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QSQR T1-8.1-2012-En
QSQR T1-8.1-2012-En
Q/SQR.04.096-2009
Replace Q/SQR.04.096 - 2007
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
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.
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.
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
m1 − m0
H= × 100[%]
m0
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Q/SQR.04.096-2009
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Q/SQR.04.096-2009
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