标准搜索结果: 'GB/T 14698-2017英文版'
| 标准号码 | 内文 | 价格(元) | 第2步 | 交付天数[PDF] | 标准名称 | 相关标准 |
| GB/T 14698-2017 |
英文版
| 300 |
购买全文
|
现货, 9秒内下载
|
饲料原料显微镜检查方法
|
GBT 14698-2017
|
标准编号: GB/T 14698-2017 (GB/T14698-2017)
中文名称: 饲料原料显微镜检查方法
英文名称: Identification method of feed material by microscopy
行业: 国家标准 (推荐)
中标分类: B46
国际标准分类: 65.120
字数估计: 10,181
发布日期: 2017-09-07
实施日期: 2018-04-01
旧标准 (被替代): GB/T 14698-2002
起草单位: 国家饲料质量监督检验中心(武汉)、新希望六和股份有限公司、广州康瑞德生物技术股份有限公司、湖南正虹科技发展股份有限公司
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/T 14698-2017: 饲料原料显微镜检查方法
GB/T 14698-2017 英文名称: Identification method of feed material by microscopy
ICS 65.120
B46
中华人民共和国国家标准
代替GB/T 14698-2002
1 范围
本标准规定了饲料原料的显微镜检查方法。
本标准适用于饲料原料的显微镜定性检查。
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 6682 分析实验室用水规格和试验方法
GB/T 14699.1 饲料 采样
GB/T 34269-2017 饲料原料显微镜检查图谱
饲料原料目录(中华人民共和国农业部公告 第1773号)
3 原理
在显微镜下观察被检查物质的外观形态、组织结构、细胞形态及染色特征等,比照GB/T 34269-
2017,对其种类和品质进行鉴别和评价。
4 仪器
4.1 体式显微镜:可放大7倍~40倍。
4.2 生物显微镜:可放大40倍~500倍。
4.3 放大镜。
4.4 标准筛:孔径为0.42mm、0.25mm、0.177mm的筛及底盘。
4.5 研钵。
4.6 点滴板:黑色和白色。
4.7 培养皿、载玻片、盖玻片。
4.8 尖头镊子、尖头探针等。
4.9 电热干燥箱、电炉、酒精灯及实验室常用仪器。
5 试剂及溶液
除另有说明,本标准所用的试剂均为分析纯,水为 GB/T 6682规定的三级水。
5.1 四氯化碳。
5.2 石油醚:沸点30℃~60℃。
5.3 丙酮溶液(3+1):3体积的丙酮与1体积的水混合。
5.4 盐酸溶液(1+1):1体积盐酸与1体积的水混合。
5.5 硫酸溶液(1+1):1体积硫酸与1体积的水混合。
5.6 硝酸溶液(1+2.5):1体积硝酸与2.5体积的水混合。
5.7 碘溶液:称取0.75g碘化钾和0.1g碘溶于30mL水中,贮存于棕色瓶内。
5.8 茚三酮溶液5g/L:称取0.5g茚三酮溶解于100mL水中,贮存于棕色瓶内,现用现配。
5.9 硝酸铵溶液:10g硝酸铁溶于100mL水中。
5.10 钼酸盐溶液:20g三氧化钼溶入30mL氨水与50mL水的混合液中,将此液缓慢倒入硝酸溶液
(5.6)中,微热溶解,冷却后与100mL硝酸铵溶液(5.9)混合。
5.11 悬浮剂Ⅰ:称取10g水合氯醛溶解于10mL水中,加入10mL丙三醇,混匀,贮存在棕色瓶中。
5.12 悬浮剂Ⅱ:称取160g水合氯醛溶解于100mL水中,并加入10mL盐酸溶液(5.4)。
5.13 硝酸银溶液:称取10g硝酸银于100mL水中。
5.14 间苯三酚溶液20g/L:称取2g间苯三酚溶解于100mL95%的乙醇中,置于棕色瓶内。
6 比照样品
6.1 饲料原料比照样品
按照《饲料原料目录》中特征描述收集和准备比照样品。
6.2 掺杂物比照样品
搜集稻谷壳粉、木屑、花生壳粉、皮革粉等可能被用于充当掺杂物或掺假物样品。
6.3 杂草种籽
搜集常与谷物混杂的杂草种籽。
7 试样制备
7.1 取样
按GB/T 14699.1采样,抽取有代表性的饲料样品,用四分法缩减取样分取到检查所需量。试样在
常温条件下储于具塞玻璃瓶中或密闭的样品袋内。
7.2 试样前处理
7.2.1 筛分
根据试样粒度情况,选用适当标准筛(4.4),将最大孔径筛置最上面,最小孔径筛置下面,最下面是
筛底盘。将四分法分取的试样置于套筛上充分振摇后,用小勺从每层筛面及筛底各取部分试样,分别平
摊于培养皿中。必要时试样可先经石油醚、丙酮、四氯化碳处理后再筛分(按照7.2.3、7.2.4和7.2.5处理)。
7.2.2 颗粒或团粒试样处理
取数粒于研钵(4.5)中,用研杆碾压使其分散成各组分,但不应将组分本身研碎。初步研磨后过孔
径为0.42mm筛。根据研磨后饲料试样的特征,依照7.2.3、7.2.4和7.2.5进行处理。
7.2.3 石油醚脱脂处理
油脂含量高或粘附有大量细颗粒试样(如:鱼粉、肉骨粉、膨化大豆等饲料原料样品),取约5g试样
置于100mL高型烧杯中,加入50mL石油醚(5.2),搅拌10s,静置沉降,小心倾析出石油醚,待样品表
面石油醚挥发后,置于干燥箱(4.9)中在约70℃开门烘10min或在通风柜内吹干,取出冷却至室温后
将样品置于培养皿(4.7)内待检。
警告---此步骤需在通风的环境或通风柜内操作,注意防爆炸、防燃烧。
7.2.4 丙酮处理
因有糖蜜而形成团块结构或水分偏高模糊不清的试样,可先用此法处理。取约10g试样置
100mL高型烧杯中,加入约70mL丙酮溶液(5.3)搅拌数分钟以溶解糖蜜,静置沉降。小心倾析,用丙
酮溶液(5.3)重复洗涤、沉降、倾析两次。稍挥干后置60℃干燥箱中20min,取出于室温下冷却。
警告:此步骤需在通风的环境或通风柜内操作,注意预防有机溶剂中毒。
7.2.5 四氯化碳浮选处理
取约10g试样置于100mL高型烧杯中,加入约90mL四氯化碳(5.1),搅拌约10s,静止2min~
5min。待上下分层清晰后,将漂浮在上层的物质用勺捞出或采用倾析过滤法分离出,待表面浮选剂挥发
后,置于干燥箱(4.9)中在(70±2)℃烘10min~20min,取出冷却至室温后将样品置于培养皿(4.7)内
10min~20min,取出冷却至室温后将样品置于培养皿(4.7)内待检。必要时可将漂浮物、沉淀物过筛。
警告:此步骤需在通风的环境或通风柜内操作,注意预防有机溶剂中毒。
8 检查步骤
8.1 感官检验
将50g~100g试样摊放于白纸上,在充足的自然光下对试样进行感官检查,检查者以视觉、触觉
直接检查试样。
仔细识别试样标示物质的特征,检查有无掺杂物、热损伤、虫蚀、活昆虫、杂草种子及霉变等情况,手
捻试样感觉其硬度大小及其是否含有裹杂物。
必要时用比照样品在相同条件下进行对比。对可疑物可利用放大镜(4.3)进行辨认。
将上述摊有试样的培养皿置体式显微镜(4.1)下观察,光源可采用充足的散射自然光或用阅读台灯
(要注意用比照样品在同一光源下对比观察),用台灯时入照光与试样平面以45°角为好。
立体显微镜上载台的衬板选择要考虑试样色泽,一般检查深色颗粒时用白色衬板;查浅色颗粒时用
黑色衬板。检查一个试样可先用白色衬板看一遍,再用黑色衬板看。
检查时先看粗颗粒,再看细颗粒。先用较低放大倍数,再用较高放大倍数。
观察时用尖镊子拨动、翻转,并用探针触探试样颗粒。系统地检查培养皿中的每一组分。
为便于观察可对试样进行茚三酮试验(9.2.6)、间苯三酚试验(9.2.7)、碘试验(9.2.8)等。在检查过
程中以比照样品在相同条件下,与被检试样进行对比观察,或参照GB/T 34269进行对比观察。
记录观察到的各种成分,对不是试样所标示的物质,若量小称为杂质,若量大,则称为掺杂物。应特
8.3 生物显微镜检查
将体式显微镜下不能确切鉴定的试样颗粒及试样制备时筛面上及筛底盘中的试样分别取少许,置
于载玻片(4.7)上,加两滴悬浮液Ⅰ(5.11),用探针(4.8)搅拌分散,浸透均匀,加盖玻片,在生物显微镜
(4.2)下观察,先在较低倍数镜下搜索观察,然后对各目标进一步加大倍数观察。与比照样品进行比较。
取下载玻片(4.7),揭开盖玻片,加一滴碘溶液(5.7),搅匀,再加盖玻片,置镜下观察。此时淀粉被染成
蓝色到黑色,酵母及其他蛋白质细胞呈黄色至棕色。如试样粒透明度低不易观察时,可取少量试样,加
入约5mL悬浮液Ⅱ(5.12),煮沸1min,冷却,取1~2滴底部沉淀物置载玻片(4.7)上,加盖玻片镜检。
9 鉴别方法和鉴别实验
9.1 主要无机组分的鉴别
上筛分,将筛出的四部分分别置于培养皿中,用体式显微镜检查,动物和鱼类的骨、鱼鳞、软体动物的外
壳一般是易于识别的。盐通常呈立方体;石灰石中的方解石呈菱形六面体。
9.2 鉴别试验
9.2.1 观察方式
鉴别试验可用肉眼或体式显微镜观察。
9.2.2 硝酸银试验
夹取未知可疑物颗粒2~5粒置于点滴板(4.6)上,滴加2滴硝酸银溶液(5.13),观察现象:
---如果生成白色晶体,并慢慢变大,说明未知颗粒是氯化物;
---如果生成黄色结晶,并生成黄色针状,说明未知颗粒为磷酸盐;
---如果颗粒慢慢变暗,说明未知颗粒是骨。
9.2.3 盐酸试验
夹取未知可疑物颗粒2~5粒置于点滴板(4.6)上,滴加2滴盐酸溶液(5.4),或夹取可疑物3~5粒
置于50mL烧杯中加入5mL盐酸溶液(5.4),观察现象:
---如果剧烈起泡,说明未知可疑颗粒为碳酸盐;
---如果慢慢起泡或不起泡,则该试样还应进行钼酸盐试验(9.2.4)和硫酸试验(9.2.5)。
9.2.4 钼酸盐试验
夹取未知可疑物颗粒2~5粒置于点滴板(4.6)上,滴加2滴钼酸盐溶液(5.10),观察现象。如果在
接近未知可疑颗粒的地方生成微小黄色结晶,说明未知可疑颗粒为磷酸盐、磷矿石或骨(所有磷酸盐均
9.2.5 硫酸试验
夹取未知可疑物颗粒2~5粒置于点滴板(4.6)上,滴加2滴盐酸溶液(5.4)后,再滴入2滴硫酸溶液
(5.5),如慢慢形成细长的白色针状物,说明未知可疑物颗粒为钙盐。
9.2.6 茚三酮试验
夹取未知可疑物颗粒2~5粒置于50mL烧杯内,滴加5~7滴茚三酮溶液(5.8)浸润未知可疑颗
粒,水浴加热到(80±5)℃,如未知颗粒显蓝紫色,说明未知可疑物颗粒含蛋白质。
9.2.7 间苯三酚试验
取试样1g~2g于50mL烧杯内,滴加10~20滴间苯三酚溶液(5.14)浸润样品,放置5min,滴加
5~10滴盐酸溶液(5.4),若呈深红色,则试样中含有木质素。
夹取未知可疑物颗粒2~5粒置于点滴板(4.6)上,滴加2滴碘溶液(5.7)到可疑物颗粒上,如呈蓝紫
色,则可疑物含有淀粉;也可取样品5g~10g置于100mL烧杯中,加入80mL水,电炉(4.9)上煮沸后
取下,静止2min后滴加5mL碘溶液(5.7),若溶液变呈蓝或蓝紫色,则样品中含淀粉类物质。
10 结果表示
结果表示应包括试样的外观、色泽及显微镜下所见到的物质,并给出所检试样是否与送检名称相符合的判定意见。
GB/T 14698-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
B 46
Replacing GB/T 14698-2002
Identification method of feed material by microscopy
ISSUED ON. SEPTEMBER 07, 2017
IMPLEMENTED ON. APRIL 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine 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 Normative references ... 4
3 Principles ... 4
4 Instruments ... 4
5 Reagents and solutions ... 5
6 Reference sample ... 6
7 Specimen preparation ... 6
8 Inspection steps ... 8
9 Identification methods and identification experiments ... 9
10 Result expression ... 11
Foreword
This standard was drafted in accordance with the rules given GB/T 1.1-2009.
This standard replaces GB/T 14698-2002 “Identification method of feed
material by microscopy”. As compared with GB/T 14698-2002, the main
technical changes of this standard are as follows.
- DELETE the relevant contents of compound feed from the text (SEE clause
1 of 2002 version);
- ADJUST the standard text structure;
- ADD the petroleum ether degreasing treatment method (SEE clause 7.2.3).
This standard was proposed by AND shall be under the jurisdiction of National
Feed Industry Standardization Technical Committee (SAC/TC 76).
The drafting organizations of this standard. National Feed Quality Supervision
and Inspection Center (Wuhan), New Hope Liuhe Co., Ltd., Guangzhou
Kangruide Biological Technology Co., Ltd., Hunan Zhenghong Technology
Development Co., Ltd.
The main drafters of this standard. Yang Haipeng, Guo Jiyuan, Liu Xianrong,
Yang Lin, Rong Jia, Zhu Zhengpeng, Hu Zhenjun, Wang Hu, Qian Ying, Jiang
Xiaoxia.
This standard replaces the standards previously issued as follows.
- GB/T 14698-1993, GB/T 14698-2002.
Identification method of feed material by microscopy
1 Scope
This standard specifies the identification method of feed material by microscopy.
This standard applies to the qualitative identification of feed material by
microscopy.
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 document.
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
GB/T 14699.1 Feed - Sampling
GB/T 34269-2017 Identification chromatogram of feed material by
microscopy
Feed material directory (Announcement of Ministry of Agriculture of People's
Republic of China No. 1773)
3 Principles
The appearance morphology, organization structure, cell morphology, and
staining characteristics of the substance under inspection are observed under
the microscope, the results are compared with GB/T 34269-2017, to identify
and evaluate its type and quality.
4 Instruments
4.1 Stereo-microscope. magnification can be 7 times ~ 40 times.
4.3 Magnifying glass.
a spoon to take some of specimens from above and below each sieve,
respectively LAY it horizontally in the culture dish. If necessary, the specimen
can be sieved after being treated by petroleum ether, acetone, carbon
tetrachloride (In accordance with clause 7.2.3, 7.2.4 and 7.2.5).
7.2.2 Particle or pellet specimen treatment
TAKE a few grains into a mortar (4.5), USE pestle to grind it to scatter it into
different compositions, BUT do not CRUSH the composition itself. After initial
grinding, MAKE it pass the sieve of bore diameter 0.42 mm. In accordance with
accordance with 7.2.3, 7.2.4 and 7.2.5.
7.2.3 Petroleum ether degreasing treatment
For the specimen of high fat content or attached with a large number of fine
particle samples (such as. fish meal, meat and bone meal, extruded soybean
and other raw materials feed samples), TAKE about 5 g of sample into a 100
mL high beaker, ADD 50 mL of petroleum ether (5.2), STIR it for 10 s, LET it be
standing to allow it to settle, carefully DECANT the petroleum ether, after the
petroleum ether at the sample surface is volatilized, PLACE it into the oven (4.9)
at about 70 °C to bake it for 10 min with the door opened, or PLACE it into a
the sample into the culture dish (4.7) to prepare for inspection.
WARNING - This procedure shall be operated in a ventilated environment
or fume hood, beware of explosion and fire.
7.2.4 Acetone treatment
For the specimen having a lump structure due to molasses OR having high
moisture content and being vague, it can be treated first using this method.
TAKE about 10 g of specimen, PLACE it into a 100 mL high beaker, ADD about
70 mL of acetone solution (5.3), STIR it for a few minutes to dissolve the
molasses, LET it be standing to allow it to settle. Carefully DECANT it, USE the
for two times. After it is slightly evaporated dry, PLACE it into a 60 °C oven for
20 min, TAKE it out, COOL it at room temperature.
WARNING - This procedure shall be operated in a ventilated environment
or fume hood, taking care to prevent organic solvent poisoning.
7.2.5 Carbon tetrachloride flotation treatment
TAKE about 10 g of specimen into a 100 mL high beaker, ADD about 90 mL of
carbon tetrachloride (5.1), STIR it for about 10 s, LET it be standing for 2 min ~
5 min. After the upper and lower layers are clearly separated, USE spoon to
During observation, USE a shape tweezers to toggle and flip, and USE a probe
the culture dish.
To facilitate observation, the ninhydrin test (9.2.6), the phloroglucinol test (9.2.7),
the iodine test (9.2.8) and the like may be performed on the specimen. During
the inspection process, MAKE comparison observation between the reference
sample and the specimen under inspection at the same conditions, or otherwise
MAKE reference to GB/T 34269 to perform comparative observation.
RECORD the various components observed, for the substance which is not
indicated by the specimen, if it is in small amount, it is called impurity, if it is in
large amount, it is called dopant. It shall pay special attention to hazardous
8.3 Biological microscopy
Specimen particles and specimen that cannot be accurately identified under a
stereomicroscope, respectively TAKE a small amount of specimen from above
the sieve and from the sieve base plate, PLACE it on the slide glass (4.7), ADD
two drops of a suspending agent I (5.11), USE the probe (4.8) to stir it to scatter
it, MAKE it uniformly soaked, USE a glass slide to cover it. Stir and disperse
with the probe (4.8), soaked and covered with a glass slip. MAKE observation
under a biological microscope (4.2), MAKE searching observation under a
lower magnification microscope first, then INCREASE the observation
TAKE off the glass slide (4.7), LIFT up the cover slip, ADD one drop of iodine
solution (5.7), STIR it uniformly, ADD the glass slip again, PLACE it under
microscope for observation. At this time, the starch is dyed blue to black, yeast
and other protein cells are yellow to brown. If sample transparency is too low to
be observed easily, it may take a small amount of specimen, ADD about 5 mL
of suspending agent II (5.12), MAKE it boiling for 1 min, COOL it down, TAKE
1 ~ 2 drops of bottom sediment...
|