GB/T 39897-2021 PDF in English
GB/T 39897-2021 (GB/T39897-2021, GBT 39897-2021, GBT39897-2021)
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Determination of volatile organic compounds and aldehydes and ketones in nonmetallic parts of vehicles
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GB/T 39897-2021: PDF in English (GBT 39897-2021) GB/T 39897-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 43.040.60
T 05
Determination of Volatile Organic Compounds and
Aldehydes and Ketones in Nonmetallic Parts of
Vehicles
ISSUED ON: MARCH 9, 2021
IMPLEMENTED ON: OCTOBER 1, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Terms and Definitions ... 4
4 Sample Preparation, Packaging, Transportation and Reception ... 6
5 Pre-treatment and Sampling Methods ... 6
6 Determination and Result Calculation ... 7
7 Test Report ... 8
Appendix A (normative) Determination Method for Volatile Organic Compounds
- Thermal Desorption / Capillary Gas Chromatography / Mass Spectrometry .. 9
Appendix B (normative) Determination Method for Aldehydes and Ketones -
Solid Phase Adsorption / High Performance Liquid Chromatography ... 15
Appendix C (normative) Sampling Method of Volatile Organic Compounds and
Aldehydes and Ketones in Nonmetallic Parts of Vehicles - Bag Method ... 20
Appendix D (normative) Sampling Method of Volatile Organic Compounds and
Aldehydes and Ketones in Nonmetallic Parts of Vehicles - Chamber Method24
Appendix E (informative) Record of Test Report on Volatile Organic Compounds
and Aldehydes and Ketones in Nonmetallic Parts of Vehicles ... 30
Determination of Volatile Organic Compounds and
Aldehydes and Ketones in Nonmetallic Parts of
Vehicles
1 Scope
This Standard specifies the terms and definitions, sample preparation, packaging,
transportation, reception, pre-treatment and sampling methods, determination and
result calculation, and test report of volatile organic compounds and aldehydes and
ketones in nonmetallic parts of vehicles.
This Standard is applicable to the sampling and determination of volatile organic
compounds and aldehydes and ketones in nonmetallic components in the passenger
compartment and luggage compartment of Category M1 and Category N1 vehicles. The
other types of vehicles may take this as a reference.
2 Normative References
The following documents are indispensable to the application of this document. In
terms of references with a specified date, only versions with a specified date are
applicable to this document. In terms of references without a specified date, the latest
version (including all the modifications) is applicable to this document.
GB/T 6388-1986 Transport Package Shipping Mark
GB/T 15089 Classification of Power-driven Vehicles and Trailers
3 Terms and Definitions
What is defined in GB/T 6388-1986 and GB/T 15089, and the following terms and
definitions are applicable to this document.
3.1 Volatile Organic Compounds
Volatile organic compounds refer to the generic term of compounds, such as: benzene,
toluene, ethylbenzene, xylene and styrene, which are measured in accordance with
Appendix A.
3.2 Aldehydes and Ketones
Aldehydes and ketones refer to the generic term of compounds, such as: formaldehyde,
Tenax tube refers to a glass or stainless-steel sampling tube with at least 200 mg of
adsorbents inside, for example, poly (di) phenylene oxide (polyphenylene oxide).
3.12 DNPH Tube
DNPH tube refers to a sampling tube filled with 2,4-dinitrophenylhydrazine (DNPH)-
coated silica gel.
3.13 PE Film
PE film refers to a type of film that is made of polyethylene and extensively applied to
industrial packaging.
4 Sample Preparation, Packaging, Transportation and
Reception
4.1 Sample Preparation
The samples shall be in the state of supply. Before delivery, the samples shall be stored
at room temperature. Meanwhile, the environmental conditions (temperature and
relative humidity) of storage shall be recorded.
4.2 Sample Packaging
4.2.1 Within a specified time after the production is offline (the time shall be negotiated
by the demand-side and the supply-side, and indicated in the test report), use non-
polluting aluminum foil and / or odorless PE film to seal and pack the samples. Then,
place them in the packaging box.
4.2.2 The packaging and shipping mark of the samples shall take Table 1 in GB/T 6388-
1986 as a reference.
4.3 Sample Transportation
During sample transportation, it is advisable to avoid direct exposure of the samples
to strong light or high-temperature environment; avoid damage to the packaging.
4.4 Sample Reception
After receiving the samples, the laboratory shall store the samples in a well-packaged
state in an environment of 23 °C ± 5 °C.
5 Pre-treatment and Sampling Methods
5.1 Pre-treatment
Appendix A
(normative)
Determination Method for Volatile Organic Compounds - Thermal
Desorption / Capillary Gas Chromatography / Mass Spectrometry
A.1 Principle
Use solid adsorbent to collect the volatile organic compounds in the air of the bag;
place the Tenax tube in the thermal desorption instrument; after being separated by
gas chromatography, use mass spectrometry for detection. Conduct qualitative
determination through the comparison with the standard mass spectrum of the target
substance to be tested and the retention time; adopt the external standard method or
internal standard method for quantitative determination.
A.2 Reagents and Materials
A.2.1 Standard sample (reference substance)
Prepare standard gas or liquid; use a constant-flow gas sampler to quantitatively
collect it in the activated sampling tube, so as to form a series of reference substances.
The analyte concentration of the series of prepared reference substances is
approximate to the concentration of the sample to be analyzed. It is also feasible to
directly use a micro-injector to take a certain volume of the prepared reference
substances with a series of concentrations; inject it into the TENAX tube; under the
condition of a nitrogen flow rate of 100 mL/min, continuously use nitrogen to blow for
1 min ~ 2 min; take it as a reference tube.
A.2.2 Carrier gas
The carrier gas shall use 99.999% high-purity helium. The carrier gas circuit shall be
equipped with purification systems, such as: oxygen and organic filters.
A.2.3 Adsorbent
The adsorbent is a solid phase with a particle size of 180 μm ~ 250 μm. Before being
installed in the tube, the adsorbent shall be activated with inert gas flow under the
maximum allowable operating temperature, cooled and sealed, and stored at a low
temperature. During use, the desorption temperature shall be lower than the activation
temperature.
A.3 Instruments and Equipment
A.5.3.1 Use a constant-flow gas sampler to respectively and accurately extract 100
mL, 400 mL, 1 L, 4 L and 10 L of 100 μg/m3 standard gas to pass through the sampling
tube; take them as a standard series. Or use a micro-injector to inject the reference
substance; take the series of standard tubes obtained through nitrogen blowing as a
standard series.
A.5.3.2 Adopt the thermal desorption gas chromatography - mass spectrometry to
analyze the standard series. Take the mass of the target component as the x-
coordinate; take the characteristic mass ion peak area (or peak height) after deducting
the blank response as the y-coordinate; draw the calibration curve. The slope of the
calibration curve is the response factor (RF); the linear correlation coefficient shall at
least reach 0.995. If the calibration curve really cannot pass through the zero point,
then, the equation of the curve shall include the intercept.
A.5.3.3 Each new calibration curve shall be analyzed and verified through a reference
substance from different sources. The reference substance shall be consecutively
analyzed for 6 times. Under the condition of a significance level of 5%, there shall be
no significant difference between the analysis result and the nominal value of the
reference substance, otherwise, correct measures shall be taken to eliminate the error
caused by reference substance from two different sources.
A.5.3.4 The daily analysis and quality control is completed by the quality control chart.
Within a certain interval, take two parallel control samples and repeat the analysis for
at least 20 times, so as to make a mean control chart (X Chart). In the daily analysis,
in accordance with the frequency of sample determination, take two parallel control
samples for simultaneous determination with the samples to be analyzed.
Successively mark the analysis results of the control samples on the control chart; in
accordance with the following rules, judge whether the analysis process is in the state
of control:
a) If this point is between the upper and lower warning lines, then, the test
process is under control and the sample analysis result is valid;
b) If this point exceeds the upper and lower warning lines, however, it is still
within the upper and lower control limits, then, this indicates that the analysis
quality has begun to deteriorate and there is a tendency of losing control. Thus,
a preliminary inspection shall be carried out and corresponding corrective
measures shall be taken;
c) If this point falls beyond the upper and lower control limits, then, the causes
shall be immediately checked and the samples shall be re-determined;
d) Although all the data are within the range of control, the continuous rise or fall
of seven points indicates that the analysis process has a tendency of losing
control. Thus, the causes shall be found out and corrected.
---Acetone is less than 0.30 μg/tube;
---Other substances are less than 0.10 μg/tube.
B.2.2 High-purity acetonitrile (mobile phase exclusive to HPLC)
UV grade purity. The mass concentration of formaldehyde shall be less than 1.5 μg/L.
Keep it away from light.
B.2.3 Standard sample (reference substance)
B.2.3.1 Use standard gas or liquid or solid to prepare standard gas of required
concentration. Use constant-flow gas sampler to quantitatively collect it in DNPH
sampling tube to form a standard series. The concentration of the analyte in the
prepared standard series is similar to the concentration of the samples to be analyzed.
During the collection, use the same flow rate as the sampling to collect the standard
gas.
B.2.3.2 2,4-dinitrophenylhydrazone liquid standard sample (reference substance) of
aldehydes and ketones may be directly purchased, or the solid standard sample
(reference substance) may also be used to prepare the standard series by yourself.
B.2.4 Filter membrane
Use 0.45 μm filter membrane for the tests.
B.3 Instruments and Equipment
Use the following instruments and equipment for determination:
a) High performance liquid chromatograph (HPLC);
b) Micro-injector;
c) Solid phase extraction device and its accessories;
d) Ultrasonic cleaner.
B.4 Sample Pre-treatment
B.4.1 Place the sampling tube on the solid phase extraction device for sample elution.
The flow direction of the eluent shall be opposite to the direction of the airflow during
sampling.
B.4.2 Accurately add 5 mL of acetonitrile to reversely elute the sampling tube; collect
the eluent in a 5 mL volumetric flask. Use 0.45 μm filter membrane to filter the eluent.
B.4.3 Use acetonitrile to reach a constant volume of 5 mL scale on the volumetric flask.
reference substance, otherwise, correct measures shall be taken to eliminate the error
caused by reference substance from two different sources.
A.5.2.5 The daily analysis and quality control is completed by the quality control chart.
Within a certain interval, take two parallel control samples and repeat the analysis for
at least 20 times, so as to make a mean control chart (X Chart). In the daily analysis,
in accordance with the frequency of sample determination, take two parallel control
samples for simultaneous determination with the samples to be analyzed.
Successively mark the analysis results of the control samples on the control chart; in
accordance with the following rules, judge whether the analysis process is in the state
of control:
a) If this point is between the upper and lower warning lines, then, the test
process is under control and the sample analysis result is valid;
b) If this point exceeds the upper and lower warning lines, however, it is still
within the upper and lower control limits, then, this indicates that the analysis
quality has begun to deteriorate and there is a tendency of losing control. Thus,
a preliminary inspection shall be carried out and corresponding corrective
measures shall be taken;
c) If this point falls beyond the upper and lower control limits, then, the causes
shall be immediately checked and the samples shall be re-determined;
d) Although all the data are within the range of control, the continuous rise or fall
of seven points indicates that the analysis process has a tendency of losing
control. Thus, the causes shall be found out and corrected.
B.5.3 Sample analysis
In accordance with the operation steps of drawing the calibration curve and the same
analysis conditions, analyze the samples.
B.6 Result Calculation
The mass concentration of the aldehydes and ketones shall be calculated in
accordance with the stipulations of 6.3.
B.7 Quality Assurance and Control
B.7.1 Interference and elimination
B.7.1.1 Avoid exposing the DNPH sampling tube directly to sunlight.
B.7.1.2 Since the formaldehyde contained in acetonitrile may be quantitatively
converted into hydrazone, the determined concentration of formaldehyde in the sample
is relatively high. Hence, in the quality control procedure, formaldehyde in acetonitrile
Appendix D
(normative)
Sampling Method of Volatile Organic Compounds and Aldehydes
and Ketones in Nonmetallic Parts of Vehicles - Chamber Method
D.1 Principle of Sampling
Place the sample in a uniformly mixed test chamber. Control the temperature, humidity
and gas exchange rate in the chamber for conditioning. After a certain time, collect the
gas in the chamber, so as to conduct qualitative and quantitative analysis on the
organic substances released by the sample.
D.2 Sampling Devices
D.2.1 Test chamber
D.2.1.1 Volume of test chamber
The volume the test chamber may be chosen between 0.5 m3 ~ 4.0 m3. The standard
test chamber has a volume of 1 m3 ± 0.05 m3 and has good air-tightness. In the test
chamber, there shall be a gas mixing device, a bracket for placing the sample (to avoid
contact between the sample and the inner wall of the chamber), and air intake and
exhaust piping, etc.
D.2.1.2 Material of chamber
The inner wall of the chamber and the bracket for placing the sample should be made
of electro-polished stainless steel. If the parts or facilities installed inside the chamber
cannot be made of electro-polished stainless steel material, then, they shall be made
of materials that have relatively weak adsorption towards the organic substances and
do not release organic substances; the surface area of the parts or facilities using these
materials cannot exceed 5% of the total surface area of the inner part of the chamber.
D.2.1.3 Air-tightness
In order to avoid uncontrollable air exchange, it is necessary to conduct air-tightness
test on the test chamber. Under the condition of applying a positive pressure of 1,000
Pa in the test chamber, it shall be ensured that the amount of air leakage per minute
is less than 0.5% of the chamber volume, or that the amount of air leakage is less than
5% of the supply air flow. In order to prevent the outside gas from entering the chamber,
it shall be ensured that the internal pressure of the test chamber is slightly higher than
the atmospheric pressure, which means it is operated under slightly positive pressure,
D.2.1.5 Chamber cleaning
By adopting suitable cleaning methods, for example, high-temperature thermal
desorption, it shall be ensured that after each test, the test chamber is thoroughly
cleaned. Before each test, a blank sample shall be collected to verify whether the
background value of the chamber satisfies the test requirements.
D.2.2 Temperature adjustment
The temperature adjustment system in the chamber shall ensure that the temperature
difference at each point inside the chamber does not exceed ± 1 °C.
D.2.3 Humidity adjustment
The humidity adjustment device shall be able to ensure that the gas entering the test
chamber has a relative humidity of 45% at 23 °C and a relative humidity of 5% at 65 °C.
In addition, during the humidity adjustment, no steam or spray can be generated.
D.2.4 Clean gas supply
D.2.4.1 The mass concentration of total volatile organic compounds in the intake air
shall not exceed 50 μg/m3; the mass concentration of single volatile organic compound
shall not exceed 5 μg/m3.
D.2.4.2 It shall be ensured that the gas exchange rate is 0.4 m3/h; the gas supply flow
rate in the chamber shall be set to 6.67 L/min ± 0.35 L/min (65 °C, ambient atmospheric
pressure), with a deviation of less than ± 5%.
D.2.5 Total hydrocarbon concentration determination device
The test chamber shall be equipped with an online hydrogen flame ionization detector
(FID) to implement real-time monitoring the total hydrocarbon concentration in the gas
of the test chamber. The maximum sampling flow of FID shall not exceed 15 mL/min.
Use N-propane as the calibration gas; use nitrogen with a purity of 99.999% as the
zero gas, or a special zero gas generator.
D.3 Preparation before Sampling
D.3.1 Chamber background
D.3.1.1 In order to assess the influence of links that might introduce pollutants on the
test, such as: the air intake, the sealing ring and the cleanliness of the test chamber,
before each test, the background concentration of the chamber shall be monitored.
The specific monitoring method is: at 65 °C, collect a background gas sample to
respectively analyze the content of target pollutants in the background gas sample.
D.3.1.2 The total mass concentration of volatile organic components shall be less than
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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