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GB 5413.30-2016

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GB 5413.30-2016 英文版 300 购买 现货,9秒内自动发货PDF,有增值税发票。 食品安全国家标准 乳和乳制品杂质度的测定 有效

   
标准编号: GB 5413.30-2016 (GB5413.30-2016)
中文名称: 食品安全国家标准 乳和乳制品杂质度的测定
英文名称: National food safety standard Determination of impurities in milk and milk products
行业: 国家标准
中标分类: X09
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB 5413.30-2010
标准依据: National Health and Family Planning Commission Notice No.17 of 2016

GB 5413.30-2016
National Food Safety Standard -- Determination of Impurities in Milk and Milk Products
中华人民共和国国家标准
食品安全国家标准
乳和乳制品杂质度的测定
2016-12-23发布
2017-06-23实施
中华人民共和国国家卫生和计划生育委员会
国 家 食 品 药 品 监 督 管 理 总 局 发 布
前言
本标准代替GB 5413.30-2010《食品安全国家标准 乳和乳制品杂质度的测定》。
本标准与GB 5413.30-2010相比,主要变化如下:
---增加了杂质度过滤板技术要求;
---简化了附录A的检验步骤,并将附录中测量杂质损失量修改为测量杂质残留量;
---将附录B中的杂质度参考标准板制作修改为液体乳和乳粉类两种标准板制作方法;
---重新确定了杂质组成成分及颗粒度的大小。
食品安全国家标准
乳和乳制品杂质度的测定
1 范围
本标准规定了乳和乳制品杂质度的测定方法。
本标准适用于生鲜乳、巴氏杀菌乳、灭菌乳、炼乳及乳粉杂质度的测定,不适用于添加影响过滤的物
质及不溶性有色物质的乳和乳制品。
2 原理
生鲜乳、液体乳、用水复原的乳粉类样品经杂质度过滤板过滤,根据残留于杂质度过滤板上直观可
见非白色杂质与杂质度参考标准板比对确定样品杂质的限量。
3 试剂和材料
除非另有说明,本方法所用试剂均为分析纯,水为GB/T 6682规定的三级水。
3.1 杂质度过滤板:直径32mm、质量135mg±15mg、厚度0.8mm~1.0mm的白色棉质板,应符合
附录A的要求。杂质度过滤板按附录A进行检验。
3.2 杂质度参考标准板:杂质度参考标准板的制作方法见附录B。
4 仪器和设备
4.1 天平:感量为0.1g。
4.2 过滤设备:杂质度过滤机或抽滤瓶,可采用正压或负压的方式实现快速过滤(每升水的过滤时间为
10s~15s)。安放杂质度过滤板后的有效过滤直径为28.6mm±0.1mm。
5 分析步骤
5.1 样品溶液的制备
5.1.1 液体乳样品充分混匀后,用量筒量取500mL立即测定。
5.1.2 准确称取62.5g±0.1g乳粉样品于1000mL烧杯中,加入500mL40℃±2℃的水,充分搅拌
溶解后,立即测定。
5.2 测定
将杂质度过滤板放置在过滤设备上,将制备的样品溶液倒入过滤设备的漏斗中,但不得溢出漏斗,
过滤。用水多次洗净烧杯,并将洗液转入漏斗过滤。分次用洗瓶洗净漏斗过滤,滤干后取出杂质度过滤
板,与杂质度标准板比对即得样品杂质度。
6 分析结果的表述
过滤后的杂质度过滤板与杂质度参考标准板比对得出的结果,即为该样品的杂质度。
当杂质度过滤板上的杂质量介于两个级别之间时,应判定为杂质量较多的级别。如出现纤维等外
来异物,判定杂质度超过最大值。
7 精密度
按本标准所述方法对同一样品做两次测定,其结果应一致。
附 录 A
杂质度过滤板的检验
A.1 试剂和材料
A.1.1 试剂
A.1.1.1 无水乙醇(C2H5OH)。
A.1.1.2 甲醛(HCHO)。
A.1.1.3 角豆胶:生化试剂。
A.1.1.4 蔗糖。
A.1.2 试剂配制
A.1.2.1 甲醛溶液(40%):量取40mL甲醛到100mL容量瓶中,用水定容至100mL,过滤备用。
A.1.2.2 角豆胶溶液:称取0.75g±0.01g角豆胶至250mL烧杯中,加2mL无水乙醇润湿,再加
50mL水,充分混合。缓慢加热排除气泡后,煮沸,使角豆胶充分溶解后,冷却。加2mL已过滤的40%
甲醛溶液,混匀后转入100mL容量瓶,用水定容。
A.1.2.3 蔗糖溶液:称取750g±0.1g蔗糖于1000mL烧杯中,加水750mL充分溶解,过滤备用。
A.1.3 材料
杂质:用地面灰土经过恒温干燥箱(100℃±1℃)烘干,用标准筛收集颗粒大小为75μm~106μm
的灰土成分,然后烘干至恒重。
A.2 仪器和设备
A.2.1 天平:感量分别为0.1g和0.1mg。
A.2.2 标准筛。
A.2.3 干燥器:含有效干燥剂。
A.2.4 恒温干燥箱;精度为±1℃。
A.2.5 过滤设备:同4.2。
A.3 检验步骤
A.3.1 杂质溶液制备:称取2.00g±0.001g杂质加入250mL烧杯中,用5mL无水乙醇润湿。加入
46mL角豆胶溶液,再加40mL蔗糖溶液,充分混合后,转入100mL容量瓶加蔗糖溶液定容,充分混
匀。移取10mL(相当于200mg杂质)于1000mL容量瓶中,用水定容,充分混匀。
A.3.2 将杂质度过滤板,放入100℃±1℃恒温干燥箱中烘干至恒重,记录质量N1。
A.3.3 将杂质度过滤板放置在过滤设备上,准确移取60mL(相当于12mg杂质)经过充分混匀的杂质
溶液,过滤,用水洗净移液器,洗液一并过滤,用200mL40℃±2℃的水分多次清洗过滤板,滤干后取
下杂质度过滤板,在100℃±1℃恒温干燥箱中烘干至恒重,记录质量N2。
A.4.1 M=N2-N1,M 应≥10mg。并且用锋利的刀片将杂质度过滤板上表层切下,查看余下部分不
应出现杂质。
A.4.2 每千片检验10片,不足1000片按1000片计。
附 录 B
杂质度参考标准板的制作
B.1 试剂和材料
B.1.1 试剂
B.1.1.1 阿拉伯胶:生化试剂。
B.1.1.2 蔗糖。
B.1.2 试剂配制
B.1.2.1 阿拉伯胶溶液(0.75%):称取1.875g阿拉伯胶于100mL烧杯中,加入20mL水并加热溶解
后,冷却。用水转移至250mL容量瓶并定容,过滤。
B.1.2.2 蔗糖溶液(50%):称取1000g蔗糖于1000mL烧杯中,加入500mL水溶解,用水转移至
2000mL容量瓶并定容,过滤。
B.1.3 材料制备
B.1.3.1 牛粪
B.1.3.1.1 A:用标准筛收集颗粒大小为0.150mm~0.200mm的牛粪,备用。
B.1.3.1.2 B:用标准筛收集颗粒大小为0.125mm~0.150mm的牛粪,备用。
B.1.3.2 焦粉
B.1.3.2.1 D:用标准筛收集颗粒大小为0.300mm~0.450mm的焦粉,备用。
B.1.3.2.2 E:用标准筛收集颗粒大小为0.200mm~0.300mm的焦粉,备用。
B.1.3.2.3 F:用标准筛收集颗粒大小为0.150mm~0.200mm的焦粉,备用。
B.2 仪器和设备
B.2.1 天平:感量分别为0.1g和0.1mg。
B.2.2 标准筛。
B.2.3 过滤设备:同4.2。
B.3 液体乳参考标准杂质板制作步骤
B.3.1.1 分别准确称取500.0mg牛粪A、B、C于3个100mL烧杯中。加水2mL,加阿拉伯胶溶液
23mL,充分混匀后,用蔗糖溶液转入500mL容量瓶中并定容,充分混匀直到杂质均匀分布,得到浓度
为1.0mg/mL的牛粪杂质参考标准液a0、b0、c0。
B.3.1.2 分别吸取牛粪杂质参考标准液a0、b0、c0 各100mL于500mL容量瓶中,用蔗糖溶液稀释并
定容,得浓度为0.2mg/mL的牛粪杂质参考标准中间液a1、b1、c1。
B.3.1.3 分别吸取牛粪杂质参考标准中间液a1、b1、c1 各10mL于100mL容量瓶中,用蔗糖溶液稀释
并定容,得浓度为0.02mg/mL的牛粪杂质参考标准工作液a2、b2、c2。
B.3.2 液体乳参考标准杂质板的制作
B.3.2.1 量取100mL蔗糖溶液,在已放置好杂质度过滤板的过滤设备上过滤,用100mL40℃±2℃
B.3.2.2 准确吸取6.25mL牛粪杂质参考标准工作液c2 于100mL容量瓶中,用蔗糖溶液稀释并定
容,混匀后并在已放置好杂质度过滤板的过滤设备上过滤,用水洗净容量瓶,洗液一并过滤。再用
100mL40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为液体乳中杂质相对含量2mg/8L的杂
质度参考标准板A2。
B.3.2.3 准确吸取12.5mL牛粪杂质参考标准工作液b2 于100mL容量瓶中,用蔗糖溶液稀释并定
容,混匀后并在已放置好杂质度过滤板的过滤设备上过滤,用水洗净容量瓶,洗液一并过滤。再用
100mL40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为液体乳中杂质相对含量4mg/8L的杂
质度参考标准板A3。
B.3.2.4 准确吸取18.75mL牛粪杂质参考标准工作液a2 于100mL容量瓶中,用蔗糖溶液稀释并定
100mL40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为液体乳中杂质相对含量6mg/8L的杂
质度参考标准板A4。
B.3.3 以500mL液体乳为取样量,按表B.1液体乳杂质度参考标准板比对表中制得的液体乳杂质度
参考标准板见图B.1。
表B.1 液体乳杂质度参考标准板比对表
参考标准板号 A1 A2 A3 A4
杂质液浓度/(mg/mL) 0 0.02 0.02 0.02
取杂质液体积/mL 0 6.25 12.5 18.75
杂质绝对含量/(mg/500mL) 0 0.125 0.250 0.375
图B.1 液体乳杂质度参考标准板
B.4 乳粉杂质度参考标准板制作步骤
B.4.1 乳粉杂质参考标准液的配制
B.4.1.1 分别准确称取500.0mg焦粉D、E、F于3个100mL烧杯中。加水2mL,加阿拉伯胶溶液
23mL,充分混匀后,用蔗糖溶液转入500mL容量瓶中并定容,充分混匀直到杂质均匀分布,得到浓度
为1.0mg/mL的焦粉杂质参考标准液d0、e0、f0。
B.4.1.2 分别吸取焦粉杂质参考标准液d0、e0、f0 各100mL于500mL容量瓶中,用蔗糖溶液稀释并定
容,得到浓度为0.2mg/mL的焦粉杂质参考标准工作液d1、e1、f1。
B.4.2 乳粉参考标准杂质板的制作
混匀后并在已放置好杂质度过滤板的过滤设备上过滤,用水洗净容量瓶,洗液一并过滤。再用100mL
40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为乳粉中杂质相对含量8mg/kg的杂质度参考标
准板B1。
B.4.2.2 准确吸取3.75mL焦粉杂质参考标准工作液e1 于100mL容量瓶中,用蔗糖溶液稀释并定
容,混匀后并在已放置好杂质度过滤板的过滤设备上过滤,用水洗净容量瓶,洗液一并过滤。再用
100mL40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为乳粉中杂质相对含量12mg/kg的杂质
度参考标准板B2。
B.4.2.3 准确吸取5mL焦粉杂质参考标准工作液d1 于100mL容量瓶中,用蔗糖溶液稀释并定容,混
匀后并在已放置好杂质度过滤板的过滤设备上过滤,用水洗净容量瓶,洗液一并过滤。再用100mL
准板B3。
B.4.2.4 准确吸取3.75mL焦粉杂质参考标准工作液d1 和2.5mL焦粉杂质参考标准工作液e1 于
100mL容量瓶中,用蔗糖溶液稀释并定容,混匀后并在已放置好杂质度过滤板的过滤设备上过滤,用
水洗净容量瓶,洗液一并过滤。再用100mL40℃±2℃的水分多次清洗过滤板,晾干,此杂质板为乳
粉中杂质相对含量20mg/kg的杂质度参考标准板B4。
B.4.3 以62.5g乳粉为取样量,按表B.2乳粉杂质度参考标准板比对表中制得的乳粉杂质度参考标准
板见图B.2。
表B.2 乳粉杂质度参考标准板比对表
参考标准板号 B1 B2 B3 B4
取杂质液体积/mL 2.5 3.75 5.0 6.25
杂质绝对含量/(mg/62.5g) 0.500 0.750 1.000 1.250
杂质相对含量/(mg/kg) 8 12 16 20
图B.2 乳粉杂质度参考标准板

GB 5413.30-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Impurities in Milk and Milk Products
食品安全国家标准
乳和乳制品杂质度的测定
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China;
China Food and Drug Administration.
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Table of Contents
Foreword ... 3 
1 Application Scope ... 4 
2 Principle ... 4 
3 Reagents and Materials ... 4 
4 Apparatus ... 4 
5 Analytical Procedures ... 5 
6 Expression of Analytical Results ... 5 
7 Accuracy ... 5 
Annex A (Normative) Testing of Impurities Filter Plate ... 6 
Annex B (Normative) Preparation of Impurities Reference Standard Plate ... 8 
Foreword
This Standard replaces GB 5413.30-2010, National Food Safety Standard –
Determination of Impurities in Milk and Milk Products.
Compared with GB 5413.30-2010, the major changes of this Standard are as follows.
-- the technical requirements for impurities filter plate are added;
-- the testing procedures in Annex A are simplified and the measurement of
impurities loss is modified into the measurement of impurities residuals in the
Annex;
-- the preparation of impurities reference standard plate is modified into the methods
for the preparation of two standard plates for liquid milk and milk powder;
-- the constituents and particle size of impurities are redefined.
National Food Safety Standard -
Determination of Impurities in Milk and Milk Products
1 Application Scope
This Standard specifies the method for the determination of impurities in milk and milk
products.
This Standard applies to the determination of impurities in fresh and raw milk,
pasteurized milk, sterilized milk, condensed milk and milk powder; it does not apply to
the determination of impurities in milk and milk products added with substances which
decrease the efficiency of filter and insoluble coloured matters.
2 Principle
The specimen of fresh and raw milk, liquid milk, water reconstituted milk powder is
filtered through impurities filter plate; the limit of impurities in the specimen is
determined by comparing the visible non-white impurities remaining on the impurities
filter plate with the impurities reference standard plate.
3 Reagents and Materials
Unless stated otherwise, the reagents used in this Method are analytically pure and
the water is grade-3 water as specified in GB/T 6682.
3.1 Impurities filter plate. white cotton plate of diameter 32 mm, mass 135 mg ± 15
mg and thickness 0.8 mm ~ 1.0 mm, which shall be as specified in Annex A. Impurities
filter plate shall be tested in accordance with Annex A.
3.2 Impurities reference standard plate. see Annex B for the method for the
preparation of impurities reference standard plate.
4 Apparatus
4.1 Balance. sensitivity 0.1 g.
4.2 Filter equipment. impurities filter machine or suction flask, which is capable of
achieving rapid filter by positive pressure or negative pressure (the filter time of each
litre of water is 10 s ~ 15 s). The effective filter diameter after mounting impurities filter
plate is 28.6 mm ± 0.1 mm.
B.1.3.2.3 F. use a standard screen to collect coke powder of particle size 0.150 mm
~ 0.200 mm as standby.
B.2 Apparatus
B.2.2 Standard screen.
B.2.3 Filter equipment. as in 4.2.
B.3 Procedures for preparing liquid milk reference standard impurities plate
B.3.1 Preparation of liquid milk impurities reference standard solution
B.3.1.1 Weigh accurately 500.0 mg of cow dung to place into three 100-mL beakers,
namely A, B and C. Add 2 mL of water, add 23 mL of Arabic gum solution, use sucrose
solution to transfer to a 500-mL volumetric flask after mixing up and add dropwise to
the scale, fully mix up until the impurities distributes uniformly, and obtain the cow dung
impurities reference standard solutions of concentration 1.0 mg/mL, namely a0, b0 and
B.3.1.2 Absorb respectively 100 mL of cow dung impurities reference standard
solutions a0, b0 and c0 to pour into 500-mL volumetric flasks, use sucrose solution to
dilute and add dropwise to the scale, and obtain the cow dung impurities reference
standard intermediate solutions of concentration 0.2 mg/mL, namely a1, b1 and c1.
B.3.1.3 Absorb respectively 10 mL of cow dung impurities reference standard
intermediate solutions a1, b1 and c1 to pour into 100-mL volumetric flasks, use sucrose
solution to dilute and add dropwise to the scale, and obtain the cow dung impurities
reference standard working solutions of concentration 0.02 mg/mL, namely a2, b2 and
c2.
B.3.2.1 Measure 100 mL of sucrose solution, filter on the filter equipment where the
impurities filter plate is mounted, use 100 mL of water of 40°C ± 2°C to wash the filter
plate for several times and dry by airing. Then the impurities plate is the impurities
reference standard plate A1 for the impurities’ relative content in the liquid milk 0 mg/kg.
B.3.2.2 Absorb accurately 6.25 mL of cow dung impurities reference standard
working solution c2 to pour into a 100-mL volumetric flask, use sucrose solution to dilute
and add dropwise to the scale, filter on the filter equipment where the impurities filter
plate is mounted after mixing up, use water to wash the volumetric flask, and filter the
washings together. Then use 100 mL of water of 40°C ± 2°C to wash the filter plate for
standard plate A2 for the impurities’ relative content in the liquid milk 2 mg/8 L.
B.3.2.3 Absorb accurately 12.5 mL cow dung impurities reference standard working
mg/mL, namely d0, e0 and f0.
B.4.1.2 Absorb 100 mL of the coke powder impurities reference standard solutions
d0, e0 and f0 to pour into 500-mL volumetric flasks respectively, use sucrose solution to
dilute and add dropwise to the scale and obtain the coke powder reference standard
working solutions of concentration 0.2 mg/mL, namely d1, e1 and f1.
B.4.2 Preparation of milk powder reference standard impurities plates
B.4.2.1 Absorb accurately 2.5 mL of the coke powder impurities reference standard
and add dropwise to the scale, filter on the filter equipment where the impurities filter
plate is mounted after mixing up, use water to wash the volumetric flask, and filter the
washings together. Then use 100 mL of water of 40°C ± 2°C to wash the filter plate for
several times, and dry by airing. The impurities plate is the impurities reference
standard plate B1 for the impurities’ relative content in milk powder 8 mg/kg.
B.4.2.2 Absorb accurately 3.75 mL of the coke powder impurities reference standard
working solution e1 to pour into a 100-mL volumetric flask, use sucrose solution to
dilute and add dropwise to the scale, filter on the filter equipment where the impurities
filter plate is mounted after mixing up, use water to wash the volumetric flask, and filter
for several times, and dry by airing. The impurities plate is the impurities reference
standard plate B2 for the impurities’ relative content in milk powder 12 mg/kg.
B.4.2.3 Absorb accurately 5 mL of the coke powder impurities reference standard
working solution d1 to pour into a 100-mL volumetric flask, use sucrose solution to
dilute and add dropwise to the scale, filter on the filter equipment where the impurities
filter plate is mounted after mixing up, use water to wash the volumetric flask, and filter
the washings together. Then use 100 mL of water of 40°C ± 2°C to wash the filter plate
for several times, and dry by airing. The impurities plate is the impurities reference
standard plate B3 for the impurities’ relative content in milk powder 16 mg/kg.
working solution d1 and 2.5 mL of the coke powder impurities reference standard
working solution e1 to pour into a 100-mL volumetric flask, use sucrose solution to
dilute and add dropwise to the scale, filter on the filter equipment where the impurities
filter plate is mounted after mixing up, use water to wash the volumetric flask, and filter
the washings together. Then use 100 mL of water of 40°C ± 2°C to wash the filter plate
for several times, and dry by airing. The impurities plate is the impurities reference
standard plate B4 for the impurities’ relative content in milk powder 20 mg/kg.
B.4.3 Use 62.5 g of milk powder as the sampling quantity and see Figure B.2 for the
milk powder impurities reference standard plates prepared in accordance with Table
   
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