4-CHLORO 2- AMINO PHENOL (4-CAP)

4-CHLORO 2- AMINO PHENOL (4-CAP)

ParametersSpecification
Cas No. 95-85-2
HPLC99% MIN
Moisture1.00% MAX
Melting Point139 – 141 ºC
Specification of 4-CHLORO 2- AMINO PHENOL (4-CAP) Doc. No. : PCI/FM-SPEC/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 1 of 1
 
Product  : 4-CHLORO 2- AMINO PHENOL (4-CAP)
CAS no. : 95 – 85 – 2
Mol. Wt. : 143.57
Empirical Formula C6H6NOCL
 
SPECIFICATION OF 4-CHLORO 2- AMINO PHENOL
Sr. No. Test Parameters Specification 
1 Appearance White or Off-White crystalline Powder
2 Purity by HPLC 99.0 % Min
3 Melting Point 139 – 141 °C
4 Salt in acetone 0.50 % Max
5 Insoluble 0.050 % Max
6 Moisture by KF 1.00 % Max
 
  STP of 4-CHLORO 2- AMINO PHENOL  (4-CAP) Doc. No. : PCI/FM-STP/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 1 of 5
 
  1. Appearance: Check Visually 
 
  1. Purity by HPLC
Instrument : HPLC with UV Detector
Standard Preparation  : Weigh 50 MG of Standard and dissolve in 30 ML Methanol and put on Ultrasonic bath for 5 mins and make up in 50 ML Volumetric Flask with Methanol.
Sample Preparation  : Weigh 50 MG of Sample and dissolve in 30 ML Methanol and put on Ultrasonic bath for 5 mins and make up in 50 ML Volumetric Flask with Methanol.
Mobile Phase Preparation : Mobile Phase A: 1.0 % W/V O-Phosphoric Acid in HPLC Water Mobile Phase B: 100 % HPLC Grade Methanol 
Injection Volume : 10 Micro Liter
Flow Rate 1.0 ML / Minute
Programming : Gradient 
Time [Mins] Mobile Phase A Mobile Phase B
0 80 % 20 %
30 10 % 90 %
32 10 % 90 %
33 80 % 20 %
41 80 % 20 %
Detector : UV Detector at 230 nm
Run Time : 41 Minutes
Column : Nucleodur C18 ec [250 mm X 4.0 mm, 5 Micron]
Column Temp : 40 °C
Calculation : Calculate Area Percentage
Remarks:  : Retention Time / Relative Retention Time shall be in match with that of the standard 
 
  STP of 4-CHLORO 2- AMINO PHENOL  (4-CAP) Doc. No. : PCI /FM-STP/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 2 of 5
 
  1. Melting Point
Instrument : Melting Point Apparatus
Procedure :
  1. Mix and homogenize the sample.
  2. Small quantity of the substance is inserted in to a capillary tube with one end sealed.
  3. Place the capillary tube and thermometer in to Melting point apparatus. 
  4. Now switch on the melting point apparatus for heating the substance in the capillary. Maintain slow heating rate.
  5. Note the temperature when substance starts to melt. This is the initial melting point.
  6. Further, continue to record the temperature and note the temperature when total substance is melted. This is the final melting point.
  7. The initial and the final melting point constitute the melting point of the substance.
 
  STP of 4-CHLORO 2- AMINO PHENOL  (4-CAP) Doc. No. : PCI/FM-STP/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 3 of 5
 
  1. Salt in Acetone
Reagent : Acetone
Procedure :
  1. Weigh accurately around 5 GM sample in 250 ML Glass Beaker. 
  2. Add 100 ML Acetone to it.
  3. Under stirring by Glass Rod until proper dissolution. 
  4. Weigh the initial weight of Glass Fiber Filter Paper  and note the weight as W1. Filter the solution using Glass Fiber Filter Paper.
  5. Wash the residual on filter paper with 3 X 25 ML Acetone.
  6. Remove the Glass Fiber Filter Paper. 
  7. Initially dry it under atmospheric condition followed by drying in oven at 105 °C. 
  8. Weigh the residual along with the paper and note the weight as W. 
Calculation : % Salt in Acetone          = (W – W1) X 100 Sample Weight 
 
  STP of 4-CHLORO 2- AMINO PHENOL  (4-CAP) Doc. No. : PCI/FM-STP/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 4 of 5
 
  1. Insoluble:
 
Reagent : HCl
Procedure :
  1. Weigh accurately around 24 GM sample in 250 ML Glass Beaker. 
  2. Add 100 ML Water to it.
  3. Mix Proper Under stirring by Glass Rod 
  4. Add 30 ml of Conc. HCL
  5. Under stirring by Glass Rod until proper dissolution.
  6. Weigh the initial weight of Glass Fiber Filter Paper and note the weight as W1. Filter the solution using Glass Fiber Filter Paper.
  7. Wash the residual on filter paper with 3 X 25 ML Water.
  8. Remove the Glass Fiber Filter Paper. 
  9. Drying in oven at 105 °C. 
  10. Weigh the Insoluble along with the paper and note the weight as W. 
  Calculation   :   % Insoluble=   (W – W1) X 100 Sample Weight 
 
  STP of 4-CHLORO 2- AMINO PHENOL  (4-CAP) Doc. No. : PCI/FM-STP/002/00
Effective Date  : 05.04.2022
Revision Date  : 04.04.2024
Page No.                    : 5 of 5
  6. Moisture by KF
Instrument : Karl Fischer Moisture Analyzer
Procedure : Derivation of KF Factor
  1. Ensure enough volume of KF reagent is available in the stock bottle.
  2. Fill the burette with the KF reagent upto the mark.
  3. Add Methanol (KF. grade) in the titration vessel, so that the electrode is dipped well.
  4. Nullify the water of the methanol by addition of KF reagent.The nullifying point would be indicated by the buzzer or light indicator.
  5. Now add only one drop of water by aid of capillary tube. The weight of the water drop added should be known accurately difference.
  6. Again ensure the burette is filled upto the mark. Slowly add the KF reagent until the nullifying point is attained.
  7. Note the volume of the burette reading.Repeat the exercise three time to achieve consistent results.
Calculation of KF Factor : KF FACTOR  = Weight of Water X 1000 
Actual Moisture Derivation 
  1. Follow point number 1 – 5 as given above I derivation of factor.
  2. Add 0.50 GM sample for evaluation in the titration vessel.
  3. Start addition of KF reagent slowly till the nullifying point is achieved.Note the volume of KF reagent consumed.
  4. Calculate the water content of the sample as follow.
Calculation of Moisture Content : Moisture Content: = B. R. X KF   Factor
LIST OF IMPURITY
RETECTION TIME IMPURITY NAME
APPROX  8.9 4 CP
APPROX  19.3 2:5 DCNB
APPROX  21.6 4 CNP

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