GB 22549-2017 English PDF (GB22549-2017)

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GB 22549-2017: Feed additive -- Dicalcium phosphate
GB 22549-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
B 46
Replacing GB/T 22549-2008
Feed additive - Dicalcium phosphate
饲料添加剂 磷酸氢钙
ISSUED ON. OCTOBER 14, 2017
IMPLEMENTED ON. MAY 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword . 3 
1 Scope .. 4 
2 Normative references . 4 
3 Classification .. 5 
4 Requirements . 5 
5 Test methods .. 5 
6 Inspection rules .. 13 
7 Labelling, packaging, transport and storage .. 14 
8 Shelf life. 15 
Foreword
Chapters 1, 4 and 6 of this standard are mandatory; the rest are
recommended.
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 22549-2008 “Feed additive - Dicalcium
phosphate”.
As compared with GB/T 22549-2008, the main technical changes except
editorial modification are as follows.
- MODIFY arsenic index parameters from 0.003% to 20 mg/kg (SEE 4.2; 5.2
of 2008 version);
- DELETE dithizone spectrophotometric method in the determination of lead
content (6.11.2 of 2008 version);
- ADD the chromium content index parameters and test methods (SEE 4.2,
5.13);
- ADD free water index parameters and test methods (SEE 4.2, 5.15).
This standard was proposed and shall be under the jurisdiction of the National
Feed Industry Standardization Technical Committee (SAC/TC 76).
Responsible drafting organizations of this standard. CNOOC Tianjin Chemical
Research Design Institute, Sichuan Feed Work Station, Sichuan Longmang
Phosphorus Chemical Co., Ltd., Sinochem Yunlong Co., Ltd.
Participating drafting organizations of this standard. Yunnan Xinlong Mineral
Feed Co., Ltd.
The main drafters of this standard. Li Guangming, Bai Fan, Fan Xianguo, Luo
Xianming, Ma Xianlin, Yang Yinggao, Wang Yonghong.
This Standard replaces the standard previously issued as follows.
- GB/T 22549-2008.
Feed additive - Dicalcium phosphate
1 Scope
This standard specifies the requirements, test methods, inspection rules, and
labeling, packaging, transportation, and storage of feed additive dicalcium
phosphate.
This standard applies to the feed additive dicalcium phosphate which is
produced by the wet-process phosphoric acid in accordance with a certain
calcium-phosphorus ratio.
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 601 Chemical reagent - Preparations of standard volumetric solutions
GB/T 602 Chemical reagent - Preparations of standard solutions for impurity
GB/T 603 Chemical reagent - Preparations of reagent solutions for use in
test methods
GB/T 6003.1-2012 Test sieves - Technical requirements and testing - Part 1.
Test sieves of metal wire cloth
GB/T 6436-2002 Determination of calcium in feed
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
GB 10648 Feed label
GB/T 13079-2006 Determination of total arsenic in feeds
GB/T 13080-2004 Determination of lead in feeds - Method using atomic
absorption spectrometry
GB/T 13082-1991 Method for determination of cadmium in feeds
GB/T 13083-2002 Determination of fluorine in feed - Ion selective electrode
quimociac precipitant form precipitates. Through the filtration, drying, weighing,
the total phosphorus content is calculated.
5.5.2 Reagents and materials
5.5.2.1 Hydrochloric acid solution. 1+1.
5.5.2.2 Nitric acid solution. 1+1.
5.5.2.3 Quimociac solution.
a) WEIGH 70 g of sodium molybdate (Na2MoO4•2H2O), DISSOLVE it in 100
mL of water;
b) WEIGH 60 g of citric acid (C6H8O7•2H2O), DISSOLVE it in 150 mL of water;
c) POUR the solution a) into solution b) whilst stirring it;
d) ADD 25 mL of concentrated nitric acid in 100 mL of water, ADD 5 mL of
quinoline;
e) POUR solution d) into solution c). After standing for 12 hours, USE glass
grit crucible, ADD 280 mL of acetone, USE water to dilute it to 1000 mL,
SHAKE it uniformly, PLACE it in a polyethylene bottle for preservation.
5.5.3 Instruments
5.5.3.1 Glass grit crucible. filter plate aperture is 5 μm ~ 15 μm.
5.5.3.2 Electric thermostatic oven. The temperature can be controlled at 180 °C
± 5 °C.
5.5.4 Analytical procedures
5.5.4.1 Preparation of test solution A
WEIGH about 1.0 g of specimen, accurate to 0.0002 g, PLACE in a 100 mL
beaker, ADD 10 mL of hydrochloric acid and a small amount of water, COVER
a watch glass, BOIL it for 10 min. After cooling, TRANSFER it into a 250 mL
volumetric flask, USE water to dilute it to the mark, SHAKE it uniformly. This
solution is the test solution A, which is used for the determination of total
phosphorus and calcium content.
5.5.4.2 Preparation of blank test solution
Except that there is no specimen added, the reagent amount added are
completely same as that for the preparation of test solution, it is subject to the
same processing as that of the specimen simultaneously.
5.9.2 Reagents
Same as in chapter 4 of GB/T 13083-2002.
5.9.3 Instruments
Same as Chapter 5 of GB/T 13083-2002.
5.9.4 Analytical procedures
5.9.4.1 Preparation of test solution
WEIGH about 0.5 g ~ 1.00 g of specimen, accurate to 0.0002 g, PLACE it in a
100 mL volumetric flask, ADD 16 mL of hydrochloric acid solution (1+4), ADD
water to dilute it to the mark, SHAKE it uniformly.
5.9.4.2 Determination
PIPETTE 25 mL of test solution, PLACE it in a 50 mL volumetric flask, USE total
ion buffer solution to dilute it to the mark, SHAKE it uniformly. MAKE
determination and calculation in accordance with chapter 7 of GB/T 13083-
2002.
5.10 Determination of arsenic content
5.10.1 Method summary
Same as clause 5.1 of GB/T 13079-2006.
5.10.2 Reagents
Same as clause 5.2 of GB/T 13079-2006.
5.10.3 Instruments
Same as clause 5.3 of GB/T 13079-2006.
5.10.4 Analytical procedure
5.10.4.1 Preparation of test solution B
WEIGH 2.0 g ~ 10.0 g of specimen, accurate to 0.0002 g, ADD 20 mL of
hydrochloric acid solution (1+1), HEAT to dissolve it, after cooling, TRANSFER
it into a 250 mL volumetric flask, ADD water to dilute it to the mark, SHAKE it
uniformly, dry FILTER it. This filtrate is test solution B, which is used for the
determination of arsenic, lead, cadmium and chromium.
5.10.4.2 Determination
6.2 Sampling
Sampling in accordance with the provisions of GB/T 14699.1.
6.3 Exit-factory inspection
In the items listed in Table 1, total phosphorus, soluble phosphorus, water-
soluble phosphorus, calcium, fluorine, free moisture, and fineness are the exit-
factory inspection items.
6.4 Type inspection
The type inspection item is all the requirements of Chapter 4. When the product
is in normal production, type inspection shall be conducted at least once every
six months. However, if one of the following situations occurs, type inspection
shall also be carried out.
a) When the product is finalized;
b) When the production process or source of raw materials has changed
significantly, which may affect product quality;
c) When the production is restored after suspension for more than three
months;
d) When ...