GB/T 43011-2023 PDF English
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Paper, board and paper products - Determination of chloropropanol content
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GB/T 43011-2023: Paper, board and paper products - Determination of chloropropanol content---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT43011-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 85.010
CCS Y 30
Paper, board and paper products - Determination of
chloropropanol content
ISSUED ON: SEPTEMBER 7, 2023
IMPLEMENTED ON: APRIL 1, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle ... 4
5 Reagents and materials ... 4
6 Apparatus ... 5
7 Analytical procedure ... 6
8 Result calculation ... 9
9 Precision ... 10
10 Detection limit and quantitation limit ... 10
11 Test report ... 11
Appendix A (Informative) Ion chromatograms and mass spectra of 1,3-DCP and
3-MCPD measured by GC-MS ... 12
Paper, board and paper products - Determination of
chloropropanol content
1 Scope
This document describes a method for the determination of content of 1,3-dichloro-2-
propanol (1,3-DCP) and 3-chloro-1,2-propanediol (3-MCPD) in paper, board and paper
products.
This document is applicable to all kinds of paper, board and paper products; is used as
a reference for pulps and papermaking wet strength agents.
2 Normative references
The contents of the following documents, through normative references in this text,
constitute indispensable provisions of this document. Among them, for dated references,
only the edition corresponding to that date applies to this document. For undated
references, the latest edition (including all amendments) applies to this document.
GB/T 462 Paper, board and pulps - Determination of moisture content of analytical
sample
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principle
After the sample is chopped, mixed or diluted, add a deuterium-labeled internal
standard solution to the specimen; use sodium chloride solution (20%) to extract it.
After concentration, use heptafluorobutyrylimidazole to derivatize it; use gas
chromatography-mass spectrometry for detection AND the internal standard method for
quantification.
5 Reagents and materials
Unless otherwise specified, use only analytically pure reagents.
6.7 Nylon microporous filter membrane: Pore size is 0.22 μm.
6.8 Vortex mixer.
6.9 Pipette: 100 μL and 1000 μL.
6.10 Other commonly-used laboratory glassware.
7 Analytical procedure
7.1 Preparation of standard solutions
7.1.1 Chloropropanol mixed standard stock solution (1000 mg/L): Respectively weigh
50 mg (accurate to 0.1 mg) of 1,3-DCP standard (5.9) and of 3-MCPD standard (5.10);
use ethyl acetate (5.3) to dissolve and transfer to a 50 mL volumetric flask; use ethyl
acetate (5.3) to dilute to the mark; seal and store at 0 °C~4 °C. The storage period is 6
months.
7.1.2 Chloropropanol mixed standard intermediate solution (10 mg/L): Accurately
pipette 0.1 mL of chloropropanol mixed standard stock solution (7.1.1) into a 10 mL
volumetric flask; use ethyl acetate (5.3) to dilute to the mark; seal and store at 0 °C~4 °C.
The storage period is 3 months.
7.1.3 Chloropropanol mixed standard intermediate solution (1 mg/L): Accurately
pipette 0.1 mL of chloropropanol mixed standard stock solution (7.1.1) into a 100 mL
volumetric flask; use ethyl acetate (5.3) to dilute to the mark; seal and store at 0 °C~4 °C.
The storage period is 3 months.
7.1.4 Chloropropanol internal standard mixed standard stock solution (1000 mg/L):
Respectively weigh 50 mg (accurate to 0.1 mg) of 1,3-DCP-D5 standard (5.11) and of
3-MCPD-D5 standard (5.12); use ethyl acetate (5.3) to dissolve and transfer to a 50 mL
volumetric flask; use ethyl acetate (5.3) to dilute to the mark; seal and store at 0 °C~4 °C.
The storage period is 6 months.
7.1.5 Chloropropanol internal standard mixed standard intermediate solution (10 mg/L):
Accurately pipette 0.1 mL of chloropropanol internal standard mixed standard stock
solution (7.1.4) into a 10 mL volumetric flask; use ethyl acetate (5.3) to dilute to the
mark; seal and store at 0 °C~4 °C. The storage period is 3 months.
7.1.6 Chloropropanol standard working solutions: Respectively pipette 0.01 mL, 0.05
mL, 0.1 mL, 0.2 mL, 0.4 mL, 0.8 mL, 1.6 mL of chloropropanol mixed standard
intermediate solution (1 mg/L) (7.1.3) AND 0.32 mL of chloropropanol mixed standard
intermediate solution (10 mg/L) (7.1.2) INTO transparent glass tubes with a stopper
(cap) of appropriate volume (5 mL or 10 mL) with good airtightness. Respectively add
20 μL of chloropropanol internal standard mixed standard intermediate solution (10
mg/L) (7.1.5); add n-hexane (5.2) to 2 mL and mix well. Prepare a series of standard
working solutions containing 10 ng, 50 ng, 100 ng, 200 ng, 400 ng, 800 ng, 1600 ng,
and 3200 ng of 1,3-DCP and 3-MCPD respectively; in which the mass of each
deuterated chloropropanol is 200 ng. Standard solutions of other concentrations can
also be prepared as needed. Prepare the standard working solution at the time of use.
7.2 Sample processing
For the sample of paper, board, paper products and pulp, weigh about 10 g of the sample;
cut it into small pieces of about 5 mm×5 mm. After mixing well, accurately weigh 1.0
g (accurate to 0.0001 g) of the specimen into a glass test tube (6.5). At the same time,
take another specimen from the sample; measure the moisture content according to
GB/T 462.
For the sample of papermaking wet strength agents, if the chloropropanol content is
high, in order to ensure the representativeness of the sampling, use water (5.1) to dilute
the sample appropriately step by step. Then accurately weigh 1.0 g (accurate to 0.0001
g) of the diluted and mixed specimen into a glass test tube (6.5), so that the
concentration of chloropropanol in the weighed specimen is within the range of the
standard working solution. If the chloropropanol content of the papermaking wet
strength agent sample is low, it is possible to directly weigh 1.0 g (accurate to 0.0001
g) of the sample into a glass test tube (6.5).
7.3 Test procedure
7.3.1 Extraction: Add 15 mL of sodium chloride solution (20%) (5.6) AND 20 μL of
chloropropanol internal standard mixed standard intermediate solution (10 mg/L) (7.1.5)
into the test tube containing the sample. After thorough mixing, use an ultrasonic
cleaner (6.3) to extract at 40 °C for 30 min, to obtain the extraction solution. During the
ultrasonic extraction process, the test tube mouth should be kept sealed until
purification.
Note: If the sample contains water-absorbing resin, increase the volume of sodium chloride solution
(20%) appropriately.
7.3.2 Purification: Weigh the macroporous diatomite (5.7) whose mass is equivalent to
half the mass of the extraction solution (7.3.1); load it into a chromatographic column
(5.8). Pour the extraction solution (7.3.1) into the diatomite chromatographic column
and balance for 10 min. Use 10 mL of n-hexane (5.2) to rinse and discard the rinsing
solution. Then use 18 mL of ethyl acetate (5.3) to elute; collect the eluent in a test tube.
Add 3 g of anhydrous sodium sulfate (5.4) into the test tube; after letting it stand for 10
min, transfer the eluent (discard the anhydrous sodium sulfate part) to another clean
stoppered test tube. Concentrate the eluent to nearly dryness by blowing nitrogen; add
2 mL of n-hexane (5.2) to reconstitute; wait for derivatization.
Note: The volume of the eluent after concentration by nitrogen blowing is approximately 0.5 mL.
7.3.3 Derivatization: Quickly add 0.04 mL of heptafluorobutyrylimidazole (5.5) to the
purification solution (7.3.2); immediately cover the test tube plug; mix by vortex for 30
s; incubate in a 70 °C thermostat water bath (6.4) for 20 min; remove and cool to room
temperature. Add 2 mL of sodium chloride solution (20%) (5.6); mix by vortex for 1
min to separate the water phase and n-hexane phase. Let it stand for a while until the
water phase becomes clear; transfer the n-hexane phase; add about 0.3 g of anhydrous
sodium sulfate (5.4) to dry it. Pass the dried n-hexane phase test solution through a
nylon microporous filter membrane (6.7); then transfer it to the injection bottle for gas
chromatography-mass spectrometry. At the same time, derivatize the chloropropanol
standard working solution (7.1.6).
7.3.4 Blank test: Except that no sample is added, the blank test is carried out in
accordance with 7.3.1~7.3.3.
7.4 Instrument reference conditions
7.4.1 Reference conditions for gas chromatography
The following operating conditions have been found to be suitable for testing:
a) Chromatographic column: Weakly polar capillary gas chromatography-mass
spectrometry column containing 5% phenyl-methylpolysiloxane (column length
is 30 m; inner diameter is 0.25 mm; film thickness is 0.25 μm); or one with
equivalent performance;
b) Carrier gas: Helium (purity >99.999%); flow rate is 1.0 mL/min;
c) Inlet temperature: 250 °C;
d) Injection volume: 1 μL; splitless injection. Splitless time is 0.5 min. Solvent delay
time is 5 min;
e) Programmed temperature rise: Keep at 50 °C for 1 min; raise to 90 °C at 2 °C/min;
then raise to 270 ℃ at 40 ℃/min; maintain for 5 min.
7.4.2 Reference conditions for mass spectrometry
The following operating conditions have been found to be suitable for testing:
a) Ion source: Electron impact ion source (EI);
b) Ionization energy: 70 eV;
c) Ion source temperature: 250 °C;
d) Transmission line temperature: 280 °C;
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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