Library Preparation for Contact and Non-Contact Parts

We, Confianca Pharmazon (Confianca Technologies LLP) have developed lab at Ahmedabad for Library Preparation.

Library Preparation :-

We do Gemba along with client (optional) to identify the product contact and non-contact parts. Based on identification of these parts, coupons shall be collected from clients. Further Analysis of these coupons shall be done at lab using 4 different technologies :- SEM with EDS, FTIR, TGA/STA and Microscopic Analysis.

 

LIST OF MATERIALS USED FOR CHARACTERIZATION

Sr. No.	Name of Material
1	PP Container
2	Hypalon Gloves for API Addition
3	TC Clamp of Pressure Vessel
4	Teflon Bush of Hydraulic cylinder
5	Product Filter
6	Gasket (Manual Valve)
7	Gasket of Pressure Vessel
8	2ml Syringe for addition of glacial Acetic acid solution in PP Container
9	Pharma Pure tubing
10	Measuring Cylinder (for addition of glacial acetic acid Solution)
11	Ceramic
12	Plunger rod with rubber stopper
13	Poly bag for API
14	SS Scoop
15	Glass bottle for Glacial Acetic acid
16	Hypalon gloves for RM dispensing.
17	Glass bottle for WFI collection and Glacial acetic acid solution preparation
18	2.0 Ltr Pressure vessel (Transfer prepared solution of glacial acetic acid)
19	Glass bottle for Filtered Glacial acetic acid.
20	SS scoop for API addition.
21	SS Spatula
22	Glass Beaker for Filtered Glacial Acetic acid solution
23	2 ml Syringe for sampling
24	Hydration Hopper
25	Manual Valve connect to bottom of Hydration hopper to Mixing/Product chamber.
26	TC clamp (Manual valve)
27	Mixing/ Product Chamber
28	Gasket of Hydraulic cylinder (Hydration hopper)
29	TC clamp Hydraulic cylinder (Hydration hopper)
30	Teflon bush of Mixing/ Product chamber.
31	Gasket of Mixing/ Product chamber.
32	TC clamp Mixing/ Product chamber.
33	Teflon bush of Hydraulic cylinder of Mixing/ Product chamber.
34	SS Blind for closer of Mixing/ Product chamber front and back
35	Viscotec pump (Outer body)
36	Rotar of Viscotec pump

Techniques and Instruments used for the Characterization of Library

TECHNIQUE USED	INSTRUMENT USED
Elemental Profiling (By Scanning Electron Microscope with EDS (Energy Dispersive Spectroscopy)	SEM Instrument: Hitachi SU 3800 EDS Detector: Smart EDX
Infrared Spectroscopy (By FTIR Spectroscopy)	FTIR-4X
Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) & Derivative Thermogravimetric Analysis (DTG)	The Hitachi NEXTA STA 200
Microscopic Imaging	Magnus TZM6 stereomicroscope (Sr. No. 25G259)

LIST OF ANNEXURES

(1) Annexure 1 – Elemental Analysis of Target Elements
(1.1) Overview
(1.2) Standard Operating Procedure for Elemental Analysis using SEM with EDS
(1.3) Sample Identification Codes for Elemental Analysis and Elemental Matrix
(1.4) Elemental Profiling Table Showing Percentage Composition of Elements Observed in Different Materials

 

(2) Annexure 2 – Material Fingerprint Profiling through IR Spectroscopy
(2.1) Overview
(2.2) Standard Procedure for IR Analysis using FTIR
(2.3) Sample Identification Codes for IR Data
(2.4) Characteristic IR Peak Data for Different Positions
(2.5) Original IR Data Records

 

3) Annexure 3 – Thermal Characterization by DSC, Thermogravimetric Analysis (TGA), and Derivative Thermogravimetric Analysis (DTG)
(3.1) Introduction
(3.2) Standard Operating Procedure (SOP) for Thermal Characterization by DSC, TGA, and DTG
(3.3) Observation Results

 

(4) Annexure 4 – Microscopic Examination
(4.1) Overview
(4.2) Standard Procedure for Microscopic Examination
(4.3) Sample Identification Codes for Microscopic Data
(4.4) Microscopic Observation Data

 

ANNEXURE:1

7.0 ELEMENTAL ANALYSIS OF TARGET ELEMENTS

(7.1) INTRODUCTION

Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM-EDS) is an advanced analytical technique used for the characterization and elemental identification of particulate matter and contaminants. The technique combines high-resolution imaging capabilities of Scanning Electron Microscopy (SEM) with elemental composition analysis provided by Energy Dispersive Spectroscopy (EDS).

SEM enables detailed examination of particle morphology, including shape, size, texture, and surface characteristics, whereas EDS facilitates identification and semi-quantitative determination of elemental composition through X-ray emission generated from the sample during electron beam interaction.

SEM-EDS is extensively applied in contamination investigations, material characterization, and root cause analysis of particulate matter due to its ability to identify unknown contaminants while preserving the structural integrity of the sample. The technique is particularly useful for differentiating metallic, polymeric, glass, rubber, and extrinsic particulate contaminants encountered during routine manufacturing processes.

 

(7.2) STANDARD OPERATING PROCEDURE FOR ELEMENTAL ANALYSIS BY SEM WITH EDS

Sample Preparation for SEM-EDS Analysis

STEP 1: Sample Preparation

The particulate sample is visually examined and prepared based on its physical state. Liquid and semi-solid samples, where applicable, are dried under controlled temperature conditions (30–40°C) to remove excess moisture before analysis.

STEP 2: Sample Mounting

The selected particulate matter is carefully mounted onto a standard SEM specimen disc (50 mm or 125 mm) using appropriate adhesive tape:

• Carbon tape for solid samples
• Copper tape for liquid or semi-solid samples

The sample is positioned carefully to avoid particle displacement during analysis.

STEP 3: Conductive Coating using Gold (If required)

Non-conductive samples are coated with a thin conductive layer of gold to minimize charging effects during electron beam interaction. The thickness of the conductive coating is selected according to sample characteristics to ensure proper imaging and elemental detection.

STEP 4: Vacuum Generation

The mounted sample is placed inside the SEM chamber. The instrument is operated under vacuum conditions, typically requiring approximately 5 minutes to establish the required vacuum environment before analysis.

STEP 5: Electron Beam and Imaging

The electron beam generated through a tungsten filament source is focused onto the sample surface using condenser and objective lenses. Appropriate imaging conditions are selected depending on the sample type:

Working Distance:

• SEM Imaging: approximately 5 mm
• EDS Analysis: approximately 10 mm

Accelerating Voltage:

• Solid Samples: 5–30 kV
• Liquid/Semi-solid Samples: 3–15 kV

Multiple microscopic images are captured at suitable magnifications to evaluate particle morphology, surface characteristics, and contamination features.

STEP 6: Elemental Analysis by EDS

The targeted particulate region is subjected to EDS analysis to identify elemental composition. The emitted X-ray spectra are analyzed to determine:

• Element identification
• Elemental percentage composition
• Material purity assessment
• Characteristic spectral peaks of detected elements

Multiple scans may be performed to improve data reliability and reproducibility.

STEP 7: Data Evaluation

The obtained SEM images and EDS elemental profiles are reviewed and interpreted to support contaminant identification, material differentiation, and contamination source investigation.

Example of SEM with EDS data of Sample Id. Exp-001.

Example of Electron Image of Sample Id . Exp-001: Site 1