GB 31604.19-2016_English: PDF (GB31604.19-2016)
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Determination of 6-caprolactam in nylon 6 resin and its products
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GB 31604.19-2016
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Preview PDF: GB 31604.19-2016
| Standard ID | GB 31604.19-2016 (GB31604.19-2016) | | Description (Translated English) | Determination of 6-caprolactam in nylon 6 resin and its products | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 8,858 | | Date of Issue | 2016-10-19 | | Date of Implementation | 2017-04-19 | | Older Standard (superseded by this standard) | SN/T 2283-2009; GB/T 5009.125-2003; GB/T 23296.20-2009 | | Regulation (derived from) | State Health and Family Planning Commission Notice No.1516 of 2016 |
GB 31604.19-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products -
Determination of caprolactam and migration quantity
ISSUED ON. OCTOBER19, 2016
IMPLEMENTED ON. APRIL19, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword . 3
1 Scope .. 4
2 Principles .. 4
3 Reagents and materials . 4
4 Instrument and equipment .. 5
5 Analytical procedures .. 5
6 Analysis results expression . 7
7 Precision . 7
8 Others .. 7
9 Principles .. 7
10 Reagents and materials . 8
11 Instrument and equipment .. 9
12 Analytical procedures .. 9
13 Analysis results expression .. 11
14 Precision .. 11
15 Others . 11
Appendix A Liquid chromatogram of standard solution .. 12
National food safety standard -
Food contact materials and products -
Determination of caprolactam and migration quantity
1 Scope
This standard specifies determination method of caprolactam and migration
quantity in food contact materials and products.
This standard applies to determination of caprolactam and migration quantity in
food contact materials and products.
Determination of caprolactam
2 Principles
After the sample is extracted by water, the caprolactam is dissolved in extracting
solution; after filtered through filter membrane, it is detected by a high-
performance liquid chromatograph (HPLC) that is equipped with an ultraviolet
detector; use external standard method to quantify.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
grade, the water is the grade-1 water specified in GB/T 6682.
3.1 Reagents
Acetonitrile (C2H3N, CAS No. 75-05-8). Chromatographically pure.
3.2 Standards
3.2.1 Caprolactam (C6H11NO, CAS number. 105-60-2). Purity ≥ 99%, or
standard substance which is identified by national authentication and awarded
a reference material certificate.
3.3 Standard solution preparation
5.2 Preparation of sample solution
WEIGH 1.0 g (accurate to 0.0001g) of crushed samples; PLACE it into a
stoppered glass tube; after adding 10 mL of water, EXTRACT for 40 min in a
boiling water bath; when cooling to room temperature, TAKE the supernatant
into 25 mL volumetric flask. Then USE 10 mL of water to extract once again as
above; COMBINE the twice-supernatant; USE water to dilute it to the mark;
TAKE 1 mL of extracting solution through 0.45 μm filter membrane; after filtering,
it is for sample injection of high performance liquid chromatography. If the
concentration of the sample solution is beyond linear range, use water to dilute
it so that the concentration is within linear range.
5.3 Preparation of blank solution
Except for not adding sample, use the same analytical procedures, reagents
and dosage as 5.2.
5.4 Reference conditions of chromatography
5.4.1 Chromatographic column. C18-column, column-length 250 mm, inner-
diameter 4.6 mm, particle-size 5 μm.
5.4.2 Detector. UV detection wavelength 210 nm.
5.4.3 Mobile phase. acetonitrile-water (20+80).
5.4.4 Flow rate. 1.0 mL/min.
5.4.5 Injection volume. 10 μL.
5.5 Drawing of standard curve
According to the measurement conditions listed in 5.4, respectively PLACE
caprolactam standard working solution into liquid chromatograph to determine.
With the caprolactam concentration of standard working solution as abscissa,
in milligrams per liter (mg/L), AND the corresponding peak area of caprolactam
as vertical axis, DRAW a standard working curve. See Figure A.1 for the
standard chromatogram.
5.6 Determination of sample solution
According to the conditions listed in 5.4, PLACE the sample solution (5.2) and
the blank solution (5.3) into liquid chromatograph to determine; OBTAIN the
peak area of caprolactam; DEDUCT blank value.
simulant test solution can not be immediately carried out the next test, the food
simulant test solution shall be stored in refrigerator at 4 °C.
The resulting food simulant test solution shall be cooled or returned to room
temperature before proceeding to the next test.
12.2 Preparation of sample solution
12.2.1 Processing of food simulants that are water-based, acidic and
alcoholic
USE graduated pipet to pipette 1 mL of food simulants that are water-based,
acidic and alcoholic obtained from the migration test; FILTER through 0.45 μm
microporous membrane to wait for determining.
12.2.2 Processing of oil-based food simulants
WEIGH 8.0 g (accurate to 0.01g) of olive oil obtained from the migration test;
PLACE it into separatory funnel; ADD 1.6 mL of water; MIX it uniformly; ADD
15 mL of n-hexane; MIX it uniformly; ADD 8 mL of ethanol-water solution (1+2);
VIBRATE it for 10 min; LET it stand for 30 min to separate the two-phase; MOVE
5 mL of lower-layer water solution; FILTER through cotton wool and 0.45 μm
microporous membrane to wait for determining.
12.3 Preparation of blank solution
Except for not adding sample, use the same analytical procedures, reagents
and dosage as 12.2.
12.4 Reference conditions of chromatography
12.4.1 Chromatographic column. C18-column, column-length 250 mm, inner-
diameter 4.6 mm, particle-size 5 μm.
12.4.2 Detector. UV detection wavelength 210 nm.
12.4.3 Mobile phase. acetonitrile-water (20+80).
12.4.4 Flow rate. 1.0 mL/min.
12.4.5 Injection volume. 10 μL.
12.5 Drawing of standard curve
According to the conditions listed in 12.4, respectively PLACE standard working
solution of food simulants that are water-based, acidic and alcoholic, and
standard working solution of oil-based food simulants into liquid chromatograph
to determine. With the caprolactam concentration of food simulants as abscissa,
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