GB 5009.90-2016_English: PDF (GB5009.90-2016)
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| GB 5009.90-2016 | English | 70 |
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National Food Safety Standard -- Determination of Iron in Foods
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GB 5009.90-2016
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| GB/T 5009.90-2003 | English | 70 |
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Determination of iron, magnesium and manganese in foods
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GB/T 5009.90-2003
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| Standard ID | GB 5009.90-2016 (GB5009.90-2016) | | Description (Translated English) | National Food Safety Standard -- Determination of Iron in Foods | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 8,893 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Older Standard (superseded by this standard) | GB/T 14609-2008 Partial; GB/T 23375-2009 Partial; GB/T 5009.90-2003 Partial; GB/T 9695.3-2009 Partial; GB/T 18932.12-2002 Partial; GB 5413.21-2010 Partial; NY/T 1201-2006 Partial | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 | | Standard ID | GB/T 5009.90-2003 (GB/T5009.90-2003) | | Description (Translated English) | Determination of iron, magnesium and mangnese in foods | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.040 | | Word Count Estimation | 5,576 | | Date of Issue | 2003-08-11 | | Date of Implementation | 2004-01-01 | | Older Standard (superseded by this standard) | GB/T 12396-1990 | | Drafting Organization | Chinese Academy of Preventive Medicine, Institute of Nutrition and Food Hygiene | | Administrative Organization | People's Republic of China Ministry of Health | | Proposing organization | Ministry of Health of the People Republic of China | | Issuing agency(ies) | People Republic of China Ministry of Health China National Standardization Management Committee | | Summary | This standard specifies: by atomic absorption spectrophotometry food in iron, magnesium and manganese. This standard applies to: all kinds of food in iron, magnesium and manganese determination. The detection limit of this method |
GB 5009.90-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of iron in foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the PRC;
State Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principles ... 4
3 Reagents and materials ... 4
4 Instrument and equipment ... 5
5 Analytical procedures ... 6
6 Analysis results expression ... 8
7 Precision... 9
8 Others ... 9
Appendix A Microwave digestion temperature-rise program ... 10
Appendix B Reference conditions of flame atomic absorption spectrometry . 11
Foreword
This standard replaces methods for the determination of iron content in 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 child"; GB/T 23375-2009 “Determination of copper, iron, zinc,
calcium, magnesium and phosphorus content in vegetables and derived
products”; GB/T 5009.90-2003 “Determination of iron, magnesium and
manganese in foods”; 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 18932.12-2002 “Method for the determination of potassium, sodium,
calcium, magnesium, zinc, iron, copper, manganese, chromium, lead, cadmium
contents in honey - Atomic absorption spectrometry”; GB/T 9695.3-2009 “Meat
and meat products - Determination of iron content”; NY/T 1201-2006
“Determination of copper, iron and zinc content in vegetables and derived
products”.
As compared with GB/T 5009.90-2003, the main changes of this standard are
as follows.
--- Standard name is changed to "National food safety standard -
Determination of iron in foods";
--- Add microwave digestion, pressure tank digestion and dry digestion;
--- Add the inductively coupled plasma emission spectrometry;
--- Add the inductively coupled plasma mass spectrometry;
--- Delete spectrophotometry.
National Food Safety Standard -
Determination of iron in foods
1 Scope
This standard specifies the determination of iron content in foods by flame
atomic absorption spectrometry, inductively coupled plasma emission
spectrometry and inductively coupled plasma mass spectrometry.
This standard applies to the determination of iron content in foods.
Method I. Flame atomic absorption spectrometry
2 Principles
After digestion, the sample is atomized by atomic absorption and the
absorbance value is measured at 248.3 nm. Within a certain concentration
range, iron absorbance value is directly proportional to iron content; compares
with the standard series for quantitation.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are guaranteed
reagent, the water is the grade-2 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Perchloric acid (HClO4).
3.1.3 Sulfuric acid (H2SO4).
3.2 Reagent preparation
3.2.1 Nitric acid solution (5+95). MEASURE 50 mL of nitric acid; POUR into
950mL of water; MIX it uniformly.
3.2.2 Nitric acid solution (1+1). MEASURE 250 mL of nitric acid; POUR into 250
mL of water; MIX it uniformly.
5.2.2 Microwave digestion
Accurately WEIGH 0.2 g ~ 0.8 g of solid sample (accurate to 0.001 g) or
accurately MOVE 1.00 mL ~ 3.00 mL of liquid sample into microwave digestion
tank; ADD 5mL of nitric acid; DIGEST the sample according to the microwave
digestion steps, digestion conditions refer to Table A.1; TAKE out the digestion
tank after cooling; CATCH-acid to about 1.0 mL on a hot plate at 140°C ~ 160°C.
After cooling, TRANSFER the digestion juice into a 25 mL volumetric flask; USE
a small amount of water to wash the inner tank and the inner caps for 2~3 times;
COMBINE washing liquid in the volumetric flask; Use water to dilute it to the
mark; MIX it uniformly for spare-use. Meanwhile, DO a sample blank test.
5.2.3 Pressure-tank digestion
Accurately WEIGH 0.3 g ~ 2 g of solid sample (accurate to 0.001 g) or
accurately MOVE 2.00 mL ~ 5.00 mL of liquid sample into digestion inner-tank;
ADD 5 mL of nitric acid; COVER inner-cap; TIGHTEN stainless steel outer-
sheath; PLACE it into constant temperature oven at 140°C ~ 160°C for 4h ~ 5h.
Slowly LOOSEN the outer tank after cooling; TAKE it out and DIGEST the inner
tank; CATCH-acid to about 1.0 mL on adjustable electric hot plate at 140°C ~
160°C. After cooling, TRANSFER the digestion juice into a 25mL volumetric
flask; USE a small amount of water to wash the inner tank and the inner caps
for 2~3 times; COMBINE washing liquid in the volumetric flask; Use water to
dilute it to the mark; MIX it uniformly for spare-use. Meanwhile do a sample
blank test.
5.2.4 Dry digestion
Accurately WEIGH 0.5 g ~ 3 g of solid sample (accurate to 0.001 g) or
accurately MOVE 2.00 mL ~ 5.00 mL of liquid sample into a crucible; HEAT it in
soft fire; CARBONIZE to smokeless; TRANSFER it into a muffle furnace; ASH
at 550°C for 3h ~ 4h. Take out after cooling; for sample that is not completely
ashed, ADD a few drops of nitric acid; HEAT in soft fire; EVAPORATE carefully;
TRANSFER it into a muffle furnace at 550°C; CONTINUE ashing for 1h ~ 2h
until the sample is in white-gray; TAKE out after cooling; DISSOLVE it with
appropriate amount of nitric acid solution (1+1); TRANSFER it into a 25 mL
volumetric flask. USE a small amount of water to wash the inner tank and the
inner caps for 2~3 times; COMBINE washing liquid in the volumetric flask; Use
water to dilute it to the mark. Meanwhile. DO a sample blank test.
5.3 Determination
5.3.1 Instrument’s test conditions
Reference conditions are shown in Table B.1.
......
GB/T 5009.90-2003
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 12396-1990
Determination of iron, magnesium and manganese in foods
ISSUED ON. AUGUST 11, 2003
IMPLEMENTED ON. JANUARY 01, 2004
Issued by. Ministry of Health 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 Principle ... 4
3 Reagents ... 4
4 Instruments ... 5
5 Analysis procedures ... 5
6 Precision ... 7
Foreword
This Standard replaces GB/T 12396-1990.
Compared with GB/T 12396-1990, main changes of this Standard are as follows.
— Changed the Chinese title to be Determination of iron, magnesium and manganese
in foods;
— Changed the structure of previous standard according to GB/T 20001.4-2001 Rules
for drafting standards - Part 4. Methods of chemical analysis.
This Standard was proposed by and shall be under the jurisdiction of the Ministry of Health
(MOH) of the People's Republic of China.
Chief draft organization of this Standard. Nutrition and Food Hygiene Research Institute of
Chinese Institute of Preventive Medicine.
Chief drafters of this Standard. Zhou Xinghan, Men Jianhua and Wang Guangya.
This Standard was issued for the first-time in 1990; this is the first revision.
Determination of iron, magnesium and manganese in foods
1 Scope
This Standard specifies the determination of iron, magnesium and manganese in foods
through atomic absorption spectrophotometric method.
This Standard is applicable to the determination of the iron, magnesium and manganese
in various foods.
The detection limit of this method. 0.2μg/mL for iron, 0.05μg/mL for magnesium, and
0.1μg/mL for manganese.
2 Principle
After the test sample is wet-digested, IMPORT it into the atomic absorption
spectrophotometer; after flame atomization, the iron, magnesium and manganese
respectively ABSORB the 248.3nm, 285.2nm and 279.5nm resonance lines; the
absorbing capacities are proportional to their contents; compare and quantify with the
standard series.
3 Reagents
3.1 Hydrochloric acid.
3.2 Nitric acid.
3.3 Perchloric acid.
3.4 Digestive fluid of mixed acid. nitric acid + perchloric acid = 4+1.
3.5 0.5mol/L nitric acid solution. measure 32mL of nitric acid, then add deionizer water
and dilute it to 1000mL.
3.6 Standard solutions
Iron, magnesium and manganese standard solutions. Accurately weigh 1.0000 g of metal
iron, metal magnesium and metal manganese respectively (purity is larger than 99.99%),
or corresponding oxide that contains 1.0000 g of pure metal. Respectively add nitric acid
to dissolve; transfer them to three 1,000mL volumetric flasks; add 0.5 mol/L nitric acid
solution and dilute to the graduation. Store it in polyethylene bottles at 4°C. Each milliliter
of the three solutions is equivalent to 1 mg of iron, magnesium and manganese
Other experimental conditions. The instrument slit, air and acetylene flow, lamp holder
height and element lamp current etc. shall be adjusted to the optimal state according to
the apparatuses’ instructions.
5.3 Result calculation
Draw standard curve according to standard solution of various concentrations and
corresponding absorbance.
For determination sample solution and reagent blank solution, the concentrations (c and
c0) are found out through the standard curve, then CALCULATE according to Formula (1).
Where.
X - element content in the sample, milligrams per hectogram (mg/100g);
c - concentration of elements in sample solution for determination (found out through
the standard curve), microgram per milliliter (μg/mL);
c0 - concentration of elements in reagent blank solution (found out through the standard
curve), microgram per milliliter (μg/mL);
V - constant volume of the sample, milliliter (mL);
f - dilution ratio;
m - mass of sample, gram (g).
The calculation result reserves two significant digits.
6 Precision
The absolute difference of two independent determination results, under repeatability
conditions, shall not be over 10% of the arithmetic mean.
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