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饲料添加剂 磷酸氢钙
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GB 22549-2017
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标准编号: GB 22549-2017 (GB22549-2017)
中文名称: 饲料添加剂 磷酸氢钙
英文名称: Feed additive -- Dicalcium phosphate
行业: 国家标准
中标分类: B46
国际标准分类: 65.120
字数估计: 10,179
发布日期: 2017-10-14
实施日期: 2018-05-01
起草单位: 中海油天津化工研究设计院、四川省饲料工作总站、四川龙蟒磷化工有限公司、中化云龙有限公司
归口单位: 全国饲料工业标准化技术委员会(SAC/TC 76)
提出机构: 全国饲料工业标准化技术委员会(SAC/TC 76)
发布机构: 中华人民共和国国家质量监督检验检疫总局、中国国家标准化管理委员会
GB 22549-2017: 饲料添加剂 磷酸氢钙
GB 22549-2017 英文名称: Feed additive -- Dicalcium phosphate
1 范围
本标准规定了饲料添加剂磷酸氢钙的要求、试验方法、检验规则以及标签、包装、运输和贮存。
本标准适用于用湿法磷酸按一定的钙磷比生产出的饲料添加剂磷酸氢钙。
2 规范性引用文件
下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件,仅注日期的版本适用于本文
件。凡是不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。
GB/T 601 化学试剂 标准滴定溶液的制备
GB/T 602 化学试剂 杂质测定用标准溶液的制备
GB/T 603 化学试剂 试验方法中所用制剂及制品的制备
GB/T 6003.1-2012 试验筛 技术要求和检验 第1部分:金属丝编织网试验筛
GB/T 6436-2002 饲料中钙的测定
GB/T 6682-2008 分析实验室用水规格和试验方法
GB 10648 饲料标签
GB/T 13079-2006 饲料中总砷的测定
GB/T 13080-2004 饲料中铅的测定 原子吸收光谱法
GB/T 13082-1991 饲料中镉的测定方法
GB/T 13083-2002 饲料中氟的测定 离子选择电极法
GB/T 13088-2006 饲料中铬的测定
GB/T 14699.1 饲料 采样
3 分类
按生产工艺不同分成Ⅰ型、Ⅱ型和Ⅲ型。
4 要求
4.1 外观:白色或略带微黄色粉末或颗粒。
4.2 饲料添加剂磷酸氢钙按本标准的试验方法检测应符合表1中的技术要求。
5 试验方法
5.1 警告
本试验方法中使用的部分试剂具有腐蚀性,操作时须小心谨慎 必要时,需在通风橱中进行。如溅
到皮肤上应立即用水冲洗,严重者应立即就医。
5.2 一般规定
本标准所用的试剂和水,在没有注明其他要求时,均指分析纯试剂和蒸馏水或GB/T 6682-2008
中规定的三级水。试验中所用的标准滴定溶液、杂质标准溶液、制剂和制品,在没有注明其他规定时,均
按GB/T 601、GB/T 602、GB/T 603的规定制备。
5.3 感官检验
在充足的自然光下,以目视法判定外观。
5.4 鉴别
5.4.1 试剂和材料
5.4.1.1 冰乙酸。
5.4.1.2 盐酸溶液:1+1。
5.4.1.3 氨水溶液:1+1。
5.4.1.4 草酸铵溶液:100g/L。
5.4.1.5 硝酸银溶液:17g/L。
5.4.2 钙离子的鉴别
取少量试样约0.1g,加5mL冰乙酸溶解,煮沸。冷却后过滤,滤液加5mL草酸铵溶液,产生白色
沉淀。此沉淀在盐酸溶液中溶解。
5.4.3 磷酸根鉴别
取少量试样约0.1g,溶于10mL水中,加1mL硝酸银溶液,生成黄色沉淀,此沉淀溶于过量氨水
溶液,不溶于冰乙酸。
5.5 总磷含量的测定
5.5.1 方法提要
在酸性介质中,试验溶液中的磷酸根全部与加入的喹钼柠酮沉淀剂形成沉淀。通过过滤、烘干、称
量,计算总磷含量。
5.5.2 试剂和材料
5.5.2.1 盐酸溶液:1+1。
5.5.2.2 硝酸溶液:1+1。
5.5.2.3 喹钼柠酮溶液:
a) 称取70g钼酸钠(Na2MoO4·2H2O)溶解于100mL水中;
b) 称取60g柠檬酸(C6H8O7·2H2O)溶解于150mL水中;
c) 在搅拌下将溶液a)倒入溶液b)中;
d) 在100mL水中加入25mL浓硝酸,加5mL喹啉;
e) 将溶液d)倒入溶液c)中,放置12h后,用玻璃砂坩埚过滤,再加入280mL丙酮,用水稀释至
1000mL摇匀,放入聚乙烯瓶中保存。
5.5.3 仪器
5.5.3.1 玻璃砂坩埚:滤板孔径为5μm~15μm。
5.5.3.2 电热恒温干燥箱:温度能控制在180℃±5℃。
5.5.4 分析步骤
5.5.4.1 试验溶液A的制备
称取约1.0g试样,精确至0.0002g,置于100mL烧杯中,加10mL盐酸和少量水,盖上表面皿,
煮沸10min。冷却后移入250mL容量瓶中,用水稀释至刻度,摇匀。此溶液为试验溶液A,用于总磷
和钙含量的测定。
5.5.4.2 空白试验溶液的制备
除不加试样外,其他加入的试剂量与试验溶液的制备完全相同,并与试样同时进行同样处理。
5.5.4.3 测定
用移液管移取20mL试验溶液A和空白试验溶液分别置于250mL烧杯中,加10mL硝酸溶液,
加水至总体积约100mL,加热至微沸,加50mL喹钼柠酮溶液,盖上表面皿,于水浴中加热至杯内物温
度达75℃±5℃,保持30s(加热时不得用明火,加试剂或加热时不能搅拌,以免生成凝块)。冷却至室
温,冷却过程中搅拌3次~4次。用预先在180℃±5℃质量恒定的玻璃砂坩埚抽滤上层清液,用倾析
法洗涤沉淀5次~6次,每次用水约20mL,将沉淀转移至玻璃砂坩埚中,继续用水洗涤3次~4次。将
玻璃砂坩埚置于电热干燥箱中,于180℃±5℃烘45min,取出,置于干燥器中冷却至室温,称量。
用移液管移取25mL试验溶液B,置于100mL容量瓶中,按GB/T 13082-1991中6.3进行测定
并计算。
5.13 铬含量的测定
用移液管移取25mL试验溶液B,置于100mL容量瓶中,按GB/T 13088-2006中3.5.2进行测
定并计算。
5.14 游离水分的测定
5.14.1 仪器
5.14.1.1 玻璃砂坩埚:滤板孔径为5μm~15μm。
5.14.1.2 电热恒温干燥箱:温度能控制在50℃±2℃。
称取约2.0g试样,精确至0.0002g,置于已在50℃±2℃下恒重的玻璃砂坩埚中,加5mL丙酮,
用细玻璃棒搅拌均匀后抽滤,再用丙酮洗涤两次,每次5mL丙酮,将盛试料的玻璃砂坩埚放在通风橱
放置10min,然后置于50℃±2℃电热恒温干燥箱中干燥2h,在干燥器中冷却20min,称量。
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 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,
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
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
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.
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
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
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
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.
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 there is significant difference between the exit-factory inspection
result and the previous type inspection result.
6.5 Determination rules
If there is an index in the inspection result that does not conform to the
requirements of this standard, the re-inspection shall be repeated on the double
that does not meet the requirements of this standard, the entire batch of
products will be unqualified.
7 Labelling, packaging, transport and storage
7.1 Labels
It is performed in accordance with GB 10648.
7.2 Packaging
Packaging materials shall be non-toxic, harmless, and moisture-proof.
7.3 Transport
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