GB/T 33345-2016 PDF in English
GB/T 33345-2016 (GB/T33345-2016, GBT 33345-2016, GBT33345-2016)
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Determination of short chain chlorinated paraffins in electrical and electronic products -- Gas chromatography-mass spectrometry
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Standards related to: GB/T 33345-2016
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GB/T 33345-2016: PDF in English (GBT 33345-2016) GB/T 33345-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 31.020
L 10
Determination of short chain chlorinated paraffins in
electrical and electronic products - Gas
chromatography-mass spectrometry
ISSUED ON. DECEMBER 13, 2016
IMPLEMENTED ON. JULY 01, 2017
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Terms and definitions... 4
4 Principle... 5
5 Reagents or materials... 5
6 Equipment... 5
7 Samples... 6
8 Test procedure... 6
9 Test... 7
10 Test data processing... 10
11 Precision... 11
Appendix A (Informative) Determination of short-chain chlorinated paraffins in
electronic and electrical products - Gas chromatography-electron
bombardment mass spectrometry... 12
Appendix B (Informative) Determination of short-chain chlorinated paraffins in
electronic and electrical products - Gas chromatography... 15
Appendix C (Informative) Standard substance test spectrum of short-chain
chlorinated paraffin... 19
Appendix D (Informative) Theoretical chlorine content... 20
Information security technology - SM4 block cipher
algorithm
Warning - Personnel using this standard shall have practical experience
in formal laboratory work. This standard does not point out all possible
safety issues. The user is responsible for taking appropriate safety and
health measures and ensuring compliance with the conditions stipulated
by relevant national laws and regulations.
1 Scope
This standard specifies the qualitative and quantitative methods for the
determination of short-chain chlorinated paraffins in electronic and electrical
products by gas chromatography-electron capture negative chemical ion
source mass spectrometer.
This standard applies to the determination of short-chain chlorinated paraffins
in electronic and electrical products, which has a limit of quantification of 100
mg/kg. Gas chromatography-electron capture negative chemical ion source
mass spectrometry is applicable to the determination of short-chain chlorinated
paraffins in electronic and electrical products which has a chlorine atom number
greater than or equal to 5.When determining short-chain chlorinated paraffins
which have chlorine atoms less than 5 in electrical and electronic products, it
may refer to the method in Appendix A or Appendix B.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 26572-2011 Requirements of concentration limits for certain restricted
substances in electrical and electronic products
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
6.3 Soxhlet extraction device, equipped with condenser and heating device, or
use an automatic Soxhlet extraction device.
6.4 Crushing device. which is equipped with cutting machines or scissors,
grinders, freezing crushing facilities and other devices, mainly used for crushing
samples.
6.5 Rotary evaporator that can be vacuumed.
6.6 Centrifuge, the speed of which is greater than or equal to 4000 r/min.
7 Samples
The polymer materials used in electronic and electrical products or the
analytical samples obtained according to the separation method in Appendix A
of GB/T 26572-2011 are first crushed to a particle size of less than 1 cm, then
crushed by the frozen crusher or equivalent equipment (6.4) to the grain size of
less than 1 mm.
8 Test procedure
8.1 Sample extraction
Use Soxhlet extraction method to process the sample, using the steps as
follows.
a) Weigh 0.5 g of the crushed sample (accurate to 0.0001 g); place it in the
cellulose filter paper cartridge after extraction and washing; then place it
in the installed Soxhlet extraction device;
b) Add about 50 mL of toluene (5.2) to the Soxhlet extraction device; the total
number of extraction cycles is not less than 60;
c) Concentrate the extract in [8.1.b)] by rotary evaporation in a water bath at
80 °C to about 1 mL. If the extract is more viscous, it can be processed
directly according to [8.2.a)]; otherwise it can be transferred to a 10.0 mL
volumetric flask; the distillation flask shall be rinsed at least 3 times by the
use of n-hexane (5.1). The rinse solution can be combined into a 10.0 mL
volumetric flask. After making the volume of n-hexane (5.1) to the mark,
follow [8.2.b)] to process it.
It is recommended that no sample is added during the extraction and cleaning
process of the cellulose filter paper cartridge; the operation shall be performed
according to the extraction procedure [8.1.b)].
Depending on the instrument used, the optimal analysis conditions may also be
different, so it is impossible to give general parameters for gas chromatography-
electron capture negative chemical ion source analysis. The set parameters
shall ensure the effective separation and determination of the tested
components. The parameters given below have proven to be feasible.
a) Chromatographic column. 15 m × 0.25 mm (inner diameter) × 0.1 μm (film
thickness), the stationary phase is 5% phenyl, 95% dimethyl polysiloxane
quartz capillary column or equivalent;
b) Inlet temperature. 280 °C;
c) Chromatographic column temperature program. Hold at 100 °C for 1 min;
then increase the temperature in a programmed manner to 300 °C at
20 °C/min; hold for 9 minutes;
d) Transmission line temperature. 300 °C;
e) Carrier gas. Helium, which has a purity greater than or equal to 99.999%;
f) Carrier gas flow rate. 1 mL/min;
g) Injection volume. 1.0 μL;
h) Sample injection mode. Adopt splitless sample injection; switch to split
mode after 1 min (split ratio 20.1);
i) Ion source temperature. 160 °C;
j) Reagent gas. Methane;
k) Reagent gas flow rate. 2.0 mL/min;
l) Ionization method. Electron capture negative chemical source ionization;
m) Determination method. Select ion scan mode, see Table 1 for qualitative
and quantitative ions;
n) Solvent delay. 5 min.
Appendix A
(Informative)
Determination of short-chain chlorinated paraffins in electronic and
electrical products - Gas chromatography-electron bombardment mass
spectrometry
Preprocess the sample according to Chapter 7 and Chapter 8, to obtain the
specimen to be tested. Then use a gas chromatography-electron bombardment
mass spectrometer to determine the concentration of short-chain chlorinated
paraffin in the specimen to be tested. Use the characteristic ion peak and
retention time to perform qualitative analysis; carry out quantitative analysis
based on the linear relationship between the corresponding peak area and
concentration of total short-chain chlorinated paraffin.
A.1 Gas chromatography electron impact mass spectrometry conditions
Depending on the instrument used, the optimal analysis conditions may also be
different, so it is impossible to give general parameters of gas chromatography
electron bombardment mass spectrometry. The set parameters shall ensure the
effective separation and determination of the tested components. The
parameters given below have proven to be feasible.
a) Chromatographic column. 15 m × 0.25 mm (inner diameter) × 0.1 μm (film
thickness), the stationary phase is 5% phenyl, 95% dimethyl polysiloxane
quartz capillary column or equivalent;
b) Chromatographic column temperature program. keep at 100 °C for 1 min,
then program to raise temperature to 300 °C at 20 °C/min, keep it for 5
min;
c) Sample inlet temperature. 280 °C;
d) Chromatography-mass spectrometry interface temperature. 300 °C;
e) Ion source and its temperature. Electron bombardment ion source,
temperature. 250 °C;
f) Carrier gas. Helium, with a purity greater than or equal to 99.999%, 1
mL/min;
g) Ionization method. EI;
h) Ionization energy. 70 eV;
Appendix B
(Informative)
Determination of short-chain chlorinated paraffins in electronic and
electrical products - Gas chromatography
Preprocess the sample according to Chapter 7 and Chapter 8 to obtain the
specimen to be tested; then use a gas chromatograph equipped with an
electron capture detector to determine the concentration of the short-chain
chlorinated paraffin in the specimen to be tested; use the retention time for
qualitative analysis; carry out quantitative analysis based on the linear
relationship between the corresponding peak area and concentration of short-
chain chlorinated paraffin. When using this method and it is find in the test
process that the chromatogram of the tested specimen has interference peaks
of medium chain chlorinated paraffin, it is recommended to use other methods
of this standard for testing.
B.1 Gas chromatography conditions
Depending on the instrument used, the optimal analysis conditions may also be
different, so it is impossible to give general parameters of gas chromatography.
The set parameters shall ensure the effective separation and determination of
the tested components. The parameters given below have proven to be feasible.
a) Chromatographic column. 30 m × 0.25 mm (inner diameter) × 0.25 μm
(film thickness), the stationary phase is 5% phenyl, 95% dimethyl
polysiloxane quartz capillary column or equivalent;
b) Chromatographic column temperature program. keep at 100 °C for 3 min;
then program to raise temperature to 300 °C at 25 °C/min; keep for 10 min;
c) Sample inlet temperature. 280 °C;
d) Carrier gas. nitrogen, purity greater than or equal to 99.99%, 1 mL/min;
e) Sampling mode. Pulsed splitless sample injection;
f) Sample injection volume. 1.0 μL;
g) Detector and its temperature. Electron capture detector (ECD),
temperature at 180 °C.
B.2 Qualitative and quantitative analysis by gas chromatography
Standard solution preparation. Use n-hexane (5.1) as the solvent, to prepare
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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