GB/T 29786-2013 English PDF (GBT29786-2013)

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GB/T 29786-2013: Determination of phthalates in electrical and electronic equipment -- Gas chromatography-mass spectrometry
GB/T 29786-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 31.020
L 10
Determination of phthalates in electrical and
electronic equipment - Gas chromatography-mass
spectrometry
ISSUED ON. OCTOBER 10, 2013
IMPLEMENTED ON. FEBRUARY 01, 2014
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Principle... 4
4 Reagents... 4
5 Instruments... 5
6 Sample preparation... 5
7 Analysis steps... 5
8 Result calculation... 7
9 Low limits of determination... 7
10 Recovery rate... 8
11 Precision... 8
Annex A (normative) Basic information of 12 common phthalates... 9
Annex B (informative) Table of quantitative and qualitative selective ion for
phthalates... 10
Annex C (informative) Chromatograms of reference materials of phthalates. 12
Determination of phthalates in electrical and
electronic equipment - Gas chromatography-mass
spectrometry
1 Scope
This Standard specifies the gas chromatography-mass spectrometry (GC-MS)
method for the determination of 12 kinds of phthalates (see Annex A for specific
names) in electrical and electronic products.
This Standard applies to the determination of the content of phthalates in
polymer materials in electronic and electrical products.
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/Z 20288-2006 General requirements for sample separation of hazardous
substances in electrical and electronic products
3 Principle
Use ethyl acetate as the extraction solvent, and perform Soxhlet extraction or
ultrasonic extraction. After the volume of the extract is constant, it is determined
by gas chromatography-mass spectrometry, and quantified by external
standard method.
4 Reagents
Unless otherwise stated, only use analytical reagents.
4.1 Ethyl acetate. chromatographically pure.
4.2 Reference materials of phthalates. purity ≥ 95 %.
filtrate is to be tested. For GC-MS (5.1) determination.
7.1.2 Ultrasonic extraction
WEIGH 0.2 g of sample (to the nearest 0.1 mg); PLACE it in a 50 mL
Erlenmeyer flask; ADD 30 mL of ethyl acetate (4.1); PERFORM ultrasonic
extraction for 20 min. TRANSFER the extract to a 100 mL round-bottomed flask;
KEEP the sample in the Erlenmeyer flask; and then ADD 30 mL of ethyl acetate
and PERFORM ultrasonic extraction for 20 min. REPEAT the above steps for
a total of 3 extractions. COMBINE the extracts; CONCENTRATE the extracts
with a rotary evaporator (5.4) to about 4 mL; TRANSFER to a 10 mL volumetric
flask. WASH with 5 mL of ethyl acetate; COMBINE the washing solution into
the volumetric flask; DILUTE with ethyl acetate to constant volume. After
filtering with organic phase filter membrane (5.5), the filtrate is to be tested. For
GC-MS (5.1) determination.
7.2 Determination
7.2.1 Reference conditions for gas chromatography-mass spectrometry
a) Chromatographic column. DB-5MS capillary column 30 m × 0.25 mm ×
0.25 μm, or equivalent;
b) Sample inlet temperature. 280 °C;
c) Interface temperature. 290 °C;
d) Heating program. the initial temperature is 60 °C, maintain for 1 min;
increase to 280 °C at 30 °C/min, maintain for 10 min;
e) Ion source temperature. 230 °C;
f) Carrier gas. helium (4.5), flow rate of 1.2 mL/min;
g) Sample injection mode. splitless injection, open the valve after 1 min;
h) Ionization method. electron ionization source (EI);
i) Electron energy. 70 eV;
j) Measurement method. scan (scan range of 50 amu ~ 500 amu) for
qualitative analysis; selective ion monitoring (SIM) for quantitation.
7.2.2 Qualitative and quantitative analysis
Analyze according to the above conditions. According to the retention time of
the chromatographic peak and refer to the qualitative ions of phthalates in
Annex B for qualitative analysis; refer to the quantitative ions in Annex B, using