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GB 5009.242-2017 English PDF (GB5009.242-2017)

GB 5009.242-2017 English PDF (GB5009.242-2017)

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GB 5009.242-2017: Food safety national standard -- Determination of manganese in food

This Standard specifies three determination methods for manganese in food, namely, flame atomic absorption spectrometry, inductively coupled plasma emission spectrometry, and inductively coupled plasma mass spectrometry.
GB 5009.242-2017
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Manganese in Food
ISSUED ON. APRIL 06, 2017
IMPLEMENTED ON. OCTOBER 06, 2017
Issued by. National Health and Family Planning Commission of PRC;
China Food and Drug Administration.
3. No action is required - Full-copy of this standard will be automatically & immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical Procedures ... 6
6 Expression of Analytical Results ... 8
7 Precision ... 8
8 Others ... 8
Appendix A Specimen Digestion Reference Conditions ... 10
Foreword
This Standard replaced the determination parts of magnesium in the following standards such as GB/T 5009.90-2003 Determination of iron, Magnesium and Manganese in Foods, GB 5413.21-2010 National Food Safety Standard Determination of Calcium, Iron, Zinc, Sodium, Potassium, Magnesium, Copper and Manganese in Foods for Infants and Young Children, Milk and Milk Products, GB/T 14609-2008 Inspection of Grain and Oils - Determination of Copper, Iron, Manganese, Zinc, Calcium, Magnesium in Cereals and Derived Products by Atomic Absorption and Flame Spectrophotometry, GB/T 23545-2009 Determination of Manganese in White Wine - Inductively Coupled Plasma Atomic Emission Spectrometry, GB/T 18932.11- 2002 Method for Determination of Potassium, Phosphorus, Iron, Calcium, Zinc, Aluminum, Sodium, Magnesium, Boron, Manganese, Copper, Barium, Titanium, Vanadium, Nickel, Cobalt and Chromium in Honey ?€? Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), GB/T 18932.12-2002 Method for the Determination of Potassium, Sodium, Calcium, Magnesium, Zine, Iron, Copper, Manganese, Chromium, Lead, Cadmium Contents in Honey - Atomic Absorption Spectrometry, and NY/T 1653-2008 Determination for Mineral Elements In Vegetables, Fruits and Derived Products by ICP - AES Method.
Compared with the above-mentioned standards, this Standard has the major changes as follows.
--- Modified the standard name into ?€?National Food Safety Standard ?€? Determination of Manganese in Food?€?;
--- Modified the contents in the specimen preparation part;
--- Modified the contents in the specimen digestion part;
--- Modified the inductively coupled plasma emission spectrometry as the second method, the inductively coupled plasma mass spectrometry as the third method as the third method.
--- Added the method?€?s limit of detection and quantification limit;
--- Added the appendix.
National Food Safety Standard -
Determination of Manganese in Food
1 Scope
This Standard specifies three determination methods for manganese in food, namely, flame atomic absorption spectrometry, inductively coupled plasma emission spectrometry, and inductively coupled plasma mass spectrometry.
This Standard is applicable to the determination of manganese in food.
The First Method of Flame Atomic Absorption Spectrometry
2 Principle
After the digestion treatment, inject the specimen into the atomic absorption spectrometer; after flame atomization, the manganese absorbs 279.5nm resonance line; under certain concentration range, its absorbance value is proportional to the manganese content; then quantify through comparison with the standard series. 3 Reagents and Materials
Unless otherwise is specified, the reagents used in this method shall be guarantee reagent; while water used in this method shall be Class-II water stipulated in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Perchloric acid (HClO4).
3.2 Reagents preparation
3.2.1 Mixed acid [perchloric acid + nitric acid (1+9)]. take 100mL of perchloric acid; slowly add 900mL of nitric acid; mix evenly.
3.2.2 Nitric acid solution (1+99). take 10mL of nitric acid; slowly add 990mL of water; 5.2.2 Digestion method of pressure tank
Take 0.3g~1g (accurate to 0.001g) of specimen into the Teflon pressure digestion inner tank; firstly, heat the sample contained ethanol or carbon dioxide at low temperature on the electric hot plat to remove the ethanol or carbon dioxide; add 5mL of nitric acid; cover it to stand for 1h or stay overnight; tighten the outer tank; place into the constant- temperature drying oven for digestion (the digestion condition can refer to Table A.1). Take out inner tank after cooling; place on the adjustable temperature-control electric hot plate; expel acid at 120??C~140??C to near dryness; use water to make constant volume to 25mL or 50mL; mix evenly for spare-use; meanwhile do the blank test. 5.2.3 Wet digestion method
Take 0.5g~5g (accurate to 0.001g) of specimen into the glass vessel or Teflon digestion vessel; firstly, heat the sample contained ethanol or carbon dioxide at low temperature on the electric hot plate to remove the ethanol or carbon dioxide; add 10mL of mixed acid; cover it to stand for 1h or stay overnight; place it on the adjustable temperature- control electric hot plate or electric hot furnace for digestion; if it turns to brown and black; add mixed acid after cooling till the white smoke appears; the digestion solution is colorless and transparent or slightly yellow; cool off; use water to make constant volume to 25mL or 50mL; mix evenly for spare-use; meanwhile do the blank test. 5.2.4 Dry digestion method
Take 0.5g~5g (accurate to 0.001g) of specimen into the crucible; carbonize on the electric furnace with slight fire to smokeless; place into 525??C??25??C muffle furnace for ashing 5h~8h; the cool off. If the ashing is not complete and there are black carbon particles; titrate small amount of nitric acid to moisten after cooling off; after drying on the electric hot plate; transfer into muffle furnace to continue ashing till white ash appears; take out after cooling to the room temperature; dissolve with nitric acid solution; use water to make constant volume to 25mL or 50mL; mix evenly for spare- use; meanwhile do the blank test.
NOTE. dry digestion method is recommended to be used for the infant formula food. 5.3 Instrument reference conditions
Optimize the instrument to the best conditions; major reference conditions. absorption wavelength 279.5nm, slit width 0.2mm, lamp current 9mA, gas flow rate 1.0L/min. 5.4 Drawing of standard curve
Separately inject the standard series working solutions into the atomic absorption spectrometer; measure their absorbance values; draw standard curve with concentration of standard working solution as abscissa, while the absorbance value as ordinate.

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