N-氟代雙苯磺酰胺
1. 目的 Purpose
建立 N-氟代雙苯磺酰胺質量標準,為產品檢測提供依據,控制 N-氟代雙苯磺酰胺產品質量。
Established a quality standard to control the quality of finished product of
N-Fluorobenzenesulfonimide .
2. 范圍 Scope
確定最最終產品 N-氟代雙苯磺酰胺質量。
Determine the quality of finished product of N-Fluorobenzenesulfonimide .
3. 參考標準 Ref. Standard
內控標準和客戶標準。
In-house and customer specifications
4. 產品信息 Product Information
產品名稱 Product Name N-Fluorobenzenesulfonimide
分子式 Molecular Formula C12H10FNO4S2 分子量 Molecular Weight 315.3
CAS 號 CAS NO. 133745-75-2
分子結構 Structure
5. 規格 Specifications
檢測項目 Items 規格 Specifications
外觀 Appearance White Crystalline Powder
純度 Purity(HPLC) ≥98%
水分 Content of water(%,K.F.) <0.5%
6. 分析方法 Test Method
6.1. 外觀 Appearance
本品為白色結晶性粉末
White Crystalline Powder,by visual.
6.2. 純度 Purity
6.2.1.儀器 Instrumentation HPLC having DAD detector.
6.2.2. 試劑 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
標準溶液的配制 Standard preparation
精密稱取 30mg 的 N-氟代雙苯磺酰胺標準品至于 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. 樣品溶液的配制 Sample preparation
精密稱取 30mg 的 N-氟代雙苯磺酰胺樣品至于 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
進一針空白(ACN),依次進入標準溶液與樣品溶液到液相色譜中。記錄色譜圖。
Inject a blank(ACN) followed by the standard and sample preparation into the
HPLC chromatograph and record the chromatograms。
扣除樣品溶液中的空白峰,按照面積歸一化法記錄色譜圖中 N-氟代雙苯磺酰胺。
Disregard the peaks in the chromatogram of sample preparation correspond to that
of blank chromatogram。Record the purity of N-Fluorobenzenesulfonimide .
6.2.5 計算 calculator
計算主峰的相對純度(面積歸一化法)
Calculate the Apparent Purity (Area%) of main component
相對純度(Apparent Purity)= (As/At)*100%
其中:
AS 代表主峰的峰面積;
AT 代表所有峰的面積和(扣除空白溶劑峰)。
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
平行取本品各約 50mg,精密稱定,依法測定(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. 取樣 Sampling:
每批至少取樣 1g,置于密閉容器中,并加貼“待驗” 標簽;取樣 2*1g,置于密閉容器
中,并加貼“留樣”標簽。
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. 分析用樣品量 Quantity of composite sample for analysis:
1g
9. 留樣量 Quantity of reserved sample:
2 x 1g
10. 危險性警告 Hazards and precautions, if any. 處理樣品應帶手套、口罩以及防護眼鏡。
Use hand gloves, goggles and nose mask while handling the product.
11. 貯存條件及推薦的包裝規格 Storage condition & preferred pack
產品保存于室溫、密閉、避光環境。
The product is stable stored at room temperature and in a hermetical, protection
from light.
12. 復驗期 Retest Period
12 個月(暫定)
twelfth months (temporary)