preparation of
a unstained sample free from matrix effects.
Considering matrix effects e.g. fat content, coatings or strong bleeding of the leather is not
feasible due to their variety. Certified reference materials are not available at the moment.
6.13 Validation
Refer to validation folder
7. Management of quality records
None
8. Appendices
None
