GB/T 39110-2020 (GB/T39110-2020, GBT 39110-2020, GBT39110-2020) & related versions
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Consumer product -- Plastics -- Rapid screening of phthalates
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GB/T 39110-2020
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GBT 39110-2020
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GB/T 39110-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.120
Y 28
Consumer product - Plastics - Rapid screening of
phthalates
ISSUED ON: OCTOBER 21, 2020
IMPLEMENTED ON: OCTOBER 21, 2020
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 Reagents ... 5
5 Instruments and equipment... 5
6 Liquid film method ... 5
7 Solid sample injection method ... 9
Annex A (normative) 6 phthalate plasticizers involved in this Standard ... 13
Annex B (informative) Selected ion monitoring chromatograms of 6 plasticizer
standard products ... 14
Consumer product - Plastics - Rapid screening of
phthalates
SAFETY WARNING: The use of tetrahydrofuran and dichloromethane
must be carried out in a fume hood.
1 Scope
This Standard specifies rapid screening methods for 6 kinds of phthalate
plasticizers in consumer plastic materials: dibutyl phthalate (DBP), butyl benzyl
phthalate (BBP), di(2-ethyl)hexyl phthalate (DEHP), di-n-octyl phthalate
(DNOP) , diisononyl phthalate (DINP) and diisodecyl phthalate (DIDP)
(hereinafter referred to as 6 plasticizers, see Annex A for details), including
liquid film method and solid sample injection method.
This Standard is applicable to rapid screening of 6 plasticizers in consumer
product that contains PVC material. Liquid film method is applicable to
qualitative and semi-quantitative analysis of plasticizers. Solid sample injection
method is applicable to rapid testing of plasticizers that do not have strict
requirements on accuracy.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 1844.1-2008, Plastics - Symbols and abbreviated terms - Part 1: Basic
polymers and their special characteristics
GB/T 1844.3-2008, Plastics - Symbols and abbreviated terms - Part 3:
Plasticizers
GB/T 2035-2008, Terms and definitions for plastics
3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T
1844.1-2008, GB/T 1844.3-2008 and GB/T 2035-2008 apply.
Take a certain mass of sample to be tested. Crush at low temperature or cut to
less than 2mm×2mm. Mix well. Accurately weigh two portions of samples,
100mg for each portion.
6.2.2 Sample extraction
Place the sample in a stoppered glass centrifuge tube. Add 3.0mL of
tetrahydrofuran (4.3). Conduct ultrasonic extraction for 20min until the sample
is fully dissolved. Add 7.0mL of methanol (4.4). Leave still. Separate out and
precipitate PVC. After centrifugation, take the supernatant and place it in the
sample cup for testing.
6.3 Determination
6.3.1 Reference working conditions for thermal cracker
Reference working conditions for thermal cracker are as follows:
a) Cracking furnace temperature: the initial temperature is 200°C; increase
to 300°C at 20°C/min, to 340°C at 5°C/min; maintain 1min;
b) Interface temperature: 320°C.
6.3.2 Reference working conditions for GC-MS
Reference working conditions for GC-MS are as follows:
a) Chromatographic column: capillary column; the stationary phase is 5%
diphenyl dimethyl polysiloxane, PY UA-5 (30m×250μm×0.25μm) or
equivalent;
b) Program temperature rise: 180°C; maintain for 1min, increase to 300°C at
20°C/min; maintain for 8min;
c) Carrier gas: helium; purity is ≥99.999%; constant pressure mode;
d) Inlet temperature: 300°C;
e) Sample injection mode: split injection, with split ratio of 20:1;
f) Chromatography-mass spectrometry interface temperature: 280°C;
g) Ion source: electron ionization source EI; ion source temperature is 230°C;
h) Electron energy: 70eV;
i) Mass analyzer: quadrupole mass analyzer;
j) Scan mode: select ion monitoring (SIM) mode to quantify;
When performing sample determination, if the retention time of the detected
chromatographic peak is consistent with the standard, and in the sample mass
spectrum after subtracting the background, all selected ions appear, and the
abundance ratio is consistent with the abundance ratio of the standard, THEN
it can be judged that the corresponding plasticizer exists in the sample.
6.5 Quantitative analysis
According to the content of the test substance in the test solution, select
standard working solutions with similar concentrations. Under the same
conditions, test the standard working solution and test solution separately. The
response value of the plasticizer to be measured in the standard working
solution and the test solution shall be within the linear range of the instrument
detection. If the detection response value of the test solution exceeds the linear
range of the instrument detection, it can be appropriately diluted and measured.
Use external standard method to conduct quantitative analysis. In the
chromatogram, select the appropriate quantitative ion for peak area integration.
DINP and DIDP shall be integrated after leveling the baselines of all isomers of
chromatographic peak groups respectively. Calculate the total area.
6.6 Result calculation
The content of each plasticizer in the sample is calculated according to formula
(1):
Where,
Xi - The content of a certain plasticizer i in the sample, in milligrams per
kilogram (mg/kg);
c - The mass concentration of a certain plasticizer i in the extract obtained
from the calibration curve, in milligrams per liter (mg/L);
V - The volume of extract, in milliliters (mL);
m - The weighed sample mass, in milligrams (mg).
The calculation result is reserved to integer digits. Keep three significant figures.
6.7 Detection limit, lower limit of quantification, recovery rate and
precision
6.7.1 Detection limit and lower limit of quantification
7.3.2 Reference working conditions for GC-MS
Reference working conditions for GC-MS are as follows:
a) Chromatographic column: capillary column; the stationary phase is 5%
diphenyl dimethyl polysiloxane, PY UA-5 (30m×250μm×0.25μm) or
equivalent;
b) Program temperature rise: 180°C; maintain 1min; increase to 300°C at
20°C/min; maintain 8min;
c) Carrier gas: helium; purity is ≥99.999%; constant pressure mode;
d) Inlet temperature: 300°C, with split ratio of 20:1;
e) Chromatography-mass interface temperature: 280°C;
f) Ion source: electron ionization source EI; ion source temperature is 230°C;
g) Electron energy: 70eV;
h) Mass analyzer: quadrupole mass analyzer;
i) Scan mode: select ion monitoring (SIM) mode to quantify;
j) Solvent delay: 3min;
k) Gain factor: 1.00.
7.3.3 Calibration working curve
Use the injection needle to transfer 1μL, 2μL, 4μL, 8μL, 10μL of the plasticizer
standard solution (4.1) into the sample cup. In order of low to high content, use
for determination by gas-mass spectrometer to obtain the standard series of
which the contents of BBP, DBP, DEHP, DNOP are 0.5μg, 1.0μg, 2.0μg, 4.0μg,
5.0μg and DINP, DIDP contents are 5μg, 10μg, 20μg, 40μg, 50μg. Use the
plasticizer content as the abscissa and the quantitative ion peak area as the
ordinate to draw a standard working curve.
The sample to be tested is directly tested on the machine under the same
conditions.
7.3.4 Blank test
Analyze the sample with high concentration of analyte. Analyze the blank
sample, that is, use the empty sample cup without samples to test until the
background concentration of each plasticizer drops to 30mg/kg or lower. In
order to reduce the blank value, it is necessary to ensure the cleanliness of all
tools used in sample preparation.
......
| Standard ID | GB/T 39110-2020 (GB/T39110-2020) | | Description (Translated English) | Consumer product -- Plastics -- Rapid screening of phthalates | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | Y28 | | Classification of International Standard | 13.120 | | Word Count Estimation | 14,114 | | Date of Issue | 2020-10-21 | | Date of Implementation | 2020-10-21 | | Drafting Organization | Shandong Institute of Product Quality Inspection, China Academy of Inspection and Quarantine, Anhui Jihong Material Technology Co., Ltd., Louis Ansett (Beijing) Technology and Trade Co., Ltd., Qingdao Zhongrui Intelligent Instrument Co., Ltd., China National Institute of Standardization, Shandong Analysis Testing Center, Guangzhou Anno Technology Co., Ltd., Beijing Product Quality Supervision and Inspection Institute, Shandong Yilala Clothing Co., Ltd. | | Administrative Organization | National Consumer Product Safety Standardization Technical Committee (SAC/TC 508) | | Proposing organization | National Consumer Product Safety Standardization Technical Committee (SAC/TC 508) | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration |
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