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N-氟代双苯磺酰胺质量检测

规格:98%
包装:20kg/桶
最小购量:1
CAS:133745-75-2
分子式:C12H10FN4S2
分子量:293.37

N-氟代双苯磺酰胺
1. 目的 Purpose
建立 N-氟代双苯磺酰胺质量标准,为产品检测提供依据,控制 N-氟代双苯磺酰胺产品质量。
Established a quality standard to control the quality of finished product of
N-Fluorobenzenesulfonimide .
2. 范围 Scope
确定最最终产品 N-氟代双苯磺酰胺质量。
Determine the quality of finished product of N-Fluorobenzenesulfonimide .
3. 参考标准 Ref. Standard
内控标准和客户标准。
In-house and customer specifications
4. 产品信息 Product Information
产品名称 Product Name N-Fluorobenzenesulfonimide
分子式 Molecular Formula C12H10FNO4S2 分子量 Molecular Weight 315.3
CAS 号 CAS NO. 133745-75-2
分子结构 Structure
5. 规格 Specifications
检测项目 Items 规格 Specifications
外观 Appearance White Crystalline Powder
纯度 Purity(HPLC) ≥98%
水分 Content of water(%,K.F.) <0.5%
6. 分析方法 Test Method
6.1. 外观 Appearance
本品为白色结晶性粉末
White Crystalline Powder,by visual.
6.2. 纯度 Purity
6.2.1.仪器 Instrumentation HPLC having DAD detector.
6.2.2. 试剂 Reagent
S.NO Name of the reagent Make Grade
1 H3PO4 - AR
2 ACN Merck or equivalent HPLC
3 Water - Milli Q
6.2.3 方法信息 Method information

Instrument: Agilent HPLC 1260 or equivalent HPLC system
Mobile Phases A: 0.1%H3PO4
Mobile Phases B: ACN
Column: PLUS C18 4.6*250mm 5um or equivalent
Flow: 1.0 mL/min
Oven: 30 °C
Diluent: ACN
Injection volume: 5 μL
Wavelength: 220 nm
Gradient elution:
min A% B% ml/min
0.00 70.0 30.0 1.0
10.00 5.0 95.0 1.0
18.00 5.0 95.0 1.0
18.01 70.0 30.0 1.0
6.2.4 溶液的配制 Solution preparation
标准溶液的配制 Standard preparation
精密称取 30mg 的 N-氟代双苯磺酰胺标准品至于 50ml 的容量瓶中。用乙腈溶解定容。
Weight accurately about 30mg of N-Fluorobenzenesulfonimide standard and transfer
into a 50ml volumetric flask,dissolve in and make up to the mark with the ACN. 样品溶液的配制 Sample preparation
精密称取 30mg 的 N-氟代双苯磺酰胺样品至于 50ml 的容量瓶中。用乙腈溶解定容。
Weight accurately about 30mg of N-Fluorobenzenesulfonimide sample and transfer
into a 50ml volumetric flask,dissolve in and make up to the mark with the ACN
进一针空白(ACN),依次进入标准溶液与样品溶液到液相色谱中。记录色谱图。
Inject a blank(ACN) followed by the standard and sample preparation into the
HPLC chromatograph and record the chromatograms。
扣除样品溶液中的空白峰,按照面积归一化法记录色谱图中 N-氟代双苯磺酰胺。
Disregard the peaks in the chromatogram of sample preparation correspond to that
of blank chromatogram。Record the purity of N-Fluorobenzenesulfonimide .
6.2.5 计算 calculator
计算主峰的相对纯度(面积归一化法)
Calculate the Apparent Purity (Area%) of main component
相对纯度(Apparent Purity)= (As/At)*100%
其中:
AS 代表主峰的峰面积;
AT 代表所有峰的面积和(扣除空白溶剂峰)。
Where:
AS is the peak area of main component;
AT is total peak area (ignore any peaks obtained from blank).
6.3 水分 Water content
平行取本品各约 50mg,精密称定,依法测定(WI-GAM006-01),水分平均值不大于 0.5%。
Accurately weighed approximately 50mg of Sample in duplicate, refer to WI-GAM006-01.
The average result is not more than 0.5%.
7. 取样 Sampling:
每批至少取样 1g,置于密闭容器中,并加贴“待验” 标签;取样 2*1g,置于密闭容器
中,并加贴“留样”标签。
Sample a minimum of about 1g from each batch into self-sealing container marked
with ‘Sample for analysis’ label and 2*1g into self-sealing container marked with ‘Sample for reserve’.
8. 分析用样品量 Quantity of composite sample for analysis:
1g
9. 留样量 Quantity of reserved sample:
2 x 1g
10. 危险性警告 Hazards and precautions, if any. 处理样品应带手套、口罩以及防护眼镜。
Use hand gloves, goggles and nose mask while handling the product.
11. 贮存条件及推荐的包装规格 Storage condition & preferred pack
产品保存于室温、密闭、避光环境。
The product is stable stored at room temperature and in a hermetical, protection
from light.
12. 复验期 Retest Period
12 个月(暂定)
twelfth months (temporary)