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Q/SQR

Enterprise Standard of Chery Automobile


Co., Ltd.

Q/SQR.04.096-2009
Replace Q/SQR.04.096 - 2007

Emission Property Testing - Formaldehyde Content Test

Released on September 05, 2009 Implemented on September 15, 2009

Issued by SAIC Chery Automobile Co., Ltd.


Q/SQR.04.096-2009

Foreword
This standard is applicable to the formaldehyde content testing of the non-metal interior trims and materials
required for Chery automobiles. Meanwhile its format and content shall be subject to GB/T1.1-2000 and
GB/T1.2-2002.
This standard substitutes Q/SQR.04.096-2007 and has the following main modifications:
(1) Add the specific sealing requirements for the storage and transportation of sample pieces under test;
(2) Change the description of "take 6 samples for each every type of material, 5 used for formaldehyde
content testing and 1 used for moisture content testing" into "take 3 samples for each every type of material, 2
used for formaldehyde content testing and 1 used for moisture content testing";
(3) Determine the steel hook attached to the polythene bottle cap to be stainless steel hook; otherwise, it
should not be used;
(4) Define the sampling method for the composite materials and thick spare parts and materials;
(5) Define the formula of starch solution.

This standard was proposed by the Materials Department of Institute of Automobile Engineering of Chery
Automobile Co., Ltd.
This standard is under the jurisdiction of the Standard Management Department of Institute of Automobile
Engineering of Chery Automobile Co., Ltd.
This standard was revised by the Materials Department of Institute of Automobile Engineering, Material Test
Department of Test Technology Center of Chery Automobile Co., Ltd.
This standard was drafted by: Xu Ling, Wang Zheng, Zhao Fei, Wu Shengjun.

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Q/SQR.04.096-2009

Emission Property Testing - Formaldehyde Content Test

1 Scope
This standard specifies the formaldehyde content test method of the non-metal interior trims and materials
required for automobiles.
This standard is applicable to the formaldehyde content test method of the non-metal interior trims and
materials required for automobiles.

2 Normative reference
The following normative documents contain provision which, through reference in this text, constitute
provisions of this standard. For dated reference, subsequent amendments to (excluding amending error in the
text), or revisions of, any of these publications do not apply. However, all parties coming to an agreement
according to this standard are encouraged to study whether the latest edition of the normative document is
applicable. For undated references, the latest edition of the normative document referred to applies.
GB 601 Preparation of Standard Solution for Chemical Reagent Titrimetric Analysis (Volumetric Analysis)

3 Test Principles
During the test, fix the specimen of certain sizes to the 1L polythene bottle containing distilled water. The
specimen should be above the distilled water without contacting the bottle wall and water. Condition the
specimen for 3 hours at 60℃. After cooling, the formaldehyde and ammonium ion emitted from the specimen
will react with the diacetone to generate the dehydroacetic acid dihydro - lutidine (DDL). DDL is a yellow
complex and allows the maximum absorption at 412nm wave length. The absorbance of solution containing
yellow complex at 412nm wave length relative to the distilled water can be measured by the spectral
photometer, which is called the acetylacetone method. The formaldehyde content emitted from the specimen
can be worked out from the measured absorbance and correction curve.

Acetylacetone Formaldehyde Ammonium ion Yellow complex

Reaction equation of acetylacetone method

4 Test conditions
4.1 Chemical reagents: ammonium acetate (analytic pure), acetylacetone (analytic pure), formaldehyde
solution (concentration of 35% ~ 40%), potassium iodide (analytic pure), iodine (analytic pure), sodium
hydroxide (analytic pure), anhydrous sodium thiosulfate (analytic pure), concentrated sulfuric acid, soluble
starch and distilled water etc.
4.2 Main instruments: spectral photometer (applicable to 412nm wave length), colorimetric cell with 1cm
optical path.

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Q/SQR.04.096-2009

4.3 Auxiliary instruments: electronic balance accurate to ± 1mg, electric drying oven with forced convection,
1L polythene bottle with threaded bottle cap and stainless steel hook.
4.4 Glass wares: volumetric flask, pipette, beaker and conical flask etc.

5 Test specimen requirements


5.1 Seal the sample pieces under test for the storage and transportation to avoid the cross contamination.
5.2 The size of specimen should be 40mm × 100mm × thickness of material to be used or part under test.
5.3 For the composite spare parts (such as the sun visor), the whole sampling is recommended; where the
specimen is thick more than 20mm, cut the back off until the thickness is 20mm.
5.4 Take 3 specimens for each spare part or material, 2 used for formaldehyde content determination and 1
used for moisture content determination.
5.5 For the soft spare part and material (such as the genuine leather), cut out the specimen with the scissors
and hang it to the hook inside the bottle cap of 1L polythene bottle. To this end, the specimen should be
provided with a notch (for the soft material).
5.6 For the hard spare part and material (such as the rigid plastics parts), cut out the specimen with the
band-sawing machine. To fix the specimen to the hook, drill a hole with the diameter more than that of the
hook on each specimen and maintain the hole 10mm from the top edge and in the middle.

6 Test Procedures
6.1 Correct the spectral photometer
Before testing, correct the spectral photometer and plot the correction curve to determine the correction factor.
The correction falls into 9 steps:
1) Prepare the acetylacetone solution with the acetylacetone and distilled water
Fill 300mL distilled water in 1000mL brown volumetric flask approximately, fill 4mL acetylacetone exactly
and then fill the distilled water to the required volume, screw on the volumetric flask cork, mix the solution
uniform and keep it at the room temperature with light protection. The solution can be kept for 4 weeks.
2) Prepare the ammonium acetate solution with the ammonium acetate and distilled water
Weigh 200g ammonium acetate, bring it to a 500mL beaker, fill 300mL distilled water approximately and heat
the beaker slightly while mixing to accelerate the dissolution of the ammonium acetate. Stop heating after the
ammonium acetate is dissolved, maintain the beaker still and wait for the solution to cool down to the room
temperature. Transfer the solution to the 1000mL volumetric flask, rinse the beaker with distilled water for
many times and fill all the solution to the volumetric flask. Then fill the distilled water to the required volume,
shake the solution uniform and keep it at the room temperature. This solution can be kept for 4 weeks.
3) Prepare the standard formaldehyde solution with the formaldehyde solution and distilled water (field
preparation)
Fill 300mL distilled water in 1000mL volumetric flask approximately, place the volumetric flask on the
electronic balance, reset the balance, drop the formaldehyde in the volumetric flask about 1g and then fill the
distilled water to the required volume, screw on the volumetric flask cork and mix the solution uniform.
4) Determine the exact concentration of standard formaldehyde solution in iodometry method
a) Prepare the following reaction solution:
——Standard iodine solution c(I2)=0.05mol/L

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Q/SQR.04.096-2009

Weigh 40g potassium iodide, dissolve it in 25mL distilled water and then add 12.7g iodine. After the iodine is
completely dissolved, transfer it to a 1000mL brown volumetric flask, fill the distilled water to the required
volume, shake the solution uniform and keep it in a dark place.
——Sodium thiosulfate solution c(Na2S2O3)=0.1mol/L
Weigh 15.8g anhydrous sodium thiosulfate, dissolve it in the distilled water and transfer it to a 1000mL brown
volumetric flask. Then fill the distilled water to the required volume, shake the solution uniform and keep it in
a dark place.
——Sodium hydroxide solution c(NaOH)=1mol/L
——Sulphuric acid solution c(H2SO4)=1mol/L
——Starch solution 1%(m/m)
Weigh 1g starch and dissolve in 100g distilled water. When preparing the starch solution, heat it to boiling
while mixing until the solution becomes transparent and then cool it down to room temperature for use.
Note: 1) use the analytic pure chemical reagent and distilled water to prepare the solution.
2) before using the sodium thiosulfate, check its concentration in the iodometry method. (refer to Clause 4.6.3
of GB601)
b) Fill 20mL standard formaldehyde solution, 25mL 0.05mol/L iodine solution and 10ml 1mol/L sodium
hydroxide solution to the 250mL conical flask in turn. Protect it against the light for minutes (cover it or place
it in a dark cabinet) and then fill 15mL 1mol/L sulphuric acid solution.
c) Retitrate the surplus iodine with the sodium thiosulfate solution as follows:
——Fill 0.1mol/L sodium thiosulfate solution to 50mL precious burette.
——Read the volume of solution in the burette (V1).
——Drop the sodium thiosulfate solution in the mixed solution with the precious burette slowly while
shaking the mixed solution uniformly.
——The original color of the mixed solution is dark red and it will become lighter along with the addition of
the sodium thiosulfate solution.
——When the mixed solution becomes pale yellow, that is, the titration end point is approaching, fill a few
drops of 1% starch solution as the indicator.
——Keep dropping the sodium thiosulfate solution to the mixed solution slowly and stop the titration
immediately when the mixed solution becomes transparent and read the volume of residual sodium thiosulfate
solution (V2)
——Work out the volume of sodium thiosulfate solution consumed by the surplus iodine (V):
V=V1-V2
d) Carry out the blank test with the distilled water in the same way:
Mix 20mL distilled water with 25mL 0.05mol/L iodine solution and 10mL 1mol/L sodium hydroxide solution.
Protect the solution against the light for 15 minutes, then fill 15mL 1mol/L sulfuric acid, retitrate the surplus
iodine with the sodium thiosulfate solution and read the volume of sodium thiosulfate solution consumed by
the blank test (V0).
e) Calculate the concentration of standard formaldehyde solution with the following formula:

(VO − V ) × 15 × c( Na 2 S 2 O3 ) × 1000
c(HCHO)=
20

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Q/SQR.04.096-2009

Where,
c(HCHO) = the concentration of standard formaldehyde solution in mg/L
VO = the volume of sodium thiosulfate solution consumed by the blank test in mL
V = the volume of sodium thiosulfate solution consumed by the test with the standard formaldehyde solution
in mL
c(Na2S2O3) = The concentration of sodium thiosulfate solution in mol/L
5) Prepare the formaldehyde correction solution with the standard formaldehyde solution and distilled water
Fill 300mL distilled water approximately to a 1000mL volumetric flask and drop a certain volume of standard
formaldehyde solution to the flask with the pipette which contains 15mg formaldehyde. This volume can be
worked out by the determined concentration of standard formaldehyde solution. Fill the distilled water to the
required volume and then the concentration of formaldehyde correction solution is 15 µg/mL.
6) Prepare 6 types of formaldehyde correction solution of different concentration by diluting the formaldehyde
correction solution with the distilled water
Prepare 6 100mL volumetric flasks, fill 0, 5, 10, 20, 50 and 100mL formaldehyde correction solution
respectively and fill the flasks to the required volume. The formaldehyde concentration of 6 diluted
formaldehyde correction solutions should be within 0 and 15µg/mL.
7) Mix the 6 diluted formaldehyde correction solutions with the acetylacetone solution ammonium acetate
solution and heat the mixed solution.
Prepare 6 50mL volumetric flasks.
Take 10mL to 50mL diluted formaldehyde correction solution with the pipette and transfer it to the 50mL
volumetric flask. The sampling must start from the least concentration solution and the pipette should be
rinsed 3 times at least with the solution to be sampled.
Fill 10mL acetylacetone solution and 10mL ammonium acetate solution to each volumetric flask and mix the
solution uniform.
Heat the mixed solution in a water bath at 40℃ for 15 minutes. The yellow DDL will be generated during this
process. The solution will be more yellow if the formaldehyde concentration is higher.
After 15 minutes, take the 6 volumetric flasks from the water bath and cool them down to the room
temperature (for 1 hour approximately) without the direct light.
8) Determine the absorbance of solution with the spectral photometer
Turn on the spectral photometer and stabilize it for a while. Then prepare 2 colorimetric cells with the optical
path of 1cm, one used for the distilled water and the other one used for the specimen.
Fill the distilled water to one colorimetric cell, wipe the outside of the cell with the clean filter paper, open the
cap of spectral photometer sample cell and place the colorimetric cell on the bracket on which the reference
colorimetric cell is placed.
Fill the reacted solution to the other colorimetric cell, wipe the outside of the cell with the clean filter paper
and place the colorimetric cell on the bracket on which the specimen colorimetric cell is placed.
Close the sample cell cap and the spectral photometer will determine and indicate the absorbance of solution
at 412nm wave length relative to that of distilled water. Then read and record the absorbance value.
Determine the relative absorbance of the rest 5 solutions in the same way. Attention should be paid to the
following items:
a) Determine the absorbance from the formaldehyde of the least concentration and end at the highest

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Q/SQR.04.096-2009

concentration;
b) Before testing any solution, wet and rinse the colorimetric cell for 3 times at least with the solution under
test.
9) Plot the correction curve and work out the correction factor
Determine the absorbance of formaldehyde correction solution diluted by the known concentration
formaldehyde with the spectral photometer and plot the correction curve of absorbance value vs known
formaldehyde concentration (between 0 and 15μg/mL) with Microsoft Excel, as shown in below figure.
The slope and relative coefficient of correction curve can be worked out with this program as well and the
correction factor f is equal to the reciprocal of correction curve slope. The correction factor f will be used for
the calculation of formaldehyde content.

1.4
y= 0.0834x
2
1.2 R = 0.9994

1.0
Absorbance

0.8
吸光度

0.6

0.4

0.2

0.0
0 5 10 15 20

甲 醛 浓 度 (μg/ml)
Formaldehyde concentration

6.2 Test process


During the preparation of specimen, take 3 specimens of appropriate sizes according to the sampling
requirements for each spare part and material, 2 for formaldehyde content determination and 1 for moisture
content determination.
1) Determine the moisture content:
a) Weigh the specimen with the analytical balance accurate to ±0.001g and record it as m1 (the mass before
drying in g).
b) Place this specimen in the electric drying oven with forced convection and dry for 24 hours at 103℃.
c) 24 hours later, take out the specimen and cool it down to the room temperature in the drier provided with
the silica gel. The cooling process requires 60 minutes approximately.
d) After cooling down, weigh the specimen accurate to ±0.001g and record it as m0 (the mass after drying in
g).
e) Calculate the moisture content H with the following formula

m1 − m0
H= × 100[%]
m0
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Q/SQR.04.096-2009

Where, m1= the mass of specimen before drying in g


m0=the mass of specimen after drying in g
2) Prepare 3 1L polythene bottles with steel hook on the cap and mark the number of 0 to 2 (0, 1 and 2) on the
bottle. The bottle 0 is used for the blank test made with distilled water and the rest 2 bottles (1 and 2) are used
for the specimen test.
3) Weigh 2 specimens (number 1 and 2) with the electronic balance accurate to ±0.001g and record the value
as m (the mass of each specimen).
4) Fill 50mL distilled water to each of the 3 polythene bottles.
5) Screw on the cap of number 0 bottle for the blank test. Hang the 2 weighed specimens to the steel hook of
the bottle cap, fasten the bottle cap and seal it. Note the specimen number should be consistent with the bottle
number.
6) Place the 3 bottles in the electric drying oven with forced convection, condition for 3 hours at 60℃ and
then take them out to cool down to the room temperature.
7) Prepare 3 50mL volumetric flasks and mark the number of 0 to 2 (0, 1 and 2) as well.
8) Open the polythene bottles in turn, take out the specimen and rotate the bottle slowly to blend the water
vapor on the bottle inside wall and the water solution.
9) Take out 10mL water solution with the pipette, transfer it to a 50mL clean volumetric flask of the same
number and fill 10mL acetylacetone solution and 10mL ammonium acetate solution to this flask. Do not
confuse the pipettes for the transfer of acetylacetone solution and ammonium acetate solution. Mix the water
solution with the acetylacetone solution and ammonium acetate solution in the same way (3 volumetric flasks
in total) and shake the solution uniform.
10) Heat the mixed solution in a water bath at 40℃ for 15 minutes. In this process, the formaldehyde will
react with the ammonium ion and acetylacetone in the ammonium acetate to generate DDL.
11) After 15 minutes, take the 3 volumetric flasks from the water bath and cool them down to the room
temperature (for 1 hour approximately) without the direct light. Turn on the spectral photometer and set the
wave length to 412nm. After the instrument operation is stable, prepare 2 colorimetric cells of 1cm optical
path, one used for reference and one used for specimen testing.
12) Fill the distilled water to one colorimetric cell, wipe the outside of the cell with the clean filter paper, open
the spectral photometer sample cell cap and place the colorimetric cell on the bracket on which the reference
colorimetric cell is placed; fill the solution used for the blank test to the other colorimetric cell, wipe the
outside of the cell with the clean filter paper and place the colorimetric cell on the bracket on which the
specimen colorimetric cell is placed. Close the sample cell cap and measure the absorbance of solution at
412nm wave length relative to that of distilled water. Then record the absorbance value as AB.
13) Determine the absorbance of all specimen test solutions relative to the distilled water in the same way and
record the absorbance value as AS.
Note: before testing any solution, wet and rinse the colorimetric cell for 3 times at least with the solution
under test.

7 Test result calculation


Calculate the formaldehyde content with the following formula:

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Q/SQR.04.096-2009

(As − AB ) × f × V × (100 + H ) ⎡ mgHCHO ⎤


formaldehyde content= × F⎢ ⎥
m × 1000 ⎣ kgatro Pr obe ⎦
Where, AS = absorbance of specimen test solution
AB = absorbance of blank test solution
f = correction factor in µg/mL
= The reciprocal of correction curve slope determined during correction (in mL/µg) (that is, f = 1/slope of
correction curve)
m= specimen mass in g
H = moisture content in %
V = volume of distilled water in the test bottle = 50mL
F = coefficient to convert to the analysis result of every kg specimen = 10
atro= completely dried specimen
Note: 1) for the individual specimen, the formaldehyde content test value can be calculated with the above
formula.
2) each spare part and material require testing two specimens. The formaldehyde content of this spare part and
material is the arithmetic average of two test values.
3) unless otherwise specified, the formaldehyde content limit of the non-metal spare part and material should
be ≤10mg/kg.

8 Test Report
The following descriptions shall be included in the test report:
1) The description of spare part and material under test, for example, the name of material or part;
2) Summary of task source (entrust);
3) Test equipment;
4) Test result: individual test value, average and report value
5) Moisture content of spare part and material under test;
6) Conclusion;
7) Report the test results to the consignor.

_________________________

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Q/SQR.04.096-2009

Prepared by:

Checked by:

Reviewed by:

Standardized by:

Approved by:

Version: 00

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